The title compound was synthesized by the solid-state reaction of (NH_4)_6Mo_7O_(24)·4H_2O, Na_2C_2O_4, NH_2OH·HCl and Bu_4NBr at 90 ℃ for 10 h and crystallized from acetone-ether. The green crystal belongs...The title compound was synthesized by the solid-state reaction of (NH_4)_6Mo_7O_(24)·4H_2O, Na_2C_2O_4, NH_2OH·HCl and Bu_4NBr at 90 ℃ for 10 h and crystallized from acetone-ether. The green crystal belongs to the monoclinic space group P2_1/n with a=9. 908(2), b= 17, 873(2), c= 13/450(2) A , β= 90. 09(1 )°,V = 2381. 6 (7 ) A￣3 , D_c = 1. 359 g/cm￣3 , Z= 2. The structure was refined to R =0. 0427 for 2562 reflections. The anion of the title compound can be described as an oxalate ligand (C_2O4￣2 ) bridging two [MoCl_2O(OH)] units, which contain Mo(V)atoms.展开更多
The title complex[Zn_2L(C_5H_7N_2)_2(C_5H_7N_2·HClO_4)_2](L=1,2-di(3', 5'-dimethylpyrazolyl) formylhydrazine and C_5H_7N_2= 3 , 5 dimethylpyrazole anion) has been synthesized by template reaction, in whic...The title complex[Zn_2L(C_5H_7N_2)_2(C_5H_7N_2·HClO_4)_2](L=1,2-di(3', 5'-dimethylpyrazolyl) formylhydrazine and C_5H_7N_2= 3 , 5 dimethylpyrazole anion) has been synthesized by template reaction, in which carbonhydrazine, 2, 4-pentanedione and zinc perchlorate hexahydrate were used as the original materials. The crystals of complex with formula C_(32)H_(46)N_(14)O_(10)Cl_2Zn_2 (Mr=988.46) are triclinic,space group P1,a= 8.275 (2),b=11.523 (3),c= 12.872(5), a=69. 90(3),β= 69.79 (2), γ=83. 52 (2)°,V=1081.6(6),Z=1,Dc=1.524g/cm￣3,μ=13.265cm￣(-1),F (000)=510. The final refinement is converged with R= 0.057. The results indicate that in one complex molecule there are three kinds of pyrazole rings all directly coordinated to the central Zn atom; and each zinc atom possesses a five-coordinated polyhedron.展开更多
Dinuclear Cu(Ⅱ) complexes (Cu,LCl4). 2H2O and Cu2L'Cl4 are pre-pared and characterized by X-ray structure analysis. (Cu2I-Cl4). 2H2O, C20 H40N6Cu2Cl4O2, Mr=665. 54, monoclinic, 6 for 188l observed reflections wit...Dinuclear Cu(Ⅱ) complexes (Cu,LCl4). 2H2O and Cu2L'Cl4 are pre-pared and characterized by X-ray structure analysis. (Cu2I-Cl4). 2H2O, C20 H40N6Cu2Cl4O2, Mr=665. 54, monoclinic, 6 for 188l observed reflections with I>3(I). Cu2L'Cl4, C20H36N6Cu2Cl4, M.=629. 41, monoclinic, for 1330 observed reflections with I>3(I). In both complexes the stereo-chemistry about Cu(Ⅱ) is 5-coordinated with two secondary amine N atoms and twoCl- occupying sites at the base of a distorted square pyramid capped by the tertiaryamine N atom. The pair of Cl' attached to the two Cu(Ⅱ) are held in anti configuration.展开更多
A new cyano-bridged Gadolinium^(Ⅲ)-Iron^(Ⅲ)complex{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)]2H_(2)0(DMF=N,N·-dimethylformamide;DMSO=dimethylsulfoxidel}was synthesized by the grinding reaction method,.It crysta-]llizes in...A new cyano-bridged Gadolinium^(Ⅲ)-Iron^(Ⅲ)complex{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)]2H_(2)0(DMF=N,N·-dimethylformamide;DMSO=dimethylsulfoxidel}was synthesized by the grinding reaction method,.It crysta-]llizes in the triclinic.,space group P1 with ceIl parameters:a=O.90363(2)nm,b=1.25078(3)nm,c=1.41303(1)nm,穋m^(-3),Z=2,Mr=756.72,F(000)=760,Ⅲ)and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ)are linked by a cyano-bridge group to construct a dinuclear compound.The{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)](Ⅲ)-Fe(Ⅲ)interaction is antiferromagnetic.CCDC:223430.展开更多
