Studies of β-Diketone Complexes of Rhenium. VI. The Crystal and Molecular Structure of cis-Dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III)

1974 ◽  
Vol 52 (9) ◽  
pp. 1704-1708 ◽  
Author(s):  
I. D. Brown ◽  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Nearest Neighbours

A compound, obtained in large yields from the reaction of acetylacetone and oxodichloroethoxobis(triphenylphosphine)rhenium(V) in benzene, has been shown by single crystal X-ray diffraction to be cis-dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III). The crystals are monoclinic with a = 13.06(1), b = 18.30(1), c = 16.55(1) Å, and β = 112.7(2)°. The space group is P21/c and there are four molecules per unit cell. A total of 3841 independent reflections, of which 2686 were observed, were examined by film methods, the intensities being measured with a microdensitometer. The structure was refined by full matrix least-squares analysis to an R2 value of 0.068. The ligands are arranged around the rhenium atom in the manner described by the compound name to give a rough octahedron of nearest neighbours and the Re—Cl (2.369 Å av.), Re—O (2.02 Å av.), and Re—P (2.474 Å av.) distances are as expected.

Studies of Rhenium β-Diketone Complexes. III. The Crystal and Molecular Structure of Bis(μ-O-1,3-diphenylpropane-1,3-dionatotricarbonylrhenium(I))

1973 ◽  
Vol 51 (2) ◽  
pp. 317-323 ◽  
Author(s):  
J. C. Barrick ◽  
M. Fredette ◽  
C. J. L. Lock
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Main Part ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
The Other ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray

One of a series of compounds obtained by the reaction of chloropentacarbonylrhenium(I) with β-diketones has been shown by single crystal X-ray diffraction to be bis(μ-O-1,3-diphenylpropane-1,3-dionatotricarbonylrhenium(I)). The crystals are monoclinic with lattice parameters a = 11.988(A) Å, b = 14.441(9) Å, c = 10.298(7) Å, β = 115.25(7)°. The space group is P21/c and there are two dimers per unit cell. A total of 1563 independent reflections were measured on a single crystal X-ray diffractometer and the structure was refined by least squares analysis to a weighted R2 value of 0.0427. The dimer units are held together by two bridging oxygen atoms, one from each of the β-ketoenolate groups; the distance of the bridging oxygen from the rhenium atom to which it is chelated (2.162(9) Å) is shorter than the distance to the other rhenium atom (2.204(7) Å). The main part of the β-ketoenolate ring is 37° from the OReO plane.

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.

Heavy transition metal complexes of biologically important molecules. I. The crystal and molecular structure of trans-dichloro(bis(isopropyl)-sulfoxide-S)(1-methylcytosine-N)platinum(II)

1976 ◽  
Vol 54 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Robert Anthony Speranzini ◽  
John Powell
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Least Squares ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal and molecular structure of trans-dichloro(bis(isopropyl)sulfoxide-S)(1-methylcytosine-N)platinum(II) has been determined by single crystal X-ray diffraction. The crystals are triclinic with a = 16.205(5), b = 8.078(2), c = 6.776(2) Å, α = 106.53(2), β = 96.35(2), γ = 98.54(2)°. The space group is [Formula: see text] and there are two molecules per unit cell. A total of 2294 independent reflections, of which 2023 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares analysis to an R2 value of 0.0427. The ligands form a rough square around the platinum atom with Pt—Cl(1), 2.304(3), Pt—Cl(2), 2.287(4), Pt—S, 2.232(2), Pt—N, 2.058(7). Distances within the ligands are normal. The plane of the cytosine ring is at 84.4° to the plane formed by the ligands around platinum.

Studies of β-Diketone Complexes of Rhenium. VII. The Crystal and Molecular Structure of Oxodichloropentane-2,4-dionatotriphenylphosphinerhenium(V)

1975 ◽  
Vol 53 (11) ◽  
pp. 1548-1553 ◽  
Author(s):  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Bonding Interaction ◽  
Ray Methods

The crystal structure of oxodichloropentane-2,4-dionatotriphenylphosphinerhenium(V) has been studied by single crystal X-ray methods. The crystals are triclinic with lattice parameters a = 11.023(8) Å, b = 13.523(8) Å, c = 9.360(7) Å, α = 90.2(1)°, β = 114.1(1)°, γ = 67.7(2)°. The space group is [Formula: see text] and there are two formula weights per unit cell. A total of 2891 reflections, of which 2447 were observed, were examined, and the structure was refined by full matrix least squares to an R2 value of 0.0782. The ligands are arranged around the rhenium atom such that the nearest six atoms are at the corners of a very distorted octahedron. Most of this distortion appears to be caused by nonbonding repulsive interactions. The short oxo–phosphine distance, 2.85(1) Å, suggests the possibility of a weak bonding interaction. Observed bond distances (Re—Cl, 2.35 Å av; Re—O(oxo), 1.69(1) Å; Re—O(diketone), 1.99(1), 2.10(1) Å; Re—P, 2.431(4) Å) are close to those observed previously in similar compounds.

