A New Sandwich Type Transition Metal Substituted Polyoxotungstate under Hydrothermal Conditions:[NH3(CH2)4NH3]6[Co4(HzO)2(B-α-GeW9034)2]}·7H2O

A new sandwich transition metal substituted polyoxotungstate,[NH3(CH2)4NH3]6 [Co4(H2O)2(B-α-GeW9O34)2]·7H2O 1,was hydrothermally synthesized and characterized by IR spectra and single-crystal X-ray diffraction.The single-crystal X-ray analysis reveals that the crystal crystallizes in monoclinic system,space group P21/c with a=16.6073(6),b=15.3333(5),C=19.9869(7)(A),β=103.41(1)°,Mr=5481.38,V=4950.8(3)(A)3,Z=2,Dc=3.677 g/cm3,F(000)=4900,μ(MoKα)=22.165 mm-1,GOOF=1.005,the final R=0.0228 and wR=0.0527.The crystal structure indicates that the[Co4(H2O)2(B-α-GeW9O34)2]12-polyoxoanion contains two trivacant Keggin[B-α-GeW9O34]10-fragments in a staggered fashion linked via a rhomb-like Co4O16 group in a centrosymmetric arrangement(C2h symmetry)leading to a sandwich-type structure.     

Syntheses and Structures of Two New Cobalt Supramolecular Complexes, [Co（4,4＇-bipy）2（H2O）4]·[Co2（4,4＇-bipy）3（H2O）8]·2TST·2（4,4＇-bipy）·4H2O and [Co（4,4＇-bipy）2（H2O）4]DSNT·4,4＇-bipy

Two new cobalt（II） supramolecular complexes [Co（4,4＇-bipy）2（H2O）4]·[Co2（4,4＇-bipy）3（H2O）8]·2TST·2（4,4＇-bipy）·4H2O 1 and [Co（4,4＇-bipy）2（H2O）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 （H3TST） and 2,4-bis（p-sulfanilato）-6-diethylamino-1,3,5-triazine （H2DSNT）, 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 P21/n with a = 13.599（4）, b = 18.988（6）, c = 22.995（7） A, β = 90.273（6）°, V = 5938（3）A^3, Z = 4, C56H59Co1.5N13O17S3, Mr = 1370.74, Dc = 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 〉 2σ（I）. The crystal structure of 2 belongs to the monoclinic system, space group C2/c with a = 18.864（6）, b = 14.283（5）, c = 20.246（7）A, β = 107.799（6）°, V = 5194（3）A^3, Z = 4, C49H52CoN12O10S2, Mr = 1092.08, Dc = 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.     

Synthesis and Crystal Structure of [VO2（C17H11N3O2） ] [VO （C4H13N3）（C6H5N3O） ]（C2H5OH）

The reaction of VO（acac）2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines （ethylenediamine or diethylenetriamine） in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2（C17H11N3O2）][VO- （C4H13N3）（C6H5N3O）]（C2H5OH） which crystallizes in the triclinic system, space group P1 with a = 8.0104（17）, b = 13.898（3）, c = 14.955（3）A, α = 89.103（4）, β = 79.551（4）, γ = 78.352（4）°, V = 1603.3（6）A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ（MoKα） = 0.71073 ]A,μ= 0.644 mm^-1, F（000） = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ（I）. According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.     

Synthesis and Structure of a POMs-based 3D Zeolike Ionic Crystal, {[Co（dpdo）2（H2O）2（CH3CN）]2（SiMo12O40）（H2O）2}n

A POMs-based 3D zeolike ionic crystal 1, {[Co（dpdo）2（CH3CN）（H2O）2]2（SiMo12O40）- （HEO）2}n （dpdo = 4,4＇-bipyridine-N,N＇-dioxide）, was constructed via self-assembly by embedding Keggintype [SiMo12O40]^4- polyanions within the intercrystalline voids as pillars and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 11.430（3）, b = 12.242（3）, c = 14.279（3）A, α = 106.196（4）,β = 94.316（4）, γ = 98.294（3）°, V = 1884.5（7）A^3 Z = 1, C44H50N10O54CoEMo12Si, Mr = 2880.17, Dc = 2.538 g/cm^3, p = 2.484 mm^-1,F（000） = 1388, the final R = 0.0383 and wR = 0.1096 for 7753 observed reflections with I 〉 2σ（I）. Flack factor is 0.22（3）. Compound 1 is a pillar-layered framework with the [SiMo12O40]^4- anions linearly located on the square voids between the 2D bilayers which are formed by the dpdo ligands and cobalt（II） ions.     

