PREPARATION AND CHARACTERIZATION OF TWIN-CUBANE-TYPE CLUSTERS WITH MOLYBDENUM-COPPER-SULFUR CORES - X-RAY STRUCTURE DETERMINATION OF 3)(6)(H2O)(OH)MO3CUS4(O))(2)]CL4-CENTER-DOT-8H(2)O

Reaction of the cubane-type cluster [Mo3CuS4(H2O)(10)](4+) (1) with co ncentrated aqueous ammonia afforded a novel twin-cubane-type cluster [ {(NH3)(6)(H2O) (OH)Mo3CuS4(O)}(2)]Cl-4. 8H(2)O (2). X-ray structure an alysis of 2 revealed that two cubane-type Mo3CuS4 cores were bridged b y two oxygen atoms. The cores are related to each other by a center of symmetry. X-ray photoelectron spectroscopy measurement of the Cu 2p(3 /2) bonding energy (934.0 eV) indicates that the oxidation state of co pper atom is + 1. On the basis of these results, the formal oxidation state Mo-3(IV,IV,IV) is ascribed to each of the cubane-type Mo3CuS4 mo ieties. (C) 1998 Elsevier Science S.A. All rights reserved.