配合物[Cu(m-TFBA)(phen)(H2O)2]·(m-TFBA)的水热合成、晶体结构及量子化学研究

以醋酸铜、间三氟甲基苯甲酸(m-TFBA)和邻菲咯啉(phen)为原料在甲醇水介质中通过水热反应,合成了一个新的单核铜(Ⅱ)配合物[Cu(m-TFBA)(phen)(H2O)2]·(m-TFBA),用元素分析、红外光谱和热重分析对配合物进行了表征.X-射线单晶衍射表明,配合物属三斜晶系,空间群P(-)1,晶胞参数:a=1.001 61(10)nm,b=1.15069(12)nm,c=1.28649(12)nm,α=82.217(2)°,β=84.767(2)°,γ=66.371(2)°,V=1.3448(2)nm3,Z=2,Dr=1.625 g·cm-3,,R1[I>2σ(I)]=0.042 1,wR2>2σ(I)=0.0958.铜(Ⅱ)分别与来自邻菲咯啉的2个氮原子、间三氟甲基苯甲酸的1个氧原子和2个水分子中的2个氧原子配位,形成变形的四方锥结构.配合物通过强的O-H…O氢键作用形成了二聚体结构,该二聚体又通过分子间弱的C-H…0氢键作用形成了一维链状结构.配合物中配位的间三氟甲基苯甲酸上的三氟甲基基团具有无序结构.对配合物中[Cu(m-TFBA)(phen)(H2O)2]+进行了量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及一些前沿分子轨道的组成特征.     

新型邻菲咯啉镁(Ⅱ)配合物 [Mg(H2O)4(phen)]( phen)[C6H4(COO)2]·H2O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)(°A), ( = 93.98(3), V = 3085.9(11)(°A)3, Z = 4, F(000) = 1336, Dc = 1.375 g/cm3, β(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.     

配合物Cu(phen)2 (dca)2的合成及晶体结构

合成了配合物Cu(phen)2 (dca)2(phen=C12H8N2为1,10-邻菲啰啉,dca-为二氰基氨基阴离子),用IR对其结构进行了初步表征,并测定了配合物的晶体结构.该晶体属单斜晶系,空间群为P21/c;晶胞参数a=0.8869(2)nm,b=1.4691(2)nm,c=1.9298(2)nm,β=100.90(1)°;V=2.4691(8)nm3,Z=4,F(000)=1132.00,Dc=1.496g/cm3,R=0.051,RW=0.068.中心铜(Ⅱ)离子分别与两个phen中的四个N原子和两个dca-的两个N原子配位,形成六配位的变形八面体结构.     

新型超分子化合物[ Co( L-alanato)2(phen) ]NO3·4H2O的水热合成及其晶体结构

以Co( NO3)2.6H2O,邻菲罗啉(phen)与L-丙氨酸(L-alanine)为原料,通过水热法合成了新型超分子化合物[ Co(L-alanato)2(phen)] NO3.4H2O(1),其结构经IR,元素分析和X-射线单晶衍射分析表征.1属三斜晶系,空间群P-1,晶胞参数a=10.121 9(5)(A),b...     

配合物[Co(p-MBA)_2(phen)(H_2O)]·(p-MBA)的水热合成、晶体结构及量子化学研究

通过水热反应,合成了一个新的单核钴髤配合物[Co(p-MBA)2(phen)(H2O)]·(p-MBA),用元素分析和红外光谱对配合物进行了表征。X-射线单晶衍射表明,配合物属三斜晶系,空间群P1,晶胞参数:a=1.06588(8)nm,b=1.12873(8)nm,c=16.1181(13)nm,α=76.9890(10)°,β=71.2280(10)°,γ=63.6830(10)°,V=1.6379(2)nm3,Z=2,Dc=1.443g·cm-3,R1[I2σ(I)]=0.0444,wR2[I2σ(I)]=0.0881。钴髤分别与来自1个邻菲咯啉的2个氮原子、2个对甲基苯甲酸根的3个氧原子和1个水分子中的1个氧原子配位,形成变形的八面体结构。配合物通过强的O-H…O氢键作用形成了二聚体结构,该二聚体又通过分子间弱的C-H…O氢键作用形成了一维链状结构。对配合物中[Co(p-MBA)(phen)(H2O)2]结构单元进行了量子化学从头计算。     

