Dimetalated Crown Ether Schiff Base Palladacycles. Influence of the Carbon Chain Length on the Coordination Mode of Bidentate Phosphines. Crystal and Molecular Structure of the Novel Complex [Pd<sub>2</sub>{1,4-[C(H)═N{9,10-(C<sub>8</sub>H<sub>16</sub>O<sub>5</sub>)C<sub>6</sub>H<sub>3</sub>}]<sub>2</sub>C<sub>6</sub>H<sub>2</sub>-<i>C2,C5</i>}(Cl)<sub>2</sub>{μ-Ph<sub>2</sub>P(CH<sub>2</sub>)<sub>5</sub>PPh<sub>2</sub>}<sub>2</sub>]
作者:Alberto Fernández、Margarita López-Torres、Samuel Castro-Juiz、Manuel Merino、Digna Vázquez-García、José M. Vila、Jesús J. Fernández
DOI:10.1021/om100833w
日期:2011.2.14
N′}(Ph2PRPh2-P,P′)2][Cl]2 (8a, R = CH2; 9a, R = (CH2)2, respectively) with two chelating phosphines. With the longer chain diphosphines Ph2P(CH2)nPPh2 (n = 4, dppb; n = 5, dpppe; n = 6, dpph) in a 1:1 palladium/diphosphine molar ratio the dinuclear compounds [Pd21,4-[C(H)═N9,10-(C8H16O5)C6H3}]2C6H2-C2,C5}(Cl)2μ-Ph2P(CH2)nPPh2}2] (10a, n = 4; 11a, n = 5; 12a, n = 6) were obtained, with two diphosphines intramolecularly
源自对苯二甲醛和4的席夫碱配体1,4- [C(H)═N9,10-(C 8 H 16 O 5)C 6 H 3 }] 2 C 6 H 4(a)的反应'-氨基苯并-15-crown-5与Pd(OAc)2在氯仿中于50°C加热96小时,得到高分子化合物[Pd 2 1,4- [C(H)═N9,10- (C 8 H ^ 16 ö 5)C 6 H ^ 3 }] 2 c ^ 6 ħ 2 - C2,C5,N,N '}(μ-O 2 CME)2] n(1a)在C2和C5苯基碳原子上进行两次CHH活化后。1a与N t Bu 4 Cl或N t Bu 4 Br的饱和溶液发生复分解反应,得到[Pd 2 1,4- [C(H)═N9,10-(C 8 H 16 O 5)C 6 H 3 }] 2 C 6 H 2 - C2,C5,N,N '}(μ-Cl)2 ] n(2a)和[Pd 2 1,4- [C(H)═N9, 10-(C