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  • crystal structure  (124)
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  • 1
    Digitale Medien
    Digitale Medien
    Langfristige Zunahme früher Bruten beim Teichrohrsänger (Acrocephalus scirpaceus) in einem südwestdeutschen Untersuchungsgebiet (1999)
    Springer
    Journal of ornithology 140 (1999), S. 81-86 
    Details
    ISSN: 1439-0361
    Schlagwort(e): Reed Warbler ; timing of breeding ; spring arrival ; global climate change ; temperature
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung In einem Untersuchungsgebiet am westlichen Bodensee (Halbinsel Mettnau) zeichnet sich zwischen 1976 und 1997 eine deutliche Zunahme früh ausgeflogener Teichrohrsänger ab, was auf ein früheres Brüten schließen läßt. Weiterhin hat sich die Erstankunft des Teichrohrsängers am Bodensee in den letzten 16 Jahren (1982–1997) im Vergleich zum Zeitraum 1961 bis 1980 um genau eine Woche verfrüht (im Mittel vom 26.4. auf den 19.4.). Während sich zwischen der jährlichen Erstankunft des Teichrohrsängers am Bodensee und der Zahl früh ausgeflogener Jungvögel kein statistisch gesicherter Zusammenhang finden läßt, ist die Temperatur in der ersten Maihälfte ein guter (statistisch signifikanter) Indikator für die Zahl früh ausgeflogener Teichrohrsänger. Die vorliegende Untersuchung zeigt, daß sich offenbar auch Langstreckenzieher an die sich abzeichnende Klimaveränderung anzupassen beginnen.
    Notizen: Summary Data from a standardized mist-netting programme (the so-called "MRI-Programm") were used to assess the timing of breeding in Reed Warblers (Acrocephalus scirpaceus) at Lake Constance (South Germany). The number of Reed Warblers fledged early in the season increased significantly between 1976 and 1997 (rs=0.614; p〈0.01). This is most probably due to a long-term increase in spring temperature as suggested by the high correlation between the number of early-fledged Reed Warblers and mean temperature in the first half of May (rs=0.416; p〈0.01). While in the period from 1961 to 1980 the mean date of spring arrival was on the 26th of April, it shifted towards the 19th April from 1981 to 1997. However, the number of early-fledged Reed Warblers and the date of spring arrival are not significantly correlated. The lack of a significant correlation may be due to a number of reasons, for instance early arriving birds do not belong to the local population or there could be an observational bias among years. Yet, the most likely explanation is that the timing of breeding in Reed Warblers is triggered by vegetation growth and food supply rather than by the timing of spring arrival. There is growing body of evidence from this and other studies that the recent climate change is responsible for the shift in both the timing of migration and breeding in birds.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02462091
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  • 2
    Digitale Medien
    Digitale Medien
    Response of five insect herbivores to multiple allelochemicals under fluctuating temperatures (1998)
    Springer
    Entomologia experimentalis et applicata 88 (1998), S. 81-96 
    Details
    ISSN: 1570-7458
    Schlagwort(e): chlorogenic acid ; Heliothis virescens ; Manduca sexta ; Pseudoplusia includens ; rutin ; Spodoptera frugiperda ; temperature ; tomatine ; Trichoplusia ni
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Analysis of the combined effects of allelochemicals on insect herbivores is useful because there may be adverse additive or even synergistic effects. Analysis of the simultaneous effects of temperature and alleochemicals is also necessary because these factors may interact. We examined the effects of three allelochemicals found in tomato (chlorogenic acid, rutin and tomatine) and thermal regime (21:10 °C and 26:15 °C, representing spring and summer respectively) on five insect herbivores (a Solanaceae specialist, Manduca sexta, and the polyphagous Heliothis virescens, Pseudoplusia includens, Spodoptera frugiperda and Trichoplusia ni). There were allelochemical interactions and thermal regime-allelochemical interactions for all species, and so the patterns were complex. In some cases, paired allelochemicals or the combination of three allelochemicals showed adverse additive effects on insect performance. But that was not always the case, and there were only a few examples of synergism. Negative effects of the allelochemicals were sometimes, but not always, damped by the cooler thermal regime. Comparing the growth rates of the five species in this study with those of a previous study (a total of seven species) revealed five patterns. For two of three pairs of closely-related species, the paired species had distinctly different patterns. For example, for H. virescens, tomatine prevented development and chlorogenic acid slowed growth, whereas for Helicoverpa zea, tomatine just slowed growth and the phenolics had little effect. The specialist Manduca sexta had a pattern that was midway between patterns of the generalists; it was not the most tolerant of the allelochemicals.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003290510565
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  • 3
    Digitale Medien
    Digitale Medien
    Environmental effects on cytoplasmic incompatibility and bacterial load in Wolbachia-infected Drosophila simulans (1998)
    Springer
    Entomologia experimentalis et applicata 86 (1998), S. 13-24 
    Details
    ISSN: 1570-7458
    Schlagwort(e): Drosophila ; cytoplasmic incompatibility ; Wolbachia ; temperature ; antibiotics ; density
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract The effects of high temperatures, antibiotics, nutrition and larval density on cytoplasmic incompatibility caused by a Wolbachia infection were investigated in Drosophila simulans. Exposure of larvae from an infected stock to moderate doses of tetracycline led to complete incompatibility when treated females were crossed to infected males; the same doses only caused a partial restoration of compatibility when treated males were crossed to uninfected females. In crosses with treated females, there was a strong correlation between dose effects on hatch rates and infection levels in embryos produced by these females. Ageing and rearing males at a high temperature led to increased compatibility. However, exposing infected females to a high temperature did not influence their compatibility with infected males. Male temperature effects depended on conditions experienced at the larval stage but not the pupal stage. Exposure to 25 °C reduced the density of Wolbachia in embryos compared with a 19 °C treatment. Low levels of nutrition led to increased compatibility, but no effect of larval crowding was detected. These findings show the ways environmental factors can influence the expression of cytoplasmic incompatibility and suggest that environmental effects may be mediated by bacterial density.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003043814761
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  • 4
    Digitale Medien
    Digitale Medien
    Different responses to temperature in three closely-related sympatric cereal aphids (1998)
    Springer
    Entomologia experimentalis et applicata 86 (1998), S. 49-58 
    Details
    ISSN: 1570-7458
    Schlagwort(e): aphids ; Sitobion ; population ; chromosomal race ; mean relative growth rate ; temperature
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Chromosomal races of the aphid Sitobion miscanthi (Takahashi), and a closely-related species S. near fragariae (Aphididae: Macrosiphini) show seasonal differences in abundance in eastern Australia. We tested whether this was related to differences in temperature response, using controlled laboratory conditions. Intrinsic rate of increase, rm, mean relative growth rate (MRGR), and longevity were compared at different temperatures, and rates of increase were compared outdoors under ambient conditions. Using laboratory data, we simulated population growth, for comparison with outdoor populations. There were significant differences in responses to temperature regimes both in the laboratory and outdoors. Outdoor populations fell well short of predicted sizes. S. miscanthi (2n=18) showed evidence of adaptation to warmer conditions. In contrast, S. nr fragariae showed consistent evidence for adaptation to cooler conditions, and S. miscanthi 2n=17 was approximately intermediate. These data indicate that temperature responses are important in the ecology, evolution and pest status of S. miscanthi clones and S. nr fragariae in Australia.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003102927699
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  • 5
    Digitale Medien
    Digitale Medien
    Flight behavior of pre- and postdiapause apple blossom weevils in relation to ambient temperature (1998)
    Springer
    Entomologia experimentalis et applicata 88 (1998), S. 97-99 
    Details
    ISSN: 1570-7458
    Schlagwort(e): Coleoptera ; Curculionidae ; Anthonomus pomorum ; temperature ; diapause ; flight behavior
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003269621622
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  • 6
    Digitale Medien
    Digitale Medien
    Effects of temperature and photoperiod on development and oviposition of the legume flower thrips, Megalurothrips sjostedti (1999)
    Springer
    Entomologia experimentalis et applicata 93 (1999), S. 149-155 
    Details
    ISSN: 1570-7458
    Schlagwort(e): Megalurothrips sjostedti ; temperature ; photoperiod ; development ; pre-oviposition ; oviposition ; diapause
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Megalurothrips sjostedti is an economic pest of cowpea in tropical Africa. There are no reports of the effect of temperature on the development of the pest and no diapause has been detected. The developmental rate and reproduction of M. sjostedti was studied under six constant temperatures (14, 17, 20, 23, 26 and 29 °C ) and a photoperiod of L12:D12 in the laboratory. Total developmental time ranged from 33.1 days at 14 °C to 19.2 days at 26 °C. At 29 °C, all larvae died during hatching. Egg, larval and pupal stages required 94.3, 97.1 and 105.3 deg-days (DD) above a threshold of 8.2, 9.1 and 10.4 °C, respectively, to complete development. Total developmental cycle was completed at 163.9 DD above a threshold of 12.6 °C. Adult longevity was lowest (11.1 days) at 29 °C and highest (28.7 days) at 14 °C. At constant temperatures, the highest pre-oviposition period was observed at 29 °C under a photoperiod of L16:D8. Egg production also ceased at this temperature/photoperiod combination. Total fecundity was highest at 26 °C under L10:D14. At cyclical temperatures, pre-oviposition period was longest (12.4 days) at 20/29 °C under L16:D8. Total fecundity was highest (168.4 eggs) at 14/26 °C under L10:D14, and lowest (8.2 eggs) at 20/29 °C under L16:D8. The significance of these findings in the management of M. sjostedti is discussed.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003896919284
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  • 7
    Digitale Medien
    Digitale Medien
    Diapause survival and post-diapause performance in bumblebee queens (Bombus terrestris) (1998)
    Springer
    Entomologia experimentalis et applicata 89 (1998), S. 207-214 
    Details
    ISSN: 1570-7458
    Schlagwort(e): Bombus terrestris ; bumblebees ; diapause ; survival ; preoviposition period ; weight ; temperature ; diapause duration
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Diapause survival and post-diapause performance (i.e., if a queen starts to lay eggs) of in total 2210 bumblebee queens (Bombus terrestris) were measured under different diapause regimes: 5 temperatures (−5, 0, 5, 10 and 15 °C) in combination with 5 durations of exposure (1, 2, 4, 6 and 8 months). The results show that weight at the start of diapause determines to a large extent whether a queen will be able to survive diapause. Queens with a wet weight below 0.6 g prior to diapause did not survive, but for those queens exceeding this threshold a higher pre- diapause weight did not increase their post-diapause performance. There was no effect of temperature on diapause survival; 76% of the variance in survival could be explained by the duration of the treatment. Neither temperature nor duration of exposure had an effect on post-diapause performance. The preoviposition period of the queens that laid eggs was also determined. The preoviposition period was affected by both temperature and duration of exposure: the preoviposition period decreased with decreasing temperature but also with increasing duration of the treatment.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003595306816
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  • 8
    Digitale Medien
    Digitale Medien
    Influence of temperature on bionomics of cotton aphid, Aphis gossypii, on cotton (1999)
    Springer
    Entomologia experimentalis et applicata 90 (1999), S. 25-35 
    Details
    ISSN: 1570-7458
    Schlagwort(e): Aphis gossypii ; development ; survival ; fecundity ; intrinsic rate of increase ; life table ; temperature
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Life table parameters of Aphis gossypii Glover (Homoptera: Aphididae) on Gossypium hirsutum L. were determined at six temperatures (10, 15, 20, 25, 30, and 35 ± 0.5 °C) in the laboratory. Relationships of life table parameters with temperature were described with mathematical equations. Development was fastest at 30 °C, with a pre-larviposition period of 4.6 d. Survival to adult was greatest at 25 °C (81%). Fecundity was highest at 25 °C, with a total fecundity of 28.3 nymphs per female and a mean reproductive rate of 3.1 nymphs per female per day. Threshold temperatures for development in the first through fourth instar and the adult were 8.2, 8.0, 7.2, 6.2 and 7.9 °C, respectively. The durations of these stages, expressed as temperature sums above these thresholds, were 24.2, 23.7, 23.0, 25.5 and 168.8 degree-days (D°), respectively. A. gossypii achieved its maximum net reproductive number (24.4 nymphs per female) and greatest intrinsic rate of increase (0.386 d−1) at 25 °C. The high relative rate of population increase at 25 °C results in a daily population increase of 47% and a doubling time of only 1.8 d, illustrating the tremendous growth capacity of A. gossypii populations under favourable conditions. Compared to literature sources, our source of A. gossypii, fed on cotton, showed a comparatively great heat tolerance.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003580413487
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  • 9
    Digitale Medien
    Digitale Medien
    The relative performance of pheromone and light traps in monitoring the seasonal activity of both sexes of the eastern hemlock looper, Lambdina fiscellaria fiscellaria (1998)
    Springer
    Entomologia experimentalis et applicata 89 (1998), S. 87-98 
    Details
    ISSN: 1570-7458
    Schlagwort(e): seasonal trapping ; light traps ; pheromone traps ; trapping periodicity ; temperature ; reproductive state ; eastern hemlock looper
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract The seasonal flight activity of both sexes of the eastern hemlock looper, Lambdina fiscellaria fiscellaria Guenée (Lepidoptera: Geometridae) was studied during two consecutive years in Quebec and Newfoundland, using light (L), pheromone (P) and combined light and pheromone (LP) traps. Moth density significantly affected the performance of the different traps, with P traps being more effective at low than high density. However, P trap catches decreased just prior to the onset of female captures, probably as a result of competition between traps and virgin calling females. Nearly all females caught in L and LP traps were already mated and even the first females caught had laid at least half of their egg complement. In Quebec under warm nights, the pattern of male activity occurred at different times, with peak P catches being later in the scotophase than those of L traps, but overall similar numbers of males were caught in both traps. In contrast, under cool nights, males were caught early in the night in both P and L traps, suggesting a strong competition effect between traps, although more males were caught in P than L traps overall. In Newfoundland, the pattern of male captures in L and P traps was similar at both high and low temperatures, so competition between trap types would always be high. Under these conditions P traps were more effective than L traps. Irrespective of the region, year or temperature, significantly more males were captured in LP, with the effect of L and P being additive. In both regions, females responded similarly to L and LP traps with peak activity occurring early in the night. Captures of females were lower than those of males under cool temperatures, suggesting that the temperature threshold for flight is higher for females. The use of L and P traps simultaneously and/or in combination is discussed in relation to integrated pest management programs and ecological considerations.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003450432755
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  • 10
    Digitale Medien
    Digitale Medien
    The smaller fruit tortrix, Grapholita lobarzewskii: predicting the phenology of adult emergence (1999)
    Springer
    Entomologia experimentalis et applicata 93 (1999), S. 297-302 
    Details
    ISSN: 1570-7458
    Schlagwort(e): smaller fruit tortrix ; Grapholita lobarzewskii ; phenology ; post-diapause development ; temperature ; thermal threshold ; thermal constant ; forecasting ; modelling
