Synthesis and Crystal Structure of a Novel Layered Lead(Ⅱ) Carboxylate-sulfonate Compound Templated by 4,4''-Bipyridine

A new lead(Ⅱ) carboxylate-sulfonate has been hydrothermally synthesized and characterized by X-ray single-crystal and elemental analyses. It crystallizes in triclinic, space group P,(1) with a=8.1573(6), b=9.4663(7), c=12.7488(9) (A), α=89.2320(10), β=80.7380(10), γ=77.9760(10)°, Z=2, V=950.10(12) (A)3, Mr=599.57, Dc=2.096 g/cm3, μ=9.032 mm-1, F(000)=572, the final R=0.0412 and wR=0.1035. It has a 1D chain structure, and the Pb(Ⅱ) is six-coordinated. Two PbO6 polyhedra are interconnected via edge-sharing into a two-core unit. Such units are further interconnected by 3-sulfonato-benzoic acids into 1D chains which are linked by hydrogen bonds into a layer structure. The 4,4'-bipyridines are located at the interlayer space and link the layers into a supramolecular structure by π-π stacking interactions.     

Crystal Structure and Characterization of a Binuclear Cd(Ⅱ) Quaternary Coordination Complex [Cd_2(phen)_2Q_2(BP)]_n(phen=1,10-Phenanthroline,BP = Biphenyl-4,4'-dicarboxylic acid,Q=8-Hydroxyquinoline Anion)

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) ,β = 111.3430(10)°,V = 2282.5(5) 3,Z = 4,Mr = 556.85,Dc = 1.620 g/cm3,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.     

Synthesis, Crystal Structure and Band Structure of Sm3In5

A new intermetallic compound, Sm3In5, has been synthesized by solid-state reaction of the corresponding pure elements in a welded niobium tube at high temperature. Its crystal structure was established by single-crystal X-ray diffraction. Sm3In5 crystallizes in orthorhombic, space group Cmcm with a = 10.0137(8), b = 8.1211(7), c = 10.3858(8) , V = 844.60(1) 3, Z = 4, Mr = 1025.15, Dc = 8.062 g/cm3, μ = 33.791 mm-1, F(000) = 1724, the final R = 0.0346 and wR = 0.0775 for 533 observed reflections with I > 2σ(I). The structure of Sm3In5 belongs to the modified Pu3Pd5 type. It is isostructural with La3In5 and β-Y3In5, containing one-dimensional (1D) [In5] cluster chains along the c-axis, which are weakly interconnected via In-In bonds (3.345 ) to form a three-dimensional (3D) structure. The samarium cations are located at the voids between the 1D [In5] cluster chains. Band structure calculations based on Density Function Theory (DFT) method indicate that Sm3In5 is metallic.     

Synthesis,Crystal Structure,Vibrational Spectroscopy,and Thermal Behavior of Y[B_2O_3（OH）]_3

The hydroxy yttrium hexaborate,Y[B2O3(OH)]3,has been synthesized under mild hydrothermal conditions at 458 K.The crystal structure was solved and refined from single-crystal X-ray diffraction.It adopts a trigonal space group R3c(No.161) with a = 8.3942(4),c = 20.6484(12) ,V = 1260.03(12) 3,YB6H3O12,Mr = 348.79,Z = 6,Dc = 2.758 g/cm3,F(000) = 1008,μ = 7.015 mm-1,R = 0.0321 and wR = 0.0772.Its crystal structure is made up of six-membered rings,alternating three-connected [BO3(OH)] tetrahedra and planar [BO3] trigonal groups,which are interconnected with each other by sharing their common oxygen corners to form a three-dimensional framework structure with six-membered ring channels that are occupied by the yttrium atoms and run along the c axis.FT-IR,Raman,and TG-DTA results are also presented.     

Synthesis,Crystal Structure and Band Structure of Tb3Co4Sn（13）

A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.     

