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.

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.

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.

Complexes of cobalt(II), nickel(II) and copper(II) with a pentadentate Bis(β-amino ketone); Crystal and molecular structure of Aqua(4,4,12,12-tetramethyl-5,8,11-triazapentadecane-2,14-dione)cobalt(II) perchlorate hydrate

1982 ◽  
Vol 35 (6) ◽  
pp. 1105 ◽  
Author(s):  
KR Morgan ◽  
GJ Gainsford ◽  
NF Curtis
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Complex Cation ◽  
Carbonyl Oxygen ◽  
Amino Ketone ◽  
X Ray ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Imine Ligands ◽  
Pentadentate Ligand

The diperchlorate salts of the mono(β-amino ketone) 10-amino-4,4-dimethyl-5,8-diazadecan-2-one and of the bis(β-amino ketone) 4,4,12,12-tetramethyl-5,8,11-triazapentadecane-2,14-dione, ttp, have been prepared by reaction of the diperchlorate of 3-azapentane-1,5-diamine with acetone. The salt [ttpH2] (ClO4)2 has been used to prepare the six-coordinate complexes [Cu(ttp)(H2O)] (ClO4)2,1.5H2O and [Ni(ttp)(H2O)] (ClO4)2,H2O, and the five-coordinate [Cu(ttp)] (CIO,),. The complex [Cu(ttp)] (ClO4), reacts with ammonia, methylamine and ethylamine to form complexes of pentadentate β-amino ketone β-amino imine ligands. The structure of [Co(ttp)(H2O)] (ClO4)2,1.5H2O has been determined by X-ray diffractometry [space group P21/c, Z 4, a 797.5(2), b 1632.8(3), c 2236.4(3) pm, β 97.504(2)�, R 0.0749, Rw 0.0765 for 1678 reflections]. The complex cation has the bis(β-amino ketone) ttp acting as a pentadentate ligand, with the three nitrogen and one carbonyl oxygen atoms coplanar, and with oxygen of a water molecule completing distorted octahedral coordination about the cobalt(II) ion.

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.

Crystal and molecular structure of B,B-bis(p-tolyl)boroxazolidine and the orthorhombic form of B,B-diphenylboroxazolidine

1976 ◽  
Vol 54 (20) ◽  
pp. 3130-3141 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Statistical Analysis ◽  
Hydrogen Bonds ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Length Variation ◽  
Full Matrix ◽  
Space Group ◽  
Phenyl Rings ◽  
Related Compounds

Crystals of B,B-bis(p-tolyl)boroxazolidine, 1c, are trigonal, a = 25.1028(9), c = 12.4184(7) Å, Z = 18, space group [Formula: see text]. And crystals of B,B-diphenylboroxazolidine, 1a, are orthorhombic, a = 17.6420(4), b = 14.2527(3), c = 10.205(1) Å, Z = 8, space group Pbca. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to final R values of 0.057 and 0.040 for 2230 and 1828 reflections with I ≥ 3σ(I) respectively. Both molecules have structures similar to related compounds and feature intermolecular N—H … O hydrogen bonds (N … O = 2.982(2) for 1c and 2.896(2) Å for 1a). Bond lengths are: for 1c; O—C, 1.413(3), O—B, 1.478(3), N—C, 1.488(3), N—B, 1.657(3), C(sp3)—C(sp3), 1.501(4), B—C, 1.616(3) and 1.623(3), mean C—C(ar), 1.395, N—H, 0.93(2) and 0.94(2), mean C(sp3)—H, 1.00, and mean C(ar)—H, 1.00 Å; for 1a; O—C, 1.409(2), O—B, 1.476(2), N—C, 1.489(2), N—B, 1.655(2), C(sp3)—C(sp3), 1.507(3), B—C, 1.613(2) and 1.620(2), mean C—C(ar), 1.391, N—H, 0.93(2) and 0.92(2), mean C(sp3)—H, 1.00, and mean C(ar)—H, 0.98 Å. A statistical analysis of the phenyl C—C distances in compounds 1a, 1b, and 1c has provided an example of statistically significant substituent-induced bond length variation in the phenyl rings.

Crystal and molecular structure of 2,6-dimethyl-3,5-di[N-methyl]carbamoyl-4-[3,4-methoxy]phenyl-l,4-dihydropyridine hemihydrate and 2,6-dimethyl-3,5-di[N-methyl]carbamoyl-4-[furan]1,4-dihydropyridine

1999 ◽  
Vol 214 (12) ◽  
Author(s):  
M. Bidya Sagar ◽  
K. Ravikumar ◽  
Y. S. Sadanandam
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal Structures ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Asymmetric Unit ◽  
Full Matrix

AbstractThe crystal structures of two dihydropyridines were solved by direct methods and refined by full-matrix least-squares procedure. 2,6-Dimethyl-3,5-di[N-methyl]-carbamoyl-4-[3,4-methoxy]phenyl-1,4-dihydropyridine hemihydrate, CBoth compounds crystallize with two molecules in the asymmetric unit. In compound

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.

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.

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