Structural Aspects of V2( µ;-S2)2(S2CNR2)4 Complexes: the X-Ray Crystal Structure of V2( µ;-S2)2(S2CNEt2)4.2CHBr3

1992 ◽  
Vol 45 (5) ◽  
pp. 897 ◽  
Author(s):  
ERT Tiekink ◽  
XF Yan ◽  
CG Young
Keyword(s):  
Crystal Structure ◽  
Vanadium Atom ◽  
Single Bond ◽  
Dimeric Complex ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Metal Metal ◽  
Structural Aspects

Brown V2(p-S2)2(S2CNEt2)4 is produced upon reaction of [vs4]3- with (Et2NCS2)2, in a synthesis similar to that described for V2( �-S2)2(S2CNBui2)4 ( Halbert , T. R., Hutchings, L. L., Rhodes, R., and Stiefel , E. I., J. Am. Chem. Soc., 1986, 108, 6437). Crystals of V2( �;-S2)2(S2CNEt2)4.2CHBr3 are orthorhombic and belong to space group Pbca , with a 10.909(2), b 20.492(2), c 20.471(2) � , V 4576.2 �3, and Z 4 dimers . The structure was solved by Patterson and Fourier methods and refined by using 1189 reflections to final R 0.061 ( Rw 0.059). The vanadium(IV) atoms in the dimeric complex are bridged by two �-k2S,S′: k2S,S′-S22- ligands [S(1)-S(2) 2.00(1) �] and a metal-metal single bond [V-V 2.900(6) �]. Each vanadium atom is further coordinated by two bidentate dithiocarbamate ligands whose arrangement defines a meso isomer with Λ and Δ configurations at the vanadium centres. This Λ Δ diastereomer differs from the Λ Λ -ΔΔ racemate structurally characterized in the case of V2(�-S2)2(S2CNBui2)4 but is the same as that found for the molybdenum(v) dication in [Mo2( �S2)2(S2CNEt2)4] (BF4)2.2CHBr3 ( Kocaba, T., Young, C. G., and Tiekink , E. R. T., Inorg. Chim. Acta, 1990, 174, 143).

Crystal structure and chemistry of natural kutinaite from Černý Důl, Krkonoše, Czech Republic

2015 ◽  
Vol 79 (5) ◽  
pp. 1099-1109 ◽  
Author(s):  
Luca Bindi ◽  
Emil Makovicky
Keyword(s):  
Crystal Structure ◽  
Czech Republic ◽  
Metal Contacts ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Metal Metal ◽  
Crystal Structure And Chemistry

AbstractWe have characterized the crystal structure of natural kutinaite, a rare mineral from the ores of Černý Důl, Czech Republic, by single-crystal X-ray diffraction and chemical analysis. We found that the structure of natural kutinaite is not identical to that of synthetic Cu14Ag6As7, previously reported to be cubic, space group Pm3m. Although topologically similar, the structure of natural kutinaite is indeed tetragonal, space group P4/mmm, with cell parameters: a = 11.789(2), c = 11.766(2) Å, V = 1635.5(4) Å3 and Z = 4. Electron microprobe analyses pointed to the (K,Tl)0.25Cu14Ag6As6.75 stoichiometry (Z = 4), or (K, Tl)Cu56Ag24As27 with Z = 16. The crystal structure of an untwinned crystal has been refined to R1 = 2.61%. It consists of clusters of eight edge-sharing tetrahedra of Cu, which alternate in a 3D chess-board manner with octahedral clusters of six Ag atoms. The latter are surrounded by triangularly coordinated copper in eight faces of a cuboctahedron. The last structure components are large cavities containing partly occupied (K,Tl) sites, coordinated by 18 Ag and As ligands. The structure is full of direct metal-metal contacts although As plays the role of anion, associating especially with copper.

Synthesis, Characterization and X-Ray Crystal Structure of {H2B(Me2C3N2H)2}MoIVO(S2PPrI2)

1994 ◽  
Vol 47 (3) ◽  
pp. 471 ◽  
Author(s):  
LJ Laughlin ◽  
JM Gulbis ◽  
ERT Tiekink ◽  
CG Young
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometric ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
R Value

Reaction of MoO (S2PPri2)2 and K{H2B(Me2C3N2H)2} in refluxing toluene produces green, diamagnetic, air-stable {H2B(Me2C3N2H)2}MoIVO(S2Ppri2)(1), which has been characterized by analytical, mass spectrometric, infrared and n.m.r. spectroscopic, and X-ray crystallographic techniques. Crystals of (1) are triclinic and belong to space group Pī , with a 10.289(1), b 13.601(2), c 8.737(1) Ǻ, α 94.31(1), β 107.71(1), γ 79.56(1)°, V 1145.2 Ǻ3 and Z 2. The structure was solved by Patterson and Fourier methods and refined by using 3631 reflections to a final R value of 0.024 ( Rw 0.041). The five-coordinate square pyramidal complex is composed of apical terminal oxo [Mo-O(1) 1.658(2)Ǻ] and bidentate H2B(Me2C3N2H)2- and S2PPri2- ligands coordinated to molybdenum. Ferrocenium oxidation of (1) produces the mononuclear molybdenum(V) complex [{H2B(Me2C3N2H)2}MoVO(S2Ppri2)]+ ( e.p.r .: g 1.964, a(95,97Mo) 41.7×10-4cm-1, a(31P) 30.1×10-4 cm-1).

