{Cu[H_2NC(CH_2OH)_3]_2}{Pic}_2·H_2O的合成与晶体结构

三羟甲基氨基甲烷与苦味酸(Pic)铜在乙醇水混合液中反应,制得少见的不对称氢键连接的超分子化合物{Cu[H2NC(CH2OH)3]2}{Pic}2?H2O。晶体属三斜晶系,空间群为P ,晶胞参数为a = 6.894(1),b = 8.219(1),c = 13.543(3) ? ?= 79.290(1),?= 8 3.36(2), ?= 84.590(1)埃轿狢20H30CuN8O22,V = 746.9(2) 3,Z = 1,Dc = 1.774 g/cm3,F(000) = 411,?= 0.844 mm-1,R = 0.0334,Rw = 0.0863。在配合物的结构单元中, Cu2+位于对称中心,分别与2个四齿配体(三羟甲基氨基甲烷)中的2个OH,1个NH2,三齿配位,呈笼状螯合。而另一个OH,因配体和中心离子构型的限制,不参与配位。     

[NiCl(Ph_2PCH_2CH_2OH)_2Cl·H_2O]~+Cl~-和[Ni(Ph_2P(O)CH_2CH_2OH)_4]~(2+)[NiCl_4]~(2-)的合成及晶体结构

通过NiCl2·6H2O与双齿配体2-(二苯基膦)乙醇(Ph2PCH2CH2OH)或其氧化物2-(二苯基氧膦)乙醇[Ph2P(O)CH2CH2OH]的反应,制得两种结构新颖的阳离子型镍配合物[NiCl(Ph2PCH2CH2OH)2 (H2O)]+Cl-(1)和[Ni(Ph2P(O)CH2CH2OH)4]2+[NiCl4]2-(2).通过元素分析、31P核磁共振及X射线单晶衍射对配合物1和2的结构进行了表征.配合物1的晶体属单斜晶系,C2/c空间群,中心金属Ni具有六配位八面体几何构型.配合物2属四方晶系,I4(1)/a空间群,中心原子Ni与PO基团中的O配位形成平面四边形构型.     

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。     

双核有机锡(Ⅳ)配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH的合成、表征和晶体结构

利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物 1由未配位的甲醇分子通过氢键作用形成二维网状结构     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability Properties of the Complex [Cd_2(phen)_2(C_(14)H_(11)O_3)_4(CH_3CH_2OH)]·(CH_3OH)·(H_2O)

A dinuclear cadmium complex [Cd2(phen)2(C14H11O3)4(CH3CH2OH)]·(CH3OH)·(H2O) has been synthesized with benzilic acid and 1,10-phenanthroline by hydrothermal method.The crystal structure was determined by X-ray diffraction with crystal parameters as follows:triclinic system with space group P1,a = 1.21298(10),b = 1.32586(11),c = 2.4815(2) nm,α = 76.2630(10),β = 81.4500(10),γ = 69.1700(10)o,V = 3.6143(5) nm3,Dc = 1.438 g/cm3,Z = 1,F(000) = 1600,the final GOOF = 0.937,R = 0.0521 and wR = 0.1328.In the title complex,the dinuclear structure is defined by carboxyl oxygen atoms adopting a monodentate bridged coordination mode.The coordination environment of Cd(Ⅱ) ion is CdO4N2,giving a distorted octahedral coordination geometry.TG analysis shows that the title complex is stable under 140 ℃.     

单核镍(Ⅱ)配合物[Ni(IDB)_2][C_6H_4(OH)COO].ClO_4.CH_3CH_2OH.H_2O的合成和晶体结构

标题配合物是由三齿配体N, N-二(2-苯并咪唑亚甲基)胺(IDB)、Ni(ClO4)2·6H2O与水杨酸钠在乙醇溶液中反应得到的紫色晶体。用X-射线衍射测定了其单晶结构。结果表明,该晶体属三斜晶系,P 空间群,化学式:C41H43ClN10NiO9,Mr = 914.01,a = 11.010(2),b = 13.800(3),c = 15.550(3) 牛 = 100.75(3),?= 102.97(3), = 107.56(3)? V = 2111.3(7) ?,Z = 2,F(000) = 952,Dc = 1.438 g/cm3,(MoK) = 0.591 mm-1,8215个独立可观测点(I>2(I))。最终偏离因子R(I>2(I)):R = 0.0591, wR = 0.1325;R(全部数据): R = 0.1302,wR = 0.1572。结构分析表明,镍(Ⅱ)分别与2个IDB配体中的苯并咪唑的4个氮和胺基的2个氮配位形成畸变的八面体构型。     

