Synthesis and Crystal Structure of a One-dimensional Mn（Ⅱ） Coordination Polymer with 1,3-bis（4-pyridyl）propane

A new 1D zigzag chain coordination polymer, { [Mn（bpp）（bac）2]·（CHaCN）}n 1 （bpp = 1,3-bis（4-pyridyl）propane, Hbac = benzoylacetone）, has been synthesized and characterized by FT-IR spectroscopy, thermal analysis and X-ray single-crystal diffraction. In the molecular structure, all Mn atoms locate in an octahedral geometry. The guest CH3CN molecules are included in the 1D channels of the 3D packing structure of 1. Crystal data： C35H35MnNaO4, Mr = 616.60, monoclinic, space group P211c, a = 17.691（4）, b = 18,955（4）, c = 9.712（6） A, β = 93.91（3）°, V = 3249.31（1） A^3, Z = 4, Dc = 1.260 g/cm^3, F（000） = 1292, 20max = 54.9°, μ = 0.447 mm^-1, the final S = 1.020, R = 0.0693 and wR = 0.1497.     

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…     

Temperature-dependent Polymorphism in Co（II） Coordination Polymers from 5-Nitroisophthalate and 1,3-Bis（4-pyridyl）propane

The solvothermal reaction of 5-nitroisophthalic acid （H2nip）, 1,3-bis（4-pyridyl）pro- pane （bpp） and Co（NO3）2·6H：O at 130 and 160 ℃ gave rise to two polymorphic complexes [Co（bpp）（H20）（nip）], （1, 2）. Complex I belongs to monoclinic, space group C2/c with a = 14.489（6）, b = 18.242（8）, c = 19.414（9） A, β = 123.09（3）°, V = 4299（3） A3, Z = 8, C21H19CoN3O7, Mr = 484.32, Dc= 1.497 g/cm3, F（000） = 1992,/l = 0.847 mm-1. In complexes I and 2, bpp connects Co（II） into different 1D chains which are bridged by nip to form similar two-fold interpenetrating 3D frameworks.     

Synthesis,Crystal Structure and Characterization of a Cobalt Coordination Polymer： [Co（1,4-ndc）（L） （H2O）]n

The title coordination polymer, [Co（1,4-ndc）（L）（H2O）]n 1 （1,4-H2ndc = 1,4-na- phthalenedicarboxylic acid and L =1-（5-（1H-imidazol- 1-yl）pentyl）- 1H-imidazole） has been hydrothermally synthesized and characterized by IR and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.4333（12）, b = 13.2963（13）, c = 13.4678（13）A, α =β = 90°, y =107.302（2）°, V= 2125.7（4）A^3, Z = 4, CoC22H22N4O5, Mr = 481.37, De = 1.504 g/cm^3, F（000） = 996, μ（MoKa） = 0.850 mm^-1, R = 0.0472 and wR = 0.0984. Compound 1 exhibits a two-dimensional layer structure. The O-H...O and C-H...O hydrogen bonds stabilize the structure of 1.     

Synthesis,Crystal Structure and Thermal Behavior of a New 2D Barium（Ⅱ） Coordination Polymer with 1H-benzimi-dazole-5,6-dicarboxylate as the Single Ligand

The self-assembly of 1H-benzimidazole-5,6-dicarboxylic acid with barium chloride under hydrothermal conditions afforded a new 2D coordination polymer,[Ba2(L)(HL)Cl]n(1,L = 1H-benzimidazole-5,6-dicarboxylate),which was characterized by elemental analysis,infrared spectroscopy,thermogravimetric analysis,and single-crystal X-ray diffraction.Compound 1 is of monoclinic system,space group P21/c with a = 10.0145(6),b=25.6854(15),c=7.3116(4) ?,β = 99.4980(10)°,V = 1854.95(19)3,C18H9Ba2ClN4O8,Z = 4,Mr=719.42,Dc = 2.576 g/cm3,μ(MoKα) = 4.427 mm-1,F(000) = 1352,the final R = 0.0202 and wR=0.0465 for 3051 observed reflections with I > 2σ(I).It exhibits an interesting two-dimensional network structure and high thermal stability(up to 420 ℃).     

