配合物[Cu(H2biim)2]Br2的合成和晶体结构

The complex [Cu(H₂biim)₂]Br₂ (H₂biim=2,2′-biimdazole) has been synthesized and structurally charac-terized. It crystallizes in the Monoclinic system, space group C2/c with a=1.422 5(4) nm, b=0.931 2(2) nm, c=1.343 1(3) nm, β=116.227(4)°, V=1.595 9(7) nm^-3, R₁=0.060 2, wR₂=0.152 8 and Z=4. The copper ion has a sligh-tly distorted square planar coordination configuration with four nitrogen atoms from two H₂biim ligands. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds and semi-coordinate bonds. CCDC: 624679.     

超分子钴(Ⅱ)配合物[CoL(H2O)2]n的合成与结构表征

A mononuclear Cobalt(Ⅱ) complex [CoL(H₂O)₂]_n (H₂L: 4,4′,6,6′-Tetrabromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction single crystal structure analysis. The crystal of the complex belongs to monoclinic space group P2₁/c with a=2.516 8(3) nm, b=1.023 43(18) nm, c=0.789 17(14) nm, β=91.375(2)°, V=2.032 1(5) nm³, Z=4, D_c=2.317 Mg·m^-3, μ(Mo Kα)=8.747 mm^-1, F(000)=1 356, R₁=0.049 7, wR₂=0.110 4. The crystal structure of [CoL(H₂O)₂]_n indicates that the complex consists of one cobalt(Ⅱ) atom, one L^2- unit and two coordinated water molecules, and the coordination number of the cobalt(Ⅱ) atom is six. One-dimensional chain supramolecular structure is formed by intermolecular hydrogen bonds and π-π stacking of neighboring benzene rings. CCDC: 652649.     

Synthesis and Structural Characterization of Manganese Carbonyl Incorporated Polyoxomolybdate (n-Bu_4N)_2[Mo_6O_(16)(OCH_3)_2{HOCH_2C(CH_2O)_3}_2{Mn(CO)_3}_2]

The polyoxoanion incorporated {Mn(CO)3+} complex, (n-Bu4N)2[Mo6O16(OCH3)2{HOCH2C(CH2O)3}2· {Mn(CO)3}2](1), has been synthesized by the reaction of (n-Bu4N)4[Mo8O26] with Mn(CO)5Br in methanol, in the presence of C(CH2OH)4. The complex 1 has been characterized by IR, UV-Vis, X-ray single crystal diffraction, and TG. Crystal data for the complex 1: C25H48MnMo3NO16 (1), Triclinic P1, a=0.9405(3) nm, b=1.3351(4) nm, c=1.5455(4) nm, α=103.206(5)o, β=102.165(5)o, γ=100.784(5)o, V=1.7896(9) nm3, Z=2, R1=0.0703, wR...     

氢键构筑的二维网状结构镍配合物[Ni(en)2(dpas)2]的合成、晶体结构及电化学性质

A new 2D Hydrogen-bonded network complex [Ni(en)2(dpas)2] (Nadpas=sodium diphenylamine sulphonic acid salt,en=ethanediamine) has been synthesized in aqueous solution,and characterized by elemental analysis,IR. The crystal structure was determined by single-crystal X-ray diffraction. The complex crystallizes in space group P21/c,with cell parameters a=0.605 6(5)nm,b=1.448 1(5) nm,c=1.711 9(5)nm,β=93.257(5)°,and V=1.498 9(14) nm3,Dc=1.497 g·cm-3,Z=2,F (000)=708,R=0.027 7,wR=0.072 5. The crystal structure shows that the nickel atom is coordinated with four nitrogen atoms from the two en and two oxygen atoms from two dpas to form a mononuclear complex. Furthermore,the adjacent complex units are extended into a 2D supramolecular network through hydrogen bonds.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Mn2（phen）2（p-CBA）4（H2O）

One novel complex Mn2(phen)2(p-CBA)4(H2O) has been hydrothermally syn- thesized from p-chlorobenzoic acid (p-CBA), 1,10-phenanthroline (phen) and anhydrous man- ganese(Ⅱ) sulfate and then characterized. Crystal data for this complex: monoclinic, space group C2/c, with a = 2.3416(3), b = 1.5604(2), c =1.5605(2) nm, β = 121.048(2)o, V = 4.8849(12) nm3, Dc = 1.510 g/cm3, Mr = 555.26, Z = 8, μ = 0.798 mm-1, F(000) = 2256, GOOF = 1.032, the final R = 0.0393 and wR = 0.0816. The crystal structure shows that two neighboring manganese(Ⅱ ) ions are linked together by two bridge-chelating p-chlorobenzoic groups and one bridging water molecule, forming a cage structure with the Mn–Mn bond distance of 0.3512 nm. Each manganese(Ⅱ ) ion is coordinated by two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three p-chlorobenzoic acid anions and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the complex was also investigated.     

