Synthesis and Structure of a NovelTetranuclear Erbium( Ⅲ) Complex with α-Alanine [Er4(Hala)6·(μ3-OH)4(H2O)8](ClO4)8·3H2O

The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-ray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a=1.306 3(2) nm, b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β=93.998(11)°, γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R1=0.065 4, wR2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er3+ ions connected by four μ3-OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ3-OH, three carboxylic oxygen atoms from three α-alanine and two oxygen atoms from water molecules, forming a square-antiprismatic coordination polyhedron.     

SYNTHESIS, CHARACTERIZATION AND STRUCTURE OF [Co(DBP)_2·3Py]_2·2CHCl_3

The mixed ligand complex of cobalt with dibutylphosphate (HDBP) and pyridine has been synthesized. Elemental analysis yields the result that the formula of this compound is Co(DBP)_2·3Py·CHCl_3 (Py=pyridine). The thermal analsyis, visible spectra and magnetic properties of it have been studied as well. Single crystal structural analysis shows that the crystal is triclinic with space group P and the unit cell parameters are as follows:a=14.490(10), α=90.37(4)°,b=15.721(7), β=96.04(5)°,c=20.109(12), γ=105.63(4)°.The final R factor is 0.0773. Two Co atoms are connected by two bridging DBP groups to form a dinuclear molecule [Co(DBP)_2·3Py]_2 which has a C_s, symmetry. Each cell contains two dinuclear molecules and four chloroform molecules. The cobalt is coordinated in an octahedral arrangement by three oxygen atoms and three nitrogen atoms, of which one oxygen atom comes from a monodentate DBP group, two oxygen atoms from two bridging DBP groups, and the three nitrogen atoms from the three pyridi     

Structure and electrospray mass spectrometry studies on dithiacyclooctan-3-ol-containing palladium (II) complex of trans -[Pd(dtco-3-OH)_2](ClO_4)_2·2DMSO

The structure of trans-[Pd(dtco-3-OH)2] (ClO4)2·2DMSO, in which dtco-3-OH is dithiacyclooctan-3-ol and DMSO is dimethyl sulfoxide, was determined by X-ray crystallographic analysis. The crystal data: space group pi, a = 0.7077(2) nm, b = 1.0788(1) nm, c = 1.1111(1) nm, α=67.710(8)°, β = 73. 59(2)°, γ = 85. 39(2)°,R1 = 0 . 0368 and Rw = 0.0998. The palladium (II) is coordinated by four sulfur atoms with a regular square planar configuration. The Pd-S distances are 0.2314(1) and 0.2317(1) nm, respectively. Both dtco-3-OH ligands are in the boat-chair configuration and two hydroxyl groups are on the opposite sites of the PdS4 coordination plane and are towards Pd(II). The Pd-O distance is 0. 285 nm, indicating a weak interaction between them. A typical hydrogen bond between the hydroxyl group of dtco-3-OH ligand and DMSO was observed in the crystal structure. An aqueous solution prepared with the crystals of the complex was used for the investigation of electrospray mass spectrometry ( ESMS ). Besid     

配位聚合物[Mn（4，4＇-bpy）1．5（H2O）3]（ClO4）·（4，4＇-bpy）（L）·H2O的水热合成和晶体结构

The title compound, [Mn（4,4＇-bpy）1.5（H2O）3]（ClO4）＇（4,4＇-bpy）（L）·H2O（1）, where L=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a=2.929 9（6） nm, b=1.0364（2） nm, c=8.2220（1） nm, α=105.300（2）°,β=97.495（2）°,）,=91.118（2）°, V=1.884 0（4） nm^3, Z=2, Mr=780.10, Dc=1.375 g·cm^-3,μ=0.483 mm-1, F（000）=812, R=0.055 4, wR= 0.135 2. The Mn atoms are octahedrally coordinated by three N atoms of three 4,4＇-bipyridine ligands and three O atoms of water. The complex shows a one-dimensional chain structure bridged by water and 4,4＇-bipyridine molecules. CCDC： 615707.     

穴状Schiff碱配合物［Gd(NO3)·L］(NO3)2的晶体结构

A new mononuclear gadolinium complex ［Gd(NO₃)·L］(NO₃)₂ of Schiff base cryptand was obtained by condensation of tris (2-aminoethyl)amine with 2,6-diformyl phenol in template procedure. The complex was characterized by elemental analysis, IR, and x-ray single crystal diffraction analysis. Gadolinium is nine-coordinate in trigonal tricapped prism with five oxygen atoms from three phenols and a bidentate nitrate group, and four nitrogen atoms from three imino C=N bonds and a tertiary amine in the cryptand. The complex crystallized in triclinic system space group P1, a=1.0839(2) nm, b=1.2600(4) nm, c=1.7595(4) nm, α=82.09(2)°, β=89.22(2)°, γ=84.06(2)°， V=2.367(2) nm³, Z=2.     

