吡唑铜(Ⅱ)配合物的合成、晶体结构及性质

本文报道了Cu(Ⅱ)的吡唑和硫氰酸根混合配体配合物[Cu(pz)₄(NCS)₂](1)(pz=吡唑)的合成、晶体结构及性质.配合物属单斜晶系,C2/c空间群,a=1.1520(4) nm,b=1.2247(4) nm,c=1.4188(5), β=106.747(8)°, Z=4, R₁=0.0554, wR₂=0.1420.配合物中Cu(Ⅱ)与4个吡唑环上的4个N原子及2个NCS^-的N原子配位形成4+2型拉长八面体配位环境,4个吡唑环上的N原子占据赤道位置, 2个NCS^-的N原子占据轴向位置.对配合物的IR、UV-Vis、ESR进行表征和分析.比较不同轴向配体对结构和性质的影响.     

新型离子型配合物的合成、晶体结构及性质

利用水热法合成了4-(N,N′-双(4-羧基苄基)氨基)苯磺酸（H₃L）的两个离子型配合物：[Mn(phen)₂(H₂O)₂]?(HL)?(H₂O)₄（1）和[Zn(phen)₂(H₂O)₂]?(HL)?(H₂O)₆（2, phen =邻菲罗啉）,其结构经FL、 IR、元素分析、X-射线单晶衍射、 X-射线粉末衍射和TG表征。结果表明：化合物1属于单斜晶体,P2₁/c空间群,晶胞参数a=11.997(1) Å, b=22.978(1) Å, c=18.093(1) Å, β=92.749(3)°, V=4981.8(3) ų, Z=4。化合物2属于单斜晶体,P2₁/c空间群,晶胞参数a=11.861(1) Å, b=22.816(1) Å, c=18.251(1) Å, β=92.832(5)°, V=4932.8(5) ų,Z=4。化合物2有较好的荧光性质;初始分解温度为80 ℃。      

硫酸根和碳酸根桥联的双核铁(Ⅲ)配合物晶体结构及紫外-可见光谱研究

室温下合成了硫酸根和碳酸根桥联的双核铁()配合物{2[(TPA)₂Fe₂O(SO₄)](ClO₄)₂·1.5H₂O(1),[(TPA)₂Fe₂O(CO₃)](ClO₄)₂·CH₃OH(2)},并用X射线衍射测定了其晶体结构.结果表明,配合物1为单斜晶系,空间群为P2₁/c,a=1.150(2)nm,b=2.659(5)nm,c=2.933(5)nm,β=99.40(3)°,R=0.0564,wR=0.1106.配合物2为单斜晶系,空间群为P2₁/c,a=1.1368(3)nm,b=1.8280(5)nm,c=2.0542(5)nm,β=94.867(5)°,R=0.0567,wR=0.1362.研究了室温下的紫外-可见光谱性质.     

Structure and Photophysical Properties of an Upconversion Holmium-mercury Compound with a 2-D Layer-like Motif

Using a hydrothermal reaction,a novel holmium-mercury compound{[Ho(IA)(HIA)₂(H2 O)₂]_2-(Hg₃Br₈)}n(nHgBr₂)·2 nNO₃(1,HIA is isonicotinc acid)was synthesized and its crystal structure was characterized by single-crystal X-ray diffraction.Compound 1 crystallizes in monoclinic system,space group P2/c with a=13.0647(6),b=9.4659(3),c=26.0832(14)?,β=97.522(4)°,V=3197.9(2)?³,C₃₆H₃₆Br₁₀Hg₄Ho₂N₈O₂₂,M_r=2863.95,Z=2,D_c=2.974 g/cm³,μ(Mo Kα)=18.331 mm^–1 and F(000)=2575.It displays a two-dimensional(2 D)layer-like structure.A solid-state photoluminescence experiment revealed that it shows upconversion green emission.The emission peaks should come from the ⁵I₈→⁵G₆ and ⁵S₂→⁵I₈ characteristic emission of the 4 f electrons of the Ho3+ion.Compound 1 has a CIE chromaticity coordinate(0.1774,0.526).A solid-state UV-visible diffuse reflectance spectrum unveiled that this compound has a wide optical band gap of 3.26 eV.     

