(2)[ 6]. However, 1 and 2 were crystallized in highly different way. 2 and the compound reported by Maiti et al.(3) [5] were crystallized in same space group P2 1 /c, while 1 in P6 5 22, aspace group rarely found in heterothiometallic clusters. This observation suggests that the coexisting anions in reaction system might play an important role in crystallization, although S 2-and SO4 2-were not included in final products. The asymmetric unit of the title crystal structure contains one and ahalf [NMe 4 ] + cations, ahalf [CuMo 2 S 8 ] 3-anion, with N2, C5 and Cu2 on special positions, thus the anionic cluster showing higher symmetry than those in 2 and 3.Two halves of the anion are related through symmetric operation 1-y,1-x, 1 6 -z.The geometric parameters of the trivalent anion in 1 is comparable to those in 2, 3 and aclose analog of tungsten [CuW 2 S 8 ] 3-(4) [7], except an otable difference among the Mo-Cu-Mo angles (166.92(4)°for the title cluster, 160.2(3)°for 2 and 162.97(2)°for 3,indicating anarrower gap toward the 170°configuration for the cluster in ORP [4]), and W-Cu-Wangle (170.3(2)°for 4).