The Crystal and Molecular Structure of (PPh3)2PtO2•2CHCl3

1971 ◽  
Vol 49 (23) ◽  
pp. 3772-3777 ◽  
Author(s):  
P. T. Cheng ◽  
C. D. Cook ◽  
S. C. Nyburg ◽  
K. Y. Wan
Keyword(s):  
Crystal And Molecular Structure ◽  
Crystal Structure Analysis ◽  
Fold Axis ◽  
Transition Elements ◽  
Monoclinic System ◽  
X Ray ◽  
System A ◽  
Oxygen Complex ◽  
Axis Of Symmetry ◽  
Oxygen Complexes

The X-ray crystal structure analysis of the chloroform adduct of the bis(triphenylphosphine) platinum di-oxygen complex (PPh3)2PtO2•2CHCl3 is reported. The crystals belong to the monoclinic System a = 15.492(7), b = 13.520(5), c = 19.187(6) Å; β = 98.97(6)°. Space group C2/c. Z = 4 molecules per cell.A total of 2740 independent X-ray reflections were measured and refinement gave a final conventional R of 6.6%.The molecule has a two-fold axis of symmetry through the Pt atom with O—O normal to the axis. The O—O distance of 1.505(16) Å is in accord with that found with other transition elements when oxygen is taken up irreversibly to form di-oxygen complexes.

The Crystal and Molecular Structure of bis(triphenylphosphine)-(ethylene)platinum, (PPh3)2PtC2H4

1972 ◽  
Vol 50 (6) ◽  
pp. 912-916 ◽  
Author(s):  
P.-T. Cheng ◽  
S. C. Nyburg
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystal Structure Analysis ◽  
Transition Elements ◽  
Triphenyl Phosphine ◽  
Monoclinic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
System A

The X-ray crystal structure analysis of the triphenyl–phosphine platinum ethylene complex (PPh3)2PtC2H4 is reported. The crystals belong to the monoclinic system a = 16.46(3), b = 10.85(2), c = 17.85(3) Å, β = 100.5(1)°, space group P21/a, Z = 4 molecules per cell.The ethylene C—C distance of 1.434(13) Å is in accord with that found when other transition elements form metallo-cyclopropanes. The structure has been refined by anisotropic full-matrix least-squares, the final R-factor being 0.043 for 4174 observed reflections.

The crystal and molecular structure of syn-2,11-dithia[3,3]metacyclophane

1979 ◽  
Vol 57 (23) ◽  
pp. 3080-3087 ◽  
Author(s):  
Willem Anker ◽  
Gordon W. Bushnell ◽  
Reginald H. Mitchell
Keyword(s):  
Crystal And Molecular Structure ◽  
Fold Axis ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
Anti Conformer ◽  
Cell Dimensions ◽  
Out Of Plane ◽  
Methylene Groups ◽  
Axis Of Symmetry

The crystal structure of syn-2,11-dithia[3,3]metacyclophane, C16H16S2, has been determined by single crystal X-ray diffraction and refined to an R-value of 0.049. The crystal is monoclinic with cell dimensions a = 1898.2(5), b = 795.7(3), c = 924.1(4) pm, β = 100.03°(4). The space group is P21/n with 4 molecules per cell, Dm = 1.34 g cm−3, Dc = 1.317 g cm−3. Of several possible syn conformations, the molecule is found in that with the largest S—S distance of 697.4 pm. The benzenoid rings form a dihedral angle of 20.6°. The distance between the pair of aromatic H atoms which are ortho to two methylene groups is 273.0 pm, with 305.2 pm between the carbon atoms to which they are attached. Small angular distortions are observed at these carbon atoms. Mean bond lengths are: C—S 181.0(12), C—C (aromatic) 138.5(8), C—C (bridge) 151.0(11) pm. Mean bond angles are: C—S—C 104°(1), S—C—C 115.4°(9). The C—C—C angles are in the range 117.9–122.7°. The molecule possesses an approximate (non-crystallographic) 2-fold axis of symmetry passing through the midpoints of C(8)—C(18) and C(4)—C(14). The aromatic rings are planar, with the methylene carbons 5–11 pm out of plane on the sulphur side. The S(1) is 171.8(2) pm from plane 1 and 136.8(2) pm from plane 2, while for S(2) the corresponding values are 136.0(2) and 175.3(2) respectively.1Hmr data have been re-examined and compared with those obtained for other cyclophanes, together with 13Cmr data and are consistent with the fact that in solution 2,11-dithia[3,3]metacyclophane, 1, exists as the syn-conformer with no appreciable participation of the anti-conformer. All related dithia[3,3]metacyclophanes which have internal aryl hydrogens (i.e., no internal substituents) likewise appear to be syn from 1Hmr data.

