New Dimeric Selenidoarsenate(III):Solvothermal Synthesis and Crystal Structure of [Co(en)_3]_2As_2Se_5

A new selenidoarsenate [Co（en）3]2As2Se5 1 （en = ethylenediamine） was synthesized by a reaction of AsCI3, CoCl2-6H2O and Se in en under mild solvothermal conditions, and the structure was determined by single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic system, space group Pbca with a = 15.5092（12）, b = 11.5756（9）, c = 17.8138（14） A, V = 3198.1（4） A^3, Mr= 1023.12, Z = 4, D, = 2.125 g/cm^3,μ = 8.807 mm^-1, F（000） = 1976, S = 1.171, the final R = 0.0591 and wR = 0.1067 for 3170 observed reflections with 1 〉 2σ（I）. 1 consists of isolated dimeric [As2Se5]^4- anion constructed by two corner-sharing AsSe3 trigonal pyramids and transition metal [Co（en）3]^2＋ cations. The optical absorption property and thermal stability of 1 are reported.

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate(Ⅲ) [C_4H_9NH_3]_2Sb_4S_7

An inorganic-organic hybrid thioantimonate（Ⅲ） [CH3（CH2）3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P1 with a = 7.0124（11）, b = 11.919（2）, c =14.879（3）A, α = 108.791（3）, β= 102.441（3）, γ = 92.846（2）°, V= 1140.1（3）A3, Mr = 859.71, Z= 2, Do = 2.504 g/cm^3 ,μ = 5.324 mm^-1, F（000） = 804, S = 1.013, the Final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with Ⅰ 〉 2 σ（Ⅰ）. 1 consists of [C4HgNH3]＋ cations and two-dimensional [Sb4ST]n^2n- anion which is composed of three SbS3 trigonal pyranaids and one SbS4 unit joined by sharing common comers. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]^＋ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.

Solvothermal Synthesis and Crystal Structure of Zn(en)_3B_5O_7(OH)_3

A new polyborate containing ehiral metal-complex Zn（en）3 B5O7（OH）3, where en = ethylenediamine, was synthesizedunder solvothermal conditions and structurally characterized by means of X-ray diffraction analysis. Crystal data： Zn（en）3 B5O7（OH）3, monoclinic, space group P21/c, a =0.8532（72） nm, b =2.3340（5） nm, c = 0.9526（92） nm, β =107. 04（3）°, Z=4, V=1.8140（6） nm^3, Dc =1.694 g/cm^3, p=1.416 mm^-1, F（000） = 960, GOF = 1. 020, R =0. 0276, Rw =0. 0828. There is a chiral Zn（en）3^2＋ complex cation and an isolated B5O7（OH）3^2- group in a Zn（en）3 B5O7（OH）3 molecule. The enantiomer of the chiral complex cation is separated orderly as ,4 and A configurations in the compound and the borate group consists of two B303 cycles linked through a bridging boron atom.

Solvothermal Synthesis,Crystal Structure and Photoluminescence Property of a 3D Lead(Ⅱ)Coordination Polymer Based on Terephthalic Acid

Solvothermal reaction of Pb（NO3）2·6H2O with rigid linear ligand terephthalic acid（H2pta） in N,N-dimethylformamide（DMF） produced a new three-dimensional（3D） lead（Ⅱ）coordination polymer[Pb2（pta）1.5（μ4-OH）（DMF）]n 1,and its structure was characterized by single-crystal X-ray diffraction analyses.In polymer 1,the μ4-OH bridges the nearby lead（Ⅱ） ions into an infinite one-dimensional（1D） chain,and then the organic ligand pta^2- joins the neighbored chains into a 3D structure by two similar connection modes in different configurations.The solid-state photoluminescent studies revealed that 1 exhibits a strong greenish emission mainly originating from ligand-to-metal charge transfer between the delocalized π bonds of the aromatic carboxylate ligand pta^2- and the p orbitals of the Pb^2＋ centers.

