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1

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The synthesis and structural analysis of Pt2Ru4(CO)18 and the products obtained from its reactions with 1, 2-bis(diphenylphosphino)ethane (1993)

Adams, Richard D. ; Chen, Gong ; Wu, Wengan

Springer

Journal of cluster science 4 (1993), S. 119-132

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ISSN: 1572-8862

Keywords: Platinum ; ruthenium ; crystal structure ; heteronuclear 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 From the reaction of Ru(CO)5 and Pt(COD)2, COD = 1, 5-cyclooctadiene, the new platinum-ruthenium heteronuclear cluster complex Pt2Ru4(CO)18,1, was obtained in 60% yield.1 has a folded ladder-like structure with alternating pairs of ruthenium atoms and platinum atoms. The cluster of1 can be split to yield the known compound PtRu2(CO)8(η2-dppe),2, (54% yield) by reaction with 1, 2-bis(diphenylphosphino)ethane, dppe, at 25°C. When1 was treated with excess dppe at 40°C, thebis-diphos compound3, PtRu2(CO)6(μ-η2-dppe)2 was obtained (39% yield). Under the similar reaction conditions,2 was converted to3 in 44% yield. All these complexes were characterized by single crystal X-ray diffraction analyses. Compounds2 and3 both contain a triangular cluster of one platinum and two ruthenium atoms, but in2 the bidentate ligand, dppe, chelates the platinum atom and in3 the two dppe ligands bridge the two Pt-Ru metal-metal bonds. Crystal data for1: space group C2/c,a=12.542(2)Å,b=15.350(4)Å,c=15.252(3)Å, β=105.32(2)°,Z=4, 2192 reflections,R=0.025. For2: space group P21/c,a=14.351(2)Å,b=13.486(3)Å,c=19.218(3)Å, β=108.48(1)°,Z=4, 3029 reflections,R=0.027. For3: space group P21/c,a=18.836(6)Å,b=15.559(5)Å,c=23.259(7)Å, β=111.26(2)°,Z=4, 4204 reflections,R=0.038.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00702713

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2

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Preparation and structural characterization of the hexatungsten cluster complex (EDTEH)2[W6(μ3-Cl)8Cl6], (EDTEH=(MeO2CCH2)2N(H)CH2CH2N(CH2CO2Me)2+ (1993)

Adams, Richard D. ; Chen, Gong ; Huang, Jianquan

Springer

Journal of cluster science 4 (1993), S. 271-277

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ISSN: 1572-8862

Keywords: Tungsten ; chloride ; hexatungsten ; 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 hexanuclear tungsten cluster complex [W6(μ3-Cl)8Cl6]2−,1 was isolated as a salt of the cation (MeO2CCH2)2N(H)CH2CH2N(CH2CO2Me)2+, EDTEH+, by crystallization from methanol solvent of the product obtained from the reaction of (H3O)2[W6(μ3-Cl)8Cl3] with the disodium salt of ethylenediaminetetraacetic acid. The compound was charcterized by single-crystal X-ray diffraction analysis. The cluster anion contains an octahedral arrangement of six tungsten atoms with chloride ligands bridging the eight triangular faces of the cluster and one chloride ligand terminally coordinated to each of the six tungsten atoms. The cation (EDTEH)+ achieves its positive charge by protonation of one of the nitrogen atoms. Crystal data: space group = P21/a,a=10.689(2) Å,b=22.931(6) Å,c=12.093(3) Å, β=98.41(2)°,Z=2, 2476 reflections,R=0.028.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00703743

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3

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Preparation and structural characterization of a hexanuclear molybdenum (II) cluster containing carboxylate ligands (Bu4N)2[Mo6(μ3-Cl)8(O2CMe)6] (1993)

Adams, Richard D. ; Chen, Gong ; Huang, Jianquan

Springer

Journal of cluster science 4 (1993), S. 151-157

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ISSN: 1572-8862

Keywords: Molybdenum ; acetate, carboxylate ; hexamolybdenum ; 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 hexamolybdenum cluster complex [Mo6(μ3-Cl)8(O2CMe)6]2−, 1 was isolated as the Bu4N+ salt in 71% yield from the reaction of (Bu4N)2[Mo6(μ3-Cl)8Cl6] with AgO2CMe in CH2Cl2 solvent. The compound was characterized by single crystal X-ray diffraction analysis. The cluster contains an octahedral arrangement of six molybdenum atoms with eight chloride ligands bridging the eight trianglar faces and six carboxylate ligands terminally coordinated through one oxygen atom to each of the six molybdenum atoms. Crystal data: space group =P21/n,a=10.713(3)Å,b=14.43(1)Å,c=21.919(4)Å, β=94.37(2)°,Z=2, 1965 reflections,R=0.036.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00702715

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4

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Synthesis, characterization and x-ray structure of V3(μ3-O)(μ-Cl)Cl6(μ-η1-η1-PhNHNH2)2(PhNHNH2)2(THF) · 6THF: A new binding mode for phenylhydrazine (1993)

Murray, H. H. ; Novick, S. G. ; Armstrong, W. H. ; [et al.]

