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.     

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).     

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.     

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.     

Synthesis and crystal structure of mer-nitroaquatriamminenitrosylruthenium(II) nitrate [RuNO(NH3)3(NO2)(H2O)](NO3)2

The reaction between mer-[RuNO(NH₃)₃(NO₂)(OH)]Cl·0.5H₂O and an excess of 16 M HNO₃ leads to the protonation of the starting complex and crystallization of the complex with a coordinated water molecule and nitrite anion. The crystal structure of the product has been determined. The coordinated water molecule tends to be a weak acid with a measured pK_a of 2.4.     

配位聚合物[Zn(phen)(H2O)2SO4]n的合成与晶体结构

通过扩散法得到了一个新的配位聚合物[Zn(phen)(H2O)2SO4]n[phen=邻菲啰啉]。通过X-ray单晶衍射对配合物的结构进行了表征。配合物属单斜晶系,Cc空间群,晶胞参数:a=15.1399(10),b=14.1420(10),c=6.6994(5),α=90°,β=103.458(1)°,γ=90°,V=1395.01(17)3,Z=2,μ=0.752 mm-1,R1=0.0214,wR2=0.0602。     

The Interaction of the Antitumor Complexes Na[trans-RuCl(4) (DMSO)(Im)] and Na[trans-RuCl(4)(DMSO)(Ind)] With Apotransferrin: a Spectroscopic Study

The interaction of two antitumor ruthenium(III) complexes,-Na[trans-RuCl(4)(DMSO)(Im)] and Na[trans-RuCl(4)(DMSO)(Ind)]- with human serum apotransferrin (apoTf) was investigated through a number of spectroscopic techniques such as UV-Vis absorption, CD and (1)H NMR spectroscopy. Interestingly, the hydrolysis profiles of these complexes in a physiological buffer are markedly affected by the presence, in solution, of apoTf suggesting the occurrence of a specific interaction of their respective hydrolysis products with the protein. The formation of stable adducts with apotransferrin has been demonstrated by CD spectroscopy, and additional information obtained through (1)H NMR of the hyperfine shifted signals. The bound ruthenium(III) species may be detached from these adducts by addition of excess citrate at low pH. The behavior of the investigated ruthenium(III) complexes with apoTf is compared with that of the recently described and strictly related ru-im and ru-ind antitumour complexes, and discussed in the frame of general strategies of drug targeting.     

(H2en)0.5[BiO(OH)2(H2O)]: The first organic templated layered bismuthate

A novel 2-D organic templated bismuth–oxygen compound (H₂en)_0.5[BiO(OH)₂(H₂O)] (1) (en = ethylenediamine) has been synthesized in the presence of ethylenediamine acting as a template under mild hydrothermal conditions. The structure was determined by single crystal X-ray diffraction and further characterized by IR spectrum, elemental analysis, scanning electron microscopy (SEM), photoluminescence and thermogravimetric analysis. In the compound, the Bi atom was coordinated by eight oxygen atoms. The BiO₈ polyhedra share edges or corners with their neighbors to result in an anionic inorganic layer with protonated ethylenediamine cations occupied between layers. At ambient temperature, 1 shows a blue emission band which may be assigned to the ¹P₁–¹S₀ transitions of the s² electron of the Bi^3 + ion. To our knowledge, 1 is the first example of layered bismuthate templated by an organic amine.     

Interaction of Cis- and Trans-RuCl (2)(DMSO)(4) With Human Serum Albumin

The interaction between cis- and trans- RuCl(2)(DMSO)(4) and human serum albumin have been investigated through UV-Vis, circular dichroism, fluorescence spectroscopy and inductively couplet plasma atomic emission spectroscopy (ICP(AES)) method Albumin can specifically bind 1 mole of cis-isomer and 2 moles of the trans-isomer RuCl(2)(DMSO)(4) complex. The interaction of RuCl(2)(DMSO)(4) with HSA causes: a conformational change with the loss of helical stability of protein; the strong quenching of the Trp 214 fluorescence indicating that the conformational change of the hydrophobic binding pocked in subdomain IIA takes place; a local perturbation of the warfarin binding site and induce some conformational changes at neighbour domains, a changing of the binding abilities towards heme.     

