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1.
A new cadmium polymer [Cd(NBA)(μ3-OH)(4,4'-bipy)1/2]n 1 (NBA=m-nitrobenzoic acid and 4,4'-bipy=4,4-bipyridine) has been synthesized by hydrothermal reaction. Its structure was determined by single-crystal X-ray diffraction method, and characterized by elemental analysis and IR spectrum. The crystal is of monoclinic, space group C2/c, with a=15.6912(9), b=25.9394(15), c=6.7332(4)(A), β=114.7700(10)°, V=2488.4(3)(A)3, C12H9CdN2O5, Mr=373.61, Z=8, Dc=1.995 g/cm3,μ=1.776 mm-1, F(000)=1464, R=0.0411 and wR=0.1128 for 2130 observed reflections (I > 2σ(I)).X-ray diffraction studies reveal that the compound features a layered structure, in which 4,4'-bipy ligands bridge Z type of double chains [Cd(μ3-OH)]n and NBA ligands locate at the two sides of the layer. The π-π interactions between the benzene rings of NBA ligands of two adjacent layers lead to the 3D framework.  相似文献   

2.
A new cadmium polymer [Cd(NBA)(μ3-OH)(4,4′-bipy)1/2]n 1 (NBA = m-nitrobenzoic acid and 4,4′-bipy = 4,4-bipyridine) has been synthesized by hydrothermal reaction. Its structure was determined by single-crystal X-ray diffraction method, and characterized by elemental analysis and IR spectrum. The crystal is of monoclinic, space group C2/c, with a = 15.6912(9), b = 25.9394(15), c = 6.7332(4) ′, β = 114.7700(10)°, V = 2488.4(3) 3, C12H9CdN2O5, Mr = 373.61, Z = 8, Dc = 1.995 g/cm3, μ = 1.776 mm-1, F(000) = 1464, R = 0.0411 and wR = 0.1128 for 2130 observed reflections (I > 2σ(I)). X-ray diffraction studies reveal that the compound features a layered structure, in which 4,4′-bipy ligands bridge Z type of double chains [Cd(μ3-OH)]n and NBA ligands locate at the two sides of the layer. The π-π interactions between the benzene rings of NBA ligands of two adjacent layers lead to the 3D framework.  相似文献   

3.
徐涵  李一志 《结构化学》2010,(11):1606-1611
A novel NiII complex [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n 1 (H2IBG = isophthaloylbisglycine and 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. It crystallizes in monoclinic, space group P2/c with a = 15.5420(7), b = 22.4344(1), c = 8.3455(5), β = 101.538(3)o, V = 2670.1(7)3, Z = 4, C22H32N4NiO13, Mr = 619.23, Dc = 1.443 g/cm3, F(000) = 1296.0, μ(MoKα) = 0.750 mm-1, the final R = 0.0570 and wR = 0.1445 for 2296 observed reflections with I 2σ(I). In the structure, the NiII metal center is coordinated in an octahedral environment arranged by two water molecules, two carboxylate oxygen atoms and two nitrogen atoms from two 4,4'-bipy ligands. Thermal decomposition and powder X-ray diffraction results indicate that the transformation from the crystal form, [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n, to the amorphous powder, Ni(IBG)(4,4'-bipy)(H2O)2, is reversible, so the latter form may be utilized as an absorbing agent for water and water vapor.  相似文献   

4.
The title compound, {CdI2(2,2'-bipy)}n, was prepared by the hydrothermal reaction of CdI2 and 2,2'-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) (A), β = 106.0629(4)°, V = 1271.00(14)(A)3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc= 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I>2σ(Ⅰ)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2'-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.  相似文献   

5.
A new metal-organic coordination polymer [Co(2-pya)2(4,4'-bipy)]2n·[(4,4'- bipy)0.5· H2O]2n(2-pya = 2-pyridinecarboxylic acid, 4,4'-bipy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.719(2), c = 10.710(2) A, V = 5527.8(14) A3, C54H46N10Co2O10, Mr = 1112.87, Dc = 1.337 g/cm3,μ(MoKα) = 0.665 mm-1, F(000) = 2296, Z = 4, the final R = 0.0633 and wR = 0.1096 for 1261 observed reflections (I > 2σ(I)). It exhibits a one-dimensional chain-like structure constructed by mixed ligands of 2-pyridinedicarboxylic acid and 4,4'-bipyridine.  相似文献   

