Two new metal-organic complexes [Cd2(1,4-BDC)(4-pytyp)(H2O)4]·(1,4-BDC)(1) and [Cu2(1,4-BDC)(4-pytyp)2(H2O)2]·(1,4-BDC)·8H2O(2)(4-pytyp = 4'-(4''-pyridyl)-2,2':6',2''-terp...Two new metal-organic complexes [Cd2(1,4-BDC)(4-pytyp)(H2O)4]·(1,4-BDC)(1) and [Cu2(1,4-BDC)(4-pytyp)2(H2O)2]·(1,4-BDC)·8H2O(2)(4-pytyp = 4'-(4''-pyridyl)-2,2':6',2''-terpyridine, 1,4-H2 BDC = 1,4-benzenedicarboxylic acid) have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The scrutiny of single-crystal structure reveals that complex 1 forms to a 3D supramolecular network linked by π-π stacking interactions and hydrogen bonds. X-ray diffraction analysis reveals that complex 2 exhibits a 3D supramolecular network linked through complicated hydrogen bonds. The thermogravimetric analysis and photoluminescent properties of 1 and 2 are discussed in detail.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
A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space gro...A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 with a = 15.630(3), b = 15.990(3), c = 16.330(3) ?, α = 89.90(3), β = 68.87(3), γ = 87.94(3)o, V = 3804.1(13) ?3, Mr = 1034.22, Z = 4, F(000) = 2060, Dc = 1.806 g/cm3, T = 293(2) K, μ = 1.468 mm-1 and λ = 0.71073 ?. The structure was refined to R = 0.0779 and wR = 0.1960 for 7034 observed reflections with I > 2σ(I).展开更多
Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR,...Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.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 cadmium complex [Cd(phen)3]·(ClO4)2·(α-FRA)-(H2O)3 was prepared by self-assembly of α-furoic acid, 1,10-phenanthroline (phen), and cadmium perchlorate. It crystallizes in the monoclinic sys...A new cadmium complex [Cd(phen)3]·(ClO4)2·(α-FRA)-(H2O)3 was prepared by self-assembly of α-furoic acid, 1,10-phenanthroline (phen), and cadmium perchlorate. It crystallizes in the monoclinic system, space group P21/n, with a = 1.28130(15), b = 2.5957(3), c = 1.35449(16) nm, β = 109.395(2)°, V = 4.2492(9) nm^3, Dc = 1.491 g/cm^3, Z = 4, F(000) = 1926, GOOF = 1.023, the final R = 0.0729 and wR = 0.2086. The crystal structure analysis indicates that the cadmium ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated.展开更多
One new luminescent material of complex {[Cd(DPA)(H_2O)_2]·(H_2O)_2}_n(1) was synthesized by evaporation methods using 3,3A-thiodipropionic acid(DPA) and cadmium nitrate as the starting materials. Compo...One new luminescent material of complex {[Cd(DPA)(H_2O)_2]·(H_2O)_2}_n(1) was synthesized by evaporation methods using 3,3A-thiodipropionic acid(DPA) and cadmium nitrate as the starting materials. Compound 1 crystallizes in the monoclinic system,space group P2_1/n with a = 7.5460(7),b = 13.372(3),c = 12.304(3) A,β = 95.95(3)o,V = 1234.8(4) A^3,D_c = 1.940 g/cm^3,C_6H_(16)O_8 SCd,M_r = 360.65,F(000) = 720,μ(Mo Ka) = 1.960 mm^-1,Z = 4,R = 0.0460 and wR = 0.1185 for 1835 observed reflections(I 〉 2σ(I)),and R = 0.0591,wR = 0.1245 for all data. The complex has been characterized by elemental analysis,FT-IR,TG,PXRD and X-ray single-crystal structure analysis and the fluorescence property has also been studied. As a result,complex 1 possesses a two-dimensional(2-D) structure through DPA ligands interconnecting Cd2+ ions. Complex 1 emits the intense fluorescence of 420 nm in the solid state at room temperature.展开更多
