The two title complexes, [Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5- (NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal = 3,5-dinitrosalicylate, 2,2'-bipy = 2,2′-bipyridine), were synthesized by the hydrother...The two title complexes, [Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5- (NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal = 3,5-dinitrosalicylate, 2,2'-bipy = 2,2′-bipyridine), were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic, space group P1, a = 5.581(4), b = 12.071(8), c = 12.88(1)A, α= 92.10(3),β= 96.73(3), γ = 102.02(2)°, C17H10N407Cd, Mr = 494.69, V= 841(1)A3, Z = 2, Dc = 1.954 g/cm3, F(000) = 488, μ= 1.353 mm^-1, R = 0.0248 and wR = 0.0761. Complex 2 crystallizes in monoclinic with space group P21/c, a = 8.604(3), b = 23.88(1), c = 8.894(3) A, β = 102.45(1)°, C17H10N407Mn, Mr = 437.23, V= 1785(1) A3, Z=.4, Dc = 1.627 g/cm3, F(000) = 884, μ = 0.791 mm^-1, R = 0.0471 and wR = 0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2)A. The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.展开更多
The reaction of 4-hydroxybenzoic acid (H2L),4, 4-diaminodiphenylmethane (DADPM) and Cd(NO3)2?H2O in methane/water gave rise to a seven-coordinate Cd(Ⅱ) complex [Cd2(HL)4(H2O)6]?H2O which has been characterized by sin...The reaction of 4-hydroxybenzoic acid (H2L),4, 4-diaminodiphenylmethane (DADPM) and Cd(NO3)2?H2O in methane/water gave rise to a seven-coordinate Cd(Ⅱ) complex [Cd2(HL)4(H2O)6]?H2O which has been characterized by single-crystal X-ray diffraction. The complex crystallizes in the orthorhombic system, space group Pna21 with unit cell parameters: a = 10.3352(3), b = 12.0481(3), c = 28.2016(1) ? V = 3511.65(13) 3, Z = 4, C28H36Cd2O20, Mr = 917.37, Dc = 1.735 g/cm3, F(000) = 1840, (MoK? = 1.29mm-1. The final R and wR are 0.0536 and 0.1086 for 4898 observed reflections with I ≥ 4(I). The Cd(Ⅱ) is seven-coordinated in a distorted pentagonal bipyramidal geometry. The inter-molecular hydrogen bonds lead to the formation of a two-dimensional layer structure.展开更多
The title complex [CdLCl2] 1 (C10H15CdCl2N3, Mr = 360.55) has been synthesized by the reaction of CdCl22.5H2O with the tridentate Schiff base L, N,N-dimethyl-N-pyridin-2-yl- methylene-1,2-diaminoethane, which is deriv...The title complex [CdLCl2] 1 (C10H15CdCl2N3, Mr = 360.55) has been synthesized by the reaction of CdCl22.5H2O with the tridentate Schiff base L, N,N-dimethyl-N-pyridin-2-yl- methylene-1,2-diaminoethane, which is derived from the condensation reaction of pyridine-2- carboxaldehyde and N,N-dimethylethylenediamine. It crystallizes in the monoclinic system, space group C2/c with a = 25.054(13), b = 7.532(4), c = 16.119(8) ? b = 116.238(8)? V = 2728(2) ?, Z = 8, Dc = 1.756 g/cm3, m(MoKa) = 1.970 mm-1, F(000) = 1424, R = 0.0297 and wR = 0.0625. Crystal analyses reveal that the cadmium atom is coordinated by two chlorine atoms and three N atoms from the tridentate ligand in a distorted tetragonal pyramidal environment. Each complex molecule is connected with four surrounding ones to form 2D network by hydrogen bonds along the bc plane. The chlorine atoms act as acceptors and the carbon atoms of the tridentate Schiff base as donors with the CH…Cl distances in the range of 3.518~3.752 ?展开更多
