A new Ni（II） complex, [Ni（ftsc）2NO3]NO3 （Hftsc = furan-2-carbaldehyde thiosemicarbazone）, has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystalfizes i...A new Ni（II） complex, [Ni（ftsc）2NO3]NO3 （Hftsc = furan-2-carbaldehyde thiosemicarbazone）, has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystalfizes in a monoclinic system, space group P2 1/n, with a = 10.5203（13）, b = 9.2094（11）, c = 20.829（3）A,β = 91.518（2）°, V= 2 017.3（5）A^3, Z = 4, F（000） = 1064, Dc = 1.716 g/cm^3, and wR = 0.0800. The complex contains a six-coordinated nickel（II） center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H…O and C-H…O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.展开更多
The reaction of anhydrous cobalt(II) dichloride with 1-methylimidazoline-2(3H)- thione in dichloromethane solution gave the title complex, [Co(C4H6N2S)2Cl2]. X-ray single-crystal analysis revealed that the complex c...The reaction of anhydrous cobalt(II) dichloride with 1-methylimidazoline-2(3H)- thione in dichloromethane solution gave the title complex, [Co(C4H6N2S)2Cl2]. X-ray single-crystal analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, a = 13.9707(10), b = 10.0435(7), c = 10.3910(6) ?, β = 91.181(3)o, V = 1457.70(17) ?3, Z = 4, C8H12Cl2N4S2Co, Mr = 358.17, Dc = 1.632 g/cm3, μ = 1.813 mm–1, F(000) = 724, the final R = 0.0710 and wR = 0.1224 for 1549 observed reflections with I > 2σ(I). The Co atom is coordinated by two S atoms from two 1-methylimidazoline-2(3H)-thione ligands and two chloride ions in a slightly distorted tetrahedral geometry. The intramolecular classical hydrogen-bonding interactions involving chloride ions and N–H groups of the heterocyclic thione ligands are observed. The offset π-π stacking interactions between the imidazole rings of adjacent molecules with a face-to-face dis- tance of 3.604 ? are found in the packing diagram.展开更多
The title compound (C6H5NH2)2PdCl2 was prepared by the reaction of N-phenylbenzaldimine with dichlorobis(benzonitrile) palladium (Ⅱ) in methanol and its structure was characterized by single-crystal X-ray diffraction...The title compound (C6H5NH2)2PdCl2 was prepared by the reaction of N-phenylbenzaldimine with dichlorobis(benzonitrile) palladium (Ⅱ) in methanol and its structure was characterized by single-crystal X-ray diffraction. The title complex crystallizes in monoclinic system, space group P21/c, C12H14Cl2N2Pd, Mr = 363.55, a = 6.0668(7), b = 4.7691(5), c = 23.006(3) ? b = 95.118(2)? V = 662.99(13) ?, Z = 2, Dc = 1.821 g/cm3, m = 1.780 mm-1, F(000) = 360, the final R = 0.0624 and wR = 0.1271 for 850 observed reflections. Two bifurcated intermolecular NH…Cl hydrogen bonds are observed, forming a strip structure.展开更多
The crystal structure of the title complex, [NiL], has been determined by using X-ray analysis (H2L = 2,3-dioxo-5,6:13,14-dibenzo-7,12-bis(methoxycarbonyl)-1,4,8,11-tetraazacyclotetra- deca-7,11-diene). Crystal data: ...The crystal structure of the title complex, [NiL], has been determined by using X-ray analysis (H2L = 2,3-dioxo-5,6:13,14-dibenzo-7,12-bis(methoxycarbonyl)-1,4,8,11-tetraazacyclotetra- deca-7,11-diene). Crystal data: C22H18N4O6Ni, Mr = 493.11, triclinic, space group P, a = 9.128(6), b = 9.941(7), c = 12.396(8) ? a = 107.11(1), b = 106.14(1), g = 97.69(1), V = 1003.9(11) 3, Z = 2, Dc = 1.631 g/cm3, m(MoKa) = 1.018 mm-1, F(000) = 508, R = 0.0584 and wR = 0.0981 for 1724 observed reflections with I > 2s(I). The Ni(II) atom is coordinated by four nitrogen donors of the macrocyclic ligand with a slightly distorted square-planar geometry. In the crystal, the CH…O hydrogen bonds link the complex molecules to form infinite 1D chains which are further linked by p…p stacking interactions to form chain-pairs.展开更多
