A new copper complex, Cu2（pba）（bpy）2Cl2·4H2O （here pba was propylenebis （oxamic acid）, bpy was bipyridine）, was synthesized. Crystal structure of the title complex was determined. It belongs to the tetrag...A new copper complex, Cu2（pba）（bpy）2Cl2·4H2O （here pba was propylenebis （oxamic acid）, bpy was bipyridine）, was synthesized. Crystal structure of the title complex was determined. It belongs to the tetragonal system, molecular formula Cu2Cl2O 10N6C 27H 32, Mr=798.58, space group P41212, a=b=9.484（4）, c=35\^918（9）, V=3235（2）3, Dx=1.64gcm -3 and F（000）=1568, μ=1\^546mm -1 for Z=4. The crystal structure was solved by direct methods for final R=0\^048 and Rw=0.060 for 1992 observed reflections with I>3σ（I）. The complex has a C2 symmetry. A chloride anion, two nitrogen atoms from bipyridine and two oxygen atoms from the oxamide carbonyl and carboxyl coordinated to the Cu II ion forming a square pyramidal geometry. In each molecule, two bpy are almost parallel.展开更多
The mononuclear copper(I) complex, [Cu(dppe)2](PF6)(CH3COCH3) [dppe = bis-(diphenylphosphino)ethane] has been synthesized and characterized by X-ray crystallography. The crystal belongs to monoclinic, Mr=1062.3, space...The mononuclear copper(I) complex, [Cu(dppe)2](PF6)(CH3COCH3) [dppe = bis-(diphenylphosphino)ethane] has been synthesized and characterized by X-ray crystallography. The crystal belongs to monoclinic, Mr=1062.3, space group P21/n with cell parameters a =14.741(2), b =19.354(8), c =18.587(3) ? = 91.41(1)°, V = 5301.5 3, Z = 4, Dc=1.302 g/cm3, F(000)= 2200, = 6.16cm-1, R=0.062, Rw = 0.068. A total of 9679 independent reflections were collected, of which 4574 reflections with I >3σ(I) were observed. The central Cu atom is coordinated by four P atoms from dppe to form a distorted tetrahedral environment. In the coordination sphere the bond lengths of CuP(1), CuP(2), CuP(3) and CuP(4) are 2.298(2), 2.305(2), 2.311(2) and 2.295? respectively; and the PCuP bond angles vary from 87.52(9) to 120.12(9)?展开更多
A mononuclear copper(II) complex, [Cu(bipy)(naph)(ClO4)] (where bipy is bipyridine and naph is 2-hydroxy-1-naphthaldehyde), was synthesized and characterized by X-ray single-crystal structure analysis. The crystal is ...A mononuclear copper(II) complex, [Cu(bipy)(naph)(ClO4)] (where bipy is bipyridine and naph is 2-hydroxy-1-naphthaldehyde), was synthesized and characterized by X-ray single-crystal structure analysis. The crystal is triclinic, space group P ?with a = 9.245(4), b = 9.962(4), c = 10.809(7) ? a = 84.83(5), b =82.35(4), g = 81.02(4), V = 972.1 ?, C21H15ClCuN2O6 Mr = 490.36, Z = 2, F(000) = 498, Dx = 1.68 g/cm3, m = 13.05 cm-1, R = 0.078, Rw = 0.081 for 2295 observed reflections with I > 3s(I). The copper(II) ion is coordinated by two nitrogen atoms of bipy and two oxygen atoms of naph in the equatorial plane, with an axial perchlorate oxygen-copper(II) bond to copper(II) ion to form square-pyramidal coordination geometry. The coordination environment of copper(II) is similar to the active site of galactose oxidase and this compound may also be considered as the structural model of galactose oxidase.展开更多
A novel binuclear copper (Ⅱ) complex,namely [Cu 2｛Ph 3P(CH 2) 2CO 2｝ 4(NO 3) 2]·(NO 3) 2 1,has been synthesized from the reaction of Cu(NO 3) 2·4H 2O with Ph 3P +(CH 2) 2CO - 2 L.The si...A novel binuclear copper (Ⅱ) complex,namely [Cu 2｛Ph 3P(CH 2) 2CO 2｝ 4(NO 3) 2]·(NO 3) 2 1,has been synthesized from the reaction of Cu(NO 3) 2·4H 2O with Ph 3P +(CH 2) 2CO - 2 L.The single crystal X ray structural analysis of 1 indicates that the compound crystallizes in space group P1(No.2) with a=12.652(3),b=18.983(4),c=9.102(3),α=97.26(2)°,β=107.38(2)°,γ=102.22(2)° and Z=1.In complex 1,a pair of Cu(Ⅱ) atoms are bridged by carboxylate groups of four ligand molecules with a Cu…Cu distance of 2.738 to form a tetrakis (carboxylato O,O) bridge dimetal core,and the apical coordination positions are occupied by monodentate nitrato anions,which is rare in the structures of similar Cu(Ⅱ) complexes in which the apical ligands are usually neutral molecules.The result shows that introducing the anionic ligands into the coordination sphere of the Cu(Ⅱ) atom significantly increases the Cu…Cu distance.展开更多
