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Synthesis, Structural Characterization and Hirshfeld Analysis of Ag(I), Au(I), Cd(II) and Hg(II) Complexes Containing Hemilabile- Ferrocenylbisphosphine [Fe{C<inf>5</inf>H<inf>4</inf>P(C<inf>6</inf>H<inf>4</inf>CH<inf>2</inf>NMe<inf>2</inf>-o)<inf>2</inf>}<inf>2</inf>]
Journal
Journal of Chemical Crystallography
ISSN
10741542
Date Issued
2023-06-01
Author(s)
Mondal, Dipanjan
Rao, Sowmya
Mague, Joel T.
Balakrishna, Maravanji S.
Abstract
The reaction between bis(phosphino)ferrocene, [Fe{C5H4P(C6H4CH2NMe2-o)2}2] (1) and AgOTf resulted in disilver complex [(AgOTf)2{µ-Fe{C5H4P(C6H4CH2NMe2)2}2}] (2) which on further treatment with 2,2′-bipyrdine yielded a mixed-ligand complex [Ag2(bipy)2{µ-Fe{C5H4P(C6H4CH2NMe2)2}2}](OTf)2 (3). Reaction of 1 with AuCl(SMe2) in 1:2 molar ratio afforded a digold complex [(AuCl)2Fe{C5H4P(C6H4CH2NMe2)2}2] (4). Treatment of 4 with anhydrous CdCl2 resulted in heterometallic complex [Fe{C5H4P(AuCl)(C6H4CH2NMe2)2(CdCl2)}2] (5). The reactions of 1 with anhydrous CdI2 and HgI2 in 1:2 molar ratios yielded bimetallic complexes [Fe{C5H4P(CdI2)(C6H4CH2NMe2)2}2] (6) and [Fe{C5H4P(HgI2)(C6H4CH2NMe2)2}2] (7), respectively. The molecular structures of 3, 4 and 7 were confirmed by single crystal X-ray analysis. Complexes 3 and 7 crystallized in the triclinic space group with P-1, whereas 4 crystallized in the monoclinic space group with C2/c. Single crystals suitable for X-ray crystallography were obtained using diffusion method where a solution of [Fe{C5H4P(C6H4CH2NMe2)2}2] (1) in dichloromethane was layered on a solution of CdI2 and HgI2 in methanol and stored at room temperature for 24 h, resulted in yellow plates of 6 and 7, respectively. All complexes crystallized with the asymmetric unit containing half a molecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of 3 are from H‧‧‧H (50.2%), C‧‧‧H/H‧‧‧C (8.3%), Cl‧‧‧H/H‧‧‧Cl (12.1%), O‧‧‧H/H‧‧‧O (11.3%), F‧‧‧H/H‧‧‧F (9.0%) contacts, while those for 4 are from H‧‧‧H (73.7%), C‧‧‧H/H‧‧‧C (8.9%), Cl‧‧‧H/H‧‧‧Cl (14.5%), Au‧‧‧H/H‧‧‧Au (1.8%) and N‧‧‧H/H‧‧‧N (0.8%) contacts, and those for 7 are from H‧‧‧H (65.5%), C‧‧‧H/H‧‧‧C (6.6%), I‧‧‧H/H‧‧‧I (24.1%) and I‧‧‧C/C‧‧‧I (2.9%) contacts. Graphical Abstract: Crystal structures of silver(I), gold(I) and mercury(II) complexes containing [Fe{C5H4P(C6H4CH2NMe2)2}2] (1) are described.[Figure not available: see fulltext.].
Volume
53
Subjects