The complex [Mo2(NCCH3)10][BF4]4 (1) acts as a source for the [Mo2]4+ core as shown by its reaction with Mo2(O2CCH3)4 and LL (LL = dppm, dppe, dppee) to yield complexes of the type [Mo2(O2CCH3)2(LL)2][BF4]2. Mononuclear compounds of the type [Mo(O)(F)(LL)2][BF4] (LL = dppe, dppee) have also been isolated from these same reactions. All of these compounds have been characterized by single crystal X-ray diffraction experiments and NMR, IR, and UV-Vis spectroscopy, where appropriate. Crystallographic data for [Mo2(O2CCH3)2-(dppm)2][BF4]2.3CH3CN (2), [Mo2(O2CCH3)2(dppe)2][BF4]2 (3), [Mo2(O2CCH3)2(dppee)2][BF4]2.2CH3CN (5) and [Mo(O)(F)(dppee)2][BF4] (6) are as follows: 2, space group, P1BAR, a = 13.432(4), b = 20.456(9), c = 12.751(4) angstrom, alpha = 104.37(3), beta = 114.00(4), gamma = 83.57(3)-degrees, V = 3097(4) angstrom3, Z = 2; 3, space group P2(1)/c, a = 12.547(6), b = 11.076(6), c = 20.245(13) angstrom, beta = 102.24(4)-degrees, V = 2750(5) angstrom3, Z = 2; 5, space group, P1BAR, a = 11.942(9), b=13.451(9), c= 11.693(12) angstrom, alpha = 95.76(9), beta = 114.62(8), gamma = 111.98(5)-degrees, V=1508(3) angstrom3, Z = 1; 6, space group, Cc, a = 17.481(4), b = 15.050(3), c = 18.150(6) angstrom, beta = 95.23(2)-degrees, V = 4755(2) angstrom3, Z = 4.