Synthesis,Crystal Structure and Electrochemical Property of a Dinuclear Manganese（Ⅱ） Complex [Mn_2（C_（12）H_8N_2）_4（C_8H_5O_4）_2]（C_8H_4O_4）·H_2O

One dinuclear manganese(II)complex [Mn2(C12H8N2)4(C8H5O4)2](C8H4O4)·H2O has been synthesized with o-phthalic acid and 1,10-phenanthroline.The crystal structure was determined by X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 1.17767(3),b = 1.22292(2),c = 1.35860(3)nm,α = 110.5300(10),β = 97.6140(10),γ = 93.7300(10)o,V = 1.80307(7)nm3,Dc = 1.404 g/cm3,Z = 2,F(000)= 784,the final GOOF = 1.047,R = 0.0398 and wR = 0.1038.The crystal structure of the title complex consists of one [Mn2(C12H8N2)4(C8H5O4)2]2+ cation,one uncoordinate o-phthalate anion(C8H4O4)2-and one uncoordinate water molecule.In [Mn2(C12H8N2)4(C8H5O4)2]2+,the central Mn(II)ion is coordinated by four nitrogen atoms and two oxygen atoms to give a distorted octahedral coordination geometry.The electrochemical property of the title complex was also studied.     

Macro-, Micro-, Nano- and Crystal Structures of a Homodinuclear Complex [NH3（ CH2）3NH3]2{Na2[（C6H4O2）2]（C6H4O2H）2}

A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[（C6H4O2）2]（C6H4OOH）2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy （SEM） indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy （TEM） reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2.     

Synthesis and Crystal Structure of an Unusual Dodecacoordinated Lanthanum Complex by Phenanthroline and Nitrate （phenH）_2[La（NO_3）_5（phen）]·CH_3OH

Lanthanum complex (phenH)2[La(NO3)5(phen)]·CH3OH (1, phen=phenanthroline) was synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a=20.3040(3), b=10.7091(1), c=19.0771(2), β=102.090(1)°, V=4056.07(8)3, Z=4, Dc=1.676 g/cm3, μ= 1.142 mm-1, F(000)=2056, the final R=0.0346 and wR=0.0793 for 9981 (Rint=0.0358) independent reflections. The mononuclear complex 1 consists of four parts: two phenH+ cations formed by the protonation of phen, one complex anion [La(NO3)5(phen)]2-, and one solvent methanol molecule. The complex anion contains one phen and five nitrate ligands which both chelate the center La(III) ion, adopting a distorted twelve-coordinated icosahedral geometry. The cations, anion and solvent molecule are linked together by hydrogen bonds. One of the protonated phenanthrolines (phenH+) acting as cation connects to the anion via N–H…O hydrogen bond directly, and the other one links to the anion through an intermediate solvent CH3OH via N–H…O and O–H…O hydrogen bonds. By the plentiful additional weak C–H…O intermolecular hydrogen bonds, the compound molecules construct a two-dimensional layer structure.     

Synthesis and Structural Characterization of Manganese Carbonyl Incorporated Polyoxomolybdate （n-Bu4N）2 [Mo6O16（OCH3）2 {HOCH2C（CH2O）3}2 {Mn（CO）3}2]

The polyoxoanion incorporated {Mn（CO）3^＋} complex, （n-Bu4N）2[Mo6O16（OCH3）2{HOCH2C（CH2O）3}2·{Mn（CO）3}2]（1）, has been synthesized by the reaction of （n-Bu4N）4[Mo8O26] with Mn（CO）5Br in methanol, in the presence of C（CH2OH）4. The complex 1 has been characterized by IR, UV-Vis, X-ray single crystal diffraction, and TG. Crystal data for the complex 1：C25H48MnMo3NO16 （1）, Triclinic Pi, a=0.9405（3） nm, b=1.3351（4） nm, c=1.5455（4） nm, α=103.206（5）°, β=102.165（5）°, γ=100.784（5）°, V=1.7896（9） nm^3, Z=2, R1=0.0703, wR2= 0.1495. The structure analysis of complex 1 shows that the complex consists of two tetrabutylammonium cations and a polyoxomolybdate anion that incorporates two fac-Mn（CO）3^＋ units. The anion of complex 1 can be considered as the dimer of two rhomb-like anions by sharing of two comers.     