Springer

Journal of cluster science 4 (1993), S. 439-451

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ISSN: 1572-8862

Keywords: Vanadium ; phenylhydrazine ; nitrogenase ; 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 Addition of phenylhydrazine to a mixture of VCl3 · THF/N,N-propyl-bis (salicyladimine) and sodium hydride yielded a trinuclear vanadium complex, V3(μ3-O)(μ-Cl)Cl6(μ-η1-η1PhNHNH2)2(PhNHN H2)2(THF), containing two bridging and two terminal phenylhydrazine ligands. The product has been crystallographically characterized (P21/n, a=12.949(2) Å,b=24.061(4) Å,c=22.504(4) Å, β=107.22(1) deg.,V=6697(2) Å3 withZ=4) and was found to contain the first example of bridging monosubstituted hydrazine (phenylhydrazine) ligands.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00703736

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5

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Effects of higher-order structure of poly(3-hydroxybutyrate) on its biodegradation. II. Effects of crystal structure on microbial degradation (1993)

Nishida, Haruo ; Tokiwa, Yutaka

Springer

Journal of polymers and the environment 1 (1993), S. 65-80

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ISSN: 1572-8900

Keywords: Biodegradable plastic ; microbial degradation ; bacterial poly(d-(−)-3-hydroxybutyrate) ; crystal structure ; physiological behavior

Source: Springer Online Journal Archives 1860-2000

Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics

Notes: Abstract As one of a series of studies concerning the relationship between the higher-order structure and the biodegradability of a biodegradable plastic, the effects of the crystal structure of the plastic on microbial degradation were investigated. Bacterial poly(d-(−)-3-hydroxybutyrate) (PHB) films which had a wide range of crystallinity were prepared by the melt-quenching method. Results of the microbial degradation indicated that the development of crystallinity evidently depressed the microbial degradability. From scanning electron microscopy (SEM) observations, it is suggested that the microbial degradation proceeded in at least two manners. One was preferential degradation of the amorphous region leaving the crystalline lamellae intact, which was considered to be a homogeneous enzymatic degradation over the surface. The other was nonpreferential spherical degradation on the surface. The SEMs indicate that the spherical holes were the result of colonization by degrading bacteria. The holes varied in size and number with the change of crystal structure. Therefore, it is considered that the crystal structure of PHB also influenced the physiological behavior of the degrading bacteria on the PHB surface.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF01457654

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6

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Analysis of atomic displacement parameters and molecular motion in crystals. Part 2. X-ray crystal structure of K2Ru(SO4)2 * 6H2O at 160 K and 295 K (1993)

Bürgi, Hans -Beat ; Raselli, Andrea

Springer

Structural chemistry 4 (1993), S. 23-31

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ISSN: 1572-9001

Keywords: Atomic displacement ; molecular motion ; vibrational analysis ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Chemistry and Pharmacology

Notes: Abstract Atomic displacement parameters determined from a single-crystal X-ray-diffraction study on K2Ru(SO4)2 * 6H2O are analyzed in the molecular mean field approximation. The motion of SO2 2− can be described with a rigid-body model, whereas for [Ru(H2O)6]2+ internal stretching motion and coupling between stretching motion and overall translation are found to be necessary for explaining the observed atomic displacement parameters. Frequencies and force constants of internal motion are not significantly affected by such couplings. K2Ru(SO4)2 * 6H2O crystallizes in the monoclinic space groupP21/c (No. 14), witha = 6.1211(7)Å,b = 12.226(2) Å,c = 8.916(2)Å,β = 105.11(1)°,Z = 2 at 160 K anda = 6.1402(7)Å,b = 12.274(2)Å,c = 8.957(1)Å,β = 105.25(1)°,Z = 2 at 295 K. The structure was refined to a finalR(F) of 0.017 at 160 K and of 0.019 at 295 K for 1438 and 1299 observed reflections withF 0 〉 6σ(F0) and sin θ/λ 〉 0.617 Å1−.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00672096

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7

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Synthesis and structural chemistry of novel heteropolymolybdates and -tungstates (1993)

Krebs, B. ; Klein, R.

Springer

Molecular engineering 3 (1993), S. 43-59

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ISSN: 1572-8951

Keywords: Heteropolymolybdates ; heteropolytungstates ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Chemistry and Pharmacology