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract The smaller fruit tortrix, Grapholita lobarzewskii Nowicki, has become a major pest in the recent past in apple orchards north of the Alps. Nevertheless little is known about the biology and the behaviour of this species. The effect of temperature on post-diapause development and survival was studied under controlled conditions in order to establish a basis for the forecasting of adult emergence. Survival was found to be highest at 17 °C and lowest at 11.8 °C. The sex ratio did not differ significantly from 1:1. Based on a linear relationship between temperature and developmental rates, thermal thresholds of 9.6 °C and 9.8 °C were determined for females and males respectively. The thermal constants, i.e., the mean developmental times in physiological time units, were found to be 342 day-degrees for females and 317 day-degrees for males, suggesting a slight protandry. Based on the mean and the variance of the developmental times, a simple temperature-driven phenology model was built using a time-varying distributed delay. The model was validated by visually comparing the predictions with independent observations on adult emergence, and by calculating the temporal deviations of the predictions. In 4 out of 5 years the mean error was less than 3 days. The model was therefore found to give reliable forecasts of the emergence of G. lobarzewskii and can be used to determine the optimal time for the exposure of pheromone traps, the application of pheromone dispensers for mating disruption, and for the timing of insecticide applications.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003905026249
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  • 11
    Digitale Medien
    Digitale Medien
    Structure of a 1:1 complex between the anthelmintic drug mebendazole and propionic acid (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 11-15 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Mebendazole–propionic acid complex ; molecular complex ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Recrystallization of the anthelmintic drug mebendazole from propionic acid yields a 1:1 molecular complex which crystallizes in the triclinic system space group $${P\bar 1}$$ , a = 5.928(2), b = 11.066(2), c = 14.337(6)Å, α = 94.89(3), β = 101.56(3), γ = 96.18(2)°, and Z = 2 complex units in the unit cell. An x-ray diffraction study revealed an R 2 2 (8) hydrogen bonding system in the complex, involving the unprotonated imidazole N and amide N–H function of the drug and the acid carboxylic group. Complex molecules form centrosymmetric dimers by intermolecular N–H···O hydrogen bonding involving the protonated imidazole N atom and the benzoyl O atom of the drug molecule.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021766300133
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  • 12
    Digitale Medien
    Digitale Medien
    Crystal structure and EPR spectra of glycilglycilglycinocopper(II)bromide sesquihydrate (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 61-68 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Cu(II) complex ; crystal structure ; EPR spectra
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound, Cu(glyglygly)Br·1·5H2O, crystallizes in the space group C2/c, with a = 21.468(7), b = 6.716(5), c = 16.166(6) Å, β = 98.39°, and Z = 8. The tripeptide is bonded to one Cu(II) ion through the nitrogen [Cu–N=1.97(1)Å] and oxygen [Cu–O=2.019(8)Å] atoms of the amino end glycine residue and to another Cu(II) through one oxygen atom [Cu–O=1.931(9)Å] of the terminal carboxyl group. This give rise to covalently bonded and infinite ···–Cu–tripeptide–Cu–··· chains. These chains are linked to one another by a network of H-bonds involving the water molecules and bromide ions. The Cu(II) ion is in a distorted tetragonal pyramidal coordination polyhedron. At the corner of the base of the pyramid are the terminal glycine nitrogen and oxygen atoms of one tripeptide, a carboxylic oxygen of another tripeptide and a bromide ion. The fivefold coordination is completed with a water molecule at the top of the pyramid [Cu–Ow=2.286(9)Å]. For all orientations of the applied magnetic field the single crystal EPR spectra display a single anisotropic exchange collapsed resonance without hyperfine structure. Its position was measured in three perpendicular planes and the crystal g-tensor evaluated from the data. This tensor is interpreted in terms of the contributing Cu(II) complexes in the unit cell to deduce the principal values g1 = 2.273, g2 = 2.050 and g3 = 2.131 for the molecular gyromagnetic tensor. We also discuss the magnitude of the exchange interaction between neighboring copper ions in the lattice on the basis of the features in the EPR spectra and the structural information.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021734820606
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  • 13
    Digitale Medien
    Digitale Medien
    Reaction of 2-methylnaphthalene with hexachlorocyclopentadiene and structural characterization of a new addition-substitution product (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 787-790 
    Details
    ISSN: 1572-8854
    Schlagwort(e): 2-Methylnaphthalene ; hexachlorocyclopentadiene ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract 2-Methylnaphthalene undergoes Diels-Alder addition and substitution with hexachlorocyclopentadiene to give two products, 1,2,3,4,5,6,7,8,13,13,14,14-dodecachloro-1,4,4a,4b,5,8,8a,12b-octahydro-10-methyl-1,4;5,8-dimethanotriphenylene 1 and 1,2,3,4,5,6,7,8,13,13,14,14-dodecachloro-1,4,4a,4b,5,8,8a,12b-octahydro-10-(1′,2′,3′,4′,5′-pentachlorocyclopentadienyl)methyl-1,4;5,8-dimethanotriphenylene 2. The molecular structure of 2 has been characterized by X-ray crystallography: C26H9Cl17, monoclinic, space group P21/c, with a = 15.316(3), b = 13.698(3), c = 16.116(3) Å, β = 96.113(3)°, and Z = 4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021819518557
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  • 14
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of [(PhenH)(PhenH2)][BiCl6]·2H2O with different o-phenanthroline protonations (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 791-796 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Halobismuthate(III) ; phenanthroline ; synthesis ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The reaction between bismuthate oxide and phen (1,10-phenanthroline) in acid medium led to the isolation of the unusual [(PhenH)(PhenH2)][BiCl6]·2H2O derivative, which has been characterized by X-ray analysis and IR spectroscopy. The compound crystallizes in the triclinic space group $$[\text[P\bar 1]]$$ with a = 8.313(2), b = 9.349(2), c = 9.807(3) Å, α = 86.39(3), β = 110.27(3) and γ = 106.48(3)°. The crystal structure is made of [BiCl6]3− anions and [(PhenH)(PhenH2)]3+ cations. A network of hydrogen bond interactions involving the two clathrated water molecules, the phenanthroline moiety and the chlorines characterizes the entire structure.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021871502627
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  • 15
    Digitale Medien
    Digitale Medien
    Tris-(thiocyanato)-bis-(hexamethylenetetramine)-nona-(aquo) lanthanum(III): synthesis, crystal structure, IR and Raman characterization (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 879-884 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Lanthanum complex ; hexamethylenetetramine ; IR spectra ; thiocyanates ; coordination number nine ; tricapped trigonal prism ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound (LaC15H42N11O9S3) was prepared and characterized by means of X-ray, IR and Raman measurements. The crystals are orthorhombic: Pnma (No. 62), a = 21.117(2), b = 14.736(2), c = 10.082(1) Å, and Z = 4. The structure consists of polyhedra with a La(III) ion in the center of them and hexamethylene molecules, which link these polyhedra. Each La(III) ion coordinates seven molecules of water and two thiocyanate ions via nitrogen atoms. The IR and Raman spectra, which have been obtained and interpreted, are in good agreement with X-ray results.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022846402229
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  • 16
    Digitale Medien
    Digitale Medien
    Preparation and crystal structures of the Ce(IV) β-diketonates, [Ce(tmhd)4] and [Ce(pmhd)4] (tmhd =2,2,6,6-tetramethylheptane-3,5-dionate and pmhd = 1-phenyl-5-methylhexane-1,3-dionate) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 267-276 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Cerium(IV) ; β-diketonate ; volatility ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The cerium(IV) β-diketonate compounds [Ce(β-diket)4] [where β-diket = tmhd (2,2,6,6-tetramethylheptane-3,5-dionate) 1, pmhd (1-phenyl-5-methylhexane-1,3-dionate) 2] were prepared by reacting cerium(IV) ammonium nitrate [CAN; Ce(NH4)2(NO3)6] with the respective Na(β-diket) compound in ethanol, and structurally characterized by single crystal X-ray diffraction. Compound 1 crystallizes in the triclinic space group $$P \bar 1$$ with a = 12.472(4), b = 19.972(5), c = 21.436(3) Å, α = 97.05(7), β = 90.16(2), γ = 106.55(3)°, V = 5076(2) Å3, Z = 4, T = 150(2) K. Compound 2 crystallizes in the monoclinic space group P21/n. with a = 14.817(6), b = 17.123(6), c = 19.146(3) Å, β = 105.46(4)°, V = 4682(3) Å3, Z = 4, T = 150(2) K. Crystals of 1 contain two independent [Ce(tmhd)4] molecules, with four chelating tmhd ligands bonded to each metal in a distorted dodecahedral arrangement; the cerium atom in 2 is also bonded to four chelating pmhd ligands but in this case the coordination geometry is closer to square antiprism. Both complexes are air and moisture stable. Sublimation studies reveal that 1 sublimes almost quantitatively, while 2 is comparatively involatile.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021897102260
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  • 17
    Digitale Medien
    Digitale Medien
    Molecular structure and spectral characteristics of bis(S-methyl-N-(2-pyridyl)methylendithiocarbazato)nickel(II), (Ni(NNS)2) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 871-874 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Nickel(II) complex ; crystal structure ; Schiff base
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract A nickel(II) complex of the pyridine-2-aldehyde Schiff base of S-methyldithiocarbazate (HNNS) has been synthesized and characterized by means of elemental analysis, IR and UV-vis spectra. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The complex crystallizes in the monoclinic, space P21/c, with a = 14.092(2), b = 16.886(2), c = 8.857(2)Å; β = 105.78(3) °, V = 2028.2(6) Å3, and Z = 4. The nickel atom is octahedrally coordinated by two uninegatively charged tridentate Schiff base in a mer-configuration via the pyridine nitrogen atom, azomethine nitrogen atom, and mecaptide sulfur atom.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022842301321
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  • 18
    Digitale Medien
    Digitale Medien
    Benztropine mesylate: crystal structure and kinetics of dehydration (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 885-892 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Benztropine mesylate ; crystal structure ; thermal analysis ; dehydration kinetics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal structure of benztropine mesylate has been determined. It is orthorhombic, Pbca, with a = 12. 885(8)Å, b = 32.012(9)Å, and c = 10.027(3) Å. It exhibits similar packing to that seen in the previously reported crystal structure of benztropine mesylate monhydrate. X-ray powder diffraction patterns have been used to identify the anhydrous and monohydrate forms. The dehydration of the monohydrate follows a first-order reaction mechanism with activation energy of 92(8) kJ mol−1.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022898419067
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  • 19
    Digitale Medien
    Digitale Medien
    Synthesis and X-ray crystallographic characterization of [Cd(NO3)2(15-Crown-5)] and [Cd(NO3)2(18-Crown-6)] (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 521-527 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Cadmium ; crown ether ; 15-crown-5 ; 18-crown-6 ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Reaction of 15-crown-5 or 18-crown-6 in 3:1 (v/v) CH3CN:CH3OH with Cd(NO3)2·4H2O followed by slow evaporation produces [Cd(NO3)2(15-crown-5)] or [Cd(NO3)2(18-crown-6)]. Crystals of [Cd(NO3)2(15-crown-5)] are orthorhombic with space group Pbca and cell parameters a = 13.562(5), b = 15.941(9), and c = 15.011(7) Å at 295 K. [Cd(NO3)2(18-crown-6)] crystallizes in the monoclinic space group C2/c with a = 11.235(2), b = 11.196(5), c = 15.385(3) Å, and β = 99.89(2)° at 295 K. The metal center in [Cd(NO3)2(15-crown-5)] rests atop the macrocyclic donor array with two cis-bound nitrate anions and adopts a distorted tricapped trigonal prismatic geometry. [Cd(NO3)2(18-crown-6)] resides on an equatorial two-fold rotation axis with Cd2+ coordinated in the 18-crown-6 cavity and the nitrate anions oriented in twisted trans positions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1023239921542
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  • 20
    Digitale Medien
    Digitale Medien
    The crystal and molecular structure of (−)—Crinine (C16H17NO3) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 577-579 
    Details
    ISSN: 1572-8854
    Schlagwort(e): (−)—Crinine ; Pancratium ; alkaloid ; Amaryllidaceae ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract (−)—Crinine, C16H17NO3, is an alkaloid extracted from the bulbs of Pancratium maritimum L. (Amaryllidaceae). The compound crystallizes in the space group P212121 with cell dimensions a = 6.040(1), b = 12.382(1), c = 17.861(2) Å, with Z = 4. The molecule has five rings and an OH group. The N-containing, five-membered ring and the D ring have envelope conformations. The A and B rings have distorted chair and half-chair conformations, respectively.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1023256425176
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  • 21
    Digitale Medien
    Digitale Medien
    Crystal structure of 2,2,4,7,7-pentamethyl-3,6-dithiaoctane tetracarbonyl tungsten(0) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 217-220 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Metal carbonyl complexes ; chelate complexes ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The x-ray crystal structure of the complex η2-PDOW(CO)4 (five-membered ring, PDO = 2, 2, 4, 7, 7-pentamethyl-3,6-dithiaoctane) is reported. The complex crystallizes in the monoclinic crystal system, space group P21/c, [#14] with unit cell parameters a = 14.002(14) Å, b = 9.340(10) Å, c = 15.094(12) Å, β = 92.67(4)°, V = 1972(3) Å3; Z = 4. The arrangement of the ligands around the metal atom is distorted from octahedral geometry. Large C–O bond distances and short W–C bond distances of the carbonyl groups located at a trans position with respect to PDO is indicative of a trans influence. The W–S(1) and W–S(2) bond distances of 2.545(3) and 2.545(2) Å, respectively, are shorter than observed for closely related complexes.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022478528825
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  • 22
    Digitale Medien
    Digitale Medien
    Crystal structure of tris(triphenylsiloxy)borane·triphenylsilanol (1:1) adduct (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 277-281 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Triphenylsiloxy ; silanol ; borane ; crystal structure ; adduct
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound crystallizes in the triclinic space group $$P \bar 1$$ , with a = 14.458(6), b = 14.630(5), c = 14.721(8) Å, α = 79.75(2), β = 80.11(3), γ = 80.50(3)°, and Z = 2. The crystal structure consists of molecules of (Ph3SiO)3B and Ph3SiOH linked by an weak B···(silanol) acceptor-donor bond, additionally stabilized by OH(silanol)···O(siloxy) hydrogen bonds. The average B–O, Si–O distances and B–O–Si angle are 1.369, 1.649 Å and 137.2°, respectively.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021849219098
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  • 23
    Digitale Medien
    Digitale Medien
    17α-acetoxy-17β-methyl-16β-phenyl-D-homo-4,6-pregnadiene-3,17a-dione: synthesis and crystal structure determination of a new rearranged pregnane derivative (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 487-491 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Steroid ; pregnadiene ; x-ray diffraction ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound is C29H34O4, tetragonal, P43, a = b = 10.310(1), c = 23.871(2)Å. The A, B, C, and D rings adopt envelope, half-chair, chair, and distorted chair conformations, respectively. The phenyl ring is planar. The methyl substituents at the A/B, C/D, and at C(17) are axial; and the –OCOCH3 group at C(17) and phenyl ring at C(16) are equatorial. The molecules in the crystal are held together by van der Waals forces and several C–H···O hydrogen bond interactions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021729007943
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  • 24
    Digitale Medien
    Digitale Medien
    Structure, absolute configuration, and conformation of the antimalarial compound, Artemisinin (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 539-543 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Antimalarial ; crystal structure ; peroxy bridge
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal and molecular structure of the antimalarial compound Artemisinin (formerly known as Qinghaosu), C15H22O5 has been determined by direct methods. Crystals are orthorhombic colorless needles, space group P212121, Z = 4. D c = 1.299 g cm −3, with unit cell parameters a = 6.3543(9), b = 9.439(3), c= 24.066(4) Å. The molecule incorporates a fused ring system containing a six-membered ring C which includes an oxygen bridge and a peroxy-bridge. The ring C has a distorted boat conformation and the C - O - O - C torsion angle is 47.8(2)°. Rings A and D have symmetrical chair and distorted chair conformations, repectively. Ring junctions A/B, A/D, and C/D are cis, junction B/D is trans. All inter-molecular contacts are van der Waals. The absolute configuration of Artemisinin was determined from the refined value of the Flack x parameter. [The atomic coordinates given in a previous structure analysis, “Crystal Structure and Absolute Configuration of Qinghaosu,” Qinghaosu Research Group, Institute of Biophysics, Academica Sinica, Scientia Sinica, Vol. XXIII No. 3, 380 (1980), do not display the molecule in its absolute configuration.]