芳氧功能化咪唑基五氯化铕[HO-4,6-di-tBu-C6H2-2-CH2{CH（NCHCHNiPr）}]2+[EuCl5（THF）]2-的合成与结构

芳氧功能化咪唑盐L+Cl-(L=HO-4,6-di-tBu-C6H2-2-CH2{CH[iPrNCHCHN]})与无水EuCl3分别按照摩尔比为1∶2和1∶3反应成功合成相同芳氧功能化咪唑基五氯化铕L+2[EuCl5(THF)]2-,产物通过元素分析、IR、X-ray射线衍射表征。晶体结构数据表明此配合物属于单斜晶体,空间群P21/c,晶胞参数a=0.96664(8)nm,b=1.63312(12)nm,c=3.6850(3)nm,β=97.600(2)°,V=5.7662(8)nm3,Mr=1060.30,Z=4,Dc=1.221 Mg/m3,μ(MoKα)=1.36 mm-1,F(000)=2200。目标化合物是由阴离子[EuCl5(THF)]2-和[HO-4,6-di-tBu-C6H2-2-CH2{CH(iPrNCHCHN)}]2+通过氢键作用而形成的空间网状结构的晶体,阴离子中中心金属(Eu)是由五个氯原子以及来自THF的氧原子形成扭曲八面体的构型。     

配合物[Cu2(C4H2O6)(Phen)2(H2O)]·8H2O的合成、晶体结构和抗菌活性

在pH≈10的乙醇-水溶液中以硫酸铜、酒石酸和邻菲咯啉反应合成了分子式为[Cu₂(C₄H₂O₆)(Phen)₂(H₂O)]·8H₂O的配合物单晶。用X-射线单晶衍射测定了晶体结构，并研究了配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌的抗菌活性。晶体属单斜晶系，空间群P2₁。标题化合物为双核铜配合物，2个铜原子配位数不同。Cu(1)是五配位的，具有扭曲的四方锥结构，5个配位原子分别是酒石酸的去质子的羟基氧和羧基氧、邻菲咯啉的2个氮原子及1个水分子的氧原子。Cu(2)为四配位的，配位原子分别是酒石酸的去质子的羟基氧和羧基氧和邻菲咯啉的2个氮原子。分子中Cu(1)…Cu(2)间的距离为0.354 8 nm。存在分子内邻菲咯啉-邻菲咯啉的面—面π-π相互作用，面间距为0.381 3 nm。配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌具有较强的抗菌活性。     

铋(Ⅲ)四氢吡咯氨荒酸配合物[Bi(S2CNC4H8)3]2的合成和晶体结构

The novel bismuth(Ⅲ) complex with dithiotetrahydropyrrolocarbamate, [Bi(S₂CNC₄H₈)₃]₂ has been synthe-sized. The crystal structure has been determined by X-ray single crystal diffraction. The crystal belongs to mono-clinic with space group C2/c, a=1.6356(9) nm, b=1.1875(6) nm, c=2.3954(13) nm, β=100.741(8)°, Z=4, V=4.571(4) nm³, D_x=1.882g·cm^-3,μ=8.267mm^-1, F(000)=2512, R=0.0404, wR=0.0622. In this binuclear complex, each Bi(Ⅲ) is seven coordinate with a distorted pentagonal bipyramidal geometry. CCDC: 179924.     

