The reaction of triphenylstannyl-bis(3,5-dimethyl-4-ethylpyrazol-1-yl)methane with W(CO)5THF yields the title compound (C37.5H39.5N4O3SnW, Mr = 896.79) which is of triclinic, space group P with a = 9.755(3), b = 13.69...The reaction of triphenylstannyl-bis(3,5-dimethyl-4-ethylpyrazol-1-yl)methane with W(CO)5THF yields the title compound (C37.5H39.5N4O3SnW, Mr = 896.79) which is of triclinic, space group P with a = 9.755(3), b = 13.696(4), c = 14.359(5) , a = 96.202(7), b = 93.313(6), g = 94.845(6)o, V = 1896(1) 3, Z = 2, Dc = 1.571 g/cm3, l(MoKa) = 0.71073 , m = 3.728 mm-1, F(000) = 881, R = 0.0491 and wR = 0.0856 for 4242 observed reflections (I≥2s(I)). The crystal structural analysis indicates that bis(3,5-dimethyl-4-ethylpyrazol-1-yl)methide acts as a tridentate monoanionic k3-[N,C,N] chelating ligand, and four-membered metallacycles are found in this heterodinuclear complex.展开更多
A new his (pyrazol-1-yl) methane ligand, [Ph-2 (HO) CCH (3, 5-Me(2)Pz)(2), Pz = pyrazole] (1), with a bulky substituent on the methine carbon atom has been successfully synthesized by the reaction of bis(3,5-dimethylp...A new his (pyrazol-1-yl) methane ligand, [Ph-2 (HO) CCH (3, 5-Me(2)Pz)(2), Pz = pyrazole] (1), with a bulky substituent on the methine carbon atom has been successfully synthesized by the reaction of bis(3,5-dimethylpyrazol-1-yl) methyllithium with benzophenone. Treatment of this ligand with W (CO)6 under UV-irradiation in THF at room temperature afforded a novel dinuclear complex CH2[3,5-Me(2)PzW(CO)(5)](2) (2) with loss of the Ph2CO fragment, which was characterized by IR, H-1 NMR spectra and elemental analyses as well as the X-ray single crystal diffraction analysis. This compound crystallizes in the orthorhombic space group Pbcn, with a = 1.7690 (3) nm, b = 1. 4460 (3) nm, c = 1.2994 (2) nm, Z = 4, V = 3.3239 (10) nm(3), D, = 1.775 g (.) cm(-3), mu = 6.967 mm(-1), F (000) = 1672, R-1 = 0.0414 and wR(2) = 0.0988. Bis (3, 5-dimethylpyrazol-1-yl) methane acts as a bridging bidentate tigand in this complex, which links two W(CO)(5) fragments. In addition, heating this complex under reflux in 1,2-dimethoxyethane (DME) gives the known chelated mononuclear complex CH2(3,5-Me(2)Pz)(2)W(CO)(4) (3).展开更多
基金the National Natural Science Foundation of China (No. 20172029)
文摘The reaction of triphenylstannyl-bis(3,5-dimethyl-4-ethylpyrazol-1-yl)methane with W(CO)5THF yields the title compound (C37.5H39.5N4O3SnW, Mr = 896.79) which is of triclinic, space group P with a = 9.755(3), b = 13.696(4), c = 14.359(5) , a = 96.202(7), b = 93.313(6), g = 94.845(6)o, V = 1896(1) 3, Z = 2, Dc = 1.571 g/cm3, l(MoKa) = 0.71073 , m = 3.728 mm-1, F(000) = 881, R = 0.0491 and wR = 0.0856 for 4242 observed reflections (I≥2s(I)). The crystal structural analysis indicates that bis(3,5-dimethyl-4-ethylpyrazol-1-yl)methide acts as a tridentate monoanionic k3-[N,C,N] chelating ligand, and four-membered metallacycles are found in this heterodinuclear complex.
基金ProjectsupportedbytheNationalNaturalScienceFoundationofChina (No .2 0 172 0 2 9)
文摘A new his (pyrazol-1-yl) methane ligand, [Ph-2 (HO) CCH (3, 5-Me(2)Pz)(2), Pz = pyrazole] (1), with a bulky substituent on the methine carbon atom has been successfully synthesized by the reaction of bis(3,5-dimethylpyrazol-1-yl) methyllithium with benzophenone. Treatment of this ligand with W (CO)6 under UV-irradiation in THF at room temperature afforded a novel dinuclear complex CH2[3,5-Me(2)PzW(CO)(5)](2) (2) with loss of the Ph2CO fragment, which was characterized by IR, H-1 NMR spectra and elemental analyses as well as the X-ray single crystal diffraction analysis. This compound crystallizes in the orthorhombic space group Pbcn, with a = 1.7690 (3) nm, b = 1. 4460 (3) nm, c = 1.2994 (2) nm, Z = 4, V = 3.3239 (10) nm(3), D, = 1.775 g (.) cm(-3), mu = 6.967 mm(-1), F (000) = 1672, R-1 = 0.0414 and wR(2) = 0.0988. Bis (3, 5-dimethylpyrazol-1-yl) methane acts as a bridging bidentate tigand in this complex, which links two W(CO)(5) fragments. In addition, heating this complex under reflux in 1,2-dimethoxyethane (DME) gives the known chelated mononuclear complex CH2(3,5-Me(2)Pz)(2)W(CO)(4) (3).