Solvothermal Synthesis,Crystal Structure and Antimicrobial Activity of a Novel Imide Nickel Complex [Ni(CH_3CONCOCH_3)_2·2(H_2O)]

A novel imide nickel complex [Ni（CH3CONCOCH3）2·2（H2O）] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl imide in enol form during the formation process of the title complex.The complex was characterized by elemental analysis,IR spectrum and X-ray single-crystal diffraction analysis.It crystallizes in the orthorhombic system,space group Pbca with a = 7.4503（7）,b = 13.1089（12）,c = 14.1303（14）,V = 1380.0（2）3,Dc = 1.420 g/cm3,Mr = 294.94,Z = 4,F（000） = 616,μ = 1.422 mm-1,the final R = 0.0487 and wR = 0.1482.The four-coordinated nickel（II） center is surrounded by 4O atoms from two imide ligands and has a distorted square planar geometry.The complex is connected to form a supramolecule with an infinite three-dimensional network through intramolecular and intermolecular hydrogen bonds.Antimicrobial activity was investigated by agar diffusion method,and the result showed that the complex was active against coli bacillus,staphylococcus aureus and bacillus subtilis.The thermal stability of the title complex was also studied by TG-DTA method.

Solvothermal Synthesis,Crystal Structure and Optical Property of Lanthanide Selenidostannate [{Tb(en)_3}_2(μ-OH)_2]Sn_2Se_6 with a 3-D H-bonded Network

An inorganic-organic hybrid lanthanide selenidostannate [{Tb（en）3}2（μ-OH）2]Sn2Se6（1） was synthesized by the solvothermal method.1 crystallizes in the monoclinic system,space group P21/n with a=10.120（2）,b=11.781（3）,c=15.403（3）,β=99.534（5）°,V=1811.1（7）3,Mr=1423.62,Z=2,Dc=2.611 g/cm3,μ=11.281 mm-1,F（000）=1312,S=1.101,the final R= 0.0400 and wR=0.0853 for 3242 observed reflections with Ⅰ 〉2σ（Ⅰ）.1 consists of a [Sn2Se6]4-and a [{Tb（en）3}2（μ-OH）2]4＋ ions.The [Sn2Se6]4-anion is constructed by two SnSe4 tetrahedra sharing a common edge.The binuclear [{Tb（en）3}2（μ-OH）2]4＋ complex is composed of two [Tb（en）3]3＋ ions joined by two μ-OH bridging ligands.The Tb3＋ ion lies in an eight-coordinated bicapped trigonal prism.In 1,the [Sn2Se6]4-and [{Tb（en）3}2（μ-OH）2]4＋ moieties are connected into a 3-D network via N-H···Se and O-H···Se H-bonds.

Solvothermal Synthesis and Characterization of [TM(1,2-dap)3]HgSb2Se5(TM = Co,Fe)with a Chain Structure

One organic-decorated quanternaery [TM（1,2-dap）3]Hg Sb2Se5（1,2-dap = 1,2-dianinopropane, TM = Co（1）, Fe（2）） compound has been solvothermally synthesized. The compounds crystallize in triclinic space group P 1, with a = 11.248（6）, b = 11.542（7）, c = 12.180（12） A, V =1268.7（16） A^3, Z = 2, F（000） = 1010 for 1 and a = 11.311（5）, b = 11.558（5）, c = 12.180（9） A, V =1276.5（12） A^3, Z = 2, F（000） = 1008 for 2. The crystal structure consists of one-dimensional anionics chains composed of Hg Se4 tetrahedra and SbSe3 trigonal pyramids sharing corners and[TM（dap）3]^2＋ cations. The [HgSb2Se＋5^2-]∞ anionic chains run along the [001] direction, and are surrounded by the [TM（dap）3]^2＋ cations. Meanwhile, 8-ring [Hg2Sb2Se4] and 6-ring [HgSb2Se2] are alternately found. The compounds were structurally characterized by elemental analysis,thermogravimetric analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy.

Solvothermal Synthesis and Characterization of (NH_3CH_2CH_2NH_3)HgSnS_4 with a Column Structure

A compound （NH3 CH2 CH2 NH3 ）HgSnS4 with a column structure was synthesized solvothermally and characterized by X-ray single-crystal diffraction. This compound crystallizes in the monoclinic space group C2/c with a = 1. 3863 （6） nm, b = 0. 6640 （ 3 ） nm, c = 2. 3198 （10） nm, β = 106. 168 （ 7 ）° and Z = 8. It consists of anionic columns of [ HgSnS4 ]^2- that are interrupted by cationic columns of [ EnH2 ]^2＋ . Its thermal and optical properties were studied.