一种新颖有机／无机杂化配位聚合物[（C7H18N）（Ag2l3）]n的合成、结构及量子化学计算

A one dimensional coordination polymer, [(C7H18N)(Ag2l3)]n((C7H18N)^ =Methyltriethylammonium) has been successfully synthesized and characterized by X-ray single-crystal diffraction method. Structure analysis shows that the compound consists of organic cations(Methyltriethylammonium) and inorganic anion chains (Ag2l3)s^-.The inorganic moiety consists of AgI4 tetrahedron, which shares the same edges with adjacent AgI4 tetrahedrons to form one-dimensional infinite double chains along a-axis. There exists weak interaction among Ag…Ag atoms in the crystal. Anion chains are surrounded by Methyhriethylammonium cations. Anion chains and cations are in combination with each other by static attracting forces in the crystal to form so-called organic-inorganic hybrid structure. According to the crystal structure data, quantum chemistry calculation with DFT on B3LYP level was used to reveal the electronic structure of title compound. CCDC: 254288.     

{Na2[μ2-(C6H4O2)2](C6H4OOH)2}4-的结构及其在固态合溶液中的NMR比较

The new compound （NH3CH2CH2NH3）2{Na2[μ2-（C6H4O2）2]（C6H4OOH）2} has been synthesized and characterized by elemental analysis, IR, UV, NMR and single crystal X-ray diffraction. The yellow crystals crystallized in the triclinic system with space group P-1 and a=0.6091（2） nm, b= 1.0274（3） nm, c= 1.2466（4） nm, α=89.073（6）°, β=89.376（6）°, γ=78.873（5）°, V=0.7653（4） nm^3, Z= 1, R1=0.0568, wR2=0.1198. Every sodium ion coordinates in trigonal prismatic fashion with two O atoms from a terminal chelating catecholato ligand and four O atoms from bridging P2 catecholato ligands, Two neighboring NaO6 trigonal prisms are face-shared and centrosymmetric with regard to the inversion center consisting of four tri-bridging O atoms to form a binuclear cluster {Na2[μ2-（C6H4O2）2]}^2- anion. The comparison of ^13C NMR spectrum of tlie complex in solid state with that in solution indicated that the rapid exchange between the bridging [μ2-（C6H4O2]^2- and terminal [C6H4OOH]^- ligands was present in solution.     

The Reaction of Molybdenum with 2,3-Dihydroxynaphthalene

[H2N（CH2）3NH312[MoO2（C10H6O2）2] （1） was synthesized by the 2,3-dihydroxynaphthalene in the mixed solvent of CH3OH, CH3CN reaction of （n-Bu4N）4[Mo8O26] with and 1,3-propanediarnine. （C5HllN2）2- [HeN（CH2）3NH2][MoO2（CloH6O2）2] （2） was obtained by the reaction of Na2MoO4.2H20 with 2,3-dihydroxynaphthalene in the same solvent above. Both of the complexes possess complex anion [Mo（VI）O2（OC10H6O）2]^2- which shows pseudo-octahedrally coordinated fashion, while the counterions are two protonated 1,3-propanediamine in complex 1 and （CsH11N2）^＋ in complex 2. （C5H11N2）＋ is the byproduct of reaction 2, which results from combination of acetonitrile with 1,3-propanediamine. Packing diagrams of the two complexes are also different. There is anti-parallel-aligned-double-meso-bilayer unit in complex 1. However there are four chiral anions arranged in anticlockwise orientation in complex 2.     

