Synthesis and Stuctural Characterization of the Complex [Et4N]2[Ni（C2S

The heteroleptic dmit complex [Et4N]2[Ni2(C2S4)(C3S5)2] has been prepared by the reaction of NiCl2.H2O with Na2dmit, NaSC2H4OH in the MeOH solution. The compound has been characterized by X-ray diffraction study, IR and UV-Vis spectroscopy. Crystallographic data : space group: P21/n, a=11.843(2), b=11.079(1), c = 15.404(1)(), β=110.33(1)°, V = 1895.1()3, Z=2, Dc=1.62 g/cm3, μ=17.6 cm-1, F(000)=956, R=0.052, Rw=0.061. In the structure of the title complex, the tto (tto=tetrathioxalato) ligand in bridging form is chelated to two nickel atoms and dmit (dmit=1,3-dithiole-2-thione-4,5-dithiolate) ligands coordinated to nickel atoms.     

三维超分子化合物[Ag4(L)4](PMBS)4·2H2O的合成、晶体结构和荧光性质

The title compound,[Ag4(L)4](PMBS)4·2H2O (1),where L=2,5-bis (4-pyridyl)-3,4-diaza-2A-hexadiene,PMBS =p-methylbenzenesulfonate was synthesized and its crystal structure was determined by X-ray diffraction structure analysis.The crystal is of triclinic,space group P1 with a=0.820 3(2) nm,b=1.3227(3) nm,c=2.0610(3) nm,α=76.155(2)°,β=78.651 (4)°,γ=89.993(3)°,V=2.126 2(8) nm3,Z=2,Dc= 1.644 g·cm-3,F(000)= 1068,R=0.052 4,wR=0.113 6.The Ag atoms are linear coordinated by two N atoms of two L ligands,while the p-methylben-zenesulfonate molecules are included in the lattice and connected to [Ag(L)]n by hydrogen bonding interactions to form a three-dimensional supramoleculur structure.CCDC:727587.     

Synthesis, Crystal Structure and Fluorescent Property of One New Complex [Na2（2-benzoylbenzoato）4（Phen）2（H2O）2]·H2O

One binuclear sodium(Ⅰ) complex [Na2(2-benzoylbenzoato)4(Phen)2(H2O)2]·H2O has been synthesized with 2-benzoylbenzoic acid and 1,10-henanthroline as ligands. The crystal structure was determined by X-ray diffraction. The crystal belongs to the triclinic system with space group P , a = 1.08096(8), b = 1.09619(8), c = 1.09740(8) nm, α = 79.0600(1), β = 71.0450(1), γ = 62.0540(1)o, V = 1.08533(1) nm3, Dc = 1.421 g/cm3, Z = 2, F(000) = 484, GOOF = 1.036, the final R = 0.0363 and wR = 0.0961. The crystal structure shows that two neighboring sodium(Ⅰ) ions are linked together by two bridging water molecules, and each end position is coordinated with one 1,10-phenanthroline molecule and one 2-benzoylbenzoato to form a binuclear structure. Each sodium(Ⅰ) ion in the molecule is coordinated with five atoms to give a distorted trigonal bipyramid. The fluorescence property of the title complex is also discussed.     

苯四甲酸桥连的镍配合物[Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O的合成及结构

At room temperature, a coordination polymer [Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O was synthesized by reaction of NiCl2·6H2O, 1,2,4,5-benzenetetracarboxylic dianhydridc and imidazole in a water/THF solution. The structure was determined by X-ray diffraction crystal structure analysis. It crystallizes in triclinic P1 space group with the crystal cell parameters of a=0.67542 (2) nm, b=1.000 14 (1) nm, c=1.09088 (3) nm, α=74.140(2)°, β= 74.388(1)°, y=73.239(2)°, and V=0.664 09(3) nm3, Z=1. The crystal structure shows that Ni1 atom is coordinated by four water and two imidazole molecules, while Ni2 is coordinated by four water molecules and two carboxyl oxygen atoms. The 1,2,4,5-benzenetetracarboxylate ions bridge Ni2 coordination centers to form one-dimensional chain structure. Moreover, the chains are further linked together by hydrogen bonds to form a two-dimensional network. CCDC: 295873.     