配合物[Cu(phen)2Cl]·ClO4·H2O的合成和晶体结构

合成了新配合物[Cu（phen）2Cl]·ClO4·H2O（phen=o—phenanthroline）,并用IR和X射线单晶衍射法对其结构进行了表征．晶体结构解析表明,标题配合物属单斜晶系,空间群为P2（1）／n,晶胞参数α=1．18086（8）nm,b=1．52855（10）nm,c=1．29572（9）nm,α=90°,β=93．1770（10）°,γ=90．000°,V=2．3352（3）nm^3,Z=4,Dc=1．641Mg／m^3,Mr=576．86,μ=1．210mm^-1,F（000）=1172,偏差因子R1=0．0481,ωR2=0．1424．在配合物[Cu（phen）2Cl]·ClO4·H2O中,Cu（Ⅱ）离子处于四个N原子和一个Cl^-离子构成的三角双锥几何构型中．分子间利用氢键作用,π-π堆积作用形成二维层状结构．层与层间通过弱氢键作用形成三维空间结构．     

配合物Zn(phen)(pimelic acid)2的合成、晶体结构及电化学分析

金属有机配合物在催化、分离、气体存储和分子识别等方面有广阔的应用前景．它们的设计与合成是近年来配位化学领域的一大热点。过去．人们主要将注意力集中在刚性配体配合物的合成上．而有关柔性配体配合物的研究比较少见。庚二酸是一种柔性二元羧酸，它是很好的化工原料。是制造二酯、聚酯、聚酰胺的中间体，是合成润滑油、增塑剂、导热油、表面活性剂、杀菌剂、杀虫剂、粘和剂、热熔涂料的原料，它作为配体可用于构筑配位聚物。     

混合配体的铜(Ⅱ)配合［Cu(C2H4O2N)(C12H8N2)(H2O)］.ClO4.2.5H2O的合成、性质及晶体结构

本文对甘氨酸、1,10 -邻菲咯啉铜 ( )固体配合物进行了合成和表征 ,并利用 X射线分析研究了其晶体结构     

配合物[Cu(p-MBA)_2(phen)]的合成、晶体结构及量子化学研究

以醋酸铜、对甲氧基苯甲酸(p-MBA)和邻菲咯啉(phen)为原料在甲醇中反应,合成了一个新的单核铜髤配合物Cu(p-MBA)2(phen),用元素分析和IR等方法对化合物的结构进行了表征。X-射线单晶衍射表明,配合物属单斜晶系,空间群P2/c,晶胞参数:a=1.26503(14)nm,b=0.95588(10)nm,c=1.02488(12)nm,β=105.723(2)°,V=1.1929(2)nm3,Z=2,Dc=1.520g·cm-3,R1[I2σ(I)]=0.0356,wR2[I2σ(I)]=0.0786。该化合物的晶体是由孤立的分子所组成,四配位的铜髤呈畸变的四面体结构,配合物通过分子间弱的C-H…O氢键和π-π堆积作用形成了二维网状结构。对其结构进行量子化学从头计算,探讨了配合物的稳定性、分子轨道能量以及一些前沿分子轨道的组成特征。     

[Mn(phen)3](ClO4)2(H2O)·0.5(azpy)的合成和晶体结构

锰在生物体系的新陈代谢过程中有重要作用。锰有机配合物的研究成为生物无机化学研究领域的一个热点[1]。本文报道用高氯酸锰、1,10 邻菲咯啉和4,4 偶氮联吡啶[2 4]合成的锰配合物[Mn(phen)3](ClO4)2(H2O)·0 5(azpy)的晶体结构。1　实验部分1 1　Mn(Ⅱ)配合物的合成将0 0724g(0 2mmol)Mn(ClO4)2·6H2O溶于8mL水,缓慢加入含有0 1190g(0 6mmol)1,10 邻菲咯啉(phen)和0 0277g(0 15mmol)4,4′ 偶氮联吡啶(azpy)的15mL甲醇溶液,搅拌0 5h,室温下静置,一周后得[Mn(phen)3](ClO4)2(H2O)·0 5(azpy)晶体。元素分析(计算值)/%:C54 19(54 …     

Synthesis,Crystal Structure and Quantum Chemistry of the Complex [Cu（p-FBA）_2（phen）（H_2O）]

