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| Titel: |
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) |
| Auteur: |
Arif, Atta M. Hefner, John G. Jones, Richard A. Koschmieder, Stefan U. |
| Verschenen in: |
Journal of coordination chemistry |
| Paginering: | Jaargang 23 (1991) nr. 1-4 pagina's 13-19 |
| Jaar: |
1991-06-01 |
| Inhoud: |
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(MoKa) = 0.71073 Å, (graphite mono-chromator), μ(MoKa) = 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° < 29 < 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) Å, β = 90.66 (2)°, U = 1060.3 (5) Å3, Dc = 1.323 g cm-3, Z = 2, γ(MoKa) = 0.71073 Å, (graphite monochromator), μ(MoKa) = 11.87 cm-1. Methods: same as for (1). Refinement of 1178 reflections (I > 3σ (I)) out of 2086 unique observed reflections (2.0° < 20 < 50.0°) gave R and Rw values of 0.056 and 0.059, respectively. |
| Uitgever: |
Taylor & Francis |
| Bronbestand: |
Elektronische Wetenschappelijke Tijdschriften |
Details van artikel 32 van 73 gevonden artikelen
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