Alkyl, hydrido-, and related compounds of ruthenium(II) with trimethylphosphine. X-Ray crystal structures of hydrido(tetrahydroborato-HH′)tris(trimethylphosphine)ruthenium(II), tri-µ-chloro-bis[tris(trimethylphosphine)ruthenium(II)] tetrafluoroborate, and bis[cis-methyltetrakis(trimethylphosphine)ruthenio]mercury(II)–tetrahydrofuran(1/1)

Author(s):  
John A. Statler ◽  
Geoffrey Wilkinson ◽  
Mark Thornton-Pett ◽  
Michael B. Hursthouse
Crystals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 807
Author(s):  
Ilya V. Kornyakov ◽  
Sergey V. Krivovichev

Single crystals of two novel shchurovskyite-related compounds, K2Cu[Cu3O]2(PO4)4 (1) and K2.35Cu0.825[Cu3O]2(PO4)4 (2), were synthesized by crystallization from gaseous phase and structurally characterized using single-crystal X-ray diffraction analysis. The crystal structures of both compounds are based upon similar Cu-based layers, formed by rods of the [O2Cu6] dimers of oxocentered (OCu4) tetrahedra. The topologies of the layers show both similarities and differences from the shchurovskyite-type layers. The layers are connected in different fashions via additional Cu atoms located in the interlayer, in contrast to shchurovskyite, where the layers are linked by Ca2+ cations. The structures of the shchurovskyite family are characterized using information-based structural complexity measures, which demonstrate that the crystal structure of 1 is the simplest one, whereas that of 2 is the most complex in the family.


1986 ◽  
Vol 15 (1) ◽  
pp. 121-124 ◽  
Author(s):  
Sadatoshi Akabori ◽  
Sadao Sato ◽  
Takehiko Tokuda ◽  
Yoichi Habata ◽  
Kayoko Kawazoe ◽  
...  

1997 ◽  
Vol 53 (1) ◽  
pp. 125-134 ◽  
Author(s):  
A. F. Jensen ◽  
V. Petříček ◽  
F. K. Larsen ◽  
E. M. McCarron

The structure of the modulated, composite crystal bismuth strontium cuprate [M′2Cu2O3]7[CuO2]10, with M′ = Bi0.04Sr0.96, has been determined and refined using a model which allows modulation of the atomic positional parameters for all atoms, as well as modulation of thermal parameters for the M′ site. The structure is orthorhombic, with c being the misfit direction and a = 11.4712 (6), b = 13.3765 (13) Å. Sublattice 1, of composition (CuO2)4, has c l = 2.7509 (10) Å, while sublattice 2, of composition (M′2Cu2O3)4, has c 2 = 3.9316 (3) Å. Superspace group Amma(001 + γ)ss\overline 1; q = γc l* with γ = 0.6997 (3); λ = 0.6565 Å, μ = 25.4 mm−1. The final residual is R all = 0.0474 for all 1174 reflections, R main = 0.0451 for the 549 main reflections, R 1.sat = 0.0562 for the 442 first-order satellite reflections and R 2.sat = 0.1044 for the 183 second-order satellite reflections. The satellite reflections have been collected with X-ray synchrotron radiation. It is shown that these reflections help to unambiguously determine the superspace group. The orthorhombic compound has a layered structure, stacked along the b axis. The first sublattice consists of layers of CuO2 ribbons, with CuO4 squares sharing edges along the c axis. The second sublattice consists of CuO4 squares, which are sharing edges in a zigzag pattern. In-between these layers the disordered layers of Bi and Sr atoms are sandwiched. A comparison with structurally and chemically related compounds is made.


2001 ◽  
Vol 79 (5-6) ◽  
pp. 731-741 ◽  
Author(s):  
Paul Beagley ◽  
Philip Davies ◽  
Harry Adams ◽  
Colin White

The syntheses of the chiral ansa-metallocene complexes TiCl2(η5:η5-C5Me4SiMe2C5H3R*) (R* = menthyl (4a) or neomenthyl (4b)) are reported; initially 4a was obtained as a 3:1 mixture of (R:S) diastereoisomers, which differ only in which face of the asymmetrically substituted cyclopentadienyl ring is bonded to the titanium (chiral descriptor shown). The major diastereomer 4aR was crystallized out optically pure from the initial reaction mixture, whereas the 4aS diastereoisomer was isolated after isomerizing a racemic mixture of 4a to a 1:3 mixture of (R:S) diastereoisomers using UV irradiation. The corresponding neomenthyl complex 4b was obtained as a 1.3:1 mixture of diastereoisomers that could not be separated. The optically pure 4aR was converted stereoselectively into the corresponding (R)-TiMe2(η5:η5-C5Me4SiMe2C5H3R*) (R* = menthyl). Syntheses of the related indenyl ligand system C5Me4SiMe2C9H7 (3) is reported but complexation to titanium proved to be problematic although ZrCl2(η5:η5-C5Me4SiMe2C9H6) (6) was isolated. The crystal structures of both 4aR and 4aS are reported and compared. Crystals of 4aR are orthorhombic, a = 27.857(11), b = 9.985(5), and c = 9.596(4) Å, Z = 4, space group P212121 (D24, No. 19), and those of 4aS are monoclinic, a = 8.5810(10), b = 38.679(4), and c = 8.5842(10) Å, β = 113.001(2)°, Z = 4, space group P21 (C22, No. 4). The structures were solved by the Patterson method and 4aR was refined by blocked-cascade least-squares procedures to R = 0.0628 (Rω = 0.0503) for 902 reflections with |F|/σ(|F|) [Formula: see text] 3.0, whereas 4aS was refined by full-matrix least-squares procedures to R = 0.0646 (wR2 = 0.1829) for 5734 reflections with |F|/σ(|F|) [Formula: see text] 4.0. Both diastereomers of 4a catalyze hydrosilylation of ketones, but as expected from a comparison of the two crystal structures, the 4aR isomer is the more stereoselective catalyst, i.e., hydrosilylation of acetophenone followed by hydrolysis gives 82% enantiomeric excess (ee) of (S)-PhCH(Me)OH with 4aR whereas only 16% ee of (R)-PhCH(Me)OH with 4aS.Key words: titanium, metallocene, chiral, structure, catalyst.


