An X-Ray Crystallographic Study of Cd[P(C-C6H11)3]2(NO3)2.CH2Cl2

1986 ◽  
Vol 39 (4) ◽  
pp. 713 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls ◽  
ERT Tiekink
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Cadmium Atom ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Full Matrix ◽  
X Ray ◽  
Crystallographic Study ◽  
Tetrahedral Environment

The crystal and molecular structure of bis ( tricyclohexylphosphine )cadmium(II) nitrate as its dichloromethane solvate, Cd [P(c-C6H11)3]2(NO3)2.CH2Cl2, has been determined by single- crystal, three-dimensional X-ray diffraction methods. The crystals of the cadmium(II) complex are monoclinic with space group C2/c, a 20.880(6), b 12.775(3), c 17.075(5) Ǻ and β 106.38(2)°, Z 4. The structure was solved by normal Fourier methods and refined by a full-matrix least-squares procedure. The refinement used the 2169 statistically independent reflections for which I ≥ 2σ(I) converged with R and Rw of 0.065 and 0.067 respectively. The crystals consist of discrete Cd [P(c-C6H11)3]2(NO3)2 molecules and CH2Cl2 in the ratio 1 : 1. There is a distorted tetrahedral environment around the cadmium atom formed from the coordination of the two phosphines and two nitrates with each nitrate essentially occupying one stereochemical position. The two markedly different Cd -O bond lengths of 2.405(9) and 2.575(8) Ǻ show gross asymmetry in the coordination of the nitrate.

Crystal and molecular structure of Octacarbonylbis(diphenylarsino)-methanedimanganese(0)

1983 ◽  
Vol 36 (4) ◽  
pp. 683 ◽  
Author(s):  
BF Hoskins ◽  
RJ Steen
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Parent Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Fourier Methods ◽  
X Ray

The crystal structure of the complex Mn2(CO)8(dam) (dam = Ph2AsCH2AsPh2) has been determined by three-dimensional X-ray diffraction methods. The crystals are triclinic, space group P1, with a 11.191(1), b 16.498(5), c 9.455(1) �, a 93.64(2), β 109.08(2), γ 89.36(2)� and contain two discrete, binuclear molecules of Mn2(CO)8(dam) per unit cell. The structure, solved by direct and Fourier methods, was refined by a least-squares procedure to R and Rw of 0.065 and 0.082 respectively for 1907 independent, statistically significant reflections collected by counter methods. The feature of particular interest in this compound is the accommodation of the bridging bidentate dam ligand [As.. .As separation 3.242(2) �] across a shorter Mn�-Mn� bond [2.962(3) �] which constrains the molecule so that a much less staggered configuration of the two manganese coordination octahedra is observed relative to the parent compound Mn2(CO)10, the rotation of the two equatorial planes in the former being 30�.

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.

Crystal and Molecular Structure of 3-Iodo-2-propynyl-N-butylcarbamate

1997 ◽  
Vol 52 (2) ◽  
pp. 256-258 ◽  
Author(s):  
Evgeni V. Avtomonov ◽  
Rainer Grüning ◽  
Jörg Lorberth
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Carbamate Group ◽  
Oxygen Atoms

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.

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.

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 ovalene: some three-dimensional refinements

1973 ◽  
Vol 137 (2-3) ◽  
Author(s):  
R. G. Hazell ◽  
G. S. Pawley
Keyword(s):  
Molecular Structure ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray

AbstractThree-dimensional x-ray diffraction data have been taken from ovalene, C

An Intermediate in the Conversion of an Acetylene to a Vinyl Derivative: The Crystal and Molecular Structure of trans-Chloromethylbis(trimethylarsine)-platinum(II) Hexafluorobut-2-yne

1972 ◽  
Vol 50 (14) ◽  
pp. 2276-2284 ◽  
Author(s):  
Brian W. Davies ◽  
Richard J. Puddephatt ◽  
Nicholas C. Payne
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Free Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Monodentate Ligand ◽  
X Ray ◽  
Trigonal Bipyramidal

The crystal and molecular structure of trans-chloromethylbis(trimethylarsine)platinum(II) hexafluorobut-2-yne has been determined from three dimensional X-ray diffraction data recorded by diffractometric methods. The structure has been refined by full-matrix least-squares methods on F using 1156 reflections to an agreement factor R = 0.077. The crystals are monoclinic, space group [Formula: see text] with a = 6.803(8), b = 14.93(2), c = 20.20(2) Å, β = 104.9(1)°, and Z = 4. The coordination of the platinum atom is trigonal bipyramidal, with the acetylene considered a monodentate ligand, and the two trimethylarsine ligands occupying the equatorial plane. The chlorine atom and the methyl ligand occupy the apical positions, with Pt—Cl and Pt—C distances of 2.47(1) Å and 2.10(4) Å, respectively. The long Pt—Cl bond length indicates the strong trans-influence of the methyl ligand. The observed C—C bond length of 1.32(4) Å in the acetylene ligand is lengthened from the value of 1.22(9) Å measured in the free ligand. The geometry of the coordinated ligand is discussed in terms of the bonding scheme proposed by Greaves etal.

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 a platinum-silatrane complex

1977 ◽  
Vol 30 (5) ◽  
pp. 1007 ◽  
Author(s):  
GR Scollary
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

A structural analysis of the platinum-silatrane complex, PtCl [Si(OCH2CH2)3N] [PMe2Ph]2, has been carried out by X-ray diffraction. Crystals are monoclinic, space group P21/c, a 6.630(4), b 17.465(6), c 22.297(6) Ǻ, β 97.4(2)�, Z 4. The structure has been refined by a full- matrix least-squares procedure to R 0.048 for 2165 reflections. Basic geometries are square (platinum), tetrahedral (silicon) and trigonal (nitrogen). Within the silatrane ligand, the Si-N non-bonding distance is 2.89(1) Ǻ.

The preparation of thiolato bridged platinum dimers; the crystal and molecular structure of cis-μμ′-bis(phenylmethanethiolato)bis(phenylmethanethiolatomethyldiphenylphos- phineplatinum(II)), cis-[(PMePh2)Pt(SCH2Ph)(μ-SCH2Ph)]2

1982 ◽  
Vol 60 (16) ◽  
pp. 2075-2081 ◽  
Author(s):  
Peter H. Bird ◽  
Upali Siriwardane ◽  
Rabin D. Lai ◽  
Alan Shaver
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Dihedral Angle ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
A Cell ◽  
Facile Route

Fusion invacuo of complexes of the type P2Pt(SR)2 is a facile route to dimers of the type [PPt(SR)(μ-SR)]2; thus, the compounds cis-P2Pt(SR)2, where P = PPh3, PMePh2, R = CH2Ph and trans-P2Pt(SR)2, where P = PPh3, PMePh2, PMe2Ph, R = 4-C6H4CH3 gave the appropriate dimers 1–5. A three-dimensional X-ray structure analysis of the complex [(PMePh2)Pt(SCH2Ph)(μ-SCH2Ph)]2, 2, has shown that it has cis geometry with the benzyl groups of the bridging thiolato ligands oriented anti with respect to each other. The dihedral angle between the two square planes is 138.8°. Crystals of 2 are triclinic, space group [Formula: see text], with two molecules in a cell of dimensions a = 10.856(3) Å, b = 19.935(5) Å, c = 12.202(4) Å, α = 82.52(2)°, β = 105.18(2)°, and γ = 92.35(2)°. Full-matrix least-squares refinement converged at R = 0.052.

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