Synthesis, Spectroscopic Characterization of Bis-[oxo-bis(4-ferrocenylbenzoato dialkyltin(IV))] and Crystal Structural Studies of the Former Compound

Abstract

Abstract: In this paper, the novel compounds { [( n Bu)₂Sn(4 Fc C₆H₄COO)]₂O}₂(1) and { [( n Oct)₂Sn(4 Fc C₆H₄COO)]₂O}₂(2)(Fc=ferrocenyl) have been synthesized and characterized by elemental analysis, IRand NMR( ¹H, ¹³C and¹¹⁹Sn) spectroscopy. The crystal structure of compound 1 has been determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group P2₁/c . The cell parameters are: a =1.2988(1) nm, b =2.4655(1) nm, c =3.4506 (1) nm, β =91.556(2)°, V =11.0454(1) nm³, Z =4. The structure was refined to final R_f=0.071, R_w= 0.074 . Compound 1 is a dimer structure mode with a four-member central endo-cyclic Sn₂O₂ unit in which the bridged oxygen atoms are tri coordinated. Each bridged oxygen atom also connects an exo-cyclic tin atom. Both endo and exo-cyclic tin atoms are all five coordination and have coordination geometry of monocapped trigonal bipyramid with very similarly distorted mode. Four carboxylate ligands are divided into two types. Two of the carboxylate ligands are bidentate and bridging to each pair of exo-and endo-cyclic tin atoms by using both oxygen atoms. The others are monodentate and coordinate each exo-cyclic tin atom. When considering further the longer distance interactions between the carboxyl oxygen in carboxylate ligand and endo cyclic tin atom (0.2775—0.2866 nm) and between the ester oxygen in carboxylate ligand and exo-cyclic tin atom(0.2980—0.3006 nm), not only carboxylate ligand chelates to exo-cyclic tin by anisobidentate mode but also their ester oxygen itself is tricoordinated and bridges to both endo and exo-cyclic tin atoms. In compound 1, the coplanarity of two conjugate systems(benzoyloxy group and substituted Cp ring) is not good. And two conjugate systems can not be coplanar with the central endo cyclic Sn₂O₂ unit. Unlike the general compounds characteristic of { [R₂Sn(O₂CR′)]₂O}₂, there is no center of symmetry in the molecule structure of compound 1.

Key words: Dialkyltin carboxylate, Ferrocene, Spectroscopic characterization, Crystal structure

CLC Number:

O627.7

TrendMD:

LU Wen-Guan, TAO Jia-Xun, WANG Yu-Zhen. Synthesis, Spectroscopic Characterization of Bis-[oxo-bis(4-ferrocenylbenzoato dialkyltin(IV))] and Crystal Structural Studies of the Former Compound[J]. Chem. J. Chinese Universities, 2000, 21(4): 501.

References

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