Syntheses and Crystal Structures of Two New Zinc(Ⅱ)Nitroxide Radical Complexes Bridged by Isophthalate

Two novel complexes [Zn(NIT3-py)(ip)]n 1 and [Zn(im3-py)(ip)]n 2 (NIT3-py =2-(3"-pyridyl)-4,4,5,5,-tetramethylimidazoline-1-oxyl-3-oxide, im3-py = 2-(3'-pyridyl)-4,4,5,5-te-tramethylimidazoline-1-oxyl, ip = isophthalate) have been synthesized and structurally determinedby X-ray diffraction.Crystal data for 1: C32H36N6O8Zn, Mr= 698.04, monoclinic, space group C with a = 23.600(3), b = 10.2073(12), c = 13.4027(16)(A), β= 92.586(2)°, V = 3225.3(7) (A)3, Dc=1.438 g/cm3, F(000) = 1456,μ(MoKα) = 0.822 mm-1, Z = 4, the final R = 0.0390 and wR = 0.1032 for 6037 independent reflections with Rint=0.0214.Crystal data for 2: C32H36N6O6Zn, Mr = 666.04,monoclinic, space group C2/c with a = 24.434(4), b = 13.543(2), c = 10.2379(16)(A), β= 109.024(2)°,V= 3202.8(9)(A)3, Dc= 1.381 g/cm3, F(000) = 1392,μ(MoKα) = 0.820 mm-1, Z= 4,the final R = 0.0304 and wR = 0.0658 for 2833 independent reflections with Rint = 0.0307.X-ray analysis reveals that both Zn(Ⅱ) ions are four-coordinated by two pyridyl-N atoms from nitroxide radicals and two carboxylate oxygen atoms to form distorted tetrahedral geometries.Each iso-phthalate dianion binds two Zn(Ⅱ) ions in a monodentate mode, leading to a 1-D chain structure.     

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

A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MnN14O12, 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), α =101.5310(10), β = 90.2610(10), γ = 116.4600(10)°, V = 1459.44(8) A3, Z = 2, Dc = 1.619 g/cm3, μ = 0.539 mm-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the MnⅡ atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate 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.     

Two Nickel（Ⅱ） Complexes Constructed by Novel Bis（3-methoxy-2-pyridyl）ether-6,6′-dicarboxylic Acid Ligand： Lattice Water Control of Structure

Under given conditions, two complexes of [Ni（H20）2BEDA]·2H2O 1 and [Ni（Py）2- BEDA]·6H2O 2 （BEDA = bis（3-methoxy-2-pyridyl）ether-6,6′-dicarboxylic acid） have been synthesized and characterized by elemental analysis and X-ray single-crystal diffraction. Crystal data for 1： C14H18NiN2O11, monoelinic C2/c, a = 14.3844（17）, b = 12.9900（15）, c = 9.6309（11） A, β = 104.3350（10）°, V= 1743.5（4） A3, Z = 4, Dc= 1.711 g/cm^3, F（000） = 928, μ = 1.179 mm^-1, Mr= 449.01, the final R = 0.0228 and wR = 0.0625. Crystal data for 2： C24H32NiN4O13, triclinic P1, a = 9.423（2）, b = 11.863（3）, c = 13.089（3） A, α = 91.511（3）, β = 92.465（3）, γ = 100.696（2）°, V = 1435.6（6） A^3, Z = 2, Dc= 1.488 g/cm^3, F（000） = 672, μ = 0.748 mm^-1, Mr= 643.25, the final R = 0.0400 and wR = 0.0975. Interestingly, in the two complexes, lattice water molecules dominate its crystal structures. Therefore, extensive intermolecular hydrogen bonds assemble 1 and 2 into 2D extended sheets and a 3D open framework, respectively. Furthermore, water molecules present in 2 are associated to form water clusters.     

