Chemical reduction of .eta.5-cyclopentadienyldicarbonylrhodium. Crystal and molecular structure of an anionic trinuclear rhodium cluster with "semi-triple-bridging" carbonyl ligands

1978 ◽  
Vol 100 (21) ◽  
pp. 6770-6772 ◽  
Author(s):  
William D. Jones ◽  
Mary Ann White ◽  
Robert G. Bergman
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Chemical Reduction ◽  
Carbonyl Ligands

Crystal and molecular structure of trans-[RhCl(CO)(PtBu2Ph)2]

2018 ◽  
Vol 73 (12) ◽  
pp. 1029-1032
Author(s):  
Peter Mayer ◽  
Hans-Christian Böttcher
Keyword(s):  
Molecular Structure ◽  
Ir Spectroscopy ◽  
Crystal And Molecular Structure ◽  
Title Complex ◽  
High Yield ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Pale Yellow ◽  
X Ray Crystallography ◽  
Type Complex

AbstractTreatment of THF solutions containing the rhodium(II) complex trans-[RhCl2(PtBu2Ph)2] (1) with [Fe2(CO)9] in the same solvent resulted in the formation of the Vaska-type complex trans-[RhCl(CO)(PtBu2Ph)2] (2) in high yield. The title complex 2 was obtained as pale yellow crystals, characterized by NMR and IR spectroscopy, as well as by microanalyses. Additionally, the molecular structure of 2 has been established by X-ray crystallography. As often reported for similar constituted compounds, the chlorido and carbonyl ligands in crystals of 2 are strongly disordered.

Preparation and crystal and molecular structure of (η3-octamethylcyclotetraphosphazane-P,P,P)tricarbonylmolybdenum(0), [η3-(CH3PNCH3)4]Mo(CO)3

1982 ◽  
Vol 60 (19) ◽  
pp. 2415-2419 ◽  
Author(s):  
Keith D. Gallicano ◽  
Norman L. Paddock ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Phosphorus Atom ◽  
Mirror Symmetry ◽  
Crystal And Molecular Structure ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Full Matrix ◽  
Carbonyl Ligands ◽  
Distorted Octahedral

The synthesis and physical properties of the phosphazane complex [η3-(CH3PNCH3)4]Mo(CO)3 are reported. Crystals of (η3-octamethylcyclotetraphosphazane-P,P,P)tricarbonylmolybdenum(0) are monoclinic, a = 8.6898(9), b = 16.0987(8), c = 14.1156(17) Å, β = 98.321(6)°, Z = 4, space group Cc. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.020 and Rw = 0.024 for 2286 reflections with I ≥ 3σ(I). The molybdenum atom is coordinated to three phosphorus atoms of the (MePNMe)4 ligand and to three carbonyl ligands in a distorted octahedral geometry. The molecule has approximate mirror symmetry in the solid state. Important bond lengths (corrected for libration) are: Mo—P = 2.537(1), 2.467(1), and 2.513(1), Mo—C = 1.971(4), 2.002(4), and 1.978(4), mean P—N = 1.704(8) for coordinated P, 1.735(7) Å for uncoordinated P. The structural evidence indicates that the phosphazane is a weaker donor to Mo(CO)3 than to three sulphur atoms, and that coordination withdraws electron density from the fourth phosphorus atom. The complex is fluxional in solution.

