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  • 1985-1989  (3,938)
  • Inorganic Chemistry  (3,415)
  • Genetics
  • 1
    Electronic Resource
    Electronic Resource
    Cocaine produces low dose locomotor depressant effects in mice (1989)
    Springer
    Psychopharmacology 99 (1989), S. 147-150 
    Details
    ISSN: 1432-2072
    Keywords: Locomotor activity ; CNS depression ; Cocaine ; Mice ; Behavior ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Cocaine produces several behavioral effects, most notably locomotor stimulation. Biochemically, cocaine is known to inhibit reuptake at the three monoamine transporter sites, and may have highest affinity at the serotonin transporter. Serotonin augmentation has been associated with decreases in behavioral activity, but cocaine has not been reported to produce behavioral depressant effects except at high doses which cause stereotypy and disruption of behavior. This study examined the effects of relatively low doses of cocaine, in the range of 0.1–10 mg/kg, on locomotor activity in C57BL/6J and DBA/2J mice. A biphasic dose-response curve was seen for both strains. At the lowest doses, activity was depressed. As the dose of cocaine increased, activity returned to baseline, and at the highest doses, increases in locomotor activity were found. DBA/2J mice were depressed at a lower dose of cocaine than were C57BL/6J mice; however, C57BL/6J mice showed locomotor depression over a broader range of doses. Activity was maximally depressed at 0.1 mg/kg for DBA/2J mice, and maximally depressed at 0.3 mg/kg for C57BL/6J mice. Thus, low doses of cocaine are shown to produce significant decreases in locomotor activity in two strains of mice. It is postulated that these low doses of cocaine which depress locomotor activity do so via inhibition of serotonin uptake, resulting in potentiation of serotonergic activity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00442799
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  • 2
    Electronic Resource
    Electronic Resource
    Convulsant properties of GABA antagonists and anticonvulsant properties of ethanol in selectively bred Long- and Short-Sleep mice (1989)
    Springer
    Psychopharmacology 98 (1989), S. 544-548 
    Details
    ISSN: 1432-2072
    Keywords: Ethanol ; Bicuculline ; Picrotoxin ; Seizures ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The convulsant potency of bicuculline, a GABA antagonist, was shown to be greater in Short-Sleep (SS) mice than in Long-Sleep (LS) mice. LS mice, selectively bred for lengthy ethanol-induced narcosis, had longer latencies to myoclonus and clonus following administration of bicuculline and picrotoxin than did ethanol-resistant SS mice. SS mice were also more susceptible to pentylenetetrazol-induced myoclonus, but not clonus. F1 hybrids showed bicuculline seizure sensitivity intermediate to the two parent lines. Ethanol weakly inhibited bicuculline-induced myoclonus in both LS and SS mice. Clonus was clearly antagonized by ethanol in both lines, but to a similar degree. These data provide evidence for a GABAergic role in geno-type-dependent sensitivity to ethanol.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00441957
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  • 3
    Electronic Resource
    Electronic Resource
    Genotype-dependent effects of GABAergic agents on sedative properties of ethanol (1989)
    Springer
    Psychopharmacology 98 (1989), S. 518-523 
    Details
    ISSN: 1432-2072
    Keywords: Ethanol ; GABA ; Bicuculline ; Sedation ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Two lines of mice, selectively bred for differential sensitivity to the soporific effects of ethanol (ETOH), were administered GABAergic drugs in an effort to evaluate a role for GABA in ETOH sensitivity. ETOH sensitive Long-Sleep mice (LS) showed potentiated ETOH sedation when administered bicuculline, muscimol and aminooxyacetic acid (AOAA). ETOH-insensitive SS mice exhibited reduced ETOH sedation in the presence of the antagonists, bicuculline and picrotoxin, and potentiated sedation in the presence of muscimol and AOAA. These changes in narcosis duration were interpreted as central effects, since blood ethanol levels at waking from ETOH sedation varied with GABAergic drug treatment. Picrotoxin antagonized pentobarbital-induced nacrosis in both lines, but to a greater extent in SS mice. These and other experiments with a genetically heterogeneous stock suggest GABA involvement in genotype-dependent ETOH sensitivity, but do not support a simple role of GABA receptor involvement.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00441952
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  • 4
    Electronic Resource
    Electronic Resource
    Modification of ethanol effects by bicuculline: genotype-dependent responses and inheritance (1989)
    Springer
    Psychopharmacology 98 (1989), S. 549-555 
    Details
    ISSN: 1432-2072
    Keywords: Ethanol (ETOH) ; GABA ; Bicuculline ; Sedation ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Genetic influences on the interaction between ethanol (ETOH) and gamma-aminobutyric acid (GABA) neurotransmitter systems were eveluated with a survey of responses to coadministration of ETOH and a GABA antagonist, bicuculline, in a battery of inbred mouse strains. The selectively bred ETOH-sensitive Long-Sleep (LS) mice, the relatively ETOH-resistant Short-Sleep (SS) mice, and a genetically heterogeneous stock (GHS) were also evaluated. The effect of bicuculline on ETOH-induced sedation, hypothermia, and blood ethanol content upon recovery from sedation was assessed. Inheritance of these responses was also examined using F1 hybrids. The effect of bicuculline on ETOH-produced narcosis varied widely among stocks and included antagonism, potentiation, and no effect. Changes in ETOH-induced narcosis produced by bicuculline were accompanied by changes in blood ethanol concentrations consistent with an hypothesis of altered central nervous system sensitivity to ETOH. Knowledge of a strain's seizure susceptibility to the GABA antagonist or of its sensitivity to the hypnotic effects of ETOH were of no predictive value in estimating the outcome of coadministration studies, suggesting at least partially separate genetic influences on each phenotype. In cross-breeding studies there was commonly dominance toward a profile of bicuculline antagonism of ETOH narcosis but different patterns of dominance were observed for seizure susceptibility, again inicating separate genetic control. The results suggest considerable complexity of GABAergic involvement in genotype-dependent ETOH sensitivity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00441958
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  • 5
    Electronic Resource
    Electronic Resource
    Optimising visual selection in early clonal generations of potato based on genetic and economic considerations (1989)
    Springer
    Theoretical and applied genetics 78 (1989), S. 665-671 
    Details
    ISSN: 1432-2242
    Keywords: Solanum tuberosum ; Genetics ; Breeding ; Plant appearance ; Economy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary In 1985, 1986 and 1987, 600 clones were visually assessed at harvest on plant appearance. The clones were harvested 80 days after planting in the first year, in the following years after approximately 80 days as well as after 145 days. The correlation coefficients between years and between harvest times were low to medium. Simulating different selection intensities using the performance of these 600 clones in two successive years, the relation between selection pressure in the first year and the retained proportion of well performing clones in the second year was described. Including the costs of testing, the most economic selection procedure was calculated. This procedure consisted in testing 1,579 first-year clones and 499 second-year clones for every 100 third-year clones required. The optimal period of the main evaluation in the second clonal year is at ware potato harvest time. This selection procedure also provides good selection possibilities for underwater weight and foliage maturity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00262562
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  • 6
    Electronic Resource
    Electronic Resource
    Population biology of two land snails (Mesomphix spp.): variation among six southern appalachian sites with differing disturbance histories (1989)
    Springer
    Oecologia 79 (1989), S. 372-382 
    Details
    ISSN: 1432-1939
    Keywords: Logging disturbance ; Land gastropods ; Ecology ; Genetics ; Population
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Ecological and genetic properties of two North American terrestrial gastropods (Mesomphix spp.) were characterized in paired control and previously logged watersheds in two North Carolina forests (Coweeta and the Great Smoky Mountains National Park) of the Southern Appalachian Biosphere Reserve Cluster. Shell growth was greater in the control sites, but density and mortality were largely independent of prior logging history and forest reserve. Based on starch gel electrophoresis data, both species showed their highest levels of genetic diversity in the Coweeta forest, the component of the reserve cluster which had the most extensive and variable history of logging disturbance. M. subplanus also exhibited higher levels of heterozygosity in logged than in control watersheds, and M. andrewsae showed over twice as many rare alleles in disturbed sites as in control sites. F-statistic analysis depicted both excess levels of homozygosity and moderate genetic differentiation among the populations, reflecting the effects of small population size and perhaps drift and inbreeding. Estimated gene flow was relatively low. These results correspond to the recent finding by Bryant et al. (1987) and others on the effects of bottlenecks, and to the contrasting history of habitat instability of the two major study forests.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00384317
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  • 7
    Electronic Resource
    Electronic Resource
    The genetic predisposition to fibrocalculous pancreatic diabetes (1989)
    Springer
    Diabetologia 32 (1989), S. 45-51 
    Details
    ISSN: 1432-0428
    Keywords: Genetics ; insulin gene ; DQβ gene ; fibrocalculous pancreatic diabetes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Fibrocalculous pancreatic diabetes (previously known as tropical pancreatic diabetes) is a rare cause of diabetes confined to countries within the tropical belt. The aetiology of fibrocalculous pancreatic diabetes is thought to be environmental although the agent(s) is unknown. We have investigated a possible genetic basis of this disease by looking for restriction fragment length polymorphisms of genes implicated in the aetiology of diabetes mellitus. Seventy-six Dravidian patients with fibrocalculous pancreatic diabetes were studied, and the restriction fragment length polymorphisms obtained compared to racially matched control subjects (n=94), patients with Type 2 (non-insulin-dependent) diabetes (n=87) and Type 1 (insulin-dependent) diabetes (n=58). No association of fibrocalculous pancreatic diabetes was found with restriction fragment length polymorphisms of the insulin receptor gene. Although no association of fibrocalculous pancreatic diabetes was found with polymorphism of the HLA DRα/DQα/DXα genes, an association was found with the Taq 1 restriction fragment length polymorphisms of the DQβ gene (DQβ T2/T6 present in 39% of patients with fibrocalculous pancreatic diabetes compared to 19% in control subjects; p=0.01; corrected p value=0.04) which is similar to that found in Type 1 but not Type 2 diabetes. An association of fibrocalculous pancreatic diabetes was also found with the hypervariable region in the 5-prime flanking region of the insulin gene; 40% of patients possessed the class 3 allele compared to 9.5% of control subjects p=0.0001; corrected p value=0.0008). In Type 2 diabetes, similar results were obtained with 33% subjects possessing the class 3 allele (p value compared to control subjects=0.0005; corrected p value=0.004). This study suggests that fibrocalculous pancreatic diabetes has a genetic component in its aetiology. Furthermore, its origin might be related to an individual with part of the genetic predisposition to diabetes (Type 1 or Type 2) who additionally has evidence of chronic calcific pancreatitis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00265403
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  • 8
    Electronic Resource
    Electronic Resource
    Homology and distribution of CO dehydrogenase structural genes in carboxydotrophic bacteria (1989)
    Springer
    Archives of microbiology 152 (1989), S. 335-341 
    Details
    ISSN: 1432-072X
    Keywords: Carboxydotrophic bacteria ; Plasmids ; CO dehydrogenase subunits ; N-terminal sequences ; Oligonucleotides ; Hybridization ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The 17 (S), 30 (M) and 87 kDa (L) subunits of CO dehydrogenases from the CO-oxidizing bacteria Pseudomonas carboxydoflava, Pseudomonas carboxydohydrogena and Pseudomonas carboxydovorans OM5 were isolated and purified. The N-terminal sequences of same subunits from different bacteria showed distinct homologies. Dot blot hybridization employing oligonucleotide probes derived from the sequences of the S-subunit of P. carboxydovorans OM5 and the M-subunit of P. carboxydohydrogena and DNA of the plasmid-containing CO-oxidizing bacteria Alcaligenes carboxydus, Azomonas B1, P. carboxydoflava, P. carboxydovorans OM2, OM4 and OM5 indicated that all genes encoding these subunits reside on plasmids. That in P. carboxydovorans OM5 CO dehydrogenase structural genes are located entirely on plasmid pHCG3 was evident from the absence of hybridization employing DNA from the cured mutant strain OM5-12. CO dehydrogenase structural genes could be identified on the chromosome of the plasmid-free bacteria Arthrobacter 11/x, Bacillus schlegelii, P. carboxydohydrogena and P. carboxydovorans OM3. There was no example of a plasmid-harboring carboxydotrophic bacterium that did not carry CO dehydrogenase structural genes on the plasmid. The N-terminal sequences of CO dehydrogenase structural genes were found to be conserved among carboxydotrophic bacteria of distinct taxonomic position, independent of the presence of plasmids. It is discussed whether this might be the consequence of horizontal gene transfer.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00425170
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  • 9
    Electronic Resource
    Electronic Resource
    Genetical control and linkage relationships of isozyme markers in sugar beet (B. vulgaris L.) (1989)
    Springer
    Theoretical and applied genetics 78 (1989), S. 97-104 
    Details
    ISSN: 1432-2242
    Keywords: Beta vulgaris ; Sugar beet ; Isozymes ; Genetics ; Linkage
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Five isozyme systems were genetically investigated. The different separation techniques, the developmental expression and the use as marker system in sugar beet genetics and breeding is discussed. Isocitrate dehydrogenase was controlled by two genes. The gene products form inter- as well as intralocus dimers, even with the gene products of the Icd gene in B. procumbens and B. patellaris. Adenylate kinase was controlled by one gene. Three different allelic forms were detected, which were active as monomeric proteins. Glucose phosphate isomerase showed two zones of activity. One zone was polymorphic. Three allelic variants, active as dimers, were found. Phosphoglucomutase also showed two major zones of activity. One zone was polymorphic and coded for monomeric enzymes. Two allelic forms were found in the accessions studied. The cathodal peroxidase system was controlled by two independent genes, of which only one was polymorphic. The gene products are active as monomers. Linkage was found between red hypocotyl color (R) and Icd 2. Pgm 1, Gpi 2, Ak 1 and the Icd 2-R linkage group segregated independently.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00299761
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  • 10
    Electronic Resource
    Electronic Resource
    The apolipoprotein multigene family: Structure, expression, evolution, and molecular genetics (1989)
    Springer
    Journal of molecular medicine 67 (1989), S. 225-237 
    Details
    ISSN: 1432-1440
    Keywords: Atherosclerosis ; Apolipoprotein ; Gene expression ; Genetics ; Evolution ; Gene duplication ; Lipid binding ; DNA polymorphism ; Hypercholesterolemia
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The plasma apolipoproteins can be classified into two subgroups: the soluble apolipoproteins including apolipoprotein (apo) A-I, A-II, A-IV, C-I, C-II, C-III, and E, and the apoBs including apoB-100 and apoB-48. The soluble apolipoproteins have very similar genomic structures, each having a total of three introns at the same locations; apoA-IV is an exception in that it has lost its first intron. Using the exon/intron junctions as reference points, we can obtain an alignment of the coding regions of all the soluble apolipoprotein genes. The mature peptide regions of the genes are almost completely made up of tandem repeats of 11 codons. The part of mature peptide region encoded by exon 3 contains a common block of 33 codons, whereas the part encoded by exon 4 contains a much more variable number of internal repeats of 11 codons. On the basis of the degree of homology of the various sequences, and the pattern of the internal repeats in these genes, an evolutionary tree has been proposed for the soluble apolipoprotein genes. ApoB-100 differs considerably from the soluble apolipoproteins. It is the largest apolipoprotein containing 4536 amino acid residues. Two types of internal repeats are identified in apoB-100: amphipathic α-helical repeats and proline-containing repeats with high β-sheet content. The apoB gene contains 29 exons and 28 introns. Its evolutionary relationship to the soluble apolipoprotein genes is unclear. The 3′ end of the apoB gene contains a region of variable number of tandem 12–16-base pair repeats. We have applied the polymerase chain reaction technique to characterize this highly polymorphic locus. The same technique can be used to accurately type other variable number of tandem repeats loci. Finally, apoB-48 was shown to be the product of an RNA editing mechanism involving an intestinal mRNA that has an in-frame UAA stop codon resulting from a C→U change in the codon CAA encoding Gln-2153 in apoB-100 mRNA. Using a molecular approach to apolipoprotein synthesis, structure and genetic analysis, we have generated information important to our understanding of lipoprotein metabolism; we also uncovered unexpected experimental results that are relevant to general cell and molecular biology and molecular evolution.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01717324
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  • 11
    Electronic Resource
    Electronic Resource
    The use of eye movement dysfunctions in exploring the genetic transmission of schizophrenia (1989)
    Springer
    European archives of psychiatry and clinical neuroscience 239 (1989), S. 43-48 
    Details
    ISSN: 1433-8491
    Keywords: Schizophrenia ; Eye movements ; Genetics ; Twins ; Latent trait
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Eye movement dysfunctions have been found in a large number of schizophrenic patients and in about half of their first-degree relatives. The distribution of these traits within the families of schizophrenic patients suggests a model of genetic transmission that fits an autosomal dominant model, which we have called the “genetic latent trait model.” The model, with seven parameters, was fitted to a U.S. population and the model was cross-validated on an independent Norwegian sample. Although the model does not invalidate other, more conventional solutions to the puzzle of schizophrenic transmission, such as multifactorial transmission, the latent trait model does more easily permit linkage studies and therefore will allow refutation or support from the use of molecular genetics techniques.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01739743
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  • 12
    Electronic Resource
    Electronic Resource
    A comparison of muscle precursor replication in crush-injured skeletal muscle of Swiss and BALBc mice (1989)
    Springer
    Cell & tissue research 255 (1989), S. 385-391 
    Details
    ISSN: 1432-0878
    Keywords: Myogenesis ; Muscle regeneration ; Genetics ; Autoradiography ; Tritiated thymidine ; Mouse (Swiss;BALBc)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Muscle precursor replication in Swiss mice, in which muscle regeneration is exceptionally vigorous, was compared with previous data for regeneration in BALBc mice. The tibialis anterior muscles of 23 male and 15 female inbred Swiss SJL/J mice were crush injured, and tritiated thymidine injected into mice at various times after injury to label replicating muscle precursors. Lesion samples were taken 10 days after injury, processed for autoradiography, and grain counts of myotube nuclei analysed. Muscle regeneration was more vigorous in male compared with female Swiss mice, and in both was strikingly greater than that in BALBc mice in which there was extensive fibrous connective tissue throughout the lesions. Autoradiographic analysis showed that muscle precursor replication started at 24 hours in Swiss mice, 6 hours earlier than the onset at 30 hours in BALBc mice. Muscle precursor replication appeared to be more active 96 hours after injury in female Swiss compared with male BALBc and male Swiss mice respectively, although numbers of precursor cells replicating at other times were similar. It is not known whether the slight difference in onset of muscle precursor replication can alone account for the more complete muscle regeneration seen in Swiss mice. Similar studies were carried out in 11 male and 10 female F1 hybrid (SJL/J x BALBc) mice. Analysis of labelled myotube nuclei showed that muscle precursors did not synthesise DNA prior to 30 hours after injury, and regeneration resembled that of the parental BALBc strain.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00224122
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  • 13
    Electronic Resource
    Electronic Resource
    Tryptophan auxotrophic mutants in Aspergillus niger: Inactivation of the trpC gene by cotransformation mutagenesis (1989)
    Springer
    Molecular genetics and genomics 219 (1989), S. 282-288 
    Details
    ISSN: 1617-4623
    Keywords: Aspergillus ; Genetics ; Transformation ; trpC lacZ gene fusion ; Gene replacement
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Aspergillus niger tryptophan auxotrophic mutants have been isolated after UV irradiation of conidiospores. The mutants belong to two different complementation groups, trpA and trpB, which complement each other in heterokaryons. Neither of the mutations could be complemented with the cloned A. niger trpC gene. To obtain A. niger trpC mutants in a direct way, gene inactivation by cotransformation was performed. For this purpose an in-frame gene fusion between the A. niger trpC and Escherichia coli lacZ genes was constructed and shown to be functionally expressed after introduction into A. niger by cotransformation with the pyrA gene as selective marker. Among the β-galactosidase expressing cotransformants, obtained with either circular or linearized vectors, no trpC mutants were detected, even after enrichment. Such mutants, however, could be obtained by cotransformation of A. niger with specific fragments of the fusion gene. Biochemical analysis of the cotransformants indicated that in nearly all cases the fusion gene had replaced the wild-type trpC gene. Genetic analysis showed that the trpC mutation is not linked to any of the A. niger loci described so far. The trpC mutants can be complemented by the cloned A. niger trpC gene as well as by the A. nidulans trpC gene.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00261189
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  • 14
    Electronic Resource
    Electronic Resource
    Synthesis and X-ray characterization of double oxides of the formula Cr1-xW1+xO4 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 153-157 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und röntgenographische Charakterisierung von Doppeloxiden der Formel Cr1-xW1+xO4Mixed-Valenz-Verbindungen der Formel Cr1-xW1+xO4 wurden bei 1300°C dargestellt. Aus Röntgenbeugungsdiagrammen konnten drei verschiedene Phasen identifiziert werden, eine vom Rutiltyp für 0,40 ≤ x ≤ 0,50 und zwei andere mit Rutil-ähnlichen Strukturen bzw. vom CrWO4-Typ für 0 ≤ x ≤ 0,25 und vom WO2-Typ für 0,80 ≤ x ≤ 1.
