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.

scholarly journals fac-[1,2-Bis(pyridin-4-yl)ethane-κN]tricarbonyl(1,10-phenanthroline-κ2N,N′)rhenium(I) hexafluoridophosphate acetonitrile monosolvate

2014 ◽  
Vol 70 (7) ◽  
pp. m278-m279 ◽  
Author(s):  
Silvana Guilardi ◽  
Antonio Otavio Toledo Patrocinio ◽  
Sinval Fernandes de Sousa ◽  
Javier Ellena
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Packing ◽  
Solvent Molecule ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Asymmetric Unit ◽  
Carbonyl Ligands ◽  
Distorted Octahedral ◽  
Phenanthroline Ligand ◽  
Solvent Molecules

The asymmetric unit of the title compound, [Re(C12H8N2)(C12H12N2)(CO)3]PF6.·CH3CN, contains one cation, one hexafluoridophosphate anion and one acetonitrile solvent molecule. The ReIion is coordinated by two N atoms from the 1,10-phenanthroline ligand and one N atom from the 1,2-bis(pyridin-4-yl)ethane ligand [mean Re—N = 2.191 (15) Å] and by three carbonyl ligands [mean Re—C = 1.926 (3) Å] in a distorted octahedral geometry. The electrostatic forces and weak C—H...F(O) hydrogen bonds pack cations and anions into the crystal with voids of 82 Å3, which are filled by solvent molecules. The crystal packing exhibits short intermolecular O...O distance of 2.795 (5) Å between two cations related by inversion.

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).

Crystal and molecular structure of [dimethyl(3,5-dimethyl-1-pyrazolyl)(ethanol-amino)gallato (N(2),O,N(3))](η3-cycloheptatrienyl)dicarbonylmolybdenum

1981 ◽  
Vol 59 (11) ◽  
pp. 1665-1670 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Amino Nitrogen ◽  
Full Matrix ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Unusual Type

Crystals of [dimethyl(3,5-dimethyl-l-pyrazolyl)(ethanolamino)gallato(N(2),O,N(3))](η3-cycloheptatrienyl)dicarbonylmolybdenum are monoclinic, a = 10.511(1), b = 8.335(1), c = 24.138(3) Å, β = 102.22(1)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was reflned by full-matrix least-squares procedures to R = 0.028 and Rw = 0.046 for 3708 reflections with I ≥ 3σ(I). The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.929(5) Å). The Mo atom is in a distorted octahedral environment with the η3-C7H7 ligand occupying one coordination site, trans to the amino nitrogen, as a π-donating ligand. Important bond distances (corrected for libration) are: Mo—O, 2.245(2), Mo—N(amino), 2.249(3), Mo—N(pyrazolyl), 2.270(3), Mo—C(O), 1.950(4) and 1.947(4), Mo—C(C7H7), 2.176(4), 2.364(4), and 2.380(4), Ga—O, 1.919(3), Ga—N, 1.984(3), and Ga—C, 1.982(5) and 1.983(5) Å. An unusual type of disorder is present in which a second image of the molecule, approximately mirrored by the plane y = 1/4, is in evidence at low occupancy.

The Crystal and Molecular Structure of Bis-[μ-2-(p-nitrophenyliminomethyl)phenolato-N,O]-bis(ethanol)bis(nitrato-O,O')dinickel(II), [Ni(slno)NO3(C2H5OH)]2, a Binuclear Ferromagnetic Salicylaldimine Derivative of Nickel Nitrate

1979 ◽  
Vol 32 (2) ◽  
pp. 331 ◽  
Author(s):  
RJ Butcher ◽  
E Sinn
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Nickel Atom ◽  
Nickel Nitrate ◽  
Distorted Octahedral Geometry ◽  
Tetrahedral Geometry ◽  
Imine Group ◽  
Phenolic Oxygen ◽  
Distorted Octahedral ◽  
Oxygen Atoms

