Synthesis,Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(IV) Complex with 5-Bromonicotinic Acid

A novel organotin complex [Ph3Sn（C2H5OH）（OCOC5H3NBr）SnPh3（OCOC5H3NBr）] has been synthesized by the reaction of 5-bromonicotinic acid with triphenyltin hydroxide in ethanol and characterized by elemental analysis, IR and ^1H NMR. The crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 15.564（2）, b = 24.975（4）, c = 12.2973（19）°A, β = 92.224（2）°, Z = 4, V = 4776.5（13）°A^3, Dc = 1.596 g/cm^3, μ（MoKα） = 2.765 mm^-1, F（000） = 2264, R = 0.0385 and wR = 0.0667. In the molecular structure of the title complex, the tin atoms are five-coordinated in a trigonal bipyramidal geometry.

Synthesis and Crystal Structural Characterization of a Thiosemicarbazone Derived from 4-Acylpyrazolone

The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocarbonyl hydrazonobenzal）-2,5-dihydro-3-methyl- 1-phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445（4）, b = 11.987（2）, c = 19.249（4） °A,, V= 4256.1（18）°A^3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm^3, T = 296（2） K, F（000） = 1744,μ（MoKα） = 0.186 cm^-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I 〉 2σ（I）. The compound was structurally characterized by elemental analyses, IR and ^1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the （001） plane.

Synthesis and Structural Characterization of 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol

2,3-Bis（hydroxymethyl）-2,3-dinitro-1,4-butanediol（C6H12N2O8） was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324（2）,b = 0.6454（3）,c = 0.7062（3） nm,α= 111.550（4）,β= 95.505（4）,γ= 113.395（4）°,V = 0.23595（16） nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F（000） = 126,R = 0.0304 and wR = 0.0907.

A Novel Dimer──Heteropolytungstate with a Vanadium Atom as the Centre ──Synthesis and Structural Characterization of (H_3O)_4[VW_(12)O_(40)Na(H_2O)_4]_2

A novel dimer tungstovanadate, (H 3O) 4[VW 12 O 40 Na(H 2O) 4] 2, was hydrothermally synthesized and structurally characterized by single crystal X ray diffraction, IR spectra, TGA DSC thermal analysis and polarograpy. The yellowish crystal crystallized in the triclinic system, space group P1, a =1 464 5(3) nm, b =1 468 6(3) nm, c =1 411 1(3) nm, α=111 82(2)°, β=93 17(3)°, γ=117 47(3)°, V =2 210 6(8) nm 3, Z=1, D c=4 552 g·cm -3 , λ (Mo Kα )=0 071 073 nm, μ =31 402 mm -1 , F(000)=2 648, R =0 078 0. The title compound consists of two Keggin structure units linked together with two hydrated sodium cations to form a dimer with a porous structure with the pore dimension of 0 766 nm×0 778 5 nm. [WT5FZ]

Hydrothermal Synthesis, Structural Characterization and Properties of Mixed Valent Decavanadium Oxide [Co_2Cl_8V_(10) O_(18)(H_2O)]Cl_2·6H_2O with Novel Three-dimensional Framework

Decavanadium oxide [Co 2Cl 8V 10 O 18 (H 2O)]Cl 2·6H 2O was synthesized hydrothermally with NH 4VO 3, Na 2MoO 4·2H 2O, H 3PO 4(85%), CoCl 2·6H 2O and hexamethylenetetraamine. The X ray diffraction analysis showed that [Co 2Cl 8V 10 O 18 (H 2O)]Cl 2·6H 2O crystallized in a monoclinic crystal system, the space group was C2/m with cell parameters a =1 6065(3) nm, b =2 2699(5) nm, c =1 3897(3) nm, β = 125.29(3)°, V =4 1363(14) nm 3, Z =2 and the final R =0 06, wR =0 1926. Its crystal structure is a 3 D open framework constructed by VO x polyhedra and CoCl 4 tetrahedra with channels along the crystallographic axes a, b, and c .

