Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XXX. Synthesis and X-Ray Structure of [Ru(dppm-P)(dppm-P,P')(η-C5H5)][PF6]0.5[PO2F2]0.5

1988 ◽  
Vol 41 (4) ◽  
pp. 597 ◽  
Author(s):  
MI Bruce ◽  
MP Cifuentes ◽  
KR Grundy ◽  
MJ Liddell ◽  
MR Snow ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Phenyl Group ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
One Pot ◽  
Full Matrix ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

An improved, one-pot synthesis is reported for the [Ru (dppm -P)(dppm -P, P′)(η-C5H5)]+ cation as its BF4- salt. The crystal structure of [Ru ( dppm - P)( dppm -P,P′)(η-C5H5)]+, obtained as the mixed PF6-/PO2F2- salt, has also been determined. There are few differences in dimensions between the mono- and bi-dentate dppm ligands; chelation sharply reduces the P-CH2-P angle, and one phenyl group on each phosphorus is bent away from the metal. Crystals are monoclinic, space group C2/c with unit cell dimensions a 21.743(3), b 23.594(3), c 21.352(3)Ǻ, β 110.17(1) and Z 8. The structure was refined by a full-matrix least-squares procedure to final R 0.078 and Rw 0.087 for 4490 reflections with I > 2.5σ(I).

The Crystal Structure of a Thiathiophthen Nitrogen Isostere, 3,5-Epidithio-2,5-diphenyl-2,4-pentadienylidene-3-aminoquinoline

1971 ◽  
Vol 49 (2) ◽  
pp. 167-172 ◽  
Author(s):  
F. Leung ◽  
S. C. Nyburg
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
Triclinic System ◽  
R Factor ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structure of a thiathiophthen nitrogen isostere (7) has been solved by X-ray analysis. The crystal belongs to the triclinic system with unit cell dimensions: a = 11.275(11), b = 9.558(10), c = 10.797(10) Å, α = 92.50(10), β = 116.98(10), γ = 92.61(10)°. There are two molecules per unit cell, space group [Formula: see text]. The data were collected by diffractometer with CuKα radiation. The structure was solved by symbolic addition procedures, and fully refined anisotropically using full-matrix least squares to an R factor of 6.3%.The S—S and S—N bond lengths were found to be 2.364 and 1.887 Å, respectively. This reveals the partial bonding character between S … S … N atoms.

Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink
Keyword(s):  
Least Squares ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).

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.

Refinement of the structure of Mg2As2O7

1970 ◽  
Vol 48 (6) ◽  
pp. 890-894 ◽  
Author(s):  
C. Calvo ◽  
K. Neelakantan
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
Space Group ◽  
Cell Dimensions ◽  
Central Oxygen ◽  
R Value ◽  
Unit Cell Dimensions

The crystal structure of Mg2As2O7 has been refined by full matrix least squares procedures using 587 observed reflections. The structure of Mg2As2O7 is of the thortveitite type, as reported by Łukaszewicz, with space group C2/m and unit cell dimensions a = 6.567(2) Å, b = 8.524(4) Å, c = 4.739(1) Å, β = 103.8(1)°, and Z = 2. The As—O—As group in the anion appears to be linear but the central oxygen atom undergoes considerable disorder in the plane perpendicular to this group. The AsO bond distances uncorrected for thermal motion are 1.67 Å for the As—O(—As) bond and 1.66 and 1.65 Å for the terminal As—O bonds. The final R value obtained is 0.088.

X-Ray structure of tris(acetonitrile)tricarbonylrhenium(I) tetrafluoroborate

1977 ◽  
Vol 55 (1) ◽  
pp. 111-114 ◽  
Author(s):  
Lillian Y. Y. Chan ◽  
E. E. Isaacs ◽  
W. A. G. Graham
Keyword(s):  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
The Mean ◽  
Unit Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data

Reaction of [n-Bu4N]2[Re4(CO)16] with AgBF4 in acetonitrile affords the compound [(CH3CN)3Re(CO)3][BF4]. The latter crystallizes in monoclinic space group P21/c with unit cell dimensions a = 11.021(5) Å, b = 11.136(5) Å, c = 12.980(6) Å, β = 96.906(25)°, and four molecules per unit cell. Data were collected by counter methods and the structure was refined using least-squares procedures to give R = 0.041. The rhenium cation is approximately octahedrally coordinated by six facially arranged ligands. The mean rhenium–nitrogen distance is 2.13 Å, and the mean rhenium–nitrogen–carbon angle in the coordinated acetonitrile is 174.7°.