配合物[Cu（C8H6CIO3）2（H2O）2]的合成与晶体结构

以硝酸铜和对氯苯氧乙酸为原料,合成了标题化合物[Cu（C8H6ClO3）2（H2O）2],并用元素分析仪、红外光谱仪、X射线单晶衍射仪表征了其组成和晶体结构．结果表明,所合成的晶体属三斜晶系,Pi空间群,a=0．51146（6）nm,b=0．70640（8）nm,c=1．326410（15）nm,a=81．7770（10）°,β=86．361（2）°,γ=76．3970（10）°,F（000）=239,Z=1;最终偏离因子R=0．0264,wR=0．0674．在配合物中,铜离子与来自两个对氯苯氧乙酸根的两个羧基氧原子、两个醚氧原子以及来自两个水分子的氧原子配位,形成变形八面体结构．     

Structure of the Manganese (V) Complex-Mn·3/2(μ-DHBQ)·4H_2O·2Cl

FewcompoundswithMninthe 5oxidationstatewerestructuraIlycharacterizedsofaLC.L.HilIlfirstdeterminedthecrystalstructUreoftheMn(V)complex:NMnTpMPP-Nitriodotrtrakis(p-methoxyphenyl)porphinnato-manganese(V).Thepapers'-'reportedseveralnovelmanganese(V)and(Vl)complexes.RecentpublicationshavebeenestablishedthatthecoordinationcompoundsofhighvaIentmanganesedisplaymanyinterestingfeatures.Theyshowabilitytoundergointramolecularinterligandormetal-ligandelectrontransferreaction,especiallyonthenatUreo…     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2(phen)2(p-MBA)4(H2O)

A novel Mn(Ⅱ)complex Mn2(phen)2(p-MBA)4(H2O)has been hydrothermally synthesized by the reaction of P-methyl benzoic acid(p-MBA)with 1,10-phenanthroline(phen).Crystal data for this complex:monoclinic,space group C2/c,a=2.3328(3),b=1.5549(2),c=1.5557(2)nm,β=121.726(2)°,V=4.7997(11)nm3,Mr=1028.85,Dc=1.424 g/cm3,Z=4,F(000)=2128,μ(MoKa)=0.590mm-1,GOOF=1.060,R=0.0333 and wR=0.0767.In the crystal,each Mn(Ⅱ)ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule.three oxygen atoms from three P-methyl benzoic acids and one oxygen atom from one water molecule,giving a six-coordinate distorted octahedral coordination geometry.Two neighboring Mn(Ⅱ)ions are bridged by two P-methyl benzoic acid groups and one water molecule,and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule,giving a binuclear cage structure,of which the Mn(Ⅱ)…Mn(Ⅱ)distance is 0.3502 nm.     

高氯酸四(DL-a-缬氨酸)八水合二钐的合成和结构

α-氨基酸在人体有极为重要的生理作用,近年来人们对其稀土配合物进行了广泛的研究。进一步研究稀土氨基酸配合物的单晶结构对于探讨稀土离子与生物体的作用是很有意义的。将高氯酸钐溶液与生化试剂DL-a-缬氨酸以1:1摩尔比混合,在75℃水浴中反应6小时,加热浓缩后,室温下缓慢挥发,即得到浅黄色透明棱状晶体。 结果与讨论     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2（phen）2（p-MBA）4（H2O）

A novel Mn（Ⅱ） complex Mn2（phen）2（p-MBA）4（H2O） has been hydrothermally synthesized by the reaction of p-methyl benzoic acid （p-MBA） with 1,10-phenanthroline （phen）. Crystal data for this complex： monoclinic, space group C2/c, a= 2.3328（3）, b =1.5549（2）, c = 1.5557（2） nm, β = 121.726（2）°, V= 4.7997（11） nm^3, Mr = 1028.85, Dc = 1.424 g/cm^3, Z = 4, F（000） = 2128, μ（MoKa） = 0.590mm^-1, GOOF = 1.060, R = 0.0333 and wR = 0.0767. In the crystal, each Mn（Ⅱ） ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule, three oxygen atoms from three p-methyl benzoic acids and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. Two neighboring Mn（Ⅱ） ions are bridged by two p-methyl benzoic acid groups and one water molecule, and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule, giving a binuclear cage structure, of which the Mn（Ⅱ）…Mn（Ⅱ） distance is 0.3502 nm.     

