A new coordination complex [Cd(pda)(pyz)(H2O)2]n(1, H2 pda = 1,4-phenylenediacetic acid, pyz = pyrazine) have been synthesized and structurally characterized. Crystal data for the title complex are as follows: orthorh...A new coordination complex [Cd(pda)(pyz)(H2O)2]n(1, H2 pda = 1,4-phenylenediacetic acid, pyz = pyrazine) have been synthesized and structurally characterized. Crystal data for the title complex are as follows: orthorhombic system, space group Ccmb with a = 11.5245(3) b = 19.5069(5) c = 11.4231(3) A, V = 2568.00(12) A3, Mr = 188.31, Z = 16, F(000) = 1480, Dc = 1.948 g/cm3, μ(Mo Kα) = 1.725 mm-1, R = 0.0195 and w R = 0.0462 for 1357 observed reflections with I 】 2σ(I). In the title complex, the central Cd(II) ion is located in a distorted octahedral coordination environment. Two Cd(II) ions are bridged by two pda2- ligands and one pyz ligand to form a bi-loop structure. Luminescent property of the complex has also been studied.展开更多
A three-dimensional coordination polymer {[Cd2(HCAM)2(H2O)4].3.SH2O}n was synthesized by the hydrothermal reaction of H3CAM (H3CAM = 4-hydroxypyridine-2,6-dicerboxylic acid) and Cd(NO3)2·4H2O. The structu...A three-dimensional coordination polymer {[Cd2(HCAM)2(H2O)4].3.SH2O}n was synthesized by the hydrothermal reaction of H3CAM (H3CAM = 4-hydroxypyridine-2,6-dicerboxylic acid) and Cd(NO3)2·4H2O. The structure was characterized by elemental analysis, thermal gravimetric analysis, infrared spectroscopy and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.4389(19), b = 11.009(2), c = 11.192(2) A, α = 87.87(3), β= 74.63(3), γ = 81.22(3)°, V= 1108.2(4) A3, Z = 2, Dc= 2.164 g/cm3,μ = 2.011 mm^-1, F(000) = 710, R = 0.0419 and wR = 0.1170. X-ray analysis reveals that the title compound adopts a one-dimensional staircase structure by carboxyl of H3CAM and water molecules, and it is further linked by hydrogen bonds to form a 3-D metal-organic open framework. The thermal gravimetric analysis displays that the framework exists stably below 300 ℃.展开更多
The structure of a binuclear cadmium(Ⅱ) quaternary complex, [Cd2(phen)2- Q2(BP)]n 1 (phen = 1,10-phenanthroline, BP = biphenyl-4,4′-dicarboxylic acid, Q = 8-hydroxy- quinoline-anion), has been determined by ...The structure of a binuclear cadmium(Ⅱ) quaternary complex, [Cd2(phen)2- Q2(BP)]n 1 (phen = 1,10-phenanthroline, BP = biphenyl-4,4′-dicarboxylic acid, Q = 8-hydroxy- quinoline-anion), has been determined by X-ray crystallography and characterized by elemental analysis, IR spectrum and thermogravimetric analysis. It crystallizes in the monoclinic system, space group P21/n with a = 13.1906(18), b = 10.9623(15), c = 16.947(2)A, β = 111.3430(10)°, V = 2282.5(5)A^3, Z = 4, Mr = 556.85, Dc = 1.620 g/cm^3, F(000) = 1116,μ= 0.994 mm^-1 and S = 1.056. In the structure, 1D chains are connected via biphenyl-4,4′-dicarboxylic acid, 8-hydroxy quinoline anion and binuclear cadmium atoms into an infinite 1-D molecular chain architecture. Via aryl ring π-π stacking interactions a supramolecular structure is formed in 1.展开更多
Two new transition metal compounds, [Mn(dpa)2(tmd)2]n (1, H2dpa = 4-hydroxy-phenyl-acetic acid, tmd = 4,4-trimethylenedipyridine) and [Co4(dpa)6(tmd)4(H2O)4]n·nH2O·nCl2 (2), have been synthesiz...Two new transition metal compounds, [Mn(dpa)2(tmd)2]n (1, H2dpa = 4-hydroxy-phenyl-acetic acid, tmd = 4,4-trimethylenedipyridine) and [Co4(dpa)6(tmd)4(H2O)4]n·nH2O·nCl2 (2), have been synthesized by hydrothermal synthesis. Compound 1 crystallizes in the monoclinic system, space group P21/n with a = 9.828(3), b = 17.493(5), c = 11.616(4), β = 110.146(6)o, V = 1874.9(10)3, C42H42MnN4O6, Mr = 753.74, Z = 2, Dc = 1.335 g/cm3, μ = 0.406 mm-1, F(000) = 790, the final R = 0.1047 and wR = 0.2021 for 2698 observed reflections (I 〉 2σ(I)). Compound 2 crystallizes in the monoclinic system, space group P21/c with a = 11.7214(13), b = 17.1582(19), c = 24.625(3), β = 103.055(3)o, V = 4824.4(9)3, C100H104Cl2Co4N8O23, Mr = 2094.55, Z = 2, Dc = 1.443 g/cm3, μ = 0.809 mm-1, F(000) = 2180, the final R = 0.0550 and wR = 0.0673 for 4104 observed reflections (I 〉 2σ(I)). These complexes were characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. The structural analyses show that the two compounds are both one-dimensional chain structures. However, compounds 1 and 2 form threedimensional supramolecular structures by hydrogen bonds, respectively.展开更多
