Eisen- und Cobaltkomplexe mit Schwefelliganden: Darstellung und Kristallstrukturen von [Fe { S2P(p-C6H4Me)2}2(MeOH)2] · 2 MeOH, [Fe { S2P(p-C6H4Me)2}2(THF)2], [Fe{ S2P(p-C6H4Me)2}2(THT)2]· THT, [Fe { S2P(p-C6H4Me)2}2(DMF)2]·2 DMF und [Co { S2P(p-C6H4Me)2}2(DMF)2] · 2 DMF / Iron and Cobalt Complexes with Sulfur-Containing Ligands: Preparation and Crystal Structures of [Fe{S,P(p-C6H4Me),},(MeOH),] • 2 MeOH, [Fe{ S,P(p-C6H4Me)2}2(THF)2], [Fe{S2P(p-C6H4Me)2}2(THT)2] · THT, [Fe{S2P(p-C6H4Me)2}2(DMF)2] · 2 DMF, and [Co{S2P(p-C6H4Me)2}2(DMF)2] · 2 DMF

Kristin Kirschbaum 1 , Klaus Greiwe 1 , Kay Müller 1 , Henry Strasdeit 1 , Bernt Krebs 1 , and Gerald Henkel 1
  • 1 Anorganisch-Chemisches Institut der Universität, Wilhelm-Klemm-Straße 8, D-4400 Münster, Bundesrepublik Deutschland Fachgebiet Anorganische Chemie/Festkörperchemie der Universität, Lotharstraße 1, D-4100 Duisburg 1, Bundesrepublik Deutschland

A series of novel Fe(II) and Co(II) complexes containing dithiophosphinate groups and neutral ligands with sulfur and oxygen donor functions was prepared in non-aqueous solutions. The reaction systems FeSO4/Na{S2P(p-C6H4Me)2} and CoCl2/Na{S2P(p-C6H4Me)2} in different organic solvents afford the mononuclear complexes [Fe{S2P(p-C6H4Me)2}2(MeOH)2], [Fe{S2P(p-C6H4Me)2}2(THF),], [Fe{S2P(p-C6H4Me)2}2(THT)2],[Fe{S,P(p-C6H4Me)2}2(DMF)2], [Co {S2P(p-C6H4Me),},(DMF)2] which were isolated as crystalline [Fe{S2P(p-C6H4Me)2}2(MeOH)2]·2MeOH (1), [Fe{S,P(p-C6H4Me)2}2(THF)2] (2), [Fe{S2P(p-C6H4Me)2}2(THT)2]-THT (3), [Fe{S2P(p-C6H4Me)2}2(DMF)2] · 2 DMF (4), and [Co{S2P(p-C6H4Me)2},(DMF)2] · 2DMF (5), respectively. Crystals of 1 are monoclinic, space group P21/c. Z – 2, a⁻ 11.013(3), b = 14.402(3), c = 11 600(3) Å. β = 106.25(2). The structure of 1 was refined to R(Rη) = 0.030 (0.040). Compound 2 is triclinic, space group P 1, Ζ = 1 with a = 6.921(2), b = 9.353(3), c = 14.436(4) Å, α = 83.56(3), β = 85.39(3) and γ = 80.46(2). Its structure was refined to R(Rw) = 0.029 (0.035). 3 crystallizes in the triclinic space group P l̄ with a = 9.204(3), b = 11.378(3), c = 11.389(4) Å α = 97.41(3), β = 114.00(2), γ = 100.69(2) and Ζ = 1. The refinement converged to R(Rw) = 0.057 (0.073). Crystals of 4 and 5 are monoclinic, space group P21/n (Z = 2): Fe(II), a = 12.395(3), b = 11.077(2), c = 16.377(4) Å, β = 95.51(2); Co(II),α= 12.299(3), b = 11.055(2), c = 16.452(4) Å, β = 95.90(2). The refinements converged to R(Rw) = 0.045 (0.046) and 0.027 (0.033), respectively. The neutral complexes 1-5 contain six-coordinated metal centers with either MS4O2 or MS6 chromophores. They represent the first examples of structurally defined mononuclear Fe(II) and Co(II) complexes containing 1,1-dithiolate groups as well as additional neutral ligands with sulfur or oxygen donor functions.

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