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1023244122450
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  • 25
    Digitale Medien
    Digitale Medien
    Crystal structure of [Mn2(III)(salpa)2Cl2(H2O)2] (H2salpa = 1-(salicylaldeneamino)-3-hydroxypropane) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 203-206 
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    ISSN: 1572-8854
    Schlagwort(e): Manganese(III) ; Schiff base ; hydrogen bonding ; crystal structure ; Jahn-Teller distortion
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The manganese complex, (Mn2(III)(salpa)2Cl2(H2O)2], has been prepared and its structure determined using x-ray crystallography. The dimer is a di-μ2-alkoxo complex which is a six-coordinate manganese dimer with unsupported alkoxide bridges and a rare example of a chloride- and water-containing manganese dimer. The complex crystallizes in the monoclinic space group P21/c with a = 9.315(5), b = 11.130(4), c = 11.637(5) Å, β = 104.33(3)°, V = 1169.0(9) Å3, and Z = 2. The structure comprises discrete binuclear clusters in which the metal atoms are bridged by two alkoxo oxygens of the salpa2− ligands. The Mn—O and Mn—N distances are in good agreement with those found for other manganese(III) Schiff base complexes. The Mn—Cl and Mn—O3 distances are 2.585(2) and 2.371(2) Å, respectively, and the Mn ··· Mn distance is 3.001(1) Å. In the crystal, there are two types of hydrogen bonding between the H2O molecule and the Cl atom with Cl ··· H(H2O) distance of 2.33(6) (intramolecule: −1 + x, y, −1 + z) and 2.68(6) Å (intermolecule: −1 + x, 0.5−y, −0.5 + z).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009526312170
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  • 26
    Digitale Medien
    Digitale Medien
    Molecular structure of ThBr4(DME)2 (DME = 1,2-dimethoxyethane) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 243-246 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Thorium ; dimethoxyethane ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The molecular structure of ThBr4(DME)2 (DME = 1,2-dimethoxyethane), the first structurally characterized thorium complex containing a simple bidentate ether ligand, is described. The eight-coordinate complex presents a distorted dodecahedral geometry, with Th—Br and Th—O bond lengths in the ranges 2.8516(13)–2.8712(13) Å and 2.564(8)–2.620(8) Å, respectively. ThBr4(DME)2 is monoclinic, space group P21/n, a = 7.672(1), b = 14.581(1), c = 15.847(2) Å, β = 102.24(1)°, V = 1732.4(3) Å3, and Z = 4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009542715804
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  • 27
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of the copper(II) complex with novel Schiff base ligand: Cu(C8H7O2N)2(OH2) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 295-298 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Copper ; crystal structure ; synthesis ; Schiff base ligand
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title complex Cu(C8H7O2N)2(OH2) crystallized in the orthorhombic space group, Pbca with unit cell parameters: a = 15.242(2), b = 11.782(4), c = 17.946(4) Å, and Z = 8. Two nitrogen atoms, two phenolic oxygen atoms of the ligand, and one water molecule are coordinated with copper to form a distorted tetragonal pyramidal polyhedron.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009569701034
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  • 28
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structures of quadruply carboxylate-bridged dimeric lanthanide(III) complexes of betaine (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 309-316 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Europium ; terbium ; betaine ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Three dimeric lanthanide(III) complexes, [Eu2(bet)8(H2O)4](CIO4)6 (1), [Tb2(bet)8(H2O)4](ClO4)6 (2), and [Eu2(bet)4(H2O)8] Cl6·6H2O (3) (bet = Me3N+CH2COO−, trimethyl-aminoacetate), have been prepared and structurally characterized by X-ray crystallography. Complex 1 crystallizes in the monoclinic space group P21/c, with a = 11.7807(8), b = 27.757(5), c = 11.7980(8) Å, β = 99.500(4)°, V = 3805.1(8) Å3, and Z = 2. Complex 2 is isomorphous to complex 1, crystallizing in the monoclinic space group P21/c, with a = 11.7769(14), b = 27.725(3), c = 11.795(5) Å, β = 99.668(14)°, V = 3797(2) Å3, and Z = 2. Complex 3 crystallizes in the orthorhombic space group Pbca, with a = 12.5664(8), b = 17.8645(9), c = 22.2573(8) Å, V = 4996.6(4) Å3 and Z = 4. Both complexes 1 and 2 comprise quadruply carboxylate-O,O′-bridged [M2(bet)4]6+ dimeric cores (M = Eu, Tb), and each metal ion is further coordinated by two terminal aqua ligands and two monodentate bet carboxylates to form a distorted square-antiprismatic coordination geometry. Complex 3 also has a [Eu2(bet)4]6+ core, in which two bet ligands act in the η1:η1:μ2 bridging fashion, and the other two bet ligands in the less common η2:η1:μ2 bridging fashion, namely bridging-chelate mode. Each europium(III) ion in complex 3 is further coordinated by four water molecules to complete a monocapped square antiprism.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009573801943
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  • 29
    Digitale Medien
    Digitale Medien
    Copper, a chemical Janus: two copper(II) complexes with different ligand in one single crystal (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1085-1088 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; copper(II) complexes ; dinuclear complexes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract A chemical Janus, binuclear copper(II) complexes, {[Cu(TPA)Cl][Cu(BPA)Cl]}(ClO4)2 (TPA = Tris(2-pyridylmethyl) amine, BPA = bis-(2-pyridylmethyl)amine) containing two different ligands has been synthesized and characterized by X-ray single crystal analysis. Crystal data: triclinic, space group P1$sm, a = 12.529(3), b = 12.655(3), c = 13.458(3) Å, α = 70.48(3), β = 67.40(3), γ = 75.81(3)°, D x = 1.648 mg m−3, and Z = 2. The molecular structure shows that the binuclear copper complex consists of two positive cation and two perchlorate anions. The positive cations moieties have different ligands. Cu(1) is coordinated by four nitrogen atoms from TPA and one chloride atom, forming a square-pyramidal geometry, whereas the coordinate number of Cu(2) is four, three of which are from BPA, one from chloride. There are two weak bonds between the Cl(2a) ion and the Cu(2) ion (2.844 Å) and the distance of Cu(2)=O(13) is 2.750(9) Å.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009549506565
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  • 30
    Digitale Medien
    Digitale Medien
    Molecular gears: Structures of (9,10-triptyceno) crown ethers (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 513-521 
    Details
    ISSN: 1572-8854
    Schlagwort(e): nanotechnology ; molecular devices ; triptycene ; crown ether ; crystal structure ; thallium
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The incorporation of 9,10-triptycene unit in a crown ether is examined from a structural perspective. Insertion of a triptycene group into 18-crown-6 stretches the crown into an ellipse, as seen in structures presented here of 9,10-triptyceno-22-crown-6 and its thallium complex. Symmetric addition of two triptycene groups into 18-crown-6 results in the sterically congested bis(9,10-triptyceno)-26-crown-6, whose crown cavity is filled with the π-clouds of two arene groups. The larger bis(9,10-triptyceno)-32-crown-8 is more sterically relaxed. The structures of these bis(triptyceno)crown ether molecules are the first with two triptycene groups simultaneously linked through their 9 and 10 positions, thereby forming a simple molecular gearing mechanism. The compound 9,10-triptyceno-22-crown-6 (1) crystallizes in the orthorhombic space group Pbca with a = 10.7962(7), b = 15.826(3), c = 31.147(5) Å, V = 5321.8(12) Å3, and Z = 8; its complex with TlNO3 (Tl-1) crystallizes in the monoclinic space group P21/c with a = 8.1884(14), b = 19.552(2), c = 20.575(4) Å, β = 97.062(8)°, V = 3269.2(9) Å3, and Z = 4; bis(9,10-triptyceno)-26-crown-6 (2) crystallizes in the triclinic space group P $$\bar 1$$ with a = 8.6488(11), b = 10.7718(12), c = 12.3324(12) Å, α = 111.58(1), β = 100.55(1), γ = 106.43(1)°, V = 970.3(5) Å3, and Z = 1; and bis(9,10-triptyceno)-32-crown-8 (3) crystallizes in the orthorhombic space group Pna21 with a = 20.186(3), b = 8.558(2), c = 25.623(2) Å, V = 4426.2(14) Å3, and Z = 4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009535632237
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  • 31
    Digitale Medien
    Digitale Medien
    The structure of bis(trimethylammonium) undecachlorotriantimonate(III) [(CH3)3NH]2Sb3Cl11 containing a novel antimony(III) anion (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 555-560 
    Details
    ISSN: 1572-8854
    Schlagwort(e): alkylammonium chloroantimonates(III) ; hydrogen bonds ; disorder ; lone electron pair ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The structure of [(CH3)3NH]2Sb3Cl11 (space group P21/n; a = 10.374(2), b = 23.723(5), c = 11.884(2) Å, β = 113.46(3)°; V = 2682.9(9) Å3) consists of a structurally novel [Sb3Cl2− 11] anion and two crystallographically nonequivalent trimethylammonium cations. The anion is composed of three deformed octahedra in the asymmetric part of the unit cell. The octahedra are connected with each other by edges and corners forming a characteristic polyanionic layer. Trimethylammonium cations, one ordered and one disordered, are connected to the inorganic sublattice by N—H· · ·Cl hydrogen bonds.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009592618124
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  • 32
    Digitale Medien
    Digitale Medien
    Crystal structure of the Λ-[4M] enantiomer of cis-diaqua-bis(1,3-dimethylpteridine-2,4(1H,3H)-dione-N5,O4) copper(II) perchlorate monohydrate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 571-574 
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    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; complexes ; pteridine ; lumazine
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Single-crystal X-ray diffraction studies have been performed on the complex cis-diaqua-bis(1,3-dimethylpteridine-2,4(1H,3H)-dione-O4,N5) copper(II) perchlorate monohydrate, [Cu(DLM)2(H2O)2](ClO4)2 · H2O. This compound crystallizes in the orthorhombic system, P212121 space group, Z = 4 with a = 8.749(1) Å, b = 14.213(1) Å, c = 21.200(2) Å, and V = 2636.2(4) Å3. The metal ion is surrounded in octahedral geometry by two mutually quasi-perpendicular N5,O4-coordinated lumazine chelators with the O4 atoms trans and the N5 atoms cis. The polyhedron is completed by two cis-coordinated water molecules. The absolute configuration of the complex can be described, following Bailar's nomenclature, as the enantiomer Λ of the stereoisomer 4M. A three-dimensional hydrogen-bond network is defined by water molecules, perchlorate anions, and the O2 of the pteridine A.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009548803103
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  • 33
    Digitale Medien
    Digitale Medien
    Synthesis and characterization of the dodecanuclear heterobimetallic Mo—Cu—S cage cluster: (Ph4P)2[{Mo2Cu2O2S2(S2)2}3(μ6-S)] (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 581-586 
    Details
    ISSN: 1572-8854
    Schlagwort(e): dodecanuclear heterobimetallic ; molybdenum-copper cluster ; cage ; μ6-S ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The complex (Ph4P)2[Mo2S2O2(S2)(S4)] reacts with CuBr to give the dodecanuclear heterobimetallic Mo—Cu—S cage cluster: (Ph4P)2[{Mo2Cu2O2S2(S2)2}3(μ6-S)] (1), which crystallizes in the triclinic space group P1¯, a = 14.445(5), b = 15.396(5), c = 18.858(5) Å, α = 103.12(3), β = 101.93(2), γ = 113.92(3)°, and V = 3517(2) Å3 for Z = 2. The anion 1 can be described as a cage with S2− at the center binding to six Cu atoms; the cage has two big windows each composed of a puckered Cu3S6 9-membered ring.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009552904012
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  • 34
    Digitale Medien
    Digitale Medien
    Crystal and molecular structure of five coordinate copper(II) complex with 2,6-bis[1-(methoxycarbonylmethyl–hydrazono)ethyl] pyridine (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 575-580 
    Details
    ISSN: 1572-8854
    Schlagwort(e): copper(II) complexes ; 2,6-diacetylpyridine derivative ; open-chain ligand ; crystal structure ; trigonal-bipyramidal geometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound was obtained by a template synthesis from 2,6-diacetylpyridine, ethylhydrazinoacetate and CuCl2·2H2O (molar ratio 1:2:1, in methanol), and its structure has been determined by single-crystal X-ray diffraction: monoclinic space group P21/c, a = 13.906(5), b = 18.199(6), c = 16.641(6) Å, β = 107.18(3)°, and z = 4. The ligand was found to be tridentate in a trigonal-bipyramidal coordination geometry with two chloride ligands. There are two independent complex molecules, one of which is hydrogen bonded to the water of crystallization.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009500919942
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  • 35
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of the heterometallic square-chain polythiometalate: {[W4Ag5S16]2 · [La(DEF)2(DMF)6][La(DEF)4(DMF)4]}n (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 629-633 
    Details
    ISSN: 1572-8854
    Schlagwort(e): heterometallic polymeric cluster ; polythiometalate ; synthesis ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The complex (NH4)2 WS4 reacts with AgNO3 and La(NO3)3 · 6H2O in a mixture of DEF/DMF (DEF—N,N′-diethylformamide), to give a new heterometallic square-chain polythiometalate {[W4Ag5S16]2 · [La(DEF)2(DMF)6] · [La(DEF)4(DMF)4]}n (1). 1 crystallizes in the monoclinic space group P2/c, a = 19.5534(8), b = 16.9552(6), c = 22.3479(9) Å, β = 106.053(1)°, V = 7120.1(5) Å3, and Z = 2. The anion polymeric chain of 1 can be regarded as an octanuclear cyclic cluster of [W4Ag4S16]4− fragments linked through Ag+ ions. The polymeric chain is extended through the parallel edges of the square unit. The mean W—Ag distance is 2.963(16) Å. The La3+ cations are coordinated by different solvent molecules, the average La—O bond of these large trivalent cations is 2.47(1) Å.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009517423576
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  • 36
    Digitale Medien
    Digitale Medien
    Absolute configuration of C23H34O8Si, the product of an asymmetric synthesis involving the Rh(II) catalyzed reaction of a chiral vinyldiazomethane with methyl-2-methyl-3-furoate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 707-711 
    Details
    ISSN: 1572-8854
    Schlagwort(e): oxabicyclo[3.2.1]octadiene ; absolute configuration ; asymmetric synthesis ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The compound under investigation crystallizes in the noncentrosymmetric orthorhombic space group P212121 with a = 7.9358(11), b = 11.0532(13), c = 29.2425(43) Å, volume = 2565.0(6) Å3, and Z = 4. The C23H34O8Si molecule contains three chiral centers (one of which is of known configuration, based upon an (R)-pantolactone auxillary group). We have determined the absolute configuration of this species (via the anomalous dispersion of Si relative to C and O) and show that it is consistent with the known configuration of the (R)-pantolactone moiety.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009532106081
