119747-30-7Relevant articles and documents
Cadmium polysulfide complexes, [Cd(Sx)(Sy)]2-: Syntheses, crystal and molecular structures, and 113Cd NMR studies
Banda, R.M. Herath,Dance, Ian G.,Bailey, Trevor D.,Craig, Donald C.,Scudder, Marcia L.
, p. 1862 - 1871 (2008/10/08)
Controlled methods for the formation of cadmium polysulfide complexes in nonaqueous solution, mainly DMF, have been developed. The preferred method is CdS + Na2S + S8 in DMF, which allows a wide range for the solution compositional variables Cd2+ + n(Sm)2- to be attained. 113Cd NMR spectroscopy reveals the existence of the series of monocadmium complexes [Cd(Sx)2]2-, which are in NMR slow exchange (2 s-1) at ambient temperature. The principal Cd NMR resonances are assigned to [Cd(S5)2]2- (740 ppm), [Cd(S5)(S6)]2- (695 ppm), and [Cd(S6)2]2- (648 ppm), with [Cd(S6)(S7)]2- (616 ppm) also postulated. Crystal structures of (Ph4P)2[Cd(S6)2] (6) and (Ph4P)2[{(S6)0.56(S 7)0.44}Cd(S6)] (7), isolated from these solutions, reveal the variability of cadmapolysulfane ring sizes and conformations in crystals. Modifications of the cadmapolysulfane ring sizes, which occur on redissolution of 6 and on deployment of sulfur addition and abstraction reagents, were clearly evident in the Cd NMR spectra. Crystal data: 6, space group P1, a = 11.849 (6) ?, b = 11.990 (6) ?, c = 19.856 (10) ?, α = 92.05 (3)°, β = 92.88 (3)°, γ = 111.88 (2)°, V = 2610 (2) ?3, 3561 observed reflections (Mo Kα, I > 3σ(I)), R = 0.055; 7, space group P1, a = 11.913 (5) ?, b = 12.010 (5) ?, c = 19.785 (8) ?, a = 92.01 (3)°, β = 93.05 (3)°, γ = 111.65 (2)°, V = 2623 (2) ?3, 5211 observed reflections (Mo Kα, I > 3σ(I)), R = 0.054.