Supramolecular Terbium-SIP Complex Pillared by 4,4＇-Bipyridyl, {[Tb（SIP）（H2O）5]2（bpy）3（H2O）}n： Synthesis,Crystal Structure and Photoluminescence

The supramolecular terbium complex, {[Tb（SIP）（H2O）5]2（bpy）3（H2O）}n （NaH2SIP = 5-sulfoisophthalic acid monosodium salt and bpy = 4,4＇-bipyridyl）, has been synthesized by the hydrothermal reaction of Tb4O7 with NaH2SIP and bpy at 165 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, powder X-ray diffraction and photoluminescence spectrum. It crystallizes in a monoclinic system, space group C2/c, with a = 30.6840（1）, b = 10.9206（2）, c = 17.4967（3） A, β= 111.931（1）°, V = 5438.65（14） A^3, Z = 4, C46H52N6O25S2Tb2, Mr = 1470.90, Dc = 1.796 g/cm^3, p = 2.747 mm^-1, F（000） = 2928, the final R = 0.0654 and wR = 0.1322 for 3806 observed reflections with I 〉 2σ（I）. In the neutral [Tb（SIP）（H2O）5]2 motif, the Tb（III） ions are linked by the SIP ligands to form a one-dimensional zigzag chain propagating along the c axis. The zigzag chains are linked together by hydrogen bonds and π-π stacking interactions to form a two-dimensional supramolecular framework. The uncoordinated bpy molecules act as pillars to extend the two-dimensional sheets into a distinctive pillared three-dimensional supramolecular structure through O-H...N hydrogen bonds. The photoluminescence of the complex was investigated at room temperature in the solid state.     

Synthesis, Characterization and Crystal Structure of [Ni（S2P{O}OC6H4CH3-p）（dppv）]

O-（p-tolyl）dithiophosphato nickel complex [Ni（S2P{O}OC6HaCH3-p）（dppv）] has been synthesized by the treatment of （dppv）NiCl2 （dppv = Ph2PCH=CHPPh2） with （p-CH3C6HaO）2P{S}SH＇Et2NH in THF. The new complex was fully characterized by elemental analysis, IR, 1H NMR, 31p NMR spectroscopies and thermo-gravimetric analysis. The molecular structure of the complex was established by X-ray crystallography. The crystal crystallizes in monoclinic, space group P21/c with a = 9.2739（5）, b = 17.8803（8）, c = 20.1879（12） A, fl = 93.269（5）, V = 3342.1（3） A3, Z = 4, C33H29NiO2P3S2, Mr = 673.30, Dc = 1.338 g/cm3, F（000） = 1392 and #（MoKa） = 0.877 rnm-l. The final R = 0.0578 and wR = 0.1045 for 4138 observed reflections with 1 〉 20（/） and R = 0.1050 and wR = 0.1204 for all data. The Ni centre atom adopts a NiP2S2 square-planar geometry with two phosphorus atoms from the dppv ligand and two sulfur atoms from the O-（p-tolyl）dithiophosphate ligand. The most interesting structural feature of the title complex resides in its 1D helical chain structure constructing via intermolecular C-H＇＂O secondary interactions along the b-axis. The adjacent helical chains running in opposite directions are connected into a 1D double-stranded helical chain and further linked into a 2D supramolecular network by weak C-H.--C interaction.     

Syntheses and Characterizations of （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 and （NH3CH2CH2NH3）2Bi2I10

The title compounds have been respectively synthesized by solution process and solvothermal reaction, and their crystal structures were determined by X-ray diffraction method. For （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 1, it crystallizes in tficlinic, space group P1^- with Mr = 2049.76, a = 8.5719（1）, b = 11.7461（3）, c = 15.700（1）A, V = 1451.4（1）A^3, Z = 1, Dc = 2.345 g/cm^3, F（000） = 924, μ（MoKα） = 8.907 mm^-1, T = 293（2） K, the final R = 0.0655 and wR = 0.0804 for 2399 observed reflections with I 〉 2σ（I）. For （NH3CH2CH2NH3）2Bi2I10 2, it crystallizes in monoclinic, space group P21/n with Mr= 1811.20, a = 8.434（4）, b = 13.862（6）, c = 13.362（6）A, V = 1499.9（12）A^3, Z = 2, Dc = 4.010 g/cm^3, F（000） = 1536,μ（MoKα） = 22.007 mm^-1, T = 293（2） K, the final R = 0.0584 and wR = 0.1451 for 1798 observed reflections with I 〉 2σ（I）. The structures of 1 and 2 contain halobismuthate monomer and dimers, respectively. It is noteworthy that the dimers and their organic counters in 2 connect each other by N…I hydrogen bonds to form a layered structure, and the electrostatic interactions and crystal packing forces between layers give rise to the packing of the crystal. The optical absorption spectra of 1 and 2 reveal the appearance of sharp optical gaps of 2.13 and 2.01 eV, respectively.     

