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  • 1985-1989  (1,542)
  • 1970-1974
  • 1988  (786)
  • 1986  (756)
  • Inorganic Chemistry  (1,307)
  • Genetics  (235)
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Psychopharmacology 94 (1988), S. 428-430 
    ISSN: 1432-2072
    Keywords: Lithium ; Clonidine ; alpha2-Adrenoceptor ; Locomotor activity ; Genetics ; Mice
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Four strains of mice (C57, BALB, DBA, C3H) were used to determine whether genetic factors influence the effects of lithium on hypoactivity induced by a low dose of the alpha2-adrenoceptor agonist clonidine (0.2 mg/kg). Lithium was administered in the diet for 3–4 weeks at a dosage that produced average serum lithium levels of 0.58–0.66 mmol/l. Locomotor activity was reduced by either clonidine or by lithium given alone. When combined, however, lithium attenuated the activity-suppressant effects of clonidine, and that action was influenced by genetic factors. The findings suggest that genetic differences in alpha2-adrenoceptors play a role in behavioural effects of lithium.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Theoretical and applied genetics 76 (1988), S. 405-410 
    ISSN: 1432-2242
    Keywords: Zea mays ; Haploid induction ; Gynogenesis ; Genetics ; Inducer line
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary The effect of genotype on maternal haploid plant production in maize was studied. The frequency of gynogenetic plants when “Stock 6” was used as pollinator varied according to the female parent genotype. No simple relation was observed between genotypic aptitudes for gynogenetic and androgenetic development, which occured after pollination of “W23” plant carrying the “indeterminate gametophyte” gene. Furthermore, the population NS, a favorably responsive genotype to anther culture, does not exhibit exceptional ability for in vivo gynogenesis. The effect of inbreeding and the influence of maternal haploid origin suggest that specific genes control maternal haploid initiation and development. However, gynogenetic development is not limited to a particular genotype. The frequency of maternal haploids may be increased by using specific pollen parents. Attempts were made to select for a high haploidyinducing trait and the present study reports the successful development of lines that can be utilized as pollen parents to induce haploids for experimental purposes and breeding programmes. When an inbred line “WS14”, derived from the cross W23 x Stock 6, was used as pollen parent, 2%–5% maternal haploids were obtained according to the female parent genotype. A high haploidy-inducing potential is a heritable trait and may be controlled by a limited number of genes. Genetic determination of the haploidy-inducing character was examined in relation to the efficiency of the selecting method and the mechanisms involved in the origin of maternal haploids.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Pediatric nephrology 2 (1988), S. 239-243 
    ISSN: 1432-198X
    Keywords: Cockayne syndrome ; Renal histology ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Two siblings with typical features of the Cockayne syndrome were studied at autopsy. Many glomeruli revealed a paucity of capillary loops and had thickened capillary walls. Some glomeruli with advanced lesions showed collapse of the glomerular tufts or complete hyalinization. Atrophy of tubules and interstitial fibrosis were also observed. There were no significant arteriosclerotic changes in the vessels. Ultrastructural studies demonstrated thickened glomerular basement membranes with bends and folds. These histopathological findings are different to those previously reported with the exception of the 1966 report by Ohno and Hirooka.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1432-1440
    Keywords: Genetics ; Hepatitis-B virus ; Immunogenetics ; Vaccination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The variation in immune responses to standard inoculation of the hepatitis-B virus vaccine suggest that host factors influence response in ways that are not presently understood. We studied 25 low/nonresponding health care workers (anti-HBs titer 〈50 IU/l) after the third inoculation of an experimental hepatitis-B vaccine to determine their immune status (through lymphocyte phenotypes) and HLA type. After application of a fourth inoculation, the seroconverting subjects showed only low anti-HBs levels; three male subjects remained anti-HBs negative. Twelve months after the fourth inoculation only 9 of 25 subjects (36%) maintained anti-HBs titer 〉10 IU/l. Almost all subjects had normal B-cell and CD-4 and CD-8 counts and ratios. Relative to other European populations HLA-A-10 (P〈0.05), B-12 (P〈0.025), CW-5 (P〈0.05), DR-3 (P〈0.025), and DR-5 (P〈0.025) were increased, whereas DR-2 (P〈0.05) was decreased. However, after correction of theP-values for the number of HLA antigens determined, these differences were no longer significant. Furthermore, these HLA types were not the same as those reported in other studies (except for DR-3). We suggest that larger sample sizes or even not yet available immunogenetic markers will be required to prove an “immunogenetic background” in low/nonresponders, if it exists.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Cellular and molecular life sciences 44 (1988), S. 491-495 
    ISSN: 1420-9071
    Keywords: Genetics ; stress ; emotionality ; locus ceruleus ; Maudsley strains
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The Maudsley Reactive and Non-Reactive strains have been developed as a model for the study of individual variations in stress-reactivity, and many differences in biobehavioral systems have been found between them. This review discusses limitations of the ‘emotionality’ construct in accounting for differences between the Maudsley strains and offers an alternative, theoretical approach. Amaral and Sinnamon have proposed that the locus ceruleus (LC) plays a stress-attenuating role in mediating behavioral, physiological and neuroendocrine response to prepotent, emergency-provoking stimuli and, building upon this formulation, it is proposed that the LC has been an important focus for gene action in the Maudsley model. It is suggested that the LC of the Non-Reactive strain is more strongly activated by stressful stimuli than the LC of Reactive rats, and is the basis of many of the behavioral and physiological differences between them. Behavioral and biochemical evidence consistent with this proposition is reviewed. Identification of the LC as a target for gene-action in the Maudsley model has an important advantage. It substitutes variations at a specific anatomic location in the brain for a loosely defined construct like emotionality, and the hypothesis is amenable to empirical tests by a variety of experimental approaches.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    European journal of pediatrics 147 (1988), S. 550-552 
    ISSN: 1432-1076
    Keywords: Pterygium syndrome ; Congenital malformations ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract We present two brothers with Multiple Pterygium Syndrome type Escobar. Characteristic findings in this autosomal recessively inherited pterygium syndrome are, in addition to multiple pterygia, short stature, cleft palate, vertebral fusion defects and minor facial anomalies. The adult height in the two male siblings was below the third centile. Secondary sexual development and testicular size were normal, in contrast with the cryptorchidism and pubertal delay documented in most young patients.
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  • 7
    ISSN: 1432-0428
    Keywords: Genetics ; Type 2 (non-insulin-dependent) diabetes ; insulin receptor ; linkage analysis ; maturity onset diabetes of the young
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The possibility of linkage between the human insulin receptor gene locus and diabetes was examined in three Type 2 (non-insulin-dependent) diabetic families and one family with maturity onset diabetes of the young. Insulin receptor gene haplotypes were established using BglII, Rsal and Sstl restriction enzyme digests of genomic DNA from all available family members. The digested DNA was subjected to agarose gel electrophoresis, Southern blotted, and hybridised to 32P-labelled human insulin receptor gene cDNA. In the pedigree with maturity onset diabetes of the young, formal linkage analysis allowed exclusion of close linkage between the insulin receptor locus and diabetes (logarithm of the odds for linkage versus non-linkage was −5.35 at recombination fraction of 0.01). This confirms the absence of linkage between insulin receptor and diabetes which has been reported in two similar pedigrees. In the three Type 2 diabetic families there were a minimum of 4 recombinants between the insulin receptor locus and diabetes, which makes a direct role for insulin receptor defects unlikely. The importance of using realistic estimates of penetrance when performing linkage analysis in a disease with a late age of onset is emphasised. In contrast to the one previous linkage analysis study of the insulin receptor gene, no specific association of diabetes with the rare Sstl Sl(-) allele was observed in either the maturity onset diabetes of the young or the Type 2 diabetic families.
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    Diabetologia 31 (1988), S. 407-414 
    ISSN: 1432-0428
    Keywords: Genetics ; Type 2 (non-insulin-dependent) diabetes ; linkage analysis ; restriction fragment length polymorphism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary In the last five years, genetic markers for a large number of diseases have been localised using linkage analysis of DNA polymorphisms in affected families. The site of the genetic defect or defects leading to Type 2 (non-insulin-dependent) diabetes mellitus, a common illness with a major genetic component, remains unknown. This is due, at least in part, to the lack of large well-defined Type 2 diabetic pedigrees suitable for linkage analysis. There are several features of the disease which make large pedigrees difficult to find. The late age of onset of most probands means that informative older generations are often dead, while there is difficulty in detecting disease in younger generations. The diagnostic criteria for diabetes are, as yet, dependent on an arbitrary cut-off along a continuum of plasma glucose. The high prevalence of the disease may also produce problems as, in any given family, diabetogenic genes may be contributed by more than one parent. Varieties of the disease with a well-defined inheritance, such as maturity onset diabetes of youth, are more suitable for linkage analysis but might be due to defects at a different gene locus. Despite these difficulties, once large well-defined pedigrees have been found, linkage analysis using both candidate genes and random highly polymorphic markers is the strategy most likely to find genetic markers for the disease.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1432-2242
    Keywords: Ornithine decarboxylase ; Chicken ; Muscle ; Genetics ; Growth differences
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Little is known about the biochemical correlates of selection for growth in farm or laboratory animals, or the identity of the gene products affected or produced by ‘trait-genes’. Modern broiler chickens have about 8-fold greater breast muscle mass than layer chickens at 7 weeks of age and over 2-fold greater breast muscle mass than their 1972 counterparts. This increase in muscle mass is associated with over 20-fold higher levels of ornithine decarboxylase (ODC) in broiler chickens at 1 week of age as compared with layer strain chickens; there is a comparable increase in a relaxed-selection strain of broilers. The increase in ODC levels is larger than the differences in muscle or body weight between broilers and layers at 7 weeks of age, occurs at an age when there is no difference in weights between the strains and precedes the major growth spurt. Increases in ODC levels and hence polyamine synthesis have been associated with, and usually precede, rapid growth and cell proliferation in a wide range of cell types and organisms in response to many different stimuli. Therefore, the correlation of ODC levels with genetic differences in muscle growth make it worth investigating the control of ODC gene expression in these strains.
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Theoretical and applied genetics 75 (1988), S. 889-901 
    ISSN: 1432-2242
    Keywords: Soybean ; Restriction fragment length polymorphism ; Genetics ; Allele ; Variation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Restriction Fragment Length Polymorphisms (RFLP) have been identified between widely distant cultivars (‘Minsoy’ and ‘Noir 1 ’) of soybean Glycine max (L.) Merrill. Using as probes randomly chosen clones of DNA, one in five probes revealed a polymorphism. More than half of these polymorphisms appear to result from rearrangements of the genomic DNA. Twenty seven markers were analyzed for linkage in F2 plants. Eleven of these markers were contained in four linkage groups. Five cultivars were compared in a search for new alleles. When RFLP markers corresponding to low copy DNA were used to analyze three other cultivars — ‘Sooty’, ‘Forrest’ and ‘Mandarin (Ottawa)’ — few new alleles were found. Using these probes, five different markers could be used to differentiate the five cultivars. Complex probes, which correspond to repeated DNA, revealed different polymorphisms in different cultivars and a single such probe could be used to distinguish the five cultivars from each other.
    Type of Medium: Electronic Resource
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  • 11
    Electronic Resource
    Electronic Resource
    Springer
    Psychopharmacology 95 (1988), S. 237-244 
    ISSN: 1432-2072
    Keywords: Morphine ; Etonitazene ; Genetics ; Mice ; Taste ; Saccharine ; Gender
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract C57BL/6J and DBA/2J mouse strains have been characterized as morphine preferrers and avoiders, respectively (Horowitz et al. 1977). Previously, sweetened morphine solutions were presented with a water alternative, primarily with male subjects. Because sweetness may affect the endogenous opioid system and rodents have shown strain and sex differences in taste preferences, this study looked for strain- and gender-related taste preferences that might have affected opiate consumption. Preference for sweetened and unsweetened morphine and etonitazene was compared across gender and strain. In all choice tests, the control was a similar tasting quinine sulphate solution. Under these conditions, C57BL/6J mice continued to show strong preference for morphine. However, DBA/2J mice drank approximately equal amounts of morphine and quinine solutions, rather than avoiding morphine as when water was the alternative. Both strains appeared surprisingly indifferent to the synthetic opioid etonitazene, compared because it is potent at concentrations having barely perceptible bitterness. This raises the possibility of unexpected differences in post-ingestional effects between morphine and etonitazene. Contrary to reports of gender differences in sweet preference in rats, none were found in either strain of mouse. Neither were there any significant sex differences in opiate preference in either strain. C57 mice preferred sweetness more than did DBA mice.
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  • 12
    ISSN: 1432-2072
    Keywords: Selective breeding ; Mouse ; Ethanol-stimulated activity ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Low doses of ethanol (EtOH) stimulate activity in an open field in many strains of laboratory mice. We are selectively breeding two lines of mice to exhibit a large (FAST) response on this test, and two other lines to exhibit a small (SLOW) response (Crabbe et al. 1987). The lines initially diverged in response to EtOH, but despite continued selection pressure, the difference between each pair of FAST and SLOW lines has not increased over generations as much as expected. Our practice has been to test animals on the 1st day after saline injection, and repeat the test after EtOH injection 24 h later. Lister (1987) recently demonstrated that the order in which an animal was exposed to EtOH and saline influenced the magnitude of the response to EtOH, with animals tested initially after EtOH having greater stimulation. Middaugh et al. (1987) recently demonstrated that the magnitude of EtOH stimulation was greater under conditions of relatively bright light than under dim light. Using non-selected Swiss mice, the current experiments essentially confirmed Lister's findings. Using FAST and SLOW mice, the predictions of both groups were tested. Both hypotheses were confirmed. Additionally, these experiments demonstrated that the magnitude of the difference between FAST and SLOW mice was greater under bright light than under dim light. The line difference was also greater when tested in the EtOH-Saline order. In experiments with Swiss mice, the possible role of peritoneal irritation in the EtOH effect was eliminated, and the optimal dose and time for demonstrating the effect was determined. These experiments confirm the importance of lighting condition, order of testing, dose, and route of administration in eliciting EtOH-stimulated open field activity in mice. They demonstrate a genotype-environment interaction, since the magnitude of difference between genetically selected lines varied as a function of the testing parameters chosen. Finally, they indicate that the differences between FAST and SLOW lines in sensitivity to EtOH generalizes to several environmental conditions. We interpret this to mean that the various EtOH-induced activation traits represented by these different environmental and testing conditions are genetically correlated.
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  • 13
    Electronic Resource
    Electronic Resource
    Springer
    Journal of neurology 235 (1988), S. 366-367 
    ISSN: 1432-1459
    Keywords: Gilles de la Tourette's syndrome ; Twin study ; Computed tomography ; Clinical neurophysiology ; Genetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A 19-year-old male twin pair were concordant for suffering from Gilles de la Tourette's syndrome in different forms and severity. CT revealed ventricular asymmetries of varying degree within the normal range and there were no neurophysiological abnormalities. The interrelationship of genetic and environmental factors in phenotyping the syndrome is discussed.
    Type of Medium: Electronic Resource
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  • 14
    Electronic Resource
    Electronic Resource
    Springer
    Journal of neurology 235 (1988), S. 422-424 
    ISSN: 1432-1459
    Keywords: Epidemiology ; Genetics ; Hereditary motor neuropathy ; Spinal muscular atrophy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary A 4-year-search for spinal muscular atrophies (hereditary motor neuropathies, HMN) in Benghazi, Libya, yielded a total of 24 patients, among whom 18 were index cases. This group comprised 6 acute infantile, 12 chronic childhood, and 3 each with adult-onset proximal, and distal forms of the disorder. Distal HMN constituted 12.5% of the total cases. The crude average annual incidence of acute infantile HMN was 0.3/100,000 total population and 1/12,500 births in Benghazi. The crude prevalence rates of chronic childhood, adult-onset proximal, and distal types of HMN were 2.3, 0.6, and 0.6/100,000 respectively. The segregation ratios, 0.26 for acute infantile HMN and 0.24 for chronic childhood HMN, suggested autosomal recessive inheritance. The consanguinity rates among parents of cases and the population did not differ significantly.
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  • 15
    ISSN: 0032-8332
    Keywords: Saimiri ; Human-type ABO blood groups ; Genetics ; Colony management
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The human-type ABO blood groups were determined for 94 families of the squirrel monkey which included 151 animals. Four phenotypes of ABO blood groups (A, B, AB, and O) were detected. Family analysis revealed that the human-type ABO blood groups in this species were governed by three alleles, codominantA andB and silentO. There were intraspecific differences in the distribution of phenotypes and gene frequency among three populations imported by different routes at different times. The usefulness of ABO blood groups for defining the genetic variability of a squirrel monkey breeding colony through successive generations is discussed on the basis of the difference in distribution of ABO blood groups between wild-originated parental and its first colony-born populations.
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  • 16
    Electronic Resource
    Electronic Resource
    Springer
    European archives of psychiatry and clinical neuroscience 237 (1988), S. 244-252 
    ISSN: 1433-8491
    Keywords: EEG ; Genetics ; MZ/DZ twins reared apart ; Within-pair similarity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Within the broader context of our investigations into the heredity of the human EEG, we analysed the EEGs of 28 pairs of monozygotic and 21 pairs of dizygotic twins who were separated as infants and reared apart. The principal goal of this study was to determine the degree to which environmental factors possibly influence the development of a person's EEG. Monozygotic twins reared apart were, with respect to their EEGs, only slightly less similar to each other (if there is any difference at all) than the same person is to himself over time. For dizygotic twins reared apart, we verified the findings of our previous study, namely, that the average within-pair similarity of EEGs estimated from a sufficiently representative sample of fraternal twins was significantly higher than the average inter-individual similarity of EEGs obtained from unrelated persons. The results on both monozygotic and dizygotic twins, yielded conclusive proof that the individual EEG pattern is predominantly determined by hereditary factors.
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  • 17
    ISSN: 1432-2242
    Keywords: Taxonomy ; Germplasm identification ; Varietal identity ; Environmental interaction ; Genetics ; Multivariate analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Separations of kafirin and alcohol soluble glutelin proteins by reversed-phase high-performance liquid chromatography (RP-HPLC) from 7 inbreds and one hybrid of sorghum [Sorghum bicolor (L.) Moench] and one source of Johnsongrass [Sorghum halapense (L.) Pers.] were compared. Objectives were to assess the stability of protein profiles for seed sources produced at different locations and in different environments to examine the potential of RP-HPLC to provide genotypic profiles for sorghum. Analyses of variance data showed that levels of variation due to environments and locations were small; the majority of variation (93%) was among genotypes. Associations among inbreds revealed by multivariate and cluster analysis showed similarity with those that would be expected on the basis of pedigree. A chi-square analysis showed no deviation in the hybrid profile from the expected 2∶1 ratio of peaks from the female and male inbred parents, respectively. Improvements in the ability to correctly assign common peaks are necessary before associations among numerous sorghum genotypes can be reliably demonstrated by analysis of data from reversed-phase high-performance liquid chromatography (RP-HPLC).