Synthesis and Crystal Structure of a Heterometallic Chain Coordination Polymer:{[Ni_2Mn_2L_2(CH_3CH_2OH)(H_2O)]·CH_3OH·2H_2O}_n

A chain-like coordination polymer with the chemical formula of {[Ni2Mn2L2(CH3CH2OH)-(H2O)]·CH3OH·2H2O}n has been synthesized by the assembly reaction of K2NiL·H2O and Mn(OAC)2·4H2O with a 1:1 mole ratio in methanol,where OAC-=CH3COO-and H4L=2-hydroxy-3-[(E)-({2-[(2-hydroxybenzoyl)imino]ethyl}imino)methyl]benzoic acid.The crystal structure was determined by single-crystal X-ray diffraction analysis.It belongs to the triclinic system,space group P1,with a=9.9464(8),b=13.4718(11),c=14.3877(12),α=87.1930(10),β=85.4280(10),γ=74.6470(10)°,V=1852.4(3)3,Z=2,Dc=1.807g/cm3,Mr=1008.03,λ(MoKα)=0.71073,μ(MoKα)=1.794 mm-1,F(000)=1032,R=0.0527 and wR=0.1284(Ⅰ2σ(Ⅰ)).The compound exhibits a chain-like structure formed by dissymmetrical tetranuclear units.     

一个锰(Ⅲ)Schiff碱配合物[Mn(napn)(CH_3OH)_2]ClO_4的合成与晶体结构

合成了一个新配合物[Mn(napn)(CH3OH)2]ClO4 (C26H26 Cl N2O8Mn,Mr = 584.88,H2napn = 双a-萘酚醛缩乙二胺),并测定了其晶体结构。晶体属于三斜晶系,空间群P ,a = 7.813(1),b = 13.025(2),c = 14.089(2) ? = 64.89(3), = 83.98(3), = 78.11(3)海琕 = 1270.16 ?,Z = 2, Dc = 1.529 g/cm3, F(000) = 604, R = 0.0837, wR = 0.1636。锰(Ⅲ)离子的配位构型为拉长的八面体。Schiff碱配体napn2-中的N2O2在赤道平面与锰(Ⅲ)形成四配位,2个CH3OH中的O原子分别在赤道平面两侧轴向位置与锰(Ⅲ)配位。由于Jahn-Teller效应,轴向上的MnO平均键长为2.52 拧A硗猓О写嬖诜肿幽诤头肿蛹淝饧?     

[Cu_3(hssal)_2(phen)_2(H_2O)_4]配合物的合成、性质和作为前驱体合成CuO的研究

用配体磺基水杨酸,1,10菲罗啉和CuCO3·Cu(OH)2·H2O反应合成了配合物[Cu3(hssal)2(phen)2(H2O)4]·2CH3OH(1)(H3hssal:磺基水杨酸;phen:1,10菲罗啉),用单晶X-射线衍射、元素分析和红外光谱对该配合物进行了表征。研究了1的固体荧光和热稳定性,并用它作为前驱体合成了CuO微晶粒子,用粉末XRD和SEM对合成的CuO进行了表征和形貌研究。     

新型含2,5-二-（3,5-二甲基吡唑-4-巯基）-1,3,4-噻二唑-M(M=Co2+,Cd2+,Mn2+)配合物的合成、晶体结构及其抑菌活性研究

将配体L[2,5-二-(3,5-二甲基吡唑-4-巯基)-1,3,4-噻二唑]与Co(NO3)2 6H2O,Cd(NO3)2 4H2O和MnCl2 4H2O进行配位反应,得到三个配合物[Co(L)2(H2O)4](NO3)2 4(CH3CH2OH)(1),[Cd(L)2(H2O)4](NO3)2 4(CH3CH2OH)(2),[Mn(L)2(Cl)2(CH3OH)2]2(CH3OH)(3),并用元素分析,FT-IR和X射线单晶衍射进行了表征.分析结果表明,配体L呈"U"形,配合物1～3呈"S"形.配合物中Co(II),Cd(II),Mn(II)的配位环境均为扭曲八面体,每个金属离子同时和两个配体进行配位.配体和配合物体外抑菌活性研究结果表明,配体及其配合物都有一定的抑菌活性.     

