Synthesis and Characterization of a Bismuth Incorporating Heptamolybdate： （NH4）4 [HMo7O24Bi（H2O）2CsH3N（CO2）2]·7H2O

A new one-dimensional molecule based on the linkage of [Mo7024] clusters and [BiL] （L = pyridine-2,6-dicarboxylic acid） assembles under ambient conditions. The title compound was characterized by X-ray powder diffraction, IR and UV spectra, thermogravimetric analysis, and single-crystal X-ray diffraction. Crystal data： C7H38BiMo7N5037, Mr = 1664.95, monoclinic, space group C2/c, a = 24.312（2）, b = 21.4869（18）, c = 18.5423（16） A, β = 111.6490（10）°, V = 9002.9（13） A3, Z = 8, μ = 5.883 mm-1, F（000） = 6304, GOF = 1.045, R = 0.0365 and wR = 0.1062.     

Synthesis and Structure of Copper(Ⅱ) Complex [Cu(C_5H_5N)_2(H_2O)(C_6H_5COO)_2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＣｅｒｔａｉｎｃｏｐｐｅｒｃｏｍｐｌｅｘｅｓｈａｖｅｂｅｅｎｓｈｏｗｎｔｏｈａｖｅｕｎｕｓｕａｌｃｈｅｍｉｃａｌｐｒｏｐｅｒｔｉｅｓｓｕｃｈａｓｏｘｙｇｅｎｔｒａｎｓｆｅｒ,ｏｘｉｄａｔｉｖｅａｄｄｉｔｉｏｎａｎｄｈｏｍｏｇｅｎｏｕｓｃａｔａｌｙｔｉｃｈｙｄｒｏｇｅｎａｔｉｏｎ[1].Ｏｘｉｄａｔｉｖｅａｄｄｉｔｉｏｎｒｅａｃｔｉｏｎｓａｒｅｋｅｙｓｔｅｐｓｉｎｔｈｅａｃｔｉｖａｔｉｏｎｏｆσｂｏｎｄｓｉｎａｇｒｅａｔｎｕｍｂｅｒｏｆｃａｔａｌｙｔｉｃｐｒｏｃｅｓｓ.Ｃｏｐ…     

Synthesis,Characterization and Standard Molar Formation Enthalpy of [Sm(C_7H_5O_3)_2(C_4H_6NO_2S)]·2H_2O

[Sm(C7H5O3)2(C4H6NO2S)]·2H2O was synthesized from the reaction of samarium chloride hexahydrate with salicylic acid and thioproline,and characterized by IR,elemental analysis and thermogravimatric analysis.The standard molar enthalpies of the solutions of SmCl3·6H2O(s),2[C7H6O3(s)],[C4H7NO2S(s)] and [Sm(C7H5O3)2·(C4H6NO2S)·2H2O(s)] in a mixed solvent of absolute ethyl alcohol,dimethyl formamide(DMF) and 3 mol/L HCl were,respectively,determined by calorimetry to be Δs Θ [SmCl3·6H2O(s),298.15 K]=(-46.68±0.15)...     

Synthesis and Structural Characterization of a Novel Coordination Polymer [Cd(C_4H_2O_4)(C_3H_4N_2)_3]_n·2nH_2O

1 INTRODUCTION In recent years, the design and synthesis of metalorganic coordination polymers have attracted considerable attention, for such supramolecular assemblies have interesting structures as well as potentiaapplications as smart optoelectronic, magnetic andporous materials. By judicious selection of ligandand metal coordination geometries, control over thetopology and geometry of the infinite networks canbe gained. As neutral donor ligands, 4,4?-bpy, pyrazine and imidazole which …     