具有开放骨架结构氟化磷酸钛的水热合成及分子动力学辅助确定骨架中模板剂的位置

在水热体系中,制备了一个具有三维开放骨架结构的氟化磷酸钛化合物Ti₄(PO₄)4(HPO₄)₂F₂.[(CH₃)₂N(CH₂)₂NH₃][H₃O](简称TP-J3J=Jilinuniversity).用X射线粉末衍射、元素分析、热重分析和X射线单晶衍射对其进行了表征.单晶结构分析表明,该化合物属于三斜晶系,P1空间群,晶胞参数a=0.6353(1)nm,b=0.8699(2)nm,c=1.1069(2)nm,α=93.94(3),β=90.13(3),γ=107.96(3),V=0.5804(2)nm³,Z=2,R₁=0.0391,wR₂=0.0959,GOF=1.052.TP-J3的骨架结构可以看作是由次级结构单元(SBU)[Ti₂(PO₄)₂(HPO₄)F]通过氧桥共顶点相连构筑而成的,在a和c方向形成了两种不同的八元环孔道,两种孔道相互交叉,形成了一种“类笼”结构.通过计算模拟确定双质子化的模板剂存在于“类笼”中,模板剂与骨架原子之间存在强烈的氢键作用,可稳定骨架的结构.     

三苄基和三丁基锡4-吡啶甲酸酯聚合物的合成、性质及晶体结构

用三苄基氯化锡及三丁基氯化锡与4-吡啶甲酸钠反应,分别合成了三苄基锡4-吡啶甲酸酯(1)和三丁基锡-4-吡啶甲酸酯(2),并进行了红外光谱、核磁共振氢谱及质谱表征.X射线单晶衍射分析结果表明,化合物1属单斜晶系,P2₁/n空间群,晶胞参数:a=0.96564(8)nm,b=1.64085(14)nm,c=1.49403(13)nm,β=97.681(2)₀,V=2.3460(3)nm₃,Z=4,D_c=1.456g/cm³.化合物2属单斜晶系,P2₁/n空间群,晶胞参数:a=0.96673(14)nm,b=2.3845(4)nm,c=0.97071(14)nm,β=112.463(3)o,V=2.0679(5)nm₃,Z=4,D_c=1.324g/cm³.两个化合物均通过4-吡啶甲酸配体的氮原子桥联,形成五配位三角双锥构型的一维无限链聚合物.     

钒氧多酸桥联大环铜配合物的合成及其晶体结构

以大环铜配合物［CuL］(ClO₄)₂(L=5,7,7,12,14,14-六甲基-1,4,8,11-四氮杂环十四-4,11-二烯)与NH₄VO₃反应合成了一个新的钒氧多酸桥联大环铜配合物［CuL］₂［H₂V₁₀O₂₈］·7H₂O(1),其结构经IR,元素分析和X-射线单晶衍射表征。1（CCDC: 1510831）属单斜晶系,P2(1)/n空间群,晶胞参数a=11.512(3) , b=18.170(4) , c=14.534(3) , β=102.997(4)°, V=2 962.3(11) ³, Dc=1.986 mg·cm^-3, Z=2, μ=2.300 mm^-1, R₁=0.047 2, wR₂=0.118 2。     

A New Borate-phosphate Compound CsNa2Lu2(BO3)(PO4)2:Crystal Structure and Tb3+ Doped Luminescence

Composite borate-phosphate compounds have always attracted much attention for their structure diversity and interesting properties.In this work,a new borate-phosphate Cs Na₂Lu₂(BO₃)(PO₄)₂ (CNLBP) was found for the first time and its structure was characterized by single-crystal X-ray diffraction method.It crystallizes in orthorhombic system,space group Cmcm with a=6.8750(5),b=14.6919(1),c=10.5581(7)?,V=1066.44(1)?³,Z=4,M_r     