Synthesis,Structure and Luminescent Properties of [Zn(btzb)2Cl2]·2H2O[btzb=1,2-Bis(5-tetrazolyl)benzene]

The title compound[Zn(btzb)2Cl2]·2H2O(1·2H2O,btzb=1,2-bis(5-tetrazolyl)benzene)was synthesized in situ by the[2 3] cycloaddition reaction of phthalonitrile with NaN3 in water in the presence of ZnCl2 under refluxing conditions.1·2H2O crystallizes in the monoclinic system,space group P21/c with a=9.0119(18),b=7.5566(15),c=18.076(5)(A),β=114.67(2)°,V=1118.6(4)(A)3,Z=2,Dc=1.784 g/cm3 T=223(2)K,C16H16N16O2Cl2Zn,Mr=600.74,F(000)=608,μ(MoKα)=1.393 mm-1,S=1.081,R=0.0306 and wR=0.0669 for 1896 observed reflections with Ⅰ ＞2σ(Ⅰ).The Zn2 ion of 1 is coordinated by four N atoms from two btzb ligands and two Cl atoms,forming a distorted octahedral coordination geometry.A number of intermolecular hydrogen bonding interactions between molecules 1 and/or the solvated water molecules result in a 3D hydrogen-bonded structure.The luminescent property of 1·2H2O was also investigated.     

Hydrothermal Synthesis and Crystal Structure of a Novel Dinuclear Co(Ⅱ) Complex: [Co2(2,2(')-bpy)2((-L)2(L)2(μ-H2O)] (HL = 4-Chlorobenzoic Acid)

A new 4-chlorobenzoic acid bridge Co(Ⅱ) complex [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ- H2O)] (HL = 4-chlorobenzoic acid) has been obtained by hydrothermal synthesis, and X-ray single-crystal diffraction analysis shows that it crystallizes in the monoclinic system, space group C2/c with a = 22.537(5), b = 16.212(3),c = 15.306(3)(A), β= 124.37(3)°, V = 4616.1(16) (A)3, Mr = 1070.45, Dc = 1.540 g/cm3, Z = 4, μ = 1.012 mm-1, F(000) = 2176, the final R = 0.0338 and Wr = 0.0810. The title complex is composed of dinuclear [Co2(2,2(')-bpy)2(μ-L)2(L)2(μ-H2O)] molecules. Each Co(Ⅱ) atom is coordinated by two nitrogen atoms from one 2,2'-bipyridine ligand, three oxygen atoms from three 4-chlorobenzoic ions and another oxygen atom from one water molecule. The two Co(Ⅱ) atoms are connected by two 4-chlorobenzoic ions and one bridged water molecule. The dinuclear molecules are interlinked by hydrogen bond and π-π stacking interactions into a three-dimensional supramolecular network.     

Hydrothermal Synthesis, Structure and Photoluminescence of a 2D Lead(Ⅱ) Coordination Polymer with (4,3 6) Topology Based on Pb and 1,2,3,4-Butanetetracarboxylate Nodes

A lead(Ⅱ) coordination polymer, {[Pb2(butca)(H2O)2](H2O)2}n (1), has been synthesized by the hydrothermal reaction of Pb(OH)2 and 1, 2, 3, 4-butanetetracarboxylic acid (H4butca) at 160 ℃. Single-crystal X-ray analyses reveal that it crystallizes in monoclinic, space group P21/c with a = 7.616(5), b = 7.584(4), c = 12.314(7) (A), β = 105.595(12)°, V = 685.0(7) (A)3, Z = 4,C8H14O12Pb2, Mr= 716.57, Dc=3.474 g/cm3,μ = 24.610 mm-1, F(000) = 644, the final R = 0.0381 and wR = 0.1176 for 1465 observed reflections with Ⅰ＞ 2σ(Ⅰ). The complex presents a 2D-layered structure featuring two different types of rings, and has a (4,3 6) topology based on Pb and butca 4- nodes. In solid state, complex 1 shows photoluminescence with the maximum emission intensity at 468 nm under 286 nm excitation.     