Solvothermal Syntheses and Crystal Structures of Two New Nonmetal Borates:C_4H_(10)N_2·B_6O_8(OH)_2 and (NH_3CH_2CH_2NH_3)B_5O_8(OH)

Two new borate compounds,C4H10N2·B6O8(OH)2 1 and (NH3CH2CH2NH3)B5O8-(OH) 2,have been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction,IR,elemental analysis and thermal analysis. Compound 1 crystallizes in the monoclinic system,space group P21/c,with a=8.3318(17),b=6.2118(12),c=12.479(3) ,β=108.96(3)o,V=610.8(2) 3,Mr=313.02,Z=2,Dc=1.702 g/cm3,μ=0.150 mm-1,F(000)=320,R =0.0387 and wR =0.0924. Its layered structure is linked by infinite covalently coordinated neutral sheets with 3,20-membered window system,which are built up from alternative B6O8(OH)2 subunits donated by two piperzazine nitrogen donors. 2 crystallizes in monoclinic,space group Cc,with a=6.7207(13),b=11.481(2),c=12.564(3) ,β=95.25(3)o,V=965.4(3) 3,Mr=261.18,Z=4,Dc=1.797 g/cm3,μ= 0.164 mm-1,F(000)=536,R=0.0396 and wR=0.0752. Its oxoborate structure is generated from the sheets of 3,9-membered boron rings bonded diamine molecules through electrostatic and H-bonding interactions to form a two-dimensional layered network.     

配位聚合物[Ni(H_2O)_6]·[Ni_2(phen)_2(BTC)_2(H_2O)_4]·4H_2O的水热合成和结构表征

采用水热法合成了新的配合物[Ni(H2O)6].[Ni2(phen)2(BTC)2(H2O)4].4H2O(phen=邻菲啰啉;BTC=均苯三甲酸),采用X射线单晶衍射结构分析及元素分析、红外光谱等表征,并用TGA检测了该配合物的热稳定性.晶体属于三斜晶系,空间群为P-1,晶胞参数a=0.84038(7)nm,b=0.92048(8)nm,c=1.64793(14)nm,α=97.3850(10)°,β=102.7930(10)°,γ=104.9700(10)°,V=1.17736(17)nm3,F(000)=622,Z=1.标题化合物的不对称结构是由NiO6单元和1个二聚物Ni2N4O12单元组成的,该二聚物单元通过2个邻菲啰啉和2个均苯三甲酸分子构筑了1个八元环.氢键将2个独立的结构单元连接成三维结构.     

两个由4-酰基吡唑啉酮衍生物构筑的Mn(Ⅱ)配合物的合成、晶体结构及性质(英文)

以4-酰基吡唑啉酮衍生物为配体合成了2个Mn(Ⅱ)配合物[Mn2L2(μ-CH3OH)2(CH3OH)2](1)和{[Mn L(μ-CH3OH)]·CH3OH·CHCl3}n(2)(H2L=N-(1-苯基-3-苄基-4-丙烯基-5-吡唑啉酮)-异烟酰肼),利用元素分析、红外光谱、紫外光谱、热重和X-射线单晶衍射分析进行了表征。结果表明反应体系的p H值影响配体的配位方式,所得配合物1为双核结构,而2为2D网状结构。热重分析表明,配合物1的稳定性高于配合物2的。     

