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  • 1
    Electronic Resource
    Electronic Resource
    Selektive Partnerwahl der Aaskrähe (Corvus corone) in der Hybridisierungszone von Rabenkrähe (C. c. corone) und Nebelkrähe (C. c. cornix) (1998)
    Springer
    Journal of ornithology 139 (1998), S. 173-177 
    Details
    ISSN: 1439-0361
    Keywords: mate choice ; taxonomy ; phenotypic hybrids ; fitness ; decision rule
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Zusammenfassung Die als Unterarten klassifizierten europäischen Formen der Aaskrähe, Rabenkrähe und Nebelkrähe, besiedeln verschiedene, aneinandergrenzende Verbreitungsgebiete und hybridisieren in der Kontaktzone. Die Nachkommen von Mischpaaren sind fruchtbar und können sowohl mit anderen Hybriden als auch mit Raben- und Nebelkrähen erfolgreich brüten. Trotzdem kommt es zu keiner völligen Vermischung der Formen und/oder Verlagerung der Verbreitungsgebiete. Vor diesem Hintergrund untersuchten wir die Partnerwahl von Aaskrähen in der Hybridisierungszone auf der nordfriesischen Insel Amrum und stellten fest, daß Partner gleichen Phänotyps häufiger miteinander verpaart waren, als stochastisch zu erwarten gewesen wäre. Unsere Daten bestätigen vergleichbare Studien aus Hybridisierungszonen in Italien und Sibirien. Wir schließen daraus, daß phänotypisch selektive Partnerwahl bei der Aaskrähe ein allgemeines Phänomen sein könnte und diskutieren, warum dieses Verhalten anfitness-relevante Parameter gekoppelt sein sollte. Um welche es sich dabei handeln könnte, wurde bisher nicht hinreichend untersucht und muß deshalb offen bleiben.
    Notes: Summary Carrion Crow and Hooded Crow are regarded as subspecies of the Crow. They show frequent hybridisation along the adjacent borders of their distribution. Mixed pairs produce fertile offspring which are able to breed successfully with both hybrids and mates of either phenotype. However, hybridisation does not lead to phenotypic changes of Carrion and Hooded Crows in general nor in their distinct distribution. We studied the mating behaviour of Crows in the hybrid zone on the Island of Amrum (Schleswig-Holstein, Germany) and found evidence that Crows may prefer mates of the same phenotype. Our data confirm previous studies which reported assortative mating with respect to plumage coloration from hybrid zones in Italy and Siberia. We discuss why this behaviour should be related tofitness traits which in our opinion have not yet been studied adequately nor identified.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01651226
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  • 2
    Electronic Resource
    Electronic Resource
    The impact of the egg parasitoid Uscana lariophaga on Callosobruchus maculatus populations and the damage to cowpea in a traditional storage system (1998)
    Springer
    Entomologia experimentalis et applicata 89 (1998), S. 289-295 
    Details
    ISSN: 1570-7458
    Keywords: Hymenoptera ; Trichogrammatidae ; Uscana lariophaga ; Coleoptera ; Bruchidae ; Callosobruchus maculatus ; cowpea ; storage pest ; biological control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract In West Africa, Uscana lariophaga (Hymenoptera: Trichogrammatidae) parasitizes the eggs of Callosobruchus maculatus (Coleoptera: Bruchidae), an important pest of stored cowpea. The impact of the egg parasitoid on pest populations was evaluated in clay pots used in traditional storage in Niger. At the beginning of the storage period cowpeas were infested with different densities of larval instars and adults of C. maculatus and inoculated with one density of U. lariophaga. The higher the initial densities of C. maculatus, the better the egg parasitoid was able to establish itself and to control the population of C. maculatus, limiting the damage to cowpea. After three months of storage, the egg parasitoid significantly reduced the number of C. maculatus adults by 68 at the lowest and 86 percent at the highest initial density of the beetle; the percentage of damaged beans was reduced by 13 and 19% respectively.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003555413273
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  • 3
    Electronic Resource
    Electronic Resource
    Suitability of new and old association hosts for the development of selected microgastrine parasitoids of gramineous stemborers (1999)
    Springer
    Entomologia experimentalis et applicata 90 (1999), S. 257-266 
    Details
    ISSN: 1570-7458
    Keywords: host suitability ; acceptance ; biological control ; new associations ; Lepidoptera ; Pyralidae ; New World ; Old World ; stemborers ; Braconidae ; larval parasitoids ; Gramineae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The present study examined the acceptability and suitability of Old World stemborers (Chilo partellus and C. orichalcociliellus) for the development of New World parasitoids (Apanteles deplanatus and A. minator) and New World stemborers (Diatraea saccharalis and D. grandiosella) for the development of Old World parasitoids (Cotesia sesamiae, C. flavipes and C. chilonis). Results revealed that acceptance and suitability were high in old associations. In new associations, parasitoids accepted about 60% of the new association hosts. In addition, 10 out of 17 new associations were successful. Apanteles species appeared to be more physiologically host specific than Cotesia species. For example, two of four new association hosts were accepted by A. deplanatus and only one (D. saccharalis) was partially suitable for progeny development. Among the Cotesia species, Cotesia flavipes appeared to have a wider host range than the two other species. It attacked all hosts offered and successfully parasitized all but one (D. grandiosella). Diatraea saccharalis was accepted and was a suitable host for the development of all parasitoid species tested, whereas D. grandiosella was unsuitable for the development of four out of five parasitoid species tested. No clear pattern was observed as behavioral acceptance did not always agree with the pattern of physiological suitability. Implications of these findings for importation biological control of stemborers are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1026435617979
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  • 4
    Electronic Resource
    Electronic Resource
    Development of an artificial host egg for in vitro egg laying of Trichogramma galloi and T. pretiosum using plastic membranes (1999)
    Springer
    Entomologia experimentalis et applicata 91 (1999), S. 327-336 
    Details
    ISSN: 1570-7458
