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 (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.

Crystal and molecular structure of 3-ethyl-4-hydroxy-1,2,3(4H)-benzotriazine and 6-chloro-4-hydroxy-3-methyl-4-phenyl-1,2,3-benzotriazine

1985 ◽  
Vol 63 (3) ◽  
pp. 581-585 ◽  
Author(s):  
Kwong Khee Lai ◽  
Carl H. Schwalbe ◽  
Keith Vaughan ◽  
Ronald J. Lafrance ◽  
Clive D. Whiston
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Tetrahedral Geometry ◽  
Orthorhombic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor

The crystal structures of the title compounds have been determined from X-ray data collected on a four-circle diffractometer and refined by the full-matrix least-squares method. The former compound crystallizes in the orthorhombic system, space group Pbcn, with a = 14.346(8), b = 7.239(1), c = 17.276(2) Å, and has been refined to a conventional R factor of 0.043 for 890 observed reflections. Corresponding results for the latter compound are monoclinic, P21/n, a = 12.222(4), b = 7.482(2), c = 14.170(8) Å, β = 94.06(4)°, R = 0.060 for 2128 observed data. The triazine rings of both compounds exhibit short N(1)—N(2) bonds and tetrahedral geometry at C(4); however, the ring is puckered in the first compound but flat in the second. Molecules in both crystals are linked by [Formula: see text] hydrogen bonds.

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.

Crystal and molecular structure of 4α-t-Butylcyclohexane-1β,2β-diol

1972 ◽  
Vol 25 (10) ◽  
pp. 2117 ◽  
Author(s):  
MD Brice ◽  
BR Penfold ◽  
WT Robinson
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Chair Conformation ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Least Squares Techniques

The crystal and molecular structure of 4α-t-butylcyclohexane-1β,2,β-diol, C10H20O2, has been determined by X-ray diffraction methods. The compound crystallizes in the triclinic space group Pi with 4 molecules in a unit cell of dimensions a = 12.268, b = 15.921, c = 6.322�, α = 82.53, β = 114.45, γ = 111.13�. The intensity data were measured by counter methods using Cu Kα radiation; the structure was solved by means of the tangent formula, and was refined using full matrix least-squares techniques to a final R-factor of 0.063 for 1199 reflections. The crystal structure consists of two sets of crystallographically non-equivalent molecules hydrogen-bonded to form discrete chains parallel to the c axis. The cyclohexane rings are in the chair conformation.

The crystal and molecular structure of zinc(II) monoglycerolate

1983 ◽  
Vol 36 (6) ◽  
pp. 1249 ◽  
Author(s):  
TW Hambley ◽  
MR Snow
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystallographic Analysis ◽  
Monoclinic Space Group ◽  
Solid Complex ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Hydrophobic Nature ◽  
Least Squares Techniques

An X-ray crystallographic analysis of zinc(II) monoglycerolate has been carried out. The crystals are monoclinic, space group P21/c with a 8.110(1), b 6.404(1), c 8.714(2)� β 93.44(1)�. The structure was refined by full-matrix least-squares techniques to an R factor (on 519F) of 0.019. The analysis reveals that the zinc atoms bridge the glycerolate molecules forming polymeric sheets lying parallel to the bc plane. Only aliphatic hydrogens are disposed into the space between the layers, a fact consistent with the lubricity and hydrophobic nature of the solid complex and the observed facile lamellar cleavage perpendicular to the a axis.

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.

