The crystal structure of two cobalt(I) complexes containing the polyphosphine ligands PhP{(CH2)nPPh2}2 (n = 2, 3)

1977 ◽  
Vol 30 (11) ◽  
pp. 2395 ◽  
Author(s):  
R Mason ◽  
GR Scollary
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Cobalt Complexes ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Independent Reflection ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bite Angle

X-ray diffraction analysis of the two complexes [CoPhP{(CH2)3PPh2}2P(OMe)3CO] BF4,thf and [CoPhP{(CH2)2PPh2}2{P(OMe)3}2] BF4 are reported. Crystals of the first complex are triclinic, space group Pī with a 14.310(1), b 11.080(2), c 16.099(3) Ǻ, α 68.30(2), β 90.78(2), γ 75.04(1)�. The structure analysis has been based on 2964 independent reflection intensities (Cu Kα automatic diffractometry) to give R 0.11. The second complex is monoclinic, space group P21/c, with a 13.18(4), b 11.49(3), c 29.66(6) Ǻ, β 101.59(2)�. Refinement by least squares has converged to R 0.093 for the 2256 independent reflection intensities, observed by Mo Kα automatic diffractometry. The preferred stereochemistries of the five-coordinate cobalt complexes are discussed in relation to the bite angle of the chelating phosphine.

THE CRYSTAL STRUCTURE OF K2TeBr6

1964 ◽  
Vol 42 (12) ◽  
pp. 2758-2767 ◽  
Author(s):  
I. D. Brown
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Least Squares ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cubic Form ◽  
Efficient Packing

Crystals of K2TeBr6 are monoclinic, space group [Formula: see text] with a = 7.521, b = 7.574, and c = 10.730 Å; β = 89° 40′. Atomic positions have been found by three dimensional X-ray diffraction analysis (least squares R = 0.12). The crystals possess a K2PtCl6 structure which is distorted to allow a more efficient packing of the comparatively large anions than is possible with the undistorted cubic form. The stereochemistry of the octahedral TeBr6− ion (Te—Br = 2.71 Å) is discussed.

Die Kristallstruktur des Tetraphenylphosphonium-Monoiodohexahydroc/ oso-Hexaborats [P(C6H5)4][B6H6I] / The Crystal Structure of Tetraphenylphosphonium Monoiodohexahydro-closo-hexaborate [P(C6H5)4][B6H6I]

1994 ◽  
Vol 49 (12) ◽  
pp. 1809-1812 ◽  
Author(s):  
W. Preetz ◽  
D. Sonnak
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structure of [P(C6H5)4][B6H6I] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1 with a = 7.5137(9), b = 12.623(2), c = 13.6363(13) Å, α = 87.787(13)°, β = 83.836(13)°, γ = 88.156(10)°. The additional H atom could be refined with B-H distances of 1.13 to 1.31 A above one of the facettes of the B6 octahedron opposite to the I substituent.

Kristallstruktur von β-VCl2(N3S2). Synthese und Kristallstruktur von [VCl(N3S2)(Pyridin)2]2·2 CH2Cl2, einem Cyclothiazenokomplex mit Vanadium(IV)/Crystal Structure of β-VCl2(N3S2). Synthesis and Crystal Structure of [VCl(N3S2)(pyridine)2]2·2 CH2Cl2, a Cyclothiazeno Complex with Vanadium (IV)

1986 ◽  
Vol 41 (11) ◽  
pp. 1420-1425 ◽  
Author(s):  
Ruth Christophersen ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Polymer Chains ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Metal Atoms ◽  
The Difference

Abstract β-VCl2(N3S2) was obtained by sublimation. It represents a new modification compared to the known α-VCl2(N3S2) which can be obtained from solution. Its crystal structure was determined by X-ray diffraction (864 observed reflexions, R = 0.034). Crystal data: triclinic, space group P1̄, Z = 2, a = 570.0, b = 779.9, c = 735.3 pm , α = 90.85°, β = 108.26°, y = 98.77°. Both modifications consist of polymer chains in which the vanadium atoms are linked alternatively by chloro and nitrogen bridges. The packing of the chains is rather similar, the only difference being that in β-VCl2(N3S2) the chains are rotated by 11° as compared to the orientation in α-VCl2(N3S2). The difference of the two modifications also shows up in the slightly different IR spectra. By reduction of VCl2(N3S2), dissolved in CH2Cl2/pyridine, with H2S, zinc or PPh3, the cyclothiazeno complex [VCl(N3S2)(pyridine)2]2·2 CH2Cl2 was obtained. It crystallizes in the monoclinic space group P 21/c, Z = 4, a = 1010.4, b = 917.3, c = 1967.8 pm, β = 103.03° (structure determination with 649 observed reflexions. R = 0.081). In this vanadium(IV) compound the metal atoms are part of planar VN3S2 rings as found in the VCl2(N3S2) modifications. The two vanadium atoms of the centrosymmetrical dimer are linked via one nitrogen atom of each of the VN3S2 rings; the resulting V2N2 ring is coplanar with the two VN3S2 rings.