Macro-, Micro-, Nano- and Crystal Structures of a Homodinuclear Complex [NH3（ CH2）3NH3]2{Na2[（C6H4O2）2]（C6H4O2H）2}

A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[（C6H4O2）2]（C6H4OOH）2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy （SEM） indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy （TEM） reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2.     

Synthesis and Crystal Structure of [Cu2（DMF）（H2O）（C7H4NO4）2（C7H3NO4）]2·3.5DMF

A new copper（H） complex [Cu2（DMF）（H2O）（C7H4NO4）2（C7H3NO4）]2-3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 10.722（3）, b = 18.170（4）, c = 20.923（7）A,α = 105.297（9）, β = 101.701（10）, γ = 105.74（1）°, V= 3615（1）A^3, Z = 2, C58.50H64.50Cu4N1l.50O3150, Mr = 1686.90, Dc = 1.550 g/cm^3,μ= 1.255 mm^-1, F（000） = 1728.00, T = 150（2） K, the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I 〉 2σ（I）. In the crystal, each formular unit consists of two dinuclear copper（H） compounds, between which the O-H…O hydrogen bonds exist. Each Cu^Ⅱ cation is six-coordinated in an octahedral geometry. The intermolecular hydrogenbonding interaction leads to a 3-D framework of the title compound.     

Three Inorganic-organic Composite Polyoxotungstates： Syntheses,Characterization and Structures of [Cu（2,2＇-bpy）2]5[α-PW11.5Cu0.5O40]·2H2O, [Co（2,2＇-bpy）2（N3）2]4H3[α-PW12O40]·3H2O and [Cu（2,2＇-bpy）2（4,4＇-bpy）]2[α-GeW12O40]-4H2O

Three new inorganic-organic composite polyoxotungstates [Cu（2,2＇-bpy）2]5[α-PW11.5Cu0.5O40]·2H2O 1, [Co（2,2＇-bpy）2（N3）2]4H3[α-PW12O40]·3H2O 2 and [Cu（2,2＇-bpy）2（4,4＇-bpy）]2[α-GeW12O40]-4H2O 3 （2,2＇-bpy = 2,2＇-bipyridine, 4,4＇-bpy = 4,4＇-bipyridine） have been hydrothermally synthesized and structurally characterized. 1 crystallizes in the orthorhombic space group Pna21 with a = 27.847（3）, b = 21.597（2）, c = 20.1179（19）A, V= 12099（2）A^3, Z= 4, GOF= 1.038, R = 0.0427 and wR = 0.1035; 2 belongs to the triclinic space group P1^- with a = 12.31150（10）, b = 16.1954（4）, c = 19.36290（10）A, α = 99.366（11）, β =105.168（8）, γ = 111.836（8）°, V = 3309.98（9）A3, Z = l, GOF = 1.024, R = 0.0739 and wR = 0.2216; and 3 crystallizes in the monoclinic space group P21/n with a = 12.858（4）, b = 20.943（6）, c = 15.598（5）A, β = 102.338（5）°, V= 4103（2）A3, Z = 2, GOF = 1.026, R = 0.0557 and wR = 0.1316. The common structural features of 1-3 are that their molecular structures all consist of a saturated a-Keggin polyoxoanion and several discrete metal-organic moieties. Intriguingly, 2 and 3 are composed of metal-organic coordination moieties with two mixed ligands.     