Three Cd(II) coordination complexes,{[Cd(bime)3](NO3)2·(H2O)3}n(1),[Cd(bime)Br2]n(2) and [(H2bime)(CdBr4)(H2O)]n(3)(bime = 1,2-bis(imidazol-1-yl)ethane),have been prepared and characteri...Three Cd(II) coordination complexes,{[Cd(bime)3](NO3)2·(H2O)3}n(1),[Cd(bime)Br2]n(2) and [(H2bime)(CdBr4)(H2O)]n(3)(bime = 1,2-bis(imidazol-1-yl)ethane),have been prepared and characterized.Single-crystal X-ray diffraction analysis reveals that 1~3 crystallize in the trigonal space group P-3,monoclinic space group C2/c and triclinic space group P1,respectively.In 1,bime bridges six-coordinated Cd(II) to generate a two-fold interpenetrating 3D coordination polymer,in which NO3- is not involved in coordination,but serves as a void filler to balance the charge of the 3D framework.The six NO3- and six uncoordinated water molecules form an unprecedented 24-membered macrocycle through hydrogen bonding interaction.In 2,bime in an anti-conformation links the CdBr2 units into a zigzag chain.In 3,bime does not take part in coordination,but is protonated to act as a counter cation of [CdBr4 ]2-.The hydrogen bonds between H2bime and [CdBr4]2- result in the formation of a supramolecular chain.展开更多
Three complexes obtained by the reaction of Pr(Ⅲ) or Nd(Ⅲ) salts with 5-methyl-2-pyrazinecarboxylic acid(Hmpca) are structurally determined by single-crystal X-ray diffraction.Complex [Pr(mpca-)3(H2O)2]2...Three complexes obtained by the reaction of Pr(Ⅲ) or Nd(Ⅲ) salts with 5-methyl-2-pyrazinecarboxylic acid(Hmpca) are structurally determined by single-crystal X-ray diffraction.Complex [Pr(mpca-)3(H2O)2]2·6H2O(1) is composed of dinuclear Pr(Ⅲ) units with two metal centers bridged by two anionic mpca-ligands in a κ^3O,O':O' bridging mode.Complexes [Pr(mpca-)3]n(2) and [Nd(mpca-)3]n(3) are isostructures,and they consist of polymeric chains based on Ln(Ⅲ) and mpca-ligands.Each pair of adjacent metal centers is linked by three mpca-molecules in a κ^3N,O:O bridging mode.展开更多
The 1-D chain coordination complex of {[Mn2(HCAM)3(H2bipy)]·5H2O}n (H3CAM = 4-hydroxypyridine-2,6-dicarboxylic acid, bipy = 4,4'-bipyridine) has been synthesized by the reaction of 4-hydroxypyridine-2,6-di...The 1-D chain coordination complex of {[Mn2(HCAM)3(H2bipy)]·5H2O}n (H3CAM = 4-hydroxypyridine-2,6-dicarboxylic acid, bipy = 4,4'-bipyridine) has been synthesized by the reaction of 4-hydroxypyridine-2,6-dicarboxylic acid, 4,4'-bipyridine and manganese carbonate under hydrothermal conditions, and its crystal structure was determined by X-ray diffraction method The crystal belongs to the monoclinic system, space group P21/n with a = 10.110(2), b = 20.159(4), c = 17.861(4)A,β = 99.67(3)°, V = 3.5884(12) nm3, Mr= 901.47, Z = 4, Dc= 1.669 g.cm^-3, μ= 0.798 mm^-1, F(000) = 1840, the final R = 0.0713 and ωR = 0.1853. The complex forms a 1-D chain bridged by HCAM, protonated 4,4-bipyridines link the 1-D chains to construct 2-D networks via N-H...O hydrogen bonds, and networks are further extended via π-π stacking and hydrogen bonds into 3-D supramolecular framework.展开更多
A novel layered mixed metal vanadium-cobadt complex, (py)5Co2(H2O)3[V4O12] 1 (py = pyridine), was hydro(solvo)thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in ort...A novel layered mixed metal vanadium-cobadt complex, (py)5Co2(H2O)3[V4O12] 1 (py = pyridine), was hydro(solvo)thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473(4), b = 11.447(2), c = 17.509(4)A^°, V = 5005.3(7)A^°3, Z = 4, Mr = 3502.1(12), Z = 4, Dc = 1.827 g/cm^3,μ(MoKα) = 2.023 mm^-1, F(000) = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ(I) and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co(py)2(H2O)2 and Co(py)3(H2O).展开更多