七配位K[InⅢ(Hdtpa)]·3.5H2O配合物的合成及结构测定

In this paper, the title complex K[InⅢ (Hdtpa)] · 3.5H2O(dtpa=diethylenetriaminepentaacetic acid) was synthesized and its crystal structure was determined by single-crystal X-ray structure analysis.The crystal belongs to monoclinic system, P21/c(No. 14) space group with a= 0. 978 1 (2) nm,b=0. 733 8(1) nm, c＝2. 962 9(6) nm, β=91.81(3)°, V=0. 212 6(1) nm3, Z=4, M=606.31, Dx=1.895 g · cm-3, μ=1. 382 1 mm-1, F(000)=1 228, R=0. 035 and Rw=0. 041 for 2 802 unique reflections. The complex anion [InⅢ (Hdtpa)]- has a pseudo-monocapped trigonal prismatic sevencoordination structure in which the seven coordinate atoms, three N and four O atoms, are all from a ligand dtpa. In addition, it can be seen that the complex anion [InⅢ (Hdtpa)]－ can furnish a free carboxyl group(-CH2COOH) being used for molecular embellishment to form the target diagnosis- and treat-drug of anticancer.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis and crystal structure of heteronuclear La(Ⅲ)-Cu(Ⅱ) complex {[LaCu_2(NTA)_2(4,4'-bpy)(H_2O)_3]NO_3·5H_2O}_n

A novel La(Ⅲ)-Cu(Ⅱ)heterometallic coordination polymer {[LaCu2(NTA)2(4,4'-bpy)(H2O)3]NO3 5H2O}n,where H3NTA denotes nitrilotriacetic acid and 4,4'-bpy denotes 4,4'-bipyridine,was synthesized and characterized by IR spectrum,elemental analysis and X-ray diffraction.The complex crystallizes in the triclnic space group PT with cell parameters a=1.33710(10)nm,b=1.44530(10)nm,c=1.0949(2)nm,α=71.905(7),β=74.327(7),γ=64.427(9),V=1.7912(4)nm3 and Z=2.It consists of heterometallic units,in which each La(Ⅲ)ion is coordinated in a distorted mono-capped square antiprism by three oxygen atoms from water molecules and six carboxyl oxygen atoms from five NTA3-ions,and each Cu(Ⅱ)ion is coordinated by one nitrogen atom from 4,4'-bpy and one nitrogen atom,three oxygen atoms from NTA3-.In the title complex,La(Ⅲ)ions and Cu(Ⅱ)ions are connected by the heterometallic bridging of NTA3-,constructing a two-dimensional network structure along the [110].And it is extended into an infinite three-dimensional network struc     

配合物[Cu(PTA)(phen)2]·(PTA)·(H2O)4的合成、晶体结构及电化学性质

The title complex has been synthesized by using terephthalic acid (PTA), 1,10-phenanthroline (phen) and copper monohydrate. It crystallizes in monoclinic space group C2/c with a=2.959 0(2) nm, b=1.466 4(10) nm, c=1.764 3(12) nm, β=105.593(11)°, V=7.372(9) nm³, Dc=1.489 g·cm^-3, Z=8, F(000)=3 416, R₁=0.043 6, wR₂= 0.151 9. The crystal structure shows that the copper atom is coordinated with four nitrogen atoms from two phens and one oxygen atom from one terephthalic acid, forming a distorted square-pyramid coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 277047.     

Synthesis,Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Cu（phen）（2,4,6-TMBA）2（H2O）]n

A one-dimensional chain coordination polymer [Cu（phen）（2,4,6-TMBA）2（H2O）]n has been synthesized by reacting 2,4,6-trimethyl-benzoic acid, 1,10-phenanthroline and Cu（Ⅱ） perchlorate and its structure was characterized. Crystal data for this complex： tetragonal, space group I41, a = 2.0293（3）, b = 2.0293（3）, c = 1.3758（2） nm, α =β= γ = 90°, V= 5.6657（13） nm3, Dc= 1.379 g/cm3, Z = 8, μ（MoKa） = 0.815 mm-1, Mr = 588.14, F（000） = 2456, S = 1.047, R = 0.0459 and wR = 0.1053. The crystal structure shows that two neighboring Cu（Ⅱ） ions are linked together by one bridging-chelating 2,4,6-trimethyl-benzoic group, forming a one-dimensional chain structure. Each Cu（Ⅱ） ion is coordinated with two nitrogen atoms from one 1,10-phenanthroline molecule, three oxygen atoms from three 2,4,6-trimethyl-benzoic acid molecules and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. The cyclic voltammetry behavior of the complex was also investigated.     