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  • 18
    ISSN: 1617-4623
    Keywords: Nicotiana plumbaginifolia ; Nitrate reductase ; Genetics ; Molybdenum cofactor biosynthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary A total of 70 cnx mutants have been characterized from a collection of 211 nitrate reductase deficient (NR-) mutants isolated from mutagenized Nicotiana plumbaginifolia protoplast cultures after chlorate selection and regeneration into plants. They are presumed to be affected in the biosynthesis of the molybdenum cofactor since they are also deficient for xanthine dehydrogenase activity but contain NR apoenzyme. The remaining clones were classified as nia mutants. Sexual crosses performed between cnx mutants allowed them to be classified into six independent complementation groups. Mutants representative of these complementation groups were used for somatic hybridization experiments with the already characterized N. plumbaginifolia mutants NX1, NX24, NX23 and CNX103 belonging to the complementation groups cnxA, B, C and D respectively. On the basis of genetic analysis and somatic hybridization experiments, two new complementation groups, cnxE and F, not previously described in higher plants, were characterized. Unphysiologically high levels of molybdate can restore the NR activity of cnxA mutant seedlings in vivo, but cannot restore NR activity to any mutant from the other cnx complementation groups.
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 139-148 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Concerning Alkali Metal Metaselenoarsenites. Preparation and Crystal structures of MAsSe2, M = K, Rb, CsThe metaselenoarsenites MAsSe2, M = K, Rb, Cs were prepared by methanolothermal reaction of M2CO3 with As2Se3 at a temperature of 130°C. Their X-ray structural analyses demonstrated that the compounds contain polymetaselenoarsenite anions [AsSe2-]∞, in which the basic units are ψ-AsSe3 tetrahedra, which are linked via shared corners into infinite chains. Vierer single chains are observed for KAsSe2 and RbAsSe2, zweier single chains for CsAsSe2. The stretching units s are respectively 3,157, 2.336 and 3,378 Å. The relationship between the conformation of metaselenoarsenite chains and cation size is discussed.
    Notes: Die Metaselenoarsenite MAsSe2, M = K, Rb, Cs wurden durch methanolothermale Reaktion von M2CO3 mit As2Se3 bei einer Temperatur von 130°C dargestellt. Ihre Röntgenstrukturanalysen ergaben, daß die Verbindungen Polymetaselenoarsenit-Anionen [AsSe2-]∞ beinhalten, in denen die Grundelemente ψ-AsSe3-Tetraeder sind, die über gemeinsame Ecken zu unendlichen Ketten verknüpft sind. Für KAsSe2 und RbAsSe2 werden Vierer-, für CsAsSe2 Zweier-Einfachketten gefunden. Die Streckungseinheiten s betragen 3,157, 2,336 bzw. 3,378 Å. Die Beziehung zwischen Konformation von Metaselenoarsenitketten und Kationgröße wird erläutert.
    Additional Material: 3 Ill.
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 102-104 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Untersuchungen an A4BX6-Verbindungen. II. Strukturverfeinerung von Rb4PbBr6 und eine Bemerkung zur Existenz von „Rb4HgI6“ und „K4CdI6“Rb4PbBr6 wurde in einer Festkörperreaktion aus den binären Komponenten präpariert und die Struktur mit Einkristalldaten verfeinert (a = 1332,9(4), c = 1647,8(5) pm, R.Gr. R3c; K4CdCl6-Typ). Rb4HgI6 und K4CdI6 ließen sich nicht darstellen. Diese Ergebnisse werden im Zusammenhang mit dem Strukturfelddiagramm für A4BX6 Verbindungen diskutiert.
    Notes: Rb4PbBr6 was prepared by solid state reaction of the binary compounds and the structure refined with single crystal data (a = 1332.9(4), c = 1647.8(5) pm; space group R3c; K4CdCl6-type arrangement). Attempts to synthesize Rb4HgI6 and K4CdI6 were unsuccessful. The results are discussed on the basis of a structure field diagram for A4BX6 compounds.
    Additional Material: 1 Tab.
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  • 21
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 131-140 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of Pb5(GeO4)2SO4 and Pb5(GeO4)2CrO4, Two Lead Apatites with Vacant Halogen SitesPb5(GeO4)2SO4 (a = 1005.8; c = 741.6 pm) and Pb5(GeO4)2CrO4 (a = 1010.5; c = 742.8 pm) are hexagonal, space group P63/m, Z = 2 formula units. They crystallize with the apatite structure type. The halogen positions in the channels are not occupied. This pecularity is caused by the Pb2+ ions on the 6h positions. Their lone pairs of electrons are sterically active, being directed into the channels. The electron lone pairs of the Pb2+ ions of the 4f positions also show sterical effect.
    Notes: Pb5(GeO4)2SO4 (a = 1005,8; c = 741,6 pm) und Pb5(GeO4)2CrO4 (a = 1010,5; c = 742,8 pm) sind hexagonal, Raumgruppe P63/m, Z = 2 Formeleinheiten. Sie kristallisierten in der Apatitstruktur, wobei die Halogenlagen in den Kanälen nicht besetzt werden. Diese Besonderheit ist durch die Pb2+-Ionen auf der Lage 6h bedingt. Ihre freien Elektronenpaare sind stereochemisch wirksam und weisen in die Kanäle hinein. Auch bei den Pb2+-Ionen auf der Lage 4f ist ein stereochemischer Einfluß des freien Elektronenpaares erkennbar.
    Additional Material: 3 Ill.
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  • 22
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Untersuchungen an A4BX6-Verbindungen. III. ns2-Kationen als Bedingung für einen Strukturtyp und ihre Wechselwirkung in ternären Halogeniden vom Typ A4BX6 (A: In, Tl; B: Cd, Pb, Ge; X: Cl, Br, I)Wir diskutieren die Art der Wechselwirkung von Kationen mit ns2-Konfiguration in ternären Halogeniden des Formeltypes A4BX6 (A: In, Tl; B: Cd, Pb, Ge; X: Cl, Br, I), die im Tl4HgBr6-Typ kristallisieren. Wir berichten über Hochdruckexperimente 'an solchen A4BX6-Verbindungen und über röntgenographische Untersuchungen und Kristallstrukturverfeinerungen an Mischkristallen des Typs A′xA4-xBX6, in denen die ns2-Kationen teilweise durch solche mit Edelgaskonfiguration substituiert sind. Die Ergebnisse unserer Experimente zeigen, daß die ns2-Kationen diesen ungewöhnlichen Strukturtyp durch Polarisationseffekte stabilisieren und durch ihre größere Elektronegativität im Vergleich zu der von Alkaliionen von ähnlicher Größe.
    Notes: We discuss the interaction of ns2-type cations in ternary halides of the formula type A4BX6 (A: In, Tl; B: Cd, Pb, Ge; X: Cl, Br, I) crystallizing in a Tl4HgBr6-type arrangement. We report on high pressure experiments on such A4BX6 compounds and on x-ray studies and structure refinements of mixed crystals of the type A′xA4-xBX6, where cations A′ with a closed shell configuration partly substitute for the ns2-type A ions. The results of our experiments show, that ns2-type cations stabilize this unusual structure type by polarization effects and by their higher electronegativity as compared with alkali ions of comparable size.
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  • 23
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 123-130 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag2PdCl4, Crystal Structure and the Crystal Chemical Relation to the NaCl TypeAg2PdCl4 single crystals show orthorhombic symmetry with the space group Cmca (No. 64) and the lattice parameters a = 10.088(2), b = 8.051(5), c = 8.078(2) å, with 4 formular units per unit cell. The atomic arrangement of Ag2PdCl4 is explored by X-ray crystal structure analysis.Silver shows a distorted octahedral arrangement of chlorine atoms. Palladium forms typical, approximately square-planar PdCl4 groups. Ag2PdCl4 is a new variant of a partially occupied sodium chloride structure type.
    Notes: Die Kristallstruktur von Ag2PdCl4 wurde mit röntgenographischen Methoden an Einkristallen ermittelt. Ag2PdCl4 kristallisiert mit orthorhombischer Symmetrie: Cmca (No. 64), a = 10,088(2), b = 8,051(5), c = 8,078(2) å mit 4 Formeleinheiten pro Elementarzelle.Silber besitzt eine verzerrt oktaedrische Chlor-Nachbarschaft, während das Palladium annähernd quadratisch planare PdCl4-Gruppen bildet. Ag2PdCl4 stellt eine neue Variante einer teilbesetzten Natriumchloridstruktur dar.
    Additional Material: 6 Ill.
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  • 24
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 145-152 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Influence of Modification of γ-Alumina by Halides on the Acidic BehaviourThe influence of modification of γ-alumina by Cl and F on the acidic properties was studied by means of i.r. spectroscopic methods using ammonia as probe molecule. The measurements show a significant rise in Lewis acidity.
    Notes: Mittels IR-spektroskopischer Methoden wurde der Einfluß der Halogen-modifizierung auf das acide Verhalten von γ-Al2O3 im Hinblick auf dessen Verwendung als Träger in Reformingkatalysatoren untersucht. Als Sondenmolekül diente NH3. Die Messungen wiesen eine deutliche Verstärkung der Lewis-aciden Eigenschaften des modifizierten Al2O3 aus.
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 141-144 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 27Al-NMR-Untersuchungen der flüssigen Phasen während der Zeolithsynthese27Al-NMR-Untersuchungen der während der Synthese der Zeolithe A, X und Y vorliegenden flüssigen Phasen zeigen, daß der molekulare Aufbau und die Menge der in den wäßrigen Lösungen vorliegenden Alumosilicationen für den entstehenden Zeolithtyp charakteristisch ist. Die Zahl der gebildeten Si—O—Al-Bindungen und ihre Mannigfaltigkeit steigt mit steigendem SiO2-Gehalt der Lösungen. Diese Ergebnisse stützen die Vorstellung, daß die Synthese von Zeolithen unter Ausbildung definierter Alumosilicate über die Lösungsphase abläuft.
    Notes: 27Al n.m.r. spectroscopy of liquid phases obtained during zeolite A, X, and Y synthesis reveals that the amount and the type of the present soluble aluminosilicate anions is characteristic for the different zeolite type; the number of the formed Si—O—Al bonds and their variety increases with increasing content of SiO2. The results support the suggestion about the formation mechanism of zeolites via distinct aluminosilicate “precursors” in solution.
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  • 26
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 160-164 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 186. Studies on Salts of Pyruvic Acid. 1. Synthesis and Characterization of PyruvatesThe title compounds M[O2C—CO—CH3], where M = Na, K, NH4, Li = H2, Have been synthesized by neutralisation of pyruvic acid under different conditions.The pyruvates were characterized by means of electron absorption, infrared, nuclear magnetic resonance, and mass spectra.
    Notes: Die Titelverbindungen M[O2C—CO—CH3] mit M = Na, K, NH4, Li · H2O wurden durch Neutralisation der Pyruvinsäure unter verschiedenen Bedingungen synthetisiert.Die Charakterisierung der Pyruvate erfolgte mit Hilfe von Elektronenabsorptions-, Infrarot-, Kernresonanz- und Massenspektren.
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  • 27
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 153-159 
    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 Silicon-Sulphur Compounds. 52. Reaction of Trialkoxysilanethiols with Carboxylic Acids. Preparation and Hydrolysis of TrialkoxyacyloxysilanesThe series of trialkoxyacyloxysilanes have been prepared almost quantitatively from trialkoxysilanethiols (RO)3SiSH (R = i-Pr, s-Bu, s-n-Am, s-i-Am) by the reaction with carboxylic acids R′COOH (R′ = Alkyl or Ph). Kinetics of the acidolysis of (RO)3SiSH as well as hydrolysis of (RO)3SiOCOR′ were investigated and consequently the reaction mechanisms are proposed.
    Notes: Durch Umsetzung von Trialkoxysilanthiolen (RO)3SiSH (R = i-Pr, s-Bu, s-n-Am, s-i-Am) und Carbonsäuren R′COOH (R′ = Alkyl bzw. Ph) wurden fast quantitativ mehrere Trialkoxyacyloxysilane (RO)3SiOCOR′ erhalten. Die Kinetik dieser Acidolysereaktion von (RO)3SiSH wie auch der Hydrolysereaktion von (RO)3SiOCOR′ wurde untersucht und in der Folge die Reaktionsmechanismen formuliert.
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  • 28
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 79-86 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of Na6Cu2O6For the first time black single crystals of Na6Cu2O6 are obtained with a = 1094.8(1), b = 1203.6(1), c = 1638.1(2) pm, space group Cmca, Z = 12. Cu3+ is coordinated by four O2-. CuO4 groups are bound to planar, isolated Cu2O66- anions. Cu—O bond distances are between 181.6(3) and 186.4(4) pm and O—Cu—O bond angels in the range 84.0(1)° and 93.7(1)°. Effective Coordination Numbers, ECoN, Mean Fictive Ionic Radii, MEFIR, and the Madelung Part of Lattice Energy, MAPLE, are calculated.
    Notes: Erstmals wurden schwarze Einkristalle von Na6Cu2O6 mit a = 1094,8(1), b = 1203,6(1), c = 1638,1(2) pm, R. Gr. Cmca, Z = 12 dargestellt. Cu3+ ist planar von vier O2-umgeben. Je zwei CuO4-Gruppen sind zu planaren, isolierten Anionen Cu2O66- verknüpft. Die Abstände Cu—O liegen zwischen 181,6(3) und 186,4(4) pm, die Winkel O—Cu—O zwischen 84,0(1)° und 93,7(1)°. Die Effektiven Koordinationszahlen, ECoN, Mittleren Fiktiven Ionenradien, MEFIR, und der Madelunganteil der Gitterenergie, MAPLE, wurden berechnet.
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  • 29
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 70-78 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, I.R. and E.P.R. Spectra, and Crystal Structure of HPPh3[WOCl4(OPPh3)]Partial hydrolysis of the alkyne complex [WCl4(PhC≡CPh)]2 in the presence of triphenylphosphine and dichloromethane as oxidizing agent and solvent yields dark green crystals of the complex HPPh3[WOCl4(OPPh3)]. Attempts to prepare the compound directly by the reaction of WOCl3 with PPh3, OPPh3 and HCl in dichloromethane were unsuccessful.HPPh3[WOCl4(OPPh3)] was characterized by its i.r. and e.p.r. spectrum. As shown by a crystals structure determination (1835 independent, observed reflections, R = 0.056) the complex crystallizes monoclinically in the space group P21/n with four formula units per unit cell. The complex consists of HPPh3+ and [WOCl4(OPPh3)]- ions, in which the tungsten atom is in a distorted octahedral environment, surrounded by four equatorial chlorine atoms, by one axial oxygen atom (bond length WO = 172 pm), and by the oxygen atom of the OPPh3 molecule (WO = 206 pm).
    Notes: HPPh3[WOCl4(OPPh3)] entsteht in Form dunkelgrüner Kristalle bei der partiellen Hydrolyse des Diphenylacetylenkomplexes [WCl4(PhC≡CPh)]2 bei Anwesenheit von Triphenylphosphan und Dichlormethan als Oxidations- und Lösungsmittel. Versuche, die Verbindung aus WOCl3, PPh3, OPPh3 und HCl in Dichlormethan direkt herzustellen, mißlangen.HPPh3[WOCl4(OPPh3)] haben wir durch das IR- und das EPR-Spektrum charakterisiert. Nach der röntgenographischen Strukturanalyse (1835 unabhängige, beobachtete, beobachtete Reflexe, R = 5,6%) kristallisiert die Verbindung monoklin in der Raumgruppe P21/n mit vier Formeleinheiten pro Elementarzelle. Sie ist aus HPPh3+-Ionen und Anionen [WOCl4(OPPh3)]- aufgebaut, in denen das Wolframatom verzerrt oktaedrisch von vier äquatorial angeordneten Chloratomen und axial von einem terminalen O-Atom (Bindungsabstand WO = 172 pm) und von dem O-Atom des OPPh3-Moleküls (WO = 206 pm) umgeben ist.
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  • 30
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 105-115 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation by Sulfonamide Substituted ThionoligandsThionoligands containing arenesulfonamido or arenesulfonylhydrazido functions as a second donor group (STAT-, PST-, BPTS- and TPTH-, meaning of the abbreviations see text) form 1,2 complexes with nickel(II), cobalt(II), and zinc(II). The six-membered chelates M(STAT)2 (M = Co, Ni) are high-spin (\documentclass{article}\pagestyle{empty}\begin{document}$ \rm{S} \mathop {\rm N}\limits^ \ominus $\end{document} coordination). On the other hand no coordination of the RSO2N group is observed in the complexes M(PST)2 (M = Co, Mn, Fe), but the formation of a four membered ring including one nitrogen atom of the heterocycle. This statement is primarily based on a comparison with complexes of teh structurally related ligands PPT- and CPT- containing no \documentclass{article}\pagestyle{empty}\begin{document}$ \rm{RSO}_2 \mathop {\rm N}\limits^ \ominus $\end{document} groups. Evidently in the chelat Co(BPTS)2 the anionic RSO2N group is a weak bidentate donor.
    Notes: Thionoliganden, die Arensulfonylamido- bzw. Arensulfonylhydrazidofunktionen als zweite Donatorgruppen enthalten (STAT-, PST-, BPTS- und TPTH-, zur Bedeutung der Abkürzungen vgl. Text), bilden mit Nickel(II), Cobalt(II) und Zink(II) 1,2-Komplexe. Die Sechsringchelate M(STAT)2 (M = Co, Ni) gehören zum High-spin-Typ (\documentclass{article}\pagestyle{empty}\begin{document}$ \rm{S} \mathop {\rm N}\limits^ \ominus $\end{document})-Koordination. Dagegen erfolgt in den Komplexen M(PST)2 (M = Co, Mn, Fe) keine Koordination über die \documentclass{article}\pagestyle{empty}\begin{document}$ \rm{RSO}_2 \mathop {\rm N}\limits^ \ominus $\end{document} Funktionen sondern über ein Stickstoffatom des Pyrimidinrings (Bildung eines Chelatvierringes). Diese Aussage wird durch einen Vergleich mit Komplexen der strukturell verwandten Liganden PPT- und CPT- gestützt, die keine RSO2N-Gruppen enthalten. In dem Chelat Co(BPTS)2 koordiniert RSO2N- offenbar als zweizähliger anionischer Ligand mit schwacher Donatorwirkung. Die Charakterisierung der neuen Chelate erfolgt anhand der magnetischen Momente, der UV/VIS- und der ESCA-Spektren. Die vorliegenden und früheren Ergebnisse ermöglichen Aussagen über die Variabilität des RSO2N-Liganden: Normalerweise erfolgt die Koordination über den N-Ligator. Es ist aber auch eine Bindung über ein Sauerstoffatom, wenn dadurch ein stabiler Chelatsechsring gebildet werden kann, oder als zweizähliger anionischer Ligand geringer Donatorstärke möglich. Die art der Koordination des RSO2N-Liganden hängt vom Zentralatom ab. Bisher konnten keine Komplexe mit einer direkten koordinativen Bindung von \documentclass{article}\pagestyle{empty}\begin{document}$ \rm{RSO}_2 \mathop {\rm N}\limits^ \ominus $\end{document} an Eisen(II) oder Mangan (II) nachgewiesen werden.
