Notizen: Synthese und Kristallstruktur von [OsCl4(CH3CN)2] · 1/2 CH3CN / Synthesis and Crystal Structure of [OsCl4(CH3CN)2] · 1/2CH3CN

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.

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.


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.


1993 ◽  
Vol 48 (2) ◽  
pp. 224-226 ◽  
Author(s):  
Jörg Lorberth ◽  
Reiner Dorn ◽  
Werner Massa ◽  
Sigrid Wocadlo

AbstractThe title compound was prepared by reacting gallane etherate H3Ga · OEt2 at -40 °C in Et2O with diethylamine upon warming to room temperature for several hours. It forms white crystals from ether solution which were identified by X-ray structure determination. Space group C 2/c, Z = 4; 930 observed unique reflections, R/wR = 0.0482/0.0450. Lattice dimensions at 193 K: a = 1292.9(3), b = 721.1(2), c = 1443.1(2) pm; β = 92.81(2)°. The structure reveals a centrosymmetric dimeric molecule with a planar square (GaN)2 fourmembered ring: average distance Ga - N = 201.7 pm, Ga ··· Ga 284.5(2) pm.


1990 ◽  
Vol 45 (5) ◽  
pp. 695-700 ◽  
Author(s):  
Gertrud Kräuter ◽  
MyLinh Ha-Eierdanz ◽  
Ulrich Müller ◽  
Kurt Dehnicke

(PPh4)2[Mn(Se4)2] has been prepared by the reaction of a lithium poiyseienide solution in DMF with MnCl2.4H2O at 100 °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 P21, Z = 4, 3622 observed unique reflexions, R = 0.076. Lattice dimensions at 19 °C: a = 1017.2(3), b = 1405.9(3), c = 3427.7(8) pm, β = 92.04(2)°. The compound consists of PPh4⁺ and [Mn(Se4)2]2- ions, in which the manganese atom is tetrahedrally surrounded by four selenium atoms of two chelating Se42- units. The structure is isotypical with that of (PPh4)2[Zn(Se4)2].


1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2


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


1991 ◽  
Vol 46 (1) ◽  
pp. 63-67 ◽  
Author(s):  
Volker Müller ◽  
Kurt Dehnicke ◽  
Dieter Fenske ◽  
Gerhard Baum

{K-[2 2 2]-Crypt}2Se7·H20 has been prepared by the reaction of a solution of potassium polyselenide in dimethylformamide at room temperature as black crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/n, Z = 4, 5055 observed unique reflexions, R = 0.103. Lattice dimensions at 20 °C: a = 1435(1), b = 1320(1), c = 2966(2) pm, β = 102.50(6)° The heptaselenide ion represents approximately part of a helical chain of polymeric selenium.


1997 ◽  
Vol 52 (7) ◽  
pp. 810-814 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Kurt Merzweiler ◽  
Clemens Bruhn

Abstract The reaction of the phosphido-bridged metal carbonyl [FeRh(CO)6(μ-PBut2)] (1) with dppm [dppm = bis(diphenylphosphino)methane] leads to the heterobimetallic complex [FeRh(μ-CO)(CO)3(μ-PBut2)(μ-dppm)] (2) in good yields. The molecular structure of 2 was determined at room temperature [triclinic, space group P1̄, a = 9.509(6), b = 13.637(5), c = 14.926(8) Å, α = 81.38(4), β = 82.75(4), γ = 71.25(4)°]. The compound acts as a homogeneous catalyst precursor in the hydroformylation reaction of ethylene, but it decomposes during this process.


1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.


1989 ◽  
Vol 44 (9) ◽  
pp. 999-1002 ◽  
Author(s):  
Wolfgang Hiller ◽  
Joachim Strähle ◽  
Alfred Zinn ◽  
Kurt Dehnicke

Ph—C(NSiMe3)2AuCl2 has been prepared by the reaction of N,N,N′-tris(trimethylsilyl)-benzamidine with AuCl3 in CH2Cl2 suspension, forming orange-red crystals, which were characterized by an X-ray structure determination.Space group P21/n, Z = 4, 2358 observed independent reflexions, R = 0.028. Lattice dimensions (20°C): a = 695.9(3); b = 1576.1(3); c = 1830.9(3) pm; β = 94.27(3)°. The compound forms monomeric molecules, in which the gold atom is in a square planar arrangement of the two nitrogen atoms of the benzamidinato chelate (Au—N 201.6(7); 203.3(6) pm) and by two chlorine atoms (Au—Cl 227.9(3); 228.5(2) pm).


Sign in / Sign up

Export Citation Format

Share Document