The preparations and single-crystal X-ray structures of the title compounds are described. All compounds are monomeric as solids with essentially planar metal-donor atom sets. Relevant crystallo raphic parameters are as follows: Ni-(S,CNEt,)(PEt,)Cl triclinic, space group Pi, a = 7.678 (2) A, b = 9.775 ( 5 ) l, c = 12.030 ( 5 ) A, a = 97.61 (4)O, p = 91.26 (3)O, y = 95.43 (3)O, V = 890.30 (64) A3, Z = 2, R = 0.055, Ni-C1 = 2.190 (2) A, Ni-S (trans P) = 1.723 (7) A, Ni-S (trans C1) = 1.728 (7) A; Pd(S2CNEt2)(PPh3)C1 triclinic, space group Pi, a = 9.894 (3) A, b = 11.731 (4) A, c = 14.115 (2) A, a = 98.19 (2)O, ,8 = 118.89 (2)O, y = 108.04 (2)O, V = 1277.09 (58) A3, Z = 2, R = 0.045, Pd-P = 2.284 (1) A, Pd-CI = 2.338 (2) A, Pd-S (trans P) = 2.352 (2) A, Pd-S (trans Cl) = 2.283 (2) A; Pt(SzCNEtz)(PPh3)C1 orthorhombic, space group P212121, a = 15.350 (4) A, b = 9.431 (2) A, c = 16.930 (6) A, V = 2451.0 (1.1) A3, Z = 4, R = 0.035, Pt-P = 2.253 (7) A, Pt-C1 = 2.331 (6) A, Pt-S (trans P) = 2.349 (7) A, Pt-S (trans C1) = 2.294 (7) A.Comparisons are made between the structural properties of the title compounds and with the structures of the parent M(S2CNEt2)2 species. These structural relationships are correlated with spectroscopic measurements, suggesting that several different, nearly equally energetic, processes lead to the observed dynamic N M R spectra of these complexes in solution.A structural trans effect P > S > C1 is observed in the metal-sulfur bonding.