Synthesis and Crystal Structure of a Novel Hexanuclear Copper-indium Thiolate Complex [（InCl）2（OMe）（μ-OMe）2（μ3-OMe）（μ-SPrn）2（CuPPh3）]2

A novel hexanuclear copper-indium thiolate complex, [（InCl）2（OMe）（μ-OMe）2（μ- OMe）（μ-SPrn）2（CuPPh3）]2 1, was synthesized from the reaction of NaSPrn, InCl3 and [Cu（Me- CN）a][PF6] in the presence of Ph3P and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P211n with a = 11.3533（8）, b = 15.4939（11）, c = 20.5189（14） A, β = 98.577（2）°, V = 3569.0（4） A3, Z = 2, C56H82Cl4Cu2In4O8P2S4, Mr = 1801.56, Dc = 1.676 g/cm3,μ（MoKa） = 2.213 mm^-1, F（000） = 1796, S = 0.985, the final R = 0.0559 and wR = 0.1099 for 8878 observed reflections with I 〉 2σ（I） and 367 variables. Complex 1 consists of two CuPPh3 fragments which symmetrically side-attach to the tetranuclear core of [InaCl4（OMe）2（μ-OMe）a（μ- OMe）2（μ-SPrn）4] by coordinating with sulfur atoms of propane-thio moieties. The average In-Ot （terminal）, In-μ-O and In-μ3-O bond distances are 2.305（4）, 2.144（4） and 2.294（4） A, respectively.     

A Polymeric Iodiplumbate（Ⅱ） Directed by Heterocyclic Monoprotonated Quaternary Ammonium

A new iodiplumbate polymer [（AOD）（Pb216）]n 1 （AOD = O-protonated 4-azonia-7- oxaspiro（4,5） decane quaternary ammonium） was synthesized by self-assembly reaction of AOD-I, Pb（NO3）2 and NaI, and structurally determined. Compound 1 crystallizes in the hexagonal system, space group P3, with a = 18.2704（8）, c = 8.1663（6） A, V= 2360.8（2） A3, Z = 3, De = 2.783 g/cm^3, F（000） = 1686, C8H17I6NOPb2, Mr = 1319.03, μ（MoKa） = 16.562 mm^-1, the final R = 0.0535 and wR = 0.1793 for 4943 observed reflections with I 〉 2σ（I）. In compound 1, three independent （PbEI6）^2-n infinite chains in each unit cell shape the sketch of compound 1 under the template of AOD-H^2＋ cation. Each （PbaI6）^2-n chain generates from the face-sharing of distorted PbI6 octahedra. （PbEI6）^2-n polyanions interact with AOD-H^2＋ cations by electrostatic interaction in the crystal to feature a so-called hybrid structure. Compound 1 was further characterized with IR, elemental analysis, fluorescence spectrum and thermal analysis. Based on the crystal structure data, DFT calculation was carried out to reveal the electronic structure of compound 1.     

Construction of a 2D Cd（II） Coordination Polymer Based on a V-shaped Bidentate Ligand

A two-dimensional（2D）coordination polymer{[Cd（bdc）（dpb）]·H2O}n（1）has been prepared by solvothermal reaction of 1,3-dipyridyl benzene（1,3-dpb）with deprotonated1,4-benzenedicarboxylate（H2bdc）,and was characterized by elemental analysis,IR spectroscopy,and X-ray single-crystal diffraction.It crystallizes in the monoclinic system,space group C2/c with a=15.1839（12）,b=20.7585（17）,c=7.2989（6）,β=117.3450（10）°,V=2043.5（3）3,C24H18N2O5Cd,Mr=526.81,Dc=1.712 g/cm3,F（000）=1056.0,μ=1.110 mm-1and Z=4.The neighboring Cd（II）ions link the bdc2-anions and 1,3-dpb to form an infinite 2D sheet,and such two2D sheets are interlocked with each other to form a 2D→2D sheet.Two groups of interlocked sheets are further linked together by intermolecularπ···πinteraction,giving a 3D supramolecular network.In addition,the fluorescence property of 1 was also studied.     

