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N,N,N ',N '-Tetrakis(2-pyridylmethyl)ethylenediamine and its analogues as hypodentate ligands. Synthesis and characterization of the rhodium(III), ruthenium(II), and palladium(II) complexes.

作者信息

Sokolov Maxim, Umakoshi Keisuke, Sasaki Yoichi

机构信息

Institute of Inorganic Chemistry, Novosibirsk, Russia.

出版信息

Inorg Chem. 2002 Dec 2;41(24):6237-43. doi: 10.1021/ic0203264.

DOI:10.1021/ic0203264
PMID:12444765
Abstract

New complexes of Rh(III), Ru(II), and Pd(II) with N,N,N',N'-tetrakis(2-pyridylmethyl)ethylenediamine (tpen) and its analogues have been prepared. The reaction of RhCl(3).nH(2)O with tpen is slow and allows one to isolate the products of three consecutive substitution steps: Rh(2)Cl(6)(tpen) (1), cis-RhCl(2)(eta(4)-tpen) (2), and RhCl(eta(5)-tpen) (3). In acetonitrile the reaction stops at the step of the formation of cis-RhCl(2)(eta(4)-tpen), whereas RhCl(eta(5)-tpen) is the final product of the further reaction in ethanol. Fully chelated Rh(tpen) could not be obtained. Bis(acetylacetonato)palladium(II), Pd(acac)(2), reacts with tpen and its analogues, N,N,N',N'-tetrakis(2-pyridylmethyl)-1,3-propanediamine (tptn) and N,N,N',N'-tetrakis(2-pyridylmethyl)-(R)-1,2-propylenediamine (R-tppn), to give Pd(eta(4)-tpen) (4), Pd(eta(4)-tppn) (5), and Pd(eta(4)-tptn) (6), respectively. Two pyridyl arms remain uncoordinated in these cases. The formation of unstable Pd(III) complexes from these Pd(II) complexes in solution was suggested on the basis of electrochemical measurements. Ruthenium(III) trichloride, RuCl(3).nH(2)O, is reduced to give a Ru(II) complex with fully coordinated tpen, Ru(tpen) (7). The same product was obtained in a more straightforward reaction of Ru(II)Cl(2)(dimethyl sulfoxide)(4) with tpen. Electrochemical studies showed a quasi-reversible Ru(tpen) couple for 7(2) (E(1/2) = 1.05 V vs Ag/AgCl). Crystal structures of 2.2CH(3)CN, 3(2).CH(3)CN, 6(2), and 7(2).0.5H(2)O were determined. Crystal data: 2.2CH(3)CN, monoclinic, C2, a = 16.974(4) A, b = 8.064(3) A, c = 13.247(3) A, beta = 106.37(2) degrees, V = 1739.9(8) A(3), Z = 2; 3(2).CH(3)CN, triclinic, P1, a = 11.430(1) A, b = 19.234(3) A, c = 8.101(1) A, alpha = 99.43(1) degrees, beta = 93.89(1) degrees, gamma = 80.10(1) degrees, V = 1729.3(4) A(3), Z = 2; 6(2), orthorhombic, Pnna, a = 8.147(1) A, b = 25.57(1) A, c = 14.770(4) A, V = 3076(3) A(3), Z = 4; 7(2).0.5H(2)O, monoclinic, P2(1)/c, a = 10.046(7) A, b = 19.049(2) A, c = 15.696(3) A, beta = 101.46(3) degrees, V = 2943(2) A(3), Z = 4.

摘要

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