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  • 31
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 96-104 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Structure Analyses of Iodocuprates (I). IX. Syntheses and Crystal Structures of Cs3Cu2I5 and RbCu2I3Cs3Cu2I5 and Rb∞1[Cu2I3] were prepared by the reaction of CsI or RbI with CuI in solution (acetonitrile or acetone) or by solid state reaction. The crystal structure analysis of Cs3Cu2I5 (orthorhombic, Pbnm, a = 1438.6(6), b = 1014.7(5), c = 1167.5(5) pm, Z = 4) shows, that the compound contains dinuclear anions Cu2I53- in which the I atoms are arranged to trigonal bipyramids; one CuI occupies one of the two I tetrahedral holes, the other a trigonal site of the neighbouring tetrahedron. Rb∞1[Cu2I3] (orthorhombic, Cmcm, a = 1070.6(7), b = 1338.3(8), c = 572.8(3) pm, Z = 4) is built up by CuI4 double chains; the compound is isomorphic with Cs∞1[Cu2I3].
    Notes: Cs3Cu2I5 und Rb∞1[Cu2I3] werden durch Umsetzung von CsI bzw. RbI mit CuI in Lösung (Acetonitril bzw. Aceton) oder durch Festkörperreaktion hergestellt. Die Kristallstrukturanalyse von Cs3Cu2I5 (orthorhombisch, Pbnm, a = 1438,6(6), b = 1014,7(5), c = 1167,5(5) pm, Z = 4) ergab, daß diese Verbindung zweikernige Anionen Cu2I53- enthält. Die Iodatome bilden eine trigonale Bipyramide mit einem CuI in einer der beiden Tetraederlücken. Das zweite CuI besetzt eine Dreiecksfläche des anderen Tetraeders. Im Rb∞1[Cu2I3] (orthorhombisch, Cmcm, a = 1070,6(7), b = 1338,3(8), c = 572,8(3) pm, Z = 4) liegen CuI4-Tetraederdoppelketten vor; die Verbindung ist isomorph mit CsCu2I3.
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  • 32
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 87-95 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 187. Studies on Salts of the Pyruvic Acid. 2. Crystal Structure of Potassium Pyruvate, Redetermination of the Structure of Sodium PyruvateThe title compounds M[O2C—CO—CH3], where M = Na and K, crystallize with Z = 4 in the monoclinic space group P21/n; cell dimensions see “Inhaltsübersicht”.The structure of the Na+ and K+ salt resp. has been determined from single crystal X-ray data measured at 20°C and refined to R's of 0.051 and 0.055 resp. (Rw = 0.055 and 0.057 resp.) for 1065 and 1308 resp. independent reflections.Both compounds are isostructural. The alkali metal ions are surrounded by seven oxygen atoms from five anions forming an irregular polyhedron.
    Notes: Die Titelverbindungen M[O2C—CO—;CH3] mit M = Na, K kristallisieren monoklin mit Z = 4 in der Raumgruppe P21/n; Na[O2C—CO—CH3] a = 21, 905(3) Å, K[O2C—CO—CH3] a = 22,027(2) Å, b = 5,269(1) Å, b = 5,835(2) Å, c = 3,671(1) Å, c = 4,004(4) Å, β = 91,34(2)°. β = 90,88(3)°. Für die Na+-bzw. K+-Verbindung wurde die Struktur aus bei 20°C vermessenen röntgenographischen Einkristalldaten unter Verwendung von 1065 bzw. 1308 symmetrieunabhängigen Reflexen bestimmt und bis auf Gütefaktoren von R = 0,051 bzw. 0,055 und Rw = 0,055 bzw. 0,057 verfeinert.Beide Verbindungen sind isostrukturell. Das jeweilige Alkalimetallion ist von sieben O-Atomen, die von fünf verschiedenen Anionen stammen, unregelmäßig koordiniert.
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  • 33
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 127-135 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Oxide Catalysts. XLV. Conversion of Aromatics on Dealuminated Zeolites ZSM-5The catalytic properties of zeolites ZSM-5 dealuminated by hydrochloric acid are investigated in the isomerization of m-Xylene, the disproportionation of toluene and in the alkylation of toluene with methanol. Besides the increase of the Si/Al ratio, the dealumination leads to an inversion of the Si/Al concentration gradient in crystallites, to a shift of acidity spectrum and consequently to a change in catalytic activity and selectivity.
    Notes: An säuredealuminierten HZSM-5-Proben werden die m-Xylen-Isomerisierung, die Toluendisproportionierung und die Toluenalkylierung mit Methanol untersucht. Die Säuredealuminierung bewirkt neben der Moduländerung eine Umkehr des Si/Al-Konzentrationsgradienten in den Zeolithkristalliten, eine Verschiebung des Aciditätsspektrums und damit eine Veränderung von Aktivität und Selektivität in den katalytischen Reaktionen.
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  • 34
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 167-172 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenyl Imidodiphosphate as Ligand in Fluoro Complexes. 1. Fluoro Complexes of TitaniumIn acetonitrile TiF4 reacts with tetraphenyl imidodiphosphate forming two tetrafluoro (I, II) and three trifluoro complexes (III, IV, V) as well as one difluorotitanium complex (VI). The difluoro complex VI is exclusively formed by sing an excess of the ligand. VI was isolated and analytically characterized. The constitution and configuration of the complexes are concluded from 19F and 31P n.m.r. data. The tetraphenyl imidodiphosphate is only bidentately bonded, i.e. as chelate or bridging ligand; in the substitution complexes III-VI it is coordinated as anion.
    Notes: TiF4 bildet mit Imidodiphosphorsäuretetraphenylester in CH3CN zwei Tetrafluoro- (I, II) und drei Trifluorokomplexe (III, IV, V) sowie einen Difluorotitan-Komplex (VI). Mit Ligandenüberschuß entsteht ausschließlich der Difluorokomplex, der isoliert und elementar-analytisch charakterisiert wurde. Die Konstitutions- und Konfigurationsaussagen zu den übrigen Komplexen basieren auf 19F- und 31P-NMR-Untersuchungen. Der Imidodiphosphorsäureestr ist in den Komplexen stets zweizähnig als Chelat- oder Brückenligand gebunden; in den Substitutions-komplexen III-VI ist er in seiner anionischen Form enthalten.
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  • 35
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 116-126 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Methyl Metal Bis(trimethylsilyl)amido Derivatives of Aluminium, Gallium, and ArsenicMeAl[N(SiMe3)2]2 (Me = CH3) has been prepared by the reaction of AlMe3 with HN(SiMe3)2 in a 1:2 molar ratio. The homologue Gallium compound (as well as the Aluminium derivative) is formed in good yields by the interaction of MeMcl2 (M = Al, Ga) with Li- and Na[N(SiMe3)2], respectively. MeAs[N(SiMe3)2]2 is formed by the reaction of AsCl3 and Na[N(SiMe3)2] in a 1:3 molar ratio. These colourless amido derivatives are monomeric in solution, they have been characterized by analyses, mass, n.m.r. (1H and 13C), and especially by i.r. and Raman spectra.
    Notes: MeAl[N(SiMe3)2]2 (Me = CH3) wurde durch Umsetzung von AlMe3 mit HN(SiMe3)2 im Molverhältnis 1:2 dargestellt. Die homologe Galliumverbindung (wie auch das Aluminiumderivat) bildet sich in guten Ausbeuten aus MeMCl2 (M =; Al, Ga) und Li- bzw. Na[N(SiMe3)2]. Schließlich entsteht MeAs[N(SiMe3)2]2 bei der Reaktion von AsCl3 mit Na[N(SiMe3)2] im Verhältnis 1:3. Diese farblosen Amidoderivate sind in Lösung monomer; sie werden elementar-analytisch, mit Hilfe der Massen- und NMR-Spektren (1H und 13C) sowie vornehmlich schwingungs-spektroskopisch (IR und Raman) charakterisiert.
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  • 36
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: mehrkernige Technetium-Cluster. I. Synthese, Kristall- und Molekularstruktur der Bromide achtkerniger prismatischer und sechskerniger oktaedrischer Cluster des TechnetiumsE werden die Synthese, Kristall- und Molekularstruktur erster Vertreter mehrkerniger Technetium-Cluster er Zusammensetzung: [Tc8Br4μ—Br8]Br. 2 H2O; [H(H2O)2][Tc8Br4μ—Br8]Br; [H(H2O)2]2[Tc8Br4μ—Br8]Br2; [H3O(H2O)3]2[Tc6Br6μ3—Br5]; [(C4H9)4N]2[Tc6Br6μ3—Br5]; [H3O(H2O)3]2[Tc6Br6μ3—Br5]. 4 H2O beschrieben. Diese Verbindungen unterscheiden sich in ihrem Bau wesentlich von bekannten Clustern anderer d-Elemente. Die Kristall- und Molekularstruktur von Hexabromotechnetiumsäure, (H3O)2TcBr6, ist untersucht worden.
    Notes: The synthesis, crystal and molecular structure of the first representatives of polynuclear technetium clusters are described. The composition of these clusters is: [Tc8Br4μ—Br8]Br. 2H2O; [H(H2O)2][Tc8Br4μ—Br8]Br; [H(H2O)2]2[Tc8Br4μ—Br8]Br2; [H3O(H2O)3]2[Tc6Br6μ3—Br5]; [(C4H9)4N]2[Tc6Br6μ3—Br5]; [H3O3]2[Tc6Br6μ3—Br5]. 4 H2O. It is shown that these clusters strongly differ in their structure from the known clusters of other d-elements. The crystal and molecular structure of hexabromotechetium acid (H3O)2TcBr6 is studied too.
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  • 37
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 48-59 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (Pentacarbonyl)tungsten Complexes of Diphosphanyl AcetylenesPreparation and properties of the following compounds are described: (Pentacarbonyl)tungsten complexes of diamidophosphoryl-diaminophosphanyl acetylenes (3, 4), of diamidothiophosphoryl-diaminophosphanyl acetylenes (5, 6) and of bis(diaminophosphanyl)-acetylenemethiodides (7, 8). Furthermore, the (pentacarbonyl)tungsten complexes of numerous halogenated diphosphanyl acetylenes have been prepared (15-21). All compounds are characterized by their n.m.r., i.r., and partly their mass spectra. Of (Pentacarbonyl)bis[bis(diethylamino)phosphanyl]acetylenemethiodide tungsten, 7, the molecular and crystal structures are reported.
    Notes: Darstellung und Eigenschaften der folgenden Verbindungen werden beschrieben: (Pentacarbonyl)wolfram-Komplexe von Diamidophosphoryl-diaminophosphanyl-acetylenen (3, 4), von Diamidothiophosphoryl-diaminophosphanyl-acetylenen (5, 6) und von Bis(diaminophosphanyl)-acetylenmethiodiden (7, 8). Weiter wurden die (Pentacarbonyl)wolfram-Komplexe zahlreicher halogenierter Diphosphanyl-acetylene (15-21) dargestellt. Alle Verbindungen sind durch ihre NMR-, IR- und teilweise ihre Massenspektren charakterisiert. Von (Pentacarbonyl){bis[bis(diethylamino)phosphanyl]acetylenmethiodid}wolfram, 7, werden die Molekül- und Kristallstruktur mitgeteilt.
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  • 38
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 77-86 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of CsVHP3O10Hitherto unknown CsVHP3O10 crystallizes from melts prepared from Cs2CO3, V2O3 and H3PO4 (2 d at 350°C; cooling rate: 10°/h). Best yields were obtained at a molar ratio 1:1:3 of the components. According to an X-ray crystal structure determination (C2/c; a = 1208.7(5), b = 877.7(3), c = 894.4(3) pm, β = 110.76(3)°; Z = 4; R = 0.043) the title compound is a catena-triphosphate. Bond lengths and angles are compared to those of triphosphates investigated earlier.
    Notes: Vorher unbekanntes CsVHP3O10 kristallisiert aus Cs2CO3/V2O3/H3PO4-Schmelzen (2 d bei 350°C, Abkühlrate: 10°/h). Optimale Ausbeuten werden bei einem molaren Verhältnis der Komponenten von 1:1:3 erzielt. Nach der Kristallstrukturanalyse (C2/c; a = 1208,7(5), b = 877,7(3), c = 894,4(3) pm, β = 110,76(3)°; Z = 4; R = 0,043) liegt ein catena-Triphosphat vor. Die Bindungslängen und -winkel im Anion werden mit denjenigen früher untersuchter catena-Triphosphate verglichen.
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  • 39
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 69-76 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Note on the Structure of A2[HgO2] (A = K, Rb), Rb2 [NiO2], and Rb1.4K0.6[NiO2]Single crystals of K2[HgO2] (I), Rb2[HgO2] (II), Rb2[NiO2] (III) and Rb1,4K0,6[NiO2] (IV) have been prepared [mercurates: colourless; niccolates: dichroitic ambercoloured/green (III) resp. yellow/green (IV)] mid characterized by X-riay single crystal methods. They crystallize tetragonally in the Na2[HgO2]-type of structure (space group I4/mmm, Z = 2) with I: a = 392.0(1), c = 1397.4(3) pm; II: a = 413.9(1), c = 1423.9(2) pm; III: a = 416.6(1), c = 1314.6(2) pm; IV: a = 409.2(2), c = 1304.4(6) pm. The crystal structures have been refined (four circle diffractometer). The Madelung parts of lattice energy, MAPLE, effective coordination numbers, ECoN, these via mean fictive ionic radii, MEFIR, are calculated and discussed.
    Notes: K2[HgO2] (I) wurde erneut, Rb2[HgO2] (II), Rb2[NiO2] (III) sowie Rb1,4K0,6[SiO2](IV) erstmals in einkristalliner Form dargestellt und röntgenographisch untersucht. Kristalle der Mercurate sind farblos, jene der Niccolate dichroitisch bernsteinfarben/grün (III) bzw. gelb/grün (IV). Die Oxide kristallisieren tetragonal im Na2[HgO2]-Typ (Raumgruppe I4/mmm, Z = 2) mit I: a = 392,0(1), c = 1397,4(3) pm; II: a = 413,9(1), c = 1423,9(2) pm; III: a = 416,6(1), c = 1314,6(2) pm; IV: a = 409,2(2), c = 1304,4(6) pm. Die Strukturparameter wurden verfeinert (Vierkreisdiffraktometerdaten). Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet und diskutiert.
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  • 40
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Eigenschaften von Bariumchlorophosphat (Apatit)-Leuchtstoffen bei Aktivierung mit zweiwertigem EuropiumEine Reihe von europiumaktivierten Barium- bzw. Calciumchlorophosphaten wurde in Pulverform dargestellt. Diese Leuchtstoffe sind isomorphe Vertreter der hexagonalen Chlorapatite (Ba, Ca, Mg)10(PO4)6Cl2. Neben Röntgendiffraktogrammen wurden Anregungs- und Emissionsspektren der Lumineszenz bei Zimmertemperatur und bei tiefen Temperaturen (T ∽ 4 K) untersucht. Steigender Calciumanteil beeinflußt die Lumineszenzeigenschaften dieser festen Lösungen durch Veränderung des am Eu2+-Ion wirkenden Kristallfelds. Das Erscheinen einer neuen Emissionsbande mit höherem Ca2+-Gehalt bei tiefen Temperaturen deutet auf Einbau der Eu2+-Ionen auf zwei verschiedenen Ba-Plätzen, so daß zwei Arten von Lumineszenzzentren auftreten. Die Lumineszenz entsteht durch Übergänge von der 4f65d- zur 4f7-Konfiguration des Eu2+.
    Notes: A series of powder materials of barium and calcium chlorophosphate activated by divalent europium have been prepared. These luminophors are isomorphous representatives of the hexagonal chlorapatites (Ba, Ca, Mg)10(PO4)6Cl2. In addition to x-ray diffractograms, excitation and emission spectra of luminescence have been studied at room and low temperatures (T ∽ 4 K). An increasing calcium content affects the luminescence properties of the solid solutions by changing the crystal field acting upon the Eu2+ ion. The appearance of a new low-temperature emission band with higher Ca2+ content indicates that the Eu2+ ions substitute on two different barium sites thus forming two types of luminescent centres. The luminescence arises from transitions between 4f65d and 4f7 configurations of Eu2+.
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  • 41
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 87-94 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of CsM2P5O16 (M = V, Fe)Upon heating of mixtures composed of Cs2CO3, H3PO4 and V2O3(Fe2O3) to 〉600°C, melts were formed, from which the title compounds crystallized during slow cooling. They form as well from CsVHP3O10 (CsFeHP3O10) by condensation, besides (CsPO3)n. According to crystal structure determinations (Pn; for M = V: a = 753.79(7), b = 941.05(12), c = 1 017.29(12) pm, β = 111.16(9)°; for M = Fe: a = 752.99(17), b = 937.77(44), c = 1 020.90(18) pm, β = 111.02(1)°; Z = 2) the anionic part of both compounds consists of catena-pentaphosphate groups. Systematic variations in the P—O bond lengths are discussed.
    Notes: Durch Erhitzen von Gemengen aus Cs2CO3, H3PO4 und V2O3(Fe2O3) auf 〉600°C entstehen Schmelzen, aus denen bei langsamem Abkühlen die vorher unbekannten Titelverbindungen kristallisieren. Sie bilden sich auch bei der thermischen Kondensation von CsVHP3O10 (CsFeHP3O10), wobei als Nebenprodukt (CsPO3)n anfällt. Nach der Röntgenstrukturanalyse (Pn; für M = V: a = 753,79(7), b = 941,05(12), c = 1 017,29(12) pm, β = 111,16(;9)° für M = Fe: a = 752,99(17), b = 937,77(44), c = 1 020,90(18) pm, β = 111,02(1)°; Z = 2) handelt es sich um catena-Pentaphosphate. Die systematische Variation der P—O-Bindungslängen im Anion wird diskutiert.