Synthesis,Properties and Crystal Structure of a New Bismuth Oxalate： Na（C5NH6） [Bi（H2O）（C2O4）2]2·4H2O

A new bismuth oxalate Na（C5NH6）[Bi（H2O）（C2O4）2]2·4H2O has been obtained under hydrothermal conditions and characterized by X-ray diffraction. It crystallizes in monoclinic, space group C2/m with a = 12.020（5）, b = 11.190（8）, c = 11.067（10）A, β= 121.78（2）°, NaBi2C13NH18O22, Mr= 981.24, V = 1265.4（16） A^3, Z = 2, Dc = 2.575 g/cm^3,μ（MoKcr） = 14.005 mm^-1, F（000） = 912, R = 0.0179 and wR = 0.0394. In the structure, the Bi（III） centers are interconnected by oxalate ligands to produce honeycomb-like layers, which are further pillared by bridging ligand oxalate molecules to form a 3-D open-framework structure. Furthermore, the title compound exhibits blue luminescence with the emission peaks located at 394nm in the solid state at room temperature, and thus it could be useful in the field of photoactive materials.     

Synthesis and Crystal Structure of a Palladium（H） Coordination Polymer [Na2Pd（2,6-pydc）2（H2O）6]n

A novel coordination polymer [Na2Pd（2,6-pydc）2（H2O）6]n （2,6-H2pydc = 2,6-pyridinedicarboxylic acid） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclirtic system, space group P21/c, with a = 11.962（2）, b = 6.5552（13）, c = 12.673（3） A, β = 91.72（3）^o, V = 993.3（3） A^3, Z = 2, Mr = 590.68, Dc = 1.975 g/cm^3,μ = 1.059 mm^-1, F（000） = 592, the final R = 0.0211 and wR = 0.0454. In the crystal the Pd（II） ion adopts a distorted four-coordinated square-planar geometry and bonds to two bidentate 2,6-pyridinedicarboxylate molecules through caronyl oxygen and pyridine nitrogen atoms. The title complex exhibits a novel three-dimensional network structure.     

Hydrothermal Synthesis and Crystal Structure of [Cu（en）2（H2O）]2{PW11.5Cu0.5O40[Cu（en）2] }·2H2O

A transition metal substituted polyoxotungstate, [Cu（en）2（H2O）]2{PW11.5Cu0.5O40[Cu（en）2] }·2H2O
1 based on Keggin frameworks, has bccn hydrothcrmally synthesized and characterized by IR, TGA and single-crystal X-ray structural analysis. It is interesting to find that the structure unit contains two different valence cations, narncly, one [Cu（1）（en）2（H2O）]^＋ and one [Cu（2）（en）2（H2O）]^2＋. Data for the crystal： orthorhombic system, space group Pbca, a = 21.585（2）, b = 20.695（2）, c = 26.137（3）A, V = 11675（2）A^3, Z = 8, Mr = 3428.23, Dc = 3.901 g/cm^3, F（000） = 12156,μ（MoKα） = 23.932 mm^-1, the final R = 0.0468 and wR = 0.0969 for 6927 observed reflections （I 〉 2σ（I））.     

Hydrothermal Synthesis and Crystal Structure of a New Polyoxovanadate： [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O （en = Ethylenediamine）

A new compound has been synthesized under hydrothermal conditions and characterized by IR, elemental analysis, XPS and single-crystal X-ray diffraction analysis. The title compound [Mn（en）3]2en0.5[HV8VV8IVO38（CI）]·4.5H2O crystallizes in monoclinic, space group C2/c, with a = 17.016（4）, b = 18.858（4）, c = 18.872（4） A, β = 93.667（4）°, V = 6043（2）A3, Z = 4, Dc = 2.242 g/cm3, Mr = 2040.12, F（000） = 4020,μ = 2.895 mm-1, Rint = 0.0921, R = 0.0649 and wR = 0.1325. Single-crystal X-ray structure analysis indicates that the title compound consists of a polyanion [HV8VV8IVO38（CI）]4- cage, two [Mn（en）3]2^2＋ cations, four and a half lattice waters and a half ethylenediamine. In addition, intermolecular O-H...N, O-H...O, N-H...O and C-H...O hydrogen bonds link the molecules together to form a three-dimensional structure.     

