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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 FeSO 4 /Na{S 2 P(p-C 6 H 4 Me) 2 } and CoCl 2 /Na{S 2 P(p-C 6 H 4 Me) 2 } in different organic solvents afford the mononuclear complexes [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (MeOH) 2 ], [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (THF),], [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (THT) 2 ],[Fe{S,P(p-C 6 H 4 Me) 2 } 2 (DMF) 2 ], [Co {S 2 P(p-C 6 H 4 Me),},(DMF) 2 ] which were isolated as crystalline [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (MeOH) 2 ]·2MeOH (1), [Fe{S,P(p-C 6 H 4 Me) 2 } 2 (THF) 2 ] (2), [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (THT) 2 ]-THT (3), [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (DMF) 2 ] · 2 DMF (4), and [Co{S 2 P(p-C 6 H 4 Me) 2 },(DMF) 2 ] · 2DMF (5), respectively. Crystals of 1 are monoclinic, space group P2 1 /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(R η ) = 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(R w ) = 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(R w ) = 0.057 (0.073). Crystals of 4 and 5 are monoclinic, space group P2 1 /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(R w ) = 0.045 (0.046) and 0.027 (0.033), respectively. The neutral complexes 1-5 contain six-coordinated metal centers with either MS 4 O 2  or MS 6  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.

zeitschrift für naturforschung b

Eisen- und Cobaltkomplexe mit Schwefelliganden: Darstellung und Kristallstrukturen von [Fe { S 2 P(p-C 6 H 4 Me) 2 } 2 (MeOH)2] · 2 MeOH, [Fe { S 2 P(p-C 6 H 4 Me) 2 } 2 (THF) 2 ], [Fe{ S 2 P(p-C 6 H 4 Me) 2 } 2 (THT) 2 ]· THT, [Fe { S 2 P(p-C 6 H 4 Me) 2 } 2 (DMF) 2 ]·2 DMF und [Co { S 2 P(p-C 6 H 4 Me) 2 } 2 (DMF) 2 ] · 2 DMF / Iron and Cobalt Complexes with Sulfur-Containing Ligands: Preparation and Crystal Structures of [Fe{S,P(p-C 6 H 4 Me),},(MeOH),] • 2 MeOH, [Fe{ S,P(p-C 6 H 4 Me) 2 } 2 (THF) 2 ], [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (THT) 2 ] · THT, [Fe{S 2 P(p-C 6 H 4 Me) 2 } 2 (DMF) 2 ] · 2 DMF, and [Co{S 2 P(p-C 6 H 4 Me) 2 } 2 (DMF) 2 ] · 2 DMF