Synthesis and Crystal Structure of trans(N)-(1,10-Phenanthroline)-bis (DL-Al aninato)-Cobalt( Ⅲ ) Chloridetrihydrate

The title compound was synthesized by the reaction of cis-[Co(phen)2Cl2]Cl·3H2O with DL-alanine at pH = 8, and isolated using a column chromatographic method. Its crystal structure was determined. The crystal structure belongs to mono-clinic system, space group P21/c, with a = 0. 9549(6) nm, b=2.3746(8) nm, c= 1.0782(4) nm, β=114.13(3)°? Z = 4, Dc= 1. 50 g/cm3. The final refinement converged to R = 0. 047 for 3246 independent observed reflections. In the octahedral coordination sphere formed by the cobalt atom and the coordinate atoms, N, O of DL-alan-inato ligands are in the configuration of trans-N ,N form.     

Hydrothermal Synthesis and Crystal Structure of Binuclear Copper(Ⅱ) Complex Bridged by 1,2,4,5-Benzenetetracarboxylato Trivalent Anion

The title complex [(phen)2Cu(Htcb)Cu(phen)2]H3tcb(tcb=1,2,4,5-benzenetetracarboxylato tetravalent anion; phen=1,10-phenanthroline) was synthesized by the hydrothermal synthesis method. The crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic system with space group P1, a=1.04174(8) nm, b=1.07119(8) nm, c=1.26360(10) nm, α=98.169(2)°, β=99.679(10)°, γ=93.658(10)°, V=1.37031(18) nm3, Z=1. The two copper(Ⅱ) cations are bridged by Htcb in the monodentate fashion, and have the same five-coordinated environment completed by the four N atoms from the two phen molecules and one O atom from the carboxylic group of Htcb respectively, which can be best described as distorted trigonal-bipyramid geometry. Moreover, the three dimensional network is formed by H-bonding interactions [O…O distance from 0.2506(10) nm to 0.3176(11) nm] and π-π stacking interactions between the phen rings of adjacent binuclear entities with a face-to-face separation of ca. 0.354 nm.     

Synthesis and Crystal Structure of（3S,4R,Z）-3,6-dimethyl-2-（3-methylbut-2-enylidene）-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol

The title compound of(3S,4R,Z)-3,6-dimethyl-2-(3-methylbut-2-enylidene)-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol,C15H22O3,as a potential gastric cytoprotective agent has been synthesized by the reduction of bisabolangelone in methanol with sodium borohydride.The title compound was characterized by IR and NMR spectra.Meanwhile,the crystal was obtained and determined by X-ray single-crystal diffraction.Crystal data:monoclinic system,space group P21 with a = 6.0692(12),b = 8.9954(18),c = 13.182(3) ,β = 92.59(3)°,V = 718.9(2) 3,Z = 2,F(000) = 272,Dc = 1.156 g/cm3,μ = 0.633 mm-1,R = 0.0362 and wR = 0.1051 for 9490 independent reflections(Rint = 0.0172) and 2461 observed reflections(I > 2σ(I)).Intermolecular O-H…O interactions link the molecules into one-dimensional infinite chains running along the b axis,which contributes to the stability of the crystal structure.     

Hydrothermal Synthesis and Crystal Structure of Inorganic-organic Hybrid Compound [H3NC2H4NH2]VOPO4

An inorganic-organic hybrid compound, [H_3NC_2H_4NH_2]VOPO_4 was synthesized by means of the hydrothermal method. It was crystallized in a monoclinic system, a space group P2_1/c, with the crystal cell parameters: a=0.92285(11) nm, b=0.72994(9) nm, c=0.98495(11) nm, β=101.280(3)°, V=0.65067(13) nm~3, M_r=223.02 g/mol, D_c=2.277 g/cm~3, Z=4, R=0.0315, ωR=0.0865, GOF=1.085. The VO_5N octahedra chains are corner-linked by PO_4 tetrahedra; the VO_5N octahedra are all trans-linked with V—O bonds being alternately short and long. The monoprotonated ethylenediamine was intercalated between the layers with one end coordinating to V and the other end as an H-bond donor interacting with a terminal O atom of PO_4 from a neighboring sheet. The elementary analysis, infrared spectrum characters and thermal stability were also given.     

Synthesis and Crystal Structure of a New Dinuclear Manganese(Ⅱ) Manganese(Ⅲ) Complex of a Macrocyclic Ligand

A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.     

