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  • 1995-1999  (777)
  • 1997  (292)
  • 1995  (485)
  • Genetics  (485)
  • Nuclear reactions
  • crystal structure
  • 1
    Electronic Resource
    Electronic Resource
    Preliminary report on the Mount Sinai Hospital Inflammatory Bowel Disease Genetics Project (1997)
    Springer
    Diseases of the colon & rectum 40 (1997), S. 553-557 
    Details
    ISSN: 1530-0358
    Keywords: Inflammatory bowel disease ; Crohn's disease ; Ulcerative colitis ; Genetics ; Family history
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract BACKGROUND: Although the etiology of inflammatory bowel disease (IBD) is unknown, there is increasing evidence that genetic predisposition plays a major etiologic role. To provide the framework for gene identification using a positional cloning approach, ascertainment of families with multiple affected members and careful documentation of pedigrees are essential. Objective: To report the initial findings of the IBD Genetics Project of the Mount Sinai Hospital IBD Research Unit. METHODS: All records of patients with ulcerative colitis and Crohn's disease followed at the Mount Sinai Hospital IBD Unit were reviewed. A questionnaire was sent to all patients to ascertain those with a family history of IBD. Patients with a presumed family history were contacted by a research assistant, and after confirmation of diagnosis, relevant clinical information, pedigrees, and consent to contact family members were obtained. Blood for DNA and cell line preparation were collected from affected and nonaffected family members. RESULTS: Of 2,504 patients registered in the IBD database, 231 (9.2 percent) were found to have an affected family member: 96 of 964 (10 percent) with Crohn's disease (CD) and 135 of 1,540 (8.8 percent) with ulcerative colitis (UC). A mean of 2.4 family members were affected. In families in which the proband had CD, 82.3 percent had only two affected family members, 78.1 percent had only family members affected with CD, and 82.3 percent had only first-degree family members affected. In families in which the proband had UC, 70.4 percent had only two affected family members, 71.1 percent had only family members affected with UC, and 65.2 percent had only first-degree family members affected. In the 231 families, there were 103 sibling pairs: 46 percent with CD, 28 percent with UC, and 26 percent with CD/UC. CONCLUSION: These data suggest that approximately 10 percent of IBD patients have affected family members, with the rate being similar in UC and CD. Future research is directed to genome scanning and linkage analysis in this cohort of patients.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02055377
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of the Isocyanide Ligated Centered Zirconium Halide Cluster [(Zr6Be)Cl12(CNXyl)6] (1997)
    Springer
    Journal of cluster science 8 (1997), S. 521-531 
    Details
    ISSN: 1572-8862
    Keywords: Zirconium clusters ; isocyanide ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The first isocyanide ligated hexanuclear zirconium halide cluster is reported. The unoxidized [(Zr6Be)Cl12(CNXyl)6] (CNXyl = 2,6-dimethylphenyl isocyanide) was obtained from the solid state precursor K3Zr6Cl15Be by dissolution in CH3CN in the presence of CNXyl. The CNXyl ligands occupy all the axial positions on the cluster. The compound was recrystallized from CH2Cl2 and Et2O. [(Zr6Be)Cl12(CNXyl)6].2CH2Cl2 crystallizes in the space group $${\text{P}}\overline {\text{1}} $$ (#2) with a = 12.092(5) Å, b=12.728(5) Å, c = 14.102(8) Å, α = 104.98(4)°, β =107.11°, γ = 100.94°, V = 1919(2) Å3, Z = l, R = 11.3% and R W = 27.0%. For the bound isocyanide ligands, v CN increases to 2140 cm−1.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022605113866
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  • 3
    Electronic Resource
    Electronic Resource
    Reactions of the Dirhenium(II) Complexes Re2 X 4(μ-dppm)2 (X=Cl, Br; dppm=Ph2PCH2PPh2) with Isocyanides. Part XV: A Fifth Structural Isomer of the [Re2Cl3(μ-dppm)2(CO)(CNXyl)2]+ Cation (Xyl = 2, 6-Dimethylphenyl) (1997)
    Springer
    Journal of cluster science 8 (1997), S. 547-551 
    Details
    ISSN: 1572-8862
    Keywords: Rhenium ; dirhenium complexes ; rhenium–rhenium multiple bonds ; isocyanide ligands ; carbonyl ligand ; structural isomers ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of the unsymmetrical, coordinatively unsaturated dirhenium(II) complex [(XylNC)(OC)CIRe(μ-dppm)2ReCl2]O3SCF3 (dppm = Ph2PCH2PPh2) with one equivalent of XylNC in CH2Cl2 affords a fifth structural isomer of the [Re2Cl3(μ-dppm)2(CO)(CNXyl)2] + cation; this is believed to have a CO-bridged structure of the type [(XylNC)ClRe(μ-Cl)(μ-CO)(μ-dppm)2ReCl(CNXyl)]+. The latter complex reacts with a further equivalent of XylNC in the presence of Tl+ to form the [Re2Cl2(μ-dppm)2(CO)(CNXyl)3]2+ cation, which has been shown by IR spectroscopy, and by the X-ray crystallographic characterization of its neutral congener Re2Cl2(μ-dppm)2(CO)(CNXyl)3, to contain a very weak and unsymmetrical CO bridge.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1022609214775
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  • 4
    Electronic Resource
    Electronic Resource
    Genetic control of Interleukin 12 responsiveness: implications for disease pathogenesis (1997)
    Springer
    Journal of molecular medicine 75 (1997), S. 502-511 
    Details
    ISSN: 1432-1440
    Keywords: Key words T helper 1/T helper 2 ; Genetics ; Interleukin 12 ; Allergy ; Autoimmunity ; Leishmania
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract  We examined the effect of genetic background on Th1/Th2 development. We discuss data demonstrating that genetic background is an important determinant of interleukin-12 (IL-12) responsiveness and the potential implications for disease progression in murine experimental leishmaniasis. Genetic analysis of the differential control of IL-12 responsiveness led to the identification of a controlling locus on the middle portion of murine chromosome 11. This genetic region (or its human counterpart, 5q31) has been associated with increased disease susceptibilities for several atopic, infectious, and autoimmune disorders. We discuss potential roles for genetic control of IL-12 responsiveness in the development of these diseases.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s001090050135
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  • 5
    Electronic Resource
    Electronic Resource
    Familial Hodgkin's disease: a disease of young adulthood? (1997)
    Springer
    Annals of hematology 74 (1997), S. 131-134 
    Details
    ISSN: 1432-0584
    Keywords: Key words Hodgkin's disease ; Sex ; Age ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract  Familial Hodgkin's disease (FHD) is estimated to represent approximately 4.5% of all cases of Hodgkin's disease (HD). Shared environmental factors, such as Epstein-Barr virus and other viral agents, and genetic determinants have all been proposed to explain familial aggregation of HD. In order to compare the characteristic features of FHD with those of the much more common sporadic form, we reviewed 28 articles on FHD, published between 1972 and 1995, and analyzed in further detail data from 18 papers, reporting on a total of 328 patients. The male-to-female ratio of the FHD population examined was 1.5, similar to that reported for sporadic HD, and lower than the one suggested for FHD by some authors. On the other hand, a significant difference was found between sporadic and familial HD according to age at diagnosis; that is, only one major peak between 15 and 34 years was present in the group of patients with FHD. Further investigation of FHD in young adulthood may provide insight into the hypothesis of a genetic or infectious etiology of the disease.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002770050270
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  • 6
    Electronic Resource
    Electronic Resource
    Genetics and cytology of a new genic male-sterile soybean [Glycine max (L.) Merr.] (1997)
    Springer
    Sexual plant reproduction 10 (1997), S. 13-21 
    Details
    ISSN: 1432-2145
    Keywords: Key words Soybean ; Male sterility ; Genetics ; Callase ; Callose
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract  Genetic and cytological studies were conducted with a new male-sterile, female-fertile soybean [Glycine max (L.) Merr.] mutant. This mutant was completely male sterile and was inherited as a single-recessive gene. No differences in female or male gamete transmission of the recessive allele were observed between reciprocal cross-pollinations in the F1 or F2 generations. This mutant was not allelic to any previously identified soybean genic male-sterile mutants: ms1, ms2, ms3, ms4, ms5, or ms6. No linkage was detected between sterility and flower color (W1 locus), or between sterility and pubescence color (T1 locus). Light microscopic and cytological observations of microsporogenesis in fertile and sterile anthers were conducted. The structure of microspore mother cells (MMC) in male-sterile plants was identical to the MMCs in male-fertile plants. Enzyme extraction analyses showed that there was no callase activity in male-sterile anthers, and this suggests that sterility was caused by retention of the callose walls, which normally are degraded around tetrads at the late tetrad stage. The tapetum from male-sterile anthers also showed abnormalities at the tetrad stage and later stages, which were expressed by an unusual formation of vacuoles, and by accumulation of densely staining material. At maturity, anthers from sterile plants were devoid of pollen grains.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s004970050062
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  • 7
    Electronic Resource
    Electronic Resource
    Effect of naltrexone on subjective alcohol response in subjects at high and low risk for future alcohol dependence (1997)
    Springer
    Psychopharmacology 129 (1997), S. 15-22 
    Details
    ISSN: 1432-2072
    Keywords: Key words Naltrexone ; Alcohol ; Genetics ; Social drinkers ; Family history of alcoholism ; Biphasic Alcohol Effects Scale
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract We investigated specific subjective effects of naltrexone pretreatment or placebo during various intervals on the breath alcohol level (BAL) curve in nonalcoholic volunteers. Fifteen high-risk (social drinkers with an alcoholic father) and 14 low-risk (no alcoholic relatives in at least two generations) subjects were tested in a double-blind, placebo-controlled study of the effects of 50 mg oral naltrexone on response to a moderate dose of alcohol. Dependent measures included subjective stimulation and sedation subscales from the Biphasic Alcohol Effects Scale (BAES) and mood subscales from the Profile of Mood States (POMS). At rising BALs, high-risk subjects showed a naltrexone-related attenuation of BAES stimulation. This effect was not evident in low-risk subjects, who directionally showed the opposite effect, although nonsignificant. For both groups, there were no significant naltrexone-related effects for BAES sedation; however, naltrexone did affect several POMS scales on alcohol response, such as decreased vigor, and increased fatigue, tension, and confusion. Confusion was significantly elevated for the high-risk group during rising BALs of the naltrexone session. The results suggest a differential response to naltrexone, based on paternal history of alcoholism and level of stimulation experienced during alcohol drinking.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002130050156
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  • 8
    Electronic Resource
    Electronic Resource
    Mitochondrial DNA polymorphisms in pathologically proven Parkinson’s disease (1997)
    Springer
    Journal of neurology 244 (1997), S. 262-265 
    Details
    ISSN: 1432-1459
    Keywords: Key words Parkinson’s disease ; Genetics ; Mitochondrial DNA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract To date, five single base pair changes of the mitochondrial DNA have been reported to occur either exclusively or with increased frequency in Caucasian patients with Parkinson’s disease (PD) and it has been postulated that these mutations might be causally related to the observed inhibition of mitochondrial respiratory chain function in PD. To evaluate these findings, we analysed the frequency of all five polymorphisms in 100 cases of pathologically proven cases of PD. We were either unable to detect the previously described polymorphisms in our series or found them to be present with the same frequency among controls. Our data do not support the hypothesis of an involvement of the mitochondrial DNA in the pathogenesis of PD.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s004150050082
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  • 9
    Electronic Resource
    Electronic Resource
    Genetics, haloperidol-induced catalepsy and haloperidol-induced changes in acoustic startle and prepulse inhibition (1997)
    Springer
    Psychopharmacology 134 (1997), S. 131-139 
    Details
    ISSN: 1432-2072
    Keywords: Key words Startle ; Prepulse inhibition ; Inbred strains ; Haloperidol ; Catalepsy ; Schizophrenia ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The acoustic startle response (ASR), prepulse inhibition (PPI) of the ASR and the effects of haloperidol on the ASR and PPI were examined in C57BL/6J (B6) and DBA/2 (D2) inbred mouse strains and their F1 and F2 progeny. The startle stimulus was a 60-ms, 110-dB, 10-kHz tone; the prepulse stimuli were 20-ms white noise bursts at 56, 68 and 80 dB against a 50-dB background presented 100-ms before the startle pulse. The B6 strain showed modest PPI (25–40%); in contrast, the D2 strain showed on average no PPI and numerous individuals showed prepulse augmentation (PPA). The F2 progeny showed an intermediate PPI; however, the extreme values ranged from 200% PPA to essentially 100% PPI. Haloperidol in dose-dependent fashion, increased PPI in both the B6 and D2 strains; the threshold dose was in the range of 0.1–0.2 mg/kg. Raclopride (0.3 mg/kg), clozapine (2 mg/kg) and risperidone (0.4 mg/kg) also increased PPI in both strains. The effects of haloperidol (0.4 mg/kg) on PPI in 140 F2 progeny were examined. For all prepulse intensities, there were highly significant (r 〉 0.80) and negative correlations between baseline PPI and the haloperidol-induced change in PPI. Thus, those animals that showed the greatest PPA showed the greatest haloperidol-induced increase in PPI. There was, however, significant variance in the haloperidol response; plots of the regression residuals showed the most and least responsive animals differed by almost 100% in effect on PPI. The F2 progeny were subsequently phenotyped for haloperidol-induced catalepsy. There was no association between the variation in effects on catalepsy and PPI. However, it was observed that those individuals with the poorest baseline PPI were catalepsy non-responsive.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002130050434
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  • 10
    Electronic Resource
    Electronic Resource
    Thermal latent coordination compounds (1997)
    Springer
    Journal of thermal analysis and calorimetry 50 (1997), S. 569-586 
    Details
    ISSN: 1572-8943
    Keywords: crystal structure ; metal(II) picolinate and quinaldinate ; thermal degradation of imidazole and pyrazole complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Complexes of the type M(Pa)2(HAz)2 and M(QA)2(HAz)2 (M=cobalt(II) and nickel(II); HPa=picolinic acid, HQa=quinaldic acid; HAz=azoles like imidazole (Him), pyrazole (HPz), benzimidazole (HBzIm) etc.) show a similar thermal behaviour. In the first step of decomposition the corresponding azolinium picolinates or quinaldinates (H2AzPa, H2AzQa) are split off with formation of polymeric mixed ligand complexes M(Pa)(Az) or M(Qa)(Az). X-ray analysis of Co(Qa)2(HBzIm)2 XIIIa illustrates a proton transfer and a subsequent thermal removal of benzimidazolinium quinaldinate (H2BzImQa): Hydrogen bridges from pyrrole nitrogen of the benzimidazole to the non-coordinated oxygen of the quinaldinate predetermine the thermal initiated proton transfer. The high volatility of the heterocyclic acids and the nitrogen coordination are responsible for the formation of the mixed ligand complex Co(Qa)(BzIm) XIVa. Exceptions are the complexes M(Pa)2(HPz)2 XIa-b and M(Qa)2(HIm)2 XVIIa-b. Pyrazole is eliminated from the complexes XIa-b with formation of the solvent-free inner complex M(Pa)2 XIIa-b. From compounds XVIIIa-b quinaldic acid or their decomposition products are split off and a high temperature modification of M(Im)2 XVIIIa-b is formed at elevated temperature. XVIIIa-b are decomposed to the cyanides M(CN)2 similarly to the thermal behaviour of Cu(Im). In the first step the thermal degradation of imidazole and pyrazole adducts of copper(II) picolinates and quinaldinates is characterized by the elimination of azoles. The reason for this thermal behaviour is the weaker coordination of the azole heterocycles in copper chelate compounds.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01979029
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  • 11
    Electronic Resource
    Electronic Resource
    Structures and tautomeric interconversions of anthraquinone imine derivatives (1997)
    Springer
    Structural chemistry 8 (1997), S. 197-204 
    Details
    ISSN: 1572-9001
    Keywords: Tautomerism ; anthraquinone ; crystal structure ; semiempirical computations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Substituted 1-hydroxy-9,10-anthraquinone-9-imines have been found to exhibit tautomeric interconversions between the 9,10- and 1,10-quinonoid forms in the solid state as well as in solution. Single-crystal X-ray crystallography was used to study the structures of 4-(N-acetyl-p-tolylamino)-9-amino-1,10-anthracenedione and 4-hydroxy-1-phenylamino-10-mesitylimino-9(10H)-anthracenone at ambient and low temperatures. The former compound gave crystals belonging to the monoclinic space group P2l/c and, at 295 K,a=9.684(2),b=16.371(3),c=12.097(2) å,Β=110.41(1)
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02263507
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  • 12
    Electronic Resource
    Electronic Resource
    Synthesis and structure of 5-methoxy-4-methylbenzopsoralen (1997)
    Springer
    Structural chemistry 8 (1997), S. 453-457 
    Details
    ISSN: 1572-9001
    Keywords: Benzopsoralen ; photochemotherapeutic agent ; crystal structure ; molecular mechanics ; AM1 theoretical calculations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 5-Methoxy-4-methyl-2H-benzofuro[3,2-g]benzo-1-pyran-2-one was synthesized and its crystal structure was determined and compared with the optimal conformation arrived at by MM and AM1 theoretical calculations. The latter indicated that the tetracyclic skeleton is planar with total length (C2–C8) 9.23 å, and that the line joining the conters of the terminal-benzene and furan rings makes an angle of 30.5
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02311704
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  • 13
    Electronic Resource
    Electronic Resource
    Behavioral phenotypes of inbred mouse strains: implications and recommendations for molecular studies (1997)
    Springer
    Psychopharmacology 132 (1997), S. 107-124 
    Details
    ISSN: 1432-2072
    Keywords: Key words Mouse ; Inbred strains ; Behavior ; Genetics ; Locomotion ; Open field activity ; Learning ; Memory ; Aggression ; Parental behaviors ; Acoustic startle ; Prepulse inhibition ; Alcohol ; Nicotine ; Cocaine ; Opiates ; Haloperidol ; Diazepam ; Breeding ; Embryonic stem cell lines ; Transgenic ; Knockouts ; Null mutation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract  Choosing the best genetic strains of mice for developing a new knockout or transgenic mouse requires extensive knowledge of the endogenous traits of inbred strains. Background genes from the parental strains may interact with the mutated gene, in a manner which could severely compromise the interpretation of the mutant phenotype. The present overview summarizes the literature on a wide variety of behavioral traits for the 129, C57BL/6, DBA/2, and many other inbred strains of mice. Strain distributions are described for open field activity, learning and memory tasks, aggression, sexual and parental behaviors, acoustic startle and prepulse inhibition, and the behavioral actions of ethanol, nicotine, cocaine, opiates, antipsychotics, and anxiolytics. Using the referenced information, molecular geneticists can choose optimal parental strains of mice, and perhaps develop new embryonic stem cell progenitors, for new knockouts and transgenics to investigate gene function, and to serve as animal models in the development of novel therapeutics for human genetic diseases.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002130050327
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  • 14
    Electronic Resource
    Electronic Resource
    The effects of cocaine on operant responding for food in several strains of mice (1997)
    Springer
    Psychopharmacology 132 (1997), S. 202-208 
    Details
    ISSN: 1432-2072
    Keywords: Key words Cocaine ; Operant behavior ; Genetics ; Mice
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract  The availability of numerous genetically homogenous mouse strains permits the analysis of genetic influences on behavior and also behavioral sensitivity (responsivity) to drugs of abuse. The current study was conducted to characterize discriminated operant responding for food in four inbred strains (Balb/cByJ, DBA/2J, C57BL/6J, SJL/J), an F1 Hybrid (C57BL/6×SJL), and one outbred strain (CD1) of mouse. The effect of cocaine on this operant behavior was also examined. Initially, all animals were trained to nosepoke for food on a continuous reinforcement schedule. The minimum response requirement for reinforcement was increased every 5 days until the animals were responding on an FR-15 schedule of reinforcement. All strains increased operant responding as the schedule of reinforcement was raised. However, significant differences in response rate and discrimination learning were observed among the various strains of mice. Cocaine administration reduced operant responding for food in Balb/cByJ, C57BL/6J, C57BL/6×SJL/J and CD1 mice at a dose of 15.0 mg/kg, whereas higher doses were required in DBA/2J mice (30.0 mg/kg) and SJL/J mice (56.0 mg/kg). These results suggest that operant performance and the effect of cocaine on this behavior is differentially influenced by genetic make-up.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002130050337
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  • 15
    Electronic Resource
    Electronic Resource
    Homoclinic chaos in a model of natural selection (1997)
    Springer
    Journal of mathematical biology 35 (1997), S. 294-320 
    Details
    ISSN: 1432-1416
    Keywords: Key words: Natural selection ; Homoclinic chaos ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Mathematics
    Notes: Abstract.  We modify a simple mathematical model for natural selection originally formulated by Robert M. May in 1983 by permitting one homozygote to have a larger selective advantage when rare than the other, and show that the new model exhibits dynamical chaos. We determine an open region of parameter space associated with homoclinic points, and prove that there are infinite sequences of period-doubling bifurcations along selected paths through parameter space. We also discuss the possibility of chaos arising from imbalance in the homozygote fitnesses in more realistic biological situations, beyond the constraints of the model.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s002850050053
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  • 16
    Electronic Resource
    Electronic Resource
    Expression of a unique plastid-localized heat-shock protein is genetically linked to acquired thermotolerance in wheat (1997)
    Springer
    Theoretical and applied genetics 95 (1997), S. 834-841 
    Details
    ISSN: 1432-2242
    Keywords: Key words Stress proteins ; Heat tolerance ; Chloroplast ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract  We have used a combination of molecular and classical genetic approaches to delineate the relationship between a specific HSP member and cell viability under heat stress. Using recombinant inbred lines (RILs) of wheat, derived from a cross of the thermotolerant cultivar ‘Mustang’ and the thermosusceptible cultivar ‘Sturdy,’ we have identified a unique HSP and a differentially expressed cDNA sequence, both related to the plastid-localized HSP26 gene family, that are closely associated with acquired thermotolerance in wheat. An isoform of HSP26 was synthesized under heat stress in all examined thermotolerant RILs and ‘Mustang’, and was absent in all examined thermosusceptible RILs and ‘Sturdy.’ Using a modified differential-display method, we have also identified a gene-specific cDNA sequence that is similar to other known members of the wheat HSP26 gene family and is selectively expressed in ‘Mustang’ and most of the examined thermotolerant RILs, but not expressed in ‘Sturdy’ and all the thermosusceptible RILs. These results suggest a genetic linkage between the acquired thermotolerance trait and the differential expression of a unique member of the HSP26 gene family.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s001220050633
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  • 17
    Electronic Resource
    Electronic Resource
    Extreme resistance to potato virus V in clones of Solanum tuberosum that are also resistant to potato viruses Y and A: evidence for a locus conferring broad-spectrum potyvirus resistance (1997)
    Springer
    Theoretical and applied genetics 95 (1997), S. 1258-1262 
    Details
    ISSN: 1432-2242
    Keywords: Key words Extreme virus resistance ; Potyviruses ; Genetics ; Genes Rysto and Ra ; Broad-spectrum resistance
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract  Extreme resistance to the potato V potyvirus (PVV) was found in four potato cultivars that contain Ry genes from Solanum stoloniferum. When plants of these cultivars, were inoculated by grafting in shoot tips from PVV-infected tomato plants, necrotic symptoms developed in some cultivars, although a full hypersensitive reaction was not elicited, while other cultivars were symptomless. PVV replication was not detected in any of the inoculated plants by ELISA, an infectivity assay of leaf extracts by manual inoculation to Nicotiana benthamiana indicator plants, or by ‘return grafting’ of shoot tips taken from newly developed shoots of the potato plants to virus-free indicator plants of tomato. These methods readily detected PVV infection in inoculated plants of cv ‘Flourball’, which does not contain an Ry gene and is susceptible, and in cvs ‘Maris Piper’ and ‘Dr Macintosh’, which contain gene Nv conditioning a hypersensitive reaction to inoculation. One of the Ry-containing cultivars, ‘Barbara’, has been previously shown to contain two genes that control extreme resistance, defined as no viral replication in intact plants, to the potyviruses potato viruses Y and A (PVY and PVA). These genes are: Ry sto , which conditions resistance to PVY and PVA, and gene Ra, which conditions resistance to PVA only. It was found that in genotypes from a progeny of the cross ‘Barbara’ (Ry sto /Ra)בFlourball’ (ry/ra), extreme resistance to PVV segregated with gene Ry sto . It is proposed that either gene Ry sto conditions broad-spectrum extreme resistance to the distinct potyviruses PVY, PVA, and PVV or that Ry sto represents a family of genetically closely linked genes each controlling resistance to a specific virus.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s001220050690
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  • 18
    Electronic Resource
    Electronic Resource
    Resistance to Phytophthora fragariae var. fragariae in strawberry: the Rpf2 gene (1997)
    Springer
    Theoretical and applied genetics 94 (1997), S. 1092-1096 
    Details
    ISSN: 1432-2242
    Keywords: Key words Fragaria×ananassa ; Genetics ; Inheritance ; Red core ; Red stele
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract   Phytophthora fragariae var. fragariae is the causal agent of red stele (red core) root rot in strawberry (Fragaria spp.). The inheritance of resistance to one isolate of this fungus was studied in 12 segregating populations of F.×ananassa derived from crosses between four resistant cultivars (‘Climax’, ‘Redgauntlet’, ‘Siletz’, and ‘Sparkle’) and three susceptible cultivars (‘Blakemore’, ‘Glasa’, and ‘Senga’ Sengana’). The analysis clearly supports the hypothesis of a single segregating dominant resistance gene. It is proposed that this gene be designated Rpf2.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s001220050520
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  • 19
    Electronic Resource
    Electronic Resource
    The crystal and molecular structures of cellulose I and II (1997)
    Springer
    Glycoconjugate journal 14 (1997), S. 677-690 
    Details
    ISSN: 1573-4986
    Keywords: molecular dynamics ; crystal structure ; cellulose I and II
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paper describes molecular dynamics (MD) simulations on the crystal structures of the Iβ and II phases of cellulose. Structural proposals for each of these were made in the 1970s on the basis of X-ray diffraction data. However, due to the limited resolution of these data some controversies remained and details on hydrogen bonding could not be directly obtained. In contrast to structure factor amplitudes in X-ray diffraction, energies, as obtained from MD simulations, are very sensitive to the positions of the hydroxyl hydrogen atoms. Therefore the latter technique is very suitable for obtaining such structural details. MD simulations of the Iβ phase clearly shows preference for one of the two possible models in which the chains are packed in a parallel orientation. Only the parallel-down mode (in the definition of Gardner and Blackwell (1974) J Biopolym 13: 1975-2001) presents a stable structure. The hydrogen bonding consists of two intramolecular hydrogen bonds parallel to the glycosidic linkage for both chains, and two intralayer hydrogen bonds. The layers are packed hydrophobically. All hydroxymethyl group are positioned in the tg conformation. For the cellulose II form it was found that, in contrast to what seemed to emerge from the X-ray fibre diffraction data, both independent chains had the gt conformation. This idea already existed because of elastic moduli calculations and 13C-solid state NMR data. Recently, the structure of cellotetraose was determined. There appear to be a striking similarity between the structure obtained from the MD simulations and this cellotetraose structure in terms of packing of the two independent molecules, the hydrogen bonding network and the conformations of the hydroxymethyl group, which were also gt for both molecules. The structure forms a 3D hydrogen bonded network, and the contribution from electrostatics to the packing is more pronounced than in case of the Iβ structure. In contrast to what is expected, in view of the irreversible transition of the cellulose I to II form, the energies of the Iβ form is found to be lower than that of II by 1 kcal mol-1 per cellobiose.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1018509231331
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  • 20
    Electronic Resource
    Electronic Resource
    Genetic aspects of childhood behavioral disorders (1997)
    Springer
    Child psychiatry & human development 27 (1997), S. 139-150 
    Details
    ISSN: 1573-3327
    Keywords: ADHD ; Tourette Syndrome ; Genetics ; Gene Selection ; Conduct Disorder
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The evidence is reviewed to support the concept that many disruptive, childhood and adolescent behavioral disorders including ADHD, Tourette syndrome, learning disabilities, substance abuse, oppositional defiant disorder and conduct disorder, are part of a spectrum of inter-related behaviors that have a strong genetic component, are polygenically inherited, share a number of genes in common that affect dopamine, serotonin and other neurotransmitters, and are transmitted from both parents. Some of the implications of this hypothesis in relation to diagnosis and treatment are reviewed, including the possibility that the genes involved may be increasing in frequency.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02353694
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  • 21
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    Electronic Resource
    The molecular complex of dibenz[a,c]anthracene and trinitrobenzene (1997)
    Springer
    Structural chemistry 8 (1997), S. 141-147 
    Details
    ISSN: 1572-9001
    Keywords: Dibenzanthracene ; trinitrobenzene complex ; trinitrobenzene complex ; π-complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the complex between the polycyclic aromatic hydrocarbon di-benz[a,c]anthracene and 1,3,5-trinitrobenzene is reported. The crystals are triclinic, space group P¯1 with unit cell dimensionsa=7.277(2) å,b=11.237(6) å, andc=13.902(5) å,α= 104.13(4)
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02262849
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  • 22
    Electronic Resource
    Electronic Resource
    Computerized EEG topography of normal preadolescent twins—Correlating similarity of background activity with genetic relatedness (1997)
    Springer
    Brain topography 9 (1997), S. 303-311 
    Details
    ISSN: 1573-6792
    Keywords: EEG normality ; Brain topography ; Twins ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The influence of genetic relatedness on the similarity degree of topographical EEG parameters was studied in a sample of 26 sets of monozygotic (MZ) and 46 sets of dizygotic (DZ) twins. All 144 subjects were healthy, primary school children, aged 7–15 years, 69 boys and 75 girls. Correlation coefficients were calculated for 50 quantitative EEG parameters of paired values obtained at each of 16 active electrode sites, in four groups of paired tracings: 1. MZ twins, 2. DZ twins, 3. The autocorrelated (A) group formed by correlating the spectral parameters from the same subjects in two different analyzed sequences, 4. The random (R) control group of 1200 unrelated pairs formed from DZ twin pairs. Sets of MZ twins and A group showed the highest degrees of similarity of spectral parameters over all brain areas except for significant differences only for some background features over posterior regions. In contrast, highly significant differences in topographic parameters were evident in comparison of MZ sets with DZ sets, particularly when MZ sets were compared with DZ subsets of opposite sex. Both number and degree of significant differences increased progressively in comparisons with groups 3 vs 2,1 vs 4, and 3 vs 4. The data gave strong evidence for a complex polygenic determination of normal human EEG topography.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01464485
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  • 23
    Electronic Resource
    Electronic Resource
    Large differences are observed between the crystal and solution quaternary structures of allosteric aspartate transcarbamylase in the R state (1997)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 27 (1997), S. 110-117 
    Details
    ISSN: 0887-3585
    Keywords: small-angle scattering ; x-rays ; allosteric enzymes ; crystal structure ; rigid body modeling ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Solution scattering curves evaluated from the crystal structures of the T and R states of the allosteric enzyme aspartate transcarbamylase from Escherichia coli were compared with the experimental x-ray scattering patterns. Whereas the scattering from the crystal structure of the T state agrees with the experiment, large deviations reflecting a significant difference between the quaternary structures in the crystal and in solution are observed for the R state. The experimental curve of the R state was fitted by rigid body movements of the subunits in the crystal R structure which displace the latter further away from the T structure along the reaction coordinates of the T→R transition observed in the crystals. Taking the crystal R structure as a reference, it was found that in solution the distance between the catalytic trimers along the threefold axis is 0.34 nm larger and the trimers are rotated by 11° in opposite directions around the same axis; each of the three regulatory dimers is rotated by 9° around the corresponding twofold axis and displaced by 0.14 nm away from the molecular center along this axis. Proteins 27:110-117 © 1997 Wiley-Liss, Inc.