    Notes: Mixed valency compounds of formula Cr1-xW1+xO4 have been prepared at 1300°C. Three phases have been identified by X-ray diffraction: one of rutile type for 0.40 ≤ x ≤ 0.50 and two others with rutile-related structures, i. e. of CrWO4-type for 0 ≤ x ≤ 0.25 and of WO2-type for 0.80 ≤ x ≤ 1.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895690116
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  • 15
    Electronic Resource
    Electronic Resource
    Dihalogen(pentafluorphenyl)sulfonium(IV)-hexafluoroarsenat C6F5SX2+AsF6- (X = Cl, Br) und Kristallstruktur von Di(pentafluorphenyl)sulfan (C6F5)2S (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 158-168 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dihalogen(Pentafluorophenyl)sulfonium(IV) Hexafluoroarsenate C6F5SX2+AsF6- (X = Cl, Br) and Crystal Structure of Di(pentafluorophenyl)sulfane (C6F5)2SThe preparation and spectroscopic characterisation of the halogensulfonium salts C6F5SCl2+AsF6- and C6F5SBr2+AsF6- is reported. The new salts are much more stable than their trifluoromethyl derivatives.In addition the crystal structure of (C6F5)2S is reported. Space group P43212, Z = 4, 478 unique observed diffractometer data, Rint. = 0.07, lattice constants: a = 569.0(5) pm, c = 3785.8(22) pm, V = 1225 times; 10-30 m3.
    Notes: Es wird über die Darstellung und spektroskopische Untersuchung der Sulfoniumsalze C6F5SCl2+AsF6- und C6F5SBr2+AsF6- berichtet. Die neuen Salze sind bedeutend stabiler als ihre Trifluormethyl-Homologen.Ergänzend wird die Kristallstruktur von (C6F5)2S mitgeteilt. Raumgruppe P43212, Z = 4, 478 unabhängige Reflexe, Rint. = 0,07, Gitterkonstanten: a = 569,0(5) pm, c = 3785,8(22) pm, V = 1225×10-30 m3.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895690117
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  • 16
    Electronic Resource
    Electronic Resource
    Berichtigung (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 192-192 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895690121
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  • 17
    Electronic Resource
    Electronic Resource
    Complex copper(II) fluorides. X. The ternary system BaF2—CuF2—InF3 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 169-176 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Komplexe Kupfer(II)-fluoride. X. Das ternäre System BaF2—CuF2—InF3Das flüssig-fest-Gleichgewichtsdiagramm des InF3—BaF2-Systems wird mittels DTA bestimmt. Die Fluoride BaInF5, das dimorphe Ba3In2F12 und auch eine kubische Phase Ba1-xInxF2+x, deren Struktur sich von der des BaF2 ableitet, wurden gefunden. Die zwei Formen des Ba3In2F12 geben feste Lösungen. Ein isothermer Ausschnitt des ternären Systems BaF2—CuF2—InF3 bei 540°C wird angegeben. Er zeigt die Existenz nur eines quaternären Fluorides: tetragonales BaCuInF7.
    Notes: The liquid-solid equilibria diagram of the InF3—BaF2 system is established by D.T.A. The fluorides BaInF5, the dimorphic Ba3In2F12, and also a cubic phase Ba1-xInxF2+x, the structure of which derives from that of BaF2, are disclosed. The two forms of Ba3In2F12 give solid solutions. An isothermal section of the ternary system BaF2—CuF2—InF3 at 540°C is given. It shows the existence of only one quaternary fluoride: tetragonal BaCuInF7.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895690118
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  • 18
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    Zum chemischen Transport von Chrom- und Manganmonophosphid mit Iod - Experimente und Modellrechnungen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 192-192 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895690122
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  • 19
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    Beiträge zur Chemie N-organylsubstituierter Metallamide. XIX. Umsetzung von [Co(NPh2)2]2 mit CO - ein neuer Weg zur Synthese eines Innerkomplexes des Cobalt(II) mit einem Anthranilsäurederivat; Molekularstruktur von [Co(NPh(o—C6CONPh2))2] (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 183-191 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of N-substituted Metal Amides. XIX. Reaction of [Co(NPh2)2]2 with CO - a New Way for the Synthesis of an Chelate Complex of Cobalt (II) with an Derivative of Anthranilic Acid; Molecular Structure of [Co(NPh(o—C6H4CONPh2))2]Reaction of CO (1 atm, room temperature) with [Co(NPh2)2]2 (I) in benzene (mole ratio 3 : 1) gives Co(CO)3(NPh2)4(benzene)1·6 (II). By adding more CO to the reaction mixture (mole ratio 6 : 1) Co4(CO)12 (III) and a dark red compound of the analytical composition C50H38CoN4O2 (IV) could be isolated. The structure of the red compound was determined by X-ray diffraction. This investigation show IV to be a cobalt(II) complex of an derivative of the anthranilic acid, [Co(NPh(o—C6H4CONPh2))2] (IV). The cobalt coordination in this compound is a distorted tetrahedron. Crystal data of IV: space group P1 with a = 12.449(1) Å, b = 12.431(1) Å, c = 13.223(1) Å, α = 95.47(1)°, β = 95.37(1)°, γ = 94.10(1)°, and Z = 2.
    Notes: Bei der Umsetzung von CO (1 atm, Raumtemperatur) mit [Co(NPh2)2]2 (I) in Benzen im Molverhältnis 3 : 1 entsteht Co2(CO)3(NPh2)4(benzen)1,6 (II); im Molverhältnis 6 : 1 bildet sich ein Reaktionsgemisch, aus dem Co4(CO)12 (III) sowie eine dunkelrote Verbindung der analytischen Zusammensetzung C50H38CoN4O2 (IV) isoliert werden kann. Die Röntgenstruktur-bestimmung von IV ergab, daß es sich um den ein Anthranilsäurederivat als Liganden enthaltenden Komplex [Co(NPh(o—C6H4CONPh2))2] IV handelt, der eine verzerrt tetraedrische Koordination aufweist.Kristalldaten für IV: Raumgruppe P1 mit a = 12,449(1) Å, b = 12,431(1) Å, c = 13,223(1) Å, α = 95,47(1)°, β = 95,37(1)°, γ = 94,10(1)° und Z = 2.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895690120
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  • 20
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    Formation and transformation of δ-Nb2O5 solid solutions in the system Nb2O5—Al2O3 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 177-182 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bildung und Umwandlung von festen Lösungen des δ-Nb2O5 im Nb2O5—Al2O3-SystemIm System Nb2O5—Al2O3 werden (bis 50 Mol-% Al2O3) mit metastabilem, hexagonalem δ-Nb2O5 feste Lösungen gebildet, bei der Präparation aus den amorphen Substanzen, die durch simultane Hydrolyse von Niob- und Aluminiumalkoxid erhalten werden. Die Werte des Gitterparameters a sind unabhängig von der Zusammensetzung, während der Parameter c linear abnimmt mit steigendem Al2O3-Gehalt. Der übergang δ-Nb2O5 (orthorhombisch) erfolgt bei 640°C bis 700°C. Die 50 Mol-% Al2O3-enthaltende feste Lösung geht bei 800° bis 860°C in monoklines NbAlO4 über.
    Notes: In the system Nb2O5—Al2O3, solid solutions of metastable δ-Nb2O5 (hexagonal) are formed up to 50 mol% Al2O3 from amorphous materials prepared by the simultaneous hydrolysis of niobium and aluminium alkoxides. The values of the lattice parameter a are relatively constant regardless of composition, while parameter c decreases linearly with increasing Al2O3 content. The δ- to γ-Nb2O5 (orthorhombic) transformation occurs at ≍ 640°C to ≍ 700°C. The solid solution containing 50 mol% Al2O3 transforms to monoclinic NbAlO4 at 800° to 860°C.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895690119
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  • 21
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    Masthead (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 570 (1989) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895700101
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  • 22
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    Die Reaktion des tert.Butyl-lithiums mit Aluminiumtribromid; Molekülstrukturen von [HAl(CMe3)2]3 und [LiHAl(CMe3)3]2 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 570 (1989), S. 37-53 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of tert.Butyl-lithium with Aluminiumtribromide; Molecular Structures of [HAl(CMe3)2]3 and [LiHAl(CMe3)3]2The reaction of tert.butyl-lithium with aluminiumtrihalide at low temperatures was reinvestigated. Four compounds were isolated: trimeric di(tert.butyl)alane(III) 1, monomeric (solution in benzene)/dimeric (solid state) lithium-tri(tert.butyl)alanate(III) 2, tri(tert.butyl)alane 3 and lithium-tetra(tert.butyl)alanate 4. X-ray structure analyses gave a planar sixmembered Al—H heterocycle for 1 and a Li—H-bridged dimer showing intramolecular interactions of lithium with C—H σ-bonds for 2.
    Notes: Die Reaktion des tert.Butyl-lithiums mit Aluminiumtrihalogenid bei tiefen Temperaturen wurde neu untersucht. Dabei isolierten wir: das trimere Di(tert.butyl)alan(III) 1, das monomere (benzolische Lösung)/dimere (Festkörper) Lithium-tri(tert.butyl)alanat(III) 2 sowie Tri(tert.butyl)alan 3 und Lithium-tetra(tert.butyl)alanat 4. Die Röntgenstrukturanalyse ergab einen planaren sechsgliedrigen Heterozyklus aus Al—H-Einheiten für 1 und ein über Li—H-Brücken verknüpftes Dimeres mit intramolekularen Wechselwirkungen zwischen den Lithiumatomen und C—H-σ-Bindungen für 2.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895700103
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  • 23
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    Zur Kenntnis von Ammonium-pentanitratopraseodymat und -neodymat (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 106-110 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Ammonium Pentanitrato Praseodymate and Neodymate(NH4)2[Pr(NO3)5] · 4 H2O (I) and (NH4)2[Nd(NO3)5] · 4 H2O (II) were obtained from Pr6O11 and Nd2O3 by reaction with nitric acid and NH4NO3. The fixed water molecules could be removed completely with formation of [NH4]2[Pr(NO3)5] (III) and [NH4]2[Nd(NO3)5] (IV). The i.r. spectra indicate only symmetrically bonded bidentate NO3- ligands. The water molecules are bonded as well by hydrogen bridges to NH4+ ions as by EDA interaction to the lanthanoid atoms. Therefore, the constitution of the complexes is described more exactly by the formula [NH4]2[Ln(NO3)5(H2O)2] · 2 H2O.
    Notes: (NH4)2[Pr(NO3)5] · 4 H2O (I) und (NH4)2[Nd(NO3)5] · 4 H2O (II) lassen sich durch Umsetzung von Pr6O11 bzw. Nd2O3 mit Salpetersäure und Ammoniumnitrat erhalten. Beide Komplexe ließen sich vollständig dehydratisieren unter Bildung von [NH4]2[Pr(NO3)5] (III) bzw. [NH4]2[Nd(NO3)5] (IV). Die Auswertung der IR-Spektren zeigt, daß in den Komplexen ausschließlich zweizähnig gebundene Nitratliganden vorliegen. I und II enthalten unterschiedlich gebundene Wassermoleküle, die teils über Wasserstoffbrücken an die NH4-Ionen, teils koordinativ an die Lanthanoidatome gebunden sind. Die Konstitution dieser Komplexe wird deshalb exakter durch die Formel [NH4]2[Ln(NO3)5(H2O)2] · 2 H2O beschrieben.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895690110
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  • 24
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    Über die Reaktionen von N-Chloracetonimin mit Molybdänpentachlorid und Wolframhexachlorid Die Kristallstruktur von Me2C=NH2[MoOCl4] (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 83-90 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of N-Chloroacetoneimine with Molybdenum Pentachloride and Tungsten Hexachloride. Crystal Structure of Me2C=NH2[MoOCl4]WCl6 reacts with N-chloroacetoneimine under elimination of chlorine and formation of pentachloro-isopropylideneimino-tungsten(VI), Cl5W=N=CMe2, a brown-black crystal powder, which was characterized by i.r. spectroscopy. MoCl5 reacts in a similar way, although only a product mixture can be obtained. Partial hydrolysis of this mixture yields isopropylideneiminium-tetrachlorooxomolybdate(V), Me2C=NH2+[MoOCl4]-, of which the crystal structure was determined (2323 unique observed reflexions, R = 0.049). Space group P21/c, Z = 4, a = 878.6, b = 907.2, c = 1252.2 pm, β = 91.29°. The compound consists of Me2C=NH2+ ions with a planar arrangement of the skeletal atoms and a CN bond length of 126.7 pm and of dimeric, centrosymmetric anions [MoOCl4]22- having Mo atoms linked via asymmetric chloro bridges (MoCl distances 238.4 and 307.6 pm). The longer Mo—Cl contacts are located in the trans-positions of the terminal oxoligands (MoO distance 164 pm).
    Notes: WCl6 reagiert mit N-chloracetonimin unter Chlorabspaltung und Bildung von Pentachlor(isopropylidenimido)wolfram(VI), Cl5W=N=CMe2, einem schwarzbraunen Kristallpulver, das durch sein IR-Spektrum charakterisiert wird. ähnlich verläuft die Umsetzung mit MoCl5, wobei allerdings kein einheitliches Produkt isoliert werden kann. Durch partielle Hydrolyse entsteht aus diesen Produkten Isopropylideniminiumtetrachloro-oxomolybdat(V), Me2C=NH2+[MoOCl4], von dem wir eine Kristallstrukturanalyse angefertigt haben (2323 unabhängige beobachtete Reflexe, R = 4,9%). Raumgruppe P21/c, Z = 4, Gitterabmessungen: a = 878,6; b = 907,2; c = 1252,2 pm; β = 91,29°. Die Verbindung besteht aus Kationen Me2C=NH2+, deren Gerüstatome in einer Ebene liegen und die eine CN-Bindungslänge von 126,7 pm haben, sowie zentrosymmetrischen dimeren Anionen [MoOCl4]22-, deren Mo-Atome über asymmetrische Chlorobrücken mit Mo—Cl-Abständen von 238,4 pm und 307,6 pm verknüpft sind. Die langen Mo—Cl-Kontakte befinden sich in trans-Stellung zu den terminal gebundenen Oxoliganden (Abstand MoO = 164 pm).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895690107
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    Bindungsverhältnisse in kristallinen Phasen von Caesiumhydrogensulfid, CsHS und CsDS (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 117-130 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemical Bonding in Crystalline Phases of Cesium Hydrogensulfides, CsHS and CsDSReaction of liquid hydrogensulfide, H2S and D2S respectively, with cesium at room temperature in pressure resistant glass tubes quickly gives the crystalline hydrosulfides, CsHS and CsDS. The compounds are characterized by thermochemical, X-ray, and neutron diffraction data.Three solid phases of CsDS are observed as a function of temperature: Changes in chemical bonding are discussed with respect to temperature and in comparison with alkali metal hydroxides, amides, halides, and further hydrogensulfides.
    Notes: Flüssiger Schwefelwasserstoff, H2S bzw. D2S, reagiert bei Raumtemperatur in druckfesten Glasgefäßen schnell mit Caesium, wobei kristallines Caesiumhydrogensulfid, CsHS bzw. CsDS entsteht. Thermochemische, Röntgen- und Neutronenbeugungsdaten charakterisieren die Verbindungen. Drei feste Phasen von CsDS wurden in Abhängigkeit von der Temperatur beobachtet: Änderungen der chemischen Bindung werden in Abhängigkeit von der Temperatur und durch Vergleich mit Alkalimetallhydroxiden, -amiden und -halogeniden sowie weiteren -hydrogensulfiden diskutiert.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895690112
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  • 26
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    Darstellung und Kristallstruktur von Lithiumhydrogensulfid, LiHS (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 111-116 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Lithiumhydrogensulfide, LiHSLithiumhydrogensulfide, LiHS, is prepared from lithiumamide, LiNH2, by reaction with liquid hydrogensulfide. At 150°C the solubility of LiHS in H2S is sufficient for the growth of single crystals in a temperature gradient within the autoclaves used. The X-ray structure determination at 295 K is characterized by the following data: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{{{\rm P4}_{\rm 2} } \mathord{\left/ {\vphantom {{{\rm P4}_{\rm 2} } {{\rm mmc,\;Z = 2,\;a = 3.916}\left({\rm 2} \right){\AA},\;c = 6.155\left(2 \right){\AA},}}} \right. \kern-\nulldelimiterspace} {{\rm mmc,\;Z = 2,\;a = 3.916}\left({\rm 2} \right){\AA},\;c = 6.155\left(2 \right){\AA},}}} \hfill \\ {{\rm Z}\left({{\rm F}_{\rm 0}^{\rm 2} \ge 3\sigma \;{\rm F}_{\rm 0}^{\rm 2} } \right) = 74,\;{\rm R = 0.011}{\rm .}} \hfill \\\end{array} $$\end{document} Lithium occupies tetrahedral sites in a distorted cubic close-packed arrangement of S; in PtS sulfur occupies tetrahedral sites in a similar way in a distorted close packing of Pt. Hydrogen atoms of the HS--ions are dynamically disordered in a split position linearly bound to S. At 228 K a thermal effect occurs in DSC-measurements indicating that below this temperature the HS--ion has fixed positions.
    Notes: Zur Darstellung von Lithiumhydrogensulfid, LiHS, wurde Lithiumamid, LiNH2, in flüssigem Schwefelwasserstoff protolysiert. Bei 150°C reicht die Löslichkeit von LiHS in H2S für die Einkristallzüchtung im Temperaturgefälle von Autoklaven aus. Die röntgenographische Strukturbestimmung bei 295 K ist durch folgende Daten charakterisiert: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{{{\rm P4}_{\rm 2} } \mathord{\left/ {\vphantom {{{\rm P4}_{\rm 2} } {{\rm mmc,\;Z = 2,\;a = 3,916}\left({\rm 2} \right){\AA},\;c = 6,155\left(2 \right){\AA},}}} \right. \kern-\nulldelimiterspace} {{\rm mmc,\;Z = 2,\;a = 3,916}\left({\rm 2} \right){\AA},\;c = 6,155\left(2 \right){\AA},}}} \hfill \\ {{\rm Z}\left({{\rm F}_{\rm 0}^{\rm 2} \ge 3\sigma\; {\rm F}_{\rm 0}^{\rm 2} } \right) = 74,\;{\rm R = 0,011}{\rm .}} \hfill \\\end{array} $$\end{document} In einer verzerrt kubisch flächenzentrierten Anordnung von S besetzt Li Tetraederlücken wie S in der ähnlich verzerrten Kugelpackung von Pt in PtS. Die Hydrogenatome der HS--Ionen sind in zwei linear über S verbundenen Positionen dynamisch fehlgeordnet. DSC-Messungen zeigen bei 228 K einen thermischen Effekt, der die Lagefixierung des HS--Ions vermuten läßt.
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    URL: http://dx.doi.org/10.1002/zaac.19895690111
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    Quantenchemische Modellrechnungen zur Baugruppenwanderung in Hexafluorosilicaten (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 131-136 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Quantum Chemical Model Calculations on the Migration of Si—F Groups in HexafluorosilicatesThe transport of different Si—F species was simulated using two [SiF6]2- octahedra as example. Activation barriers and charge distributions were calculated with the EHT method.Bearing in mind the structure of cubic hexafluorosilicates calculations were carried out on the migration both along an edge and along a (110) face of the elementary cell. At first [SiF2]2+ and SiF4 groups were removed from an [Si2F12]4- unit to produce a surface vacancy. During a second step planar SiF4 groups were moved to the neighbouring lattice position.A diffusion of planar SiF4 is favoured, if the electrostatic interaction between moved and fixed fluorine atoms is as small as possible.
    Notes: Das EHT-Verfahren wurde genutzt, um am Beispiel von zwei [Sif6]2--Baueinheiten den Transport verschiedener SiF-Spezies zu simulieren und dabei die auftretenden Aktivierungsbarrieren und Ladungsverteilungen zu berechnen. Ausgehend von der Struktur kubischer Alkalihexafluorosilicate wurden Rechnungen zum Transport entlang der Kante und entlang einer (110)-Fläche der Elementarzelle durchgeführt. Dabei wurden zunächst [SiF2]2+- bzw. SiF4-Gruppen aus dem [Si2F12]4--Verband zur Schaffung eines freien Oberflächenplatzes entfernt. In einem zweiten Schritt wurden im Modell [SiF8]4- planare SiF4-Gruppen zum jeweils benachbarten Gitterplatz transportiert.Der Transport eines [SiF2]2+-Moleküls erfordert einen wesentlich höheren Energieaufwand als der Transport von planarem SiF4. Eine Diffusion von planarem SiF4 wird begünstigt, wenn eine möglichst geringe elektrostatische Wechselwirkung zwischen den bewegten und feststehenden Fluoratomen stattfindet.
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    URL: http://dx.doi.org/10.1002/zaac.19895690113
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    Struktur und Eigenschaften quaternärer Chalkogenide MIAIIIBIVX4VI. III. Über die Verbindungen AgTiZrTe4 und Ag2TiZrTe4 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 145-152 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Properties of Quaternary Chalcogenides MIAIIIBIVX4VI. III. On the Compounds AgTiZrTe4 and Ag2TiZrTe4Preparation and properties of the compounds AgTiZrTe4 and Ag2TiZrTe4 are reported. The structure deduced from X-ray diffraction diagrams is closely related to the structure of TiZrTe4 showing an ordered accomodation of Ti and Zr atoms at the octahedral sites of the CdI2 type structure. The interlayers free of Ti and Zr atoms are suggested to be in part occupied by Ag+ ions in an ordered sequency, which allows to explain the occurrence of 8 Te layers in the repeating unit.