一维链状配位聚合物[Cu(CH3COO)(C5H5N)2]n的合成与晶体结构

The coordination polymer [Cu(CH3COO)(C5H5N)2]n was synthesized and its crystal structure has been determined by X-ray diffraction technique.The crystal belongs to monoclinic,space group C2/c with a=1.183 2(1) nm,b=1.512 1(2) nm,c=1.3911(1) nm,β=97.137(3)°,V=2.469 6(4) nm3,C12H13CuN2O2,Mr=280.78,Z=8,Dc=1.510 g·cm-3,μ=1.759 mm-1,F(000)=1 152,R1=0.048 2 and wR2=0.122 5 for 1 515 observed reflections [1>2σ(Ⅰ)].In the crystal the copper(Ⅲ) atom is tetra-coordinated primarily by two oxygen atoms of two symmetry-related carbexyl groups of acetate anions and two nitrogen atoms of two pyridine ligands in a parallelogram fashion.All of the pyridine rings linked to Cu(1) and Cu(2) are arranged centrosymmetrically on Cu(1).The neighboring copper complex molecules are linked together by the carboxylate oxygen atom of acetate anions to form an infinite one-dimensional linear chain structure.Moreover,π-π stacking interactions between intrachain pyridine molecules play the crucial role in constructing of the supramolecular structure.CCDC:709977.     

METAL CLUSTERS SYNTHESIZED BY SOLID STATE REACTION——PREPARATION AND CRYSTAL STRUCTURE OF TWO MIXED METAL CLUSTERS,Ni_2Nb_2Te_4(Ⅰ) AND Ni_2Ta-2Te_4(Ⅱ)

The two title compounds obtained by solid state reaction at high temperature were char-acierized as isomorphism by single--crystal X--ray diffraction. The space group of both crys-tals is C_(2v)~4-Pma2, with lattice constants a = 7.955(1), b=6.258 (1), c=7 .203(2)A forI, and a =7.914 (1), b=6.237 (1), c=7.236 (1) ? for Ⅱ, Z=2. The structures were de-termined by normal method and refined to the final R = 0.074 and 0.083, respectively. Theresults show that the structure may be regarded as building by cluster unit with formulaNi_2M_2Te_4 (M =Nb or Ta) in which two Ni atoms and two M atoms form a rhombus, whilethe Te atoms are distorted tetrahedrally coordinated with both kinds of metal atoms. In thecluster unit there exist interactions between Ni atoms as well as between Ni and M atoms.In addition, all the cluster units are linked together not only by bridging Te atoms, but alsoby weaker metal-metal interactions, so as to form two--dimensional network. Therefore, thestructure may be represented by the for     

RESEARCH ON TRINUCLEAR MOLYBDENUM CLUSTER COMPOUNDS——CRYSTAL AND MOLECULAR STRUCTURE OF (Et_4N)_2[Mo_3(μ_3-O)(μ_3-Cl)(μ_2-Cl)_3Cl_6]·EtOH

The title crystal belongs to the monoclinic system. The space group is P2_1/c with unit cell parameters: a=11.379(3), b=20.766(2), c=14.487(3), β=91.49(2)°, V=3519(2)~3Z=4, D_c=1.819g.cm~(-3), D_0=1.81g.cm~(-3). The crystal structure was solved by the heavy atom method and difference Fourier synthesis and refined by the full-matrix least-squares to a final R factor of 0.040 based on 3261 unique reflections with intensities I≥3σ(I). The structure consists of two sots of tetraethylammonium cations and trinuclear Me cluster anions. In the cluster anion the three Mo atoms form an isosceles triangle with Mo-Mo distances of 2.601(1), 2.608(1), 2.642(1), respectively, showing a strong bonding interaction between the metal atoms. One μ_3-O atom and one μ_3-Cl atom are situated above and below the triangle respectively, binding the three Me atoms to form a triangular bipyramidal cluster core. Each pair of Mo atoms is bridged further by a μ_2-Cl atom situated on the Mo_3 triangular plane. In addition, each     