A Novel Dimer--Heteropolytungstate with a Vanadium Atom as the Centre--Synthesis and Structural Characterization of (H3O)4[VW12O40Na(H2O)4]2

A novel dimer-tungstovanadate,(H3O)4［VW12O40Na(H2O)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 ,a=1.464 5(3) nm,b=1.4686(3) nm,c=1.4111(3) nm,α=111.82(2)°,βA novel dimer-tungstovanadate,(H3O)4［VW12O40Na(H2O)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 ,a=1.464 5(3) nm,b=1.4686(3) nm,c=1.4111(3) nm,α=111.82(2)°,β=93.17(3)°,γ=117.47(3)°,V=2.2106(8) nm3,Z=1,Dc=4.552 g.cm-3,λ(Mo Kα)=0.071073 nm,μ=31.402 mm-1,F(000)=2648,R=0.0780.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×0.7785 nm.     

The structure-directing effect of n-propylamine in the crystallization of open-framework aluminophosphates

Using n-propylamine as a template,deioned water and secondary-butanol(butan-2-ol)as solvents,a three-dimensional(3D)open-framework aluminophosphate[C3NH10]·[HAl3P3O13](1)and a two-dimensional layered aluminophosphate[C3NH10]3·[Al3P4O16](2)were crystallized from the initial mixtures with compositions of Al2O3:2.4 P2O5:5.0 n-propylamine:100 H2O/butan-2-ol,respectively.They are characterized by X-ray powder diffraction(XRD),thermogravimetric(TG),and elemental(CHN)analyses and structurally determined by single-crystal X-ray diffraction analysis.Compound 1 crystallizes in the monoclinic space group P21/c with a=0.85831(13)nm,b=1.7677(3)nm,c=1.04353(12)nm,=123.887(9)°,and V=1.3143(3)nm3.Compound 2 crystallizes in the monoclinic space group P21/c with a=1.1313(2)nm,b=1.4874(3)nm,c=1.8020(6)nm,=125.07(2)°,and V=2.4817(11)nm3.The results show that the properties of solvent have a significant influence on the structure-directing effect of n-propylamine in the crystallization of the open-framework aluminophosphates.     

一维链状化合物[Ag(L)]·H2O的合成、晶体结构和荧光性质

The title compound,[Ag(L)]·H2O,1,where HL=4-(isonicotinamido)benzoic acid,was synthesized in methanol solution and its crystal structure was determined by X-ray diffraction analysis.The crystal is of monoclinic.space group P21/c with a=0.571 8(8)nm,b=1.357 2(18)nm,c=1.5580(2)nm,β=91.090(2)°,V=1.2090(3)nm3,Z=4,Dc=2.009 g·cm-3,F(000)=722,Rint=0.042 9,R=0.027 1,wR=0.055 6.In complex 1,the Ag atoms are linearly coordinated by one O atom and one N atom of two ligand molecules.Each I- ligand in turn uses its one carboxylate group and one pyridinyl groups to connect two metal centers,then the one-dimensional (1D) chains is formed.On the other hand,the 1D chains are further connected by O1W-H1WB…O2 hydrogen bonds and Ag-O weak interactions to give a two-dimensional (2D) layer,finally,the 2D net extents to three-dimensional (3D) supramolecular framework by O1W-H1WB…O1 as well as N2-H2…O2 interactions.CCDC:762259.     

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.     

Synthesis, Crystal Structures and Characterization of Ba5LiTiNb9O30

A new niobate compound with the chemical composition of Ba5LiTiNb9O30 was synthesized by doping Li^ into the system BaO-TiO2-Nb2O5 in conventional solid state reaction method. The crystalline structure was determined by X-ray diffraction analysis (XRD). The results showed that crystal structure of Ba5LiTiNb9O30 belongs to tetragonal tungsten bronze structure with space group P4bm and its unit cell parameters: a=b=1.2512(2) nm, c=0.4008(5)nm. The microstructure of reaction products was observed by scanning electron microscopy (SEM).     

Dawson结构α-H6P2W18O62·3(CH3)2NH·H2O的合成、表征和晶体结构

由二甲胺与H6P2W18O62·nH2O合成了电荷转移化合物α-H6P2W18O62·3(CH3)2NH·H2O.单晶结构解析结果表明晶体属单斜晶系,空间群为P21/c,晶胞参数a=1.2964(3)nm,b=1.3621(3)nm,c=4.155 9(8)nm,β=90.02(3)°,V=7.338(3)nm3,Z=4.标题化合物具有可逆光色性.热分析表明,化合物阴离子在430.5℃左右分解.     