Hydrothermal Syntheses and Structural Characterizations of Two ML-Containing Polyoxomolybdates:[Cu~Ⅱ_2(HL)_3]_2[Mo_8O_(26)]·(H_2O)_4 and [Ni~Ⅱ(HL)_3]_2(Mo_8O_(26))·(H_2O)_3(HL=3-(2-Pyridyl)pyrazole)

Two new polyoxomolybdate compounds,namely CuII2(HL)3]2[Mo8O26]·(H2O)4(1) and [NiII(HL)3]2(Mo8O26)·(H2O)3(2)(HL = 3-(2-pyridyl)pyrazole),were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu(II) ions linked by three 3-(2-pyridyl)pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-(2-pyridyl)pyrazole ligands.Crystal data of 1:C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850(2),b = 18.510(4),c = 17.230(3) ,β = 100.57(3)°,V = 3401.6(12) 3,Z = 4,Dc = 2.324 g/cm3,F(000) = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775(Ⅰ 2σ(Ⅰ));Crystal data for 2:C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799(2),b = 14.7970(13),c = 23.141(2) ,β = 91.6180(10)°,V = 7119.0(11) 3,Z = 4,Dc = 2.077 g/cm3,F(000) = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696(Ⅰ 2σ(Ⅰ)).     

Synthesis, Crystal Structure and Photoluminescent Property of a Novel Silver(Ⅰ) Compound {[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n

Self-assembly of Ag(Ⅰ) nitrate, 1,3-bis(4-pyridyl)propane (bpp) and phthalic acid monopotassium salt (KHphth) in CH3OH-H2O solution produced the title complex,{[Ag(bpp)]2(Hphth)(NO3)·(H2O)2}n, which was characterized by single-crystal X-ray diffraction,elemental analysis, IR spectrum, and photoluminescent spectrum. Single-crystal X-ray analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, with α =15.4174(5), b = 8.6398(2), c = 25.2466(8) (A), β = 91.072(1)°, V = 3362.34(17) (A)3, Z = 4,C34H37N5O9Ag2, Mr = 875.43, Dc = 1.729 g/cm3, μ = 1.228 mm-1, F(000) = 1768, the final R =0.0749 and wR = 0.1580 for 5754 reflections with I ＞ 2σ(I). The Ag atom is coordinated by two N atoms from two bpp molecules in an approximately linear geometry. The Ag(Ⅰ) ions are linked by the bpp molecules to form one-dimensional zigzag chains propagating along the c axis. The Hphth-and nitrate counter-ions are bridged by solvent water molecules through hydrogen bonds to generate a one-dimensional chain extending along the b axis. Electrostatic interactions between cations and anions, extensive hydrogen bonds and π-π interactions are responsible for the three-dimensional supramolecular structure. In the solid state, the compound exhibits blue photoluminescence with the maximum at 436 nm upon excitation at 344 nm.     

A One-dimensional Pseudo-helical Coordination Polymer with 4,4'-(Hexafluoroisopropylidene)bis(benzoic acid)

The title complex [Zn2(hfipbb)2(2,2'-bpy)2]n 1 has been hydrothermally synthesized crystal X-ray analysis reveals that 1 presents a one-dimensional coordination polymer with pseudo-helical chain structure. Two Zn(Ⅱ) atoms in an unsymmetrical unit of 1 aoopt distorted octahedrai and square-pyramidal coordination geometries, respectively, The packing of parallel Crystal data: C54H32F12N4O8Zn2, Mr = 1223.58, monoclinic, space group P21/c, a = 27.557(6), b =16.751(3), c = 11.350(2) (A°), β= 99.21(3)°, V= 5171.5(18) (A°)3, Z= 4, Dc = 1.572 g/cm3, F(000) = 2464,μ= 1.030 mm-1, the final R = 0.0552 and wR = 0.1070 for 6631 observed reflections (I> 2σ(I)).     

Two Cobalt(Ⅱ) Complexes Derived from the Hydrolysis Product of Di-Schiff Base Ligand N,N'-Bis-(1-benzimidazo-2-ylethylidene)-ethane-1,2-diamine: Preparation,Characterization and Crystal Structure of the 6-Coordinate Species [CoL2]X·H2O (X = ClO4-,NO3-)