配位聚合物[Mn(4,4′-bpy)_(1.5)(H_2O)_3](ClO_4)·(4,4′-bpy)(L)·H_2O的水热合成和晶体结构(英文)

The title compound, [Mn(4,4'-bpy)1.5(H2O)3](ClO4)·(4,4'-bpy)(L)·H2O(1), where L=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 0(1) nm, α=105.300(2)°, β=97.495(2)°, γ=91.118(2)°, V=1.884 0(4) nm3, Z=2, Mr=780.10, Dc=1.375 g·cm-3, μ=0.483 mm-1, F(000)=812, R=0.055 4, wR=0.135 2. The Mn atoms are octahedrally coordinated by three N atoms of three 4,4'-bipyridine ligands and three O atoms of water. The complex shows a one-dimensional chain structure bridged by water and 4,4'-bipyridine molecules. CCDC: 615707.     

Synthesis, Crystal Structure and Electrochemical Properties of One-dimensional Chain Coordination Polymer [Co(II)(C_6H_5CH=CHCOOH)_2(4,4′-bipy)(H_2O)_5]_n

A one-dimensional chain coordination polymer [Co(II)(C6H5CH=CHCOOH)2(4,4′- bipy)(H2O)5]n has been synthesized with cinnamylic acid, 4,4′-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a = 1.1481(3), b = 1.1230(2), c = 1.1759(3) nm, β = 97.054(4)o, V = 1.5046(6) nm3, Mr= 617.50, Dc = 1.363 g/cm3, Z = 2, μ(MoKα) = 0.627 mm-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(II) ions are linked together by one 4,4′-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(II) ion is coordinated with two nitrogen atoms from two 4,4′-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Mn2（phen）2（p-CBA）4（H2O）

One novel complex Mn2(phen)2(p-CBA)4(H2O) has been hydrothermally syn- thesized from p-chlorobenzoic acid (p-CBA), 1,10-phenanthroline (phen) and anhydrous man- ganese(Ⅱ) sulfate and then characterized. Crystal data for this complex: monoclinic, space group C2/c, with a = 2.3416(3), b = 1.5604(2), c =1.5605(2) nm, β = 121.048(2)o, V = 4.8849(12) nm3, Dc = 1.510 g/cm3, Mr = 555.26, Z = 8, μ = 0.798 mm-1, F(000) = 2256, GOOF = 1.032, the final R = 0.0393 and wR = 0.0816. The crystal structure shows that two neighboring manganese(Ⅱ ) ions are linked together by two bridge-chelating p-chlorobenzoic groups and one bridging water molecule, forming a cage structure with the Mn–Mn bond distance of 0.3512 nm. Each manganese(Ⅱ ) ion is coordinated by two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three p-chlorobenzoic acid anions and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the complex was also investigated.     

Synthesis, molecular structure and intramolecular aromatic-ring stacking interaction of a novel binuclear Cu(Ⅱ) complex with 1, 10-phenanthroline and phenylacetate

The complex [Cu(phen)2(POAc)3]ClO·4H2O has been synthesized and investigated by elemental analysis, IR spec-troscopy and X-ray diffraction methods, where phen = 1,10-phenanthroline, POAc = phenylacetate group). The complex crystallizes in the triclinic space group PI with two molecules in a unit cell of dimensions a = 1.0579(2) nm, b = 1.2423(3) nm, c = 1.9190(4) nm, α = 71.84(1)°, β = 80.50(2)°, γ = 88.60(1)°, V = 2.3625(9) nm3, R = 0.0407 and Rw = 0.0656. The complex results from bridging of two Cu(phen)2 units by three carboxylate groups, and each Cu2 ion is in a distorted square pyramidal geometry with two nitrogen atoms of phen and three carboxylate oxygen atoms of POAc. It has been showed that intramolecular stacking interactions occur between the phenyl moieties of POAc and aromatic rings of phen, leading to a novel molecule structure with two coordinating modes of carboxylate ligands, of which two phenylacetates are μ2-carboxylate-O-bridging ligands, and the other is a μ2-carboxylate-     

Synthesis,Crystal Structure and Fluorescent and Thermal Stability Properties of the Zinc(Ⅱ) Complex [Zn(C_(15)H_(11)O_3)_2(C_(12)H_8N_2)_2]·5H_2O

A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.     