Two Alkali Metal Germanophosphates Na3[Ge(OH)(PO4)2]·2H2O and Li2Na[GeO(HPO4)(PO4)]:Crystal Structures and Thermal Stability

Two new alkali metal germanophosphates,namely,Na₃[Ge(OH)(PO₄)₂]·2 H2 O and Li₂Na[GeO(HPO₄)(PO₄)],have been prepared by solvothermal method,and their crystal structures were determined by single-crystal X-ray diffraction.The title two compounds crystalize in the same orthorhombic space group Pbcm(No.57)and feature similar chain-like structure which is built from zig-zag GeO₆ octahedral thread loop branched by PO₄ tetrahedra.For Na₃[Ge(OH)(PO₄)₂]·2 H₂O,a=10.1650(9),b=13.1975(12),c=6.9751(7)?,V=935.73(15)?³,Z=4,R=0.0356 and wR=0.1109;and for Li₂Na[GeO(HPO₄)(PO₄)],a=6.9855(5),b=14.5809(18),c=6.6620(5)?,V=678.56(11)?³,Z=4,R=0.0286,and w R=0.0762.The partial substitution of Na ions by Li ions not only significantly influences the total structural features and the water molecule contents,but also impacts on their thermal stabilities.Li₂Na[GeO(HPO₄)(PO₄)]is thermally stable up to 400℃,whereas only 150℃ for Na₃[Ge(OH)(PO₄)₂]·2 H2 O.     

Synthesis and Crystal Structure of [Mn（DPMT）2Cl2（H2O）2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

CRYSTAL AND MOLECULAR STRUCTURE OF μ-ACYL Fe-S COMPLEX (μ-C_2H_5S)[μ-CO-C(CH_3 )=CH_2]Fe_2(CO)_6

<正> The crystal and molecular structure of(u-C2H5S)[μ-CO-C(CH3)-CH2]Fe2(CO)6, Mr = 409.958 has been determined by X-ray diffraction method. Crystals of this complex are monoclinic, belonging to space group P21/c, and the cell parameters are a = 9.191(1), b = 9.666(1), c = 18.47(2)A,β=98.71(1)° V= 1621.9A3,Z=4,Dc=1.68g/cm3.Thg final R and Rw equal 0.058 and 0.089 for 1948 observed unique reflections. The acyl and ethyl-thio groups are bridged to two iron atoms to form an envelope type of structure. The bond lengths of Fe(1)-0(1), Fe(2)-C(1), Fe(l)-S, Fe(2)-S, Fe(l)-Fe(2) involved in the envelope structure are 1.992, 1.980, 2.260, 2.242 and 2.552A, respectively.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

Synthesis and Crystal Structure of Sm Cu7.73In3.27: a New 3D Framework Based on [Cu5In4M4]（M=Cu/In） Cluster

A new intermetallic compound, SmC u7.73In3.27, has been synthesized by solid-state reaction of the corresponding pure elements at high temperature, and structurally characterized by single-crystal X-ray diffraction study. SmC u7.73In3.27 crystallizes in tetragonal space group P4/mbm with a = 8.6213(4), c = 10.2538(9), V = 762.13(8) A3, Z = 4, Mr = 1018.90, Dc = 8.880 g/cm3, μ =38.244 mm-1, F(000) = 1789, and the final R = 0.0374 and w R = 0.0836 for 514 observed reflections with I 2σ(I). The structure of SmC u7.69In3.31 belongs to a new structure type and features a three-dimensional(3D) [Cu5In2M4](M = Cu/In) framework composed of [Cu5In4M4] clusters interconnected via sharing In atoms as well as Cu–In and In–In bonds. The Sm atoms are located in the one-dimensional(1D) tunnels along the c-axis. The structural relationship of the title compound with other similar Sm-Cu-In phases was also studied. Band structure calculations based on Density Functional Theory(DFT) method indicate that SmC u7.69In3.31 is metallic.     