    Notes: Es wird über die Darstellung der Verbindungen AgTiZrTe4 und Ag2TiZrTe4 und deren Eigenschaften berichtet. Röntgenpulverdiffraktogramme lassen auf enge strukturchemische Beziehungen zum TiZrTe4 mit geordneter Verteilung der Ti- und Zr-Atome auf den Oktaederplätzen des CdI2-Strukturtyps schließen. Für die Ag+-Ionen wird eine partielle Besetzung der Tetraederlücken in den von Ti- bzw. Zr-Atomen freien Zwischenschichten in geordneter Abfolge in Betracht gezogen, die das Auftreten von 8 Te-Schichten in der Wiederholungseinheit erklärt.
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    URL: http://dx.doi.org/10.1002/zaac.19895690115
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    Über Chalkogenolate. 191. Ester der 2-Oxophenyldithioessigsäure 2. Kristall- und Molekülstruktur des Methylesters (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 569 (1989), S. 137-144 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 191. Esters of 2-Oxophenyldithioacetic Acid. 2. Crystal and Molecular Structure of the Methyl EsterThe title compound C6H5—CO—CS—SCH3 crystallizes with Z = 2 in the triclinic space group P1 with cell dimensions (-60°C) a = 6.236(4) Å, b = 7.972(2) Å, c = 9.589(4) Å, α = 88.42(3)°, β = 75.39(5)°, γ = 81.54(4)°. The structure has been determined from single crystal X-ray data measured at -60°C and refined to R = 0.085 and Rw = 0.087 for 2307 independent reflections. With nearly 20° the C=O bond is turned out of the plane of the phenyl ring.
    Notes: Die Titelverbindung C6H5—CO—CS—SCH3 kristallisiert triklin mit Z = 2 in der Raumgruppe P1 mit den Gitterdimensionen (-60°C) a = 6,236(4) Å, b = 7,972(2) Å, c = 9,589(4) Å, α = 88,42(3)°, β = 75,39(5)°, γ = 81,54(4)°. Die Kristallstruktur wurde aus bei -60°C vermessenen röntgenographischen Einkristalldaten unter Verwendung von 2307 symmetrieunabhängigen Reflexen bestimmt und bis auf Zuverlässigkeitsfaktoren von R = 0,085 und Rw = 0,087 verfeinert. Im Molekül ist die C=O-Bindung etwa 20° aus der Ebene des Phenylrings herausgedreht.
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    URL: http://dx.doi.org/10.1002/zaac.19895690114
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    Crystal structure of cadmium cyclohexaphosphate hexahydrate: Cd3P6O18 · 6 H2O (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 570 (1989), S. 138-144 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur eines Cadmiumcyclohexaphosphates: Cd3P6O18 · 6 H2OEs werden die Darstellung und die Kristallstruktur von Cd3P6O18 · 6 H2O beschrieben. Die Verbindung besitzt trigonale (rhomboedrische) Symmetrie, die Elementarzellendaten sind: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm a}_{\rm H} = 15.056(10)} & {{\rm c}_{\rm H} = 16.080(10){\rm }{\AA}} \\ \end{array} $$\end{document} oder \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm a}_{\rm R} = 10.212(10){\rm }{\AA}} & {{\rm \alpha }_{\rm R} = 94.98}\deg \\ \end{array} $$\end{document}Die Raumgruppe ist R3 mit Z = 6 in der hexagonalen Aufstellung. Die Kristallstruktur wurde mit Hilfe von 1355 unabhängigen Reflexen bis zu einem R-Wert von 0,013 bestimmt. Die P6O18-Ringanionen weisen eine dreizähnige Symmetrie auf. Das Cadmium-Koordinationspolyeder ist ein leicht verzerrtes Oktaeder, das von vier Sauerstoff-Atomen und zwei Wassermolekülen gebildet wird. Die Wassermoleküle verknüpfen diese Oktaeder zu Sechsringen mit der Symmetrie 3, diese Ringe wechseln sich entlang der 3-Achse mit den P6O18-Ring-Anionen ab.
    Notes: Chemical preparation and crystal structure of Cd3P6O18 · 6 H2O are described. This compound is trigonal (rhomboedral) with the following unit-cell dimensions: \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm a}_{\rm h} = 15.056(10)} & {{\rm c}_{\rm h} = 16.080(10){\rm }{\AA}} \\ \end{array} $$\end{document} or \documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{*{20}c} {{\rm a}_{\rm r} = 10.212(10){\rm }{\AA}} & {{\rm \alpha }_{\rm r} = 94.98}\deg \\ \end{array} $$\end{document}The space group is R3 with Z = 6 for the hexagonal description. The crystal structure has been solved by using 1355 unique reflexions with a final R value 0.013.The P6O18 ring anions have a threefold symmetry. The cadmium coordination polyhedron is a slightly distorted octahedron built up by four oxygen atoms and two water molecules. The water molecules link themselves as to build six-member rings having a 3 symmetry alterning with the P6O18 phosphoric rings along the 3 axes.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895700114
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  • 31
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    Electronic Resource
    Transition metal Complexes with the Thiosemicarbazide-based Ligands. VI. Nickel and zinc complexes with S-alkylisothiosemicarbazides (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 570 (1989), S. 167-176 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Übergangsmetall-Komplexe mit Thiosemicarbazid-Liganden. VI. Komplexe von NiII und ZnII mit S-AlkylisothiosemicarbazidDurch Umsetzung der ethanolischen Lösung von Ni(OAc)2 · 4 H2O mit S-Alkylisothiosemicarbazid-Iodwasserstoff (L—R · HI; R = Me, Et, n-Pr, n-Bu) und Pyridin wurden die oktaedrischen Bisligand-Komplexe der allgemeinen Formel [Ni(L—R)2Py2]I2 erhalten. Durch Erhitzen bei 95°C bzw. 110°C wurden die Komplexe in die quadratisch-planaren [Ni(L—R)2]I2 (R = Me, Et) - und [Ni(L—R)2I2] (R = n-Pr, n-Bu) - Komplexe mit verzerrt-oktaedrischer Konfiguration überführt. Ferner wurde in ethanolischer Lösung Zn(L—Me)2I2 dargestellt. Die Verbindungen wurden durch Elementaranalyse, TG, magnetische und spektroskopische Messungen charakterisiert.
    Notes: The reaction of warm ethanolic solution of Ni(OAc)2 · 4 H2O with S-alkylisothiosemicarbazide-hydrogeniodide (L—R · HI; R = Me, Et, n-Pr, n-Bu) and pyridine yielded the octahedral bis(ligand) complexes of the general formula [Ni(L—R)2Py2]I2. By the isothermal heating at 95 and 110°C, these complexes were transformed into the square-planar [Ni(L—R)2]I2 (R = Me, Et) complexes and the [Ni(L—R)2I2] (R = n-Pr, n-Bu) complexes of distorted octahedral configuration. Besides, the Zn(L—Me)2I2 complex was prepared. The compounds have been characterized by elemental analysis, magnetic measurements, diffuse reflectance spectra and TG analysis.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895700118
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  • 32
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    Electronic Resource
    Structure of molten systems KF—K2TiF6 and KCL-K2TiF6 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 570 (1989), S. 184-192 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Struktur der geschmolzenen Systeme KF—K2TiF6 und KCl—K2TiF6Die kongruent schmelzenden Verbindungen K3TiF7 und K3TiF6Cl, die in den Systemen KF—K2TiF6 bzw. KCl—K2TiF6 gebildet werden, zeigen einen starken Einfluß auf die Struktur (ionische Zusammensetzung) der Schmelzen der entsprechenden Systeme. In Anbetracht der relativ niedrigen Symmetrie und des hohen Energiezustandes der TiF73-- und TiF6Cl3--Ionen, sollte für sie ein hoher thermischer Dissoziationsgrad erwartet werden. Diese Annahme wird durch zwei verschiedene Methoden - die thermodynamische Analyse der Phasengleichgewichte und der Volumeneigenschaften bestätigt. Die Werte der Schmelzenthalpie für K2TiF6, K3TiF7 und K3TiF6Cl, die zu den Berechnungen verwendet werden, wurden ebenfalls bestimmt.
    Notes: Congruently melting compounds K3TiF7 and K3TiF6Cl which are formed in the systems KF—K2TiF6 and KCl—K2TiF6, respectively, exhibit a strong influence on the structure (ionic composition) of the melts of the corresponding systems. Considering the relatively low symmetry and a high energetic state of the TiF73- and TiF6Cl3- complex ions, a high degree of their thermal dissociation might be expected. This assumption was confirmed by two different methods based on a thermodynamic analysis of the phase equilibria and of the volume properties of the investigated systems, respectively. In connection with the former method, the values of the enthalpy of fusion of K2TiF6, K3TiF7, and K3TiF6Cl which were used in the calculations have also been estimated.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895700120
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  • 33
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    Experimente zur Mischkristallbildung zwischen Zinktantalaten und -antimonaten: ZnTa2-xSbxO6 und Zn4Ta2-xSbxO9 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 568 (1989), S. 22-28 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Experiments about the Mixed Crystal Formation between Zincoxotantalates and -antimonates: ZnTa2-xSbxO6 and Zn4Ta2-xSbxO9In the area of substituted oxotantalates of zinc two new phases of the composition A: ZnTa1·8Sb0·2O6 and B: Zn4Ta1·2Sb0·8O9 were prepared and investigated by X-ray single crystal technique. A crystallizes with tetragonal symmetry (space group D4h14-P42/mnm, a = 4.7314; c = 9.2160 Å; Z = 2). B is monoclinic (space group C2h6-C2/c; a = 15.103; b = 8.839; c = 10.378 Å; β = 93.81°; Z = 8). A crystallizes with trirutile structure, although there is a small replacement of Ta5+ by Sb5+. B maintains the Zn4Ta2O9 structure. One of the point positions of the M5+ ions is occupied statistically by Ta5+/Sb5+ and Zn2+. B is a metastable compound.
    Notes: Im Bereich substituierter Oxotantalate des Zinks wurden zwei neue Phasen A: ZnTa1,8Sb0,2O6 und B: Zn4Ta1,2Sb0,8O9 an Einkristallen röntgenographisch untersucht. A kristallisiert tetragonal (Raumgruppe D4h14-P42/mnm, a = 4,7314; c = 9,2160 Å; Z = 2), B monoklin (Raumgruppe C2h6-C2/c, a = 15,103; b = 8,839; c = 10,378 Å; β = 93,81°; Z = 8). A kristallisiert trotz des geringen Ersatzes von Ta5+ gegen Sb5+ im Trirutiltyp. B behält die Struktur von Zn4Ta2O9 bei. Eine Position der oktaedrisch koordinierten M5+-Ionen ist mit Zn2+ statistisch besetzt. B ist metastabil.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895680104
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  • 34
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    Ein Oxowolframat mit „Kanalstruktur“: KNa3WO5 (Mit einer Bemerkung über den Aufbau von Na4WO5) (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 143-156 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Oxotungstate with „Channel Structure“: KNa3WO5 (With a Remark on Na4WO5)For the first time single crystals of Na4WO5 were prepared by heating of annealing mixtures of Na2WO4 [2] and Na2O [Na:W = 4,2:1, Ni-cylinder, 725°C, 28 d]. Four-circle-diffraktometer data [PW 1100, 1900 IO(hkl), ω-2Θ scan, AgKα-radiation, R = 6,5%, RW = 5,7%] determine the triclinic structure of Na4WO5 with a = 569.4(2), b = 847.7(2), c = 565.7(1) pm, α = 101.29(2)°, β = 102.25(3)°, γ = 109.20(3)°. It is isotypic with the NaCl-type of structure Li4WO5. By heating Na4WO5 with K2O [Na:K:W = 4:3:1, Au-tube, 750°C, 35 d] colourless single crystals of KNa3WO5 were obtained for the first time. The structure determination [four-circle-diffraktometer data, PW 1100, ω-2Θ scan, 943 IO(hkl), MoKα-Strahlung R = 4.9%, RW = 3.9%] proves space group C2/m with a = 907.8(3), b = 753.9(2), c = 911.8(3) pm, β = 104.07(4)°, Z = 4. The structure is characterised by undulating layers of Na, W and O and two different kinds of channels.The Madelung Part of Lattice Energie, MAPLE, Effective Coordination Numbers, ECON, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.
    Notes: Neu dargestellt wurden farblose Einkristalle von Na4WO5 durch Tempern inniger Gemenge von Na2WO4 [2] und Na2O [Na:W = 4,2:1, Ni-Bömbchen, 725°C, 28 d]. Nach Vierkreisdiffraktometerdaten [PW 1100, 1900 IO(hkl), ω-2Θ-scan, AgKα-Strahlung, R = 6,5%, RW = 5,7%] kristallisiert Na4WO5 triklin mit a = 569,4(2), b = 847,7(2), c = 565,7(1) pm, 101,29(2)°, β = 102,25(3)°, γ = 109,20(3)°, Z = 2. Es ist isotyp mit der Kochsalzvarianten Li4WO5.Durch Erhitzen von Na4WO5 im Gemenge mit K2O [Na:K:W = 4:3:1, Au-Rohr, 750°C, 35 d] wurden erstmals farblose Einkristalle von KNa3WO5 erhalten. Die Strukturaufklärung [Vierkreisdiffraktometerdaten, PW 1100, ω-2Θ-scan, 943 IO(hkl), MoKα-Strahlung R = 4,9%, RW = 3,9%] belegt die Raumgruppe C2/m mit a = 907,8(3), b = 753,9(2), c = 911,8(3) pm, β = 104,07 (4)°, Z = 4. Der Aufbau ist durch gewellte Schichten aus Na, W und O und zwei verschiedene Sorten von Kanälen charakterisiert.Der Madelunganteil der Gitterenergie, MAPLE, Effektive Koordinationszahlen, ECON, diese über Mittlere Fiktive Ionenradien, werden berechnet und diskutiert.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730115
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  • 35
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    Darstellung von CF3SClF+MF6- (M = As, Sb) und Kristallstruktur von CF3SCl2+SbF6- (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 185-194 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of CF3SClF+MF6- (M = As, Sb) and Crystal Structure of CF3SCl2+SbF6-CF3SClF+MF6- (M = As, Sb) is prepared by oxidative fluorination of CF3SCl with XeF+MF6-. The new salt is characterized by IR, Raman and NMR spectra in comparison with CF3SF2+MF6- and CF3SCl2+MF6-. In SO2 solution CF3SClF+SbF6- symmetrizises into CF3SF2+SbF6- and crystalline CF3SCl2+SbF6- with the monoclinic space group P21/c with a = 773.5(14) pm, b = 954.8(15) pm, c = 1242.0(18) pm, β = 100.24(8)°, Z = 4.
    Notes: Die Darstellung von CF3SClF+MF6- (M = As, Sb) erfolgt durch oxidative Fluorierung von CF3SCl mit XeF+MF6-. Das Salz wird schwingungs- und NMR-spektroskopisch charakterisiert, orientierend an den bekannten Daten von CF3SF2+MF6- und CF3SCl2+MF6-. In einer SO2-Lösung symmetrisiert sich CF3SClF+SbF6- zu CF3SF2+SbF6- und einkristallinem CF3SCl2+SbF6- mit der monoklinen Raumgruppe P21/c, a = 773,5(14) pm, b = 954,8(15) pm, c = 1242,0(18) pm, β = 100,24(8)°, Z = 4.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895730118
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  • 36
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    Zwei neue Rubidiumlithiumzincate: RbLiZnO2 und RbLiZn2O3 (mit einer Bemerkung über CsLiZnO2) (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 568 (1989), S. 136-146 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Rubidium Lithium Zincates: RbLiZnO2 and RbLiZn2O3For the first time colourless single crystals of RbLiZnO2 (A) and RbLiZn2O3 (B) have been prepared. Both crystallize tetragonally, A: space group I4/mmm, Z = 2, a = 351.84(4), c = 1153.3(2) pm; B: space group P42/mnm, Z = 4, a = 1 033.8(1), c = 342.8(1) pm. The crystal structures have been determined from four circle diffractometer data (MoKα; A: 155 hkl, R = 7.9%, Rw = 7.6%; B: 384 hkl, R = 7.0%, Rw = 4.6%). RbLiZnO2 has the BaZn2P2 type of structure while RbLiZn2O3 exhibits a new structure type with linear chains of face shared cubes ∞1[O4/2RbO4/2RbO4/2] as characteristic feature. For both oxides the Madelung part of lattice energy (MAPLE), and effective coordination numbers (ECoN) are calculated.
    Notes: Neu dargestellt wurden die Oxide RbLiZnO2 (A) und RbLiZn2O3 (B) in Form farbloser Einkristalle durch Tempern entsprechender Gemenge der binären Oxide. Beide Zincate kristallisieren tetragonal, A: Raumgr. I4/mmm, Z = 2, a = 351,84(4), c = 1153,3(2) pm; B: Raumgr. P42/mnm, Z = 4, a = 1 033,8(1), c = 342,8(1) pm. Die Kristallstrukturen wurden aus Vierkreisdiffraktometerdaten (MoKα) bestimmt (A: 155 hkl, R = 7,9%, Rw = 7,6%; B: 384 hkl, R = 7,0%, Rw = 4,6%). RbLiZnO2 kristallisiert im BaZn2P2-Strukturtyp, RbLiZn2O3 zeigt eine neue Struktur mit charakteristischen Würfel-Doppelketten ∞1[O4/2RbO4/2RbO4/2]. Der Madelunganteil der Gitterenergie (MAPLE) sowie effektive Koordinationszahlen (ECoN) wurden jeweils berechnet.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895680116
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  • 37
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    Zur Kenntnis des α-NaFeO2-Types: Über KPrO2 [1] (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 568 (1989), S. 147-150 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the α-NaFeO2-Type: On KPrO2For the first time we obtained yellow-green single crystals of KPrO2 by annealing K2PrO3 in Ni-cylinders [1 000°C; 4 weeks]. The structure determination confirms the trigonal rhombohedral α-NaFeO2-type: a = 365.11(3), c = 1 859.65(21) pm, c/a = 5.09, Z = 3, spacegroup R3m, fourcircle diffractometer data (Philips PW 1100), MoKα, 134 Io(hkl), R = 2.58%, Rw = 2,42%.
    Notes: Erstmals erhielten wir gelbgrüne Einkristalle von KPrO2 durch Tempern von K2PrO3 in Ni-Bömbchen [1000°C; 4 Wochen]. Es liegt der trigonal-rhomboedrische α-NaFeO2 Typ vor: a = 365,11(3), c = 1 859,65(21) pm, c/a = 5,09, Z = 3, Raumgruppe R3m, Vierkreisdiffraktometerdaten (Philips PW 1100), MoKα, 134 Io(hkl), R = 2,58%, Rw = 2,42%.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19895680117
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  • 38
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    Herstellung keramischer Pulver. II. Über die Bildung von Mg2TiO4, MgTiO3 und MgTi2O5 durch Hydrolyse von 2-Ethoxyethylaten (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 208-214 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Ceramic Powders. II. Mg2TiO4, MgTiO3, and MgTi2O5 Formed by Hydrolysis of 2-EthoxyethylatesSolutions of 2-ethoxyethylates of magnesium and titanium in 2-ethoxyethanol submitted to hydrolysis, evaporation and heating of the residue up to 450°C allow to prepare Mg2TiO4, MgTiO3, and MgTi2O5 in an amorphous state with smaller than 1% of volatile components. Highly dispersed powders showing an increased sintering activity are obtained as a result of recrystallization. Mg2TiO4 is formed as inverse spinel phase in a metastable state.
    Notes: Die 2-Ethoxyethylate von Magnesium und Titan bilden in 2-Ethoxyethanol stabile Lösungen, deren Hydrolyse nach dem Abdestillieren des Lösungsmittels und Erhitzen des Rückstandes bis auf 450°C die Herstellung von Mg2TiO4, MgTiO3 und MgTi2O5 im amorphen Zustand mit weniger als 1% flüchtigen Bestandteilen gestattet. Die Rekristallisation führt zu hochdispersen sinteraktiven Pulvern, im Fall von Mg2TiO4 zur Bildung der inversen Spinellphase unter metastabilen Bedingungen.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730121
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  • 39
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    Electronic Resource
    The electrochemical synthesis of neutral Nickel(II) Complexes of Schiff Base Ligands: The crystal structure of bis-{N-[2-(2-pyridyl)ethyl]salicylideneiminato}nickel(II) trihydrate (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 215-222 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Elektrochemische Synthese von neutralen Nickel(II)-Komplexen mit Schiffschen Basen: Kristallstruktur von Bis-{N-[2-(2-pyridyl) äthyl]-salicylideneiminato}nickel(II) TrihydratNickel(II)-Komplexe mit im Pyridin-Ring substituiertem N-2-(2-pyridyl)-äthyl-salicylideneiminat wurden durch Elektrolyse einer nicht wäßrigen Lösung des entsprechenden Liganden hergestellt; als Anode diente ein Ni-Draht. Die Struktur von Bis-{N-[2-(2-pyridyl)äthyl]-salicylideneiminato}nickel(II). Trihydrat wurde röntgenographisch bestimmt. Der Komplex kristallisiert triklin in der Raumgruppe P1 mit den Gitterkonstanten a = 13,055(4) Å, b = 13,097(6)Å, c = 16,189(5) Å, α = 102,92(3)°, β = 99,80(3)°, γ = 90,42(3)° und Z = 4. Eine Least-squares-Verfeinerung führte zu einem R-Wert von 0,047. Das Molekül ist nicht zentrosymmetrisch, da die zwei dreizähnigen Liganden eine meridionale Konfiguration um das oktaedrisch koordinierte Nickel(II) annehmen.