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  • 42
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 95-100 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na2H3IO6, a Variant of the Marcasite StructureSingle crystals of Na2H3IO6 were grown for the first time. According to the results of an X-ray crystal structure determination(Pnnm; a = 469.7(3), b = 529.9(2), c = 1005.2(6) pm; Z = 2; 296 diffractometer data; RW = 0.051) iodine is in an octahedral coordination. Sodium is surrounded by six oxygen in a strongly distorted octahedral arrangement. IO6 and NaO6 groups are linked via common vertices and edges in the sense of the rutile or marcasite type of structure. The corresponding structural relationship is discussed.
    Notes: Erstmals wurden Einkristalle von Na2H3IO6 erhalten. Nach der Röntgen-strukturanalyse (Pnnm; a = 469,7(3), b = 529,9(2), c = 1005,2(6) pm; Z = 2; 296 Diffraktometerdaten, RW = 0,051) ist Iod oktaedrisch und Natrium stark verzerrt oktaedrisch von Sauerstoff koordiniert. Die Verknüpfung der Oktaeder erfolgt im Sinne der Rutil- bzw. Markasitstruktur; die entsprechende Strukturverwandtschaft wird diskutiert.
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  • 43
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    Zeitschrift für anorganische Chemie 567 (1988), S. 122-130 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR-Untersuchungen an Stannabicycloundecanen des Typs RSn(CH2CH2CH2)3NEs werden 1H-, 13C- und 119Sn-NMR-Daten von sieben Stannabicycloundecanen des Typs RSn(CH2CH2CH2)3N (1, R = Cl; 2, R = Br; 3, R = I; 4, R = OH; 5, R = SPh; 6, R = Me; 7, R = Sn(CH2CH2CH2)3N) mitgeteilt. Aus den Protonen-NMR-Koaleszenzdaten bei tiefer Temperatur wird ΔGTc* für die Racemisierung des Bicyclo[3.3.3]-Gerüstes zu 37 ± 1 kJ/mol bestimmt. Die Werte sind unabhängig vom Substituenten R. In den entsprechenden Siliciumderivaten (R = Me) werden geringere Aktivierungsparameter gefunden.
    Notes: The 1H, 13C, and 119Sn NMR data of seven stannabicycloundecanes of the type RSn(CH2CH2CH2)3N (1, R = Cl; 2, R = Br; 3, R = I; 4, R = OH; 5, R = SPh; 6, R = Me; 7, R = Sn(CH2CH2CH2)3N) are reported. From 1H NMR coalescence data at low temperature the free activation enthalpies for the racemisation of the bicyclo[3.3.3]skeleton were estimated to be 37 ± 1 kJ/mol. They are independent of the substituent R. However, it decreases when the tin atom is replaced by silicon for R = Me.
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  • 44
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Monohalogenobenzoylhydrazone. V. Spektroskopische Untersuchungen und Bindungs-verhältnisse einiger neuer Antimon(III)-Komplexe von p-Chlorobenzoyl-di-(2-pyridyl)-ketohydrazon mittels experimenteller und quantenchemischer MethodenBei der Reaktion von Antimon(III)-chlorid, -bromid und -iodid mit dem p-Chlorobenzoylhydrazon des Di-(2-pyridyl)keton (DpClBHH) in methanolischer Lösung werden Komplexe des Typs SbX2(DpClBH) erhalten. Die Struktur dieser Verbindungen wird an Hand der spektroskopischen Daten diskutiert. Der Ligand koordiniert dreizähnig über die Carbonyl- und Azomethin-Gruppe sowie über den Stickstoff der Pyridyl-Gruppe. Eine verzerrt oktaedrische Koordination des Metalls wird vorgeschlagen. EH-MO-Rechnungen wurden zur Analyse der Elektronen-spektren und der Bindungsverhältnisse herangezogen. Weiterhin dienen Grenzorbital-Betrachtungen aus CNDO/2-Rechnungen zur Klärung der Metall-Liganden-Bindung.
    Notes: Reactions of antimony(III) chloride, bromide, and iodide with p-chlorobenzoylhydrazone of di-(2-pyridyl)ketone (DpClBHH) in methanolic solutions afford the complexes SbX2(DpClBH). The structures of the new compounds are discussed in relation to their spectroscopic properties. In these complexes the ligand behaved as terdentate, coordination occuring through the carbonyl and azomethine groups, as well as the nitrogen atom of the pyridyl group. Consequently, a distorted octahedral environment around the metal is proposed. Moreover, EHMO calculations have been used in the analysis of the bonding in the SbCl2(DpClBH) complex, as well as to interpret the electronic spectral data. In addition, CNDO/2 calculations performed on the aforesaid ligand have been used to throw light on the mode of attachment of the ligand to the metal ion by means of some quantum-chemical indices related to the frontier MO's.
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  • 45
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    Zeitschrift für anorganische Chemie 567 (1988), S. 173-178 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mössbauer Studies of Thiospinels. VII. The System Cd0.9Fe0.1Cr2(SxSe1-x)4In order to investigate the influence of mixed anions on 57Fe-Mössbauer spectra of thiospinels with tetrahedral FeII polycrystalline samples of the spinel system Cd0.9Fe0.1Cr2(SxSe1-x)4 have been prepared in the range 0.22 ≤ x ≤ 1. Room temperature Mössbauer spectra consist of several overlapping doublets of almost identical isomer shifts but different quadrupole splittings. The FeII-doublets are attributed to the five different coordination polyhedras S4, S3Se, S2Se2, SSe3, and Se4.
    Notes: Um den Einfluß eines gemischten Anionengitters auf die 57Fe-Mößbauer-Spektren von Thiospinellen mit tetraedrischem FeII zu untersuchen, wurden von dem spinell-system Cd0,9Fe0,1Cr2(SxSe1-x)4 im Bereich 0,22 ≤ x ≤ 1 polykristalline Proben hergestellt. Die Raumtemperatur-Mößbauer-Spektren der Spinellmischkristalle bestehen aus mehreren überlappenden Dubletts nahezu gleicher Isomerieverschiebung aber verschiedener Quadrupolaufspaltung. Die FeII-Dubletts können den Koordinationspolyedern S4, S3Se, S2Se2, SSe3 und Se4 zugeordnet werden.
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  • 46
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    Zeitschrift für anorganische Chemie 567 (1988), S. 145-152 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Characterization of Non-Framework Aluminium in Zeolites Y by the Ferron MethodBy using the ferron method it is shown that the non-framework aluminium occuring in dealuminated zeolites Y exists in form of different kinds of Al-oxo-hydroxo-species. At the beginning of dealumination (673 K) besides polymeric species with relatively low degree of polymerization monomeric and a special kind of oligomeric cations occur. These special cations alter into a mixture of oligomeric species with increasing temperature of dealumination (813 K). Simultaneously the degree of polymerization of the polymeric species increases.
    Notes: Mit der Ferronmethode wird gezeigt, daß das in thermisch behandelten Y-Zeolithen auftretende Extragitter-Aluminium aus unterschiedlichen Arten von Al-oxo-hydroxo-Spezies besteht. Am Anfang der Dealuminierung (673 K) liegen neben monomeren spezielle oligomere Kationen vor; gleichzeitig werden aber auch polymere Spezies mit relativ niedrigem Polymerisationsgrad gebildet. Mit steigender Temperatur der thermischen Behandlung (813 K) entsteht aus den oligomeren Teilchen ein Gemisch niedermolekularer Kationen. Die polymeren Spezies unterliegen dabei einer Veränderung im Sinne einer zunehmenden Kondensation bzw. Polymerisation.
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  • 47
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    Zeitschrift für anorganische Chemie 565 (1988), S. 47-53 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 188. Preparation and Properties of Esters of Dithiopropionic AcidThe orange colored title compounds C2H5—CS—SR with R = CH3, C2H5, C(CH3)3, and CH2—C6H5 have been prepared in one-pot synthesis by reaction of ethyl bromide with magnesium followed by CS2 insertion and alkylation with the corresponding alkyl halide. Their electron absorption, infrared, nuclear magnetic resonance, and mass spectra are communicated.
    Notes: Die orangefarbene Titelverbindungen C2H5—CS—SR mit R = CH3, C2H5, C(CH3)3 und CH2—C6H5 wurden im Eintopfverfahren durch Umsetzung von Ethylbromid mit Magnesium, anschließender CS2-Insertion und Alkylierung mit dem entsprechenden Alkylhalogenid hergestellt. Ihre Elektronenabsorptions-, Infrarot-, Kernresonanz- und Massenspektren werden mitgeteilt.
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  • 48
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    Zeitschrift für anorganische Chemie 565 (1988), S. 34-40 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Unusual System of Hydrogen Bonds in Rubidium Hydroxide Dihydrate, RbOH · 2 H2ORbOH · 2H2O was obtained by the reaction of Rb with H2O and dehydration of the resulting solution by concentrated sulfuric acid. The compound melts at 310 K. The structure was determined by X-ray single crystal methods: The H positions of H2O were found. The structure consists of a threedimensional H-bonded network of H2O molecules and OH-ions. Hydroxide ions are acceptors for four protons of four adjacent water molecules with d(O—O) = 2×2.59 Å and 2×2.82 Å. Oxygen of OH-ions is disordered over a distance of 1.27 Å. Rb has 8 H2O molecules as nearest neighbours, d(Rb—O) = 3.03 Å to 3.07 Å, OH-ions are further removed with d(Rb—O) ≥ 3.45 Å.
    Notes: RbOH · 2H2O wird durch Umsetzung von Rb mit H2O und Entwässern der entstehenden Lösung über konzentrierter H2SO4 erhalten. Die Verbindung schmilzt bei 310 K. An Einkristallen wurde ihre Struktur röntgenographisch bestimmt: Die H-Lagen an den H2O-Molekülen konnten ermittelt werden. Die Struktur zeigt ein brückengebundenes Gerüst von H2O-Molekülen und OH--Ionen. Die Hydroxidionen dienen als Akzeptoren für je ein Proton von vier benachbarten H2O-Molekülen mit d(O—O) = 2×2,59 Å und 2×2,82 Å. Der Sauerstoff des OH--Ions ist fehlgeordnet mit einem Abstand von 1,27 Å. Rb hat 8 H2O-Moleküle als nächste Nachbarn, d(Rb—O) = 3,03 bis 3,07 Å, OH--Ionen sind weiter entfernt mit d(Rb—O) ≥ 3,45 Å.
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  • 49
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    Zeitschrift für anorganische Chemie 565 (1988), S. 54-66 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of M1—LnTa3O9 (Ln = Pr, Nd), X-Ray and Electronmicroscopical InvestigationsNew ternary compounds M1—LnTa3O9 (Ln = Pr, Nd) could be prepared by chemical transport reaction in a temperature gradient T2 → T1 (T2 = 1100°C; T1 = 1000°C; CI2 as transport agent). M1 NdTa3O9 crystallizes in the monoclinic space group P 21/m with a = 5.3840(9) Å, b = 7.550(1) Å, c = 8.1911(9) Å and β = 92.46(1)°. The structure was refined to give R = 6.29% and Rw = 6.20%. It is built of double and single chains of corner-sharing TaO6 octahedra extended along the b-axis. Tunnels running along [010] are created by the framework of TaO6 octahedra. Ln (Ln = Pr, Nd) is located in these tunnels to levels of y = 1/4 and 3/4. A structure refinement for isostructural M1—PrTa3O9 led to a = 5.4051(7) Å, b = 7.5680(2) Å, c = 8.1964(9) Å, β = 92.38(2)° and R = 7.72%, Rw = 7.57%. By grinding in an agate mortar M1—LnTa3O9 transforms into M2—LnTa3O9, a new modification with a higher density.High resolution transmission electron microscopy images of the M1—PrTa3O9 structure were made along the [010] direction. They could be interpreted by comparing them with images calculated on the basis of the multi-slice method.
    Notes: Durch chemischen Transport im Temperaturgefälle T2 → T1 (T2 = 1100°C; T1 = 1000°C) mit dem Transportmittel Chlor (p(Cl2; 20°C) = 1 atm) wurden die neuen Verbindungen M1—LnTa3O9 (Ln = Pr, Nd) erhalten. Die Strukturbestimmung über Einkristalldaten ergab für M1—NdTa3O9: RG P21/m;a = 5,3840(9) Å, b = 7,550(1) Å, c = 8,1911(9) Å, β = 92,46(1)°; Z = 2; R = 6,29%, Rw = 6,20%. Es liegen TaO6-Oktaeder vor, die allseitig über Ecken miteinander verknüpft und zum Teil auch über Kanten zu Oktaederpaaren verbunden sind. In Richtung [010] wechseln sich Oktaeder und Oktaederpaare ab. In den längs b verlaufenden Kanälen zwischen den Oktaederpaaren befinden sich die Nd-Teilchen. Die Strukturverfeinerung am isotypen M1—PrTa3O9 führte zu den Gitterkonstanten a = 5,4051(7) Å, b = 7,5680(2) Å, c = 8,1964(9) Å, β = 92,38(2)° und R = 7,72%, Rw = 7,57%.Beim Zerreiben der Kristalle von M1—LnTa3O9 (Ln = Pr, Nd) erfolgt eine tribochemische Umwandlung in eine weitere neue Modifikation M2—LnTa3O9 mit signifikant höherer Dichte.Von M1—PrTa3O9 konnten hochaufgelöste elektronenmikroskopische Durchstrahlungsaufnahmen längs [010] erhalten werden. In Übereinstimmung mit der rechnerischen Kontrastsimulation sind die unbesetzten Kanäle bei einem Defokus von -1150 Å deutlich als heller Kontrast erkennbar.
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  • 50
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 67-80 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of New CeTa3O9 ModificationsThe modifications M—, O— and P—CeTa3O9 could be prepared by chemical transport reactions (T2 → T1; T2 = 1100°C; T1 = 1000°C) with chlorine as transport agent.M—CeTa3O9 crystallizes in the monoclinic space group C 2/m with a = 12.415(1) Å, b = 7.6317(8) Å, c = 6.5976(8) Å, β = 93.31(1)°; Z = 4; R = 4.88%, Rw = 3.67%. The structure consists of two types of Ta—O-polyhedra. Especially remarkable are chains of edge sharing pentagonal TaO7-bipyramids which are connected by TaO6-octahedra at opposite sides. Tunnels running along [010] are created by the framework of Ta—O-polyhedra and are filled with Ce in levels of y = 1/2 and y = 0.O—CeTa3O9 crystallizes orthorhombically with a = 6.5429(7) Å, b = 7.6491(7) Å, c = 12.583(1) Å and is isostructural to O—LaTa3O9 (space group: Pnma). O—CeTa3O9 contains the same characteristic structural units namely pentagonal TaO7-bipyramides and TaO6-octahedra. The difference between O— and M—CeTa3O9 is based on the orientation of the tunnels: in the orthorhombic modification they are arranged zigzag-like, in the latter parallel.Both modifications of CeTa3O9 can be irreversibly converted into the well-known perovskite-related P—CeTa3O9 structure with a lower density by heating in air to 1200°C.
    Notes: Durch chemischen Transport (T2 → T1; T2 = 1100°C; T1 = 1000°C) mit dem Transportmittel Chlor (p(Cl2; 298 K) = 1 atm) wurden Kristalle der neuen Modifikationen M— und O—CeTa3O9 sowie von der Perowskitvariante P—CeTa3O9 erhalten. Nach der Strukturbestimmung über Einkristalldaten ist M—CeTa3O9 monoklin (C 2/m) mit a = 12,415(1) Å, b = 7,6317(8) Å, c = 6,5976(8) Å, β = 93,31(1)°; Z = 4; R = 4,88%, Rw = 3,67%. Man erkennt aus kantenverknüpften pentagonalen TaO7-Bipyramiden bestehende Bänder längs c, die miteinander durch TaO6-Oktaeder verbunden sind. In den so gebildeten Kanälen sind die Cer-Teilchen lokalisiert.O—CeTa3O9 kristallisiert orthorhombisch mit a = 6,5429(7) Å, b = 7,6491(7) Å, c = 12,583(1) Å und ist nach Pulveraufnahmen isotyp mit der bereits näher untersuchten Verbindung O—LaTa3O9. Beide orthorhombischen Oxide sind wie M—CeTa3O9 durch ein Netzwerk kantenverknüpfter TaO7- und TaO6-Polyedern gekennzeichnet; in [010]-Richtung liegen nur Eckenverknüpfungen vor. Die TaO6-Oktaeder sind in der a—c-Ebene jeweils so angeordnet, daß die mit Ce (La) besetzten Kanäle bei O—CeTa3O9 zick-zack-förmig, bei M—CeTa3O9 parallel zueinander orientiert erscheinen.O— und M—CeTa3O9 zeigen beim Erhitzen (1200°C; an Luft) eine nicht reversible Umwandlung in die bekannte Perowskitmodifikation P—CeTa3O9 (Ce1/3TaO3) mit deutlich geringerer röntgenographischer Dichte.
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  • 51
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 106-110 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of NaRhO2For the first time black single crystals of NaRhO2 (from Li2O, NAO0,50 α-Rh2O3, Li: Na: Rh = 1,15:2.18:1, Pd-cylinder, 950°C, 18 d, in 18 d cooled down) have been prepared and investigated by X-ray. NaRhO2 crystallizes in the α-NaFeO2-type: a = 309.71(4), c = 1552,75(34) pm, c/a = 5.01, space group R3m, Z = 3; fourcircle diffractometer data (Philips PW 1100): 124 of 126 I0(hkl): AgKα; R = Rw = 3.44%). The Madelung Part of Lattice Energy, MAPLE, and peculiarities of this type of structure are discussed.
    Notes: Erstmals wurden schwarze Einkristalle von NaRhO2 (aus Li2O, NaO0,50 und α-Rh2O3, Li: Na: Rh = 1,15:2,18:1, Pd-Bömbchen, 950°C, 18 d, 18 d abgekühlt) dargestellt und röntgenographisch untersucht. NaRhO2 kristallisiert im rhomboedrischen α-NaFeO2-Typ: a = 309,71(4), c = 1552,75(34) pm, c/a = 5,01, Raumgruppe R3m, Z = 3; Vierkreisdiffraktometerdaten (Philips PW 1100): 124 von 126 I0(hkl); AgKα; R = Rw = 3,44%). Der Madelunganteil der Gitterenergie, MAPLE, und Charakteristika des Strukturtyps werden diskutiert.