6.
A new Zn(II) coordination polymer [Zn3(BTC)2(4,4'-bpy)(CO)2]n(1, H3 BTC =1,3,5-benzenetricarboxylic acid, 4,4'-bpy = 4,4'-bipyridine) has been prepared through urothermal reaction of zinc nitrate hexahydrate with 1,3,5-benzenetricarboxylic acid and 4,4'-bipyridine, and characterized by elemental analysis, IR spectroscopy, TGA and powder XRD, and its crystal structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in the monoclinic system, space group C2/c, with a = 10.262(3), b = 18.838(5), c =15.083(4) A, β = 99.203(4)o, V = 2878.3(14) A3, C30H14Zn3N2O14, Mr = 822.54, Z = 4, Dc = 1.898g/cm3, μ = 2.561 mm-1, F(000) = 1640, R = 0.0363 and w R = 0.0932 for 2828 observed reflections(I 2σ(I)). X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn(II) atoms which are connected by BTC3- ligands and 4,4'-bpy coligands to form a 3D framework with 1D channels. The solid luminescence of ligand and the title complex was also studied at room temperature.  相似文献   

7.
A novel MnⅡ complex [{Mn(IBG)(2,2'-bipy)(H2O)}·4H2O]n 1(H2IBG=isophtha-loylbisglycine and 2,2'-bipy = 2,2'-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction,elemental analysis,IR spectra and thermogravimetric analysis.It crystallizes in monoclinic,space group P21/n,with a=13.667(2),b=14.045(2),c=14.195(2),β=101.483(3)°,V=2670.1(7)3,Z=4,C22H26N4O11Mn,Mr=577.41,Dc=1.436 g/cm3,F(000)=1196.0,μ(MoKα)=0.558 mm-1,the final R=0.0578 and wR=0.1460 for 2974 observed reflections with I2σ(I).In the structure,the MnⅡ atom is coordinated in a distorted octahedral environment arranged by one water molecule,one 2,2'-bipy ligand and two IBG ligands.  相似文献   

8.
A new two-dimensional Cd(Ⅱ) coordination polymer, [Cd(2,5-pdch)(H2O)]n·2n(ClO4)·nH2O (2,5-pdch = pyridine-2,5-dicarbohydrazide), was prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 10.905(2), b = 11.602(1), c = 15.034(2) A, β = 117.794 (10°, V = 1682.8(4A3, Z = 4, C7H13CdCl2NsO12, Mr = 542.52, Dc = 2.141 g/cm^3,/μ = 1.691 mm^-1, F(000) = 1072, 2(MoKa) = 0.71073A, the final R = 0.0608 and wR = 0.1329 for 2972 observed reflections with I 〉 2σ(I). Single-crystal X-ray diffraction analysis reveals that the Cd(Ⅱ) atom displays a distorted pentagonal-bipyramidal geometry coordinated by three N atoms and three O atoms from three different 2,5-pdch ligands, and one water molecule. Interestingly, each two Cd(Ⅱ) atoms are bridged by two carbohydrazide groups of the 2,5-pdch ligands to form a dimeric unit, and such dimeric units are further connected by the 2,5-pdch ligand to generate a two-dimensional (4,4)-network.  相似文献   