以2,2′-联嘧啶(bpy)和马来二腈基阴离子(mnt)为配体合成了一个双核钴混配配合物(C4H9)4N2(Co(mnt)2)2(bpy)(1)(C56H78Co2N14S8)((C4H9)4N=tetrabutylammonium,mnt=maleonitriledithiolate and bpy=2,2′-bipyrimidyl),并用X-射线单晶...以2,2′-联嘧啶(bpy)和马来二腈基阴离子(mnt)为配体合成了一个双核钴混配配合物(C4H9)4N2(Co(mnt)2)2(bpy)(1)(C56H78Co2N14S8)((C4H9)4N=tetrabutylammonium,mnt=maleonitriledithiolate and bpy=2,2′-bipyrimidyl),并用X-射线单晶衍射方法测定了该配合物的晶体结构:配合物属单斜晶系,P21/c空间群,a=2.368 2(2)nm,b=1.582 11(13)nm,c=1.873 85(16)nm,β=105.834(2)。此外,还对该配合物进行了热重(TGA)、紫外可见光谱(UV)、红外光谱(IR)、X-射线光电子能谱(XPS)、变温磁化率和电化学循环伏安(CVs)等性质的研究;数据表明相邻的金属钴离子之间存在反铁磁相互作用。展开更多
The X-ray crystallographic structure was reported for a dinuclear copper（Ⅱ） complex with a tetraanionic ligand of p-tert-butylsulfonylcalix[4]arene [Cu2L（CH3OH）6]·4CH3OH （H4L=p-tert-butylsuffonylcalix[4]ar...The X-ray crystallographic structure was reported for a dinuclear copper（Ⅱ） complex with a tetraanionic ligand of p-tert-butylsulfonylcalix[4]arene [Cu2L（CH3OH）6]·4CH3OH （H4L=p-tert-butylsuffonylcalix[4]arene）. The complex belongs to triclinic system, P1^-- space group, with a = 1.2303（3） nm, b = 1.2377（3） nm, c = 1.3110（3） nm, a =66.862（4）°, β= 67.206（4）°, γ=61.711（3）°, Z= 1, V= 1.5659（7） nm^3, Dc= 1.371 g/cm^3, F（000） = 682,μ（Mo Kα） = 0.883 mm^-1, R1 =0.0325, wR2=0.0870. In this complex, the calix[4]arene acts as a bis-tridentate chelating ligand with the 1,2-alternate conformation.展开更多
文摘The title compound was synthesized by the solid-state reaction of (NH_4)_6Mo_7O_(24)·4H_2O, Na_2C_2O_4, NH_2OH·HCl and Bu_4NBr at 90 ℃ for 10 h and crystallized from acetone-ether. The green crystal belongs to the monoclinic space group P2_1/n with a=9. 908(2), b= 17, 873(2), c= 13/450(2) A , β= 90. 09(1 )°,V = 2381. 6 (7 ) A￣3 , D_c = 1. 359 g/cm￣3 , Z= 2. The structure was refined to R =0. 0427 for 2562 reflections. The anion of the title compound can be described as an oxalate ligand (C_2O4￣2 ) bridging two [MoCl_2O(OH)] units, which contain Mo(V)atoms.
文摘The title complex[Zn_2L(C_5H_7N_2)_2(C_5H_7N_2·HClO_4)_2](L=1,2-di(3', 5'-dimethylpyrazolyl) formylhydrazine and C_5H_7N_2= 3 , 5 dimethylpyrazole anion) has been synthesized by template reaction, in which carbonhydrazine, 2, 4-pentanedione and zinc perchlorate hexahydrate were used as the original materials. The crystals of complex with formula C_(32)H_(46)N_(14)O_(10)Cl_2Zn_2 (Mr=988.46) are triclinic,space group P1,a= 8.275 (2),b=11.523 (3),c= 12.872(5), a=69. 90(3),β= 69.79 (2), γ=83. 52 (2)°,V=1081.6(6),Z=1,Dc=1.524g/cm￣3,μ=13.265cm￣(-1),F (000)=510. The final refinement is converged with R= 0.057. The results indicate that in one complex molecule there are three kinds of pyrazole rings all directly coordinated to the central Zn atom; and each zinc atom possesses a five-coordinated polyhedron.