The title complex [Cu2(-dppm)2(-Et2dtc)](ClO4)EtOH0.25H2O (dppm = bis- (diphenylphosphino)methane, Et2dtc = diethyldithiocarbamate) has been synthesized and characterized by single-crystal X-ray diffraction analysis. ...The title complex [Cu2(-dppm)2(-Et2dtc)](ClO4)EtOH0.25H2O (dppm = bis- (diphenylphosphino)methane, Et2dtc = diethyldithiocarbamate) has been synthesized and characterized by single-crystal X-ray diffraction analysis. The crystal structure is of monoclinic, space group C2/c with a = 42.587(1), b = 14.1653(4), c = 20.5649(5) ? = 105.945(1)? V =11928.6 3, C57H60.5ClCu2NO5.25P4S2, Mr = 1194.09, Z = 8, Dc = 1.330 g/cm3, (MoK) = 0.98 mm-1 and F(000) = 4948. A total of 15243 reflections were collected, of which 7322 were unique. The structure was refined to R = 0.0739 and wR = 0.1846 for 5135 observed reflections with I > 2(I). The crystal structure consists of the complex cation [Cu2(-dppm)2(-Et2dtc)]+, anion ClO4- and solvate H2O and EtOH, where the dinuclear Cu(Ⅰ) atoms are bridged doubly by two dppm ligands and singly by Et2dtc to give three five-membered rings. The Cu(Ⅰ) atom is in an approxi- mately trigonal-planar environment with the P2S chromophore. The short Cu贩稢u separation (2.7111 ? suggests the presence of metal-metal contact.展开更多
The complex[Cu (dppe)2](NO3)2 was prepared by the reaction of copper(Ⅱ) nitrate with bis(diphenylphosphino) ethane(dppe) in methanol and its crystal structure was determined by X-ray diffraction.The structure was so...The complex[Cu (dppe)2](NO3)2 was prepared by the reaction of copper(Ⅱ) nitrate with bis(diphenylphosphino) ethane(dppe) in methanol and its crystal structure was determined by X-ray diffraction.The structure was solved by direct methods and refined by block-diagonal and full-matrix least-squares methods to a final R of 0.043 for 4085 independent reflections of I>3σ(I).The crystal is monoclinic, space group P21/n,Mr=984.41 with cell parameters a=12.896(2),b=22.250(4),c=17.512(5)A,β=101.6(3)°, V=4922.3 A3,Z=4,Dc=1.590 g/cm3,F(000)=1900,μ=10.573 cm-1. In this complex, C52H48CuN2O6P4, dppe functions as a bidentate chelate ligand. The four phosphorus atoms from two dppe are coordinated to the distorted tetrahedral copper.展开更多
Four cyanide-bridged heterometallic complexes { [CuPb（L1）][FenI（bpb）（CN）2] }2-（C104）2.2H20.2CH3CN （1）, { [CuPb（LI）]2[FeII （CN）6]（HzO）z}＇10H20 （2）, {[Cu2（L2）][Fent（bpb）（CN）2]2}＇2H20＇2CH3OH （...Four cyanide-bridged heterometallic complexes { [CuPb（L1）][FenI（bpb）（CN）2] }2-（C104）2.2H20.2CH3CN （1）, { [CuPb（LI）]2[FeII （CN）6]（HzO）z}＇10H20 （2）, {[Cu2（L2）][Fent（bpb）（CN）2]2}＇2H20＇2CH3OH （3） and {[Cu2（L2）]3[FeIII（CN）6]z（H20）2}-10H20 （4） have been synthesized by treating K[Fem（bpb）（CN）2] [bpb2-=l,2-bis（pyridine-2-carboxamido）benzenate] and K3[Feln（CN）]6 with dinuc[ear compartmental macrocyclic Schiff-base complexes [CuPh（LI）].（C104）2 or [Cu2（L2）]-（CIO4）2, in which H2LJ was derived from 2,6-diformyl-4-methyl-phenol, ethylenediamine, and diethylenetriamine in the molar ratio of 2：1：1 and H2L2 from 2,6-diformyl-4-methyl-phenol and propylenediamine in the molar ratio of 1：1. Single crystal X-ray diffraction analysis reveals that compound 1 displays a cyclic hexanuclear heterotrimetallic molecular structure with alternating [Fem（bpb）（CN）2]- and [CuPb（L＋）]2＋ units. Complex 2 is of a neutral dumb-bell-type pentanuclear molecular configuration consisting of one [Fe（CN）6]4- anion sandwiched in two [CuPu（L1）]2＋ cations, and the pentanuclear moieties are further connected by the hydro- gen bonding to give a 2D supramolecular framework. Heterobimetallic complex 3 is a tetranuclear molecule composed of a centrosymmetric [Cuz（L2）]2＋ segment and two terminal cyanide-containing blocks [Fetn（bpb）（CN）2]-. Octanuclear compound 4 is built from two [Fe（CN）6]3- anions sandwiched in the three [Cu2L2]2＋ cations. Investigation of their magnetic properties reveals the overall antiferromagnetic behavior in the series of complexes except 2.展开更多