Two complexes, [Cd(nphth)(2,2'-bipy)(H20)]2.2H20 (1) and [Cd(nphth)(4,4'- bipy)(H20)], (2) (nphth = 3-nitrophthalate, 2,2'-bipy = 2,2'-bipyridine, 4,4'-bipy = 4,4'-bipyridine), were synthesized...Two complexes, [Cd(nphth)(2,2'-bipy)(H20)]2.2H20 (1) and [Cd(nphth)(4,4'- bipy)(H20)], (2) (nphth = 3-nitrophthalate, 2,2'-bipy = 2,2'-bipyridine, 4,4'-bipy = 4,4'-bipyridine), were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in triclinic with space group Pi, a = 0.7599(4), b = 1.0551(6), c = 1.2448(6) nm, α = 88.96(2), β = 75.40(2), γ= 76.76(2)°, V= 0.9393(9) nm3, Z = 1, Dc = 1.816 Mg/m3, F(000) = 512, μ = 1.217 mm-1, S = 0.946, the final R = 0.0238 and wR = 0.0631, Complex 2 crystallizes in monoclinic, space group P21/c, a = 0.737(5), b = 2.338(1), c = 1.0030(6) nm, β = 96:359(9)°, V= 1.803(2) nm3, Z = 4, Dc = 1.826 Mg/m3, F (000) = 984,μ = 1.260 mm-1, S = 1.016, the final R = 0.0455 and wR = 0.1007. Complex 1 exhibits a discrete cyclic binuclear structure and complex 2 possesses a 2D layer structure with cyclic binuclear unit. The fluorescent spectrum study shows that complex 1 exhibits fluorescent emission in the solid state at room temperature.展开更多
A novel metal-organic coordination polymer [Cu2(phen)(ipt)2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic,...A novel metal-organic coordination polymer [Cu2(phen)(ipt)2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 12.338(3), b = 12.167(3), c = 18.167(4)A, β= 111.686(14)°, V = 2534.1(10)A^3, C28H18Cu2N2O9, Mr = 653.52, Dc = 1.713 g/cm^3,μ(MoKα) = 1.740 mm^-1, F(000) = 1320, Z = 4, the final R = 0.0443 and wR = 0.0853 for 3543 observed reflections (1 〉 2σ(I)). It exhibits a novel two-dimensional network with tetra-Cu-ipt-as building units.展开更多
A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis...A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The compound crystallizes in triclinic,space group P1 with a=7.2472(5),b=10.6966(8),c=16.2376(12),α=98.2960(10),β=91.6430(10),γ=97.4810(10)o,V=1233.53(16)3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ(MoKα)=13.697 mm-1,F(000)=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections (I 〉 2σ(I)).In the crystal structure,the Pb(1) atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb(2) atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.展开更多
A metal-organic coordination compound formulated as [Cd(pzdc)(2,2'-bipy)]n·nH2O 1 (Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and structural...A metal-organic coordination compound formulated as [Cd(pzdc)(2,2'-bipy)]n·nH2O 1 (Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081(13), b = 14.4328(17), c = 10.2530(12) A, β = 98.504(2)°, V= 1581.8(3) ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ(MoKa) = 1.420 mm^-1, F(000) = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections (I 〉 2σ(I)). It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.展开更多
A metal-organic coordination compound formulated as [Mn(pzdc)(phen)]n·nH2O 1 (H2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characteriz...A metal-organic coordination compound formulated as [Mn(pzdc)(phen)]n·nH2O 1 (H2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,TG and single-crystal X-ray diffraction.The title compound crystallizes in the monoclinic system,space group P21/n with a= 11.7689(18),b=11.7458(18),c=13.360(2),β=110.341(2)o,V=1731.7(5)3,C18H12MnN4O5,Mr=419.26,Dc=1.608 g/cm3,μ(MoKα)=0.803 mm-1,F(000)=852,Z=4,the final R=0.0323 and wR=0.0823 for 2831 observed reflections (I 〉 2σ(I)).It exhibits an interesting two-dimen-sional network structure.展开更多
A zinc complex, [Zn(iso)_2(H_2O)_4](iso=C_6H_4NO_2^-), was synthesized and characterized by elemental analysis, thermal analysis and IR spectrum studies. The crystal structure of the complex was determined by X-ray di...A zinc complex, [Zn(iso)_2(H_2O)_4](iso=C_6H_4NO_2^-), was synthesized and characterized by elemental analysis, thermal analysis and IR spectrum studies. The crystal structure of the complex was determined by X-ray diffraction. The crystal crystallizes in the triclinic system, molecular formula ZnC12H16N2O8, Mr=381.64, space group P with a = 6.338(1), b =6.919(1), c=9.277(1), α=96.28(1), β=104.91(1), γ=112.85(1)°, V=352.12(9)?3, Z=1, Dc=1.80g?cm-3 and F(000)=196, μ =1.791mm-1. The crystal structure was solved by direct methods for final R=0.0204 and Rw=0.0542 for 1258 observed reflections with [Fo>4σ(Fo)]. The crystal structure reveals that zinc ion is trans-octahedral with two pyridyl nitrogens and two aque oxygens at the equational positions and two aqua oxygens at the axial positions. The complex forms a three-dimensional network through intermolecular hydrogen bonds.展开更多
