氨基硫脲缩(4-醛基吡啶)氟硅酸盐的合成和晶体结构

氨基硫脲缩(4-醛基吡啶)4-C5H4NCHNNHCSNH2(HL)和氟硅酸钾K2S iF6反应制备了标题化合物[H(4-C5H4NCHNNHCSNH2)]2S iF6.2H2O(1),用元素分析和X射线单晶衍射对其结构进行了表征.结构解析表明,化合物1属于单斜晶系,P21/c空间群,晶胞参数为:a=0.674 3(2)nm,b=1.349 6(3)nm,c=1.235 7(3)nm,β=94.283(4),°V=1.121 4(5)nm3,Z=2,Mr=540.61,Dc=1.607 g/cm3.μ=0.371 mm-1,F(000)=560,R1=0.036 8,wR2=0.105 4.该化合物由质子化的正一价氨基硫脲缩(4-醛基吡啶)阳离子和氟硅酸根阴离子以及水分子组成.     

Preparation,Characterization and Crystal Structure Determination of a Nickel Complex [Ni（ftsc）2NOa]NO3 （Hftsc = Furan-2-carbaldehyde Thiosemicarbazone）

A new Ni（II） complex, [Ni（ftsc）2NO3]NO3 （Hftsc = furan-2-carbaldehyde thiosemicarbazone）, has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystalfizes in a monoclinic system, space group P2 1/n, with a = 10.5203（13）, b = 9.2094（11）, c = 20.829（3）A,β = 91.518（2）°, V= 2 017.3（5）A^3, Z = 4, F（000） = 1064, Dc = 1.716 g/cm^3, and wR = 0.0800. The complex contains a six-coordinated nickel（II） center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H…O and C-H…O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.     

一维链状银配合物的合成及晶体结构

The complex [Ag(L)]NO₃ (1) [L=1,5-bis(imidazol-1-yl)pentane] was synthesized in ethanol and water, and characterized by elemental analysis and X-ray crystal structural analysis. The result shows that the complex crystallizes in monoclinic, space group P2₁/c with a=0.695 7(4) nm, b=0.988 7(4) nm, c=1.974 8(7) nm, β=91.934(19)°, V=1.357 5(10) nm³, Z=4, D_calc=1.831 g·cm^-3, F(000)=752, μ=1.50 cm^-1, the final R=0.036 6, wR=0.091 0. The coordination environment of Ag(Ⅰ) is nearly linear with two N atoms, and each L ligand links two Ag(Ⅰ) atoms using its two imidazolyl N atoms to generate an infinite one-dimensional (1D) chain structure. The 1D chains are further connected by C-H…O hydrogen bonds to give a three-dimensional structure. CCDC: 609514.     

Preparation,Characterization and Crystal Structure Determination of a Nickel Complex [Ni(ftsc)_2NO_3]NO_3(Hftsc=Furan-2-carbaldehyde Thiosemicarbazone)

A new Ni(II) complex, [Ni(ftsc)2NO3]NO3 (Hftsc=furan-2-carbaldehyde thiosemicarba-zone), has been synthesized and characterized by IR, UV spectra and single-crystal X-ray diffraction analysis. It crystallizes in a monoclinic system, space group P21/n, with a=10.5203(13), b=9.2094(11), c=20.829(3), β=91.518(2)°, V=2 017.3(5)3, Z=4, F(000)=1064, Dc=1.716 g/cm3, and wR= 0.0800. The complex contains a six-coordinated nickel(II) center which is bound to two imine nitrogen atoms and two thiolato sulfur atoms of two ligands as well as two oxygen atoms from a nitrate anion to assume a distorted octahedral coordination geometry. In addition, intermolecular N-H···O and C-H···O hydrogen bonds between adjacent molecules link the molecules together to form a three-dimensional structure.     

