[NiCl(Ph_2PCH_2CH_2OH)_2Cl·H_2O]~+Cl~-和[Ni(Ph_2P(O)CH_2CH_2OH)_4]~(2+)[NiCl_4]~(2-)的合成及晶体结构

通过NiCl2·6H2O与双齿配体2-(二苯基膦)乙醇(Ph2PCH2CH2OH)或其氧化物2-(二苯基氧膦)乙醇[Ph2P(O)CH2CH2OH]的反应,制得两种结构新颖的阳离子型镍配合物[NiCl(Ph2PCH2CH2OH)2 (H2O)]+Cl-(1)和[Ni(Ph2P(O)CH2CH2OH)4]2+[NiCl4]2-(2).通过元素分析、31P核磁共振及X射线单晶衍射对配合物1和2的结构进行了表征.配合物1的晶体属单斜晶系,C2/c空间群,中心金属Ni具有六配位八面体几何构型.配合物2属四方晶系,I4(1)/a空间群,中心原子Ni与PO基团中的O配位形成平面四边形构型.     

Crystal Structure of [CH_3CH(OH)COO]_2Fe(H_2O)_2·H_2O

<正> The title compound C6H16O9Fe, Mr = 288. 13, was synthesized and crystallized in monoclinic space group P21/c, a = 9. 409(4), b = 5. 812(4), c= 22. 122(7)(?) , β=90. 80(3)°. V = 1209. 6(?)3, Z = 4, Dc=1. 572g/cm3, F(000) = 592, μ = 12. 73cm-1, R = 0. 063, Rw= 0. 068 for 1191 observed reflections. The iron atom is surrounded by O(1 - 6) in a distorted octahedron.     

Syntheses and Structures of Two New Cobalt Supramolecular Complexes, [Co(4,4'-bipy)_2(H_2O)_4]· [Co_2(4,4'-bipy)3O(H_2O)_8]·2TST·2(4,4'-bipy)·4H_2 and [Co(4,4'-bipy)_2(H_2O)_4]DSNT'4,4'-bipy

Two new cobalt(Ⅱ) supramolecular complexes [Co(4,4'-bipy)_2(H_2O) _4]·[Co_2(4,4'-bipy)3-(H_2O) _8]·2TST-2(4,4'-bipy)·4H_2O 1 and [Co(4,4'-bipy) _2(H_2O) _4]DSNT·4,4'-bipy 2 based upon the assembly of Co(Ⅱ), 4,4'-bipyridine (4,4'-bipy) and two new multifunctional organic ligands, 2,4,6-tris(4-sulfophenyl-amino)-1,3,5-triazine (H_3TST) and 2,4-bis(p-sulfanilato)-6-diethylamino-1,3,5-triazine (H_2DSNT), have been prepared by hydrothermal method and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal structure of 1 is of monoclinic, space group P2_(1/n) with α= 13.599(4), b = 18.988(6), c = 22.995(7) A, β = 90.273(6)°, V= 5938(3) A~3, Z = 4, C_(56)H_(59)CO_(1.5)N_(13)O_(17)S_3, M_r = 1370.74, D_c = 1.533 g/cm~3,μ = 0.613 mm~(-1), F(000) = 2842, GOOF = 1.018, the final R = 0.0796 and wR = 0.1498 for 9019 observed reflections with I > 2o(I). The crystal structure of 2 belongs to the monoclinic system, space group C2/c with α = 18.864(6), b = 14.283(5), c = 20.246(7) A, β = 107.799(6)°, V = 5194(3) A~3, Z = 4, C_(49)H_(52)CoN_(12)O_(10)S_2, M_r = 1092.08, D_c = 1.397 g/cm~3, μ= 0.480 mm~(-1), F(000) = 2276, GOOF = 1.059, the final R = 0.0665 and wR = 0.1900 for 4887 observed reflections with I> 2σ(I). The results of X-ray crystal structure analysis revealed that complexes 1 and 2 exhibit layered supramolecular frameworks stabilized by electrostatic interactions, π-π interactions and hydrogen bonds.     