Synthesis, Crystal Structure and Characterization of a New Manganese(Ⅱ)Tetracarboxylate

By hydrothermal synthesis,a manganese(Ⅱ)tetracarboxylate [Mn(2,2'-bipyridi-ne)btec)o.5(H2O)]2n(H4btec=1,2,4,5-benzenetetracarboxylic acid)was obtained and characteri-zed by single-crystal X-ray diffraction,IR,elemental analysis and thermogravimetrie analysis.It crystallizes in triclinic,space group P(1),with a=7.721(4),b=8.905(5),c=10.712(6)(A),α=80.899(8),β=70.371(8),γ=78.201(8)°,z=2,V=675.8(7)(A)3,Mr=354.20,Dc=1.741 g/cm3,μ=1.007mm-1,F(000)=360,S=0.956,(△/σ)max=0.000,the final R=0.0490 and wR=0.1262.This compound presents an infinite 1D polymer featuring a double-chain structure.The Mn(Ⅱ)ion is five-coordinated.The four carboxylate groups of btec4- are all deprotonated and coordinated to four Mn atoms in a monodentate fashion,forming a 1D double chain structure with a cavity.Such chains are interconnected by π-π stacking interactions into 2D layers which are further interlinked into a supramolecular structure by hydrogen bonds.     

Synthesis and Crystal and Band Structures of YbCu_6In_6 with 3D Framework

A new intermetallic compound,YbCu6In6,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.YbCu6In6 crystallizes in tetragonal space group I4/mmm with a = 9.2283(5),c = 5.4015(4),V = 460.00(5) 3,Z = 2,Mr = 1243.20,Dc = 8.976 g/cm3,μ = 38.243 mm-1,F(000) = 1076,and the final R = 0.0258 and wR = 0.0602 for 173 observed reflections with I > 2σ(I).The structure of YbCu6In6 belongs to the ThMn12 type.It is isostructural with RECu6In6(RE = Y,Ce,Pr,Nd,Gd,Tb,Dy),containing one-dimensional(1D) [Cu10In6] cluster chain along the c axis,which is interconnected via sharing the Cu(1) atoms to form a three-dimensional(3D) [Cu6In6] framework with Yb atoms encapsulated in the 1D tunnels along the c axis.Band structure calculations based on Density Functional Theory(DFT) method indicate that YbCu6In6 is metallic.     

Synthesis and Crystal Structure of a Novel Compound:[Nd_3(OH)_7(O_2CC_6H_4SO_3)(H_2O)]_n·nH_2O with a Pillar-layered Structure

A novel Nd(Ⅲ) compound,[Nd3(OH)7(O2CC6H4SO3)(H2O)]n·nH2O 1,has been synthesized by the hydrothermal reaction of Nd2O3 and 3-sulfobenzoic acid monosodium salt. It was characterized by IR spectroscopy,elemental analysis,thermogravimetric analysis and single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 13.024(3),b = 10.961(2),c = 12.792(3) ,β = 91.271(3)°,V = 1825.6(7) 3,Z = 4,Mr = 787.97,Dc = 2.867 g/cm3,μ = 8.584 mm-1,F(000) = 1460,S = 1.035,R = 0.0442 and wR = 0.1166 (I 2σ(I)). In this compound,the cross-linkage of Nd atoms by bridging hydroxy groups results in a Nd-O inorganic 200 layer,and such layers are linked by the 3-O3S-C6H4-CO2 dianions into a pillar-layered structure. The lattice water molecules are located in the cavity.     

Structure and Fluorescence Property of a 2D Bilayer Cd(Ⅱ) Coordination Polymer Induced by H-bonding and π-π Interaction

Solvothermal reactions of 4,4'-oxybis(benzoic acid) (H2oba) with 1,3-dipyridyl benzene (1,3-dpb) produced a two-dimensional (2D) cadmium(Ⅱ) coordination polymer {[Cd(oba)(dpb)]·H2O}n (1). The complex 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 = 13.6692(9), b = 25.9647(17), c = 8.7912(6) , α = 125.0370(10), γ = 2544.7(3)°, V = 2544.7(3) 3, C30H22N2O6Cd, Mr = 618.91, Dc =1.609 g/cm3, F(000) = 1248, μ = 0.904 mm-1 and Z = 4. The neighboring Cd(Ⅱ) ions are linked by oba2-anions and 1,3-dpb to form an infinitely 2D wavelike sheet, and two such 2D sheets are interlocked with each other by H-bonding to form a 2D → 2D structure. The adjacent two groups of interlocked structures are further linked to form a bilayer 2D supramolecular network by π-π interactions. In addition, the fluorescence property of 1 was also studied.     