Synthesis and Structure of {（Tab-Tab）[Ag2（μ-Cl）41.2MeCN}n （Tab = 4-（Trimethylammonio）benzenethiolate）

In the presence of Et4NCl·H2O, reaction of AgCl with TabHPF6 in MeCN afforded the title complex {（Tab-Tab）[Ag2（μ-Cl）4]-2MeCN}n 1. 1 crystallizes in the orthorhombic space group Pbcn with a = 16.782（3）, b = 6.8358（14）, c = 26.194（5） A, V = 3004.9（10） A3, Z = 8,μ = 1.817 mm^-1, Dc = 1.711 g/cm3, T= 223 K, C1lH16AgCl2N2S, Mr= 387.10, F（000） = 1544, S= 1.160, R = 0.0528 and wR = 0.0896 for 2732 observed reflections with I 〉 2σ（I）. 1 contains a 1D linear [Ag2Cl4]n^2n- chain coupled with the [Tab-Tab]2＋ dications. Intermolecular hydrogen bonding interactions between the protons of methyl groups from the Tab-Tab dications and the chlorides result in the formation of a 2D hydrogen-bonded network.     

Syntheses and Crystal Structures of Two Nickel（Ⅱ） Complexes [Ni（dmpzm）2（L）]Cl·nH2O（L = HCO2, OAc; n = 2, 3; dmpzm = 1,1＇-Methylenebis（3,5-dimethyl-1H-pyrazole））

Reactions of NiCl2-6H2O with dmpzm and formic or acetic acid at PH = 7 produced the two title compounds, [Ni（dmpzm）2（HCO2）]Cl·2H2O 1 and [Ni（dmpzm）2（OAc）]C2·H2O 2 （dmpzm = 1,1 ＇-methylenebis（3,5-dimethyl-lH-pyrazole））. 1 and 2 were characterized by elemental analysis, IR spectra, and thermogravimetric analysis. 1 crystallizes in the orthorhombic system, space group Pcca with a = 18.700（2）, b = 8.6843（9）, c = 18.098（2）A, V= 2939.1（5）A^3, Z = 4, Dc = 1.319 g/cm^3, T = 193 K, C23H37CINsNiO4, Mr = 583.75, F（000） = 1232, p（MoKa） = 0.792 cm^-1, S = 1.079, R = 0.0772 and wR = 0.1958 for 2265 observed reflections with I〉 2σ（I）. 2 crystallizes in the orthorhombic system, space group Pcca with a = 17.011（3）, b = 18.630（4）, c = 19.300（4）A, V = 6117（2）A^3, Z = 8, Dc = 1.337 g/cm^3, T= 193（2） K, C24H41C1N8NiO5, Mr = 615.79, F（000） = 2608, μ（MoKa） = 0.768 cm^-1, S = 1.059, R = 0.0518 and wR = 0.1109 for 5124 observed reflections with I 〉 2σ（I）. The Ni atoms in 1 or 2 are chelated by two dmpzm ligands and one formate or acetate anion, forming slightly distorted octahedral geometries. In the crystals of 1 or 2, intermolecular hydrogen bonding interactions result in the formation of 2D hydrogen-bonded frameworks.     

Synthesis and Crystal Structure of a Novel Tetranuclear Complex [Pb4（HQ）6（NO3）2]

Reaction of 8-hydroxyquinoline （HQ） with Pb（NO3）2 in water resulted in the formation of a tetranuclear complex [Pb4（HQ）6（NO3）2] 1. It has been characterized by IR, elemental analyses and X-ray diffraction. Crystal data for this complex： triclinic system, space group P1, a = 9.7399（6）, b = 11.6535（8）, c = 12.6806（8） A, α = 62.8050（10）, β = 78.4910（10）, γ = 80.5490（10）°, C54H36N8O12Pb4, Mr= 1817.67, Z = 1, V = 1250.04（14）A^3, Dc = 2.415 g/cm^3,μ = 13.503 mm^-1, -12≤h≤8, -14≤k≤13, -15≤1≤15, F（000） = 840, Rint = 0.0217, R= 0.0348 and wR = 0.0927. X-ray crystal structure analysis revealed that in 1 each Pb（ II ） contains a stereo- chemically active lone pair of electrons. The Pb…C interaction, C-H……O weak interaction and π…π stacking interactions are observed in the complex. In the solid state, the complex possesses strong photoluminescent emission at 485 and 528 nm.     