Solvothermal Synthesis and Structure Characterization of a 3D Hydrogen-bonded Copper Compound [Cu(H_2dhpmc)_2]·2H_2O

The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes in monoclinic system, space group P21/c with a = 5.0497(9), b = 10.0196(6), c = 13.715(2) ? b = 96.237(1)? V = 689.8(2) 3, Z = 2, Dc = 1.973 g/cm3, ?= 1.654 mm-1, F(000) = 414, R = 0.0736 and wR = 0.1351. Each Cu(Ⅱ) is coordinated to four oxygen atoms of two 2, 4-dihydroxypyrimidine-5-carboxylic acid ligands in the equatorial position and two oxygen atoms of two water molecules in the axial position to form an axially elongated octahedral geometry. The title complex is further linked into a three-dimensional structure through the weak interactions of hydrogen bonds between the oxygen atoms and the nitrogen atoms.

Synthesis and Crystal Structure of a Magnesium Metal-organic Framework

A magnesium metal organic framework, [N-H2（CH3）2][-N（CH3）4][Mgs（bpdc）3（O2CH）6]· 3H2O （1, bpdcH2 = 4,4＇-biphenyldicarboxylic acid）, has been solvothermally synthesized and structurally characterized. 1 crystallizes in the trigonal system, space group R-3, with a = 11.3427（3）, c = 41.5662（18） A, V = 4631.3（3） A^3, Z = 3 and the final R = 0.0457. Its structure features a pillared-layered three-dimensional network with 8.21 A cavities, in which cationic [NH2（CH3）2]^＋ or [N（CH3）4]^＋ and lattice water molecules are located. Thermal stability of the title compound has also been investigated.

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates:C_4H_(10)N_2·B_6O_8(OH)_2 and (NH_3CH_2CH_2NH_3)B_5O_8(OH)

Two new borate compounds, C4H10N2·B6O8（OH）2 and （NH3CH2CH2NH3）B5O8 （OH）2, have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction, IR, elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system, space group P21/c, with a = 8.3318（17）, b = 6.2118（12）, c = 12.479（3） A, β = 108.96（3）°, V = 610.8（2） A^3, Mr = 313.02, Z = 2, 13,.= 1.702 g/cm^,/J = 0.150 mm^-1, F（000） = 320, R = 0.0387 and wR = 0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system, which are built up from alternative B6O8（OH）2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic, space group Co, with a = 6.7207（13）, b = 11.481 （2）, c = 12.564（3）A,β = 95.25（3）°, V = 965.4（3） A^3, Mr = 261.18, Z = 4, Dc = 1.797 g/cm^3,/t = 0.164 mm^-1, F（000） = 536, R = 0.0396 and wR = 0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.

Solvothermal Synthesis and Crystal Structure of a Novel Inorganic-Organic Hybrid Material, Fe_2O(OH)(C_5H_4NCOO)SO_4

A novel inorganic organic hybrid material, Fe 2O(OH)(C 5H 4 ~NCOO)SO 4 was synthesized via solvothermal route using a reaction of FeCl 3·6H 2O, KCNS, and 4 cyanopyridine in aqueous solution of H 2O 2 and ethanol at 130 ℃ for 3 d. The compound crystallized in monoclinic space group P 2 1, with cell parameters a =0 73850(15) nm, b =0 65100(13) nm, c =1 0546(2) nm, β =90 36(3)°, V =0 50700(18) nm 3 and Z =2. The structure is constructed with inorganic layered [Fe 2O(OH)SO 4] + cations linked by organic (C 5H 4NCOO) - anions. The compound is thermally stable up to approximately 240 ℃.