Microwave Synthesis and Crystal Structure of Bis {2- [（2,4-dichloro-phenylimino）- methyl]-4,6-diiodo-phenol}-copper（II）

Bis{2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P2 1 /n with a=14.7558(17), b=20.770(2), c=20.3260(19) , β=90.6110(10)°, V=6229.2(11) 3 and Z=8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.     

Synthesis and Crystal Structure of a New Tetracopper Complex [Cu(H_2O)_3Cu(HCDTA)]_2(ClO_4)_2·H_2O

A new tetracopper complex [Cu(H2O)3Cu(HCDTA)]2(ClO4)2·H2O (CDTA = transcyclohexane-1,2-diamine-N,N,N′,N′-tetraacetate) has been prepared and characterized by singlecrystal X-ray diffraction analysis. The crystal adopts space group C2/c with a = 16.990(10), b = 9.150(5), c = 29.318(17) , β = 104.289(9)°, V = 4417(4) 3, Z = 4, C28H52Cl2Cu4N4O31, Mr = 1265.80, Dc = 1.904 g/cm3, μ = 2.130 mm-1, F(000) = 2584, T = 293(2) K, the final R = 0.0328 and wR = 0.0809 for 4938 observed reflections (I 2σ(I)). The tetracopper units are interconnected by weak covalent bonds into a layered structure.     

Structure and Properties of a New Rare-earth Borate LiSrY_2（BO_3）_3

The structure of LiSrY2(BO3)3 has been solved by single-crystal X-ray diffraction analysis at 298 and 113 K on different diffractometers.It crystallizes in trigonal with space group P-3m1(No.164).The cell parameters at room temperature are as follows:a = 10.3345(9),c = 6.4049(11) ,V = 592.41(13) 3,Z = 3,Mr = 448.81,F(000) = 618,μ = 21.327 mm-1 and Dc = 3.774 g/cm3.The crystal structure consists of gear-like [BY6O33] groups which are linked together by corner-sharing to form a two-dimensional layer parallel to the ab plane.These layers are connected one after another by sharing oxygen atoms with B(2) atoms along the c direction to construct a three-dimensional framework.Li and Sr atoms just occupy the cavities formed by oxygen atoms.In addition,the vibrational spectroscopy of LiSrY2(BO3)3 and photoluminescence properties of the Eu3+ doped LiSrY2(BO3)3 were also studied.     

Urothermal Synthesis and Crystal Structure of a Zn（Ⅱ） Coordination Polymer with a 3-D Supramolecular Structure

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).     

Synthesis and Crystal Structure of a 1D Coordination Polymer: {[Cu(HSSA)(py) 3]·H2O}n (H3SSA=5-Sulfosalicylic Acid, py=Pyridine)

The title compound [Cu(HSSA)(py)3H2O]n (H3SSA = 5-sulfosalicylic acid,py = pyridine) Ⅰ has been synthesized and structurally determined by single-crystal X-ray diffraction. Ⅰ was further characterized by elemental analyses,thermogravimetric analyses,IR and UV-visible spectroscopy. The crystal belongs to the monoclinic system,space group P21/c with a = 9.4564(10),b = 18.2679(19),c = 15.7284(12) ,β = 126.045(4)o,V = 2196.9(4) 3,Z = 4,Dc = 1.618 g/cm3,Mr = 535.02,μ = 1.141 mm-1,F(000) = 1100,λ(MoKα) = 0.71073 ,the final R = 0.0429 and wR = 0.1044 for all observed reflections. In the structure,every two Cu(Ⅱ) atoms are bridged by a bivalent 5-sulfosalicylic anion to form a 1D chain-like coordination polymer. Lattice waters between chains link them to form 2D layers which are further linked by C-H···O hydrogen bonds to form a three-dimensional supramolecular network.     