The Crystal and Molecular Structure of Chloro-mer-Tris(dimethylphenylphosphine)-cis-dihydridoiridium(III) by X-Ray and Neutron Diffraction

1988 ◽  
Vol 41 (5) ◽  
pp. 641 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Molecular Structure ◽  
Neutron Diffraction ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Neutron Data ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The structure of mer-(Pme2Ph)3Cl-cis-H2IrIII (1) has been determined by single-crystal X-ray and neutron diffraction analyses. Crystals are monoclinic, space group P21, with a 11.476(4), b 14.069(5), c 8.286(3)Ǻ, β 92.45(1)° and Z 2. Full-matrix least-squares analyses converged 0.022 for 7773 X-ray data and R(F2) = 0.062 for 1538 neutron data. Ir -H [1.557(11)Ǻ trans to Cl, 1.603(10) Ǻ trans to P] and Ir -P distances [2.292(1)Ǻ trans to P, 2.328(1)Ǻ trans to H] both exhibit trans lengthening effects. Consistent with the increased hydride content the Ir -P distances in (1) are c. 0.04 Ǻ shorter than for the corresponding bonds in its dichloro monohydrido analogues and c. 0.08 Ǻ shorter than those in the trichloride . In contrast Ir-Cl [2.505(1)Ǻ] is not significantly different to the corresponding distance (2.504 Ǻ av.) in mer -(PMe2Ph)3-cis-Cl2HIrIII.

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.

Crystal and Molecular Structure of mer-cis-(PEt2Ph)2(PPri3)H-trans-Cl2IrIII

1996 ◽  
Vol 49 (11) ◽  
pp. 1253 ◽  
Author(s):  
EJ Ditzel ◽  
KD Griffiths ◽  
GB Robertson
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Crystal And Molecular Structure ◽  
Structure Refinement ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Metal Ligand

The structure of mer-cis-(PEt2Ph)2(PPri3)H-trans-Cl2IrIII (4) has been determined by single-crystal X-ray diffraction analysis. Crystals are monoclinic, space group P21/c, with a 11.607(1), b 21.553(1), c 14.066(1) Ǻ, β 109.04(1)? and Z 4. Structure refinement by full-matrix least-squares analysis (3244 unique reflections, 316 parameters) converged with R 0.034 and Rw 0.041. The PEt2Ph ligands are similarly disposed to their PMe2Ph counterparts in mer-cis-(PEt2Ph)2(PPri3)H-trans-Cl2IrIII (2) but the PPri3 ligands are differently oriented and differently configured. Metal-ligand distances [ Ir -P(1,2,3) 2.333(2), 2.404(2), 2.368(2) Ǻ; Ir-Cl (1,2) 2.388(2), 2.400(2) Ǻ] are all within c. 0.02 Ǻ of those in (2). The P-Ir -P(trans) angle is 155.3(1)°.

Studies of the rhenium–oxygen bond. II. The crystal and molecular structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2ORe(C5H5N)2Cl2O

1978 ◽  
Vol 56 (2) ◽  
pp. 179-188 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Full Matrix ◽  
X Ray ◽  
Ray Methods ◽  
Oxygen Bond

The crystal structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2•O•Re(C5H5N)2Cl2O bas been studied by single crystal X-ray methods. The crystals were orthorhombic with lattice parameters a = 15.367(2), b = 10.283(2), c = 16.685(2) Å. The space group was Pna21 and there were four formula weights per unit cell. A total of 3339 reflections, of which 2990 were observed, were examined, and the structure refined by full matrix least squares (treating the pyridine rings as groups) to an R2 value of 0.0449. The dimer had a roughly rectilinear O—Re—O—Re—O backbone with pairs of chlorine atoms and pyridine molecules arranged cis in each half of the dimer. The two halves of the dimer were arranged such that the pairs of cis atoms in one half were rotated about the Re(1)–Re(2) axis almost 113 ° when compared to the corresponding pair in the other half. Important bond lengths (Re—O(terminal), 1.715(16), 1.764(16); Re—O(bridging), 1.943(16), 1.903(16); Re—Cl, 2.356(5)–2.390(5); Re—N, 2.116(16)–2.180(16)) were close to previously observed values. The molecule was markedly disturbed from the idealized structure and this was caused by intramolecular non-bonded interactions.

The crystal and molecular structure of (±)-('E')-N-Acetylpiperidine-2-carboxylic acid

1980 ◽  
Vol 33 (1) ◽  
pp. 215 ◽  
Author(s):  
ID Rae ◽  
CL Raston ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Carboxylic Acid ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of N-acetylpiperidine-2-carboxylic acid has been determined by single-crystal X-ray diffraction methods at 295(1) K and refined by least squares to a residual of 0.039 for 846 'observed' reflections. Crystals are orthorhombic, with space group Pbca, a 13.684(6), b 11.602(4), c 11.171(4)Ǻ, Z 8. The ring is a chair structure in which, contrary to an earlier proposal based on 1H n.m.r. studies, there is almost perfect staggering about the C(2)-C(3) bond.

The crystal and molecular structure of dipyrrolidylthiuram disulfide

1983 ◽  
Vol 36 (7) ◽  
pp. 1371 ◽  
Author(s):  
GA Williams ◽  
JR Statham ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Dihedral Angle ◽  
Crystal And Molecular Structure ◽  
Structural Parameters ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray

The crystal structure of dipyrrolidylthiuram disulfide has been determined by single-crystal X-ray diffraction techniques at 295 K. Crystals are monoclinic, space group C2/c, unit cell a 13.835(3), b 10.422(2), c 9.427(3) �, β 97.08(2)� and Z 4. Automatic diffractometry has provided significant Bragg intensities for 1402 independent reflections, and the structure has been refined by least-squares methods to R 0.037. The structure consists of discrete C4H8NC(S)S2C(S)NC4H8 molecules. Half of each molecule is crystallographically unique with distances S-S 2.002(1), and C-S 1.804(2) and 1.645(2) �. The dihedral angle between planar C2NC(S)S portions is 87.9�. The relevance of the derived structural parameters to the question of why the tris(pyrrolidine-1-carbodithioato)iron(III) complex is, uniquely, high spin is discussed.

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