scholarly journals Synthese und Kristallstruktur von (PPh4)2Te4 / Synthesis and Crystal Structure of (PPh4)2Te4

1991 ◽  
Vol 46 (8) ◽  
pp. 1015-1019 ◽  
Author(s):  
Hans Wolkers ◽  
Bernhard Schreiner ◽  
Rüdiger Staffel ◽  
Ulrich Müller ◽  
Kurt Dehnicke

(PPh4)2Te4 has been prepared by the reaction of Na2Te3 with PPh4Cl in DMF solution in the presence of MnCl2 or FeCl2. The compound forms dark red crystals, which were characterized by IR spectroscopy as well as by an X-ray crystal structure determination (6109 observed independent reflections, R = 0.030). Crystal data: triclinic, space group PĪ, Z = 2, a = 1046.7(2), b = 1130.1(2), c = 1967.8(4) pm, α = 93.63(3), β = 90.43(3), γ = 108.89(3)° at —60 °C. The cations are grouped in pairs (PPh4+)2 around inversion centres, each pair being surrounded by eight Te42- ions, arranged as in the CsCl type lattice. The chain-like Te42- ions have no close contacts with one another.

1990 ◽  
Vol 45 (10) ◽  
pp. 1393-1397 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke

[VCl2(15-crown-5)]+[VOCl4]- has been prepared by the reaction of VCl4 with 15-crown-5 in acetonitrile solution in the presence of water, forming black-brown single crystals. They were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1530 observed unique reflexions, R = 0.052. Lattice dimensions at -120°C: a = 1128.5(4), b = 1063.3(3), c = 1680(1) pm. The compound forms ions, in which the cation contains vanadium(+III), which is seven coordinate by the five oxygen atoms of the crown ether molecule and by two chlorine atoms in axial positions of a pentagonal bipyramide. The [VOCl4]- anion contains vanadium (+V) with approximately tetragonal symmetry


1990 ◽  
Vol 45 (8) ◽  
pp. 1210-1212 ◽  
Author(s):  
Dieter Fenske ◽  
Gerhard Baum ◽  
Hans-Walter Swidersky ◽  
Kurt Dehnicke

[OsCl4(CH3CN)2] · 1/2CH3CN has been prepared by the reaction of OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The compound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N-atoms of the ciscoordinated acetonitrile molecules. The included CH3CN molecules are disordered in two positions.


1985 ◽  
Vol 40 (4) ◽  
pp. 562-564 ◽  
Author(s):  
Abdulalah T. Mohammed ◽  
Ulrich Muller

(PPh4)2[Sb2Br8] can be prepared from SbBr3 and PPh4Br in CH2Br2 or from Sb2S3, PPh4Br and HBr in 1,2-dichloroethane. Its crystal structure was de­termined with X-ray diffraction data (2764 observed reflexions, R = 0.039). Crystal data: triclinic, space group P1̄, a = 1024.9. b = 1127.1, c = 1282.4 pm, α = 111.80, β = 94.52, γ = 106.92°, Z = 1. The centrosymmetric [Sb2Br8]2- ions consist of two square pyramids sharing a basal edge. The cations are grouped to (PPh4+)2 pairs similarly as in (PPh4)2[As2Cl8]; although the latter compound has a comparable general crystal packing, it is not isotopic. IR and Raman spectral data are reported.


1998 ◽  
Vol 53 (7) ◽  
pp. 774-776 ◽  
Author(s):  
Mitra Ghassemzadeh ◽  
Kioumars Aghapoor ◽  
Bernhard Neumiiller

T etrakis-μ-acetato-bis(acetonitrile-N )-dicopper( II) bisacetonitrile (1) was syn thesized and characterized by IR spectroscopy and by an X-ray structure determination [Space group P21/n, Z = 2, lattice dimensions at - 70 °C: a = 1064.2(1), b = 1018.4(1), c = 1088.3(1) pm, β = 101.59(1)°, R1 = 0.048]. A ccording to the structural data the blue compound consists of centrosymmetric dimers [Cu2(OAc)4(NCMe)2] and noncoordinated acetonitrile molecules.


2013 ◽  
Vol 634-638 ◽  
pp. 2600-2604
Author(s):  
Shao Wei Tong ◽  
Jian Guo ◽  
Wen Dong Song ◽  
Jing Bo An

A new coordination polymer based on cadmium nitrate and 2-(4-pyridyl-1H-benzimidazole- 5,6-dicarboxylate (H2pbd) , namely [Cd( pbd)2•(H2O)2]n•n(H2O)2, have been synthesized under hydrothermal conditions and characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction. The crystal of the complex crystallizes in triclinic, space group P-1 with a = 7.7200 Å, b = 8.1029Å, c = 13.0801Å, α= 96.1270(10) º, β = 102.1280(10)º, γ= 112.479(2) º, V = 723.15(12) Å3, Z =1, C28 H22 Cd N6 O12 and F(000) = 376.0. The H2pbd ligands links the Cd(II) atoms into a double stranded chain.


