Reaction of Bis(phosphine)(hydrotris(3,5-dimethylpyrazolyl)borato)rhodium(I) with Phenylacetylene, <i>p</i>-Nitrobenzaldehyde, and Triphenyltin Hydride: Structures of [Rh(Tp*)(PPh<sub>3</sub>)<sub>2</sub>], [Rh(Tp*)(H)(C<sub>2</sub>Ph){P(4-C<sub>6</sub>H<sub>4</sub>F)<sub>3</sub>}], [Rh(Tp*)(H)(COC<sub>6</sub>H<sub>4</sub>-4-NO<sub>2</sub>)(PPh<sub>3</sub>)], and [Rh(Tp*)(H)(SnPh<sub>3</sub>)(PPh<sub>3</sub>)]
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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-C6H4F, 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 1a, 2b, 3a, and 4a have been structurally characterized. In 1a the Tp* ligand is bidentate, in 2b, 3a, and 4a it is tridentate. Crystal data for 1a: space group P21/c; a = 11.9664(19), b = 21.355(3), c = 20.685(3) Å; β = 112.576(7)°; V = 4880.8(12) Å3; Z = 4; R = 0.0441. Data for 2b: space group P1̄; a = 10.130(3), b = 12.869(4), c = 17.038(5) Å; α = 78.641(6), β = 76.040(5), γ = 81.210(6)°; V = 2100.3(11) Å3; Z = 2; R = 0.0493. Data for 3a: space group P1̄; a = 10.0073(11), b = 10.5116(12), c = 19.874(2) Å; α = 83.728(2), β = 88.759(2), γ = 65.756(2)°; V =1894.2(4) Å3; Z = 2; R = 0.0253. Data for 4a: space group P21/c; a = 15.545(2), b = 18.110(2), c = 17.810(2) Å; β = 95.094(3)°; V = 4994.1(10) Å3; Z = 4; R = 0.0256. NMR data (1H, 31P, 103Rh, 119Sn) are also reported.