钴配合物[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4的合成与晶体结构研究

用硫酸钴、4,4'-联吡啶和2-磺酸基乙基膦酸合成了一个新颖的钴化合物:[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4,并对其进行了红外.元素分析、热重测试,通过单晶衍射仪测定了其晶体结构.结果表明,配合物属单斜晶系C2/c空间群,分子式为C_(22)H_(45)Co_2N_4O_(22)PS_2,分子量为930.57,晶胞参数为a=19.8456(18),b=11.2957(10),c=34.719(3)(A),β=106.095(3)°,晶胞体积为7477.9(12)(A)~3,Z=8,Dc=1.653 g/cm~3,F(000)=3856,μ=1.131 mm~(-1),最终残差因子R_1=0.0726,wR_2= 0.1719(相对于5612个I>2σ(I)的可观测衍射点).在这个化合物中,二齿配体4,4'-联吡啶把Co(II)桥连成[Co(4,4'-bipy)]~(2+)链.化合物中的[Co(4,4'-bipy)]~(2+)链有三个不同的朝向.2-磺酸基乙基膦酸没有参与配位而是做为一个有机模板剂填充在[Co(4,4'-bipy)]~(2+)链形成的空隙中.     

一维链状高价锰配合物[Mn_2(C_7H_4O_3)_4(CH_3OH)_2]·4H_2O_2CH_3OH的合成与结构

合成了一维链状高价锰配合物[Mn2(C7H4O3)4(CH3OH)2]4H2O2CH3OH,并对其进行了IR、X-射线衍射、UV-Vis和TG-DSC等表征。单晶衍射结果表明,该配合物晶体属三斜晶型,空间群P?晶胞参数a=7.653(5),b=10.486(7),c=12.943(8),=103.24(1),?=104.55(1),?=110.11(1),V=885.4(9)3,Z=1。UV-Vis光谱在547nm有一个吸收峰,相应于Mn(Ⅳ)的d-d电子跃迁光谱。     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex:[NdFe(CN)_6(DMF)_4(H_2O)_3]H_2O

1 INTRODUCTION In recent years, cyano-bridged heterometallic coordination compounds have inspired remarkable attention due to their rich and interesting structures and magnetic behaviors. However, these studies were mainly focused on the transition metals. Although several unusual cyanide bridging lanthanide-transition metal complexes have been re- ported[1～6], this field continuously possesses tre- mendous researching potentialities. As regardsPrussian Blue lanthanide complex, divers…     

Synthesis and Crystal Structure of (CH_2)_3(3,5-Me_2Pz)_2. [PhBr_2Sn(CH_2)SnBr_2Ph].2HBr.H_2O (Pz=pyrazole)

1 INTRODUCTION The coordination chemistry of tin or organotin toward poly(pyrazol-1-yl)borate ligands has been extensively investigated in recent years owing to the antitumor activity of some related organotin derivatives containing N-donor ligands. A number of organotin(Ⅳ) complexes containing poly(pyrazol- 1-yl)borate ligands have been synthesized and characterized[1~3], some of which have also shown interesting structural characteristics and reactivities[4~6]. Recently, poly(pyrazol…     

双核有机锡(Ⅳ)配合物[Ph_3Sn(CH_3OH)O_2CC_6H_4CO_2(CH_3OH)-SnPh_3]·2CH_3OH和[Ph_3SnS_2CN(CH_2CH_2)_2NCS_2SnPh_3]·2CH_3OH的合成、表征和晶体结构

利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物 1由未配位的甲醇分子通过氢键作用形成二维网状结构     

Synthesis and Crystal Structure of [Cu (C_8H_4O_2F_3S) (2, 2' -bipy) ]

1INTRODUCTIONCoppercomplexesarewidelyusedascatalystsinthedecompositionofdisubsti-tutedperoxides"'-Theelectronicstructureandbondingatthecatalystscanbeprof-itablypursuedbystudyingmodelcomplexes.Generally,theCu(I)complexesareob-tainedbyreactionofCu(l)saltswithligands.Wereporthereamethodofpreparingcopper(I)complexbythereactionofCupowderwith2-thenoyltrifluoroacetone,2,2'-bipyinmethanol.2EXPERIMENTALReactionwascarriedoutundernitrogenatmosphere.2,2-bipy(1mmol)wasaddedtoamixtureof2-thenoyl…     

Synthesis, Crystal Structure and Luminescence Property of [Co(hmz)_2(H_2O)_4]·2H_2O