1989 ◽  
Vol 44 (4) ◽  
pp. 495-498 ◽  
Author(s):  
Wolfgang Hiller ◽  
Eva Hartmann ◽  
Kurt Dehnicke

The title compound has been prepared by the reaction of FeCl3 with N, N, N′-tris(trimethylsilyl) benzamidine in CH2Cl2 solution as dark red, moisture-sensitive crystals. The complex was characterized by its IR spectrum as well as by an X-ray structure determination.Crystal data: space group P21/n, Z = 2 (1178 observed independent reflexions, R = 0.089). Lattice dimensions (20 °C): a = 1240.2(2), b = 645.7(3), c = 1779.7(3) pm, β = 91.31(2)°. The compound forms centrosymmetric molecules, in which the iron atoms are members of two fused planar heterocycles with the NN group as the com m on edge. The NN bond length (142.5(9) pm) is very close to the NN bond length of hydrazine.


1990 ◽  
Vol 45 (8) ◽  
pp. 1128-1132 ◽  
Author(s):  
Ulrich Müller ◽  
My-Linh Ha-Eierdanz ◽  
Gertrud Kräuter ◽  
Kurt Dehnicke

(PPh4)4[Cu2Se14] has been prepared by the reaction of a lithium polyselenide solution in DMF with CuCl at 120 °C in the presence of PPh4Br. The compound forms black crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P 21, Z = 2, 2690 observed unique reflexions, R = 0.095. Lattice dimensions at 19 °C: a = 2139.5(9), b = 1611.7(3), c = 1365.1(3) pm, β = 93.54(3)°. The compound consists of PPh4+ and [Cu2Se14]4- ions, in which the two copper atoms are bridged by an Se52- chain. One of the Cu atoms is a member of a CuSe4 ring, the other one of a CuSe5 ring; the coordination at each Cu atom is trigonal-planar.


1991 ◽  
Vol 46 (3) ◽  
pp. 307-314 ◽  
Author(s):  
Evamarie Hey-Hawkins ◽  
Hans Georg von Schnering

NaSi reacts with MoCl5 and 15-crown-5 in toluene with reduction of Mo(V) to Mo(IV). Work-up in DME yields MoCl4(DME)· 15-crown-5 (1). MoCl4(DME) (2) is prepared more conveniently from MoCl5/DME. 1 and 2 were characterized spectroscopically and by X-ray structure determination. Crystal data: 1, space group P212121 (No. 19), Z = 4, 2765 observed independent reflexions, R = 0.026, cell dimensions (110 K): a = 16.292(4), b = 12.884(3), c = 10.452(2) Å. 2, space group I4̄2d (No. 122), Z = 8, 558 observed independent reflexions, R = 0.037, cell dimensions (292 K): a = b = 9.562(2), c = 23.777(6)Å. The MoCl4(DME) molecule of 1 and 2 forms a distorted octahedron. There are four non-coordinating 15-crown-5 molecules present in the unit cell of 1. The UV/VIS spectrum and the magnetic properties of 2 are discussed.


1987 ◽  
Vol 42 (4) ◽  
pp. 410-414 ◽  
Author(s):  
Aida El-Kholi ◽  
Ruth Christophersen ◽  
Ulrich Müller ◽  
Kurt Dehnicke

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.


2013 ◽  
Vol 781-784 ◽  
pp. 571-575
Author(s):  
Liang Jun Gao ◽  
Wen Dong Song

A new coordination polymer based on cobalt nitrate and 2-4-pyridyl-1H-benzimidazole- 5,6-dicarboxylate (H2pbd), namely [Co (pbd)2·(H2O)2]n·n (H2O)2, have been synthesized under hydrothermal conditions and characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffraction. The crystal of the complex crystallizes in triclinic, space group P-1 with a=7.6708(6)Å, b=8.0009(8)Å, c=12.8348(12)Å, α=96.4040(10) o, β=102.9480(10) o, γ=112.142(2) o, V=694.11(11)Å3, Z=1, C28H22CoN6O12 and F(000)=376.0. The H2pbd ligand links the Co (II) atoms into a double stranded chain.


Sign in / Sign up

Export Citation Format

Share Document