The reactions of Co(CIO4)2.6H2O and Co(NO3)2·6H2O with the di-Schiff base ligand N,N'-bis-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine (LA) in ethanol have been investigated.The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2](CIO4)2·H2O 1 and [CoL2](NO3)2·H2O 2 as isolatable products (L = N-(1-benzimidazo-2-yl-ethylidene)-ethane-1,2-diamine), where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA.Both complexes were characterized by X-ray crystallography.Crystal data for complex 1: monoclinic, space group P21/c, a = 11.9214(10), b = 23.5828(17), c = 14.0387(12)(A), β= 135.219[4]°,C22H30CI2CoN9O9,Mr = 680.37, V = 2780.1(4)(A)3, Z = 4, Dc = 1.625 g/cm3,μ(MoKa) = 0.876 mm-1, F(000) = 1404,the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections (I＞2σ(I)).Crystal data for complex 2: monoclinic, space group P21/c, a = 18.2162(16), b = 10.0610(6), c = 18.593(2)(A),β=130.099(3)°, C22H30CoN10O7, Mr = 605.49, V = 2606.5(4)(A)3, Z = 4, Dc = 1.543 g/cm3,μ(MoKα)= 0.722 mm-1, F(000) = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections (I ＞ 2σ(I)).X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere.In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4- (or NO3-) groups to form a 3D framework.In complex 2, the strong π-π interactions increase the stability of the structure.     

一个新颖的(5,6)-连接三维超分子网络拓扑结构(英文)

A new complex,[Co(HL)2(H2O)4]·H2O(1)(H2L =5-carboxy-1-carboxymethyl-2-oxidopyridinium),was synthesized and characterized by X-ray single-crystal diffraction,elemental analysis,and IR spectra.The crystal is monoclinic,space group P21/c with a=0.512 69(2) nm,b=2.275 31(1) nm,c=1.003 95(6) nm,β=98.015(3)°,V= 1.159 7(1) nm3,Z=2,Mr=541.29,F(000)=558,Dc=1.550 g·cm-3,μ=0.816 mm-1,the final R=0.044 5 and wR=0.142 1 for 2 015 observed reflections(I2σ(I)).Complex 1 can be considered constructed from 2D layers,which consist of left-and right-handed helical chains and further linked into a 3D supramolecular architecture by hydrogen bonds.Topology analysis reveals that complex 1 shows an unprecedented 3D binodal(5,6)-connected topology.     

Synthesis and Crystal Structure of a Manganese(Ⅱ) Complex with 2-(4'-Chlorine-benzoyl)-benzoic Acid and 1,10-Phenanthroline

A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with a = 12.154(5), b = 18.166(7), c =31.197(13) (A°), V = 6887(5) (A°)3, C80H48C14Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm3, μ(MoKa) =0.591 mm-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.     

Hydrogen-bonded Three-Dimensional Networks Encapsulating One-dimensional Covalent Chains: [Cu(3-ampy)(H2O)4](SO4)·(H2O) (3-ampy = 3-Aminopyridine)

A three-dimensional complex [Cu(3-ampy)(H2O)4](SO4)·(H2O) (3-ampy = 3-aminopyridine) has been synthesized. Crystallographic data: C5H16CuN2O9S, Mr = 343.80, triclinic, space group P, a = 7.675(2), b = 8.225(3), c = 10.845(3) (A), α= 86.996(4), β = 76.292(4),γ = 68.890(4)°, V = 620.0(3) (A)3, Z = 2, Dc = 1.841 g/cm3, F(000) = 354 and μ = 1.971 mm-1. The structure was refined to R = 0.0269 and wR = 0.0659 for 1838 observed reflections (I ＞ 2σ(Ⅰ)). The structure consists of [Cu(3-ampy)(H2O)4]2 cations, SO42- anions and lattice water molecules. 3-Ampy acting as a bidentate bridging ligand generates a 1D covalent chain. A supramolecular 2D framework is formed through π-π stacking of pyridine rings. The lattice water molecules and SO42- anions are located between the adjacent 2D frameworks. The hydrogen bonding interactions from lattice water molecules and SO42- anions to coordinate water extend the 2D framework into a 3D network.     