[Ni(C_5H_5N)_2(C_7·H_6O_2N)_2]H_2O三元配合物的合成及晶体结构

合成了标题化合物。该化合物的分子式[Ni(C5H5N)2(C7H6O2N)2]H2O(C24H24N4NiO3),分子量475.18,采用单色的MoKα (λ = 0.71073 )射线测定,共收集7408个数据,其中独立衍射点2567个(Rint = 0.0272),I > 2s(I)可观测点数1926个,结果表明该化合物属单斜晶系, 空间群C2/c其晶胞参数为: a = 14.466(2),b = 12.193(2),c = 14.072(2) ;β = 116.229(2)°,V = 2226.6(5) 3,Z = 4,Dc = 1.418 g/cm3 ,μ = 0.905 mm-1,F(000) = 992. 2个水杨醛亚胺各提供2个配位原子参与配位,2个吡啶各提供1个配位原子参与配位,该配合物是六配位的八面体构型,同时讨论了该体系中不同配位原子的配位能力的差异。     

Synthesis and Crystal Structure of a New Charge-assisted Hydrogen-bonded Host Framework [Co(en)_3]_2[Zr_2(C_2O_4)_7]·2H_2O

Using the deep eutectic solvent formed of oxalic acid and choline chloride, a new charge-assisted hydrogen-bonded host framework [Co(en)3]2[Zr2(C2O4)7]·2H2O(1) has been obtained. The title complex crystallizes in the monoclinic, space group P21/n(No. 14) with a = 7.7448(10), b = 14.5683(19), c = 19.375(3), β = 92.124(2)o, V = 2184.5(5) 3, Z = 4, Dc = 1.996 g.cm-3, F(000) = 1332, μ = 1.328 mm-1, R = 0.0353 and w R = 0.0718(Ⅰ 2σ(Ⅰ)). Single-crystal structure analysis reveals that the title complex possesses a 3D network assembled through a multitude of charge-assisted hydrogen bonds between the in situ generated anionic coordination complexes [Zr2(C2O4)7]6- and metal complexes Co(en)33+.     

Bismuth(Ⅲ) Complexes with N,N-Di(2-hydroxylethyl)amino-dithiocarboxylate: Synthesis and Crystal Structure of {Bi[S_2CN(C_2H_4OH)_2]_2[1,10-Phen]_2(NO_3)}·3H_2O and {Bi[S_2CN(C_2H_4OH)_2]_3}_2

Introduction The chemistry of organotin(IV) dithiocarbamate complexes was extensively studied due to their biological activities.1-5 To date, a large number of transition-metal complexes with dithiocarbamate have been synthesized and structurally characterized,6-9 including Ni(S2CNC4H8O)2, Cu(S2CNC4H8)2, Zn(S2CNC4H8O)2 and Fe(S2CNC4H8O)2(DMF). However, the chemistry of main-group metal complexes with dithiocarbamate has been scarcely studied, and few reports have appeared on the s…     

Synthesis and Crystal Structure of [Cu(phen)_2(SO_4)(H_2O)]·0.5C_4H_4O_4·7H_2O

1INTRODUCTION The construction of metal-organic coordination polymers based on covalent interactions[1]or supra-molecular contacts such as hydrogen-bonding and/orπ-πinteractions)[2]is now of great interest not only due to the enormous variety of intriguing structural topologies themselves,but also to their unexpected physical and chemical properties for potential prac-tical applications as functional materials.Many N-containing ligands,such as4,4?-bipyridine,2,2?-bi-pyridine and1,10-phen…     

Synthesis and Crystal Structure of [Ni(C_5H_2N_2O_4)(2,2''''bipy)(H_2O)_2]·H_2O

1 INTRODUCTION Orotic acid (H3dtpc), an important pyrimidine derivative as the effective precursor in the biosynthesis of pyrimidine base of nucleic acids in living organisms, plays a unique role in bioinorganic and pharmaceutical. Aside from the biological interest, orotic acid is also interesting in coordination chemistry. Its ketonic and enolic tautomers along with asymmetric geometry make it to be a very good versatile polydentate ligand[1~5]. The incorporation of metals into supram…     

