Mono-, Bi-, and Trinuclear Metallocyclophanes Formed in Reactions between [Mo(NO){HB(3,5-Me2C3HN2)3}I2] and Xylenedithiols. The X-ray Crystal Str
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The reactions between[Mo(NO)(tp*)I2] {tp* =HB(3,5-Me2C3HN2)3}and HE-EH {HE-EH =1,3-(HSCH2)2C6H4and 1,4-(HSCH2)2C6H4}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, from1,3-(SCH2)2C6H4,[Mo(NO)(tp*){(3-SCH2C6H4CH2)2S}].The reaction between [Mo(NO)(tp*)I2]and 1,2-(HSCH2)2C6H4 affords, asits major product, the chelate complex[Mo(NO)(tp*){1,2-(SCH2)2C6H4}],nometallomacrocycles being found among the reaction products in thiscase. Cyclic voltammograms of themacrocyclic complexes contain single reduction waves in the region-1.374 to -1.486 V (vs ferrocene/ferrocenium), and the binuclear metallomacrocycles show noelectrochemically resolvable metal-metal interactions.The molecular structures of[Mo(NO){HB(3,5-Me2C3HN2)3}{1,4-(SCH2)2C6H4}n](n = 2, 3) have been determinedcrystallographically:[Mo(NO){HB(3,5-Me2C3HN2)3}{1,4-(SCH2)2C6H4}2],C31H38BMoN7OS4,orthorhombic,space group Pna21, a =16.193(8) Å, b = 12.878(5) Å, c =16.620(5) Å, Z = 4;[Mo(NO){HB(3,5-Me2C3HN2)3}{1,4-(SCH2)2C6H4}3],C39H46BMoN7OS6,monoclinic space group P21/n,a = 19.140(5) Å, b =10.708(3)Å, c = 22.072(5) Å, ges/gifchars/beta2.gif" BORDER=0 ALIGN="middle"> = 100.73(2)ges/entities/deg.gif">,Z = 4.

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