    Keywords: biological control ; in vitro rearing ; rearing techniques ; host selection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract An artificial host egg was developed as a first attempt to improve the techniques for in vitro rearing of Trichogramma galloi Zucchi and T. pretiosum Riley (Hymenoptera, Trichogrammatidae). Plastic membranes (polyethylene, polypropylene and polystyrene) of different thickness were tested for their usefulness in manufacturing artificial eggs, using a thermal system to produce semi-spherical cupules on the plastic surface. These artificial eggs were filled with larval hemolymph of Helicoverpa zea (Boddie) (Lepidoptera, Noctuidae), and the optimal size of the artificial egg and density of females/artificial egg for the highest host acceptance (percentage of artificial eggs with at least one parasitoid egg) as well as the ideal level of parasitism (eggs/artificial egg) were determined. High-density polyethylene 7–8 and 9–10 μm thick resulted in the best acceptance and level of parasitization for both parasitoid species. Six females per artificial egg resulted in the best rate of parasitization for these parasitoids, although these data were not different when using 4 or 5 females of T. galloi. The size, shape and surface texture of the artificial eggs were found to provide enough cues to elicit parasitization behavior in Trichogramma females, since no chemical stimulus was provided.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003649316161
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  • 5
    Electronic Resource
    Electronic Resource
    Spatial and temporal distribution of endemic and released entomopathogenic nematode populations in turfgrass (1998)
    Springer
    Entomologia experimentalis et applicata 86 (1998), S. 1-11 
    Details
    ISSN: 1570-7458
    Keywords: Heterorhabditidae ; Steinernematidae ; Heterorhabditis bacteriophora ; Steinernema carpocapsae ; Steinernema feltiae ; entomopathogenic nematodes ; turfgrass ; Japanese beetle ; Popillia japonica ; population dynamics ; spatial distribution ; edaphic factors ; biological control ; colonization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Entomopathogenic nematodes (Rhabdita: Heterorhabditidae and Steinernematidae) have been effective as inundative biological control agents of scarab larvae (Coleoptera: Scarabaeidae) in turfgrass. Entomopathogenic nematodes also occur naturally in turfgrass and endemic or inoculated populations may be able to provide effective long-term control. Variation in Heterorhabditis bacteriophora and Steinernema carpocapsae spatial and temporal distribution along transects placed at different turfgrass sites in central New Jersey, USA, was investigated. H. bacteriophora tended to be recovered from fewer sections in a transect than S. carpocapsae, but the two species, overall, did not differ in patchiness of distribution. In one transect with a H. bacteriophora population S. feltiae was also recovered, but the two populations seldom overlapped spatially. In transects with adequate scarab larvae density for analysis, H. bacteriophora density and Popillia japonica larvae density were inversely correlated. This suggests that endemic H. bacteriophora populations may suppress P. japonica populations. In one transect, an epizootic of H. bacteriophora in an undetermined host may have occurred. Edaphic factors were relatively uniform along transects and were, at most, weakly correlated with nematode recovery. Uniform inoculative releases of H. bacteriophora tended to return to patterns of distribution typical of endemic populations.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003130111093
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  • 6
    Electronic Resource
    Electronic Resource
    Change in foraging behaviour of the predatory mite Phytoseiulus persimilis after exposure to dead conspecifics and their products (1998)
    Springer
    Entomologia experimentalis et applicata 88 (1998), S. 295-300 
    Details
    ISSN: 1570-7458
    Keywords: Acari ; Phytoseiidae ; biological control ; infochemicals ; disease ; transmission
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Adult females of the predatory mite Phytoseiulus persimilis Athias-Henriot are strongly attracted to infochemicals released by plants infested with their prey, the two-spotted spider mite (Tetranychus urticae Koch), thereby effectively locating their prey. However, we found a consistently lower degree of attraction to these infochemicals for a population of P. persimilis, which is called non-responding population. Here we demonstrate that this low degree of attraction is a contagious phenomenon and that it cannot be explained by differences in abiotic conditions, physiological state and experience of predators or by genetic differences between predator populations. Female predators exposed to dead conspecifics of the non-responding population and their products showed a lower degree of attraction to plant odours and a higher mortality than predators exposed to products of a living conspecific of the non-responding population. This was true 6–7 days after contact with dead conspecifics and their products whereas 2 days after contact no effects were detected. The present results are discussed in view of our hypothesis that the change in foraging behaviour as well as the high mortality rate are symptoms of a contagious disease affecting the non-responding population.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003456317538
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  • 7
    Electronic Resource
    Electronic Resource
    Sub-lethal effects of foliar pubescence on the egg parasitoid Copidosoma koehleri and influence on parasitism of potato moth, Phthorimaea operculella (1998)
    Springer
    Entomologia experimentalis et applicata 87 (1998), S. 115-118 
    Details
    ISSN: 1570-7458
    Keywords: tritrophic interactions ; solanaceae ; parasitoids ; biological control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003123502651
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  • 8
    Electronic Resource
    Electronic Resource
    Potential for intraguild predation and competition among predatory Coccinellidae and Chrysopidae (1998)
    Springer
    Entomologia experimentalis et applicata 89 (1998), S. 47-55 
    Details
    ISSN: 1570-7458
    Keywords: Chrysoperla carnea ; Coccinella septempunctata ; Coleomegilla maculata ; Harmonia axyridis ; Ostrinia nubilalis ; Acyrthosiphon pisum ; prey suitability ; biological control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract In a laboratory study two coccinellid species, Coleomegilla maculata (DeGeer) and Harmonia axyridis Pallas, completed preimaginal development on lacewing eggs, Chrysoperla carnea Stephens or pea aphids, Acyrthosiphon pisum (Harris) in similar times. Preimaginal survival on C. carnea eggs was similar to survival on A. pisum for all stages of C. maculata and H. axyridis. Coccinellid adults that developed on C. carnea eggs were smaller than adults reared on A. pisum. Coccinella septempunctata L. did not complete preimaginal development on C. carnea eggs. Chrysoperla carnea preimaginal developmental time was approximately 20 days when fed either C. maculata eggs or A. pisum. Chrysoperla carnea fed C. maculata eggs developed into smaller adults, compared to adults reared as larvae on A. pisum, Ostrinia nubilalis (Hübner) eggs, or A. pisum alternated daily with O. nubilalis eggs. C. carnea did not complete preimaginal development on H. axyridis eggs. Cannibalism occurred more frequently between C. carnea third instars than between C. maculata fourth instars. When a C. carnea third instar was paired with a C. maculata fourth instar, more C. maculata were preyed upon by C. carnea, regardless of the herbivorous prey density. In the field these two predator species may negatively affect each other and reduce their suppression of pest densities.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003426815471
