金属硫族化合物[Ni(en)3](Hen)SbSe4,[Sb(en)3]In3Te7的溶剂热生长及晶体结构

以溶剂热生长技术(Solvothermal technique)在180 C下以氯化物与具有氧化性的M 2Q(M=K,Rb;Q=Te,Se)反应,制备出新的硫族化合物[Ni(en)3](Hen)SbSe4(1),[Sb(en)3]In3Te7(2).化合物1的阳离子基团为过渡金属Ni与乙二胺(en)的配合物[Ni(en)3]2+及质子化的[Hen]+阳离子,阴离子基团为具有分立结构的[SbSe4]3-.化合物2的阳离子基团为[Sb(en)3]3+,阴离子基团为具有二维结构的2∞[In3Te7]3-.单晶X射线衍射结果表明,晶体1属三斜晶系,P1空间群,晶胞数据a=0.881 43(18)nm,b=0.962 35(19)nm,c=1.427 8(3)nm,α=104.74(3)°,β=92.47(3)°,γ=109.55(3)°,V=1.092 7(4)nm3,Z=2.晶体2属单斜晶系,P21/c空间群,晶胞数据:a=1.069 1(2)nm,b=1.693 2(3)nm,c=1.515 2(3)nm,α=90°,β=94.86(3)°,γ=90°.V=2.732 8(9)nm3,Z=4.     

有机杂化硫代碲酸盐化合物(H_2en)TeS_3和[Ni(en)_3]TeS_3的溶剂热合成与表征

用低温溶剂热法合成了2种分立结构的有机杂化硫代碲(Ⅳ)酸盐化合物(H2en)TeS3(1)和[Ni(en)3]TeS3(2)(en=乙二胺),通过X-射线单晶衍射,红外光谱,元素分析等手段对它们的结构进行了表征。晶体结构解析结果表明:2个化合物均属单斜晶系,空间群分别为P21和P21/c。化合物1和2具有孤立三角锥[TeS3]2-阴离子,化合物1的平衡阳离子为双质子化乙二胺[H2en]2+,阴离子基团[TeS3]2-和阳离子基团[H2en]2+之间通过N-H…S氢键连接。化合物2的阳离子基团为过渡金属Ni与乙二胺的配合物[Ni(en)3]2+。另外,对该2种晶体进行了紫外-可见漫反射光谱测试和热重分析。     

[Cu(en)_2]~(2+)修饰的二维仲钨酸化合物:[{Na_3(H_2O)_(10)}_2H_2{Cu(en)_2(H_2W_(12)O_(42))}]·16H_2O(英文)

利用水热合成法制备了一种基于[Cu(en)2]2+修饰的仲钨酸化合物:[{Na3(H2O)10}2H2{Cu(en)2(H2W12O42)}].16H2O(en=乙二胺)(1),借助元素分析、X射线单晶衍射分析I、R、UV、热分析和X射线光电子能谱对这种化合物进行了结构和性质研究.化合物(1)属于三斜晶系,P-1空间群.晶胞参数为:a=1.183 2(5)nm,b=1.296 0(6)nm,c=1.416 9(6)nm,α=63.348 0(10)°,β=82.844 0(10)°,γ=68.907 0(10)°,V=1.810 0(14)nm3,Z=1,R1[I2σ(I)]=0.024 7,wR2[I2σ(I)]=0.058 2.化合物(1)通过仲钨酸阴离子,铜离子和[Na3(H2O)10]3+三核簇形成了新型的二维层状结构.     

以有机溶剂热生长技术制备金属硫族化合物[Mn(en)_3]PdSe_2及其晶体结构分析

以有机溶剂热生长技术 (solvothermaltechnique) ,即在 180℃乙二胺 (en)溶液中 ,以MnCl3,PdCl2 ,K2 Se在密闭容器中反应 7d ,制备出新的硫族化合物 [Mn(en) 3]PdSe2 ,其阴离子基团为 [PdSe2 ]2 -,阳离子基团为过渡金属Mn与乙二胺 (en)的配合物 :[Mn(en) 3]2 +.以单晶X射线衍射技术解得该晶体结构属正交晶系 ,空间群为Pbcn ,[Mn(en) 3]·PdSe2 (Ⅰ )的晶胞数据 :a =1.1484( 2 ) ,b=1.5 0 5 7( 3 ) ,c =0 .93 62 2 ( 19)nm ,Z =4.     

