摘要
Bis(diphenylphosphinyl)butadiyne reacted with methylcyclopentadiene at room temperature and four isomeric products were obtained. Crystal structures of isomers 1 and 3 have been determined. Crystal data for compound 1 C40H36O2P2·2CHCl3: monoclinic, space group C12/c1 with a = 17.983(2), b = 11.8723(12), c = 20.081(2) A, β = 111.218(3)°, V= 3996.5(8) A^3, Z = 4, Mr= 849.36, Dc = 1.412 g/cm^3, F(000) = 1752,μ = 0.546 mm^-1, the final R = 0.0351 and wR = 0.0951 for 3965 observed reflections (I 〉 2σ(I)); and those for compound 3 C40H36O2P2·H2O: triclinic, space group PI with a = 10.4144(15), b = 13.0558(18), c = 13.742(2) A, a = 70.453(8), β = 75.382(8), γ = 72.312(8)°, V = 1653.7(4) A^3, Z = 2, Mr= 628.64, Dc = 1.262 g/cm^3, F(000) = 664,μ = 0.169 mm^-1, the final R = 0.0593 and wR = 0.1296 for 4891 observed reflections (I 〉 2σ(I)). The structures of the other two isomers are identified via IR, ^1H NMR and MS spectra.
Bis(diphenylphosphinyl)butadiyne reacted with methylcyclopentadiene at room temperature and four isomeric products were obtained. Crystal structures of isomers 1 and 3 have been determined. Crystal data for compound 1 C40H36O2P2·2CHCl3: monoclinic, space group C12/c1 with a = 17.983(2), b = 11.8723(12), c = 20.081(2) A, β = 111.218(3)°, V= 3996.5(8) A^3, Z = 4, Mr= 849.36, Dc = 1.412 g/cm^3, F(000) = 1752,μ = 0.546 mm^-1, the final R = 0.0351 and wR = 0.0951 for 3965 observed reflections (I 〉 2σ(I)); and those for compound 3 C40H36O2P2·H2O: triclinic, space group PI with a = 10.4144(15), b = 13.0558(18), c = 13.742(2) A, a = 70.453(8), β = 75.382(8), γ = 72.312(8)°, V = 1653.7(4) A^3, Z = 2, Mr= 628.64, Dc = 1.262 g/cm^3, F(000) = 664,μ = 0.169 mm^-1, the final R = 0.0593 and wR = 0.1296 for 4891 observed reflections (I 〉 2σ(I)). The structures of the other two isomers are identified via IR, ^1H NMR and MS spectra.
基金
Sponsored by the Scientific Research Foundation for the Returned Overseas Chinese Scholars and the State Education Ministry