scholarly journals Synthese und Kristallstruktur von [Ag(PhN3C6H4N3(H)Ph)]4, einem tetrameren Ag(I)-Komplex mit überbrückenden Bistriazenido-Liganden / Synthesis and Crystal Structure of [Ag(PhN3C6H4N3(H)Ph)]4, a Tetrameric Ag(I) Complex with Bridging Bistriazenido Ligands

1990 ◽  
Vol 45 (5) ◽  
pp. 689-694 ◽  
Author(s):  
Manfredo Hörner ◽  
Antônio Gilberto Pedroso ◽  
Carlos Roberto de Menezes Peixoto ◽  
Johannes Beck

[Ag(PhN3C6H4N3(H)Ph)]4 is obtained by the reaction of AgNO3 with [PhN3C6H4N3(H)Ph)]Na in tetrahydrofurane in form of brown crystals. The crystal structure determination (orthorhombic space group Pbcn, a = 1989.7(8), b = 1917.5(3), c = 1767.1(4) pm, Z = 4, 1784 reflections for 200 parameters, final R = 0.059) shows the complex to be isotypic to the previous described copper analogue. The complex is built of a rhombus of four silver atoms and four bridging bistriazenido units. One nitrogen atom of a neutral nitrogen chain completes the coordination sphere of each silver atom to a distorted trigonal bipyramidal environment of two other silver atoms and three nitrogen atoms. The Ag–Ag distances are in the range from 279.9 to 310.3 pm, the Ag–N distances from 217 to 236 pm.

1992 ◽  
Vol 47 (3) ◽  
pp. 301-304 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke

The title compound has been prepared by the reaction o f [WCl4(NSeCl)]2 with PPh4Cl in CH2Cl2 solution. It forms red crystals, which were characterized by an X-ray structure determination. Space group P21/c, Z = 4, 3856 observed unique reflections, R = 0.073. Lattice dimensions at 25 °C: a = 2266.0(5), b = 1121.0(2), c = 2013.0(4) pm, β = 109.66(3)°. The structure consists o f PPh4+ ions and anions [WCl5(NSeCl2)]2-, in which the tungsten atom is surrounded in a distorted octahedral way by five chlorine atoms and by the nitrogen atom of the (NSeCl2)3- ligand. The W = N = SeCl2 group is characterized by WN and SeN double bonds; the selenium atom has a pseudo trigonal-bipyramidal coordination with the N atom and two lone pairs in equatorial and the chlorine atoms in axial positions.


1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.


Author(s):  
Glen G. Briand ◽  
Andreas Decken ◽  
Courtney M. Dickie ◽  
Gregory MacNeil

The dinuclear title compound, [In2(CH3)2(C7H7S)4] or [Me(2-MeC6H4S)In-μ-(2-MeC6H4S)2InMe(2-MeC6H4S)], was prepared from the 1:2 reaction of Me3In and 2-MeC6H4SH in toluene. Its crystal structure exhibits a four-membered In2S2ring coreviabridging (2-MeC6H4S) groups. The dimeric units are further associated into a one-dimensional polymeric structure extending parallel to theaaxisviaintermolecular In...S contacts. The In atoms are then in distorted trigonal–bipyramidal CS4bonding environments.


1990 ◽  
Vol 45 (2) ◽  
pp. 175-183 ◽  
Author(s):  
Peter G. Jones ◽  
Anke Meyer ◽  
Reinhard Schmutzler

The reactions of 4-chloro-1,3,5,7-tetramethyl-2,2,6,6-tetraoxa-2,6-dithia-1,3,5,7-tetraaza-4λ5-phosphaspiro[3.3]heptane (1) with trimethylsilyl compounds and sodium azide led to a series of spirocyclic N,N′-dimethylsulphamide-substituted phosphoranes (2—5). The nature of the pentaaza-spirophosphorane (4) was confirmed by an X-ray crystal structure determination (C2/c, a = 991.8(4), b = 1185.6(6), c = 1224.9(5) pm,β = 108.64(3)°, Z = 4, R = 0.041 for 1065 unique observed reflections); a crystallographic twofold axis passes through phosphorus and the nitrogen atom of the NMe2 group. The geometry at phosphorus is to a good approximation trigonal bipyramidal. The azido-spirophosphorane (5) undergoes Staudinger-type reactions with phosphorus(III) compounds (PPh3, dppm) to form the mixed-valence phosphorus compounds 6—8. The reaction of N,N′-dimethylsulphamide or N,N′-dimethyl-N,N′-bis(trimethylsilyl)-sulphamide with dichlorophosphines RPCl2 (R = Me, Ph) in a molar ratio 1:2 leads to the formation of the acyclic N,N′-dimethylsulphamide-bridged diphosphorus compounds 9 and 10, respectively. The spectroscopic properties (and, for 4, the X-ray crystal structure) of the products are compared with those of analogous urea-bridged phosphorus compounds.