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  • 9
    Electronic Resource
    Electronic Resource
    Do sympatric Trichogramma species parasitize the pest insect Helicoverpa armigera and the beneficial insect Chrysoperla carnea in different proportions? (1999)
    Springer
    Entomologia experimentalis et applicata 92 (1999), S. 101-107 
    Details
    ISSN: 1570-7458
    Keywords: Trichogramma spp. ; Helicoverpa armigera ; Chrysoperla carnea ; Portugal ; parasitism ; biological control ; non-target species
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Parasitism of two host species by five Trichogramma species (Hymenoptera, Trichogrammatidae) was studied in the laboratory. The host species were: i) the bollworm Helicoverpa armigera Hübner (Lepidoptera, Noctuidae), an important pest of many crops in the tropics and subtropics, and ii) one of its natural enemies, the lacewing Chrysoperla carnea Stephens (Neuroptera, Chrysopidae), a predator often used as a biological control agent. The proportion of H. armigera eggs parasitized from the total number of parasitized hosts differed between Trichogramma species. The average number of parasitized eggs per female in 24 h by Trichogramma pintoi and T. bourarachae was 10 of H. armigera and about 0.5 of C. carnea. For the other three Trichogramma species (T. cordubensis, T. evanescens and T. turkestanica) these averages varied from 6 to 11 H. armigera eggs and from 3 to 4 C. carnea eggs. Total adult offspring production, contacts with hosts, secondary clutch size and sex-ratio of each Trichogramma species were determined as well. The results show that sympatric Trichogramma may parasitize target and non-target species in different proportions. If this difference corresponds to the field situation, simple laboratory tests could be performed to select not only efficient biogical control agents, but also species which are the least detrimental to non-target hosts.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003772905954
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  • 10
    Electronic Resource
    Electronic Resource
    Influence of host density on the reproductive strategy of Cephalonomia stephanoderis, a parasitoid of the coffee berry borer (1999)
    Springer
    Entomologia experimentalis et applicata 92 (1999), S. 21-28 
    Details
    ISSN: 1570-7458
    Keywords: host feeding ; host paralysis ; oviposition ; pre-oviposition phase ; Hypothenemus hampei ; Scolytidae ; biological control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The effect of the density of the coffee berry borer, Hypothenemus hampei (Coleoptera: Scolytidae) on reproductive and host-feeding behaviours of the parasitoid Cephalonomia stephanoderis (Hymenoptera: Bethylidae) was evaluated under laboratory conditions. The number of hosts used for oviposition was density-dependent at low host density. Beyond a density of six hosts/day, the oviposition rate reached a maximum of 1.2 eggs/day due to egg limitation. Cephalonomia stephanoderis females responded to increasing host availability with a linear increase in host feeding. Overall, parasitoids killed more coffee berry borers by feeding and paralysis than by parasitism. At low host density, the pre-oviposition phase was extended, oogenesis was delayed, more males were produced, and host feeding occasionally occurred concurrently with oviposition. We suggest that the efficacy of C. stephanoderis as a biological control agent depends on seasonal variations in host density. Inoculative vs inundative releases in coffee plantations are discussed in relation to the abundance of the coffee berry borer during the fructification and interharvest periods.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003745606862
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  • 11
    Electronic Resource
    Electronic Resource
    Response of an aphid parasitoid, Aphelinus asychis to its host, plant, host-plant complex, and to malathion (1999)
    Springer
    Entomologia experimentalis et applicata 91 (1999), S. 449-457 
    Details
    ISSN: 1570-7458
    Keywords: Schizaphis graminum ; Aphelinus asychis ; aphid ; parasitoid ; natural enemy ; biological control ; greenbug ; host selection ; plant volatile
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Aphelinus asychis (Walker) can be valuable as a biocontrol agent of the aphid, Schizaphis graminum (Rondani), a major pest on grain crops in the United States. This study reports the wind tunnel, and olfactometric responses of this parasitoid to the host (aphid), plant (sorghum), and host-plant complex (aphid-infested sorghum). In addition, the parasitoids' response to malathion-treated plants is also presented. The goal of the present study was to test the hypothesis that volatiles associated with the host attract natural enemies, as reported in cases of many hymenopterous parasitoids, and also to learn about the effects of insecticides on these parasitoids. In wind tunnel studies, these parasitoids moved upwind in the direction of the host-infested plant. There was no direct flight observed, however, these parasitoids were observed to hop and jump, and sometimes walk to their host. In the olfactometer experiments, we found that A. asychis is attracted to host-plant complex. The parasitoids' response to malathion in the olfactometer suggested that a malathion formulation when applied to plants can lure these beneficials, thus providing new insight into the ongoing task of integrating chemical and biological control of insect pests.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003766928069
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  • 12
    Electronic Resource
    Electronic Resource
    Life table characteristics of Macrolophus caliginosus preying upon Tetranychus urticae (1999)
    Springer
    Entomologia experimentalis et applicata 93 (1999), S. 267-273 
    Details
    ISSN: 1570-7458
    Keywords: Macrolophus caliginosus ; mirid bug ; life table ; longevity ; fecundity ; development time ; mortality ; sex ratio ; oviposition period ; intrinsic rate of increase ; spider mite ; Tetranychus urticae ; tomato ; biological control ; glasshouse pests
