HYDROGEN-BONDING OF CHCL3 TO COORDINATED NITRIC-OXIDE IN A BINUCLEAR METALLOMACROCYCLE AND THE CRYSTAL-STRUCTURES OF ,5-ME2C3HN2)(3))(2,7-O2C10H6)](2).2CHCL(3).CH2CL2, ME2C3HN2)(3))(2,7-O2C10H6)]2.0.67CHCL(3).2.7H(2)O, AND (HB(3,5-ME2C3HN2)(3))(2,7-O2C10H6)](2).3(CH3)(2)CO

The reaction between [Mo(NO)(Tp)I-2] {Tp(*-) = hydrotris(3,5-dimethyl pyrazol-1-yl)borate) and 2,7-dihydroxynaphthalene affords, as its majo r product, the binuclear complex [Mo(NO)(Tp)(2,7-O2C10H6)](2) The rea ction appears to proceed under kinetic control so that shorter reactio n times afford the syn-isomer (47% yield after 40 min) while longer re action times allow the and-isomer (43% yield after 48 h) to be obtaine d. The molecular structures of anti-[Mo(NO)(HB(3,5-Me2C3HN2)(3))} 2,7- O2C10H6)](2).2CHCl(3).CH2Cl2 (1), syn-[Mo(NO){HB(3,5-Me2C3HN2)(3))(2,7 -O2C10H6)](2). e2C3HN2)(3)}(2,7-O2C10H6)](2).0.67CHCl(3).2.7H(2)O (2) and syn-[MoNO)(HB(3,5-Me2C3HN2)(3)}(2,7 CO (3) have been determined cr ystallographically (1) C50H56B2N14O6Mo2.2CHCl(3).CH2Cl2, triclinic, sp ace group P (1) over bar, a = 11.535 (2) Angstrom, b = 14.032(3) Angst rom, c = 11.247(3) Angstrom, alpha = 94.70(1)degrees, beta = 102.30(2) degrees, gamma = 110.31(2)degrees, Z = 1; (2) C50H56B2N14O6Mo2.0.67CHC l(3).2.7H(2)O, monoclinic space group P2(1)/m, a = 23.770(7) Angstrom, b = 26.600(10) Angstrom, c = 11.224(4) Angstrom, beta = 99.86(2)degre es, Z = 4; (3) C50H56B2N14O6Mo2.3C(3)H(6)O, triclinic, space group P ( 1) over bar, a = 16.929(3) Angstrom b = 17.465 Angstrom, c = 12.739(2) Angstrom, alpha = 100;06(1)degrees, beta = 94.93(2)degrees, gamma = 1 14.13(1)degrees, Z = 2. In 1 each nitric oxide ligand is hydrogen bond ed [C-H 0.98, H ... O 2.26, C ... O 3.13(2) Angstrom, C-H ... 147 degr ees} to a chloroform molecule which lies within a cavity in the molecu lr having as its base a bridging 2,7-naphthalenediyl fragment and as i ts sides a part of each HB(3,5-Me2C3HN2)(3) ligand. No hydrogen bondin g interactions with nitric oxide are apparent in the strucutres of 2 a nd 3.