The Preparation, Physical Properties, and Structure of Oxotetrachloroaquorhenium(VI), ReOCl4(OH2)

1972 ◽  
Vol 50 (12) ◽  
pp. 1811-1818 ◽  
Author(s):  
P. W. Frais ◽  
C. J. L. Lock
Keyword(s):  
Molecular Structure ◽  
Infrared Spectroscopy ◽  
Physical Properties ◽  
Single Crystal ◽  
Least Squares ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
First Time

Oxotetrachloroaquorhenium(VI), ReOCl4•H2O, has been prepared and characterized for the first time by analysis, infrared spectroscopy and single crystal X-ray diffraction. The crystals were orthorhombic, a = 10.834(8), b = 11.089(8), c = 5.517(4) Å, Pn21a, Z = 4. Intensity data were recorded by integrating film methods and measured with a Joyce–Loebl microdensitometer, and 624 observable of the 704 measured independent reflections were given non-zero weight in the final cycle of full matrix least-squares refinement where R1 = 0.0572 and R2 = 0.0687. The molecular structure is based on a very distorted octahedron with a strongly bonded oxo-group (Re—O, 1.63(2) Å) trans (177(2)°) to a weakly bonded aquo-group (Re—O, 2.27 (2) Å). The Re—Cl distances do not differ significantly (2.29(1) Å av). The chlorine atoms are bent away from the oxo-group (angles vary from (94–102°(1)).

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.

The Structure and Physical Properties of μ-oxo-bis{oxotrichloro(O-perrhenylchloride)rhenium(VI)}, and the Non-existence of β-ReOCl3

1972 ◽  
Vol 50 (22) ◽  
pp. 3607-3618 ◽  
Author(s):  
C. Calvo ◽  
P. W. Frais ◽  
C. J. L. Lock
Keyword(s):  
Oxygen Atom ◽  
Infrared Spectrum ◽  
Physical Properties ◽  
Single Crystal ◽  
Least Squares ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Weak Bond ◽  
X Ray ◽  
Chloride Molecule

The compound previously reported as β-ReOCl3 has been shown by analysis and single crystal X-ray diffraction to be μ-oxo-bis{oxotrichloro(O-perrhenyl chloride)rhenium(VI)}, (Re2O3Cl6)(ReO3Cl)2. The crystals were triclinic, a = 6.112(5), b = 12.876(9), c = 6.020(5) Å, α = 88.30(5), β = 95.88(5), γ = 105.36(5)°, [Formula: see text]. Intensities were measured by a densitometer from photographs recorded on an integrating precession camera. The structure was refined by full matrix least squares to give a final R2 of 0.072. The molecule is composed of a dimeric Re2O3Cl6 unit with a bridging oxygen atom on the center of symmetry and an Re—O (bridge) distance of 1.847(1) Å. The remaining oxo-group on each rhenium is cis to the bridge and is strongly bonded (1.69(2) Å), and the position trans to the terminal oxo-group is filled by a weak bond to an oxygen atom of a perrhenyl chloride molecule. The infrared spectrum of the compound has been explained in terms of the 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 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.

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

Structural Systematics of Metal Acetylide Complexes. II. X-Ray Studies of Some Nickel σ-Acetylide Complexes

1998 ◽  
Vol 51 (3) ◽  
pp. 219 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Trans Influence

The structures of Ni(C≡CR)(PPh3)(η-C5H5) (R = Ph (1), C6H4-4-NO2 (2), 4-C6H4C6H4-4′-NO2 (3), (E)-4-C6H4CH=CHC6H4-4′-NO2 (4), 4-C6H4C≡CC6H4-4′-NO2 (5), 4-C6H4N=CHC6H4-4′-NO2 (6)) have been determined by single-crystal X-ray diffraction studies, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a 10·094(2), b13·429(3), c 18·835(5) Å,α 103·24(2), β 91·50(2), γ 90·10(2)°, Z 4, 5844 unique reflections (595 parameters), converging at R 0·033 and Rw 0·024. For (2), crystals are orthorhombic, space group Pna21, with a 16·799(2), b 8·681(2), c 17·485(2) Å, Z 4, 1774 unique reflections (325 parameters), converging at R 0·031 and Rw 0·029. For (3), crystals are monoclinic, space group P 21/c, with a 11·140(3), b 18·282(4), c 15·296(2) Å, β 105·18(2)°, Z 4, 3132 unique reflections (397 parameters), converging at R 0·039 and Rw 0·024. For (4), crystals are monoclinic, space group P 21/n, with a 12·929(7), b 16·953(8), c 15·601(7) Å, β 112·55(3), Z 4, 3023 unique reflections (397 parameters), converging at R 0·039 and Rw 0·025. For (5), crystals are monoclinic, space group P 21/n, with a 12·710(5), b 16·882(3), c 15·693(4) Å, β 111·37(3)°, Z 4, 3216 unique reflections (397 parameters), converging at R 0·035 and Rw 0·030. For (6), crystals are monoclinic, space group P 21/n, with a 12·594(1), b 16·936(2), c 15·611(1) Å, β 112·476(5)°, Z 4, 3564 unique reflections (397 parameters), converging at R 0·038 and Rw 0·041. For structurally characterized 18-electron (cyclopentadienyl)nickel(II) acetylide complexes, statistically insignificant decreases in the average Ni-C(1) distance and trans influence and an increase in the average C(1)-C(2) parameter are observed on introduction of an acceptor substituent at the alkynyl ligand.