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  • 37
    Digitale Medien
    Digitale Medien
    Absolute configuration of C20H30O6Si, a species with a (1R,5R)-8-oxabicyclo[3.2.1]octa-2,6-diene core produced selectivity by the rhodium(II) octanoate catalyzed decomposition of a chiral vinyldiazomethane in the presence of furan (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 713-717 
    Details
    ISSN: 1572-8854
    Schlagwort(e): oxabicyclo[3.2.1]octadiene ; absolute configuration ; asymmetric synthesis ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The compound under investigation crystallizes in the noncentrosymmetric monoclinic space group P21 with a = 9.1798(23), b = 6.6606(18), c = 17.6591(41) Å, β = 94.342(20)° and Z = 2. The C20H30O6Si molecule contains three chiral centers (one of which is of known configuration, based upon an (R)-pantolactone auxiliary group). We have determined the absolute configuration of this species (via the anomalous dispersion of Si relative to C and O) and show that it is consistent with the known configuration of the (R)-pantolactone moiety
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009584122919
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  • 38
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of 1,1′-di(ethylpropionato)-2,2′-biimidazole, a macromolecular precursor (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 765-768 
    Details
    ISSN: 1572-8854
    Schlagwort(e): 2,2′-biimidazole ; diester ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract 1,1,′-Di(ethylpropionato)-2,2′-biimidazole, C16H22N4O4, crystallizes from ice-cold ethanol in the space group P $$\bar 1$$ , with a = 4.6742(9), b = 9.1119(13), c = 10.175(2) Å, α = 96.22(1), β = 96.29(2), γ = 97.53(1)°, and Z = 1. The molecule crystallizes with coplanar rings and the substituents assume a trans conformation with a center of inversion between the bridging carbon atoms.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009535501461
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  • 39
    Digitale Medien
    Digitale Medien
    The crystal and molecular structure of mercury(II) bis(isopropyl)dithiophosphate, Hg[S2P(OPri)2]2, revisited: new comments about its supramolecular self-organization (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 831-836 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Hg coordination ; crystal structure ; organomercury derivatives
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal structure of the title compound, Hg[S2P(OPri)2]2, has been determined by single-crystal X-ray diffraction. The compound crystallizes in the centrosymmetric P21/c space group with a = 11.800(1), b = 8.925(2), c = 22.167(2) Å, β = 94.988(7)°, and Z = 4. The same compound has been previously reported but the structure is described there in the space group C2/c. In both cases, one phosphorodithioate moiety acts as a chelating group and the other as a bridging group between neighboring mercury atoms (related to one another by the twofold screw axis), giving rise to an infinite polymer along the direction of the b axis. It turns out that in spite of the difference in space group symmetry, the structures are remarkable similar in that they are formed from infinite polymers of similar geometry. The coordination around the Hg ion shows, however, significant differences, mainly for the bridging Hg—S(4) bond length, which is 0.16 Å smaller than that previously reported.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009508122842
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  • 40
    Digitale Medien
    Digitale Medien
    Generation and intermolecular trapping of a cage-annulated cycloalkylidenecarbene (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 329-333 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Carbene ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Base-promoted reaction of 11-methylenepentacyclo[5.4.0.02,6.03,10.05, 9]undecan-8-one (5) with diethyl diazomethylphosphonate when performed in the presence of excess cyclohexene, resulted in the formation of the corresponding cycloalkylidenecarbene, 6, which subsequently was trapped in situ to afford 8-methylene-11-(7′-bicyclo[4.1.0]heptylidene)pentacyclo-[5.4.0.02, 6.03, 10.05, 9]undecane (7, obtained in 44% yield as a mixture of exo, endo isomers). Subsequent reaction of 7 with dichlorocarbene (generated under phase transfer catalytic conditions) produced the corresponding mono- and di-:CCl2 adducts [i.e., 8 (64% yield) and 9 (5% yield), respectively]. The structure of 9 was established unequivocally via application of single crystal X-ray analysis: Triclinic, P1¯, a = 6.276(2), b = 8.700(2), c = 18.550(3) Å, α = 76.52(3), β = 87.59(3), γ = 70.88(4)° Z = 2; D calc 1.486 g cm−3.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009530019690
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  • 41
    Digitale Medien
    Digitale Medien
    Crystal structure of the addition compound of N,N′-bi(2-pyridylmethyl)-oxamide and complex of manganese with 1,10-phenanthroline (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 623-627 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; manganese complex ; disubsituted oxamide ; addition compound
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The structure of the addition compound, Mn(phen)3(PMoxdH2)(ClO4)2 was established by X-ray crystallography, where PMoxdH2 is N,N′-bi(2-pyridylmethyl)-oxamide. Six nitrogen atoms of the three 1,10-phenanthroline bind to the manganese ion and the oxygen atom of PMoxdH2 is uncoordinated. The addition compound crystallizes in the monoclinic space group C2/c, with lattice parameters a = 23.780(6), b = 11.948(5), c = 18.466(6) Å, β = 117.38(3)°, V = 4659(3) Å3, and Z = 4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009565306738
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  • 42
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structures of two potential gem-di(pyrazolyl)cycloalkane ligands, 1,1-di(pyrazol-1-yl)cyclohexane [C6H10(C3N2H3)2] and 1,1-di(pyrazol-1-yl)cyclopentane [C5H8(C3N2H3)2] (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 659-665 
    Details
    ISSN: 1572-8854
    Schlagwort(e): pyrazolyl derivative ; substituted cyclopentane ; substituted cyclohexane ; crystal structure ; bidentate ligand
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The species 1,1-di(pyrazol-1-yl)cyclohexane, C12H16N4, crystallizes in the monoclinic space group P21/c with a = 8.340(2), b = 14.281(5), c = 10.153(3) Å, β = 106.86(2)°, and Z = 4. The cyclohexane moiety has the chair conformation. The congener, 1,1-di(pyrazol-1-yl)cyclopentane, C11H14N4, while not isomorphous, also crystallizes in space group P21/c with a = 14.350(2), b = 6.776(1), c = 11.043(2) Å, β = 100.68(1)°, and Z = 4. The cyclopentane ring has a conformation in which four carbon atoms are essentially coplanar, while the fifth (that with the two pyrazolyl substituents) lies 0.63 Å from this plane, resulting in a bend of 41.3° across the C(2)···C(5) vector. The hydrogen atoms in each structure were located directly and their coordinates refined.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009515602446
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  • 43
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 719-723 
    Details
    ISSN: 1572-8854
    Schlagwort(e): synthesis ; crystal structure ; independent molecules
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The x-ray crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one has been determined. Yellow block shaped crystals of C9H10OS4 crystallize in the space group P $${\bar 1}$$ with cell dimensions a = 8.872(4), b = 9.330(8), c = 14.333(12) Å, α = 95.23(7), β = 91.09(5), γ = 107.60(5)°, V = 1124.8(14) Å3, and Z = 4. This compound has two S---S contacts [3.574, 3.610 Å] shorter than 3.70 Å and the usual disordered ethylene moiety [C(3)—C(8)] of the six-membered ring is fixed by the cis-cyclohexylene subsitituent. This means that it may be a new precursor for conducting and strong near-IR absorbing nickel-dithiolenes. Also, it provides the first example of polymorphism of the dmit derivatives and contains two independent molecules I and II in the asymmetric unit.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009536206989
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  • 44
    Digitale Medien
    Digitale Medien
    The crystal and molecular structure of 2-S-methylthiouracil (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 725-727 
    Details
    ISSN: 1572-8854
    Schlagwort(e): 2-thiouracil derivatives ; crystal structure ; S-methyl-thiouracil ; hydrogen bonding ; structural methylation and metallation effects
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract 2-S-Methylthiouracil crystallizes in the triclinic space group P $${\bar 1}$$ with unit cell dimensions a = 5.508(4), b = 7.175(3), c = 8.522(2) Å, α = 80.83(2), β = 80.43(3), γ = 76.86(3)°, and Z = 2. The molecule exists in the crystal in the lactam form and is essentially planar. The molecular packing consists of molecules linked in centrosymmetric hydrogen-bonded pairs. The effects of methylation and subsequent metallation on the 2-thiouracil structure are discussed.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009588223827
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  • 45
    Digitale Medien
    Digitale Medien
    Crystal structure and emission study of [(PPh3)2Cu(dmp)-O-(dmp)Cu(PPh3)2]2+ (dmp = 2,9-dimethyl-1,10-phenanthroline) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 797-802 
    Details
    ISSN: 1572-8854
    Schlagwort(e): synthesis ; crystal structure ; Cu(I) complex ; μ-oxo-bis(2,9-dimethyl-1,10-phenanthroline) ; luminescence
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The synthesis and crystal structure of a luminescent dinuclear Cu(I) complex as the BF− 4 salt from toluene and methanol containing triphenylphosphine and μ-oxo-bis(2,9-dimethyl-1,10-phenanthroline) is described. The coordination geometry about the Cu(I) center is distorted tetrahedral. An unusual feature of the structure is a pseudo-inversion center located near the oxygen atom at approximately 0.51, 0.26, 0.25, such that all of the atoms except for the oxygen are related by a pseudo-inversion center to another atom in the same molecule, as well as by crystallographic inversion to the other molecule in the unit cell. The complex displays luminescence from an MLCT band in fluid solution and emission from both a metal-centered charge-transfer and intraligand (phenanthroline) state at 77K in a chloroform snow. Crystal data: triclinic, P $$\bar 1$$ , a = 15.163(2), b = 16.985(2), c = 18.731(2) Å, α = 106.458(9), β = 91.416(8), γ = 102.557(9)°, V = 4496(1) Å3, and Z = 2.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009595720117
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  • 46
    Digitale Medien
    Digitale Medien
    Structural analysis of tris(tetra-n-butylammonium) hexakisisothiocyanatoyttrate(III) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 729-733 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; yttrium complexes ; isothiocyanate complexes ; octahedral coordination
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The structural analysis of [(n-C4H9)4N]3[Y(NCS)6] (I) using single-crystal diffraction data and full-matrix least squares refinement has been carried out. The hexaisothiocyanate complex crystallizes in the centrosymmetric triclinic space group P $${\bar 1}$$ (No. 2) with unit cell constants of a = 12.431(1), b = 12.866(1), c = 22.750(2) Å, α = 90.78(1), β = 92.05(1), γ = 96.67(1)°, and Z = 2. The molecular unit consists of three separate cationic tetra-n-butylammonium groups and an independent hexakisisothiocyanatoyttrate anionic group in which the six thiocyanate ligands are octahedrally coordinated through the N atom to the Y central ion. Selected bond distances and angles are presented as well as the synthesis and peripheral studies of (I).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009540307898
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  • 47
    Digitale Medien
    Digitale Medien
    Synthesis and structure of bis(dibenzoylmethane)copper(II) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 793-796 
    Details
    ISSN: 1572-8854
    Schlagwort(e): copper complex ; crystal structure ; dibenzoylmethane complex
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Bis(dibenzoylmethane)copper Cu(dbm)2 has been synthesized and its structure determined by x-ray diffraction. It crystallizes in the monoclinic system, space group C2/c, with a = 25.936(3), b = 5.9806(8), c = 16.4908(16) Å, β = 114.998(8)°, Z = 4, and V = 2318.3(4) Å3. The Cu atom is located at a symmetry center and surrounded by four O atoms from two dbm molecules to form a plane square coordination environment. On the a–c plane the molecules are orderly arranged to result in a layered structure, and parallel to crystallographic b-axis they form a molecular column due to the effect of aromatic stacking.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009543703278
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  • 48
    Digitale Medien
    Digitale Medien
    Crystal structure of [WBr2(CO)(PPh2Cy)2(η2-MeC2Me)]·CH2Cl2 (Cy = cyclohexyl) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 809-812 
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    ISSN: 1572-8854
    Schlagwort(e): tungsten(II) ; dibromo ; carbonyl ; diphenylcyclohexylphosphine ; but-2-yne ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract [WBr2(Co)(PPh2Cy)2(η2-MeC2Me)]·CH2Cl2 (Cy = cyclohexyl) crystallizes in the monoclinic space group, P21/n, with a = 10.606(12), b = 23.11(3), c = 18.19(2) Å, β = 106.070(10) Dcalc = 1.610g cm−3 for Z = 4. The tungsten coordination geometry can best be considered as a distorted octahedron, with the but-2-yne ligand occupying one coordination site, which has a trans-Br(2) group. The equatorial plane is made up of trans-PPh2Cy groups, with the bromo and carbonyl ligands occupying the other two sites.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009599821025
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  • 49
    Digitale Medien
    Digitale Medien
    1-(Ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil: a nucleoside analog (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 837-839 
    Details
    ISSN: 1572-8854
    Schlagwort(e): acyclonucleoside analog ; 6-(phenyl selenyl) uracil derivative ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The compound, 1-(ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil, crystallizes in the monoclinic space group P21/n with unit cell parameters a = 5.304(1), b = 21.261(4), c = 13.996(4) Å, β = 94.30(2)°, and Z = 4. The acyclic chain C1′, O4′, C4′, C5′ is in fully extended form and nearly perpendicular to the uracil base. The molecules are held together by van der Waal's forces.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009560106913
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  • 50
    Digitale Medien
    Digitale Medien