Synthesis and Crystal Structure of 2,5-Di- （pyridin-3-yl）-1,3,4-oxadiazolendium Nitrate

In order to continue our studies on the synthesis, properties and coordination of s-tetrazine, 3,6-di-(pyridin-3-yl)-s-tetrazine (II, 3-dptz) was synthesized and characterized by 1H- NMR, MS and IR spectra. And the coordination reaction of 3-dptz with nitrate of Cu(II) was studied. 3-dptz reacting with CuII salt [Cu(NO3)2·2H2O] generates a new salt, nitrate of 2,5-di-(pyridin-3- yl)-1,3,4-oxadiazolene (III). III was determined by IR spectra and single-crystal X-ray diffraction to give the following crystal data: space group P21/c, a = 4.9112(1), b = 8.4101(3), c = 29.499(1) , β = 93.266(2)o, V = 1216.44(7) nm3, Mr = 287.24, Z = 4, Dc = 1.568 g/cm3,μ= 0.122 mm-1, F(000) = 592, R = 0.0430 and wR = 0.1240. The results show that III is composed of one cation and one nitrate anion. The cation consists of one H+ and one 2,5-di-(pyridin-3-yl)-1,3,4-oxadiazol molecule, with the former being attached to the latter via electrovalent bond with N3 atom. And the O(42) atom in the nitrate anion is disordered. Intra- and intermolecular H-bonds are observed in the crystal of the title compound. The mechanism of metal-assisted decomposition was also discussed briefly.     

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.     

Synthesis,Crystal Structure of Cis—dioxo—catecholatotungsten（VI） Complex and Its NMR Studies on the Interaction with ATP

Cis-dioxo-catecholatotungsten(VI) complex anion[W^(VI)O2-(OC6H4O)2]^2- was obtained with discrete protonated ethylenediamine (NH2CH2CH2NH3)^ cations by the reaction of tetrabutyl ammonium decatungstate with catechol in the mixed solvent of CH3OH,CH3CN and ethylenediamine,and compared with its molybdenum anaogue [Mo^(V) O2(OC6H4O)2]^3- by crystal structure,UV,EPR,The results of the UV and EPR spectra show that tungsten is less redox active than molybdenum since the molybdenum is reduced from Mo(VI) to Mo(V) but tungsten stays in the original highest oxidized state Mo(VI) when they are crystallized from the solution above.It is worthy to note that [W^(VI)O2(OC6H4O)]^2- shows the same coordination structure as its molybdenum analogue in which the metal center exhibits distorted octahedral coordination geometry with two cis-dioxocatecholate ligands and might have the related coordination structure feature with the cofactor of flavoenzyme because [Mo^(V)O2(OC6H4O)2]^3- presented essentially the same EPR spectra as flavoenzyme.The NMR studies on the interaction of the title complex with ATP reveal that the reduction of W(VI) to W(V) occurs when the title complex is dissolved in D2O and the W(V) is oxidized again when ATP solution is mixed with original solution and the hydrolysis of the catecholato ligand take places at mean time being monitored by ^1H NMR and ^13C NMR spectra.     

Cleavage of the Fe—Fe Bond of （Me2SiSiMe2） [η^5－C5H4Fe（CO）2]2 with Na／Hg and Molecular Structure of the Ring－Opened Complex

The reaction of the rifle cyclic complex (1) with sodium amalgam in THF resulted in the expected cleavage of the Fe-Fe bond to afford his-sodium salt ( Me2SiSiMe2 ) [η^5-C5H4Fe(CO)2]2 (4). The latter was not isolated and was used directly to react with MeI, PhCH2Cl, CH3C(O)Cl, PhC(O)Cl,Cy3SnCl (Cy= cyclohexyl) or Ph3SnCl to afford corresponding ring-opened derivatives (Me2SiSiMe2) [η^5-C5H4Fe(CO)2]2 [5, R=Me; 6, R=PhCH2; 7, R=CH3C(O); 8, R=PhC(O); 9, R = Cy3Sn or 10, R = Ph3Sn ]. The crystal and molecular structures of 10 were determined by X-ray diffraction analysis. The molecule took the desired ant/ conformation around the Si-Si bond. The length of the Si--Si bond is 0.2343(3)nm, which is essentially identical to that in the cyclic structure of 1[0.2346(4) tun]. This result unambiguously demonstrates that the Si--Si bond in the cyclic structure of 1 is not subject to obvious strain.     

