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A Tetranuclear Propane-1,3-Dithiolate Complex, [Fe2(CO)5{Ph2P(CH2)3}{(µ-SCH2)2CH2}]2, with a Bridging 1,6-Bis(diphenylphosphino)hexane Ligand

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Abstract

The 2:1 molar reaction of [Fe2(CO)6{(µ-SCH2)2CH2}] (1) and a bidentate diphosphine ligand, 1,6-bis(diphenylphosphino)hexane (dpph), in the presence of Me3NO resulted in the isolation of [Fe2(CO)5{Ph2P(CH2)3}{(µ-SCH2)2CH2}]2 (2) as red crystals in 71 % yield. The dpph ligand in compound 2, coordinates two Fe2S2 subunits as bridging mode and hence makes a linkage between two [Fe2(CO)5{(µ-SCH2)2CH2}] fragments. Each Fe2S2 butterfly of the complex consists of two fused Fe(S-C-C-C-S) six-membered rings, one of which attains a chair conformation, and the other is necessarily in a boat conformation. Compound 2 has unequivocally been characterized by elemental analysis, IR, 1H NMR and 31P NMR spectroscopy together with single crystal X-ray diffraction studies. Crystals of 2 are triclinic, space group P-1, a = 9.918(4) Å, b = 10.347(3) Å, c = 14.581(5) Å, α = 72.239(12)º, β = 80.342(12)º, γ = 68.550(14)º and Z = 1.

Graphic Abstract

A novel tetranuclear propane-1,3-dithiolate complex, [Fe2(CO)5{Ph2P(CH2)3}{(μ-SCH2)2CH2}]2 (2), bearing a bridging bis(diphenylphosphino)hexane (dpph) ligand, was synthesized from the Me3NO aided room temperature displacement of carbonyls from [Fe2(CO)6{(μ-SCH2)2CH2}] (1), and structurally characterized.

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Data Availability

Crystallographic data for the structural analysis of compound 2 have been deposited to the Cambridge Crystallographic Data Centre with CCDC number 2074713. These data may be obtained free of charge from The Director, Cambridge Crystallographic Database Centre, 12 Union Road Cambridge, CB2 1EZ, United Kingdom. (http://www.ccdc.cam.ac.uk).

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Acknowledgements

The authors acknowledge the University Grant Commission, Government of the People’s Republic of Bangladesh and Jahangirnagar University, for financial support, and Mr. Md. Emdad Hossain, Scientist, Wazed Miah Science Research Centre, Jahangirnagar University, for recording IR and 1H NMR spectra of the complex.

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  1. Department of Chemistry, Jahangirnagar University, Savar, 1342, Dhaka, Bangladesh

    Md. Mahfujar Rohman, Md Imran Hossain, Shafikul Islam & Md. Manzurul Karim

  2. Wazed Miah Science Research Center, Jahangirnagar University, Savar, 1342, Dhaka, Bangladesh

    Nikhil C. Bhoumik

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The draft manuscript was prepared by the corresponding author (SI). All authors contributed to edit the manuscript except MMK since he passed away while the research work was in progress. The final version of the manuscript was approved by all authors.

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Rohman, M.M., Hossain, M.I., Bhoumik, N.C. et al. A Tetranuclear Propane-1,3-Dithiolate Complex, [Fe2(CO)5{Ph2P(CH2)3}{(µ-SCH2)2CH2}]2, with a Bridging 1,6-Bis(diphenylphosphino)hexane Ligand. J Chem Crystallogr 52, 223–232 (2022). https://doi.org/10.1007/s10870-021-00910-4

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