Synthesis and Crystal Structure of 4,5-Bis（2-chloroethylthio）phthalonitrile

A novel phthalonitrile compound,[C12H10Cl2N2S2],has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 10.6417(8),b = 7.5737(6),c = 18.2758(14),β = 105.2480(10)°,Mr = 317.24,V = 1421.12(19)3,Z = 4,Dc = 1.483 g/cm3,F(000) = 648,μ = 0.733 mm-1,R = 0.0173 and wR = 0.2183.In the structure,the C atoms of the aromatic ring,the two cyanide groups and the two S atoms are almost coplanar(maximum deviation from the mean plane = 0.049(7) ).Two potential weak intermolecular interactions of C-H…N and one type of π…π stacking interaction with a centroid-centroid separation of 3.751(8) stabilize the crystal structure.     

丙酮酸异烟酰腙四核有机锡配合物的合成、表征及{[nBu2Sn(C9H8N3O3)O]SnBu3n}2的晶体结构

The tetranuclear alkyltin(Ⅳ) compounds {[R2Sn(C9H8N3O3)O]SnR3}2 [R=n-Bu (1), 4-CNC6H4CH2 (2),C6H5CH2 (3), 4-ClC6H4CH2 (4)] were prepared by the reaction of Schiff base ligand pyruvic acid isonicotinyl hydrazone with (R3Sn)2O in the corresponding molar ratio of 1:1. All compounds have been characterized by elemental analysis, IR and ^1H NMR spectra. The crystal structure of compound 1 was determined by X-ray single crystal diffractional analysis. This compound exhibits a dimeric structure containing distannoxane units with two types of the tin atoms. For the first tin atom, it appears to be seven-coordinated with a distorted pentagonal bipyramid geometry, and the other is five-coordinated with a distorted trigonal bipyramidal geometry. The molecules are packed in the unit cell in two-dimensional network structure through an interaction between the N atoms of the pyridine and the tin atoms of an adjacent molecule.     

Reduced graphene oxide doping flower-like Fe7S8 nanosheets for high performance potassium ion storage

Finding easy-to-operate strategy to obtain anode material with well-designed structure and excellent electrochemical performance is necessary to promote the development of the future potassium-ion batteries(PIBs).In this work,we synthesized reduced graphene oxide doping flower-like Fe₇S₈ nanosheets electrode materials using one-step hydrothermal strategy.The rGO@Fe₇S₈ composite is composed of homogeneous Fe₇S₈ and reduced graphene oxide thin nanosheets.This unique structure not only promotes the penetration of electrolyte and increases the conductive of the pure Fe₇S₈ electrode materials,but also relieves the volume expansion of K⁺ during charge/discharge process.When applied this interesting anode electrode for PIBs,the rGO@Fe₇S₈ exhibits excellent electrochemical performance.It delivers a high reversible specific capacity of 445 mAh g^-1 at 50 mA g^-1,excellent rate performance(284 mAhg^-1at 500 mA g^-1 and 237 mAh g^-1 at 1000 mA g^-1),and a high cycling stability at 100 mA g^-1(maintained 355 mAh g^-1 after 300 cycles).     

Regulating the d band in WS2@NC hierarchical nanospheres for efficient lithium polysulfide conversion in lithium-sulfur batteries

The performance of lithium-sulfur batteries is deteriorated by the inferior conductivity of sulfur,the shuttle effect of lithium polysulfides(LiPSs),sluggish redox kinetics of polysulfide intermediates and serious volumetric expansion of sulfur.To overcome these challenges,we report a versatile route to prepare multi-functional nanocomposites with tuable hierarchical structure via ammonium hydroxide(NH₃·H₂ O)induced self-assembly.The versatility of the system has been demonstrated that the organization of the hierarchical structure can be regulated by adding different amounts of NH₃·H₂ O,and WS₂ and Co₉S₈ with nitrogen-doped carbon coating(denoted as WS₂@NC and Co₉S₈@NC)can be prepared by adding different precursor salts.When the as-prepared materials are applied for Li-S batteries,the WS₂@NC composite exhibits a reversible capacity of 1107.4 mAh g^-1 at 0.1 C after 500 cycles and even 728.9 mAh g^-1 at2 C for 1000 cycles,which is significantly better than the Co₉S₈ counterpart and other reported WS₂ sulfur hosts.Experimentally,the advantageous performance of WS₂ could be attributed to its higher surface area and total pore volume,giving rise to the easier access to electrolyte and better ability to buffer the volume change during the charge/discharge process.Theoretically,the density function theory(DFT)calculation reveals that the as-prepared WS₂ has a higher binding energy towards LiPSs as well as a lower energy barrier for Li⁺diffusion on the surface than Co₉S₈.More significantly,the density of states(DOS)analysis further confirms that the superior performance is mainly ascribed to the more prominent shifting and the more charge compensation from d band of W than Co,which increase electronic concentration and give more hybridization of d-p orbitals in the Fermi level of the adsorbed Li2 S4 to accelerate the lithium polysulfide interfacial redox and conversion dynamics in WS₂.By proposing this mechanism,this work sheds new light on the understanding of catalytic conversion of lithium polysulfides at the atomic level and the strategy to develop advanced cathode materials for high-performance lithium-sulfur batteries.     