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  • 52
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 81-90 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chloro-Fluro-Exchange by Halogenated 1.3-DisilazanesAminofluorosilance (1-4) are obtained in the reaction of difluorosilanes with lithiated amines. Disilazanes (5,6) are formed in the reaction of LiNH(C6H3-iPr2) with CMe3SiF3 and C6H5SiF3. Lithium salts of 1-4 are dimers in n-hexane (7-10) and LiF adducts of iminosilanes in THF (11-14). The latter react with chlorsilanes (RSiCl3, R = Cl, H, Me) to give the substituted compounds 15-21 and LiCl. An intermolecular F/Cl exchange occurs with 15-20 which depends on the temperature, the solvents and ligands. 22-27 are formed.
    Notes: Aminofluorsilance (1-4) werden durch die Reaktion der Difluorsilane mit lithiierten Aminen erhalten. CMe3SiF3 und C6H5SiF3 reagieren zu Disilazanen (5,6). Die Lithiumsalze von 1-4 bilden in n-Hexan Dimere (7-10) und in THF LiF-Addukte von Iminosilanen (11-14). Letztere reagieren mit Chlorsilanen (RSiCl3, R = Cl, H, Me) unter LiCl-Abspaltung und Substitution zu 15-21 . 15-20 unterliegen einem intermolekularen F/Cl-Austausch, der temperatur-, lösungsmittel- und substituentenabhängig ist. Es entstehen 22-27 .
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  • 53
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 91-105 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfur Dioxide as Ligand and Synton. VII. Phosphane Sulfur Dioxide Nickel (0) and Palladium (0) ComplexesSynthesis and properties of phosphane sulfur dioxid d10-metal complexes of the types ML2(SO2)2, ML2(SO2), and ML3(SO2) (M = Ni(0), Pd(0); L = t-phosphane) are described. In dependence on the phosphane coligands nickel(0) complexes with η1-planar, η1-pyramidal and η2-S.O. (side on) coordinated SO2 are formed. In the case of the palladium(0)-SO2 complexes hithero prepared the dominating coordination mode is the η1-pyramidal one.
    Notes: Synthese und Eigenschaften von Phosphan-Schwefeldioxid-d10-Metallkomplexen der Typen ML2(SO2)2, ML2(SO2) und ML3(SO2) (M = Ni(0), Pd(0); L = t-Phosphan) werden beschrieben. In Abhängigkeit der Phosphan-Coliganden entstehen Nickel(0)-SO2-Komplexe mit η1-planar, η1-pyramidal und η2-S.O (side on) koordiniertem SO2. Dagegen dominiert im Falle der bislang dargestellten Palladium(0)-SO2-Komplexe die η1-pyramidale Koordinationsgeometrie.
    Additional Material: 5 Ill.
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  • 54
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations of the Anion Constitution in Mixtures of Diethyl-di(2-hydroxyethyl)ammonium and Triethyl-(2-hydroxyethyl)ammonium Silicate Solutions. Formation of Diethyl-di(2-hydroxyethyl)-/Triethyl- (2-hydroxyethyl)ammonium Silicate HydratesOrganoammonium silicate solutions with a molar ratio base to silicon dioxide of 2 to 1 (cSiO2 =.1 and 1.7 mol · kg-1) and 1 to 1 (cSiO2 = 2.5 mol · kg-1) have been investigated with various amount of diethyl-di(2-hydroxyethyl)- and triethyl-(2-hydroxyethyl)ammonium hydroxide. Double-three and double-four ring silicate ions have been found in all solutions by 29Si n.m.r. spectroscopy. The amount of double-four ring species increases with increasing amount of diethyl-di-(2-hydroxyethyl)ammonium hydroxide. The substances crystallized are organoammonium double-four ring silicate hydrates, in which both of the mentioned base cations are present.
    Notes: Untersucht werden Organoammoniumsilicatlösungen mit einem molaren Verhältnis Base zu Siliciumdioxid von 2 zu 1 (SiO2-Konzentration von 1,1 und 1,7 mol · kg-1) und 1 zu 1 (SiO2-Konzentration von 2,5 mol · kg-1), wobei als Basekomponente unterschiedliche Anteile an Diethyl-di(2-hydroxyethyl)- und Triethyl-(2-hydroxyethyl)ammoniumhydroxid vorliegen. In allen Lösungen werden 29Si-NMR-spektroskopisch Doppeldreiring- und Doppelvierringsilicationen nachgewiesen, der Gehalt an Doppelvierringspezies erhöht sich mit steigendem Anteil an Diethyl-di(2-hydroxyethyl)ammoniumhydroxid. Auskristallisierende Substanzen sind Organoammonium-Doppelvierring-Silicathydrate, in denen stets beide Basekationen nebeneinander vorliegen.
    Additional Material: 4 Ill.
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  • 55
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 127-136 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Verbindungsbildung im System TeO2—Ta2O5Drei Verbindungen existieren im System TeO2—Ta2O5: 3TeO2 · Ta2O5 (tetragonal), 2TeO2 · Ta2O5 (tetragonal und orthorhombisch) und TeO2 · 3Ta2O5 (orthorhombisch). Es wird gezeigt, daß die bisher als 7TeO2 · 3Ta2O5 und 2TeO2 · Ta2O5 (Hochtemperaturform) bezeichneten Verbindungen die stabilen Modifikationen von 2TeO2 · Ta2O5 (orthorhombisch) bzw. TeO2 · 3Ta2O5 sind.
    Notes: Three compounds exist in the system TeO2—Ta2O5: 3TeO2 · Ta2O5 (tetragonal), 2TeO2 · Ta2O5 (tetragonal and orthorhombic), and TeO2 · 3Ta2O5 (orthorhombie). The compounds previously denoted as 7TeO2 · 3Ta2O5 and 2TeO2 · Ta2O5 (high-temperature form) are shown to be stable modifications of 2TeO2 · Ta2O5 (orthorhombie) and TeO2 · 3Ta2O5, respectively.
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  • 56
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cobalt Chelates as Hydrogenation Catalysts. VI. Spectrophotometric Investigation of the Adduct Formation of [Co(dpnH)]+ with PyridineThe investigation of the adduct formation of the [Co(dpnH)]+ complex with pyridine by spectrophotometric measurements causes some difficulties due to the unfavourable overlapping of the spectra of the starting complex, the mono- and the bis-adduct in the spectral range used (17000-32000 cm-1). Therefore, the adduct formation constant β2 can only be determined, if the waveleagths for the evaluation of the data are suitably selected. The thermodynamic parameters, calculated from the temperature dependence of β1 (δRH° = -9.1 ± 0.5 kJ · mol-1, δRS° = -5.6 ± 1.7 J · mol-1 · K-1), differ clearly from those which have been obtained from kinetic measurements [3]. The reason for this difference, which is quite beyond the error limit of the applied methods, is most probably the neglect of analogous adduct equilibria with the solvent.
    Notes: Die Untersuchung der Adduktbildung des [Co(dpnH)]+-Komplexes mit Pyridin durch spektralphotometrische Messungen bereitet Schwierigkeiten, da sich die Spektren des Ausgangskomplexes, des Mono- und des Bis-Addukts im untersuchten Spektralbereich (17000-32000 cm-1) ungünstig überlagern. Die Adduktbildungskonstante β2 läßt sich daher nur ermitteln, wenn die Wellenzahlen für die Auswertung der Messungen geeignet ausgewählt werden. Die aus der Temperaturabhängigkeit von β1 berechneten thermodynamischen Parameter (δRH° = -9,1 ± 0,5 kJ · mol-1, δRS° = -5,6 ± 1,7 J · mol-1 · K-1) unterscheiden sich jedoch deutlich von den Werten, die durch kinetische Messungen [3] bestimmt worden sind. Ursache für diese, weit außerhalb der Fehlergrenze der Methoden liegenden Differenzen ist sehr wahrscheinlich die Vernachlässigung von analogen Adduktgleichgewichten mit dem Lösungsmittel.
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  • 57
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 154-162 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About the Chemistry of the Oxidation of Gaseous Mixtures of C2F3Cl3, SiCl4, GeCl4, and POCl3 at High TemperaturesThe formation of gaseous compounds during the oxidation of gaseous mixtures of C2F3Cl3, SiCl4, POCl3, and GeCl4 within a reactor of quartz glass was investigated in the temperature range from 1273 to 2223 K by infrared spectroscopy in the effluent gases. At the low temperature CO, COF2, COFCl, and CF4 are formed as intermediates, which react in contact with SiO2 at higher temperatures to the stable final products CO2, Cl2, SiF4, POF3, and GeF4. The dependence of these reactions on temperature and the velocity of the gases is discussed.
    Notes: Die bei der Oxydation von gasförmigen Gemischen von C2F3Cl3, SiCl4, POCl3 und GeCl4 im Temperaturbereich von 1273 bis 2223 K im Quarzglasreaktor entstehenden Verbindungen werden in den Abgasen IR-spektroskopisch untersucht. Danach entstehen bei der tiefen Temperatur als Zwischenprodukte CO, COF2, COFCl und CF4, die bei der hohen Temperatur unter Wechselwirkung mit SiO2 in die Endprodukte CO2, Cl2, SiF4, POF3 und GeF4 übergeführt werden. Die Abhängigkeit dieser Reaktionen von Temperatur und Strömungsgeschwindigkeit wird diskutiert.
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  • 58
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 147-153 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Thermal Analysis, and X-Ray Crystal Structure of [Ni(NH3)6][S(O)C=C(CN)2] · 1.5 H2O, a Salt with the Nickel (II) Hexammine CationThe compound [Ni(NH3)6][S(O)C=C(CN)2] · 1.5 H2O is obtained by reaction of solutions of nickel acetate tetrahydrate in ammonia and K2[S(O)C=C(CN)2] · H2O in water. The salt crystallizes with the monoclinic space group P 21/a. The lattice constants are a = 15.183(1), b = 13.084(1), c = 14.386(1) Å, β = 100.96(7)° and Z = 8.The X-ray structure revealed two crystallographically independent nickel hexammine cations besides pseudochalcogenolate anions. The latter are associated with water molecules and exhibit strong delocalized π-electron systems.The thermal decomposition proceeds in three different steps. The first and second step refer to evolution of ammonia while in a third step H2O is squeezed out. This results in a decomposition of the substance.
    Notes: Die Verbindung [Ni(NH3)6][S(O)C=C(CN)2] · 1,5H2O ist durch Reaktion einer ammoniakalischen Lösung von Nickelacetat-Tetrahydrat mit K2[S(O)C=C(CN)2] · H2O, gelöst in Wasser, zugänglich. Das Salz kristallisiert monoklin mit der Raumgruppe P 21/a. Die Gitterkonstanten betragen a = 15,183(1), b = 13,084(1), c = 14,3886(1) Å, β = 100,96(7)° und Z = 8.Nach der Röntgenstrukturanalyse (R = 0,07, Rw = 0,06 für 1109 beobachtete Reflexe) liegen jeweils zwei kristallographisch verschiedene Nickelhexamminkationen neben Pseudochalkogenoanionen vor. Letztere sind ausschließlich mit Hydratwassermolekülen assoziiert und weisen mit ihren Bindungslängen auf stark delokalisierte π-Elektronensysteme hin.Die thermogravimetrische Analyse zeigt einen stufenförmigen Abbau der Solvensmoleküle, wobei zunächst in zwei Schritten Ammoniak entweicht. Der Abspaltung des Hydratwassers schließt sich die Zersetzung der Substanz an.
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  • 59
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 171-180 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and I.R. Spectroscopic Investigations of SilylaminosilanesThe silylaminosilanes Me3-n(Me3SiNH)nSiH (n = 1-3) and (RMe2SiNH)3SiH were prepared by coammonolysis of dimethylorganochlorosilanes RMe2SiCl with chlorohydridosilanes Me3-nClnSiH (n = 1-3). The reaction of chlorohydridosilanes Me3-nClnSiH (n = 2,3) with hexamethyldisilzane yields the resp. silylaminosilanes Me3-n(Me3SiNH)nSiH(n = 2,3).The i.r. and 1H-n.m.r. data of the compounds are given and the relative basicity were measured by means of the V(C—D) band shift of CDCl3 associated to the silylaminosilanes. A dependence of the frequency of the Si—H stretching vibration and the number of trimethylsilylamino groups in Me3-n(Me3SiNH)nSiH and the substituents R in (RMe2SiNH)3SiH was found. All the methyl(silylamino)silanes Me3-n(Me3SiNH)nSiH show the same basicity, whereas the basicity of tris(dimethyl-organosilylamino)silanes is mainly determined by the steric effect of the substituents R.
    Notes: Die Silylaminosilane Me3-n(Me3SiNH)nSiH (n = 1-3) und (RMe2SiNH)3SiH (R = Et, n-Bu, Ph, C6H5CH2) wurden durch Coammonolyse der Dimethylorgano-chlorsilane RMe2SiCl mit den Chlorhydridsilanen Me3-nClnSiH (n = 1-3) dargestellt. Die Reaktion der Chlorhydridsilane Me3-nClnSiH (n = 2,3) mit Hexamethyldisilazan ergibt die entsprechenden Silylaminosilane Me3-n(Me3SiNH)nSiH (n = 2,3).Die IR- und 1H-NMR-Daten der Verbindungen sind angegeben, und die relative Basizität wurde gemessen an der Bandenverschiebung Δ∼ der V(C—D)-Bande des CDCl3 bei Assoziation an die Silyl-aminosilane. Die Bandenlage der Si—H-Valenzschwingung zeigt eine Abhängigkeit von der Anzahl der Trimethylsilylaminogruppen in den Me3-n(Me3SiNH)nSiH und den Substituenten R in den (RMe2SiNH)3SiH. Die Basizität der Methyl-silylamino-silane Me3-n(Me3SiNH)nSiH ist gleich, die der Tris-(dimethylorganosilylamino)-silane (RMe2SiNH)3SiH wird vorwiegend durch den sterischen Effekt der Substituenten R bestimmt.
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  • 60
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 192-192 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstracts.
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  • 61
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 566 (1988) 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 62
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 565 (1988), S. 163-170 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung, chemische und strukturelle Charakterisierung von Molybdän(III)- Wolfram (III)-Komplexen mit 1-(4-pyridyl)pyridinium als Kation(Py2)HMoCl5 · H2O wurde aus der salzsauren Lösung von (NH4)2MoCl5 · H2O dargestellt ((Py2)H2+ = 1-(4-pyridyl)pyridinium-Ion, C10N2H102+). Diese nichtreaktive, luftbeständige Verbindung, kristallisiert orthorombisch. Die Gitterkonstanten sind: a = 12,895(4), b = 6,914(2), c = 16,388(7) Å, Z = 4. Die Elementarzelle enthält MoCl5 · H2O2-- Oktaeder und (Py2)H2+. Die Abstände Mo—Cl betragen 2,406(3) bis 2,446(4) Å. Die Bindung Mo—O(H2O) beträgt 2,19(1) Å. Der Winkel zwischen zwei Pyridinringen des Kations ist 38°. Die Anionen bilden Schichten auf den Ebenen mit Z = 1/4 und Z = 3/4. Zwischen den Schichten be-finden sich die (Py2)H2+-Kationen.(Py2)MX4Py2-Komplexe (M = Mo, W; X = Cl, Br; Py = Pyridin) mit deprotoniertem (Py2)H2+ als Kation, wurden aus den Lösungen von (PyH)MX4Py2 in konz. Ammoniak-Lösung durch Zusatz von (Py2)HCl2 hergestellt. Alle vier Verbindungen kristallisieren triklin. Die Gitterkonstanten sind vergleichbar. Die Stabilität gegen Oxydation und Substitution kann man der geringen Löslichkeit der Substanzen zuschreiben.
    Notes: 1-(4-pyridyl)pyridinium ion (C10H10N22+, (Py2)H2+) precipitates from the hydrochloric acid solution of (NH4)2MoCl5 · H2O sparingly soluble (Py2)HMoCl5 · H2O. This unreactive, air stable compound crystallizes in the orthorhombic unit cell with a = 12.895(4), b = 6.914(2), c = 16.388(7) Å, Z = 4. The ionic structure contains octahedral MoCl5 · H2O2- and (Py2)H2+. The bond lengths Mo—Cl are between 2.406(3) to 2.446(4) Å. The bond length Mo—O(H2O) is 2.19(1) Å. Planar pyridine rings of the cation are rotated around the common axis by 38°. Anions are located in layers at Z = 1/4 and 3/4. Between the layers (Py2)H2+ cations are situated.(Py2)MX4Py2 (M = Mo, W; X = Cl, Br; Py = Pyridine) with deprotonated (Py2)H2+ are prepared from the solutions of (PyH)MoX4Py2 in aqueous ammonia to which (Py2)HCl2 was added. All four compounds crystallize in the triclinic crystal system. Unit cell dimensions are comparable. The stability of the compounds against oxidation and substitution could have its origin in the low solubility.
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  • 63
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    Zeitschrift für anorganische Chemie 566 (1988), S. 90-102 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Reactions of Methylene-bridged Phosphorus(III)-Phosphorus(V) CompoundsThe synthesis of methylene-bridged diphosphorus compounds of the type Y2PCH2P(S)X2 (with Y = F, Cl, OPri, NMe2, Ph) is reported. Reactions of these compounds with bicycloheptadiene-metaltetracarbonyls to form complexes of the type (L—L′)M(CO)4 and (L—L′)2M(CO)4, respectively, as well as some oxidation reactions and the conversion of the phosphine F2PCH2P(S)F2 to the cyclotetraphosphine [PCH2P(S)F2]4 are described.
    Notes: Über die Darstellung von methylenverbrückten Diphosphorverbindungen der Zusammensetzung Y2PCH2P(S)X2 (mit Y = F, Cl, OPri, NMe2, Ph; X = F, OPri, NMe2, Ph) wird berichtet. Umsetzungen der erhaltenen Verbindungen mit Bicycloheptadien-Metalltetracarbonylen zu Komplexen des Typs (L—L′)M(CO)4 bzw. (L—L′)2M(CO)4 (mit M = Cr, Mo, W), einige Oxidationsreaktionen und die Umwandlung des Phosphans F2PCH2P(S)F2 zum Cyclotetraphosphan [PCH2P(S)F2]4 werden beschrieben.