    Mercury(II) halide complexes with N-donor organic ligands: crystal and molecular structure of HgI2R, R = 1,10-phenanthroline, 2,9-dimethyl-1,10-phenanthroline, bipyridine (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 825-830 
    Details
    ISSN: 1572-8854
    Schlagwort(e): mercury halides ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The synthesis, characterization and single crystal X-ray structure of three compounds of general formula HgI2R (R = phen[1], dmph [2] and bpy[3]) are presented. The crystal data for the three compounds are: [1], triclinic, space group P $$\bar 1$$ (#2) a = 7.902(2), b = 9.479(2), c = 10.002(2) Å, α = 91.45(2), β = 111.34(2), γ = 100.82(2)° [2]: monoclinic, space group C2/c (#15) a = 15.670(3), b = 11.640(2), c = 9.730(2) Å, β = 114.57(3)° [3]: triclinic, space group P1¯ (#2) a = 9.472(1), b = 9.507(1), c = 9.023(1) Å, α = 98.46(1), β = 102.89(1), γ = 119.62(1)°. Compounds [1] and [2] are monomers, with highly distorted tetrahedral environments around Hg. In [3], instead, there is a significant intermolecular I···Hg interaction leading to the formation of softly bound dimers linking two pentacoordinated cations. The structure is compared with related ones in the literature.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009556006004
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  • 51
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of [WI(CO)(cis-dppen) η2-MeC2Me)2]I·CH2Cl2 {cis-dppen = bis(diphenylphosphino)ethene} (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 907-911 
    Details
    ISSN: 1572-8854
    Schlagwort(e): tungsten(II) ; Iodo ; carbonyl ; cis-bis(diphenylphosphino)ethene ; but-2-yne ; cationic ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The complex [WI(CO)(cis-dppen)(η2-MeC2Me)2]I·CH2Cl2(1) is prepared as a by-product from the reaction of equimolar quantities of [WI2(CO)(NCMe)(η2-MeC2Me)2] and cisdppen {dppen = bis(diphenylphosphino)ethene}. Complex 1, [WI(CO)(cis-dppen)(η2-MeC2Me)2]I·CH2Cl2 crystallizes in the triclinic space group $${\text{P}}\bar 1$$ with a = 11.189(13), b = 12.331(14), c = 15.395(17) Å, α = 83.61(1), β = 86.06(1), γ = 64.48(1)°, U = 1904 Å3, and Z = 2. The metal environment in the cation can best be considered as a distorted octahedron with the two but-2-yne groups taking up individual sites trans to phosphorus atoms of the dppen ligand. The coordination sphere is completed by mutually trans-carbonyl and iodide groups.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009526012075
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  • 52
    Digitale Medien
    Digitale Medien
    4-(1,4-Dimethoxy-2-naphthyl)-4- hydroxycyclohexanone and its ethylene ketal (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 955-959 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; intramolecular hydrogen bond ; 4-(1,4-dimethoxy-2-naphthyl)-4-hydroxycyclohexanone
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Intramolecular hydrogen bonding in the solid state is reported for the title compound and its ethylene ketal. The title compound crystallizes in the triclinic space group, $$P\bar 1$$ with a = 9.590(3), b = 9.620(3), c = 9.844(2) Å, α = 97.67(2), β = 105.25(2), γ = 115.47(2), and Z = 2. The ethylene ketal crystallizes in the monoclinic space group, P21/c, with a = 7.230(2), b = 22.639(3), c = 10.839(2) Å, β = 101.47(2), and Z = 4. The intramolecular hydrogen bond length of 1.79 Å is the same for the ketone and ketal, but the O—H---O valence angle is 144° for the ketone and 165° for the ketal.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009538414801
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  • 53
    Digitale Medien
    Digitale Medien
    Crystal structure and physical characterization of neotame methanol solvate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 967-975 
    Details
    ISSN: 1572-8854
    Schlagwort(e): neotame ; crystal structure ; methanol solvate ; thermal analysis ; powder X-ray diffractometry ; 13C solid-state nuclear magnetic resonance spectroscopy
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal structure of the methanol solvate (empirical formula: 2C20H30N2O5·3CH3OH) of a new dipeptide sweetener, neotame (N-(3,3-dimethylbutyl)-L-α-aspartyl-L-phenylalanine 1-methyl ester), has been determined. Crystal data: a = 9.8989(1), b = 18.1331(1), c = 27.5725(1) Å, orthorhombic, space group P212121, with Z = 4. Each unit cell includes 8 neotame and 12 methanol molecules. Disorder exists in one neotame molecule and one methanol molecule. The crystals were characterized by the following techniques: hot-stage microscopy (HSM), Karl-Fischer titrimetry (KFT), powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC), thermogravimetry (TGA), 13C solid-state nuclear magnetic resonance (SSNMR) spectroscopy. Under HSM at a heating rate of 10°C/min in silicone oil, the sample melts at 64–84°C and liberates bubbles at 71–86°C. DSC in open pans shows two overlapping endotherms at 56 and 71°C, probably due to melting and desolvation, respectively. TGA in open pans shows 5.9% weight loss due to desolvation below 70°C. Under house vacuum (23 mm Hg) over phosphorus pentoxide at 23°C, the methanol solvate produces pure amorphous anhydrate, which converts to crystalline neotame monohydrate in the presence of moisture.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009542515709
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  • 54
    Digitale Medien
    Digitale Medien
    A study of two geometric isomers of 1,1′-bi-3-cyanocyclohex-2-enylidene (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 977-982 
    Details
    ISSN: 1572-8854
    Schlagwort(e): cyano allyl radical ; thermal arrangement ; crystal structure ; isomer ; NMR, MM2
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The preparation, separation, crystal structure and 1H NMR spectra are reported for the two geometrical isomers of 1,1′-bi-3-cyanocyclohex-2-enylidene. The E-isomer crystallized as thin plates in the monoclinic space group P21/n with a = 5.3980(5), b = 7.0757(7), c = 15.300(2) Å, β = 94.571(2)°, and Z = 2. The structure has symmetry C2h. The Z-isomer crystallized as needles in the triclinic space group P1¯ with a = 7.0790(6), b = 11.3155(9),c = 15.386(1) Å, α = 104.943° β = 90.164(2)°, γ = 99.494(2)°, and Z = 4. The compound crystallized with two molecules per asymmetric unit. In C6D6, 1H NMR signals of the 2-vinyl protons appear almost identical. However, in a mixture of C6D6 and pyridine-d 5, the 2-vinyl protons can be distinguished. The structures compare favorably with MM2 calculations.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009594532547
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  • 55
    Digitale Medien
    Digitale Medien
    X-ray crystal structure of tetraaquabis (xanthosinato)nickel(II) hexahydrate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1009-1013 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; nickel complex ; xanthosine
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The complex [Ni(XsH−1)2(H2O)4]·6H2O (XsH−1: xanthosinate) was isolated from the reaction of nickel carbonate with xanthosine in aqueous solution. The octahedral coordination is supported by the reflectance measurements. Single-crystal X-ray diffraction studies show that the crystals belong to the triclinic P1 space group, with a = 7.152(1), b = 8.830(1),c = 13.783(1) Å, α = 82.024(1)°, β = 86.155(1)°, γ = 70.900(1)°, and D = 1.643 mg/m3, forZ = 1. Nickel is six coordinate with four water molecules, and two N7 atoms from xanthosinato ligands. A complicated hydrogen-bonding network is present, all possible donors taking part in it.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009568616134
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  • 56
    Digitale Medien
    Digitale Medien
    Reactions of [Mn2(μ-pyS)2(CO)6] (pySH=pyridine-2-thiol) with triphenylphosphine (PPh3), diphenylphosphine (PHPh2) and bis(diphenylphosphino)methane (dppm): X-ray crystal structure of [Mn(pyS)(η1-dppm)2(CO)2] (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1001-1007 
    Details
    ISSN: 1572-8854
    Schlagwort(e): manganese ; pyridine-2-thiolate ; bis(diphenylphosphino)methane ; carbonyl ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The dimeric complex [Mn2(μ-pyS)2(CO)6] (1) reacted with 2 M equivalents of both PPh3 and PHPh2 to give the respective monomeric phosphine complexes [Mn(pyS)(L)(CO)3][L = PPh3 (2) and PHPh2 (3)]; with 4 M equivalents of dppm, it yielded the complex [Mn(pyS)(η1-dppm)2(CO)2](4). An X-ray structure determination of 4 shows that it crystallizes in the monoclinic space group P21/n with a = 11.027(3), b = 24.984(7), c = 18.379(5) Å, β = 99.870(8)°, V = 4988(2) Å3, and Z = 4. The complex has an octahedral geometry with the chelating pyS ligand and two CO groups occupying the equatorial sites and the two monodentate dppm ligands lying in the trans positions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009516632064
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  • 57
    Digitale Medien
    Digitale Medien
    Crystal structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1037-1041 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; imidazolidine ; triazene ; bis-triazene ; methoxy substituent ; π-π stacking
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal and molecular structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine (1) has been determined by single crystal X-ray diffraction analysis. This novel bis-triazene assumes a close-to planar structure with the aryltriazene moieties aligned in diametrically opposed directions, unlike many other previously reported bis-triazenes, which assume a folded structure. The structure of 1 is compared with the closely related, non-cyclic bis-triazene analogue (2), and also compared with the structure of the simple mono-triazene (3). Crystal data: 1 C17H20N6O2, monoclinic, space group C2/c, a = 34.948(3), b = 5.925(5), c = 8.1225(6) Å, β = 100.8420(10)°, and V = 1652.0(2) Å3, for Z = 4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009529002022
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  • 58
    Digitale Medien
    Digitale Medien
    Crystal structure of 2-{(R)-1-hydroxy-1-[(2S)-1-tritylaziridin-2-yl] methyl}acrylate and spectroscopic properties of the (R,S) and (S,S) stereoisomers (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1053-1056 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; tritylaziridine ; acrylate ; spectroscopic features
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal and molecular structure of 2-{(R)-1-Hydroxy-1-[(2S)-1-tritylaziridin-2-y1] methy1}acrylate is described. Crystal data: C26H25NO3, orthorhombic, space group P212121, a = 9.6954(5), b = 13.1458(5), c = 16.7885(7) Å, V = 2139.8(2) Å3, Z = 4. The (R,S) diastereomer shows an intramolecular hydrogen bonding N···H—O under formation of a five-membered ring with N···O distance of 2.664 Å. IR, 1H NMR and 13C NMR data are discussed. The 1H NMR of the (R,S) diastereomer shows a singlet- whereas the (S,S) diastereomer exhibits a doublet-pattern for the hydroxyl proton.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009585119769
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  • 59
    Digitale Medien
    Digitale Medien
    Absolute configuration of C27H41NO8Si, the diastereoselective product of the rhodium(II) octanoate catalyzed decomposition of a chiral vinyldiazomethane in the presence of 2-acetylpyrrole: A structural study rendered difficult by disorder of a “heavy” atom (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1061-1066 
    Details
    ISSN: 1572-8854
    Schlagwort(e): absolute configuration ; asymmetric synthesis ; azabicyclo[3.2.1]octadiene ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound crystallized in space group P21 with a = 12.647(8), b = 14.542(4), c = 17.077(16) Å, β = 97.51(6)°, and D calc = 1.143 mg/m3 for Z = 4. There are two chemically-equivalent C27H41NO8Si molecules in the crystallographic asymmetric unit. Each contains three chiral centers, one of known absolute configuration based upon the (R)-pantolactone,—CH*—CMe2—CH2—O—CO—, moiety. The structural study was greatly complicated by disorder of an —OSiMe2(t-Bu) group in one molecule.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009589220678
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  • 60
    Digitale Medien
    Digitale Medien
    Cluster Complexes of Polythioether Macrocycles: The Synthesis and Molecular Structures of Ru6(CO)13(cis-SCH2 CHMe(CH2SCH2CHMe)2CH2)(μ6-C) and Ru6(CO)13(trans-SCH2 CHMe(CH2SCH2CHMe)2CH2)(μ6-C) (1998)
    Springer
    Journal of cluster science 9 (1998), S. 93-105 
    Details
    ISSN: 1572-8862
    Schlagwort(e): Ruthenium ; thioether macrocycle ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Maschinenbau , Physik
    Notizen: Abstract The reaction of a mixture of cis-3,7,11-trimethyl-1,5,9-trithiacyclododecane, cis-Me312S3, 1 and trans-3,7,11-trimethyl-l,5,9-trithiacyclododecane, trans-Me312S3, 2, with Ru6(CO)17(μ 6-C), 3, yielded three new cluster compounds Ru6(CO)13(μ-η3-cis-SCH2CHMe(CH2SCH2CHMe)2CH2)(μ 6-C) 4, and two isomers of Ru6(CO)13(μ-η3-cis-SCH2CHMe(CH2SCH2CHMe)2CH2)(μ 6-C) 5a and 5b. The molecular structures of 4 and 5b were established by single crystal X-ray diffraction analyses. In both complexes, the macrocycles have adopted tridentate coordination with one of the sulfur atoms in a bridging position. Two carbonyl ligands occupy bridging positions in each compound. Crystal Data for 4·Me2CO: space group=P21/n, a=11.295(1) Å, b=17.547(3) Å, c=20.318(3) Å, β=93.71(1)°, Z=4, 2900 reflections, R=0.025. Crystal Data for 5b·1.5 C6H6: space group=Pbca, a=31.8900(8) Å, b=23.4330(6) Å, c=21.6240(4) Å, Z=16, 12163 reflections, R=0.040.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022681523508
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  • 61
    Digitale Medien
    Digitale Medien
    The First New Hydrogen-Bonded Heterohexanuclear Complex [(salen)Cu]4[(salen)Fe(H2O)2]2(ClO4)2: Molecular and Crystal Structure and Magnetic Properties (1998)
    Springer
    Journal of cluster science 9 (1998), S. 465-471 
    Details
    ISSN: 1572-8862
    Schlagwort(e): Mixed-metal cluster ; crystal structure ; magnetic properties
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Maschinenbau , Physik
    Notizen: Abstract The preparation, magnetic properties, and crystal structure of [(salen)Cu]4[(salen)Fe(H2O)2]2(ClO4)2 via hydrogen bonding are described [salen=N,N′-ethylenebis (salicylideneiminate)]. Crystals are triclinic, of space group $$\rm P\bar 1$$ , with cell constants a=12.853(3), b=13.921(3), c=14.251(3) Å, α=68.68(3)°, β=87.86(3)°, γ=86.82(3)°, and Z=1. The structure was solved and refined to R=0.064 and R′=0.068. The structure comprises the hexanuclear units which result from the linking of four mononuclear fragments [(salen)Cu] and two mononuclear fragment [(salen)Fe(H2O)]+, through Cu -O ⋯ H -O -Fe -O -H ⋯ O -Cu hydrogen bonds of coordinating H2O. In this complex, FeIII ions are in almost square-planar surroundings. The temperature dependences of the magnetic susceptibilities of the complex have been studied in the 4.2–300 K range, indicating the presence of an antiferromagnetic interactions between metal ions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021990516837
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  • 62
    Digitale Medien
    Digitale Medien