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  • 24
    Electronic Resource
    Electronic Resource
    Bactericidal antibody recognition of a PorA epitope of Neisseria meningitidis: Crystal structure of a Fab fragment in complex with a fluorescein-conjugated peptide (1997)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 29 (1997), S. 113-125 
    Details
    ISSN: 0887-3585
    Keywords: bactericidal antibody ; crystal structure ; Neisseria meningitidis ; peptide-fluorescein conjugate ; PorA outer membrane protein ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Class 1 outer membrane protein PorA of Neisseria meningitidis is a vaccine candidate against bacterial meningitis. Antibodies against PorA are able to induce complement-mediated bacterial killing and thereby play an important role in protection against meningococcal disease. Bactericidal antibodies are all directed against variable regions VR1 and VR2 of the PorA sequence, corresponding to loops 1 and 4 of a two-dimensional topology model of the porin with eight extracellular loops. We have determined the crystal structure to 2.6 Å resolution of the Fab fragment of bactericidal antibody MN12H2 against meningococcal PorA in complex with a linear fluorescein-conjugated peptide TKDTNNNL derived from the VR2 sequence of sero-subtype P1.7,16 (residues 180-187) from meningococcal strain H44/76. The peptide folds deeply into the binding cavity of the Fab molecule in a type I β-turn, with the minimal P1.16 epitope DTNNN virtually completely buried. The structure reveals H-bonds and van der Waals interactions with all minimal epitope residues and one essential salt bridge between Asp-182 of the peptide and His-31 of the MN12H2 light chain. The key components of the recognition of PorA epitope P1.16 by bactericidal antibody MN12H2 correspond well with available thermodynamic data from binding studies. Furthermore, they indicate the structural basis of an increased endemic incidence of infection by group B meningococci in England and Wales since 1981 associated with the occurrence of an Neisseria meningitidis escape mutant (strain MC58). The observed three-dimensional conformation of the peptide provides a rationale for the development of a synthetic peptide vaccine against meningococcal disease. Proteins 29:113-125, 1997. © 1997 Wiley-Liss, Inc.
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  • 25
    Electronic Resource
    Electronic Resource
    Computational, pulse-radiolytic, and structural investigations of lysine-136 and its role in the electrostatic triad of human C u,Z n superoxide dismutase (1997)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 29 (1997), S. 103-112 
    Details
    ISSN: 0887-3585
    Keywords: Brownian dynamics ; molecular recognition ; site-directed mutagenesis ; facilitated diffusion ; crystal structure ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Key charged residues in Cu,Zn superoxide dismutase (Cu,Zn SOD) promote electrostatic steering of the superoxide substrate to the active site Cu ion, resulting in dismutation of superoxide to oxygen and hydrogen peroxide. Lys-136, along with the adjacent residues Glu-132 and Glu-133, forms a proposed electrostatic triad contributing to substrate recognition. Human Cu,Zn SODs with single-site replacements of Lys-136 by Arg, Ala, Gln, or Glu or with a triple-site substitution (Glu-132 and Glu-133 to Gln and Lys-136 to Ala) were made to test hypotheses regarding contributions of these residues to Cu,Zn SOD activity. The structural effects of these mutations were modeled computationally and validated by the X-ray crystallographic structure determination of Cu,Zn SOD having the Lys-136-to-Glu replacement. Brownian dynamics simulations and multiple-site titration calculations predicted mutant reaction rates as well as ionic strength and pH effects measured by pulse-radiolytic experiments. Lys-136-to-Glu charge reversal decreased dismutation activity 50% from 2.2 × 109 to 1.2 × 109 M-1 s-1 due to repulsion of negatively charged superoxide, whereas charge-neutralizing substitutions (Lys-136 to Gln or Ala) had a less dramatic influence. In contrast, the triple-mutant Cu,Zn SOD (all three charges in the electrostatic triad neutralized) surprisingly doubled the reaction rate compared with wild-type enzyme but introduced phosphate inhibition. Computational and experimental reaction rates decreased with increasing ionic strength in all of the Lys-136 mutants, with charge reversal having a more pronounced effect than charge neutralization, implying that local electrostatic effects still govern the dismutation rates. Multiple-site titration analysis showed that deprotonation events throughout the enzyme are likely responsible for the gradual decrease in SOD activity above pH 9.5 and predicted a pKa value of 11.7 for Lys-136. Overall, Lys-136 and Glu-132 make comparable contributions to substrate recognition but are less critical to enzyme function than Arg-143, which is both mechanistically and electrostatically essential. Thus, the sequence-conserved residues of this electrostatic triad are evidently important solely for their electrostatic properties, which maintain the high catalytic rate and turnover of Cu,Zn SOD while simultaneously providing specificity by selecting against binding by other anions. Proteins 29:103-112, 1997. © 1997 Wiley-Liss, Inc.
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  • 26
    Electronic Resource
    Electronic Resource
    The crystal structure of 1,4-benzenedithiol by rietveld analysis and studies on the mechanism of solid-state addition polymerization of 1,4-benzenedithiol to 1,4-diethynylbenzene (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 35 (1997), S. 1621-1625 
    Details
    ISSN: 0887-624X
    Keywords: 1,4-benzenedithiol ; 1,4-diethynylbenzene ; crystal structure ; solid-state polymerization ; layer structure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal structure of 1,4-benzenedithiol (BDT) was determined by the Rietveld method based on the calculation of the atomic coordinates of the BDT molecule using the Molecular Mechanics Program (MMP2). The refined crystal structure of BDT was monoclinic P21/c with dimensions, a = 7.795, b = 7.290, c = 5.955 Å, β = 92.16°, z = 2. The R factor of the refined structure was 0.038. Using above results, the mechanism of solid-state addition polymerization of BDT to 1,4-diethynylbenzene (DEB) was studied. Sublimed BDT piles up onto glass plate substrate and forms the layer structure along with the a axis. An inclination angle of the piled BDT column was 60° toward the substrate surface. DEB crystal structure was also monoclinic P21/c with a = 4.007, b = 6.018; c = 15.340 Å, β = 91.42°, z = 2. Sublimation of equimolar mixture of BDT and DEB gave a crystal having 1 : 1 composition, in which DEB column is situated between the columns of BDT. Relative arrangement of both monomers was suitable for the addition of —SH and —C=CH groups, since the distance between the two groups is 3.3 Å by CERIUS II calculation. Therefore, the addition polymerization of BDT to DEB easily proceeded by UV irradiation and the resulting polymer had a highly layer structure along with the a axis of BDT crystal. Tentatively estimated crystal structure of polymer obtained is monoclinic with a = 7.73, b = 7.30, c = 5.95 Å, β = 92.16°. © 1997 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 35: 1621-1625, 1997
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  • 27
    Electronic Resource
    Electronic Resource
    Crystal Structures of 1,3-Calix[4]-bis-crown-6·3CH3CN and 1,3-Calix[4]-bis-(benzo-crown-6)·3 CH3CN (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 27 (1997), S. 169-178 
    Details
    ISSN: 1573-1111
    Keywords: Bridged calix[4]arene ; ditopic receptor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures of a new solvate of the ditopic receptor 1,3-calix[4]-bis-crown-6, Bis-C6, and of 1,3-calix[4]-bis-(benzo-crown-6), Bis-benzoC6, are reported. Bis-C6.3 CH3CN (1) crystallizes in the monoclinic space group P21/n, a = 14.388(3), b = 26.947(8), c = 14.707(4) Å, β = 113.19(3)°, V = 5241(5) Å3, Z = 4. Refinement led to a final conventional R value of 0.092 for 2723 reflections. The structure of (1) differs from the previously reported structure of Bis-C6.4 CH3CN by the conformation of one crown either chain. Two acetonitrile molecules are in the close neighbourhood of the crown ether cavities. Bis-benzoC6.3 CH3CN (2) crystallizes in the monoclinic space group P21/c, a = 10.391(4), b = 17.264(11), c = 30.426(9) Å, β = 94.62(3)°, V = 5440(7) Å3, Z = 4. Refinement led to a final conventional R value of 0.106 for 2965 reflections. Two acetonitrile molecules are located near the crown ether cavities, as in (1). One of the crown ether conformations is the same as in the binuclear caesium complex of Bis-benzoC6, supporting the hypothesis of a preorganization of this ligand towards the complexation of this ion; the second crown ether chain is partially disordered.
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    URL: http://dx.doi.org/10.1023/A:1007990208036
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  • 28
    Electronic Resource
    Electronic Resource
    X-Ray Structure and Proton NMR Study of a Hexacoordinated Lithium Complex (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 28 (1997), S. 125-140 
    Details
    ISSN: 1573-1111
    Keywords: X-ray ; crystal structure ; Li-complex ; triamides ; 1H-NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of the lithium complex with1,3,5-tris[oxymethylene(N,N-dicyclohexyl)carboxyamido]cyclohexanehas been determined by the X-ray method.The compound is triclinic, space group P¯1,a = 15.623(3), b = 19.279(4),c = 19.295(4)Å α = 102.32(3), β = 92.45(3),γ = 105.67(3)0, V = 5436(2)Å3, Z = 4. Itscomposition is represented by the formulaC48H82N3O6LiI 0.5H2O. The lithium cationis encapsulated in a polar pseudo-cavity of six oxygen atoms of the ligandmolecule and displays a distorted trigonal prism coordination. The conformationof the ligand in the solid state complex has been compared with the conformationof the complex in solution determined by 1H-NMR measurements. Supplementary data relevant to this publication have been deposited with the British Library, No. SUP 82224 (21 pages).
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    URL: http://dx.doi.org/10.1023/A:1007955923966
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  • 29
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    Electronic Resource
    Inclusion Compounds of NaI with 13-Membered Azo- and Azoxycrown Ethers (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 28 (1997), S. 17-32 
    Details
    ISSN: 1573-1111
    Keywords: Azocrown ether ; azoxycrown ether ; sodium complexes ; crystal structure ; X-ray analysis ; conformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Sodium iodide complexes of 13-membered azo-(I)and azoxycrown ethers (II) have been synthesized. Compound I[Na(L1 trans)2]⋅I⋅H2O is triclinic witha = 11.53(2), b = 15.74(2), c = 19.17(2) Å,α = 98.93(9), β = 105.51(9),γ = 89.20(9) deg.; Z = 4, space groupP1. Compound II [Na(L2)2]⋅I is orthorhombic witha = 12.451(2), b = 13.796(3), c = 18.667(4)Å; Z = 4, space group P212121. In bothcomplexes the cation is coordinated tochain oxygen atoms and to one nitrogen atom of the azoor azoxy unit. The ability of bothligands to form complexes in relation to thegeometry of the azo or azoxy subunit of themacrocycle is discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1007929726695
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  • 30
    Electronic Resource
    Electronic Resource
    Polymorphism of Inclusion Complexes and Unsolvated Hosts. II. Structure of the β-Dimorph of the Host-Guest Complex of Dianilinegossypol with Ethylacetate (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 27 (1997), S. 105-112 
    Details
    ISSN: 1573-1111
    Keywords: β-Dimorph ; crystal structure ; dianilinegossypol ethylacetate 1 : 1 clathrate ; packing motifs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Depending on crystallization conditions, dianilinegossypol and ethylacetate form low (ambient temperature, α-phase) and high temperature (t = 35°C, β-phase) clathrate modifications. The structure of the α-phase has been discussed earlier [1]. Crystals of the 1 : 1 β-phase complex, C42H40O6N2·C4O2H8, are monoclinic, space group P21/c, a = 11.362(6), b = 19.479(9), c = 19.085(9) Å, β = 103.21(4)°, V = 4112(3)Å3, Z = 4, R = 0.084 for 3210 observed reflections. In these complexes centrosymmetric dimers of dianilinegossypol molecules formed via O(5)—H···O(3) hydrogen bonds are associated into columns by a weak O(8)—H···O(7) H-bond. A difference in the structure of these two phases is in the packing mode of the columns. The angle formed by intersecting host columns is about 126° for the α-phase and 104° for the β-modification. Guest molecules are hydrogen bonded to the host molecules via an O(1)—H···O(10) bond and are accommodated in channels in α-phase complex and in cavities in β-phase complex.
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    URL: http://dx.doi.org/10.1023/A:1007908530132
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  • 31
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    Crystal Structure of a Uranyl/p-tert-Butylcalix[5]arene Complex (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 27 (1997), S. 13-20 
    Details
    ISSN: 1573-1111
    Keywords: Uranyl complexes ; calixarenes ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The synthesis and crystal structure of the inclusion complex between uranyl and p-tert-butylcalix[5]arene are reported. [UO2 (p-tert-butylcalix[5]arene-4H]2- · $${\text{2HNE}}_{{\text{t}}_{\text{3}} }^{\text{ + }} $$ &·2MeOH(1) crystallizes in the monoclinic space group C2/c, a = 30.06(2), b = 18.20(3), c = 31.35(2) Å, β = 128.51(6)°, V = 13423(40) Å3, Z = 8. Refinement led to a final conventional R value of 0.043 for 4155 reflections. The uranyl ion is bonded, in its equatorial plane, to the five oxygen atoms of the calixarene, four of which are deprotonated. A protonated triethylamine molecule is located inside the calixarene cavity and hydrogen bonded to a uranyl oxygen atom, and another one outside and hydrogen bonded to a calixarene oxygen atom. The calixarene conformation is the usual cone one.
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    URL: http://dx.doi.org/10.1023/A:1007938218723
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  • 32
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    Electronic Resource
    Synthesis, Structure and Alkali Metal Ion Binding Properties of a Podand Polyether Derived from Calix[4]arene, 5,11,17,23-tetra-tert-butyl-25,27-di(phenylmethoxy)-26,28-di(2‘-methoxyethoxy)-calix[4]arene (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 27 (1997), S. 291-302 
    Details
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; polyether ; crystal structure ; alkali metal ion binding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The ligand 5,11,17,23-tetra-t-butyl-25,27-di(phenylmethoxy)-26,28-di(2-methoxy-ethoxy)calix[4]arene,designed as an analogue of some calixcrown speciesin order to evaluate possible origins of their selectivity in alkali metal ion binding, has been synthesised and structurally characterised by X-ray crystallography. The crystals are monoclinic, P21/n, a = 15.940(6), b = 19.388(5), c = 20.020(5) Å,β = 109.10(2) deg., Z = 4, conventional R on |F| being 0.073 for 3454 independent, ’observed‘ (I 〉 3σ(I)) reflections. 1H-NMR studies in 1:1 CD3CN/CDCl3solvent have shown that the ligand exerts a strong preference for the lighteralkali metal ions (Li+ and Na+) contrary to the binding behaviour of knowncalixcrowns. This may reflect interactions restricted to the lower rim donor atoms without concomitant interaction with the calixarene π-electrons, perhaps because the latter interactions are substituted by those with the benzyl group π-electrons.
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    URL: http://dx.doi.org/10.1023/A:1007981710765
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  • 33
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    Polymorphism of Inclusion Complexes and Unsolvated Hosts. V. Crystal Structure of the α-Dimorph of the 1 : 2 Dianilinegossypol–DMSO Complex and a 1 : 1 : 1 Inclusion Complex Based on a Mixed Dianilinegossypol/1,4-Dioxane Host Matrix and 1,2-Dichloroethane Guest (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 29 (1997), S. 23-32 
    Details
    ISSN: 1573-1111
    Keywords: Dianilinegossypol ; crystal structure ; host–guest complexes ; H-bond ; α- and β-dimorphs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Dianilinegossypol forms a 1 : 2 host-guest complex with DMSO:monoclinic, space group P21/n, a = 8.522(3), b = 18.034(4), c= 28.462(6) Å, β = 94.14(2)°, V = 4362Å3, Z = 4, D x = 1.26 g cm-3, T = 295 K.Final R value is 0.102 for 1793 observed reflections. A 1 : 1 : 1 adduct ofdianilinegossypol with 1,4-dioxane and 1,2-dichloroethane is found to beisostructural with the dianilinegossypol complex with DMSO: monoclinic,space group P21/n, a = 8.281(2), b = 19.245(3), c = 27.970(7)Å, β = 95.18°, V = 4439 Å3, Z = 4, D x =1.28 g cm-3, T = 295 K. Final R value is 0.114 for 2458observed reflections.The host molecules are associated by O(4)—H ...O(3) H-bonds toinfinite chains running in the direction of the c-axis The chains areincorporated into layers through 1,4-dioxane or DMSO molecules havingH-bonds with dianilinegossypol molecules. Another DMSO or 1,2-dichloroethanemolecule is included as a guest in the channels formed between the layers.At 60 °C a cryptate-type inclusion complex of dianilinegossypol isformed with DMSO or 1,4-dioxane. It is isostructural with the acetonecomplex reported in Part IV of the present series.