A novel complex, [Mn(2-NCP)(H2BTC)(H2O)]n(1, 1,3,5-H3BTC = 1,3,5-benzenetricarboxylic acid, 2-HNCP = 2-(2-carboxyphenyl)-1 H-imidazo(4,5-f)-(1,10)phenanthroline), was hydrothermally synthesized and structurally charac...A novel complex, [Mn(2-NCP)(H2BTC)(H2O)]n(1, 1,3,5-H3BTC = 1,3,5-benzenetricarboxylic acid, 2-HNCP = 2-(2-carboxyphenyl)-1 H-imidazo(4,5-f)-(1,10)phenanthroline), was hydrothermally synthesized and structurally characterized by elemental analysis, IR, XRD and single-crystal X-ray diffraction. Structural analyses reveal that complex 1 exhibits a(6, 6)-connected topology network with a Schlafli symbol of(6^3). The adjacent 2D layers are further stacked via strong hydrogen-bonding interactions, giving a 3 D supramolecular framework. In addition, the structure of complex 1 was calculated by the B3LYP/LANL2 DZ method by Gaussian program. The results from natural bond orbital(NBO) analysis shows obvious covalent interaction between the coordinated atoms and Mn(Ⅱ) ion.展开更多
One novel binuclear Co(Ⅱ) coordination polymer ∞ [Co2(4,4'-bpy)2(L)4] (1, bpy = bipyridine, HL = 2-fluorbenzoic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis...One novel binuclear Co(Ⅱ) coordination polymer ∞ [Co2(4,4'-bpy)2(L)4] (1, bpy = bipyridine, HL = 2-fluorbenzoic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.163(2), b = 21.943(4), c = 9.6381(19) A, β = 113.92(3)°, V= 2158.2(7) A3, Z= 4, Dc = 1.518 g/cm^3, Mr = 493.31, F(000) =1004, R = 0.0303 and wR = 0.0808 for 3614 observed reflections (I〉 2σ(I)). Complex I exhibits a 3D Schlafli symbol (4.62)(4.66.83) topological framework, and the magnetic characterization shows weak antiferromagnetic coupling exchange between two Co ions.展开更多
Reaction of Zn(ClO4)2·6H2O with septadentate 2,6-bis[bis(2-benzimidazolylme-thyl)amino methyl]-4-methylphenol (Hbbap) and sodium isonicotinate yielded a dinuclear zinc complex[Zn2(bbap) (Iso) (Hiso)] (ClO4)2·...Reaction of Zn(ClO4)2·6H2O with septadentate 2,6-bis[bis(2-benzimidazolylme-thyl)amino methyl]-4-methylphenol (Hbbap) and sodium isonicotinate yielded a dinuclear zinc complex[Zn2(bbap) (Iso) (Hiso)] (ClO4)2·[Zn2 (bbap) (Iso) (H2O)] (ClO4)2·4H2O(1a·1b·4H2O). Hiso isisonicotinic acid and Iso is isonicotinate anion. The structure has been established by X-raycrystallography and shows that the two zinc ions are bridged by the phenoxy unit of bbap- ligand,and the presence of unusual monodentate O-coordination of carboxylate group from isonicotinicacid. The coordination geometry around the zinc ion is approximately trigonal bipyramidal.展开更多
Reaction of Cu(ClO4)2'6H2O with tripodal ligand tri s (2-benzi nd dazol yl methyl ) aInine(ntb) and sodium isonicotinate (Iso) yielded a mononuclear complex lCu(ntb)(lso)]ClO4.3.5H2O. Thestructure has been establi...Reaction of Cu(ClO4)2'6H2O with tripodal ligand tri s (2-benzi nd dazol yl methyl ) aInine(ntb) and sodium isonicotinate (Iso) yielded a mononuclear complex lCu(ntb)(lso)]ClO4.3.5H2O. Thestructure has been established by X-ray crystallography The Cu (Ⅱ) atom is in a distorted trigonalbipyranddal environment with three benzimindazole N atoms of ntb defining the equatorial plane, oneandne N atom of ntb, and one O atom of the carboxylate group of isonicotinate occupying the axialpositions.展开更多
[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15c...[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .展开更多
基金Supported by the National Natural Science Foundation of China(No.21301069)the Natural Science Foundation of Shandong Province(No.ZR2012BQ004)
文摘A new coordination complex [Cd(pda)(pyz)(H2O)2]n(1, H2 pda = 1,4-phenylenediacetic acid, pyz = pyrazine) have been synthesized and structurally characterized. Crystal data for the title complex are as follows: orthorhombic system, space group Ccmb with a = 11.5245(3) b = 19.5069(5) c = 11.4231(3) A, V = 2568.00(12) A3, Mr = 188.31, Z = 16, F(000) = 1480, Dc = 1.948 g/cm3, μ(Mo Kα) = 1.725 mm-1, R = 0.0195 and w R = 0.0462 for 1357 observed reflections with I 】 2σ(I). In the title complex, the central Cd(II) ion is located in a distorted octahedral coordination environment. Two Cd(II) ions are bridged by two pda2- ligands and one pyz ligand to form a bi-loop structure. Luminescent property of the complex has also been studied.