Solvothermal Synthesis, Crystal Structure and Property of a Three-dimensional Fe(Ⅱ) Complex: [Fe(INAIP)(DMF)]_(n)·0.5nDMF

A Fe-based metal-organic framework, [Fe(INAIP)(DMF)]_(n)·0.5nDMF(1), has been synthesized by the reaction of 5-(isonicotinamido)isophthalic acid(H_(2)INAIP) with FeSO_(4)·7H_(2)O under DMF reaction solvent. Single-crystal X-ray diffraction analysis indicates that complex 1 displays a two-fold interpenetrated three-dimensional(3D) framework with sra topology. The TG, magnetic and adsorption properties of the complex were also studied.

Synthesis and Crystal Structure of a Puckered Rhombus Grid-like Coordination Polymer with Bridging Ligand Containing Sulfanyl Linker

A new coordination polymer with sulfide moieties, [Co(ptmb)2]·0.25H2O (ptmb=4-(4-pyridylthiomethyl)-benzoate), was synthesized by self-assembly of Co(NO3)2·6H2O with Hptmb under solvothermal conditions. X-ray single crystal diffraction study shows that it is a 2D layer structure consisting of puckered rhombus grid with di-mensions 1.175 nm×1.110 nm.

Synthesis, Crystal Structure, Vibrational Spectroscopy and Thermal Behavior of the First Alkali Metal Hydrated Hexaborate： K2[B6O9（OH）2]

New hydrated potassium hexaborate K2[B6O9（OH）2] has been synthesized under mild solvothermal conditions. The structure was determined by single-crystal X-ray diffraction and further characterized by FT-IR, Rarnan spectra and DTA-TG. It crystallizes in the monoclinic system with space group P21/n, a=0.9036（2） nm, b=0.66052（18） nm, c=1.5997（4） nm, β=91.862（4）°, V=0.9543（4） nm^3 and Z=4. Its crystal structure consists of K-O polyhedra and 1-D stepped polyborate chains constructed by new [B6O9（OH）2]2- fundamental building blocks. 1-D polyborate chains contain 3,8-membered boron rings. Adjacent chains are further linked via H-bonding interactions into 2-D layers. The K^＋ cations reside not only between the layers but also in the 8-membered boron rings of the chains, compensating the negative charges of the borate chains and holding the layers together into the 3-D structure through bonding with oxygen atoms of the chains.

Synthesis,Crystal Structure and Luminescent Properties of a Nd(Ⅲ) Complex Constructed from 2-Pyridyl-4,5-imidazoledicarboxylic Acid

A new Nd（Ⅲ） coordination polymer [Nd（pidc）（H2O）4]·pidc-·7H2O（1,pidc2-= 2-py-ridyl-4,5-imidazoledicarboxylate） has been synthesized by solvothermal reaction at 120 ℃ and structurally characterized.The complex belongs to triclinic,space group P with a = 9.022（2）,b = 13.731（3）,c = 13.782（3） ,α = 70.87（3）,β = 71.71（3）,γ = 71.71（3）,V = 1488.6（7） 3,Z = 2,Dc = 1.798 g/cm3,S = 1.04,μ = 1.839 mm-1,F（000） = 814,Mr = 805.76,Rint = 0.081 and wR = 0.1644 for 5242 observed reflections（I 〉 2（I））.Each Nd3＋ ion is nine-coordinated by five O atoms from three pidc ligands,and four O atoms from lattice water molecules.Each pidc is coordinated to three Nd3＋ ions with a μ3-κO：κO＇：κO＂,κO＇＂-μ2 coordination mode into 1D chains,which can be further built into a 3D framework through intermolecular N-H···O and O-H···O hydrogen bonds.Photolu-minescent studies have shown that 1 exhibits emission at 439 nm（λex = 395 nm）.

A Chinese Lantern-like 2D Cu(Ⅱ) Coordination Polymer Constructed by Bis-imidazole and Dicarboxylate Co-ligands: Synthesis, Crystal Structure and Photocatalytic Activity

A new Cu(II) coordination polymer, {[Cu(1,3-BIP)(TFBDC)]·DMF}n(1,1,3-BIP is a 1,3-bis(imidazole)propane, and H2TFBDC is 2,3,5,6-tetrafluoroterephthalic acid) was prepared under solvothermal conditions and characterized by single-crystal and powder X-ray diffraction, IR spectra, thermogravimetric analyses and elemental analyses. The single-crystal X-ray diffraction reveals that metal coordination polymer 1(MCP 1) shows a two-dimensional sheet layer structure, which is further reinforced through strong intermolecular hydrogen bonding to form a 3 D supramolecular framework. Furthermore, the photocatalytic experiment result indicates the degradation ratios of methyl orange(MO) reach 83.4% within 180 minutes when MCP 1 acts as catalyst.