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The life table characteristics of the polyphagous mirid Macrolophus caliginosus Wagner (Heteroptera: Miridae) preying on various stages of Tetranychus urticae Koch (Acari: Tetranychidae) with tomato as host plant were described at 22 °C. The following average parameters were obtained: Female longevity: 28.7 days; fecundity: 0.7 eggs/female/day; egg mortality: 2.6%; pre-oviposition period: 5.5 days; oviposition period: 18.1 days; post-oviposition period: 3.2 days; juvenile development time: 26.8 days; juvenile mortality: 34.9%; and sex ratio (♀/(♀+♂): 0.46. Life table parameters were estimated as net reproduction rate (R 0): 6.15; intrinsic rate of increase (r m): 0.031 day−1; finite rate of increase (λ): 1.032; mean generation time (T c): 58.17 days; and doubling time (T 2) 22.2 days. The parameters obtained were in accordance with those reported for M. caliginosus fed on another mite species (T. turkestani Ugarov & Nikolski (Acari: Tetranychidae)). However, compared to the performance of M. caliginosus fed on common glasshouse insect pests, a diet consisting of only mites appeared to be inferior. However, being a voracious predator, M. caliginosus may be a valuable addition to existing methods of mite control.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003948313507
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  • 13
    Electronic Resource
    Electronic Resource
    Absence of odour-mediated avoidance of heterospecific competitors by the predatory mite Phytoseiulus persimilis (1999)
    Springer
    Entomologia experimentalis et applicata 92 (1999), S. 73-82 
    Details
    ISSN: 1570-7458
    Keywords: biological control ; food web interactions ; volatiles ; Phytoseiidae ; predatory bugs ; thrips ; predator-predator interactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Arthropods use odours associated with the presence of their food, enemies and competitors when searching for patches. Responses to these odours therefore determine the spatial distribution of animals, and are decisive for the occurrence and strength of interactions among species. Therefore, a logical first step in studying food web interactions is the analysis of behaviour of individuals that are searching for patches of food. We followed this approach when studying interactions in an artificial food web occurring on greenhouse cucumber in the Netherlands. In an earlier paper we found that one of the predators of the food web, the predatory mite Phytoseiulus persimilis Athias-Henriot, used to control spider mites, discriminates between odours from plants with spider mites, Tetranychus urticae Koch, and plants with spider mites plus conspecific predators. The odours used for discrimination are produced by adult prey in response to the presence of predators, and probably serve as an alarm pheromone to warn related spider mites. Other predator species may also trigger production of this alarm pheromone, which P. persimilis could use in turn to avoid plants with heterospecific predators. We therefore studied the response of the latter to odours from plants with spider mites and 3 other predator species, i.e. the generalist predatory bug Orius laevigatus (Fieber), the polyphagous thrips Frankliniella occidentalis and the spider-mite predator Neoseiulus californicus (McGregor). Both olfactometer and greenhouse release experiments yielded no evidence that P. persimilis avoids plants with any of the 3 heterospecific predators. This suggests that these predators do not elicit production of alarm pheromones in spider mites, and we argue that this is caused by a lack of coevolutionary history. The consequences of the lack of avoidance of heterospecific predators for interactions in food webs and biological control are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003708512701
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  • 14
    Electronic Resource
    Electronic Resource
    The epizootiology of a Metarhizium infection in mini-nests of the leaf-cutting ant Atta sexdens rubropilosa (1999)
    Springer
    Entomologia experimentalis et applicata 93 (1999), S. 51-61 
    Details
    ISSN: 1570-7458
    Keywords: Metarhizium anisopliae ; Atta sexdens rubropilosa ; leaf-cutting ants ; biological control ; social homeostasis ; entomopathogenic fungus
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract There is growing interest in the use of entomopathogenic organisms to control leaf-cutting ants (Hymenoptera: Formicidae: Attini). However, the way leaf-cutting ants react as a colony to biohazards is poorly understood. We investigated the effects of Metarhizium anisopliae (Metschnikoff) (Deuteromycotina: Hyphomycetes) applied to the foraging arenas of mini-nests (queenless sub-colonies) of the leaf-cutting ant Atta sexdens rubropilosa (Forel). Dry spores were applied either alone or mixed with citrus powder, at 0.5 g or 0.05 g per mini-nest. The spores were removed four days after application, and all dead ants removed every three days. Ant numbers near the Metarhizium increased as the ants attempted to clean up the biohazard. The ants attempted to place the spores in piles, which they then covered over with other material. They were able to deal with the low doses in this way, but the high doses overwhelmed them. All treated mini-nests suffered increased ant mortality during the first ten days after application. This mortality was particularly high in the media worker caste which had played the major role in attempting to clean up the spores. Foraging activity decreased, as did the health of the fungus gardens. The mini-nests exposed to the low dose of spores mixed with citrus powder then recovered fully. The health of the other treated mini-nests declined gradually until around 26 days after application, when they began deteriorating sharply. However, the decline of these mini-nests after day 26 was not due directly to the pathogenic action of the Metarhizium, nor to the initial ant mortality it had caused. The results suggest that the social stress caused by even such a short-lived Metarhizium epizootic was sufficient to cause the decline and ultimate death of the mini-nests. This has important implications for the control of leaf-cutting ants. It also demonstrates how important the social homeostasis of the colony is to leaf-cutting ants.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003830625680
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  • 15
    Electronic Resource
    Electronic Resource
    Within-plant distribution of Rhopalosiphum padi on wheat seedlings is affected by induced responses (1999)
    Springer
    Entomologia experimentalis et applicata 93 (1999), S. 227-230 
    Details
    ISSN: 1570-7458
    Keywords: Rhopalosiphum padi ; cereal aphids ; wheat ; induced responses ; feeding site