The complex [Cd(H2mbdpz)(N3)2]n 1 (H2mbdpz = 4,4′-methylenebis(3,5-dimethylpyrazole)) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in the...The complex [Cd(H2mbdpz)(N3)2]n 1 (H2mbdpz = 4,4′-methylenebis(3,5-dimethylpyrazole)) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in the monoclinic system, space groups C2/c with a = 22.154(5), b = 7.4835(15), c = 21.044(8)A^°,β= 115.51(3)°, V= 3148.7(17)A^°3, Z= 8, C11H16CdN10, Mr = 400.75, Dc = 1.691 g/cm^3,μ = 1.401 mm^-1, F(000) = 1599, T= 293(2) K, the final R = 0.0228 and wR = 0.0581 for 3604 observed reflections with I 〉 2σ(I). The structural determination revealed that the coordination environment of Cd(Ⅱ) atom is a distorted octahedron consisting of two nitrogen donors of two H2mbdpz ligands and four nitrogen donors from four azide ligands. The azide moieties act as bridges in two modes: end-on (μ1,1-) and end-to-end (μ1,3-), and H2mbdpz also serves as a bridge with a bis-monodentate coordination. Both bridging ligands link the Cd(Ⅱ) atoms to form a distorted two-dimensional (6,3) layer.展开更多
A novel coordination polymer [{Cd(hmbdc)(H20)3}-2H20],, (hmbdc = 5-hydroxyisophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crys...A novel coordination polymer [{Cd(hmbdc)(H20)3}-2H20],, (hmbdc = 5-hydroxyisophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2Jc, with a = 9.599(3), b = 18.699(5), c = 7.557(2) A, r= 108.198(4)°, V= 1288.6(6) A3, Z= 4, M,.= 382.60, Dc = 1.972 g/cm^, F(000) = 760, p = 1.740, the final R =0.0555 and wR = 0.0995 for 1732 observed reflections with 1 〉 2σ(I). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.展开更多
A polynuclear complex [Cd(endc)(H20)]n·nH2O (endc = endo-norbornene-cis- 5,6-dicarboxylate anion) has been synthesized by the hydrothermal reaction of cadmium nitrate tetrahydrate with endo-norbornene-cis-5...A polynuclear complex [Cd(endc)(H20)]n·nH2O (endc = endo-norbornene-cis- 5,6-dicarboxylate anion) has been synthesized by the hydrothermal reaction of cadmium nitrate tetrahydrate with endo-norbornene-cis-5,6-dicarboxylic acid in 1:1 molar ratio, and structurally characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with α = 1.16471(7), b = 0.95334(7), c = 0.91109(9) nm, Z= 4, V= 1.01035(14) nm^3, D, = 2.160 g/cm^3,μ = 2.172 mm^-1, F(000) = 648, R = 0.0302 and wR = 0.0752. According to structural analysis, each Cd(II) ion is coordinated to six O atoms from three endc anions and one water molecule, giving a distorted octahedral geometry. Two- dimensional layer arrangement of the title complex is constructed from the bridging nature of endc. It is worth notice that adjacent two-dimensional layers are joined together to form a three-dimensional supramolecular framework via intermolecular hydrogen bonding interactions.展开更多
A new flexible double betaine L (L = 1,4-bis(pyridinio-4-carboxylato-N-methyl)benzene, C20H16N2O4) and its cadmium(Ⅱ) complex [Cd(H2O)aL(NO3)]NO3.H2O 1 were synthesized. Complex 1 was obtained by self-assem...A new flexible double betaine L (L = 1,4-bis(pyridinio-4-carboxylato-N-methyl)benzene, C20H16N2O4) and its cadmium(Ⅱ) complex [Cd(H2O)aL(NO3)]NO3.H2O 1 were synthesized. Complex 1 was obtained by self-assembly reaction of [Cd(NO3)2]-4H2O and L in hot water,and its crystal structure was determined by single-crystal X-ray diffraction analysis. Crystallographic data for complex 1: C20H24CdN4O14.H2O, Mr = 674.85, monoclinic, space group P21/c, a =13.7854(3), b = 14.2820(3), c = 14.9188(4) ,A°, β = 116.418(1)°, V = 2630.5(1)A°^3, Z = 4, Dc= 1.704g/cm^3,/J(MoKα) = 0.911 mm^-1, F(000) = 1368, the final R = 0.0315 and wR = 0.0768 for 3637 observed reflections with I 〉 2σ(I). In complex 1, L acts as a monodentate ligand to link a Cd(Ⅱ) ion in a novel coordination mode of double betaines. The mononuclear [Cd(H2O)aL(NO3)] units are connected through intermolecular hydrogen bonds and π-π stacking reactions to generate a 3D network.展开更多