    Notes: Nickel(II) complexes with N-2-(2-pyridyl)ethyl-ring substituted salicylideneiminatos have been synthesized by an electrochemical procedure using a sacrificial anode in non-aqueous solution of the corresponding ligand. The structure of bis{N-[2-(2-pyridyl)]-salicylideneiminato}-nickel (II) trihydrate has been determined by X-ray diffraction. Crystals are triclinic, space group P1, with four formula units in a cell of dimensions a = 13.055(4) Å, b = 13.097(6) Å, c = 16.189(5) Å, and α = 102.92(3)°, β = 99.80(3)°, γ = 90.42(3)°. Full matrix least squares refinement on R converged with a conventional agreement factor of 0.047. The molecule is non-centrosymmetric with two terdentate ligands in a meridional configuration around octahedral nickel(II).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730122
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  • 40
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    Beiträge zur Untersuchung anorganischer nichtstöchiometrischer Verbindungen. XXXVIII. Quaternäre Nioboxidfluoride des Cadmiums und Mangans mit LiNb6O15F-Struktur (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 240-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895730125
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  • 41
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    Pollucite- and Leucite-related Phases: A2BX5O12 and ACX2O6 (A = K, Rb, Cs; B = Be, Mg, Fe, Co, Ni, Cu, Zn, Cd; C = B, Al, Ga, Fe, Cr; X = Si, Ge) (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 223-230 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pollucit- und Leucit-verwandte Phasen: A2BX5O12 und ACX2O6 (A = K, Rb, Cs; B = Be, Mg, Fe, Co, Ni, Cu, Zn, Cd; C = B, Al, Ga, Fe, Cr; X = Si, Ge)Darstellung und kristallographische Daten von 29 neuen Phasen dieser Strukturfamilie werden angegeben. Ein Überblick über die gesamte Strukturfamilie, die bis jetzt 59 Phasen enthält, wird gegeben. Die Familie enthält wenigstens sieben Strukturvarianten, von denen zwei die Pollucit-, CsAlSi2O6, und Leucit-, KAlSi2O6, Struktur sind. Beziehungen zwischen der Kationengröße und dem Strukturtyp werden vorgestellt. Ungewöhnliche Variationen in den Größen der Einheitszelle als Funktion der Kationengröße werden diskutiert, und auf die mögliche Bedeutung für das „partially collapsed framework“-Konzept von Taylor und Henderson wird hingewiesen.
    Notes: Synthesis and crystallographic data on 29 new phases in this family are given. A survey of the crystal chemistry of the complete family, containing 59 phases to date, is presented. The family contains at least seven structural variations, two of which are the pollucite, CsAlSi2O6 and leucite, KAlSi2O6 structures. Correlations between cation size and structure type are presented. Unusual variations in unit cell dimensions as a function of cation size are discussed and the possible relevance of the „partially collapsed framework“ concept of Taylor and Henderson indicated.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730123
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    Untersuchungen zur heterogen-katalysierten Ringalkylierung von Toluen mit Methanol an modifizierten ZSM-5-Zeolithen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 231-239 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies of the Heterogeneous Catalytical Ring Alkylation of Toluene with Methanol on Modified Zeolites ZSM-5Various ways for controlling the catalytic activity, the shape selectivity, and the deactivation behaviour of modified zeolites ZSM-5 has been shown by the example of the heterogeneous catalytical conversion of toluene with methanol. The preferred formation of the industrially interesting para-xylene is possible by use of ZSM-5-zeolites composed of large crystals, by dealumination of the external surface after hydrothermal treatment, by poisoning of external active centres after impregnation with inorganic salts as well as by isomorphic incorporation of boron for silicon and/or aluminium in the zeolite framework.
    Notes: Am Beispiel der heterogen-katalysierten Umsetzung von Toluen mit Methanol wurden verschiedene Wege zur Steuerung der katalytischen Aktivität, der Formselektivität und des Desaktivierungsverhaltens modifizierter H-ZSM-5-Zeolithe aufgezeigt. Eine Ausprägung der bei der Toluenmethylierung technisch interessanten para-Xylen-Selektivität gelingt durch den Einsatz von großkristallinen ZSM-5-Zeolithen, durch Dealuminieren der äußeren Oberfläche mittels hydrothermaler Behandlung, durch Vergiften äußerer aktiver Zentren mittels Tränkung anorganischer Salze sowie durch den isomorphen Einbau von Bor für Silicium und/oder Aluminium im Zeolithgerüst.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730124
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    Die Reaktion von Trichloracetyltrischwefeltrinitrid mit Molybdänpentachlorid. Die Kristallstrukturen von CCl3CO-NS3N2 und (PPh4)2[MoCl3(N2SCOCCl3)]2 · 2CH2Cl2 · 2CCl4 Z. anorg. allg. Chem. 562 (1988) 31 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 240-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895730126
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  • 44
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    Synthese und Charakterisierung von Sulfinato-Nickel(II)-Komplexen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 240-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895730127
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  • 45
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    Masthead (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895750101
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  • 46
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    Günther Rienäcker zum Gedenken (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 7-9 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895750102
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  • 47
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    Synthese, IR-Spektrum und Kristallstruktur von N,N'-Bis(trimethylsilyl)benzamidinium-tetrachloroferrat(III) (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 10-16 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, IR Spectrum, and Crystal Structure of N,N'-Bis(trimethylsilyl)benzamidinium Tetrachloroferrate(III)The title compound [C6H5—C(NHSiMe3)2][FeCl4] is obtained by the reaction of FeCl3 with N,N,N'-tris(trimethylsilyl)benzamidine in the presence of tetrahydrofurane, forming yellow, moisture sensitive crystals. The compound is characterized by its IR spectrum as well as by an X-ray structure determination. Space group P21/n, Z = 8, 5974 independent observed reflexions, R = 0.066. The lattice dimensions are at -70°C: a = 2110.7, b = 1109.5, c = 2120.4 pm; β = 111.17º. The compound forms ion pairs, in which the H atoms of the amidinium cation are coordinated with one chlorine ligand of the FeCl4- ion in a chelating manner.
    Notes: Die Titelverbindung [C6H5—C(NHSiMe3)2][FeCl4] entsteht in Form gelber feuchtigkeitsempfindlicher Kristalle bei der Einwirkung von Eisen(III)chlorid auf N,N,N'-Tris(trimethylsilyl)benzamidin in Gegenwart von Tetrahydrofuran. Die Verbindung wurde durch das IR-Spektrum und durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/n, Z = 8, 5974 unabhängige beobachtete Reflexe, R = 6,6%. Die Gitterkonstanten betragen bei -70°: a = 2110,7; b = 1109,5; c = 2120,4 pm; β = 111,17º. Die Verbindung bildet Ionenpaare, in denen die H-Atome des Amidiniumkations eines der Chloratome des FeCl4--Anions chelatartig umgeben.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895750103
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  • 48
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    Ni5HfB2O10 mit geordneter MetallverteilungProfessor Reginald Gruehn zum 60. Geburtstage am 6. Oktober 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 26-30 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ni5HfB2O10 with Ordered Metal DistributionNi5HfB2O10 was prepared for the first time and investigated by X-ray methods. It crystallizes with orthorhombic symmetry, space group D2h16 - Pnma, a = 9.328; b = 6.120; c = 12.334 Å; Z = 4. In opposition to the Ni5TiB2O10-type all metal point positions are strongly ordered. The authors are in doubt about the partly statistic metal distribution within Ni5M4+B2O10 (M4+ = Ti, Zr, Ge).
    Notes: Ni5HfB2O10 wurde erstmals dargestellt und an Einkristallen untersucht. Ni5HfB2O10 kristallisiert orthorhombisch, Raumgruppe D2h16 - Pnma, a = 9,328; b = 6,120; c = 12,334 Å, Z = 4. Im Gegensatz zum Ni5TiB2O10-Typ weist NiHfB2O10 eine total geordnete Metallverteilung auf. Die partiell statistische Verteilung von Ni2+ mit M4+ (M4+ = Ti, Zr, Ge) wird in Frage gestellt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895750105
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  • 49
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    27Al-NMR-Untersuchungen an Alkalifluoroaluminaten (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 17-25 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 27Al NMR Studies on Alkali FluoroaluminatesThe 27Al NMR spectra of the alkali fluoroaluminates sensitively reflect the kind of condensation of the AlF6 octahedra. Whereas the chemical shift of the octahedral Al is shown to be rather independent on structural details, clear differences in the electric field gradients of isolated and condensed AlF6 octahedra were found. In contrast to the isolated octahedra which show only weak effects of quadrupole interaction, both for chains and layers of AlF6 octahedra axial EFG tensors result with quadrupolar coupling constants of between 10 and 13 MHz; for the threefold chains in CsAlF4 only a value of 7.5 MHz is obtained.
    Notes: Die 27Al-NMR-Spektren der Alkalifluoroaluminate spiegeln in empfindlicher Weise die Verknüpfung der AlF6-Oktaeder wider. Während sich die chemische Verschiebung für das oktaedrisch koordinierte Aluminium als nahezu unbeeinflußt von strukturellen Details erweist, ergeben sich deutliche Unterschiede in den elektrischen Feldgradienten (EFG) zwischen isolierten und verknüpften AlF6-Oktaedern. Im Gegensatz zu den isolierten Oktaedern, bei denen Quadrupolwechselwirkungseffekte nur eine untergeordnete Rolle spielen, ergeben sich sowohl für Ketten als auch schichtförmige Verknüpfung der AlF6-Oktaeder axiale EFG-Tensoren mit Quadrupolkopplungskonstanten zwischen 10 und 13 MHz, bei Verknüpfung als Dreierstrangkette im CsAlF4 lediglich ein Wert von 7,5 MHz.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895750104
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  • 50
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    Chemische, thermoanalytische und röntgenorgraphische Untersuchungen zur Bildung des β-Ca2[P2O7] aus dem Ca2[P4O12] · 4 H2OProfessor Lothar Kolditz zum 60. Geburtstage gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989), S. 267-271 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemical, Thermoanalytical, and X-ray Investigations to the Formation of the β-Ca2[P2O7] from the Ca2[P4O12] · 4 H2OThe formation of β-Ca2[P2O7] from Ca2[P4O12] · 4 H2O (modification I) proceeds crystallographically oriented in several steps: In one of these steps an X-ray amorphous phase is formed and simultaneously cyclotetraphosphate reorganizes to polyphosphate. The dehydration proceeds in 2 steps: At 120°C 3 molecules and at 220°C 1 molecule are lost, respectively. The formation of diphosphate from polyphosphate, which is connected with the loss of P2O5, takes place at 850°C according to high temperature Guinier.
    Notes: Die Bildung des β-Ca2[P2O7] aus dem Ca2[P4O12] · 4 H2O (Form I) läuft über mehrere Stufen kristallographisch orientiert ab. Eine der Zwischenstufen ist röntgenamorph. Bei ihrer Bildung entsteht aus dem Cyclotetraphosphat höherkondensiertes Polyphosphat. Die Wasserabgabe erfolgt in zwei Schritten: Bei 120°C werden 3 Mol, bei 220°C ein Mol H2O abgegeben. Der mit P2O5-Abgabe verbundene übergang Poly- in Diphosphat erfolgt laut Heizguinier bei 850°C.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895760130
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    Masthead (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 572 (1989) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895720101
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  • 52
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    Metallorganische Chemie mit P/N-Chelatliganden. I. Molybdän- und Eisen(0)-Verbindungen des 2-Diphenylphosphinomethylpyridins (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 74-82 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organometallic Chemistry with P/N-Chelating Ligands. I. Molybdenum and Iron(0) Compounds of 2-DiphenylphosphinomethylpyridineThe reaction of 2-diphenylphosphinomethylpyridine 1 (PN) with norbornadiene-tetracarbonylmolybdenum gives (PN)Mo(CO)4 2 in good yield. The acetonitrile ligands in (π-C3H5)Mo(CO)2(CH3CN)2Br 3 are easily exchanged by 1. The thus formed complex (π-C3H5)(PN)Mo(CO)2Br 4 undergoes a reductive deallylation with further 1 to afford cis-(PN)2Mo(CO)2 6. Deallylation of 3 by triphenylphosphine and subsequent reaction with 1 yields the complex cis-(CO)2-trans-(PPh3)2Mo(PN) 7. Ligand 1 displays a chelating function in all of the molybdenum complexes. The structures of the (PN)-complexes are deduced mainly from the nmr data. The initial product of the photochemical reaction of 1 with ironpentacarbonyl is (PN)Fe(CO)4 8, followed by trans-(PN)2Fe(CO)3 9. In both cases 1 is bonded via the phosphorus atom only. Prolonged irradiation affords the chelated tricarbonyl (PN)Fe(CO)3 10. The thermal reaction of 1 with Fe2(CO)9 is different in that the first product is a sensitive red compound 11, which still contains bridging carbonyl groups and has to be formulated as (PN)Fe2(CO)7. Longer reaction times, but also the reaction of 8 with Fe2(CO)9 finally give a new type of complex, (PN)Fe2(CO)6 12, without bridging carbonyls.
    Notes: Mit 2-Diphenylphosphinomethylpyridin 1 (PN) wird aus Norbornadien-tetracarbonylmolybdän (PN)Mo(CO)4 2 erhalten. Im π-Allyl-Komplex (π-C3H5)Mo(CO)2(CH3CN)2Br 3 läßt sich das Acetonitril leicht gegen 1 austauschen. Der so gebildete Komplex (ß-C3H5)(PN)Mo(CO)2Br 4 reagiert mit weiterem 1 unter reduktiver Entallylierung zu cis-(PN)2Mo(CO)2 6, während man durch vorangehende Entallylierung von 3 durch Triphenylphosphin und nachfolgende Reaktion mit 1 den Komplex cis-(CO)2-trans-(PPh3)2Mo(PN) 7 erhält. In allen Molybdänkomplexen hat 1 Chelatfunktion. Die Strukturen können für die (PN)-Komplexe insbesondere aus den NMR-Spektren erschlossen werden. Mit Eisenpentacarbonyl wird photochemisch zunächst (PN)Fe(CO)4 8, als nächstes trans-(PN)2Fe(CO)3 9 gebildet. In beiden Fällen ist 1 nur über den Phosphor gebunden. Bei längerer Bestrahlung wird auch das Chelat-tricarbonyl (PN)Fe(CO)3 10 erhalten. Anders verläuft die thermische Reaktion von 1 mit Fe2(CO)9, bei der zunächst ein empfindliches, rotes Produkt 11 gebildet wird, das noch Brückencarbonylgruppen enthält und als (PN)Fe2(CO)7 formuliert werden muß. Längere Reaktionszeiten, aber auch die Reaktion von 8 mit Fe2(CO)9 ergeben schließlich ein neuartiges Produkt (PN)Fe2(CO)6 12 ohne Brückencarbonyl.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895770108
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    Beiträge zur Chemie organometallischer metallacyclischer Übergangsmetallverbindungen. I. Synthese und Eigenschaften von Li2(solv)x und seine Umsetzung mit CO2 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 115-121 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Organometallic Metallacyclic Transition Metal Compounds. I. Synthesis and Properties of Li2(solv)x and its Reaction with CO2The reaction of ZrCl4(thf)2 with LiCH2CH2CH2CH2Li at -78°C in diethyl ether and addition of tetrahydrofuran (thf) yield Li2Zr(C4H8)3(thf)5,5 (I). The displacement of thf by dioxane (dx) or tetramethylethylenediamine (tmed) gives Li2Zr(C4H8)3(dx)3 (Ia) or Li2Zr(C4H8)3(tmed)3 (Ib). I decomposes at room temperature, Ia and Ib however are stable at room temperature for a short time.The reaction between I and CO2 and subsequent treatment of the reaction mixtures with water yield .
    Notes: Die Umsetzung von ZrCl4(thf)2 mit LiCH2CH2CH2CH2Li bei -78°C in Diethylether führt nach Zugabe von Tetrahydrofuran (thf) zur Bildung von Li2Zr(C4H8)3(thf)5,5 (I). Der Austausch von thf gegen 1,4-Dioxan (dx) bzw. Tetramethylethylendiamin (tmed) ergibt die kristallinen Verbindungen Li2Zr(C4H8)3(dx)3 (Ia) bzw. Li2Zr(C4H8)3(tmed)3 (Ib). Während die Zer-setzung von I bei Raumtemperatur sehr bald unter Dunkelfärbung beginnt, sind Ia und Ib begrenzte Zeit bei Raumtemperatur lagerfähig.Die Umsetzung von I mit CO2 und anschließende Hydrolyse der Reaktionsprodukte ergeben .
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    URL: http://dx.doi.org/10.1002/zaac.19895770113
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    Synthese und Struktur der ersten sechsgliedrigen Selena- und PlatinatriazaphosphorineProfessor Lothar Kolditz zum 60. Geburtstage gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989), S. 255-266 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Strukture of the First Six-membered Selena- and PlatinatriazaphosphorinesThe reaction of PhCN with Li[N(SiMe3)2], Ph2PCl and Me3SiN3 leads to the starting material (Me3Si)2NC(Ph)NP(Ph)2N(SiMe3) 1. 1-Chloro-3,3,5-triphenyl-1λ4,2,4,6,3λ5-selenatriazaphosphorine 2 is formed when 1 is treated with SeCl4. (Ph3P)2Pt(C2H4) as well as (Ph3P)4Pt react with 1 to yield the six-membered platinum containing heterocycles 2 and 4. The six-membered rings 2 and 4 were characterized by and X-ray single crystal structure analysis.
    Notes: Die Reaktion von PhCN mit Li[N(SiMe3)2], Ph2PCl und Me3SiN3 führt zu der Ausgangsverbindung (Me3Si)2NC(Ph)NP(Ph)2N(SiMe3) 1. Mit SeCl4 und 1 entsteht das 1-Chlor-3,3,5-triphenyl-1λ4,2,4,6,3λ5-selenatriazaphosphorin 2. Sowohl (Ph3P)2Pt(C2H4) als auch (Ph3P)4Pt reagieren mit 1 unter Bildung der sechsgliedrigen, platinhaltigen Heterocyclen 2 und 4. Die sechsgliedrigen Ringe 2 und 4 werden durch eine Einkristall-Röntgenstrukturanalyse charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19895760129
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    Zur Darstellung von Cyclophosphaten, Cyclophosphatophosphonaten, Diphosphonaten und Diphosphiten in HarnstoffschmelzenProfessor Lothar Kolditz zum 60. Geburtstage gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989), S. 272-280 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of Cyclophosphates, Cyclophosphatophosphonates, Diphosphonates, and Di-phosphites in Urea MeltsAmmonium cyclotriphosphate (NH4)P3O9, ammonium cyclotetraphosphate [PIV—PIV —O—]2, ammonium cyclotriphosphatophosphonates Ammonium organyldiphosphonates And ammonium diphosphites are prepared in high yields on heating acidic phosphates, phosphonates, and phosphites in urea or urea/ammonium nitrate melts. The mechanism of the dehydration of phosphorus compounds containing POH groups in molten urea is discussed.
    Notes: Durch Erhitzen (140-200°C) von sauren Phosphaten, Phosphonaten und Phosphiten in Harnstoff- oder Harnstoff/Ammoniumnitrat-Schmelzen wurden in hohen Ausbeuten hergestellt: Ammoniumcyclotriphosphat (NH4)3P3O9, Ammoniumcyclotetraphosphat [PIV—PIV—O—]2, Ammoniumcyclotriphosphatophosphonate (Dioxatriphosphinane)Ammoniumorganyldiphosphonate und Ammoniumdiphosphit (NH4)2P2O5.Der Mechanismus der Dehydratisierung von POH-Gruppen enthaltenden Phosphorverbindungen in geschmolzenem Harnstoff wird diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19895760131
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    Masthead (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895770101
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    Über die durch Riesencluster des Palladiums katalysierte Oxydation von AmeisensäureProfessor Lothar Kolditz zum 60. Geburtstage gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989), S. 284-292 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Oxidation of Formic Acid Catalyzed by Giant Palladium ClustersLiquid-phase oxidation of formic acid by oxygen in acetonitrile solutions is catalyzed by giant clusters Pd561Phen60(OAc)180 or Pd561Phen60(O)60 at 20-70°C. The reaction is first-order in the cluster and formic acid concentrations. Dependence of the reaction rates on O2 concentration is described by Michaelis-type equation. Kinetic isotope effects are found to be k(HCOOH)/k(HCOOD) = 1.1 ± 0.1 and k(HCOOH)/k(DCOOD) = 1.0 ± 0.1. On the base of the kinetic data the reaction mechanism is discussed.