The compound [Cd(L)2(NO3)]NO3·0.5H2O (L = N-benzyl-2-(quinolin-8-yloxy)aceta- mide) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction, elemental analysis, IR and UV sp...The compound [Cd(L)2(NO3)]NO3·0.5H2O (L = N-benzyl-2-(quinolin-8-yloxy)aceta- mide) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction, elemental analysis, IR and UV spectroscopy. The crystal belongs to the triclinic system, space group P1 with a = 11.7175(13), b = 11.8873(13), c = 14.0958(16) A, α = 74.889(2), β= 78.228(2), γ = 78.831(2)°, V= 1835.0(4) A3, Z= 1, Dc= 1.502 Mg/m3, Mr = 1660.17,μ = 0.662 mm-1, F(000) = 846, 2(MoKa) = 0.71073 A, the final R = 0.0585 and wR = 0.0577 for all observed reflections. The results show that the Cd(II) ion with a square antiprismatic geometry is coordinated by a N206 donor set, two NO2 sets from two ligands and two O atoms from a bidendate nitrate group. In the crystal, the O-H...O and N-H...O hydrogen bonds are helpful to consolidate the three- dimensional network.展开更多
A new cadmium(Ⅱ) complex[Cd(Hminic)(IP)]n(1,Hminic = 2-hydroxy-6-methylisonicotinic acid,IP = imidazo[4,5-f]-l,10-phenanthroline),has been synthesized by the reaction of a Hminic and auxiliary N-containing li...A new cadmium(Ⅱ) complex[Cd(Hminic)(IP)]n(1,Hminic = 2-hydroxy-6-methylisonicotinic acid,IP = imidazo[4,5-f]-l,10-phenanthroline),has been synthesized by the reaction of a Hminic and auxiliary N-containing ligands with Cd(Ⅱ) ion under hydrothermal conditions.The complex was studied by elemental analysis,IR spectroscopy and X-ray crystallography.It is formulated as C(20)H(13)CdN5O3,crystallizes in monoclinic system,space group C2/c with α=9.6764(8),b = 26.767(2),c = 14.1332(11) A and β= 97.4510(10)°.V= 3629.7(5) A^3,Z = 8,Mr=483.75,Dc = 1.770 g/cm^3,F(000) = 1484 and μ= 1.237 mm^(-1).The final refinement gave R = 0.0309 and wR = 0.0703 for 4151 reflections with I 〉2σ(I).In the structure of 1,two Cd(Ⅱ) atoms are joined by a pair of μ2-hydroxyl oxygen atoms giving rise to a dinuclear Cd(Ⅱ) unit which is bridged by Hminic linkers to form a 1D ladder-like polymer chain.The chelating ligand IP coordinated to the Cd(Ⅱ) atom,and alternately attached to both sides of the ladder-like polymer chain.Adjacent chains are further bound together by strong intermolecular hydrogen bonds and face-to-face π…πinteractions,resulting in the formation of a 3D supramolecular architecture.Furthermore,the thermal stability and luminescent properties of this complex and the free ligands have been investigated.展开更多
The title complex 1,[Cd 4 Cu 2 (pdc) 4 (H 2 O) 14 ] (H 3 pdc=3,5-pyrazoledicarboxylic acid),has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crysta...The title complex 1,[Cd 4 Cu 2 (pdc) 4 (H 2 O) 14 ] (H 3 pdc=3,5-pyrazoledicarboxylic acid),has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1 with a=0.67235(10),b=1.27935(18),c=1.28569(17) nm,α=112.633(2),β=102.971(3),γ=97.089(2)o,V=0.9673(2) nm 3,C 20 H 32 Cd 4 Cu 2 N 8 O 30,M r=1441.22,D c=2.474 g/cm 3,μ(MoKα)=3.356 mm 1,F(000)=698,S=1.003,Z=1,the final R=0.0471 and wR=0.0748 for I 2σ(Ⅰ).In 1,two deprotonated 3,5-pyrazoledicarboxylic acids (pdc 3),one copper(Ⅱ) ion and one cadmium(Ⅱ) ion firstly form a pyrazole-bridged Cu II Cd II dinuclear unit,two of which related by an inversion center are connected by another two cadmium(Ⅱ) ions through chelating carboxylate groups to construct the copper(Ⅱ)-cadmium(Ⅱ) heterometallic hexanuclear complexes.Plenty of hydrogen bond interactions existing in the system further lead to a three-dimensional (3D) supramolecular framework.展开更多