Darstellung, Reaktionen und Kristallstrukturen von (Me3NCH2Ph)2 Fe2I6 und Fe2I4(SPPh3)2 · PhMe (Ph = C6H5, Me = CH3) / Preparation, Reactions, and Crystal Structure of (Me3NCH2Ph)2Fe2I6 and Fe2I4(SPPh3)2 · PhMe (Ph = C6H5, Me = CH3)

1988 ◽  
Vol 43 (3) ◽  
pp. 289-294 ◽  
Author(s):  
Wolfgang Saak ◽  
Detlev Haase ◽  
Siegfried Pohl
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Donor Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Molar Ratios

The reaction of FeI2, with (Me3NCH2Ph)I in CH2Cl2 and with Ph3PS in toluene (molar ratios 1:1) yields (Me3NCH2Ph)2Fe2I6 (1) and Fe2I6(SPPh3)2·C6H5CH3 (2), respectively. The structures of 1 and 2 were determined from single crystal X-ray diffraction data. 1 crystallizes in the monoclinic space group P21/n with a = 895.7(2), b = 1400.5(2), c = 1360.6(3) pm. β = 95.82(2)°, Z = 2. The anion of 1, Fe2I62-, has edge-sharing double-tetrahedra. The bridging and terminal F e - I bond lengths were found to be 269.9/270.7 and 260.3/258.6 pm, respectively (Fe-Fe: 358.2 pm). 2 crystallizes in the triclinic space group P1̄ with a = 987.6(1), b = 1119.3(1), c = 1159.4(1) pm, α = 101.10(1), β = 99.15(1), γ = 102.83(1)°, Z = 1. The molecules of 2 consist of centrosymmetric dinuclear Fe2I2 units (like for Fe2I62- in 1), with F e - I distances of 266.4 and 273.4 pm. The distorted tetrahedra around Fe are completed by an iodide ion (Fe-I: 256.9 pm) and Ph3PS with the sulfur as donor atom. The Fe-Fe distance was found to be 339.7 pm.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

Darstellung von Mononitropentahydrohexaborat(2-) und Kristallstruktur von M2[B6H5(NO2)], M = K, Cs / Preparation of Mononitropentahydrohexaborate(2—) and Crystal Structure of M2[B6H5(NO2)], M = K, Cs

1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.

Crystal Structure and Vibrational Behaviour of Aqua Di(saccharinato)di(nicotinamide)copper(II)

2002 ◽  
Vol 57 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Beatriz S. Parajón-Costaa ◽  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Eduardo E Castellano
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of [Cu(sac)2(nic)2(H2O)] (sac = saccharinate anion; nic = nicotinamide) has been determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group C2/c with Z = 4 and the Cu(II) ion presents a CuN4O square pyramidal coordination. Some comparisons with related structures are made and the most important features of its IR spectrum were also discussed.

Anionische Komplexe [Mo2(O2CPh)4X2]2⊖ mit X = N3, Cl, Br. Die Kristallstruktur von (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 / Anionic Complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, Cl, Br. The Crystal Structure of (PPh4)2[Mo2(O2C-Ph)4Cl2] · 2CH2Cl2

1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Diffraction Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Anionic Complexes

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

The crystal structure of dibutyl-bis(pentamethylenedithiocarbamato)tin(IV)

1986 ◽  
Vol 51 (11) ◽  
pp. 2521-2527 ◽  
Author(s):  
Jan Lokaj ◽  
Eleonóra Kellö ◽  
Viktor Kettmann ◽  
Viktor Vrábel ◽  
Vladimír Rattay
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Coordination Polyhedron ◽  
Crystal And Molecular Structure ◽  
Distorted Octahedron ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal and molecular structure of SnBu2(pmdtc)2 has been solved by X-ray diffraction methods and refined by a block-diagonal least-squares procedure to R = 0.083 for 895 observed reflections. Monoclinic, space group C2, a = 19.893(6), b = 7.773(8), c = 12.947(8) . 10-10 m, β = 129.07(5)°, Z = 2, C20H38N2S4Sn. Measured and calculated densities are Dm = 1.38(2), Dc = 1.36 Mg m-3. Sn atom, placed on the twofold axes, is coordinated with four S atoms in the distances Sn-S 2.966(6) and 2.476(3) . 10-10 m. Coordination polyhedron is a strongly distorted octahedron. Ligand S2CN is planar.

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