THE CRYSTAL-STRUCTURES OF [MOCL2(NO)(2)(OPET(3))](2), [MOCL3(NO)(OPPH(3))(2)CENTER-DOT-MOCL4(OPPH(3))(2)], [MOCL2(NO)(PPH(3))(2)(CH3CN)], AND [MOCL4(NPP3)(OPPH(3))]
Philipp, G; Wocadlo, S; Massa, W; Dehnicke, K; Fenske, D; Maichlemossmer, C; Niquet, E; Strahle, J
The title compounds have been prepared by reactions of MoCl2(NO)(2) with PPh(3), OPPh(3), or Me(3)SiNPR(3) (R = Et, Ph) in dichloromethane and acetonitrile suspension, respectively. All complexes were characterized by IR spectroscopy and by crystal structure determinations. [MoCl2(NO)(2)(OPEt(3))](2): Space group C2/c, Z = 4, 2950 observed unique reflections. R = 0.029. Lattice dimensions at -70 degrees C: a = 2390.5(11), b = 875.5(5), c = 1399.1(6) pm, beta = 113.18(2)degrees. The complex forms a centrosymmetric dimer with MoCl2Mo bridges, the nitrosyl groups being in a cis-arrangement. The OPEt(3) ligand is coordinated in trans position to one of the nitrosyl ligands.
[MoCl3(NO)(OPPh(3))(2).MoCl4(OPPh(3))(2)]: Space group P2(1)/c, Z = 4, 10243 observed unique reflections, R = 0.060. Lattice dimensions at -60 degrees C: a = 1900.4(3), b = 1689.1(5), c = 2209.3(7) pm, beta = 95.92(2)degrees. The structure consists of the two independent complexes
[MoCl3(NO)(OPPh(3))(2)] and [MoCl4(OPPh(3))(2)]. In both complexes the OPPh(3) groups are in a cis-arrangement at the octahedrally coordinated Mo atoms; in the nitrosyl complex one of the OPPh(3) molecules is in trans-position to the nitrosyl ligand.
[MoCl2(NO)(PPh(3))(2)(CH3CN)]: Space group P2(1)/n, Z = 4, 5107 observed unique reflections, R = 0.028. Lattice dimensions at 20 degrees C: a = 1006.5(2), b = 1527.2(2), c = 2342.3(2) pm. beta = 90.97(1)degrees. The PPh(3) molecules are in tuans-positions to one another at the octahedrally coordinated Mo atom, whereas the acetonitrile molecule is in Irans-position to the nitrosyl ligand.
[MoCl4(NPPh(3))(OPPh(3))]: Space group P2(1), Z = 2, 3323 observed unique reflections, R = 0.057. Lattice dimensions at -70 degrees C: a = 985.7(8), b = 1471.2(9), c = 1215.9(11) pm, beta = 100.50(3)degrees. The OPPh(3) molecule coordinates in trans-position to the phosphorane iminato ligand at the octahedrally coordinated Mo atom.