新型氮杂环卡宾银(I)配合物的合成及其晶体结构

以取代苄氯(1a~1c)为起始原料,与咪唑经氮烷基化反应制得苄基咪唑氯盐(2a~2c); 2a~2c与氧化银经原位去质子化反应合成了3种新型的氮杂环卡宾银配合物--(NHC)AgCl［NHC: 1,3-二(4-甲氧基苄基)咪唑-2-亚基(3a), 1,3-二(3-甲氧基苄基)咪唑-2-亚基(3b)］和［(NHC)AgCl]₂［NHC=1,3-二(4-氯苄基)咪唑-2-亚基(3c)］,其结构经¹H NMR, ¹³C NMR, IR,元素分析和X-射线单晶衍射表征。3a~3c单晶结构均属单斜晶系,3a为P2₁/n空间群,3b和3c为P2₁/c空间群,3a和3b为单核银配合物,3c为双核银配合物。     

配合物[Co(NH3)5Br]Br2的精密X射线粉末衍射与指标化研究

以多晶衍射中的从头结构测定对其数据收集与处理的要求为依据, 获得[Co(NH₃)₅Br]－Br₂配合物的精密X射线粉末衍射谱的方法, 总结了指标化实验中的问题与对策, 得到标题配合物的正交晶系(空间群为Pnma或Pn2₁a), 晶胞参数:a=1.3710(1)um, b=1.0715(1)um, c=0.6947(1)um, V＝1.0206(1)um₃, Z＝4, D_x＝2.50g·cm^-3, F_{30＝81(0.0071, 52), M20＝41.}     

Hydrothermal Synthesis and Structure of [CH_3NH_3]_2[(V~ⅣO)_2(V~ⅤO_4)_2]: A New Layered Mixed-valence Vanadium Oxide Incorporated with Organic Cations

IntroductionLayered intercalation compounds haveattracted increasing research attention due to theirapplications in diverse areas,for instance,some ofthem are used as rechargeable batteries,heterogeneous catalysts,and an exchange[1— 12 ] . Inprevious literatures,several layered mixed- valencevanadium oxides were reported,such as VO2 · 1 /2 H2 O[13 ] ,[H2 N( CH2 ) 4 NH2 ]V4O9[14 ] ,NH4V3 O8[15] ,( C6H14 · N2 ) V6O14 · 1 / 2 H2 O[16] ,[HN( C2 H4) 3 NH]V6O14 [17] ,NMe4V6O14 [18]…     

镧系四元混配化合物[Ln(BA)2(NO3)(phen)]2的合成、晶体结构和波谱研究

在酸性介质、含水溶剂中合成了四元混配化合物[Ln(BA)₂(NO₃)(phen)]₂(BA=苯甲酸根;Ln=La,Ce,Pr,Nd,Sm,Eu,Dy,Gd,Tb,Er),用元素分析、IR、DTA-TG等方法对配合物进行了表征.研究了配合物的顺磁性能和荧光性能.镨配合物的单晶衍射结果表明,配合物属三斜晶系,双核,Pr³⁺的配位数为9,4个BA呈二种配位方式,丰富了四元配合物的结构表现形式.     

Solvothermal Synthesis, Structural Characterization and Properties of Two New Layered Lanthanide Sulfates

Two new layered lanthanide sulfates,[C₁₀H₁₀N₂][Pr₂(SO₄)₄(H₂O)₂](1)and[H₅O₂][Sm(SO₄)₂(H₂O)₃](2)were synthesized via solvothermal reaction and structurally characterized by single-crystal X-ray diffraction(XRD), infrared(IR) spectroscopy, thermal analysis, fluorescent spectra and inductively coupled plasma(ICP). Crystal data for compound 1, triclinic, P space group, a=0.8052(4) nm, b=0.9438(4) nm, c=1.4990(7) nm, α=79.450(5)°, β= 83.703(5)°, γ=74.048(5)°, V=1.0746(9) nm³, Z=2; for compound 2, monoclinic, P2₁/c space group, a=0.6599(11) nm, b=1.8940(3) nm, c=0.8765(14) nm, β=96.596(2)°, V=1.0883(3) nm³, Z=4. Structure analysis indicates that both the compounds exhibit a 2D corrugated layer structure, with protonated 4,4'-bipyridine cations and water dimmers (H₅O₂)⁺ located between the inorganic layers of compounds 1 and 2, respectively. Luminescent properties of compounds 1 and 2 were further investigated.     