The crystal and molecular structure of 6,7-bis(methoxycarbonyloxy)-1,2,3,4-tetrahydroisoquinoline-[1,2-c]-oxazol-2-one-[3,4-b]-1-chloro-3-methoxycarbonyloxy-6,7-methylenedioxyindane

1979 ◽  
Vol 57 (2) ◽  
pp. 157-159 ◽  
Author(s):  
Winnie Wong-Ng ◽  
S. C. Nyburg
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystal Structure Analysis ◽  
Intensity Data ◽  
Monoclinic System ◽  
Compound A ◽  
X Ray ◽  
Chloro Derivative ◽  
Nitrogen Ring ◽  
Synthetic Intermediate

A synthetic intermediate expected to be a spirobenzylisoquinoline bromo-derivative proved, on X-ray crystal structure analysis, to be the title compound, a chloro-derivative with the isoquinoline nitrogen ring-closed. Crystals belong to the monoclinic system, space group P21/c, a = 13.68(2), b = 10.81(2), c = 22.12(4) Å, β = 129.2(4)°, Z = 4 molecules per cell. Intensity data were collected by diffractometer and the structure refined to a conventional R of 0.051.

The crystal and molecular structure of copper(II) bis-(ethylenediamine)nitrate selenocyanate

1982 ◽  
Vol 47 (2) ◽  
pp. 409-420 ◽  
Author(s):  
Viktor Vrábel ◽  
Ján Garaj
Keyword(s):  
Crystal Structure ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Central Atom ◽  
Covalent Bond ◽  
Axial Direction ◽  
Analysis Method ◽  
Monoclinic System ◽  
X Ray ◽  
Intermolecular Contacts

The crystal structure of [Cuen2(NO3)]SeCN was solved by the single-crystal X-ray structural analysis method. The compound crystallizes in the monoclinic system with space group Pc. The unit cell has dimensions: a = 0.9254(3), b = 1.4018(3), c = 0.9722(5) nm, β = 99.20(3)°. The structure was refined by the least squares method to a final value of R = 6.8% for 1965 observed reflections. The crystal structure consits of polymeric cation chain [Cuen2(NO3)]+ and of free uncoordinated SeCN- anions. The nitrate ion NO-3 forms a bridging unit between two [Cuen3]2+ cations. The coordination polyhedron around the Cu(II) atom is a deformed octahedron, formed of two ethylendiamine molecules and two oxygen atoms of the NO-3 ions, bonded to divalent copper in the axial direction along the long coordinates. The crystal structure contains selenocyanate which is not bonded through a covalent bond to the central atom, but there are intermolecular contacts with its immediate surroundings.

Weak interactions observed in ruthenium and iridium complexes containing hydride, amine, and bulky phospyhine ligands

1997 ◽  
Vol 75 (5) ◽  
pp. 475-482 ◽  
Author(s):  
Wei Xu ◽  
Alan J. Lough ◽  
Robert H. Morris
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Weak Interactions ◽  
Crystal Structure Analysis ◽  
Monoclinic Space Group ◽  
Iridium Complexes ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Van Der Waals Contacts

New amineruthenium and amineiridium hydride derivatives have been synthesized and characterized with the objective of observing intramolecular [Formula: see text] or [Formula: see text] interactions. These include RuHCl(CO)(L)(PPri3)2 (1a, L = NH2NH2; 1b, L = NH3) and IrCl2(L)(H)(PCy3)2 (2a, L = SC(NH2)2; 2b, L = NH3; 2c, L = NH2NH2; 2d, L = NH2(CH2)3NH2; 2e, L = NH2OH). Instead, weak [Formula: see text] van der Waals contacts have been detected in the solid state by X-ray analysis and in solution by NMR T1 measurements and nOe techniques. Both X-ray crystal structure analysis and minimum T1 measurements indicate that the [Formula: see text] distances in the [Formula: see text] interactions are ca•2.0–2.2 Å. The weak interactions might influence the course of deuteration of these complexes under D2 gas. The crystal and molecular structure of IrCl2(NH3)(H)(PCy3)22a has been determined by X-ray diffraction at 173 K: monoclinic, space group P21/n, a = 14.859(2) Å, b = 18.579(3) Å, c = 18.548(3) Å, β = 97.29(1)°, V = 5079.1(13) Å3, Z = 4, full-matrix least-squares refinement on F2 for 10 953 independent reflections; R[F2 > 4σ(F2)] = 0.0283, wR(F2) = 0.0704. Keywords: ruthenium, iridium, hydride, dihydrogen, complexes, hydrogen bond, NMR, X-ray.

The crystal and molecular structure of tris-butyl-tin(IV)-(1-pyrrolidinecarbodithioato)-3-propionate

1989 ◽  
Vol 54 (3) ◽  
pp. 684-690 ◽  
Author(s):  
Jan Lokaj ◽  
Viktor Vrábel ◽  
Eleonóra Kellö ◽  
Vladimír Ratay
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structure of Bu3Sn(pyrn-dtc-prop) was solved by the X-ray structural analysis method and refined by the block diagonal least squares method to R = 0.053 for 1 930 observed reflections. The compound crystallizes in the monoclinic system with a space group of P21/c, Z = 4, F(000) = 1 056, with unit cell dimensions of a = 1.4758(5), b = 0.9970(3), c = 1.9166(6) nm; β = 113.90(2)°. The measured and calculated crystal densities were Dm = 1.32 and Dc = 1.31.103 kg m-3. The tin atom is coordinated by three carbon atoms at distances of Sn-C 0.2117(8), 0.2133(8), 0.2158(11) nm and two oxygen atoms O(1) and O(2) at distances of Sn-O 0.2210(5) and 0.2399(5) nm. The coordination polyhedron is a deformed trigonal bipyramid. The S2CN ligand is approximately planar.

