Synthesis and crystal structure of trans-nitrosoaquatetraammineruthenium(II) sulphate hydrosulphate, [Ru(NO)(NH3)4(H2O)](SO4)(HSO4)

The reaction between [RuNO(NH₃)₄OH]Cl₂ and an excess of 2 M H₂SO₄ leads to the protonation of the starting complex and crystallisation of the title complex with sulphate and hydrosulphate anions. The crystal structure of the product has been determined. The linear nitroso group and water molecule are coordinated in trans positions.     

Hydrothermal synthesis,crystal structure and photoluminescent property of a novel 3-D [La2(C2O4)2(NO3)(OH)(H2O)] · 3H2O

A novel 3D [La₂(C₂O₄)₂(NO₃) (OH)(H₂O)] · 3H₂O 1 has been synthesized under hydrothermal conditions and characterized by elemental analyses, IR, TGA, X-ray powder diffraction, X-ray single crystal diffraction and photoluminescence. The bridging modes of both nitrates and oxalates in compound 1 are uncommon. We have unexpectedly generated an unusual compound by using the simplest ligands, oxalates and nitrates in the presence of nicotinate (HIN).     

Interaction of [Rh(2)(O(2)CCH(3))(4)(H(2)O)(2)] and [Rh(2)(O(2)CCH(OH)Ph)(2)(phen)(2)(H(2)O)(2)](O(2)C-CH(OH)Ph)(2) With Sulfhydryl Compounds and Ceruloplasmin

The interaction of binuclear rhodium(II) complexes [Rh(2)(OOCCH(3))(4)(H(2)O)(2)], [Rh(2){OOCCH(OH)Ph}(2)(phen)(2)(H(2)O)(2)] {OOCCH(OH)Ph}(2), [Rh(2)(OOCCH(3))(2)(bpy)(2)(H(2)O)(2)](OOCCH(3))(2) and [Rh(2)Cl(2)(OOCMe)(2)(bpy)(2)](3H(2)O) with ceruloplasmin, cysteine, glutathione and coenzyme A have been investigated using. UV-Vis and CD spectroscopies. The complexes containing phen or bpy at pH = 7.4 and 4.0 are readily reduced with sulfhydryl compounds, while rhodium(II) acetate is relatively stable in these conditions. Complex [Rh(2){OOCCH(OH)Ph}(2)(phen)(2)(H(2)O)(2)] strongly changes structure of ceruloplasmin leading to the decrease of of alpha-helix content and loss of oxidase activity.     

Synthesis and Anti-Candida Activity of Cobalt(II) Complexes of Benzene-1,2-Dioxyacetic Acid (bdoaH(2)). X-Ray Crystal Structures of [Co(bdoa)(H(2)O)(3)] 3.5H(2)O and {[CO(phen)(3)](bdoa)}(2)24H(2)O (phen = 1,10-Phenanthroline)

Co(CH(3)CO(2))(2)4H(2)O reacts with benzene-1,2-dioxyacetic acid (bdoaH(2)) to give the Co(2+) complexes [Co(bdoa)(H(2)O)(3)]H(2)O (1a) and [Co(bdoa)(H(2)O)(3)] 3.5H(2)O (1b). Subsequent reaction of 1a with 1,10- phenanthroline produces [CO(phen)(3)] bdoa10H(2)O (2a) and {[CO(phen)(3)](bdoa)}(2)24H(2)O (2b). Molecular structures of 1b and 2b were determined crystallographically. In 1b the bdoa(2-)- ligates the metal by two carboxylate oxygens and two ethereal oxygens, whereas in 2b the bdoa(2-) is uncoordinated. The Mn(2+) and Cu(2+) complexes [Mn(bdoa)(phen)(2)]H(2)O (3) and [Cu(pdoa)(imid)(2)] (4) were also synthesised, 1a-4 and other metal complexes of bdoa H(2) (metal = Mn(2+), Co(2+) ,Cu(2+), Cu(+) ) were screened for their ability to inhibit the growth ofhe yeast Candida albicans. Complexes incorporating the 1,10-phenanthroline ligand were the most active.     

