Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group ...Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group C2/c with a=24. 825(8) . b=14.716(5) , c=18. 419(10)A,β=94. 57(3)°, V=6707. 54 A￣3;Z=4, Dc=1. 248 g/cm￣3. μ= 5. 002 cm￣(-1). F(000)=2664. The structure was solved by direct methods and refined to final R(Rω)=0.059(0.059) for 3183 observed reflections with I≥2.5σ(I). The centrosymmetric anion of the title compound contains two [V(mp)_3]￣(2-) fragments linked by a sodium ion, the crystallographic center of symmetry , through the μ2-O bridges. The Ⅴ(Ⅳ) atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.展开更多
The title compound 1,4-bis(benztriazol-1-ylmethyl)-2,4,5,6-trimethylbenzene crys- tallizes in the monoclinic system, space group Pbca with a = 9.842(5), b = 9.455(5), c = 22.165(12) ?, V = 2062.6(18) ?3, Dc = 1.277 ...The title compound 1,4-bis(benztriazol-1-ylmethyl)-2,4,5,6-trimethylbenzene crys- tallizes in the monoclinic system, space group Pbca with a = 9.842(5), b = 9.455(5), c = 22.165(12) ?, V = 2062.6(18) ?3, Dc = 1.277 g/cm3, Z = 4, C24H24N6, Mr = 396.49, μ(MoKa) = 0.079 mm-1 and F(000) = 840. The structure was refined to R = 0.0662 and wR = 0.1891 for 1163 observed reflections (I > 2σ(I)). The title molecule has trans-conformation about the central phenyl ring. The zigzag-like molecules are connected by face-to-face π…π stacking to form an infinite 2D layer.展开更多
A binuclear copper（I） complex [Cu2（dppm）2（C7H6N2）2]（NO3）2 （C7H6N2 = benzimidazole, dppm = Ph2PCH2PPh2） has been synthesized and characterized by X-ray crystallography.The crystal belongs to monoclinic, space...A binuclear copper（I） complex [Cu2（dppm）2（C7H6N2）2]（NO3）2 （C7H6N2 = benzimidazole, dppm = Ph2PCH2PPh2） has been synthesized and characterized by X-ray crystallography.The crystal belongs to monoclinic, space group C2/c with a = 14.167（3）, b = 21.209（4）, c =20.680（4）A°, β = 103.93（3）°, C32H28CuN3O3P2, Mr = 628.05, Z = 8, μ = 0.868 mm^-1, V = 6031 （2） ,A°^3,F（000） = 2592, De= 1.383 g/cm^3, R = 0.0593 and wR = 0.1736. A total of 5297 independent reflections were collected, of which 3503 were observed with 1 〉 2σ（/）. The central copper atom is tri-coordinated by phosphorus atoms from bridging dppm and nitrogen atom from benzimidazole. In the coordination sphere, the bond lengths of Cu-P（1） and Cu-P（2） are 2.2607（17） and 2.2503（16） A°,respectively and the P-Cu-P bond angle is 127.26（6）°.展开更多
The compound 1,3,5-tris(benzimidazol-1-ylmethyl)-2,4,6-trimethylbenzene, crystallizes in the monoclinic system, space group P21/c, with a = 17.571(4), b = 10.860(2), c = 14.126(3) ?; ( = 92.89(3)(, V = 2692(1) ?3, Dc ...The compound 1,3,5-tris(benzimidazol-1-ylmethyl)-2,4,6-trimethylbenzene, crystallizes in the monoclinic system, space group P21/c, with a = 17.571(4), b = 10.860(2), c = 14.126(3) ?; ( = 92.89(3)(, V = 2692(1) ?3, Dc = 1.260 g/cm3, Z = 4, C33H30N6, Mr = 510.63, ((MoK() = 0.077mm-1, F (000) = 1080. The structure was refined to R = 0.0592, wR = 0.1379 for 1492 (I(2((I)) reflections. The title molecule has cis, trans, trans-conformation about the central phenyl ring. The screw-related molecules are connected by hydrogen bonds C-H(((N (x, -0.5-y, 0.5+z) and form the infinite helical chains. The polar molecular chains are antiparallelly stacked through edge-to-face C-H…πinteractions.展开更多