Synthesis, Crystal Structure and Luminescence Property of a 2D Mn（II） Coordination Polymer Based on Isoniazid

A novel 2D Mn(Ⅱ) coordination polymer [Mn(CH3COO)2(INH)]n(INH=isoniazid) has been synthesized in DMF solution with isoniazid and Mn(CH3COO)2 . The polymer was characterized by single-crystal X-ray diffraction analysis, FTIR and X-ray powder diffraction (XRPD). The crystal belongs to the monoclinic system, space group P2 1 /c with a=9.3251(18), b=16.340(3), c=8.8096(17) , β=94.747(3)°, V=1337.7(4) 3 , Z=4, μ(MoKα)=1.006 mm -1 , F(000)=636, R=0.0754 and wR=0.1375 (I > 2σ(I)). In the complex, each Mn(Ⅱ) atom is coordinated to three CH3COO- groups and two INH ligands. The Mn(Ⅱ) atoms locate in a distorted coordination octahedron and are bridged by CH3COO- ions to form a 1D S shaped chain extending along the c direction. The INH molecules act as bridges to link the Mn(Ⅱ) atoms of adjacent chains and further construct a lamellar polymer. The remaining coordination site is occupied by an O atom of the other CH3COO-. The experimental results show that the title complex has good luminescence property and could be used as potential optical materials.     

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?     

Synthesis and Crystal Structure of a New Three-dimensional Coordination Polymer： [Mn（2,3- pdc） （H2O）]n （2,3-pdc = Pyridine-2,3-dicarboxylate）

A new three-dimensional coordination polymer [Mn（2,3-pdc）（H20）]n （2,3-pdc = pyridine-2,3-dicarboxylate） 1 has been hydrothermally synthesized and structurally characterized. The crystal belongs to the monoclinic system, space group P21/c with a = 6.4168（5）, b = 10.7939（9）, c = 11.1549（10） A, β = 94.733（4）°, V = 769.98（11） A3, Z = 4, Mr = 238.06, De = 2.054 g/cm3, μ（MoKa） = 1.707 mm-1, F（000） = 476, Rint = 0.0326; R = 0.0499 and wR = 0.1636 for 1564 observed reflections with I 〉 2σ（I）. X-ray diffraction analyses reveal that the title compound is a three-dimensional coordination polymer consisting of one MnⅡ center with a distorted octahedral environment arranged by four 2,3-pdc ligands and one water molecule.     

Synthesis and Structure of a Mn（II）-triazolyl Coordination Polymer Consisting of Dinuclear Units

The reaction of bis(1,2,4-triazolyl-4-yl) (btr) and MnClO4·6H2O gave rise to a Mn(Ⅱ) complex comprised of unprecedented dinuclear Mn(Ⅱ) units, {[Mn2(btr)3(H2O)5]-(ClO4)4(H2O)2]n(1). Single-crystal X-ray diffraction analysis revealed that 1 crystallizes in the monoclinic space group C2/c. btr adopts two types of bridging modes. One serves as a μ-N1:N2 bridge through one triazolyl ring of btr forming a dinuclear Mn(Ⅱ) unit, and the other adopts an exo-bidentate mode using two nitrogen atoms from each triazolyl ring and links the dinuclear units into a 2D cationic layer. ClO4- acts as a counter anion and does not take part in coordination. Interestingly, 2D layers are packed in an ABCABC mode. ClO4- and uncoordinated water molecules locate between the adjacent layers, and extensive hydrogen bonds further stabilize the whole framework.     