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  • 64
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    Zeitschrift für anorganische Chemie 566 (1988), S. 103-110 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. IX. Trimethyl(dimesylamino)stannane: Solid State Structure and Reactions with Covalent ChloridesTrimethyl(dimesylamino)stannane, (CH3)3SnN(SO2CH3)2, is prepared from (CH3)3SnOH and HN(SO2CH3)2 in aqueous solution or from (CH3)3SnCl and AgN(SO2CH3)2 in acetonitrile. It crystallizes in the monoclinic space group Ce. In the crystal structure the Sn atoms are linked by bridging (CH3SO2)2N groups to form infinite zigzag chains in the direction of the b axis. Each Sn atom is surrounded by three C atoms and two O atoms of different mesyl groups in a strongly distorted trigonal bipyramidal arrangement. The approximately linear OSnO group (O—Sn—O angle 172.9°) is not perpendicular to the equatorial plane of the Sn atom; the O—Sn—C angles are in the range from 66.4 to 116.1°. The Sn—O distances amount to 227.5 and 230.1 pm. The very short S—N distances (159.6 and 162.3 pm) and the large S—N—S angle (116.1°) are consistent with (p—d)π interactions between nitrogen and sulfur. The compound is cleaved quantitatively by methane- and ethanesulfonyl chorides, benzoyl chlorides, hydrogen chloride, and chlorine, yielding (CH3)3SnCl and trisulfonyl amines, N-benzoyl dimesylamine, dimesylamine, and N-chloro dimesylamine, respectively.
    Notes: Trimethyl(dimesylamino)stannan, (CH3)3SnN(SO2CH3)2, wird aus (CH3)3SnOH und HN(SO2CH3)2 in Wasser oder aus (CH3)3SnCl und AgN(SO2CH3)2 in Acetonitril erhalten. Es kristallisiert monoklin in der Raumgruppe Cc. In der Kristallstruktur sind die Sn-Atome über (CH3SO2)2N-Brücken zu unendlichen Zick-Zack-Ketten in Richtung der b-Achse verknüpft. Jedes Sn-Atom ist von drei C-Atomen und zwei O-Atomen verschiedener Mesylgruppen in einer stark verzerrten trigonal-bipyramidalen Anordnung umgeben. Die nahezu lineare OSnO-Gruppe (O—Sn—O-Winkel 172,9°) steht nicht senkrecht auf der Äquatorebene des Sn-Atoms; es treten O—Sn—C-Winkel von 66,4 bis 116,1° auf. Die Sn—O-Abstände betragen 227,5 und 230,1 pm. Die sehr kurzen S—N-Abstände von 159,6 und 162,3 pm sowie der große S—N—S-Winkel von 116,1° deuten auf (p-d)π-Wechselwirkungen zwischen Stickstoff und Schwefel. Die Verbindung wird durch Methan-und Ethansulfonylchlorid, Benzoylchlorid, Chlorwasserstoff bzw. Chlor quantitativ unter Bildung von (CH3)3SnCl und Trisulfonylaminen, N-Benzoyl-dimesylamin, Dimesylamin bzw. N-Chlor-dimesylamin gespalten.
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  • 65
    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 Silicon-Sulfur Compounds. 50. Bis(triorganoxysilyl)-polysulfides and the Structure of Bis(tri-tert-butoxysilyl)disulfideDisilylated polysulfides (RO)3SiSnSi(OR)3, R = i-Pr, tert-Bu, 2,6-Me2C6H3, n = 2-5, were obtained by reaction of (RO)3SiSNa with I2 or SnCl2, respectively. The reaction of [(t-BuO)3Si]2S2 with Ph3SiH yielded the mixed sulfide (t-BuO)3SiSSiPh3 and with Ph3P or Bu3P, by extrusion of one sulfur atom, the [(t-BuO)3Si]2S. The X-ray crystal structure of [(t-BuO)3Si]2S2 was determined. The S—S bond length is 209,2 pm, Si—S 213,2 pm. The mean value of the Si—S—S angle is 100,7°, and the torsion angle Si—S—S—Si -127,6°.
    Notes: Disilylierte Polysulfide (RO)3SiSnSi(OR)3, R = i-Pr, t-Bu, 2,6-Me2C6H3, n = 2-5, wurden durch Reaktion von (RO)3SiSNa mit I2 bzw. SnCl2 dargestellt. Die Umsetzung von [(t-BuO)3Si]2S2 mit Ph3SiH liefert ein gemischtes Sulfid (t-BuO)3SiSSiPh3 und mit Ph3P oder Bu3P, durch Abbau eines S-Atoms, [(t-BuO)3Si]2S. Die Kristall-Struktur von [(t-BuO)3Si]2S2 wurde bestimmt. Die S—S-Bindungslänge beträgt 209,2 pm, Si—S 213,2 pm. Der Mittelwert für den Si—S—S-Winkel beträgt 100,7°, der Torsionswinkel Si—S—S—Si -127,6°.
    Additional Material: 3 Ill.
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  • 66
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 561 (1988), S. 157-166 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Methylene Compounds of Non-Metals. VI. Amides of Methane-bis(phosphonous Acid), -bis(phosphonic Acid) and -bis(thiophosphonic Acid)Symmetrical- and asymmetrical-substituted amides of methane-bis(phosphonous acid), -bis(phosphonic acid) and -bis(thiophosphonic acid) have been obtained by stepwise aminolysis of the chlorides Cl2(Z)PCH2P(Z)Cl2 (1: Z = electron pair; 7: Z = S; 13: Z = O) and the fluoride F2(S)PCH2P(S)F2 19 with dimethylaminotrimethylsilane. Oxidation reactions of trivalent phosphonous amides with sulfur and dimethylsulfoxide have also been investigated.
    Notes: Symmetrisch- und asymmetrisch-substituierte Amide der Methan-bis-(phosphonigsäure), -bis(phosphonsäure) und -bis(thiophosphonsäure) wurden durch stufenweise Aminolyse von Chloriden der Zusammensetzung Cl2(Z)PCH2P(Z)Cl2 (1: Z = Elektronenpaar; 7: Z = S; 13: Z = O) und des Fluorids F2(S)PCH2P(S)F2 19 mit Dimethylaminotrimethylsilan erhalten. Die Oxidation von Amiden des dreibindigen Phosphors mit Schwefel und Dimethylsulfoxid wurde ebenfalls untersucht.
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  • 67
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    Zeitschrift für anorganische Chemie 561 (1988), S. 185-191 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphidation of Tungsten MetalA study was undertaken concerning the phosphidation of tungsten at 800, 900, and 1000°C in phosphorus vapor at 1 atm by a sealed-tube method. X-ray diffraction patterns and an electron probe microanalysis of the products showed that all the phosphide films were composed of two layers, that is, their outer layers were composed of WP2 and their inner layers composed of WP. All the phosphidation reactions proceeded according to a parabolic rate law. The parabolic rate constant was given as a function of the absolute temperature by the following expression. Kp = 3.06X10-5 exp(-103 KJ mol-1/RT) kg2m-4s-1, (1 atm, 1073-1273 K). Tungsten metal was appreciably superior to iron, nickel, and chromium, which are the main constituent metals of stainless steel, and titanium with respect to phosphidation resistance.
    Notes: Die Reaktion von Wolframmetall bei der Phosphidierung bei 800, 900 und 1000°C in Phosphordampf (1 atm) wurde im geschlossenen Quarzrohr untersucht. Aus Röntgenbeugungsbildern und Elektronenstrahl-Mikroanalysen der Produkte folgt, daß alle Phosphidfilme aus zwei Schichten bestanden, ihre Außenschichten bestanden aus WP2 und ihre Innenschichten aus WP. Alle Phosphidierungsreaktionen verliefen nach dem parabolischen Zeitgesetz. Die parabolische Geschwindigkeitskonstante als Funktion der absoluten Temperatur lautet Kp = 3,06X10-5 exp(-103 KJ mol-1/RT) kg2m-4s-1, (1 atm, 1073-1273 K). Wolframmetall ist „phosphorfester“ als Eisen, Nickel und Chrom, welche Hauptbestandteile der nichtrostenden Stähle sind, und Titan.
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  • 68
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    Zeitschrift für anorganische Chemie 561 (1988), S. 174-184 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Isolierung und spektrale Charakterisierung von Eisen(III)-iodidEisen(III)-iodid wurde zum ersten Mal in reiner Form als dunkelvioletter Feststoff aus einer Lösung in n-Hexan durch Bestrahlung von Fe(CO)4I2 und I2 mit Tageslicht erhalten. Seine Zusammensetzung wurde durch Elementaranalyse und quantitative Umsetzung mit n-Bu4N+I- zu dem bekannten n-Bu4N+FeI4- bestätigt. Obwohl die Verbindung im festem Zustand stabil ist, zersetzt sich FeI3 quantitativ in Lösung zu FeI2 und 0,5 mol I2.
    Notes: Ferric iodide is isolated pure for the first time as a dark purple solid when a hexane solution of diiodotetracarbonyliron(II) and diiodine is exposed to actinic radiation. Its identity is confirmed by elemental analysis and quantitative conversion to the known tetraiodoferrate(III) by treatment with tetra-n-butylammonium iodide. Although persistent in the solid state, ferric iodide is readily decomposed in solution to ferrous iodide and 0.5 mol diiodine quantitatively.
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  • 69
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    Zeitschrift für anorganische Chemie 561 (1988), S. 192-192 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 70
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988) 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 71
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    Zeitschrift für anorganische Chemie 561 (1988), S. 192-192 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 72
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    Zeitschrift für anorganische Chemie 562 (1988), S. 17-22 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of 1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxane1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxane 1 crystallizes monoclinically (P21/n; a = 2237.5; b = 801.4; c = 1396.6 pm, β = 106.29°; Z = 4). The X-ray structural analysis shows a bent configuration of the molecule with Si—O—Si angle = 140°, d(Si—O) = 163.8 pm. The staggered conformation of the six Si—C bonds is distorted. The methyl groups are in gauche position.The results are discussed with respect to an intramolecular H…O interaction in the structure of 1,1,3,3-tetraphenyldisiloxane.
    Notes: 1,3-Dimethyl-1,1,3,3-tetraphenyldisiloxan 1 kristallisiert monoklin (P21/n; a = 2237,5; b = 801,4; c = 1396,6 pm; β = 106,29°; Z = 4). Die Kristallstrukturanalyse ergab eine gewinkelte Konfiguration des Moleküls mit Si—O—Si = 140° und d(Si—O) = 163,8 pm. Die Substituenten an dem Silicium-Atom zeigen eine Abweichung von einer gestaffelten Anordnung der sechs Si—C-Bindungen. Die Methylgruppen sind in gauche-Position.Die Ergebnisse werden im Zusammenhang mit der Struktur des 1,1,3,3-Tetraphenyldisiloxans hinsichtlich einer intramolekularen H…O-Wechselwirkung diskutiert.
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  • 73
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    Zeitschrift für anorganische Chemie 562 (1988), S. 23-30 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Cs4Sn5S12 · 2 H2O, a Cesium(I) Thiostannate(IV) with Fivefold and Sixfold Coordinated TinCs4Sn5S12 · 2 H2O was prepared by hydrothermal reaction of Cs2CO3 with SnS2 at a temperature of 130°C. An X-ray structural analysis demonstrated that the compound contains polythiostannate(IV) sheet anions [Sn5S124-]∞, for which the basic elements are trigonal SnS5-bipyramids and SnS6-octahedra. Five of the six independent sulphur atoms in the asymmetric unit are coordinated by two tin atoms, one by three tin atoms.
    Notes: Cs4Sn5S12 · 2 H2O wurde durch hydrothermale Reaktion von Cs2CO3 mit SnS2 bei einer Temperatur von 130°C dargestellt. Eine Röntgenstrukturanalyse ergab, daß die Verbindung schichtartige Polythiostannat(IV)-Anionen [Sn5S124-]∞ beinhaltet, in denen die Grundelemente trigonale SnS5-Bipyramide sowie SnS6-Oktaeder sind. Von den sechs unabhängigen Schwefelatomen der asymmetrischen Einheit werden fünf zweimal und eins dreimal von Zinnatomen koordiniert.
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  • 74
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    Zeitschrift für anorganische Chemie 562 (1988), S. 7-16 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phase Diagrams of Chalcides and Pnictides of Ruthenium and Osmium with Pyrite, Marcasite, Loellingite, and Arsenopyrite StructureThe phase diagrams of ruthenium and osmium chalcide and pnictide systems were studied by X-ray phase analyses. In the systems RuPS—RuPSe, OsPS—OsPSe, RuPS—OsPS, and RuPSe—OsPSe complete series of arsenopyrite type solid solutions are formed. In the heterotype systems PuP2—RuPS—RuS2, RuP2—RuPSe—RuSe2, RuP2—RuTe2, and OsP2—OsTe2 (endmember phases, loellingite, arsenopyrite, and pyrite (marcasite) structure) no mutual solubility was observed, whereas in the analogous system RuSb2-2xTe3x a complete series of mixed crystal with x 〈 0.25, loellingite, x = 0.25-0.65, arsenopyrite, x 〉 0.65, marcasite, and x = 1, marcasite and pyrite structure with a continuous run of the unit cell dimensions are formed. In the systems MP2—MTe2 the hitherto unknown ternary compounds OsPTe (arsenopyrite type, a = 622.91(4), b = 616.04(4), c = 624.49(4) pm, and β = 112.01(1)°) and RuPTe (structure unknown) were obtained. The FIR spectra of these compounds and of the RuSb2—RuTe2 solid solutions are reported and discussed with respect to the internal and external modes present.
    Notes: Die Phasendiagramme von Pnictid-Chalkogenid-Systemen des Rutheniums und Osmiums wurden mit Hilfe von Röntgenguinier-Aufnahmen abgeschreckter Präparate untersucht. In den Systemen RuPS—RuPSe, OsPS—OsPSe, RuPS—OsPS und RuPSe—OsPSe (Randphasen Arsenopyrittyp) werden lückenlose Mischkristallreihen gebildet. In den Systemen RuP2—RuPS—RuS2, RuP2—RuPSe—RuSe2, RuP2—RuTe2 und OsP2—OsTe2 (Randphasen Löllingit-, Arsenopyrit- und Pyrit- bzw. Markasittyp) konnte keine Mischkristallbildung beobachtet werden, wohingegen im analogen System RuSb2-2xTe3x eine lückenlose Mischkristallreihe (x 〈 0,25: Löllingit-, x = 0,25-0,65: Arsenopyrit-, x 〉 0,65: Markasit- und x = 1: Markasit- oder Pyritstruktur) mit einem kontinuierlichen Verlauf der Gitterkonstanten gebildet wird. Als bisher unbekannte ternäre Verbindungen wurden OsPTe (Arsenopyrittyp, a = 622,91(4), b = 616,04(4), c = 624,49(4) pm und β = 112,01(1)°) sowie RuPTe (Strukturtyp unbekannt) erhalten. Die FIR-Spektren dieser Verbindungen sowie die der RuSb2—RuTe2-Mischkristalle werden mitgeteilt und diskutiert.
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    Zeitschrift für anorganische Chemie 562 (1988), S. 42-48 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dibromomethylsulfoniumsalts  -  Preparation and Crystal StructureThe salts CH3SBr2+A- (A- = SbCl6-, AsF6-) were prepared by various routes and characterized by their Ramanspectra. CH3SBr2+AsF6- crystallized in the monoclinic space group P21/c with a = 770,5(4) pm, b = 942,4(12) pm, c = 1329,3(14) pm, β = 100,28(6)°, Z = 4. Distances and bond angles in the cation are as expected.
    Notes: Es wurden die Salze CH3SBr2+A- (A- = SbCl6-, AsF6-) auf unterschiedlichen Wegen dargestellt und durch ihre Ramanspektren charakterisiert. CH3SBr2+AsF6- kristallisiert in der monoklinen Raumgruppe P21/c mit a = 770,5(4) pm, b = 942,4(12) pm, c = 1329,3(14) pm, β = 100,28(6)°, Z = 4. Die Abstände und Winkel im Kation entsprechen den Erwartungen.
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  • 76
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    Zeitschrift für anorganische Chemie 562 (1988), S. 62-72 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Heterogeneous Equilibria and Chemical Vapour Transport in the System Ti—O—C—ClThe phase diagram Ti—O—C—Cl contains Ti2O3 and Ti3O5 in equilibrium with the TixCyO1-y phase. All the other titanium oxides are in equilibrium with carbon under their decomposition pressures. Ti2O3, TiO2, and TinO2n-1 can be grown by CVT using CCl4 or Cl2 in the presence of carbon as transport media. TiC transport is impossible. The presence of Cl2, however, reduces the synthesis temperature considerably. No phase containing C is deposited even under conditions, where its deposition is predicted by a thermodynamic analysis. The transport behaviour however can be explained by this analysis, assuming a metastable state, in which the Boudouard reaction is thought to be completely hindered.
    Notes: Im Phasendiagramm Ti—O—C—Cl existieren nur Ti2O3 und Ti3O5 neben der Oxidcarbidphase TixCyO1-y, alle anderen Titanoxide sind bei ihrem Zersetzungsdruck im Gleichgewicht mit C. Ti2O3, TiO2 und TinO2n-1 können durch chemischen Transport mit CCl4 oder mit Cl2 in Gegenwart von festem C in Form kleiner Einkristalle abgeschieden werden. TiC läßt sich nicht transportieren, jedoch wird durch Chlorzusatz die Synthesetemperatur beträchtlich gesenkt. Eine kohlenstoffhaltige Phase wird auch nicht unter solchen Bedingungen abgeschieden, wo deren Auftreten aus einer thermodynamischen Analyse zu folgern wäre. Dagegen erklärt die thermodynamische Analyse das Transportverhalten für einen metastabilen Zustand richtig, für den eine vollständige Hemmung der Boudouard-Reaktion angenommen wird.
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  • 77
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    Zeitschrift für anorganische Chemie 562 (1988), S. 73-86 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Redox Reactions in Condensed Oxide Systems. VIII. On the Mechanism of Spinel Formation in the System ZnxMn3-xO4Spinel formation has been studied in sandwich arrangements of ZnO/Mn3O4 and ZnO/α-Mn2O3 ceramic disks measuring the chemical diffusion coefficients by chemical analyses and with micro probe. The reaction with α-Mn2O3 yields ZnxMn1-xIIMn2IIIO4 (0 〈 x ≤ 1) accompanied by O2 evolution in the front. On the other hand, in accordance with the phase diagram Zn(Znx-1Mnx-1IVMn4-2xIII)O4(1 〈 x 〈 1.5) is formed by oxygen contamination at the side neighboured to ZnO. The reaction rate of ZnO with Mn3O4 is increasing when the O2 partial pressure is increasing from normal atmosphere to pure oxygen yielding values which characterize the reaction of ZnO with α-Mn2O3. Migrating of ZnO into Mn3O4 or α-Mn2O3 only is observed for the reaction in the air, while in pure oxygen reversal diffusion of manganese oxide into the ZnO pellet takes place in part, too.
