配合物[Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N的结构与磁性研究

The complex [Mn(C₁₃H₈N₂OBr)₂(C₅H₅N)₂]·3C₅H₅N has been synthesized and characterized by X-Ray diffraction, IR and variable temperature (～10 to ～278K) magnetic susceptibility. X-Ray diffraction result for the single crystal shows that the crystal belongs to monoclinic, space group P2₁/c, a=1.0969(3)nm, b=2.0903(5)nm, c=2.0481(6)nm, β=97.366(6), V=4.657(2)nm³, Z=4, D_c=1.47g·cm^-3。     

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.     

一个新的三维配位聚合物Na[Cu2(malonate)2]·(ClO4)·(H2O)2的合成与表征(英)

通过Cu(ClO₄)₂和丙二酸在水溶液中的自组装合成了一个新的3D配位聚合物：Na[Cu₂(malonate)₂]·(ClO₄)·(H₂O)₂。X-射线结构分析表明该化合物晶体属于正交晶系Pnma空间群(a=1.256 5(3)，b=1.0594 3(2)，c=1.0755 6(14) nm，V=1.431 7(4) nm³，Z=4)。该聚合物的空间堆积在沿b轴和c轴方向分别形成大小为0.98 nm × 0.83 nm和0.40 nm × 0.40 nm的方形孔洞，在沿a轴方向形成大小为0.85 nm × 0.40 nm的砖墙形孔洞。磁性测试结果表明该化合物显示出铁磁性。导电性能测试实验表明它是一个半导体，经拟合得到其活化能为0.80 eV。     

混配配合物[Zn(CF3COO)2(C7H6NS)2]的合成、晶体结构及表征

A mixed complex [Zn(CF₃COO)₂(C₇H₆NS)₂] was synthesized based on the reaction of Zn(CF₃COO)₂ and 2-aminobenzothiazol (C₇H₆NS) in methanol. The structure of the complex was characterized by elemental analysis, IR, ¹H NMR and thermal analysis. The crystal structure of the complex was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group C2/c, a=3.174 3(9) nm, b=1.010 0(3) nm, c=1.723 1(5) nm, β=118.841(4)°, V=4.839(2) nm³; D_c=1.625 g·cm^-3; Z=8; F(000)=2 368; μ=1.266 mm^-1. CCDC: 600233.     

以吡啶为配体的镍配合物[Ni(py)3(H2O)3] (1, 5-nds)的合成、晶体结构及性质研究

采用缓慢蒸发法, 在水溶剂中合成了含氮配体单核Ni(Ⅱ)配合物[Ni(py)₃(H₂O)₃] (1, 5-nds)(py=pyridine, 1, 5-nds=1, 5-萘二磺酸根离子)。采用X射线单晶衍射、红外光谱、热分析和紫外可见光谱等方法对配合物进行了表征。X射线单晶衍射表征结果表 明, 该配合物晶体属于单斜晶系, 空间群为C2/c。晶体学参数:a=1.569 46(17) nm, b=1.219 95(12) nm, c=1.454 71(16) nm, β=14.547 1(16)°, V=2.765 1(5) nm³, Z=4。考察了该配合物的磁性和荧光性质。     

发光的二维Cu(Ⅰ)分子箱[CuCl(DBBD)2]n

Hydrothermal treatment of CuCl and atropisomeric ligand racemic-diethyl (R,S)-4,4′-biquinoline-6,6′-diethyl-3,3′-dicarboxylate (DBBD) (1) in the presence of H₂O and C₂H₅OH over 4 days at 104～109 ℃ yielded colorless block crystals [CuCl(DBBD)₂]_n (2). The compound exhibits strong red fluorescent emission with a wavelength of 650 nm. The crystal of [CuCl(DBBD)₂]_n belongs to monoclinic system with space group C2/c, and a=1.656 58(17) nm, b=2.025 0(2) nm, c=1.548 73(16) nm, β=107.879(2)°, V=4.944 4(9) nm³, D_c=1.417 g·cm^-3, Z=8. CCDC: 292932.     

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。     

Ln(NO3)3·C26H38N2O4(Ln=La、Ce)配合物的合成和La(NO3)3·C26H38N2O4·CH3CN的晶体结构

合成了2个新的希土冠醚配合物Ln(NO₃)₃·C₂₆H₃₈N₂O₄(Ln=La、Ce; C₂₆H₃₈N₂O₄=1, 7, 10, 16-四氧-4，13-二氮杂-N，N′-二苄基环十八烷)。通过元素分析，红外光谱，拉曼光谱及其 ¹H核磁共振谱进行表征。用四圆衍射仪测定了La(NO₃)₃·C₂₆H₃₈N₂O₄·CH₃CN的晶体结构。晶体属三斜晶系，P1空间群，晶胞参数：a=1.2869(4) nm, b=1.5868(6) nm, c=0.9147(2) nm; α=101.89(2)°, β=105.38(2)°, γ=71.96(3)°; Z=2。d_cald.=1.58 g·cm^-3, μ(MoKα)=13.25 cm^-1。中心镧离子与冠醚配体中的4个氧原子和2个氮原子配位，3个硝酸根中的6个氧原子也与La³⁺配位，形成配位数为12的配合物。     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to monoclinic system with space group P2₁/c, a=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.     