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    URL: http://dx.doi.org/10.1023/A:1007992116261
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  • 34
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    p-tert-Butylcalix[5]arene: a New Synthetic Pathway and Crystal Structure of the N,N-Dimethylformamide Complex (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 29 (1997), S. 175-185 
    Details
    ISSN: 1573-1111
    Keywords: p-tert-Butylcalix[5]arene ; synthesis ; complexation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The formation of p-tert-butylcalix[5]arene by the opening ofp-tert-butyldihomooxacalix [4]arene and the addition of a monomer has beenstudied. Various facets, including the effects of bases and the nature ofthe monomer added to the p-tert-butyldihomooxacalix[4]arene, have beeninvestigated. p-tert-Butylcalix[5]arene can be prepared in yields up to30%. The structure of its 1 : 2 complex with DMF has been determinedby X-ray crystallography. Crystals are triclinic, space group P¯1, a =1428.2(3) pm, b = 1837.3(3) pm, c = 1276.1(2) pm, α = 108.98(1)°,β = 105.02(2)°, γ = 95.21(1)°, Z = 2, D c = 1.059 kg m-3,final R value = 0.087. The macrocycle adopts a cone conformation, one guestenclosed inside the cavity, the other one outside.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1007907525620
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    Synthesis of Two New Glycophanes Comprised of Thioglucose Molecules Linked by Hydrocarbons (1997)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 29 (1997), S. 335-346 
    Details
    ISSN: 1573-1111
    Keywords: Glycophane ; macrocycle ; carbohydrate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Preparation of two new glycophanes is reported. These compounds arecomprised of two glucose molecules linked by hydrocarbon units at the 1,1′ and 3, 3′ or 3, 3′ and 6, 6′ positions. Thecrystal structure of one of the glycophanes is also described.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1007952822709
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  • 36
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    Synthesis, conformation, and biological activity of two fMLP-OMe analogues containing the new 2-[2′-(methylthio) ethyl] methionine residue (1997)
    New York : Wiley-Blackwell
    Biopolymers 42 (1997), S. 415-426 
    Details
    ISSN: 0006-3525
    Keywords: chemotaxis ; conformation ; crystal structure ; Cα-tetrasubstituted amino acids ; formylpeptides ; 2-[2′-(methylthio)ethyl]methionine ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new Cα-tetrasubstituted α-amino acid residue 2-[2′-(methylthio) ethyl]methionine (Dmt) has been introduced into the reference chemotactic tripeptide HCO-Met-Leu-Phe-OMe (fMLP-OMe) in place of the leucine or methionine, respectively. The biological activity of the new analogues [Dmt2] fMLP-OMe (2) and [Dmt1] fMLP-OMe (3) has been determined; whereas 2 is active toward human neutrophils, stimulating directed migration, superoxide anion generation, and lysozyme release, 3 results practically inactive in all tested assays. A conformational analysis on 2 and 3 has been performed in solution by using ir absorption and 1H-nmr. The conformation of 2 was also examined in the crystal by x-ray diffraction methods. Both 2 and 3 adopt fully extended conformation in correspondence with the Dmt residue. Biological and conformational results are discussed and compared with related previously studied models. © 1997 John Wiley & Sons, Inc. Biopoly 42: 415-426, 1997
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  • 37
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    Role of two consecutive α,β-dehydrophenylalanines in peptide structure: Crystal and molecular structure of Boc-Leu-ΔPhe-ΔPhe-Ala-Phe-NHMe (1997)
    New York : Wiley-Blackwell
    Biopolymers 42 (1997), S. 373-382 
    Details
    ISSN: 0006-3525
    Keywords: x-ray diffraction ; crystal structure ; dehydrophenylalanine ; constrained peptides ; 310-helix ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An Nα-protected model pentapeptide containing two consecutive ΔPhe residues, Boc-Leu-ΔPhe-ΔPhe-Ala-Phe-NHMe, has been synthesized by solution methods and fully characterized. 1H-nmr studies provided evidence for the occurrence of a significant population of a conformer having three consecutive, intramolecularly H-bonded β-bends in solution. The solid state structure has been determined by x-ray diffraction methods. The crystals grown from aqueous methanol are orthorhombic, space group P212121, a = 11.503(2), b = 16.554(2), c = 22.107(3) Å, V = 4209(1) Å,3 and Z = 4. The x-ray data were collected on a CAD4 diffractometer using CuKa radiation (λ = 1.5418 Å). The structure was determined using direct methods and refined by full-matrix least-squares procedure. The R factor is 5.3%. The molecule is characterized by a right handed 310-helical conformation (〈φ〉 = -68.2°, 〈ψ〉 = -26.3°), which is made up of two consecutive type III β-bends and one type I β-bend. In the solid state the helical molecules are aligned head-to-tail, thus forming long rod like structures. A comparison with other peptide structures containing consecutive ΔPhe residues is also provided. The present study confirms that the -ΔPhe-ΔPhe-sequence can be accommodated in helical structures. © 1997 John Wiley & Sons, Inc. Biopoly 42: 373-382, 1997
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  • 38
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    Electronic Resource
    RNA crystallography (1997)
    New York : Wiley-Blackwell
    Biopolymers 44 (1997), S. 3-21 
    Details
    ISSN: 0006-3525
    Keywords: RNA ; x-ray crystallography ; crystal structure ; transfer RNA ; ribozyme ; catalytic RNA ; internal loop ; review ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The current state of three-dimensional structure analysis of RNA by x-ray crystallograpy is summarized. The methods of sample preparation, crystallization, data collection, and structure solution are discussed, followed by a review of the RNA structures that have been determined and of common structural features, and finally, an appraisal of future prospects for x-ray crystal structure analysis of RNA. © 1997 John Wiley & Sons, Inc. Biopoly 44: 3-21, 1997
    Additional Material: 5 Ill.
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  • 39
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    Crystalline structure of poly(methyl-n-propylsilane) (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 1533-1543 
    Details
    ISSN: 0887-6266
    Keywords: polysilane ; lamellar microstructure ; crystal structure ; crystallization kinetics ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The thermal behavior and physical structure of atactic poly(methyl-n-propylsilane) (PMPrS) have been investigated by complementary techniques. Temperature-dependent wide-angle X-ray scattering as well as thermal analysis clearly indicate that atactic PMPrS crystallizes below 40°C in a monoclinic lattice with PMPrS adopting an all-trans planar zigzag conformation. Above 40°C, the polymer is in the isotropic amorphous state. A restricted analysis of the structure factors of PMPrS has been performed, indicating that the zigzag planes most probably lie in (110) planes. The chains pack with little interpenetration, and the crystals may be considered as bundles of long, closely packed prisms. The restricted interlocking of neighboring chains results, in turn, in a poor register of the chains along the c-axis. Moreover, transmission electron microscopy reveals that the crystallized polymer adopts a lamellar microstructure, with parallel lamellae tending to form tight bundles. Both electron microscopy and small-angle X-ray scattering indicate crystal thicknesses of about 60 Å. Finally, PMPrS was found to crystallize with a nucleation-controlled type of kinetics. Avrami exponents were calculated as n ≈ 1, suggesting a fibrillar growth geometry compatible with the absence of spherulitic superstructure. A double-melting behavior is also observed for PMPrS. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 1533-1543, 1997
    Additional Material: 11 Ill.
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  • 40
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    Electron diffraction and computer modeling of poly(naphthalic anhydride) crystal structure (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 1575-1588 
    Details
    ISSN: 0887-6266
    Keywords: poly(naphthalic anhydride) ; crystal structure ; electron diffraction ; confined thin film melt polymerization ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Single crystals of poly(naphthalic anhydride) (PNA) have been grown using our confined thin film melt polymerization technique. Lamellae, 70-100 Å thick, are found for the crystals polymerized at 180°C with thinner lamellae for a 200°C polymerization temperature. In addition, irregular lath-shaped crystals are found for both polymerization temperatures, apparently formed by a solid-state polymerization process within the original needle-like monomer crystals. The crystal structure of PNA has been studied by electron diffraction (ED) and computer modeling based on seven different zonal ED patterns. It is found that, in most cases, two or three different zonal patterns are superimposed with a common plane, suggesting variable chain tilting even in individual lamellae. Shearing of the material shortly after the initiation of polymerization, permitted obtaining an additional [010] zone ED pattern. A monoclinic unit cell with one chain, two repeat units is proposed based on measurements of 21 independent reflections; the space group is Pc11; a = 6.26 Å, b = 4.33 Å, c = 18.60 Å, and α = 122.5°. The computer-simulated (Cerius2) molecular conformation and chain packing are described with the corresponding simulated electron diffraction patterns being in good agreement with the observed ones. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 1575-1588, 1997
    Additional Material: 10 Ill.
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  • 41
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    Hexabromotricyclobutabenzene and Hexabromohexaradialene: Their Nickel-Mediated One-Pot Syntheses and Crystal Structure (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 208-210 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; cyclobutenes ; nickel ; radialenes ; radical reactions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of hexakis(dibromomethyl)benzene with [(Bu3P)2-Ni(COD)] (COD = 1,5-cyclooctadiene) in DMF at 65-70°C yielded a mixture of the title compounds. The mixture was separated by column chromatography to yield hexabromotricyclobutabenzene (3 a) and hexabromohexaradialene (4) in 24 and 16% yields, respectively. 1H and 13C NMR spectroscopy suggest that 3 is obtained as the syn-all-trans isomer 3 a, and the symmetric anti-all-trans isomer 3 b is not obtained at all. The X-ray structures of 3 a and 4 are reported. The hexaradialene 4 has a chair conformation, and deviates from planarity by 43.6°. Heat or radical impurities cause the clean transformation of 3 a to 4.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19970030207
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  • 42
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    Two New Closely Related MoV Hydroxymonophosphates Built Up of Cd[Mo6P4O25(OH)6]2 And Cd[Mo6P4O26(OH)5]2 ClustersDedicated to Professor H. G. von Schnering on the occasion of his retirement (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 1797-1800 
    Details
    ISSN: 0947-6539
    Keywords: cadmium ; crystal structure ; hydrothermal synthesis ; hydroxyphosphate ; molybdenum ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two new molybdenum(v) hydroxyphosphates have been synthesized hydrothermally, Na2Cd3(Mo2O4OH)6-(PO4)2(PO3OH)6[N(CH3)4]4·10H20 (1) and Cd9(Mo2O4OH)12(PO4)6(PO3OH)10-[N(CH3)4]8·15H2O (2). Their structures have been determined from single-crystal X-ray diffraction. The water molecules and hydroxyl groups have been deduced from valence calculations. Both compounds crystallize in the triclinic space group P1, with the cell parameters for 1 a = 12.340(2), b = 12.596(1), c = 14.717(2) Å, α = 107.24(1)°, β = 89.83(1)°, γ = 114.31(1)°, V = 1972.3(4) Å3, and for 2 a = 11.942(1), b = 13.339(2), c = 26.765(3) Å, α = 85.33(1)°, β = 86.87(1)°, γ = 64.08(1)°, V = 3821.3(9) Å3. The two frameworks can be described on the basis of similar [Mo6P4X31]n- (X = O, OH) anionic clusters, but 1 is a tridimensional structure, whereas 2 exhibits a monodimensional structure.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19970031111
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  • 43
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    Morphology, crystal structure, and orientation of poly-p-oxybenzoate on mica (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 1807-1820 
    Details
    ISSN: 0887-6266
    Keywords: poly(p-oxybenzoate) ; confined thin film melt polymerization ; epitaxy ; mica substrate ; morphology ; crystal structure ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polymerization of p-acetoxybenzoic acid between mica sheets, from both the melt and dilute solution, in a wide range of polymerization temperatures (180-400°C) yields an epitaxial-like overgrowth of PpOBA on the mica cleavage surface. The PpOBA overgrowth forms long rows by lateral aggregation of ribbon crystals situated in three substrate directions rotated by 60°. The c-axes of the PpOBA phase I and II lattices are parallel to the 001 plane of the mica, coinciding with the a-axes of the mica hexagonal structure. The aI- and bII-axes lie predominantly on the mica surface. The surface-orienting effect is tentatively attributed to surface steps and or/polar effects; lattice matching does not occur. The recrystallization of bulk polymer samples previously prepared also leads to ordering between mica like that in melt or solution polymerization. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 1807-1820, 1997
    Additional Material: 12 Ill.
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  • 44
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    Structural transformation of ultra-high modulus and molecular weight polyethylene fibers by high-temperature wide-angle X-ray diffraction (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 623-630 
    Details
    ISSN: 0887-6266
    Keywords: ultra-high modulus and molecular weight polyethylene fibers (UHM-WPE) ; high-temperature wide-angle x-ray diffraction (HTWAXD) ; crystal structure ; orthorhombic/monoclinic/pseudohexagonal transformation ; annealing and thermal behavior ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Wide-angle x-ray diffraction (WAXD) of the ultra-high modulus and molecular weight polyethylene (UHMWPE) fibers at room temperature shows a predominantly orthorhombic structure with trace amount of nonorthorhombic crystals and very low amorphous contents. The calculated unit cell dimensions a and b of the orthorhombic crystals are 7.36 (±0.04) Å, and 4.89 (±0.04) Å, respectively. The apparent crystallite sizes perpendicular to the orthorhombic 110 and 200 reflection planes are 169.8 and 143.4 Å, respectively. The crystallite size perpendicular to the nonorthorhombic 010 reflection is 149.4 Å. The crystal density is calculated to be 1.02 g/cc. With increasing temperature, the thermal expansion coefficient in the a direction is much higher than that in the b direction which explains the structural transformation from the orthorhombic crystals to a pseudohexagonal form. Tension along the fiber axis while being heated during the high-temperature x-ray diffraction (HTWAXD) scanning has shown enhanced structural transformation from the orthorhombic form to the monoclinic form. Structural transformation from the orthorhombic form to the pseudohexagonal phase is not observed on the UHMWPE fibers under axial tension or annealing conditions in HTWAXD. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys, 35: 623-630, 1997
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  • 45
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    A study of the dilation of the unit cell of metallocene isotactic poly(propylenes): The monoclinic form (1997)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 35 (1997), S. 2511-2521 
    Details
    ISSN: 0887-6266
    Keywords: isotactic poly(propylenes) ; unit-cell density ; crystal structure ; unit-cell parameters ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The lattice parameters of a series of monoclinic metallocene poly(propylenes) of constant molecular weight are measured as a function of defect content, that vary between 0.3 and 2.35 total defects per 100 monomeric units. The parameters are also measured as a function of molecular weight for a fixed defect content and as a function of the crystallization temperature. The b axis is found to increase with decreasing isothermal crystallization temperature whereas only small changes are found for samples rapidly crystallized. The a and c axis showed basically no variation with crystallization temperature. The parameters of the unit cell were essentially constant with varying defect content in the poly(propylene) chain. Lack of observed effect on the dilation of the unit cell by increasing defects is a consequence of the rapid crystallization required to ensure formation of monoclinic crystals. The unit cell parameters increased as a mild function of the molecular weight. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 2511-2521, 1997
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  • 46
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    Crystal structure of the bovine α-chymotrypsin:kunitz inhibitor complex. An example of multiple protein:protein recognition sitesThis paper is dedicated to Professor A. Ballio on the occasion of his 75th birthday. (1997)
    Chicester [u.a.] : Wiley-Blackwell
    Journal of Molecular Recognition 10 (1997), S. 26-35 
    Details
    ISSN: 0952-3499
    Keywords: bovine α-chymotrypsin ; bovine basic pancreatic trypsin inhibitor (Kunitz-type inhibitor) ; serine proteinase:Kunitz inhibitor complex ; crystal structure ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: The crystal structure of bovine α-chymotrypsin (α-CHT) in complex with the bovine basic pancreatic trypsin inhibitor (BPTI) has been solved and refined at 2.8 Å resolution (R-factor=0.18). The proteinase:inhibitor complex forms a compact dimer (two α-CHT and two BPTI molecules), which may be stabilized by surface-bound sulphate ions, in the crystalline state. Each BPTI molecule, at opposite ends, is contacting both proteinase molecules in the dimer, through the reactive site loop and through residues next to the inhibitor's C-terminal region. Specific recognition between α-CHT and BPTI occurs at the (re)active site interface according to structural rules inferred from the analysis of homologous serine proteinase:inhibitor complexes. Lys15, the P1 residue of BPTI, however, does not occupy the α-CHT S1 specificity pocket, being hydrogen bonded to backbone atoms of the enzyme surface residues Gly216 and Ser217. © 1997 John Wiley & Sons, Ltd.
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    Metal-Template Electrophilic Substitution on Phenols: Synthesis and Crystal Structure of Bromomagnesium Phenolate and Its Reactive Complex with para-IsopropylbenzaldehydeDedicated to the memory of Professor Giuseppe Casnati on the 4th anniversary of his death (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 1269-1272 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; electrophilic aromatic substitutions ; magnesium ; regioselectivity ; template synthesis ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal structures of the bromomagnesium phenolate 5 and its complex 7 with para-isopropylbenzaldehyde are reported; for the first time it has been possible to demonstrate that the reactive complex 7, responsible for the complete ortho-regioselective control in the alkylation of phenoxymagnesium bromides with aldehydes, is not obtained by simple replacement of the ethereal ligand but by expansion of the metal coordination sphere from 4 (usual tetrahedral configuration) to 5. We infer from 1H NMR studies that the magnesium coordination of complex 7 in solution is analogous to that shown in the solid state, with a complexed ethereal molecule.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19970030814
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    Synthesis of Pyrazinoporphyrazine Derivatives Functionalised with Tetrathiafulvalene (TTF) Units: X-Ray Crystal Structures of Two Related ttf Cyclophanes and Two Bis(1,3-Dithiole-2-Thione) IntermediatesDedicated to Professor Fabian Gerson on the occasion of his retirement (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 1679-1690 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; cyclophanes ; electrochemistry ; porphyrazines ; tetrathiafulvalenes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The pyrazinoporphyrazine system 13 (metal-free, zinc and copper derivatives) has been synthesised by tetramerisation of 2,3-dicyanopyrazine monomer unit 10. The structure of 13a-c has been established by 1H NMR spectroscopy, UV/Vis spectrophotometry, MALDI-TOF mass spectrometry, cyclic voltammetry and differential pulse voltammetry. The electrochemical redox behaviour of 13a-c is strongly solvent dependent. The expected two-stage oxidation of the tetrathiafulvalene (TTF) units of 13a-c was observed in a range of solvents; in addition, oxidation and reduction of the pyrazinoporphyrazine core of the metal-free derivative 13a was detected in benzonitrile. On excitation of 13 in the Q-band region no fluorescence was observed, which is presumably the consequence of intramolecular charge transfer between the TTF moieties and the excited state of the central porphyrazine. Molecular modelling studies on 13a and 13c are reported. During the course of this work, the novel TTF macrocycles 11 and 20 were synthesised; their X-ray crystal structures reveal severely bent TTF units, the conformations of which are discussed in detail. The X-ray crystal structures of the bis(1,3-dithiole) systems 15 and 18 have also been determined.
    Additional Material: 10 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19970031018
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    The Unusual Properties of 5-Methyl-4,5,6,7-Tetrahydro-1H-Indazole in the Solid State (1997)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 3 (1997), S. 121-126 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; NMR spectroscopy ; proton transfer ; pyrazoles ; tautomerism ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The crystal structure of the title compound was determined by X-ray analysis at 200 K. Three independent molecules form a trimer joined by strong and linear N-H … N hydrogen bonds. There is another centrosymmetrically related trimer in the unit cell. Both tautomers (1H and 2H) are present in each trimer. Disorder of the NH protons involved in the N-H … N hydrogen bonds has been observed. Solid-state 13C CPMAS NMR was used to establish the dynamic nature of the NH-proton disorder, the title compound being the first example of proton transfer in a tautomeric mixture of pyrazoles with an equilibrium constant other than 1.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19970030119
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  • 50
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    Synthese und Kristallstruktur von Bis(1,2-dimethyl-5-nitro-imidazol)dichlorocobalt(II) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1201-1202 
    Details
    ISSN: 0044-2313
    Keywords: Cobalt(II) complex ; 1,2-dimethyl-5-nitro-imidazole ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Crystal Structure of Bis(1,2-dimetyl-5-nitro-imidazole)dichlorocobalt(II)Bis(1,2-dimethyl-5-nitro-imidazol)dichlorocobalt(II) was obtained by reaction of CoCl2 · 6 H2O with 1,2-dimethyl-5-nitro-imidazole in methanol. The compound forms blue crystals which were characterized by IR and UV-vis spectroscopy and by an X-ray crystal structure determination. Co(C5H7N3O2)2Cl2: tetragonal, space group I42d, Z = 8, a = 1142.1(1) pm, c = 2577.3(2) pm. R = 0.036 for 670 independent reflexions. The Co atom is tetrahedrally surrounded by two chlorine and two N atoms at distances of 222.8(2) and 203.5(4) pm.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230802
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    Tetraammin-Lithium-Kationen zur Stabilisierung phenylsubstituierter Zintl-Anionen: Die Verbindung [Li(NH3)4]2[Sn2Ph4] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1503-1505 
    Details
    ISSN: 0044-2313
    Keywords: Ditetraammine lithium tetraphenyldistannide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH3)4]2[Sn2Ph4]Ruby-red, brittle single crystals of [Li(NH3)4]2[Sn2Ph4] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at -35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1, Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R1 (F02 ≥ 4σF02) = 5.13%, wR2 (F02 ≥ 4σF02) = 10.5%, N(F02 ≥ 4σF02) = 779, N(Var.) = 163.The compound contains to Sb2Ph4 isosteric centres [Sn2Ph4]2- as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231006
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    Bi13Pt3I7: Ein Subiodid mit einer pseudosymmetrischen Schichtstruktur (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1535-1541 
    Details
    ISSN: 0044-2313
    Keywords: Bismuth platinum iodide ; subhalide ; crystal structure ; pseudo-symmetry ; stacking faults ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bi13Pt3I7: A Subiodide with a Pseudo-Symmetric Layer StructureThe reaction of PtI2 with Bi and BiI at 630 K yields black, lustrous, air insensitive crystals of the subiodide Bi13Pt3I7. The layered crystal structure (triclinic, C1, a = 1581.0(2) pm, b = 912.6(1) pm, c = 2149.6(6) pm, α = 90.03(2)°, β = 96.96(2)°, γ = 90.11(1)°, V = 3078.6 · 106 pm3) contains edge-sharing [PtBi8/2] cubes, which form nets of Kagomé type. Iodine atoms fill the hexagonal-prismatic voids therein. These ∞2[(PtBi8/2)3I] layers are alternately separated by layers of iodine atoms or ∞1[BiI4-] zigzag-chains. The marked pseudo-symmetry of the structure favours stacking faults, which cause streaks of diffuse scattering in the diffraction pattern.
    Notes: Aus der Reaktion von PtI2 mit Bi und BiI bei 630 K erhält man schwarze, metallisch glänzende und luftbeständige Kristalle des Subiodids Bi13Pt3I7. In der schichtartig aufgebauten Kristallstruktur (triklin, C1, a = 1581,0(2) pm, b = 912,6(1) pm, c = 2149,6(6) pm, α = 90,03(2)°, β = 96,96(2)°, γ = 90,11(1)°, V = 3078,6 · 106 pm3) liegen Kagomé-Netze aus kantenverknüpften [PtBi8/2]-Würfeln vor, deren hexagonal-prismatische Lücken mit Iodatomen gefüllt sind. Diese ∞2[(PtBi8/2)3I]-Schichten sind abwechselnd durch eine Lage von Iodatomen oder eine Schicht aus parallel angeordneten ∞1[BiI4-]-Zickzackketten getrennt. Die in der Struktur stark ausgeprägte Pseudosymmetrie begünstigt Stapelfehler, welche sich auch in diffusen Streifen im Beugungsbild äußern.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231011
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  • 53
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    Zur Kristallstruktur von CaZn2(OH)6 · 2 H2O (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1287-1289 
    Details
    ISSN: 0044-2313
    Keywords: Calcium hexahydroxodizincate dihydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of CaZn2(OH)6 · 2 H2OThe electrochemical oxidation of zinc in a zinc/iron-pair leads in an aqueous NH3 solution of calciumhydroxide at room temperature to colourless crystals of CaZn2(OH)6 · 2 H2O. The X-ray structure determination was now successful including all hydrogen positions.P21/c, Z = 2, a = 6.372(1) Å, b = 10.940(2) Å, c = 5.749(2) Å, β = 101.94(2)° N(F2o ≥ 3σF2o) = 809, N(Var.) = 69, R/RW = 0.011/0.012The compound CaZn2(OH)6 · 2H2O contains Zn2+ in tetrahedral coordination by OH- and Ca2+ in octahedral coordination by four OH- and two H2O. The tetrahedra around Zn2+ form corner sharing chains, three-dimensionally linked by isolated polyhedra around Ca2+. Weak hydrogen bridge bonds result between H2O as donor and OH-.