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003874225681
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  • 16
    Electronic Resource
    Electronic Resource
    Visual learning in larval Orius majusculus a polyphagous predator (1999)
    Springer
    Entomologia experimentalis et applicata 90 (1999), S. 103-107 
    Details
    ISSN: 1570-7458
    Keywords: learning ; Orius majusculus (Reuter) ; Heteroptera ; Anthocoridae ; predator ; biological control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003587014243
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    Life-history and oviposition behaviour of Amitus bennetti, a parasitoid of Bemisia argentifolii (1999)
    Springer
    Entomologia experimentalis et applicata 90 (1999), S. 183-189 
    Details
    ISSN: 1570-7458
    Keywords: Hymenoptera ; Aphelinidae ; Platygasteridae ; Hemiptera ; Aleyrodidae ; whiteflies ; Bemisia ; Amitus bennetti ; parasitoid ; biological control ; life history ; instar preference ; oviposition behaviour
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Amitus bennetti Viggiani & Evans (Hymenoptera: Platygasteridae) is a recently described parasitoid of the silverleaf whitefly, Bemisia argentifolii Bellows & Perring (Homoptera: Aleyrodidae). Behaviour and life history of the parasitoid are described. The first nymphal instar of B. argentifolii is preferred by the parasitoid, but the 1st through 4th instar may be parasitised. Females first investigate hosts with their antennae, then walk over the host, and eventually step with their front legs on the leaf and insert their ovipositor inside the host facing away from the host, while the hind legs are still on the host. The time from encounter to oviposition (=latency to oviposition) is shortest on the 1st instar. Oviposition duration (mean=39 s) comprises 50% of the handling time. Development time from egg to adult decreases from 72 days at 15 °C to 42 days at 20 °C to 28 days at 25 °C. We estimate that 400 degree days is required for development, with a development threshold of 10 °C. Adult longevity in the absence of hosts was 29, 26 and 19 days and with hosts present 8, 8 and 5 days at 15, 20 and 25 °C, respectively. Amitus bennetti is proovigenic and oviposits most eggs shortly after adult emergence. During the first day of their adult lives females laid 1, 31 and 49 eggs at 15, 20 and 25 °C, respectively. Compared with other parasitoid species, the development time of A. bennetti is very long, and the implications of this for management of B. argentifolii are discussed.
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    URL: http://dx.doi.org/10.1023/A:1003599814671
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    Comparison of Diuraphis noxia resistance in wheat isolines and plant introduction lines (1999)
    Springer
    Entomologia experimentalis et applicata 92 (1999), S. 157-164 
    Details
    ISSN: 1570-7458
    Keywords: plant resistance ; antibiosis ; tolerance ; antixenosis ; Russian wheat aphid ; wheat ; Homoptera ; Aphididae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The Russian wheat aphid, Diuraphis noxia (Mordvilko), is one of the most important aphid pests of wheat, Triticum aestivum L., worldwide. Among the various pest management options, plant resistance is an economical management tactic to control D. noxia in cereal crops such as wheat. Researchers have identified D. noxia resistant germplasm and it has been incorporated into wheat. This study compared D. noxia resistance between the ‘Betta’ wheat isolines Betta-Dn1, Betta-Dn2, and Betta-Dn5 and their corresponding donor gene plant introduction (PI) lines PI 137739 (Dn1), PI 262660 (Dn2), and PI 294994 (Dn5). Although the Betta isolines and PI lines showed D. noxia resistance when compared with Betta wheat, the degree of resistance in the isolines to D. noxia was different from their corresponding PI donors. Aphid number, aphid fecundity, and biomass per aphid were not different between Betta-Dn1 and PI 137739 or Betta-Dn2 and PI 262660; however, the same parameters were significantly lower on PI 294994 compared with Betta-Dn5. This indicated that aphid resistance in PI 137739 and PI 262660 was probably governed by a single dominant gene, while the resistance in PI 294994 was controlled by more than one gene. Additionally, plant biomass reduction was aphid density dependent, which suggested that use of appropriate aphid infestation level is important when using plant biomass reduction as an indicator of resistance. Plant resistance categorization showed that there was no detectable difference in antixenosis among the seven lines evaluated. However, the higher aphid fecundity observed on PI 262660 compared with PI 137739 and PI 294994, in addition to no significant differences among the three PIs in plant biomass reduction, suggested PI 262660 was a tolerant line, while PI 137739 and PI 294994 were antibiotic lines. Plant tolerance could not be elucidated among the three Betta isolines using aphid fecundity and plant biomass reduction as indicators.
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    Jasmonic acid induces the production of gerbera volatiles that attract the biological control agent Phytoseiulus persimilis (1999)
    Springer
    Entomologia experimentalis et applicata 93 (1999), S. 77-86 
    Details
    ISSN: 1570-7458
    Keywords: Acari ; behaviour ; biological control ; Gerbera jamesonii ; herbivore induced synomones ; infochemicals ; indirect defence ; Phytoseiidae ; semiochemicals ; terpenoids ; Tetranychus urticae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Jasmonic acid (JA) is a plant hormone that is involved in the induction of plant defence in response to herbivore attack. We studied the effect of exposure of gerbera leaves to JA on indirect plant defence, i.e. attraction of natural enemies of herbivores. Treatment of gerbera leaves with JA or feeding damage by the herbivorous spider mite Tetranychus urticae, both induced the production of a complex odour blend that attracts the predatory mite Phytoseiulus persimilis. This phytoseiid predator is a very effective biological control agent of the spider mite T. urticae. Comparison of headspace composition of gerbera leaves exposed to either JA or T. urticae revealed a large degree of resemblance, but some quantitative and qualitative differences were recorded. The major chemical group in both treatments is formed by the terpenoids which quantitatively comprised up to 80% of the total odour blend. These terpenoids included (E)-4,8-dimethyl-1,3,7-nonatriene, (E)-β-ocimene and linalool that are known to attract P. persimilis. Aldehydes, alcohols, esters and ketones, together with nitrogenous compounds formed the remaining constituents of the odour blend. The induction of predator attractants in plants by JA may be applied in biological control programs, which is discussed in this paper.