Hydrothermal Synthesis and Crystal Structure of a Novel Polyoxometalate K（C4N2H12）4（C4N2H11）2- [Mo8^VMo4^（VI）CdP8O54（OH）8]F·6H2O

The title compound 1 has been synthesized by the reaction of H2MoO4,CdCl2,H3PO4,KF,piperazine hexahydrate and water in aqueous solution under mild hydrothermal conditions. Single-crystal X-ray analysis reveals that the title compound crystallizes in the triclinic system,space group P1 with a = 14.049（3）,b = 15.972（3）,c = 20.043（4） A,α = 85.82（3）,β = 81.28（3）,γ = 67.15（3）°,V = 4095.9（14） A^3,Mr = 3204.62,Z = 2,Dc = 2.598 g/c^m3,μ = 2.360 mm^-1,F（000） = 3124,the final R = 0.0314,wR = 0.0826 and S = 0.989 for 18592 observed reflections with I 〉 2σ（I）. The crystal packing is stabilized by N–H… and O–H… intraand intermolecular hydrogen bonds to form an infinite 3D network.     

Syntheses, Crystal Structures and Magnetism of Two New Coordination Polymers [Ni（bix）2Cl2]n and [Co（bix）Cl2]n

The self-assembly reactions of MIICl2 (M = Ni, Co) with the flexible bix ligand [bix = 1,4-bis(imidazole-1-ylmethyl)benzene] yielded a 2D network [NiII(bix)2Cl2]n 1 and a 1D chain [CoII(bix)Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231(7), b = 12.7787(9), c = 13.9374(13) , β = 105.419(4)o, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0(2) 3, Dc = 1.518 g/cm3, μ = 0.969 mm-1, F(000) = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections (I > 2σ(I)). Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696(6), b = 10.2128(6), c = 14.4943(9) , C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01(17) 3, Dc = 1.453 g/cm3, μ = 1.334 mm-1, F(000) = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections (I > 2σ(I)). Magnetic properties of the title complexes were also investigated.     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

CRYSTAL STRUCTURES OF TWO DITHIOLATO-COPPER COMPLEXES (Ph_4P)Cu(BDT)_2 AND (Ph_4P)Cu(TDT)_2

<正> [(C6H5)4P]Cu(S2C6H4)2(Ⅰ),Mr = 683. 39,monoclinic,space group C2/c,a=16. 099 (4),b= 11. 913(3) ,c = 16: 715(9) A ,β=97. 13(4)°, v = 3180. 7 A3,z=4.MoKa radiation,λ= 0. 71069A ,Dc= 1. 427g/cm3,μ= 10. 1cm-1,F(000) = 1400,R=0. 061 and Rw = 0. 068 for 2189 reflections with Ⅰ>3σ(Ⅰ). [(C6H5)4P]Cu (S2C7H6)2(Ⅰ),Mr = 711. 45,monoclinic,space group C2/c,a=16. 501(6),b = 37. 461 (15),c=16. 684(4)A,β=96. 70(4)°, v= 10248. 8(46) A3,z= 12. MoKa radiation, λ= 0. 71069A,Dc=1.383g/cm3,μ=9. 45cm-1,F(000).= 4416,R= 0. 074 and Rw= 0. 078 for 2085 reflections with I>2σ(I)(1). The copper atom in the complexes is surrounded by four sulfur atoms from two dithiolato ligands in an approximate, square-plane. The average Cu-S distances of the copmplexes(Ⅰ) and (Ⅱ) are 2. 179 and 2. 178 A, respectively.     

