Citation:
Lu Wen-Guan, Tao Jia-Xun, Li Xu-Yu, Wang Yu-Zhen. Synthesis and Characterization of Bis-[oxo-bis(β-ferrocenyl trans-propenoic di-n-butyltin(IV))][J]. Acta Physico-Chimica Sinica,
;2001, 17(09): 836-839.
doi:
10.3866/PKU.WHXB20010916
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The novel complex {[FcCH=CHCO2Sn(nBu)2]2O}2(A) has been synthesized by the reaction of (nBu)2SnO with βFcCH=CHCO2H (Fc=ferrocenyl). This molecule has a center of the structure SnO(Sn2)OSn by elemental analysis, IR and NMR (1H, 13C and 119Sn) spectra. A principle is put firstly forward to assign each carbon peak of the alkyl groups in the type of complex[(RCOOSnR′2)2O]2:(1) to distinguish the endo and exocyclic tin using 119Sn NMR spectrum. The 119Sn signal with larger linewidth should be assigned as an endocyclic tin; (2) to find out which proton of the alkyl chain bonded with endo(or exo)cyclic tin using 1H119Sn HMQC spectrum. The proton of cross peaks through 4J(1H119Sn) coupling which occurs simultaneously to both endo and exocyclic tin should belong to one of the alkyl chain binding directly to endocyclic tin. The proton of cross peak through 4J(1H-119Sn) coupling which occurs only to endo cyclic tin should belong to one of the alkyl chain binding directly to exocyclic tin; (3)to assign each 13C peak of the CH2 groups on alkyl chains through 2D 13C-1H COSY spectrum; (4)to find out which 13C peak of alkyl chains is bonded with endo or exocyclic tin, according to general principle that the 13C peak with higher field should correspond to the proton peak with higher field, that is, if the chemical shift of proton on the alkyl chain bonding directly to endocyclic tin locates at higher field, its related 13C peak located at higher field should belong to endocyclic tin.
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