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Divalent Lanthanide Phosphides. Synthesis and X-ray Crystal Structure Determination of Yb[PPh2]2 (N-Melm)4: The Missing Link1

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Pages 273-277 | Received 29 Mar 1995, Published online: 19 Aug 2006

References

  • Reported in part at the 209th National Meeting of The American Chemical Society, Anaheim, CA, April 1995, INOR 137
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  • Crystal data for 2 (C40H44N8P2Yb): Mr = 871.81 monoclinic, space group P21/n with a = 9.881 (1) Å, b = 17.717 (2) Å, c = 11.153 (2) Å, β = 95.61 (1)°, V = 1943.1 (5) Å3, ρ = 1.490g cm−3, Z = 2, F(000) = 880, μ(Mo-Kα) = 25.28 cm−1; Enraf Nonius CAD4 diffractometer. The structure was solved by direct methods. Data were corrected for Lorentz and polarization effects as well as for absorption (DIFABS). Data collected at 217K with Mo-Kα (λ = 0.71069 Å). From 4402 measured [(sin Θ/λ)max = 0.64 Å−1] and 4396 unique reflections, 3435 were considered “observed” [F0 > 4 σ(F0)] and used for refinement. All non-H atoms were refined with anisotropic displacement parameters. All H-atoms were calculated and allowed to ride on their corresponding carbon atom with fixed isotropic contributions (Uiso(fix) = 0.08 Å2). The structure converged for 232 refined parameters to an R 1 (wR2) value of 0.0201 (0.0469). The function minimized was [Σw(F2 0 – F2 0)2]/Σ[w(F2 0)2]1/2, w = q/σ2(F2 0) + (ap)2 + bp, p = max(F2 0, o) + 2F2 0/3 a = 0.0243, b = 1.31. Residual electron densities: + 0.278/ − 0.562eÅ−3
  • Dunne , B. J. and Orpen , A. G. 1991 . Acta Cryst. , C47 : 345
  • Nief , F. , Ricard , L. and Mathey , F. 1993 . Polyhedron , 12 : 19
  • Karsch , H. H. , Ferazin , G. , Steigelmann , O. , Kooijman , H. and Hiller , W. 1993 . Angew. Chem. Int. Ed. Engl. , 32 : 1739
  • Tilley , T. D. , Andersen , R. A. and Zalkin , A. 1982 . J. Am. Chem. Soc. , 104 : 3725
  • Tilley , T. D. , Andersen , R. A. and Zalkin , A. 1983 . Inorg. Chem. , 22 : 856
  • Shannon , R. D. 1976 . Acta Cryst. , A32 : 751

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