Hydrothermal Synthesis and Crystal Structure of a New 2D Mn（Ⅱ） Coordination Polymer with 4,4′-Sulfonyldi Benzoic Acid and 1,4-Bis（imidazol-1-ylmethyl）benzene Ligands

A novel manganese coordination polymer [Mn2(sfdb)2(biyb)2(H2O)2]n (1, H2sfdb=4,4′-sulfonyldibenzoic acid, biyb=1,4-bis(imidazol-1-ylmethyl)benze) has been hydrothermally synthesized and structurally characterized by single-crystal X-ray determination, IR and thermogravimetric analysis (TGA). Complex 1 crystallizes in the triclinic system, space group P with a=10.138(4), b=11.187(5), c=13.582(6) γ, α=69.146(7), β=89.628(7), γ=77.076(7)°, Mn2C56H48N8O14S2, Mr=1231.02, V=1398.5(10) ·3, Dc=1.462 g/cm3, F(000)=634, μ=0.600 mm-1, S=1.088 and Z =1. The final refinement gave R=0.0570 and wR=0.1229 for 4889 observed reflections with I > 2σ(I). Interestingly, in complex 1, the sfdb2- and biyb ligands connect the Mn(II) ions into two-dimensional 2-fold interpenetrating layers, and such layers are further connected with each other to generate a 3D supramolecular structure through hydrogen bonding interaction.     

Synthesis and Crystal Structure of a Puckered Rhombus Grid-like Coordination Polymer with Bridging Ligand Containing Sulfanyl Linker

Introduction The design and construction of metal-organic frameworks (MOFs), obtained by metal-directed self-assembly from labile metal centers and multidentate bridging ligands, is a rapidly developing area of su-pramolecular chemistry.1-3 Besides the aesthetic struc-tural and fascinating functional motifs, they are of in-terest both for understanding the mechanisms of the assembly process and for the host-guest chemistry asso-ciated with their large central cavities.4-13 It has been documen…     

Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Nickle （II） Achieved from 5-Iodo-isophthalic Acid Ligand

A new coordination polymer [Ni（L）（m-bix）（H2O）]n （1, H2L = 5-iodo-isophthalic acid, m-bix=1,3-bis（imidazol-1-ylmethyl）-benzene） has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, powder XRD and single-crystal X-ray analysis. The crystal is of triclinic, space group Pī with a = 9.1638（3）, b = 10.2319（3）, c = 13.2463（4） ？, α = 80.1710（10）, β = 83.671（2）, γ = 70.3790（10）o,C22H19NiIN4O5, Mr = 605.02, V = 1150.85（6） ？3, Dc = 1.746 g/cm3, F（000） = 600, μ = 2.225 mm-1, S = 1.045 and Z = 2. The final R = 0.0388 and wR = 0.1257 for 5089 observed reflections with I 〉 2σ（I）. In the title complex, the M and P layers are arranged alternately to give a double-layer structure by the symmetry related hydrogen bonds, and these double-layers are further joined together to achieve a 2D supramolecular architecture through I···π interaction involving iodine atoms and imidazole rings. The thermal stability of the title complex was studied by thermal gravimetric （TG） and differential thermal analysis （DTA）.     

Synthesis and Crystal Structure of a New Hexadentate Ligand N,N＇-Bis（di（2-pyridyl）methyl）ethylenediamine

The reaction of di(2-pyridyl)ketone with ethylenediamine produced hexadentate Schiff base 1 which can be reduced to form a new ligand N,N-bis(di(2-pyridyl)-methyl)ethylene- diamine (BDPM) in ethanol solution. The two compounds were characterized by elemental analyses and spectroscopic methods. Their structures were determined by X-ray diffraction study. Crystal data for 1: C24H20N6, Mr = 392.5, monoclinic, P21/c, a = 13.871(3), b = 13.510(2), c = 12.153(2) ? b = 112.97(2)? Z = 4, V = 2094.1(6) ?, Dc = 1.245 g/cm3, m(MoKa) = 0.078 mm-1, F(000) = 824, the final R = 0.0545 and wR = 0.0557 for 2048 observed reflections (I > 2s(I)); for BDPM: C24H24N6, Mr = 396.49, monoclinic, C2/c, a = 21.411(3), b = 8.053(1), c = 11.868(1) ? b = 92.63(1)? Z = 4, V = 2044.2(4) 3, Dc = 1.288 g/cm3, m(MoKa) = 0.080 mm-1, F(000) = 840, the final R = 0.0401 and wR = 0.0939 for 1673 observed reflections (I > 2s(I)).     