A noval cobalt(II) coordination polymer, {[Co(bpmb)(H2O)2(C2H5OH)2]?NO3)2}∞ (1), where bpmb=N,N'- bis(3-pyridylmethyl)-1,4-benzenedicarboxamide, was synthesized by self-assembly of the two topic ligands with coba...A noval cobalt(II) coordination polymer, {[Co(bpmb)(H2O)2(C2H5OH)2]?NO3)2}∞ (1), where bpmb=N,N'- bis(3-pyridylmethyl)-1,4-benzenedicarboxamide, was synthesized by self-assembly of the two topic ligands with cobalt nitrate in ethanol solution, and characterized structurally by X-ray crystallography analysis. The crystal data belong to triclinic, space group P1with cell parameters a=0.8911(3) nm, b=0.9042(3) nm, c=1.0068(3) nm, =73.083(5)? =81.069(5)? =76.210(5)? R1=0.0518, wR2=0.0947. The results of structure analysis indicate that each bpmb ligand coordinates two Co(II) atoms and each metal atom is in octahedral coordination geometry with four oxygen atoms of two ethanol and two water molecules, two nitrogen atoms from two different bpmb ligands in trans position forming an infinite 1D chain-like structure. There are hydrogen bonding and - stacking interaction among these chains,leading to supramolecular formation with 3D net structure.展开更多
A dipyrazol-bridged macrocyclic palladium(II) complex [{Pd(en)}4L4](NO3)8 (en=ethylenediamine, L=3,3′,5,5′-tetramethyldipyrazol) 1 was prepared in water through a macrocyclization of cis-(ethylenediamine)Pd(II) nitr...A dipyrazol-bridged macrocyclic palladium(II) complex [{Pd(en)}4L4](NO3)8 (en=ethylenediamine, L=3,3′,5,5′-tetramethyldipyrazol) 1 was prepared in water through a macrocyclization of cis-(ethylenediamine)Pd(II) nitrate and the neutral form of the dipyrazol ligand 3,3′,5,5′-tetramethyldipyrazol. This cationic palladium macrocycle is highly distorted rather than a planar macrocycle and can hold eight nitrate anions around the macrocyclic framework through both hydrogen bonding and electrostatic interactions. CCDC: 192017.展开更多
A novel pyrazolato-bridged di-palladium髤 complex, {[(phen)Pd(Me2Pz-H)]2(μ-Me2Pz)}(NO3)(BF4)2(MeCN)(Me2Pz-H=3,5-dimethyl pyrazole; μ-Me2Pz=3,5-dimethyl pyrazolate), was synthesized and characterized by the element a...A novel pyrazolato-bridged di-palladium髤 complex, {[(phen)Pd(Me2Pz-H)]2(μ-Me2Pz)}(NO3)(BF4)2(MeCN)(Me2Pz-H=3,5-dimethyl pyrazole; μ-Me2Pz=3,5-dimethyl pyrazolate), was synthesized and characterized by the element analysis and single crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with unit cell parameters: a=1.131 6(3) nm, b=1.858 5(4) nm, c=2.127 0(5) nm, β=90.037(4)°, and V=4.473 2(18) nm3, Z=4, R=0.043 3, wR=0.123 7. The X-ray crystal structure analysis revealed that two Pd髤 atoms were bridged by one pyrazolate, and the other two pyrazole molecules were coordinated to the two Pd髤 atoms, respectively. The Pd...Pd separation within the complex is 0.349 2(1)nm, indicating quite weak interaction. CCDC: 290065.展开更多
A new cadmium-organic framework, [Cd2（TBDC）2（DMF）2（H2O）]n （1）, was synthesized by solvothermal reaction of rigid carboxylate ligand 2,3,5,6-tetramethyl-l,4-ben- zenedicarboxylate （H2TBDC） and cadmium nitrate...A new cadmium-organic framework, [Cd2（TBDC）2（DMF）2（H2O）]n （1）, was synthesized by solvothermal reaction of rigid carboxylate ligand 2,3,5,6-tetramethyl-l,4-ben- zenedicarboxylate （H2TBDC） and cadmium nitrate and characterized by elemental analysis, infrared spectrum, thermal analysis, PXRD, single-crystal X-ray diffraction and photoluminescence in the solid state. Compound 1 crystallizes in orthorhombic, space group Pca21 with a = 21.487（6）, b = 7.790（2）, c = 20.666（6） A, C30H40Cd2N2O11, Mr = 829.44, V= 3459.3（16） A3, Z = 4, Dc = 1.593 g.cm-3,μ = 1.29 mm-1, F（000） = 1672, 2.7〈θ〈27.2°, λ（MoKa） = 0.71073 A, T= 293（2） K, the final R = 0.026, wR = 0.0548 and S = 1.027. X-ray diffraction analysis reveals that complex 1 possesses a 3D framework and exhibits rnsw net. Thus, the solid-state luminescent spectrum of 1 displays that the emission of cadmium（lI） complex shows a peak at 317 nm upon 250 nm excitation at room temperature.展开更多