The crystal and molecular structure of the complex bis-[μ-2-(p-nitrophenyliminomethyl)phenolato- N,O]-bis(ethanol)bis(nitrato-O,O')dinickel(11) and its magnetic properties are reported. Crystal data: space group PI, Z 1, a 8.882(2), b 9.332(3), c 12.533(4) �, α 94.40(2),B 109.99(2), γ 111.61(2)�, U 883 �3, R 2.8%, Rw 3.3% for 2154 reflections. The compound is prepared from the reaction of bis(N-p-nitrophenylsalicylaldimine)nickel(II) with nickel nitrate in hot triethoxymethane, and on cooling the solution deposited pale green transparent crystals. The structure contains neutral dimeric units with bridging through the phenolic oxygen atoms and has distorted octahedral geometry about each crystallographically identical nickel atom. The six donor atoms are made up of two oxygen atoms from the bidentate nitrate, oxygen from ethanol, nitrogen from the imine group and two bridging phenolic oxygen atoms. The Ni2O2 group is strictly planar possessing a crystallographic centre of symmetry. The angles subtended at the bridging oxygen atoms indicate a tetrahedral geometry and it is demonstrated that this is important in explaining the ferromagnetic intradimer interaction. The presence of hydrogen bonding between the ethanol hydrogen and the nitrate group of an adjacent molecule appears to be an important stabilizing factor in determining the structure and provides a possible pathway for the antiferromagnetic interdimer exchange interaction.

Crystal and molecular structure of (η3-2-methylallyl)[dimethyl(ethanolamino)-(3,5-dimethyl-1-pyrazolyl)gallato(N(2),N(3),O)] dicarbonylmolybdenum, [Me2Ga(N2C5H7)(OCH2CH2NH2)]Mo(CO)2(η3-C4H7)

1979 ◽  
Vol 57 (11) ◽  
pp. 1335-1340 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Full Matrix ◽  
Distorted Octahedral Environment ◽  
Coordination Sites ◽  
Octahedral Environment ◽  
Distorted Octahedral

Crystals of (η3-2-methylallyl)[dimethyl(ethanolamino)(3,5-dimethyl-1-pyrazolyl)gallato-(N(2),N(3),O)]dicarbonylmolybdenum are triclinic, a = 7.6047(5), b = 10.882(1), c = 12.633(1) Å, α = 77.07(1), β = 89.19(1), γ = 71.91(1)°, Z = 2, space group [Formula: see text]. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.024 and Rw = 0.030 for 3835 reflections with I ≥ 3σ(I). The crystal structure consists of discrete molecular units, each linked to four others by weak [Formula: see text] hydrogen bonds [Formula: see text] The Mo atom is in a distorted octahedral environment with the η3-C4H7 ligand occupying one of the six coordination sites as a π-donating ligand. Important bond distances (corrected for libration) are: Mo—C(allyl), 2.335(3), 2.372(3), 2.324(3); Mo—C(O), 1.902(3) and 1.961(2); Mo—O, 2.269(2); Mo—N(pz), 2.222(2); Mo—N(amino), 2.285(2); Ga—O, 1.924(2); Ga—N, 2.006(2); and Ga—C, 1.968(4) and 1.981(4) Å.

The crystal and molecular structure of gold tris(fluorosulfate)

1991 ◽  
Vol 69 (3) ◽  
pp. 391-396 ◽  
Author(s):  
H. Willner ◽  
S. J. Rettig ◽  
J. Trotter ◽  
F. Aubke
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Gold Atom ◽  
Coordination Geometry ◽  
Full Matrix ◽  
Distorted Octahedral Coordination ◽  
Square Planar ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

Single crystals of gold(III) tris(fluorosulfate) are obtained by recrystallization from bis(fluorosulfuryl) peroxide, S2O6F2, under O2 pressure. The crystals of [Au(SO3F)3]2 are monoclinic, a = 9.700(4), b = 9.222(2), c = 10.810(4)Å, β = 94.43(3)°, Z = 2, space group P21/a. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures, R(F) = 0.038 and Rw(F) = 0.050 for 1491 reflections with I ≥ 3σ(I). The structure consists of centrosymmetric [Au(SO3F)3]2 dimers containing two bidentate, symmetrically bridging and four monodentate, terminal SO3F ligands. The Au(III) ions have square-planar coordination geometry with bridging Au—O = 2.020(7) and 2.016(6) Å, and terminal Au—O = 1.959(7) and 1.956(9) Å. The dimeric [Au(SO3F)3]2 units are linked in the solid state by weak Au—O interactions (2.757(8) and 2.960(7) Å), resulting in a distorted octahedral coordination geometry about each gold atom. Key words: gold(III) tris(fluorosulfate), crystal structure.

