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Preparation and Structure of Two Ditungsten Compounds Synthesized with the 3,5-Dichlorophenylformamidinate Ligand

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journal contribution
posted on 15.04.1999, 00:00 by Kathryn M. Carlson-Day, Judith L. Eglin, Laura T. Smith, Richard J. Staples
The structure, preparation, and spectroscopy of a W2(II, II) paddlewheel complex with four formamidinate ligands is reported. Upon exposure to air and moisture in solution, the W2(II, II) core undergoes an oxidative addition reaction to form a W2(III, III) edge-sharing bioctahedral (ESBO) complex with two bridging hydroxides. The products, W2(μ-DCPF)4 (1) and W2(μ-OH)2(μ-DCPF)22-DCPF)2 (2) where DCPF is [(3,5-Cl2C6H3)NC(H)N(3,5-Cl2C6H3)-], were characterized by UV−vis and 1H NMR spectroscopy. Structural data are presented for W2(μ-DCPF)4 with four bridging formamidinate ligands and W2(μ-OH)2(μ-DCPF)22-DCPF)2 with the formamidinate ligands in both chelating and bridging positions. Crystallographic data for W2(μ-DCPF)4 (1) and W2(μ-OH)2(μ-DCPF)22-DCPF)2 (2) are as follows:  (1), C68H60Cl16N8O4W2, a = 12.6906(3) Å, b = 12.7818(4) Å, c = 13.0450(3) Å, α = 109.173(1)°, β = 93.865(1)°, γ = 103.746(1)°, triclinic, P1̄ (No. 2), and Z = 1 and (2), C59H35Cl16N8O2W2, a = 17.1524(1) Å, b = 20.6568(3) Å, c = 19.3959(3) Å, β = 102.791(1)°, monoclinic, C2/c (No. 15), and Z = 4.