complex[Ni(La) 2 ](NO 3 )2 (1)with bidentate racemic1,2,2-trimethylcyclopentane-1,3-diamine lig-and has been synthesized and characterized by IR,EA,ES-MS,and its X-ray diffracti on study reveals that the nickel (Ⅱ)ab...complex[Ni(La) 2 ](NO 3 )2 (1)with bidentate racemic1,2,2-trimethylcyclopentane-1,3-diamine lig-and has been synthesized and characterized by IR,EA,ES-MS,and its X-ray diffracti on study reveals that the nickel (Ⅱ)abstract: center is tetra-coordinated by one D-and one L-diamine ligands,and a thre e-dimensional hydrogen-bond-sustained network is formed in the solid state by means of the eight-membered N-H...O hydrogen bond cy-cle.This compound also su pplies a good comparison to the chiral complex[Ni(L b )2 ]Cl 2 ·2H 2 O(2)(L b =D-(+)abstract:-1,2,2-trimethylcyclopentane-1,3-diamine)abstract:.CCDC:218122.展开更多
RAJ S.Shanmuga Sundara FUN Hoong Kun (X ray Crystallography Unit, School of Physics, Universiti Sains Malaysia 11800 USM, Penang, Malaysia) The complex [Co(Im)6](Cin)2 (Im=imidazole,Cin=cinnamate) was prepared by reac...RAJ S.Shanmuga Sundara FUN Hoong Kun (X ray Crystallography Unit, School of Physics, Universiti Sains Malaysia 11800 USM, Penang, Malaysia) The complex [Co(Im)6](Cin)2 (Im=imidazole,Cin=cinnamate) was prepared by reaction of Co(PhCHCHCOO)2 with imidazole in ethanol. It has been determined by single crystal X ray analyses. The crystals are triclinic, space group , with a=9.7601(3),b=10.5935(3),c=11.3269(2)? ,α =69.948(1),β =71.027(1),γ =62.803(1)° , and Z=1. The crystal structure of the title complex consists of monomeric [Co(Im)6]2+ cations and cinnamate anions in which the cobalt? ion assumes a centrosymmetric octahedral geometry with the CoN6 chromophore. In the solid state, the complex forms a three dimensional network through N- H… O hydrogen bonds, the intermolecular hydrogen bonds connect the [Co(Im)6]2+ cations and cinnamate anions.The cinnamate anions are nearly planar.展开更多
The crystal and molecular structure of [CoCl2(N4 trzCH2CH2COPh)4]·6H2O (trz=1,2,4 triazole) has been determined by X ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with unit cell pa...The crystal and molecular structure of [CoCl2(N4 trzCH2CH2COPh)4]·6H2O (trz=1,2,4 triazole) has been determined by X ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with unit cell parameters a=0.8039(2)nm, b=1.0822(2)nm, c=2.9013(6)nm, β=94.79(3)°, and Z=4. Each cobalt atom is coordinated by four N atoms of triazole from four 1 propiophenone 1,2,4 triazole ligands and two chloride anion in cis arrangement with almost perfect octahedral coordination geometry. In addition to the coordinating cobalt complex, there are six uncoordinated water molecules, which complete the crystal structure. In the solid state, the title compound forms three dimensional network structure through hydrogen bonds. The intermolecular hydrogen bonds connect the [CoCl2(C2H2N3CH2CH2COPh)4] and H2O moieties. CCDC: 200711.展开更多
基金the National Natural Science Foundation of China (No. 20431010)
文摘The two title complexes, [Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5- (NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal = 3,5-dinitrosalicylate, 2,2'-bipy = 2,2′-bipyridine), were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic, space group P1, a = 5.581(4), b = 12.071(8), c = 12.88(1)A, α= 92.10(3),β= 96.73(3), γ = 102.02(2)°, C17H10N407Cd, Mr = 494.69, V= 841(1)A3, Z = 2, Dc = 1.954 g/cm3, F(000) = 488, μ= 1.353 mm^-1, R = 0.0248 and wR = 0.0761. Complex 2 crystallizes in monoclinic with space group P21/c, a = 8.604(3), b = 23.88(1), c = 8.894(3) A, β = 102.45(1)°, C17H10N407Mn, Mr = 437.23, V= 1785(1) A3, Z=.4, Dc = 1.627 g/cm3, F(000) = 884, μ = 0.791 mm^-1, R = 0.0471 and wR = 0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2)A. The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.