1－苯基－3－甲基－4－（6－氢－4－氨基－5－硫杂－2，3－吡嗪）－吡唑啉酮光致变色超分子化合物的合成、结构与性能

通过1－苯基－3－甲基－4－氯乙酰基－吡唑啉酮－5（PMCP）和氨基硫脲（ TSC）缩合，形成了一种含NNS六元杂环的光致变色化合物（PMCP－TSC）。利用元 素分析，MS，”1H NMR，IR和UV光谱进行了表征。通过紫外可见光谱对它的光致 变色性质进行了研究，测出了光致变色反应的动力学常数。并用X线单晶衍射仪测 定了PMCP－TSC变色后的晶体结构，该晶体属单斜晶系，具有P2_1/c空间群，a = 0.105 10(2) nm, b = 0.150 61(3) nm, c = 0.993 70(10) nm, β = 107.890 (10)°, V = 1.496 9(4) nm~3, Z - 4, D_c = 1.417 Mg/m~3, μ = 0.232 mm~(- 1), F(000) = 672, R = 0.033 4, wR = 0.089 6。结构分析表明：其光致变色现 象是由于它在溶剂与光的共同作用下发生了从醇式到酮式的异构化。同时该化合物 经分子间氢键形成二聚体，又通过甲醇与本体分子之间的氢键使化合物形成具有三 维网络结构的超分子化合物。     

Synthesis and Crystal Structure of the Organotin Complex [(o-Cl-PhCH_2)_3SnOCOC_(10)H_8N]·0.5C_6H_6

1 INTRODUCTION There is increasing interest in the study of orga-notin carboxylic ester compounds due to their insec-ticidal, fungicidal and antibiotic activities[1, as well 2]as structure diversity. In recent years many organo-tin carboxylic ester compounds with good biologi-cal activity have been synthesized[3, . Previous stu- 4]dies show that the coordination geometry of centralatom Sn …     

Cd[CH_3O(OH)C_6H_3CH=N(CH_2)_2OH]_2Br_2的合成、结构及微观二阶非线性光学系数

合成了标题配合物Cd[CH3O(OH)C6H3CH =N(CH2 ) 2 OH]2 Br2 ,对其进行了元素分析、红外和X射线结构分析。该配合物单晶的分子式为 :CdC2 0 H2 6N2 O6Br2 ,Mr=662 .66属于单斜晶系 ,P2 1 /n空间群 ,晶胞参数a =7.851 2 (2 ) ,b =1 7.391 (3) ,c=1 7.575(4) ,β =90 .86(3)°,V =2 392 (1 ) 3,Z =4,Dc=1 .834g·cm- 3,μ(MoKα) =4.2 4 1 9mm- 1 ,F(0 0 0 ) =1 30 4。用直接法解得结构 .R =0 .0 74,Rw=0 .0 84.在 2 99± 1K的温度下收集到 3744个独立衍射点 ,其中 2 4 70个为可观察的衍射点 [I≥ 3σ(I) ]。同时在 1 .0 64μm的Nd :YAG激光器上对配合物进行了粉末SHG实验 ,并用MOPAC软件包采用PM 3方法解得其分子的微观二阶极化率为 3.341× 1 0 - 30 esu。进一步讨论了微观二阶非线性极化率、宏观激光倍频效应和分子结构、晶体结构之间的关系。     

Growth and Spectroscopic Properties of Nd3＋：Sr3Gd2（BO3）4 Crystal

<正>This paper reports the growth,X-ray diffraction and spectroscopy of Nd~(3+):Sr_3Gd_2(BO_3)_4 crystal.A Nd~(3+):Sr_3Gd_2(BO_3)_4 crystal with dimensions ofφ20×45 mm~3 has been grown by the Czochralski method.Nd~(3+):Sr_3Gd_2(BO_3)_4 crystal belongs to the orthorhombic system,space group Pnma(D_(2h))with a=0.7401,b=1.604 and c=0.8755 nm.The absorption and emission spectra of Nd~(3+):Sr_3Gd_2(BO_3)_4 were investigated.The absorption cross sectionσ_a is 3.11×10~(-20)cm~2 at 808 nm. The absorption transition at 808 nm has an FWHM of 14 nm.The luminescence lifetimeτ_f is 51.7 us.The emission cross sectionσ_e at 1064 nm wavelength is 1.09×10~(-19)cm~2.     