A New Two-dimensional Zinc Coordination Polymer Constructed by 1,3-Bis(4-pyridyl)-propane and Terephthalate: Synthesis and Crystal Structure

A new zinc coordination polymer, [Zn2(bpp)(tpa)2H2O] 1 (bpp=1,3-bis(4-pyridyl)-propane and tpa=terephthalate) has been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. X-ray crystal structure analysis reveals that complex 1 crystallizes in monoclinic, space group P2/c with a=18.348(2), b=10.9080(14), c=13.7924(18), β=98.156(2)°, V=2732.5(6)3 , Z=4, C29H24N2O9Zn2 , Mr=675.24, Z=4, F(000)=1376, Dc=1.641 mg/m3 , μ=1.815 mm-1 , the final R=0.0443 and wR=0.0769 for 2715 observed reflections (I>2σ(I)). The title complex exhibits a two-dimensional (4, 4) sheet structure which is further stacked through face-to-face π-π interactions between the monodentately coordinated pyridine ring of bpp ligand and the phenyl ring of terephthalate ligand to form a 3-dimensional supramolecular structure. Thermogravimetric analyses show that the host framework of the complex is thermally stable up to ca. 400 ℃.     

Synthesis and Crystal Structure of cis—[meso—1,3—Bis（propylsulfinyl）propane]dichloroplatinum（Ⅱ）

1 INTRODUCTION A number of Pt complexes with monosulfoxide have been isolated and characterized[1]. It was indicated that the sulfoxide group trends to coordinate to soft metals (Pt, Pd, etc.) by its sulfur atom[2]. Pt(Ⅱ) trends to bond to disulfoxides in cis-mode and such complexes have potential antitumor activity[2]. However, only few examples of such complexes have been structurally characterized[3]. We will report herein the crystal structure of a new Pt(Ⅱ) complex with a disulf…     

1,3-二(4-吡啶基)丙烷Cd(Ⅱ)配合物的合成、晶体结构及发光性质研究

以1,3-二(4-吡啶基)丙烷(L)为配体,合成了一种新的Cd(Ⅱ)配合物{[CdL2(H2O)2].2(C7H6N5)}n(C7H6N5=5-(3-氨基苯基)四唑离子)。X射线单晶衍射结构分析表明该配合物为一维链状结构,Cd(Ⅱ)分别与4个1,3-二(4-吡啶基)丙烷配体的4个氮原子,2个配位水分子的氧原子形成了六配位的扭曲八面体几何构型,1,3-二(4-吡啶基)丙烷配体桥梁相邻的Cd(Ⅱ)离子形成了一维的无限延伸的链状结构,分子间通过O-H…N、N-H…N氢键作用构筑成三维超分子网络结构。     

有机-无机杂化材料[Ag(bpp)]2(tdc)·8H2O的合成，结构和光学性能(bpp=1，3-bis(4-pyridyl)propane，tdc=thiophene-2，5-dicarboxylate)

在室温下，AgNO₃、1，3-二(4-吡啶基)丙烷和2,5-噻吩二甲酸在丙酮水溶液中反应,经数周后得到完整无色晶体[Ag(bpp)]₂(tdc)·8H₂O。该晶体由荷正电的类似正弦曲线形状的配位聚合物链，[Ag(bpp)]_∞，和有机负离子tdc^2-构成,其间分布着起重要作用的结晶水分子。相邻的阳离子链通过静电作用与tdc^2-阴离子堆积构成晶体的三维骨架, 结晶水分子分布其间并形成氢键，对晶体堆积起定位作用。[Ag(bpp)]₂(tdc)·8H₂O的晶体学数据:单斜晶系,空间群C2/c，a=3.544 7 nm，b=0.920 03 nm，c=2.411 9 nm，β=106.56°，V=7.546 nm³和Z=8；残差因子R₁=0.046 3，wR₂=0.114 2。UV/Vis/NIR漫反射光谱法测定表明其具有很强的选择性光吸收特性。     

Three Mn(II) complexes with 1,3-bis(4-pyridyl)propane and their supramolecular nets

Three complexes, [Mn(bpp)₄(H₂O)₂](ClO₄)₂?·?1.5H₂O (1), [Mn(bpp)₃Br₂]?·?2H₂O (2), and [Mn(bpp)₂(H₂O)₂](ClO₄)?·?I?·?H₂O?·?bpp (3) (bpp?=?1,3-bis(4-pyridyl)propane), were synthesized and structurally characterized by single-crystal X-ray diffraction. Complex 1 is mononuclear where M(II) is coordinated to a monodentate TT-bpp, three monodentate TG-bpp, and two water molecules. Complex 2 possesses a single-stranded helical chain formed from MnN₄Br₂ octahedra by a single TT-bpp, with pendant monodentate TG-bpp ligands. Complex 3 consists of a ribbon-type double-stranded chain formed from MnN₄O₂ octahedra by double TG-bpp ligands. 2-D supramolecular architectures of 1–3 are formed by hydrogen bonds. The fluorescence of the three complexes comes from the π*–π transition of the ligand.     

