Mo2(CO)8-n(m-SR)2Ln [R = Ph, Me3C, PhCH2, CH2CO2Et; L = MeCN, PPh3; n = 0, 2] were prepared by oxidation of (Et4N)2[Mo2(m-SR)2(CO)8] with I and characterized by elemental anal., IR spectroscopy and x-ray crystallog. A new route to prepare these Mo(I) complexes was discussed. The crystal and mol. structure of Mo2(CO)6(m-SPh)2(MeCN)2 was determine from 3-dimensional x-ray data. It crystallizes in the monoclinic, space group P21/c, a 9.241(2), b 9.330(3) c 15.458(4) ? b 105.77(2)? Z = 2, R = 0.033 for 1628 reflections with I>3s (I). The distance of Mo-Mo is 2.978 ?indicating formation of a Mo-Mo bond and the distance of the Mo-S bond is 2.469 ? In comparison with its analogs Mo2(CO)8(m-SCH2CO2Et)2, Mo2(CO)8(m-SCMe3)2 and Mo2(CO)6(m-SCH2CO2Et)2(MeCN)2, the structure relevant to its chem. was discussed.

Key words: CRYSTAL STRUCTURE DETERMINATION, MOLECULAR STRUCTURE, X-RAY DIFFRACTION ANALYSIS, CARBONYL COMPLEX, NITROGENASE, MOLYBDENUM COMPLEX, TRIPHENYLPHOSPHINE, DIPHENYLMETHANE P, TERT.-BUTYL GROUP, ACETIC ACID P