Synthesis,Characterization and Crystal Structure of One Ni_2（salen）_2 Complex

A homochiral complex,Ni 2 (salen) 2 (1,salen=(R,R)-(-)-N,N-bis(3-tert-butyl-5-(4ethynylpyridyl)salicyl-idene)-1,2-diaminocyclohexane),has been synthesized and characterized by IR,microanalysis,CD spectra,TGA,powder and single-crystal X-ray crystallography.It crystallizes in triclinic,space group P1 with a=11.896(2),b=12.571(3),c=13.197(3),α=65.61(3),β=73.90(3),γ=75.87(3)o,V=1707.9(6) 3,Z=2,C 42 H 42 N 4 NiO 2,M r=693.51,D c=1.349 g/cm 3,F(000)=732,μ=0.612 mm-1,GOOF=1.015,the final R=0.0290 and wR=0.0796 for 9002 observed reflections with I > 2σ(Ⅰ).The complex architecture is constructed by intermolecular π···π interaction and assembled into a 2D structure via C-H···π interactions between the cyclohexanes and pyridine rings.     

One—dimensional Chain Topology in [Ag（C6H6NCl）2]（ClO4）,Generated through Weak Interaction between Molecules

1 INTRODUCTION It is known that the research of supramolecular chemistry and crystal engineering of coordination compound receives great interest nowadays.[1~6] Supramolecules are not just collection of molecules, generally, the formation of a supramolecule is through hydrogen bonding, π-π stacking interaction and the weak interaction between molecules.[1] Recently, more and more supramolecular compounds containing polymeric Ag(I) species have been described due to the coordination mode…     

Synthesis and Structure of Bis（indene—1,2,3—trione 2—oximato）bis （aqua）Mn（Ⅱ）：Mn（C9H4NO3）2（H2O）2

1 INTRODUCTION The interest in the complexes of transition metals with ligands ketoxime[1, 2] as potential models for metal binding sites in ferroverdin[3, 4] has prompted the investigation on the structures and the overall coordination geometry of the metal centers in these complexes. Oxime derivatives are interesting ligands since the ketoximes are found to chelate transition metals through the N (oxime) and O (ketone) atoms[5, 6]. However, monodentate coordination via only one O or …     

Crystal Structure of Bis(3-hydroxy-2-pyridyl)disulfide

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Synthesis and Crystal Structure of a 2D Coordination Polymer： [Nd2（PDB）2（CH3COO）2（H2O）3]

A novel coordination polymer [Nd2（PDB）2（CH3COO）2（H2O）3] （H2PDB = pyridine3,4-dicarboxylic acid） has been synthesized by the reaction of Nd（CH3COO）3 with pyridine3,4-dicarboxylic acid under hydrothermal conditions. Elemental analysis, IR spectra and X-ray crystal structure analysis were carried out to determine the composition and crystal structure of the title complex which belongs to the triclinic system, space group P^-1 with a = 6.9409（14）, b = 7.5497（15）, c = 22.530（5）A, α = 84.79（3）, β = 88.15（3）, γ= 75.55（3）^o, C18H18N2O15Nd2, Mr = 790.82, Z = 2, V = 1138.5（4） A^3, Dc = 2.307 g/cm^3,μ = 4.593 mm^-1, -6≤h≤8, -5≤k ≤8, -26≤l≤ 26, F（000） = 760, Rint = 0.0298, R= 0.0314 and wR= 0.0695 （I〉 2σ（I））. Nd（1） and Nd（2） are linked into zigzag chains by carboxylate groups of acetate with interesting μ3-η^2：η^2 fashion. The zigzag chains are bridged by PDB to form a 2D framework, and a 3D supramolecular network is further constructed via π-π stacking.     

Crystal Structure of {(PPh_3)_2RuB_(10)H_8[(CH_3)_2CHO]_2}

1INTRODUCTIONFromreactionsof[RuCl,(PPh,),jwithcloso-[B,,H,,j'-respectivelyinEtOH/CH,Cl,t'i,CH,COOH/THF"'andC,H,COOH/CH,Cl,">solution,itcanbefoundthatbothalcoholandorganicacidcanreplacehydrogenatomsinborane.Further-more,accordingtotheirdifferentreactiontime(3h,1OOhand113hrespectively),wecanknowthatalcoholismoreactivetoreplacehydrogenatomsinborane.NowinordertoconfirmthisrulefurtherweusePhCH(OH)COOH/(CH3)2CHOHsolutioninsteadofabove-mentionedsolutions.Newcompounds(I)and(II…     

Synthesis and Crystal Structure of a Distorted 2D （6,3） Layer Complex, [Cd（H2mbdpz）（N3）2]n （H2mbdpz = 4,4′-Methylenebis（3,5-dimethylpyrazole）） Containing both End-on and End-to-end Azide Bridges

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.