基金supported by the Natural Science Foundation of Hebei Province(B2009000969)
文摘A three-dimensional coordination polymer {[Cd2(HCAM)2(H2O)4].3.SH2O}n was synthesized by the hydrothermal reaction of H3CAM (H3CAM = 4-hydroxypyridine-2,6-dicerboxylic acid) and Cd(NO3)2·4H2O. The structure was characterized by elemental analysis, thermal gravimetric analysis, infrared spectroscopy and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.4389(19), b = 11.009(2), c = 11.192(2) A, α = 87.87(3), β= 74.63(3), γ = 81.22(3)°, V= 1108.2(4) A3, Z = 2, Dc= 2.164 g/cm3,μ = 2.011 mm^-1, F(000) = 710, R = 0.0419 and wR = 0.1170. X-ray analysis reveals that the title compound adopts a one-dimensional staircase structure by carboxyl of H3CAM and water molecules, and it is further linked by hydrogen bonds to form a 3-D metal-organic open framework. The thermal gravimetric analysis displays that the framework exists stably below 300 ℃.
基金Siping Sci-tech Development Planning Project(No.2005012)
文摘The structure of a binuclear cadmium(Ⅱ) quaternary complex, [Cd2(phen)2- Q2(BP)]n 1 (phen = 1,10-phenanthroline, BP = biphenyl-4,4′-dicarboxylic acid, Q = 8-hydroxy- quinoline-anion), has been determined by X-ray crystallography and characterized by elemental analysis, IR spectrum and thermogravimetric analysis. It crystallizes in the monoclinic system, space group P21/n with a = 13.1906(18), b = 10.9623(15), c = 16.947(2)A, β = 111.3430(10)°, V = 2282.5(5)A^3, Z = 4, Mr = 556.85, Dc = 1.620 g/cm^3, F(000) = 1116,μ= 0.994 mm^-1 and S = 1.056. In the structure, 1D chains are connected via biphenyl-4,4′-dicarboxylic acid, 8-hydroxy quinoline anion and binuclear cadmium atoms into an infinite 1-D molecular chain architecture. Via aryl ring π-π stacking interactions a supramolecular structure is formed in 1.
基金Supported by the Natural Science Foundation of Anhui Province (090416239)the Science and Technology Play (?) Projects of Anhui Province (09020203071)+2 种基金the National Natural Science Foundation of China (20871089)the Foundation of Anhui Provincial Education Department for Outstanding Young Talents in University (2009SQRZ172)the Scientific Research Foundation for the Professors (Doctors) of Suzhou University (2010jb01)
文摘Two new transition metal compounds, [Mn(dpa)2(tmd)2]n (1, H2dpa = 4-hydroxy-phenyl-acetic acid, tmd = 4,4-trimethylenedipyridine) and [Co4(dpa)6(tmd)4(H2O)4]n·nH2O·nCl2 (2), have been synthesized by hydrothermal synthesis. Compound 1 crystallizes in the monoclinic system, space group P21/n with a = 9.828(3), b = 17.493(5), c = 11.616(4), β = 110.146(6)o, V = 1874.9(10)3, C42H42MnN4O6, Mr = 753.74, Z = 2, Dc = 1.335 g/cm3, μ = 0.406 mm-1, F(000) = 790, the final R = 0.1047 and wR = 0.2021 for 2698 observed reflections (I 〉 2σ(I)). Compound 2 crystallizes in the monoclinic system, space group P21/c with a = 11.7214(13), b = 17.1582(19), c = 24.625(3), β = 103.055(3)o, V = 4824.4(9)3, C100H104Cl2Co4N8O23, Mr = 2094.55, Z = 2, Dc = 1.443 g/cm3, μ = 0.809 mm-1, F(000) = 2180, the final R = 0.0550 and wR = 0.0673 for 4104 observed reflections (I 〉 2σ(I)). These complexes were characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. The structural analyses show that the two compounds are both one-dimensional chain structures. However, compounds 1 and 2 form threedimensional supramolecular structures by hydrogen bonds, respectively.