[Ho_2(phen)_4(H_2O)_4(OH)_2](phen)_2(NO_3)_4的合成、晶体结构及磁性

在甲醇与水的混合溶剂中,经浓硝酸硝化的Ho_2O_3与1,10-邻菲啰啉反应形 成氢氧根桥联的双核钬配合物[Ho_2(phen)_4(H_2O)_4(OH)_2] (phen)_2(NO_3)_4 （phen = 1,10-邻菲啰啉）。单晶X射线衍射晶体结构测定表明晶体属三斜晶系, P1-bar (no. 2)空间群,晶胞参数a = 1.1241(1) nm, b = 1.1439(1) nm, c = 1. 4058 (1) nm, α = 93.989(7)°, β = 98.173(7)°, γ = 108.19(1)°, V = 1.6874(4) nm~3, Z = 1, D_c = 1.737 g/cm~3, F(000) = 880,7752个独立衍射 点中,5702个可观测点满足F_o~2 ≥ 2σ (F_o~2),R_1 = 0.0499, wR_2 = 0. 858。标题配合物由中心对称的双核[Ho_2(phen)_4(H_2O)_4-(OH)_2]~(4+)配阳离 子,邻菲啰啉phen分子及硝酸根NO_3~-阴离子组成。敏个稀土原子与2个邻菲啰啉 配体,2相水分子和2个氢氧根配位形成配位数为8的[HoN_4O_4]四方反棱柱。配位 多面体通过两氢氧根基团形成共棱的[Ho_2N_8O_6]双四方反棱柱[d(Ho-N) = 0. 2549～0.2565 nm, d(Ho-O_(H_2O) = 0.2356, 0.2366 nm, d(Ho-O_(OH)) = 0. 2223, 0.2240 nm]。通过氢键和芳环堆积作用,配阳离子和邻菲啰啉分子排列形成 平行于（10 1-bar）的两维层结构,NO_3~-阴离子位于层之间。标题配合物为顺磁 物质,在5 ～300K区间内遵循Curie-Weiss定律X_m (T + 4.43) = 14.72 cm~3·K ·mol~(-1)(X_m为每摩尔Ho~(3+)离子磁化率）,其Ho~(3+)离子的室温有效磁矩为 10.76 B. M.,与Ho~(3+)自由离子的磁矩基本相同,表明稀土离子间不存在磁交换 作用。     

Mn(Ⅲ)Schiff碱配合物的合成、结构及性能

合成Schiff碱配体C20H14N2(OH)2(N,N' 双水杨醛缩邻苯二胺)及相应的两个新Mn(Ⅲ)C20H14N2(OH)2 配合物[Mn(C20H14N2O2)(H2O)(CH3OH)]ClO4(1)和[Mn(C20H14N2O2)(C7H5O2)]·CH3CN(2)(C7H5O2 为水杨醛),并测定了它们的晶体结构。结果表明,配合物1属单斜晶系 ,晶胞参数为 :a=1.1748(7)nm,b=1.3985(7)nm,c=1.3538(4)nm,β=92.63°,V=2.222(2)nm3,空间群为P21/n,Z=4;配合物2也属单斜晶系 ,空间群P21/n ,晶胞参数 :a=1.0252(2)nm ,b=2.0146(3)nm,c=1.2494(4)nm,β=111.12(2)°,V=2.407(2)nm3,Z=4。紫外 可见光谱表明,配合物1和2分别在584nm和592nm处有一吸收,属于MnⅢ的d d跃迁光谱。     

SYNTHESIS AND STRUCTURE OF (Ph_4P)_2[Ni_3(μ-SC_3H_6S)_4]·2CH_3CN

<正> (Ph4P)2[Ni3(u-SC3H6S)4].2CH3CN was obtained from the reaction of NiCl2.6H2O,Na2(1,2-pdt)(pdtH2=CH3CH(SH)CH2SH) and Ph4PBr.Mr=1361. 80, P21/c,a=10.802(2),b=30.111 (7),c=9. 907(3) A ,B=93. 60(3) ;V= 3216. 0 A3;Z=2,Dc=1. 41g/cm3. The three Ni atoms of the anion are linearly arranged and bridged by four sulfur atoms from the four 1 ,2-propyldithiolato ligands.     