Compound 5-methyl-2-phenyl-4-[（Z）-3-tolylamino-phenylmethylene]pyrazol-3（2H）-one （C24H21N3O） crystallizes in the triclinic system, space group P1, with a = 9.267（3）, b = 9.904（4）,c = 12.035（4） A°, α ...Compound 5-methyl-2-phenyl-4-[（Z）-3-tolylamino-phenylmethylene]pyrazol-3（2H）-one （C24H21N3O） crystallizes in the triclinic system, space group P1, with a = 9.267（3）, b = 9.904（4）,c = 12.035（4） A°, α = 97.896（6）, β = 103.865（6）, γ = 107.950（6）°, Mr= 367.44, Z = 2, V = 993.2（6）A°^3,Dc = 1.229 g/cm^3,μ（MoKa） = 0.077 mm^-1 and F（000） = 388. The structure was refined to R =0.0444 and wR = 0.1199 for 2903 observed reflections （I 〉 2σ（I））. The results of ^1H NMR and single-crystal X-ray diffraction studies showed the enamine character of the compound. The strong intramolecular hydrogen bonds in the large conjugate system, together with weak intermolecular C-H……π hydrogen bonding and π……π stacking, lead to the formation of a multi-dimensional supramolecular network.展开更多
This paper presents the synthetic and structure studies of molybdenum（tungsten）-copper-sulphur-dialkyldithiocarbamate cluster compounds.The reactions of（M=Mo,W;n=0,2）,CuCl,and R<sub>2</sub>dtc￣-（R<...This paper presents the synthetic and structure studies of molybdenum（tungsten）-copper-sulphur-dialkyldithiocarbamate cluster compounds.The reactions of（M=Mo,W;n=0,2）,CuCl,and R<sub>2</sub>dtc￣-（R<sub>2</sub>=Me<sub>2</sub>,Et<sub>2</sub>,C<sub>4</sub>H<sub>8</sub>,C<sub>5</sub>H<sub>1</sub>0） yield a series of tetra-,hexa-,and heptanuclear cluster compounds.Their spectroscopic properties and the synthetic reaction mechanism are discussed.展开更多
Co_6(μ_3-S)_8(Ph_2PCH_2P(O)Ph_2)_6, MW=3012.5, space group R, has the hexagonal parameters, a=26.764(10), c=16.979 (10), V=10532.8~3, Z=3. Mo Kα radiation, λ= 0.71069, Dc=1.425 g/cm^3, μ=9.94 cm^(-3), F(000)=4650,...Co_6(μ_3-S)_8(Ph_2PCH_2P(O)Ph_2)_6, MW=3012.5, space group R, has the hexagonal parameters, a=26.764(10), c=16.979 (10), V=10532.8~3, Z=3. Mo Kα radiation, λ= 0.71069, Dc=1.425 g/cm^3, μ=9.94 cm^(-3), F(000)=4650, R=0.073 and Rw=0.077 for 1965 observed unique reflections with I>3σ(I). The molecular structure consists of a distorted octahed- ral Co_6-core. The Co-Co and Co-S distances fall in the range of 2.805-2.838 and 2.213-2.253, respectively.展开更多
Co_6 (μ_3-Se)_8 (PEt_3)_6·THF, MW=1766.4, space group R, has the trigonal parameters, a=11.890(2)°, α=92.72(2)°, V=1670.4~3, Z=1. Mo Kα radiation, λ=0.71073, Dc=1.749 g/cm^3, μ= 59.18 cm^(-3), F(00...Co_6 (μ_3-Se)_8 (PEt_3)_6·THF, MW=1766.4, space group R, has the trigonal parameters, a=11.890(2)°, α=92.72(2)°, V=1670.4~3, Z=1. Mo Kα radiation, λ=0.71073, Dc=1.749 g/cm^3, μ= 59.18 cm^(-3), F(000)=870, R=0.058 and Rw=0.067 for 1529 observed unique reflections with I>3σ(I). The molecular structure consists of an idealized octahedral Co_6-core. The Co-Co distances fall in the range of 2.909-2.9122.展开更多
文摘Et_4N)_3 [V(mp)_3Na(mp)_3V] was obtained from the reaction of (NH_4)_3VS_4, FeCl_2, Na_2mp(H_2mp=o-mercaptophenol,o-HSC_6H_4OH) and Et_4NCl in CH_3CN. C_(60)H_(84)N_3NaO_6S_6V_2, M_r=1260. 61, monoclinic, space group C2/c with a=24. 825(8) . b=14.716(5) , c=18. 419(10)A,β=94. 57(3)°, V=6707. 54 A￣3;Z=4, Dc=1. 248 g/cm￣3. μ= 5. 002 cm￣(-1). F(000)=2664. The structure was solved by direct methods and refined to final R(Rω)=0.059(0.059) for 3183 observed reflections with I≥2.5σ(I). The centrosymmetric anion of the title compound contains two [V(mp)_3]￣(2-) fragments linked by a sodium ion, the crystallographic center of symmetry , through the μ2-O bridges. The Ⅴ(Ⅳ) atom is in a coordination environment intermediate between a trigonal prism and an ideal octahedron.
文摘The title compound 1,4-bis(benztriazol-1-ylmethyl)-2,4,5,6-trimethylbenzene crys- tallizes in the monoclinic system, space group Pbca with a = 9.842(5), b = 9.455(5), c = 22.165(12) ?, V = 2062.6(18) ?3, Dc = 1.277 g/cm3, Z = 4, C24H24N6, Mr = 396.49, μ(MoKa) = 0.079 mm-1 and F(000) = 840. The structure was refined to R = 0.0662 and wR = 0.1891 for 1163 observed reflections (I > 2σ(I)). The title molecule has trans-conformation about the central phenyl ring. The zigzag-like molecules are connected by face-to-face π…π stacking to form an infinite 2D layer.