    Notes: Die elektrochemische Oxidation von Zink in einem Zink/Eisen-Paar führt in einer wäßrigen NH3-Lösung von Calciumhydroxid bei Raumtemperatur zu farblosen Kristallen von CaZn2(OH)6 · 2 H2O. An ihnen wurde röntgenographisch die Struktur jetzt einschließlich aller H-Lagen bestimmt.P21/c, Z = 2, a = 6,372(1) Å, b = 10,940(2) Å, c = 5,749(2) Å, β = 101,94(2)° Z(F2o ≥ 3σF2o) = 809, Z(Var.) = 69, R/RW = 0,011/0,012In CaZn2(OH)6 · 2 H2O ist Zn2+ tetraedrisch von OH- und Ca2+ oktaedrisch von vier OH- und zwei H2O umgeben. Die Tetraeder um Zn2+ bilden Ketten über gemeinsame Ecken, die durch voneinander isolierten Oktaedern um Ca2+ dreidimensional verknüpft werden. Es liegen schwache H-Brückenbindungen von H2O als Donator zu OH- vor.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230819
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    Pseudoelementverbindungen. XI. [1] Untersuchungen zum Komplexbildungsverhalten von Cyanamidonitrat [NO2NCN]-Professor Wolfgang Beck zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1299-1305 
    Details
    ISSN: 0044-2313
    Keywords: Pseudoelement compounds ; cyanamidonitrate ; copper(I) ; silver(I) ; platinum(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pseudoelement Compounds. XI. [1] Investigations on the Coordination Behaviour of Cyanamidonitrate [NO2NCN]-With the ionic, potentially ambidentate ligand cyanamidonitrate complexes of the types [MX(PPh3)3], [MX(PPh3)2]2 (M=CuI, AgI) and trans-[Pt(H)X(PPh3)2] (X-=[NO2NCN]-) are introduced. The new compounds are characterized by 1H NMR, 31P NMR, and IR spectroscopy. The crystal structures of [Cu(NO2NCN)(PPh3)2]2 and [Ag(NO2NCN)(PPh3)2]2 are reported. In the complexes [MX(PPh3)3] and trans-[Pt(H)X(PPh3)2] cyanamidonitrate is unidentately coordinated through the nitrile group end-on. In the dimeric complexes [MX(PPh3)2]2 the anion acts bidentately as a bridging ligand. Surprisingly, both coordinative bonds are formed through nitrogen atoms of the NCN group.
    Notes: Es werden mit dem ionischen, potentiell ambidenten Liganden Cyanamidonitrat Komplexe der Typen [MX(PPh3)3], [MX(PPh3)2]2 (M=CuI, AgI) sowie trans-[Pt(H)X(PPh3)2] (X-=[NO2NCN]-) vorgestellt. Die Verbindungen wurden 1H-NMR-, 31P-NMR- und IR-spektroskopisch charakterisiert. Für [Cu(NO2NCN)(PPh3)2]2 und [Ag(NO2NCN)(PPh3)2]2 liegen Kristallstrukturanalysen vor.Cyanamidonitrat wird in den Komplexen [MX(PPh3)3] und trans-[Pt(H)X(PPh3)2] einzähnig über das endständige N-Atom der Nitrilgruppe koordiniert. In den dimeren Komplexen [MX(PPh3)2]2 liegt das Anion als zweizähniger Brükkenligand vor. Überraschend werden beide koordinativen Bindungen über die Stickstoffatome der NCN-Gruppe ausgebildet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230821
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    Kristallstruktur der Tieftemperaturmodifikation von RuTe2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1657-1660 
    Details
    ISSN: 0044-2313
    Keywords: Ruthenium ; chalcogenide ; chemical transport ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of the Low Temperature Modification of RuTe2Black shining, platelet like single crystals of α-RuTe2 were obtained by chemical transport reaction with Cl2/AlCl3 (crystal dimensions up to 1 mm). The crystal structure of this low temperature modification of α-RuTe2 hitherto only known from powder measurements, was redetermined at room temperature by single crystal X-ray diffraction on a four-circle diffractometer. α-RuTe2 crystallizes in the marcasit structure typ in the orthorhombic spacegroup Pnnm (No. 58) with the lattice constants a = 528.12(13), b = 639.43(19), c = 400.85(13) pm.
    Notes: Durch chemischen Transport mit dem Transportmittel Cl2/AlCl3 konnten schwarzglänzende, plattenartige Einkristalle von α-RuTe2 erhalten werden (Kantenlänge bis zu 1 mm). Die Kristallstruktur dieser bisher nur aus Pulverdaten bekannten Tieftemperaturmodifikation von RuTe2 wurde röntgenographisch an einem Einkristall auf einem Vierkreisdiffraktometer bei Raumtemperatur neu bestimmt. α-RuTe2 kristallisiert im Markasit-Strukturtyp in der orthorhombischen Raumgruppe Pnnm (Nr. 58) mit den Gitterkonstanten a = 528,12(13), b = 639,43(19), c = 400,85(13) pm.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231029
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    Mesityloxomolybdän- und -wolfram-Verbindungen. I. Die Struktur von LiMoO2Me2Mes(OEt2)2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1661-1664 
    Details
    ISSN: 0044-2313
    Keywords: Organo molybdenum compounds ; oxo complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mesityl Oxo Molybdenum and Tungsten Compounds. I. Structure of LiMoO2Me2Mes(OEt2)2LiMoO2Me2Mes(OEt2)2 2 is prepared by literature method [2] from MoO2Mes2 1 and LiMe. Its x-ray structure and NMR-spectral data are presented. 2 adopts a dimer structure in which two [MoO2Me2Mes]- anions are linked via two bridging [Li(OEt2)2]+ cations bonded to the oxo ligands. The resulting [‥OMoOLi‥]2 ring is planar.
    Notes: Die Struktur der bekannten, aus MoO2Mes2 1 und LiMe dargestellten Verbindung LiMoO2Me2Mes(OEt2)2 2 [2] sowie ihre NMR-spektroskopischen Daten werden mitgeteilt. 2 bildet ein in der Raumgruppe P1 kristallisierendes Dimer durch Verknüpfung zweier [MoO2Me2Mes]--Anionen über Oxo-Liganden durch zwei Kationen [Li(OEt2)2]+. Der gebildete [‥OMoOLi‥]2- Achtring ist eben.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231030
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    Die 3-(N,N-Dimethylamino)prop-1-enyl-Gruppe als Chelatligand in Organoindium-Verbindungen (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1679-1683 
    Details
    ISSN: 0044-2313
    Keywords: Organoindium compounds ; chelate complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The 3-(N,N-Dimethylamino)prop-1-enyl Group as a Chelate Ligand in Indium OrganylsInBr3 reacts with Me2NCH2CH=CHMgCl (molar ratio 1 : 2) to form (Me2NCH2CH=CH)2InBr (1) as the first indium alkenyl compound with amino-functionalized alkenyl groups. The X-ray structure determination shows the formation of a chelate complex. 1 crystallizes in the orthorhombic space group Fddd with the unit cell parameters a = 14.904(2) Å, b = 17.140(1) Å and c = 21.035(2) Å. By reaction of Me2InBr with Me2NCH2CH=CHMgCl (molar ratio 1 : 1) (Me2NCH2CH=CH)InMe2 (2) is formed as a colorless, at room temperature liquid, monomeric compound. The n.m.r. and mass spectra are discussed.
    Notes: InBr3 reagiert mit Me2NCH2CH=CHMgCl (Molverhältnis 1 : 2) in Diethylether als Lösungsmittel zu (Me2NCH2CH=CH)2InBr (1), der ersten Indium-Alkenylverbindung mit aminofunktionalisierten Alkenylresten. Die Röntgenkristallstrukturanalyse zeigt das Vorliegen eines Chelatkomplexes an. 1 kristallisiert orthorhombisch in der Raumgruppe Fddd mit Z = 16, a = 14,904(2) Å, b = 17,1405(14) Å und c = 21,035(2) Å. Aus Me2InBr und Me2NCH2CH=CHMgCl (Molverhältnis 1 : 1) wurde (Me2NCH2CH=CH)InMe2 (2) als farblose, bei Raumtemperatur flüssige, monomere Verbindung erhalten. Die 1H- und 13C-NMR-Spektren sowie Massenspektren werden mitgeteilt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231033
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    Contributions on thermal behaviour and crystal chemistry of anhydrous phosphates. XIX. Tri-chromium(II)-bis-phosphate Cr3(PO4)2 (≙ Cr6(PO4)4) - A transition metal(II)-orthophosphate with new structure type (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1672-1678 
    Details
    ISSN: 0044-2313
    Keywords: Chromium(II)-orthophosphate ; crystal growth ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Beiträge zum thermischen Verhalten und zur Kristallchemie von wasserfreien Phosphaten. XIX. Tri-chrom(II)-bis-phosphat Cr3(PO4)2 (≙ Cr6(PO4)4) - Ein Übergangsmetall(II)- Orthophosphat mit neuem StrukturtypIntensiv blau-violette Kristalle des bislang unbekannten Tri-chrom(II)-bis-phosphats, Cr3(PO4)2, entstehen bei der Reduktion von CrPO4 mit Chrom oberhalb von 1050°C (evakuierte Quarzglasampullen, wenige mg NH4I oder I2 als Mineralisator). Die Kristallstruktur von Cr3(PO4)2 enthält sechs kristallographisch unabhängige Cr2+ in der Elementarzelle (P212121, Z = 8, a = 8,4849(10) Å, b = 10,3317(10) Å, c = 14,206(3) Å). Davon sind fünf in der ersten Koordinationssphäre von vier Sauerstoffatomen leicht verzerrt quadratisch-planar umgeben (1,96 Å ≤ d(Cr—O) ≤ 2.15 Å). Deren Koordination wird vervollständigt durch zwei bzw. drei weiter entfernte Sauerstoffatome (2,32 Å ≤ d(Cr—O) ≤ 3,21 Å). Das sechste Cr2+-Ion ist stark verzerrt oktaedrisch koordiniert (d(Cr—O): 1,97, 2,04, 2,15, 2,28, 2,29, 2,53 Å).Die vier kristallographisch unterschiedlichen [PO4]-Gruppen zeigen nur geringe Abweichungen von der Geometric eines idealen Tetraeders (1,51 Å ≤ d(P—O) ≤ 1,57 Å; 104,3° ≤ ∠(O—P—O) ≤ 114,4°).Für die Cr2+ wurde mit μexp = 4,28(2) μB (θP = -54,8(5) K) ein ungewöhnlich niedriges mittleres magnetische Moment gefunden.
    Notes: Deep blue-violet single crystals of hitherto unknown chromous orthophosphate have been obtained reducing CrPO4 by elemental Cr at temperatures above 1050°C in evacuated silica ampoules (NH4I or I2 as mineraliser). The complex structure of Cr3(PO4)2 (P212121, Z = 8, a = 8.4849(10) Å, b = 10.3317(10) Å, c = 14.206(2) Å) contains six crystallographically independent Cr2+ per unit cell. Five of them are coordinated by four oxygen atoms which form a distorted (roof shaped) square plane as first coordination sphere at interatomic distances 1.96 Å ≤ d(Cr—O) ≤ 2.15 Å. Their coordination is completed by additional oxygen atoms (2 or 3) at distances 2.32 Å ≤ d(Cr—O) ≤ 3.21 Å. The sixth Cr2+ shows six-fold octahedral coordination with strong radial distortion (d(Cr—O): 1.97, 2.04, 2.15, 2.28, 2.29, 2.53 Å).The four different [PO4] groups exhibit only minor deviations from ideal tetrahedral geometry (1.51 Å ≤ d(P—O) ≤ 1.57 Å, 104.3° ≤ ∠(O—P—O) ≤ 114.4°).An unusually low magnetic moment μexp = 4.28(2) μB (θP = -54.8(5) K) has been observed for Cr2+.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231032
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    Über den Einfluß von Temperatur, Druck und Substitution auf die Kristallstruktur von ARh2P2 (A = Ca, Sr, Eu, Ba)Professor Welf Bronger zum 65. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1418-1424 
    Details
    ISSN: 0044-2313
    Keywords: Ternary Rhodium phosphides ; crystal structure ; phase transition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About the Effect of Temperature, Pressure, and Substitution on the Crystal Structure of ARh2P2 (A = Ca, Sr, Eu, Ba)Four compounds ARh2P2 (A = Ca, Sr, Eu, Ba) were prepared by heating mixtures of the elements and investigated by means of single crystal X-ray methods. They crystallize in the ThCr2Si2 type structure (I4/mmm; Z = 2) with P—P distances along [001] reaching from 2.26 Å (CaRh2P2) to 3.74 Å (BaRh2P2). With increasing temperature (EuRh2P2) or increasing pressure (SrRh2P2) a first order phase transition occurs with strong changes of the P—P distances. Substitution of the atoms changes the bond lengths of the compounds too.
    Notes: Vier Verbindungen ARh2P2 (A = Ca, Sr, Eu, Ba) wurden durch Erhitzen entsprechender Elementgemenge dargestellt und hinsichtlich ihrer Kristallstruktur mit Hilfe von Einkristallmethoden charakterisiert. Sie kristallisieren in der tetragonalen ThCr2Si2-Struktur (I4/mmm; Z = 2) und unterscheiden sich im wesentlichen durch ihre P—P-Abstände längs [001]. Diese reichen von 2,26 Å bei CaRh2P2 bis 3,74 Å bei BaRh2P2 und verändern sich drastisch im Zuge von Phasenumwandlungen 1. Ordnung durch Temperaturerhöhung bei EuRh2P2 sowie unter erhöhtem Druck bei SrRh2P2. Substitution übt ebenfalls einen großen Einfluß auf den Strukturfeinbau der Verbindungen aus.
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    URL: http://dx.doi.org/10.1002/zaac.19976230917
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    Zur Kristallstruktur von Tb2Se3 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1744-1746 
    Details
    ISSN: 0044-2313
    Keywords: Terbium sesquiselenide ; chemical transport ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Tb2Se3Single crystals of Tb2Se3 could be prepared by chemical transport reaction with AlCl3. By starting from TbSe1.9 and terbium metal black needles of Tb2Se3 in the U2S3 type structure with the space group Pnma and a = 1113,0(1) pm, b = 402,4(1) pm and c = 1095,1(3) pm were obtained.
    Notes: Einkristalle von Tb2Se3 konnten durch chemischen Transport mit AlCl3 dargestellt werden. Ausgehend von pulverförmigem TbSe1,9 und Terbiummetall wurden schwarze, nadelförmige Einkristalle von Tb2Se3 im U2S3-Strukturtyp mit der Raumgruppe Pnma und a = 1113,0(1) pm, b = 402,4(1) pm und c = 1095,1(3) pm erhalten.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19976231113
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    Nitridsulfidchloride der Lanthanide: III. Synthese und Kristallstruktur von Pr5N3S2Cl2Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1747-1752 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanides ; nitride sulfide chlorides ; Pr5N3S2Cl2 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitride Sulfide Chlorides of the Lanthanides. III. Synthesis and Crystal Structure of Pr5N3S2Cl2By reacting praseodymium with sulfur, sodium azide and praseodymium trichloride in sealed, evacuated silica tubes (850°C, 7 d), the nitride sulfide chloride Pr5N3S2Cl2 is obtained in case of a 4:2:1:1 molar ratio of the reactants (Pr:S:NaN3:PrCl3). A slight excess of trichloride or the addition of NaCl as a flux supports the yield of brownish red, rod-shaped transparent crystals which prove to be stable against hydrolysis. The crystal structure (monoclinic, C2/m (no. 12), a = 1540.2(1), b = 400.92(3), c = 1656.3(1) pm, β = 101.24(1)°, Z = 4, R = 0.039, Rw = 0.028) was determined by means of X-ray single crystal data. Thus five crystallographically different cations (Pr3+) are present which with three distinct kinds of nitride anions (N3-) build up two types of translationally commensurate chains from interconnected [NPr4] tetrahedra. With an additional edge per “chain-link” in chain I, two single chains ∞1[NPr3/3ePr1/1t]3+ (≡∞1[NPr2]3+) of cis-edge connected [NPr4] tetrahedra (known from the Sm4N2S3-type structure) are condensed into the double chain ∞1[(N1){(Pr1)(2+2)/(2+2)e,e(Pr2)(2+1)/(2+1)e,v}(N2)(Pr3)1/1t]3+ (≡∞1[N2Pr3]3+). Chain II consists of two single chains ∞1[NPr2/2vPr2/1t] 6+ (≡∞1[NPr3]6+) of vertex-connected [NPr4] tetrahedra (known from the Sm3NS3-type structure), which are condensed to the double chain ∞1[(N3)(Pr4)2/2e(Pr5)2/2v]3+ (≡∞1[NPr2]3+) via an additional edge per “chain-link” too. Both types of chains are bundled along [010] like a closest packing of rods. Four crystallographically different but by X-ray diffraction indistinguishable anions S2- and Cl- hold both cationic double chains together and also adjust the charge balance in a molar ratio of 1 : 1.
    Notes: Durch Umsetzung von Praseodym mit Schwefel, Natriumazid und Praseodymtrichlorid in evakuierten Quarzglasampullen (850°C, 7 d) wird bei molaren Verhältnissen der Edukte (Pr:S:NaN3:PrCl3) von 4:2:1:1 das Nitridsulfidchlorid Pr5N3S2Cl2 erhalten. Ein geringer Überschuß an Trichlorid oder der Zusatz von NaCl als Flußmittel fördert die Bildung von braunroten, stäbchenförmigen, transparenten Kristallen, die sich als unempfindlich gegenüber Hydrolyse erweisen. Die Kristallstruktur (monoklin, C2/m (Nr. 12); a = 1540,2(1); b = 400,92(3); c = 1656,3(1) pm; β = 101,24(1)°, Z = 4; R = 0,039; Rw = 0,028) wurde röntgenographisch anhand von Einkristalldaten bestimmt. Danach liegen fünf kristallographisch unterschiedliche Kationen. (Pr3+) vor, die mit drei verschiedenen Sorten von Nitridionen (N3-) zwei Typen translationskommensurabler Stränge aus verknüpften [NPr4]-Tetraedern bilden. In Strang I werden zwei Einfachketten ∞1[NPr3/3kPr1/1t]3+ (≡∞1[NPr2]3+) cis-kantenverknüpfter [NPr4]-Tetraeder (bekannt aus der Sm4N2S3-Struktur) über eine zusätzliche Kante pro „Kettenglied“ zur Doppelkette ∞1[(N1){(Pr1)(2+2)/(2+2)k,k(Pr2)(2+1)/(2+1)k,e}(N2)(Pr3)1/1t]3+ (≡∞1[N2Pr3]3+) verknüpft. Strang II besteht aus zwei Einfachketten ∞1[NPr2/2ePr2/1t]6+ (≡∞1[NPr3]6+) eckenverknüpfter [NPr4]-Tetraeder (bekannt aus der Sm3NS3-Struktur), die über eine zusätzliche Kante pro „Kettenglied“ zur Doppelkette ∞1[(N3)(Pr4)2/2k(Pr5)2/2e]3+ (≡∞1[NPr2]3+) kondensiert sind. Beide Strangsorten ordnen sich längs [010] nach dem Motiv einer dichtesten Stabpackung an. Vier kristallographisch unterschiedliche, röntgenographisch jedoch nicht unterscheidbare Anionen S2- und Cl- sorgen für den Zusammenhalt der kationischen Doppelketten und regeln im molaren Verhältnis von 1 : 1 auch den Ladungsausgleich.
    Additional Material: 5 Ill.
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    Darstellung und Struktur eines Ammoniumdiamidodioxophosphats(V), NH4PO2(NH2)2Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1786-1790 
    Details
    ISSN: 0044-2313
    Keywords: Ammonium diamido dioxo phosphate(V) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of an Ammonium Diamidodioxophosphate(V), NH4PO2(NH2)2The ammonolysis of P3N5 under ammonothermal conditions (T = 400°C, p(NH3) = 6 kbar, 14 d in autoclaves) in the presence of small definite amounts of water leads to the formation of NH4PO2(NH2)2. The structure was solved by single crystal X-ray methods.NH4PO2(NH2)2: P21/c (Nr. 14), a = 6.886(1) Å, b = 8.366(2) Å, c = 9.151(2) Å, β = 111.78(3)°, Z = 4, R1/wR2 = 0.026/0.072, Z(Fo2 〉 2σ(Fo2)) = 1183, N(variables) = 87. In NH4PO2(NH2)2 the anions [PO2(NH2)2]- are linked to chains by N—H … N and N—H … O bridge bonds. The ammonium ions are located between these chains and are donors for N—H … O bridge bonds which connect the chains three-dimensionally.
    Notes: Bei Ammonolysen von P3N5 unter ammonothermalen Bedingungen (T = 400°C und p(NH3) = 6 kbar 14 d in Autoklaven) führt eine geringe, definierte Menge Wasser zur Bildung von NH4PO2(NH2)2. Die Struktur wurde röntgenographisch am Einkristall bestimmt.NH4PO2(NH2)2: P21/c (Nr. 14), a = 6,886(1) Å, b = 8,366(2) Å, c = 9,151(2) Å, β = 111,78(3)°, Z = 4, R1/wR2 = 0,026/0,072, Z(Fo2 〉 2σ(Fo2)) = 1183, Z(Variable) = 87. In NH4PO2(NH2)2 sind Anionen [PO2(NH2)2]-, über N—H … N und N—H … O Brückenbindungen zu unendlichen Ketten verknüpft. Die Ammoniumionen liegen zwischen den Ketten und wirken als Donatoren für N—H … O Brückenbindungen, die die Ketten dreidimensional verknüpfen.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231121
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    Die Kristallstruktur von (Al0,5Ga0,5)CuOAsO4 - Kupfer zwischen planarer und geschlossener KoordinationProfessor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1781-1785 
    Details
    ISSN: 0044-2313
    Keywords: Copper ; aluminium ; gallium ; oxide arsenate ; crystal structure ; oxidation of alloys ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of (Al0,5Ga0,5)CuOAsO4 - Copper Intermediate between Planar and Closed CoordinationSingle crystals of the new oxide arsenate (Al0.5Ga0.5)CuOAsO4 (monoclinic, P21/c, a = 734.3(2) pm, b = 1024.79(9) pm, c = 563.4(2) pm, β = 99.93(1)°, Z = 4) were obtained by reaction of Al/As/Cu/Ga-alloys with oxygen. The crystal structure was determined from four-circle diffractometer data (w2R = 0.039 for 1211 F2 values and 76 parameters). The structure contains [Cu2O6] double squares arranged in slabs perpendicular to the a axis such that a [4 + 1]-coordination of the copper atoms by oxygen atoms results which is intermediate between square-planar and square-pyramidal. Along [100] layers of corner sharing (Al/Ga)O4 and AsO4 tetrahedra are alternating with buckled Cu layers.
    Notes: Einkristalle des neuen Oxidarsenats (Al0,5Ga0,5)CuOAsO4 (monoklin, P21/c, a = 734,3(2) pm, b = 1024,79(9) pm, c = 563,4(2) pm, β = 99,93(1)°, Z = 4) wurden durch Oxidation von Al/As/Cu/Ga-Legierungen im Sauerstoffstrom erhalten. Die Kristallstruktur wurde aus Vierkreisdiffraktometer-Daten bestimmt (w2R = 0,039 für 1211 F2-Werte und 76 Parameter). [Cu2O6]-Doppelquadrate sind in Schichten senkrecht zur a-Achse so angeordnet, daß für Kupfer eine [4 + 1]-Koordination durch Sauerstoffatome resultiert, die als Übergang von quadratisch-planarer zu quadratisch-pyramidaler Koordination interpretiert werden kann. In [100]-Richtung wechseln Schichten aus eckenverknüpften (Al/Ga)O4- und AsO4-Tetraedern mit gewellten Cu-Schichten ab.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231120
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    Na4AuTl, die erste ternäre Verbindung im System Natrium/Gold/Thallium (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1621-1624 
    Details
    ISSN: 0044-2313
    Keywords: Sodium auride thallide ; gold chains ; thallium dumb-bells, synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na4AuTl, the First Ternary Compound in the System Sodium/Gold/ThalliumSilver coloured, brittle single crystals of Na4AuTl were obtained by the reaction of NaN3, gold sponge and TlN3 at 773 K. The structure was determined from X-ray single-crystal diffractometry data: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm space}\,{\rm group}\,{\rm Fmmm,}\,{\rm Z = 8,}\,{\rm a = 5}{\rm .453(1)}\mathop {\rm A}\limits^ \circ,\,{\rm b = 10}{\rm .006(2)}\,\,\mathop {\rm A}\limits^ \circ,\,{\rm c = 23}{\rm .387(5)}\,\mathop {\rm A}\limits^ \circ $$\end{document} Na4AuTl crystallizes in a new structure type with separated gold and thallium partial structures. These consist of linear ∞1[Au2/2] chains and [Tl2] dumb-bells. Structural relationships between Na2Au and the Na Au partial structure of Na4AuTl are discussed.