Synthesis,crystal structure and water-induced reversible crystal-to-amorphous transformation property of [Co2(2,4-pydc)2(bpa)(H2O)6](H2O)2

The dinuclear Co^II coordination compound with empirical formula [Co₂(2,4-pydc)₂(bpa)(H₂O)₆](H₂O)₂ (1); bpa = 1,2-bis(2,4-pyridyl)ethane, 2,4-pydc = 2,4-pyridinedicarboxylate anion, has been synthesized and õcharacterized by elemental analysis, single crystal X-ray diffraction, IR and UV–vis spectra, TGA and XRPD. Compound 1 is a symmetry-related dinuclear compound consisting of two six coordinated cobalt atoms, one bpa ligand, two 2,4-pydc ligands and two lattice water molecules. Each Co^II ion is coordinated by one oxygen atom and one nitrogen atom from 2,4-pydc bidentate chelate ligand, one nitrogen atom of bpa bidentate bridging ligand and three water molecules, giving a distorted octahedral geometry with CoN₂O₄ chromophore. The crystal packing of this compound reveals a novel 3D supramolecular network, formed by hydrogen-bonding and C–H⋯π interactions. Investigations of the dynamic structural transformation behavior demonstrate that the title compound exhibits a solvent-induced reversible crystal-to-amorphous transformation with chromotropism when exposed to water vapor. This indicates that the dehydrated amorphous form, Co₂(2,4-pydc)₂(bpa)(H₂O)₂ (1A), may be utilized as an indicator for humidity.     

[Nd(6-OHnicH)3(H2O)6]n配合物的合成和晶体结构研究

在水热反应条件下,采用6-羟基吡啶-3-甲酸(6-OHnicH)与稀土金属离子钕合成了标题化合物。运用元素分析、红外光谱、X-射线衍射等进行了表征。X-射线衍射结果表明:该配合物属于三斜晶系,空间群是P-1,晶胞参数为:a=7.1693(8),b=10.3227(12),c=16.7831(19),α=73.3000(10)°,β=88.0070(10)°,γ=88.2180(10)°,Z=2。该配合物最终通过分子间氢键作用堆积为三维网状结构。     

Synthesis and Biological Activity of Manganese (II) Complexes of Phthalic and Isophthalic Acid: X-Ray Crystal Structures of [Mn(ph)(Phen)(2)(H(2)O)]. 4H(2)O, [Mn(Phen)(2)(H(2)O)(2)](2)(Isoph)(2)(Phen). 12H(2)O and {[Mn(Isoph)(bipy)](4). 2.75biby}(n)(phH(2) = Phthalic Acid; isoph = Isophthalic Acid; phen = 1,10-Phenanthroline; bipy = 2,2-Bipyridine)

Manganese(II) acetate reacts with phthalic acid (phH(2)) to give [Mn(ph)].0.5H(2)O (1). Reaction of 1 with 1,10-phenanthroline produces [Mn(ph)(phen)].2H(2)O (2) and [Mn(ph)(phen)(2)(H(2)O)].4H(2)O (3). Reaction of isophthalic acid (isophH(2)) with manganese(II) acetate results in the formation of [Mn(isoph)].2H(2)O (4). The addition of the N,N-donor ligands 1,10-phenanthroline or 2,2'-bipyridine to 4 leads to the formation of [Mn(2) (isoph)(2)(phen)(3))].4H(2)O (5), [(Mn(phen)(2)(H(2)O)(2)](2)(isoph)(2)(phen).12H(2)O (6) and {[Mn(isoph)(bipy)](4).2.75 biby}(n) (7), respectively. Molecular structures of 3, 6 and 7 were determined crystallographically. In 3 the phthalate ligand is bound to the manganese via just one of its carboxylate groups in a monodentate mode with the remaining coordination sites filled by four phenanthroline nitrogen and one water oxygen atoms. In 6 the isophthalates are uncoordinated with the octahedral manganese center ligated by two phenanthrolines and two waters. In 7 the Isophthalate ligands act as bridges resulting in a polymeric structure. One of the carboxylate groups is chelating a single manganese with the other binding two metal centres in a bridging bidentate mode. The phthalate and isophthalate complexes, the metal free ligands and a number of simple manganes salts were each tested for their ability, to inhibit the growth of Candida albicans. Only the "metal free" 1,10-phenanthroline and its manganese complexes were found to be active.     