9.
Two novel silver(I) complexes {[Ag(OTf)(PPh3)(4,4'-bipy)]}∞(1) and {[Ag2-(OTf)2(dppb)3](CH3CN)4}∞(2)(OTf = trifluoromethanesulfonate, PPh3 = triphenylphophine, 4,4'-bipy = 4,4'-bipyridine, dppb = bis(diphenylphosphino)butane) have been synthesized and characterized by IR, single-crystal X-ray diffraction, fluorescence spectrum and 1H NMR spectroscopy. Complex 1 crystallizes in orthorhombic, space group Pna21 with a = 19.259(2), b = 9.85070(12), c = 16.3827(17) ?, V = 3108.0(5) ?3, C29H23F3N2O3 PSAg, Mr = 675.39, Z = 4, Dc = 1.443 g/cm3, F(000) = 1360, μ = 0.816 mm-1, the final R = 0.0675 and w R = 0.1722 for 3662 observed reflections(I 2σ(I)). Complex 2 crystallizes in triclinic, space group P1 with a = 12.9370(11), b = 13.5261(13), c = 16.4539(15) ?, α = 106.7120(10), β = 97.3830(10), γ = 113.027(2)?, V = 2441.2(4)?3, C94H96F6N4O6P6S2Ag2, Mr = 1957.43, Z = 1, Dc = 1.331 g/cm3, F(000) = 1006, μ = 0.605 mm-1, the final R = 0.0717 and w R = 0.1795 for 5128 observed reflections(I 2σ(I)). Complex 1 is of zigzag chain structure, in which each Ag atom is coordinated by one OTf- anion, two N atoms from two 4,4'-bipy molecules and one P atom from PPh3 ligand. In 2, the central Ag atom is coordinated with one OTf- anion and three P atoms from three dppb ligands, which leads to the formation of a zigzag ring-bridge-ring chain with each ring consisting of two Ag atoms and two dppb ligands.  相似文献   

10.
The title compound,a mixed(phthalocyaninato)(porphyrinato) yttrium double-decker complex 1,has been synthesized and structurally characterized by X-ray single-crystal diffraction method.Crystal data:monoclinic,space group C2/c,Z = 8,C79H52Cl10N12O4Y,Mr = 1676.74,a = 38.217(3),b = 18.9867(13),c = 26.200(3) ,β = 128.0190(10)°,V = 14977(2) 3,Dc = 1.487 g/cm3,μ(MoKα) = 1.196 mm-1,F(000) = 6808,R = 0.0745 and wR = 0.2208 for observed reflections with I > 2σ(I).X-ray analysis reveals that the coordination polyhedron adopts a slightly distorted square-antiprismatic structure around the metal center.Both phthalocyanine and porphyrin ligands are saucer-shaped,with the skew angle of the two ligand planes approximately 45°.  相似文献   

11.
A novel polyoxometalate {[AgI(4,4'-bipy)]3[PW12O40]}·(4,4'-bipy)·4H2O 1 has been synthesized hydrothermally and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of 1 belongs to the triclinic system, space group P1 with a = 11.3710(17), b = 12.0701(16), c = 13.1061(12) , α = 112.838(3), β = 94.545(6), γ = 99.526(4)°, V = 1614.4(4) 3, Mr = 3825.40, Z = 1, Dc = 3.935, μ = 22.289mm-1, F(000) = 1692, the final R = 0.0507 and wR = 0.1054. X-ray diffraction analysis reveals that the molecular structure of 1 consists of three coordinated cations [AgI(4,4'-bipy)]+, a polyanion unit [PW12O40]3-, and a discrete 4,4′-bipy molecule. Significantly, there exist two crystallographically independent silver(I) centers in 1 and all [AgI(4,4'-bipy)]+ cations are linked with each other to form a one-dimensional Ag-4,4'-bipy polymer chain. The neighboring polymer chains are further interconnected to form a 3D framework by the covalent effect of silver atoms and terminal oxygen atoms of the polyanion. The electrochemical behaviors of 1 have also been studied in detail by cyclic voltammograms.  相似文献   

12.
A novel coordination polymer [Mg(L)(H2O)2]·H2O] (LH2=L-cysteic acid) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction.The crystal crystallizes in orthorhombic system, space group P212121, with a=5.962(3), b=11.224(6), c=13.664(7)(A), V=914.3(8) (A)3, Z=4, Mr=245.50, Dc=1.783 g/cm3,μ=0.445 mm-1,flack parameter=0.32(16), F(000)=512, the final R=0.0458 and wR=0.1172 for 1578 observed reflections with I > 2σ(Ⅰ). The Mg(Ⅱ) atom shows an octahedral geometry defined by two carboxyl O atoms from two different L-cysteic acid ligands, one carboxyl O atom and one amino N atom from the adjacent ligand, and two aqua ligands. The Mg(Ⅱ) atoms are bridged by L-cysteic acid ligands, leading to a 1D infinite zigzag chain. In the structure there are extensive hydrogen bonds,through which the complex completes its 3D framework structure.  相似文献   

