A Ni（Ⅱ） complex [Ni（bdpm）2（OAc）]2（N3）2.5H20 （bdpm = bis（3,5-dimethylpyrazol-1-yl）-methane） was synthesized and characterized by elemental analysis, 1R and single-crystal X-ray diffraction. It crystallizes...A Ni（Ⅱ） complex [Ni（bdpm）2（OAc）]2（N3）2.5H20 （bdpm = bis（3,5-dimethylpyrazol-1-yl）-methane） was synthesized and characterized by elemental analysis, 1R and single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 18.630（2）, b = 16.6624（19）, c = 19.821（2） A, fl = 90.146（2）°, V = 6152.9（12） A3, Z = 4, C48H80N22Ni2O9, Mr = 1226.76, Dc = 1.324 g/cm^3, F（000） = 2600 and μ = 0.680 mm^-1. The structure was refined to the final R = 0.0578 and wR = 0.1337 for 10848 independent reflections （Rint = 0.0311） and 6915 observed reflections （1 〉 2σ（I））. The complex contains two asymmetric molecules in the cell with small difference in bond distances and bond angles. Each Ni（Ⅱ） ion is bound by four nitrogen atoms of two chelating bdpm groups in a six-membered boat conformation and two oxygen atoms from one chelating bidentate acetate group to form a distorted octahedral geometry. The complex also contains azide anion outside acting as counteranion and two crystalline water molecules to link two discrete mononuclear cations though hydrogen bonds.展开更多
A cobalt coordination polymer, {[Co2（tdc）2（bimm）2]·（3 DMF）}n, was synthesized based on 2,5-thiophenedicarboxylic acid（H2 tdc） and bis（imidazol-1-yl）methane（bimm） mixed ligands. The asymmetric unit of ...A cobalt coordination polymer, {[Co2（tdc）2（bimm）2]·（3 DMF）}n, was synthesized based on 2,5-thiophenedicarboxylic acid（H2 tdc） and bis（imidazol-1-yl）methane（bimm） mixed ligands. The asymmetric unit of the complex contains two Co2＋） cations, two tdc2-dianions, two neutral bimm ligands, and three free DMF molecules. In the complex, deprotonated tdc2-dianions alternately bridge the adjacent Co2＋ cations to generate chains, which are further connected by the flexible bimm ligands to form a 3 D structure containing adamantanoid-like subunits. In topology, the structure of 1 represents a 4-connected uninodal two-fold interpenetrated dia（66） topology. Moreover, the solid UV-Vis absorption spectra of the complex have also been investigated.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
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 zinc（Ⅱ） coordination polymer [Zn2（2-mBIM）2（SUC）2]n （1, 2-mBIM = bis（2-methylimidazo-1-yl） methane, SUC = succinate anion） has been synthesized and characterized by X-ray diffraction. Complex 1 crystallize...A zinc（Ⅱ） coordination polymer [Zn2（2-mBIM）2（SUC）2]n （1, 2-mBIM = bis（2-methylimidazo-1-yl） methane, SUC = succinate anion） has been synthesized and characterized by X-ray diffraction. Complex 1 crystallizes in the triclinic space group P1 with a = 9.4871（8）, b = 12.9789（5）, c = 14.0230（5）, α = 90.474（1）, β = 90.3560（10）, γ = 109.691（1）°, V = 1529.94（15）3 , Z = 2, Dc = 1.553 mg/m3 , μ = 1.63 mm-1 , F（000） = 736, the final R = 0.0645 and wR = 0.0951 for 4067 observed reflections with I 〉 2σ（I）. Each Zn atom was coordinated by two individual 2-mBIM ligands in a cis-conformation and two monodentate coordinated succinate anions in a gauche conformation, resulting in the formation of a two-dimensional supramolecular network containing a cationic 16-membered macrometallacycle and a 28-membered macrometallacycle. The result also indicates that the conformation of the ligands has a strong influence on the structure of the supramolecular network.展开更多
The reactions of the mixture of 1- and 2-[2,2-bis（3,5-dimethylpyrazol-l-yl）-1-phenylethyl]-1,3-cyclopentadiene （bpzpcpH） and mixture of 1- and 2-[2,2-bis（3,5-dimethylpyrazol-l-yl）-I,l-diphenylethyl]-l,3-cyclopen...The reactions of the mixture of 1- and 2-[2,2-bis（3,5-dimethylpyrazol-l-yl）-1-phenylethyl]-1,3-cyclopentadiene （bpzpcpH） and mixture of 1- and 2-[2,2-bis（3,5-dimethylpyrazol-l-yl）-I,l-diphenylethyl]-l,3-cyclopentadiene （bpzdpcpH） with W（CO）sTHF have been carried out. The former yields complex （bpzpcpH）W（CO）4, in which the bpzpcpH acts as a k2-（N,N） bidentate ligand, and the cyclopentadiene moiety does not participate in the coordination to the tungsten atom. While the latter gives complex （bpzdpcpH）W（CO）3, in which the cyclopentadiene moiety coordinates to the tungsten atom in η2-fashion instead of general η5-coordinated mode, causing bpzdpcpH to act as a tridentate k3-（π,N,N） ligand,展开更多