Preparation and crystal and molecular structure of (η3-nonamethylcyclotetraphosphazanium-P,P,P)tricarbonylmolybdenum(0) iodide – acetonitrile (1:1), [(η3-Me(MeNPMe)4)Mo(CO)3]I•MeCN

1984 ◽  
Vol 62 (9) ◽  
pp. 1869-1873 ◽  
Author(s):  
Keith D. Gallicano ◽  
Norman L. Paddock ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Mirror Symmetry ◽  
Crystal And Molecular Structure ◽  
Complex Cation ◽  
Neutral Species ◽  
Full Matrix ◽  
Carbonyl Ligands ◽  
Fourier Techniques ◽  
Distorted Octahedral ◽  
Solvent Molecules

The synthesis and physical properties of [(η3-Me(MeNPMe)4)Mo(CO)3]l are reported. Crystals of (η3-nonamethylcyclotetraphosphazanium-P,P,P)tricarbonylmolybdenum(0) iodide – acetonitrile (1:1) are orthorhombic, a = 13.1938(4), b = 13.7847(5), c = 29.281(2) Å, Z = 8, space group Pcab. The structure was solved by Patterson and Fourier techniques and was refined by full-matrix least-squares procedures to R = 0.030 and Rw = 0.034 for 2388 reflections with I ≥ 3σ(I). The structure consists of discrete cations, anions, and solvent molecules. The complex cation has approximate mirror symmetry in the solid state, the Mo atom being coordinated to three phosphazane P atoms and three carbonyl ligands in a distorted octahedral arrangement. Important bond lengths (corrected for libration) are: Mo—P = 2.483(2), 2.439(2), and 2.474(2), mean Mo—C = 1.984(3), mean P—N = 1.710(11) for coordinated P and 1.669(5) Å for quaternized P. The stronger bonding of the cationic ligand to the metal relative to that of the neutral species (CH3NPCH3)4Mo(CO)3, and the strengthening of the ring bonds in both molecules relative to (CH3NPCH3)4, are discussed in terms of d-orbital contraction.

Structural studies in the ruthenium(II)/(±)-ortho-Phenylenebis{methyl(phenyl)-phosphine/arsine} system. III. Crystal structures of Dichlorocarbonyl(dimethyl sulfoxide)-[ortho-phenylenebis {methyl(phenyl)phosphine}]ruthenium(II) and of cis-dicarbonyldichloro[(±)-ortho-phenylenebis{methyl(phenyl)arsine}]ruthenium(II)

1983 ◽  
Vol 36 (2) ◽  
pp. 271 ◽  
Author(s):  
SR Hall ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Dimethyl Sulfoxide ◽  
Crystal And Molecular Structure ◽  
Title Complex ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carbonyl Ligands ◽  
Methyl Phenyl

The crystal and molecular structure of the title complex, cis-[Ru(CO)Cl2(dmso)(opmpp)] (1) (dmso ≡ dimethyl sulfoxide, Me2SO; opmpp ≡ (�)-ortho-phenylenebis {methyl(phenyl)phosphine},[o-C6H4(PMePh)2]), has been determined by a single-crystal X-ray diffraction study at 295(1) K, being refined to a residual of 0.050 for 6115 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 11.180(7), b 12.957(6), c 17.567(9) �, β 90.88(5)�, Z 4. The ruthenium-chlorine distances, trans to phosphine and carbonyl ligands, respectively, are 2.469(2), 2.446(2) �; the ruthenium-phosphine distances, trans to the chloride and dimethyl sulfoxide ligands, respectively, are 2.292(1), 2.313(2) �. Ruthenium-sulfur (dmso) is 2.380(2) �, while the ruthenium-carbon(CO) is c. 1.72 �. For cis-[Ru(CO)2Cl2(opmpa)] (2) (opmpa ≡ (�)-ortho-phenylenebis{methyl(phenyl)- arsine}, [o-C6H4(AsMePh)2]), refinement led to a residual of 0.036 for 2423 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 10.497(3), b 11.586(7), c 20.341(9) �, β 105.31(4)�, Z 4. Ruthenium-arsine distances, trans to carbonyl and chlorine ligands, respectively, are 2.404(1), 2.455(1) �. Ruthenium-chlorine distances, trans to arsine and carbonyl ligands, respectively, are 2.443(3), 2.433(2) �, while ruthenium-carbon(CO) distances, trans to arsine and chlorine ligands, respectively, are 1 .920(8), 1 .872(8) �.

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