Gallium and Indium Complexes of Bis(amino thiol) (N(2)S(2)) Ligands |
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Authors: | Zheng Yong Yong Saluja Sunita Yap Glenn P A Blumenstein Michael Rheingold Arnold L Francesconi Lynn C |
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Institution: | Chemistry Departments Hunter College of the City University of New York, New York, New York 10021, and University of Delaware, Newark, Delaware 19716. |
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Abstract: | Three methods have been developed to prepare gallium and indium complexes of three tetradentate N(2)S(2) ligands of the general formula M(N(2)S(2))R (M = Ga, In; R = Cl, Br, SCN, O(2)CC(6)H(5)-O,O'). The ancillary ligand (Cl, SCN, O(2)CC(6)H(5)-O,O') was varied with the tetradentate ligand BAT-TM. X-ray crystallography shows that the coordination geometry about the d(10) metal ion is influenced by the steric requirements of the ligands. X-ray crystallography of four molecules results in the following data: GaCl(BAT-TM) (1), formula = C(10)H(22)ClGaN(2)S(2), space group = Pnma, a = 12.387(4) ?, b = 21.116(6) ?, c = 5.986(2) ?, V = 1565.8(9) ?(3), Z = 4; InCl(BAT-TM) (2), formula = C(10)H(22)ClInN(2)S(2), space group = Pnma, a = 12.968(9) ?, b = 29.29(1) ?, c = 5.866(2) ?, V = 1620(2) ?(3), Z = 4; InNCS(BAT-TM) (3), formula = C(11)H(24)ClInN(3)S(3), space group = Pbca, a = 11.812(3) ?, b = 11.679(3) ?, c = 24.238(9) ?, V = 3449.7 (17) ?(3), Z = 8; In(O,O'-O(2)CC(6)H(5))(BAT-TM) (4), formula = C(19)H(29)O(2)InN(2)S(2), space group = P2(1)/n, a = 10.783(2) ?, b = 18.708(4) ?, c = 12.335(4) ?, V = 2321.7(9) ?(3), Z = 4. Proton NMR studies show that the complexes are stable in solution; in polar solvents such as acetonitrile, for certain molecules, two metal-ligand complexes are observed. Similarly, two metal-ligand complexes are seen in NMR data taken in 80% acetonitrile/20% D(2)O (pD = 4.6) mixture. HPLC studies (acetonitrile/50 mM sodium acetate, pH = 4.6) show that the lipophilicity of the ligand determines the retention time of the complex. |
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