Complexes of dodecamethylcyclohexaphosphazene with palladium(II) chloride and platinum(II) chloride. Crystal and molecular structure of cis-dichloro[η2-dodecamethylcyclohexaphosphazene (N,N′)] palladium(II) sesquihydrate

1981 ◽  
Vol 59 (16) ◽  
pp. 2429-2434 ◽  
Author(s):  
Norman L. Paddock ◽  
T. N. Ranganathan ◽  
Steven J. Rettig ◽  
Rajendra D. Sharma ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Bond Order ◽  
Nmr Spectra ◽  
Crystal And Molecular Structure ◽  
Model Calculations ◽  
Full Matrix ◽  
X Ray ◽  
Square Planar ◽  
The Mean ◽  
C Nmr

Dodecamethylcyclohexaphosphazene N6P6Me12, 1, forms 1:1 complexes with palladium(II) chloride, 2, and platinum(II) chloride, 3. Their 31P, 1H, and 13C nmr spectra show them to be rigid molecules in solution, with an approximate plane of symmetry. Crystals of 2 are orthorhombic, a = 17.4030(3), b = 15.4897(5), c = 10.7417(2) Å, Z = 4, space group P21212. The structure was determined from diffractometer X-ray data and refined by full-matrix least-squares methods to R = 0.031 for 3545 reflections with I ≥ 3σ(I). The metal atom has square planar coordination, and forms 6- and 10-membered chelate rings with the phosphazene ligand. The mean P—N bond length is 1.609 Å; the variation of bond lengths within the ring is consistent with model calculations of changes in bond order arising from the localization of bonding electrons.

The crystal and molecular structure of cis-dichloro(2,2′-o-phenylenebisbenzothiazole)copper(II)

1979 ◽  
Vol 57 (11) ◽  
pp. 1368-1371 ◽  
Author(s):  
Richard G. Ball ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Coordination Geometry ◽  
Full Matrix ◽  
X Ray ◽  
Square Planar ◽  
The Mean ◽  
Final Agreement ◽  
Cl Atoms ◽  
Least Squares Techniques

The molecular structure of cis-dichloro(2,2′-o-phenylenebisbenzothiazole)copper(II) has been determined by single crystal X-ray diffractometry. The crystal is monoclinic, P21/n, a = 8.408(1), b = 15.819(1), c = 14.229(2) Å, β = 93.19(1)°, and Z = 4. The structure has been refined by full-matrix least-squares techniques on F, using 3316 unique reflections for which F2 > 3σ(F2), to a final agreement factor of 0.028. The complex adopts an approximately square planar coordination geometry with the Cu bound to two cis Cl atoms and the N atoms of the chelating benzothiazole ligand. The mean Cu—N and Cu—Cl distances are 2.016(6) and 2.217(6) Å, respectively.

The Crystal and Molecular Structure of the Dihydrochloride of 2-trans-6-Diethyl-2,4,4,6,8,8-hexamethylcyclotetraphosphazene

1975 ◽  
Vol 53 (16) ◽  
pp. 2413-2418 ◽  
Author(s):  
Harry P. Calhoun ◽  
Richard T. Oakley ◽  
Norman L. Paddock ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Crystal And Molecular Structure ◽  
Chair Conformation ◽  
Electrostatic Repulsion ◽  
Electron Localization ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
The Mean

Octamethylcyclotetraphosphazene is deprotonated by methyllithium to form carbanions, which react with methyl iodide to give ethyl derivatives N4P4Me8−nEtn, [Formula: see text] the structure of the dihydrochloride of the diethyl derivative, N4P4Me6Et2•2HCl has been determined. Its crystals are monoclinic, a = 9.928(5), b = 15.482(6), c = 6.329(2) Å, β = 103.29(2)°, space group P21/n. The structure was determined from diffractometer X-ray data and refined by full-matrix least squares methods to R 0.079 for 715 observed reflections. The N4P4Me6Et2H22+ ion lies on a crystallographic center of symmetry and the eight-membered phosphazene ring has the "chair" conformation. There are two significantly different P—N bond lengths, 1.665(6) and 1.572(7) Å, and two significantly different P—N—P angles, 126.7(6) and 139.8(6)°. The mean P—C bond length is 1.801(7) Å, and the mean N—P—N and C—P—C angles are 112.2(4) and 107.6° respectively. Bond lengths and angles in the phosphazene ring show the characteristic effects of π-electron localization found in other protonated phosphazene derivatives. The two ethyl groups are in tran-antipodal positions, corresponding to the least intramolecular electrostatic repulsion in the carbanion.