文摘A new copper complex, Cu2（pba）（bpy）2Cl2·4H2O （here pba was propylenebis （oxamic acid）, bpy was bipyridine）, was synthesized. Crystal structure of the title complex was determined. It belongs to the tetragonal system, molecular formula Cu2Cl2O 10N6C 27H 32, Mr=798.58, space group P41212, a=b=9.484（4）, c=35\^918（9）, V=3235（2）3, Dx=1.64gcm -3 and F（000）=1568, μ=1\^546mm -1 for Z=4. The crystal structure was solved by direct methods for final R=0\^048 and Rw=0.060 for 1992 observed reflections with I>3σ（I）. The complex has a C2 symmetry. A chloride anion, two nitrogen atoms from bipyridine and two oxygen atoms from the oxamide carbonyl and carboxyl coordinated to the Cu II ion forming a square pyramidal geometry. In each molecule, two bpy are almost parallel.
基金We thank NSFC(No.29871009) Henan Province Outstanding Youth Science Foundation Natural Science Foundation for the financial support of this research.
文摘The mononuclear copper(I) complex, [Cu(dppe)2](PF6)(CH3COCH3) [dppe = bis-(diphenylphosphino)ethane] has been synthesized and characterized by X-ray crystallography. The crystal belongs to monoclinic, Mr=1062.3, space group P21/n with cell parameters a =14.741(2), b =19.354(8), c =18.587(3) ? = 91.41(1)°, V = 5301.5 3, Z = 4, Dc=1.302 g/cm3, F(000)= 2200, = 6.16cm-1, R=0.062, Rw = 0.068. A total of 9679 independent reflections were collected, of which 4574 reflections with I >3σ(I) were observed. The central Cu atom is coordinated by four P atoms from dppe to form a distorted tetrahedral environment. In the coordination sphere the bond lengths of CuP(1), CuP(2), CuP(3) and CuP(4) are 2.298(2), 2.305(2), 2.311(2) and 2.295? respectively; and the PCuP bond angles vary from 87.52(9) to 120.12(9)?
基金Supported by the National Natural Science Foundation of China (No. 29971017) the Teaching and Research Award Program for Outstanding Young Teachers in Higher Education Institutions of MOE China.
文摘A mononuclear copper(II) complex, [Cu(bipy)(naph)(ClO4)] (where bipy is bipyridine and naph is 2-hydroxy-1-naphthaldehyde), was synthesized and characterized by X-ray single-crystal structure analysis. The crystal is triclinic, space group P ?with a = 9.245(4), b = 9.962(4), c = 10.809(7) ? a = 84.83(5), b =82.35(4), g = 81.02(4), V = 972.1 ?, C21H15ClCuN2O6 Mr = 490.36, Z = 2, F(000) = 498, Dx = 1.68 g/cm3, m = 13.05 cm-1, R = 0.078, Rw = 0.081 for 2295 observed reflections with I > 3s(I). The copper(II) ion is coordinated by two nitrogen atoms of bipy and two oxygen atoms of naph in the equatorial plane, with an axial perchlorate oxygen-copper(II) bond to copper(II) ion to form square-pyramidal coordination geometry. The coordination environment of copper(II) is similar to the active site of galactose oxidase and this compound may also be considered as the structural model of galactose oxidase.
文摘A novel binuclear copper (Ⅱ) complex,namely [Cu 2｛Ph 3P(CH 2) 2CO 2｝ 4(NO 3) 2]·(NO 3) 2 1,has been synthesized from the reaction of Cu(NO 3) 2·4H 2O with Ph 3P +(CH 2) 2CO - 2 L.The single crystal X ray structural analysis of 1 indicates that the compound crystallizes in space group P1(No.2) with a=12.652(3),b=18.983(4),c=9.102(3),α=97.26(2)°,β=107.38(2)°,γ=102.22(2)° and Z=1.In complex 1,a pair of Cu(Ⅱ) atoms are bridged by carboxylate groups of four ligand molecules with a Cu…Cu distance of 2.738 to form a tetrakis (carboxylato O,O) bridge dimetal core,and the apical coordination positions are occupied by monodentate nitrato anions,which is rare in the structures of similar Cu(Ⅱ) complexes in which the apical ligands are usually neutral molecules.The result shows that introducing the anionic ligands into the coordination sphere of the Cu(Ⅱ) atom significantly increases the Cu…Cu distance.