Synthesis and Crystal Structure of a New Complex （H3IDC）（Prz）0.5（H2O）

The compound （H3IDC）（Prz）0.5（H2O） （H3IDC = imidazole-4,5-dicarboxylate, Prz = piperazine） has been prepared from a hydrothermal approach and was characterized by IR analysis and X-ray diffraction. Its crystal structure consists of discrete 4,5-imidazole-dicarboxylate, H2O and piperazine molecules. The whole structural motif was assembled by three different non-covalent interactions of O-H…O, N-H…O and π-π stacking, which play an important role in packing the molecules. Interestingly, the connections between imidazole-4,5-dicarboxylate molecule and water molecule result in a helical polymeric chain. Crystal data for compound 1： monoclinic system, space group P21/c, a = 6.4600（13）, b = 19.910（4）, c = 6.9123（14） A^°, β = 94.26（3）°, V= 886.6（3） A^°^3, Z= 4, C7H10O5N3, Mr = 216.18.     

一维螺旋状3，6-哒嗪二甲酸镉(Ⅱ)配位聚合物的合成与结构

Using the ligand pyridazine-3，6-dicarboxylate (H₂pzdc)， a coordination polymer [Cd₂(pzdc)₂(H₂O)₄] was synthesized and characterized by elemental analysis， thermal analysis， IR and single-crystal X-ray diffraction. The complex crystallizes in the tetragonal system with space group I4₁/a. The crystallographic data are: a=1.470 6(4) nm， c=1.489 8(6) nm， V=3.222 0(19) nm³， Z=16， μ=2.725 mm^-1， D_c=2.594 g·cm^-3， R₁=0.017 8， wR₂=0.044 6. In the complex， the cadmium(Ⅱ) ions with the eight-coordinated dodecahedral geometry are linked by the pzdc ligands to generate one-dimensional chains， which are associated into the three-dimensional architecture via O-H…O hydrogen bonding. CCDC: 658853.     

系列Mn(II)配位超分子的合成、晶体结构和表面光电压研究

采用水热合成方法得到了三种Mn(II)配位超分子: Mn(2,5-dcp)₂(H₂O)₂ (1), Mn(INA)₂(H₂O)₄ (2)和Mn(phen)₂Cl₂ (3) (2,5-dcp＝pyridine-2,5-dicarboxylic acid, INA＝iso-nicotinic acid, phen＝1,10-phenanthroline). 通过X射线单晶衍射、红外光谱(IR)、紫外光谱(UV-Vis)及表面光电压光谱(SPS)等方法对化合物进行了表征. 三种化合物中均存在大量的氢键, 使化合物晶体构成了无限延伸的三维网络结构. 表面光电压谱显示了化合物1～3在300～600 nm范围内呈现出正的光伏响应带, 具有P-型半导体的特征. 讨论了氢键在超分子构建中的作用以及不同配位环境对于配合物表面光电压的影响.     

钴与吡啶-2,6-二甲酸和邻菲咯啉三元配合物的合成与晶体结构

合成了钴(Ⅱ)与吡啶-2,6-二甲酸和邻菲咯啉三元配合物Co(DPC)(phen)(H_2O)]·2H_2O(DPC=C7H3O4N;phen=C12H8N2·H_2O),并获得其单晶。晶体学数据如下：C19H17CoN3O7, Mr = 458.29,三斜晶系, P空间群。 a = 7.818(1), b = 9.290(2), c = 14.048(3) ?, α = 81.477(1), β = 81.456(8), γ = 72.970(2)°, V = 958.7(3) ?3, Z =2, F(000) = 470, Dc= 1.588Mg/m3, μ(MoKα) = 0.944mm-1。中心Co(Ⅱ)离子为6配位,6个配位原子形成一个畸变的八面体构型。     

Synthesis and Crystal Structure of a Novel Tetranuclear Manganese(II) Complex with a Tripodal Peptide Ligand

1 INTRODUCTION Amides play an important role in the evolution ofnature. The amidate participates in the coordinationof iron with the ligands containing biomolecules, suchas antitumor drug bleomycin[1] and nitrile hydra-tase[2]. Bleomycin is a clinically useful antitumoragent which catalyzes the cleavage of oxidative DNAand oxidizes a number of organic substrates with di-oxygen or H2O2 . This has raised more interest in [3]the coordination of amide complexes[4, . …     