A novel metal-organic complex Cu(p-FBA)2(phen)(H2O) (p-FBA = p-fluorobenzoic acid,phen = 1,10-phenanthroline) has been synthesized and structurally characterized by X-ray single-crystal diffraction,elemental analysis and IR spectra. The crystal belongs to triclinic,space group P1 with a = 7.8043(7),b = 10.4069(9),c = 14.3658(13) ,α = 105.3170(10),β = 96.877(2),γ = 96.7580(10)o,V = 1103.56(17) 3,Mr = 539.96,Z = 2,Dc = 1.625 g/cm3,μ = 1.050 mm-1,F(000) = 550,the final R = 0.0324 and wR = 0.0952. In the crystal,the structure consists of discrete molecules containing a five-coordinate copper(Ⅱ ) in a distorted square pyramidal configuration. Intramolecular O-H···O hydrogen bonds,weak intermolecular C-H···O hydrogen bonds and π-π stacking link the molecules into a one-dimensional chain structure. The study on the title complex has been performed with quantum chemistry calculation by means of G03W package on the Lanl2dz basis set. The stabilities of the complex together with the orbital energies and composition characteristics of some frontier molecular orbitals have been investigated.     

配合物[Zn(p-ABA)2(phen)·(H2O)]·H2O的水热合成、晶体结构及热稳定性

在甲醇水混合溶剂中，以对乙酰氨基苯甲酸(p-ABA)，1，10-邻菲咯啉(phen)为配体与高氯酸锌合成了标题配合物[Zn(p-ABA)₂(phen)·(H₂O)]·H₂O。配合物(C₃₀H₂₆N₄O₈Zn，分子量为637.93)晶体属单斜晶系，空间群P2₁/c。晶体结构表明:锌原子与2个对乙酰氨基苯甲酸的2个氧原子，1个1，10-邻菲咯啉中的2个氮原子以及水分子中的氧原子配位，晶胞参数:a=1.362 77(17) nm， b=1.882 3(2) nm，c=1.252 53(16) nm;β=114.500(2)°，V=2.923 6(6) nm³，D_c=1.449 g·cm^-3，Z=4，F(000)=1 320，R₁=0.041 4，wR₂=0.087 8。形成五配位的三角双锥结构。对配合物热稳定性进行分析，结果表明，配合物在230.0 ℃以下稳定性好。     

Synthesis and Crystal Structure of a Ternary Complex: [Ni(phen)2(pmal)]·8H2O

A new ternary complex [Ni(phen)(pmal)]·8H2O (phen = 1,10-phenanthroline,pmal2- = phenethyl malonic acid) has been synthesized by the reaction of nickel acetate, phen and phenethyl malonic acid. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex: triclinic system, space group P1, a = 10.387(5), b = 13.112(6), c = 14.229(6) (A), α = 76.176(7), β =83.778(8), y = 71.770(6)°, C35H42N4O12Ni, Mr= 769.44, Z = 2, F(000) = 808, V = 1786.1 (A)3, Dc =1.431 g/cm3, μ = 0.612 mm-1, the final R = 0.0653 and wR = 0.1033 for 9379 (Rint = 0.0244)independent reflections and 4730 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the coordination geometry of Ni(Ⅱ) is a distorted octahedron. A novel two-dimensional structure is constructed from (H2O)4 and (H2O)12 water clusters, and the complex forms a 3-D network supramolecular structure by hydrogen bonds and π-π stacking of neighboring phens.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Zn（phen）（m-CBA）2（H2O）

A novel complex Zn(phen)(m-CBA)2(H2O) with m-chlorobenzoic acid (m-CBA), 1,10-phenanthroline (phen) and zinc chloride has been hydrothermally synthesized and characterized. Crystal data for this complex: triclinic, space group P1, a = 0.8361(5), b = 1.2455(7), c = 1.3107(7) nm, α = 115.637(8), β = 91.014(9), γ = 104.857(8)o, V = 1.1763(11) nm3, Dc = 1.623 g/cm3, Z = 2, F(000) = 584, GOOF = 1.078, the final R = 0.0453 and wR = 0.1192. Structure analysis shows that the zinc ion coordinates with two nitrogen atoms of one 1,10-phenanthroline molecule, three oxygen atoms from two m-chlorobenzoic acid molecules and one water molecule, giving a distorted square-pyramidal coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

之字链聚合物[Zn(o-bda)(phen)(H2O)]n·nH2O的结构

[Zn(o-bda)(phen)(H₂O)]_n·nH₂O (C22H20N2O6Zn) (1) [where o-bda is o-phenylenediacetic acid dianion and phen is 1,10-phenanthroline] crystallizes in triclinic system, space group P1 with a=0.826 5(4) nm, b=1.042 4(5) nm, c=1.238 1(6) nm, α=76.987(9)°, β=70.987(9)°, γ=78.281(8)°, V=0.9728(8) nm³, Z=2, D_c=1.617 g·cm^-3, μ=1.308 mm^-1 and F(000)=488. Zn(Ⅱ) ion has a distorted trigonal bipyramid coordination geometry formed by two carboxyl O atoms from two different o-bda groups, two N atoms from the phen ligand and one terminal water molecule. Adjacent Zn(Ⅱ) ions are interlinked by o-bda groups into a infinite zigzag chain structure with a Zn…Zn distance of 0.825 6(4) nm. The adjacent zigzag chains may also be paired under direction of supramolecular recognition and attraction through both π-π stacking and hydrogen bonding interactions into molecular zippers, which further interlinked into a three-dimensional supramolecular network by these noncovalent interactions. CCDC: 600935.     