    Notes: Silberfarbene, spröde Einkristalle eines bislang unbekannten Na4AuTl wurden durch Umsetzung von NaN3, Goldschwamm und TlN3 bei 773 K erhalten. Die Struktur wurde aus Röntgen-Einkristall-Diffraktometerdaten bestimmt: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm Raumgruppe}\,{\rm Fmmm,}\,{\rm Z = 8,}\,{\rm a = 5,453(1)}\mathop {\rm A}\limits^ \circ,\,{\rm b = 10,006(2)}\,\,\mathop {\rm A}\limits^ \circ,\,{\rm c = 23,387(5)}\,\mathop {\rm A}\limits^ \circ $$\end{document} Na4AuTl kristallisiert in einem neuen Strukturtyp mit voneinander separierten Gold- und Thallium-Teilstrukturen, die aus linearen ∞1[Au2/2]-Ketten und [Tl2]-Hanteln aufgebaut sind. Strukturbeziehungen zwischen Na2Au und der Na—Au-Teilstruktur von Na4AuTl werden diskutiert.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231023
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    Untersuchungen an Natriumtrifluormethylsulfonat - Kristallstruktur und Phasenumwandlung des Monohydrats und Natriumionenleitfähigkeit des wasserfreien Salzes (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1625-1632 
    Details
    ISSN: 0044-2313
    Keywords: Sodium trifluormethanesulfonate ; monohydrate ; crystal structure ; phase transition ; sodium ionic conduction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Sodium Trifluormethanesulfonate - Crystal Structure and Phase Transition of Sodium Trifluormethanesulfonate Monohydrate and Sodium Ion Conductivity of Anhydrous Sodium TrifluormethanesulfonateAccording to the results of temperature dependent powder diffractometry (Guinier-Simon-technique) sodium trifluormethanesulfonate monohydrate is dimorphous. The phase transition occurs at -35°C. The room-temperature modification crystallizes monoclinic in space group P21/c with the lattice parameters a = 941.6(5) pm, b = 654.3(2) pm, c = 1062.4(5) pm and β = 107.73(2)°. The crystal structure consists of double layers of trifluormethanesulfonate anions, the lipophilic CF3-groups pointing at each other. Sodium is coordinated by four oxygen atoms from four different anions and by two molecules of crystal water. The resulting polyhedron may be addressed as a distorted octahedron. The low-temperature modification crystallizes orthorhombic in space group Pnma with the lattice parameters a = 645.31(9) pm, b = 538.03(9) pm, c = 1745.3(3) pm. The loss of crystal water occurs at 136°C. Anhydrous sodium trifluormethanesulfonate shows a phase transition at 252°C. The high-temperature modification is a good sodium ionic conductor (σ = 4.1 · 10-1 Ω-1 cm-1 at 250°C).
    Notes: Nach Kühl-Guinier-Simon-Untersuchungen ist Natriumtrifluormethylsulfonatmonohydrat dimorph. Die Phasenumwandlung erfolgt bei -35°C. Die Raumtemperaturmodifikation kristallisiert monoklin in der Raumgruppe P21/c mit den Gitterkonstanten a = 941,6(5) pm, b = 654,3(2) pm, c = 1062,4(5) pm und β = 107,73(2)°. In der Kristallstruktur liegen Doppelschichten aus Trifluormethylsulfonatanionen vor, in denen die unpolaren CF3-Gruppen einander zugewandt sind. Natrium wird von jeweils einem Sauerstoffatom aus vier verschiedenen Anionen sowie von zwei Kristallwassermolekülen koordiniert und erreicht eine verzerrt oktaedrische Koordination. Die Tieftemperaturmodifikation kristallisiert orthorhombisch in der Raumgruppe Pnma mit den Gitterkonstanten a = 645,31(9) pm, b = 538,03(9) pm, c = 1745,3(3) pm. Die Abgabe von einem Mol Kristallwasser erfolgt bei 136°C. Wasserfreies Natriumtrifluormethylsulfonat zeigt eine Phasenumwandlung in eine Hochtemperaturmodifikation bei 252°C, die eine gute Natriumionenleitfähigkeit zeigt (σ = 4,1 · 10-1 Ω-1 cm-1 bei 250°C).
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231024
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    Darstellung und Kristallstrukturanalyse von Bis(π-pentamethylcyclopentadienyl) (2-methylen)(3-diphenylmethylen)oxatitanacyclobutan Cp*2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 654-658 
    Details
    ISSN: 0044-2313
    Keywords: Titanium ; vinylidcne complexes ; cycloaddition reaction ; oxatitanacyclobnlanes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Bis(π-pentamethylcyclopentadienyl) (2-methylene)(3-diphenylmethylene)oxatitanacyclobutane Cp*2 The title complex 5 was synthesized by a [2 + 2]-cycloaddition reaction of diphenytkelene and the titanaallene fragment [Cp2*Ti=C=CH2] (3). Complex 5 was characterized using 1H and 13C NMR spectra and by X-ray structure analysis, respectively.
    Notes: Der Titelkomplex 5 wurde durch [2 + 2]-Cycloaddition von Diphenylketen mit dem Titanaallenfragment [Cp2*Ti=C=CH2] (3) erhalten. Verbindung 5 wurde 1H- und 13C-NMR-spektroskopisch, sowie durch eine Einkristallstrukturanalyse charakterisiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301104
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    Derivate des Imidazols. XXIII. 2-Iminoimidazolin-Derivate des Magnesiums und AluminiumsProfessor Günter Schmid zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 554-560 
    Details
    ISSN: 0044-2313
    Keywords: Magnesium ; aluminium ; 2-iminoimidazoline complexes ; imidazole derivatives ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Imidazole Derivatives. XXIII. 2-Iminoimidazoline Derivatives of Magnesium and Aluminum1,3-dimethyl-2-iminoimidazoline (7, ImNH) forms with MgI2 the complex [(ImNH)4Mg]I2 (8). Whose X-ray structure analysis implies the presence of NHN bridges in the cation. With MeMgI and n-Bu2Mg the polymeric coordination compounds [(ImN)MgI]n (9) and [(ImN)2Mg]n (10) are formed. 7 and it's trimethylsilyl derivative 12 react with AlMe2Cl to give the ionic complexes [(ImNR)2AlMe2]Cl (11, 13, R = H, SiMe3) which are stable with respect to the formation of imidazol-2-imino complexes. The adduct ImNSiMe3 · AlCl3 (14) accessible from the reaction of 12 and AlCl3 eliminates chlorotrimethylsilane on heating to give the trimeric imino complex [(ImN)AlCl2]3 (15); the X-ray structure of 15 confirms the high π-donor properties of the imino substituent.
    Notes: 1,3-Dimethyl-2-iminoirnidazolin (7, ImNH) bildet mit MgI2 den Komplex [(ImNH)4Mg]I2 (8), dessen Kristallstrukturanalyse das Vorliegen von NHN-Brücken innerhalb des Kations glaubhaft macht. Mit MeMgI und n-Bu2Mg werden die Koordinationspolymeren [(ImN)Mgl]n (9) und [(ImN)2Mg]n (10) gebildet. 7 und dessen Trimethylsilyl-Derivat ImNSiMe3 (12) reagieren mit AlMe2Cl zu den ionischen Komplexen [(ImNR)2AlMe2]Cl (11, 13; R = H, SiMe3), die sich als thermisch stabil bezüglich der Bildung von Imidazol-2-imino-Komplexen erweisen. Das aus 12 und AlCl3 zugängliche Addukt ImNSiMe3 · AlCl3, (14) eliminiert bei thermischer Belastung Chlortrimethylsilan: die strukturanalytische Charakterisierung des trimeren Imino-Komplexes [(ImN)AlCl2]3 (15) belegt die hohe π-Donorkapazität des Imino-Substituenten.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230186
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    K3[SnSb3], eine Zintl-Phase mit ∞1[SnSb3]3--BändernProfessor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 561-564 
    Details
    ISSN: 0044-2313
    Keywords: Tripotassium triantimonidostannate(II) ; anionic chains of six-membered rings ; crystal structure ; Zintl phase ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: K3[SnSb3], a Zintl Phase with ∞1[SnSb3]3- ChainsThe metallic lustrous air sensitive compound K3[SnSb3] was prepared from melts of mixtures of the elements. K3[SnSb3] crystallizes in the monoclinic system, group C2/m (No 12), Z = 2, with lattice constants a = 1768.6(2) pm, b = 428.1(1) pm. c = 604.5(1) pm, β = 95.72(5)°. In the anionic partial structure six-membered rings [Sn2Sb4] with chair conformation are connected via common edges to infinite chains ∞1[SnSb3]3-. The potassium cations separate the chains from each other.
    Notes: Die metallisch glänzende, sehr hydrolyseempfindliche Verbindung K3[SnSb3] wurde aus Schmelzreaktionen, ausgehend von Gemengen der Elemente erhalten. K3[SnSb3] kristallisiert monoklin in der Raumgruppe C2/m (Nr, 12), Z = 2, mit den Gitterkonstanten a = 1768,6(2) pm, b = 428,1(1) pm, c = 694,5(1) pm, β = 95,72(5)°. In der Anionenteilstruktur sind [Sn2Sb4]-Sechsringe in Sesselkonformation über zwei gegenüberliegende Kanten zu eindimensional unendlichen ∞1[SnSb3]3--Bändern verknüpft. Die Kaliumkationen separieren die Bänder voneinander.
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    URL: http://dx.doi.org/10.1002/zaac.19976230187
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    Se17[NbCl6]2 und Se17[TaBr6]2 - zwei neue Vertreter des Strukturtyps Se17[MX6]2Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 780-784 
    Details
    ISSN: 0044-2313
    Keywords: Heptadecaselenium(2+) ; Hexachloroniobate(-) ; Hexabromotantalate(-) ; solvothermal reactions ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Se17[NbCl6]2 and Se17[TaBr6]2 - Two New Compounds in the Structure Type Sel7[MX6]2The reaction of Se, SeCl4 and NbCl5 in SnCl4 in a sealed glass ampoule at 150°C yields Se17[NbCl6]2 and from Se, SeBr4 and TaBr5 in SiBr4 under the same conditions Se17[TaBr6]2 is formed. Both compounds crystallize triclinic in form of black moisture sensitive crystals, space group P1, Z = 2 (Se17[NbCl6]2: a = 1322.3(5) pm, b = 1309.0(6) pm, c = 1144.9(4) pm, α = 99.18(3)°, β = 99.55(3)°, γ = 112.17(3)°; Se17[TaBr6]2; 1354.5(7) pm, b = 1346.0(9) pm c = 1179.5(6) pm, α = 99.26(5)°, β = 97.81(4)°, γ = 112.52(5)°). Both are isotypic to the previously reported Se17[WCl6]2. The structures are built of octahedral [NbCl6] and [TaBr6] ions, respectively, and of (Se17)2+ ions The cations consist of two Se7 rings which are connected by a Se3 chain, and thus contain two three-coordinate Se atoms which carry formally the positive charge.
    Notes: Durch solvothermale Reaktion von Se, SeCl4 und NbCl5 in SnCl4 in einer geschlossenen Ampulle bei 150°C entsteht Se17[NbCl6]2 und aus Se, SeBr4 und TaBr5 in SiBr4 unter analogen Bedingungen Se17[TaBr6]2. Beide Verbindungen kristallisieren triklin in Form schwarzer, hydrolyseempfindlicher Kristalle, Raumgruppe P1, Z = 2 (Se17[NbCl6]2: a = 1322,3(5) pm, b = 1309,0(6) pm, c = 1144,9(4) pm, α = 99,18(3)°, β = 99,55(3)°, γ = 112,17(3)°; Se17[TaBr6]2: 1354,5(7) pm, b = 1346,0(9) pm, c = 1179,5(6) pm, α = 99,26(5)° β = 97,81(4)°, γ = 112,52(5)°) und sind isotyp zu Se17[WCl6]2 Die Strukturen sind aus oktaedrischen [NbCl6]- - bzw. [TaBr6]-- und aus (Se17)2+-Ionen aufgebaut, die aus jeweils zwei Se7-Ringen bestehen, die über eine Se3-Brücke verknüpft sind. Jedes Ion enthält zwei dreibindige Se-Atome, die formal die positive Ladung tragen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301123
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    Darstellung und Kristallstruktur von Diammonium-heptachloropentaoxotriniobat(V) (NH4)2[Nb3O5Cl7]Professor Joachim Strähle zum 61. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 805-809 
    Details
    ISSN: 0044-2313
    Keywords: Diammoniuni heptachloropentaoxotriniobate(V) ; niobiumoxochlorides ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Diammoniuni Heptachloropentaoxotriniobate(V) (NH4)2[Nb3O5Cl7]Colourless sometimes pale blue crystals of (NH4)2[Nb3O5Cl7] are prepared in silica tubes from a mixture of NbCI5, NH4CI and As2O3 at 1050 K. (NH4)2[Nb3O5Cl7] crystallizes in space group C2/c with Z = 4. The lattice constants at 293 K are a = 1680.6(8) pm, b = 886.6(1) pm, c = 1104.3(5) pm and β = 111.35(2)°. The structure consists of layers of [(Nb3O5Cl7)2-]∞2. Within a layer the niobium centered octahedra are corner sharing. The structure of the anion shows a new kind of octahedral connectivity for a layered MX4-structure. The ammonium ions are located in between the polyanionic layers.
    Notes: Man erhält (NH4)2[Nb3O5Cl7] in kristalliner Form in Quarzglasampullen aus NbCl5, NH4Cl und As2O3 bei 1050 K. Die Kristalle sind farblos manchmal blaßblau. (NH4)2[Nb3O5Cl7] kristallisiert bei 293 K monoklin in der Raumgruppe C2/c mit Z = 4 und den Gitterkonstanten a = 1680,6(8) pm, b = 886,6(1) pm, c = 1104,3(5) pm und β = 111,35(2)° Die Struktur besteht aus [(Nb3O5Cl7)2-]∞2-Schichten in denen die Oktaederbasisflächen über Ecken verknüpft sind. Die Struktur des Polyanions zeigt eine neuartige Oktaederverknüpfung für eine MX4-Schichtstruktur. Zwischen diesen Schichten befinden sich die Ammoniumionen.
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    Die Kristallstrukturen von CsBiO2 und Cs3BiO3Professor Joachim Strähle zum 60.Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 832-836 
    Details
    ISSN: 0044-2313
    Keywords: Cesiumbismuthate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structures of CsBiO2 and Cs3BiO3CsBiO2 (pale yellow) and Cs3BiO3 (yellow) were obtained by solid state reactions of the binary components Cs2O und Bi2O3 at temperatures of 700°C and 550°C, respectively, The crystal structure of CsBiO2 (C2/c, a = 827.4(2), b = 920.4(2), c = 597.87(9) pm, β = 122.51(1)°, Z = 4, 975 diffractometer data, R1 = 0.058, wR2 = 0.077) contains infinite ∞1[BiO2/2O′2/2] chains. The structure determination of Cs3BiO3 (P213, a = 920,86(8), Z = 4, 289 diffractometer data, R1 = 0,048, wR2 = 0.081) reveals ‘isolated’ BiO33- groups. In this structure the cation arrangement is the same as that of the atoms in the intermetallic phase Cs3Bi.
    Notes: CsBiO2 (hellgelb) und Cs3BiO3 (gelb) wurden durch Festkörperreaktion aus den binären Komponenten Cs2O und Bi2O3 bei Temperaturen von 700°C bzw. 550°C dargestellt. In CsBiO2 liegen nach der Einkristallröntgenstrukturanalyse (C2/c; a = 827,4(2); b = 920,4(2); c = 597,87(9) pm; β = 122,51(1)°; Z = 4; 975 Diffraktometerdaten; R1 = 0,058; wR2 = 0,077) unendlich ausgedehnte ∞1[BiO2/2O′2/2]-Ketten vor. Die Kristallstruktur von Cs3BiO3 (P213; a = 920,86(8) pm; Z = 4; 289 Diffraktometerdaten; R1 = 0,048; wR2 = 0,081) enthält ‚isolierte‘ pyramidale BiO33--Anionen. Die Kationenanordnung in Cs3BiO3 entspricht der Atom-anordnung in der intermetallischen Phase Cs3Bi.
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    Zur Struktur platinreicher Aluminium-Platin-Legierungen (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 362-368 
    Details
    ISSN: 0044-2313
    Keywords: Aluminium/platinum alloys ; crystal structure ; phase transitions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Structure of Platinum-rich Aluminium/Platinum AlloysPlatinum-rich aluminium/platinum alloys have been synthesised via a coupled reaction between aluminium oxide and platinum in a stream of hydrogen at temperatures in the region of 1200°C. The phase richest in aluminium that was prepared was the alloy Al1.16Pt2.84 which crystallises in the AuCu3 structure type. In accordance with the composition, the platinum sites are statistically occupied to a slight extent by aluminium atoms. In a phase somewhat poorer in aluminium (Al1.05Pt2.95), the edge-sharing octahedra consisting almost exclusively of platinum atoms are twisted with respect to each other. The severity of the limited tetragonal distortion which results increases with further decrease in the aluminium content in the phase. A two phase region exists between the limiting composition of this phase and that of the aluminium-poor Pt/Al mixed crystal possessing a statistical atom distribution.By heating the alloys with the slight tetragonal distortion, a second order phase transition into the cubic phase occurs whilst the alloys with a stronger tetragonal distortion undergo a corresponding phase transition which is first order. This result conforms with the idea that, in the former case, the distortion of the platinum octahedra is progressively relieved while in the second case this event results discontinously. Consequently, both the tetragonal and the cubic phase are observed simultaneously in a distinct temperature region.
    Notes: Über eine gekoppelte Reaktion konnten aus Aluminiumoxid und Platin im Wasserstoffstrom bei Temperaturen um 1200°C platinreiche Aluminium-Platin-Legierungen synthetisiert werden.Als aluminiumreichste Phase wurde die im AuCu3-Typ kristallisierende Legierung- Al1,16Pt2,84 erhalten. Entsprechend der Zusammensetzung sind Platinatomlagen zu einem geringen Anteil statistisch durch Aluminiumatome belegt. In einer etwas aluminiumärmeren Phase (Al1,05Pt2,95) sind die fast ausschließlich durch Platinatome gebildeten eckenverknüpften Oktaeder gegeneinander verdreht. Die dadurch be dingte tetragonale Verzerrung nimmt mit weiter sinkendem Aluminiumgehali zu. Zwischen der Grenzzusammensetzung dieser Phase und einem aluminiumarmen Pt-Al-Mischkristall mit statistischer Atomverteilung liegt ein Zweiphasen gebiet.Beim Aufheizen gehen Legierungen mit geringer tetragonaler Verzerrung in einem Reaktionsablauf zweiter Ordnung in die kubische Phase über, bei Legierungen mit stärkerer tetragonaler Verzerrung verläuft eine entsprechende Phasenumwandlung nach der ersten Ordnung ab. Dieses Verhalten entspricht der Vorstellung, daß im ersten Fall die Verdrehung der Platinoktaeder kontinuierlich mit steigender Temperatur aufgehoben wird, wogegen im zweiten Fall dieser Vorgang diskontinuierlich erfolgt und deshalb in einem gewissen Temperaturbereich die tetragonale und die kubische Phase nebeneinander beobachtet werden.
    Additional Material: 11 Ill.
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    Structures of Bromine Oxygen Compounds (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 379-383 
    Details
    ISSN: 0044-2313
    Keywords: Bromine oxygen compounds ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturen von Brom-Sauerstoff VerbindungenDie Kristallstrukturen von Br2O, BrO2F und O2Br—OTeF5 werden beschrieben. Br2O wurde nach einer neuen Methode aus BrOTeF5 und H2O als gelbbrau ner, kristalliner Feststoff erhalten. In der Kristallstruktur (a = 390.4(l), b = 686.2(1), c = 1062.2(2) pm, Raumgruppe Pc21n (Nr. 33), Z = 4) erscheinen gewinkelte (114.2(2)°) Moleküle, die im festen Zustand starke Br … Br Wechsel wirkungen haben, so daß sich eine Kettenstruktur ergibt. BrO2F wurde in bekannter Weise aus KBrO3 und BrF5 her gestellt. Es ist extrem empfindlich gegen. Reduktion. Durch Sublimation erzeugte Einkristalle ergaben eine sechsfache Fehlordnung, die die Sauerstoff- und Fluoratome ununterscheidbar macht (a - ()51.1(2) pm, (α = 47.05(2)°, Raum gruppe R3c, Z = 2). Das BrC2F-Molekül ist pyramidal aufgebaut mit einem durchschnittlichen Bindungswinkel von 103.8(5)°. O2Br-OTeF5 wurde durch Ozonisierung von BrO TeF5 hergestellt und ist ein farbloser Feststoff unterhalb sei ner Schmelz- und Zersetzungstemperatur von -20°C. Es wurde durch Schwingungs- und Kernresonanzspektroskopie und einer Einkristallstrukturanalyse vollständig charakterisiert (a = 517.40(1), b = 614.00(1), c = 1950.70(1) pm, β = 90.61(1)°, Raumgruppe P21/c, Z = 4). Das Molekül hat die erwartete pyramidale Molekülgestalt der BrO3-Gruppe.
    Notes: The crystal structures of Br2O, BrO2F, and O2Br—OTeF5 are reported. Br2O is prepared in a novel manner from BrOTeF5 and H2O, and obtained pure as a yellow brown crystalline solid. The single crystal structure determination a = 390.4(1), b = 686.2(1), c = 1062.2(2) pm, space group Pc21n (No. 33), Z = 4) reveals bent 114.2(2)° Br—O—Br molecules that have strong Br … Br interactions in the solid state resulting in a chain. BrO2F is prepared in the known manner from KBrO3 and BrF5. It is extremely sensitive towards reduction. Crystals obtained by sublimation are rhomboedric with a sixfold disorder making oxygen and fluorine atoms undistinguishable (a = 051.1(2) pm, α = 47.05(2)°, space group R3c, Z = 2). The BrO2F molecular shape is pyramidal with an averaged bond angle of 103.8(3)°. O2Br—O—TeF5 is prepared by ozonisation of Br—O—TeF5 as a colorless solid, mp -20°C. It is fully characterized by vibrational and nmr spetroscopy and a single crystal structure determination (a = 517.40(1), b = 614.00(1), c = 1950.70(1) pm, β= 90.6(1)°, space group P21/c, Z = 4). The molecule has the expected pyramidal geometry at the BrO3 group.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230160
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    Dimere IrII-Phthalocyaninate mit (Ir—Ir)-Bindung;Kristallstruktur von Di(pyridinphthalocyaninato(2—)-iridium(II)) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 369-378 
    Details
    ISSN: 0044-2313
    Keywords: Iridium compound ; phthalocyaninatc complex ; electrochemistry ; optical spectra ; vibrational spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimeric IrII Phthalocyaninates with an Ir—Ir Bond;Crystal Structure of Di(pyridinephthalocyaninato(2-)-iridium(II))Blue, diamagnetic di(iridiumphthalocyaninate(2-)), [(Irpc2-)2] is prepared by controlled thermal decomposition of di(acido)phthalocyaninatoiridates in an inert, high-boiling solvent like 1-chloronaphthalene or under reduced pressure (T 〈 350°C). It is soluble in pyridine (py) yielding the blue violet, diamagnetic py adduct [{lr(py)pc2-}2]. This crystallizes in the orthorhombic space group P212121 (no, 19) with Z = 4. The short Ir—Ir distance (2.707(1) Å) indicates a strong Ir—Ir single bond. Due to the axial coordination of the py ligands the Ir atoms are virtually bond in the centre (Ct) of the pc ligands (d(Ir—Ct) = 0.06(1) Å). The pc ligands are staggered (α(N—Ir—Ir′—N′) = 43(1)°). In spite of the short interplanar distance (d(Ct—Ct) = 2.827(7) Å) the pc ligands are only slightly distorted (one wagging, one doming). One py ligand is disordered. Ir—Npy distances are 2.35(2) and 2.291(1) Å. Due the labilizing trans influence of the Ir—Ir bond these distances are rather long. The (Npy-Ir1—Ir2—N′py) skeleton is almost linear 177.2(4)°). The Ir—Niso distance is 1.99(2) A. Four quasi-reversible one electron transfer processes at -1.34, -0.82, 0.55 and 0.82 V are observed in the differential pulse voltammogram of [{Ir(py)pc2-)2]. The process at 0.55 V is assigned to the redox couple [{Ir(py2-}2]/[{(py)pc-Ir-;Irpc2-(py)}]+, according to the VIS spectrum of the product obtained by oxidation with iodine. In the UV-VIS-NIR spectrum of the dimer dissolved in pyridine the B region is split into two bands at 14970 (B-) and 17300 cm-1 (B+) of equal intensity due to strong excitonic coupling. The excitonic coupling/structure relationship of different mono- and dinuclear diphthalocyaninates is discussed. The Ir—Ir stretching vibration at 135 cm-1 is selectively enhanced in the FT-Raman spectrum.