Two new ternary complexes [Zη(3-aba)2(phen)]·2.58H2O 1 and {[Cd(3-aba)- (phen)2]·(NO3)·(1.5H2O) }n 2 (3-aba = 3-aminobenzoic acid anion, phen = 1,10-phenanthroline) were synthesized and c...Two new ternary complexes [Zη(3-aba)2(phen)]·2.58H2O 1 and {[Cd(3-aba)- (phen)2]·(NO3)·(1.5H2O) }n 2 (3-aba = 3-aminobenzoic acid anion, phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, IR, UV spectrum and X-ray diffraction. Complex 1 crystallizes in the rhombohedral system, space group R3 with a = 3.5733(3), b = 3.5733(3), c = 1.1231(2) nm; V= 12.419(3) nm^3, C26H25.17NaO6.58Zn, Mr= 564.37, Z= 18, F(000) = 5253, μ= 0.937 mm^-1, Dc = 1.358 g/cm^3, R = 0.0668 and wR = 0.1690 for 2424 observed reflections (I〉 2σ(I)). Complex 2 belongs to the tetragonal system, space group P4/ncc with a = 2.88451(10), b = 2.88451(10), c = 1.55571(11) nm, V= 12.9441(11) nm^3, C31H25CdN6O6.50, Mr = 697.97, Z = 16, F(000) = 5648,μ=0.727 mm^-1, Dc= 1.433 g/cm^3, R = 0.0607 and wR = 0.1742 for 3468 observed reflections (I 〉 2σ(I)). Complex 1 displays a mononuclear structure. The carboxylate group of 3-aminobenzoic acid anion coordinates to Zn(Ⅱ) in a chelating bidentate mode, and the nitrogen atom of the ligand does not involve in coordination. Complex 2 exhibits a one-dimensional chain structure with 3-aminobenzoic acid anion coordinating to Cd(Ⅱ) in a μ2-bridging mode through its nitrogen atom and one of its oxygen atoms.展开更多
基金Supported by the Program for New Century Excellent Talents in University(NCET-10-0176)the Natural Science Foundation of Jilin Province(No.20130521019JH)the fund of Jilin Provincial Education Department of China(No.2014154)
文摘Two new metal-organic complexes [Cd2(1,4-BDC)(4-pytyp)(H2O)4]·(1,4-BDC)(1) and [Cu2(1,4-BDC)(4-pytyp)2(H2O)2]·(1,4-BDC)·8H2O(2)(4-pytyp = 4'-(4''-pyridyl)-2,2':6',2''-terpyridine, 1,4-H2 BDC = 1,4-benzenedicarboxylic acid) have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The scrutiny of single-crystal structure reveals that complex 1 forms to a 3D supramolecular network linked by π-π stacking interactions and hydrogen bonds. X-ray diffraction analysis reveals that complex 2 exhibits a 3D supramolecular network linked through complicated hydrogen bonds. The thermogravimetric analysis and photoluminescent properties of 1 and 2 are discussed in detail.
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This project was supported by the National Natural Science Foundation of China(No.50372028)
文摘A new bicadmium(??) complex [Cd2L](ClO4)2?1.25H2O (C28H35Cd2Cl4N6O13.25) was synthesized and characterized by X-ray diffraction and ES mass spectral analyses. It crystallizes in the triclinic system, space group P1 with a = 15.630(3), b = 15.990(3), c = 16.330(3) ?, α = 89.90(3), β = 68.87(3), γ = 87.94(3)o, V = 3804.1(13) ?3, Mr = 1034.22, Z = 4, F(000) = 2060, Dc = 1.806 g/cm3, T = 293(2) K, μ = 1.468 mm-1 and λ = 0.71073 ?. The structure was refined to R = 0.0779 and wR = 0.1960 for 7034 observed reflections with I > 2σ(I).
基金Supported by the Natural Science Foundation of Education Department of Henan Province (No. 2011B150025)
文摘Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.