Spectroscopic, thermal and structural studies of cocrystal of 2,2′-diamino-4,4′-bis(1,3-thiazole) with 4,4′-bipyridine, 1,2-bis(4-pyridyl)ethylene and 1,3-bis(4-pyridyl)propane

Three new cocrystals based upon 2,2′-diamino-4,4′-bis(1,3-thiazole) (DABTZ) with 4,4′-bipyridine (4,4′-bipy), 1,2-bis(4-pyridyl)ethylene (bpe) and 1,3-bis(4-pyridyl)propane (bpp): [(DABTZ) (4,4′-bipy)], [(DABTZ) (bpe)] and [(DABTZ) (bpp)] have been synthesized and characterized by elemental analysis, IR-, ¹H NMR-, ¹³C NMR spectroscopy and studied by thermal and X-ray crystallography. Self-assembly of these compounds in the solid state is likely caused by both hydrogen bonding, and π-π stacking.     

Synthesis and Crystal Structure of 4-（4,6-Dimethoxylpyrimidin-2-yl）- 3-thiourea Carboxylic Acid Ethyl Ester

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.     

Synthesis and Crystal Structure of 4-(4,6-Dimethoxylpyrimidin-2-yl)-3-thiourea Carboxylic Acid Ethyl Ester

4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine,potassium thiocyanate and methyl chloroformate in ethyl acetate.Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamidc at room temperature.The crystal structure was determined by X-ray diffraction analysis.Crystallographic data:C10H14N4O4S,Mr=286.31,monoclinic,space group C2/c with a=2.5309(3),b=0.67682(6),c=1.74237(19)nm,β=114.744(3)°,V=2.7106(5)nm3,Dc=1.403 g/cm3,μ=0.225mm-1,F(000)=1200,Z=8,R=0.0514 and wR=0.1529.     

高柔性线型配体1,4-双(2-甲基-8-喹啉氧基)-丁烷的合成与表征

2-甲基-8-羟基喹啉和二溴丁烷在正丁基锂的存在下反应,生成标题化合物(C24H24N2O2, Mr = 372.46)。X-射线单晶结构分析表明此晶体属于单斜晶系,空间群P21/c, a = 5.7002(5), b = 12.186(1), c = 14.312(1) , b = 92.503(2), V = 993.2(2) 3, Z = 2, m = 0.080 mm-1, Dc = 1.245 g/cm3, F(000) = 396, R = 0.0505, wR = 0.0705. 结果表明,该化合物的2个配位端基2-甲基-8-羟基-喹啉基处于间隔基团-(CH2)4-的两侧,整个分子呈现中心对称的反式构象。此外,通过分子间的p…p 堆积作用和 CH…p 作用,使分子堆积成三维网络结构。     

Synthesis and Crystal Structure of Dichlorobis(1-methylimidazoline-2(3H)-thione-S) Cobalt(II)

The reaction of anhydrous cobalt(II) dichloride with 1-methylimidazoline-2(3H)thione in dichloromethane solution gave the title complex, [Co(C4H6N2S)2Cl2]. X-ray single-crystal analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, a = 13.9707(10), b = 10.0435(7), c = 10.3910(6) (A), β = 91.181(3)o, V = 1457.70(17) (A)3, Z = 4, C8H12Cl2N4S2Co, Mr = 358.17, Dc = 1.632 g/cm3, μ = 1.813 mm-1, F(000) = 724, the final R = 0.0710 and wR = 0.1224 for 1549 observed reflections with I > 2((I). The Co atom is coordinated by two S atoms from two 1-methylimidazoline-2(3H)-thione ligands and two chloride ions in a slightly distorted tetrahedral geometry. The intramolecular classical hydrogen-bonding interactions involving chloride ions and N-H groups of the heterocyclic thione ligands are observed. The offset π-π stacking interactions between the imidazole rings of adjacent molecules with a face-to-face distance of 3.604 (A) are found in the packing diagram.