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Ferrocenyl β-diketonato-based Cu(II)-oxo clusters with Cu7 and Cu10 cores

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Pages 329-333 | Received 08 Nov 2012, Accepted 14 Nov 2012, Published online: 21 Jan 2013

References

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  • Crystal structure analysis: Data collections were performed at 100 K with Cu K α (λ = 1.54184 Å) for 3 and with Mo K α radiation (λ = 0.71073 Å) for 2 with an Oxford Gemini S diffractometer. Of 39114/61152 collected 9990/24166 reflections were independent (R int = 0.0872/0.0337) for 3/2, respectively. Both structures were solved by direct methods and refined by full-matrix least-squares on F 2 with the SHELXTL-97 program package [42]. For 3, the two ferrocenyl fragments comprising Fe5/C47–C56 and Fe6/C57–C66 and the atoms O5/O6/C71 were refined, disordered with split occupancies of 0.49/0.51, 0.50/0.50 and 0.52/0.48, respectively. For 2, the methyl and ferrocenyl substituents of one fb ligand (C95 and C85–C94/Fe7) and one Et2O molecule were refined, disordered with split occupancies of 0.73/0.27 and 0.54/0.46, respectively. A further Et2O molecule was refined with an occupation factor of 0.5. Crystal data for C150H148Cu7Fe12O21Si2 (3): M = 3457.84 g mol–1, monoclinic, P2/n, a = 18.5088(3), b = 15.0688(2), c = 25.0369(3) Å, β = 102.874(1), V = 6807.39(16) Å3, Z = 2, D c = 1.687 g cm−3, μ = 11.758 mm−1, R 1 = 01368 (all data), wR 2 = 0.1268 (all data) and goodness-of-fit on F 2 is 0.874. Crystal data for C252H286Cu20Fe16O55Si8 (2): M = 6583.93 g mol−1, triclinic, P−1, a = 15.4764(8), b = 17.4332(10), c = 28.2358(14) Å, α = 96.937(4), β = 90.083(4), c = 112.707(5), V = 6966.6(6) Å3, Z = 1, D c = 1.569 g cm−3, μ = 2.394 mm−1, R 1 = 0.0849 (all data), wR 2 = 0.1648 (all data) and goodness-of-fit on F 2 is 1.189. Crystallographic data have been deposited with the Cambridge Crystallographic Data Centre (CCDC 901760 (2), 901761 (3)). Bond lengths, bond and torsion angles of 2 and 3 are given in tables 1–4 in the Supplementary material.
  • rmsd = root mean square deviation from planarity. hdp = highest deviation from planarity.
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