Functionalized cyclopalladated compounds with bidentate Group 15 donor atom ligands: the crystal and molecular structures of [{Pd[5-(COH)C6H3C(H)
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- 作者：Ares ; Raquel ; Ló ; pez-Torres ; Margarita ; Ferná ; ndez ; Alberto ; Pereira ; Ma Teresa ; et. al.
- 关键词：Palladium ; Metallation ; Phosphines ; As ligands ; X-ray diffraction
- 刊名：Journal of Organometallic Chemistry
- 出版年：2003
- 出版时间：January 3, 2003
- 年：2003
- 卷：665
- 期：1-2
- 页码：76-86
- 全文大小：559 K
文摘
The chloro-bridged dinuclear compound [{Pd[5-(COH)C6H3C(H)
N(Cy)-C2,N]}(μ-Cl)]2 (1), reacts with tertiary diphosphines in 1:1 molar ratio to give [{Pd[5-(COH)C6H3C(H)NCy-C2,N](Cl)}2(μ-Ph2PRPPh2)] (R: CH2, 2; CH2CH2, 3; (CH2)4, 4; (CH2)6, 5; Fe(C5H4)2, 6; trans-CHCH, 7; C≡C, 8). Treatment of 1 with Ph2PCH2CH2AsPh2 (arphos) gives the dinuclear complex [{Pd[5-(COH)C6H3C(H)N(Cy)-C2,N](Cl)}2(μ-Ph2PCH2CH2AsPh2)] (9). The reaction of 1 with tertiary diphosphines or arphos in 1:2 molar ratio in the presence of NH4PF6 yields the mononuclear compounds [Pd{5-(COH)C6H3C(H)NCy-C2,N}(Ph2PRPPh2-P,P)][PF6] (R: (CH2)4, 10; (CH2)6, 11; Fe(C5H4)2, 12; 1,2-C6H4, 13; cis-CHCH, 14; NH, 15) and [Pd{5-(COH)C6H3C(H)N(Cy)-C2,N}(Ph2PCH2CH2AsPh2-P,As)][PF6] (16). 1H-, 31P-{1H}- and 13C-{1H}-NMR, IR and mass spectroscopic data are given. The crystal structures of compounds 3, 6, 9 and 16 have been determined by X-ray crystallography.
N(Cy)-C2,N]}(μ-Cl)]2 (1), reacts with tertiary diphosphines in 1:1 molar ratio to give [{Pd[5-(COH)C6H3C(H)NCy-C2,N](Cl)}2(μ-Ph2PRPPh2)] (R: CH2, 2; CH2CH2, 3; (CH2)4, 4; (CH2)6, 5; Fe(C5H4)2, 6; trans-CHCH, 7; C≡C, 8). Treatment of 1 with Ph2PCH2CH2AsPh2 (arphos) gives the dinuclear complex [{Pd[5-(COH)C6H3C(H)N(Cy)-C2,N](Cl)}2(μ-Ph2PCH2CH2AsPh2)] (9). The reaction of 1 with tertiary diphosphines or arphos in 1:2 molar ratio in the presence of NH4PF6 yields the mononuclear compounds [Pd{5-(COH)C6H3C(H)NCy-C2,N}(Ph2PRPPh2-P,P)][PF6] (R: (CH2)4, 10; (CH2)6, 11; Fe(C5H4)2, 12; 1,2-C6H4, 13; cis-CHCH, 14; NH, 15) and [Pd{5-(COH)C6H3C(H)N(Cy)-C2,N}(Ph2PCH2CH2AsPh2-P,As)][PF6] (16). 1H-, 31P-{1H}- and 13C-{1H}-NMR, IR and mass spectroscopic data are given. The crystal structures of compounds 3, 6, 9 and 16 have been determined by X-ray crystallography.