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Syntheses, molecular structures, and self-assemblies of SFe3, S2Fe3, S3Fe5, SeFe3, and Se2Fe3 clusters with chelating diaminocarbenes

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The reactions of substituted thioureas and selenoureas with iron carbonyls have been systematically investigated, and five types of SFe3, S2Fe3, S3Fe5, SeFe3, and Se2Fe3 clusters with chelating diaminocarbenes have been synthesized and characterized by X-ray crystallography. The reactions of C3H5NHC(=S)NHAr with Fe3(CO)12 afford (μ3-S)Fe3(CO)7(μ-CO)(κ3 C,C,C-C3H5NHCNHAr) (1, Ar = Ph; 2, Ar = 4-H2NC6H4). In contrast, the reactions of (2-C5H4N)NHC(=S)NHN=CHAr with Fe2(CO)9 form (μ3-S)2Fe3(CO)72 N,C-(2-C5H4N)NHCNHN=CHAr) (3, Ar = Ph; 4, Ar = 4-CH3C6H4). Likewise, reactions of GNHC(=S)NHC(=O)Ph with Fe3(CO)12 provide (μ3-S)2Fe3(CO)72 N,C-GNHCNHC(=O)Ph) (5, G = 2-C5H4N; 6, G = 2-C4H3N2) as well as Fe3(CO)8(μ-CO)22 N,C-(2-C4H3N2)NHCNHC(=O)Ph). The reaction of (2-C5H4N)NHC(=S)NH2 with Fe3(CO)12 gives (μ3-S)2Fe3(CO)72 N,C-(2-C5H4N)NHCNH2) (7). The reactions of GNHC(=S)NHPh with Fe3(CO)12 produce (μ3-S)2Fe3(CO)72 N,C-GNHCNHPh) (8, G = 2-C5H4N; 9, G = 2-C4H3N2). Analogously, (2-C5H4N)NHC(=S)NH(2-CH3C6H4) offers (μ3-S)2Fe3(CO)72 N,C-(2-C5H4N)NHCNH(2-CH3C6H4)) (10). However, (2-C5H4N)NHC(=S)NH(2-CH3OC6H4) generates (μ3-S)24-S)Fe5(CO)10(μ-CO)22 N,C-(2-C5H4N)NHCNH(2-CH3OC6H4)) (11). Furthermore, the reactions of (2-C5H4N)NHC(=S)NHR with Fe3(CO)12 form (μ3-S)24-S)Fe5(CO)10(μ-CO)22 N,C-(2-C5H4N)NHCNHR) (12, R = 2-H2NC6H4; 13, R = 4-H2NC6H4; 14, R = 2-C5H4N). Surprisingly, the reaction of (2-C5H4N)NHC(=S)NHC3H5 with Fe3(CO)12 leads to (μ3-S)24-S)Fe5(CO)10(μ-CO)22 N,C-(2-C5H4N)NHCNHC3H5) (15). The reaction of C3H5NHC(=Se)NHPh with Fe3(CO)12 affords (μ3-Se)Fe3(CO)7(μ-CO)(κ3 C,C,C-C3H5NHCNHPh) (16) as well as [(κ2 N,C-PhNCNHC3H5)Fe2(CO)64-Se)Fe2(CO)6]24-Se). As with (2-C4H3N2)NHC(=S)NHPh, (2-C4H3N2)NHC(=Se)NHPh offers (μ3-Se)2Fe3(CO)72 N,C-(2-C4H3N2)NHCNHPh) (17). Unlike (2-C5H4N)NHC(=S)NH(2-CH3OC6H4), (2-C5H4N)NHC(=Se)NH(2-CH3OC6H4) yields (μ3-Se)2Fe3(CO)72 N,C-(2-C5H4N)NHCNH(2-CH3OC6H4)) (18). By virtue of N–HN, N–HO, and C–HO intermolecular hydrogen bonds along with other non-covalent interactions, these new organometallic clusters exhibit interesting supramolecular structures.
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Keywords: Diaminocarbene; Fe/S cluster; Fe/Se cluster; Selenourea; Thiourea

Document Type: Research Article

Affiliations: College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou, PR China

Publication date: November 2, 2015

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