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。     

Synthesis and Crystal Structure of （H3O）2[Cu3Cl3（H2O）3（NC9H12.5O6）2]

1 INTRODUCTION The polydentate ligand nitrilotripropionic acid, H3ntp[N(CH2CH2COOH)3], has attracted conside- rable research interest in constructing coordination polymers, designing organic-inorganic hybrid mate- rials[1], synthesizing supramolecular compounds[2], etc. due to its high degree of flexibility with three carboxylic acid moieties allowing for a variety of coordination through oxygen atoms[3]. It also pro- vides other versatile properties such as the possibili- ty of inter-…     

[Pb2(TNR)2(CHZ)2(H2O)2]4H2O的结构及热分解机理

The coordination compound of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O was prepared by using the aqueous solution of carbohydrazide, lead nitrate and sodium styphnate. The molecular structure of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O(C 7H 13 N 7O 12 Pb, Mr=594.43) was determined by using a single crystal diffraction analysis .The thermal decomposition mechanism of the title compound was studied by TGDTG, DSC and IR techniques. The crystal belongs to monoclinic with space group P2 1/n.The unit cell parameters are as follows: a=0.64700(10)nm, b=1.6074(3)nm, c=1.4883(3)nm,β=97.42(2)°,V=1.5349(5)nm3, Z=2, DC=2.572g•cm -3 ,μ(Mo, Kα)=11.080cm -1 , F(000)=1128. R=0.0422, Rw=0.0735. The binuclear lead coordination compound is bridged by two carbohydrazide molecules. The molecule has a symmetrical center. TNR 2- ,CHZ and H 2O coordinate with the central ions simultaneously.     

一维链状配位聚合物[Cu(CH3COO)(C5H5N)2]n的合成与晶体结构

The coordination polymer [Cu(CH3COO)(C5H5N)2]n was synthesized and its crystal structure has been determined by X-ray diffraction technique.The crystal belongs to monoclinic,space group C2/c with a=1.183 2(1) nm,b=1.512 1(2) nm,c=1.3911(1) nm,β=97.137(3)°,V=2.469 6(4) nm3,C12H13CuN2O2,Mr=280.78,Z=8,Dc=1.510 g·cm-3,μ=1.759 mm-1,F(000)=1 152,R1=0.048 2 and wR2=0.122 5 for 1 515 observed reflections [1>2σ(Ⅰ)].In the crystal the copper(Ⅲ) atom is tetra-coordinated primarily by two oxygen atoms of two symmetry-related carbexyl groups of acetate anions and two nitrogen atoms of two pyridine ligands in a parallelogram fashion.All of the pyridine rings linked to Cu(1) and Cu(2) are arranged centrosymmetrically on Cu(1).The neighboring copper complex molecules are linked together by the carboxylate oxygen atom of acetate anions to form an infinite one-dimensional linear chain structure.Moreover,π-π stacking interactions between intrachain pyridine molecules play the crucial role in constructing of the supramolecular structure.CCDC:709977.     

配合物Pb(cbba)_2(phen)_2的水热合成、晶体结构与荧光性能研究(英文)

A new metal-organic complex Pb(cbba)2(phen)2 (1, H2cbba=2-(4′-chlorine-benzoyl)benzoic acid, phen= 1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, fluorescence spectrum and single-crystal X-ray diffraction. The compound crystallizes in orthorhombic, space group Pbcn with a=1.474 49(7) nm, b=0.953 90(4) nm, c=3.031 65(14) nm, V=4.264 1(3) nm3, C52H32Cl2N4O6Pb, Mr=1 086.91, Dc=1.693 g·cm-3, μ(Mo Kα)=4.141 mm-1, F(000)=2 144, Z=4, the final R=0.018 3 and wR=0.045 7 for 3 582 observed reflections (I2σ(I)). In the crystal structure, the lead atom is six-coordinated with two carboxylate oxygen atoms from different cbba ligands and four nitrogen atoms from different phen ligands, showing a distorted octahedral geometry. Furthermore, 1 shows yellow photoluminescent property at room temperature.     

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.     