Crystal structure of 8-Hydroxy-1H-naphtho[2,1,8-mna]xanthen-1-one

1984 ◽  
Vol 37 (8) ◽  
pp. 1763
Author(s):  
IR Castleden ◽  
LM Engelhardt ◽  
SR Hall ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Interplanar Spacing ◽  
Charge Transfer Complexes ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal structure of 8-hydroxy-1H-naphtho[2,1,8-mna]xanthen-1-one, C19H10O3, obtained as an indefinite methanolsolvate, has been determined at 295K by single-crystal X-ray diffraction methods, being refined by full matrix least squares to a residual of 0.056 for 892 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 5.128(4), b 10.024(9), c 27.45(2) �, β 107.73(6)�, Z 4. The packing of the molecules is typically that of charge-transfer complexes, with an interplanar spacing of c.3.5 �.

scholarly journals Crystal structure of Tetraaqua(ethylenediamine)nickel(II) sulfate dihydrate and of Tetraaqua(2,2'-bipyridyl)nickel(II) sulfate dihydrate

1984 ◽  
Vol 37 (5) ◽  
pp. 921 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Atoms

The crystal structures of the title compounds, [Ni(OH2)4(en)] [SO4].2H2O, (1), and [Ni(OH2)4(bpy)]- [SO4].2H2O, (2), have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by full matrix least-squares methods to residuals of 0.028,0.031 for 1852, 4323 independent 'observed' reflections respectively. Crystals of (1) are monoclinic, C2/c, a 9.459(4), b 12.192(7), c 12.294(3) �, β 119.84(4)�, Z 4. In the cation, Ni-N is 2.061(2) �; Ni-O (trans to O, N respectively) are 2.106(2), 2.063(2) �. Instead of being enlarged above 90� as predicted from repulsion theory, the angle between the pair of oxygen atoms trans to nitrogen is diminished, being 87 14(7)�. Crystals of (2) are triclinic, P1, a 11.476(5), b 9.351(5), c 7.793(4) �, α 77.63(4), β 83.52(3), γ87.40(4)�, Z 2. In the cation, Ni-N are both 2.063(2) �. Ni-O (trans to N, O respectively) are 2.060(2), 2.O42(2); 2.O80(2), 2�. The short Ni-O distance [2.042(2)�] is associated with the coordination of a trigonal water molecule.

Studies of β-Diketone Complexes of Rhenium(V). The Molecular and Crystal Structure of trans-Dichlorobis(pentane-2,4-dionato)rhenium(IV)

1973 ◽  
Vol 51 (13) ◽  
pp. 2073-2076 ◽  
Author(s):  
I. D. Brown ◽  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Molecular And Crystal Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
Dimeric Structure

One of the compounds obtained by reacting acetylacetone with oxoethoxodichlorobis(triphenylphosphine)rhenium(V) has been shown by single crystal X-ray diffraction to be trans-dichlorobis(pentane-2,4-dionato)rhenium(IV). The crystals are triclinic, a = 8.032(4), b = 8.344(6), c = 7.429(6) Å, α = 118.1(2), β = 92.3(2), γ = 55.5(2)°, [Formula: see text], Z = 1. Intensities were measured with a microdensitometer from photographs recorded on an integrating precession camera. Of the 991 measured reflections all were observed and 984 were used in the refinement. The structure was refined by full matrix least squares to an R2 value of 0.0685. The compound was found to be a trans-monomer, in contrast to the dimeric structure claimed to exist in solution. The ligand atoms bonded to rhenium lie almost exactly at the apices of an octahedron and the bond lengths (Re—Cl, 2.326(8); Re—O1, 1.97(1); Re—O2, 2.01(1) Å) are in the range expected.

Crystal structure of Tris(N,N-diethyldithiocarbamato)thallium(III)

1978 ◽  
Vol 31 (9) ◽  
pp. 1927 ◽  
Author(s):  
DL Kepert ◽  
CL Raston ◽  
NK Roberts ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Electron Pair ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The crystal structure of the title compound, [Tl(S2CNEt2)3], has been determined by single-crystal X-ray diffraction methods at 295 K and refined by full-matrix least squares to a residual of 0.050 for 2517 'observed' reflections. Crystals are monoclinic, with space group A2/a, a 14.789(7), b 10.428(4), c 18.207(9) Ǻ, β 118.11(4)°, Z 4, and are isostructural with those of the previously determined gallium and indium analogues, the molecule having 2 symmetry with <Tl-S> 2.666 Ǻ. As in the dimethyl/thallium analogue, the departure of the TlS6 core symmetry from 3 is large and is examined in terms of electron-pair repulsion theory.

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