A Tetranuclear Propane-1,3-Dithiolate Complex, [Fe.sub.2hexane Ligand

• Published in: Journal of chemical crystallography Vol. 52; no. 2; p. 223
• Main Authors: Rohman, Md. Mahfujar, Hossain, Md Imran, Bhoumik, Nikhil C, Islam, Shafikul, Karim, Md. Manzurul
• Format: Journal Article
• Language: English
• Published: Springer 01-06-2022
• Subjects: Diffraction; Nuclear magnetic resonance spectroscopy; Propane; X-rays
• ISSN: 1074-1542
• DOI: 10.1007/s10870-021-00910-4

The 2:1 molar reaction of [Fe.sub.2(CO).sub.6{([micro]-SCH.sub.2).sub.2CH.sub.2}] (1) and a bidentate diphosphine ligand, 1,6-bis(diphenylphosphino)hexane (dpph), in the presence of Me.sub.3NO resulted in the isolation of [Fe.sub.2(CO).sub.5{Ph.sub.2P(CH.sub.2).sub.3}{([micro]-SCH.sub.2).sub.2CH.sub.2}].sub.2 (2) as red crystals in 71 % yield. The dpph ligand in compound 2, coordinates two Fe.sub.2S.sub.2 subunits as bridging mode and hence makes a linkage between two [Fe.sub.2(CO).sub.5{([micro]-SCH.sub.2).sub.2CH.sub.2}] fragments. Each Fe.sub.2S.sub.2 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, .sup.1H NMR and .sup.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, [alpha] = 72.239(12)º, [beta] = 80.342(12)º, [gamma] = 68.550(14)º and Z = 1. Graphic A novel tetranuclear propane-1,3-dithiolate complex, [Fe.sub.2(CO).sub.5{Ph.sub.2P(CH.sub.2).sub.3}{([mu]-SCH.sub.2).sub.2CH.sub.2}].sub.2 (2), bearing a bridging bis(diphenylphosphino)hexane (dpph) ligand, was synthesized from the Me.sub.3NO aided room temperature displacement of carbonyls from [Fe.sub.2(CO).sub.6{([mu]-SCH.sub.2).sub.2CH.sub.2}] (1), and structurally characterized.