A Novel Cadmium Aminophosphonate: X-ray Powder Diffraction Structure, Solid-State IR and NMR Spectroscopic Determination of the Fine Structure of the Organic Moieties
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- 作者：Ekaterina V. Bakhmutova-Albert ; Naima Bestaoui ; Vladimir I. Bakhmutov ; Abraham Clearfield ; Anna Vega Rodriguez ; and Ricardo Llavona
- 刊名：Inorganic Chemistry
- 出版年：2004
- 出版时间：February 23, 2004
- 年：2004
- 卷：43
- 期：4
- 页码：1264 - 1272
- 全文大小：211K
- 年卷期：v.43,no.4(February 23, 2004)
- ISSN：1520-510X
文摘
A new divalent cadmium phosphonate, Cd2Cl2(H2O)4(H2L), has been synthesized from the ethylenediamine-N,N'-bis(methylenephosphonic acid) (H4L). The obtained microcrystalline compound has been characterized by solid-state IR spectra and 13C, 31P, and 113Cd CP MAS NMR. The static 13P NMR spectra have been also recorded togive the 
11, 22, and 33 chemical shift parameters for both compounds. The spectral data, collected for Cd2Cl2(H2O)4(H2L), are in an agreement with its X-ray powder diffraction structure solved with the cell dimensions a =16.6105(10), b = 7.1572(4), and c = 6.8171(4) Å and 
= 98.327(4)
. The octahedral coordination sphere of thecadmium atoms consists of two phosphonate oxygen atoms, two water oxygen atoms, and the two chlorine atoms.Cadmium atoms are bridged by the chlorine atoms forming four-membered rings. The phosphorus atoms exhibita tetrahedral coordination with two oxygen atoms bonded to the cadmium atoms with P-O distances of 1.503(10)and 1.504(10) Å. The third oxygen atom, showing a longer P-O distance (1.546(9) Å), is not bonded to the metalcenter, nor is it bonded to a proton. The combined IR and NMR proton-phosphorus cross-polarization kinetic datatogether with the X-ray data confirm that the cadmium phosphonate has the zwitterionic structure (NH2+CH2P(O2Cd2)O-)similar to the initial aminophosphonic acid H4L.
11, 22, and 33 chemical shift parameters for both compounds. The spectral data, collected for Cd2Cl2(H2O)4(H2L), are in an agreement with its X-ray powder diffraction structure solved with the cell dimensions a =16.6105(10), b = 7.1572(4), and c = 6.8171(4) Å and = 98.327(4). The octahedral coordination sphere of thecadmium atoms consists of two phosphonate oxygen atoms, two water oxygen atoms, and the two chlorine atoms.Cadmium atoms are bridged by the chlorine atoms forming four-membered rings. The phosphorus atoms exhibita tetrahedral coordination with two oxygen atoms bonded to the cadmium atoms with P-O distances of 1.503(10)and 1.504(10) Å. The third oxygen atom, showing a longer P-O distance (1.546(9) Å), is not bonded to the metalcenter, nor is it bonded to a proton. The combined IR and NMR proton-phosphorus cross-polarization kinetic datatogether with the X-ray data confirm that the cadmium phosphonate has the zwitterionic structure (NH2+CH2P(O2Cd2)O-)similar to the initial aminophosphonic acid H4L.