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    URL: http://dx.doi.org/10.1023/A:1003826309751
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    Influence of cereal leaf epicuticular wax on Diuraphis noxia probing behavior and nymphoposition (1998)
    Springer
    Entomologia experimentalis et applicata 89 (1998), S. 111-118 
    Details
    ISSN: 1570-7458
    Keywords: leaf surface wax ; probing behavior ; nymphoposition ; Russian wheat aphid ; wheat ; barley ; oat ; Homoptera ; Aphididae
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The effect of cereal leaf surface wax on Diuraphis noxia (Mordvilko), the Russian wheat aphid, probing behavior and nymphoposition was evaluated. Ultrastructure of leaf epicuticular wax from wheat (Triticum aestivum L.) c.v. ‘Arapahoe’ and ‘Halt’ was different from barley (Hordeum vulgare L.) c.v. ‘Morex’, and oat (Avena sativa L.) c.v. ‘Border’. Both wheat cultivars had similar rod-shaped epicuticular wax, while barley and oat plants had flakes. The chemical composition comparison of gas chromatograms also indicated that the extract of the two wheat cultivars had similar pattern of peaks, while the barley and oat leaves had similar peaks. Cereal variety significantly affected aphid probing behavior (P 〈 0.05), but wax removal using ethyl ether swab did not (P 〈 0.05). Aphids initiated significantly more probes on Border oat leaves than on Morex barley irrespective of wax removal, although total probing duration per aphid was not significantly different among the four cereals examined. Accumulative salivation duration per aphid on oat leaves with wax was significantly longer than other cereal leaves with wax, while accumulative ingestion duration per aphid on Arapahoe wheat and Morex barley was significantly longer than on oat. Nymphoposition of D. noxia on cereal leaves maintained on the benzimidazole-agar medium showed that aphids produced a greater number of nymphs on Morex barley and less on Border oat leaves, although wax removal did not affect aphid nymphoposition. Removal of leaf epicuticular waxes from the 4 cereal genotypes using ethyl ether swab indicated that the influence of wax on plant resistance to D. noxia probing and reproduction was limited. Morex barley was the most favorable, while Border oat was the least favorable cereal host of D. noxia.
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    Reduction of insect cold-hardiness using ice-nucleating active fungi and surfactants (1998)
    Springer
    Entomologia experimentalis et applicata 89 (1998), S. 103-109 
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    ISSN: 1570-7458
    Keywords: Insecta ; supercooling capacity ; cold tolerance ; Hippodamia convergens ; Fusarium avenaceum ; Fusarium acuminatum ; pleomorphism ; biological control
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The supercooling point (SCP) of an insect model, the lady beetle Hippodamia convergens Guérin-Menéville (Coleoptera, Coccinellidae) was markedly elevated by treatment with aqueous suspensions of the filamentous, ice nucleation active (INA) fungi Fusarium avenaceum and slightly elevated by Fusarium acuminatum. Addition of the surfactant Tween 80 to the fungal suspensions further reduced the supercooling capacity of adult beetles. When used alone the surfactant Triton X-100 produced a greater SCP elevation than Tween 20 or Tween 80. The emulsifier gum arabic was ineffective in elevating beetle SCPs when applied alone and when added to INA fungal preparations it decreased their efficacy. Aqueous suspensions of both viable sporulating and viable pleomorphic (a permanent, degenerative, nonsporulating cultural state) forms of both fungal species were more effective in elevating the SCP than killed preparations except for the pleomorphic F. acuminatum suspension in which the killed form was slightly more active. Application of INA fungi applied in combination with surfactants may be useful in the development of methods for the biological control of overwintering freeze-susceptible insect pests by decreasing their capacity to avoid lethal freezing by supercooling.
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    Effect of a co-occurring aphid on the susceptibility of the Russian wheat aphid to lacewing predators (1998)
    Springer
    Entomologia experimentalis et applicata 87 (1998), S. 103-108 
    Details
    ISSN: 1570-7458
    Keywords: predator foraging ; biological control ; Chrysoperla plorabunda ; Diuraphis noxia ; Rhopalosiphum padi
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Previous field experiments indicated that the presence of the bird cherry-oat aphid, Rhopalosiphum padi (L.), on perennial grasses can decrease the effectiveness of predatory lacewings, Chrysoperla plorabunda (Fitch), in reducing populations of the Russian wheat aphid, Diuraphis noxia (Mordvilko). We tested the hypothesis that R. padi deflects predation away from D. noxia because it feeds in sites that are more accessible to predators. We quantified the behavior of lacewing larvae on crested wheatgrass plants bearing either D. noxia alone or an equal mixture of D. noxia and R. padi. On non-flowering plants, R. padi typically occurred on leaf sheaths or open blades, and was encountered and captured more often than D. noxia, which usually fed within immature, rolled leaves. Overall time-budgets of lacewings did not differ between the pure-D. noxia and mixed-species treatments, but 〉75% of the time spent consuming aphids in the mixed-species treatment was devoted to R. padi. On flowering plants, D. noxia usually aggregated on the flag leaf below the inflorescence, whereas R. padi occurred mostly on leaf sheaths. Predators again captured R. padi more often than D. noxia, and spent more time consuming aphids in the mixed-species treatment than in the pure-D. noxia treatment. These behavioral observations support the hypothesis that non-target prey can hamper the short-term effectiveness of biological-control agents against D. noxia.
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    Salivation into sieve elements in relation to plant chemistry: the case of the aphid Sitobion fragariae and the wheat, Triticum aestivum (1999)
    Springer
    Entomologia experimentalis et applicata 91 (1999), S. 111-114 
    Details
    ISSN: 1570-7458
    Keywords: sieve element ; salivation ; aphid ; plant resistance ; wheat ; Sitobion fragariae ; Triticum aestivum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Extended sieve element salivation (E1 waveform in the electrical penetration graph) is a characteristic activity during early sieve element punctures, particularly in resistant plants. In order to explore a chemically-mediated mechanism of resistance associated with sieve element salivation, we compared the pattern of feeding behaviour of the aphid, Sitobion fragariae (Walker), on two cultivars of the wheat Triticum aestivum L., with different concentrations of hydroxamic acids (Hx). During 24 h of electronic monitoring, aphids dedicated over 50% of the total time to phloem ingestion from the sieve elements. Total time allocated to E1 in the experiment, time to first E1 within the experiment, time allocated to E1 before a sustained phloem ingestion (E2) and the contribution of sieve element salivation to the phloem phase (E1/[E1+E2]) were significantly higher in the high-Hx cultivar. The increased salivation in plants with higher contents of Hx suggests the existence, at least in this system, of a chemically-mediated sieve element constraint.
