Hydrogen Bonding of CHCl(3) to Coordinated Nitric Oxide in a Binuclear Metallomacrocycle and the Crystal Structures of anti-[Mo(NO){HB(3,5-Me(2)C(3)HN(2))(3)}(2,7-O(2)C(10)H(6))](2).2CHCl(3).CH(2)Cl(2), syn-[Mo(NO){HB(3,5-Me(2)C(3)HN(2))(3)}(2,7-O(2)C(10)H(6))](2).0.67CHCl(3).2.7H(2)O, and syn-[Mo(NO){HB(3,5-Me(2)C(3)HN(2))(3)}(2,7-O(2)C(10)H(6))](2).3(CH(3))(2)CO.

The reaction between [Mo(NO)(Tp)I(2)] {Tp(-) = hydrotris(3,5-dimethylpyrazol-1-yl)borate} and 2,7-dihydroxynaphthalene affords, as its major product, the binuclear complex [Mo(NO)(Tp)(2,7-O(2)C(10)H(6))](2). The reaction appears to proceed under kinetic control so that shorter reaction times afford the syn-isomer (47% yield after 40 min) while longer reaction times allow the anti-isomer (43% yield after 48 h) to be obtained. The molecular structures of anti-[Mo(NO){HB(3,5-Me(2)C(3)HN(2))(3)}(2,7-O(2)C(10)H(6))](2).