Pyrazine and 2,5-dimethylpyrazine complexes of copper(I) trifluoromethanesulfonate. The crystal and molecular structure of poly-μ-2,5-dimethylpyrazine-(2,5-dimethylpyrazine)-(trifluoromethanesulfonato-O)copper(I)

1990 ◽  
Vol 68 (10) ◽  
pp. 1901-1907 ◽  
Author(s):  
Tom Otieno ◽  
Steven J. Rettig ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Crystal And Molecular Structure ◽  
Copper Ions ◽  
Heavy Atom ◽  
Electronic Spectroscopy ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Full Matrix ◽  
X Ray ◽  
Neutral Ligands ◽  
Spectroscopy Studies

The complexes CuL2(CF3SO3) where L is pyrazine and 2,5-dimethylpyrazine have been prepared by the reaction of copper(I) triflate with the neutral ligand in methanol. Single crystal X-ray diffraction studies on the 2,5-Me2pyz complex are reported. Crystals of the compound are triclinic, a = 9.424(4), b = 12.103(4), c = 9.113(4) Å, α = 110.97(3), β = 117.20(3), γ = 80.26(3)°, Z = 2, space group [Formula: see text]. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.033 and Rw = 0.039 for 3326 reflections with I ≥ 3σ(1). The structure is similar to that of the pyz analogue involving chains of copper ions linked by bridging 2,5-Me2pyz ligands and monodenate triflate and terminal 2,5-Me2pyz ligands completing a distorted tetrahedral CuN3O chromophore. Mono-pyrazine and -2,5-dimethylpyrazine complexes of the type CuL(CF3SO3) were obtained by thermolysis of the corresponding bis-ligand complexes. These compounds are assigned a polymeric structure involving bridging neutral ligands and monodenate triflate groups on the basis of infrared spectroscopy studies. Electronic spectroscopy and differential scanning calorimetry studies are also reported. Keywords: pyrazine and 2,5-dimethylpyrazine complexes, copper(I) triflate, crystal structure.

Synthesis, structure, and vibrational spectrum of poly-μ-pyrazine(pyrazine)(trifluoromethanesulfonato-O)copper(I)

1989 ◽  
Vol 67 (11) ◽  
pp. 1964-1969 ◽  
Author(s):  
T. Otieno ◽  
S. J. Rettig ◽  
R. C. Thompson ◽  
J. Trotter
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Copper Ions ◽  
Heavy Atom ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Methanol Solutions ◽  
Infrared And Raman Spectroscopy ◽  
Spectroscopy Studies

Orange–brown crystals of composition Cu(pyz)2(CF3SO3) (pyz = pyrazine, 1,4-diazine) were obtained from methanol solutions containing Cu(CF3SO3)2 and pyrazine in approximate 1:2 mole ratio. Single crystal X-ray diffraction and infrared and Raman spectroscopy studies are reported. Crystals of the title compound are triclinic, a = 8.312(2), b = 10.903(3), c = 8.201(2) Å, α = 92.53(2), β = 113.77(2), γ = 91.40(2)°, Z = 2, space group [Formula: see text] The structure was solved by heavy atom methods and was refined by full-matrix least-squares to R = 0.035 and Rw = 0.044 for 2458 reflections with 1 ≥ 3σ(I). The compound contains chains of copper ions linked by bidentate bridging pyrazine ligands. The coordination around each copper is completed by monodentate pyrazine and trifluoromethanesulfonato groups to produce a distorted tetrahedral CuN3O chromophore. Keywords: crystal structure, μ-pyrazine copper(I) triflate polymer, vibrational spectra.

Perchlorate and difluorophosphate coordination derivatives of rhenium carbonyl

1980 ◽  
Vol 33 (11) ◽  
pp. 2369 ◽  
Author(s):  
E Horn ◽  
MR Snow
Keyword(s):  
Heavy Atom ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Rhenium Carbonyl ◽  
Hydrolysis Of ◽  
Derivatives Of

The complexes Re(CO)5ClO4, Re(CO)5PO2F2, L2(CO)3Re(OClO3) and L2(CO)3Re(PO2F2), where L2 = 2,2?-bipyridyl (bpy), have been synthesized by bromide abstraction reactions from the respective rhenium carbonyl bromide precursors. The complexes were characterized by infrared and mass spectroscopy. The crystal structure of (bpy)(CO)3Re(PO2F2) has been determined from X-ray diffraction data by the heavy-atom technique. The crystals are triclinic, space group Pī with a 8.620(3), b 15.912(5), c 6.466(3) Ǻ, α 102.08(8), β 83.29(8), γ 95.08(4) and Z 2. The structure has been refined by full-matrix least-squares from 2829 reflections to R = 0.084, Rw = 0.088. The coordination geometry about rhenium is that of a distorted octahedron. Difluorophosphate coordinates to the metal centre by one of its oxygen atoms. Formation of the difluorophosphate by hydrolysis of hexafluorophosphate was shown by 31P n.m.r. spectra.