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Supported by the construct program of the key discipline in hunan provincethe Research Award Fund for the Outstanding Young Teachers of Hengyang Normal University (2006)
文摘A new cadmium complex [Cd(phen)3]·(ClO4)2·(α-FRA)-(H2O)3 was prepared by self-assembly of α-furoic acid, 1,10-phenanthroline (phen), and cadmium perchlorate. It crystallizes in the monoclinic system, space group P21/n, with a = 1.28130(15), b = 2.5957(3), c = 1.35449(16) nm, β = 109.395(2)°, V = 4.2492(9) nm^3, Dc = 1.491 g/cm^3, Z = 4, F(000) = 1926, GOOF = 1.023, the final R = 0.0729 and wR = 0.2086. The crystal structure analysis indicates that the cadmium ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated.
基金supported by the National Natural Science Foundation of China(No.51302067)the Team of Guangdong Ocean University(No.1312435)
文摘One new luminescent material of complex {[Cd(DPA)(H_2O)_2]·(H_2O)_2}_n(1) was synthesized by evaporation methods using 3,3A-thiodipropionic acid(DPA) and cadmium nitrate as the starting materials. Compound 1 crystallizes in the monoclinic system,space group P2_1/n with a = 7.5460(7),b = 13.372(3),c = 12.304(3) A,β = 95.95(3)o,V = 1234.8(4) A^3,D_c = 1.940 g/cm^3,C_6H_(16)O_8 SCd,M_r = 360.65,F(000) = 720,μ(Mo Ka) = 1.960 mm^-1,Z = 4,R = 0.0460 and wR = 0.1185 for 1835 observed reflections(I 〉 2σ(I)),and R = 0.0591,wR = 0.1245 for all data. The complex has been characterized by elemental analysis,FT-IR,TG,PXRD and X-ray single-crystal structure analysis and the fluorescence property has also been studied. As a result,complex 1 possesses a two-dimensional(2-D) structure through DPA ligands interconnecting Cd2+ ions. Complex 1 emits the intense fluorescence of 420 nm in the solid state at room temperature.
基金supported by the National Natural Science Foundation of China(21001040)
文摘The compound [Cd(L)2(NO3)]NO3·0.5H2O (L = N-benzyl-2-(quinolin-8-yloxy)aceta- mide) 1 has been synthesized and structurally determined by single-crystal X-ray diffraction, elemental analysis, IR and UV spectroscopy. The crystal belongs to the triclinic system, space group P1 with a = 11.7175(13), b = 11.8873(13), c = 14.0958(16) A, α = 74.889(2), β= 78.228(2), γ = 78.831(2)°, V= 1835.0(4) A3, Z= 1, Dc= 1.502 Mg/m3, Mr = 1660.17,μ = 0.662 mm-1, F(000) = 846, 2(MoKa) = 0.71073 A, the final R = 0.0585 and wR = 0.0577 for all observed reflections. The results show that the Cd(II) ion with a square antiprismatic geometry is coordinated by a N206 donor set, two NO2 sets from two ligands and two O atoms from a bidendate nitrate group. In the crystal, the O-H...O and N-H...O hydrogen bonds are helpful to consolidate the three- dimensional network.
基金supported by the National Natural Science Foundation of China(No.21273101)Tackle Key Problem of Science and Technology Project of Henan Province(No.142102310483)+1 种基金Program for Science&Technology Innovation Talents and Research Team in Universities of Henan(No.2014HASTIT014 and 4IRTSTHN008)Key Program of Foundation of Education Committee of Henan Province(No.14B150033)
文摘A new cadmium(Ⅱ) complex[Cd(Hminic)(IP)]n(1,Hminic = 2-hydroxy-6-methylisonicotinic acid,IP = imidazo[4,5-f]-l,10-phenanthroline),has been synthesized by the reaction of a Hminic and auxiliary N-containing ligands with Cd(Ⅱ) ion under hydrothermal conditions.The complex was studied by elemental analysis,IR spectroscopy and X-ray crystallography.It is formulated as C(20)H(13)CdN5O3,crystallizes in monoclinic system,space group C2/c with α=9.6764(8),b = 26.767(2),c = 14.1332(11) A and β= 97.4510(10)°.V= 3629.7(5) A^3,Z = 8,Mr=483.75,Dc = 1.770 g/cm^3,F(000) = 1484 and μ= 1.237 mm^(-1).The final refinement gave R = 0.0309 and wR = 0.0703 for 4151 reflections with I 〉2σ(I).In the structure of 1,two Cd(Ⅱ) atoms are joined by a pair of μ2-hydroxyl oxygen atoms giving rise to a dinuclear Cd(Ⅱ) unit which is bridged by Hminic linkers to form a 1D ladder-like polymer chain.The chelating ligand IP coordinated to the Cd(Ⅱ) atom,and alternately attached to both sides of the ladder-like polymer chain.Adjacent chains are further bound together by strong intermolecular hydrogen bonds and face-to-face π…πinteractions,resulting in the formation of a 3D supramolecular architecture.Furthermore,the thermal stability and luminescent properties of this complex and the free ligands have been investigated.
