期刊
JOURNAL OF ORGANOMETALLIC CHEMISTRY
卷 694, 期 15, 页码 2434-2441出版社
ELSEVIER SCIENCE SA
DOI: 10.1016/j.jorganchem.2009.03.013
关键词
Crystal structures of diorganotin(IV) complexes; C-13/Sn-119 NMR; H,H-COSY; gs-HMQC and gs-HMBC
资金
- University Grant Commission, New Delhi, India
- Czech Republic [203/03/1118]
- [PSW-004/03-04]
Two diorganotin(IV) complexes of the general formula R2Sn[Ph(O)C=CH-C(Me)=N-C6H4(O)] (R = Ph, 1a; R = Me, 1b) have been synthesized from the corresponding diorganotin(IV) dichlorides and the ligand, 3-(2-hydroxyphenylimino)-1-phenylbutan-1-one (1) in methanol at room temperature in presence of triethylamine. Both compounds have been characterized by elemental analyses, IR and H-1, C-13, N-15, Sn-119 NMR spectra. The structures of the free ligand and the complexes have been confirmed by single crystal X-ray diffraction. There are three independent molecules in the crystal structure of the ligand 1 and in all three the O-bound proton is transferred to the imine nitrogen and makes an intramolecular N-H center dot center dot center dot O hydrogen bond with the carbonyl oxygen. In turn this makes an intermolecular hydrogen bond with the phenolic H atom. The crystal structure of 1 is trigonal and a new polymorph; triclinic and monoclinic forms have already been published. In 1a, the central tin atom adopts distorted trigonal-bipyramidal coordination geometry whereas in dimeric 1b it is distorted octahedral when including the intermolecular Sn-O(phenolic) bond [2.7998(20)angstrom]. The delta (Sn-119) values for the complexes 1a and 1b are -306.6 and -127.9 ppm, respectively, thus indicating penta-coordinated Sn centres in solution. (C) 2009 Published by Elsevier B.V.
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