Cyclo-thiazenokomplexe von Vanadium(V) Die Kristallstruktur von (AsPh4)2[V(N3)3(N3S2)]2 · CH2Cl2 / Cyclo-thiazeno Complexes of Vanadium(V) The Crystal Structure of (AsPh4)2[V(N3)3(N3S2)]2 · CH2Cl2

1984 ◽  
Vol 39 (12) ◽  
pp. 1686-1695 ◽  
Author(s):  
Jürgen Hanich ◽  
Magda Krestel ◽  
Ulrich Müller ◽  
Kurt Dehnicke ◽  
Dieter Rehder
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Nmr Spectra ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Nmr Data ◽  
Donor Acceptor

An improved synthesis for [VCl2(N3S2)]∞, was found in the reaction of VOCl3 with (NSCl)3; when the reaction is performed in H2CCl2 and (NSCl)3 is used in excess, the thiazyl-solvate [VCl2(N3S2) · NSCl]2 is obtained. [VCl2(N3S2)] reacts with AsPh4Cl to form (AsPh4)2[VCl3(N 3S2)]2; this reacts with AgN3 in CH2Cl2 suspension to yield (AsPh4)2[V (N3)3(N3S2)]2 · CH2Cl2. The compounds were characterized by their IR and 51V NMR spectra. The latter are compared with new 51V NMR data for [VO2Cl2]⊖ and [VOCl4]⊖ ; a decrease of 51V shielding in the order [VO2Cl2]⊖ > [VOCl4]⊖ > [VX3(N3S2)]22⊖ (X - N3 > Cl) is found, which is interpreted in terms of increasing polarizability of the ligands and of ring contributions to the extreme deshielding observed with the thiazenovanadates.The crystal structure of (AsPh4)2[V(N3)3(N3S2)]2 · CH2Cl2 was determined from X-ray diffraction data (1496 observed reflexions, R = 0.058). It crystallizes in the triclinic space group P 1̄ with one formula unit per unit cell and with the lattice constants a - 1087, b = 1317, c = 1350 pm, α = 58.8, β = 85.9, γ = 68.0°. The structure consists of AsPh4⊕ ions, CH2Cl2 molecules and centrosymmetric [V(N3)3(N3S2)]22⊖ anions. In the latter. N3S2 ligands are bonded to the V atoms in a chelate manner with short V = N bonds (189 and 172 pm) forming planar VN3S2 rings. The dimerization is accomplished by V -N donor-acceptor interactions (224 pm) involving one N atom of each VN3S2 ring. The vanadium coordination number of 6 is com pleted by three azido groups with V -N bond distances of 200 to 204 pm.

scholarly journals Chemie polyfunktioneller Moleküle, 106. Kupfer(I)halogenid — Komplexe des Bis(diphenylphosphino)amins / Chemistry of Polyfunctional Molecules, 106. Copper(I) Halide Complexes of Bis(diphenylphosphino)amine

1990 ◽  
Vol 45 (12) ◽  
pp. 1657-1668 ◽  
Author(s):  
Jochen Ellermann ◽  
Falk A. Knoch ◽  
Klaus J. Meier
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Conductivity Data ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
H Nmr ◽  
Nmr Data ◽  
Halide Complexes

Reaction of Copper(I) halides CuX (X = Cl, Br, I) in methanol with bis(diphenylphosphino)amine (dppa, 1) yields complexes [Cu3X2(dppa)3]X (X = Cl, Br, I: 2a–c). The derivates [Cu3X2(dppa)3]PF6 (2a′–c′) have been synthesized by metatheses of 2a–c with NH4PF6. The IR, Raman, 31P{1H} NMR, 1H{31Ρ} NMR, 13C{1H} NMR spectra, and FD mass spectra as well as the conductivity data are reported and discussed together with the X-ray crystal structure of 2a · 5 CH3OH. The structure consists of the trinuclear cations [Cu3Cl2(dppa)3]+, distorted tetrahedral anions [Cl( · · · HOCH3)4]- and molecules of methanol of crystallization, hydrogen bridged to the solvated anions. The Cu3Cl2 core of the cations corresponds closely to a trigonal bipyramid with the copper atoms in the equatorial and the chlorine atoms in the axial positions. The colourless prisms of 2a · 5 CH3OH crystallize in the triclinic space group P1̅, with the lattice constants a = 1368.0(4); b = 1486.7(4); c = 2036.8(10) pm; α = 74.52(3); β = 74.73(3); γ = 82.26(2)°. Raman and 31P{1H} NMR data of the complexes [Cu(X)dppm]4 (dppm = (C6H5)2PCH2P(C6H5)2; X = Br, I) described earlier suggest that these compounds should also be formulated as [Cu3X2(dppm)3]X (4b, c).The Raman spectra of the cations of 2a–c, 2a′–c′ and 4a–c show bands at 165 (X = Cl), 145 (X = Br) and 125 (X = I) cm-1, which can be assigned to the symmetric (XCu3X) stretching mode of the XCu3X unit.