A new binuclear Cr(III) citrate anion: Synthesis,characterization and crystal structure of [Cr(CO(NH2)2)6]2[Cr2(CO(NH2)2)2(C6H4O7)2]3

The new anion [Cr₂(CO(NH₂)₂)₂(C₆H₄O₇)₂]^2 − has been isolated in the complex [Cr(CO(NH₂)₂)₆]₂[Cr₂(CO(NH₂)₂)₂(C₆H₄O₇)₂]₃. The crystals of this complex were obtained by a one-pot synthetic method using 1:1 molar ratio of hexaureachromium(III) chloride and trisodium citrate in aqueous medium. It was characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffraction analysis. The compound crystallizes in space group R‾3 of the trigonal system with three formula units in a cell of dimensions a = b = 24.7461(4) Å, c = 13.7204(3) Å and γ = 120°. The crystal structure comprises the columns consisting of [Cr(CO(NH₂)₂)₆]^3 + cations surrounded by a cylinder of complex anions, [Cr₂(CO(NH₂)₂)₂(C₆H₄O₇)₂]^2 − which are packed in a honeycomb-like manner. This supramolecular architecture is formed and stabilized by inter- and intramolecular NH⋯O hydrogen bonds.     

[Fe(C7H5O3)(C9H6NO)2]三元配合物的合成及抑菌性能

以水杨酸、8-羟基喹啉为配体与铁(Ⅲ)合成了三元配合物,用元素分析、红外光谱、紫外可见光谱、荧光光谱对其进行表征,确定其化学组成为[Fe(C7H5O3)(C9H6NO)2]。其中,水杨酸脱质子以羧酸根与Fe3+成键,酚羟基不参与配位,而8-羟基喹啉脱质子以酚羟基氧和杂环上的氮原子双齿配位,形成五元螯环。配合物在整个可见光区都有较强吸收,粉末及其浓溶液均呈黑色,稀溶液呈紫色。以300 nm为激发波长时,三元配合物在409 nm处有较强的发射荧光。采用分光光度法研究其对大肠杆菌生长的作用,配合物浓度低于2 mmol/L时,促进大肠杆菌的生长,高于2 mmol/L时抑制其生长,浓度越大抑制作用越强,即配合物对大肠杆菌的生长具有双向生物效应。     

[Pb(DNI)_2(H_2O)_4]的制备和晶体结构

通过2,4-二硝基咪唑(2,4-DNI)的钠盐水溶液与硝酸铅的水溶液反应,制备出了2,4-二硝基咪唑铅配合物;采用自然挥发法培养出了适于X光结构测定的单晶,X射线衍射测定结果为,晶体属单斜晶系,空间群为Cc,晶体学参数为:a=6.517(3)×10-1nm,b=17.131(6)×10-1nm,c=14.082(7)×10-1nm,α=90.00(3)°,β=97.80(4)°,γ=90.00(4)°,V=1 557.5(12)×10-3nm3,Z=4,Dc=2.531 g/cm3,μ=11.001 mm-1,F(000)=1 120,最后偏离因子R为0.022 6。根据红外光谱、元素分析和X射线衍射分析结果,确定了2,4-二硝基咪唑铅配合物的化学组成为C6H10O12N8Pb,分子结构式为[Pb(DNI)2(H2O)4]。     

[Fe(C7H5O3)(C9H6NO)2]三元配合物的合成及抑菌性能

本文以水杨酸、8-羟基喹啉为配体与铁(Ⅲ)合成了三元配合物,用元素分析、红外光谱、紫外可见光谱、荧光光谱等手段对其进行表征,确定其化学组成为[Fe(C7H5O3)(C9H6NO)2]。其中水杨酸脱质子以羧酸根与Fe3+成键,酚羟基不参与配位,而8-羟基喹啉脱质子以酚羟基氧和杂环上的氮原子双齿配位,形成五元螯环。配合物在整个可见光区都有较强吸收,粉末及其浓溶液均呈黑色,稀溶液显紫色。以300 nm为激发波长时,三元配合物在409 nm处有较强的发射荧光。采用分光光度法研究其对大肠杆菌生长的作用,配合物摩尔浓度低于2 mmol/L时,促进大肠杆菌的生长,高于2 mmol/L时抑制其生长,浓度越大抑制作用越强,即配合物对大肠杆菌的生长具有双向生物效应。     

