Synthesis and structural characterization of some molybdenum carbonyl nitrosyl complexes of diethyldithiocarbamate
Journal
Inorganica Chimica Acta
Journal Volume
229
Journal Issue
1-2
Pages
153-163
Date Issued
1995
Author(s)
Abstract
Ten complexes, M′[Mo(Et2NCS2)(CO)2(NO)X] (M′+ = PPN+ or Et4N+; X- = NCS- (1), NO3- (2), N3- (3), Br- (4) or Cl- (5) and [Mo(Et2NCS2)(CO)(NO)L2] (L2 = py and CO (6); dppe (7); 2PPh3 (8); 2P(OMe)3 (10)), have been prepared. Crystal structures of 1, 3, 4, 6, 7, 8 and 10 were determined from single crystal X-ray data. The structures show clearly that the stronger electron-withdrawing NO, compared with CO, prefers the location trans to the better electron donor such as NCS- in 1, N3- in 3 and Br- in 4, unless some other apparent counteracting factors are also involved. The two bulky phosphine ligands are as expected trans to each other in 8 and 10 and a chelate dppe found in 7. Although the structure of 6 has NO trans to py, the spectral data of 6 (and 7), both in solution and in the solid state, reveal the presence of two different structures. Crystal data: 1, space group P21/n, a = 9.879(2), b = 30.302(3), c = 14.858(4) A ̊, β = 97.00(2)°, Z = 4; 3, space group P21/c, a = 16.806(5), b = 16.128(3), c = 18.025(4) A ̊, β = 116.94(2)°, Z = 4; 4, space group Ia, a = 14.773(8), b = 8.982(2), c = 17.748(5) A ̊, β = 96.49(5)°, Z = 4; 6, space group P21/c, a = 13.499(4), b = 10.033(5), c = 12.962(2) A ̊, β = 91.66(2)°, Z = 4; 7, space group P21/n, a = 11.634(3), b = 19.881(4), c = 15.225(4) A ̊, β = 111.10(2)°, Z = 4; 8, space group P21/n, a = 11.767(2), b = 18.851(4), c = 19.436(4) A ̊, β = 107.12(2)°, Z = 4; 10, space group P21/n, a = 8.732(2), b = 23.98(3), c = 11.303(3) A ̊, β = 97.66(2)°, Z = 4. © 1995.
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