2002 ◽  
Vol 57 (6) ◽  
pp. 599-604 ◽  
Author(s):  
Franziska Emmerling ◽  
Mamdouh Idilbi ◽  
Caroline Röhr

Abstract The title compounds have been synthesized via oxidation of the elemental pnicogenes (M = As, Bi) with the hyperoxides AO2 (A = K, Rb, Cs) and their crystal structures were determined on the basis of single crystal X-ray data. In K3AsO4 (orthorhombic, Cccm, a = 1060:1(1), b = 1135:2(1), c = 1694:0(2) pm, Z = 16) and Cs3AsO4(orthorhombic, Pnma, a = 1254:3(2), b = 902:9(2), c = 658:5(3) pm, Z = 4) isolated tetrahedra [AsO4]3- with distances As-O between 167.0 and 170.5 pm are present, which are arranged in a nearly cubic close packing. The structure of K3BiO4 (triclinic, P1̄, a = 643:18(6), b = 657:27(6), c = 762:41(7) pm, α = 101:724(2)°, β = 96:472(2)°, γ = 105:465(2)°, Z = 2) contains centrosymmetric dimers [O3BiO2BiO3]6-, in which the Bi(V) atoms are surrounded by five O atoms in a distorted trigonal bipyramidal geometry with distances Bi-O in the range of 199.5 to 233.1 pm.


2001 ◽  
Vol 56 (9) ◽  
pp. 927-930
Author(s):  
Alfonso Castiñeiras ◽  
Ricardo Domínguez ◽  
Jairo Bordinhão ◽  
Julieta Saldanha de Oliveira ◽  
Adaílton João Bortoluzzi ◽  
...  

AbstractThe reaction of zinc(II) acetate dihydrate and the tetra-dentate N-Oxo-2-acetylpyridine 4N-methylthiosemicarbazone (H4MLO) produces the novel complex [Zn(C9H11N4OS)2·H2O] (1). The complex crystallizesoin the orthorhombic space group Pbca with a = 15.871(3), b =16.890(3), c = 17.189(3) Å ,V - 4608(1) Å3, Z = 8 . The Zn(II) ion is tetra-coordinated via the thiolate sulfur atom and the azomethine nitrogen atom of two deprotonated ligands. In the solid state, 1 is polymerized via hydrogen bonds with a water molecule of crystallization.


1996 ◽  
Vol 51 (8) ◽  
pp. 1127-1131 ◽  
Author(s):  
J. Beck

Red crystals of (TeCl3)3MoCl6(Cl) are obtained by reacting MoCl4 with TeCl4 in a 1:3 molar ratio in a sealed evacuated ampoule at 170°. The crystal structure determination (orthorhombic, space group Cmc21, a = 1541.6(2), b = 1268.1(1), c = 1180.6(1) pm) shows the presence of trigonal-pyramidal [TeCl3]+ ions, octahedral [MoCI6]2- ions, and isolated Cl- ions. The ions are linked by long Te-Cl bridges resulting in distorted TeCl6 octahedra. The octahedra are connected by joint edges and corners to zig-zag chains running along the polar c axis.


1988 ◽  
Vol 43 (1) ◽  
pp. 132-133 ◽  
Author(s):  
W. Hiller ◽  
A. Castiñeiras ◽  
M. E. García- Fernandez ◽  
M. R. Bermejo ◽  
J. Bravo ◽  
...  

Abstract The unit cell of TlBrI2 (4-methylpyridine-N-oxide) 2 is orthorhombic, space group Pnna. with a = 1126.9(3),b = 919.8(2),c = 1210.4(3) pm.and Z = 4. The structure consists of discrete TlBrI2 (4-methyl-pyridine-N-oxide)2 molecules which have a distorted trigonal-bipyramidal geometry. The thallium atom is coordinated to two iodine atoms and a bromine atom in equatorial positions, and by two 4-methyl-pyridine-N-oxide ligands in the axial positions.


1976 ◽  
Vol 29 (1) ◽  
pp. 213 ◽  
Author(s):  
BF Hoskins ◽  
RL Martin ◽  
NM Rohde

The syntheses and Mossbauer spectra of four sulphur-chelated compounds of tin(11) are reported. A single-crystal X-ray structure determination of Sn(dedtc)2 has established that the molecule possesses a strongly distorted trigonal bipyramidal configuration with a sterically active lone pair of electrons occupying an equatorial coordination position. While the Mossbauer quadrupole splitting for tin(11) compounds, in general, is consistent with a sterically active pair of electrons, its magnitude appears to be more sensitive to the nature of the ligand rather than the tin stereochemistry.


1997 ◽  
Vol 52 (12) ◽  
pp. 1484-1490 ◽  
Author(s):  
Thomas Miekisch ◽  
Klaus Harms ◽  
Sigrid Wocadlo ◽  
Werner Massa ◽  
Bernhard Neumüller ◽  
...  

Abstract [Ti3Cl8(NPMe3)3]Cl has been prepared by the reaction of TiCl3(THF)3 with Me3SiNPMe3 in dichloromethane forming green moisture sensitive crystals. According to the crystal structure determination the titanium atoms of the cation [Ti3Cl8(NPMe3)3]+ are linked by two μ3-N atoms of two NPMe3- groups forming a distorted trigonal-bipyramidal arrangement. The third NPMe3- group and two of the chlorine atoms have μ2-bridging functions. The mixed-valence complex [V2Cl4(NPPh3)3] is formed as dark green moisture sensitive crystals by the reaction of vanadium trichloride with Me3SiNPPh3 in boiling toluene. According to the crystal structure determination the vanadium atoms are linked by two μ2-N atoms of two NPPh3- groups forming a nonplanar V2N2 four-membered ring with a V-V distance of 266.8(1) pm which corresponds to a (σ, 1/2π) bond type. This is confirmed by the measurement of the magnetic susceptibility which leads to a magnetic moment of 1.45(5) B. M., corresponding to the remaining d1 -electron.


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