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.

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 Dithiocyanato(triphenylarsine)mercury(II)

1975 ◽  
Vol 53 (22) ◽  
pp. 3383-3387 ◽  
Author(s):  
Joseph Hubert ◽  
André L. Beauchamp ◽  
Roland Rivest
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Coordination Number ◽  
Diffraction Data ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heavy Atom Method

The crystal and molecular structure of dithiocyanato(triphenylarsine)mercury(II) has been determined from X-ray diffraction data. The crystals are monoclinic, space group P21/c, with a = 10.290(7), b = 21.199(23), c = 10.719(7) Å, β = 112.00(2)°, and Z = 4. The structure has been solved by the heavy-atom method and refined by block-diagonal least-squares calculations. The agreement factor R obtained for 2607 'observed' reflections is 0.030. The crystal consists of single molecules. The 'characteristic' coordination number of mercury is three, with two sulfur and one arsenic atoms at the apexes of a triangle. The nitrogen atoms of the thiocyanate groups are at 2.67 and 2.74 Å from the adjoining mercury atoms and therefore link the different molecules together.

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.

Synthesis, structure, and magnetic properties of diphenylphosphinates of cobalt(II) and manganese(II). The crystal and molecular structures of the γ forms of poly-bis(μ-diphenylphosphinato)cobalt(II) and manganese(II)

1991 ◽  
Vol 69 (2) ◽  
pp. 277-285 ◽  
Author(s):  
Jing-Long Du ◽  
Steven J. Rettig ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Magnetic Properties ◽  
Heavy Atom ◽  
Molecular Structures ◽  
Antiferromagnetic Coupling ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Lattice Constants ◽  
Linear Chains

The synthesis of the β and γ forms of M(Ph2PO2)2 where M = Co and Mn are described and the compounds are characterized by infrared spectroscopy, differential scanning calorimetry, X-ray powder diffraction, and low-temperature (2–80 K) magnetic susceptibility studies. Single crystal X-ray diffraction studies are reported on the γ forms. Crystals of the γ forms of poly-bis(μ-diphenylphosphinato)cobalt(II) and poly-bis(μ-diphenylphosphinato)manganese(II) are isomorphous, crystallizing with 4 formula units per unit-cell in the monoclinic space group P21/c. Lattice constants are a = 8.080(2), 8.161(1), b = 23.550(6), 23.751(1), c = 11.726(3), 11.6946(6) Ǻ, and β = 92.88(2), 93.026(8)° for the Co and Mn derivatives respectively. The structures were solved by heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.039 and 0.045 for 4041 and 2878 reflections with I ≥ 3σ(I), respectively. Both crystal structures consist of double phosphinate-bridged chain polymers containing tetrahedrally coordinated metal atoms: Co—O = 1.950(2)–1.963(2) Ǻ, O—Co—O = 104.81(8)–117.77(9)°, Mn—O = 2.016(3)–2.033(3) Ǻ, O—Mn—O = 103.2(1)–114.7(1)°. All four compounds exhibit antiferromagnetic coupling and magnetic susceptibilities have been analyzed according to two Heisenberg models for linear chains of metal ions with S = 3/2 for cobalt and S = 5/2 for manganese. The Weng model (with values for the Wagner and Friedberg model in parentheses) gives –J = 0.25 (0.26) cm−1 and 0.55 (0.60) cm−1 for the β and γ forms, respectively, of Co(Ph2PO2)2, and 0.34 (0.36) cm−1 and 0.17 (0.17) cm−1 for the β and γ forms, respectively, of Mn(Ph2PO2)2. Key words: crystal structure, diphenylphosphinates of cobalt(II) and manganese(II), magnetic properties.

Weak interactions observed in ruthenium and iridium complexes containing hydride, amine, and bulky phospyhine ligands

1997 ◽  
Vol 75 (5) ◽  
pp. 475-482 ◽  
Author(s):  
Wei Xu ◽  
Alan J. Lough ◽  
Robert H. Morris
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Weak Interactions ◽  
Crystal Structure Analysis ◽  
Monoclinic Space Group ◽  
Iridium Complexes ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Van Der Waals Contacts