    Direct Evidence for Metal Triangle Mobility within a Relatively Rigid Ligand Polytope: Dynamic Disorder in the X-Ray Crystal Structures of Ru3(CO)11(L), L=CN t Bu, PMe3, and Ru3(CO)9{P(OMe)3}3 (1998)
    Springer
    Journal of cluster science 9 (1998), S. 505-528 
    Details
    ISSN: 1572-8862
    Schlagwort(e): Dynamic disorder ; crystal structure ; ruthenium cluster
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Maschinenbau , Physik
    Notizen: Abstract The disorder in the X-ray crystal structures of Ru3(CO)11(L), L=CN t Bu 1 and PMe3 3 has been re-examined. Crystallographic data for 1 at 100 K: C16H9NO11Ru3, space group P21/n, a=11.796(5), b=11.748(2), c=16.040(7) Å, β=109.81(3)°, Z=4, 6077 reflections, R=0.028. For 3 at 223 K: C14H9O11PRu3, space group P21/n, a=8.5971(15), b=12.391(7), c=40.345(8) Å, β=94.43(2)°, Z=8, 7966 reflections, R=0.031. The disorder present in 1 and 3 at room temperature disappears reversibly on cooling, showing that it is dynamic in origin. The ligator atoms of the isonitrile and phosphine ligands move by a maximum of ∼0.8 Å, indicating that the whole cluster does not rotate intact within the crystal lattice, but rather that the Ru3 triangle effectively oscillates within a relatively rigid ligand polyhedron. The crystal structure of Ru3(CO)9{P(OMe)3 3} 7, which crystallizes in triclinic (7-t) and monoclinic (7-m) modifications is also reported. Both modifications have two independent molecules in the asymmetric unit, and both modifications display dynamic disorder in the metal framework. Crystalllographic data for 7-t at 173 K: C18H27O18P3Ru3, space group P-1, a=11.8085(18), b=15.915(2), c=17.350(3) Å, α=99.929(14), β=101.811(14), γ=90.630(12)°, Z=4, 11242 reflections, R=0.048. For 7-m at 120 K: C18H27O18P3Ru3, space group P21/c, a=11.708(8), b=15.922(5), c=33.950(10) Å, β=99.29(4), Z=8, 10191 reflections, R=0.027.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021946701816
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  • 63
    Digitale Medien
    Digitale Medien
    Temperature Effects on Soil Mineralization of Polylactic Acid Plastic in Laboratory Respirometers (1999)
    Springer
    Journal of polymers and the environment 7 (1999), S. 101-108 
    Details
    ISSN: 1572-8900
    Schlagwort(e): Polylactic acid ; temperature ; respirometers ; soil degradation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Energietechnik , Maschinenbau
    Notizen: Abstract A respirometric system was used to analyze the biodegradation of high molecular weight (120,000 to 200,000 g mol−1) polylactic acid (PLA) plastic films in soil under laboratory conditions. The respirometric system consisted of air-conditioning pretraps, a soil reactor, and a carbon dioxide (CO2) posttrap. A 200-g homogeneous soil mixture of all-purpose potting soil : manure soil : sand [1 : 1 : 1 (w/w)] and 1.5 g of PLA plastic films in 1 × 1-cm2 squares was added to each bottle. The respirometers were placed in a 28, 40, or 55°C water bath for 182 days. Treatments (three replicates) included native corn starch (positive control), polyethylene (Glad Cling Wrap; negative control), and three PLA films: Ca-I (Cargill Dow Polymers LLC, monolayer), GII (Cargill Dow Polymers LLC, Generation II), and Ch-I (Chronopol; monolayer). The degree of polymer mineralization was indicated by the cumulative CO2 liberated from each respirometer. The initial average mineralization rate and total percentage mineralized of the PLA plastic films at 28, 40, and 55°C was 24.3, 41.5, and 76.9 mg/day with a 27, 45, and 70% carbon loss, respectively. No decrease in soil pH was observed after 182 days of mineralization. Hence, increase in soil temperature drastically enhanced the biodegradation of PLA plastic films in soil under laboratory conditions (P 〈 0.0001).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021812418325
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  • 64
    Digitale Medien
    Digitale Medien
    Electroless deposition of Ni–B, Co–B and Ni–Co–B alloys using dimethylamineborane as a reducing agent (1998)
    Springer
    Journal of applied electrochemistry 28 (1998), S. 559-563 
    Details
    ISSN: 1572-8838
    Schlagwort(e): electroless Ni–Co–B alloy ; dimethylamineborane ; complexing agent ; deposition rate ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Elektrotechnik, Elektronik, Nachrichtentechnik
    Notizen: Abstract Fundamental aspects of electroless Ni–B, Co–B and Ni–Co–B alloys have been systematically examined. The composition, crystal structure and deposition rate of the alloys were determined as a function of the concentration of reducing agent (dimethylamineborane) and complexing agents (tartrate, citrate, malonate and succinic acid), bath pH and Ni2+/Co2+ ratio. Changes in the deposition rate and metallurgical features of the alloys induced by the change in plating parameters are discussed, based on electrochemical polarization data and the formation enthalpy of the nickel and cobalt borides.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003233715362
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  • 65
    Digitale Medien
    Digitale Medien
    Structural and magnetic properties of a syn-anti carboxylate bridged one-dimensional copper(II) complex with ferromagnetic exchange interaction (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 771-777 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Copper ; 1,10-phenanthroline ; trifluoroacetate ; crystal structure ; magnetic exchange
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The compound [Cu(phen)(O2CCF3)2]n (phen = 1,10-phenanthroline) has been synthesized and its crystal structure determined. It crystallizes in monoclinic space group C2/c, with a = 19.229(7), b = 11.281(5), c = 7.621(2) Å, β = 104.305(12)°, and Z = 4. The crystal structure is polymeric, being built from infinite zigzag chains of trifluoroacetate bridged copper(II), with the phenanthroline ligands being stacked between the chains. The variable-temperature (13–300 K) magnetic susceptibility and ESR data are reported and a weak ferromagnetic exchange interaction is observed with the exchange parameter estimated as J = 2.9 cm−1.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021820729518
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  • 66
    Digitale Medien
    Digitale Medien
    Crystal structure of chloro(dicarbonyl) bis(acetonitrile) (π-2-methallyl) molybdenum(II) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 839-841 
    Details
    ISSN: 1572-8854
    Schlagwort(e): π-allyl ; carbonyl ; nitrile ; chloro ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound crystallizes in the monoclinic spacegroup P21/m with a = 6.796(9), b = 12.145(14), c = 7.749(8)Å, β = 101.86(1)°, and Z = 2. The crystal structure consists of molecules of [MoCl(CO)2(NCMe)2(η3-C3H4Me-2)] with crystallographically imposed Cs symmetry and has a pseudo-octahedral geometry, with the π-allyl group trans- to the chloro group and the two cis-carbonyl and acetonitrile groups occupying the equatorial plane.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021836022191
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  • 67
    Digitale Medien
    Digitale Medien
    The true nature of a complex of 1,10-phenanthroline with the ammonium ion; crystal structure of bis-phenanthrolineprotium perchlorate (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 611-619 
    Details
    ISSN: 1572-8854
    Schlagwort(e): 1,10-Phenanthroline ; bis-phenanthrolineprotium ; adduct ; crystal structure ; hydrogen bonding
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Herzog's reported bis-1,10-phenanthrolineammonium perchlorate, [(phen)2(NH4)](ClO4) is in fact the known 2:1 adduct of l,10-phenanthroline (phen) with perchloric acid, [(phen)2H](CIO4). Its crystal structure, mode of formation, and properties are described. The compound crystallizes in the triclinic space group with $$P\bar 1$$ , a = 7.2510(8), b = 13.120(2), c = 22.083(12) Å, α = 77.4550(12), β = 84.45(2), γ = 82.204(14)°, V = 2026.7(6) Å3, Z = 4, and D c = 1.510 g cm−3. It contains cationic columns of alternating 1,10-phenanthroline and its conjugate acid.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022460909589
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  • 68
    Digitale Medien
    Digitale Medien
    Crystal structure of the cytotoxic marine alkaloid 2-bromoleptoclinidinone (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 645-648 
    Details
    ISSN: 1572-8854
    Schlagwort(e): 2-Bromoleptoclinidinone ; marine alkaloid ; cytotoxic ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract 2-Bromoleptoclinidinone methanol solvate, C18H8BrN3O·CH4O, crystallizes in the orthorhombic space group Pbca with a = 15.7013(2), b = 7.3308(1), and c = 26.9326(1) Å. The molecule is essentially planar, with the largest deviations occurring at bromine (−0.21 Å), carbonyl oxygen O(l) (+0.19 Å) and in ring-A (C(9) −0.15 Å, C(10) −0.15 Å). Methanol occupies the 1,10-phenanthroline-like metal binding site of the title compound.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022421328245
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  • 69
    Digitale Medien
    Digitale Medien
    Crystal structure of [Co(bipy)(maleato) (H2O)3]·H2O (bipy = 2,2′-bipyridine) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1081-1084 
    Details
    ISSN: 1572-8854
    Schlagwort(e): cobalt(II) ; bipyridine ; maleato ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Preparation of the mononuclear cobalt(II) complex, [Co(bipy)(maleato) (H2O)3]·H2O (1) where bipy = 2,2′-bipyridine, were accomplished by reaction of an aqueous solution containing sodium maleate and an ethanolic solution of Co(NO3)2·6H2O and bipy. The crystal structure of complex (1) was determined by X-ray crystallography. The complex crystallizes in the monoclinic space group P21/n with a = 9.477(3), b = 7.660(2), c =23.526 (3) Å, β = 97.64(2)°, V = 1692.6(6) Å3, and Z = 4. The structure consists of discrete mononuclear cobalt molecules. The cobalt atom is six-coordinate and presents a slightly distorted octahedral geometry, which consists of the two imine N atoms of bipy, a terminal carboxylate O atom from maleato ligand, and a water O atom in the basal plane with Co—N bond distances of 2.116(2) and 2.124(3) Å and Co—O distances of 2.075(2) and 2.088(2) Å, respectively. The relatively shorter Co—O distances are due to the trans effect of the bipy ligand. The octahedral coordination is completed the other two water molecules. The coordinate and the lattice water molecules were identified by TG study.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009597422495
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  • 70
    Digitale Medien
    Digitale Medien
    Crystal and molecular structure determination, TGA, DTA, and infrared and Raman spectra of rubidium nitroprusside monohydrate, Rb2[Fe(CN)5NO]·H2O (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 75-80 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Rubidium nitroprusside monohydrate ; crystal structure ; properties
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal structure of rubidium nitroprusside monohydrate, Rb2[Fe(CN)5NO] · H2O, has been determined from X-ray diffraction data and refined using direct and Fourier methods to R = 0.066 and Rw = 0.075, employing 1894 independent reflections with I 〉 3 (I). The substance crystallizes in the monoclinic space group C2/c (C 6 2h), with a = 13.987(2), b = 10.241(1), c = 18.151(1) Å, β = 110.94°, and Z = 8. Anions are located at C 1 sites, one per asymmetric unit, and are slightly distorted octahedra. TGA, DTA, FTIR, and FTIR Raman results were interpreted on the basis of the formula of the compound, its crystal structure, and the behavior of other nitroprussides.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009575415668
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  • 71
    Digitale Medien
    Digitale Medien
    Crystal structure of methyl trans-3-[(2-(methoxycarbonyl)phenyl)sulfinyl]acrylate: a product resulting from trapping of a sulfenic acid by methyl propiolate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1133-1136 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; methyl propiolate ; sulfenic acid ; vinyl sulfoxide ; leinamycin
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Evidence for the formation of unstable sulfenic acids (RSOH) as reaction intermediates is commonly provided by trapping these compounds with methyl propiolate. The crystal structure of a vinyl sulfoxide derived from the trapping of a sulfenic acid with methyl propiolate is reported here. The title compound C12H12O5S crystallized in the triclinic space group,P1¯ with unit cell parameters: a = 6.1600(4), b = 9.7286(7), c = 11.3698(8) Å, α = 112.024(1), β = 94.662(1), γ = 95.429(1)°, and Z = 2.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009518127038
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  • 72
    Digitale Medien
    Digitale Medien
    9[1-(2-Hydroxy ethoxy)-3-hydroxy propyl] guanine: a nucleoside analog (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1137-1139 
    Details
    ISSN: 1572-8854
    Schlagwort(e): acyclic nucleoside analog ; acyclovir ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The compound 9[1-(2-hydroxy ethoxy)-3-hydroxy propyl] guanine crystalizes in the tetragonal system, space group P41212 with a = 11.106 (1), c = 20.558 (2) Å, and Z = 8. The acyclic chain C1′¯O1′¯C4′¯C5′¯O5′ is in the extended configuration and the glycosidic torsion angle (C4¯N9¯C1′¯O1′) is 125.1 (8)°. The molecules are held together by Van der Waal's forces.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009570111108
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  • 73
    Digitale Medien
    Digitale Medien
    Structure, thermal behavior, and IR investigation of a new organic sulfate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1205-1210 
    Details
    ISSN: 1572-8854
    Schlagwort(e): organic sulfate ; crystal structure ; DTA/TG/DSC ; vibrational spectra
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract [1-(2-ammoniumethyl) piperazinium] sulfate denoted PIPS has a monoclinic unit cell. The parameters are: a = 6.6521(3), b = 7.8756(5), c = 19.197(1) Å, β = 94.43(1)° and the space group is P21/n. The preparation, thermal analysis, and IR spectrometric investigation are described. The PIPS structure exhibits a complex three-dimensional network of H-bonds connecting all its components.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009559718165
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  • 74
    Digitale Medien
    Digitale Medien
    Structure of de-oxy corticosterone-21-hemisuccinate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1265-1269 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; corticosteroid ; de-oxy corticosterone-21-hemisuccinate
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Synthetic glucocorticoid de-oxy corticosterone-21-hemisuccinate crystallizes in the monoclinic space group C2, with a = 21.896(2), b = 7.596(3) and c = 14.291(3) Å, Z = 4. Ring A is a distorted half chair, ring B and C are in the chair configuration and ring D is in the 14α-half chair configuration. The ring junctions B/C and C/D are both trans. The molecule as a whole is slightly convex towards the β-side, with an angle of 18.4(2)° between the C(10)--C(19) and C(13)--C(18) vectors. In addition to packing and stacking interaction, intermolecular hydrogen bonding plays an important role in structural association. The X-ray structure determination of the title compound was undertaken to study its high binding affinity to serum protein like globulin.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009504923424