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    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
    Keywords: Mebendazole–propionic acid complex ; molecular complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: Cu(II) complex ; crystal structure ; EPR spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: 2-Methylnaphthalene ; hexachlorocyclopentadiene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: Halobismuthate(III) ; phenanthroline ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: Lanthanum complex ; hexamethylenetetramine ; IR spectra ; thiocyanates ; coordination number nine ; tricapped trigonal prism ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: Cerium(IV) ; β-diketonate ; volatility ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: Nickel(II) complex ; crystal structure ; Schiff base
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Benztropine mesylate: crystal structure and kinetics of dehydration (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 885-892 
    Details
    ISSN: 1572-8854
    Keywords: Benztropine mesylate ; crystal structure ; thermal analysis ; dehydration kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: Cadmium ; crown ether ; 15-crown-5 ; 18-crown-6 ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    The crystal and molecular structure of (−)—Crinine (C16H17NO3) (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 577-579 
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    ISSN: 1572-8854
    Keywords: (−)—Crinine ; Pancratium ; alkaloid ; Amaryllidaceae ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: Metal carbonyl complexes ; chelate complexes ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Crystal structure of tris(triphenylsiloxy)borane·triphenylsilanol (1:1) adduct (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 277-281 
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    ISSN: 1572-8854
    Keywords: Triphenylsiloxy ; silanol ; borane ; crystal structure ; adduct
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 36
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    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 
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    ISSN: 1572-8854
    Keywords: Steroid ; pregnadiene ; x-ray diffraction ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Structure, absolute configuration, and conformation of the antimalarial compound, Artemisinin (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 539-543 
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    ISSN: 1572-8854
    Keywords: Antimalarial ; crystal structure ; peroxy bridge
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.]
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    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
    Keywords: Manganese(III) ; Schiff base ; hydrogen bonding ; crystal structure ; Jahn-Teller distortion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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).
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    Molecular structure of ThBr4(DME)2 (DME = 1,2-dimethoxyethane) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 243-246 
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    ISSN: 1572-8854
    Keywords: Thorium ; dimethoxyethane ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: Copper ; crystal structure ; synthesis ; Schiff base ligand
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: Europium ; terbium ; betaine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: crystal structure ; copper(II) complexes ; dinuclear complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Molecular gears: Structures of (9,10-triptyceno) crown ethers (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 513-521 
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    ISSN: 1572-8854
    Keywords: nanotechnology ; molecular devices ; triptycene ; crown ether ; crystal structure ; thallium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: alkylammonium chloroantimonates(III) ; hydrogen bonds ; disorder ; lone electron pair ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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
    Keywords: crystal structure ; complexes ; pteridine ; lumazine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: dodecanuclear heterobimetallic ; molybdenum-copper cluster ; cage ; μ6-S ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: copper(II) complexes ; 2,6-diacetylpyridine derivative ; open-chain ligand ; crystal structure ; trigonal-bipyramidal geometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: heterometallic polymeric cluster ; polythiometalate ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: oxabicyclo[3.2.1]octadiene ; absolute configuration ; asymmetric synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009532106081
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    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 
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    ISSN: 1572-8854
    Keywords: oxabicyclo[3.2.1]octadiene ; absolute configuration ; asymmetric synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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
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    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 
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    ISSN: 1572-8854
    Keywords: 2,2′-biimidazole ; diester ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 52
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    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 
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    ISSN: 1572-8854
    Keywords: Hg coordination ; crystal structure ; organomercury derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 53
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    Generation and intermolecular trapping of a cage-annulated cycloalkylidenecarbene (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 329-333 
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    ISSN: 1572-8854
    Keywords: Carbene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 54
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    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 
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    ISSN: 1572-8854
    Keywords: crystal structure ; manganese complex ; disubsituted oxamide ; addition compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 55
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    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 
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    ISSN: 1572-8854
    Keywords: pyrazolyl derivative ; substituted cyclopentane ; substituted cyclohexane ; crystal structure ; bidentate ligand
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: synthesis ; crystal structure ; independent molecules
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 57
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    The crystal and molecular structure of 2-S-methylthiouracil (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 725-727 
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    ISSN: 1572-8854
    Keywords: 2-thiouracil derivatives ; crystal structure ; S-methyl-thiouracil ; hydrogen bonding ; structural methylation and metallation effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: synthesis ; crystal structure ; Cu(I) complex ; μ-oxo-bis(2,9-dimethyl-1,10-phenanthroline) ; luminescence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Structural analysis of tris(tetra-n-butylammonium) hexakisisothiocyanatoyttrate(III) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 729-733 
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    ISSN: 1572-8854
    Keywords: crystal structure ; yttrium complexes ; isothiocyanate complexes ; octahedral coordination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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).