基金This work was financially supported by the National Natural Science Foundation of China the Key Project of Chinese Academy of Sciences
文摘The reaction of 4-hydroxybenzoic acid (H2L),4, 4-diaminodiphenylmethane (DADPM) and Cd(NO3)2?H2O in methane/water gave rise to a seven-coordinate Cd(Ⅱ) complex [Cd2(HL)4(H2O)6]?H2O which has been characterized by single-crystal X-ray diffraction. The complex crystallizes in the orthorhombic system, space group Pna21 with unit cell parameters: a = 10.3352(3), b = 12.0481(3), c = 28.2016(1) ? V = 3511.65(13) 3, Z = 4, C28H36Cd2O20, Mr = 917.37, Dc = 1.735 g/cm3, F(000) = 1840, (MoK? = 1.29mm-1. The final R and wR are 0.0536 and 0.1086 for 4898 observed reflections with I ≥ 4(I). The Cd(Ⅱ) is seven-coordinated in a distorted pentagonal bipyramidal geometry. The inter-molecular hydrogen bonds lead to the formation of a two-dimensional layer structure.
基金Supported by the National Natural Science Foundation of China (No. 20171026) and Natural Science Foundation of Tianjin (No. 013605811)
文摘The title complex [CdLCl2] 1 (C10H15CdCl2N3, Mr = 360.55) has been synthesized by the reaction of CdCl22.5H2O with the tridentate Schiff base L, N,N-dimethyl-N-pyridin-2-yl- methylene-1,2-diaminoethane, which is derived from the condensation reaction of pyridine-2- carboxaldehyde and N,N-dimethylethylenediamine. It crystallizes in the monoclinic system, space group C2/c with a = 25.054(13), b = 7.532(4), c = 16.119(8) ? b = 116.238(8)? V = 2728(2) ?, Z = 8, Dc = 1.756 g/cm3, m(MoKa) = 1.970 mm-1, F(000) = 1424, R = 0.0297 and wR = 0.0625. Crystal analyses reveal that the cadmium atom is coordinated by two chlorine atoms and three N atoms from the tridentate ligand in a distorted tetragonal pyramidal environment. Each complex molecule is connected with four surrounding ones to form 2D network by hydrogen bonds along the bc plane. The chlorine atoms act as acceptors and the carbon atoms of the tridentate Schiff base as donors with the CH…Cl distances in the range of 3.518~3.752 ?
基金supported by the Scientific Research Fund of Hebei Provincial Education Department (2006114)
文摘The complex [Cd(H2mbdpz)(N3)2]n 1 (H2mbdpz = 4,4′-methylenebis(3,5-dimethylpyrazole)) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in the monoclinic system, space groups C2/c with a = 22.154(5), b = 7.4835(15), c = 21.044(8)A^°,β= 115.51(3)°, V= 3148.7(17)A^°3, Z= 8, C11H16CdN10, Mr = 400.75, Dc = 1.691 g/cm^3,μ = 1.401 mm^-1, F(000) = 1599, T= 293(2) K, the final R = 0.0228 and wR = 0.0581 for 3604 observed reflections with I 〉 2σ(I). The structural determination revealed that the coordination environment of Cd(Ⅱ) atom is a distorted octahedron consisting of two nitrogen donors of two H2mbdpz ligands and four nitrogen donors from four azide ligands. The azide moieties act as bridges in two modes: end-on (μ1,1-) and end-to-end (μ1,3-), and H2mbdpz also serves as a bridge with a bis-monodentate coordination. Both bridging ligands link the Cd(Ⅱ) atoms to form a distorted two-dimensional (6,3) layer.
基金Supported by the National Natural Science Foundation of China (20571039, 20171020) the Ministry of Education of China (20050284031)
文摘A novel coordination polymer [{Cd(hmbdc)(H20)3}-2H20],, (hmbdc = 5-hydroxyisophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2Jc, with a = 9.599(3), b = 18.699(5), c = 7.557(2) A, r= 108.198(4)°, V= 1288.6(6) A3, Z= 4, M,.= 382.60, Dc = 1.972 g/cm^, F(000) = 760, p = 1.740, the final R =0.0555 and wR = 0.0995 for 1732 observed reflections with 1 〉 2σ(I). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.
基金This work was supported by the National Natural Science Foundation of China (No. 20571057)
文摘A polynuclear complex [Cd(endc)(H20)]n·nH2O (endc = endo-norbornene-cis- 5,6-dicarboxylate anion) has been synthesized by the hydrothermal reaction of cadmium nitrate tetrahydrate with endo-norbornene-cis-5,6-dicarboxylic acid in 1:1 molar ratio, and structurally characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/c with α = 1.16471(7), b = 0.95334(7), c = 0.91109(9) nm, Z= 4, V= 1.01035(14) nm^3, D, = 2.160 g/cm^3,μ = 2.172 mm^-1, F(000) = 648, R = 0.0302 and wR = 0.0752. According to structural analysis, each Cd(II) ion is coordinated to six O atoms from three endc anions and one water molecule, giving a distorted octahedral geometry. Two- dimensional layer arrangement of the title complex is constructed from the bridging nature of endc. It is worth notice that adjacent two-dimensional layers are joined together to form a three-dimensional supramolecular framework via intermolecular hydrogen bonding interactions.