二硝酸N，N′-二癸酰基哌嗪合铀酰(II)配合物的合成和晶体结构

The complex UO₂(DDPEZ)(NO₃)₂ has been prepared and characterized by IR spectroscopy and XPS spectra. The crystal structure of the complex has been determined by X-ray diffraction. The crystal belongs to Triclinic system and space group P1, with cell parameters: a=0.664 2(3) nm, b=0.805 0(2) nm, c=1.515 6(5) nm, α=104.39(2)°, β=91.13(3)°, γ=94.84(3)°, and V=0.781 4(5) nm³, Z=2, D_c=1 676 kg·m^-3, μ(Mo Kα)=0.071 073 nm, F(000)=390, final R=0.037 9 and wR=0.091 7 for observed reflections[I>2σ(I)]. The results indicated that uranyl ion is coordinated with six oxygen atoms, four of them from two nitrate groups and two from carbonyl groups of different organic ligands. CCDC: 284452.     

CRYSTAL STRUCTURE OF (C_5H_9C_5H_4)_3Er_4(μ_2-Cl)_6(μ_3-Cl)(μ_4-O)-(THF)_3

<正> The crystal of (C5H9C5H4)Er4(μ2-Cl)6(μ3-Cl)(μ4-O)(THF)3 belongs to triclinic space group P1, with a = 11. 909(4), b = 15.343(5), c=15. 619 (4)(?), α=104. 18(2), β=98. 81(3), γ= 111. 06(2)°, V = 2486(1)(?)3, Z = 2, Dc = 2. 07g/cm3, λ(MoKα) = 0.71073(?), μ= 73. 4cm-1, F(000) = 1476, Mr=1549. 25. The structure was solved by Patterson and Fourier techniques and refined by block diagonel least-squares method to final R = 0. 078 and Rw = 0. 084 for 5594 reflections with I≥1. 5σ(I). The results revealed that the complex is composed of four Er atoms bridged by seven Cl and one oxygen atoms with three of the Er atoms bonded each to a cyclopentylcyclopentadienyl group, and one Er atom, bonded to three THF. The Er atoms constitute a pseudo-tetrahedron.     

Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis,Crystal Structure and Thermal Stability Properties of a Binuclear Copper(Ⅱ) Coordination Polymer {[Cu_2(4,4'-bipy)_2(o-ABA)_4(H_2O)_2][(H_2O)_2]}_n

One-dimensional chain copper(Ⅱ) coordination polymer has been synthesized and characterized in the solvent mixture of water and alcohol with o-acetamidobenzoic acid,4,4'-bipyridine and copper perchlorate.It is of tetragonal,space group P41212 with a=1.57756(10),b= 1.57756(10),c=2.1438(3)nm,V=5.3352(8) nm3,Dc=1.524 g/cm3,Z=4,F(000)=2536,R= 0.0479 and wR=0.0979.The crystal structure shows two coordination modes.The copper(1) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule and two oxygen atoms from two o-acetamidobenzoic acid molecules,forming a distorted tetrahedral coordination geometry;the copper(2) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule,four oxygen atoms from two o-acetamidobenzoic acid molecules and two water molecules,generating a distorted octahedral coordination geometry.The result of TG analysis shows that the title complex is stable below 180.0 ℃.     

CRYSTAL STRUCTURE OF CK(C_(12)H_(24)O_6)]_2Pd(SCN)_4(H_2O)

<正> [K(C_12H_24O_6)]_2Pd(SCN)_4(H_2O),MT=963.59,monoclinic, P21/n,a= 11. 075(1),b= 12. 231(1),c= 15. 863(2) A ,β=93. 25(1)°,V=2145. 3A3,Z=2, Dc=1. 492gcm-3,λ(MoKa) = 0. 71073A μ=8. 64cm-1,F(000) = 996,final R=0. 045 for 1835 observable reflections. The Pd2+ ion coordinates with four S atoms from SCN- groups forming a regular square planar configuration. The K+ ion is surrounded by six ether oxygen atoms,one O atom from water molecule coordinated to two K+ions and one N atom from SCN- group to form a distorted hexagonal bipyramid. Two K atoms are linked with one Pd atom by two bridging SCN- groups forming a chain molecular array in the crystal.