MoFe3S4Cl3(3,6-(C3H5)2C6H2O2)(THF).

Article abstract of DOI:10.1021/ja00351a032

Reaction of the doubly-bridged double-cubane cluster left bracket Mo//F//o 6S//8(SEt)//6(al//2cat)//2 right bracket **4**- (al//2cat equals 3,6-dialycatecholate) with 6 equiv of acetyl chloride in (2m double prime afforded, after recrystallization from acetone/THF, the single-cubane compound (Et//4N)//2 left bracket MoFe//3S//4Cl//3(al//2cat)(THF) right bracket . 0. 5CH//3COCH//3. The acetone-free 21 crystallizes from n-butyronitrile/THF in monoclinic space group C2/c with a equals 23. 829 (5) A, b equals 11. 452 (3) A, c equals 16. 870 (3) A, beta equals 106. 15 (2) degree , and Z equals 4. With use of 2451 unique data (F//o **2 greater than 3 sigma (F//o **2) the structure was refined to R (R//w) equals 3. 88% (3. 94%). The cluster left bracket MoFe//3S//4Cl//3-(al//2cat)(THF) right bracket **2**-(1) has a cubane-type left bracket MoFe//3( mu //3-S)//4 right bracket **3** plus core with tetrahedral Fe atoms terminally coordinated by chloride and a Mo atom whose coordination external to the core is completed by a catecholate chelate ring and a THF molecule (Mo-O and a Mo atom whose coordination external to the core is completed by a catecholate chelate ring and a THF molecule (MO-0 equals 2. 352 (6) A). An imposed mirror plane bisects the core and the chelate ring, resulting in cluster C//s symmetry and two types of Fe sites (2m plus M prime ) In solution the cluster solvates left bracket MoFe//3S//4Cl//3(al//2cat)(solv) right bracket **2**-(solv equals MeCN (2), Me//2SO (3)) are formed.