Darstellung, Reaktivität und Kristallstruktur von [(CO)3Mn(dppm)2(μ-S)Rh(CO)] / Synthesis, Reactivity and Crystal Structure of [(CO)3Mn(dppm)2(μ-S)Rh(CO)]

1992 ◽  
Vol 47 (5) ◽  
pp. 668-674 ◽  
Author(s):  
O. Heyke ◽  
G. Beuter ◽  
I.-P. Lorenz
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
Frame Structure ◽  
Dimeric Complex ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Group 2

The reaction of [(CO)3Mn(dppm)2Rh(CO)] (1) with H2S in dichloromethane yields [(CO)3Mn(dppm)2(μ-S)Rh(CO)] (2), which is characterized by IR, 31P{1H}, 1H, 13C{1H} nmr and mass spectra. The crystal structure of 2 was determined by X-ray diffraction: space group P21/n, Z = 4, a = 1232.6(3), b = 2558.8(4), c = 1640.8(2) pm, β = 97.74(2)°, R/Rw = 0.048/0.057. The dimeric complex shows A-frame structure possessing a bridging sulfur and a semibridging CO group. 2 cannot be oxidized to the corresponding SO2 bridged complex [(CO)3Mn(dppm)2(μ-SO2)Rh(CO)] (3). The reaction of 2 with SO2, however, yields the SO2 bridged complex [(CO)2Mn(dppm)2(μ-S)(μ-SO2)Rh(CO)] (5); in dichloromethane 2 is readily chlorinated to afford the salt [(CO)3Mn(dppm),(μ-S)RhCl]Cl (4).

Notizen: Die Kristallstruktur von KLiTe / The Crystal Structure of KLiTe

1993 ◽  
Vol 48 (12) ◽  
pp. 1835-1836 ◽  
Author(s):  
Horst Sabrowsky ◽  
Rolf-Dieter Hitzbleck ◽  
Petra Vogt
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

The crystal structure of KLiTe described earlier as a dark grey powder compound has been determined by X-ray diffraction of single crystals. Very hygroscopic KLiTe crystallizes in the tetragonal space group P4/nmm (Z = 2) with the cell parameters a = 483.0(1) and c = 770.4(2) pm. The structure was determined from 211 independent reflections by Patterson and Fourier methods (R = 0.013; wR = 0.013).

Synthese und Kristallstruktur von [N(PPh3)2][VCl3(N3S2)]·C7H8 / Synthesis and Crystal Structure of [N(PPh3)2][VCl3(N3S2)]·C7H8

1987 ◽  
Vol 42 (4) ◽  
pp. 410-414 ◽  
Author(s):  
Aida El-Kholi ◽  
Ruth Christophersen ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Subsequent Treatment ◽  
Vanadium Atom ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Chlorine Atoms ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

Abstract [N(PPh3)2][VCl3(N3S2)]·C7H8 is formed by the reaction of VCl2 (N3S2) with excess PPh3 in CH2C12 and subsequent treatment of the reaction mixture with toluene, as well as by the reaction of VCl2(N3S2) with [N(PPh3)2]Cl in CH2Cl2 in the presence of toluene. The compound forms red crystals, which have been characterized by IR spectroscopy. The crystal structure was determined by X-ray diffraction (1433 observed, independent reflexions, R = 0.070). Crystal data: mono-clinic, space group Cc, Z = 4, a = 994.1, b = 2148.0, c = 2055.2 pm, β = 90.03°. The compound consists of [N(PPh3)2]⊕ cations and [VCl3(N3S2)]⊖ anions, in which the vanadium atom is five-coordinated by threee chlorine atoms and two nitrogen atoms, and is part of a planar VN3S2 ring.

Preparation of Cr2(CO)8(NO)2 and X-ray crystal structures of Cr2(CO)8(NO)2 and Cr2(CO)9NO−. Stereochemical comparisons to Cr2(CO)102−

1991 ◽  
Vol 69 (12) ◽  
pp. 2136-2141 ◽  
Author(s):  
A. P. Masters ◽  
M. Parvez ◽  
T. S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Key Words ◽  
Crystal Structures ◽  
Quantitative Yield ◽  
Space Group ◽  
X Ray ◽  
Metal Metal ◽  
Chromium Carbonyl ◽  
The One

