Synthesis and crystal structure of [(PPh3)(CH3COS)(2)NiB10H10]center dot 0.4(C5H12)

The title compound [(PPh3) (CH3COS)(2)NiB10H10] . 0. 4(C5H12) has been synt hesized by the reaction of [NiCl2(PPh3)(2)], closo-[B10H10](2-) and CH3COSH in CH2Cl2 solution. It was recrystallized from n-pentane/CH2Cl2 solution a nd its structure was determined by X-ray diffraction analysis. The crystal is triclinic, space group P (1) over bar, M-r = 618. 23, with a = 10. 049 ( 1), b = 12. 638 (2), c = 14. 077 (2) Angstrom, alpha = 110. 13 (1), beta = 87. 65 (1), gamma = 96. 01 (1)degrees, V = 1669. 3 (4) Angstrom(3), D-c = 1 . 230 g/cm(3), Z = 2, lambda (MoK alpha) = 0. 71073 Angstrom, mu = 7. 76 cm (-1), F(000) = 642. The final refinement is converged with R = 0. 042 (5986 observed reflections with I greater than or equal to 2 sigma(I)), wR(2) = 0. 151. The cluster is a nido eleven-vertex {NiB10} cage with the Ni atom i n the open NiB4 face. Cyclizations resulting in two five-membered rings, Ni (7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2) -O(2)-B(3), have occurred.