Studies of the rhenium-oxygen bond. III. The crystal and molecular structure of 1-oxo-6-ethoxo-2,4-dichloro-3,5-dipyridinerhenium(V)

1977 ◽  
Vol 55 (2) ◽  
pp. 333-339 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Dominant Factor ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Bond

The crystal and molecular structure of the title compound has been examined by single crystal X-ray diffraction. The crystals are monoclinic with a = 28.045(10), b = 8.766(3), c = 12.376(5) Å, β = 91.14(3)°. The space group is C2/c and there are eight molecules per unit cell. A total of 5053 independent reflections, of which 2860 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares to an R2 value of 0.0449. The ligands form a very rough octahedron around the rhenium atom with Re—Cl(1), 2.441(3); Re—Cl(2), 2.366(3), Re—O(1), 1.684(7); Re—O(2), 1.896(6); Re—N(1), 2.144(7); Re—N(2), 2.132(7) Å. The pyridine rings are a dominant factor in determining the details of the molecular structure.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

The Crystal and Molecular Structure of Dinitrato(triphenylphosphine)mercury(II)

1974 ◽  
Vol 52 (2) ◽  
pp. 198-202 ◽  
Author(s):  
Simon H. Whitlow
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Bond Distance ◽  
The Other ◽  
Tetrahedral Coordination ◽  
X Ray ◽  
R Factor ◽  
Computer Controlled ◽  
Distorted Tetrahedral Coordination

The structure of dinitrato(triphenylphosphine)mercury(II), Hg(N03)2.P(C6H5)3, has been determined from single–crystal X-ray data measured on a computer–controlled diffractometer. The crystals are monoclinic, have a unit cell of dimensions a = 10.39(1), b = 9.56(1), c = 19.44(2) Å, β = 94.3(1)°, which contains 4 molecules, and they belong to the space group, P21/c. The structure has been refined by least–squares methods from 2470 independent observed reflections to a conventional R-factor of 0.061. The Hg atom has a distorted tetrahedral coordination with Hg—O bond lengths of 2.190(8), 2.428(8), and 2.560(9) Å and an Hg—P bond distance of 2.359(3) Å. There are 2 distinct types of NO3 groups bonded to Hg. One is an unshared, unidentate ligand and the other acts as a bridging group joining 2 Hg atoms. Chains of—Hg—NO3—Hg—atoms are formed which follow crystallographic two-fold screw axes in the b-direction.

Nitrones and oximes of bifunctional carbonyl compounds and their reaction products with diarylborinic acids. Crystal and molecular structure of examples of five-, six-, and seven-membered boron chelates

2000 ◽  
Vol 78 (10) ◽  
pp. 1325-1344
Author(s):  
Wolfgang Kliegel ◽  
Gottfried Lubkowitz ◽  
Jens O Pokriefke ◽  
Steven J Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Carbonyl Compounds ◽  
Spectroscopic Data ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Reaction Products ◽  
Boron Chelates ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

Synthesis has been carried out of diarylboron chelates of 2- and 3-hydroxynitrones, of 2- and 3-hydroxyoximes, and of 2-carboxynitrones and a 2-carboxyoxime. The structures have been determined from spectroscopic data and from X-ray analyses of 5d, 9a, 11b, and 19. Crystals (at 180 K) of 5d are monoclinic, a = 10.543(2), b = 19.085(4), c = 10.2667(3) Å, β = 90.4978(7)°, Z = 4, space group P21/c; those of 9a are orthorhombic, a = 10.9913(5), b = 14.9329(7), c = 10.2460(13) Å, Z = 4, space group P212121; those of 11b are monoclinic, a = 11.227(2), b = 9.967(2), c = 17.0537(4) Å, β = 105.4179(5)°, Z = 4, space group P21/n; those of 19 are monoclinic, a = 11.1847(15), b = 13.715(3), c = 11.5559(5) Å, β = 104.8730(10)°, Z = 4, space group P21/n. The structures were solved by direct methods and refined by full-matrix least-squares procedures to R(F, I [Formula: see text] 3σ(I)) = 0.049, 0.047, 0.042, and 0.047, respectively, for CCD data for 5d, 9a, 11b, and 19. The four molecules contain five-, seven-, six-, and five-membered rings, respectively, with O-B-N groups in the 5d, 11b, and 19, and O-B-O in 9a; the rings exhibit various deviations from planarity, particularly the seven-membered ring.Key words: diarylboron chelates, hydroxyoximes, hydroxynitrones, carboxyoximes, carboxynitrones, organoboron compounds, crystal structure.

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