MONONUCLEAR COMPLEXES OF CR(II) AND FE(II) WITH TERMINAL SH-GROUPS - SYNTHESIS AND X-RAY CRYSTAL-STRUCTURES OF TRANS-M(SH)2(DMPE)2 (M = CR, FE - DMPE = 1,2-BIS(DIMETHYLPHOSPHINO)ETHANE)

The reaction of two equivalents of NaSH with MCl2(dmpe)2(M = Cr, Fe,) at — −78°C gives trans-M(SH)2(dmpe)2(M = Cr, (1), 30% Fe, (2) 98%). The complexes have been characterized spectroscopically, and the trans geometry has been confirmed by single crystal X-ray diffraction studies. Crystal data (1): C12H34CrP4S2, M = 418.42, monoclinic, P21/n, a = 8.857 (I), b= 12.719 (2), c = 9.648 (I)Å, β = 92.14(1)°, U= 1086.2 (5)Å, Dc= 1.279gcm−3, Z = 2, λ(MoKα) = 0.71073Å, (graphite monochromator), μ(MoKα) = 9.80cm−1. Methods: MULTAN, difference Fourier, full-matrix least-squares. Refinement of 1149 reflections (I > 3σ(I)) out of 1901 unique observed reflections (3.0° < 20 < 48.0°) gave R and Rw values of 0.092 and 0.096, respectively. Crystal data (2): C12H34FeP4S2, M = 422.28, monoclinic, P21/n, a = 8.834 (2), b = 12.594 (2), c = 9.532 (2) A, β = 90.66 (2)°, U = 1060.3 (5) A3, Dc= 1.323gcm−3, Z = 2, λ(MoKα) = 0.71073Å, (graphite monochromator), μ(MoKα) = 11.87cm−1. Methods: same as for (1). Refinement of 1178 reflections (I> 3a (I)) out of 2086 unique observed reflections (2.0° < 20 < 50.0°) gave R and Rw values of 0.056 and 0.059, respectively. © 1991, Taylor & Francis Group, LLC. All rights reserved.