Synthesis and Crystal Structure of [Cu2(OAc)4(NCMe)2] · 2MeCN

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. 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.


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.


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].


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


1996 ◽  
Vol 51 (9) ◽  
pp. 1359-1362 ◽  
Author(s):  
Frank Weller ◽  
Fritjof Schmock ◽  
Kurt Dehnicke

The title compound was prepared from Me3SiNPPh3 and an excess of titanium tetrachloride. It forms yellow-orange crystals, which were characterized by IR spectroscopy and by crystal structure determination. Space group P21/n, Z = 2; lattice dimensions at 20°C: a = 1189.2(1), b - 1718.5(1), c = 1238.1(1) pm, β = 93.363(7)°. The compound forms centrosymmetric dimers in which the titanium atoms are triply and doubly bridged by chlorine atoms to give face- and edgesharing octahedra, respectively. In the linear units [Ti]=N =PPh3 the Ti-N bond distance of 171.6(3) pm corresponds to a double bond.


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).


1991 ◽  
Vol 46 (8) ◽  
pp. 1011-1014 ◽  
Author(s):  
Dieter Fenske ◽  
Sylvia Magull ◽  
Kurt Dehnicke

[Rb(18-crown-6)]2[Zn(Se4)(Se6)] has been prepared by the reaction of a lithium polyselenide solution in DMF with zinc acetate in the presence of rubidium iodide and 18-crown-6. It forms dark red crystals, which were characterized by FIR spectroscopy as well as by an X-ray structure determination. Space group C2/c, Z = 4, 3012 observed unique reflections, R = 0.073. Lattice dimensions at —50 °C: a = 1963.1(14), b = 1125.9(9), c = 2060.3(16) pm, β = 90.05(3)°. The compound has a complex ionic structure, in which the zinc atom of the anion [Zn(Se4)(Se6)]2- is coordinated tetrahedrally by four selenium atoms of a Se42- and a Se62- unit in five and seven membered rings, respectively. The complex cations [Rb(18-crown-6)]+ have Rb · · · Se contacts of 360.7 and 372.0 pm with selenium atoms of the ZnSe4-ring.


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.


2000 ◽  
Vol 55 (6) ◽  
pp. 484-486 ◽  
Author(s):  
B. v. Malottki ◽  
W. Preetz

By reaction of (n-Bu4N)2[ReBr6] with pyridine and (n-Bu4N)BH4 in dichloromethane various bromo-pyridine-rhenium(III) complexes are formed which can be separated by chromatography. Electrochemical oxidation of (n-Bu4N)2[ReBr5Py] leads to (n-Bu4N)[ReBr5Py]. X-ray structure determination on a single crystal has been performed of (n-Bu4N)[ReBr5Py] (monoclinic, space group P21/n a = 11,248(5), b = 17,192(5), c = 15,206(5) Å, β = 97,600(5)°, Z = 4).


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