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)

Structure refinement and crystal chemistry of tokkoite and tinaksite from the Murun massif (Russia)

2017 ◽  
Vol 81 (2) ◽  
pp. 251-272 ◽  
Author(s):  
M. Lacalamita ◽  
E. Mesto ◽  
E. Kaneva ◽  
F. Scordari ◽  
G. Pedrazzi ◽  
...  
Keyword(s):  
Exchange Reaction ◽  
Diffraction Data ◽  
Structure Refinement ◽  
Local Stress ◽  
Geometrical Parameters ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Mössbauer Analysis

AbstractThe structures of tokkoite, K2Ca4[Si7O18OH](OH,F) and tinaksite, K2Ca2NaTi[Si7O18OH]O from the Murun massif (Russia) were refined from single-crystal X-ray diffraction data in the triclinic space group P1̄. Average crystallographic data are a ≈ 10.423, b ≈ 12.477, c ≈ 7.112 Å, α ≈ 89.92°, β ≈ 99.68°, γ ≈ 92.97°, V ≈ 910.5 Å3 for tokkoite; a ≈ 10.373, b ≈ 12.176, c ≈ 7.057 Å, α ≈ 90.82°, β ≈ 99.22°, γ ≈ 92.80°, V ≈ 878.5 Å3 for tinaksite. The substantial similarities between the geometrical parameters of the tokkoite and tinaksite structures led us to conclude that the two minerals are isostructural. However, major differences of tokkoite with respect to tinaksite are larger lattice constants, especially concerning the b parameter, longer <M–O> distances, especially <M1–O>; larger values of the M1–M3 and O20–O2 bond lengths, and a stronger distortion of the M1 polyhedron. Mössbauer analysis showed that significant trivalent iron is present, VIFe3+ 40.0(7)% in tokkoite and 12.8(3)% in tinaksite. It is confirmed that 2Ca(M1+M2)2+ + (F,OH)(O20)–↔ Ti(M1)4+ + Na(M2)+ + O(O20)– is the exchange reaction that describes the relation between tokkoite and tinaksite. In addition, this exchange reaction causes local stress involving mainly the M1 site and its interaction with the M2 and M3 sites.

(Ph4P)2 Mn2Br6 und (Ph3PCH2Ph)2Mn2I6 (Ph = C6H5) / (Ph4P)2Mn2Br6 and (Ph 3PCH2Ph)2Mn2I6 (Ph = C6H5

1988 ◽  
Vol 43 (2) ◽  
pp. 171-174 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Peter Stolz
Keyword(s):  
Single Crystal ◽  
Diffraction Data ◽  
Unit Cell ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
The Mean ◽  
The Difference

(Ph4P)2Mn2Br6 (1) and (Ph3PCH2Ph)2Mn2I6 (2) were prepared from the reaction of manganese dihalide with the corresponding phosphonium halide in CH2Cl2.The structures of 1 and 2 were determined from single crystal X-ray diffraction data.Both compounds crystallize in the triclinic space group P 1 with one formula unit per unit cell.1:a = 998.1(1), b = 1005.7(1), c = 1313.3(2) pm, α = 108.51(1), β = 94.25(1), γ = 100.36(1)°.2: a = 1058.6(2), b = 1236.3(2), c = 1248.4(3) pm, α = 63.53(1), β = 74.15(1), γ = 74.65(1)°.The structures of 1 and 2 exhibit discrete, dimeric anions formed by the fusion of two identical tetrahedral-like units with a common halogen-halogen edge. The mean Mn-Hal bond lengths were found to be 251.8 pm (Mn-Br) and 272.2 pm (Mn-I). The difference between the bridging and terminal Mn-Hal bond lengths is about 12-13 pm in both compounds

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

Die Kristallstruktur von Tricarbonyl(2.6-di-tert-butyl-pyridin)chrom(0) bei 200 K / Crystal Structure of Tricarbonyl(2,6-di/tert-butyl-pyridine)chromium(0) at 200 K

1984 ◽  
Vol 39 (2) ◽  
pp. 213-216 ◽  
Author(s):  
Roland E. Schmidt ◽  
Werner Massa
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Pyridine Ring ◽  
Chromium Atom ◽  
Methyl Groups ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lattice Constants ◽  
Tert Butyl