Hydrothermal Synthesis, Crystal Structure and Optical Properties of [M（en）3]（ndt）·H2O （M=Ni^Ⅱ, Co^Ⅱ, Mn^Ⅱ and ndt= 1,5-Naphthalenedithiolate）

Three novel compounds [Ni（en）3]（ndt）·H2O （1）, [Co（en）3]（ndt）·H2O （2） and [Mn（en）3]（ndt）·H2O （3） （en= ethylenediamine, ndt= 1,5-naphthalenedithiolate） have been synthesized under hydrothermal conditions, The structures were characterized by single crystal X-ray diffraction and all belong to monoclinic space group Cc. The [M（en）3]^2＋ cations （M=Ni^Ⅱ, Co^Ⅱ, Mn^Ⅱ）, ndt anions and crystallized water molecules assemble an iso-structural three-dimensional network through H-bonding interactions. Optical absorption properties and band gaps of such three compouds were determined with UV/Vis/NIR diffuse reflectance spectra.

Syntheses,Crystal Structures and Photoluminescence Properties of Two Cadmium(Ⅱ)Coordination Polymers

The solvothermal reaction of CdCl2·2.5H2O with terephthalic acid yields two new three-dimensional(3D)cadmium(II)coordination polymers(CPs),namely{[Cd(C8H4O4)Cl]·C2H8N}n and[Cd(C8H4O4)]n,we use the abbreviations CP1 and CP2 to refer to them,respectively.The compounds are characterized in detail by single-crystal X-ray diffraction,powder X-ray diffraction,IR spectroscopy,elemental analysis and thermogravimetric analysis(TGA).The results indicate that compounds CP1 and CP2 are 3D frameworks,and both the compounds feature a uninodal 4-connected framework with a dia net.The empty spaces of such 3D framework are filed by the other two identical frameworks,leading to a 3-fold interpenetrated network.In addition,the photochemical properties of the frameworks are also investigated.The two frameworks show strong solid-state fluorescence emission at 463 and 503 nm,respectively,which are obvious red-shift compared to the emission of ligand.

Three Two-dimensional Heterometallic Chalcogenides[TM(tren)][InSbSe_3S](TM = Fe, Co, Mn): Syntheses,Crystal Structures, and Properties

Three two-dimensional(2-D) heterometallic chalcogenides [TM(tren)][InSbSe_3S](TM = Fe(1), Co(2), Mn(3); tren = tris(2-aminoethyl)-amine) have been solvothermally synthesized in this paper. Single-crystal X-ray analysis indicates that they are isostructural to each other except the different transition metal ions. These compounds contain an unsaturated complex cation [TM(tren)]^(2+), which can be further coordinated by the 2-D [InSbSSe_3]_n^(2n-) anion, resulting in a new neutral organic-decorated heterometallic chalcogenide. These compounds crystallize in monoclinic space group P21/c, with a = 11.768(12), b = 13.884(14), c = 11.095(11) ?, Z = 4, D_c =2.910 Mg·m^(-3), F(000) = 1304, M_r = 707.60 for 1; a = 11.843(9), b = 14.064(10), c = 10.979(8) ?, Z= 4, Dc = 2.875 Mg·m^(-3), F(000) = 1308, M_r = 710.68 for 2; a = 11.969(10), b = 14.191(11), c =11.112(9) ?, Z = 4, D_c = 2.779 Mg·m^(-3), F(000) = 1300, Mr = 706.69 for 3. The maximum and minimum peaks of compounds 1～3 are 6.996 and –2.880 e·?^(-3), 2.242 and –3.066 e·?^(-3), 3.655 and –3.569 e·?^(-3), respectively. These compounds were structurally characterized by powder X-ray diffraction measurement, thermal analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy. A solid-state UV/Vis reflectance spectroscopy measurement on 1, 2 and 3 confirmed that these compounds are semiconductor materials.