    Notes: Die Flüssigphasenoxydation von Ameisensäure durch molekularen Sauerstoff wird in Acetonitrillösung und Temperaturen von 20 bis 70°C durch die Riesencluster des Palladiums Pd561Phen60(OAc)180 oder Pd561Phen60(O)60(PF)60 katalysiert. Diese Oxydation verläuft als Reaktion erster Ordnung bezüglich der Cluster- und Ameisensäurekonzentration. Eine Beziehung vom Typ der Michaelis-Gleichung beschreibt die Abhängigkeit der Reaktionsgeschwindigkeit von der O2-Konzentration. Die kinetischen Isotopieeffekte betragen: k(HCOOH)/k(HCOOD) = 1,1 ± 0,1 und k(HCOOH)/k(DCOOD) = 1,0 ± 0,1. Auf der Grundlage der kinetischen Daten wird der Reaktionsmechanismus diskutiert.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895760133
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    Theoretische Untersuchungen zum Charge-Transfer in Akzeptorligand-d6-Metall-Komplexen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 23-38 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Theoretical Investigations on the Charge Transfer of d6-Metal Complexes with Acceptor LigandsOn the basis of the electronic structure of pentaammineruthenium(II) and pentacyanoferrate(II) complexes with aromatic N-heterocyclic ligands L the different tendency of the complex fragments to charge-transfer interactions with acceptor molecules is discussed. The increased energy and the reduced absorption intensity of the metal oxidation band of [Fe(CN)5L]3- are due to the diminished orbital interaction between the pentacyanoferrate(II) fragment and the nitrogen acceptor ligand caused by π-bonding interaction of the central metal with the cyanide co-ligands. The possibility of the variation of the energy of the acceptor levels connected with the position of the MLCT bands of the mixed-ligand complexes has been investigated by numerous azine and α-diimine ligands of different structure. Besides inductive and mesomeric effects the steric influences on the π-acceptor ability of the ligand and on the energy and absorption intensity of the MLCT band are examined.
    Notes: Auf der Grundlage der Elektronenstruktur von Pentamminruthenium(II)-und Pentacyanoferrat(II)-Komplexen mit aromatischen N-heterocyclischen Liganden wird die unterschiedliche Tendenz der Komplexfragmente zur Charge-Transfer-Wechselwirkung mit Akzeptorliganden diskutiert. Die verringerte Orbitalwechselwirkung des Pentacyanoferrat(II)-Fragments mit dem N-Akzeptor ist die Ursache für die höhere Energie und die reduzierte Absorptionsintensität der Metalloxydationsbande. Sie resultiert aus der zusätzlichen π-Bindungswechselwirkung zwischen dem Metallzentrum und den Cyanidliganden. Am Beispiel unterschiedlicher Azin- und α-Diiminliganden werden Möglichkeiten zur Variation der Energie des Akzeptorniveaus und damit der energetischen Position der MLCT-Bande untersucht. Neben induktiven und mesomeren Effekten werden vor allem die sterischen Einflüsse auf die π-Akzeptorfähigkeit des Liganden und ihre Auswirkung auf die Energie und die Absorptionsintensität der MLCT-Bande betrachtet.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895770104
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    Zum relativen Donor-Akzeptor-Verhalten einzähniger Liganden. Eine EHT-Studie (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 59-73 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Relative Donor-Acceptor-Properties of Monodentate Ligands. An EHT-StudyThe relative donor-acceptor properties of some important monodentate ligands are investigated by means of the extended Hückel method and a suitable graduation is determined. Charge gradations are discussed and results compared with known facts. Acceptor properties of ligands with phosphorous and sulfur atoms are described in the best manner using charge iterations at the atoms mentioned.
    Notes: Mit Hilfe der EHT-Methode werden die relativen Donor- und Akzeptor-Eigenschaften einiger wichtiger einzähniger Komplexliganden untersucht und eine entsprechende Abstufung ermittelt. Ladungsdifferenzierungen werden diskutiert und die Ergebnisse mit bekannten Erkenntnissen verglichen. Durch die Ladungsiteration an Phosphor- und Schwefelliganden lassen sich die Akzeptoreigenschaften dieser Moleküle relativ gut beschreiben.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895770107
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    Semichinon- und Catecholat-Koordinationsverbindungen der späten 3d-Metalle (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 93-101 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Semiquinone and Catecholate Coordination Compounds of the Late 3d-Metals9,10-Phenanthrenequinone reacts on a different way with olefine complexes of iron, cobalt, and nickel, obtaining semiquinone and catecholate coordination compounds. These compounds are also formed by a reducing process of metal salts and phenanthrenequinone. Some mono- and dimeric semiquinone complexes are prepared by an additional coordination of tetramethyl-ethylenediamine or inner complexes of salene type as chelate ligands. The new chelates are characterized by the magnetic moments, the u.v./vis., the i.r., and the e.s.r. spectra.
    Notes: 9,10-Phenanthrenchinon reagiert auf unterschiedliche Weise mit Olefinkomplexen des Eisens, Cobalts und Nickels, wobei Semichinon- oder Catecholat-Komplexe entstehen. Diese Verbindungen können auch durch reduktive Umsetzung aus den Metallsalzen und Phenanthrenchinon erhalten werden. Zusätzliche Koordination von Tetramethylethylendiamin oder von Salen-Innerkomplexen führt zu einer Reihe von mono- und dinuclearen Semichinon-Komplex-verbindungen. Die Charakterisierung der Produkte erfolgt anhand der magnetischen Momente und mittels IR-, UV/VIS- sowie ESR-Spektroskopie.
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    Neutronenbeugung an Li2CuO2Professor Kurt Issleib zum 70. Geburtstage am 19. November 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 18-26 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Neutron Diffraction on Li2CuO2Li2CuO2 was investigated by neutron powder diffraction at 300 K and 4.2 K (diffractometer SV7 at FRJ-2 in KFA Jülich, λ = 109 pm).The crystallographic orthorhombique space group Immm determined previously by x-ray diffraction on single crystals was confirmed. Lattice parameters and atomic positional parameters were refined: a = 366.14(8), b = 286.14(6), c = 939.4(2) pm; z(Li) = 0.7122(17), z(O) = 0.6411(7).Li2CuO2 orders antiferromagnetically below 10 K with an antiparallel coupling of the magnetic moments of Cu2+ in (0, 0, 0) and (1/2, 1/2, 1/2). The moments are orientated perpendicular to the c-axis. The ordered magnetic moment is μ = 0.9(1) μB per Cu2+ at 4.2 K. The magnetic Bravais-Lattice is PI, the magnetic space group is PImmm with similar parameters.
    Notes: Li2CuO2 wurde mit Neutronenpulverdiffraktometrie bei 300 K und 4,2 K untersucht (Diffraktometer SV7 am FRJ-2 in KFA Jülich, λ = 109 pm).Die aus Röntgen-Einkristalldaten bestimmte orthorhombische Raumgruppe Immm wurde bestätigt, Gitterkonstanten und Atompositionsparameter wurden verfeinert: a = 366,14(8), b = 286,14(6), c = 939,4(2) pm; z(Li) = 0,7122(17), z(O) = 0,6411(7).Unterhalb von 10K ordnet Li2CuO2 antiferromagnetisch mit einer antiparallelen Einstellung der magnetischen Momente von Cu2+ in (0, 0, 0) und (1/2, 1/2, 1/2). Die Momentorientierung ist senkrecht zur c-Achse. Das geordnete magnetische Moment beträgt μ = 0,9(1) μB pro Cu2+ bei 4,2 K. Das magnetische Bravais-Gitter ist PI, die magnetische Raumgruppe bei gleichen Gitterkonstanten PImmm.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895780103
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    Pseudochalkogenverbindungen. XXIPseudochalkogenverbindungen XX: Köhler, H.; Ahmed, S.; Jäger, L.; Kolbe, A. Z. Anorg. allg. Chem. 576 (1989) 197.. Zur Synthese und Struktur von Phosphor(III)-und Phosphor(V)-organocyanamiden (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 69-74 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pseudochalcogen Compounds. XXI. Synthesis of Phosphorus(III) and Phosphorus(V) OrganocyanamidesThe synthesis of a series of phosphorus(III) and phosphorus(V) organocyanamides of the general formulas P(YR)3, P(X)(YR)3, P(X)(OR′)(YR)2, and P(X)(OR′)2(YR) (Y : NCN; X : O, S) by reactions of the corresponding phosphorus and organophosphorus chlorides with metal organocyanamides is reported. The cyanamide structure (P—N(CN)—R) of the new compounds is confirmed by infrared data as well as by a modified synthetic route. A comparison of 31P-NMR data of homologous cyanamide- and oxo-phosphorus derivatives is confirming the pseudochalcogen character of the NCN-group.
    Notes: Es wird über die Synthese einer Reihe von Phosphor(III)- und Phosphor(V)-organocyanamiden der allgemeinen Formeln P(YR)3, P(X)(YR)3, P(X)(OR′)(YR)2 und P(X) (OR′)2(YR)(Y : NCN, X : O, S) durch Reaktionen der entsprechenden Phosphor- und Organophosphorchloride mit Metall-organocyanamiden berichtet. Der in den neuen Verbindungen generell vorliegende Cyanamid-Bindungstyp (P—N(CN)R) folgt aus IR-Daten ebenso wie aus einem modifizierten Syntheseweg. Ein Vergleich der 31P-NMR chemischen Verschiebungen homologer Oxo- und Cyanamido-Phosphor-Derivate bestätigen den Pseudochalkogen-Charakter der NCN-Gruppe.
    Additional Material: 4 Tab.
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    Über Phospholkomplexe einiger 3d-ÜbergangselementeProfessor Kurt Issleib zum 70. Geburtstage am 19. November 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 81-88 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Phosphole Complexes of 3d Transition MetalsThe 2-ethoxy-, 2-cyclohexanoxy-, 2-phenoxy-, 2-(4′-methylphenoxy)- and 2-(4′-chlorphenoxy)-benzo[1,3,2]-dioxaphospholcomplexes of chromium(III), iron(II), cobalt(II), and nickel(II) are synthesized and characterized by N.M.R., I.R. and U.V.-VIS spectroscopy and by magnetic investigations. When titanium(IV) ore copper(II) halides are used redox-reactions can be observed. The corresponding copper(I) complexes are isolated.
    Notes: Es werden 2-Ethoxy-, 2-Cyclohexanoxy-, 2-Phenoxy-, 2-(4′-Methylphenoxy)- und 2-(4′-Chlorphenoxy)benzo[1,3,2]dioxaphospholkomplexe des Chrom(III), Eisen(II), Cobalt(II) und Nickel(II) synthetisiert und mittels NMR-, IR- und UV-VIS-Spektroskopie sowie durch magnetische Untersuchungen charakterisiert. Im Falle des Titan(IV) und des Kupfer(II) werden Redoxreaktionen beobachtet, es werden entsprechende Kupfer(I)-Komplexe isoliert und im Falle des 2-(4′-Chlorphenoxy)-benzol[1,3,2]dioxaphospholliganden der Kupfer(II)-Komplex nachgewiesen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895780110
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    Übergangsmetallkomplexe mit Schwefelliganden. XLIV. Ruthenium(II)-Komplexe mit dem sterisch anspruchsvollen Thioether-Thiolat-Liganden ‚buS4‘2- (= 1,2-Bis(3,5-di(tertiärbutyl)-2-mercaptophenylthio)-ethan (2-)) sowie den Koliganden PPh3, PMe3, CO, NH3 und N2H4 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 234-244 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Transition Metal Complexes with Sulfur Ligands. XLIV. Ruthenium(II) Complexes with the Sterically Demanding Thioether-thiolate Ligand ‚buS4‘2-(= 1,2-Bis(3,5-di(tertiarybutyl)-2-mercaptophenylthio) ethane (2-)) and PPh3, CO, PMe3, NH3, and N2H4 ColigandsThe coordination properties of the sterically demanding thioether-thiolate ligand ‘buS4’2- (= 1,2-Bis(3,5-di(tertiarybutyl)-2-mercaptophenylthio)ethane (2-)) towards Ruthenium were investigated. [Ru(PPh3)2 (‘buS4’)], 1, was obtained from [RuCl2(PPh3)3] and ‘buS4’—Li2. One PPh3 ligand in 1 is labile towards substitution and can be exchanged by L = CO (2), PMe3 (3), or NH3 (5) yielding [Ru(L)(PPh3)(‘buS4’)]. The PMe3 complex [Ru(PMe3)2(‘buS4’)], 4, is thermically inert as well as 2, 3, and [Ru(CO)2(‘buS4’)], 6, which was obtained from [RuCl2(CO)3THF] and ‘buS4’—Li2. Considering the thermical reaction inertness of 6, its fast reaction with N2H4 yielding [Ru(N2H4) (CO) (‘buS4’)], 7, is remarkable; the reaction probably takes place via 19e- intermediates. All ‘buS4’ complexes are better soluble in organic solvents than the corresponding [Ru(‘S4’)] parent compounds, their ν(CO)frequencies or 31PNMR shifts, however, are nearly identical, allowing the conclusion that the influence of the t-butyl groups is topological and not electronic. All now complexes were characterized by elemental analyses as well as IR, NMR, and mass spectroscopy.
    Notes: Die Koordinationseigenschaften des sterisch anspruchsvollen Thioether-Thiolat-Liganden ‚buS4‘2- (= 1,2-Bis(3,5-di(tertiärbutyl)-2-mercaptophenylthio)ethan (2-)) gegen-über Ruthenium wurden untersucht. Dabei wurde [Ru(PPh3)2(‚buS4‘)], 1, aus [RuCl2(PPh3)3] und ‚buS4‘—Li2 erhalten. Ein PPh3-Ligand in 1 ist substitutionslabil und kann durch L = CO (2), PMe3 (3 oder NH3 (5) unter Bildung von [Ru(L)(PPh3))(‚buS4‘)] ersetzt werden. Der zu 1 analoge PMe3-Komplex [Ru(PMe3)2(‚buS4‘)], 4, ist thermisch inert, ebenso wie 2, 3 und [Ru(CO)2(‚buS4‘)], 6, das aus [RuCl2 (CO)3THF] und, ‚buS4‘—Li2 erhalten wurde. In Anbetracht der thermischen Reaktionsträgheit von 6 ist seine rasche Reaktion mit N2H4 zu [Ru(N2H4)(CO)(‚buS4‘)], 7, bemerkenswert; die Reaktion verläuft wahrscheinlich über 19e--Zwischenstufen. Alle ‚buS4‘-Komplexe sind in organischen Lösungsmitteln besser löslich als ihre [Ru(‚S4‘)]-Stammverbindungen, n̈(CO)-Frequenzen oder 31P-Verschiebungen sind jedoch nahezu identisch, woraus auf einen topologischen, nicht aber elektronischen Einfluß der t-Butylgruppen geschlossen werden muß.Alle neuen Komplexe wurden elementaranalytisch sowie IR-, NMR- und massenspektroskopisch charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19895770127
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    Komplexbildung des Kupfer(II) mit Opioidpeptiden (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 293-300 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation of Copper(II) with Opioid PeptidesComplex compounds of copper(II) with the neuropeptide enkephaline were detected as CuH-(n-1)L + nLi+ ions by means of FAB mass spectrometry. Formation constants of proton and copper(II) complexes of four opioid peptides (L-I — L-IV) were determined potentiometrically. Complexes with methionine-containing ligands show the highest stability. Under physiological pH values all brain-existent enkephaline may be bound by endogeneous copper provided that [Cu2+] 〉 10-7 M.
    Notes: Mit Hilfe der FAB-Massenspektrometrie werden die Komplexverbindungen des Kupfer(II) mit dem Neuropeptid Enkephalin als Ionen der Zusammensetzung CuH-(n-1)L + nLi+ registriert. Die Protonierungs- und Komplexbildungskonstanten von vier Oligopeptiden bzw. ihren Kupfer(II)-Komplexen (L-I — L-IV) werden durch potentiometrische Titration ermittelt. Die höchste Stabilität zeigen Komplexe mit methioninhaltigen Liganden. Bei physiologischen pH-Werten kann das gesamte im Gehirn enthaltene Enkephalin an endogenem Kupfer bei [Cu2+] 〉 10-7 M gebunden sein.
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    URL: http://dx.doi.org/10.1002/zaac.19895770133
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    Cycloadditionsreaktionen im System 2-Isocyanato-4,4,5,5-tetramethyl-1,3,2-dioxaphospholan/1,1,1,5,5,5-Hexafluor-4-trimethylsiloxy-3-penten-2-on (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 572 (1989), S. 135-139 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cycloaddition Reactions in the System 2-Isocyanato-4,4,5,5-tetramethyl-1,3,2-dioxaphospholane/1,1,1,5,5,5-Hexafluor-4-trimethylsiloxy-3-pentene-2-oneThe two title compounds react to give in a (3+2) cycloaddition the spiro iminophosphoran 3 and its dimer 4, respectively. The (2+2) cycloaddition of hexafluoracetone and 3 yields the oxazaphosphetane 5, which decomposes rapidely into the Staudinger product 6. The hydrolytical cleavage of the trimethylsilyl group furnishes the tricyclic phosphorane 7. The 3JPH coupling in 3 is surprisingly large (51.6 Hz).
    Notes: Die beiden Titelverbindungen ergeben in einer (3+2)-Cycloaddition das Spiroiminophosphoran 3 bzw. dessen Dimeres 4. Eine (2+2)-Cycloaddition von Hexafluoraceton an 3 läßt das Oxazaphosphetan 5 entstehen, das rasch in das Staudinger-Produkt 6 zerfällt. Über die hydrolytische Abspaltung der Trimethylsilylgruppe von 3 wird das tricyclische Phosphoran 7 erhalten. Die Kopplungskonstante 3JPH in 3 von 51,6 Hz ist überraschend groß.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895720116
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    Basische Metalle. LXIV. Lewis-basische Bis(trimethylphosphan)cobalt-Komplexe mit Indenyl und Trifluormethylcyclopentadienyl als Liganden (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 283-292 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Basic Metals. LXIV. Lewis-basic Bis(trimethylphosphine)cobalt Complexes with Indenyl and Trifluormethylcyclopentadienyl as LigandsThe half-sandwich type compounds C9H7Co(PMe3)2 (1) and (C5H4CF3)Co(PMe3)2 (6) are prepared from CoCl(PMe3)3 and C9H7Li or TlC5H4CF3, respectively. They behave like metal bases and react with HBF4, CH3I (or CF3SO3CH3), I2, and CH3COCl by oxidative addition to give the cationic complexes [C9H7CoX(PMe3)2]+ and [(C5H4CF3)CoX(PMe3)2]+ (X = H, CH3, I, COCH3) which are isolated as the PF6 salts (2-5 and 7-10). The 1HNMR and the IR spectra of the compounds 1-10 are discussed, also in comparison to those of the corresponding cyclopentadienylcobalt complexes.
    Notes: Die Halbsandwichverbindungen C9H7Co(PMe3)2 (1) und (C5H4CF3)Co(PMe3)2 (6) werden aus CoCl(PMe3)3 und C9H7Li bzw. TlC5H4CF3 synthetisiert. Sie verhalten sich wie Metall-Basen und reagieren mit HBF4, CH3I (oder CF3SO3CH3), I2 und CH3COCl unter oxidativer Addition zu den kationischen Komplexen [C9H7CoX(PMe3)2]+-und [(C5H4CF3)CoX(PMe3)2]+ (X = H, CH3, I, COCH3), die als PF6-Salze (2-5 und 7-10) isoliert werden. Die 1H-NMR- und IR-Daten der Verbindungen 1-10 weden, auch im Vergleich zu denen der entsprechenden Cyclopentadienylcobalt-Komplexe, diskutiert.
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    Selektive Cyclotetramerisierung von Propargylalkohol: katalytische Reaktionen hoher Selektivität und Geschwindigkeit an Nickelkomplexen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 577 (1989), S. 270-282 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Selective Cyclotetramerization of Propargylic Alcohol: Catalytic Reactions with High Selectivity and Reaction Rate by Nickel ComplexesIt is shown propargylic alcohol reacts with different nickel catalysts to form cyclotetrameres in a selective reaction. Main product of the reaction is 1,3,5,7-tetrakis(hydroxymethyl)-cycloocta(1,3,5,7)-tetraene.The reaction is extremely fast; when it is carried out without solvents at 114°C turnover numbers of 106 catalytic cycles/mol Ni × h can be observed. The influence of phosphines is different: In solvents aromatic compounds, and cyclotetrameres are formed, when solvents are not used, phosphines have no controlling effect.The reaction can also be catalyzed by iron complexes to form cyclotetrameres, cobalt complexes yield a mixture of cyclotrimeres and cyclotetrameres.Supported Nickel or Raney-Nickel can also catalyze the cyclotetramerization.The investigations show that the 1-azadiene ligands in bis(cinnemaldehydeanil)-nickel(0) are substituted by propargylic alcohol in a fast reaction. After the substitution the catalytic reaction takes place at “ligand free nickel”.