Synthesis and Structural Characterization of {[Mn(phen)_2(OAc)(H_2O)]ClO_4}_2H_2O

The crystal structure of the title compound {[Mn(phen)2(OAc)(H2O)]ClO4}2H2O (phen = 1,10-phenanthroline) has been synthesized and determined by X-ray diffraction. The crystal is of triclinic, space group P?with a = 12.7955(4), b = 15.0544(4), c = 16.2183(4) , ?= 64.479(1), b =67.526(1), g = 83.582(1), C52H40Cl2Mn2N8O15, Mr = 1197.70, V = 2600.1(1) ?, Dc = 1.530 g/cm3, F(000) = 1224, = 0.666 cm-1 and Z = 2. The final refinement gave R = 0.0691 and wR = 0.1821 for 6131 observed reflections with I > 2s(I). The cell of the complex contains two uniform mono-manganese molecules [Mn(phen)2(OAc)(H2O)]ClO4 and a solvate water molecule. Four nitrogen atoms from two chelating phenanthroline ligands and one oxygen atom from acetate ligate to the MnⅡ ion, forming a distorted octahedral geometry together with one coordinated water molecule. One ClO4- anion and one water molecule exist outside the cation [Mn(phen)2(OAc)- (H2O)]+ as a counter ion and solvate molecule, respectively.

Hydrothermal Synthesis, Structural Characterization and Proton-conducting Property of a 3-D Framework Based on Zr_3Na_3-Substituted Polyoxometalate Building Blocks

A novel Zr-substituted polyoxometalate（POM） H2K3[Na6（H2O）9][Zr3Na3O3（H2O）3-（GeW9O（34））2]·12H2O（1） has been made under hydrothermal conditions. 1 was characterized by infrared spectrum, thermogravimetric analysis, powder X-ray diffraction and single-crystal X-ray diffraction. Crystal data are： H（50）O（95）Na9K3Ge2Zr3W（1）8, hexagonal space group P63/mmc, a = 15.2251（6）, b = 15.2251（6）, c = 25.035（2） , V = 5025.7（6） 3, Z = 2, Dc = 3.716 mg/m3, μ = 21.648 mm（-1）, F（000） = 4726, the final R = 0.0259 and w R = 0.0647 for 1487 observed reflections with I 2σ（I）. Single-crystal X-ray structure analysis reveals that 1 exhibits a 3-dimensional framework structure based on Zr3Na3-substituted polyanions [Zr3Na3O3（H2O）3（GeW9O（34））2]（11-） and [Na6（H2O）9]（6＋） clusters building blocks. UV-Vis spectrum indicates that 1 is a wide-gap semiconductor. In addition, the proton-conducting property of 1 was also investigated.

Synthesis and Structural Characterization of an Arene-ruthenium Complex [（η^6-p-cymene）Ru（μ-N3） （N3）]2

An arene-ruthenium dimeric complex, [（η^6-p-cymene）Ru（μ-N3）（N3）]2 1, was synthesized from the reaction of [（η^6-p-cymene）Ru（μ-Cl）（Cl）]2 with an excess NaN3 and charac- terized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1^- with a = 8.2321（8）, b = 8.2155（8）, c = 9.9976（11）A, α= 81.786（5）, β= 82.906（5）, γ= 77.134（5）°, V= 649.46（11）A^3, Z= 1, Mr = 638.68, Dc = 1.633 g/cm3,/t（MoKα） = 1.195 mm^-1, F（000） = 320, S = 0.974, the fmal R = 0.0282 and wR = 0.0644 for 2363 observed reflections with I 〉 2σ（I） and 157 variables. The neutral molecule is dimeric with two azide ligands bridging two ruthenium atoms to adopt an octahedral coordination geometry. The average Ru-Nt （terminal） and Ru-Nb （bridge） bond lengths are 2.092（3） and 2.147（2）A, respectively.

Synthesis and Structural Characterizations of a New Lithium Salt for Lithium-ion Batteries

A novel crystal [（CH3O）2CO]3Li2[C2BF2O4]2 was synthesized and fully characterized by FT-IR and single-crystal X-ray diffraction analysis. It crystallizes in monoclinic system, P2Jn space group, with a = 8.1749（2）, b = 10.7449（2）, c = 12.8665（3） A, βl = 94.654（2）°, V= 1126.45（4） A3, Z = 2, Dc = 1.644 g/cm, F（000） = 568, p = 1.498 mm^-1, Mr= 557.77 g/mol, the final R = 0.0334 and wR = 0.0903. The structure analysis revealed that each Li atom is three-coordinated and adopts 1.5 O atoms of two different dimethyl carbonates and one O atom of C2BF2O4-. Thermal stability and infrared spectra analysis were studied and discussed.