(TAGH)2(TNR)的合成、晶体结构及热分析

合成了三氨基胍三硝基间苯二酚盐(TAGH)2(TNR) (TAG: 三氨基胍; TNR: 2,4,6-三硝基间苯二酚), 并对其进行了元素分析及红外光谱表征. 利用X射线单晶衍射分析测定了其晶体结构. 该晶体属于单斜晶系, 空间群为C2/c, 晶体学数据为, a=2.2892(6) nm, b=1.2802(3) nm, c=1.3661(4) nm, β=111.174(5)°, V=3.7333(16) nm3, Z=8. 该化合物是由二个C(N2H3)+3与一个(C6HN3O8)2-相结合而成的离子型化合物. 用差示扫描量热法、热重法和微商热重法研究了该化合物的热分解过程, 研究结果表明, 在10 K·min-1的升温速率下, 该化合物只有一个剧烈的放热分解过程, 该过程发生在450.1-477.7 K之间, 且分解产物主要是气体产物.     

草酰胺桥联异三核配合物Cu(NiL)2(ClO4)2的合成、光谱表征和晶体结构(英)

A novel oxamido-bridged trinuclear complex Cu(NiL)₂(ClO₄)₂(where H₂L=2,3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,3-dien) has been synthesized and characterized by elemental analysis, IR spectrum, UV-Visible spectrum and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P2₁/n. The lattice parameters are: a=1.052 4(6) nm, b=1.182 1(6) nm, c=1.586 2(9) nm, β=91.657(9)°, and V=1.972 6(19) nm³, Z=2. The results show that the coordination geometry around copper(Ⅱ) in the title complex is hexa-coordinated octahedron. CCDC: 232608.     

二维Hofmann类双金属配合物Cu(DMF)_2[Pt(CN)_4]的合成及晶体结构(英文)

A two-dimensional cyanide-bridged Cu(Ⅱ)-Pt(Ⅱ) bimetallic complex has been synthesized by solution diffusion method using [Pt (CN)4]2- and [Cu (L)]2+ (L =3,10-diethanol-1,3,5,8,10,12-hexaazacyclotetradecane) as building blocks. Unexpectedly, the obtained complex Cu(DMF)2[Pt(CN)4] (1) is an analogue of the well-known Hofmann -type clathrate without macrocyclic ligand. Single-crystal X-ray diffraction reveals that 1 crystallizes in monoclinic, space group C2/m, a=1.624 8(6) nm, b=0.739 3(3) nm, c=0.695 5(3) nm, β=108.969(4)°. The crystal structure of 1 consists of two-dimensional corrugated metal cyanide sheets without interpenetration stacking along the a axis in an ABAB packing mode.     

有机锡配合物{[(n-C8H17)2Sn(O2CCH2CS2NC4H8O)]2O}2的合成，表征及晶体结构

The title complex {[(n-C₈H₁₇)₂Sn(O₂CCH₂CS₂NC₄H₈O)]₂O}₂ has been synthesized by the reaction of (morpholinylthiocarbamoylthio)acetic acid with the di-n-octyltin oxide in 1∶1 molar ratio. The complex was characterized by elemental analysis, IR and ¹H NMR. The crystal and molecular structure of complex was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system with space group P1 and unit cell dimensions: a=1.201 5(9) nm, b=1.481 8(11) nm, c=1.894 1(14) nm, α=72.485(10)°, β=88.586(10)°, γ=66.893(9)°, and Z=1, μ=1.034 mm^-1, V=2.941(4) nm³, D_c=1.295 g·cm^-3, F(000)=1 196, R₁=0.058 8, wR₂=0.155 8. The complex is a centrosymmetric structure with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom. The endo-cyclic tin atoms and the exo-cyclic tin atom are all five-coordinate and have coordination geometry of distorted trigonal bipyramid with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are monodentate and connecting to each of exo-cyclic tin atoms by using one oxygen atom, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom. CCDC: 277048.     

有机锡化合物[n-Bu2Sn(OH)OS(O)2(p-ClPh)]2的合成、晶体结构和催化性能

An organotin compound, [n-Bu₂Sn(OH)OS(O)₂(p-ClPh)]₂, has been synthesized by the reaction of n-Bu₂SnO with p-ClPhSO₃H and characterized by IR, elemental analysis and X-ray diffraction single crystal structure analysis. The results show that it possesses a polymeric sheet structure with repeating 20-membered macrocycles by virtue of the bridging bidentate sulfonate groups; the crystal belongs to monoclinic, space group P2₁/c with a=1.460 72(12) nm, b=0.897 41(11) nm, c=2.896 94(14) nm, β=107.629(4)°, V=3.619 2(6) nm^-3, Z=4; all the tin atoms are six-coordinated in a distorted octahedral geometry. The compound showed the very high catalytic activity in the transesterification of dimethyl carbonate and phenol to diphenyl carbonate. CCDC: 751163.