    Notes: Es wird gezeigt, daß Propargylalkohol an vielen Nickelkatalysatoren selektiv zu Cyclotetrameren umgesetzt werden kann. Hauptprodukt der Reaktion 1,3,5,7-Tetrakis-(hydroxymethyl)-cycloocta(1,3,5,7)-tetraen. Die Reaktion ist extrem schnell; wenn ohne Lösungsmittel bei 114°C gearbeitet wird, können 106 katalytische Cyclen/Mol Ni × h erreicht werden. Der Einfluß von Phosphinen auf die katalytische Reaktion ist unterschiedlich: In Lösungsmitteln werden zunehmend Aromaten gebildet, wenn ohne Verwendung von Lösungsmitteln gearbeitet wird, haben Phosphine keinen steuernden Effekt.Die Reaktion kann auch durch Eisen(II)-Verbindungen katalysiert werden, während Cobaltkomplexe ein Gemisch von Cyclotrimeren und Cyclotetrameren bilden.Elementares Nickel auf Trägern oder Raney-Nickel können ebenfalls die katalytische Cyclotetramerisierung auslösen.Die Untersuchungen zeigen, daß 1-Azadienliganden in Bis(zimtanil)-nickel(0) in einer schnellen Reaktion durch Propargylalkohol substituiert werden. Nach der Substitution findet die katalytische Reaktion am „ligandfreien Nickel“ statt.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895770131
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    Silylphosphane mit Adamantan-Struktur durch Umsetzung von P4 und Na/K mit Dichlorsilanen sowie deren 31P-NMR-SpektrenProfessor Kurt Issleib zum 70. Geburtstage am 19. November 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 27-36 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silylphosphanes with an Admantane Skeleton Formed in Reactions of P4 and Na/K with Dichlorsilanes, and their 31P NMR SpectraThe reactions of P4 and Na/K (molar ratio 1:3) with EtMeSiCl2, Et2SiCl2, and PhMeSiCl2 give access to the silylphosphanes with adamantane structure (EtMeSi)6P4 1, (Et2Si)6P4 2, and (PhMeSi)6P4 3. Likewise, the Si-functional adamantanes [Vinyl(Me)Si]6P4 4, (MeHSi)6P4 5, and (MeHSi)(Et2Si)6P4 6 can be obtained by the reaction of alkali phosphides with Vinyl(Me)SiCl2, MeHSiCl2, or Et2SiCl2/MeHSiCl2 (molar ratio 5:1), respectively. The compounds form colorless crystals (3 crystallies reluctantly). The reactions of the alkali phosphides with t-Bu2SiCl2 and Ph2SiCl2 do not lead to the corresponding adamantanes; t-Bu2SiCl2 doesn't react product mixture of the more reactive Ph2SiCl2 traces of (Ph2Si)6P4 could not be detected. The 31P-NMR-spectra of the compounds 1-6 are interpreted.
    Notes: Durch Umsetzung von P4 und Na/K (Molverhältnis 1:3) mit EtMeSiCl2, Et2SiCl2, PhMeSiCl2 werden die Silylphosphane mit Adamantanstruktur (EtMeSi)6P4 1, (Et2Si)6P4 2, (PhMeSi)6P4 3 zugänglich. Entsprechend lassen sich die Si-funktionellen Adamantane [Vinyl(Me)Si]6P4 4, (MeHSi)6P4 5 und (MeHSi)(Et2Si)5P4 6 durch Umsetzung des Alkaliphosphides mit Vinyl(Me)SiCl2; MeHSiCl2 bzw. Et2SiCl2/MeHSiCl2 (Molverhältnis 5:1) darstellen. Die Verbindungen sind kristallin (3 kristallisiert nur schwer). Die Umsetzungen des Alkaliphosphides mit (t-Bu)2SiCl2 und Ph2SiCl2 führen nicht zu den entsprechenden Adamantanen; (t-Bu)2SiCl2 reagiert unter den Darstellungsbedingungen der übrigen noch nicht, und in den Reaktionsprodukten des reaktionsfähigeren Ph2SiCl2 konnte das (Ph2Si)6P4 nicht nachgewiesen werden. Die 31P-NMR-Spektren der Verbindungen 1-6 werden interpretiert.
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    Über BaNiDy2O5 und BaNiLu2O5 mit oktaedrisch und tetragonal pyramidal koordiniertem Ni2+ (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 572 (1989), S. 181-185 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About BaNiDy2O5 and BaNiLu2O5 with Octahedral and Tetragonal Pyramidal Coordinated Ni2+(I) BaNiDy2O5 and (II) BaNiLu2O5 were prepared for the first time and investigated by X-ray single crystal technique. [I: a = 3.773; b = 5.777; c = 11.352 Å; Z = 2; space group D2h25 - Immm; II: a = 6.931; b = 12.109; c = 5.634 Å; Z = 4; space group D2h16-Pbnm]. I crystallizes with an octahedral coordination of Ni2+ by O2-, II on the contrary is surrounded by a tetragonal pyramidal oxygen environment. II belongs to the series of BaCuLn2O5 compounds.
    Notes: (I) BaNiDy2O5 und (II) BaNiLu2O5 wurden erstmals dargestellt und mit Einkristallröntgenbeugungsmethoden untersucht [I: a = 3,773; b = 5,777; c = 11,352 Å; Z = 2; Raumgruppe D2h25-Immm; II: a = 6,931; b = 12,109; c = 5,634 Å; Z = 4; Raumgruppe D2h16-Pbnm]. I kristallisiert mit oktaedrisch koordiniertem Ni2+, II dagegen mit der Koordinationszahl 5 in Form einer tetragonalen Pyramide. II gehört somit zur Reihe der BaCuLn2O5-Verbindungen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895720122
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    Darstellung und Charakterisierung der trans-Dioxo-Osmate(VI), [OsO2(CN)2X2]2-, X = NCO, NCS, SeCN, 1/2 (C2O4); [OsO2(CN)2X2], X = py, 1/2 bipy und [OsO2(CN)2X]22-, X = OH, OCH3 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 572 (1989), S. 151-163 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Characterization of the trans-Dioxoosmates, [OsO2(CN)2X2]2-, X = NCO, NCS, SeCN, 1/2 (C2O4); [OsO2(CN)2X2)], X = py, 1/2 bipy and [OsO2(CN)2X]22-, X = OH, OCH3By careful acidification of the aqueous solution of [OsO2(OH)4]2- in the presence of the required amount of cyanide ions with oxalic acid or acetic acid the osmyl complexes [OsO2(CN)2(C2O4)]2- or [OsO2(CN)2(OH)]22- are prepared for the first time, respectively. By acidolytic ligand substitution from [OsO2(CN)2(OH)]22- the new compounds [OsO2(CN)2(OCH3)]22-, [OsO2(CN)2(NCO)2]2-, [OsO2(CN)2(NCS)2]2-, [OsO2(CN)2(SeCN)2]2-, [OsO2(CN)2(py)2], and [OsO2(CN)2(bipy)] are formed. The IR and Raman spectra are assigned assuming D2h or C2v local symmetry. In respect to the relative high frequencies of vCO and vCS coordination via N is deduced for NCO and NCS, whereas the low vCSe frequency gives evidence for Se linkage of the SeCN. At 10 K the absorption spectra reveal a distinct vibrational fine structure. The excitation of one electron from the ground state of OsVI, 1Ag[ag2](dxy), D2h, or 1A1[a12](dxy), C2v, into the lowest unoccupied b2g/b3g or b1/b2 (dxz, dyz) orbitals gives triplet terms of lower energy (615-450 nm) and singlet terms at higher energy (475-390 nm). On both bands a progression of 723-757 cm-1 is superposed caused by coupling of the d—d transition with vas(Os = O). Two more intense absorptions in the UV region are assigned to charge transfer transitions from pπ orbitals of the oxo ligands into the lowest unoccupied niveau at OsVI. The triplet terms are observed at 390-340, the singlet terms at 340-280 nm. The averaged progression of vibrational coupling with vs (Os = O) is 690-738 cm-1, the singlet triplet energy distances are in the order of 3 600 cm-1.
    Notes: Durch vorsichtiges Ansäuern der wäßrigen Lösung von [OsO2(OH)4]2- in Gegenwart der erforderlichen Menge Cyanidionen mit Oxalsäure bzw. Essigsäure sind die Osmylkomplexe [OsO2(CN)2(C2O4)]2- bzw. [OsO2(CN)2(OH)]22- erstmals hergestellt worden. Durch acidolytische Ligandensubstitution entstehen aus [OsO2(CN)2(OH)]22- die neuen Verbindungen [OsO2(CN)2(OCH3]22-, [OsO2(CN)2(NCO)2]2-, [OsO2(CN)2(NCS)2]2-, [OsO2(CN)2(SeCN)2]2-, [OsO2(CN)2(py)2] und [OsO2(CN)2(bipy)]. Die IR- und Raman-Spektren werden gemäß der lokalen Symmetrie D2h oder C2v zugeordnet. Aus der relativ hohen Frequenz von vCO und vCS wird für NCO und NCS die Koordination über N, aus der niedrigen Lage von vCSe die Koordination von SeCN über Se abgeleitet. Die an den festen Komplexen bei 10 K registrierten Absorptionsspektren zeigen eine ausgeprägte Schwingungsfeinstruktur. Bei Anregung eines Elektrons von OsVI aus dem Grundzustand 1Ag[ag2](dxy) bei D2h- bzw. 1A1[a12](dxy) bei C2v-Symmetrie in die niedrigsten, unbesetzten b2g/b3g- bzw. b1/b2-(dxz, dyz)-Orbitale entstehen energieärmere Triplett-Terme (615-450 nm), sowie energiereichere Singulett-Terme (475-390 nm). Die auf beiden Banden gefundene mittlere Progression von 723-757 cm-1 beruht auf der Kopplung des d-d-Übergangs mit vas (Os = O). Zwei viel intensivere Bandensysteme im UV-Bereich werden den Charge-Transfer-Übergängen von pπ-Orbitalen der Oxoliganden in das niedrigste unbesetzte Niveau am OsVI zugeordnet. Die Triplett-Terme werden bei 390-340, die Singulett-Terme bei 340-280 nm beobachtet. Die mittlere Progression der Schwingungskopplung mit vs(Os = O) beträgt 690-738 cm-1, die Singulett-Triplett-Abstände liegen bei 3 600 cm-1.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895720119
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    Kristall- und Molekülstruktur von Bis[1,2-bis(diphenyl-phosphino)-ethan]nickel(O) (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 177-184 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of Bis[1,2-bis(diphenylphosphino)ethane]nickel(O)The title compound [Ni(dppe)2] (dppe = Ph2PCH2CH2PPh2) crystallizes in the monoclinic space group P21/n with lattice parameters a = 983.2(2), b = 2119.2(3), c = 2145.1(4) pm, β = 91.97(1)°, and a unit cell contents of four molecules. The structure was solved by heavy atom method and refined to an R-value of 0.063 (RW = 0.052), using 2779 observed unique reflexions. The Ni atom as the spiro centre is distorted-tetrahedrally coordinated by the four P atoms of the two bidentate chelating ligands. The Ni—P bond lengths are very similar with a mean value of 216(1) pm. The mean value of Tolman's cone angle for the dppe ligand calculated from the molecular structure of [Ni(dppe)2] amounts to 129.8°.
    Notes: Die Titelverbindung [Ni(dppe)2] (dppe = Ph2PCH2CH2PPh2) kristallisiert in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 983,2(2), b = 2119,2(3), c = 2145,1(4) pm, β = 91,97(1)° und vier Molekülen pro Elementarzelle. Die Struktur wurde auf der Grundlage von 2779 beobachteten symmetrieunabhängigen Reflexintensitäten nach der Schweratommethode gelöst und bis zu einem R-Wert von 0,063 (RW = 0,052) verfeinert. Das Ni-Atom als Spirozentrum ist verzerrt tetraedrisch von den vier P-Atomen der beiden zweizähnigen Chelatliganden umgeben. Die sehr ähnlichen Ni-P-Abstände weisen einen Mittelwert von 216(1) pm auf. Der aus der Molekülstruktur von [Ni(dppe)2] berechnete mittlere Öffnungswinkel für den Tolman-Kegel von dppe beträgt 129,8°.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895780120
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    Zur Reaktivität von Disilylphosphidokomplexen des Eisens und Rutheniums gegenüber 2,4,6-t-Bu3C6H2AsCl2. Bildung und Struktur von Arsaphosphenylkomplexen, Diphosphaarsiranen, Phosphadiarsiranen und 1,2-Diphospha-3,4-diarsetanen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 578 (1989), S. 205-224 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reactivity of Disilylphosphido Complexes of Iron and Ruthenium towards 2,4,6-t-Bu3C6H2AsCl2. Generation and Structures of Arsaphosphenyl Complexes, Diphospha-ariranes, Phosphadiarsiranes, and 1,2-Diphospha-3,4-diarsetanesThe reaction of (η5-C5Me5)(CO)2Fe—P(SiMe3)2 (1a) with 2,4,6-t-Bu3C6H2AsCl2 (= Aryl AsCl2) (6) leads to the formation of the heterocycles [(η5-C5Me5)(CO)2Fe—P]2As-Aryl (7a), (η5-C5Me5)(CO)2Fe—P(As-Aryl)2 (8a), and [(η5-C5Me5)(CO)2Fe—P-As-Aryl]2(9a). The instable arsaphosphenyl complex [(η5-C5Me5)(CO)2Fe—P=As-Aryl] can be intercepted as its Cr(CO)5-adduct 13a. Analogously the ring compounds (η5-C5Me5)(CO)2Ru—P]2(As-Aryl)(7b) and (η5-C5Me5)(CO)2Ru—P(As-Aryl)2 (8b) are obtained by treatment of (η5-C5Me5)(CO)2Ru—P(SiMe3)2 (1b) with 6. Here again the primarily generated arsaphosphene has to be stabilized by coordination to Cr(CO)5 which gave E-(η5-C5Me5)(CO)2Ru—P[Cr(CO)5 = As-Aryl (E-13b) and its Z-isomer (Z-13b). A comparable reaction sequence furnished the phosphaarsenyl complex (η5-C5Me5)(CO)(PPh)3Fe—P[Cr(CO)5] = As-Aryl (13c).The molecular structures of 7a and 9a were elucidated by x-ray diffraction analysis. The most interesting feature of 7a is the AsP2-triangle, in which the As—P(2) bond length (235,0(2) pm) is slightly elongated with respect to the As—P(1) distance (231,6(1) pm). This effect is presumably due to severe steric interactions at the cis-substituted As—P(2) bond. Molecule 9a displays the picture of a bended 1,2-diphospha-3,4-diarsetane (interplanar angle 137.6°) with its substituents in the all trans-orientation. The As—P and P—P separations are normal whereas the As—As bond (249,7(4) pm) is slightly widened with respect to the calculated value for a single bond (ca 244 pm).
    Notes: Bei der Umsetzung von (η5-C5Me5)(CO)2Fe—P(SiMe3)2 (1a) mit 2,4,6-t-Bu3C6H2AsCl2 (= Aryl AsCl2) (6) werden die Heterocyclen [(η5-C5Me5)(CO)2Fe—P]2 As-Aryl (7a), (η5-C5Me5)(CO)2Fe—P(As-Aryl)2 (8a) und [(η5-C5Me5)(CO)2Fe—P]-As-Aryl(2 9a) erhalten. Der nur in Lösung nachweisbare Arsaphosphenylkomplex [(η5-C5Me5)(CO)2Fe—P=As-Aryl] läßt sich als stabiles Cr(CO)5-Addukt 13a abfangen. Analog bilden sich aus (η5-C5Me5)(CO)2Ru—P(SiMe3)2 (1b) und 6 die Ringe [(η5-C5Me5)(CO)2Ru—P]2As-Aryl (7b) und (η5-C5Me5)(CO)2Ru—P(As-Aryl)2 (8b). Auch hier kann ein primär entstandenes Arsaphosphen in Form der Cr(CO)5-Addukte.E-(η5-C5Me5)(CO)2Ru—P[Cr(CO)5] = As-Aryl (E-13b) und dessen Z-Isomer (Z-13b) abgefangen werden. Die gleiche Reaktionssequenz führt zu dem Phosphaarsenylkomplex (η5-C5Me5)(CO)(PPh3Fe)—P[Cr(CO)5] = As-Aryl (13c).Die Strukturen der Ringverbindungen 7a und 9a wurde mittels Röntgenbeugungsanalyse bestimmt. Das Grundgerüst von 7a besteht aus einem AsP2-Dreieck, in dem die As—P(2)-Bindung (235,0(2)pm) mit den Substituenten in cis-Orientierung gegenüber dem As—P(1)-Abstand (231,6(1)pm) geringfügig verlängert ist. Das Molekül 9a zeigt das Bild eines gefalteten 1,2-Diphospha-3,4-diarsetans (Diederwinkel 137,6°) mit den Substituenten in all-trans Orientierung. Der As—As-Abstand (249,7(4) pm) erscheint aufgrund sterischer Spannungen aufgeweitet (dber etwa 244 pm), während die As—P- und P—P-Abstände keine Besonderheiten aufweisen.
    Additional Material: 2 Ill.
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    Masthead (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895760101
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    Experimente und Modellrechnungen zum chemischen Transport von V2O5 mit NH4Cl (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 240-240 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895750128
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    Professor Lothar Kolditz zum 60. Geburtstage am 30. September 1989 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989), S. 7-9 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895760102
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    Zur Reaktion aromatischer Phosphan-Derivate mit Elektronen. IV. Die Bedeutung niedrig liegender unbesetzter Orbitale Phosphor für Beweglichkeit und Koordinationsfähigkeit von PR2-Substituenten in reduzierten p-PhenylendiphosphanenProfessor Gerhard Fritz zum 70. Geburtstage am 14. Dezember 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 47-56 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Aromatic Phosphanes with Electrons. IV. Significance of Low-Lying Orbitals at Phosphorus for the Mobility and Coordinative Characteristics of PR2 Substituents in Reduced p-PhenylenediphosphanesDinuclear complexes of the ligands 1,4-R2P—C6H4—PR2 (R = Me, Ph) with the carbonylmetal fragments (C5H4CH3)Mn(CO)2 and M(CO)5 (M = Cr, Mo, W) were studied by cyclic voltammetry. The dimanganese complex shows reversible oxidation to ESR-detectable MnII but no detectable splitting of the cyclovoltammetric wave, the p-phenylenediphosphane bridge does apparently not permit effective metal-metal interaction. The free ligands are reversibly reduced to persistent, ESR-detectable anion radicals with hindered rotation of the PR2 substituents. The carbonylmetal complexes, on the other hand, show dissociation on electron uptake despite their less negative reduction potentials. This behaviour stands in contrast to main-group element complexes of these ligands and is attributed to the competition between the metal carbonyl fragment and the added electron for the low-lying unoccupied orbitals (σ*) at phosphorus.
    Notes: Zweikernige Komplexe der Liganden 1,4-R2P—C6H4—PR2 (R = Me, Ph) mit den Carbonylmetall-Fragmenten (C5H4CH3)Mn(CO)2 und M(CO)5 (M = Cr, Mo, W) wurden durch cyclische Voltammetrie in DMF untersucht. Der Dimangan-Komplex zeigt simultane reversible Oxidation beider Metallzentren zu ESR-spektroskopisch nachweisbarem MnII, die p-Phenylendiphosphan-Brücke bewirkt demnach keine effektive Metall-Metall-Wechselwirkung. Die freien Liganden sind reversibel zu beständigen, ESR-spektroskopisch nachweisbaren Radikalanionen mit eingeschränkter Rotation der PR2-Substituenten reduzierbar. Obwohl Koordination der Carbonylmetall-Fragmente die Elektronenaufnahme erwartungsgemäß erleichtert, findet nach chemischer oder elektrochemischer Reduktion Dissoziation der Komplexe statt. Dieses im Gegensatz zu Hauptgruppenelement-Komplexen der Liganden stehende Verhalten ist auf die Konkurrenz von Metallcarbonyl und addiertem Elektron um die niedrig liegenden unbesetzten Orbitale (σ*) am Phosphor zurückzuführen.
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    URL: http://dx.doi.org/10.1002/zaac.19895790106
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    Darstellung und Strukturen von Chlorostannaten(II). I. Neue Trichlorostannate(II) einwertiger KationenProfessor Gerhard Fritz zum 70. Geburtstage am 14. Dezember 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 87-98 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structures of Chlorostannates(II). I. Some New Trichlorostannates of Monovalent CationsKSnCl3 · 1/2 CH3CN is obtained by recrystallizing KSnC13 from acetonitrile. The compound forms monoclinic crystals, space group P21/c (a = 4.525(6), b = 20.34(2), c = 8.061(7) Å, β = 90.93(9)°). [Cu(CH3CN)3]SnCl3 is prepared by reacting equimolar amounts of CuCl and SnCl2 in acetonitrile. It crystallizes in the monoclinic space group P21/n (a = 7.984(9), b = 20.77(2), c = 8.34(2) Å, β = 101.6(1)°). Whereas in KSnCl3 · l/2 CH3CN there is a three dimensional connection of the SnCl3- ions, in which the potassium ions participate, the trichlorostannate ions in [Cu(CH3CN)3]SnCl3 are linked to one dimensional chains by Sn…Cl bridges.
    Notes: KSnCl3 · 1/2 CH3CN wird durch Umkristallisieren von KSnCl3 aus Acetonitril erhalten. Die Verbindung kristallisiert monoklin, Raumgruppe P21/c (a = 4,525(6), b = 20,34(2), c = 8,061(7) Å, β = 90,93(9)°). Durch Umsetzung von CuCl mit einer äquimolaren Menge an SnCl2 in Acetonitril erhält man [Cu(CH3CN)3]SnCl3 das in der monoklinen Raumgruppe P21/n kristallisiert (a = 7,984(9), b = 20,77(2), c = 8,34(2) Å β = 101,6(1)°). Während in KSnCl3 · 1/2 CH3CN eine dreidimensionale Verknüpfung der SnCl3minus;-lonen vorliegt, an der auch die Kaliumionen beteiligt sind, sind die Trichlorostannationen in [Cu(CH3CN)3]SnCl3 durch Sn…Cl-Brücken zu eindimensionalen Ketten verknüpft.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790110
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    Al2Cl6-Komplexe des ChromsProfessor Reginald Gruehn zum 60. Geburtstage am 6. Oktober 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 139-142 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A12Cl6 Complexes of ChromiumThe equation \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm CrCl_{3,s} + 1,5 Al_2Cl_{6,g} = CrA1_3Cl_{12,g}} $$\end{document} is measured (Extinction, max. 19.2 kK). The photometric measurement yields e. g. log Kp = -5260/T + 6.459.