Synthesis and Structural Chemistry of Two Novel Transition Metal Organic Phosphonates

Two novel transition metal phosphonate compounds, [Co（H2BDPP）（phen）]n 1 （BDPP = p-O3PCH2（C6H4）CH2PO3, phen = 1,10-phenanthroline） and [Pb3（BCP）2]n 2 （BCP = OOC（C6H4）CH2PO3）, have been synthesized and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in the monoclinic system, space group C2/c with a = 21.169（4）, b = 12.001（2）, c = 7.6211（15）A, β = 98.03（3）°, V= 1917.2（6）A^3, C20H18N2O6P2Co, Mr = 505.22, Z = 8, De= 1.737 g/cm^3, p = 1.107 mm^-1, F（000） = 1020, the final R= 0.0450 and wR = 0.1306 for 2072 observed reflections （I 〉 2σ（I）. Compound 2 crystallizes in the monoclinic system, space group C2/c with a = 4.7167（9）, b = 18.753（2）, c = 22.781（3）A, β = 91.07（3）°, V= 2014.7（14）A^, C8H6O5PPb1.5, Mr = 523.88, Z = 8, Dc = 3.454 g/cm^3, p = 25.222 mm^-1, F（000） = 1856, the final R = 0.0441 and wR = 0.1906 for 2259 observed reflections （I 〉 2σ（I）. In compound 1, the 1D chain running along the c axis is bridged by four ligands （trans- HO3PCH2C6H4CH2PO3H） in four different directions to extend the structure into a three- dimensional network. In compound 2, the Pb（II） displays 4- and 5-coordination modes. There is a one-dimensional P-O-Pb band along the a axis formed by PO3 groups and Pb（II） cations. These bands are joined by μ2-O of -COO to yield two-dimensional inorganic P-O-Pb layers which are pillared by the OOCC6HaCH2PO3 ligands to form a three-dimensional network. Moreover, compound 2 displays a strong emission band attributed to the ligand-centered （LC） transition.

Synthesis and Structural Characterization of a New 3D Lead Coordination Polymer with a Tetrazole-1-acetate Ligand

One new lead coordination polymer, [Pb（tza）2] n （1, Htza = tetrazole-1-acetic acid） has been synthesized under hydrothermal conditions and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis （TGA）, fluorescence spectra and single-crystal X-ray diffraction. Coordination polymer 1 is of monoclinio system, space group C2/c with a = 15.4388（16）, b = 10.4039（11）, c = 8.3360（8） A, β = 119.2070（10）°, V= 1168.7（2） A3, C6H6N8O4Pb, Z = 4, Mr = 461.38, Dc = 2.622 g/cm3,/z（MoKa） = 14.463 mm^-1, F（O00） = 848, the final R = 0.0373 and wR = 0.0904 for 2744 observed reflections with I 〉 20（I）. 1 is a 3D coordination framework built from Pb-carboxylate chains and the tetrazole nitrogen atoms of tza ligands. Furthermore, the luminescent property of 1 has also been investigated.

Synthesis and Structural Characterization of a New Polyoxovanadium Borate: (H_3NCH_2CH_2NH_3)_4[(VO)_6(B_(10)O_(22))_2]·(H_3O)_7

The title compound (H3NCH2CH2NH3)4[(VO)6(B10O22)2]·(H3O)7 1 has been synthe- sized by the hydrothermal method and determined by X-ray crystallography. Crystallographic data: monoclinic, space group C2/c, a = 20.250(4), b = 13.448(3), c = 21.655(4) ?, β = 97.05(3)°, Mr = 851.74 (C4H30.5B10N4O28.5V3), V = 5852(2) ?3, Z = 8, Dc = 1.933 g/cm3, μ = 1.057 mm-1, F(000) = 3436, R = 0.0500 and wR = 0.1442 for 4511 observed reflections with I > 2σ(I). The structure con- sists of [(VO)6(B10O22)2]15- cluster anions that have a central band of six trans-edge-sharing VO5 square pyramids capped by two [B10O22]14- polyborate ligands. Other characterizations are also describ- ed by elemental analysis, IR spectrum and thermal analysis.