    Notes: Blaues, diamagnetisches Di(iridiumphthalo cyaninat(2—), [(Irpc2-)2] wird durch kontrollierten thermischen Abbau von Di(acido)phthalocyaninatoiridaten in einem inerten, hochsiedenden Lösungsmittel wie 1-Chlor-naphthalin oder unter vermindertem Druck (T 〈 350°C) dar gestellt. Es ist in Pyridin (py) unter Adduktbildung als blau violettes, diamagnetisches [{Ir(py)pc2-}22] löslich. Letzteres kristallisiert orthorhombisch -in der Raumgruppe P212121 (Nr. 19) mit Z = 4. Der sehr kurze (Ir—Ir)-Abstand (2,707(1) Å weist auf eine starke (Ir—Ir)-Einfachbindung. In folge der Koordination der py-Liganden in axialer Position befinden sich die Ir-Atome praktisch im Zentrum (Ct) der pc2--Liganden (d(Ir—Ct) = 0,06(1) Å). Die beiden pc2--Liganden sind gestaffelt angeordnet (α(N—Ir—Ir′—N′) = 43(1)°). Trotz des kurzen Interplanar-Abstandes (d(Ct-Ct) = 2,827(7) Å) ist der eine pc2--Ligand kaum propellerartig, der andere kaum konkav verzerrt. Ein py-Ligand ist fehlgeordnet. Die (Ir—Npy)-Bindungslängen betragen 2,35(2) und 2,291(1) Å. Sie sind u.a. wegen des labilisierenden trans-Einflusses der (Ir—Ir)-Bindung ungewöhnlich lang. Das (Npy—Ir1—Ir2—N′py)-Gerüst ist fast linear (177,2(4)°). Der (Ir—Niso)-Abstand beträgt 1,99(2) Å. Im differentiellen Pulsvoltammogramm von [{Ir(py)pc2-}2] beobachtet man vier quasi-reversible Einelektronen-Transfer-Prozesse bei -1,34, -0,82, 0,55 und 0,82V. In Übereinstimmung mit dem VIS-Spektrum des mit lod erhaltenen Oxydationsproduktes wird der Prozeß bei 0,55 V dem Redoxpaar [{Ir(py)pc2-)2]/ [{(py)pc-Ir-Irpc2-(py)}]+ zugeordnet. Im UV-VIS-NIR-Spektrum ist der B-Bereich des in Pyridin gelosten Dimeren auf-grund der starken excitonischen Wechselwirkung in zwei etwa gleich intensive Banden bei 14970 (B-) und 17300cm-1 (B+) aufgespalten. Die Abhängigkeit der Excitonen-Kopplung von der Struktur verschiedener ein- und zweikerniger Diphthalocyaninate wird diskutiert. Im FT-Raman-Spektrum wird die Ir—Ir-Valenzschwingung bei 135cm-1 selektiv angeregt.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230159
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    Element-Element-Bindungen. VIII. Synthese, Molekül- und Kristallstruktur des Dibrom(2,4,6-trimethylphenyl)bismutansProfessor Hans Bürger zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 941-956 
    Details
    ISSN: 0044-2313
    Keywords: Dichloro(2,4,6-trimethylphenyl)bismuthane ; dibromo(2,4,6-trimethylphenyl)bismuthane ; crystal structure ; Bi—Br‥Bi bridges ; η6-arene‥Bi contacts ; ir and Raman data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Element-Element Bonds. VIII. Synthesis, Molecular and Crystal Structure of Dibromo(2,4,6-trimethylphenyl)bismuthaneDichloro- (1) und dibromo(2,4,6-trimethylphenyl)bismuthane (2) are obtained in relatively high yields from metathesis reactions of the corresponding bismuth(III) halides with tris(2,4,6-trimethylphenyl)bismuthane. An X-ray structure determination of the dibromo derivative 2 (monoclinic, P21/c; a = 896.2(2); b = 1531.9(3); c = 1713.3(3) pm; β = 94.31(3)° at -100±3°C; Z = 8 molecules; R = 0.059) shows two crystallographically independent molecules to build up a zigzag chain via strong Bi—Br‥Bi bridges (Bi—Br 282 and 281; Br‥Bi 302 and 302 pm) and relatively weak η6-arene‥Bi interactions (mean values Bi‥C 348 and 359 pm); for sterical reasons one bromo substituent of each molecule is not involved in coordinative bonding (Bi—Br 262 and 261 pm). To allow a better comparison of Bi—Cipso bond lengths and arene‥Bi contacts, relevant values of a greater number of related compounds have been compiled; for some of these examples arene‥Bi interactions had not been reported before. Ir and Raman bands below 350 cm-1 are assigned to stretching frequencies of the BiCl2 (1) and BiBr2 (2) fragments, respectively.
    Notes: Dichlor- (1) und Dibrom(2,4,6-trimethylphenyl)bismutan (2) erhält man in guter Ausbeute über eine Metathese des entsprechenden Bismut(III)-halogenids mit Tris(2,4,6-trimethylphenyl)bismutan. Nach den Ergebnissen einer Röntgenstrukturanalyse am Dibrom-Derivat 2 (monoklin, P21/c; a = 896,2(2); b = 1531,9(3); c = 1713,3(3) pm; β = 94,31(3)° bei -100±3°C; Z = 8 Moleküle; R = 0,059) assoziieren die beiden kristallographisch unabhängigen Moleküle über starke Bi—Br‥Bi-Brücken (Bi—Br 282 und 281; Br—Bi 302 und 302 pm) und verhältnismäßig schwache η6-Aren‥Bi-Wechselwirkungen (Mittelwerte Bi‥C 348 und 359 pm) zu Zickzack-Ketten; aus sterischen Gründen bleibt jeweils ein Brom-Substituent ohne eine weitere koordinative Bindung (Bi—Br 262 und 261 pm). Zur besseren Einordnung sind die Bi-Cipso-Abstände und die Aren‥Bi-Kontakte entsprechenden Werten aus einer größeren Zahl verwandter Verbindungen gegenübergestellt; bei einigen Beispielen wird erstmals auf bestehende Aren‥Bi-Wechselwirkungen hingewiesen. IR- und Raman-Banden unterhalb 350 cm-1 lassen sich den Valenzschwingungen des BiCl2- (1) bzw. BiBr2- Fragments (2) zuordnen.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301148
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    Darstellung, Eigenschaften und Kristallstruktur von μ-Carbidodi(pyridinphthalocyaninato(2-)eisen(IV)) und -ruthenium(IV) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 967-972 
    Details
    ISSN: 0044-2313
    Keywords: Phthalocyaninates(2-) ; ruthenium compounds ; iron compounds ; vibrational spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Properties, and Crystal Structure μ-Carbidodi(pyridinephthalocyaninato(2-)iron(IV)) and -ruthenium(IV))Soluble μ-carbidodi(pyridinephthalocyaninato-(2-)iron(IV)) and -ruthenium(IV) is prepared as a pyridine solvate, [{M(py)pc2-)2(μ-C)] · py (M = Fe, Ru) by the reaction of μ-carbidodi(phthalocyaninato(2-)iron(IV)) and -ruthenium(IV)) with pyridine. The isotypic complexes crystallize in the orthorhombic space group P212121 (No. 19) with lattice parameters (in Å): a = 12.692(3)713.002(3) (Fe/Ru); b = 22.186(2)722.635(6); c = 23,653(2)/23.901(6). The M atoms are virtually in the centre (Ct) of the (Np)4 plane (d(M-Ct) = 0.039(6)70.054(8) Å; Np: pyrrole-N atom). The averaged (M-Npy) distance (py: pyridine) is 1.94(1)/2.010(8) Å. The M-(μ-C)-M core is almost linear. The (M-(μ-C)) distance is 1.69(2)71.77(1) Å. The pc2- ligands are in a hitherto unknown convex staggered conformation. The asymmetric (M-(μ-C)-M) stretching vibration is observed in the IR spectrum at 9117974 cm-1, while the corresponding symmetric one is selectively enhanced only in the RR spectrum at 477 cm-1 of the iron complex.
    Notes: Lösliches μ-Carbidodi(pyridinphthalocyaninato(2-)eisen(IV) und -ruthenium(IV) wird durch die Umsetzung von μ-Carbidodi(phthalocyaninato(2-)eisen(IV) und -ruthenium(IV) mit Pyridin als Pyridin-Solvat, [{M(py)pc2-}2(μ-C)] · py (M = Fe, Ru) isoliert. Die isotypen isotypen Komplexe kristallisieren orthorombisch in der Raumgruppe P212121 (Nr. 19) mit den Gitterkonstanten (in Å): a = 12,692(3)/13,002(3) (Fe/Ru); b = 22,186(2)/22,635(6); c = 23,653(2)/23,901(6). Die M-Atom befinden sich fast im Zentrum (Ct) der (Np)4-Ebene (Np: Pyrrol-N-Atom): d(M-Ct) = 0,039(6)/0,054(8) Å. Der mittlere (M-Np)-Abstand beträgt 1,94(1)/2,010(8) Å. Die (M-(μ-C)-Abstand beträgt 1,69(2)/1,77(1) Å. Die pc2--Liganden sind in einer bislang unbekannten komplexen Staffel-Konformation einander zugeneigt. Die asymmetrische (M-(μ-C)-M)-Valenzschwingung liegt im IR-Spektrum bei 911/974 cm-1, die symmetrische beobachtet man dagegen nur im RR-Spektrum des Eisen-Komplexes bei 477 cm-1.
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    URL: http://dx.doi.org/10.1002/zaac.199762301151
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    Darstellung und Eigenschaften von Phthalocyaninato(2-)indaten(III) mit zweizähnigen Oxo-Liganden; Kristallstruktur von Tetra(n-butyl)ammoniumcarbonato(O,O′)-phthalocyaninato(2-)indat(III) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 973-980 
    Details
    ISSN: 0044-2313
    Keywords: Phthalocyaninates ; indium compounds ; optical spectra ; vibrational spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Properties of Phthalocyaninato(2-)indates(III) with Bidentate Oxo Ligands; Crystal Structure of Tetra(n-butyl)ammonium Carbonato(O,O′)phthalocyaninato(2-)indate(III)Tetra(n-butyl)ammonium acidophthalocyaninato(2-)indate(III) of selected bidentate dioxo ligands (oxalate, catecholate, sulfate and carbonate) are obtained by the reaction of tetra(n-butyl)ammonium cis-dihydroxophthalocyaninato(2-)indate(III) with oxalic acid, catechol, hydrogensulfate and ammonium carbaminate. The carbonato complex crystallizes monoclinic in the space group P21/c (No. 14). InIII is hexa-coordinated by four isoindole nitrogen atoms (Niso) and two oxygen atoms of the carbonate in a cis arrangement. InIII is directed out of the centre (Ct) of the (Niso)4 plane towards the carbonate ligand (d(In-Ct)) = 0.903(1) Å. The averaged (In-Niso) and (In-O) distance is 2.1865(4) and 2.1585(5) Å, the (O-In-O′) angle 60.1(2)°. The phthalocyaninate(2-) ligand (pc2-) is in a concave distortion. The optical spectra show the typical π-π* transition of the pc2- ligand at 14600 (B region), 28000 (Q), 35000 (N) und 40500 cm-1 (L). In the IR spectra, the internal vibrations of the oxalate, sulfate and carbonate ligand and the asymmetric (In-O) stretching vibrations are well separated from the internal vibrations of the pc2- skeleton. Spectra-structure correlations are discussed.
    Notes: Tetra(n-butyl)ammoniumacidophthalocyaninato(2-)indate(III) ausgewählter zweizähniger Dioxo-Acidoliganden wie Oxalat, Katecholat, Sulfat und Carbonat werden durch die Reaktion von Tetra(n-butyl)ammoniumcis-dihydroxophthalocyaninato(2-)indat(III) mit Oxalsäure, Brenzkatechin, Hydrogensulfat und Ammoniumcarbaminat dargestellt. Der Carbonat-Komplex kristallisiert monoklin in der Raumgruppe P21/c (Nr. 14). Hexakoordiniertes InIII ist von den vier Isoindol-Stickstoffatomen (Niso) und zwei Sauerstoffatomen des Carbonats in cis-Anordnung umgeben. InIII ist aus dem Zentrum (Ct) der Ebene der vier Niso- Atome in Richtung des Carbonat-Liganden verschoben (d(In-Ct)) = 0,903(1) Å. Die mittleren (In-Niso)- und (In-O)-Abstände betragen 2,1865(4) und 2,1585(5) Å, der (O-In-O′)-Winkel 60,1(2)°. Der Phthalocyaninat(2-)-Ligand (pc2-) ist konkav verzerrt. Die optischen Spektren zeigen nur die typischen, vom Axialliganden unabhängigen π-π*-Übergänge des pc2- -Liganden bei 14600 (B-Bereich), 28000 (Q), 35000 (N) und 40500 cm-1 (L). In den IR-Spektren absorbieren die internen Schwingungen des Oxalat-, Sulfat- und Carbonat-Liganden sowie die asymmetrische (In-O)-Valenzschwingung weitgehend separiert von den pc2--Gerüstschwingungen. Die Spektren-Struktur-Korrelation wird diskutiert.
    Additional Material: 5 Ill.
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    Synthesis and Characterization of Bis(tetrabutylammonium) bis(isotrithionedithiolato-S,S′)nitridotechnetate(V), (Bu4N)2[TcN(dmit)2]Dedicated to Professor Joachim Strähle on the Occasion of his 60th Birthday (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 880-882 
    Details
    ISSN: 0044-2313
    Keywords: Technetium ; nitrido complexes ; crystal structure ; sulfur ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Charakterisierung von Bis(tetrabutylammonium) bis(isotrithiodithiolat-S,S′)nitridotechnetat(V), (Bu4N)2[TcN(dmit)2](Bu4N)2[TcN(dmit)2] (dmit2- = isotrithiodithiolat) wurde aus Na2dmit, (Bu4N)[TcNCl4] und (Bu4N)Cl in Acetonitril hergestellt. Die Verbindung kristallisiert monoklin, Raumgruppe C2/c mit a = 23,143(5), b = 8,342(2), c = 26,382(5) Å, β = 95,12(3), Z = 4. Die Bindungslänge Tc≡N beträgt 1,615(6) Å. Tc und N(l) befinden sich auf einer zweizähligen kristallographischen Achse. Der Komplex hat quadratisch-pyramidale Geometrie. Die vier Schwefelatome bilden die Grundfläche der Pyramide, deren Spitze vom Nitrido-Stickstoff eingenommen wird. Das Technetiumatom befindet sich um 0,62 Å über der Grundfläche.
    Notes: (Bu4N)2[TcN(dmit)2] (dmit2- = isotrithionedithiolate) was prepared from Na2dmit, (Bu4N)[TcNCl4] and (Bu4N)Cl in acetonitrile. The compound crystallises in the monoclinic space group C2/c with a unit cell of the dimensions a = 23.143(5), b = 8.342(2), c = 26.382(5) Å, β = 95.12(3), Z = 4. The Tc≡N bond distance is comparatively short at 1.615(6) Å. Tc and N(1) are situated on a two-fold crystallographic axis. The general coordination geometry is a square pyramid with the four sulfur atoms forming the basal plane and the nitrido nitrogen at the apex. The technetium is located 0.62 Å above the plane defined by the four sulphurs.
    Additional Material: 1 Ill.
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    Gold(III)-Komplexe mit 2-(N,N-Dimethylaminomethyl)phenyl (damp-). Darstellung und Kristallstrukturen von [Au(damp-C,N)Cl2], [Au(damp-C,N)(OOCCH3)2] und [Au(damp-C,N)(mnt)] (mnt2- = 1,2-Dicyanoethen-1,2-dithiolat)Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 873-879 
    Details
    ISSN: 0044-2313
    Keywords: Gold(III) ; complexes ; dichloro-2-(N,N-dimethylaminomethyl)phenylgoId(III) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Gold(III) Complexes with 2-(N,N-dimethylaminomethyl)phenyl (damp-). Syntheses and Structures of [Au(damp-C,N)Cl2], [Au(damp-C,N)(OOCCH3)2] and [Au(damp-C,N)(mnt)] (mnt2- = 1.2-dicyanoethene-1.2-dithiolate)Dichloro-2-(N,N-dimethylaminomethyl)phenylgold(III), [Au(damp-C,N)Cl2], was prepared by the reaction of [Hg(damp)Cl] with Na[AuCl4] and crystallizes monoclinic, space group P21/c a = 7.896(3), b = 9.487(2), c = 15.107(6) Å, β = 100.22(3)°, Z = 4. The crystal structure consists of monomeric [Au(damp-C,N)Cl2] units with square-planar coordinated gold atoms. The shortest Au-Au distances are 4.977 Å. [Au(damp-C,N)(OOCCH3)2] can be synthesized by the reaction of [Au(damp-C,N)Cl2] and AgOOCCH3 in CH2Cl2. Single crystals of the composition [Au(damp-C,N)(OOCCH3)2]. 0.5 H2O were obtained from moist CH2Cl2: monoclinic, space group C2/c, a = 16.626(8), b = 10.640(1), c = 16.271(7) Å, β = 91.90(2)°, Z = 8. The gold atom is square-planar coordinated. The acetato ligands are bound monodentately. The solvent water forms strong hydrogen bridges to the complex molecules in the solid state structure.The chloro ligands in [Au(damp-C,N)Cl2] can easily be replaced by dianionic chelate ligands. The reaction with Na2mnt (mnt2- = 1.2-dicyanoethene-l.2-dithiolate) gives in almost quantitative yield the neutral complex [Au(damp-C,N)(mnt)], which crystallizes orthorhombic, space group Pna21 with a = 7.651(1), b = 14.476(1), c = 13.353(1 ) Å, Z = 4. The gold atom is square-planar coordinated. The Au-S distances are 2.363(2) Å and 2.270(2) Å, respectively.
    Notes: Dichloro-2-(N,N-dimethylaminomethyl)-phenylgold(III), [Au(damp-C,N)Cl2], hergestellt durch Umsetzung von [Hg(damp)Cl] mit Na[AuCl4], kristallisiert monoklin, Raumgruppe P21/c mit a = 7,896(3); b = 9,487(2); c = 15,107(6) Å; β = 100,22(3)°, Z = 4. Die Kristallstruktur besteht aus monomeren [Au(damp-CN)Cl2]-Einheiten mit quadratisch-planar koordinierten Goldatomen. Die kleinsten Gold-Gold-Abstände betragen 4,977 Å.[Au(damp-C,N)(OOCCH3)2] wird durch Reaktion von [Au(damp-C,N)Cl2] mit AgOOCCH3 in CH2Cl2 hergestellt und aus feuchtem CH2C12 als [Au(damp-C,N)(OOCCH3)2] · 0,5 H2O kristallisiert: monoklin, Raumgruppe C2/c a = 16,626(8); b = 10,640(1); c = 16,271(7) Å; β = 91,90(2)°, Z = 8. Das Goldatom ist quadratisch-planar koordiniert. Die Acetatoliganden binden jeweils einzähnig. Das in das Kristallgitter eingebaute Lösungsmittel ist durch Wasserstoffbrücken in die Festkörperstruktur eingebunden.Die Chloroliganden von [Au(damp-C,N)Cl2] können leicht durch zweifach negativ geladene Chelatliganden ausgetauscht werden. Die Reaktion mit Na2mnt in Aceton er gibt in nahczu quantitativer Ausbeute den Neutralkomplex [Au(damp-C,N)(mnt)], der in der orthorhombischen Raumgruppe Pna21 kristallisiert (a = 7,651(1); b = 14,476(1); c = 13,353(1) Å, Z = 4). Das Goldatom befindet sich in einer quadratisch-planaren Koordinationsumgebung. Die Au-S-Abstände betragen 2,363(2) bzw. 2,270(2) Å.
    Additional Material: 4 Ill.
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    Synthesis and crystal structure of M[Nb6Cl15] (M = In, Tl): New Ternary Niobium Halides with Bridged [Nb6Cl18]4- Clusters (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 908-912 
    Details
    ISSN: 0044-2313
    Keywords: In[Nb6Cl15] ; Tl[Nb6Cl15] ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von M[Nb6Cl15] (M = In, Tl): Neue ternäre Niobhalogenide mit verbrückten [Nb6Cl18]4- -ClusternDie neuen ternären Niobchloride M[Nb6Cl15] (M = In, Tl) wurden durch Festkörperreaktionen stöchiometrischer Gemische von NbCl5, Niobmetall und MCl3 bei 720°C dargestellt. Die Kristallstruktur von In[Nb6Cl15] wurde aus Einkristall-Röntgendaten bestimmt und in der orthorhombischen Symmetrie (Raumgruppe Pmma, Z = 4) mit a = 1786.6(1) pm, b = 1345,52(9) pm, c = 929,34(8) pm, R = 0,028, Rw = 0,037, GooF = 1,06 für alle symmetrieunabhängigen 1552 Reflexe verfeinert. Die Gitter-parameter der isotypen Verbindung Tl[Nb6Cl15] wurden aus Röntgen-Pulverdiffraktometerdaten verfeinert: a = 1785,9(2) pm, b = 1347,2(2) pm, c = 930,2(1) pm. Die Struktur besteht aus [Nb6Cl18]4--Clustern, die über terminale Chlorid-Liganden miteinander verbunden sind und zwei Sorten senkrecht zueinander stehender Ketten bilden, Diese Ketten sind über weitere terminale Liganden zu einem dreidimensionalen Netzwerk verbunden. Die In+- und Tl+-Ionen sind zehnfach koordiniert (in Form eines verzerrten zweifach bekappten Würfels), mit acht inneren und zwei äußeren Chlorid-Liganden.
    Notes: New ternary niobium chlorides corresponding to the formula M[Nb6Cl15] (M = In, T1) were synthesized from solid state reactions of NbCl5, niobium metal, and MCl3 at 720°C. The crystal structure of In[Nb6Cl15] was determined from single crystal X-ray diffraction studies. The structure was refined in the orthorhombic symmetry (space group Pmma, Z = 4) with a = 1786.6(1) pm, b = 1345.52(8) pm, c = 929.34(8) pm, RF = 0.028 and Rw = 0.037, GooF = 1.06 for all 1552 unique reflections. The lattice parameters of the isotypic Tl[Nb6Cl15] compound were refined from X-ray powder diffraction data: a = 1785.9(2) pm, b = 1347.2(2) pm, c = 930.2(1) pm. The structure of In[Nb6Cl15] is made up of [Nb6Cl18]4- clusters linked to each other through terminal chloride ligands to form two sets of chains perpendicular to each other. The chains are linked through other terminal ligands to yield a three-dimensional network. The In+ or Tl+ ions are located in a ten coordination site (distorted bicapped cubic geometry) made up of eight inner and two outer chloride ligands.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301143
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    Zur Struktur und Reaktivität des Diammoniumhexafluoromanganats(IV) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1259-1263 
    Details
    ISSN: 0044-2313
    Keywords: Ammonium fluoromanganates ; redox behavior ; di(ammonium) hexafluoromanganate(IV) ; crystal structure ; tri(ammonium) hexafluoromanganate(III) ; high temperature modification ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About the Structure and Reactivity of Diammonium Hexafluoromanganate(IV)Electrolytic oxidation of an aqueous suspension of MnF2 containing NH4F, and subsequent crystallization in 40% HF yields yellow crystals of (NH4)2MnF6. It crystallizes in the hexagonal K2MnF6 type structure with the space group P63mc and a = 5.903; c = 9.565 Å; Z = 2. With in situ powder diffraction studies it is shown, that (NH4)2MnF6 is gradually reduced in a NH3 atmosphere between 30 and 230 °C to afford (NH4)3MnF6, (NH4)2MnF5, and finally NH4MnF3. (NH4)3MnF6, thereby, forms a hitherto unknown cubic (a = 9.082 Å) high temperature modification with the cryolite type structure. Under N2 the thermal decomposition of (NH4)2MnF6 proceeds via NH4MnF4 to yield MnF2.