A new mononuclear Co(II) complex, [Co(hmz)2(H2O)4]·2H2O, has been synthesized by the reaction of Co(CH3COO)2·4H2O with 1-(4-hydroxyphenyl)-5-mercaptotetrazole (Hhmz). It crystallizes in the monoclinic system, space group P21/n with a = 13.502(5), b = 6.718(3), c = 13.972(6) , β = 117.532(4)o, V = 1123.9(8) 3, Z = 2, M r = 553.45, F(000) = 570, Dc = 1.635 g/cm3, μ = 1.008 mm–1, the final R = 0.0272 and wR = 0.0684 for 2194 observed reflections (I > 2σ(I)). The Co(II) is six-coordinated by two nitrogen atoms from two hmz–1 ligands and four water molecules, forming an octahedral geometry. The intermolecular hydrogen bonding and offset-panel π-π stacking interactions between the adjacent molecules extend the compound into a three- dimensional supramolecular framework. The title compound emits strong blue fluorescent light (λem(max) = 427 nm) at room temperature and is red-shifted compared with free ligand Hhmz (λem(max) = 342 nm).     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C_(13)H_9N_2O)Cl]_2·(CH_3CN)_2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2), has been synthesized and characterized by X-ray structure determination. It crystallizes in the tricli- nic system, space group P1, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) , α = 81.338(3), β = 88.173(4), γ = 66.199(3)o, V = 718.9(2) 3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3, μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions, and one chlorine atom). Two copper(II) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(II)–Cu(II) binuclear entity, and the distance between two copper(II) atoms is 3.0144(15) .     

[Nd(4-PYA)_3(H_2O)_2]_n的合成及其晶体结构

3-(4-吡啶基)丙烯酸(4-HPYA)和Nd(NO3)3通过水热法合成了一种新的一维链状配位聚合物[Nd(4-PYA)3(H2O)2]n(1),其结构经IR,元素分析和X-射线单晶衍射表征。1属三斜晶系,P-1空间群,晶胞参数:a=0.829 23(13)nm,b=1.272 60(2)nm,c=1.435 00(12)nm,α=112.371(2)°,β=98.856(3)°,γ=100.239(2)°,V=1.336 6(3)nm3,Mr=660.72,Z=2,Dc=1.642 g.cm-3,F(000)=662,μ=2.002mm-1,R1=0.052 3,wR2=0.141 9。1通过分子间氢键作用将一维链紧密堆积成三维网状结构。     

Structure of Complex [Ni_2L_2](py)_2(H_2O)_2(L=1,3-Di[o-(o-vanillideneimino) phenoxo]-2-propanol Dianion) with New Nucleating Ligand

Accordingtotheclassificationofdinucleatingligands',thetitleligandL'-(H,L)shou1dbecompartmentalized,havingthepotentialbridgingthehydroxogroup,O(7)orO(7a),inthemiddleofthemolecularchain.However,thisnewcomplexL2'alsointerestinglybelongstoanotherclass,whereitstwosetsofdonoratomscoordinatetothetwocentermetals,respectively.SeeFigUrel.TheSchiffbaseH2Lwassynthesizedbycondensingo-vanillinanditscorrespondingdiamine.TheprecursorcomplexwaspreparedbydirectlyrefluxingequimolarratiosofHzLandNi(OAc)24H…     

CRYSTAL STRUCTURE OF DI - NITRATOBIS(ETHYLCAPROLACTAM)URANYL(Ⅱ) UO_2[CH_2(CH_2)_4CONC_2H_5]_2(NO_3)_2

The crystal structure of Di-nitratobis(ethylcaprolactam)uranyl(Ⅱ) UO_2[CH_2(CH_2)_4CONC_2H_5]_2(NO_3)_2 was established by a single-crystal X-ray diffraction study.It is triclinie, space group P1, with a=7.171(2), b=8.655(3), c=10.182(5)A, α=78.27(3), β=70.63(3), γ=81.76(3)°, V=581.7(4)A~3, Z=l, Dc=1.94 g.cm~(-3).Final R value is 0.0218.The result reveals that uranyl ion is coordinated to six oxygen atoms, two of them are from two carbonyl groups of ethylcaprolactam and the other four are from two nitrate groups.     

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.     

