The reactions between [Mo(NO)(tp*)I-2] {tp* = HB(3,5-Me2C3HN2)(3)} and HE-EH {HE-EH = 1,3-(HSCH2)(2)C6H4 and 1,4-(HSCH2)(2)C6H4} afford the cyclic dimers [Mo(NO)(tp*)(E-E)](2) and cyclic trimers [Mo(NO)(tp*)(E-E)](3). These reactions also produce the monometallomacrocycles [Mo(NO)(tp*)(E-E)(x) (x = 2, 3) and,:from 1,3-(SCH2)(2)C6H4, [Mo(NO)(tp*) {3-SCH2C6H4CH2)(2)S}]. The reaction between [Mo(NO)(tp*)I-2] and 1,2-(HSCH2)(2)C6H4 affords, as its major product, the chelate complex [Mo(NO)(tp*){1,2-(SCH2)(2)C6H4}], no metdlomacrocycles being found among the reaction products in this case. Cyclic voltammograms of the macrocyclic complexes contain single reduction waves in the region -1.374 to -1.486 V (vs ferrocene/ferrocenium), and the binuclear metallomacrocycles show no electrochemically resolvable metal-metal interactions. The molecular structures of [Mo(NO){HB(3,5-Me2C3HN2)(3)}{1,4-(SCH2)(2)C6H4}(n)]( )(n = 2, 3) have been determined crystallographically : [Mo(NO){HB(3,5-Me2C3HN2)(3)}{1,4-(SCH2)(2)C6H4}(2)], C31K38BMoN7OS4, orthorhombic, space group Pna2(1), a = 16.193(8) Angstrom, b = 12.878(5) Angstrom, c = 16.620(5) Angstrom, Z = 4; [Mo(NO){HB(3,5-Me2C3HN2)(3)}{1,4-(SCH2)(2)C6H4}(3)], C39H46BMoN7OS6, monoclinic space group P2(1)/n, a.= 19.140(5) Angstrom, b = 10.708(3) Angstrom, c = 22.072(5) Angstrom, B = 100.73(2)degrees, Z = 4.