Synthesis and Crystal Structure ofa Seven—coordinate Cadmium（Ⅱ）Complex

1 INTRODUCTION In the last decade, there has been great interest in the crystal engineering of supramolecular architectures organized by coordinate covalent bonds, hydrogen bonds and their combination owing to their fascinating structural diversity and potential applications as functional materials[1~3]. The self-assembly of coordinate polymers and supramolecules is highly influenced by factors such as ligands, metal ions, the counter ions, solvent, template, reaction temperature, pH va…     

Synthesis and Crystal Structure of a Spiral-chain Manganese(Ⅲ) Complex Containing Azide Bridge,[Mn(bzan)N_3]_n

1 INTRODUCTION It is now recognized that manganese plays an important role in numerous redox processes associating with the metabolism of dioxygen. This has prompted recent attempts to understand the coordination chemistry of Mn(Ⅲ) ions which are now believed to play a role in at least three enzymes: manganese superoxide dismutase (MnSOD)[1], manganese catalase[2] and photosynthetic oxygen- evolving complexes (OEC)[3]. New model complexes have appeared during the last ten years. Her…     

Synthesis and Crystal Structure of Zn(II) Complex with Tridentate Ligand N-(2-Hydroxy-1-naphthylidene)-L-serine

1 INTRODUCTION As the basic building blocks of proteins or enzy- mes, amino acids are versatile ligands showing flexi- ble coordination modes[1]. Recently, researchers have synthesized some metal complexes with amino acids and their derivatives[2～6]. Considerable efforts have been devoted to the preparation and structure of amino acid Schiff base complexes with transition metals[6～11]. In such cases, some Zn(II) complexes have been reported. However, most of them have been carried out…     

Synthesis, Crystal Structure and Thermal Property of a Manganese(II) 4-Carboxyphenoxyacetate Complex

1 INTRODUCTION Organic aromatic carboxylic acids which com-monly possess multiple coordination modes are ex-cellent candidates for constructing supramolecularmetal complexes[1～6]. 4-Carboxyphenoxyacetic acid(4-CPOAH2), widely used in biological activitystudies, is a multidentate flexible ligand that not onlyhas versatile binding possibilities but also can formregular hydrogen bonds as both hydrogen-bond donorand acceptor. However, there have been few reportson the coordination chemistr…     

Synthesis and Crystal Structure of a Dinuclear Cu(II) Complex with Tridentate Schiff Base and Azido Bridge

1 INTRODUCTION The azido ligand is an efficient superexchange path-way for propagating magnetic interaction between theparamagnetic centers, such as copper(II), giving di-nuclear, tetranuclear, 1D, 2D and 3D complexes[1～4].The versatility of this ligand due to its diverse bin-ding modes leads to the variation in magnetic pro-perties that depend on its orientation with respect tothe magnetic centers. In general, the bridging modesobserved for the azido group are endtoend and en-don. In…     

Synthesis and Crystal Structure of a Co（II） Coordination Polymer Derived from a Flexible Bipyridyl Derivative Ligand

1 INTRODUCTION The infinite networks constructed from transition metal complexes have attracted considerable current interest in recent years. The motivation behind this activity has been stimulated by their potential appli- cations in selective inclusion of ions, molecular re- cognition, host-guest chemistry, ion exchange, cata- lysis, electrical conductivity, magnetism, optics and so on[1～4]. It is well known that the diversity in structures and topologies of supramolecules is attri- b…     

Synthesis, Crystal Structure and Spectrum Properties of Trinuclear Manganese Coordination Compound Mn3（2,2＇-bipy）e（3,5-DMBA）6

A novel complex Mn3(2,2'-bipy)ff3,5-DMBA)6 with 3,5-dimethylbenzoic acid (3,5-DMBA) and 2,2'-bipyridine (2,2'-bipy) has been synthesized by means of a solvent method. It crystallizes in the monoclinic ...