Solid and Solution Structural Studies of Dimeric and Tetrameric Molybdenum(Ⅵ) Malate Complexes

Reactions of potassium molybdate with racemic malic acid (H3mal = C4H6O5) result in the isolation of two mesomeric molybdenum malate complexes Ks[(MoO2)2O(R-mal)2][(MoO2)2O(S- mal)2]·4H2O 1 and (Him)2K6[(MoO2)4O3(R-mal)2][(MoO2)4O3(S-mal)2]·8H2O 2. Complex 1 belongs to the monoclinic system, space group C2/c with a = 14.8637(3), b = 6.9544(1), c = 19.6783(5) A, β = 100.081(2)°, V= 2002.70(7)A3, Mr = 1452.88, Z= 2, F(000) = 1416, T= 173 K, Dc = 2.409 g/cm3, μ(MoKa) = 2.167, R = 0.0283 and wR = 0.0733.2 is of triclinic system, space group P1 with a = 8.7707(2), b = 9.3310(3), c = 17.9093(7) A, α = 83.781(3), β = 85.626(2), γ= 84.822(2)°, V = 1447.84(8) A3, Mr = 2160.68, Z = 1, F(000) = 1048, T= 173 K, Dc = 2.478 g/cm3, μ(MoKα) = 2.230, R = 0.0234 and wR = 0.0584.1 is the first isolated dinuclear molybdenum(Ⅵ) malato complex in 1:1 molar ratio. The molybdenum atoms in the two complexes are six-coordinated in an approximately octahedral geometry. Two malates coordinate tridentately with the Mo atom via their α-alkoxy, α-carboxy and α-carboxy groups in 1 and 2. β-Carboxy group in 2 further links with the other two Mo atoms to give a tetrameric unit. The solution 1H and 13C NMR spectra indicate that dimeric malate molybdenum in 1 dissociates partly in solution and exists in an equilibrium with tetrameric species, while 2 is stable and retains its tetrameric structure without any dissociation.     

Synthesis and Crystal Structure of μ1,1,3 Formic Bridging 3D Microporous Ni(Ⅱ) Complex

A μ1,1,3 formic bridging Ni2 complex [Ni3(HCOO)6·H2O]]n 1 has been synthesi-zed under hydrothermal conditions. The single-crystal X-ray diffraction analysis shows that 1 exhibits a 3D open microporous tube formed by covalent and coordination bonds. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.1487(13), b = 9.7763(11), c =17.9685(17) A, β= 126.948(6)°, C6H6Ni3O13, Mr = 462.02, V = 1565.2(3) A3 Z = 4, Dc= 1.961 g/cm3, μ = 3.630 mm-1, F(000) = 917.7, Rint = 0.0234, the final R = 0.0234 and wR = 0.0734 for 3469 observed reflections (Ⅰ>2σ(Ⅰ)).     

Synthesis, Crystal Structure and Characterization of the Coordination Polymer [Ni2(2-mpac)4(4,4'-bpy)·2H2O]n

Utilizing mononuclear complex Ni(2-mpac)2(H2O)2 as the molecular building block,a novel coordination polymer [Ni2(2-mpac)4(4,4'-bpy)·2H2O]n (1,2-mpac = 5-methyl-2-pyrazinecarboxylic acid, 4,4'-bpy = 4,4'-bipyridine) was successfully synthesized and structurally characterized by X-ray single-crystal diffraction method. Crystal data: monoclinic, space group C2/c, a = 23.870(1),b = 9.887(4), c = 18.929(9) (A),β= 126.840(5)°, V = 3575(3) (A)3, Z = 4, S = 1.046, μ = 1.594 mm-1,F(000) = 1768 and Dc = 1.127 g·cm-3. The final R = 0.0351 and wR = 0.0792 for 2372 observed reflections with Ⅰ＞ 2σ(Ⅰ) and R = 0.0564 and wR = 0.0938 for all reflections.     

