Structural studies in the ruthenium(II)/(±)-ortho-Phenylenebis{methyl(phenyl)-phosphine/arsine) system. II. Crystal structure of trans-Dichloro[(±)-ortho-phenylenebis{methyl(phenyl)-phosphine}][(±)-ortho-phenylenebis(methyl(pheny1)-phosphine) P-oxide]ruthenium(II)

1983 ◽  
Vol 36 (2) ◽  
pp. 267 ◽  
Author(s):  
SR Hall ◽  
BW Skelton ◽  
AH White

The crystal and molecular structure of the title complex, trans-[RuCl2{(�)-o-C5H4(PMePh)2}{(�)- o-C5H4(PMePh)(P(O)MePh)}], has been established by a single-crystal X-ray diffraction study at 295(1) K, being refined to a residual of 0.037 for 2669 independent 'observed' reflections. Crystals are orthorhombic, P212121, a 16.655(5), b 15.805(4), c 14.823(8) �, Z 4. The chlorine atoms lie trans to each other in the coordination sphere of the six-coordinate ruthenium, with the O-C6H4(PMePh)2 and o-C6H4(PMePh)(P(O)MePh) ligands being P,P? and O,P' bidentate respectively. The ruthenium-chlorine distances are 2.434(2) and 2.425(2) �; the two mutually trans ruthenium- phosphine distances are 2.310(3) and 2.346(2) �, but that which is trans to the oxygen is unusually short, being 2 219(2) �. The ruthenium-oxygen distance is 2.166(5)�.

1983 ◽  
Vol 36 (2) ◽  
pp. 259 ◽  
Author(s):  
SC Grocott ◽  
BW Skelton ◽  
AH White

The crystal and molecular structure of the title complex, trans-[RuH(CO)(opmpp)2]+ (PF6)-.2(CH3)2- CO [opmpp ≡ (�)-ortho-phenylenebis {methyl(phenyl)phosphine) , o-C6H4(PMePh)2], has been established by a single-crystal X-ray diffraction study at 295(1) K, being refined to a residual of 0.066 for 2293 independent 'observed' reflections. Crystals are monoclinic, C2/c, a 11.943(4), b 26.151(9), c 15.974(6) �, β 90.97(7)�, Z 4. In the model adopted, the ruthenium atom is located on a crystallographic twofold axis; the carbonyl and hydrido ligands lie trans to each other and are disordered about the ruthenium atom. The ruthenium-phosphorus distances are 2.320(2) and 2.317(2)�.


1983 ◽  
Vol 36 (2) ◽  
pp. 271 ◽  
Author(s):  
SR Hall ◽  
BW Skelton ◽  
AH White

The crystal and molecular structure of the title complex, cis-[Ru(CO)Cl2(dmso)(opmpp)] (1) (dmso ≡ dimethyl sulfoxide, Me2SO; opmpp ≡ (�)-ortho-phenylenebis {methyl(phenyl)phosphine},[o-C6H4(PMePh)2]), has been determined by a single-crystal X-ray diffraction study at 295(1) K, being refined to a residual of 0.050 for 6115 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 11.180(7), b 12.957(6), c 17.567(9) �, β 90.88(5)�, Z 4. The ruthenium-chlorine distances, trans to phosphine and carbonyl ligands, respectively, are 2.469(2), 2.446(2) �; the ruthenium-phosphine distances, trans to the chloride and dimethyl sulfoxide ligands, respectively, are 2.292(1), 2.313(2) �. Ruthenium-sulfur (dmso) is 2.380(2) �, while the ruthenium-carbon(CO) is c. 1.72 �. For cis-[Ru(CO)2Cl2(opmpa)] (2) (opmpa ≡ (�)-ortho-phenylenebis{methyl(phenyl)- arsine}, [o-C6H4(AsMePh)2]), refinement led to a residual of 0.036 for 2423 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 10.497(3), b 11.586(7), c 20.341(9) �, β 105.31(4)�, Z 4. Ruthenium-arsine distances, trans to carbonyl and chlorine ligands, respectively, are 2.404(1), 2.455(1) �. Ruthenium-chlorine distances, trans to arsine and carbonyl ligands, respectively, are 2.443(3), 2.433(2) �, while ruthenium-carbon(CO) distances, trans to arsine and chlorine ligands, respectively, are 1 .920(8), 1 .872(8) �.


2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.


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.


1997 ◽  
Vol 52 (2) ◽  
pp. 256-258 ◽  
Author(s):  
Evgeni V. Avtomonov ◽  
Rainer Grüning ◽  
Jörg Lorberth

Abstract The crystal structure of the title compound has been determined by X-ray diffraction methods. Due to the Lewis acidic character of the iodine substituent a “zig-zag” chain is formed via intermolecular interactions (2.933(4) A) between iodine and oxygen atoms of theocarbamate moiety. A three-dimensional network is formed through hydrogen-bridging (2.04 A) between NH-groups and the oxygen atoms of the neighbouring carbamate group of the next molecule.


1989 ◽  
Vol 44 (2) ◽  
pp. 169-174 ◽  
Author(s):  
Bruno Lunelli ◽  
Magda Monari

Abstract The crystal and molecular structure of the dithallium salt of the 1,2-dicyanim inocyclobuten-3,4-dione dianion and of 1,2-diiodocyclobuten-3,4-dione, determined by X-ray diffraction, are reported and discussed. Results of FT-IR and calorimetric measurements are also presented.


1989 ◽  
Vol 44 (1) ◽  
pp. 5-8
Author(s):  
Michel Mégnamisi-Bélombé

Abstract trans-Dichloro(ethanedial-dioximato)(ethanediaI-dioxime)rhodium (III), RhCl2(GH)(GH2), has been synthesized and its structure determined by single crystal X-ray diffraction at room temperature. C4H7Cl2N4O4Rh, Mr = 348.94. monoclinic space group P21/ɑ; a = 10.543(3), b = 8.363(2), c = 11.512(3)Å ; β = 92.79(2)°; V = 1024Å3; Z = 4; Dc = 2.26 Mg m-3. Final Rw = 0.075 for 2035 reflections and 139 parameters. The coordination geometry around Rh is a dis­torted (4+2) octahedron, with four chelating N atoms lying in the equatorial plane and the two Cl atoms in the apical positions. The H atoms of the oxime groups are involved in relatively weak intramolecular O-H-O bridgings, as well as in very strong intermolecular bridgings which extend throughout the crystal structure and propagate nearly parallel to the [101] crystallographic direction.


1998 ◽  
Vol 53 (5-6) ◽  
pp. 634-636 ◽  
Author(s):  
Martina Näveke ◽  
Armand Blaschette ◽  
Peter G. Jones

Abstract The crystal structure of the known title compound was determined by low-temperature X-ray diffraction (orthorhombic, space group Pbcn, Z = 4). The molecule displays an unusually short O-N bond, a relatively long C-O bond and a moderately pyramidal O-NS2 skeleton (O-N 133.1, C-O 148.5 pm, sum of bond angles at N: 347.4°).


1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.


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