    Notes: Durch elektrolytische Oxidation einer NH4F-haltigen, wäßrigen MnF2-Suspension und anschließendes Umkristallisieren in 40%iger HF wird (NH4)2MnF6 in Form von gelben Kristallen erhalten. Es kristallisiert hexagonal im K2MnF6-Typ mit der Raumgruppe P63mc und a = 5,903; c = 9,565 Å; Z = 2. Mithilfe der in situ-Pulverdiffraktometrie wird gezeigt, daß (NH4)2MnF6 in einer NH3- Atmosphäre zwischen 30 und 230 °C über die Stufen (NH4)3MnF6 und (NH4)2MnF5 schrittweise zu NH4MnF3 reduziert wird. (NH4)3MnF6 entsteht dabei in einer bisher unbekannten, kubischen (a = 9,082 Å) Hochtemperaturmodifikation mit der Kryolith-Struktur. Unter N2 verläuft der thermische Abbau von (NH4)2MnF6 über NH4MnF4 zu MnF2.
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    URL: http://dx.doi.org/10.1002/zaac.19976230813
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    Bi24Ru3Br20: Ein pseudo-tetragonales Subbromid mit [RuBi6Br12]-Clustern und [Ru2Bi17Br4]-Gruppen (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1591-1598 
    Details
    ISSN: 0044-2313
    Keywords: Bismuth ruthenium bromide ; subhalide ; cluster ; crystal structure ; pseudo-symmetry ; twinning ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bi24Ru3Br20: A Pseudo-Tetragonal Structure with [RuBi6Br12] Clusters and [Ru2Bi17Br4] GroupsThe melting reaction of Ru with Bi and BiBr yields black, lustrous, air insensitive crystals of the subbromide Bi24Ru3Br20. The orthorhombic crystal structure (space group Pc21n, a = b = 1377.8(1) pm, c = 3222.3(4) pm, V = 6117.0 · 106 pm3) deceives pseudo-symmetry with respect to the tetragonal space group P4/ncc leading to multiply twinned crystals. The structure can formally be subdivided in [RuBi6Br12] clusters, [Ru2Bi17Br4] stacks, and [BiBr4] groups.
    Notes: Aus der Schmelzreaktion von Ru mit Bi und BiBr3 werden schwarze, metallisch glänzende und luftbeständige Kristalle des Subbromids Bi24Ru3Br20 erhalten. Die orthorhombische Kristallstruktur (Raumgruppe Pc21n, a = b = 1377,8(1) pm, c = 3222,3(4) pm, V = 6117,0 · 106 pm3) täuscht die Pseudosymmetrie der tetragonalen Raumgruppe P4/ncc vor, was zu mehrfach verzwillingten Kristallen führt. Die Struktur läßt sich formal in [RuBi6Br12]-Cluster, [Ru2Bi17Br4]-Stapel und [BiBr4]-Gruppen aufgliedern.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231019
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    Synthese und Eigenschaften von Eisen(II)-Komplexen mit vier- und fünfzähnigen N,S-Chelatliganden. Kristallstruktur von [Fe(GBMA)py] · py (GBMA2- = Glyoxal-bis-(2-mercaptoanil)) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1644-1650 
    Details
    ISSN: 0044-2313
    Keywords: Iron(II) complexes ; Schiff's base ligands ; crystal structure ; magnetic properties ; Mössbauer spectra ; electrochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Iron(II) Complexes with tetra- and pentadentate N,S-Chelate Ligands. Crystal Structure of [Fe(GBMA)py] · py (GBMA2- = Glyoxal bis-(2-mercaptoanil))The complexes glyoxal-bis-(2-mercaptoanil)iron(II) [Fe(GBMA)], diacetyl-bis-(2-mercaptoanil)iron(II), [Fe(DBMA)] and o-phthalaldehyde-bis-(2-mercaptoanil)iron(II) [Fe(PhBMA)] have been synthesized by reaction of the corresponding protonated ligands with anhydrous iron(II)-acetate. Pyridine-2,6-dialdehyde-bis-(2-mercaptoanil)iron(II), [Fe(PyBMA)] was obtained by a template synthesis with pyridine-2,6-dialdehyde, 2-aminothiophenol and iron(II)-acetate. Recrystallizing the complexes [Fe(GBMA)] and [Fe(DBMA)] from pyridine afforded [Fe(GBMA)py] · py and [Fe(DBMA)py] · py. For all complexes the magnetic properties have been determined, and the Mössbauer spectra were recorded at 82 K. Compounds [Fe(GBMA)] and [Fe(DBMA)] show quasi reversible redox properties in the cyclovoltammogram, while for [Fe(PhBMA)] an irreversible oxidation was observed. [Fe(GBMA)py] · py crystallizes in the monoclinic space group P21 with a = 1288.7(1), b = 1242.63(5), c = 1396.0(1) pm, β = 98.24(1)°, and Z = 4. In the neutral complex the Fe atom has a square pyramidal coordination with the pyridine nitrogen atom in apical position. The basal plane is formed by two nitrogen and two sulfur atoms of the ligand GBMA2-. The iron is located 40 pm above the pyramidal base. Its average distances to the donor atoms of the GBMA ligand are Fe—N = 190 pm, and Fe—S = 222 pm, while the distance to the nitrogen atom of the coordinated pyridine molecule is 207 pm.
    Notes: Die Komplexe Glyoxal-bis-(2-mercaptoanil)eisen(II), [Fe(GBMA)], Diacetyl-bis-(2-mercaptoanil)eisen(II), [Fe(DBMA)] und o-Phthaldialdehyd-bis-(2-mercaptoanil)eisen(II), [Fe(PhBMA)] wurden durch direkte Umsetzung der entsprechenden protonierten Liganden mit wasserfreiem Eisen(II)-acetat dargestellt. Die Synthese von Pyridin-2,6-dialdehyd-bis-(2-mercaptoanil)eisen(II), [Fe(PyBMA)] erfolgte mit Hilfe einer Templatsynthese aus 2,6-Pyridindialdehyd, 2-Aminothiophenol und Eisen(II)-acetat. Durch Umkristallisieren in Pyridin wurden aus [Fe(GBMA)] und [Fe(DBMA)] die Verbindungen [Fe(GBMA)py] · py und [Fe(DBMA)py] · py erhalten. Von allen Komplexen wurden die magnetischen Eigenschaften bestimmt und die Mössbauer-Spektren bei 82 K registriert. [Fe(GBMA)] und [Fe(DBMA)] zeigen im Cyclovoltammogramm quasireversibles Redoxverhalten, während bei [Fe(PhBMA)] eine irreversible Oxidation beobachtet wird. [Fe(GBMA)py] · py kristallisiert monoklin in der Raumgruppe P21 mit a = 1288,7(1), b = 1242,63(5), c = 1396,0(1) pm, β = 98,24(1)° und Z = 4. Im Neutralkomplex ist das Fe-Atom quadratisch-pyramidal mit dem Pyridin-Stickstoffatom in apikaler Position koordiniert. Die Pyramidenbasis wird von den zwei Stickstoff- und Schwefelatomen des Liganden GBMA2- aufgespannt. Das Fe-Atom befindet sich 40 pm oberhalb der Pyramidenbasis. Die Abstände zu den Donoratomen des GBMA-Liganden betragen im Mittel Fe—N = 190 pm und Fe—S = 222 pm. Der Fe—N-Abstand zum Pyridinstickstoffatom liegt bei 207 pm.
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    Zur Kenntnis von cis-NatriumhyponitritProfessor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1803-1809 
    Details
    ISSN: 0044-2313
    Keywords: Hyponitrites ; cis-Na2N2O2 ; preparation ; properties ; crystal structure ; vibrational spectra ; 15N-MAS-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: To the Knowledge of cis-Sodium HyponitriteSurprisingly, cis-sodium hyponitrite can be prepared by reacting gaseous N2O and solid Na2O. For the first time, the structure of a simple salt of cis hyponitrous acid has been determinated unambigously. According to an abinitio structure determination based on powder data, cis-Na2N2O2 crystallizes monoclinic (P21/c, a = 5.107(1); b = 9.211(1); c = 6.159(1) Å; β = 97.91(1)°; Z = 4). Results of spectroscopic investigations (vibrational spectroscopy, 15N-MAS-NMR) agree with the symmetry of the cis-N2O22- anion as it has been proved by the crystal structure. Consider able differences regarding some chemical and physical properties have been observed for samples of cis-Na2N2O2 synthesized via different routes.
    Notes: Durch Gas-Festkörper-Reaktion von N2O und Na2O läßt sich überraschend cis-Natriumhyponitrit darstellen. Auf der Basis der so erhaltenen reinen, gut kristallisierten Präparate gelang erstmals die eindeutige strukturelle Charakterisierung eines einfachen Salzes der cis-Hyposalpetrigen Säure. Gemäß der voraussetzungsfrei anhand von Pulverdaten durchgeführten Strukturbestimmung kristallisiert cis-Na2N2O2 monoklin (P21/c, a = 5,107(1); b = 9,211(1); c = 6,159(1) Å; β = 97,91(1)°; Z = 4). Die Resultate der spektroskopischen Untersuchungen (Schwingungsspektroskopie, 15N-MAS-NMR) stehen im Einklang mit der durch die Kristallstrukturanalyse ermittelten Symmetrie des cis-N2O22--Anions. Präparate von cis-Na2N2O2, die auf verschiedenen Synthesewegen dargestellt wurden, zeigen auffallende Unterschiede in einigen chemischen und physikalischen Eigenschaften.
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    URL: http://dx.doi.org/10.1002/zaac.19976231124
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    Lewis-Säure-Base-Reaktionen von Goldtrihalogeniden mit Bismuttrihalogeniden - Synthese und Kristallstrukturen von AuBiX6 (X = Cl, Br)Professor Rudolf Hoppe zum 75. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1810-1814 
    Details
    ISSN: 0044-2313
    Keywords: Gold trichloride ; gold tribromide ; bismuth trichloride ; bismuth tribromide ; solvothermal synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Lewis-Acid-Base-Reactions of Gold Trihalides with Bismuth Trihalides - Synthesis and Structures of AuBiX6 (X = CI, Br)Gold trihalides AuX3 (X = Cl, Br) react with bismuth trihalides in sealed glass ampoules to the 1 : 1 adducts AuBiX6 (X = Cl, Br). AuBiCl6 is obtained by a chemical transport reaction at 220°C, whereas AuBiBr6 was synthesized by solvothermal reaction in SiBr4 at 150°C. Both compounds crystallize triclinic, space group P1, Z = 4. AuBiCl6; a = 698.3(4) pm; b = 1009.3(5) pm; c = 1381(1) pm; α = 104.98(5)°; β = 94.73(5)°; γ = 110.06(3)°; V = 867(1) · 106 pm3. AuBiBr6: a = 735.7(4) pm; b = 1055.7(5) pm; c = 1445(1) pm; α =104.88(5)°; β = 94.25(5)°; γ = 110.18(4)°; V =1001(1) ·106pm3. The structures are build formally of square-planar [AuX4]- and chains of edge-connected ([BiX4/2]+)n units. Since each Bi ion is surrounded by eight halogenide ions in a square-antiprismatic form, the structure can alternatively be described as consisting of chains of edge sharing ([BiX4X4/2]3-)n antiprisms connected by Au3+ ions.
    Notes: Goldtrihalogenide AuX3 (X = CI, Br) reagieren mit den entsprechenden Bismuttrihalogeniden BiX3 (X = Cl, Br) in geschlossenen Ampullen zu den 1 : 1-Addukten AuBiX6. AuBiCl6 entsteht bei 220°C unter den Bedingungen des chemischen Transportes, während AuBiBr6 wegen der geringen thermischen Stabilität von AuBr3 unter solvothermalen Bedingungen in SiBr4 als Lösungsmittel bei 150°C dargestellt wurde. Beide Verbindungen sind isotyp und kristallisieren triklin in der Raumgruppe P1, Z = 4, mit den Gitterkonstanten a = 698,3(4) pm; b = 1009,3(5) pm; c = 1381(1) pm; α = 104,98(5)°; β = 94,73(5)°; γ = 110,06(3)° für AuBiCl6 und a = 735,7(4) pm; b = 1055,7(5) pm; c = 1445(1) pm; α = 104,88(5)°; β = 94,25(5)°; γ = 110,18(4)° für AuBiBr6. Die Strukturen sind aus quadratisch-planaren [AuX4]--Ionen und Ketten aus kantenverknüpften ([BiX4/2]+)n-Einheiten aufgebaut. Da die Bi-Ionen von acht Halogenid-Ionen in Form eines quadratischen Antiprismas umgeben sind, kann die Struktur alternativ so beschrieben werden, daß sie aus Ketten kantenverknüpfter ([BiX4X4/2]3- )n-Antiprismen besteht, die über Au3+ -Ionen verbunden sind.
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    URL: http://dx.doi.org/10.1002/zaac.19976231125
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    tBu6As8 - Eine Verbindung bekannter Zusammensetzung und neuer Struktur (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1040-1042 
    Details
    ISSN: 0044-2313
    Keywords: 2,2′,3,3′,4,4′-hexatertiarybutyl-1,1′-bicyclotetraarsane ; arsenic polycycles ; structural isomers ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: tBu6As8 - a Compound of Known Composition and New StructureThe compound 2,2′,3,3′,4,4′-hexatertiarybutyl-1,1′-bicyclotetraarsane (1) can be obtained in good yields through the reaction of (tBuAs)4 with [Co2(CO)8]. 1 is the structural isomer of 2,3,4,6,7,8-hexatertiarybutylbicyclo-[3.3.0]octaarsane (2) described in 1981 by Baudler et al. [3]. 1 was characterized by 1H-NMR spectroscopy, mass spectroscopy and crystal structure analysis. Isomerisation into 2 can be observed, by tempering a solution of 1 in toluene for ten hours at 90°C.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230705
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  • 87
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    Über Ag2SnO3, das erste Silberstannat (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1441-1446 
    Details
    ISSN: 0044-2313
    Keywords: Disilvermetastannate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Ag2SnO3, the First Silver StannateFor the first time, crystals of red Ag2SnO3 have been obtained by solid state reaction of freshly prepared K2Sn(OH)6 and Ag2O at 430°C while applying an oxygen pressure of 350 bar. Ag2SnO3 shows a one dimensional incommensurate superstructure with a′ = 33.1 Å. Here we report on the basic structure of Ag2SnO3. According to the results of X-ray crystal structure determination the basic structure of Ag2SnO3 may be described in P6322 (a = 5.6230(4) Å, c = 12.6694(14) Å, Z = 4, 968 independent reflections, R1 = 5.6%, wR2 = 12.5%). Within the layered “SnO3” partial structure two third of the octahedral voids are occupied by tin. Those SnO3 layers are connected to each other by almost linearly coordinated silver atoms. Additionally, silver occupies the free octahedral voids within the SnO3 sheets. As expressed by the formula Ag[Ag1/3Sn2/3]O2 the structure may be described as a super structure of Delafossite CuFeO2.
    Notes: Rotes Ag2SnO3 wurde erstmals durch Festkörperreaktion von Ag2O und frisch bereitetem K2Sn(OH)6-Gel bei 430°C unter einem ständigen Sauerstoffdruck von 350 bar erhalten. Ag2SnO3 zeigt eine eindimensionale inkommensurable Überstruktur entlang [100] mit a′ = 33,1 Å. Wir berichten hier über die Basisstruktur von Ag2SnO3. Nach den Ergebnissen der Röntgenstrukturanalyse läßt sich die Basisstruktur von Ag2SnO3 in der Raumgruppe P6322 beschreiben (a = 5,6230(4) Å, c = 12,6694(14) Å, Z = 4, 968 symmetrieunabhängige Reflexe, R1 = 5.6%, wR2 = 12,5%). Die, SnO3-Teilstruktur besteht aus Sauerstoffdoppelschichten, innerhalb derer 2/3 der Oktaederlücken von Zinn besetzt sind. Die Schichten sind über nahezu linear koordiniertes Silber verknüpft, zusätzlich ist Silber in freie Oktaederlükken der Sn/O-Schichtpakete eingelagert. Die Struktur von Ag2SnO3 läßt sich als Überstrukturvariante der Delafossitstruktur mit Ag[Ag1/3Sn2/3]O2 beschreiben.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230920
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    Kristallstruktur von Na4HP3O10 · H2O (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 55-58 
    Details
    ISSN: 0044-2313
    Keywords: Tetrasodium triphosphate monohydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Na4HP3O10 · H2ONa4HP3O10 · H2O crystallizes orthorhombic in space group Pben with a = 693.2(5) pm, b = 1203.3(4) pm, c = 1188.5(4) pm; Z = 4. The obtained X-ray diffraction data (9268 symmetrical independent reflections, R = 0.047) allowed to locate and refine all the hydrogen atoms. The structure of Na4HP3O10 · H2O contains alternating layers of triphosphate anions and sodium cations. The triphosphate ions have site symmetry C2 and are linked by strong oxygen-hydrogen bonds (244 pm). The results of thermochemical analyses as well as the vibrational spectrum and data of 31P-MAS-NMR are submitted.
    Notes: Na4HP3O10 · H2O kristallisiert orthorhombisch in der Raumgruppe Pbcn mit a = 693,2(5) pm, b = 1203,3(4) pm, c = 1188,5(4) pm; Z = 4. Die erhaltenen Röntgenbeugungsdaten (9268 symmtrieunabhängige Reflexe, R = 0,047) ermöglichten die Lokalisierung und Verfeinerung sämtlicher Wasserstoffatome. Die Struktur von Na4HP3O10 · H2O besteht aus alternierenden Schichten von Triphosphatanionen und Natrium-Kationen. Die Triphosphationen weisen die Lagesymmetrie C2 auf und sind über starke Wasserstoffbrückenbindungen (244pm) miteinander verknüpft. Die Ergebnisse thermischer Analysen, sowie das Schwingungsspektrum und die 31P-MAS-NMR-Daten werden mitgeteilt.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230109
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    The Na/V/P/N(C2H5)3/H2O system at 473 K and the new open framework structure of the vanadium phosphate phase Nav[((V4-w4+V1+w5+) O9)(PO4)2] · (PO4)x · (OH)y · z H2O (with v = 2.8 to 4.0, w = -0.1 to 1.1, x = 0 to 0.2, y = 0 to 2.1, and z = 7 to 10) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 45-54 
    Details
    ISSN: 0044-2313
    Keywords: Vanadium phosphate ; mixed valence compound V4+/V5+ ; microporosity ; disorder ; open framework ; crystal structure ; single crystal X-ray diffraction ; anti-Keggin group ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Das System Na/V/P/N(C2H5)3/H2O bei 473 K und die neue offene Struktur der Vanadiumphosphat-Phase Nav[((V4-w4+V1+w5+) O9)(PO4)2] · (PO4)x · (OH)y · zH2O (v = 2,8 bis 4,0; w = -0,1 bis 1,1; x = 0 bis 0,2; y = 0 bis 2,1; z = 7 bis 10)Eine Untersuchung des Na/V/P/N(C2H5)3/H2O-Systems bei 473 K unter hydrothermalen Bedingungen ergibt verschiedene Phasen im pH-Bereich von 2,65 bis 12. Bei niedrigen pH-Werten wurde die NaV4+OPO4-Phase erhalten. Im schwach sauren, neutralen und schwach basischen Bereich wurde die Nav[((V4-w4+V1+w5+) O9)(PO4)2] · (PO4)X · (OH)y · zH2O-Phase (oder kurz FVP-1) (mit v = 2.8 bis 4.0, w = -0.1 bis 1.1, x = 0 bis 0.2, y = 0 bis 2.1 and z = 7 bis 10) gefunden. Ihre Kristallstruktur wurde in der Raumgruppe Im3m mit a = 16.025 Å gelöst. Die Kristallstruktur enthält V4+V5+O9(PO4)2-Gruppen, in welchen die Vanadiumatome in quadratisch pyramidaler Koordination mit den Sauerstoffatomen vorliegen. Die Gruppen besitzen die Gestalt einer Pickelhaube, wobei die Spitze die Vanadylgruppe des zentralen V5+ Polyeders ist. Sie sind statistisch um eine Spiegelebene angeordnet und bilden eine V10/2O18/2(PO4)2-Gruppe. Diese sind über die Phosphattetraeder miteinander verknüpft und bilden dabei ein offenes poröses Gerüst, das die Topologie des NbO-Netzes hat. Das Gerüst hat einen freien mittleren Kanaldurchmesser von 4.1 Å und eine Dichte von 10.2 Vanadium- und Phosphatpolyedern pro 1000 Å3. Dieses und zwei verwandte kürzlich gefundene Strukturen sind mikroporöse Gerüste mit der bisher größten gefundenen Porösität. Kein Aluminosilicat oder Aluminophosphat mit einem ähnlich großen Porenanteil ist bisher bekannt geworden. Die FVP-1 Phase kollabiert nicht beim Heizen in Luft bis 523 K und im Vakuum bis 623 K. Sie dehydratisiert und rehydratisiert reversibel. Redoxtitrationen von 19 Proben zeigten, daß das V4+/V5+ Verhältnis zwischen 4.1(2)/0.9(2) un d2.9(2)/2.1(2) variiert. Synthesen mit V25+O5 als Vanadiumquelle ergaben kleinere V4+/V5+ Verhältnisse als solche mit V4+OSO4. Die Tatsache, daß FVP-1 Unordnungserscheinungen zeigt, macht es möglicherweise für katalytische Anwendungen interessant.
    Notes: An examination of the Na/V/P/N(C2H5)3/H2O system at 473 K under hydrothermal conditions yields several different phases in the pH range of 2.65 to 12. At low pH values a NaV4+OPO4 phase was obtained. In the weakly acid, neutral or low basic pH ranges the Nav[((V4-w4+V1+w5+) O9)(PO4)2] · (PO4)x · (OH)y · zH2O (or FVP-1 for short) phase was found (with v = 2.8 to 4.0, w = -0.1 to 1.1, x = 0 to 0.2, y = 0 to 2.1 and z = 7 to 10). Its crystal structure was solved in space group Im3m with a = 16.025 Å. It contains V44+V5+O9(PO4)2 groups in which the vanadium atoms have a square pyramidal coordination of oxygen atoms in the shape of a spiked helmet, where the spike is the vanadyl group of the central V5+ coordination polyhedron. These groups are statistically arranged around a mirror plane yielding an V10/2O18/2(PO4)2 grouping and connect to form an open porous framework by bridging via the phosphate groups following the topology of the NbO type net. The framework has a mean free channel diameter of about 4.1 Å and a density of 10.2 vanadium and phosphorus polyhedra per 1000 Å3. This makes it, together with two other recently found related frameworks, the most open microporous framework described so far. No aluminosilicates or aluminophosphates of similar openness are known. In air the FVP-1 phase does not collapse when heated to 523 K, in vacuum it remains stable to 623 K. It dehydrates and rehydrates reversibly. Redox titrations of 19 samples show that the V4+/V5+ ratios vary from 4.1(2)/0.9(2) to 2.9(2)/2.1(2). Syntheses using V2O5 as a source of vanadium yield samples with lower V4+/V5+ ratios than those based on VOSO4. The fact that FVP-1 displays disorder makes the compound possibly interesting for potential catalytic applications.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230108
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    Darstellung und Kristallstruktur von [Tl2(PhN3C6H4CH2C6H4N3Ph)3], einem zweikernigen TlIII-Komplex mit einem neuen, überbrückenden Bistriazenido-Liganden (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 65-68 
    Details
    ISSN: 0044-2313
    Keywords: Thallium(III) complex ; di(4,4′-phenyltriazenido)-phenylmethane ligand ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [Tl2(PhN3C6H4CH2C6H4N3Ph)3], a Dinuclear TlIII Complex with a Novel, Bridging Bistriazenido LigandTris[di(4,4′-phenyltriazenido)phenylmethane]-dithallium(III) is formed by the reaction of TlNO3 with di(4,4′-phenyltriazeno)phenylmethane in the presence of NaOH and air in an ethanol/H2O mixture. The compound is obtained as red, needlelike crystals from THF-hexane. It crystallizes monoclinic, space group I 2/a (a = 1375.2(5) pm, b = 2615(2) pm, c = 1957.0(8) pm, β = 93.49(3)°) with four dinuclear complexes in the unit cell. Each complex contains three doubly deprotonated bistriazenido ions (PhN3C6H4CH2C6H4N3Ph)2- and two Tl3+ ions. The Tl ions are each coordinated by three chelating triazenido groups resulting in a trigonal prismatic coordination of six N atoms. The Tl-N distances vary between 227 and 239 pm, all N-N distance of the triazenido groups are equal within standard deviations with a mean of 130 pm.