Synthesis and Crystal Structure of (C_6N_3H_(18))_2Ti_4O_4(C_2O_4)_7·4H_2O

1 INTRODUCTION The open-framework inorganic materials have been synthesized before the early 1980s[1]. Parti- cularly, metal phosphates have been investigated widely during the past few years[2, 3]. In recent years, considerable efforts have been devote…     

Synthesis,Structure and Characterization of a New Complex: [Mn(C_6H_(12)N_4)_2(H_2O)_4][Mn(H_2O)_6][SO_4]_2·6H_2O

A novel complex,[Mn(C_6H_(12)N_4)_2(H_2O)_4][Mn(H_2O)_6][SO_4]_2·6H_2O,was synthesized and hexagonal single crystals with centimeter-scale sizes were obtained by the method of solvent evaporation.It was characterized by elemental analysis,infrared spectrum,thermogravimetric analysis and X-ray single-crystal diffraction.The complex belongs to triclinic crystal system,space group P■ with a=9.3390(8),b=13.3520(13),c=16.3207(13)?,α=100.7160(3)°,β=90.1020(10)°,γ=109.9490(5)°,V=1874.9(3)?~3,Z=2,D_c=1.542 g/cm~3,M_r=870.64,μ=0.876 mm~(-1),T=293(2) K,F(000)=916 and S=0.990.The crystal structure determination displayed a distorted octahedral geometry around the manganese atom,which is bound to two nitrogen atoms from hexamethylenetetramine,acting as monodentate ligands,and to four aqua ligands.Variable-temperature magnetic measurements of the complex indicate the presence of weak antiferromagnetic interaction between manganese centers.     

Synthesis and Crystal Structure of[C_6H_5CH_2C_5H_4ErCl_2(THF)_3]·THF

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｃ_６Ｈ_５ＣＨ_２Ｃ_５Ｈ_４ＥｒＣｌ_２（ＴＨＦ）_３］·ＴＨＦＧａｏＦｕ－Ｘｉｎｇ；ＷｅｉＧｅ－Ｃｈｅｎｇ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ；ＣｈｅｎＷｅｎ－Ｑｉ（ＣｈａｎｇｃｈｕｎＩｎｓｔｉ?..     

4[CuCl(C_5H_5N)_4]·[W_10O_(32)]·2(C_5H_5N)·3H_2O的合成及晶体结构

标题化合物是通过(NH_4)_2WS_4,CuCl_2·2H_2O在吡咤溶液中反应制得。晶体呈蓝色,属三斜晶系,空间群,晶胞参数为:a=13.555(7),b=13.666(5),c=17.860(13),a=69.08(4)°β=87.39(5)°,γ=70.72(4)。V=2907(3),Z=1,D_m=2.56g cm~(-3).结构由Patterson法和Fourier法测出。对5692个收集到的独立衍射数据进行计算,最后R= 0.046.结构测定表明,晶体由W_(10)O_(32)~(4-),[CuCl(C_5H_5N)_4]~+,C_5H_5N和H_2O所组成。W_(10)O_(32)~(4-)的结构见图1,W原子处在O原子的八面体配位中,彼此共边和共顶点相连。[CuCl(C_5H_5N)_4]~+的结构见图2,Cu原子由1个Cl和4个N原子配位,呈略有变形的四方锥形,这种离子是首次报导。C_5H_5N和H_2O填入正负离子堆积的空隙中。     

Synthesis and Structure Investigation of a Transition Metal Ion Bridging Bis(diphosphopentamolybdates),[H_2BIIM]_3[HBIIM]_4[Mn(H_2O)_4(P_2Mo_5O_(23))_2]·7H_2O

A novel transition metal ion bridging bis(diphosphopentamolybdates) has been synthesized and characterized by elemental analysis,IR spectrum,UV spectrum and single-crystal X-ray diffraction.The single-crystal structure analysis shows that the compound consists of seven charge-compensating 2,2'-biimidazole cations (BIIM=2,2'-biimidazole) and one dumbbell-like [Mn(H2O)4(P2Mo5O23)2]10-heteropolyanion which is constructed by two [P2Mo5O23]6-clusters bridged through one [Mn(H2O)4]2+ cation.     