基金This work was supported by the NSF for Distinguished Young Scientist of China (20425104) and the NSF of Fujian Province (2005I017, A0420002)
文摘A new flexible double betaine L (L = 1,4-bis(pyridinio-4-carboxylato-N-methyl)benzene, C20H16N2O4) and its cadmium(Ⅱ) complex [Cd(H2O)aL(NO3)]NO3.H2O 1 were synthesized. Complex 1 was obtained by self-assembly reaction of [Cd(NO3)2]-4H2O and L in hot water,and its crystal structure was determined by single-crystal X-ray diffraction analysis. Crystallographic data for complex 1: C20H24CdN4O14.H2O, Mr = 674.85, monoclinic, space group P21/c, a =13.7854(3), b = 14.2820(3), c = 14.9188(4) ,A°, β = 116.418(1)°, V = 2630.5(1)A°^3, Z = 4, Dc= 1.704g/cm^3,/J(MoKα) = 0.911 mm^-1, F(000) = 1368, the final R = 0.0315 and wR = 0.0768 for 3637 observed reflections with I 〉 2σ(I). In complex 1, L acts as a monodentate ligand to link a Cd(Ⅱ) ion in a novel coordination mode of double betaines. The mononuclear [Cd(H2O)aL(NO3)] units are connected through intermolecular hydrogen bonds and π-π stacking reactions to generate a 3D network.
文摘complex[Ni(La) 2 ](NO 3 )2 (1)with bidentate racemic1,2,2-trimethylcyclopentane-1,3-diamine lig-and has been synthesized and characterized by IR,EA,ES-MS,and its X-ray diffracti on study reveals that the nickel (Ⅱ)abstract: center is tetra-coordinated by one D-and one L-diamine ligands,and a thre e-dimensional hydrogen-bond-sustained network is formed in the solid state by means of the eight-membered N-H...O hydrogen bond cy-cle.This compound also su pplies a good comparison to the chiral complex[Ni(L b )2 ]Cl 2 ·2H 2 O(2)(L b =D-(+)abstract:-1,2,2-trimethylcyclopentane-1,3-diamine)abstract:.CCDC:218122.
文摘RAJ S.Shanmuga Sundara FUN Hoong Kun (X ray Crystallography Unit, School of Physics, Universiti Sains Malaysia 11800 USM, Penang, Malaysia) The complex [Co(Im)6](Cin)2 (Im=imidazole,Cin=cinnamate) was prepared by reaction of Co(PhCHCHCOO)2 with imidazole in ethanol. It has been determined by single crystal X ray analyses. The crystals are triclinic, space group , with a=9.7601(3),b=10.5935(3),c=11.3269(2)? ,α =69.948(1),β =71.027(1),γ =62.803(1)° , and Z=1. The crystal structure of the title complex consists of monomeric [Co(Im)6]2+ cations and cinnamate anions in which the cobalt? ion assumes a centrosymmetric octahedral geometry with the CoN6 chromophore. In the solid state, the complex forms a three dimensional network through N- H… O hydrogen bonds, the intermolecular hydrogen bonds connect the [Co(Im)6]2+ cations and cinnamate anions.The cinnamate anions are nearly planar.
文摘The crystal and molecular structure of [CoCl2(N4 trzCH2CH2COPh)4]·6H2O (trz=1,2,4 triazole) has been determined by X ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with unit cell parameters a=0.8039(2)nm, b=1.0822(2)nm, c=2.9013(6)nm, β=94.79(3)°, and Z=4. Each cobalt atom is coordinated by four N atoms of triazole from four 1 propiophenone 1,2,4 triazole ligands and two chloride anion in cis arrangement with almost perfect octahedral coordination geometry. In addition to the coordinating cobalt complex, there are six uncoordinated water molecules, which complete the crystal structure. In the solid state, the title compound forms three dimensional network structure through hydrogen bonds. The intermolecular hydrogen bonds connect the [CoCl2(C2H2N3CH2CH2COPh)4] and H2O moieties. CCDC: 200711.