基金supported by the National Natural Science Foundation of China(20971122)
文摘Three Cd(II) coordination complexes,{[Cd(bime)3](NO3)2·(H2O)3}n(1),[Cd(bime)Br2]n(2) and [(H2bime)(CdBr4)(H2O)]n(3)(bime = 1,2-bis(imidazol-1-yl)ethane),have been prepared and characterized.Single-crystal X-ray diffraction analysis reveals that 1~3 crystallize in the trigonal space group P-3,monoclinic space group C2/c and triclinic space group P1,respectively.In 1,bime bridges six-coordinated Cd(II) to generate a two-fold interpenetrating 3D coordination polymer,in which NO3- is not involved in coordination,but serves as a void filler to balance the charge of the 3D framework.The six NO3- and six uncoordinated water molecules form an unprecedented 24-membered macrocycle through hydrogen bonding interaction.In 2,bime in an anti-conformation links the CdBr2 units into a zigzag chain.In 3,bime does not take part in coordination,but is protonated to act as a counter cation of [CdBr4 ]2-.The hydrogen bonds between H2bime and [CdBr4]2- result in the formation of a supramolecular chain.
基金Supported by the National Natural Science Foundation of China (Nos. 20971065,20771005)National Basic Research Program of China (2007CB925103)+1 种基金the Young Teachers Program of College in Anhui Province (2008jql138)the Natural Science Foundation of Anhui Province (090416239)
文摘Three complexes obtained by the reaction of Pr(Ⅲ) or Nd(Ⅲ) salts with 5-methyl-2-pyrazinecarboxylic acid(Hmpca) are structurally determined by single-crystal X-ray diffraction.Complex [Pr(mpca-)3(H2O)2]2·6H2O(1) is composed of dinuclear Pr(Ⅲ) units with two metal centers bridged by two anionic mpca-ligands in a κ^3O,O':O' bridging mode.Complexes [Pr(mpca-)3]n(2) and [Nd(mpca-)3]n(3) are isostructures,and they consist of polymeric chains based on Ln(Ⅲ) and mpca-ligands.Each pair of adjacent metal centers is linked by three mpca-molecules in a κ^3N,O:O bridging mode.
基金Supported by the National Natural Science Foundation of China (No.20671064)Doctor Foundation of Liaoning Province (No.20071016)
文摘The 1-D chain coordination complex of {[Mn2(HCAM)3(H2bipy)]·5H2O}n (H3CAM = 4-hydroxypyridine-2,6-dicarboxylic acid, bipy = 4,4'-bipyridine) has been synthesized by the reaction of 4-hydroxypyridine-2,6-dicarboxylic acid, 4,4'-bipyridine and manganese carbonate under hydrothermal conditions, and its crystal structure was determined by X-ray diffraction method The crystal belongs to the monoclinic system, space group P21/n with a = 10.110(2), b = 20.159(4), c = 17.861(4)A,β = 99.67(3)°, V = 3.5884(12) nm3, Mr= 901.47, Z = 4, Dc= 1.669 g.cm^-3, μ= 0.798 mm^-1, F(000) = 1840, the final R = 0.0713 and ωR = 0.1853. The complex forms a 1-D chain bridged by HCAM, protonated 4,4-bipyridines link the 1-D chains to construct 2-D networks via N-H...O hydrogen bonds, and networks are further extended via π-π stacking and hydrogen bonds into 3-D supramolecular framework.
基金supported by the Science and Technological Fund of Anhui Province for Outstanding Youth and the Program for New Century Excellent Talents in University (06046100 and NCET-06-0556)
文摘A novel layered mixed metal vanadium-cobadt complex, (py)5Co2(H2O)3[V4O12] 1 (py = pyridine), was hydro(solvo)thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pca21 with a = 17.473(4), b = 11.447(2), c = 17.509(4)A^°, V = 5005.3(7)A^°3, Z = 4, Mr = 3502.1(12), Z = 4, Dc = 1.827 g/cm^3,μ(MoKα) = 2.023 mm^-1, F(000) = 1928, S = 1.020, the final R = 0.0400 and wR= 0.1063 for 6035 observed reflections with I 〉 2σ(I) and 460 variables. Complex 1 consists of tetrahedral VO4 groups to form the large layers which are alternately bonded by two cobalt complex species Co(py)2(H2O)2 and Co(py)3(H2O).