Preparation,Crystal Structure,Thermal Decomposition and Explosive Properties of K2（tza）2（H2O） （tza=Tetrazole-1-acetic Acid）

A new energetic compound based on the tetrazole-1-acetic acid (tza) and potassium(I) salt, K2(tza)2(H2O), was synthesized and characterized by elemental analysis and FT-IR spectrum. Its crystal structure was determined by single-crystal X-ray diffraction analysis. The results show that the crystal belongs to the orthorhombic system, space group Pna21 with a = 1.11972(17) nm, b = 0.46647(7) nm, c = 2.5158(4) nm, V = 1.3140(3) nm3, K2C6H8N8O5, Mr = 350.40 g·mol-1, Dc = 1.771 g·cm-3, μ(MoKα) = 0.759 mm-1, F(000) = 712, Z = 4, R = 0.023 and wR = 0.0527 for 2961 observed reflections (I > 2σ(I)). The K(I) cation is six-coordinated with four O atoms from three carboxylate groups, one O atom from one H2O molecule and one N atom from tetrazolyl ring, in which each tza is coordinated in a tridentate chelating bridging coordination mode. The thermal decomposition mechanism of the title complex was studied by DSC and TG-DTG techniques. Under nitrogen atmosphere at a heating rate of 10 K·min-1, the thermal decomposition of the complex contains one main exothermic process between 191.7 and 243.8 ℃ in the DSC curve. Its combustion heat was mensurated by oxygen bomb calorimetry. The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. The sensitivity properties of K2(tza)2(H2O) were also determined with standard methods, which was very sensitive to flame.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-（2-Pyridyl）benzimidazoleH2]2＋ ·[SbCls]2-}2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 2.366 mm-1, S = 1.010, F（000） = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3＋ ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb...Cl. Moreover, the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-（2-pyridyl）benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

Crystal Structure of Indenyl—3—indenyl

1 INTRODUCTION Indene is an intermediate used for the synthesis of organometallic complexes involving silylene-bridged indenyl[1～5]. In the process of synthesizing (CH3)(C6H5)Si(Ind)2[6], a new compound as a by-product which is a dimer of indene was obtained, and only one similar crystal was found in CCDC[7]. Up to now, there are no crystal structure reports on this kind of structure. The present paper will describe the crystal structure of the title compound. 2 EXPERIMEN…     

One Novel Mn(Ⅱ) Complex with 1-Substituted-1H-1,2,3-triazole-4-carboxylic Acid:Crystal Structure,Fluorescence and Hirshfeld Surface Analysis

The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric unit consists of a [Mn(pmta_)3]ˉ anion, half [Mn(H_2O)_6]~(2+) counter cation and two lattice H_2O molecules, and the intra- and intermolecular hydrogen bonds connect the complex into a supramolecular structure. The liquid-state fluorescence spectra of complex 1 have been determined. Hirshfeld surface analysis was also studied. The main intermolecular interactions in the complex are O···H and H···H contacts.     

Synthesis of a new salt containing polyoxometallate anion and M-Cu-S cluster cation [MS_4Cu_4(γ-MePy)_8][M_6O_19] (M = Mo,W).Crystal structure of [WS_4Cu_4(γ-MePy)_8][W_6O_19]

Reactions of (NH4)2MS4, AgBr and CuBr in r-methylpyridine produced one new compound, [MS4Cu4(r-MePy)8]M6O19] (1, M = W; 2, M = Mo), of which 1 was characterized by single crystal X-ray analysis. The crystal data: orthorhombic, Pbcn, a = 15.434(4),b= 16.732(2), c = 28.657(7) A, V = 7400.8(8) A3, Z = 4, R = 0.072 for 3121 independent data. The compound is the first example which contains both polyoxotnngstate anion and heteropolynuclear cluster cation. In the structure of the cation four edges of the tetrahedral WS42- core are coordinated by four copper atoms, giving a WS4Cu4 aggregate of approximate D2h symmetry. The differences between the reaction of Cu+ with MS42- and that of Ag+ with MS42- in pyridine and its derivatives are discussed.     

Preparation,Crystal Structure and Density Functional Theory Calculations of the Ion-pair Compound [Cl2Bz（3-MeQl）]（TCNQ）

A novel compound [Cl2Bz(3-MeQl) ](TCNQ) ([Cl2Bz(3-MeQl) ]+ = 1-(3,4-dichlo-robenzyl) 3-methlquinoline cation,TCNQ-= 7,7,8,8-tetracyanoquinodimethanide anion) has been synthesized by the reaction of [Cl2Bz(3-MeQl) ]Br and LiTCNQ,and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic,space group P21/c. The structure analysis shows that the anions are stacked into a column with isolated π-dimers,and there is one type of TCNQ entries(TCNQ) ,in agreement with the IR spectra analysis and density functional theory calculations of the compound. The most prominent structural features are the completely segregated stacking columns of the TCNQ- anions and [Cl2Bz(3-MeQl)]+ cations.     

Synthesis, Crystal Structure and Magnetic Properties of a Sandwich-type Polyoxometalate [H2N（CH2CH2）20]10[Mn2（AsVMo9Oa3）2]·12H2O

A new heteropolymolybdoarsenate [H2N(CH2CH2)2O]10[Mn2(AsVMo9O33)2]·12H2O(1) has been synthesized in aqueous solution and characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction. The crystal is made up of sandwich-type [Mn2(AsVMo9O33)2]10- anions, [H2N(CH2CH2)2O]+ cations and H2O molecules of crystallization. The magnetic properties of 1 have been studied by measuring its magnetic susceptibility in the temperature range of 2.0-300.0 K, indicating the existence of antiferromagnetic interactions.     

Hydrothermal Synthesis,Crystal Structure and Electrochemical Properties of a New Dinuclear Copper Complex [C2H6ON]2[Cu2Cl2（μ-CH3COO）4]

The hydrothermal reaction of copper chloride dihydrate and 5,5-dimethyl-imidazolidine,-2,4-dione with a mole ratio of 1：1 in acetonitrile resulted in the formation of a new acetate-bridged dinuclear copper complex, [C2H6ON]2[Cu2Cl2（μ-CH3COO）4]. Protonated acetamide in eaolie form and acetic acid were yielded by the hydrolysis of acetonitrile under hydrothennal condition. The rifle complex （C12H24Cl2Cu2N2O10） was characterized by X-ray single-crystal diffraction, IR spectrum, elemental and electrochemical analysis. It crystallizes in the monoclinic system, space group P21/c with a = 8.298004）, b = 14.358（2）, c = 12.0010（2） A^°, β= 130.620（3）°, V = 1085.3（2） A^°^3, Dc = 1.696 g/cm^3, 34, = 554.31, Z = 2, F（000） = 564 and μ = 2.254 mm^-1. The crystal structure consists of a tetraacetate-bridging dinulcear copper complex anion [Cu2Cl2（μ-CH3COO）4]^2-, with the chlorine anions in the axial positions, and two protonated acetamide cations [C2H6ON]^＋, which were connected through hydrogen bonds to form a three-dimensional infinite network.     

Synthesis,Crystal Structure and Photoluminescence of [Gd（C6NO2H5）3- （H2O）2]2n·（nH5O2）（nHgCl5）（2nHgCl4）·（2nH2O）

A heterometallic 4f-5d inorganic-organic metaMsonicotinato hybrid [Gd（C6NO2H5）3- （H2O）2]2n·（nH5O2）（nHgCl5）（2nHgCl4）·（2nH2O） 1 has been synthesized via hydrothermal reaction and structurally characterized. Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell： a = 24.234（8）, b = 20.816（7）, c = 15.333（3）A , β= 128.091（8）°, V = 6088（3）A^3, C36H47Cl13Gd2Hg3N6O20, Mr = 2260.92, Dc = 2.467 g/cm^3, S = 0.896, μ（MoKα） = 10.331 mm^-1, F（000） = 4216, R = 0.0344 and wR = 0.0629. The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure. Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.