Chalkogenolat-Ionen und ihre Derivate, V Kristall- und Molekülstruktur von 2.8-Dimethyldibenzo [c.g] [1.2.5.6] tetrathiacyclooktadien, einem Oxidationsprodukt von 4-Methylbenzol-1.2-dithiol/Chalcogenolates and their Derivatives, V Crystal and Molecular Structure of 2.8-Dimethyldibenzo[c,g][1,2,5,6]tetrathiaocin, an Oxidation Product of 4-Methylbenzene-1,2-dithiol

1979 ◽  
Vol 34 (1) ◽  
pp. 48-51 ◽  
Author(s):  
Jürgen Kopf ◽  
Klaus von Deuten ◽  
Bahman Nakhdjavan ◽  
Günter Klar
Keyword(s):  
Molecular Structure ◽  
Dihedral Angle ◽  
Oxidation Product ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
The Mean ◽  
Ray Methods ◽  
Anti Form

Abstract The structure of 2,8-dimethyldibenzo[c,g][1,2,5,6]tetrathiaocin (1b) has been determined by X-ray methods and discussed in connection with the preferred conformations of diaryl disulfides. The compound has the anti-form I. The SS-distance is 205.8 pm, the mean CSS-angle 104.1°, and the CSS/SSC-dihedral angle 111.1°.

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.

Structure cristalline et moléculaire d'un composé tricyclique contenant le cycle à dix chaînons dioxo diaza diphosphécine

1992 ◽  
Vol 70 (3) ◽  
pp. 809-816 ◽  
Author(s):  
Brigitte Duthu ◽  
Karim El Abed ◽  
Douraid Houalla ◽  
Robert Wolf ◽  
Joël Jaud
Keyword(s):  
Molecular Structure ◽  
Comparative Analysis ◽  
Double Bond ◽  
Mass Spectroscopy ◽  
Crystal And Molecular Structure ◽  
Accurate Information ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Parameters ◽  
C Nmr

The sulfuration of the tricyclic organophosphorous dimer 2 leads easily to the dithiotricyclic derivative 3, which has been characterized by 31P, 1H, and 13C NMR, elemental analysis, and mass spectroscopy. Its crystal and molecular structure has been established by X-ray diffraction and compared to that of 2, which was previously determined. The comparative analysis of X-ray diffraction and NMR parameters gives accurate information about the molecular structure of both compounds. A numerical value of the anistropy cone of the P=S double bond is proposed. Keywords: phosphecine, NMR, X-ray, tricycle.

The Crystal and Molecular Structure of bis(triphenylphosphine)-(ethylene)platinum, (PPh3)2PtC2H4

1972 ◽  
Vol 50 (6) ◽  
pp. 912-916 ◽  
Author(s):  
P.-T. Cheng ◽  
S. C. Nyburg
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystal Structure Analysis ◽  
Transition Elements ◽  
Triphenyl Phosphine ◽  
Monoclinic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
System A

The X-ray crystal structure analysis of the triphenyl–phosphine platinum ethylene complex (PPh3)2PtC2H4 is reported. The crystals belong to the monoclinic system a = 16.46(3), b = 10.85(2), c = 17.85(3) Å, β = 100.5(1)°, space group P21/a, Z = 4 molecules per cell.The ethylene C—C distance of 1.434(13) Å is in accord with that found when other transition elements form metallo-cyclopropanes. The structure has been refined by anisotropic full-matrix least-squares, the final R-factor being 0.043 for 4174 observed reflections.

The Crystal and Molecular Structure of Pentane-2,4-dionato-(2,3,5,6-tetrahepto-2,3-dicarbomethoxo[2.2.1]bicycloheptadiene)rhodium(I), Rh(C5H7O2) (C7H6(CO2CH3)2)

1975 ◽  
Vol 53 (18) ◽  
pp. 2707-2713 ◽  
Author(s):  
Debbie Allen ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
John Powell
Keyword(s):  
Crystal And Molecular Structure ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Square Planar ◽  
Rhodium Atom