基金supported by the National Natural Science Foundation of China(21371088)the Education Department of Fujian Province(No.JK2012048,JA12310,JB12207)
文摘Two complexes, [Cd(nphth)(2,2'-bipy)(H20)]2.2H20 (1) and [Cd(nphth)(4,4'- bipy)(H20)], (2) (nphth = 3-nitrophthalate, 2,2'-bipy = 2,2'-bipyridine, 4,4'-bipy = 4,4'-bipyridine), were synthesized by hydrothermal reactions and structurally characterized. Complex 1 crystallizes in triclinic with space group Pi, a = 0.7599(4), b = 1.0551(6), c = 1.2448(6) nm, α = 88.96(2), β = 75.40(2), γ= 76.76(2)°, V= 0.9393(9) nm3, Z = 1, Dc = 1.816 Mg/m3, F(000) = 512, μ = 1.217 mm-1, S = 0.946, the final R = 0.0238 and wR = 0.0631, Complex 2 crystallizes in monoclinic, space group P21/c, a = 0.737(5), b = 2.338(1), c = 1.0030(6) nm, β = 96:359(9)°, V= 1.803(2) nm3, Z = 4, Dc = 1.826 Mg/m3, F (000) = 984,μ = 1.260 mm-1, S = 1.016, the final R = 0.0455 and wR = 0.1007. Complex 1 exhibits a discrete cyclic binuclear structure and complex 2 possesses a 2D layer structure with cyclic binuclear unit. The fluorescent spectrum study shows that complex 1 exhibits fluorescent emission in the solid state at room temperature.
文摘A novel metal-organic coordination polymer [Cu2(phen)(ipt)2]2n-nH2O 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/c with a = 12.338(3), b = 12.167(3), c = 18.167(4)A, β= 111.686(14)°, V = 2534.1(10)A^3, C28H18Cu2N2O9, Mr = 653.52, Dc = 1.713 g/cm^3,μ(MoKα) = 1.740 mm^-1, F(000) = 1320, Z = 4, the final R = 0.0443 and wR = 0.0853 for 3543 observed reflections (1 〉 2σ(I)). It exhibits a novel two-dimensional network with tetra-Cu-ipt-as building units.
基金Supported by the Science and Technology Research Projects of the Education Office of Jilin Province (No. 2007. 213)
文摘A new metal-organic complex [Pb2(PDB)2(phen)]n·nH2O (H2PDB=pyridine-3,4-dicarboxylic acid,phen=1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR spectrum,TG and single-crystal X-ray diffraction.The compound crystallizes in triclinic,space group P1 with a=7.2472(5),b=10.6966(8),c=16.2376(12),α=98.2960(10),β=91.6430(10),γ=97.4810(10)o,V=1233.53(16)3,C26H16O9N4Pb2,Mr=942.81,Dc=2.538 g/cm3,μ(MoKα)=13.697 mm-1,F(000)=872,Z=2,the final R=0.0247 and wR=0.0654 for 3886 observed reflections (I 〉 2σ(I)).In the crystal structure,the Pb(1) atom is six-coordinated with four carboxylate oxygen atoms from three different PDB ligands and two nitrogen atoms from phen ligand,showing a distorted octahedral geometry;the Pb(2) atom is four-coordinated with four carboxylate oxygen atoms from four different PDB ligands,showing a distorted tetrahedral geometry.It exhibits a three-dimensional supramolecular network structure formed by hydrogen bonds and π-π interactions.
基金supported by science and technology research projects of the Education Office of Jilin Provinc (No 2007 213)
文摘A metal-organic coordination compound formulated as [Cd(pzdc)(2,2'-bipy)]n·nH2O 1 (Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081(13), b = 14.4328(17), c = 10.2530(12) A, β = 98.504(2)°, V= 1581.8(3) ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ(MoKa) = 1.420 mm^-1, F(000) = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections (I 〉 2σ(I)). It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.
基金supported by the Science and Technology Research Projects of the Education Office of Jilin Province (No. 2007. 213)
文摘A metal-organic coordination compound formulated as [Mn(pzdc)(phen)]n·nH2O 1 (H2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,TG and single-crystal X-ray diffraction.The title compound crystallizes in the monoclinic system,space group P21/n with a= 11.7689(18),b=11.7458(18),c=13.360(2),β=110.341(2)o,V=1731.7(5)3,C18H12MnN4O5,Mr=419.26,Dc=1.608 g/cm3,μ(MoKα)=0.803 mm-1,F(000)=852,Z=4,the final R=0.0323 and wR=0.0823 for 2831 observed reflections (I 〉 2σ(I)).It exhibits an interesting two-dimen-sional network structure.