Synthesis and Crystal Structure of a Dicyanamide-bridged One-dimensional Gadolinium(Ⅲ) Complex [Gd(dca)3(phen)2(H2O)]n

A chainlike coordination polymer [Gd(dca)3(phen)2(H2O)]n (dca = dicyanamide,phen = 1,10-phenanthroline) has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 10.6581(13), b = 15.6129(16), c = 17.733(3) (A), β = 90.499(5)°, V = 2950.8(7) (A)3, Z = 4,C30H18GdN13O, Mr = 733.82, Dc= 1.652 g/cm3, F(000) = 1444, λ(MoKα) = 0.71073 (A),μ = 2.297 mm-1, R = 0.0258 and wR = 0.0616 for 4570 observed reflections (I ＞ 2σ(Ⅰ)). In this complex, the gadolinium atom is nine-coordinated by four dca anions, two chelated phen ligands and one H2O molecule in a distorted tricapped trigonal prism. Two bridging dca anions connect the Gd(Ⅲ) ions yielding chainlike polymers that are linked by hydrogen bonds and π-π interactions to form a three-dimensional network.     

配合物[Co(phen)2(m-chlorobenzoic acid)2·(H2O)]·(H2O)2的水热合成、晶体结构电化学分析

The title complex has been synthesized with m-chlorobenzoic acid, 1,10-phenanthroline and cobalt perchlorate anhydrous in the solvent mixture of water and methanol. Crystal data for this complex: triclinic, space group P1, a=0.870 7(3) nm, b=1.284 4(4) nm, c=1.692 9(5) nm; α=75.430(5)°, β=77.562(5)°, γ=86.346(5)°, V=1.789 4(9) nm³, D_c=1.456 g·cm^-3, Z=2, F(000)=806. Final GooF=1.065, R₁=0.068 4, wR₂=0.127 5. The crystal stru-cture shows that the Cobaly ion is coordinated with four nitrogen atoms from two 1,10-phenanthroline molecules and two oxygen atoms from one m-chlorobenzoic acid molecule and one water molecule respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619087.     

Synthesis and Crystal Structure of a Ternary Complex:[Ni(phen)_2(pmal)]·8H_2O

1 INTRODUCTION Molecular structures of metallic complex and intermolecular weak interaction mode have become the focal fields of crystal engineering and supra- molecular chemistry. As we all known, intermole- cular weak interactions include hydrogen bonds[1, 2], π-π staking interaction[3, 4], metal-metal weak inte- raction[5, 6] and chelate-ring-chelate-ring weak inte- raction, et al.[7] Binary, ternary and quaternary car- boxylic acid ligands possess versatile coordination modes with me…     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

Synthesis and Crystal Structure of a Novel Zinc Phosphonate Compound： [Zn（phen）（m-OOCC6H4PO3H）]

A novel zinc（H） metal phosphonate compound [Zn（phen）（m-OOCC6H4PO3H）] 1 （phen = phenanthroline） has been synthesized under hydrothermal conditions. Single-crystal X-ray structure analysis reveals that compound 1 belongs to the triclinic system, space group P1 with a = 9.3356（19）, b = 10.203（2）,c = 10.743（2）A,α = 76.3030（70）, β= 69.2317（51）, y = 84.3833（74）°,V = 929.4（3） ,A3, Z = 2, C2OH15N2O5PZn, Mr = 459.68, Dc = 1.643 g/cm^3,μ= 1.444, mm^-1, F（000） = 468, the final R = 0.0330 and wR = 0.0848. In the structure, the central ion Zn（H） is five-coordinated, linking three O atoms with one from carboxyl and the other two from phosphonyl group. The remained two coordinate sites were occupied by two N atoms from one phen molecule to form the asymmetric unit. Then every two adjacent asymmetric units are bridged by the O atoms from phosphonate group and carboxyl to give rise to a 1D chain along the b axis. These chains are constructed by weak π-π stacking interactions and C-H…π interactions to generate a 3D supramolecular framework.