新型环形聚阴离子[{WO(H_2O)}_3(AsW_8O31)_3]~21-的结构及表征

在pH=3.0的水溶液中，Na_2WO_4·2H_2O与NaAsO_2·6H_2O和NH_4Cl反应，得 到了新的杂多钨酸盐(MH_4)_19Na_2[{WO(H_2O)}_3(AsW_8O31)_3]·45H_2O单晶， 用X射线单晶衍射法及元素分析确定了其结构，晶体属单斜晶系，空间群C2/c，晶 胞参数为：a=3.1165(11)nm, b=1.7388(7)nm, c=2.2789(9)nm, β=97.342(6)°, V=12.248(8)nm~3, Z=4, R_1=0.0571,wR_2=0.0741[I＞2σ(I)]. 环型聚阴离子 [{WO(H_2O)}_3(AsW_8O31)_3]~21-是由三个{WO(H_2O)}桥连三个新发现的 {AsW_8O31}单元构成的，环聚离子[{WO(H_2O)}_3(AsW_8O31)_3]~21-具有近似D_ (3h)对称性。对该化合物还进行了~183W NMR, IR和TG表征。     

3-羟基-1-金刚烷甲酸钴邻菲略啉配合物的合成和晶体结构

以硫酸钻、邻菲咯啉（phen）和3-羟基-1-金刚烷甲酸（HOC10H14COOH）为原料,合成了配合物[Co（HOG10H14COO）2（H2O）（phen）]·H2O;利用元素分析、红外光谱、热重分析对产物进行了表征,采用单晶X射线衍射方法测定了其晶体结构．结果表明,所合成的配合物C34H42N2O8Co属于单斜晶系,空间群C2／c,a=2．69798（7）nm,b=1．14319（3）nm,c=2．29092（6）nm,β=120．498（1）°,V665．63,F（000）=2808,Dc=1．452g·cm^-3,μ（Mo-Kα）=0．765mm^-1;R1=0.0805,wR2=0.2209,其通过氢键和π-π堆积作用相结合,形成稳定的二维超分子结构．     

六钨酸盐为模板的三维网状超分子化合物[La2(DNBA)4(DMF)8][W6O19]的合成和晶体结构

0 Introduction polyoxometalates (POMs), in addition to their im- portance in catalysis, biochemical separation and medicinal chemistry, play an important role for the design of new materials with novel electronic, magnet- ic and topological properties[1￣…     

钒氧配合物[VOL(C9H6NO)]·CH2Cl2的合成与晶体结构

A oxovanadium(Ⅴ) complex of [VOL(C₉H₆NO)]·CH₂Cl₂[H₂L=2-hydroxy-1-naphthaldehyde 4-methoxy-benzoylhydrazone, C₉H₆NO^-=8-hydroxyquinoline anion] has been synthesized and characterized by elemental analyses, IR and single crystal X-ray diffraction. The crystal crystallizes in triclinic system, the space group is P1, with the crystal cell parameters a=1.087 0(2) nm, b=1.107 1(2) nm, c=1.269 3(3) nm, α=67.84(3)°, β=79.26(3)°, γ=73.85(3)° and V=1.353 1(6) nm³ , M_r=614.34, R=0.0503, wR=0.1409. The V(Ⅴ) atom is six-coordinated by one O atom of oxo group, two O atoms and one N atom of the tridentate hydrazone ligand, as well as one N atom and one O atom of 8-hydroxyquinoline ligand, thus defining a distorted octahedral VO(ONO)(NO) geometry. A two-dimensional supramolecular layer structure is formed through π-π stacking interactions. CCDC: 268672.     

5-苯基-3,5-二乙氧基-2(5H)-呋喃酮的晶体结构

标题化合物C14H16O4的晶体结构用X-射线单晶衍射法测定。晶体属三斜晶系,P空间群,晶胞参数a =8.696(2), b=8.943(2) , c=9.379(2) ?, ( = 69.28(3), ( =76.67(3), ( =80.28(3)o, V=660.8(3) ? 3, Z=2, Mr=248.28, Dx=1.248 g/cm3, F(000)=264, μ(MoK()=0.0851 mm—1。晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.061, wR=0.089。标题化合物有2个环：呋喃酮环和苯环。由C(1),C(2),C(3),C(4),O(4)构成的五元呋喃酮环的5个原子较好地处于1个平面上,平均偏差为0.0078?。O(2),O(3) 两个原子与呋喃酮环共平面。呋喃酮环和苯环之间的两面角为79.39o。