1996 ◽  
Vol 51 (6) ◽  
pp. 826-831 ◽  
Author(s):  
Stefan Peschel ◽  
Werner Paulus ◽  
Dietrich Babel

Abstract The crystal structures of four isotypic cyano complexes, belonging to the monoclinic type of cryolite (P21/n, Z = 2), were determined by single crystal X-ray methods and in one case also by neutron diffraction: Rb2LiFe(CN)6 (a = 717.3, b = 748.0, c = 1030.2 pm, β = 90.24°; Fe - C = 193.6, C - N = 114.5, Li - N = 227.0 pm), Rb,NaFe(CN)6 (a = 724.5, b = 772.5, c = 1055.2 pm, β = 90.39°; Fe - C = 193.9, C - N = 114.2, Na - N = 250.4 pm), Rb,LiCo(CN)6 (a = 715.5, b = 741.2, c = 1025.0 pm, β = 90.14°; Co - C = 189.6, C - N = 114.3, Li - N = 226.9 pm), Rb2NaCo(CN)6 (a = 722.5, b = 766.3, c = 1049.2 pm, β = 90.33°; Co - C = 189.9 (188.8), C - N = 113.4 (7/5.5), Na - N = 250.6 (249.6 pm). The irregular [RbN8l coordination polyhedra exhibit average distances close to Rb - N = 336 pm. Details are discussed and the results compared with those of related compounds


1997 ◽  
Vol 52 (1) ◽  
pp. 17-24 ◽  
Author(s):  
Henry Strasdeit ◽  
Angelika von Döllen ◽  
Anne-Kathrin Duhme

The rac-lipoato (lip-) complexes [Zn(lip)2(H2O)2] (1) and [Cd(lip)2(H2O)2] (2) were obtained in good yields from solutions of sodium lipoate and the respective metal nitrate in methanol/water. 1 and 2 form pale yellow, moderately light-sensitive crystals.Both compounds were structurally characterized by single-crystal X-ray diffraction. 1: C2/c, a = 39.958(6), b = 5.360(1), c = 10.794(1) Å, β = 95.76(1)°, Z = 4, wR2 = 0.150 (all data). 2: C2/c, a = 38.200(2), b = 5.472(1), c = 11.179(1) Å, β = 92.72(1)°, Z = 4, wR2 = 0.090 (all data). The metal ions are hexacoordinated by the oxygen atoms of two chelating carboxylate ligands and two aqua ligands. The crystal structures are very similar but not isotypic. They are layer structures, in which the complexes within a layer are interconnected by a network of hydrogen bonds. Adjacent layers have contacts via the 1,2-dithiolanyl rings of their lipoato ligands.Crystals of 1 and 2 decompose on exposure to visible light or ultraviolet radiation in the 280-390 nm range. Photopolymerization by formation of intermolecular S-S bonds is very probably involved. Furthermore, the infrared spectra reveal the transformation of COO- into COOH groups


1997 ◽  
Vol 36 (6) ◽  
pp. 1218-1226 ◽  
Author(s):  
Francesco Bigoli ◽  
Paola Deplano ◽  
Francesco A. Devillanova ◽  
John. R. Ferraro ◽  
Vito Lippolis ◽  
...  

Author(s):  
A. Zangvil ◽  
L.J. Gauckler ◽  
G. Schneider ◽  
M. Rühle

The use of high temperature special ceramics which are usually complex materials based on oxides, nitrides, carbides and borides of silicon and aluminum, is critically dependent on their thermomechanical and other physical properties. The investigations of the phase diagrams, crystal structures and microstructural features are essential for better understanding of the macro-properties. Phase diagrams and crystal structures have been studied mainly by X-ray diffraction (XRD). Transmission electron microscopy (TEM) has contributed to this field to a very limited extent; it has been used more extensively in the study of microstructure, phase transformations and lattice defects. Often only TEM can give solutions to numerous problems in the above fields, since the various phases exist in extremely fine grains and subgrain structures; single crystals of appreciable size are often not available. Examples with some of our experimental results from two multicomponent systems are presented here. The standard ion thinning technique was used for the preparation of thin foil samples, which were then investigated with JEOL 200A and Siemens ELMISKOP 102 (for the lattice resolution work) electron microscopes.


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