配位聚合物[Ni(H_2O)_6]·[Ni_2(phen)_2(BTC)_2(H_2O)_4]·4H_2O的水热合成和结构表征

采用水热法合成了新的配合物[Ni(H2O)6].[Ni2(phen)2(BTC)2(H2O)4].4H2O(phen=邻菲啰啉;BTC=均苯三甲酸),采用X射线单晶衍射结构分析及元素分析、红外光谱等表征,并用TGA检测了该配合物的热稳定性.晶体属于三斜晶系,空间群为P-1,晶胞参数a=0.84038(7)nm,b=0.92048(8)nm,c=1.64793(14)nm,α=97.3850(10)°,β=102.7930(10)°,γ=104.9700(10)°,V=1.17736(17)nm3,F(000)=622,Z=1.标题化合物的不对称结构是由NiO6单元和1个二聚物Ni2N4O12单元组成的,该二聚物单元通过2个邻菲啰啉和2个均苯三甲酸分子构筑了1个八元环.氢键将2个独立的结构单元连接成三维结构.     

[Tb(CH_3COO)_3(H_2O)_2]_2的合成及其结构测定

2-羟基吡啶、希土高氯酸盐和乙酸钴在乙腈中反应,制备了九配位化合物[Tb(CH_3COO)_3·2H_2O]_2该晶体为三斜晶系,P~(?)空间群,其晶胞参数为a=8.870(4)(?),b=9.247(1)(?),c=10.586(1)(?),α=65.13(1)°,β=64.43(2)°,γ=62.16(4)°,V=665.97(?)~3,Z=1,F(000)=394。测定了配合物的红外光谱。讨论了它的生成机制。     

新型杂多蓝化合物[NH_3(CH_2)_2NH_3]_5[Cd(H_2O)][CdMo_(12)~ⅤO_(30)(HPO_4)_6(H_2PO_4)_2]·5H_2O的合成与晶体结构

利用水热法首次合成了具有两种配位环境Cd原子的新型杂多蓝化合物[NH3(CH2)2NH3]5[Cd(H2O)][CdMo12ⅤO30(HPO4)6(H2PO4)2].5H2O.通过元素分析I、CP、TG和X射线单晶衍射确定了其组成,使用IR和EPR进行了结构表征.通过N2吸附脱附测定了比表面积和孔径,为催化研究提供了基础数据.结果表明:该晶体为三斜晶系,P-1空间群;晶胞参数a=1.200 2(2)nm,b=1.465 1(3)nm,c=2.119 2(4)nm,V=3.564 2(12)nm3,β=83.01(3)°,Z=2,F(000)=293 2,R1=0.030 0,wR2=0.071 6.     

[Gd(Gly)_3(H_2O)_2]Cl_3·H_2O的合成与晶体结构

标题配合物在水溶液中合成 ,缓慢挥发水溶液 ( p H=4～ 5)得到其针状单晶 .研究了配合物的热分析与红外光谱 ,测定了配合物的晶体结构 .结果表明 ,晶体属正交晶系 ,空间群 P2 12 12 1,晶胞参数为 :a=1 .1 960 ( 2 ) nm,b=3 .0 789( 6) nm,c=0 .4 7652 ( 1 0 ) nm.V=1 .7547( 1 6) nm3 ,Z=4 ,Dc=1 .987g/cm3 .晶体是一维链状配合物 .相邻 Gd3 离子通过 2个简单羧基桥和 1个μ2 羧基桥联结起来 ,还有 2个水分子配位于每个 Gd3 离子 ,所以 Gd3 的配位数为 9,形成变形的单帽四方反棱柱体 .该配位多面体是摩尔比为 1∶ 3的稀土甘氨酸配合物中报道的第 1个例子 .得到了该配合物的配位键的键焓     

[Cu(TOL)_4]Cl_2·2C_2H_5OH·2H_2O的合成和晶体结构

三唑醇(Triadimenol,简写TOL)是一内吸性的广谱低毒杀菌剂,主要用于禾谷类作物,腥黑穗病、丝黑穗病、散黑穗病、白粉病、锈病等病害的防治犤1～3犦。其化学名称为1-(4-氯苯氧基)-3,3-二甲基-1-(1H-1,2,4三唑-1基)丁基-2-醇,结构式如下:以农药为配体的金属配合物近年来逐渐被人重视犤4,5犦,它不仅保持了某些金属离子的杀菌特性,扩大了杀菌谱,而且作为一种缓释技术,使农药具有提高持效、延长半衰期、降低对哺乳动物的毒性以及使农药从非内吸性转化为内吸性等优越性。铜化合物作为杀菌剂使用已有60多年的历史,至今仍无抗性,由于其广谱、低毒,…