New amineruthenium and amineiridium hydride derivatives have been synthesized and characterized with the objective of observing intramolecular [Formula: see text] or [Formula: see text] interactions. These include RuHCl(CO)(L)(PPri3)2 (1a, L = NH2NH2; 1b, L = NH3) and IrCl2(L)(H)(PCy3)2 (2a, L = SC(NH2)2; 2b, L = NH3; 2c, L = NH2NH2; 2d, L = NH2(CH2)3NH2; 2e, L = NH2OH). Instead, weak [Formula: see text] van der Waals contacts have been detected in the solid state by X-ray analysis and in solution by NMR T1 measurements and nOe techniques. Both X-ray crystal structure analysis and minimum T1 measurements indicate that the [Formula: see text] distances in the [Formula: see text] interactions are ca•2.0–2.2 Å. The weak interactions might influence the course of deuteration of these complexes under D2 gas. The crystal and molecular structure of IrCl2(NH3)(H)(PCy3)22a has been determined by X-ray diffraction at 173 K: monoclinic, space group P21/n, a = 14.859(2) Å, b = 18.579(3) Å, c = 18.548(3) Å, β = 97.29(1)°, V = 5079.1(13) Å3, Z = 4, full-matrix least-squares refinement on F2 for 10 953 independent reflections; R[F2 > 4σ(F2)] = 0.0283, wR(F2) = 0.0704. Keywords: ruthenium, iridium, hydride, dihydrogen, complexes, hydrogen bond, NMR, X-ray.

Synthesis, IR and X-Ray Studies of a Dioxouranium(VI) Nitrate Complex with N,N′-Tetraethyl-N″ -trichloracetylphosphortriamide

1997 ◽  
Vol 52 (10) ◽  
pp. 1194-1198 ◽  
Author(s):  
Vladimir M. Amirkhanov ◽  
Joachim Sieler ◽  
Victor A. Trush ◽  
Vladimir A. Ovchynnikov ◽  
Konstantin V. Domasevitch
Keyword(s):  
Crystal And Molecular Structure ◽  
Carbonyl Groups ◽  
Nitrate Complex ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Phosphoryl Oxygen ◽  
Neutral Ligands ◽  
Ambidentate Ligand ◽  
Ir Spectroscopic

A new dioxouranium(VI) nitrate complex with N,N′-tetraethyl-N″-trichloracetylphosphortriamide (HL = CCl3C(O)N(H)P(O)(NEt2)2) of composition UO2 (HL)2(NO3)2 (1) has been synthesised. The IR spectroscopic data reveal that the ambidentate ligand is coordinated to the metal center in a monodentate manner via the phosphoryl oxygen atom. The crystal and molecular structure of 1 has been determined from X-ray diffraction data (triclinic, space group P1̄ with a = 9.225(2), b = 10.360(2), c = 12.249(2) Å, α = 100.02 (1), β = 103.81(1), γ = 108.80 (1)°, Z = 1; R = 0.037 for 4092 unique reflections. The structure is made up of centrosymmetric molecules in which the neutral ligands HL are monocoordinated. Phosphoryl and carbonyl groups of the HL moieties are in the trans positions to each other. The axial vertices of the distorted hexagonal bipyramid of uranium are occupied by two oxo ligands [U-O 1.753(5) Å] while six oxygen atoms of phosphoryl and nitrate groups lie in the equatorial plane [U-O 2.347(5)-2.547(6)Å],

An X-Ray Crystallographic Study of Cd[P(C-C6H11)3]2(NO3)2.CH2Cl2

1986 ◽  
Vol 39 (4) ◽  
pp. 713 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls ◽  
ERT Tiekink
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Cadmium Atom ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Full Matrix ◽  
X Ray ◽  
Crystallographic Study ◽  
Tetrahedral Environment

The crystal and molecular structure of bis ( tricyclohexylphosphine )cadmium(II) nitrate as its dichloromethane solvate, Cd [P(c-C6H11)3]2(NO3)2.CH2Cl2, has been determined by single- crystal, three-dimensional X-ray diffraction methods. The crystals of the cadmium(II) complex are monoclinic with space group C2/c, a 20.880(6), b 12.775(3), c 17.075(5) Ǻ and β 106.38(2)°, Z 4. The structure was solved by normal Fourier methods and refined by a full-matrix least-squares procedure. The refinement used the 2169 statistically independent reflections for which I ≥ 2σ(I) converged with R and Rw of 0.065 and 0.067 respectively. The crystals consist of discrete Cd [P(c-C6H11)3]2(NO3)2 molecules and CH2Cl2 in the ratio 1 : 1. There is a distorted tetrahedral environment around the cadmium atom formed from the coordination of the two phosphines and two nitrates with each nitrate essentially occupying one stereochemical position. The two markedly different Cd -O bond lengths of 2.405(9) and 2.575(8) Ǻ show gross asymmetry in the coordination of the nitrate.

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