Synthesis and Structure Characterization of a Tetranuclear Manganese(Ⅲ) Complex:[Mn_4O_2(O_2CMe)_6(MeOH)_2(dbm)_2]·2MeCOOH·2CH_2Cl_2

The title compound, [Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2 (Hdbm = dibenzoylmethane), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1, with a = 10.729(3), b = 12.269(3), c = 13.085(4) , α = 106.367(3), β = 107.643(2), γ = 94.771(2)o, V = 1547.9(7) 3, Z = 1, C50H64Cl4Mn4O24, Mr = 1410.57, Dc = 1.513 g/cm3, F(000) = 724, Rint = 0.0147, T = 293(2) K and μ = 1.046 mm–1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with I > 2σ(I). The structure of the complex consists of one [Mn4(μ3-O)2]8+ core with four coplanar Mn atoms disposed in an extended “butterfly-like” arrangement and two O atoms triply bridging each “wing”, and the peripheral ligation is provided by six μ2-MeCO2– , two terminal μ2-dbm– groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms. Intermolecular O…H–O hydrogen bonding interactions are found within the structure of the compound.     

三核铁簇硫酸盐K_2(H_3O)_3[Fe_3(H_2O)_3O(SO_4)_6]·6H_2O的合成与晶体结构

在室温条件下合成了含三核铁簇的硫酸盐配合物K2(H3O)3[Fe3(H2O)3O(SO4)6].6 H2O,借助IR光谱、紫外-可见吸收光谱、X射线光电子能谱(XPS)和X射线单晶衍射等测试手段对其结构进行了表征.结果表明,标题化合物属于六方晶系,P6(3)/m空间群,晶胞参数为:a=b=0.963 7(2)nm,c=1.885 1(9)nm,V=1.516 3(9)nm3,Z=2,Dc=2.316 g/cm3,GOOF=1.089,R1=0.062 8,wR2=0.165 1.其分子由1个三核铁簇阴离子[Fe3(H2O)3O(SO4)6]5-、2个K+离子、3个水合质子H3O+和6个结晶水分子组成.     

SYNTHESIS AND STRUCTURE OF THE DINUCLEAR MANGANESE-SULFUR COMPLEX (Ph_4As)_2Mn_2(SC_3H_6S)_4

<正> (Ph4As)2[Mn2(SC3H8S)4] was obtained from the reaction of MnCl2-4H2O,Na2(1,2-pdt)(1,2-H2pdt=CH3CH(SH)CH2SH),and Ph4AsCl.C80H64As2Mn2S8, Mr =1301.41,orthorhombic,Pbca; a=10.854(2), b =22.562(6), c =24.545(6)A; V=6010.8A3;Z =4,Dc=1.44g/cm3. The centrosymmetic anion of title compound is a dimer of (Mn(pdt)2]- bridged by one sulfur atom each of the two bridging pdt2-, The atom Mo(Ⅲ) is in a distorted trigonal bipyramidal geometry.     

新型邻菲咯啉镁(II)配合物[Mg(H_2O)_4(phen)](phen)[C_6H_4(COO)_2]·H_2O的水热合成和晶体结构

合成了新型邻菲咯啉镁(II)配合物 [Mg(H2O)4(phen)](phen)[C6H4(COO)2]?H2O, 并对其进行了元素分析、IR、TG、X-射线衍射等表征。单晶衍射结果表明, 该配合物晶体属单斜晶系, 空间群为 P21/c, 晶胞参数:a = 11.873(2), b = 31.992(6), c = 8.144(2) ?, β = 93.98(3), V = 3085.9(11)?3, Z = 4, F(000) = 1336, Dc = 1.375 g/cm3, μ(MoKα) = 0.120 mm?1。对于 6889[ Rint = 0.0264]个独立衍射点, 有 3939 个可观测点满足(I≥2σ (I)), 最终的偏离因子 R = 0.0430, wR = 0.1294。标题配合物由 1 个邻菲咯啉合镁阳离子[Mg(H2O)4(phen)]2+、1 个邻苯二甲酸根阴离子C6H4(COO)2)2–、1 个溶剂邻菲咯啉分子和 1 个结晶水分子组成。中心 Mg(II)离子为六配位, 六个配位原子形成畸变的 MgN2O4八面体构型。