Synthesis,Structure and Photoluminescent Property of a New 2D Zn（Ⅱ） Coordination Polymer Constructed by Biphenyl-3,3＇,5,5＇-tetracarboxylate

A new 2D Zn(II) coordination polymer,[Zn(btc)0.5(phen)]n(1,H4btc = biphenyl-3,3',5,5'-tetracarboxylic acid,phen = 1,10-phenanthroline),has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis,elemental analysis and IR spectro-scopy.Complex 1 crystallizes in the triclinic system,space group P1 with a = 7.6878(6),b = 10.3453(8),c = 10.9589(9) ,α = 113.3540(10),β = 90.5460(10),γ = 90.4280(10)°,V = 800.09(11) 3,Z = 2,Dc = 1.696 Mg.m-3,μ = 1.566 mm-1,F(000) = 414,the final R = 0.0359 and wR = 0.0778 for 2441 observed reflections with I > 2σ(I).Complex 1 has a 2D layered network containing dinuclear Zn(II) structural units.The 2D layers are further linked by the phen molecules through π-π stacking interactions into a 3D supramolecular framework.The photoluminescent property of 1 was also studied in the solid state at room temperature.     

Synthesis and Crystal Structure of Cis-syn Cyclobutane 1-（Carboxyethyl）thymine Dimer Monopentyl Amide Monotryptophan Methyl Ester Amide

The crystal structure of the title compound (C34H47N7O9, Mr = 697.79) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21 with a = 9.000(8), b = 11.360(10), c = 17.841(15) , β = 97.083(14)°, V = 1810(3) 3, Z = 2, F(000) = 744, Dc = 1.280 g/cm3, μ = 0.094 mm-1, the final R = 0.0721 and wR = 0.1942 for 2479 observed reflections with I > 2σ(I). The two methyl groups attached to the cyclobutane ring are cis oriented. An intramolecular hydrogen bond (N(6)-H(6)…O(8)) introduces rigidity into the title molecule and the crystal structure is stabilized by intermolecular N-H…O hydrogen bonds.     

Two Zinc（Ⅱ） Carboxyarylphosphonates with Unusual Polynuclear Zn（Ⅱ） Units：Syntheses and Crystal Structures

[Zn2(PCP)(phen)(H2O)F]n 1 and {[Zn3(MCP)2(phen)2(H2O)]·2.5H2O}n 2(PCP = p-O2C(C6H4)PO33-,MCP = m-O2C(C6H4)PO33- and phen = phenanthroline) were obtained by hydrothermal synthesis and characterized by X-ray single-crystal diffraction.Compound 1 crystallizes in the monoclinic P21/c space group with a = 7.908(2),b = 20.254(3),c = 13.477(2) ,β = 107.76(3)°,V = 2055.7(8) 3,Z = 4,C20H16FN2O6PZn2,Mr = 561.10,Dc = 1.813 g/cm3,μ = 2.463 mm-1,F(000) = 1128,the final R = 0.0340 and wR = 0.0794.Compound 2 crystallizes in the monoclinic P21/n space group with a = 15.629(3),b = 18.141(4),c = 17.723(7) ,β = 121.89(2)°,V = 4267(2) 3,Z = 4,C40H31N4O13.5P2Zn3,Mr = 1041.70,Dc = 1.620 g/cm3,μ = 1.818 mm-1,F(000) = 2108,the final R = 0.0669 and wR = 0.1775.In compound 1,the tetranuclear Zn4 units are linked together by μ4-PCP3- to build 2D(4,4) layers,which are further interconnected through the μ2-bridging fluorion into a 3D framework with 1D phen ligands-filled channels.As for the 3D supramolecular framework of 2,the novel hexanuclear Zn6 units with "chair" conformation are extended by the moieties of μ4-MCP3- ligand to a 2D(4,4) layer on the bc plane,which is viewed as the 2-folded layers in 1.In both compounds,the structures are stabilized by hydrogen bonding interactions and π-π stacking interactions between the phen rings.Additionally,FT-IR spectroscopy and the fluorescent properties are discussed.     