基金This work was supported by the National Natural Science Foundation of China (No. 20271017) and Henan Provincial Innovation Foundation (No. 0421001300)
文摘A binuclear copper（I） complex [Cu2（dppm）2（C7H6N2）2]（NO3）2 （C7H6N2 = benzimidazole, dppm = Ph2PCH2PPh2） has been synthesized and characterized by X-ray crystallography.The crystal belongs to monoclinic, space group C2/c with a = 14.167（3）, b = 21.209（4）, c =20.680（4）A°, β = 103.93（3）°, C32H28CuN3O3P2, Mr = 628.05, Z = 8, μ = 0.868 mm^-1, V = 6031 （2） ,A°^3,F（000） = 2592, De= 1.383 g/cm^3, R = 0.0593 and wR = 0.1736. A total of 5297 independent reflections were collected, of which 3503 were observed with 1 〉 2σ（/）. The central copper atom is tri-coordinated by phosphorus atoms from bridging dppm and nitrogen atom from benzimidazole. In the coordination sphere, the bond lengths of Cu-P（1） and Cu-P（2） are 2.2607（17） and 2.2503（16） A°,respectively and the P-Cu-P bond angle is 127.26（6）°.
基金the National Natural Science Foundation of China and Natural Science Foundation of Guangdong Province.
文摘The compound 1,3,5-tris(benzimidazol-1-ylmethyl)-2,4,6-trimethylbenzene, crystallizes in the monoclinic system, space group P21/c, with a = 17.571(4), b = 10.860(2), c = 14.126(3) ?; ( = 92.89(3)(, V = 2692(1) ?3, Dc = 1.260 g/cm3, Z = 4, C33H30N6, Mr = 510.63, ((MoK() = 0.077mm-1, F (000) = 1080. The structure was refined to R = 0.0592, wR = 0.1379 for 1492 (I(2((I)) reflections. The title molecule has cis, trans, trans-conformation about the central phenyl ring. The screw-related molecules are connected by hydrogen bonds C-H(((N (x, -0.5-y, 0.5+z) and form the infinite helical chains. The polar molecular chains are antiparallelly stacked through edge-to-face C-H…πinteractions.
文摘Compound 5-methyl-2-phenyl-4-[（Z）-3-tolylamino-phenylmethylene]pyrazol-3（2H）-one （C24H21N3O） crystallizes in the triclinic system, space group P1, with a = 9.267（3）, b = 9.904（4）,c = 12.035（4） A°, α = 97.896（6）, β = 103.865（6）, γ = 107.950（6）°, Mr= 367.44, Z = 2, V = 993.2（6）A°^3,Dc = 1.229 g/cm^3,μ（MoKa） = 0.077 mm^-1 and F（000） = 388. The structure was refined to R =0.0444 and wR = 0.1199 for 2903 observed reflections （I 〉 2σ（I））. The results of ^1H NMR and single-crystal X-ray diffraction studies showed the enamine character of the compound. The strong intramolecular hydrogen bonds in the large conjugate system, together with weak intermolecular C-H……π hydrogen bonding and π……π stacking, lead to the formation of a multi-dimensional supramolecular network.
文摘This paper presents the synthetic and structure studies of molybdenum（tungsten）-copper-sulphur-dialkyldithiocarbamate cluster compounds.The reactions of（M=Mo,W;n=0,2）,CuCl,and R<sub>2</sub>dtc￣-（R<sub>2</sub>=Me<sub>2</sub>,Et<sub>2</sub>,C<sub>4</sub>H<sub>8</sub>,C<sub>5</sub>H<sub>1</sub>0） yield a series of tetra-,hexa-,and heptanuclear cluster compounds.Their spectroscopic properties and the synthetic reaction mechanism are discussed.
基金Project supported by the National Natural Science Foundation of China.
文摘Co_6(μ_3-S)_8(Ph_2PCH_2P(O)Ph_2)_6, MW=3012.5, space group R, has the hexagonal parameters, a=26.764(10), c=16.979 (10), V=10532.8~3, Z=3. Mo Kα radiation, λ= 0.71069, Dc=1.425 g/cm^3, μ=9.94 cm^(-3), F(000)=4650, R=0.073 and Rw=0.077 for 1965 observed unique reflections with I>3σ(I). The molecular structure consists of a distorted octahed- ral Co_6-core. The Co-Co and Co-S distances fall in the range of 2.805-2.838 and 2.213-2.253, respectively.
基金This work was supported by the National Natural Science Foundation of China.
文摘Co_6 (μ_3-Se)_8 (PEt_3)_6·THF, MW=1766.4, space group R, has the trigonal parameters, a=11.890(2)°, α=92.72(2)°, V=1670.4~3, Z=1. Mo Kα radiation, λ=0.71073, Dc=1.749 g/cm^3, μ= 59.18 cm^(-3), F(000)=870, R=0.058 and Rw=0.067 for 1529 observed unique reflections with I>3σ(I). The molecular structure consists of an idealized octahedral Co_6-core. The Co-Co distances fall in the range of 2.909-2.9122.