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    Synthesis and structure of bis(dibenzoylmethane)copper(II) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 793-796 
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    ISSN: 1572-8854
    Keywords: copper complex ; crystal structure ; dibenzoylmethane complex
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 61
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    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
    Keywords: tungsten(II) ; dibromo ; carbonyl ; diphenylcyclohexylphosphine ; but-2-yne ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 62
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    1-(Ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil: a nucleoside analog (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 837-839 
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    ISSN: 1572-8854
    Keywords: acyclonucleoside analog ; 6-(phenyl selenyl) uracil derivative ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: mercury halides ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: tungsten(II) ; Iodo ; carbonyl ; cis-bis(diphenylphosphino)ethene ; but-2-yne ; cationic ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    4-(1,4-Dimethoxy-2-naphthyl)-4- hydroxycyclohexanone and its ethylene ketal (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 955-959 
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    ISSN: 1572-8854
    Keywords: crystal structure ; intramolecular hydrogen bond ; 4-(1,4-dimethoxy-2-naphthyl)-4-hydroxycyclohexanone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Crystal structure and physical characterization of neotame methanol solvate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 967-975 
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    ISSN: 1572-8854
    Keywords: neotame ; crystal structure ; methanol solvate ; thermal analysis ; powder X-ray diffractometry ; 13C solid-state nuclear magnetic resonance spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: cyano allyl radical ; thermal arrangement ; crystal structure ; isomer ; NMR, MM2
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    X-ray crystal structure of tetraaquabis (xanthosinato)nickel(II) hexahydrate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1009-1013 
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    ISSN: 1572-8854
    Keywords: crystal structure ; nickel complex ; xanthosine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: manganese ; pyridine-2-thiolate ; bis(diphenylphosphino)methane ; carbonyl ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 70
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    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
    Keywords: crystal structure ; imidazolidine ; triazene ; bis-triazene ; methoxy substituent ; π-π stacking
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 71
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    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 
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    ISSN: 1572-8854
    Keywords: crystal structure ; tritylaziridine ; acrylate ; spectroscopic features
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 72
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    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 
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    ISSN: 1572-8854
    Keywords: absolute configuration ; asymmetric synthesis ; azabicyclo[3.2.1]octadiene ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 73
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    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
    Keywords: Ruthenium ; thioether macrocycle ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of 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.
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    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 
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    ISSN: 1572-8862
    Keywords: Mixed-metal cluster ; crystal structure ; magnetic properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The 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.
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    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
    Keywords: Dynamic disorder ; crystal structure ; ruthenium cluster
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The 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.
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    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
    Keywords: electroless Ni–Co–B alloy ; dimethylamineborane ; complexing agent ; deposition rate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Electrical Engineering, Measurement and Control Technology
    Notes: 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.
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  • 77
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    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 
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    ISSN: 1572-8854
    Keywords: Copper ; 1,10-phenanthroline ; trifluoroacetate ; crystal structure ; magnetic exchange
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 78
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    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
    Keywords: π-allyl ; carbonyl ; nitrile ; chloro ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 79
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    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
    Keywords: 1,10-Phenanthroline ; bis-phenanthrolineprotium ; adduct ; crystal structure ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Crystal structure of the cytotoxic marine alkaloid 2-bromoleptoclinidinone (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 645-648 
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    ISSN: 1572-8854
    Keywords: 2-Bromoleptoclinidinone ; marine alkaloid ; cytotoxic ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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  • 81
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    Crystal structure of [Co(bipy)(maleato) (H2O)3]·H2O (bipy = 2,2′-bipyridine) (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1081-1084 
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    ISSN: 1572-8854
    Keywords: cobalt(II) ; bipyridine ; maleato ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: Rubidium nitroprusside monohydrate ; crystal structure ; properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    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 
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    ISSN: 1572-8854
    Keywords: crystal structure ; methyl propiolate ; sulfenic acid ; vinyl sulfoxide ; leinamycin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    9[1-(2-Hydroxy ethoxy)-3-hydroxy propyl] guanine: a nucleoside analog (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1137-1139 
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    ISSN: 1572-8854
    Keywords: acyclic nucleoside analog ; acyclovir ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Structure, thermal behavior, and IR investigation of a new organic sulfate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1205-1210 
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    ISSN: 1572-8854
    Keywords: organic sulfate ; crystal structure ; DTA/TG/DSC ; vibrational spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    Structure of de-oxy corticosterone-21-hemisuccinate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 1265-1269 
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    ISSN: 1572-8854
    Keywords: crystal structure ; corticosteroid ; de-oxy corticosterone-21-hemisuccinate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009504923424
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  • 87
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    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
    Keywords: crystal structure ; pyrazolo[3,4-d]pyrimidine ; fungicidal activity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009565209312
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  • 88
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    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
    Keywords: Manganese (II) ; phenanthroline ; polymeric complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009574128099
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  • 89
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    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
    Keywords: crown ether ; crystal structure ; lariat ; sodium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009552806586
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  • 90
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    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
    Keywords: crystal structure ; pregnen ; progestin ; 4-pregnen-21-ol-3,20-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009556907495
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  • 91
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    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
    Keywords: orotic acid complex ; crystal structure ; copper(II) complex
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009596719033
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  • 92
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    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
    Keywords: pseudo-square pyramidal Cu(II) complex ; trans-4-styrylpyridine ; crystal structure ; IR, electronic, and EPR spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009510910121
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  • 93
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    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
    Keywords: crystal structure ; ab initio calculations ; conjugation ; phosphabutadienes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009527413755
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  • 94
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    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
    Keywords: contrast agents ; crystal structure ; ortho ester
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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)°.
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    URL: http://dx.doi.org/10.1023/A:1009531514664
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  • 95
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    Structure refinement and Raman spectrum of silver azide (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 561-564 
    Details
    ISSN: 1572-8854
    Keywords: crystal structure ; Raman spectrum ; silver azide ; azide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009544702195
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  • 96
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    Structure of adamantan-1-ammonium 1-adamantanecarboxylate (1999)
    Springer
    Journal of chemical crystallography 29 (1999), S. 845-848 
    Details
    ISSN: 1572-8854
    Keywords: crystal structure ; centrosymmetric ; aminoadamantane derivative ; antiviral ; dispiro compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009564307821
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  • 97
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    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
    Keywords: cyclohexaphosphates ; organometallic compound ; crystal growth ; X-ray diffraction ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1009521911166
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  • 98
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    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
    Keywords: Quinoline ; chloroquine ; antimalarial ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1022810821793
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  • 99
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    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
    Keywords: Co(III) complex ; crystal structure ; kinetics ; steric effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1021786804676
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  • 100
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    Crystal structure of NH3(CH2)2NH3BiCl5·2H2O (1998)
    Springer
    Journal of chemical crystallography 28 (1998), S. 209-212 
    Details
    ISSN: 1572-8854
    Keywords: Bismuth ; crystal structure ; inorganic polymer
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: 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.
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    URL: http://dx.doi.org/10.1023/A:1022474327917
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