有机锡化合物{n-Bu2Sn[2,6-(O2C)2C5H3N](H2O)}2的合成和晶体结构

利用二丁基氧化锡与2,6-吡啶二甲酸反应合成了目标化合物{n-Bu2Sn[2,6-(O2C)2C5H3N](H2O)}2。用元素分析、红外光谱、核磁共振氢谱以及X-射线单晶衍射进行了表征和结构测定。X-射线单晶衍射测定表明,该化合物为四方晶系,空间群P4(2)/n,a=1.7721(5)nm,b=1.7721(5)nm,c=1.1164(4)nm,α=β=γ=90,°Z=4,V=3.5060nm3,F(000)=1680,R1=0.0344,wR2=0.0853。化合物中两个锡原子呈七配位畸变五角双锥构型。     

[Ni（IMI）6]（NO3）2的制备与晶体结构

咪唑(IMI)与硝酸镍反应,得到硝酸六咪唑合镍配合物,并培养出单晶。元素分析、红外光谱、X射线单晶衍射等分析表明,该晶体属于单斜晶系,空间群为P21/n,晶胞参数a=1.235 0(3)nm,b=1.235 0(3)nm,c=1.480 0(3)nm,β=90.579(2)°,V=1.955 0(7)nm3,Dc=1.491 g/cm3,Z=4,F(000)=900,R1=0.034 4,wR2=0.095 5。该化合物的分子式为[Ni(IMI)6](NO3)2,是由6个咪唑分子直接与二价镍离子配位,硝酸根离子结合形成的配合物。     

Hydrothermal synthesis and crystal structure of a new copper(II) molybdenum(VI) arsenate(III), (C5H5NH)2(H3O)2[(CuO6)Mo6O18(As3O3)2]

A new copper(II) molybdenum(VI) arsenate(III), (C₅H₅NH)₂(H₃O)₂[(CuO₆)Mo₆O₁₈(As₃O₃)₂], has been hydrothermally synthesized and characterized by single crystal X-ray diffraction and TG analysis. The compound crystallizes in the monoclinic space group P2₁/n with a=9.303(2), b=20.731(4), c=12.617(3) Å, β=104.17(3)°, V=2359.3(8) ų, Z=2 and R1(wR2)=0.0296(0.0683). The structure is composed of pyridinium cations, proton hydrates and [(CuO₆)Mo₆O₁₈(As₃O₃)₂]⁴⁻ polyanions. The polyanion framework derives from the Anderson type; the central octahedron is filled up by copper(II) and is capped on both sides by a cyclic As₃O₆ group.     

First X-ray crystal structure of cation [cis-Co(en)2(H2O)Cl]2+: Synthesis,spectroscopic and X-ray structural study of [cis-Co(en)2(H2O)Cl](C6H5SO3)2·H2O

A new cobalt(III) complex salt, [cis-Co(en)₂(H₂O)Cl](C₆H₅SO₃)₂ · H₂O] (I) has been synthesized and characterized by single crystal X-ray structure determination and NMR spectroscopy. This is a first report of the cobalt(III) cation in cis-configuration. The crystal lattice of the complex salt is stabilized by electrostatic forces of attraction and hydrogen bonding interactions.     