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  • 75
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of 1-phenyl-3-methylthio-4-imino-5-allyl-pyrazolo[3,4-d]pyrimidine (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1291-1293 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; pyrazolo[3,4-d]pyrimidine ; fungicidal activity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound 1-phenyl-3-methylthio-4-imino-5-allyl-pyrazolo[3,4-d]pyrimidine, C15H15N5S, has been synthesized and characterized by x-ray diffraction: orthorhombic, space group Pbca, with a = 17.3480(9), b = 8.5022(5), c = 19.8132(11) Å. Z = 8, V = 2922.4(3) Å3. The compound shows a fully delocalized pyrazolo[3,4-d]pyrimidine system with a sp2 hybridization of the N(4) atom.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009565209312
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  • 76
    Digitale Medien
    Digitale Medien
    Crystal structure of [Mn(II)(phen)(ClCH2COO)2]n (phen = 1,10−phenanthroline) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 199-201 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Manganese (II) ; phenanthroline ; polymeric complex ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract A new polymeric manganese(II) complex, [Mn(II)(phen)(ClCH2COO)2]n, was obtained from the reaction of Mn(ClCH2COO)2 with phen and its structure was determined by x-ray crystallography. The complex crystallizes in the monoclinic system, space group C2/c with a = 19.706(4), b = 11.381(3), c = 7.482(3) Å, β = 94.01(3)°, V = 1674.0(8) Å3, and Z = 4. The structure consists of an infinite chain. The manganese atom is located on a twofold axis and presents a distorted octahedral coordination sphere, which consists of the two N atoms of a phen ligand (Mn—N = 2.304(2) Å) and four carboxylato ligands. The Mn···Mn distance within the chain is 4.53 Å, and the carboxylato bridges present a syn-anti conformation.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009574128099
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  • 77
    Digitale Medien
    Digitale Medien
    Synthesis of a new dibenzo-14-crown-4 lariat ether and structure of its sodium perrhenate complex (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1255-1259 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crown ether ; crystal structure ; lariat ; sodium
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract A dibenzo-14-crown-4 ether with a novel monooxyacetone sidearm is prepared and its structure with sodium perrhenate is determined. The structure crystallizes in P21/c with cell dimensions: a = 8.107(2) Å, b = 28.138(3) Å, c = 10.293(2) Å, and β = 104.173(9)°; giving a volume of 2276.6(7) Å3. This structure is compared to other sodium complexes of dibenzo-14-crown-4 lariat ethers and is found to be the only one with intramolecular bonding between the sidearm and the cation. Possible reasons for this observation are discussed.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009552806586
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  • 78
    Digitale Medien
    Digitale Medien
    Structure of de-oxy corticosterone (4-pregnen-21-ol-3,20-dione) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1271-1275 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; pregnen ; progestin ; 4-pregnen-21-ol-3,20-dione
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Synthetic steroid de-oxy corticosterone (4-pregnen-21-ol-3,20-dione) crystallizes in the monoclinic space group P21, with a = 11.706(2); b = 11.171(3), c = 13.966(3) Å, and β = 100.94(2)°, Z = 4. Ring A tends to acquire the conformation of a half-boat, rings B and C are in the chair configuration, and ring D is a 13β, 14α-half-chair. The ring junctions B/C and C/D are both trans, whereas the ring junction A/B is quasi-trans. The molecule as a whole is slightly convex toward the β-side, with an angle of 16.01(0.36)° between the C10--C19 and C13--C18 vectors. Molecular packing and stacking interactions play the major role in structural association. Cohesion of the crystal is due to van der Waals interactions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009556907495
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  • 79
    Digitale Medien
    Digitale Medien
    Polymeric copper(II)-orotato complexes, [(C5H2N2O4)Cu(H2O)2]n (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 565-569 
    Details
    ISSN: 1572-8854
    Schlagwort(e): orotic acid complex ; crystal structure ; copper(II) complex
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The compound [(C5H2N2O4)Cu(H2O)2]n has been synthesized and its structure determined at room temperature. The primary coordination sphere at the Cu ion is square planar with the orotate dianion coordinating at the metal through heterocyclic nitrogen atom and adjacent oxygen of the carboxylate group, the remaining coordination sites are occupied by two water molecules. The orotate dianion is tricoordinated to one copper via N1 and one oxygen of the carboxylato group and to another copper atom via the other oxygen of the carboxylato group. The coordination at copper is extended to five by the other oxygen of the carboxylate group of another orotate molecule. Thus, the molecules are associated to form chains, the carboxylato group acting as a bridge between the metal ions, the orotato-group being tridentate. The title compound crystallizes in the monoclinic space group. P21/n1 with a = 9.515(5), b = 6.925(2), c = 11.861(6) Å, β = 95.285(9)°, D calc = 2.17 g cm−3, and z = 4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009596719033
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  • 80
    Digitale Medien
    Digitale Medien
    X-ray crystal structure and spectroscopy of a pseudo-square pyramidal Cu(II) complex, trans-dinitratotetrakis (trans-4-styrylpyridine)copper(II) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 413-420 
    Details
    ISSN: 1572-8854
    Schlagwort(e): pseudo-square pyramidal Cu(II) complex ; trans-4-styrylpyridine ; crystal structure ; IR, electronic, and EPR spectra
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Single crystals of the title Cu(II) complex, [Cu(stpy)4(ONO2)(ONO2)′] [stpy = trans-4-styryl-pyridine] have been prepared and characterized by elemental and thermal analyses, IR, electronic and EPR spectral measurements, and X-ray crystal structure determination. The complex crystallizes in the monoclinic space group P21/c with unit-cell parameters, a = 12.985(2), b = 22.865(8), c = 17.024(10) Å, β = 112.29(3)°, and Z = 4. The structure consists of discrete monomeric units of [Cu(stpy)4(ONO2)(ONO2)′]. The equatorial positions of the Cu(II) polyhedron are occupied by nitrogen atoms of the four stpy ligands and the axial positions by the oxygens of two unidentate nitrate anions. One of these oxygens is at rather longer distance [2.609(3) Å] and may be considered to be semicoordinated. If this semibond is ignored, the coordination geometry lies closer to an idealized square pyramid than to the trigonal bipyramid geometry. IR spectra reveal nitrogen coordination from stpy and asymmetry in the monodentate oxygen binding of the two nitrate ligands. The optical reflectance band at 600 nm suggests pseudo-square-based pyramidal geometry around Cu(II). Well-resolved Cu(II) hyperfine features in the EPR spectra reveal the absence of exchange interactions between adjacent copper centers. Optical and EPR spectra of a methanolic solution of the complex indicate solvent interactions. Thermogravimetric analysis shows the complex to be stable up to 175°C.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009510910121
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  • 81
    Digitale Medien
    Digitale Medien
    Molecular structure of 1-phenyl-1-dimethylamino-4,4-bis(trimethylsilyl)-2-aza-3λ3-phosphabutadiene-1,3 (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 475-480 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; ab initio calculations ; conjugation ; phosphabutadienes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal and molecular structure of 1-phenyl-1-dimethylamino-4,4-bis(trimethylsilyl)-2-aza-3λ3-phosphabutadiene-1,3, Me2N(Ph)C=N—P=C(SiMe3)2 (1), has been determined. Crystal data: triclinic, P1¯, a = 8.975(4), b = 10.001(5), c = 12.440(6) Å, α = 79.04(4), β = 77.98(4), γ = 73.07(4)°, V = 1034.7 Å3, Z = 2, and D c = 1.08 g cm−3. The main geometrical parameters of 1 as well as ab initio (HF/6-31+G**) calculations of the model systems show no clear evidence of high efficiency of the π(C=N)—π (P=C) conjugation.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009527413755
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  • 82
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of 1-(4-bromobenzyl)-4-methyl-2,6,7-trioxabicyclo[2.2.2]octane (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 493-496 
    Details
    ISSN: 1572-8854
    Schlagwort(e): contrast agents ; crystal structure ; ortho ester
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract 1-(4-Bromobenzyl)-4-methyl-2,6,7-trioxabicyclo[2.2.2]octane, C13H15BrO3, has been synthesized from 4-bromophenylacetic acid chloride via the oxetan ester (3-methyl-3-oxetanyl)methyl-2-(4-bromophenyl)acetate. The crystal structure of the title compound has been determined at low temperature (120 K), by X-ray diffraction methods. This compound crystallizes in the monoclinic space group P21/n (No. 14), Z = 4, with lattice parametersa = 6.019(5), b = 20.990(5), c = 9.915(2) Å, and β = 101.29(1)°.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009531514664
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  • 83
    Digitale Medien
    Digitale Medien
    Structure refinement and Raman spectrum of silver azide (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 561-564 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; Raman spectrum ; silver azide ; azide
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Silver nitrate reacts with sodium azide to give white powdery silver azide, which can be crystallized in aqueous ammonia. The compound belongs to orthorhombic space group Ibam with a = 5.600(1), b = 5.980(6), c = 5.998(1) Å, and Z = 4. The layer-type structure is constructed from edge-sharing regular rectangles, each composed of silver atoms at its vertices with an enclosed azide anion in a tilted orientation. The linear and asymmetrical structure of the azide anion in crystalline silver azide has been confirmed by its Raman spectrum.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009544702195
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  • 84
    Digitale Medien
    Digitale Medien
    Structure of adamantan-1-ammonium 1-adamantanecarboxylate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 845-848 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; centrosymmetric ; aminoadamantane derivative ; antiviral ; dispiro compound
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Adamantan-1-ammonium 1-adamantanecarboxylate, C21H33NO2 (I) is a novel dispiro-type compound. Aminoadamantane derivatives, in which the spiro carbon atoms are part of heterocyclic rings, are of potential interest as biological active substances and antiviral agents. Complex (I) crystallizes in the centrosymmetric space group C2/c (No. 15) with eight molecules in the unit cell with a = 25.227(4), b = 6.527(1), c = 22.489(4) Å, and β = 90.75(1)°. The two spiro units are a 1-adamantylammonium cation and a 1-adamantane carbonyloxy anion. The complex units are stabilized by a network of intermolecular carbonyloxy-to-amine hydrogen bonding and van der Waals cohesive forces. Germane bond lengths are: C—N = 1.479(9) and C—O (mean) = 1.25(2) Å.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009564307821
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  • 85
    Digitale Medien
    Digitale Medien
    Structural characterization of a series of cyclohexaphosphates: M0.5((C6H5CH2)2NH2)5P6O18·H2O (M = Co, Cu, Cd) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 891-899 
    Details
    ISSN: 1572-8854
    Schlagwort(e): cyclohexaphosphates ; organometallic compound ; crystal growth ; X-ray diffraction ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Three new cyclohexaphosphates with general formula M0.5((C6H5CH2)2NH2)5P6O18·H2O (M=Co, Cu, Cd) are reported. They crystallize with monoclinic unit-cells and are isotropic. We have determined their structure from the salt M=Co. This later exhibits the following unit-cell parameters: a = 22.739(5), b = 17.682(3), c = 18.342(3) Å, β = 91.22(1)°, Z = 4,P21/n, V = 7373 Å3, and Dx = 1.373 g cm−3. The atomic arrangement can be described as layers containing P6O18 ring anions and CoO6 octahedra spreading in the (101) planes and intercalated by the dibenzylammonium groups and the water molecules. Synthesis and characterization by X-ray diffraction, IR absorption, and TA are described.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009521911166
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  • 86
    Digitale Medien
    Digitale Medien
    Effects of Temperature and Relative Humidity on Polylactic Acid Plastic Degradation (1999)
    Springer
    Journal of polymers and the environment 7 (1999), S. 83-92 
    Details
    ISSN: 1572-8900
    Schlagwort(e): Polylactic acid ; temperature ; relative humidity ; degradation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Energietechnik , Maschinenbau
    Notizen: Abstract Three high molecular weight (120,000 to 200,000 g mol−1) polylactic acid (PLA) plastic films from Chronopol (Ch-I) and Cargill Dow Polymers (GII and Ca-I) were analyzed for their degradation under various temperature and relative humidity (RH) conditions. Two sets of plastic films, each containing 11 samples, were randomly hung in a temperature/humidity-controlled chamber by means of plastic-coated paper clips. The tested conditions were 28, 40, and 55°C at 50 and 100% RH, respectively, and 55°C at 10% RH. The three tested PLA films started to lose their tensile properties when their weight-average molecular weight (M w) was in the range of 50,000 to 75,000 g mol−1. The average degradation rate of Ch-I, GII, and Ca-I was 28,931, 27,361, and 63,025 M w/week, respectively. Hence, GII had a faster degradation rate than Ch-I and Ca-I under all tested conditions. The degradation rate of PLA plastics was enhanced by the increase in temperature and relative humidity. This trend was observed in all three PLA plastics (Ca-I, GII, and Ch-I). Of the three tested films, Ch-I was the first to lose its mechanical properties, whereas Ca-I demonstrated the slowest loss, with mechanical properties under all tested conditions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021808317416
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  • 87
    Digitale Medien
    Digitale Medien
    Electrochemical synthesis of cupric oxide powder Part II: Process conditions (1999)
    Springer
    Journal of applied electrochemistry 29 (1999), S. 81-85 
    Details
    ISSN: 1572-8838
    Schlagwort(e): cupric oxide ; powder ; current density ; temperature ; sodium sulfate