Synthesis and Crystal Structure of a One-dimensional Silver(Ⅰ) Coordination Polymer with 4,4'-Bipyridine

The title compound,{[Ag2(bipy)2(H2O2]·pydc·2H2O}n(bipy=4,4'-bipyridine,pydc=pyridine-3,5-dicarboxylate),has been synthesized by the reaction of Ag2O with pydc and bipy in CH3OH solution.It crystallizes in the monoclinic system,space group C2/c with a=21.419(8),b=7.515(3),c=18.070(7)(A),β=108.273(6)°,Mr=765.27,V=2761.9(17)(A)3,Z=4,Dc=1.840 g/cm3,F(000)=1528,μ=1.478 mm-1,the final R=0.0307 and wR=0.0681.The structure determined demonstrated that the Ag(Ⅰ)is three-coordinated by two nitrogen atoms from bipy and one water molecule,forming a one-dimensional coordination polymer[Ag2(bipy)2(H2O)2]n2n ,which is further linked to generate a two-dimensional layer structure via Ag…Ag attractions.     

A Zn(Ⅱ) 5-Aminoisophthalate Coordination Polymer

The title compound, [Zn(AIP)(4,4-bipy)0.5(H2O)]n·0.75nH2O 1, was synthesized via the hydrothermal reaction of Zn(OAc)2 with 5-aminoisophthalic acid (H2AIP) and characterized by elemental analysis and infrared spectra. The complex crystallizes in monoclinic system, space group P21/c with a = 12.672(1), b = 7.6557(4), c = 16.181(1) (A),β = 109.187(2)o, V = 1482.6(2) (A)3, Z = 1, C52H52N8O23Zn4, Mr = 1418.58, Dc = 1.589 g/cm3, F(000) = 724 and μ(MoKα) = 1.685mm-1. The final R = 0.0702 and wR = 0.1524 for 1847 observed reflections with Ⅰ ＞ 2σ(I), and R = 0.0873 and wR = 0.1664 for all data. X-ray diffraction studies reveal that the title compound has an interesting 2D microporous architecture with guest water molecules inside the channel.     

Syntheses and Crystal Structures of Two Cyano-bridged Bimetallic Complexes [Ln(DMSO)2(H2O)(μ-CN)4Fe(CN)2](Ln= Ce and Eu, DMSO= Dimethylsulfoxide) with Layered Structure

Two new bimetallic cyano-bridged complexes [Ln(DMSO)2(H2O)(μ-CN)4Fe(CN)2] (Ln = Ce 1, Eu 2) have been prepared by the grinding reaction method and structurally characterized by X-ray single-crystal structure analysis. Crystallographic data for 1: C10H14CeFeN6O3S2, Mr = 526.36, monoclinic, P2/n, a = 7.852(4), b = 10.729(5), c = 11.181(5) (A), β = 96.992(8)°, V = 935.0(7) A3, Z = 2, Dc = 1.870 g/cm3, μ = 3.421 mm-1, F(000) = 512, R = 0.0363 and wR = 0.0971; and those for 2: C10H14EuFeN6O3S2, Mr = 538.20, monoclinic, P2/n, a = 7.739(5), b = 10.668(7), c = 11.008(7) A, β = 96.943(3)°, V = 902.1(11) A3, Z = 2, Dc = 1.981 g/cm3, μ= 4.499 mm-1, F(000) = 522, R = 0.0345 and wR = 0.0855. In each complex the lanthanide ion is seven-coordinated in a pentagonal bipyramidal arrangement, and the Fe(Ⅲ) ion is in a nearly regular octahedral environment. The title complexes can be described as two-dimensional (2-D) stair-like structures, which are further connected by hydrogen bonds to form three-dimensional (3-D) frameworks.     

配位聚合物[Mn(4,4′-bpy)_(1.5)(H_2O)_3](ClO_4)·(4,4′-bpy)(L)·H_2O的水热合成和晶体结构(英文)

The title compound, [Mn(4,4'-bpy)1.5(H2O)3](ClO4)·(4,4'-bpy)(L)·H2O(1), where L=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 0(1) nm, α=105.300(2)°, β=97.495(2)°, γ=91.118(2)°, V=1.884 0(4) nm3, Z=2, Mr=780.10, Dc=1.375 g·cm-3, μ=0.483 mm-1, F(000)=812, R=0.055 4, wR=0.135 2. The Mn atoms are octahedrally coordinated by three N atoms of three 4,4'-bipyridine ligands and three O atoms of water. The complex shows a one-dimensional chain structure bridged by water and 4,4'-bipyridine molecules. CCDC: 615707.