Notes: Abstract The chemistry of polynuclear oxometalate anions is dominated by molybdenum and tungsten in their highest oxidation state. During the past twenty years this class of compounds has attracted much attention because of their variable applications, e.g. as reagents in analytical procedures, as industrial catalysts and as potential anticancer drugs. In order to obtain model systems for the investigation of the catalytic activity of heteropolyanions we have synthesized and structurally characterized some organo derivatives of polyoxoanions. We secondly focus on Sb(III) and Bi(III) heteropolytungstates to examine the important influence of the unshared electron pair on the resulting structures and properties. Some of these compounds may be regarded as supramolecular aggregates showing inclusion phenomena. In 9 two [SbW9O33]9− anions are linked by a set of six sodium ions forming a nearly planar hexagon. The sodium ions are enveloped by an oxygen cage formed by terminal oxygen atoms of the polyanions and by water molecules. Furthermore, the four anions [Sb2W22O74(OH)2]12−, [Sb2W20Fe2O70(H2O)6]8−, [Sb2W20Co2O70(H2O)6]10− and [Bi2W20Fe2O68(OH)2(H2O)6]6− (in10, 11, 12, 13) may be regarded as transition metal complexes of novel [Sb2W20O70]14− or [Bi2W20O70]14− anions which are serving as ligands. The octahedral coordination sphere of each transition metal is formed by three oxygen atoms of the anion and completed by three water molecules. The Sb(III) heteropolyanion, [Na2Sb8W36O132(H2O)4]22− in (14) includes two sodium and four antimony ions besides four water molecules. Each anion consists of four β-B-SbW9-Keggin fragments linked together by four SbO4-groups, incorporating two sodium and four water molecules effecting an additional connection of the subunits.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00999623

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8

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Redetermination of the cobaltocene crystal structure at 100 K and 297 K: Comparison with ferrocene and nickelocene (1993)

Antipin, M. Yu. ; Boese, R. ; Augart, N. ; [et al.]

Springer

Structural chemistry 4 (1993), S. 91-101

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ISSN: 1572-9001

Keywords: Cobaltocene ; molecular geometry ; crystal structure

Source: Springer Online Journal Archives 1860-2000

Topics: Chemistry and Pharmacology

Notes: Abstract The molecular and crystal structures of the monoclinic modification of cobaltocene Cp2Co (P21/n, Z=2) was determined at 100 K and 297 K with new sets of X-ray diffraction data (MoKα radiation, 3995 and 6534 reflections, refinement toR = 0.026 and 0.030 using 1061 and 1299 independent observable reflections, respectively). At 297 K the structure is disordered (similar to the isomorphous ferrocene and nickelocene) with two distinct orientations of the ring, differing in occupancy factors (80% and 20%) and by a rotation angle in the ring plane of approximately 34°. Just as for nickelocene but in contrast to ferrocene, no sharp phase transition was found on cooling Cp2Co to 100 K, but an essential ordering of the Cp-ring position was detected with a decrease of the contribution of the second minor orientation to nearly 10%. On the basis of a careful analysis of the molecular geometry, crystal packing, and anisotropic atomic displacement parameters, a dynamic temperature-dependent nature of the disorder in Cp2Co is assumed.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00677370

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9

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Structural, immunocytochemical and initial biochemical characterization of NAOH-extracted gap junctions from an insect, Heliothis virescens (1993)

Ryerse, J. S.

Springer

Cell & tissue research 274 (1993), S. 393-403

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ISSN: 1432-0878

Keywords: Gap junction ; Cell junction ; Immunocytochemistry ; Biochemistry ; Heliothis virescens (Insecta)

Source: Springer Online Journal Archives 1860-2000

Topics: Biology , Medicine

Notes: Abstract Subcellular fractions enriched in gap junctions with an ultrastructure similar to those in intact insect tissue have been obtained by extracting crude membranes from the tobacco budworm Heliothis virescens (Lepidoptera: Noctuidae) with 2.5 mM NaOH. n-Octyl-β-d-glucopyranoside (OG) was used to further purify integral membrane proteins in the NaOH-extracted fractions. A polyclonal antibody (R16) is described that specifically labels nonextracted and NaOH-extracted gap junctions in cell fractions by electron microscope immunocytochemistry. R16 immunostaining of sectioned Heliothis testis at the light-microscope level yields a pattern of immunoreactivity consistent with the distribution of gap junctions in the tissue. R16 identifies a 40-kDa protein as a candidate gap junction protein on immunoblots of crude membrane, NaOH-extracted and NaOH/OG-extracted fractions.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00318758

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10

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Polar bonds in π-complexes. Preparation and crystal structures of cyclopentadienylcarbonyl iron(II) and ruthenium(II) benzoates andp-fluorobenzoates (1993)

Batsanov, A. S. ; Manole, O. S. ; Struchkov, Yu. T. ; [et al.]

Springer

Russian chemical bulletin 42 (1993), S. 359-364

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ISSN: 1573-9171

Keywords: iron(II) and ruthenium(II) complexes ; synthesis ; carbonyl, cyclopentadienyl, benzoate ligands ; crystal structure ; X-ray diffraction

Source: Springer Online Journal Archives 1860-2000

Topics: Chemistry and Pharmacology

Notes: Abstract Complexes of Fe(II) and Ru(II) of the general formula Cp(OC)2MOC(O)C6H4X-p, where M=Fe, X=H, F (1, 2) or M=Ru, X=H, F (3, 4) have been prepared by reactingp-XC6H4COOAg with [CpFe(CO)2]2 or CpRu(CO)2I. The crystal structures of complexes1–3 have been determined using X-ray diffraction. Compounds1 and3 are isomorphous. The COO group in1–3 is coordinated as a monodentate ligand. As the latter and the CO ligands are electronically non-equivalent, the coordination of the Cp ligand to the metal is slightly asymmetric.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1007/BF00697097

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