Refinement of the Crystal Structure of Synthetic Chervetite, Pb2V2O7

1973 ◽  
Vol 51 (1) ◽  
pp. 70-76 ◽  
Author(s):  
Robert D. Shannon ◽  
Crispin Calvo
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Unit Cell ◽  
Type Structure ◽  
Covalent Bonds ◽  
Full Matrix ◽  
Space Group ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The structure of synthetic chervetite has been refined by full matrix least-squares to a ωR = 0.029 using 1105 reflections. Unit cell dimensions are a = 13.3689(7), b = 7.1607(4), c = 7.1027(4) Å, β = 105935(5)°, and the space group is P21/a. The structure, originally solved by Kawahara, is a dichromate-type structure with a V2O74− group eclipsed to within 11 ± 5°. The Pb2+ ions are irregularly coordinated to 8 or 9 oxygens with distances from 2.40 to 3.20 Å. The distortion of the Pb–O distances is considerably greater than the corresponding distortions of the Sr–O distances in the similar β-Sr2V2O7 structure and is related to the tendency of Pb2+ to form directional covalent bonds. The V–O distances range from 1,665 to 1.720 Å for terminal oxygens and are 1.812 and 1.821 Å for the bridging oxygens. The V–O distances are consistent with the strengths of the Pb—O bonds.

The crystal structure of benzenediazonium tetrafluoroborate, C6H5N2+•BF4−1

1982 ◽  
Vol 60 (22) ◽  
pp. 2852-2855 ◽  
Author(s):  
Miroslaw Cygler ◽  
Maria Przybylska ◽  
Richard MacLeod Elofson
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Benzene Ring ◽  
Positive Charge ◽  
Unit Cell ◽  
Full Matrix ◽  
Bond Lengths ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Close Contacts

Benzenediazonium tetrafluoroborate, C6H5N2+•BF4−, crystallizes in space group P21/a with unit cell dimensions a = 17.347(2), b = 8.396(1), c = 5.685(1) Å, β = 92.14(1)°, Z = 4. The structure was solved by direct phasing methods using the program SHELX 76. The parameters were refined by full-matrix least-squares to a final R = 0.063 for 1346 observed reflections. The bond lengths and angles agree very well with those of Rømming for benzenediazonium chloride. The C—N and N≡N bond lengths are 1.415(3) and 1.083(3) Å, respectively, and the bonds of the benzene ring do not show any significant differences as they vary from 1.371(5) to 1.383(4) Å. There are three [Formula: see text] close contacts of ≤ 2.84 Å and the positive charge appears to be shared between the nitrogen atoms.

scholarly journals Molekül- und Kristallstruktur von C7H7Mo(CO)2-SnCl3 / The Crystal Structure of C7H7Mo(CO)2-SnCl3

1975 ◽  
Vol 30 (1-2) ◽  
pp. 22-25 ◽  
Author(s):  
M. L. Ziegler ◽  
H.-E. Sasse ◽  
B. Nuber
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Title Compound ◽  
Three Dimensional ◽  
Unit Cell ◽  
Fourier Methods ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Group D

The structure of the title compound has been determined from three dimensional X-ray data by Patterson and Fourier methods. The crystals are orthorombic, with unit cell dimensions a = 1181,50 pm, b = 943,68 pm, c = 1181,50 pm, space group D2h16 and Z = 4. Least squares refinement, by use of 1540 independent reflections measured on a diffractometer has reached R = 5,9%.There are discrete C7H7Mo(CO)2 SnCl3 molecules, the molybdenum-tin bond has been dicussed together with the corresponding bonds in other C7H7Mo(CO)2 SnR3 compounds.

Kristallstruktur von Bis(N.N′-bis(8-chinoyl)äthylendiaminato)nickel(II) / Crystal Structure of Bis(N,N′-bis(8-chinoyl)ethylenediaminato)nickel(II)

1977 ◽  
Vol 32 (2) ◽  
pp. 131-133 ◽  
Author(s):  
H. Endres ◽  
H. J. Keller ◽  
A. Poveda
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Least Squares ◽  
Title Compound ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Cell Dimensions ◽  
Planar Molecules ◽  
Unit Cell Dimensions

The title compound NiC20H16N4 crystallizes in the monoclinic space group Ρ21/a with unit cell dimensions a = 12.07(2) Å, b= 10.712(4) Å, c = 13.50(3) Å, β= 113.1(1)°. The structure was refined by a blockmatrix least squares procedure to R = 0.126, based on 1258 observed intensities. The planar molecules form centro-symmetric dimers in the solid state with interplane distances of 3.3 A.

The Crystal Structure of Dimethylsulfoxidepentammineruthenium(II) Hexafluorophosphate

1971 ◽  
Vol 49 (22) ◽  
pp. 3590-3595 ◽  
Author(s):  
Frank C. March ◽  
George Ferguson
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Sulfur Atom ◽  
Three Dimensional ◽  
Bond Distance ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Sulfur Donor

The crystal structure of dimethylsulfoxidepentammineruthenium(II) hexafluorophosphate ( [Ru(NH3)5DMSO]2+ 2PF6−) has been determined from three-dimensional X-ray data. The crystals are monoclinic, space group P21/c, with four formula units in a unit cell of dimensions a = 8.805(2), b = 17.335(5), c = 12.373(2) Å, β = 94.24(2)°. The structure has been refined by full matrix least-squares methods to a final residual R of 0.054 for 1987 reflections greater than 3σ. The DMSO ligand coordinates through the sulfur atom and the S—O bond distance (1.527(7) Å) is considerably longer than that found for other sulfur–donor complexes of the ligand. The Ru—S bond distance is 2.188(3) Å.

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