    Notes: Die Spinellbildung wird an Sinterpreßlingen von ZnO/Mn3O4 und ZnO/α-Mn2O3 durch Ermittlung der chemischen Diffusionskoeffizienten untersucht. Dazu werden analytische Bestimmungen und Messungen des Konzentrationsprofils mit Hilfe der Mikrosonde ausgeführt. Bei der Umsetzung mit α-Mn2O3 verläuft die Entstehung von ZnxMn1-xIIMn2IIIO4 (0 〈 x ≤ 1) in der Reaktionsfront unter O2-Abspaltung. Auf der an ZnO angrenzenden Seite bildet sich in Übereinstimmung mit dem Phasendiagramm unter O2-Aufnahme Zn(Zn1-xMnx-1IVMn4-2xIII)O4(1 〈 x 〈 1,5). Unter reinem Sauerstoff wird die Reaktionsgeschwindigkeit von ZnO mit Mn3O4 gegenüber der Umsetzung an der Luft auf Werte erhöht, die etwa auch für die Reaktion von ZnO mit α-Mn2O3 zutreffen. An der Luft wird stets nur die Einwanderung von ZnO in Mn3O4 bzw. α-Mn2O3 beobachtet, unter reinem Sauerstoff dagegen partiell auch Transport von Manganoxid in das Zinkoxid.
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  • 78
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Trichloroacetyl Trisulfurtrinitride with Molybdenum Pentachloride. Crystal Structures of CC13CO—NS3N2 and (PPh4)2[MOCl3(N2SCOCCl3)]2 · 2 CH2C12 · 2 CC14CCl3CO—NS3N2 is formed along with [CCl3CN2S2]Cl by the reaction of (NSCl)3 with trichloroacetanhydride. When warmed with molybdenum pentachloride in CCl4, it yields a mixture of MoCl3(N3S2) and MoCl2(N2SCOCCl3), which can be converted to PPh4[MoCl4(N3S2)] and (PPh4)2[MoCl3(N2SCOCCl3)]2 by addition of tetraphenylphosphonium chloride in CH2Cl2. The crystal structures of the title compounds were determined by X-ray diffraction.CCl3CO—NS3N2. Space group Pna21, Z = 4, a = 588.4, b = 887.7, c = 1788.2 pm; 700 independent observed reflexions, R = 0.065. The compound consists of monomer molecules in which the trichloroacetyl group is bonded via an N atom to an S3N2 ring; the conformation is such that remarkably short O…S contact distances result.(PPh4)2[MoCl3(N2SCOCCl3)]2 · 2 CH2Cl2 · 2 CCl4. Space group Pccn, Z = 8, a = 1720.8, b = 1757.2, c = 2545.9 pm; 3102 reflexions, R = 0.107. The compound consists of PPh4+ ions, dimer [MoCl3(N2SCOCCl3)]22- anions and solvent molecules, part of which is strongly disordered. In the centrosymmetric anion the Mo atoms are linked by a short MoMo bond (256 pm) and by two N atoms, one from each of the two N2SCO chelate groups.
    Notes: CC13CO—NS3N2 wird neben [CCI3CN2S2]Cl aus (NSCI)3 und Trichlor-acetanhydrid erhalten. Es reagiert beim Erwärmen in CCI4 mit Molybdänpentachlorid zu einem Gemisch von MoCI3(N3S2) und MoCl2(N2SCOCCl3), das sich mit Tetraphenylphosphoniumchlorid in CH2Cl2 unter Bildung von PPh4[MoC14(N3S2)] und (PPh4)2[MoC13(N2SCOCC13)]2, umsetzt. Die Titelverbindungen haben wir durch röntgenographische Strukturanalysen charakterisiert.CC13CO—NS3N2. Raumgruppe Pna21, Z = 4, Gitterabmessungen a = 588,4; b = 887,7; c = 1788,2 pm (700 unabhängige beobachtete Reflexe, R = 6,5%). Die Verbindung besteht aus monomeren Molekülen, in denen der Trichloracetylrest über ein N-Atom an den S3N2-Fünfring gebunden ist, mit einer Konformation, die zu auffällig kurzen O…Kontakten von 308 und 286 pm führt.(PPh4)2[MoCl3(N2SCOCCl3)]2 · 2 CH2Cl2 · 2 CCl4. Raumgruppe Pccn, Z = 8, Gitterabmessungen a = 1720,8; b = 1757,2; c = 2545,9 pm (3102 unabhängige beobachtete Reflexe, R = 10,7%). Die Verbindung besteht aus PPh4⊕-Ionen, dimeren Anionen [MoCl3(N2SCOCCl3)]22⊖ und eingelagerten Lösungsmittelmolekülen, die zum Teil stark fehlgeordnet sind. Im zentrosymmetrischen Anion sind die Molybdänatome über eine kurze MoMo-Bindung von 256 pm und zugleich von je einem N-Atom der beiden N2SCO-Chelatgruppen miteinander verknüpft.
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  • 79
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of the Arsino Sulfur Diimides tBu2As(NSN)AstBu2 and tBuAs(NSN)2AstBu with Trinuclear Clusters M3(CO)12 (M = Fe, Ru)  -  X-Ray Structure Analysis of Fe2(CO)6[μ-tBuAs(NSN)AstBu]In the reaction of bis(di-tert-butyl-arsino)sulfur diimide, tBu2As(NSN)AstBu2 (1), with Ru3(CO)12 a trinuclear cluster (μ2-H)Ru3(CO)8(μ3-AstBu)(μ2-NSNAstBu2) (6b) was obtained containing a hydride bridge, a triply-bridging tBuAs unit and a fragment (NSNAstBu2) in which the NSN chain of the original sulfur diimide 1 is maintained. The known cluster Fe3(CO)9(μ3-S)(μ3-AstBu) (7) was formed  -  as a result of further fragmentation of 1  -  in the analogous reaction with Fe3(CO)12.The reaction of the eight-membered heterocycle tBuAs(NSN) 2As tBu (2) with Ru3(CO)12 gave a complex Ru3(CO)10(μ-tBuAs(NSN)2AstBu) (8b) in which the intact sulfur diimide ligand is coordinated via the two arsenic atoms to two vicinal ruthenium atoms. In the corresponding reaction with Fe3(CO)12, however, a complex Fe2(CO)6[μ-tBuAs(NSN)AStBu] (9) was obtained where the sulfur diimide ligand is formed by loss of an NSN bridge from 2. The two triruthenium clusters 6b and 8b correspond to the known triosmium clusters 6a and Sa, respectively, the structures of which had been determined by X-ray crystallographic methods. A crystal structure analysis was carried out for 9: The sulfur diimide fragment tBUAs(NSN)AstBu behaves as a six-electron ligand for the Fe2(CO)6 framework, it is planar and perpendicular to the Fe-Fe bond (2.728(1) Å). Both the (nonbonding) As…As distance (2.976(21) Å) and the angles at the sulfur (121.0(2)°) and the nitrogen atoms (124.4(2)°) of the sulfur diimide ligand are smaller than the corresponding data in reference compounds which also contain two arsino substituents in cis, cis configuration (Z, Z) at the central NSN skeleton.
    Notes: Bei der Umsetzung von Bis(di-tert-butyl-arsino)schwefeldiimid, tBu2As(NSN)AstBu2 (1), mit Ru3(CO)12 wurde ein dreikerniger Cluster (μ2-H)Ru3(CO)8(μ3-AstBu)(μ2-NSNAstBu2) (6b) isoliert, der eine Hydridbrücke, eine dreifach verbrückende tBuAs-Einheit sowie ein Bruchstück (NSNAstBu2) enthält, in dem die NSN-Kette des ursprünglichen Schwefeldiimids 1 noch erhalten geblieben ist. Bei der analogen Reaktion mit Fe3(CO)12 bildet sich  -  unter weitergehender Fragmentierung von 1  -  der bekannte Cluster Fe3(CO)9(μ3-S)(μ3-AstBu) (7).Die Umsetzung des Achtring-Heterocyclus tBuAs(NSN)2AstBu (2) mit Ru3(CO)12 ergab einen Komplex Ru3(CO)10(μ-tBuAs(NSN)2AstBu) (8b), in dem der unversehrte Schwefeldiimid-Ligand über beide Arsenatome an zwei benachbarte Rutheniumatome koordiniert ist. Bei der entsprechenden Reaktion mit Fe3(CO)12 wurde dagegen ein Komplex Fe2(CO)6[μ-tBuAs(NSN)AstBu] (9) erhalten, dessen Schwefeldiimid-Ligand aus 2 unter Verlust einer NSN-Brücke entsteht.Die beiden Triruthenium-Cluster 6b und 8b entsprechen den bekannten Triosmium-Clustern 6a bzw. 8a, deren Struktur früher röntgenographisch bestimmt worden war. Für 9 wurde eine Kristallstrukturanalyse durchgeführt: Das Schwefeldiimid-Fragment tBuAs(NSN)AstBu wirkt als Sechselektronenligand für das Fe2(CO)6-Gerüst; es ist eben und steht zur Fe - Fe-Bindung (2,728(1) Å) senkrecht. Sowohl der (nicht-bindende) As…As-Abstand (2,976(1) Å) als auch die Winkel am Schwefel (121,0(2)°) und an den Stickstoffatomen (124,4(2)°) des Schwefeldiimid-Liganden sind kleiner als die entsprechenden Größen in Vergleichsverbindungen, die ebenfalls zwei Arsino-Substituenten in cis, cis-Konfiguration (Z, Z) am zentralen NSN-Gerüst enthalten.
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  • 80
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Silyl Triazenes tBu3Si—N=N—NR—SitBu3 (R = Na, H, Me, SnMe3)Yellow triazenide (1) is prepared by reaction of tBu3SiN3 and tBu3SiNa in tetrahydrofuran (thf) in quantitative yield. It slowly decomposes above 200°C in a first order reaction to N2 and (tBu3Si)2NNa and reacts with MeOH, Me2SO4, Me3SnCl under formation of metastable, yellow silyl triazenes tBu3Si—N=N—NR—SitBu3 with R = H (2), Me (3), SnMe3 (4). Structures of the triazenes 2 and 4 have been determined by X-ray crystallography (for data cf. Table 1). The heavy atom framework in 2 (SiNNNSi) and 4 (SiNNNSnSi), respectively, is planar with zigzag configurated SiNNNSi chains. 2 and 4 are (from 1H-NMR) fluxional molecules: —N=N—NR—⇄—RN—N=N—.
    Notes: Das gelbe Triazenid (1) entsteht aus tBu3SiN3 und tBu3SiNa in Tetrahydrofuran (THF) in quantitativer Ausbeute. Es zerfällt ab 200°C langsam nach erster Reaktionsordnung in N2 und (tBu3Si)2NNa und reagiert mit MeOH, Me2SO4, Me3SnCl unter Bildung der metastabilen, gelben Silyltriazene tBu3Si—N=N—NR—SitBu3 mit R = H (2), Me (3), SnMe3 (4). Die Strukturen der Triazene 2 und 4 wurden durch Röntgenstrukturanalyse gelöst (Daten Tab. 1). Das Gerüst der Schweren Atome in 2 (SiNNNSi) bzw. 4 (SiNNNSnSi) ist planar mit zickzack-konfigurierten SiNNNSi-Ketten. Laut 1H-NMR sind 2 und 4 fluktuierende Moleküle: —N=N—NR—⇄—RN—N=N—.
    Additional Material: 2 Ill.
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  • 81
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 87-90 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal-Chemistry of Oxotantalates M4Ta2O9. I. About Mg4Ta2O9 and Mg2Ni2Ta2O9Single crystals of (A) Mg4Ta2O9 and (B) Mg2Ni2Ta2O9 were prepared by recrystallisation of a CO2-Laser-beam heated flux. Single crystal X-ray structure analysis lead to a trigonal symmetry, space group D3d4 - P3c1 with A: a = 5.1654; c = 14.0463 Å; B: a = 5.1362; c = 14.0577 Å; Z = 2. Both compounds crystallizes with a corund related structure type. In B are the metalpositions occupied statistically by Mg2+ and Ni2+.
    Notes: Mit CO2-Laser-Technik wurden aus Schmelzen Einkristalle von (A) Mg4Ta2O9 und (B) Mg2Ni2Ta2O9 dargestellt. Die Einkristallstrukturaufklärung ergab trigonale Symmetrie, Raumgruppe D3d4 - P3c1 mit A: a = 5,1654; c = 14,0463 Å; B: a = 5,1362; c = 14,0577 Å; Z = 2. Beide Verbindungen kristallisieren in einem vom Korund abgeleiteten Strukturtyp. B enthält Mg2+ und Ni2+ in statistischer Verteilung auf den Metallpositionen.
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  • 82
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 115-122 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Ca4Fe3F10 and Cs3TINi3F10Single crystals of Cs4Fe3F10 (orthorhombic, a = 629.4, b = 1450,7, c = 1410.9 pm) and Cs3TlNi3F10 (orthorhombic, a = 610.1, b = 1442.0, c = 1366.8 pm) have been prepared. Results of X-ray investigation: Cs4Fe3F10 is isotypic to Cs4Mg3F10 and crystallizes in the space group Cmca (R = 3.97%, Rw = 2.75%, 1020 of 1020 I0(hkl), fourcircle diffractometer AED 2, Fa. Siemens). A monoclinic distortion could not be observed as supposed present.Cs4-xTlxNi3F10 (x≈1), R = 7.75%, Rw = 4.96%, 1079 of 1294 I0(hkl), fourcircle diffraktometer PW 1100, Fa. Philips) confirm the possibility to substitute Cs against Tl in the Cs4Mg3F10-type.
    Notes: Cs4Fe3F10 (orthorhombisch, a = 629,4, b = 1450,7, c = 1410,9 pm) und Cs3TlNi3F10 (orthorhombisch, a = 610,1 b = 1442,0, c = 1366,8 pm) wurden in Form von Ein-kristallen dargestellt und röntgenographisch untersucht. Cs4Fe3F10 ist entgegen der bisherigen Annahme nicht monoklin verzerrt; es kristallisiert in der Raumgruppe Cmca (R = 3,97%, Rw = 2,75%, 1020 von 1020 I0) (hkl), Vierkreisdiffraktometer AED 2, Fa. Siemens). Cs4-xTlxNi3F10 (x≈1) (R = 7,75%, Rw = 4,06%, 1079 von 1294 I0(hkl), Vierkreisdiffraktometer PW 1100, Fa. Philips) zeigt, daß teilweiser Ersatz von Cs+ im Cs4Mg3F10-Strukturtyp gegen einfach positiv geladene Kationen vergleichbarer Größe (in diesem Fall Tl+ mit einem „einsamen“ Elektronenpaar) möglich ist.
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  • 83
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 562 (1988), S. 165-169 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fest-Flüssig-Phasengleichgewichte des Systems KCl—MgCl2—H 2O bei erhöhten Temperaturen. II. Isothermen bei 130, 140 und 150°CExperimentelle Ergebnisse der Fest-Flüssig-Phasengleichgewichte im System KCl—MgCl2—H2O bei 130, 140 und 150°C werden vorgestellt. Eine bereits beschriebene „analytische“ Methode wurde angewendet.
    Notes: Experimental results are reported for the solid-liquid phase equilibria of the ternary system KCl—MgCl2—H2O at 130, 140, and 150°C. An “analytic” method, described previously, was used.
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  • 84
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 185-191 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: EPR Spectra of Soluble Alkylammonium Fluoroferrates(III)The existence of (FeF6)3- has been proved in methanolic solution of alkylammonium fluoroferrates (III) with excess of fluorides. Information about structures of the investigated polycrystalline compounds (NH3CH3)FeF4, (NH3CH3)2FeF5, and (NH3CH3)3FeF6 has been obtained by fitting experimental EPR curves with the help of model functions.
    Notes: In methanolischer Lösung von Alkylammoniumfluoroferraten(III) wird das Vorliegen von (FeF6)3-bei Fluoridüberschuß nachgewiesen. Für die untersuchten polykristallinen Verbindungen (NH3CH3)FeF4, (NH3CH2)2FeF5 und (NH3CH3)3FeF6 werden durch Anpassung von Modellfunktionen an die experimentellen EPR-Spektren Strukturaussagen abgeleitet.
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  • 85
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Diphenylfluorophosphane with Aldehydes. Crystal Structure of [α-(Difluorodiphenyl-λ5-phosphanyl)] Piperonyl DiphenylphosphiniteDiphenylfluorophosphane, Ph2PF, reacts with aldehydes forming phosphinito phosphoranes, Ph2F2P—CHR—O—PPh2. [α-(Difluorodiphenyl-λ5-phosphanyl)] piperonyl diphenyl-phosphinite, obtained by the reaction of Ph2PF with piperonal, crystallizes in the triclinic space group P1 with a = 969.3 pm, b = 2360 pm, c = 607,3 pm, α = 88.33°, β = 102.79°, γ = 92.40° and Z = 2.
    Notes: Diphenylfluorphosphan, Ph2PF, reagiert mit Aldehyden unter Bildung von Phosphinitophosphoranen, Ph2F2P—CHR—O—PPh2. Der mit Piperonal erhaltene Diphenyl-phosphinigsäure-[α-(difluorodiphenyl-λ5-phosphanyl)]piperonylestr kristallisiert in der triklinen Raumgruppe P1 mit a = 969,3 pm, b = 2360 pm, c = 607,3 pm, α = 88,33°, β = 102,79°, γ = 92,40° und Z = 2.
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  • 86
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 87
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 180-184 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zur Kristallchemie der Verbindungen des Typs MX · MgX2 · 6H2OVon den Verbindungen des Typs MX · MgX2 · 6 H2O wurden unter Variation der M+- und X--Ionen die Doppelsalzhexahydrate CsCl · MgCl2 · 6 H2O, Li(H2O)Cl · MgCl2 · 6 H2O, NH4Br · MgBr2 · 6 H2O, RbBr · MgBr2 · 6 H2O. CsBr · MgBr2 · 6 H2O, KI · MgI2 · 6 H2O, NH4I · MgI2 · 6 H2O und RbI · MgI2 · 6 H2O synthetisiert. Durch röntgenographische Untersuchungen an Pulverpräparaten wurden die Gitterparameter und die Raumgruppe bestimmt. Aus den Ergebnissen wurde die Zuordnung zu Strukturtypen vorgenommen. Danach besteht die Struktur aus einer Verknüpfung aller (M+)X6--Oktaeder untereinander über gemeinsame Ecken zu perowskitanalogen Baueinheiten, in deren Hohlräumen die Mg(H2O)62+-Oktaeder angeordnet sind. Ein “Toleranzfaktor” t von 1,045 bis 1,061, berechnet aus den Radienverhältnissen, stellt ein Charakteristikum für die obere Existenzgrenze dieser Struktur dar. Carnallit besitzt einen höheren Wert und deshalb eine andere Struktur.