    Notes: Chrom(III)-chlorid gibt mit Aluminium(III)-chlorid einen Komplex: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm CrCl_{3,s} + 1,5 Al_2Cl_{6,g} = CrA1_3Cl_{12,g} [1, 2, 3]} $$\end{document}(Extinktion, max 19,2 kK). Die photometrische Messung in Abhängigkeit von der Temperatur (lineare Abhängigkeit 690 bis 800 K) ergab z. B. log Kp = -5260/T + 6,469.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790117
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  • 80
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    Erste Abbauprodukte von Hexahydraten MCl3 · 6H2O (M = V, Ti, Cr, Al) mit einer Verfeinerung der Struktur von [Cr(H2O)6]Cl3Professor Reginald Gruehn zum 60. Geburtstage am 6. Oktober 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 143-150 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: First Dehydration Products of Hexahydrates MCl3 · 6H2O (M = V, Ti, Cr, Al) with a Refinement of the Structure of [Cr(H2O)6]Cl3The thermal dehydration of AlCl3 · 6H2O and TiCl3 · 6H2O occurs in one step; isomeric hexahydrates of CrCl3 give several amorphous intermediate products. The first compounds, yielded when dehydrating VCl3. 6H2O and VBr3 · 6H2O, are crystalline. In an HX-stream at ≈ 100°C tetrahydrates are formed. With imperfect single crystals of VCl3 · 4H2O a monoclinic unit cell, space group C2/m was found: a = 1204.1 pm; b = 715.5 pm; c = 971,8 pm; β = 112,88°; Z = 4. The structure dates for [Cr(H2O)6]Cl3 were refined by single crystal measurements.
    Notes: Der thermische Abbau von AlCl3 · 6H2O und TiCl3 · 6H2O verläuft in einer Stufe; im Falle der beiden isomeren Hexahydrate des CrCl3 verläuft der Abbau mehrstufig, jedoch über röntgenamorphe Zwischenprodukte. Nur von VCl3 · 6H2O und VBr3 · 6H2O ist das erste Abbauprodukt kristallin; durch Erhitzen im HX-Strom auf ≈ 100°C entstehen die Tetrahydrate. Für VCl3 ·4 H2O ließ sich die Struktur nur unter Benutzung schlechter Einkristalle bestimmen: monokline Zelle in der R.G. C2/m mit a = 1204,1 pm; b = 715,5 pm; c = 971,8 pm; β = 112,88°; Z = 4. Die Strukturdaten von [Cr(H2O)6]Cl3 wurden anhand von Einkristalluntersuchungen verbessert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790118
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    Ein N/P-Analogon des Cyclotetraphosphazens: Reaktionen und Struktur des Octaphenyl-1,5,2λ5,3,4λ5,6λ5,7,8λ5-diazahexaphosphocins und seines PdCl2-KomplexesProfessor Kurt Issleib zum 70. Geburtstage am 19. November 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 158-172 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An N/P-Analogue of Cyclotetraphosphazene: Reactions and Structure of Octaphenyl-1,5,2λ5,3, 4λ5,6λ5,7,8λ5-diazahexaphosphocin and its PdCl2-ComplexThe eight-membered heterocycle 6 indicated in the title is analogous to the octaphenyl cyclotetraphosphazene in which two antipodal nitrogen ring members have been replaced by two-coordinate phosphorus. It can be obtained from (Ph2P)2NLi and P4. Very strong nucleophiles attack the PP-bonds and eventually degrade the ring in a way reverting the synthesis. 6 is selectively methylated at the two-coordinate phosphorus and forms cis-chelates with PdCl2 and PtCl2 by coordinating both of these phosphorus members.The structur of 6 and its PdC12-complex 8 were investigated by X-ray analysis and allowes multiple comparisons. All in all 6 certainly resembles a cyclophosphazene, its two-coordinate phosphorus displays phosphide character however. This is also confirmed by an MNDO calculation.
    Notes: Die im Titel genannte Achtringverbindung 6 stellt ein Analogon zum Octaphenyl-cyclotetraphosphazen dar, in dem zwei gegenüberliegende Stickstoff-Ringglieder durch zweifach-koordinierten Phosphor ersetzt sind. Sie ist aus (Ph2P)2NLi und P4 zugänglich und wird von sehr starken Nucleophilen an den PP-Bindungen angegriffen und im Sinne einer Syntheseumkehr abgebaut. Sie wird selektiv am zweifach-koordinierten Phosphor methyliert und bildet mit PdCl2 und PtCl2 durch Koordination dieser Phosphorglieder cis-Chelate.Die Strukturen von 6 und des PdC12-Komplexes 8 wurden röntgenographisch bestimmt und ermöglichen eingehende Strukturvergleiche. Insgesamt ergibt sich bei aller Cyclophosphazen-Ähnlichkeit ein phosphidischer Charakter des zweifach-koordinierten Phosphors in 6. Eine MNDO-Berechnung bestätigt das ebenfalls.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790120
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  • 82
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    Die Struktur der Fluoridhydrate CoAlF5 · 7 H2O und MnFeF5 · 7 H2OProfessor Walter Rüdorff in memoriam (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 191-199 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Structure of the Fluoride Hydrates CoAlF5 · 7H2O and MnFeF5 · 7H2OSingle crystals of fluoride hydrates CoAlF5 · 7H2O and MnFeF5 · 7H2O have been prepared and characterized by X-ray methods. The Co/Al compound crystallizes in space group C2/m (a = 1091.7(7), b = 1386.3(14), c = 652.5(6) pm, β = 100.30(6)°, Z = 4). H2O/F- disorder occurs over two trans positions in the ligand sphere of Al3+, whereas the Mn/Fe compound shows an ordered variety with [FeF6]3- and [FeF4(H2O)2]- anions crystallizing in space group C2/c (a = 1118.2(3), b = 1416.8(4), c = 1326.4(3) pm, β = 100.51(2)°, Z = 8). Both structures exhibit strong hydrogen bonds between [MII(H2O)6]2+ cations and the fluorine ligands in the coordination sphere around the tervalent metals. The complex cations and anions are grouped like in CsCl type salts.
    Notes: Erstmals wurden die Fluoridhydrate CoAlF5 · 7H2O und MnFeF5 · 7H2O in einkristalliner Form präpariert und röntgenographisch untersucht. Die Co/Al-Verbindung kristallisiert in der Raumgruppe C2/m (a = 1091,7(7), b = 1386,3(14), c = 652,5(6) pm, β = 100,30(6)°, Z = 4) mit H2O/F--Fehlordnung auf 2 trans-ständigen Lagen in der Al3+-Koordinationssphäre, wogegen die Mn/Fe-Verbindung eine geordnete Variante mit den Anionen [FeF6]3- und [FeF4(H2O)2]- in Raumgruppe C2/c bildet (a = 1118,2(3), b = 1416,8(4), c = 1326,4(3) pm, β = 100,51(2)°, Z = 8). Beiden Strukturen gemeinsam sind starke Wasserstoffbrückenbindungen zwischen den [MII(H2O)6]2+-Kationen einerseits und der Fluoridkoordinationssphäre der dreiwertigen Metalle andererseits. Die komplexen Kationen und Anionen sind wie im CsCl-Typ angeordnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790122
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    Darstellung, Eigenschaften sowie Reaktionen metallhaltiger Heterocyclen. LXVI. Nickelinduzierte Cyclocodimerisierung eines Thioxophosphor(V)-Kations mit einem aktivierten AlkinProfessor Walter Rüdorff in memoriam (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 200-204 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metall Containing Heterocycles: Preparation, Properties, Reactions. LXVI. Nickel Induced Cyclocodimerization of a Thioxophosphorus (V) Cation with an Activated AlkyneThe action of di-tert-butylthioxophosphorane (t-Bu)2P(H)S on nickelocene in ether results in the formation of the first kinetically stabilized (η2-diorganothioxophosphorus)nickel complex [(η5-C5H5)Ni(η2-S=P(t-Bu)2)] (1). In presence of the acetylene dicarboxylic acid dimethyl ester H3CO2CC—CCO2CH3 with (t-Bu)2P=S a cyclocodimerization occurs with formation of the S and P isomeric thiaphosphanickelacyclopentadiene (η5-C5H5) (2S) and thiaphosphanickelacyclopentene (η5-C5H5) (2P) (R=CO2CH3), respectively. The composition and structure of the compounds 1, 2S, and 2P were determined from the mass, IR, and NMR spectra.
    Notes: Durch Einwirkung von Di-tert-butylthioxophosphoran (t-Bu)2P(H)S auf Nickelocen in Ether erhält man den ersten kinetisch stabilisierten (η2-Diorganothioxophosphor)- nickel-Komplex [(η5-C5H5)Ni(η2-S=P(t-Bu)2)] (1). Bei Anwesenheit des Acetylendicarbonsäure-dimethylesters H3CO2CC≡CCO2CH3 tritt mit (t-Bu),P=S Cyclocodimerisierung ein, unter Bildung des S- bzw. P-isomeren Thiaphosphanickelacyclopentadiens (η5-C5H5) (2S) und Thiaphosphanickelacyclopentens (η5-C5H5)(2P) (R=CO2CH3). Die Zusammensetzung und Struktur der Verbindungen 1, 2S und 2P ergibt sich aus den Massen-, IR- und NMR-Spektren.
    Additional Material: 1 Tab.
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  • 84
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    Herstellung und Eigenschaften von Aluminiumaquoxid. II. Böhmit aus Natriumaluminat und Salpetersäure (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 221-230 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Properties of Aluminium Hydroxide. II. Boehmite from Sodium Aluminate and Nitric AcidA report is given on the physical-chemical characteristics of aluminium hydroxide which contain mainly boehmite, having been obtained by continuous precipitation from sodium aluminate solution with nitric acid using technical raw materials and conditions being very similar to those applied in production. The influence of the reaction conditions (pH value, temperature, concentration and residence time in the precipitation suspension) on the chemical composition, structure and texture of the hydrogels is studied.With rising precipitation temperature the pH range extends, within which already after short residence times pure-phase, relatively well crystalline boehmite hydrogels are obtained in the precipitated solution.
    Notes: Es wird über die physikalisch-chemischen Charakteristika von vorwiegend Böhmit enthaltenden Aluminiumaquoxiden berichtet, die durch kontinuierliches Fällen aus Natriumaluminatlösung mit Salpetersäure unter Anwendung technischer Rohstoffe und produktionsnaher Bedingungen erhalten wurden. Der Einfluß der Reaktionsbedingungen (pH-Wert, Temperatur, Konzentration und Verweilzeit in der Fällsuspension) auf die chemische Zusammensetzung, Struktur und Textur der Hydrogele wird untersucht. In einem mit ansteigender Temperatur sich ausweitenden pH-Bereich entstehen innerhalb kurzer Verweilzeiten in der Fällsuspension phasenreine, relativ gut kristalline Böhmitniederschlage stabiler Zusammensetzung. Infolge von Heterogenitäten in der kollektiven Packung der Einzelkristallite besitzt der kompaktdisperse Böhmit eine bimodale Porenstruktur, mit Hohlräumen, deren Abmessungen im wesentlichen kleiner als 10 nm und größer als 50 nm sind.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790126
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    Beiträge zur Untersuchung anorganischer nichtstöchiometrischer Verbindungen. XLI. Neue Oxidhalogenide in den Systemen Cu/Nb/O/X (X = Cl, Br, I). Präparation, thermisches Verhalten sowie Strukturuntersuchungen mit der hochauflösenden Transmissionselektronenmikroskopie (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 240-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895790128
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  • 86
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    Masthead (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 568 (1989) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895680101
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  • 87
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    Zum chemischen Transport von Chrom- und Manganmonophosphid mit Iod. Experimente und Modellrechnungen (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 24-42 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Chemical Vapour Transport of Chromium and Manganese Monophosphide. Experimental Results and Thermochemical CalculationsUsing iodine as transport agent well shaped crystals of a volume up to V ≍ 50 mm3 (CrP) or an edgelength of approximately 1 ≍ 10 mm (MnP) can be grown.CrP has been deposited at the lower temperature of a temperature gradient (1050 → 950°C). At a density of the transport agent higher than D = 26 · 10-6 [mol I2/cm3] CrP and CrI2,1 coexist in the deposition region at the lower temperature. The determined composition of the condensed phases under equilibrium conditions are in accordance with thermochemical calculations assuming the heat of formation of CrP to be ΔFH298o= -25.5 ± 2 [kcal/mol]. Furthermore these calculations show that the solution of CrP in the gas phase leads to CrI2,g, Cr2I4,g, P2,g and P4,g, while I2,g, HIg, PI3,g and P2I4,g have to be considered as transport agents.The migration of MnP (1000 → 1100°C) results from an exothermic reaction. MnPs exists besides MnI2,1 in the source region. Thermochemical calculations are in good agreement with the experimental results and suggest the following heterogenous equilibrium to be responsible for the observed behaviour: \documentclass{article}\pagestyle{empty}\begin{document}$${\rm MnP}_{\rm s} + 2{\rm HI}_{\rm g} {\rm = 1/2 Mn}_{\rm 2} {\rm I}_{{\rm 4,g}} {\rm + 1/4P}_{{\rm 4,g}} {\rm + H}_{{\rm 2,g}} $$\end{document}.
    Notes: Transportexperimente mit CrP sowie MnP unter Zusatz von Iod als Transportmittel ergaben gut ausgebildete Kristalle, deren Größe maximal V ≍ 50 mm3 (CrP), bzw. 1 ≍ 10 mm (MnP) erreichte.CrP wird in der weniger heißen Zone abgeschieden (1050 → 950°C). Bei Transportmitteldichten D ≤ 26 · 10-6 [mol I2/cm3] liegt CrP neben CrI2,1 in der Senke vor. Modellrechnungen erlauben eine Eingrenzung der Bildungsenthalpie ΔnBH298o(CrPs) = -25,5 ± 2 [kcal/mol] anhand der experimentell ermittelten Zusammensetzungen der Gleichgewichtsbodenkörper; sie zeigen ferner, daß die Löslichkeit von CrP in der Gasphase durch CrI2,g, Cr2I4,g, P2,g und P4,g bedingt wird und I2,g, HIg, PI3,g und P2I4,g als Transportmittel anzusehen sind.MnP wandert im Temperaturgradienten (1000 → 1100°C) aufgrund einer exothermen Reaktion, wobei im Quellenraum neben MnP auch MnI2,1 auftreten kann. Thermodynamische Modellrechnungen zum chemischen Transport von MnP mit Iod geben die beobachteten Transportraten und die Phasenverhältnisse im Bodenkörper gut wieder. Danach ist das heterogene Gleichgewicht\documentclass{article}\pagestyle{empty}\begin{document}$${\rm MnP}_{\rm s} + 2{\rm HI}_{\rm g} {\rm = 1/2 Mn}_{\rm 2} {\rm I}_{{\rm 4,g}} {\rm + 1/4P}_{{\rm 4,g}} {\rm + H}_{{\rm 2,g}} $$\end{document} entscheidend.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730105
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    Über Chalkogenolate. 193. S-Bis(trimethylsilyl)aminoester von Dithiocarbamidsäuren 2. Spektroskopische Charakterisierung (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 75-88 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 193. S-Bis(trimethylsilyl)amino Esters of Dithiocarbamic Acids. 2. Spectroscopic CharacterizationElectron absorption, infrared, and nuclear magnetic resonance spectra (1H, 13C, 29Si, 15N) of the title compounds RR′N—CS—S—N[Si(CH3)3]2 with R = R′ = CH3, C2H5, CH(CH3)2, CH2—C6H5 as well as with R = CH3 and R′ = C6H5 are communicated and discussed.Coupling constants have been determined (data see „Inhaltsübersicht“).For the compound with R = R′ = CH3 the free activation energy of the rotation barrier around the N—CS bond is ΔG* = 58 kJ/mol at -2°C (coalescence temperature).
    Notes: Elektronenabsorptions-, Infrarot- und Kernresonanzspektren (1H, 13C, 29Si, 15N) der Titelverbindungen RR′N—CS—S—N[Si(CH3)3]2 mit R = R′ = CH3, C2H5, CH(CH3)2, CH2—C6H5 sowie mit R = CH3 und R′ = C6H5 werden mitgeteilt und diskutiert.Folgende Kopplungskonstanten wurden ermittelt (R = R′ = CH3):\documentclass{article}\pagestyle{empty}\begin{document}$$ \begin{array}{l} ^{\rm 1} {\rm J}\left({{}^{\rm 1}{\rm H} - {}^{12}{\rm C}} \right) = 119{\rm Hz},{}^2{\rm J}({}^1{\rm H} - {}^{29}{\rm Si} = 6,5{\rm Hz}, \\ ^{\rm 1} {\rm J}\left({{}^{{\rm 13}}{\rm C} - {}^{12}{\rm Si}} \right) = 57,7{\rm Hz},{}^2{\rm J}({}^{13}{\rm C} - {}^{15}{\rm N} = 1,97{\rm Hz}, \\ ^{\rm 1} {\rm J}\left({{}^{{\rm 29}}{\rm Si} - {}^{15}{\rm N}} \right) = 8,97{\rm Hz},{}^3{\rm J}({}^{15}{\rm N} - {}^1{\rm H)} \approx 0,5{\rm Hz}{\rm .} \\ \end{array} $$\end{document}Für die Verbindung mit R = R′ = CH3 beträgt die freie Aktivierungsenergie der Rotationsbarriere um die N—CS-Bindung ΔG* = 58 kJ/mol bei der Koaleszenztemperatur (-2°C).
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    URL: http://dx.doi.org/10.1002/zaac.19895730108
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    Kronenthioetherkomplexe des Cobalt(III): Ligandenstruktur und Redoxreaktivität Struktur, Elektrochemie und Kinetik des Elektronenaustausches von [Co(tacn)(ttcn)]Br3 · 3 H2O (tacn = 1,4,7-Triazacyclononan, ttcn = 1,4,7-Trithiacyclononan) (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 43-62 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crown Thioether Complexes of Cobalt(III): Ligand Structure and Redoxreactivity. Crystal Structure, Electrochemistry, and Kinetics of the Electron Transfer Exchange Reactions of [Co(tacn)(ttcn)] Br3 · 3 H2O (tacn = 1,4,7-Triazacyclonone, ttcn = 1,4,7-Trithiacyclononane)Synthesis, crystal structure and redoxreactivity of [Co(tacn)(ttcn)]Br3 · 3 H2O (tacn = 1,4,7-triazacyclononane, ttcn = 1,4,7-trithiacyclononane) are reported. Average Co—S and Co—N bond distances are 2.247 Å and 1.961 Å, respectively. Cyclic voltammetry revealed two reversible electron transfer waves at +0.01 V vs. NHE ([Co(tacn)(ttcn)]3+/2+) and at -1.15 V vs. NHE ([Co(tacn)(ttcn)]2+/1+) at 25°C, I = 0.1 M. Electron transfer self exchange rate constants, k11, M-1 s-1, have been determined for the couples [Co(tacn)(ttcn)]3+/2+, [Co(ttcn)2]3+/2+, and [Fe(tacn)2]3+/2+ to be 4.2 X 104 (25°C; I = 0,1 M); 1.6 X 105 M-1 s-1 (25°C; I = 0.2 M); 4.6 x 103 M-1s-1 (25°C, I = 0.05) M-1 s-1, respectively. k11 for [Co(ttcn)2]3+/2+ has been determined using 1H NMR line-broadening techniques; for [Co(tacn)(tten)]3+/2+ and [Fe(tacn)2]3+/2+ the kinetics of the cross-reactions ([Ru(NH3)6]2+, respectively) have been measured, and K11 was evaluated using the Marcus-cross-relationship.
    Notes: Synthese, Kristallstruktur und Redoxreaktivität von [Co(tacn)(ttcn)]Br3 · 3 H2O (tacn = 1,4,7-Triazacyclononan; ttcn = 1,4,7-Trithiacyclononan) werden beschrieben. Mittlere Co—S- und Co—N-Bindungsabstände werden zu 2,247 Å bzw. 1,961 Å bestimmt. Das Redoxpotential für [Co(tacn)(ttcn)]3+/2+ bei 25°C (I = 0,1 M) ist + 0,01, während es für das Paar [Co(tacn) (ttcn)]2+/1+ bei -1,15 V gegen NHE mittels der cyclischen Voltammetrie bestimmt wurde. Die Elektronenaustauschgeschwindigkeitskonstante, k11, M-1 s-1, für [Co(tacn)(ttcn)]3+/2+ wurde über die Messung der Kinetik der gekreuzten Redoxreaktionen zwischen [Co(tacn)(ttcn)]3+ und [[Ru(NH3)6]2+ mit Hilfe der Marcus-Gleichung bestimmt: 4,2 X 104 M-1 s-1 (25°C, I = 0,1 M). Für das analoge Komplexpaar [Co(ttcn)2]3+/2+ wurde diese Konstante durch 1H-NMR-Linienverbreiterungsmethoden direkt gemessen: k11 = 1,6 X 105 M-1 s-1 (25°C; I = 0,2 M). Für [Fe(tacn)2]3+/2+ wurde diese Konstante pulsradiolytisch bestimmt: 4,6 X 103 M-1 s-1 (25°C, I = 0,05M).