基金the Ministry of Education of China (No. 207068)the Natural Science Foundation of Henan Province (No. 0611023000)the Education Department of Henan Province (No. 2007150003, 2007150011)
文摘A new Ni（II） complex, [Ni（ftsc）2NO3]NO3 （Hftsc = furan-2-carbaldehyde thiosemicarbazone）, has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystalfizes in a monoclinic system, space group P2 1/n, with a = 10.5203（13）, b = 9.2094（11）, c = 20.829（3）A,β = 91.518（2）°, V= 2 017.3（5）A^3, Z = 4, F（000） = 1064, Dc = 1.716 g/cm^3, and wR = 0.0800. The complex contains a six-coordinated nickel（II） center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H…O and C-H…O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.
基金Supported by the National Natural Science Foundation of China (20325106 20333070)and the "One-hundred Talent" Project from the Chinese Academy of Sciences
文摘The reaction of anhydrous cobalt(II) dichloride with 1-methylimidazoline-2(3H)- thione in dichloromethane solution gave the title complex, [Co(C4H6N2S)2Cl2]. X-ray single-crystal analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, a = 13.9707(10), b = 10.0435(7), c = 10.3910(6) ?, β = 91.181(3)o, V = 1457.70(17) ?3, Z = 4, C8H12Cl2N4S2Co, Mr = 358.17, Dc = 1.632 g/cm3, μ = 1.813 mm–1, F(000) = 724, the final R = 0.0710 and wR = 0.1224 for 1549 observed reflections with I > 2σ(I). The Co atom is coordinated by two S atoms from two 1-methylimidazoline-2(3H)-thione ligands and two chloride ions in a slightly distorted tetrahedral geometry. The intramolecular classical hydrogen-bonding interactions involving chloride ions and N–H groups of the heterocyclic thione ligands are observed. The offset π-π stacking interactions between the imidazole rings of adjacent molecules with a face-to-face dis- tance of 3.604 ? are found in the packing diagram.
基金This work was financially supported by the NNSF of China (No. 29733090 and No. 20173063) Key Project in KIP of CAS (KJCX2-H3) and the NSF of Fujian Province (E0020001)
文摘The title compound (C6H5NH2)2PdCl2 was prepared by the reaction of N-phenylbenzaldimine with dichlorobis(benzonitrile) palladium (Ⅱ) in methanol and its structure was characterized by single-crystal X-ray diffraction. The title complex crystallizes in monoclinic system, space group P21/c, C12H14Cl2N2Pd, Mr = 363.55, a = 6.0668(7), b = 4.7691(5), c = 23.006(3) ? b = 95.118(2)? V = 662.99(13) ?, Z = 2, Dc = 1.821 g/cm3, m = 1.780 mm-1, F(000) = 360, the final R = 0.0624 and wR = 0.1271 for 850 observed reflections. Two bifurcated intermolecular NH…Cl hydrogen bonds are observed, forming a strip structure.
基金This work was supported by the National Natural Science Foundation of China (20071019, 50172021 and 90101028)
文摘The crystal structure of the title complex, [NiL], has been determined by using X-ray analysis (H2L = 2,3-dioxo-5,6:13,14-dibenzo-7,12-bis(methoxycarbonyl)-1,4,8,11-tetraazacyclotetra- deca-7,11-diene). Crystal data: C22H18N4O6Ni, Mr = 493.11, triclinic, space group P, a = 9.128(6), b = 9.941(7), c = 12.396(8) ? a = 107.11(1), b = 106.14(1), g = 97.69(1), V = 1003.9(11) 3, Z = 2, Dc = 1.631 g/cm3, m(MoKa) = 1.018 mm-1, F(000) = 508, R = 0.0584 and wR = 0.0981 for 1724 observed reflections with I > 2s(I). The Ni(II) atom is coordinated by four nitrogen donors of the macrocyclic ligand with a slightly distorted square-planar geometry. In the crystal, the CH…O hydrogen bonds link the complex molecules to form infinite 1D chains which are further linked by p…p stacking interactions to form chain-pairs.
文摘A noval cobalt(II) coordination polymer, {[Co(bpmb)(H2O)2(C2H5OH)2]?NO3)2}∞ (1), where bpmb=N,N'- bis(3-pyridylmethyl)-1,4-benzenedicarboxamide, was synthesized by self-assembly of the two topic ligands with cobalt nitrate in ethanol solution, and characterized structurally by X-ray crystallography analysis. The crystal data belong to triclinic, space group P1with cell parameters a=0.8911(3) nm, b=0.9042(3) nm, c=1.0068(3) nm, =73.083(5)? =81.069(5)? =76.210(5)? R1=0.0518, wR2=0.0947. The results of structure analysis indicate that each bpmb ligand coordinates two Co(II) atoms and each metal atom is in octahedral coordination geometry with four oxygen atoms of two ethanol and two water molecules, two nitrogen atoms from two different bpmb ligands in trans position forming an infinite 1D chain-like structure. There are hydrogen bonding and - stacking interaction among these chains,leading to supramolecular formation with 3D net structure.
文摘A dipyrazol-bridged macrocyclic palladium(II) complex [{Pd(en)}4L4](NO3)8 (en=ethylenediamine, L=3,3′,5,5′-tetramethyldipyrazol) 1 was prepared in water through a macrocyclization of cis-(ethylenediamine)Pd(II) nitrate and the neutral form of the dipyrazol ligand 3,3′,5,5′-tetramethyldipyrazol. This cationic palladium macrocycle is highly distorted rather than a planar macrocycle and can hold eight nitrate anions around the macrocyclic framework through both hydrogen bonding and electrostatic interactions. CCDC: 192017.
文摘A novel pyrazolato-bridged di-palladium髤 complex, {[(phen)Pd(Me2Pz-H)]2(μ-Me2Pz)}(NO3)(BF4)2(MeCN)(Me2Pz-H=3,5-dimethyl pyrazole; μ-Me2Pz=3,5-dimethyl pyrazolate), was synthesized and characterized by the element analysis and single crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with unit cell parameters: a=1.131 6(3) nm, b=1.858 5(4) nm, c=2.127 0(5) nm, β=90.037(4)°, and V=4.473 2(18) nm3, Z=4, R=0.043 3, wR=0.123 7. The X-ray crystal structure analysis revealed that two Pd髤 atoms were bridged by one pyrazolate, and the other two pyrazole molecules were coordinated to the two Pd髤 atoms, respectively. The Pd...Pd separation within the complex is 0.349 2(1)nm, indicating quite weak interaction. CCDC: 290065.
基金Supported by the NNSFC(Nos.90922014,21271117)NCET-11-0309+2 种基金the Shandong Natural Science Fund for Distinguished Young Scholars(JQ201003)Independent Innovation Foundation of Shandong University(2010JQ011)Fundamental Research Funds for the Central Universities(13CX05010A)
文摘A new cadmium-organic framework, [Cd2（TBDC）2（DMF）2（H2O）]n （1）, was synthesized by solvothermal reaction of rigid carboxylate ligand 2,3,5,6-tetramethyl-l,4-ben- zenedicarboxylate （H2TBDC） and cadmium nitrate and characterized by elemental analysis, infrared spectrum, thermal analysis, PXRD, single-crystal X-ray diffraction and photoluminescence in the solid state. Compound 1 crystallizes in orthorhombic, space group Pca21 with a = 21.487（6）, b = 7.790（2）, c = 20.666（6） A, C30H40Cd2N2O11, Mr = 829.44, V= 3459.3（16） A3, Z = 4, Dc = 1.593 g.cm-3,μ = 1.29 mm-1, F（000） = 1672, 2.7〈θ〈27.2°, λ（MoKa） = 0.71073 A, T= 293（2） K, the final R = 0.026, wR = 0.0548 and S = 1.027. X-ray diffraction analysis reveals that complex 1 possesses a 3D framework and exhibits rnsw net. Thus, the solid-state luminescent spectrum of 1 displays that the emission of cadmium（lI） complex shows a peak at 317 nm upon 250 nm excitation at room temperature.