The crystal and molecular structures of pentane-2,4-dionato-(2,3,5,6-tetrahapto-2,3-dicarbomethoxo[2.2.1]bicycloheptadienerhodium(I), Rh(C5H7O2)(C7H6(CO2CH3)2), have been measured by single crystal X-ray diffraction. The orange crystals are monoclinic, space group P21/c, Z = 4, a = 9.245(4), b = 9.003(4), c = 21.680(15) Å, β = 113.41(5)°. The calculated and observed densities are 1.645 and 1.642(5) respectively. Intensity data were collected on a Syntex [Formula: see text] diffractometer and a full matrix least squares refinement on 3010 observed reflections leads to a conventional R = 0.0660. The structure can be considered as a roughly square planar arrangement of ligands around the rhodium atom composed of two β-ketoenolate oxygen atoms (Rh—O, 2.037(5) and 2.025(5) Å ) and the centers of the two ethylenic groups. The Rh—C distances for the olefin group attached to the two carbomethoxo groups, 2.117(8), 2.108(8) Å, appear to be slightly larger than those for the other olefinic group, 2.087(7), 2.082(6), and the corresponding C=C distances of 1.375(10) and 1.410(9) Å are different at the 95% confidence level.

Crystal and molecular structure of 3-ethyl-4-hydroxy-1,2,3(4H)-benzotriazine and 6-chloro-4-hydroxy-3-methyl-4-phenyl-1,2,3-benzotriazine

1985 ◽  
Vol 63 (3) ◽  
pp. 581-585 ◽  
Author(s):  
Kwong Khee Lai ◽  
Carl H. Schwalbe ◽  
Keith Vaughan ◽  
Ronald J. Lafrance ◽  
Clive D. Whiston
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Tetrahedral Geometry ◽  
Orthorhombic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor

The crystal structures of the title compounds have been determined from X-ray data collected on a four-circle diffractometer and refined by the full-matrix least-squares method. The former compound crystallizes in the orthorhombic system, space group Pbcn, with a = 14.346(8), b = 7.239(1), c = 17.276(2) Å, and has been refined to a conventional R factor of 0.043 for 890 observed reflections. Corresponding results for the latter compound are monoclinic, P21/n, a = 12.222(4), b = 7.482(2), c = 14.170(8) Å, β = 94.06(4)°, R = 0.060 for 2128 observed data. The triazine rings of both compounds exhibit short N(1)—N(2) bonds and tetrahedral geometry at C(4); however, the ring is puckered in the first compound but flat in the second. Molecules in both crystals are linked by [Formula: see text] hydrogen bonds.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

3-Methylpyridine complexes of cobalt(II) and nickel(II) hexafluorophosphate and hexafluoroarsenate. Crystal and molecular structure of Ni(H2O)2(3-CH3C5H4N)6(PF6)2

1983 ◽  
Vol 61 (7) ◽  
pp. 1651-1658 ◽  
Author(s):  
Raymond M. Morrison ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Atom ◽  
Water Molecule ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Water Molecules ◽  
Magnetic Studies ◽  
Full Matrix ◽  
Mild Conditions ◽  
Square Planar

Reaction of aqueous solutions containing CO2+ or Ni2+ and PF6−, or AsF6− with excess 3-methylpyridine yields crystals of compounds of composition M(H2O)2(3mpy)6(EF6)2. Blue crystals of diaquohexakis(3-methylpyridine)nickel(II) hexafluorophosphate, C36H46F12NiN6O2P2, are monoclinic, a = 10.497(1), b = 20.074(3), c = 21.836(5) Å, β = 103.93(2)°, Z = 4, space group Cc. The structure was determined with MoKα CAD4 diffractometer data by direct methods, and refined by full-matrix least-squares procedures to R = 0.048 for 2723 reflections with I ≥ 3σ(I). The structure consists of {Ni(3mpy)4[(OH2)(3mpy)]2}2+ cations and PF6− anions. The cation contains a NiN4O2 chromophore with water molecules occupying trans positions of a distorted octahedron about nickel. One additional 3-methylpyridine molecule is H-bonded to each of the water molecules with [Formula: see text] distances of 2.717(11) and 2.719(11) Å. Weak interaction of each water molecule via its second hydrogen atom with a PF6− ion is indicated by the positioning of the anions. The [Formula: see text] distances are 2.958(11) and 2.959(11) Å. Two other complexes of this type, where M is Ni and E is As and where M is Co and E is P, are reported here and on the basis of spectroscopic and magnetic studies are assigned structures similar to the Ni/P complex.Decomposition of the aquo complexes under mild conditions yields compounds of composition M(3mpy)4(EF6)2. Ni(3mpy)4(PF6)2 is assigned a square planar structure with weakly interacting PF6−, anions in axial positions. Both Co(3mpy)4(EF6)2 complexes, where E is P or As, have tetrahedral [Co(3mpy)4]2+ cations and non-coordinated anions.

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