    Notes: Tris[di(4,4′-phenyltriazenido)phenylmethan]-di-thallium(III) entsteht durch Reaktion von TlNO3 mit Di(4,4′-phenyltriazeno)phenylmethan in Gegenwart von NaOH und Luft in einem Ethanol/H2O-Gemisch. Die Verbindung kann in Form roter, nudelförmiger Kristalle aus einem THF/Hexan-Gemisch erhalten werden. Sie kristallisiert monoklin in der Raumgruppe I 2/a mit den Gitterkonstanten a = 1375,2(5) pm, b = 2615(2) pm, c = 1957,0(8) pm, β = 93,49(3)° mit vier zweikernigen Komplexen in der Elementarzelle, von denen jeder aus drei doppelt deprotonierten Bistriazenido-Ionen (PhN3C6H4CH2C6H4N3Ph)2- und zwei Tl3+-Ionen aufgebaut ist. Die Tl-Ionen sind jeweils von drei Triazenidogruppen chelatförmig koordiniert, wodurch für die Kationen ein trigonal prismatisches Koordinationspolyeder aus sechs N-Atomen resultiert. Die Tl-N-Abstände variieren zwischen 227 und 239 pm, alle N-N-Abstände in den Triazenidogruppen sind innerhalb der Standardabweichungen gleich und betrugen im Mittel 130 pm.
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    URL: http://dx.doi.org/10.1002/zaac.19976230111
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    Synthese und Kristallstruktur von BaZn2(OH)6 · 5 H20 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 423-428 
    Details
    ISSN: 0044-2313
    Keywords: Barium hexahydroxodizincate pentahydrate ; synthesis ; crystal structure ; hydroxozincate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of BaZn2(OH)6 · 5 H2OThe electrochemical corrosion of zinc in a zinc/iron pair leads in an ammonia containing solution of barium hydroxide at room temperature to colourless platelets of crystals of BaZn2(OH)6 · 5H2O. The X-ray structure determination on these crystals was successful including all hydrogen positions: P21/c, Z = 4, a = 6.181(2) Å, b = 16.126(3) Å, c = 11.121(2) Å, β = 99.69(2)° Z(Fo2 ≥ 3 σ Fo2) = 3281, Z(Var.) = 178, R/Rw = 0.020/0.021 BaZn2(OH)6 · 5 H2O crystallizes in a layer structure. The layers contain Zn2+ in tetrahedral coordination by OH- and Ba2+ in an onefold capped tetragonal antiprism of 6 H2O and 3 OH-. Hydrogen bridge bonds of a further H2O molecule between the layers to OH- and H2O connect these three-dimensionally.
    Notes: Die elektrochemische Korrosion von Zink in einem Zink/Eisen-Paar führt in einer ammoniakalischen wäßrigen Lösung von Bariumhydroxid bei Raumtemperatur zu plättchenförmigen farblosen Kristallen von BaZn2(OH)6 · 5H2O. An ihnen wurde röntgenographisch die Struktur einschließlich aller H-Lagen bestimmt: P21/c, Z = 4, a = 6,181(2) Å, b = 16,126(3) Å, c = 11,121(2) Å, β = 99,69(2)° Z(Fo2 ≥ 3 σ Fo2) = 3281, Z(Var.) = 178, R/Rw = 0,020/0,021 BaZn2(OH)6 · 5H2O kristallisiert in einer Schichtstruktur. Innerhalb der Schichten ist Zn2+ tetraedrisch von OH- und Ba2+ einfach überkappt tetragonal antiprismatisch von 6H2O und 3OH- umgeben. Über Wasserstoffbrückenbindungen eines weiteren Moleküls H2Q zu OH- und H2O sind die Schichten dreidimensional verknüpft.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230167
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    Synthesis and Crystal Structure of Ba4Mo2O5F7(HF2)3 · H2O (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 439-443 
    Details
    ISSN: 0044-2313
    Keywords: Barium ; molybdenum oxyfluoride ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von Ba4Mo2O5F7(HF2)3 · H2OEinkristalle von Ba4Mo2O5F7(HF2)3 · H2O wurden durch hydrothermale Synthese erhalten. Die Röntgenstrukturbestimmung ergab: Raumgruppe Pnnm, Z = 4, a = 16,497(1), b = 8,6939(5), c = 11,5174(6) Å (R = 0,0295, Rw = 0,0354 für 2425 unabhängige Reflexe und 126 Parameter). Mo ist im MoO3F3 verzerrt oktaedrisch umgeben. Zwei Oktaeder bilden, übereck verbunden durch O2-, (Mo2O5F6)4--Einheiten entlang der c-Achse. Die Ba-Atome liegen in zwei unterschiedlichen Umgebungen vor: einem quasi dreifach bekappten Kubus für Ba1 und Ba3 und einem dreifach bekappten trigonalen Prisma für Ba2.
    Notes: Single crystals of Ba4Mo2O5F7(HF2)3 · H2O are grown by hydrothermal synthesis. The structure is determined from X-Ray diffraction data: space group Pnnm, Z = 4, a = 16.497(1) Å, b = 8.6939(5) Å, c = 11.5174(6) Å (R = 0.0295, Rw = 0.0354 for 2425 independent reflections and 126 adjustable parameters). Mo atoms are in a distorted octahedral environment MoO3F3; two octahedra are linked by one O2- corner forming (Mo2O5F6)4- units lying along the c axis. Ba atoms present two kinds of environment: a quasi tricapped cube for Ba1 and Ba3 and a tricapped tricapped trigonal prism for Ba2.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230170
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    Darstellung und Kristallstruktur eines Kaliumnitridophosphats, K3P6N11 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 429-433 
    Details
    ISSN: 0044-2313
    Keywords: Potassium nitridophosphate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of a Potassium Nitridophate, K3P6N11Single phase microcrystalline K3P6N11 was obtained by the reaction of P3N5 KNH2 in supercritical ammonia (6 kbr, 500°C) after 7 d reaction time in autoclaves. The structure was solved by X-ray powder diffraction methods. K3P6N11: P4132, a = 10.388(3) Å, Z = 4, RBragg (F02) = 0.087, 51 reflections K3P6N11 contains two- and three-fold corner-sharing tetrahedra PN4. These form a three-dimensional framework with potassium in voids coordinated by (2 + 6) N for K(1) and (3 + 3 + 3) N for K(2).
    Notes: Röntgenographisch phasenreines mikrokristallines K3P6N11 entsteht bei der Umsetzung von P3N5 mit KNH2 in Ammoniak unter ammonothermalen Bedingungen (6kbar, 500°C) nach 7d Reaktionszeit in Autoklaven. Die Struktur konnte über eine Röntgenstrukturanalyse am Pulver geklärt werden. K3P6N11: P4132, a = 10,388(3) Å, Z = 4, RBragg (F02) = 0,087, 51 Reflexe K3P6N11 ist aus zweifach- und dreifach eckenverknüpften Tetraedern PN4 aufgebaut, die ein dreidimensionales Gerüst bilden, in dessen Hohlräumen die Kaliumionen K(l) von (2 + 6) N von K(2) von (3 + 3 + 3) N umgeben sind.
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    URL: http://dx.doi.org/10.1002/zaac.19976230168
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    Synthese und Struktur von Li2Ta2O3F6 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 456-460 
    Details
    ISSN: 0044-2313
    Keywords: Oxofluorotantalate(V) ; synthesis ; crystal structure ; lithium hexafluorotantalate(V) ; high-temperature modification ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Li2Ta2O3F6Colourless crystals of Li2Ta2O3F6 are obtained by heating a mixture of LiTaF6 and LiTaO3 in a sealed nickel tube to 700°C for 5 days, followed by slow cooling to room temperature. Li2Ta2O3F6 is also a product of controlled hydrolysis of LiTaF6. It crystallizes in the trigonal space group P3121 with a = 558.11(3), c = 2096.10(4) pm, and Z = 3. The structure is built up by corner-sharing TaO3F3-octahedra forming anionic double layers parallel (001). The lithium cations are intercalated between these double layers having a square-pyramidal coordination by fluorine atoms. For the educt LiTaF6 a new high-temperature modification was found, which is reversibly formed at 150°C. It crystallizes with a = 783.5 pm in the cubic NaSbF6 type.
    Notes: Farblose Kristalle von Li2Ta2O3F6 entstehen beim längeren Erhitzen eines Gemenges aus LiTaF6 und LiTaO3 in einer Nickelampulle auf 700°C und anschließendem langsamen Abkühlen. Li2Ta2O3F6 bildet sich außerdem bei der kontrollierten Hydrolyse von LiTaF6. Es kristallisiert trigonal in der Raumgruppe P3121 mit a = 558,11(3); c = 2096,10(4) pm und Z = 3. In der Verbindung sind TaO3F3-Oktaeder über Ecken zu anionischen Doppelschichten parallel (001) verknüpft. Die Lithiumionen sind zwischen den Doppelschichten eingebaut und tetragonal-pyramidal durch Fluoratome koordiniert. Für das Edukt LiTaF6 wurde eine neue Hochtemperaturphase gefunden, die sich bei 150°C reversibel bildet und im kubischen NaSbF6-Typ mit a = 783,5 pm kristallisiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230173
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    Reindarstellung und Kristallstruktur von Lithiumnitridhydrid, Li4NH, Li4ND (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1912-1916 
    Details
    ISSN: 0044-2313
    Keywords: Lithium nitride hydride ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Lithium Nitride Hydride, Li4NH, Li4NDSingle phase Li4NH was prepared by the reaction of Li3N and LiH at 490°C. Its structure has been solved from x-ray and time-of-flight neutron powder diffraction data.Li4NH crystallizes in an ordered variant of the Li2O structure. N and H occupy the sites of two interpenetrating “extended” diamond lattices. Li occupies all N2H2 tetrahedral voids and is found to be shifted into a N2H tetrahedral face. As a result H is in compressed tetrahedral coordination by Li, while N is in bisdisphenoidal coordination by Li. Alternatively, the Li4NH structure may be regarded as a [Li4N]+threedimensional net, its voids being filled up with H-.Li4NH is a reactive solid, which decomposes to imide when in contact with N2 or H2 at some 400°C.
    Notes: Li4NH wurde durch Reaktion von Li3N und LiH bei 490°C erhalten. Die vollständige Strukturbestimmung gelang über Röntgen- und Flugzeit-Neutronen-Pulverdiffraktion.Li4NH kristallisiert in einer Ordnungsvariante der Li2O-Struktur (Raumgruppe I41/a, a = 489.18(1), c = 993.21(3) pm, Z = 4). N und H besetzen die Plätze von zwei ineinander gestellten gestreckten Diamantgittern. Li besetzt, in Richtung einer N2H-Dreiecksfläche ausgelenkt, alle N2H2-Tetraederlücken. Als Folge ist H gestaucht tetraedrisch und N verzerrt kubisch von Li koordiniert. Alternativ läßt slch die Struktur der Titelverbindung als ein [Li4N]+-Raumnetz deuten, in dessen Hohlräume zum Ladungsausgleich Hydridionen eingebaut sind.Li4NH reagiert bei höheren Temperaturen mit N2 bzw. H2 unter Imidbildung.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231215
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  • 96
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    Ternäre Hydroxide. I. Synthese, Struktur und Eigenschaften von Li2[Sn(OH)6] · 2 H2OProfessor Roger Blacknik zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1978-1982 
    Details
    ISSN: 0044-2313
    Keywords: Lithium hexahydroxostannate(IV) dihydrat ; single crystal growth ; crystal structure ; IR-data ; thermal decomposition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Hydroxides. I. Synthesis, Structure, and Properties of Li2[Sn(OH)6] · 2 H2OColourless crystals of Li2[Sn(OH)6] · 2 H2O were synthesized by reaction of SnCl4 with LiOH in aqueous solution. The crystal structure was determined from single crystal data.Li2[Sn(OH)6] · 2 H2O: monoclinic, P21/n (Nr. 14), a = 502.3(1), b = 692.3(1), c = 1020.2(3) pm, β = 99.78(1)°, V = 349.6(2) · 106 pm3, Z = 2, R/Rw = 0.0192/0.0472, N(I) 〉 2σ(I) = 1527, N(Par.) = 54.Within the crystal structure only slightly distorted octahedrally [Sn(OH)6]2- ions are bonded via hydrogen bonds with water molecules forming layers, which themselve are linked by tetrahedrally coordinated Li ions; the structure is in accordance with the IR-data and the results of the 119Sn solid state NMR-spectroscopy; the hydrat water is eliminated at 117.1°C, the condensation reaction - forming the ternary oxide - takes place at 257.7°C.
    Notes: Farblose Kristalle von Li2[Sn(OH)6] · 2 H2O wurden durch Umsetzung von SnCl4 mit LiOH in wäßriger Phase erhalten. Die Kristallstruktur der Verbindung konnte an Einkristallen aufgeklärt werden.Li2[Sn(OH)6] · 2 H2O: monoklin, P21/n (Nr. 14), a = 502.3(1), b = 692.3(1), c = 1020.2(3) pm, β = 99.78(1)°, V = 349.6(2) · 106 pm3, Z = 2, R/Rw = 0.0192/0.0472, N(I) 〉 2σ(I) = 1527, N(Par.) = 54.Innerhalb des Kristallverbandes sind nur wenig verzerrte, oktaedrische [Sn(OH)6]2--Ionen über Wasserstoffbrückenbindungen mit Wassermolekülen zu Schichten verknüpft, die ihrerseits untereinander über tetraedrisch koordinierte Lithium-Ionen verbunden sind; die Struktur ist in Übereinstimmung mit den IR-Daten und Ergebnissen der 119Sn-Festkörper-NMR-Spektroskopie; Hydratwasser wird bei 117.1°C abgespalten, die Kondensationsreaktion zum ternären Oxid erfolgt bei 257.7°C.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976231224
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  • 97
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    Crystal Structures of trans-[Ta6Cl12(OH)4(H2O)2] · 10 H2O and (NMe4)2[Ta6Cl12(OH)6] · 21 H2O (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 59-64 
    Details
    ISSN: 0044-2313
    Keywords: Hexanuclear tantalum chloro cluster ; tantalum cluster hydroxide ; mixed coordinated clusters ; intercluster bridges ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Kristallstrukturen von trans-[Ta6Cl12(OH)4(H2O)2] · 10 H2O und (NMe4)2[Ta6Cl12(OH)6] · 21 H2ODie Verbindungen trans-[Ta6Cl12(OH)4(H20)2] · 10H2O 1, (NMe4)2[Ta6Cl12(OH)6] · 21H2O 2 und Na2[Ta6Cll2(OH)6] · 16H2O 3 enthalten oktaedrische Tantalchlorocluster und können aus alkalischer Lösung (Methanol/Wasser) erhalten werden. Die Strukturen von 1 und 2 werden beschrieben. Kristallographische Daten s. Abstract.Die Verbindung 1 enthält neutrale, gemischt-koordinierte trans-[Ta6Cl12(OH)4(H2O)2]- Einheiten mit Ta—OH- und Ta—OH2Abständen von 210,4(5) und 214,5(5) pm. Ein koordiniertes Wassermolekül eines Clusters und eine OH Gruppe eines benachbarten Clusters bilden H3O2--Brücken mit einem O … H—O-Abstand von 253,7(7) pm zwischen den beiden Clustern aus. Die zwölf Ta—Cl-Abstände liegen zwischen 244,1(2) und 245,2(2) pm. Die Struktur von 2 ist aus [Ta6Cl12(OH)6]2--Anionen, NMe4+-Kationen und über H-Brücken gebundenen Wassermolekülen aufgebaut.
    Notes: The compounds trans-[Ta6Cl12(OH)4 (H2O)2] · 10 H2O 1, (NMe4)2[Ta6Cl12(OH)6] · 21 H2O 2 and Na2[Ta6Cl12(OH)6] · 16 H2O 3 containing octahedral tantalum chloro clusters were isolated from alkaline methanol/water solutions of [Ta6Cl12]4+. Crystal structures were solved for 1 and 2. Crystal data: 1, monoclinic, space group P21/c (No. 14), a = 938.5(2) pm, b = 1220.3(2) pm, c = 1391.7(4) pm, β = 103.87(2)°, V = 1547.5(6) × 106 pm3, Z = 2; 2, rhombohedral, space group R3 (No. 148), a = 1201.4(2) pm, c = 3110.8(6) pm, V = 3888.5(12) × 106 pm3, Z = 3; 3, cubic F lattice, a = 1451(2) pm, V = 3055(13) × 106 pm3, Z = 4.The cluster in 1 contains the neutral, mixed-coordinated trans-[Ta6Cl12(OH)4 (H2O)2] cluster with Ta—OH and Ta—OH2 distances of 210.4(5) pm and 214.5(5) pm, respectively. One coordinated H2O molecule from one cluster and a coordinated OH- group from a neighbouring cluster form H3O2- intercluster bridges with the O … H—O distance 253.7(7) pm. Twelve Ta—Cl (bridging) distances range from 244.1(2) to 245.2(2) pm. The structure of 2 is built of [Ta6Cl12(OH)6]2- anions, NMe4+ cations and water molecules, the latter linked to the anions by hydrogen bonds.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230110
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    Zur Synthese und Reaktivität von Komplexen des Samariums mit Bis(diphenylchalkogenophosphoryl)amid. Kristallstrukturen von [{η2-(Ph2PS)2N}2Sm(thf)2],[{η3-(Ph2PSe)2N}{η2-(Ph2PSe)2N}Sm(thf)2],[{η3-(Ph2PSe)2N}2Sm(SePh)(thf)] und [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)]Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 755-761 
    Details
    ISSN: 0044-2313
    Keywords: Samarium complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Reactivity of Samarium Complexes with Bis(diphenylchalcogenophosphoryl)amides. The Structures of [{η2-(Ph2PS)2N}2Sm(thf)2],[{η3-(Ph2PSe)2N}{η2-(Ph2PSe)2N}Sm(thf)2],[{η3-(Ph2PSe)2N}2Sm(SePh)(thf)], and [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)]The reaction of potassium-bis(diphenylchalcogenophosphoryl)amides with [SmI2(thf)5] affords complexes containing divalent samarium ions. Different structural types were characterised [{η2-(Ph2PS)2N}2Sm(thf)2] 1 and [{η3-(Ph2PSe)2N}{η2-(Ph2PSe) 2N}Sm(thf)2] 2 The ligands bind either bidentate through the two chalcogen atoms or tridentate through the chalcogen atoms and the nitrogen atom. On oxidation of 2 with diphenyldiselenide and dimesityldiselenide complexes [{η3-(Ph2PSe)2N}2Sm(SePh)(thf)] 3 or [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)] 4 are formed.(1: Space group Pbca (No. 61), Z = 4, a = 10.761(3) Å, b = 17.677(9) Å, c = 29.179(9) Å;2: Space group P1 (No. 2), Z = 2, a = 11.152(3) Å, b = 17.727(9) Å, c = 17.777(6) Å, α = 75.33(3)°, β = 77.74(3)°, γ = 72.21(3)°;3: Space group P21/c (No. 14), Z = 4, a = 13.399(2) Å, b = 45.868(6) Å, c = 11.9110(10) Å, β = 106.422(10)°;4: Space group P21/n (No. 14), Z = 4, a = 12.034(2) Å, b = 36.533(3) Å, c = 14.6617(10) Å, β = 96.889(12)°)
    Notes: Durch Umsetzungen von Kalium-Bis(diphenylchalkogenophosphoryl)amid mit [SmI2(thf)5] bilden sich Komplexe mit zweiwertigen Samariumionen. Es werden verschiedene Strukturtypen charakterisiert: [{η2-(Ph2PS)2N}2Sm(thf)2] 1 bzw. [{η3-(Ph2PSe)2N}{η2-(Ph2PSe) 2N}Sm(thf)2] 2. Der Ligand bindet entweder zweizähnig über die beiden Chalkogenatome oder dreizähnig über die Chalkogenatome und das Stickstoffatom. Wird 2 mit Diphenyldiselenid oder Dimesityldiselenid oxidiert, bilden sich die Komplexe [{η3-(Ph2PSe)2N}2Sm(SePh)(thf)] 3 bzw. [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)] 4.(1: Raumgruppe Pbca, (Nr.61), Z = 4, a = 10,761(3) Å, b = 17,677(9) Å, c = 29,179(9) Å;2: Raumgruppe P1 (Nr.2), Z = 2, a = 11,152(3) Å, b = 17,727(9) Å, c = 17,777(6) Å, α = 75,33(3)°, β = 77,74(3)°, γ = 72,21(3)°;3: Raumgruppe P21/c (Nr. 14), Z = 4, a = 13,399(2) Å, b = 45,868(6) Å, c = 11,9110(10) Å, β = 106,422(10)°;4: Raumgruppe P21/n (Nr. 14), Z = 4, a = 12,034(2) Å, b = 36,533(3) Å, c = 14,6617(10) Å, β = 96,889(12)°)
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301119
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    RhTeCl - das erste Chalkogenidhalogenid eines Platinmetalls mit Schichtstruktur (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 583-586 
    Details
    ISSN: 0044-2313
    Keywords: Rhodium ; chalkogenide halide ; chemical transport ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: RhTeCl - the First Chalcogenide Halide of a Platinum Metal with Layer StructureBlack, platelet like crystals of RhTeCl were obtained by chemical transport reaction. The crystal structure of this new chalkogenide halide of a platinum metal was determined at room temperature by single crystal X-ray diffraction on an “Imaging-Plate” -diffractometer. In contradiction to other known chalkogenide halides of platinum metals RhTeCl crystallizes in a layer structure which is derivable from the CdI2-structure type and which can be refined in the monoclinic spacegroup Cm with the lattice constants a = 1298.81(24), b = 364.05(4), c = 665.28(13) pm, β = 118.76(2)°.
    Notes: Durch chemischen Transport konnten schwarze, plättchenförmige Einkristalle von RhTeCl erhalten werden. Die Kristallstruktur dieses bisher unbekannten Chalkogenidhalogenids eines Platinmetalls wurde röntgenographisch bei Raumtemperatur an einem Einkristall mittels IPDS-Diffraktometerdaten bestimmt. RhTeCl besitzt im Gegensatz zu anderen bekannten Verbindungen dieser Substanzklasse eine schichtartige Kristallstruktur, die sich vom CdI2-Strukturtyp ableiten und mit den Gitterkonstanten a = 1298,81(24), b = 364,05(4), c = 665,28(13) pm, β = 118,76(2)° in der monoklinen Raumgruppe Cm verfeinern läßt.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230191
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  • 100
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    Über das neue gemischtvalente Ge7F16: [GeF6]2--Oktaeder zwischen [Ge6F10]2+-Schichten - zur stereochemischen Aktivität freier Elektronenpaare (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 596-602 
    Details
    ISSN: 0044-2313
    Keywords: Germanium fluoride ; stereochemical activity ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About the New Mixed Valent Ge7F16: [GeF6]2- Octahedra between [Ge6F10]2+ Sheets - a Contribution to the Stereochemical Activity of Lone PairsFor the first time Ge7F16 colourless transparent single crystals have been prepared by the reduction of GeF4 with Ge at 300°C. The extremely hygroscopic fluoride crystallizes in a new structure type in Cc with a = 1818.0(6) pm, b = 754.3(2) pm, c = 1030.4(3) pm, β = 90.33(3)° und Z = 4.Ge7F16 is a mixed valent fluoride according to 6GeF2 × GeF4. Characteristical building units of the new structure type are [Ge6F10]2+ sheets, which are connected via [GeF6]2- octahedra. The Ge2+ within the sheets are coordinated by three nearest F- with distances of 183-218 pm and together with these form distorted trigonal pyramids. The structure of Ge7F16 can be considered as a member of the homologues series Gem4+Gen2+F4m+2n with m = 1 and n = 6. Bond order summations, band structure calculations and calculations of the Madelung part of the lattice energy. MAPLE, have been used for the discussion of the bonding situation.
    Notes: Neu dargestellt wurden farblose transparente Einkristalle von Ge7F16 durch Reduktion von GeF4 mit Ge bei 300°C. Das äußerst hygroskopische Fluorid kristallisiert in einem neuen Strukturtyp in der Raumgruppe Cc (Nr. 9) mit a = 1818.0(6) pm, b = 754.3(2) pm, c = 1030.4(3) pm, β = 90.33(3)° und Z = 4.Ge7F16 ist gemäß 6GeF2 × GeF4 ein gemischtvalentes Fluorid. Charakteristische Baugruppen des neuen Strukturtyps sind [Ge6F10]2+-Schichten, die über [GeF6]2--Oktaeder verbrückt sind. Die Ge2+ innerhalb der Schichten sind von je drei nächsten F- im Abstand von 183-218 pm koordiniert und bilden mit diesen verzerrte trigonale Pyramiden. Die Struktur von Ge7F16 läßt sich als Glied der homologen Reihe Gem4+Gen2+F4m+2n mit m = 1 und n = 6 beschreiben. Die Bindungsverhältnisse werden anhand von Bindungsordnungssummationen, Bandstrukturrechnungen und Berechnungen des Madelunganteils der Gitterenergie, MAPLE. diskutiert.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230193
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