13.
崔广华  彭献  董桂英  李峰峰 《结构化学》2009,28(10):1265-1269
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.  相似文献   

14.
A new metal-organic coordination polymer [Cd(5-hip)(phen)]n·nH2O 1 has been hydro- ermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The crystal of the complex crystallizes in monoclinic, space group P2/n with a = 8.8071(17), b =12.386(2), c = 16.981(3) A, β = 100.182(2)°, V = 1823.2(6) A^3, Mr=. 490.73, Dc =1.788 g/cm^3,μ(MoKa) = 1.240 mm^-1, F(000) = 976, Z= 4, the final R = 0.0458 and wR = 0.1373 for 2864 observed reflections (I 〉 2σ(I)). The Cd atoms are coordinated by two N atoms from the phen ligands and four O atoms from 5-hydroxyisophthalate ligands in a highly distorted octahedral geometry.  相似文献   

15.
《结构化学》2009,28(11)
Two new cobalt(Ⅱ) supramolecular complexes [Co(4,4'-bipy)_2(H_2O) _4]·[Co_2(4,4'-bipy)3-(H_2O) _8]·2TST-2(4,4'-bipy)·4H_2O 1 and [Co(4,4'-bipy) _2(H_2O) _4]DSNT·4,4'-bipy 2 based upon the assembly of Co(Ⅱ), 4,4'-bipyridine (4,4'-bipy) and two new multifunctional organic ligands, 2,4,6-tris(4-sulfophenyl-amino)-1,3,5-triazine (H_3TST) and 2,4-bis(p-sulfanilato)-6-diethylamino-1,3,5-triazine (H_2DSNT), have been prepared by hydrothermal method and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structure of 1 is of monoclinic, space group P2_(1/n) with α= 13.599(4), b = 18.988(6), c = 22.995(7) A, β = 90.273(6)°, V= 5938(3) A~3, Z = 4, C_(56)H_(59)CO_(1.5)N_(13)O_(17)S_3, M_r = 1370.74, D_c = 1.533 g/cm~3,μ = 0.613 mm~(-1), F(000) = 2842, GOOF = 1.018, the final R = 0.0796 and wR = 0.1498 for 9019 observed reflections with I > 2o(I). The crystal structure of 2 belongs to the monoclinic system, space group C2/c with α = 18.864(6), b = 14.283(5), c = 20.246(7) A, β = 107.799(6)°, V = 5194(3) A~3, Z = 4, C_(49)H_(52)CoN_(12)O_(10)S_2, M_r = 1092.08, D_c = 1.397 g/cm~3, μ= 0.480 mm~(-1), F(000) = 2276, GOOF = 1.059, the final R = 0.0665 and wR = 0.1900 for 4887 observed reflections with I> 2σ(I). The results of X-ray crystal structure analysis revealed that complexes 1 and 2 exhibit layered supramolecular frameworks stabilized by electrostatic interactions, π-π interactions and hydrogen bonds.  相似文献   

16.
A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I >2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).  相似文献   

17.
WANG Jing  SU  Ting-Ting 《结构化学》2011,30(3):438-442
The hydrothermal reaction of Cd(OAc)2·2H2O, 4,4'-bpy and cyclohexane-1,2,4,5-tetracarboxylic acid (H4L) yields a three-dimensional (3D) coordination porous framework [Cd2LI(4,4'-bpy)1.5(H2O)2]n·2nH2O, which was characterized by single-crystal X-ray diffraction (MoKα radiation, λ = 0.71073), elemental analysis and IR. This complex crystallizes in the monoclinic system, space group C2/c with a = 25.951(3), b = 11.6618(12), c = 20.046(2) , β = 114.863(2)o, V = 5504.4(10) 3, Z = 8, Dc = 1.900 g/cm3, Mr = 787.30, μ = 1.615 mm-1, F(000) = 3128, the final R = 0.0978 and wR = 0.1780. The structure of the complex is a 3D coordination Cd-carboxylate framework consisting of 1D hexagonal channels along the c-axis filled with the bridging 4,4'-bpy ligands. The 4,4'-bpy ligands with two kinds of conformations are located alternately in the channels through coordination and hydrogen interactions to support the whole porous framework, in which the conformation-flexible cyclohexane-1,2,4,5-tetracarboxylate ligand adopts the I (e,a,a,e) conformation and acts as a pentadentate ligand to connect five Cd(Ⅱ) atoms via the carboxylate groups in different coordination modes.  相似文献   