基金This work was supported by the Natural Science Foundation of South China University of Technology (20501008) and Guangdong Provincial Laboratory for Green Chemical Technology
文摘A Ni（Ⅱ） complex [Ni（bdpm）2（OAc）]2（N3）2.5H20 （bdpm = bis（3,5-dimethylpyrazol-1-yl）-methane） was synthesized and characterized by elemental analysis, 1R and single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 18.630（2）, b = 16.6624（19）, c = 19.821（2） A, fl = 90.146（2）°, V = 6152.9（12） A3, Z = 4, C48H80N22Ni2O9, Mr = 1226.76, Dc = 1.324 g/cm^3, F（000） = 2600 and μ = 0.680 mm^-1. The structure was refined to the final R = 0.0578 and wR = 0.1337 for 10848 independent reflections （Rint = 0.0311） and 6915 observed reflections （1 〉 2σ（I））. The complex contains two asymmetric molecules in the cell with small difference in bond distances and bond angles. Each Ni（Ⅱ） ion is bound by four nitrogen atoms of two chelating bdpm groups in a six-membered boat conformation and two oxygen atoms from one chelating bidentate acetate group to form a distorted octahedral geometry. The complex also contains azide anion outside acting as counteranion and two crystalline water molecules to link two discrete mononuclear cations though hydrogen bonds.
基金supported by the Natural Science Foundation of Henan Province(172102310333)
文摘A cobalt coordination polymer, {[Co2（tdc）2（bimm）2]·（3 DMF）}n, was synthesized based on 2,5-thiophenedicarboxylic acid（H2 tdc） and bis（imidazol-1-yl）methane（bimm） mixed ligands. The asymmetric unit of the complex contains two Co2＋） cations, two tdc2-dianions, two neutral bimm ligands, and three free DMF molecules. In the complex, deprotonated tdc2-dianions alternately bridge the adjacent Co2＋ cations to generate chains, which are further connected by the flexible bimm ligands to form a 3 D structure containing adamantanoid-like subunits. In topology, the structure of 1 represents a 4-connected uninodal two-fold interpenetrated dia（66） topology. Moreover, the solid UV-Vis absorption spectra of the complex have also been investigated.
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).
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supported by the National Natural Science Foundation of China (No. 21171053)the Science Foundation of HBDE (Z20102501)the Open Research Foundation in the State Key Laboratory of Coordination Chemistry
文摘A zinc（Ⅱ） coordination polymer [Zn2（2-mBIM）2（SUC）2]n （1, 2-mBIM = bis（2-methylimidazo-1-yl） methane, SUC = succinate anion） has been synthesized and characterized by X-ray diffraction. Complex 1 crystallizes in the triclinic space group P1 with a = 9.4871（8）, b = 12.9789（5）, c = 14.0230（5）, α = 90.474（1）, β = 90.3560（10）, γ = 109.691（1）°, V = 1529.94（15）3 , Z = 2, Dc = 1.553 mg/m3 , μ = 1.63 mm-1 , F（000） = 736, the final R = 0.0645 and wR = 0.0951 for 4067 observed reflections with I 〉 2σ（I）. Each Zn atom was coordinated by two individual 2-mBIM ligands in a cis-conformation and two monodentate coordinated succinate anions in a gauche conformation, resulting in the formation of a two-dimensional supramolecular network containing a cationic 16-membered macrometallacycle and a 28-membered macrometallacycle. The result also indicates that the conformation of the ligands has a strong influence on the structure of the supramolecular network.
基金Project supported by the National Natural Science Foundation of China （No. 20672059）.
文摘The reactions of the mixture of 1- and 2-[2,2-bis（3,5-dimethylpyrazol-l-yl）-1-phenylethyl]-1,3-cyclopentadiene （bpzpcpH） and mixture of 1- and 2-[2,2-bis（3,5-dimethylpyrazol-l-yl）-I,l-diphenylethyl]-l,3-cyclopentadiene （bpzdpcpH） with W（CO）sTHF have been carried out. The former yields complex （bpzpcpH）W（CO）4, in which the bpzpcpH acts as a k2-（N,N） bidentate ligand, and the cyclopentadiene moiety does not participate in the coordination to the tungsten atom. While the latter gives complex （bpzdpcpH）W（CO）3, in which the cyclopentadiene moiety coordinates to the tungsten atom in η2-fashion instead of general η5-coordinated mode, causing bpzdpcpH to act as a tridentate k3-（π,N,N） ligand,