    Notes: The following MX · MgX2 · 6H2O compounds (double salt hexahydrates) were synthesized by variation of the M+ and X- ions: CsCl · MgCl2 · 6 H2O, Li(H2O)Cl · MgCl2 · 6H2O, NH4Br · MgBr2 · 6 H2O, RbBr · MgBr2 · 6 H2O, CsBr. MgBr2 · 6 H2O, KI · MgI2 · 6 H2O, NH4I. Mgl2 · 6 H2O and RbI · MgI2 · 6H2O. By X-ray analysis of powder samples the lattice parameters and the space group were determined. On the basis of the results thus obtained, an identification with structural types was carried out. In accordance with the findings, the structure is made up of (M+)X6-octahedra which are linked into perovskite type units by sharing vertices. Their interstices are occupied by the Mg(H2O)62+ octahedra. A “tolerance factor” t which has been calculated on the basis of the proportion of radii and which attains values between 1.045 and 1.061 is a criterion for the upper limit of the area of existence of this structure. Carnallite has a higher to value and, therefore, a different structure.
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  • 88
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988) 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 89
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 192-192 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 90
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 7-16 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Electronmicroscopical Investigation of Monoclinic (Zn,Nb)12O29 and (Mg,Nb)12O29Different chlorinating transport agents were tried for the chemical transport of Zn2/3Nb11 1/3O29 and Mg2/3Nb11 1/3O29. With NH4Cl we succeeded in getting solid solutions of M2/3Nb11 1/3O29 (M = Zn or Mg) and Nb12O29. Only Mg2/3Nb11 1/3O29 could be deposited as a pure phase using HgCl2 as transport agent. The investigation of the transport products with a transmission electron microscope confirmed the expected structure of edge sharing [3×4] blocks like Nb12O29. Nevertheless many different defective crystal areas were observed.
    Notes: Verschiedene chlorierende Transportmittel wurden für den chemischen Transport von Zn2/3Nb11 1/3O29 und Mg2/3Nb11 1/3O29 erprobt. Mit NH4Cl gelang es, Mischkristalle von M2/3Nb11 1/3O29 (mit M = Zn oder Mg) und Nb12O29 zu erhalten. Phasenrein ließ sich nur Mg2/3Nb11 1/3O29 mit dem Transportmittel HgCl2 abscheiden. Die Untersuchung der Transportprodukte mit dem Transmissionselektronenmikroskop bestätigte den Aufbau aus kantenverknüpften [3×4]-Blöcken wie bei Nb12O29. In vielen Kristallbereichen wurde allerdings eine unterschiedliche Fehlordnung beobachtet.
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  • 91
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 26-30 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About a Compound Formation MO:M2O3. X. On BaCr2O4For the first time single crystals of BaCr2O4 were prepared as a high temperature compound of the SrCr2O4-type. It crystallizes with orthorhomibic symmetry, space group D2h13 - Pmmn, a = 12,286; b = 5,921; c = 5,146 Å Z = 4. The crystal structure are described and the relationship to the metastable compounds α-CaCr2O4 and SrCr2O4 are discussed.
    Notes: BaCr2O4 wurde erstmals einkristallin als Hochtemperaturverbindung vom SrCr2O4-Typ dargestellt. Es kristallisiert orthorhombisch, Raumgruppe D2h13 - Pmmn mit a = 12,286; b = 5,921; c = 5,146 Å Z = 4. Die Struktur wird beschrieben und das Verhalten gegenüber den entropiestabilisierten metastabilen Verbindungen α-CaCr2O4 diskutiert.
    Additional Material: 2 Ill.
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  • 92
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 17-25 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hexafluorotitanic(IV) Acid: Studies on Formation and Structure of Crystalline HydratesThe system hexafluorotitanic(IV) acid  -  water was investigated y low-temperature difference thermal analysis (DTA) and temperature-dependent X-ray powder diffraction in the water-rich range of 80-100 mol% H2O. A quasi-binary behavior was found, and the melting diagram was constructed. It shows the existence of three crystalline hydrates H2TiF6 · nH2O with n = 4, 6, and (probably) 10. The tetrahydrate and the hexahydrate melt congruently at -12 and 0°C, respectively; the most water-rich hydrate decomposes in the sub-solidus range at -79°C into solid hexahydrate and ice. The tetrahydrate exhibits a phase transition in the solid state at -57°C. Single crystals were grown of the hexahydrate and a trihydrate, too, and were used for complete structure determination of these compounds from X-ray data. The ionic formulae of the oxonium salts are (H5O2)2TiF6 · 2 H2O and (H3O)(H5O2)TiF6, respectively. The structures are governed by extensive hydrogen bonding. The hexahydrate is isotypic to H2SiF6 · 6 H2O.
    Notes: Das System Hexafluorotitan(IV)-säure-Wasser wurde mit Tieftemperatur Differenzthermoanalyse (DTA) und temperaturabhängiger Röntgenpulverbeugung im wasserreichen Bereich von 80 bis 100 Mol-% H2O untersucht. Es wurde quasibinäres Verhalten festgestellt und das Schmelzdiagramm konstruiert. Dieses zeigt die Existenz von drei kristallinen Hydraten H2TiF6. nH2O mit n = 4,6 und (wahrscheinlich) 10. Das Tetrahydrat und das Hexahydrat schmelzen kongruent bei -12 und 0°C; das wasserreichste Hydrat zerfällt im Subsolidusbereich bei -79°C in festes Hexahydrat und Eis. Das Tetrahydrat durchläuft im festen Zustand eine Phasenumwandlung bei-57°C. Einkristalle werden vom Hexahydrat und auch von einem Trihydrat erhalten und dienten zur vollständigen Strukturbestimmung dieser Verbindungen aus Röntgenbeugungsdaten. Die ionischen Formeln der Oxoniumsalze lauten (H5O2)2TiF6 · 2 H2O bzw. (H3O)(H5O2)TiF6. Die Strukturen sind durch zahlreiche Wasserstoffbrücken geprägt. Das Hexahydrat ist isotyp zu H2SiF6 · 6 H2O.
    Additional Material: 3 Ill.
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  • 93
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 37-44 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thiobromo Complexes of Arsenic and Antimony. Preparation and Crystal Structures of (PPh4)2[As2SBr6] · CH2Br2 and (PPh4)2[Sb2SBr6] · CH2Br2(PPh4)2[As2SBr6] · CH2Br2 is formed by the reaction of As2S3, PPh4I and HI in dibromomethane. It can also be obtained, as well as (PPh4)2[Sb2SBr6] · CH2Br2, from (PPh4)2[As2Br8] and (PPh4)3[Sb2Br9], respectively, with bistrimethylsilylsulfide. The crystal structures of the title compounds were determined by X-ray diffraction. They are isotypic with (PPh4)2[As2SCl6] · C2H4Cl2. In the anions [M2SBr6]2- the M atoms (As or Sb) have a distorted octahedral coordination, the two octahedra share acommon face with one bridging S and two Br atoms; the lone electron pairs occupy the trans positions to the S atom. Crystal data: triclinic, space group P1, Z = 2; (PPh4)2[As2SBr6] · CH2Br2, a = 119.1, b = 1203.6, c = 2067.5 pm α= 94.89, β = 97.78, γ = 112.20°, 3046 independent observed reflexions, R = 0.083; (PPh4)2[Sb2SBr6] · CH2Br2, a = 1198.9, b = 1224.3, c = 2085.5pm, α = 95.04, β = 98.48, γ = 112.13°C, 2380 reflexions, R = 0.079.
    Notes: (PPh4)2[As2SBr6] · CH2Br2 entsteht bei der Reaktion von As2S3, PPh4I und HI in Dibrommethan. Es kann, ebenso wie (PPh4)2[Sb2SBr6] · CH2Br2, auch aus (PPh4)2[As2Br8] bzw. (PPh4)3[Sb2Br9] und Bistrimethylsilylsulfid in CH2Br2 erhalten werden. Von den beiden Titelverbindungen wurden die Kristallstrukturen durch Röntgenbeugung bestimmt. Sie sind isotyp zu (PPh4)2[As2SCl6] · C2H4Cl2. In den Anionen [M2SBr6]2- sind die Atome M (= As bzw. Sb) verzerrt oktaedrisch koordiniert, die beiden Oktaeder sind über das S- und zwei Br-Atome flächenverknüpft; die Oktaederspitze in trans-Stellung zum S-Atom wird jeweils vom einsamen Elektronenpaar eingenommen.Kristalldaten: Triklin, Raumgruppe P1, Z = 2; (PPh4)2[As2SBr6]· CH2Br2, a = 1191,1, b = 1203,6 c = 2067,5 pm, α = 94,89, β = 97,78 γ = 112,20°, 3046 unabhängige beobachtete Reflexe, R = 8,3% (PPh4)2[Sb2SBr6]·CH2Br2, a = 1198,9 b = 1224,3, c = 2085,5 pm, α = 95,04, β = 98,48, γ = 112,13°, 2380 Reflexe, R = 7,9%.
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  • 94
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 61-71 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel Beryllates of the Alkali Metals: Na6Be8O11For the first time transparent, colourless single crystals of Na6Be8O11 have been prepared (Na2O/BeO; Na:Be = 6:8, Ni-tube; 650°, 14 d). The compound crystallizes triclinic (P1) with a = 532.1(1) pm, b = 642.4(2) pm, c = 839.1(2) pm, α = 101.7°, γ = 105.8°, Z = 2, dx = 2.42 g/cm3, dpyk=2.51 g/cm3. The crystal structure was solved by four-circle diffractometer data [Siemens AED 2, MoKα, R = 7.9%, Rw = 6.2%, 1429 I0(hkl)].Effektive Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.
    Notes: Neu dargestellt wurde Na6Be8O11 in Form trikliner, farblos-durchsichtiger Einkristalle [a = 532,1(1) pm, c = 839,1(2) pm, α = 101,7°, β = 96,4°, γ = 105,8°, Z = 2, dx = 2,42 g/cm3, dpyk = 2,51 g/cm3]. Die Kristallstruktur wurde über Vierkreisdiffraktometerdaten [Siemens AED 2, MoKα, R = 7,9%, Rw = 6,2%, für 1429 von 1459 I0(hkl)] aufgeklärt. Na6Be8O11 ist gegenüber Luftfeuchtigkeit empfindlich.Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet.
    Additional Material: 7 Ill.
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  • 95
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 45-60 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel Oxoplumbates(II) with Isolated Anion Structure: Rb4[PbO3] and Cs4 [PbO3]For the first time Rb4[PbO3] have been prepared as single crystals. The structure determination (four-circle diffractometer data) [Rb4[PbO3]: 1818 I0 (hkl), MoKα, R = 6.49%, Rw = 6.83%, space group Pbca (a = 681.2(1), b = 1178.7(1), c = 1979,9(1) pm), Z = 8; Cs4[PbO3]: 3663 Io (hkl), AgKα, R = 11.35%, Rw = 9.82%, space group P21 (a = 1188.1(2), b = 734.4(1), c = 1176.2(2) pm, β = 111.52(2)°), Z = 4] proves in both cases the expected “isolated” [PbO3] groups. Comparing the oxides the arrangements of these groups shows surprising differences (see text). The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, have been calculated.
    Notes: Erstmals dargestellt wurden Rb4[PbO3] und Cs4[PbO3] in Form von Einkristallen. Nach der Strukturbestimmung mit Vierkreisdiffraktometerdaten [Rb4[PbO3]: 1818 I0 (hkl), Mokα, R = 6,49%, Rw = 6,83%, Raumgruppe Pbca (a = 681,2(1), b = 1178,7(1), c = 1979,9(1) pm), Z = 8; Cs4[PbO3]: 3663 Io (hkl), AgKα, R = 11,35%, Rw = 9,82%, Raumgruppe P21 (a = 1188,1(2), b = 734,4(1), c = 1176,2(2) pm, β = 111,52(2)°), Z = 4] liegen bei beiden Oxiden „isolierte“ [PbO3]-Gruppen von, deren Anordnung zueinander sich jedoch grundsätzlich unterscheidet, (Einzelheiten vgl. Text). Der Madelunganteil der Gitterenergie, MAPLE, und Effektive Koordinationszahlen, ECoN, werden angegeben.
    Additional Material: 3 Ill.
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  • 96
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 31-36 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Chemistry of Oxotantalates M4Ta2O9. III. A Contribution on the Crystal Chemistry of Zn4-xMgxTa2O9 and Zn2.1Mg0.9Ta2O8X-ray powder and single crystal investigations of the Zn4-xMgxTa2O9 system show the instability of the Zn4Ta2O9-type against the substitution of Mg2+ ions. In all cases of substitution, oxides of the formula Zn4-xMgxTa2O9 crystallizes with a corund related structure. The metal positions (M2+) are occupied statistically by Zn2+. Compounds of the type Zn3-xMgxTa2O8 have the structure of Zn3Nb2O8. One of the point positions is occupied by Mg2+ and Zn2+. The existence of The existence of the different structure types and the polyhedra deformation are discussed in respect to the Mg2+ contents in Zn3-xMgxTa2O8.
    Notes: Untersuchungen mit Röntgenpulver- und Einkristalltechnik im System Zn4-xMgxTa2O9 zeigen, daß beim Einbau von Mg2+ der Zn4Ta2O9-Typ verlassen wird. Alle Misch kristalle kristallisieren im aufgefüllten Korundtyp. Zn2+ und Mg2+ besetzen im Metallteilgitter die vorhandenen Positionen statistisch. Verbindungen vom Typ Zn3-xMgxTa2O8 kristallisieren nicht im Zn3Ta2O8-Typ, sondern wie Zn3Nb2O8. Eine Metallpunktlage ist mit Mg2+ und Zn2+ besetzt. Die Existenz der verschiedenen Strukturtypen und die Polyederdeformation werden im Hinblick auf den Ersatz von Zn2+ gegen Mg2+ diskutiert.
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  • 97
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 81-84 
    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 Organo Transition Metal Compounds. 53. Synthesis and Properties of Manganese Tetravinyloxide, Mn(OCH=CH2)4 · 0.5 THFTetrakis(1-Norbornyl)manganese (I) reacts with boiling tetrahydrofuran forming ethylene, norbornane, and manganese tetravinyloxide Mn(OCH=CH2)4 · 0.5 THF (II) as the first manganese tetraalcoxide. The compound was characterized by elementary analysis, the i.r. and 1H n.m.r. spectrum, the effective magnetic moment, and the protolysis products.
    Notes: Tetrakis(1-norbornyl)mangan (I) reagiert mit siedendem Tetrahydrofuran unter Abspaltung von Ethylen und Norbornan zu Mangantetravinyloxid, Mn(OCH=CH2)4 · 0,5 THF (II), als dem ersten bekannt gewordenen Mangan(IV)-alkoxid. Die Verbindung wurde durch Elementaranalyse, das IR- und 1H-NMR-Spektrum, das effektive magnetische Moment und durch die Protolyseprodukte charakterisiert.
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  • 98
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 72-80 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Method for the Identification of T-Atom Vacancies in the Lattices of ZeolitesSilanol groups in the lattices of zeolites can be silylated with trimethylchlorosilane and the products can be characterized by means of 29Si (CP) MAS NMR. T-atom vacancies are indicated by the formation of silylation products with three or four siloxy-linkages under mild reaction conditions as this requires the presence of three or silanol groups in favourable geometrical arrangements.
    Notes: Am Beispiel der Zeolithe ZSM-5 und Y wird gezeigt, wie amn Gitter-Leer-stellen in Zeolithen identifizieren kann. Terminale Hydroxylgruppen, die auch Gitter-Leerstellen umgeben, werden dabei mit Trimethylchlorsilan (TCS) silyliert und die Produkte mit 29Si-(CP)-MAS-NMR untersucht. Die Anwesenheit von Gitter-Leerstellen wird angezeigt durch die Bildung von Silylierungsprodukten mit drei oder vier Siloxybindungen, die Insertion des TCS zwischen drei beziehungsweise vier terminalen Hydroxylgruppen im Zeolithgitter unter sehr milden Reaktions bedingungen entstehen.
    Additional Material: 4 Ill.
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  • 99
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 96-100 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Tris(pyridinium)bromine-bis(bromotrichloraluminate(III))The compound [(PyH)3Br] [AlCl3Br]2 is formed by melting stoichiometric amounts of PyHBr and AlCl3 in the ratio of 3:2. It crystallizes in the space group P21 with lattice constants a= 745.6(2), b = 1415.6(2), c = 1363.1(1) pm, β = 93.00(1)°, Z = 2. The atomic parameters were refined from 2827 measured intensities to a weighted value of R = 5.8%. The cation consists of three pyridinium ions with N—H—Br-hydrogenbonds to a central positioned bromide ion. The N—Br-distances are 334(2), 330(2) and 323(3) pm.
    Notes: Die Verbindung [(PyH)3Br] [AlCl3Br]2 kann durch Zusammenschmelzen stöchiometrischer Mengen PyHBr und AlCl3 im molaren Verhältnis 3:2 erhalten werden. Sie kristallisiert in der Raumgruppe P21 (monoklin) mit den Gitterkonstanten a= 745,6(2), b = 1415,6(2), c = 1363,1(1) pm, β = 93,00(1)°, Z = 2. Zur Strukturbestimmung wurden 2827 Reflexintensitäten gemessen; es wurde ein gewichteter R-Wert von 5,8% erreicht. Das Kation dieser Verbindung besteht aus einem von drei Pyridinium-Ionen über N—H—Br-Wasserstoffbrücken koordinierte zentralen Bromid-Ion. Die N—Br-Abstände betragen 334(2), 330(2) und 323(3) pm.
    Additional Material: 4 Ill.
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  • 100
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 564 (1988), S. 101-103 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of N,N′-Bis(trimethylsilyl)-imidazoliumiodide [(Me3Si)2(C3H3N2)]+I-Me3SiI forms with N-Trimethylsiylimidazole (NTMSI) a 1:1 compound which is stable at room temperature. Single crystals can be isolated from a solution of chloroform. The X-ray crystal structure investigation proves an ionic structure.
    Notes: Me3SiI bildet mit N-Trimethylsilylimidazol (NTMSI) eine bei Raumtemperatur beständige 1:1-Verbindung. Aus einer Lösung in Chloroform lassen sich Einkristalle isolieren. Die Röntgenstrukturanalyse beweist eine ionische Struktur.
    Additional Material: 1 Ill.
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