二维网状有机锑对氨基苯乙酸酯的合成、表征及晶体结构研究

The title complex bis(4-aminophenylacetate)triphenylantimony(V) has been synthesized by the reaction of triphenylantimony dibromide with 4-aminophenylacetic acid in 1∶2 molar ratio. The complex was characterized by elemental analysis, IR spectra, NMR ( ¹H, ¹³C) and X-ray diffraction crystal structure analysis. This complex crystallizes in the monoclinic system, space group C2/c with a=2.279 4(2) nm, b=0.957 10(10) nm, c=1.335 49(15) nm, β=93.781(2)°. The molecular structure adopts a distorted trigonal bipyramidal geometry around the antimony atom. In the crystal structure molecules are connected by intermolecular N-H…O hydrogen-bonding interactions forming a two-dimensional network structure. CCDC: 726039.     

Dawson结构α-H_6P_2W_(18)O_(62)·3(CH_3)_2NH·H_2O的合成、表征和晶体结构(英文)

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=4.1559(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.     

高氯酸化三邻菲啰啉合镍晶体结构研究

用Ni(ClO4)2合成了高氯酸阴离子和三邻菲啰啉合镍阳离子组成的盐晶体, 晶体结构由X射线衍射确定. 晶体属P21/n空间群, a=0.9388(2) nm, b=3.0139(5) nm, c=1.2974(2) nm, β=111.054(3)º, V=3.426(1) nm3. 采用hyperchem程序包的半经验方法ZINDO/1计算了该配合物的最优化结构, 原子电荷分布很好地佐证了晶体结构的配位环境.     

N,N''''-双(4-甲基-2-苯并噻唑基)-2,6-吡啶二酰胺钴(Ⅱ) 配合物的合成和晶体结构

0IntroductionCobaltcomplexeswithnonmacrocyclicchelatingligandscontainingtheamidefunctionalityhavere鄄ceivedmuchattentioninpastyears[1~3].Somestudieshaverevealedthatdeprotonatednitrogensoforganicamides,beinganionicinnature,arecapableofstabi鄄lizingthetriva…     

[Eu2(TCM)2(DMSO)6]·2DMSO双核笼状稀土配合物的合成与结构

报道一个H3TCM配体在较小尺寸的溶剂DMSO中与稀土离子Eu3+通过自组装形成的双核笼状结构, 从中可进一步看出溶剂分子的尺寸对该双核结构的影响.     

{Cu2(tacn)2[μ-(MeN)2C2O2]}[(MeNH)2C2O2](ClO4)2的合 成、结构及性质研究

合成了双核配合物{Cu2(tacn)2[μ-(MeN)2C2O2]}[(MeNH)2C2O2](ClO4)2(tacn=1,4,7-三氮杂环壬烷)。通过元素分析、红外光谱、ESR谱和电子光谱对配合物进行表征，并利用单晶X射线衍射法测定其结构，晶体属单斜晶系，空间群为P21/n,a=0.72572(16)nm,b=2.5616(6)nm,c=0.9128(2)nm,β=90.096(5)°，V=1.6969(7)nm^3,Dcald=1.590Mg.m^-^3,Z=2,F(000)=840,R1=0.0529,wR2=0.1341,Gof=1.028,△ρ=632～390e.nm^-^3。晶体由对称的双核Cu单元、中性草酰胺分子及高氯酸根堆积而成。两个铜原子配位数为五，处于变形四方锥的配位环境中。在5～300K范围内磁性测定表明：配合物中存在反铁磁偶合相互作用，经理论拟合：g=1.98,J=-219cm^-^1。     

砷配合物As(S2CNCy2)2I和As(S2CNC6H12)3的合成和晶体结构

合成了2种砷的氨荒酸配合物As(S₂CNCy₂)₂I (1)和As(S₂CNC₆H₁₂)₃ (2)。通过元素分析和红外光谱对其进行了表征,用X-射线单晶衍射测定了它们的晶体结构。配合物1的晶体属单斜晶系，空间群为P2₁/n，晶胞参数a=1.020 9(4) nm，b=1.468 0(5) nm，c=1.521 8(5) nm，β=92.135(5)°和Z=4。配合物2的晶体属三方晶系，空间群为R3，使用六方坐标，晶胞参数a=1.622 1(4) nm，c=2.119 4(6) nm，并有Z=6。测试结果表明，配合物1为单核结构，中心砷原子为五配位的三角双锥配位构型，此外，在该配合物分子间存在弱的As…S相互作用(As…S 0.351 2(4) nm)，使得该配合物以弱桥连二聚体存在。在配合物2中，3个配体分别以双齿形式与砷原子配位，形成六配位的畸变三棱柱体结构。