超分子化合物[Ni(C_6H_4O_2N)_2·(H_2O)_4]_n的水热合成及晶体结构

用皮考林酸和六水合氯化镍反应制备了一种三维氢键超分子配合物,经X射线衍射分析确定了单晶结构.该晶体属单斜晶系,P21/m空间群,晶胞参数为:a=0.976 0(2)nm,b=0.522 54(10)nm,c=1.450 1(3)nm,Mr=374.98,α=90.08(3)°,β=90.08(3)°,γ=90°,V=0.739 63(3)nm3,Z=2,ρ=1.684 g/cm3,F(000)=388,μ=1.357 mm-1,R=0.039 0,wR=0.090 8.共收集2 656个衍射数据,其中1 569个为独立衍射点(Rint=0.033 2),可观测点数1 382个(I>2σ(I)).结果表明,在组成该超分子体系的基本结构单元[N i(C6H4O2N)2.(H2O)4]中,N i(Ⅱ)离子形成六配位的稍拉长的八面体构型,配合物单元之间通过氢键相互连接,形成了无限延伸的具有网状结构的三维超分子体系.     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

三价铬丙二酸配合物[Cr(C_3H_2O_4)(H_2O)_4][Cr(C_3H_2O_4)_2(H_2O)_2]·4H_2O的合成、晶体结构及性质研究

在三重桥氧三核铬羧酸配合物的系列研究中,采用与铬的一元羧酸配合物类似的实验条件,以丙二酸为配体合成了不同构型的配合物[Cr(C_3H_2O_4)(H_2O)_4)][Cr(C_3H_2O_4)_2(H_2O)_2]·4H_2O,通过X射线衍射测定了其单晶结构,并对-COO的配位方式作了讨论,还研究了配合物的红外光谱、拉曼光谱、紫外可见光谱、质谱、磁化率等性质,探讨了性质与结构的关系,并由此论证了二元羧酸和铬形成的双齿螯合构型化合物的稳定性.     

Non-Isothermal Decomposion Kinetics of Supermolecule Compound [Eu(C_(10)H_9N_2O_4)(C_(10)H_8N_2O_4)(H_2O)_3]_2·phen·4H_2O

Europium(Ⅲ) compound with 2-oxopropionic acid salicyloyl hydrazone (C_(10)H_(10)N_2O_4,H_3L) and 1,10-phenan-throline (C_(12)H_8N_2,phen) has been prepared.A yellow prismatic crystal of the compound was obtained,and themolecule crystallized in the triclinic space group P-1.There are two 9-coordinated complex molecules in everystructure unit,where every Eu atom is coordinated by three water molecules and two tridentate C_(10)H_(10)N_2O_4 ligands,forming two stable pentacycles.The coordination polyhedron around Eu~(3+) was described as a single cap squareantiprism.In the crystal cell,there are one free 1,10-phenanthroline and four water molecules.The thermaldecomposition of the compound and its kinetics were studied by non-isothermal thermogravimetry.The Kissinger'smethod and Ozawa's method were used to calculate the activation energy value of the first-step decomposition.Thestages of the decompositions were identified by TG-DTG-DSC curve.The non-isothermal kinetic data were ana-lyzed by means of integral and differential methods.The possible reaction mechanism and the kinetic equationswere investigated by comparing the kinetic parameters.     

Synthesis, Spectroscopic Properties and Crystal Structure of (C_4N_2H_(12))_2Zr(C_2O_4)_4·H_2O

1 INTRODUCTION The researches on transition metal coordination complexes have been rapidly expanded because of their fascinating structural diversity and potential applications[1～4]. As we know, zirconium oxalates can be used as precursors in the synth…