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Inorg. Chem. 1990, 29, 412-416 Contribution from the Departments of Chemistry, L a Trobe University, Bundoora, Victoria 3083, Australia, and University of Arizona, Tucson, Arizona 8572 1
Synthesis and Characterization of Tetrasulfidomolybdenum(1V) Complexes of Hydrotris(3,5-dimethyl-l-pyrazolyl) borate and the X-ray Crystal Structure of
(HB( 3,5-Me2C3N2H)3)MoC1(S4)~0.5Et20 Charles G. Young,*Ja Ian P. McInerney,la Michael A.
Bruck,lb
and John H. Enemarklb
Received April 19, 1989 The reactions of cis-(HB(Me2pz),JMoO2X[HB(Me,pz)< = hydrotris(3,5-dimethyl-l-pyrazolyl)borateanion; X = F, C1, Br, NCS] with sulfiding agents in refluxing 1,2-dichloroethane result in the formation of the intensely colored (blue, X = F, CI, Br; green, X = NCS), monomeric, diamagnetic tetrasulfidomolybdenum(1V) complexes (HB(Me, z),}MoX(S4). (HB(Me2pz)3JMoC1(S4)-0.5Et20crystallizes in triclinic space group Pf with a = 10.236 (1) A, b = 15.359 (3) c = 17.333 (3) A, a = 102.30 (l)', /3 = 97.85 ( 1 ) O , y = 104.00 ( 1 ) O , V = 2531.9 A', and Z = 4. The structure was solved by Patterson and Fourier methods, followed by least-squares refinement, for 6090 reflections, to a conventional R value of 0.046 (R, = 0.055). The complex possesses a distorted octahedral coordination sphere composed ofjacial tridentate HB(Me2pz)