Synthesis,Structural Characterization and Properties of Bis(1,5-diamino-1Htetrazolium)3,3'-bis(nitramino)-4,4'-azofurazan

An energetic salt of bis（l,5-diamino-lH-tetrazolium）3,3＂-bis（nitramino）-4, 4x-azo- furazan （C6H10N2206） was synthesized with the total yield of 61.7% by using 3,4-diaminofurazan （DAF） as the starting material. The structure of the title compound was confirmed by NMR, IR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group P21/c with a = 10.739（2）, b = 6.4765（12）, c = 14.138（3） A, fl= 108.787（3）°, V= 930.9（3） A3, Z = 1, Mr= 486.36, Dc = 1.735 g.cm3, μ= 0.15 mm-1, F（000） = 496, R = 0.042 and wR = 0.121. The thermal stability was analyzed by subsequently differential scanning calorimetry （DSC）. And the enthalpy of formation and detonation was calculated theoretically, showing the first decomposition temperature was 142.1℃, the enthalpy of formation was 1614.23 kJ.mol1 and the detonation velocity and detonation pressure were 8.781 km.s-1 and 30.7 GPa, respectively.

Synthesis and Structural Characterization of Bis(2,2'-bpy)bis(azide)cobalt(Ⅲ)nitrate dihydrate

The title complex [CoIII(2, 2?bpy)2(N3)2]種O3?H2O was obtained by an auto-oxidization reaction of cobalt nitrate with 2, 2-bpy and sodium azide in aqueous solution at room temperature, and violet single crystals were prepared in ethanol solution. The structure was determined by X-ray crystallography. The crystal is of triclinic, space group P ?with a = 8.285(4), b = 11.990(8), c = 12.596(7) ? a = 86.630(3), b = 86.280(5), g = 71.130(10)? C20H20CoN11O5, Mr = 553.40, Z = 2, V = 1180.6(12) ?, F(000) = 568, Dc = 1.557 g/cm3, m = 0.784 mm-1, R = 0.0403 and wR = 0.1008. The title complex consists of a [CoⅢ(2, 2?bpy)2(N3)2]+ cation, a NO3- anion and two lattice water molecules. The center CoⅢ ion coordinated by two chelating 2, 2?bpy ligands and two terminal azide groups with a CoN6 coordination environment exhibits a distorted octahedral geometry.

Synthesis and X-ray Structural Studies of 2-(2-Benzofuroylimino)-3-aryl-4-phenyl-1,3-thiazolines

The synthesis for acyliminothiazolines by treatment of N, N□-substituted thioureas with α-bromoacetophenone under aqueous media was described. 2-（2-Benzofuroylimino）-3-aryl- 4-phenyl-1,3- thiazolines were characterized by infrared, NMR spectroscopy and elemental analysis. The single crystals of compounds 4a and 4b were grown by slow evaporation of 80% ethanol solution at room temperature. Compounds 4a and 4b crystallize in triclinic space group P1 and monoclinic space group P21/c, respectively.

Hydrothermal Synthesis, Structural Characterization and Catalysis Property of a Zr-substituted Polyoxometalate Based on [Zr2(μ-OH)2(α-Si W11O39)2]^10- Building Blocks

A new Zr-substituted polyoxometalate（POM） [（CH3）4N]6H2Cs2（H2O）4[Zr2（μ2-OH）2（α-SiW11O39）2]·27H2O（1） was prepared by the reaction of K10[A-α-SiW9O（34）]·25H2O with ZrCl4 in 0.5 mol/L NaAc-HAc（Ac = CH3COO^-） buffer solution（pH = 4.5）. 1 was characterized by elemental and thermogravimetric analyses, powder X-ray diffraction and single-crystal X-ray diffraction. The title compound crystallizes in monoclinic system, space group P21/m with a = 13.1865（16）, b = 20.964（3）, c = 21.432（3） A^°, V = 5923.9（12） A^°3, Z = 2, Dc = 3.833 mg/m^3, μ = 22.175 mm^-1, F（000） = 6116, the final R = 0.0697 and wR = 0.1959 for 10319 observed reflections with I 〉 2σ（I）. Single-crystal X-ray structure analysis reveals that 1 exhibits a one-dimensional chain structure based on sandwiched-type POM anions [Zr2（μ2-OH）2（α-SiW11O（39））2]^10- linked by Cs＋cations. In addition, catalytic tests indicate that 1 provides a sufficient driving force for the conversion from thioethers to sulfoxides/sulfones by H2O2.