Crystal and molecular structure of bis(perchlorato)(γ-C-meso-5,5,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)copper(II)

1978 ◽  
Vol 56 (3) ◽  
pp. 267-272 ◽  
Author(s):  
Ei-Ichiro Ochiai ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Macrocyclic Ligand ◽  
Coordination Geometry ◽  
Full Matrix ◽  
Bond Lengths ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

Crystals of bis(perchlorato) (γ-C-meso-5,5,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)copper(II) are monoclinic, a = 14.061(1), b = 8.908(1), c = 19.710(1) Å, β = 90.912(5)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.054 and Rw of 0.069 for 2945 reflections with I ≥ 3σ(I). The copper(II) ion has tetragonally distorted octahedral coordination geometry. The four nitrogen atoms of the macrocyclic ligand occupy the equatorial sites and two perchlorate oxygen atoms are in the axial positions. Bond lengths (corrected for libration) are: Cu—N, 2.024(4)–2.051(4), Cu—O, 2.657(5) and 2.697(5), Cl—O, 1.420(4)–1.473(6), N—C, 1.463(6)–1.508(6), and C—C, 1.498(8)–1.542(8) Å.

N,N-Ethylenebis(salicylideneimine) derivatives of gallium trimethyl: crystal and molecular structure of N,N-ethylenebis(salicylideneiminato) bis(dimethylgallium)

1977 ◽  
Vol 55 (13) ◽  
pp. 2540-2546 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Weighted Mean ◽  
Full Matrix ◽  
Derivatives Of ◽  
Distorted Tetrahedral Coordination

Crystals of N,N-ethylenebis(salicylideneiminato)bis(dimethylgallium) are orthorhombic, a = 22.781(1), b = 9.4869(6), c = 19.700(2) Å, Z = 8, space group Pbca. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.036 and Rw of 0.029 for 2248 reflections with I ≥ 3σ(I). Details of the preparation and physical properties of (C16H14N2O2)(GaMe2)2 and (C16H15N2O2)(GaMe2) are given. The (C16H14N2O2)(GaMe2)2 molecule is approximately centrosymmetric in the solid state. A "GaMe2" unit is coordinated to each of the two salicylideneiminato moieties of the N,N-ethylenebis(salicylideneiminato) ligand. The gallium atoms have a distorted tetrahedral coordination geometry, with bond angles at gallium ranging from 92.7(1) to 124.6(3)°. Important bond lengths (corrected for libration) are: Ga—O, 1.886(2) and 1.884(2), Ga—N, 2.033(3) and 2.042(3), and weighted mean Ga—C, 1.959(9) Å.

Dichlorido(N,N′-dibenzylideneethane-1,2-diamine-κ2 N,N′)[(2,2-dimethyl-1,3-dioxolane-4,5-diyl)bis(diphenylmethanolato)-κ2 O,O′]titanium(IV)

2007 ◽  
Vol 63 (11) ◽  
pp. m2842-m2843 ◽  
Author(s):  
Chien-An Chen ◽  
Liang-Ying Chiang ◽  
Han-Mou Gau
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Chloride Ions ◽  
Octahedral Geometry ◽  
Metal Center ◽  
Distorted Octahedral Geometry ◽  
Titanium Metal ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Chloride Ligands

The title compound, [TiCl2(C31H28O4)(C16H16N2)], is a titanium(IV) complex of the bidentate 2,2-dimethyl-α,α,α′,α′-tetraphenyl-1,3-dioxolane-4,5-dimethanolate (TADDOLate) ligand containing also two chloride ions and a bidentate neutral N,N′-dibenzylideneethane-1,2-diamine ligand. The molecular structure has a distorted octahedral geometry around the titanium metal center. The Ti—N bond lengths of 2.246 (2) and 2.2476 (17) Å are long, indicating weak bonding between the titanium(IV) metal center and the imine N atoms. Though the two chloride ligands are trans to each other, they bend away from the Ti–TADDOLate bonds with a Cl—Ti—Cl angle of 163.96 (3)°.

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