화학공학소재연구정보센터
Inorganic Chemistry, Vol.41, No.15, 3859-3865, 2002
Reaction of bis(phosphine)(hydrotris(3,5-dimethylpyrazolyl)borato)rhodium(I) with phenylacetylene, p-nitrobenzaidehyde, and triphenyltin hydride: Structures of [Rh(Tp*)(PPh3)(2)], [Rh(Tp*)(H)(C2Ph){P(4-C6H4F)(3)}], [Rh(Tp*)(H)(COC6H4-4-NO2)(PPh3)], and [Rh(Tp*)(H)(SnPh3)(PPh3)]
The complexes [Rh(Tp*)(PPh3)(2)] (1a) and [Rh(Tp*){P(4-C6H4F)(3)}(2)] (1b) combine with PhC2H, 4-NO2-C6H4CHO and Ph3SnH to give [Rh(Tp*)(H)(C2Ph)(PR3)] (R = Ph, 2a; R = 4-C6H6F, 2b), [Rh(Tp*)(H)(COC6H4-4-NO2)(PR3)] (R = Ph, 3a), and [Rh(Tp*)(H)(SnPh3)(PR3)] (R = Ph, 4a; R = 4-C6H4F, 4b) in moderate to good yield. Complexes la, 2b, 3a, and 4a have been structurally characterized. In la the Tp* ligand is bidentate, in 2b, 3a, and 4a it is tridentate. Crystal data for 1a: space group P2(1)/c; a = 11.9664(19), b = 21.355(3), c = 20.685(3) Angstrom; beta = 112.576(7)degrees; V = 4880.8(12) Angstrom(3); Z = 4; R = 0.0441. Data for 2b: space group P (1) over bar; a = 10.130(3), b = 12.869(4), c = 17.038(5) Angstrom; alpha = 78.641(6), beta = 76.040(5), gamma = 81.210(6)degrees; V = 2100.3(11) Angstrom(3); Z = 2; R = 0.0493. Data for 3a: space group P (1) over bar; a = 10.0073(11), b = 10.5116(12), c = 19.874(2) Angstrom; alpha = 83.728(2), beta = 88.759(2), gamma = 65.756(2)degrees; V = 1894.2(4) Angstrom(3); Z = 2; R = 0.0253. Data for 4a: space group P2(1)/c; a = 15.545(2), b = 18.110(2), c = 17.810(2) Angstrom; beta = 95.094(3)degrees; V = 4994.1 (10) Angstrom(3); Z = 4; R = 0.0256. NMR data (H-1, P-31, Rh-103, Sn-119) are also reported.