18.
The reaction of Cd(NO_3)_2·4H_2O with 4,4?-dipyridylacetylene(4,4?-DPA) and 2-nitroterephthalic acid(2-NO_2-H_2BDC) in DMF/H_2O mixed solvent has afforded a compound {[Cd(2-NO_2-BDC)(4,4?-DPA)]·(DMF)}_n(1). Compound 1 has been characterized by single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetry analysis, and IR spectrum. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 12.1488(3), b = 14.6689(3), c = 13.1615(3) ?, β = 111.809(3)o, V = 2177.63(9) ?~3, Z = 4, C_(23)H_(18)N_4O_7 Cd, M_r = 574.81, D_c = 1.753 g/cm~3, μ = 8.523 mm~(-1), F(000) = 1152, the final R = 0.0411 and wR = 0.1064 for 3589 observed reflections with I 2s(I). In compound 1, the Cd(Ⅱ) ions are linked by the carboxylate groups of 2-NO_2-BDC ligands to give a two-dimensional layered structure based on the centrosymmetric dinuclear Cd_2(COO)_2 units, which are further connected by the 4,4?-DPA ligands to produce a three-dimensional framework with pcu topology. Careful examination revealed that compound 1 is a 2-fold interpenetrating framework. Furthermore, the gas adsorption properties of 1 for N_2 and CO_2 have also been investigated.  相似文献   

19.
By the reactions of manganese(II) acetate, 2-sulfoethylphosphonic acid, 1,10-phen (1,10-phen = 1, 10-phenanthroline) or cobalt(II) acetate, 4,4'-bipy and 2-carboxyethylphosphonic acid, two novel compounds of [Mn(H2O)2(C12H8N2)(HO3PCH2CH2CO2)] (1) and[Co(H2O)4 (C10H8N2)]· (HO3PCH2CH2CO2) (2) have been synthesized and characterized by IR spectroscopy, elemental analyses and single-crystal X-ray diffraction. Compound 1 has a 0D structure. Two Mn(II) ions are linked by two 2-carboxyethylphosphonic acid ligands, forming a centrosymmetric dimer. These dimers are further interlinked into a 2D layer structure by π-π stacking interactions and hydrogen bonds. Compound 2 has a 1D chain structure. The 2-carbo- xyethylphosphonic acid remains uncoor- dinated and acts as the organic template. By the bridge of 4,4'-bipy, the [Co(4,4'-bipy)]2+ chains are formed.  相似文献   

20.
The title compound, a novel Ag(Ⅰ) carboxyarylphosphonate [Ag(H2BCP)(4,4'- bipy)]·2H2O (H3BCP = p-H2O3PCH2C6H4COOH, 4,4'-bipy = 4,4'-bipyridine), was synthesized by a hydrothermal reaction and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. It belongs to monoclinic system, space group P21/c with a = 5.7038(11), b = 22.397(4), c = 5.602(4) ?, β = 106.26(3)°, V = 1913.4(7) 3, Z = 4, C18H20N2O7PAg, Mr = 515.20, Dc = 1.788 g/cm3, μ = 1.182 mm-1, F(000) = 1040, the final R = 0.0404 and wR = 0.1216 for 4178 observed reflections with I 2σ(Ⅰ). In the structure, the Ag(Ⅰ) cations are bridged by 4,4'-bipy to give rise to 1D chains running along the b axis. These chains are linked further by the interactions of O (from BCP ligands) and Ag atoms to yield 2D layers. Hydrogen bonding interactions and weak π-π stacking interactions between 4,4'-bipy rings assemble such adjacent layers to generate a 3D supramolecular architecture.  相似文献   

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