Crystal Structure of [Et_4N][Sm(S_2CNEt_2)_4]

The crystal structure of .[Et4N][Sm(S2CNEt2)4] was determined by X-ray diffraction technique. The crystal crystallizes in monoclinic system, space group P21/n with a= 1. 1695(3), b=2.0821(6), c=1.7420(7) nm, β=99. 79(3)°? Z=4, Dc= 1. 39 g/ cm3, μ(Mo/KTσ) = 18. 4 cm-1, F(000) = 1812. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R of 0. 053 for 3116 (Ⅰ> 3σ- (Ⅰ)) reflections. Each asymmetric unit contains two ions [Sm (S2CNEt2)4]-1 and [Et4N] +1, having distance between central atoms N5 and Sm3+ to be 0. 6522 nm. The atom Sm is coordinated by eight sulphur atoms. The Sm-S distance lies in the range of 0. 285-0. 290 nm with an average of 0. 288 nm.     

杂-双核配合物[CaCu(C3H2O4)2(H2O)4]n的合成、晶体结构及热稳定性

The title complex, [CaCu(C3H2O4)2(H2O)4]n, with a formula of C6H12CaCuO12 and Mr=379.78 has been sy-nthesized and characterized by single crystal X-ray diffraction structure analysis, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is Orthorhombic, space group Pbcn with a=0.669 21(5) nm, b=1.370 23(5) nm, c=1.322 39(10) nm, V=1.212 59(16) nm3, Dc=2.080 g·cm-3, μ=2.288 mm-1, F(000)=772 and Z=4. The final R=0.054 0 and wR=0.112 8 for 1 189 observed reflections with I>2σ(I). The structure of the title complex consists of CaO8 polyhedra and CuO6 elongated octahedra linked together by malonate ligands. The Ca(Ⅱ) cation, on a twofold axis, is coordinated by two water molecules and six malonate O atoms. The Cu(Ⅱ) cation, which lies in a centre of symmetry in an octahedral arrangement, is coordinated by four malonate O atoms and two water molecules. The structure comprises alternating layers along the [101] plane, with the shortest Cu…Cu distance of 0.762 46(6) nm. The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds. Its thermo gravimetric analysis was determined by TG-DTG techniques. CCDC:663184.     

Synthesis,Crystal and Band Structures,and Optical Properties of Mercury Pnictide Halide Hg19As10Br18

A mercury pnictide halide semiconductor Hg19As10Br18(1) has been prepared by the solid-state reaction and structurally characterized by single-crystal X-ray diffraction analysis.Compound 1 crystallizes in triclinic,space group P with a = 11.262(4),b = 11.352(4),c = 12.309(5) ,α = 105.724(2),β = 105.788(4),γ = 109.0780(10)° and V = 1314.3(8) 3.The structure of 1 is composed of parallel perovskite-like layers bridged by the linearly coordinated Br atoms to form a three-dimensional framework.The optical properties were investigated in terms of the diffuse reflectance spectrum.The electronic band structure along with density of states(DOS) calculated by DFT method indicates that compound 1 is a semiconductor with an indirect band gap,and that the optical absorption is mainly originated from the charge transitions from Br-4p and As-4p to the Hg-6s states.