η3- Allymetall-Schwefel-Cluster des Nickels, Palladiums und Platins / η3-Allyl Metal Sulfur Cluster Compounds of Nickel, Palladium, and Platinum

1979 ◽  
Vol 34 (4) ◽  
pp. 609-613 ◽  
Author(s):  
Borislav Bogdanović ◽  
Richard Goddard ◽  
Peter Göttsch ◽  
Carl Krüger ◽  
Klaus Schlichte ◽  
...  

AbstractNovel cluster compounds of the composition [(η3-C3H5)2M2S]x, wherein M represents nickel, palladium or platinum are obtained by reaction of 2,5-disubstituted-1,6,6a-trithiopentalenes or H2S with (η3-C3H5)2M in THF solution. The molecular structure of one of these new cluster types [(η3-C3H5Ni)2S]3 has been established by X-ray methods. It is best described as being a fraction of a NiS-framework in which peripheral coordination sites are occupied by partial disordered η3-allyl groups. Molecular data (cell data: a = 19.868(4), b = 8.988(2), c = 14.501(3) Å, β = 115.30(2)°, space group C2/c, Z = 4, R = 0.106) are compared with the parent Bs-NiS lattice. Spectroscopic evidence for the structural similarity of the related Pd- and Pt-compounds is given.

1980 ◽  
Vol 33 (6) ◽  
pp. 1373 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp

The crystal and molecular structure of a platinum(0) complex of cyclooctyne, [(coct)Pt(PPh3)2], has been determined from three- dimensional X-ray data collected by counter methods. The complex crystallizes in the space group P21/n [a non-standard setting of space group P21/c (C2h5, No. 14)], with a 20.660(9), b 12.299(5), c 15.470(7) Ǻ, β 110.26(2)°, Z 4. The structure was solved by conventional Patterson and Fourier methods and was refined by block-diagonal least-squares techniques to weighted and unweighted R-factors of 0.048 and 0.047 respectively, for the 4733 unique reflections with I/σ(I) ≥ 3.0. The molecule is essentially square planar about the 'central' platinum atom, with the triphenylphosphine groups occupying cis coordination sites. The Pt-C distances are equal within experimental error [2.034(9) and 2.037(9) Ǻ] and compare favourably with the corresponding distances in the platinum(0)-cyclohexyne and -cycloheptyne analogues. The acetylenic C=C distance is 1.279(13) Ǻ and shows the normal bond lengthening consequent upon coordination.


1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2


1979 ◽  
Vol 34 (1) ◽  
pp. 48-51 ◽  
Author(s):  
Jürgen Kopf ◽  
Klaus von Deuten ◽  
Bahman Nakhdjavan ◽  
Günter Klar

Abstract The structure of 2,8-dimethyldibenzo[c,g][1,2,5,6]tetrathiaocin (1b) has been determined by X-ray methods and discussed in connection with the preferred conformations of diaryl disulfides. The compound has the anti-form I. The SS-distance is 205.8 pm, the mean CSS-angle 104.1°, and the CSS/SSC-dihedral angle 111.1°.


1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.


2006 ◽  
Vol 62 (5) ◽  
pp. i117-i119 ◽  
Author(s):  
María A. Castellanos R. ◽  
Sylvain Bernès ◽  
Marina Vega-González

A high-precision structure of tetracobalt diniobium nonaoxide, Co4Nb2O9, is presented, based on X-ray single-crystal data. The space group and cation distribution previously obtained from powder data [Bertaut, Corliss, Forrat, Aleonard & Pauthenet (1961). J. Phys. Chem. Solids, 21, 234–251] are confirmed.


1985 ◽  
Vol 40 (6) ◽  
pp. 726-729 ◽  
Author(s):  
Klaus Güde ◽  
Christoph Hebecker

Abstract Single crystals of KSc2F7 have been prepared from a mixture of KF and ScF3 . The samples were investigated by X-ray methods. KSc2F7 crystallizes orthorhombically with a = 10.643(2), b = 6.540(1), c = 4.030(1) Å. These data indicate a close crystallographic connection to the monoclinic unit cell of KIn2F7 [1], But in contrast to KIn2F7 , KSc2 F7 crystallizes in space group No. 65. Cmmm - D192h. The R-value for 341 observed independent reflections is 0.060.


1988 ◽  
Vol 43 (4) ◽  
pp. 497-498
Author(s):  
Franz A. Mautner ◽  
Harald Krischner ◽  
Christoph Kratky

Abstract The crystal structure of Rb2Ca(N3)4 · 4H2O has been determined by single crystal X-ray methods. The compound is isotypic with K2Ca(N3)4 · 4 H2O and crystallizes in the orthorhombic space group Ccca, Z = 4, a = 1949.1(12) pm, b = 1099.5(3) pm, c - 622.2(1) pm.


1984 ◽  
Vol 39 (5) ◽  
pp. 582-585 ◽  
Author(s):  
Klaus Brodersen ◽  
Manfred Cygan ◽  
Hans-Ulrich Hummel

Single crystals of SrHg(SeCN)4 · 4 pyridine are prepared by reaction of K2Hg(SeCN)4 with SrCl2 in CH3OH/C2H5OH in the presence of pyridine.The crystal structure was solved with X-ray methods (Mr = 1024.1, space group P4̄n2, Z = 2, a = 9.552(2) Å, c = 17.610(7) Å, V = 1606.7 Å3, λ(AgKα) = 0.5583 Å, dc = 2.12 g cm-3, μ(AgKα) = 57.40 cm-1, F(000) = 943.7, T = 298 K. Final R = 0.043 for 1050 independent reflections).The structure consists of nearly tetrahedral Hg(SeCN)4-units. The SeCN-group is linear within the experimental error. The N-atoms of SeCN and pyridine contribute to the Archimedean antiprismatic coordination of strontium


1995 ◽  
Vol 50 (4) ◽  
pp. 577-580 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of (Cu0.22Mg0.78)BaNd2Mo4O16 have been prepared by crystallization from melts and investigated by X-ray methods. The compound crystallizes monoclinically, space group C62h - C12/c1, Z = 4, a = 5.351(1), b = 12.891(2), c = 19.391(4) Å,β = 90.899(14)° and is isotypic to CuKHo2Mo4O16. The crystal structure is dominated by BaO10 and NdO8 polyhedra forming a three-dimensional polyhedra network, which is filled by axially distorted (Cu,Mg)O6 octahedra and MoO4 tetrahedra.


1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.


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