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Elektrotechnik, Elektronik, Nachrichtentechnik
    Notizen: Abstract Electrosynthesis of cupric oxide powder was carried out on a laboratory scale in an electrochemical cell under various experimental conditions. The electrolysis was appraised in terms of the particle size of the cupric oxide product and the anodic dissolution of the copper electrode. Using a previously determined pH value of 7.50, the other optimum electrolysis operating conditions established were a current density of 4000Am−2, temperature of 353K, and Na2SO4 concentration of 0.5m. The optimum values of current efficiency, cell voltage and specific energy consumption for the electrochemical synthesis of cupric oxide powder were determined.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1003464914657
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  • 88
    Digitale Medien
    Digitale Medien
    Sulfate solubility algorithms for CaSO4–NaCl–H2O and Na2SO4–NaCl–H2O in chlor alkali brine at 25, 65, 75 and 85 ∘C (1999)
    Springer
    Journal of applied electrochemistry 29 (1999), S. 525-528 
    Details
    ISSN: 1572-8838
    Schlagwort(e): brine ; chlor-alkali cells ; solubility ; sulfate ions ; temperature
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Elektrotechnik, Elektronik, Nachrichtentechnik
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1026405806916
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  • 89
    Digitale Medien
    Digitale Medien
    Synthesis and crystal structure of N 12-(7-chloro-4-quinolinyl)-N 1,N 1-diethy1-1,12-diaminododecane (AQ-40) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 925-929 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Quinoline ; chloroquine ; antimalarial ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The preparation of N12-(7-chloro-4-quinolinyl)-N 1,N 1-diethyl-1,12-diaminododecane, AQ-40, was accomplished by a five-step process in 80% overall yield from 12-aminododecanoic acid and 4,7-dichloroquinoline. AQ-40 crystallizes as a monohydrate from reagent grade chloroform/ diethyl ether mixtures in the triclinc space group P-1 with a = 8.667(2), b = 8.9425(10), c = 17.217(3) Å, α = 99.34(1), β = 99.89(2), γ = 91.56(1)°, V = 1295.0 Å3 and Z = 2. The l2-(N 1,N 1-diethylamino)dodecyl side chain is in the fully extended conformation and the water molecule forms hydrogen bonds to the two tertiary nitrogen atoms as well as with the secondary amino group. The nitrogen of the secondary amino group bound to the four-position of the quinoline moiety is virtually planar. This together with the rather short C–N distance of 1.347(3) Å to the quinoline moiety suggests involvement of the lone pair on this nitrogen with the π system of the ring.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022810821793
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  • 90
    Digitale Medien
    Digitale Medien
    Molecular structure of trans-[Co(NH3)4(NH2CH3)Cl](ClO4)2 (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 69-72 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Co(III) complex ; crystal structure ; kinetics ; steric effects
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title compound crystallizes in the orthorhombic space group Pnma, with a = 7.9209(5), b = 9.818(1), c = 16.867(2) Å, and Z = 4. The structure was solved employing 1864 independent x-ray reflections with I〉2σ(I) by Patterson and difference Fourier techniques and refined by full-matrix least-squares to R = 0.036. The trans-[CO(NH3)4(NH2CH3)Cl](ClO4)2 molecule is on a crystallographic mirror plane. The cobalt ion is in an elongated octahedral coordination with four equatorial ammonia ligands [average Co–N distance equal to 1.966(2) Å], an axial methylamine [Co–N=1.965(3)Å], and an axial chlorine ion [Co–Cl=2.2771(9)Å]. Kinetic steric effects of the complex are interpreted in terms of structural results.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021786804676
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  • 91
    Digitale Medien
    Digitale Medien
    Crystal structure of NH3(CH2)2NH3BiCl5·2H2O (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 209-212 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Bismuth ; crystal structure ; inorganic polymer
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The ethylenediammonium pentachlorobismuthate(III) dihydrate salt is monoclinic with the following unit cell dimensions: a = 10.902(8)Å, b = 7.926(6)Å, c = 15.199(6)Å, β = 96.40(1)°, space group P21/n with Z = 4. The structure shows a layer arrangement parallel to the $$\vec a$$ axis: planes of the [Bi2Cl10]4− bioctahedra alternate with planes of [NH3(CH2)2NH3]2+ dications. The [Bi2Cl10]4− bioctahedra are connected through O(W)–H··· Cl hydrogen bonds, so that infinite unidimensional chains of composition [Bi2Cl10(H2O)2] n 4n− are formed in the structure parallel to the $$\vec a$$ axis. These chains are themselves interconnected by means of the N–H···Cl bonds originating from the [NH3(CH2)2NH3]2+ entities, forming a three-dimensional network.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022474327917
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  • 92
    Digitale Medien
    Digitale Medien
    The synthesis and X-ray structure of [Sr2(OSiPh3)4(NH3)5]·0.5C7H8 (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 221-226 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Strontium ; triphenylsiloxy ; crystal structure ; ammonia
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The title complex [Sr2(OSiPh3)4(NH3)5]·0.5C7H8 was prepared by the reaction of strontium metal granules with triphenylsilanol in an ammoniacal-toluene solution at −40°C. It crystallizes in monoclinic space group P21/n with a = 14.465(3), b = 20.715 (6), c = 25.199(6) Å, β = 95.98(2)°, and Z = 4. The complex has a dimeric structure with one terminal and three bridging triphenylsiloxy ligands, the remaining coordination sites being occupied by five ammonia molecules. The central Sr2O4N5 moiety adopts a distorted M2X9 face-sharing bioctahedral arrangement.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022430612896
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  • 93
    Digitale Medien
    Digitale Medien
    Crystal structure of mixed rubidium–ammonium hydrogen sulfate Rb0.7(NH4)0.3HSO4 at room temperature (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 335-338 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Mixed rubidium–ammonium acid sulfate ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The structure of Rb0.7(NH4)0.3HSO4 has been determined by X-ray analysis. The mixed compound crystallizes in the monoclinic space group P21/n with unit cell parameters a = 14.374(6) Å, b = 4.618(6) Å, c = 14.412(2) Å, β = 118.03(2)°, V = 844.4(4) Å3, and D cal = 1.536 g cm−3 for Z = 8. The mixed compound Rb0.7(NH4)0.3HSO4 is a chain-based structure. The Rb+ and NH4 + cations are intercalated between chains, formed of HSO4 - groups linked with OH⋯O hydrogen-bonding. Rb0.7(NH4)0.3HSO4 presents a new type of structural arrangement different from those of pure RbHSO4 and NH4HSO4.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022451822967
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  • 94
    Digitale Medien
    Digitale Medien
    The crystal and molecular structures of isoperezone, aminoperezone, and isoaminoperezone: a comparative study of their crystal packing (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 529-537 
    Details
    ISSN: 1572-8854
    Schlagwort(e): 2-[1,5-Dimethyl-4-hexenyl]-6-hydroxy-5-methyl-1,4-benzoquinone ; 2-[1,5-dimethyl-4-hexenyl]-6-amino-3-hydroxy-5-methyl-1,4-benzoquinone ; 2-[1,5-dimethyl-4-hexenyl]-3-amino-6-hydroxy-5-methyl-1,4-benzoquinone ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal structures of isoperezone (1), aminoperezone (2), and isoaminoperezone (3) have been determined by single-crystal X-ray diffraction. Compound (1) yields orange crystals, orthorhombic space group P212121 with unit cell dimensions a = 6.271(6), b = 30.373(7), c = 7.257(1) Å, and Z = 4; compound (2) yields purple crystals, orthorhombic space group P212121 with unit cell dimensions a = 6.498(3), b = 7.500(1) c = 29.200(6) Å, and Z = 4; compound (3) yields purple crystals, monoclinic space group P21 with unit cell dimensions a = 7.354(1), b = 7.511(1), c = 13.283(1) Å, β = 102,07(1)°, and Z = 2. The side chains in (1)–(3) are oriented out of the plane of the quinone ring at an angle of 124, 144, and 97°, respectively. The molecules in the crystal are held together by hydrogen-bonding networks and van der Waals interactions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1023292005612
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  • 95
    Digitale Medien
    Digitale Medien
    Crystal structure of [WI2(CO)3{P(OMe)3}2] (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 639-643 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Tungsten(II) ; diiodo ; carbonyl ; trimethylphosphite ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract [WI2(CO)3{P(OMe)3}2]crystallizes in the orthorhombic space group Pca21, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)3 octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1022469211406
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  • 96
    Digitale Medien
    Digitale Medien
    Asymmetric hetero-Diels-Alder reactions: X-ray structures of three novel chiral dihydropyrimidines (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 663-671 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Pyrimidine ; carboxamide ; sulfonyl ; chiral ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract Three novel dihydropyrimidine compounds N8,6-di(4-nitrophenyl)-(3R)-ethyl-(7R)-methyl-5-oxo-2,3,6,7-tetrahydrooxazolo[3,2,c] pyrimidine-8-carboxamide (2), N8,6-di((4-methylphenyl)-sulfonyl)-(3R)-ethyl-5-oxo-(7R)-phenyl-2,3,6,7-tetrahydrooxazolo [3,2,c]pyrimidine-8-carboxamide (3) and N8,6-di ((4-methylphenyl)sulfonyl)-(3R)-ethyl-(7R)-methyl-5-oxo-2,3,6,7-tetrahydrooxazolo[3,2,c] pyrimidine-8-carboxamide (4) have been prepared (from 2-amino-1-butanol of 64.4% e.e.) and structurally characterized by X-ray crystallography. All three compounds contain stereogenic centers, but the crystal of (2) chosen was found to be racemic whilst those of (3) and (4) were found to be homochiral. Compound (2) crystallizes in the monoclinic space group P21/c, with a = 17.958(4), b = 12.431(2), c = 9.653(2) Å, β = 96.20(3)°, U = 2142.3(7) Å3, Z = 4, and D c = 1.449 g cm−3. Compounds (3) and (4) both crystallize in the monoclinic space group P21, with a = 9.349(2), b = 5.824(5), c = 26.513(8) Å, β = 99.43(2)°, U = 1424.1(13) Å3, Z = 2 and D c = 1.389 g cm−3 for (3), and a = 5.9526(9), b = 16.3521(10), c = 13.2263(11) Å, β = 92.81(12)°, U = 1285.9(2) Å3, Z = 2 and D c = 1.378 g cm−3 for (4).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021791832534
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  • 97
    Digitale Medien
    Digitale Medien
    The synthesis and crystallographic characterization of the heterotrimetallic linear complex [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 713-716 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Heterotrimetallic sulfido cluster ; linear ; synthesis ; crystal structure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The complex Cu(PPh3)3I reacts with [Et4N]2MoS4 and FeBr2 to give the heterotrimetallic complexes [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1). [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1) crystallizes in the triclinic space group P-1, a = 13.537(4), b = 15.316(4), c = 12.381(4) Å, α = 105.16(2), β = 93.27(3), γ = 101.18(2)°, and V = 2415.0(12) Å3 for Z = 2. The three metal atoms of the structure [Et4N][(Ph3P)2{CuS2MoS2Fe}Br2] (1) are nearly distributed along a line, where three metal atoms (Mo, Cu, Fe) are each in an approximate tetrahedral coordination, the lengths Mo-Fe and Mo-Cu distances are 2.772(2) and 2.798(2) Å, respectively.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021756319330
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  • 98
    Digitale Medien
    Digitale Medien
    The structural characterization of YbI2(DME)3 (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1107-1110 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; ytterbium ; lanthanide ; coordination complex
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The preparation and structural characterization of [YbI2(DME)2] are reported. The complex crystallizes in the triclinic space group P 1¯: a = 13.0094 (10), b=14.504(3), c = 14.668 (3) Å, α = 115.281(10) β = 106.74(2), γ = 105.97(2)°. The metal center of the complex exhibits a distorted pentagonal bipyramidal coordination geometry which involves a rare example of a monodentate DME ligand.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009557708382
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  • 99
    Digitale Medien
    Digitale Medien
    [CaSb2(EDTA)2(H2O)8]n: synthesis, crystal structure, and thermal behavior (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 447-452 
    Details
    ISSN: 1572-8854
    Schlagwort(e): Bimetallic EDTA complex ; crystal structure ; antimony
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The synthesis and crystal structure of a new EDTA complex, [CaSb2(EDTA)2(H2O)8]n, are reported. This compound crystallizes in the monoclinic space group P21/n, with a = 7.132(1) Å, b = 21.893(3) Å, c = 10.891(2) Å, β = 91.15(2)°. Sb(EDTA) entities are connected through carboxylate bridges to the calcium atoms resulting in layers parallel to the (101) plane. These layers are linked through a weak Sb···O bond (3.171 Å). Pyrolysis of this complex under sulfur vapor, between 400 and 800°C, leads to a mixture of the monometallic sulfides. Pyrolysis in air above 700°C allows the easy preparation of the mixed oxide CaSb2O6.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1021716605217
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  • 100
    Digitale Medien
    Digitale Medien
    Crystal structure of phenyl-substituted cyclopentenes (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1127-1132 
    Details
    ISSN: 1572-8854
    Schlagwort(e): crystal structure ; phenyl-substituted cyclopentenes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Geologie und Paläontologie , Physik
    Notizen: Abstract The crystal structures of two stereoisomers of tetraphenyl- and pentaphenyl-substituted cyclopentenes 1 and 2 have been determined by X-ray analysis. An envelope conformation 1E has been ascertained for the cis isomer 1a, whereas the cis, cis isomer 2a, which crystallizes in two different space groups, P1¯ and P21/n, displays a twisted 2T1 conformation. The phenyl substituents are all tilted with respect to the cyclopentene ring in both structures. Compound 1a crystallizes in the space group P21/a with a = 18.553(3), b = 6.006(2), c = 19.355(5), β = 102.67(4)°, and V = 2104.2(g) Å3 for Z = 4; compound 2a I crystallizes in P21/n with a = 10.064(2), b = 20.756(5), c = 12.245(3) Å, β = 95.21(2)°, and V = 2547(1) Å3 for Z = 4; compound 2aII crystallizes in P1¯ with a = 10.117(3), b = 11.750(2), c = 12.359(2) Å, α = 111.25(2), β = 94.84(2), γ = 108.78(2)°, and V = 1262.3(6) Å3 for Z = 2.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1009566010200
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