文摘Dinuclear Cu(Ⅱ) complexes (Cu,LCl4). 2H2O and Cu2L'Cl4 are pre-pared and characterized by X-ray structure analysis. (Cu2I-Cl4). 2H2O, C20 H40N6Cu2Cl4O2, Mr=665. 54, monoclinic, 6 for 188l observed reflections with I>3(I). Cu2L'Cl4, C20H36N6Cu2Cl4, M.=629. 41, monoclinic, for 1330 observed reflections with I>3(I). In both complexes the stereo-chemistry about Cu(Ⅱ) is 5-coordinated with two secondary amine N atoms and twoCl- occupying sites at the base of a distorted square pyramid capped by the tertiaryamine N atom. The pair of Cl' attached to the two Cu(Ⅱ) are held in anti configuration.
文摘A new cyano-bridged Gadolinium^(Ⅲ)-Iron^(Ⅲ)complex{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)]2H_(2)0(DMF=N,N·-dimethylformamide;DMSO=dimethylsulfoxidel}was synthesized by the grinding reaction method,.It crysta-]llizes in the triclinic.,space group P1 with ceIl parameters:a=O.90363(2)nm,b=1.25078(3)nm,c=1.41303(1)nm,穋m^(-3),Z=2,Mr=756.72,F(000)=760,Ⅲ)and the approxi-mately oriented octahedrally sixfold-coordinated Fe(Ⅲ)are linked by a cyano-bridge group to construct a dinuclear compound.The{[Gd(DMF)_(3)(DMSO)(H_(2)O)_(3)](Ⅲ)-Fe(Ⅲ)interaction is antiferromagnetic.CCDC:223430.
基金grateful for the financial support of the National Basic Research program of China(2010CB923402)National Nature Science Foundation of China(NSFC:21021062 and 91122031)+1 种基金Jiangsu Science & Technology Department(BK2011550)the Center of Analysis and Determining of Nanjing University~~
文摘以2,2′-联嘧啶(bpy)和马来二腈基阴离子(mnt)为配体合成了一个双核钴混配配合物(C4H9)4N2(Co(mnt)2)2(bpy)(1)(C56H78Co2N14S8)((C4H9)4N=tetrabutylammonium,mnt=maleonitriledithiolate and bpy=2,2′-bipyrimidyl),并用X-射线单晶衍射方法测定了该配合物的晶体结构:配合物属单斜晶系,P21/c空间群,a=2.368 2(2)nm,b=1.582 11(13)nm,c=1.873 85(16)nm,β=105.834(2)。此外,还对该配合物进行了热重(TGA)、紫外可见光谱(UV)、红外光谱(IR)、X-射线光电子能谱(XPS)、变温磁化率和电化学循环伏安(CVs)等性质的研究;数据表明相邻的金属钴离子之间存在反铁磁相互作用。
基金Project supported by the Municipal Natural Science Foundation of Beijing （No. 2022011）.
文摘The X-ray crystallographic structure was reported for a dinuclear copper（Ⅱ） complex with a tetraanionic ligand of p-tert-butylsulfonylcalix[4]arene [Cu2L（CH3OH）6]·4CH3OH （H4L=p-tert-butylsuffonylcalix[4]arene）. The complex belongs to triclinic system, P1^-- space group, with a = 1.2303（3） nm, b = 1.2377（3） nm, c = 1.3110（3） nm, a =66.862（4）°, β= 67.206（4）°, γ=61.711（3）°, Z= 1, V= 1.5659（7） nm^3, Dc= 1.371 g/cm^3, F（000） = 682,μ（Mo Kα） = 0.883 mm^-1, R1 =0.0325, wR2=0.0870. In this complex, the calix[4]arene acts as a bis-tridentate chelating ligand with the 1,2-alternate conformation.