Synthesis and Crystal Structure of a New Complex {[ Co^ⅢL2]·[Co^Ⅱ（H2O）6]0.6·2.25H2O }4 （H2L = N-（2-Hydroxyphenyl）salicylidenimine）

The reaction of Co（OAc）2·4H2O with the Schiff base H2L in a methanol solution affords the red crystals of { [Co^ⅢL2]·[Co^Ⅱ（H2O）6]0.5·2.25H2O}4 1 （H2L = N-（2-hydroxyphenyl） salicylidenimine）. The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n, C104Hi14Co6NaO37, Mr = 2421.61, a = 10.625（3）, b = 16.335（4）, c = 15.265（4）A^°, β = 102.990（4）°, V= 2581.6（11）A^°^3, Z = 1, Dc= 1.558 g/cm^3,μ = 1.034 mm^-1, F（000） = 1252, R = 0.0414 and wR = 0.1167 for 5889 reflections. The Co（HI） atom is six-coordinated by two nitrogen atoms and four oxygen atoms of two tridentate L ligands. The abundant hydrogen bonding interactions extend the complex into a one-dimensional supra- molecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.     

Synthesis,Crystal Structure and Photoluminescence of [Gd（C6NO2H5）3- （H2O）2]2n·（nH5O2）（nHgCl5）（2nHgCl4）·（2nH2O）

A heterometallic 4f-5d inorganic-organic metaMsonicotinato hybrid [Gd（C6NO2H5）3- （H2O）2]2n·（nH5O2）（nHgCl5）（2nHgCl4）·（2nH2O） 1 has been synthesized via hydrothermal reaction and structurally characterized. Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell： a = 24.234（8）, b = 20.816（7）, c = 15.333（3）A , β= 128.091（8）°, V = 6088（3）A^3, C36H47Cl13Gd2Hg3N6O20, Mr = 2260.92, Dc = 2.467 g/cm^3, S = 0.896, μ（MoKα） = 10.331 mm^-1, F（000） = 4216, R = 0.0344 and wR = 0.0629. The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure. Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.     

Synthesis and Crystal Structure of a New Dimolybdenum（V） Complex Na4[Mo2O4（HNTA）2]2·19H2O

The new binuclear molybdenum（V） complex Na4[Mo2O4（HNTA）2]2·19H2O （NTA = nitrilotriacetate） has been prepared and characterized by single-crystal X-ray diffraction analysis and IR. The crystal has space group Pnma with a = 10.2239（2）,b = 23.8174（3）,c = 23.1845（4） A,V = 5645.58（16）A^3,Z = 4,C24H66Mo4N4Na4O51,Mr = 1702.50,Dc = 1.958 g/cm^3,μ = 1.027 mm^-1,F（000） = 3280,T = 293（2） K,the final R = 0.0609 and wR = 0.1449 for 5512 observed reflections （I 〉 2σ（I））. Each MoV atom has a distorted octahedral coordination geometry,and the two coordination octahedra share a common edge to form a dioxo-bridged Mo2O4 unit which is coordinated by NTA ligands. The dianionic binuclear units [Mo2O4（HNTA）2]^2- are interconnected by Na^＋ into a layered structure.     

A Novel 3D Heterobimetallic Cyano-bridged Coor- dination Polymer {（NH4）2[Cd（H20）Fe（CN）6]}n： Synthesis and Crystal Structure①

A novel heterobimetaUic coordination polymer, {（NH4）2[Cd（H20）Fe（CN）6]}n 1, has been synthesized by using the slow diffusion method and structurally characterized by elemental analysis, 1R spectroscopy and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group P21/n, a = 7.4202（16）, b = 14.939（3）, c = 10.868（2） A and ,8 = 91.660（3）°. For 1, five CN groups of Fe（CN）6]4- are involved in bridging. The polymer displays a 3D open microporous framework with 5-connected uninodal （46.64） topology.     

A 3D Supramolecular Framework Based on 1D {[Co（proH）（H2O）3]2[P2Mo5O23]}n Chains and 1D Helical Water Chains

A three-dimensional supramolecular architecture, {[Co（proH）（H2O）3]2[P2Mo5O23]}·7H2O （1, pro = praline）, has been synthesized and characterized by IR, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. 1 crystallizes in monoclinic, space group C2 with a = 20.600（3）, b = 11.6980（11）, c = 9.2944（10）A, β = 107.837（4）°, V = 2132.1（4） A^3, Z = 2, C10H46Co2Mo5N2O40P2, Mr = 1493.99, Dc = 2.327 g/cm^3, F（000） = 1468, μ（MoKα） = 2.375 mm^-1, the final R = 0.0339 and wR = 0.0844 for 4169 observed reflections with I 〉 2σ（I）. Singlecrystal X-ray crystallographic analysis reveals that the helical water chains and {[Co（proH）- （H2O）3]2[P2Mo5O23]}n chains are perpendicular to each other and extend into an overall three-dimensional supramolecular architecture by hydrogen-bonding interactions. The magnetic investigation indicates weak antiferromagnetic interactions in the compound.     