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730106
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  • 90
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    Ein neuer Strukturtyp bei Barium-Lanthanoid-Aluminaten: Ba6Dy2Al4O15 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 89-94 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Structure on Barium Lanthanoid Aluminates: Ba6Dy2Al4O15Ba6Dy2Al4O15 was prepared and investigated by X-ray single crystal technique. It shows a new structure type and belongs to the space group D2h17-Cmcm; a = 5.898; b = 10.183; c = 14.877 Å; Z = 2. The crystal structure of this compound is determined by a BaO-network consisting of 8+1 coordinated Ba2+ ions. Furthermore by corner connected double-tetrahedra around Al3+ and isolated Dy3+ octahedra. One of the oxygen pointpositions is partially occupied by O2- and belongs only to the Ba2+ ions.
    Notes: Mit Einkristall-Röntgenbeugungsmethoden wurde an Ba6Dy2Al4O15 ein neuer Strukturtyp gefunden. Es kristallisiert orthorhombisch, Raumgruppe D2h17-Cmcm, a = 5,898; b = 10,183; c = 14,877 Å, Z = 2. Den Aufbau dieser Verbindung bestimmt ein BaO-Gerüst mit einer 8+1-Sauerstoffkoordination um Ba2+, ferner eckenverknüpfte Doppeltetraeder um Al3+ und isolierte Oktaeder um Dy3+. Ein O2- auf einer partiell besetzten Punktlage ausschließlich zu den Ba2+-Ionen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730109
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  • 91
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    „LaTa5O14“, ein Derivat der tetragonalen Wolframbronzen Präparation und Struktur (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 107-118 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: „LaTa5O14“, a Derivative of the Tetragonal Tungsten Bronzes. Preparation and Structure„LaTa5O14“ single crystals were synthesized for the first time by heating mixtures La2O3/Ta2O5 (1:5) at temperatures of T = 1 685°C in air. „LaTa5O14“ crystallizes in the orthorhombic space group Cmmm with a = 16.977(1) Å, b = 17.594(1) Å and c = 3.8480(4) Å. The structure was refined to give R = 6.36% and Rw = 3.27%. The Ta atoms are partly surrounded by O octahedrally, partly pentagonal-bipyramidal. The unit cell is built up by layers of composition [Ta22O62]14- connected along the [001] direction with holes filled up totally or partly with La. The relationship to the tetragonal tungsten bronzes will be discussed.
    Notes: Im System La2O3/Ta2O5 gelang erstmals die Darstellung von gelben „LaTa5O14“-Einkristallen durch Tempern der Gemenge La2O3/Ta2O5 (1:5) bei T = 1 685°C an Luft. „LaTa5O14“ kristallisiert orthorhombisch in der Raumgruppe Cmmm mit den Gitterkonstanten a = 16,977(1) Å, b = 17,594(1) Å und c = 3,8480(4) Å. Die Struktur wurde bis R = 6,36% bzw. Rw = 3,27% verfeinert. Ta(1), Ta(3) und Ta(4) sind oktaedrisch, Ta(2) ist pentagonal-bipyramidal von O umgeben. Schichten aus diesen Polyedern sind über O-Teilchen entlang [001] miteinander eckenverknüpft. Vom Ta-O-Netzwerk der Zusammensetzung [Ta22O62]14- gebildete Lücken sind ganz oder teilweise mit La-Teilchen gefüllt; die Verbindung besitzt deshalb nur annähernd die Zusammensetzung LaTa5O14. Eine Verwandtschaft zu den tetragonalen Wolframbronzen ist erkennbar.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730111
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  • 92
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    Beiträge zur Untersuchung anorganischer nichtstöchiometrischer Verbindungen. XXXVII. Präparation und durchstrahlungselektronenmikroskopische Untersuchung von (Cu, Nb)12O29 und (Cu, Nb)15O37 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 95-106 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Investigation of Inorganic Non-stoichiometric Compounds. XXXVII. Preparation and Transmission Electronmicroscopical Investigation of (Cu, Nb)12O29 and (Cu, Nb)15O37With gaseous HgCl2 the compound CuNb2O6 decomposes and Nb2O5 is formed, if the reaction products CuCl and CuO can migrate in a gradient of temperature (1 000 → 900°C) to the colder end of a closed ampoule. By breaking off the decomposition (Cu, Nb)12O29 and (Cu, Nb)15O37 were isolated as metastable intermediate products. The results of the high resolution transmission electronmicroscopical investigations show that the new oxides are built of edgesharing [3 × 4] and [3 × 5] blocks, respectively, in a monoclinical arrangement and are members of the structure family M3nO8n-3 (n = 4 and 5, respectively). The real structures showed different defects; during the investigation of a crystal an unusual in-situ reaction caused by the electron beam had been observed.
    Notes: Unter Einwirkung von gasförmigen HgCl2 geht CuNb2O6 in Nb2O5 über wenn die Reaktionsprodukte CuCl und CuO im Temperaturgefälle (z. B. 1 000 → 900°C) an das kältere Ende einer geschlossenen Ampulle wandern können. Durch Abbrechen des Abbauvorganges ließen sich (Cu, Nb)12O29 und (Cu, Nb)15O37 als metastabile Zwischenprodukte erhalten. Nach dem Ergebnis der hochauflösenden Durchstrahlungs-Elektronenmikroskopie sind die neuen Oxide aus kantenverknüpften [3 × 4]- bzw. [3 × 5]-Blöcken in monokliner Anordnung aufgebaut und damit als Mitglieder der Strukturfamilie M3nO8n-3 (n = 4 bzw. 5) anzusehen. Die Realstrukturen zeigten eine unterschiedliche Fehlordnung; während der Untersuchung wurde bei einem Kristall eine ungewöhnliche in-situ-Reaktion durch Einwirkung des Elektronenstrahls beobachtet.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730110
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  • 93
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    Elektronenmikroskopische Untersuchung in Hochauflösung an La3TaO5(OH)Cl3 und Pr3TaO4Cl6 - Vergleich mit der rechnerischen Simulation (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 119-127 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: High Resolution Electron Microscopy Investigation of La3TaO5(OH)Cl3 and Pr3TaO4Cl6 - A Comparison with Calculated ImagesThe phases La3TaO5(OH)Cl3 and Pr3TaO4Cl6 prepared by chemical transport have been investigated by high resolution electron microscopy. The micrographs taken agree well with simulated images. In spite of the close relationship of both structures the simulated images are not as similar as expected. The unoccupied channels at the corners of the cell can be seen distinctly. According to the resolution of our electron microscope La3TaO5(OH)Cl3 lattice constants of which are too small does not show any further detail, whereas the sites of the heavy atoms of Pr3TaO4Cl6 can be recognized at a suitable value of defocus.
    Notes: Kristalline Proben von La3TaO5(OH)Cl3 und der neuen Verbindung Pr3TaO4Cl6 konnten durch eine chemische Transportreaktion erhalten werden. Bei elektronenmikroskopischen Untersuchungen in Hochauflösung zeigten die Aufnahmen eine gute Übereinstimmung mit Bildern, die mit einem Kontrastprogramm simuliert worden waren. Wie eine Gegenüberstellung von zwei simulierten Defokusserien ergab, ist die enge strukturelle Verwandtschaft der beiden Oxidchloride hier nicht unmittelbar wiederzufinden. Man erkennt bei beiden Verbindungen die an den Eckpunkten der Zelle gelegenen unbesetzten Kanäle, die sich deutlich vom übrigen Kontrastmuster abheben. Bei La3TaO5(OH)Cl3, der Verbindung mit den kürzeren Gitterkonstanten, reichte das Auflösungsvermögen unseres Mikroskops für weitere Details im Innern der Elementarzelle nicht aus, während bei Pr3TaO4Cl6 die Schweratomlagen bei geeigneten Defokusbedingungen noch zu erkennen sind.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730112
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  • 94
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    Ein Wechsel des Strukturtyps in den Oxiden BaCoGd2O5, BaCoDy2O5 und BaCoY2O5 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 128-132 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Change of Structure Type in the Oxides BaCoGd2O5, BaCoDy2O5, and BaCoY2O5(I) BaCoGd2O5, (II) BaCoDy2O5, and (III) BaCoY2O5 were prepared for the first time and examined by single crystal work. (I) and (II) belong to the BaNiLn2O5-type. (I): a = 3.770; b = 5.860; c = 11.620 Å; Z = 2; (II): a = 3.755; b = 5.798; c = 11.514 Å; Z = 2; space group D2h25-Immm. (III) crystallizes in the BaCuLn2O5-type, space group D2h16-Pnma, a = 12.287; b = 5.713; c = 7.067 Å; Z = 4. The coordination of Co2+ changes from (I, II) to (III) from octahedral to tetragonal pyramidal.
    Notes: (I) BaCoGd2O5, (II) BaCoDy2O5 und (III) BaCoY2O5 wurden neu dargestellt und an Einkristallen mit Röntgenbeugungsmethoden die Kristallstruktur bestimmt. (I) und (II) gehören zum BaNiLn2O5-Typ mit (I): a = 3,770; b = 5,860; c = 11,620 Å; Z = 2; (II): a = 3,755; b = 5,798; c = 11,514 Å; Z = 2; beide kristallisieren in der Raumgruppe D2h25-Immm. (III) kristallisiert im BaCuLn2O5-Typ, Raumgruppe D2h16-Pnma, mit a = 12,287; b = 5,713; c = 7,067 Å; Z = 4. Die Koordination um Co2+ wechselt von (I, II) nach (III) von oktaedrisch nach tetragonal-pyramidal.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730113
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  • 95
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    Neues über Oxotellurate(VI) der Alkalimetalle Zur Existenz und Konstitution von Li6TeO6 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 133-142 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Oxotellurates(VI) of the Alkali Metals. Existence and Constitution of Li6TeO6For the first time Li6TeO6 is prepared as transparent, colourless single crystals, and the structure has been determined [four-circle diffractometer data, Siemens AED2, MoKα, 371 out of 371 IO(hkl), R = RW = 0.7%, R3, a = 791.99(6) pm, c = 696.44(7) pm, Z = 3].The structure refinement shows that Li6TeO6 is a variant of the NaCl-Typ. Nevertheless there is a relationship with α-Li6UO6 [2]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, the latter derived from Mean Effective Fictive Ionic Radii, MEFIR, are calculated and discussed.
    Notes: Erstmals wurden klar durchscheinende, farblose Einkristalle von Li6TeO6 dargestellt und strukturell untersucht. [Vierkreisdiffraktometerdaten, Siemens AED2, MoKα-Strahlung, 371 von 371 IO(hkl), R = RW = 0,7%, R3, a = 791,99(6) pm, c = 696,44(7) pm, Z = 3].Die Strukturbestimmung zeigt, daß Li6TeO6 eine Variante des NaCl-Typs ist. Dennoch besteht Verwandtschaft mit α-Li6UO6 [2]. Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, diese über Mittlere Effektive Ionenradien, MEFIR, werden berechnet und diskutiert.
    Additional Material: 12 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730114
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  • 96
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    Zwei neue Ordnungs-Varianten des NaCl-Typs: Li4MoO5 und Li4WO5 (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 157-169 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Two New Variants of the NaCl Type of Structure: On Li4MoO5 and Li4WO5For the first time in form of colourless, transparent single crystals of Li4MoO5 [annealed mixtures of Li2O and MoO3, Li:Mo = 4.2:1, Ni-cylinder, 950°C, 28 d] as well as Li4WO5 [annealed mixtures of Li2O and WO3, Li:W = 4.4:1, Au-tube, 950°C, 28 d, slowly cooling] have been prepared. Single crystal data show isotypic oxides of the Li4TeO5-type, a deformed variant of the NaCl-type of structure [Li4MoO5: 1379 IO(hkl), four-circle-diffraktometer Philips PW 1100, ω--2Θ scan, AgKα, R = 8.7% and RW = 8.3%, space group P1 with a = 511.9(1), b = 772.7(2), c = 506.4(1) pm, α = 101.70(1)°, β = 101.48(1)°, γ = 108.58(2)°, Z = 2 and Li4WO5: 1027 IO(hkl), Philips PW 1100, ω-2Θ scan, MoKα, R = 4.0% und RW = 3.7%, space group P1 with a = 510.94(5), b = 771.59(7), c = 506.09(4) pm, α = 101.804(8)°, β = 101.78(1)°, γ = 108.770(9)°, Z = 2]. The structural relations are deduced from Schlegel Diagrams. The Madelung Part of Lattice Energie, MAPLE, and Effective Coordination Numbers, ECON, these via Mean Fictive Ionic Radii, MEFIR, are calculated and discussed.
    Notes: Erstmals wurde in Form farbloser, transparenter Einkristalle Li4MoO5 [aus Gemengen von Li2O und MoO3. Li:Mo = 4,2:1, Ni-Bömbchen, 950°C, 28 d] sowie Li4WO5 [aus Gemengen von Li2O und WO3, Li:W = 4,4:1, Au-Rohr, 900°C, 30 d] dargestellt. Nach Einkristalldaten liegt bei den isotypen Oxiden vom Li4TeO5-Typ eine Ordnungsvariante des NaCl-Typs [Li4MoO5: 1379 IO(hkl), Vierkreisdiffraktometer Philips PW 1100, ω-2Θ scan, AgKα, R = 8,7% und RW = 8,3%, Raumgruppe P1 mit a = 511,9(1), b = 772,7(2), c = 506,4(1) pm, α = 101,70(1)°, β = 101,48(1)°, γ = 108,58(2)°, Z = 2 bzw. Li4WO5: 1027 IO(hkl), Philips PW 1100, ω-2Θ scan, MoKα, R = 4,0% und RW = 3,7%, Raumgruppe P1 mit a = 510,94(5), b = 771,59(7), c = 506,09(4) pm, α = 101,804(8)°, β = 101,78(1)°, γ = 108,770(9)°, Z = 2] vor.Die strukturellen Zusammenhänge werden aus den Schlegel-Diagrammen abgeleitet. Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECON, diese über Mittlere Fiktive Ionenradien, MEFIR, berechnet, werden mitgeteilt und diskutiert.
    Additional Material: 15 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730116
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    On [Na(POCl3)4]+ Complex Ion Formation: Conductivity, Raman, and NMR studies in the system phosphoryl chloride-sodium tetrachloro aluminate and related compounds (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 573 (1989), S. 170-184 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Über die Bildung von [Na(POCl3)4]+-Komplexionen. Leitfähigkeits-, Raman- und NMR-Untersuchungen im System Phosphorylchlorid-Natriumtetrachloroaluminat bzw. analoger VerbindungenLeitfähigkeiten, Raman- sowie 27Al-, 23Na- und 31P-NMR-Spektren des Systems POCl3-NaAlCl4 wurden in Abhängigkeit vom Molenbruch x(NaAlCl4) im lösungsmittelreichen Gebiet gemessen. Zusätzlich erfolgte die Registrierung der Raman-Spektren der Lösungen von NaFeCl4, LiAlCl4, LiFeCl4 und KAlCl4 in POCl3. In den Li+- bzw. Na+-Ionen enthaltenden Proben konnte unter bestimmten Bedingungen ein von Temperatur und Salzkonzentration abhängiger Phasenübergang von der flüssigen in die feste Phase beobachtet werden. Deutliche Veränderungen in den Ramanspektren der Elektrolytlösungen im Vergleich zum reinen Lösungsmittel POCl3 belegen die Existenz von intermolekularen Wechselwirkungen, durch die das POCl3-Molekül beeinflußt wird. Die Annahme der Bildung von [M(POCl3)4]+-Solvaten (M = Li, Na) aufgrund der Ramanergebnisse wird durch die Resultate der NMR-Spektroskopie unterstützt.
    Notes: The system POCl3-NaAlCl4 was investigated by measuring the conductivity and the Raman and NMR spectra (27Al, 23Na and 31P) as a function of the mol fraction x of NaAlCl4 in POCl3. Additionally, Raman spectra of POCl3 solutions of NaFeCl4, LiAlCl4, LiFeCl4, and KAlCl4 were recorded. In solutions containing Li+ or Na+ ions a liquid to solid (or jelly) phase transition was observed under certain conditions, dependent on salt concentration and temperature. Observed changes in the Raman spectra of the electrolyte solutions in comparison to the pure solvent POCl3 demonstrate the existence of interactions. Clearly, the POCl3 eigenfrequencies and hence the molecules are pertubed. The formation of [M(POCl3)4]+ complexes (M = Li, Na) can be deduced from the Raman measurements. NMR investigations support this conclusion. For assigning of Raman spectra, (Li+, K+) cation and ([FeCl4]-, [SbCl6]-) anion substitutions were employed.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895730117
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  • 98
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    Zum Aufbau von RbNa5Be8O11Professor Reginald Gruehn zum 60. Geburtstage am 6. Oktober 1989 gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 77-89 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On RbNa5Be8O11For the first time RbNa5Be8O11 was obtained by annealing intimate mixtures of the binary oxides (Rb:Na:Be = 1.1:5.5:8, Ni-cylinder, 650°C, 21d). The compound crystallizes triclinic (P 1) with a = 1 063.4 pm, b = 645.6 pm, c = 948.8 pm, α = 110.2º, β = 114.9º, γ = 90.8º, Z = 2. The crystal structure was solved by four-circle-diffractometer data [Siemens AED2, 3099 I0 (hkl), R = 5.1%, Rw = 3.8%]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, are calculated.
    Notes: RbNa5Be8O11 wurde erstmals durch Erhitzen inniger Gemenge der binären Oxide in Form von farblosen Einkristallen und Pulver erhalten (vor Verreiben: Rb:Na:Be = 1,1:5,5:8; Ni-Zylinder, 650°C, 21d). RbNa5Be8O11 kristallisiert triklin (P 1) mit a = 1 063,4 pm, b = 645,6 pm, c = 948,8 pm, α = 110,2º, β = 114,9º, γ = 90,8º, Z = 2. Die Kristallstruktur wurde über Vierkreisdiffraktometerdaten [Siemens AED2, 3099 I0(hkl), R = 5,1%, Rw = 3,8%] aufgeklärt. Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, werden berechnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895750111
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  • 99
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    Über die Umsetzung von NN-Dihalogenperfluoralkanaminen mit Schwefel und SchwefelderivatenAus der Dissertation von Martin Geisel, Univ. Göttingen 1984. (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 90-96 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of NN-Dihaloperfluoroalkaneamines with Sulfur and Sulfur DerivativesReactions of NN-Dihaloperfluoroalkaneamines RfNX2 (Rf = CF3, C2F5; X = Cl, Br) with S8, S4N4 and A = SX2 (A = RfN, O) are described. The products isolated are: Sulfurdihalideimides RfNSX2 (Rf = CF3, C2F5; X = Cl, Br), Sulfurdiimides RfNSNRf and Bis(sulfurdiimido)sulfides (RfNSN)2S(Rf = CF3, C2F5). Thionylimides RfNSO were not obtained in preparative quantities.
    Notes: Umsetzungen der NN-Dihalogenperfluoralkanamine RfNX2 (Rf = CF3, C2F5; X = Cl, Br) mit S8, S4N4 und A = SX2 (A = RfN, O) werden beschrieben. Dabei lassen sich als Produkte isolieren: Schwefeldihalogenidimide RfNSX2 (Rf = CF3, C2F5, X = Cl, Br), Schwefeldiimide RfNSNRf und Bis(schwefeldiimido)sulfide (RfNSN)2S (Rf = CF3, C2F5). Thionylimide RfNSO sind auf diesem Wege nicht in präparativem Maßstab zugänglich.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895750112
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  • 100
    Electronic Resource
    Electronic Resource
    Untersuchungen Zur Jarositbildung (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 575 (1989), S. 115-120 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Study of Jarosite FormationThe reaction of solutions of ferric sulphate with potassium hydroxide yields Jarosite KFe3(OH)6(SO4)2 as the only compound detectable by X-rays, if the mole ratio b = KOH : Fe3+ is in the range 0.5 ≤ b ≤ 2.0 independent of the temperature of reaction. At first amorphous ferric oxide hydrate is precipitated in solutions with 1 ≤ b ≤ 2. This precipitate reacts with aquo-iron complexes of the solution in a way of a acid-base comproportionation and yields Jarosite. In solutions with b ≥ 2.5 the formation of Jarosite is impossible. By raising the temperature of reaction from 20 to 95°C the degree of reaction is increased, because the equilibria of the hydrolysis are shifted to the side of the hydroxo complexes.
    Notes: Beim Umsetzen von Eisen(III)-sulfatlösung mit Kalilauge erhält man beim Einhalten eines Molverhältnisses b = KOH:Fe3+ im Bereich 0,5 ≤ b ≤ 2,0 unabhängig von der Reaktionstemperatur die Verbindung Jarosit KFe3(OH)6(SO4)2 als einziges röntgenographisch nachweisbares Reaktionsprodukt. In Lösungen mit 1 ≤ b ≤ 2 fällt beim Zugeben der Kalilauge zunächst amorphes Eisenoxidhydrat aus, das im Verlaufe der weiteren Reaktion mit noch in Lösung befindlichen Eisen(III)-aquoionen im Sinne einer Säure-Basen-Komproportionierung zu Jarosit umgesetzt wird. Bei b ≥ 2,5 wird das Eisen quantitativ als Oxidhydrat gefällt und Jarosit nicht gebildet. Beim Verändern der Temperatur von 20 auf 95°C vergrößert sich der Umsetzungsgrad durch Verschieben der Hydrolysegleichgewichte auf die Seite der Hydroxokomplexe.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895750114
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