文摘A zinc complex, [Zn(iso)_2(H_2O)_4](iso=C_6H_4NO_2^-), was synthesized and characterized by elemental analysis, thermal analysis and IR spectrum studies. The crystal structure of the complex was determined by X-ray diffraction. The crystal crystallizes in the triclinic system, molecular formula ZnC12H16N2O8, Mr=381.64, space group P with a = 6.338(1), b =6.919(1), c=9.277(1), α=96.28(1), β=104.91(1), γ=112.85(1)°, V=352.12(9)?3, Z=1, Dc=1.80g?cm-3 and F(000)=196, μ =1.791mm-1. The crystal structure was solved by direct methods for final R=0.0204 and Rw=0.0542 for 1258 observed reflections with [Fo>4σ(Fo)]. The crystal structure reveals that zinc ion is trans-octahedral with two pyridyl nitrogens and two aque oxygens at the equational positions and two aqua oxygens at the axial positions. The complex forms a three-dimensional network through intermolecular hydrogen bonds.
基金supported by the National Natural Science Foundation of China(No.21576112)the Project of Department of Science&Technology of Jilin Province(No.20180623042TC)+3 种基金Natural Science Foundation Project of Jilin Province(No.20170520143JH)the China Postdoctoral Science Foundation(No.2017M611732)the Science and Technology Research Projects of the Education Department of Jilin Province(No.JJKH20180791KJ)the Science and Technology Development Plan of Siping City(2017056)
文摘A novel complex, [Mn(2-NCP)(H2BTC)(H2O)]n(1, 1,3,5-H3BTC = 1,3,5-benzenetricarboxylic acid, 2-HNCP = 2-(2-carboxyphenyl)-1 H-imidazo(4,5-f)-(1,10)phenanthroline), was hydrothermally synthesized and structurally characterized by elemental analysis, IR, XRD and single-crystal X-ray diffraction. Structural analyses reveal that complex 1 exhibits a(6, 6)-connected topology network with a Schlafli symbol of(6^3). The adjacent 2D layers are further stacked via strong hydrogen-bonding interactions, giving a 3 D supramolecular framework. In addition, the structure of complex 1 was calculated by the B3LYP/LANL2 DZ method by Gaussian program. The results from natural bond orbital(NBO) analysis shows obvious covalent interaction between the coordinated atoms and Mn(Ⅱ) ion.
基金supported by the National Natural Science Foundation of China(51343003)the Scientific Research Projects of Zhejiang Provincial Education Department(Y201224707)
文摘One novel binuclear Co(Ⅱ) coordination polymer ∞ [Co2(4,4'-bpy)2(L)4] (1, bpy = bipyridine, HL = 2-fluorbenzoic acid) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.163(2), b = 21.943(4), c = 9.6381(19) A, β = 113.92(3)°, V= 2158.2(7) A3, Z= 4, Dc = 1.518 g/cm^3, Mr = 493.31, F(000) =1004, R = 0.0303 and wR = 0.0808 for 3614 observed reflections (I〉 2σ(I)). Complex I exhibits a 3D Schlafli symbol (4.62)(4.66.83) topological framework, and the magnetic characterization shows weak antiferromagnetic coupling exchange between two Co ions.
文摘Reaction of Zn(ClO4)2·6H2O with septadentate 2,6-bis[bis(2-benzimidazolylme-thyl)amino methyl]-4-methylphenol (Hbbap) and sodium isonicotinate yielded a dinuclear zinc complex[Zn2(bbap) (Iso) (Hiso)] (ClO4)2·[Zn2 (bbap) (Iso) (H2O)] (ClO4)2·4H2O(1a·1b·4H2O). Hiso isisonicotinic acid and Iso is isonicotinate anion. The structure has been established by X-raycrystallography and shows that the two zinc ions are bridged by the phenoxy unit of bbap- ligand,and the presence of unusual monodentate O-coordination of carboxylate group from isonicotinicacid. The coordination geometry around the zinc ion is approximately trigonal bipyramidal.
文摘Reaction of Cu(ClO4)2'6H2O with tripodal ligand tri s (2-benzi nd dazol yl methyl ) aInine(ntb) and sodium isonicotinate (Iso) yielded a mononuclear complex lCu(ntb)(lso)]ClO4.3.5H2O. Thestructure has been established by X-ray crystallography The Cu (Ⅱ) atom is in a distorted trigonalbipyranddal environment with three benzimindazole N atoms of ntb defining the equatorial plane, oneandne N atom of ntb, and one O atom of the carboxylate group of isonicotinate occupying the axialpositions.
基金Project supported by the National Natural Science Foundation of China
文摘[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .