Synthesis and Crystal Structure of Two Coordination Complexes Based on H2dpa and Tmd Ligands

Two new transition metal compounds, [Mn(dpa)2(tmd)2]n (1, H2dpa = 4-hydroxy-phenyl-acetic acid, tmd = 4,4-trimethylenedipyridine) and [Co4(dpa)6(tmd)4(H2O)4]n·nH2O·nCl2 (2), have been synthesized by hydrothermal synthesis. Compound 1 crystallizes in the monoclinic system, space group P21/n with a = 9.828(3), b = 17.493(5), c = 11.616(4), β = 110.146(6)o, V = 1874.9(10)3, C42H42MnN4O6, Mr = 753.74, Z = 2, Dc = 1.335 g/cm3, μ = 0.406 mm–1, F(000) = 790, the final R = 0.1047 and wR = 0.2021 for 2698 observed reflections (I > 2σ(I)). Compound 2 crystallizes in the monoclinic system, space group P21/c with a = 11.7214(13), b = 17.1582(19), c = 24.625(3), β = 103.055(3)o, V = 4824.4(9)3, C100H104Cl2Co4N8O23, Mr = 2094.55, Z = 2, Dc = 1.443 g/cm3, μ = 0.809 mm–1, F(000) = 2180, the final R = 0.0550 and wR = 0.0673 for 4104 observed reflections (I > 2σ(I)). These complexes were characterized by elemental analysis, IR spectroscopy, and X-ray single-crystal diffraction. The structural analyses show that the two compounds are both one-dimensional chain structures. However, compounds 1 and 2 form threedimensional supramolecular structures by hydrogen bonds, respectively.     

An Organic-inorganic Hybrid Sandwich-type Arsenotungstate [H_2dap]_2H_2[Ni(dap)_2][Ni(dap)_2(H_2O)_2]- [Ni_4(H_2O)_2(B-α-As~VW_9O_(34))_2]·8H_2O

A new organic-inorganic hybrid sandwich-type arsenotungstate[H2dap]2H2[Ni(dap)2] [Ni(dap)2(H2O)2][Ni4(H2O)2(B-α-AsVW9O34)2]·8H2O 1 (dap = 1,2-diaminopropane) has been synthesized by the reaction of Na6[AsIII2W21O69(H2O)]·nH2O, NiCl2·6H2O and dap under hydro- thermal conditions and structurally characterized by elemental analysis, IR spectroscopy, thermo- gravimetric analysis and single-crystal X-ray diffraction. 1 crystallizes in the monoclinic space group P21/n with a = 13.5133(19), b = 19.043(3), c = 17.647(2) , β = 102.585(2)°, V = 4432.0(11) 3, T = 296(2) K, Z = 2, μ = 25.350 mm–1, GOOF = 1.058, R = 0.0353 and wR = 0.0838. The molecular unit of 1 consists of two diprotonated [H2dap]2+ cations, two protons, one four-coordinate [Ni(dap)2]2+ cation, one six-coordinate [Ni(dap)2(H2O)2]2+ cation, one classic tetra-NiII substituted sandwich-type [Ni4(H2O)2(B-α-AsVW9O34)2]10– polyoxoanion and eight lattice water molecules. Furthermore, some reported different types of transition-metal substituted sandwich-type poly- oxoanions are summarized and compared.     

《结构化学》简介

<正>《结构化学》是由中国科学院主管,中国化学会、中国科学院福建物质结构研究所主办的学术性期刊。1982年由我国著名化学家卢嘉锡院士创办并担任主编,现任主编是著名化学家吴新涛院士。《结构化学》主要报道晶体学,量子化学,药物、材料和催化剂等领域物质性     

ZnTPP Axially Coordinated with a Novel Dipyridylamine Ligand: Hydrothermal Synthesis and Crystal Structure

A novel complex ZnTPPL1·3DMF 1(TPP = tetraphenylporphyrin,L1 = N-(4-(9-carbazolyl) phenyl)-N,N-di(4-pyridyl)amine) was prepared by a hydrothermal method and characterized by elemental analysis,IR,and single-crystal X-ray diffraction analysis.Compound 1 crystallizes in triclinic,space group P1 with a = 13.3082(2),b = 14.3276(2),c = 18.6120(3) ,α = 109.853(1),β = 95.054(1),γ = 98.832(1)°,V = 3260.57(9) 3,Z = 2,Dc = 1.334 g/cm3,C81H69N11O3Zn,Mr = 1309.84,μ(MoKα) = 0.438 mm-1,F(000) = 1372,GOF = 1.159,the final R = 0.0482 and wR = 0.1479 for 12091 observed reflections(Ⅰ 2σ(Ⅰ)).Crystal structure analyses revealed that L1 utilizes one pyridyl N atom to bind Zn via axial coordination,affording a 1:1 complex.The binding constant was estimated to be 1.74(7) × 104 M-1 from electronic spectra measurements.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Novel Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]_2·[BiCl_6]·Cl}

A novel supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2·[BiCl6]·Cl},was synthesized by the hydrothermal reaction of o-phenylenediamine and α-pyridinecarboxylic acid with BiCl3 in 6.0 mol·L-1 HCl solution,and characterized by elemental analysis,IR,X-ray single-crystal diffraction and photoluminescence spectroscopy.The crystal (C24H22N6Cl7Bi,Mr= 851.61) belongs to the triclinic system,space group P1 with a =7.2887(18),b =9.548(2),c= 12.469(3),α=85.306(4),β=82.814(4),γ=71.349(4)°,Z=1,V=814.9(3)3,Dc=1.735 g/cm3,μ(MoKα)=6.007 mm-1,F(000)=410,R=0.0307 and wR=0.0787.The bismuth ion and six chlorine ions construct a distorted octahedral configuration.The three-dimensional supramolecular network is built from electrostatic attractions,hydrogen bonds and π-π interaction between the BiCl6 anion,Cl anion and [2-(2-pyridyl)benzimidazoleH2] cation.The photoluminescence spectroscopy study shows that the title compound has a blue fluorescent emission at 450 nm in the solid state.     

Syntheses and Crystal Structures of Two 1D Chain Coordination Polymers Based on 2-Benzoylbenzoic Acid

Two new coordination polymers,[Co(BYBA)2(4,4'-bpy)(H2O)2]·H2O (1) and [Zn(BYBA)2(4,4'-bpy)] (2) (4,4'-bpy=4,4'-bipyridine,BYBAH= 2-benzoylbenzoic acid),have been synthesized by hydrothermal conditions and characterized by single-crystal X-ray diffraction,elemental analyses,IR spectra and fluorescence spectrum.Crystal data for 1:C38H32CoN2O9,Mr= 719.59,monoclinic,space group P2/c,a=22.981(2),b=11.4438(11),c=12.9327(12),β=94.642(1)°,V=3390.0(5)3,Z=4,Dc=1.410 g/cm3,F(000)=1492,R=0.0488 and wR=0.1201;and those for 2:C38H26ZnN2O6,Mr=672.00,triclinic,space group P1,a=8.7032(10),b=11.4882(13),c=16.872(2),α=107.146(1),β=99.055(1),γ=90.851(2)°,V=1588.5(3)3,Z= 2,Dc=1.405 g/cm3,F(000)=692,R=0.0409 and wR=0.0894.Complex 1 exhibits 1D polymeric chains which are linked into a 2D sheet by π···π interactions.Complex 2 is composed by 1D zigzag chains connected through C-H···π stacking interactions to generate a 2D layer.     

A Novel Copper（Ⅱ） Coordination Polymer with Figure-of-eight-shaped Channels Occupied by Flexible Monodentate and Bidentate N,N＇-bipyrdyl Ligands

A copper（Ⅱ） coordination polymer, [Cu3（HOA）2（bpp）4]n （1, HnOA = 3,3＇,4,4＇- oxidiphthalic acid, bpp = 1,3-bis（4-pyridyl） propane）, has been hydrothermally synthesized. The crystal structure is of monocl...     

Unprecedented Pseudo Water Tapes Stabilized by a One-dimensional Cu（Ⅱ） Coordination Polymer

A new compound,[Cu(mal)(tmdpy)(H2O)]·4H2O(1,H2mal = malonic acid,tmdpy = 4,4'-trimethylenedipyridine) has been synthesized by the hydrothermal synthesis and structurally characterized by X-ray crystallography. It crystallizes in triclinic,space group P1 with a = 9.1662(6),b = 10.6266(7),c = 11.3056(7) ,α = 84.6390(10),β = 72.1030(10),γ = 73.0420(10) o,V = 1002.37(11) 3,C16H26CuN2O9,Mr = 453.93,Z = 2,Dc = 1.504 g/cm3,μ = 1.140 mm-1,F(000) = 474,R = 0.0375 and wR = 0.0975 for 3187 observed reflections(I > 2σ(I)) . In the structure of 1,the tmdpy ligands link the [Cu(mal)(H2O) ] units into an infinite chain,and the water molecules and carboxylate oxygen donors(O(2) and O(4)) from the mal ligands cooperatively built an interesting hydrogen bonding network with unprecedented pseudo water tape substructures.     

β-Ni(OH)_2纳米线的相转化法制备及电化学性能

采用简单的相转化方法合成出直径为20~30 nm、长度为几微米的β-Ni(OH)_2纳米线.利用XRD和FESEM表征了样品的结构和形貌,并采用循环伏安法、恒流充放电和交流阻抗谱等测试了样品的电化学性能.结果表明,在氢氧化钠溶液中,水热时间为30 min时,Paraotwayite型α-Ni(OH)_2纳米线转化为β-Ni(OH)_2纳米线.在不同扫描速率下,电极材料α-Ni(OH)_2和β-Ni(OH)_2纳米线的可逆性和倍率性能均优于β-Ni(OH)_2纳米片.     

分级花状氧化铁微球的水热合成及吸附性能研究

以六次甲基四胺、硫酸亚铁、柠檬酸钠为原料,采用水热合成方法制备了三氧化二铁(Fe_2O_3)粉体。以铅离子为水体中的模拟污染物,研究了Fe_2O_3对水体中重金属离子的吸附性能,结果表明,当柠檬酸钠的浓度为0.004 mol/L、水热温度为100℃和水热时间为8 h时,所制备的Fe_2O_3的吸附性能最好,其对铅离子的吸附容量为426.09 mg/g。X射线衍射(XRD)图片和扫描电子显微镜(SEM)照片显示所制备的粉体为低结晶度的分级花状Fe_2O_3微球。