Synthesis and Structural Characterization of a Salt {[Co(Phen)_3][Mo_2S_2(μ-S)_2(edt)_2]}_2·(DMSO)_2·(Et_2O)(Phen = 1,10-Phenanthroline, edt=Ethane-1,2-dithiolate)

Reaction of [Et4N]2[Mo2S2(μ-S)2(edt)2] with CoCl2?6H2O and Phen in MeCN followed by recrystallization in DMSO/Et2O gave rise to dark-red block crystals of {[Co(Phen)3]- [Mo2S2(μ-S)2(edt)2]}2?(DMSO)2?(Et2O) 1 (C88H86Co2Mo4N12O3S18). 1 crystallizes in the monoclinic system, space group P21/c with a = 24.631(4), b = 16.117(3), c = 24.791(4) ?, β = 92.835o, V = 9829.3(3) ?3, Z = 4, Mr = 2438.57, Dc = 1.648 g/cm3, F(000) = 4928, μ = 12.61 cm-1, R = 0.0936 and wR = 0.1682 for 12998 observed reflections with I > 2.0σ(I). In the structure of 1, the Co atom of the [Co(Phen)3]2+ dication is octahedrally coordinated by three Phen ligands. The Mo atom of the [Mo2S2(μ-S)2(edt)2]2- dianion is coordinated by two μ-S, one terminal S and two S atoms from edt, forming a distorted square pyramidal geometry. The mean Co–N and Mo…Mo bond distances are 2.139 and 2.872 ?, respectively.

Synthesis and Structural Characterization of [Cu(DMF)6][(η^5-C5Me5)WS3(CuBr)3]2·Et2O

The reactions of [PPh4][(h5-C5Me5)WS3] with four equiv of CuBr in DMF gave rise to a new cluster salt [Cu(DMF)6][(h5-C5Me5)WS3(CuBr)3]2稥t2O 1. The crystal structure of 1 (C42H76N6O7Br6Cu7S6W2, Mr = 2261.40) was determined by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic, space group Pbcm with a = 9.419(1), b = 28.237(1), c = 16.488(3) ? V = 7054.6(8) 3, Z = 4, Dc = 2.129 g/cm3, F(000) = 4332, m (Mo Ka) = 89.46 cm-1 and T = 193 K. With the use of 5746 observed reflections (I > 3.0s(I)), the structure was refined to R = 0.045 and Rw = 0.060. 1 is composed of one [(h5-C5Me5)WS3(CuBr)3]22- dianion, one [Cu(DMF)6]2+ cation and one Et2O solvent molecule. The cluster dianion contains two incomplete-cubane (h5-C5Me5)WS3(CuBr)3 fragments connected by a pair of CuBrCu bridges to form a double incomplete-cubane structure. The range of WCu distance is 2.657(1)~2.677(2) ?in the W2Cu6S6 cluster core.

One-pot Synthesis and X-ray Structure Determination of 7-(Diethylamino)-3-(4-aminophenyl)coumarin

7-（Diethylamino）-3-（4-aminophenyl）coumarin has been synthesized in a new one-pot synthesis by a three-step process starting from 4-（diethylamino）salicylaldehyde and 4-nitrophenylacetonitrile. The product was obtained in a good yield with a high degree of purity and characterized by NMR, IR and HR-MS. The orange crystals of the title compound were grown from ethyl acetate solution. The solid state structure was established by X-ray crystallography analysis. The crystal belongs to the orthorombic system, space group Pccn with a = 11.1095（5）, b = 33.0187（15）, c = 17.2865（7） A, V= 6341.1（5） A3, C19H20N2O2, Mr = 308.37, ρcalc = 1.292 g·cm^-3, = 0.085 mm^-1, F（000） = 2624, the final R = 0.0480 and wR = 0.1265 （I〉 2σ（I））.