A Strong Deviation from Vegard’s Rule: X-Ray Powder Investigations of the Three Quasi-Binary Phase Systems BiOX–BiOY (X, Y = Cl, Br, I)

2005 ◽  
Vol 60 (12) ◽  
pp. 1255-1263 ◽  
Author(s):  
Egbert Keller ◽  
Volker Krämer
Keyword(s):  
Crystal Structure ◽  
Crystal Structure Analysis ◽  
X Ray ◽  
Binary Phase ◽  
Concentration Parameter ◽  
System A ◽  
Strong Deviation ◽  
Phase Systems ◽  
Rich Side ◽  
Single Crystal Structure Analysis

The three quasi-binary phase systems BiOX-BiOY (X, Y = Cl, Br, I) have been investigated by X-ray powder methods. No quaternary phases were found in the three systems. BiOCl-BiOBr and BiOBr-BiOI form systems of unlimited mutual solubility. BiOCl-BiOI is a system of limited solubility at the iodine-rich side. In the BiOBr-BiOI system a strong deviation from Vegard’s rule is observed with respect to one of the lattice parameters. A few methods to quantify such a deviation are briefly discussed and a possible explanation for the strong deviation in the BiOBr-BiOI system is proposed. Error calculations have been performed to estimate uncertainties in the concentration parameter x of the investigated mixtures. The crystal structure of BiOI has been re-determined by single crystal structure analysis.

Dodecamethyl Bisimidotriphosphoramide (TRIPA), Part III [1, 2] The Crystal and Molecular Structure of TRIPA · H2O

1980 ◽  
Vol 35 (10) ◽  
pp. 1203-1206 ◽  
Author(s):  
Johannes C. P. M. Lapidaire ◽  
Anthoni J. De Kok
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Van Der Waals ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray

Abstract The crystal and molecular structure of dodecamethyl bisimidotriphosphoramide mono-hydrate (TRIPA • H2O, C12H38N7O4P3) has been determined by single crystal X-ray diffraction techniques. The compound crystallises in the monoclinic system, space group P2i/n with a = 9.236(3), b = 14.016(4), c = 17.534(5) A, β = 97.32(4)°, Z = 4. The building units are dimers of TRIPA • H2O. These units are separated by normal van der Waals distances. The two molecules in the dimer are connected by four hydrogen bridges involving two water molecules. The nitrogen atoms display a nearly planar hybridisation.

The crystal and molecular structure of aqua-bis(ethylenediamine)cupric-tris(cyano)-selenocyanatodicuprate

1982 ◽  
Vol 47 (10) ◽  
pp. 2623-2632 ◽  
Author(s):  
Viktor Vrábel ◽  
Jan Lokaj ◽  
Ján Garaj ◽  
František Pavelčík
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Triclinic System

The crystal structure of [Cu(H2O)(en)2][Cu2(CN)3(SeCN)] was solved by single crystal X-ray structural analysis in the triclinic system with a space group of P1 and in the monoclinic system with a space group of C2. In the triclinic system the unit cell has dimensions of a = 0.8445(3), b = 0.7903(3), c = 0.8444(3) nm, α = 119.58(2), β = 118.59(2) and γ = 93.63(3)° and, in the monoclinic system, a = 1.3331(4), b = 0.8670(2), c = 0.8267(3), β = 122.60(2)°. The structure was refined by the least squares method to final value of R = 5.5% in the triclinic system and R = 7.8% in the monoclinic system. The coordination sphere around the Cu(II) atom is square pyramidal, formed of two ethylenediamine molecules and one water molecule. The Cu(I) atoms are tetrahedrally coordinated by bridging SeCN and CN ligands to form infinite three-dimensional chains. The SeCN group is bonded to the Cu(I) atoms through the Se atom at distances of 0.2731(3) and 0.2745(3) nm.

The crystal structure of C.I. Pigment Red 2, 1′-(2,5-dichlorophenyl)azo-2′hydroxy-3′-phenylamidonaphthalene

1977 ◽  
Vol 146 (4-6) ◽  
Author(s):  
A. Whitaker
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Parameters ◽  
Intramolecular Hydrogen

AbstractThe crystal and molecular structure of C.I. Pigment Red 2, l′-(2,5-dichlorophenyl)azo-2′-hydroxy-3′-phenylamidonaphthalene has been determined by x-ray diffraction techniques. It crystallizes in the monoclinic system with cell parametersThe hydrogen atoms have been found and included but not refined. The final residual is 15.3%. The molecule is probably in the form of the hydrazone tautomer. The intramolecular hydrogen bonds keep most of the molecule approximately planar while it appears that the remainder is held in the same plane due to steric hinderence between the molecules. The molecules are packed in columns with alternate molecules antiparallel and are linked by van der Waals forces.

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