基金Nanjing University of Posts and Telecommunications (No. NY209032)Key Laboratory of Functional Inorganic Material Chemistry(Heilongjiang University),Ministry of Education,Science Foundation for Youths of Guangxi Province (No. 0991089)the Major State Basic Research Development Program of China (973 Program,No. 2009CB930600)
文摘The title complex 1,[Cd 4 Cu 2 (pdc) 4 (H 2 O) 14 ] (H 3 pdc=3,5-pyrazoledicarboxylic acid),has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1 with a=0.67235(10),b=1.27935(18),c=1.28569(17) nm,α=112.633(2),β=102.971(3),γ=97.089(2)o,V=0.9673(2) nm 3,C 20 H 32 Cd 4 Cu 2 N 8 O 30,M r=1441.22,D c=2.474 g/cm 3,μ(MoKα)=3.356 mm 1,F(000)=698,S=1.003,Z=1,the final R=0.0471 and wR=0.0748 for I 2σ(Ⅰ).In 1,two deprotonated 3,5-pyrazoledicarboxylic acids (pdc 3),one copper(Ⅱ) ion and one cadmium(Ⅱ) ion firstly form a pyrazole-bridged Cu II Cd II dinuclear unit,two of which related by an inversion center are connected by another two cadmium(Ⅱ) ions through chelating carboxylate groups to construct the copper(Ⅱ)-cadmium(Ⅱ) heterometallic hexanuclear complexes.Plenty of hydrogen bond interactions existing in the system further lead to a three-dimensional (3D) supramolecular framework.
基金This work was supported by the Natural Science Foundation of Guangxi Province (No. 0229004)
文摘Two new ternary complexes [Zη(3-aba)2(phen)]·2.58H2O 1 and {[Cd(3-aba)- (phen)2]·(NO3)·(1.5H2O) }n 2 (3-aba = 3-aminobenzoic acid anion, phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, IR, UV spectrum and X-ray diffraction. Complex 1 crystallizes in the rhombohedral system, space group R3 with a = 3.5733(3), b = 3.5733(3), c = 1.1231(2) nm; V= 12.419(3) nm^3, C26H25.17NaO6.58Zn, Mr= 564.37, Z= 18, F(000) = 5253, μ= 0.937 mm^-1, Dc = 1.358 g/cm^3, R = 0.0668 and wR = 0.1690 for 2424 observed reflections (I〉 2σ(I)). Complex 2 belongs to the tetragonal system, space group P4/ncc with a = 2.88451(10), b = 2.88451(10), c = 1.55571(11) nm, V= 12.9441(11) nm^3, C31H25CdN6O6.50, Mr = 697.97, Z = 16, F(000) = 5648,μ=0.727 mm^-1, Dc= 1.433 g/cm^3, R = 0.0607 and wR = 0.1742 for 3468 observed reflections (I 〉 2σ(I)). Complex 1 displays a mononuclear structure. The carboxylate group of 3-aminobenzoic acid anion coordinates to Zn(Ⅱ) in a chelating bidentate mode, and the nitrogen atom of the ligand does not involve in coordination. Complex 2 exhibits a one-dimensional chain structure with 3-aminobenzoic acid anion coordinating to Cd(Ⅱ) in a μ2-bridging mode through its nitrogen atom and one of its oxygen atoms.