Hydrothermal Synthesis and Structure of One New Vanadoarsenate [Zn（dien）（Hdien）]2[As6V15O42（H2O）]·4H2O

One new arsenic-vanadium cluster, [Zn（dien）（Hdien）]2[As6V15O42（H2O）]·4H2O （1, dien = diethylenetriamine）, has been hydrothermally synthesized and characterized by IR, elemental analysis, TGA, magnetic property and single-crystal X-ray diffraction analysis. Crystal data for 1： monoclinic, space group P21/n, a = 13.959（3）, b = 22.428（5）, c = 22.831（5） A^°, β = 90.733（4）°, Z = 4. X-ray crystallographic study showed that compound 1 is constructed from [As6V15O42（H2O）]^6- polyoxoanions linked together by novel [Zn（dien）（Hdien）]^3＋ complex fragments via hydrogen bonds into a three-dimensional network. Variable temperature susceptibility measurement demonstrates the presence of antiferromagnetic interaction between V^IV cations in 1.     

Synthesis and Crystal Structure of a Co（ Ⅱ ） Complex with Taurine-5-methyl-2-hydroxyisophthalaldehyde Schiff Bases [Co（C13H16N2O7S2）（H2O）3]2·H2O

The title complex [CoL（H20）3]2·H2O （C26H46N4O21S4CO2）, where L = taurine-5- methyl-2-hydroxyisophthalaldehydes, has been synthesized and characterized by IR and X-ray diffraction analysis. The crystal of the complex belongs to the triclinic system, space group P1, with a = 11.197（4）, b = 13.309（5）, c = 14.486（5） ]A, a = 78.827（13）,β = 70.547（11）, γ = 81.058（13）°, Mr = 996.77, S = 1.08, V= 1987.2（13） A3, Z = 2, Dc = 1.666 g/cm3, F（000） = 1032,μ = 1.131 mm^-1, R = 0.0633 and wR = 0.1293. According to the structural analysis, the Co（ Ⅱ ） ion adopts a slightly distorted six-coordinated octahedral geometry. One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom. Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds, thus generating an infinite chain constructed by hydrogen bonds.     

Synthesis and Crystal Structure of a Three-dimensional Manganese（Ⅱ） Complex （tataH）2[Mn（pydc）2]·4H2O （tata = 2,4,6-Trlamino-1,3,5-trlazine,pydcH2 =Pyridine-2,6-dicarboxylic Acid）

A manganese（Ⅱ） complex （tataH）2[Mn（pydc）2]·4H2O （C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847（3）, b = 10.9813（3）, c = 15.2616（5）A, a = 101.5310（10）, β = 90.2610（10）, γ = 116.4600（ 10）% V = 1459.44（8）A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F（000） = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D＇…A＇ H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between （tataH）^＋, [Mn（pydc）2]^2- and crystal water.     

A Novel Composite Based On Phosphotungstate Anion [n-Bu4N][Cu（2,2-bipy）3][PW12O40]·CH3CN·H2O

A novel composite, [C16H36N][Cu（2,2-bipy）3][PW12O40]·CH3CN·H2O based on Keggin-type phosphotungstate, has been synthesized in acetonitrile at moderate temperature and then characterized by IR and single-crystal X-ray structural analysis. The crystal is of monoclinic system, space group P21/n with a = 20.489（4）, b = 17.249（3）, c = 23.723（4）A, β = 95.114（2）^o, V = 8350（3）A3, Mr = 3710.79, Z = 4, Dc = 2.952 g/cm^3, F（000） = 6676, μ = 16.808 mm^-1, the final R = 0.0551 and wR = 0.1269 for 9460 observed reflections with I 〉 20（I）. Interestingly, it is found that the structure unit contains two different cations of [C16H36N]^＋ and [Cu（2,2-bipy）3]^2＋.