Based on single crystal X-ray diffraction data the crystal structure of tricarbonyl(2,6-dwmbutyl- pyridine)chromium(0) has been determined at 200 K: space group P 21/n, Z = 4, lattice constants a = 680.6(5), b - 1383.3(10), c = 1763.0(16) pm, β = 96.53(8)°, refinement to Rw - 0.048 for 1672 independent reflections with FO > 2 σ. The chromium atom is η6π6- bonded to the essentially planar pyridine ring (Cr-C: 219-222 pm, Cr-N: 221 pm). The CO ligands show “eclipsed” orientation with respect to the 2, 4 and 6 position of the pyridine ring. Two CO groups fit into the gaps formed by two methyl groups of the tert-butyl substituents in 2 and 6 position, respectively. The results are discussed in context with related arene and λ3-phosphorine complexes

Crystal Structure of 3Ni(N03)2.16C6 H5NH2

1990 ◽  
Vol 45 (9-10) ◽  
pp. 1185-1189
Author(s):  
Michael Mahr ◽  
Inge Pabst ◽  
Konrad G. Weil
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Ion Pairs ◽  
X Ray Diffraction ◽  
Nickel Ion ◽  
Ionic Solutions ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Contact Ion Pairs

Abstract The Compound 3Ni(NO3)2 -16C6H5NH2 was obtained by crystallization from solutions of Ni(NO3)2 • 6C6H5NH2 -2H2O in aniline. Its crystal structure was determined by single crystal X-ray diffraction. The crystals are triclinic, space group P1 with lattice constants a = 985.2 pm, ft = 1004.5 pm and c = 2514.3 pm, a = 96.34°, ß = 92.63° and y = 89.82°. The structure shows units of four aniline molecules and two slightly distorted nitrate ions in the coordination sphere of each nickel ion. These units are similar to contact ion pairs in concentrated ionic solutions.

Die Kristallstrukturen von PPh4[SnCl3] und PPh4[SnBr3]/ The Crystal Structures of PPh4[SnCl3] and PPh4[SnBr3]

1982 ◽  
Vol 37 (9) ◽  
pp. 1122-1126 ◽  
Author(s):  
Ulrich Müller ◽  
Norbert Mronga ◽  
Christina Schumacher ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Vibrational Spectra ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
The Ideal

AbstractPPh4[SnCl3] and PPh4[SnBr3] were prepared by reaction of PPh4X with SnX2 in CH2X2 solutions (X - Cl, Br). The vibrational spectra of the [SnX3]⊖ ions show three SnX3 stretching frequencies, which is caused by deviations from the ideal C3v symmetry. In the crystal structure determinations these deviations show up by slightly different Sn-X bond lengths which are explained by differing hydrogen bridges to phenyl-H atoms. The isotypic crystal structures of both compounds were determined and refined from X-ray diffraction data (R values: 0.042 and 0.034). Although triclinic (space group P1̄), the structures are closely related to the tetragonal AsPh4[RuNCl4] structure type. Very pure SnBr2 is prepared by the reaction of PPh4[SnBr3] with AlBr3 in CH2Br2 solution.

Cyclothiazeno-Vanadiumdibromid, VBr2(N3S2) / Cyclo-Thiazeno Vanadium Dibromide, VBr2(N3S2)

1985 ◽  
Vol 40 (11) ◽  
pp. 1457-1462 ◽  
Author(s):  
Jürgen Hanich ◽  
Wolfgang Willing ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

VBr2(N3S2) was synthesized by reaction of VCl2(N3S2) with Me3SiBr. It reacts with PPh4Br in dibromomethane solution to form (PPh4)2[VBr3(N3S2)]2. The compounds were characterized by their IR and 51V NMR spectra. The crystal structure of VBr2(N3S2) was determined by X-ray diffraction (2060 reflexions. R = 0.114). Crystal data: triclinic, space group P1̄, a = 586.4, b = 794.2, c = 744.6 pm. α - 89.25, β - 108.58, γ = 99.67°. Z = 2. The vanadium atoms form planar, six-membered rings wjith the N3S2 groups, with short VN distances (172 and 185 pm). Bromine- bridged dimers are associated via V−N links to form chains in a similar way as in some tetrahalides. The structure is similar to that of VCl2(N3S2), but the chains are rotated by 17° along their axes.

Crystal structure and spectra of the mixed-ligands complex 1-(2-thenoyl)-2-(2,2′-dipyridyl methylene)hydrazino-acetato lead (II)

1994 ◽  
Vol 209 (12) ◽  
Author(s):  
P. C. Christidis ◽  
I. A. Tossidis ◽  
C. A. Hondroudis
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Title Compound ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Mixed Ligands

AbstractThe crystal structure of the title compound has been determined from three-dimensional X-ray diffraction data. The crystals are triclinic, space group

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