Cr2(CO)8(NO)2 (1) has been prepared and characterized, and the crystal structure determined, along with that of the related salt Cr2(CO)9NO− monoanion (2) as the CH2Cl2-solvated PPN+ salt (where PPN+ denotes the (PPh3)2N+ monocation). Both 1 and 2 possess a metal–metal bonded structure analogous to that of Mn2(CO)10 and the electronically equivalent Cr2(CO)102− dianion. Although Cr2(CO)8(NO)2 (1) is slowly formed in poor yield from Cr(CO)4NO− and Cr(CO)4NOBr, it can be prepared in an almost quantitative yield by the one-electron oxidation of the monoanion with trityl hexafluorophosphate. The slowness of the former reaction makes Cr(CO)4NO− useful as a two-electron reductant of organohalide bonds. Triclinic crystals of 1 incorporate two distinct molecules in die [Formula: see text] space group, although the geometries of each are almost identical. Triclinic crystals of monoanion (2) also belong to the [Formula: see text] space group. The Cr—Cr bond length is 3.00–3.02 Å in 1 and 2.995 Å in 2, compared to 2.904 Å for the central Mn—Mn bond in Mn2(CO)10. Key words: chromium nitrosyl, chromium carbonyl, X-ray crystal structure, metalate anion, metal–metal dimer.

Kristallstruktur von Na4OBr2 / Crystal Structure of Na4OBr2

1990 ◽  
Vol 45 (2) ◽  
pp. 105-106 ◽  
Author(s):  
Karin Hippler ◽  
Stephan Sitta ◽  
Petra Vogt ◽  
Horst Sabrowsky
Keyword(s):  
Crystal Structure ◽  
Structure Type ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Group I

The colourless compound Na4OBr2 has been prepared and its crystal structure determined by X-ray diffraction. Very hygroscopic Na4OBr2 crystallizes in the tetragonal space group I 4/mmm (Z = 2) with the cell parameters a = 452.1(3) and c = 1490.8(1) pm. The structure was solved from 267 symmetry independent reflections by Patterson and Fourier methods (R = 0.028; wR = 0.029). Na4OBr2 crystallizes in the anti-K2NiF4-structure type and is isotypic to Na4OI2 and K4OBr2 which have been described earlier.

Die Kristallstruktur von CsNaTe / The Crystal Structure o f CsNaTe

1996 ◽  
Vol 51 (11) ◽  
pp. 1576-1578 ◽  
Author(s):  
Karsten Fischer ◽  
Elisabeth Feldbaum -Möller ◽  
Petra Vogt ◽  
Michael Wachhold ◽  
Volker Winter ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

The crystal structure of CsNaTe has been determined by X-ray diffraction of single crystals. The hygroscopic CsNaTe crystallizes in the tetragonal space group P4/nmm (Z = 2) with the cell parameters a = 527.6(1) and c = 847.8(2) pm. The structure was determined from 237 independent reflections by Patterson and Fourier methods (R1 = 0.065; wR2 = 0.080).

The crystal structure of Hexakis(2-pyridone)copper(II) perchlorate

1975 ◽  
Vol 28 (12) ◽  
pp. 2615 ◽  
Author(s):  
D Taylor
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Equatorial Plane ◽  
Copper Atom ◽  
Tautomeric Form ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Axial Ligands

Crystals of hexakis(2-pyridone)copper(II) perchlorate, [Cu(C5H5NO)6] (ClO4)2, are monoclinic, a 9.453(2), b 10.492(3), c 17.794(4) Ǻ, β 95.57(2)�, space group P21/c with Z = 2. The structure was solved by Fourier methods using X-ray diffractometer data and refined by block-diagonal least-squares to convergence at R 0.037, Rw 0.044 for 3054 independent reflections. The octahedral coordination of the copper atom in the centrosymmetric cation is tetragonally distorted with Cu-O bond lengths of 1.922(2), 1.952(2) and 2.546(2) Ǻ. The ligands are in the pyridone tautomeric form and coordinate the copper atom through the exocyclic oxygen atoms. There are N-H...O bonding interactions between the ligands in the equatorial plane and the axial ligands (N...O distances of 2.781(3) and 2.894(3) Ǻ). The perchlorate ions (Cl-O, 1.412-1.436 Ǻ) are hydrogen-bonded to the N-H groups of the axial ligands (N...O 2.958 Ǻ.

Zur Komplexchemie der Alkalimetalle: Kristallstruktur von RbLiS / On the Complex Chemistry of the Alkali Metals: The Crystal Structure of RbLiS

1989 ◽  
Vol 44 (8) ◽  
pp. 893-895 ◽  
Author(s):  
Horst Sabrowsky ◽  
Karin Hippler ◽  
Rolf-Dieter Hitzbleck ◽  
Stephan Sitta ◽  
Alfred Thimm ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Alkali Metals ◽  
Double Layers ◽  
X Ray Diffraction ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Complex Chemistry

The colourless compound RbLiS has been prepared as described earlier (H. Sabrowsky, A. Thimm, and P. Vogt-Mertens, Z. Naturforsch. 40b, 1759 (1985)) and its crystal structure determined by X-ray diffraction. Very hygroscopic RbLiS crystallizes in the tetragonal space group P4/nmm (Z = 2) with the cell parameters a = 4.424(3) Å, c = 7.255(2) Å. The structure was solved from 1635 counter reflections (155 symmetry independent reflections) by Patterson and Fourier methods (R = 0.031; wR = 0.031).The structure is characterized by layers of ∞2[LiS4/4]-tetrahedrons separated by double-layers of Rb+ to form a PbFCl-type geometry.

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