稀土配合物[Ln(C3H7NO2)-x-(C3H4N2)(H2O)](ClO4)3(Ln=La,-x-=3;Ln=Pr,Nd,Sm,-x-=2)的合成、表征与热分析

合成了稀土高氯酸盐与咪唑、DL α 丙氨酸的4种配合物晶体。经傅里叶变换红外光谱(FTIR)、元素分析和化学分析测定后确定其组成为[Ln(C3H7NO2)x(C3H4N2)(H2O)](ClO4)3(Ln=La,x=3;Ln=Pr,Nd,Sm,x=2)。用差示扫描量热法(DSC)测定了4种配合物的热分解数据,4个配合物开始熔化分解的温度分别为502 5K,532 4K,495 7K,516 7K,配合物有较高的热稳定性。     

Synthesis,characterizations, and crystal structure of a novel layered phosphonate: Zn2Cl[O3PCH2N(CH2CH2)2O][O3PCH2NH(CH2CH2)2O]

A novel layered zinc phosphonate, Zn₂Cl[O₃PCH₂N(CH₂CH₂)₂O][O₃PCH₂NH(CH₂CH₂)₂O] 1 has been synthesized by hydrothermal reaction at 180 °C and structurally characterized by single crystal X-ray diffraction as well as with infrared spectroscopy, elemental analysis and thermogravimetric analysis. The interconnection of Zn(1)O₄, Zn(2)O₂NCl and CPO₃ tetrahedra via corner-sharing forms a double layer structure with a channel system along b-axis direction. The result of connections in this manner is the formation of 8- and 16-atom windows that are parallel to one another and run in the a-axis direction. The morpholinyl groups of the ligands are orientated toward the interlayer space.     

三维超分子化合物[Zn(C6H4O2N)2·(H2O)4]n的水热合成及晶体结构

用2-羧基吡啶和六水合氯化锌反应制备了一种新的三维氢键超分子配合物,经X-射线衍射分析确定了单晶结构。该晶体属单斜晶系,P2(1)/n空间群,晶胞参数为:a=9.836(2),b=5.2256(10),c=14.611(3),Mr=381.64,β=90.01(3)°,V=751.0(3)3,Z=2,Dc=1.688Mg.m-3,F(000)=392,μ=1.680mm-1,R=0.0258,wR=0.0612。共收集2159个衍射数据,其中1273个为独立衍射点(Rint=0.0332),可观测点数1139个(I>2σ(I))。结果表明,在组成该超分子体系的基本结构单元[Zn(C6H4O2N)2.(H2O)4]中,Zn(Ⅱ)离子形成六配位的畸变的八面体构型,配合物单元之间通过氢键OH…O相互连接,形成了无限延伸的具有网状结构的三维超分子体系。     

Synthesis,characterizations, and crystal structure of a novel 2D metal phosphonate: Na2[Cd2(H2O)3(O3PCH(OH)CO2)2] · 2H2O

A novel cadmium phosphonate compound Na₂[Cd₂(H₂O)₃(O₃PCH(OH)CO₂)₂] · 2H₂O (1) has been synthesized by hydrothermal reaction at 120 °C and characterized by single-crystal X-ray diffraction as well as with infrared spectroscopy, elemental analysis and thermogravimetric analysis. The structure of compound 1 comprises CdO₆ octahedra and CdO₇ pentagonal bipyramid connected by [O₃PCH(OH)CO₂]³⁻ to form a 2D layered structure with a one-dimensional channel system and the charge-compensating Na⁺ cations being located between two adjacent layers.     

三维超分子化合物[Zn(C6H4O2N)2·(H2O)4]n的水热合成及晶体结构

用2-羧基吡啶和六水合氯化锌反应制备了一种新的三维氢键超分子配合物,经X-射线衍射分析确定了单晶结构.该晶体属单斜晶系,P2(1)/n空间群,晶胞参数为a=9.836(2)(A),b=5.2256(10)(A),c=14.611(3)(A),Mr=381.64,β=90.01(3)°,V=751.0(3)(A)3,Z=2,Dc=1.688Mg·m-3,F(000)=392,μ=1.680mm-1,R=0.0258,wR=0.0612.共收集2159个衍射数据,其中1273个为独立衍射点(Rint=0.0332),可观测点数1139个(I＞2σ(I)).结果表明,在组成该超分子体系的基本结构单元[Zn(C6H4O2N)2·(H2O)4]中,Zn(Ⅱ)离子形成六配位的畸变的八面体构型,配合物单元之间通过氢键OH…O相互连接,形成了无限延伸的具有网状结构的三维超分子体系.