Abstract: | Two triangular molybdenum‐tellurium clusters, Mo3Te7‐S2CN (CH2CH2OH2]3I (1) and Mo3Te4Y3S2P(iPrO)2]3I (Y3 = 1. 43Te+ 1.57S) (2), were obtained from the reaction of K · HOdtc HOdtc = S2CN(CH2CH2OH)2] or K·iPr2dtp (iPr2dtp = S2POCH(CH3)2]2) with a mixed product of elements Mo, Te(S) and I2 at high temperature. The structures of the two compounds were determined by X‐ray crystallography study. Crystal data are, (1): monoclinic, P21/n, a = 1.6256(3), b = 1.3264(2), c = 1.8808(4) nm, β=96.923°, V = 4.025.9 (14) nm3, Dcal = 3.050g·cm‐3, Z = 4, and (2): monoclinic, P21/n, a = 1.4564(2), b = 2.3917(4), c = 1.5094(3) nm, β = 114.35(2)°, V = 4.0259(14) nm3, Dcal = 2.449 g·cm?3 and Z = 4. Single crystal analyses show that 1 consists of discrete Mo3Te7S2CN(CH2CH2OH)2]3I connected into three‐dimensional framework via hydrogen bonds, while 2 forms a linear chain via Te(S)—I interaction. |