基金Supported by the Government of Guangdong province
文摘The title complex [Cu2(-dppm)2(-Et2dtc)](ClO4)EtOH0.25H2O (dppm = bis- (diphenylphosphino)methane, Et2dtc = diethyldithiocarbamate) has been synthesized and characterized by single-crystal X-ray diffraction analysis. The crystal structure is of monoclinic, space group C2/c with a = 42.587(1), b = 14.1653(4), c = 20.5649(5) ? = 105.945(1)? V =11928.6 3, C57H60.5ClCu2NO5.25P4S2, Mr = 1194.09, Z = 8, Dc = 1.330 g/cm3, (MoK) = 0.98 mm-1 and F(000) = 4948. A total of 15243 reflections were collected, of which 7322 were unique. The structure was refined to R = 0.0739 and wR = 0.1846 for 5135 observed reflections with I > 2(I). The crystal structure consists of the complex cation [Cu2(-dppm)2(-Et2dtc)]+, anion ClO4- and solvate H2O and EtOH, where the dinuclear Cu(Ⅰ) atoms are bridged doubly by two dppm ligands and singly by Et2dtc to give three five-membered rings. The Cu(Ⅰ) atom is in an approxi- mately trigonal-planar environment with the P2S chromophore. The short Cu贩稢u separation (2.7111 ? suggests the presence of metal-metal contact.
文摘The complex[Cu (dppe)2](NO3)2 was prepared by the reaction of copper(Ⅱ) nitrate with bis(diphenylphosphino) ethane(dppe) in methanol and its crystal structure was determined by X-ray diffraction.The structure was solved by direct methods and refined by block-diagonal and full-matrix least-squares methods to a final R of 0.043 for 4085 independent reflections of I>3σ(I).The crystal is monoclinic, space group P21/n,Mr=984.41 with cell parameters a=12.896(2),b=22.250(4),c=17.512(5)A,β=101.6(3)°, V=4922.3 A3,Z=4,Dc=1.590 g/cm3,F(000)=1900,μ=10.573 cm-1. In this complex, C52H48CuN2O6P4, dppe functions as a bidentate chelate ligand. The four phosphorus atoms from two dppe are coordinated to the distorted tetrahedral copper.
基金financially supported by the National Natural Science Foundation of ChinaMinistry of Education of China+1 种基金Beijing Municipal Commission of EducationFundamental Research Funds for the Central Universities
文摘Four cyanide-bridged heterometallic complexes { [CuPb（L1）][FenI（bpb）（CN）2] }2-（C104）2.2H20.2CH3CN （1）, { [CuPb（LI）]2[FeII （CN）6]（HzO）z}＇10H20 （2）, {[Cu2（L2）][Fent（bpb）（CN）2]2}＇2H20＇2CH3OH （3） and {[Cu2（L2）]3[FeIII（CN）6]z（H20）2}-10H20 （4） have been synthesized by treating K[Fem（bpb）（CN）2] [bpb2-=l,2-bis（pyridine-2-carboxamido）benzenate] and K3[Feln（CN）]6 with dinuc[ear compartmental macrocyclic Schiff-base complexes [CuPh（LI）].（C104）2 or [Cu2（L2）]-（CIO4）2, in which H2LJ was derived from 2,6-diformyl-4-methyl-phenol, ethylenediamine, and diethylenetriamine in the molar ratio of 2：1：1 and H2L2 from 2,6-diformyl-4-methyl-phenol and propylenediamine in the molar ratio of 1：1. Single crystal X-ray diffraction analysis reveals that compound 1 displays a cyclic hexanuclear heterotrimetallic molecular structure with alternating [Fem（bpb）（CN）2]- and [CuPb（L＋）]2＋ units. Complex 2 is of a neutral dumb-bell-type pentanuclear molecular configuration consisting of one [Fe（CN）6]4- anion sandwiched in two [CuPu（L1）]2＋ cations, and the pentanuclear moieties are further connected by the hydro- gen bonding to give a 2D supramolecular framework. Heterobimetallic complex 3 is a tetranuclear molecule composed of a centrosymmetric [Cuz（L2）]2＋ segment and two terminal cyanide-containing blocks [Fetn（bpb）（CN）2]-. Octanuclear compound 4 is built from two [Fe（CN）6]3- anions sandwiched in the three [Cu2L2]2＋ cations. Investigation of their magnetic properties reveals the overall antiferromagnetic behavior in the series of complexes except 2.