锕系元素冠醚配合物研究(Ⅲ)——二水合硝酸铀酰苯并-15-冠-5配合物的晶体结构

锕系元素冠醚配合物中,研究得最多的是铀酰与冠醚形成的配合物,以往的工作主要集中在配合物的合成及性质研究方面,而对其结构很少研究。迄今为止,只测定过硝酸铀酰与18-冠-6配合物的晶体结构,铀酰与其它种类冠醚形成的配合物的结构文献中还未见报道。我们在乙腈溶液中培养出硝酸铀酰与苯并-15-冠-5的配合物[UO_2(NO_3)_2(H_2O)_2]·(B15C5)单晶,并研究该配合物的晶体及分子结构。     

Studies on α-Methacrylate Copper(Ⅱ) Complexes with Imidazole

Two complexes of α-methacrylate copper(Ⅱ) with imidazole, Cu[CH₂=C(CH₃)COO]₂· (imH)₂(1) and Cu ₂[CH₂C(CH₃)COO]₄(imH)₂(2) were prepared and characterized. The single crystal X-ray diffraction study of complex 1 showed that the copper(Ⅱ) atom in the symmetric centre of the square planar environment was coordinated by two monodentate α methacrylate groups and two imidazole ligands that were in trans position with each other. Each molecular unit is linked with four neighbouring units by means of hydrogen bond interactions, forming a two-dimensional supermolecular compound( d_N…O =0.278 1 nm). Complex 1 crystallizes in monoclinic, space group P2₁/n with a =1.023 94(12) nm, b =0.842 94(8) nm, c =1.079 35(10) nm, β=117.231(7)°, Z =2. The forming mechanism of the complexes was discussed.     

杂氮硅三环化合物(Ⅰ)和(Ⅱ)晶体结构的研究

杂氮硅三环化合物Ⅰ和的分子结构用直接法解,经全矩阵最小二乘修正,得到它们的晶体学参数。并对它们的结构进行了比较和讨论。     

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.     

一氯甲酸甲酯二-三苯基膦合铂络合物晶体结构、分子结构的研究

本文确立一氯甲酸甲酯二-三苯基膦合铂络合物是浅黄透明晶体,属于单斜晶系,P2₁/n空间群.并测定了晶胞参数.分子式为Pt[P(C₆H₅)₃)]₂·COOCH₃Cl,该化合物是配位键结合的新型络合物.     

F-(H2O)n(n=1～4)体系的结构、偶极矩、极化率和一阶超极化率的从头计算

用MP2方法得到F^-(H₂O)_n(n=1～4)体系的优化几何结构.依据优化结构计算偶极矩μ₀、极化率α₀、各向异性极化率Δα和一阶超极化率β₀,研究了基组效应.讨论了溶剂水分子数、溶剂水分子排布及溶剂层数变化诸因素对体系超极化率等性质的影响.     

The Synthesis and Structure of Tris-nitrato-Aqua-(2,6-Diacetyl-Pyridine) Bis (semicarbazone)lanthanum(III)

The complex of (La(DAPSC)(NO3)3 H2O) · H2O was prepared. Its crystal data are: triclinic, space group P- , a =8.736(1), b = 12.108(3), c =12.412(3)(A) , α=110.35(2)°, β =94.88(1)°, γ = 95.35(2)°, v =1215.78(A)3 , Z =2.It was found that two arms of the ligand DAPSC can be opened to accept the La(Ⅲ). This is obviously different from the complex of Sm(Ⅲ) with DAPSC. DAPSC can be expanded easily, but it is hard to be compressed.