以有机溶剂热生长技术制备金属硫族化合物 [Mn(en)~3]PdSe~2及其晶体结构分 析

以有机溶剂热生长技术(solvothermaltechnique),即在180℃乙二胺(en)溶液中,以MnCl~3,PdCl~2,K~2Se在密闭容器中反应7d,制备出新的硫族化合物[Mn(en)~3]PdSe~2,其阴离子基团为[PdSe~2]^2^-,阳离子基团为过渡金属Mn与乙二胺(en)的配合物：[Mn(en)~3]^2^+。以单晶X射线衍射技术解得该晶体结构属正交晶系,空间群为Pbcn,[Mn(en)~3]PdSe~2(Ⅰ)的晶胞数据：a=1.1484(2),b=1.5057(3),c=0.93622(19)nm,Z=4。     

[(enH)_2(enH_2)Sn_2Se_6]的合成、结构及性能研究

采用溶剂热法 ,以K2 Se∶SnCl2 ·2H2 O∶Se∶en =1∶1∶4∶48的摩尔比 ,在 15 0℃下反应 5d ,生成黄色透明柱状晶体[(enH2 ) 2 Sn2 Se6·en] .该晶体属于三斜晶系 ,空间群为P 1,晶胞参数 ,a =0 865 9( 2 )nm ,b =1 10 5 5 ( 2 )nm ,c =0 663 60 ( 10 )nm ,α =10 4 44 ( 3 )° ,β =110 93 ( 3 )° ,γ =79 74( 3 )° ,V =0 5 7198( 19)nm3 ,Z =1.[(enH) 2 (enH2 )Sn2 Se6]晶体由质子化的乙二胺正离子 (enH) + ,(enH2 ) 2 + 和二聚硒代锡酸根负离子 (Sn2 Se6) 4 -堆积而成 .在AxSn2 Se6系列化合物 ,正离子A的大小对晶体结构的类型产生重要的影响 .研究表明 ,此晶体具有 1 76eV的能隙 (Eg) ,是个半导体 ,对太阳辐射具有选择吸收特性 ,在温度低于 180℃时是稳定的 .     

[M(en)3]2Sn2Se6(M=Mn,Zn)的制备及其热稳定性

用有机溶剂热生长技术(SolvothermalTechnique)制备过渡金属锰和锌硒化物[Mn(en)3]2Sn2Se6(Ⅰ),[Zn(en)3]2Sn2Se6(Ⅱ).用单晶X射线衍射技术对其进行晶体结构分析.[Zn(en)3]2Sn2Se6样品的热分析结果表明,该化合物的热分解分三步进行.光学性质测试表明它们是半导体材料,[Mn(en)3]2Sn2Se6的能带隙为1.76eV.[Zn(en)3]2Sn2Se6的能带隙为2.49eV.     

Cu(en)_2Ag(SCN)_3的晶体结构

Cu(en)_2Ag(SCN)_3系棱柱状蓝紫色晶体,晶胞参数:a=7.126(2),b=12.587(5),c=17.585(5);空间群为P2_12_12_1;Z=4;ρobs.=1.90,ρcalc.=1.96克/厘米~3。在CAD-4四圆衍射仪上收集到1430个独立衍射点。晶体结构由三维Patterson函数和电子密度函数解出,经全矩阵最小二乘方精修,偏离因子R=0.036。结构分析的结果表明,晶体中的Ag原子由硫氰酸根的S原子按畸变四面体方式配位,其中有二个S原子分别为相邻两个Ag原子所共有,从而使一个一个的AgS_4四面体共有顶点,沿着α轴方向无限延伸。Cu原子系四方单锥配位,由两个乙二胺的N原子形成平面正方形配位(Cu—N_(en)=1.998～2.024);另外,一个SCN的N原子处在正方形的上方,形成Cu原子的四角锥构型,其与Cu原子的距离略长些(Cu—N_(SCN)=2.388)。     