Synthesis,Structure and Characterization of a Cd(Ⅱ) Polymer Based on 6-Hydroxynicotinic Acid

A new 2D layered Cd(II) coordination polymer,[Cd(HnicO)(phen)(NO3)]n 1(H2nicO = 6-hydroxynicotinic acid,phen = 1,10-phenanthroline),has been hydrothermally synthesized and characterized by elemental analysis,IR,and single-crystal X-ray diffraction.It crystallizes in the monoclinic system,space group P21/c with a = 11.1107(2),b = 13.7639(2),c = 12.1457(4) ,β = 108.695(1)°,V = 1759.40(7) 3,Z = 4,Mr = 492.72,F(000) = 976,Dc = 1.860 g/cm3,μ = 1.289 mm-1,the final R = 0.0205 and wR = 0.0550 for 3663 observed reflections(I > 2σ(I)).X-ray single-crystal structural analyses reveal that in complex 1,the H2nicO ligands and Cd(II) nodes define the structure to be(4,4) 2D nets which are further assembled into the final 3D architecture via supramolecular interactions such as hydrogen bonds and aromatic interactions.Moreover,the solid-state luminescent study shows the title polymer possesses intense luminescent property at room temperature.     

Synthesis and Crystal Structure of a Cu(Ⅱ) Coordination Polymer: [Cu(L)(1,10-phen)]_n

A new complex [Cu(L)(1,10-phen)]n(1, L = N-3-pyridine sulfonyl amino acid) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction analysis, and its crystal belongs to monoclinic, space group P21/c with a = 11.481(2), b = 18.094(4), c = 8.5198(17) , β = 102.26(3)°,V = 1729.5(6) 3, Z = 4, Dc = 1.759 g/cm3, F(000) = 932, μ = 1.422 mm-1, R = 0.0368 and wR = 0.0893. In 1, the Cu(Ⅱ) ion adopts a slightly distorted five-coordinated square pyramidal geometry. The L2- ligand adopts O of the carboxyl bridging adjacent Cu(Ⅱ) units to form an infinite chain structure along the c axis. Also, π-π stacking interactions between the adjacent chains expanded the 1-D structures into a 3-D supramolecular structure.     

Synthesis, Crystal Structure and Catalytic Behavior of 1-Ethyl-3-benyl-imidazolyl Tetranuclear N-Heterocyclic Carbene Silver Bromide

The title complex [Ag(carbene)2]2[Ag2Br4] has been synthesized by the reaction of Ag2O with 1-ethyl-3-benyl-imidazolium bromide in DMSO at room temperature, and characterized by elemental analysis, 1H NMR and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P with a = 10.1597(10), b =11.0646(11), c = 13.0245(14) , α = 102.230(2), β = 90.606, γ = 113.9250(10)o, V = 1300.3(2) 3, Mr = 748.06, Z = 2, Dc = 1.911 g/cm3, μ(MoKα) = 4.60 mm-1 and F(000) = 728. The structure was refined to R = 0.0316 and wR = 0.0835 for 3744 observed reflections with I > 2σ(I). The title compound crystallizes as a centrosymmetric tetranuclear compound. One half of the molecule comprises the asymmetric unit of the structure. The Ag(1) atom is nearly linear or T-shaped when the Ag(1)-Ag(2) interaction is taken into consideration, which is bi-coordinated by two carbene carbon atoms. The Ag(2) atom adopts tetrahedral geometry. The catalytic behavior of the title complex has been investigated, and the results indicate it has a highly catalytic activation for L-lactide polymerization.