金属碲化物[Ga(en)~3]In~3Te~7晶体结构和性质的研究

以有机溶剂热生长技术(solvothermaltechnique),即在180℃乙二胺(en)溶液中,以GaCl~3,InCl~3,Rb~2Te和Te在密闭容器中反应7d,制备出新的硫族化合物[Ga(en)~3]In~3Te~7。其阴离子基团为Zintlanion:~∞^2[In~3Te~7]^3^-,阳离子基团为Ga与乙二胺(en)的配合物:[Ga(en)~3]^3^+。以单晶X射线衍射技术解得该晶体结构属单钭晶系,空间群为P2~1/c,(no.14),{Ga(en)~3]In~3Te~7的晶胞数据：a=1.0460(2)nm,b=1.6981(3)nm,c=1.4994(6)nm,α=90°,β=95.46(2)°,γ=90°,V=2.651(1)nm^3,Z=4。热分析结果表明,该化合物的热分解分三步进行。光学性质测试表明它们是半导体材料,禁带宽度为1.65eV。     

二维钨-钒簇聚物[Cu(en)_2]_2·[W_(4.5)~ⅥW_2~ⅤV~ⅤV_(9.5)~ⅣO_(44){Cu(en)_2(H_2O)}_2]·3H_2O的合成与表征

采用水热法合成了一个钨-钒簇聚物[Cu(en)2]2[WⅥ4.5WⅤ2VⅤVⅣ9.5O4 4{Cu(en)2(H2O)}2]·3H2O(1,en=乙二胺),并通过X射线单晶衍射、元素分析、傅里叶变换红外光谱、X射线粉末衍射、热重分析、价键计算、X射线光电子能谱、电子顺磁共振和磁性分析对其结构和性能进行了表征.结果表明,化合物1是以双支撑的四帽Keggin结构[WⅥ4.5WⅤ2VⅣ9.5O4 0(VⅤO4){Cu(en)2(H2O)}2]4-钨-钒簇合物阴离子为基本结构单元,与4个[Cu(en)2]2+配合物阳离子以共价键和弱键相连接形成二维层状结构,相邻层又通过氢键连接成三维超分子网络.研究了化合物1的磁性及光催化降解罗丹明B的活性.     

Solvothermal Syntheses and Characterization of Three One-dimension Cadmium Selenidoarsenates [Ni(1,2-dap)3][As2CdSe4],[Zn(1,2-dap)3][As2CdSe4] and [Ni(en)3][As2CdSe4]

Three new cadmium selenidoarsenates,[Ni(1,2-dap)3][As2CdSe4](1)(1,2-dap=l,2-diaminopropane),[Zn( 1,2-dap)3][As2CdSe4](2) and [Ni(en)3][As2CdSe4](3)(en=ethylenediamine), were synthesized under solvothermal conditions. And they are isostnictural and monoclinic crystalls. As seen from their structures, they exhibited one-dimensional(1D) chains composed of [As2CdSe4]^2- anions and [TM(amine)3]^2+(TM=Ni,Zn;amine=1,2-dap, en) cations. Their absorption edges are 2.32, 1.84 and 2.38 eV and they show the properties of the semiconductor. These compounds were also characterized by means of single-crystal X-ray ditlraction(XRD), powder X-ray diflraction (PXRD), solid-state optical absorption spectrometry, and so on.     

Solvothermal Synthesis and Crystal Structure of [H2N（CH2）2NH3]{Co[H2N（CH2）2NH2]3}[SbSe4]

1 INTRODUCTION The chalcogenidometallates with open frame- works have attracted considerable interest as pos- sible zeolite-like materials, of which highly interes- ting properties could be expected. Over the last de- cades a large number of thioanti…     

[(enH)2(enH2)Sn2Se6]的合成、结构及性能研究

采用溶剂热法,以K2Se:SnCl2·2H2O∶Se∶en=1∶1∶4∶48的摩尔比,在150 ℃下反应5d,生成黄色透明柱状晶体[(enH2)2Sn2Se6·en]。该晶体属于三斜晶系 ,空间群为Pl^-,晶胞参数,a=0.8659(2)nm,b=1.1055(2)nm,c=0.66360(10)nm, a=104.44(3)°,β=110.93(3)°,γ=79.74(3)°,V=0.57198(19)nm^3,Z=1.[ (enH2)Sn2Se6]晶体由质子化的乙二胺正离子（enH)^+,(enH2)^2+和二聚硒代锡根 负离子（Sn2Se6)^4-堆积而成。在AxSn2Se6系列化合物,正离子A的大小对晶体结 构的类型产生重要的影响。研究表明,此晶体具有1.76eV的能隙（Eg）,是个半导 体,对太阳辐射具有选择吸收特性,在温度低于180℃时是稳定的。     

Combination of lacunary polyoxometalates and high-nuclear transition-metal clusters under hydrothermal conditions. 5. A novel tetrameric cluster of [{Fe(II)Fe(III)(12)(mu(3)-OH)(12)(mu(4)-PO(4))(4)}(B-alpha-PW(9)O(34))(4)](22)(-)

A novel tetrameric cluster, (enH2)3.5H15[{FeIIFeIII12(mu3-OH)12(mu4-PO4)4}(B-alpha-PW9O34)4].83H2O (1; en = ethylenediamine), has been hydrothermally synthesized and characterized by IR, optical diffuse reflectance, thermogravimetric analysis, and single-crystal X-ray diffraction. The skeleton of 1 is composed of four tri-FeIII-substituted [FeIII3(mu3-OH)3(B-alpha-PW9O34)]3- Keggin moieties fused together through a FeII2O2 unit and four mu4-PO4 bridges, resulting in a unique tetramer with C2 symmetry. Magnetic measurements indicate that 1 reveals the antiferromagnetic interactions between FeII and FeIII centers.     

From one-dimensional chains to three-dimensional networks: solvothermal synthesis of thiogallates in ethylenediamine

Five new thiogallates have been prepared solvothermally in the presence of ethylenediamine and characterized by single-crystal X-ray diffraction, thermogravimetry, and elemental analysis. [enH2][Ga4S7(en)2] (1), which crystallizes in the monoclinic space group P2(1)/c with lattice parameters a = 12.8698(12) angstroms, b = 10.4812(9) angstroms, c = 16.5473(14) angstroms and beta = 102.457(4) degrees (Z = 4), exhibits a layered structure in which both covalently and hydrogen-bonded template molecules coexist. The structures of [M(en)3](0.5)[GaS2] (M = Mn (2) (orthorhombic, Cmcm, a = 9.5555(6) angstroms, b = 15.0696(10) angstroms, c = 12.2893(7) angstroms, Z = 8) M = Co (3) (orthorhombic, Cmcm, a = 9.4660(7) angstroms, b = 15.0990(11) angstroms, c = 12.2540(8) angstroms, Z = 8), M = Ni (4) (orthorhombic, Cmcm, a = 9.4510(10) angstroms, b = 15.1416(15) angstroms, c = 12.2387(11) angstroms, Z = 8)) and Mn(en)2Ga2S4 (5) (monoclinic, C2/c, a = 14.3002(11) angstroms, b = 7.9509(5) angstroms, c = 12.1184(6) angstroms, beta = 100.191(4) degrees , Z = 4) are closely related and contain one-dimensional [GaS2]- chains, which are separated by [M(en)3]2+ counterions in 2, 3, and 4, and linked into a three-dimensional structure by [Mn(en)2]2+ units in 5.     

A novel polyoxovanadium borate incorporating an organic amine ligand: synthesis and structure of [V12B16O50(OH)7(en)]7-

A novel 1D chain organic-inorganic hybrid polyoxovanadium borate Na[V(12)B(16)O(50)(OH)(7)(en)](2)(enH(2))(6)(enH)(2)(OH)(H(2)O)(19) (1, en = ethylenediamine), based on a [V(12)B(16)O(50)(OH)(7)(en)](7-) cluster unit, has been hydrothermally synthesized and characterized. Interestingly, organic amine is incorporating into the V(12)B(16) clusters.     

Syntheses, Crystal Structures and Thermal and Optical Properties of Two Organic Templated Gallium Antimony Sulfides

Two new gallium antimony sulfides,[enH2][Ga2Sb2S7]·en(1) and [puH]2[Ga2Sb2S7](2)(en = ethylenediamine,pu = propyleneurea),have been solvothermally synthesized.In the pre-paration of compound 2,the protonated propyleneurea cation as counterion and template was in situ synthesized by the reaction of 1,3-diaminopropane with CO2 in pyridine.Both structures contain a two-dimensional network composed of novel heterometallic clusters of {Ga2Sb2S9} as the second-dary building unit.The thermal and optical properties of compounds 1 and 2 were characterized by TGA and UV-Vis,respectively.     

Solvothermal synthesis of three new dimeric thiogermanates (enH)4Ge2S6, [Mn(en)3]2Ge2S6 and [Ni(en)3]2Ge2S6 from germanium dioxide and sulfur powder

Three new thiogermanates (enH)₄Ge₂S₆ (1) and [M(en)₃]₂Ge₂S₆ (M=Mn (2), Ni (3); en=ethylenediamine) were synthesized using GeO₂ and S₈ as starting materials in molar ratio of 1:0.5 under solvothermal conditions. These compounds suggest that the dimeric [Ge₂S₆]⁴⁻ anion is likely to be the main germanium-containing species in en system and it also might be preferred as counter anions by the transition metal complex cations in crystallization. The cations of [Mn(en)₃]²⁺ and [Ni(en)₃]²⁺ are even better mineralizers than the protonated amine of [enH]⁺. The crystal systems of [Ge₂S₆]⁴⁻ compounds are related to entities of cations and intermolecular reactions between cations and [Ge₂S₆]⁴⁻ anions. The compounds remove ethylenediamine and H₂S molecules in multi steps when being heated under nitrogen stream.     

Solvothermal Synthesis and Crystal Structure of Zn（en）3 B5O7（OH）3

Introduction Boratecompounds,inwhichboronisboundonly tooxygen,areofconsiderablemineralogicalandindus trialimportance.Thesecompoundscontaininganionic componentscomposedofBO3andBO4groups,which maybelinkedtogetherbysharingoxygenatoms,can formisolatedringsand…     

Crystal structure and EPR studies of doped Cu2+ ion in [Zn(sac)2(en)2] single crystal

The tran-bis(ethylenediamine)bis(saccharinato)Zinc(II), [Zn(sac)₂(en)₂] (ZSED), (en: ethylenediamine and sac: saccharinate) complex has been synthesized and its crystal structure has been determined by X-ray diffraction analysis. The compound crystallizes in space group P2₁/c. The Zn(II) ion is hexa-coordinated by four nitrogens of two bidentate en ligands composing the basal plane and two nitrogen atoms from the monodentate two sac ligands (N-bonded) occuping the axial sites, adopting an elongated octahedral sphere. Both en and sac ligands occupy the trans positions of the coordination octahedron. The Zn(II) ion in title compound sits on a inversion centre and is octahedrally coordinated two bidentate en (ethylenediamine) and two sac (saccharinate) (N-bonded) ligands. The magnetic environments of Cu²⁺ doped [Zn(sac)₂(en)₂] complex have been identified by electron paramagnetic resonance (EPR) technique. Cu²⁺ doped ZSED single crystals have been studied at room temperature in three mutually perpendicular planes. The calculated results of the Cu²⁺ doped ZSED indicate that Cu²⁺ ion contains two magnetically inequivalent Cu²⁺ sites in distinct orientations occupying substitutional positions in the host lattice and show very high angular dependence.