三维网状化合物[(H2DABCO)CaCl4(H2O)2]的合成、结构及性能

将1,4-二氮杂二环[2,2,2]辛烷(DABCO)、氯化钙、盐酸以一定比例溶入甲醇溶液,通过自然蒸发方式获得一种具有三维网状结构的新颖有机-无机杂化化合物[(H2 DABCO)CaCl4(H2 O)2],以红外光谱(IR)、元素分析、单晶X衍射、X-射线粉末衍射、热重分析(TG)、变温-变频介电等测试,确定化合物的结...     

A novel coordination polymer with double chains structure: hydrothermal syntheses,structures and magnetic properties of [Cu(phen)(H2O)2SO4]n (phen=1,10-phenanthroline)

A coordination polymer [Cu(phen)(H₂O)₂(SO₄)]_n (1) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, thermogravimetric analysis, and single crystal X-ray diffraction. This compound displays a novel double chains structure, in which each one-dimensional chain is constituted by the distorted octahedral complex of copper(II) bridged through bidentate sulfate ligands. Magnetic susceptibility measurement of 1 has been performed down to 2 K. Although paramagnetic behavior is dominantly manifested, compound 1 shows a weak antiferromagnetic interaction on cooling from room temperature to 2 K.     

二维层状磷酸铝化合物[Al(HPO4)(H2PO4)(C10H8N2)]的合成与表征

利用溶剂热法成功地合成出一个二维层状磷酸铝化合物[Al(HPO4)(H2PO4)(C10H8N2)].通过X-ray粉末衍射、单晶X射线、ICP、元素分析及热重分析等对该化合物进行了表征.该化合物属于单斜晶系,空间群P21/c(No.14),晶胞参数a = 10.932(2) ?,b = 15.7183(3) ?, c = 8.4177(17) ?,α = 90o,β = 108. 95(3)o ,γ = 90o, V=1368.0(5)?3,Z=4.其骨架由AlO4N2八面体通过共顶点与H2PO4和HPO4四面体连接而形成(4,12)网络层状结构.该网层结构按AA方式堆积,同时相邻层的2,2'-联吡啶分子之间具有Pi-Pi键相互作用.该工作进一步丰富了磷酸铝化合物的结构化学,并且为实现定向设计和合成提供了实验和理论依据.     

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。     

A new inorganic (carbon-free) chelate ring: SnO2N2. Eight-coordinated tin(IV) in Sn(O2N2Ph)4 and a self-assembled 20-membered macrocycle in [Me3Sn(O2N2Ph)]4

The reaction of cupferron (NH₄L, L=PhN(O)NO⁻) with tin(IV) and trimethyltin(IV) halides yields cupferronato complexes SnL₄ (1) and [Me₃SnL]₄ (2) which were characterised by FT-IR and FT-Raman spectroscopy. The first X-ray diffraction analysis of the complexes reveals a slightly distorted dodecahedral and trigonal-bipyramidal coordination of the central metal atoms in 1 and 2, respectively. The N-nitroso-N-phenylhydroxylaminato [PhN(O)NO⁻] ligand behaves as chelating in 1 and bridging in 2 leading to a novel five-membered chelate ring, SnO₂N₂ in 1 and an unprecedented 20-membered inorganic metallomacrocycle, Sn₄O₈N₈ in 2.     

Single crystal structure of a heterometallic one-dimensional polymer: [{Cu(1,10-phen)}2(V2O4)(O3PCH2CH2CH2CH2PO3H)2(H2O)]n

A heterometallic one-dimensional polymer [{Cu(1,10-phen)}₂(V₂O₄)(O₃PCH₂CH₂CH₂CH₂PO₃H)₂(H₂O)]_n 1 (1,10-phen=1,10-phenanthroline) has been synthesized under hydrothermal conditions. The structure of 1 shows a stepped chain with two parallel 1,4-butylenediphosphonate ligands as linking units.     

Synthesis and crystal structure of two novel polymeric PbII compounds: [Pb(phen)(N3)2]n and [Pb(deta)(N3) · (N3)]n

Two novel 1D polymeric Pb(II) complex containing the Pb₂-(μ-N₃)₂ units, [Pb(phen)(N₃)₂]_n (1) and [Pb(deta)(N₃) · (N₃)]_n (2) (deta and phen are the abbreviations of diethylentriamine and 1,10-phenanthroline, respectively) have been synthesized and characterized by single-crystal X-ray diffraction. Compounds of (1) and (2) are six, PbN₆, and five, PbN₅, coordinated polymers, respectively. Both of them hold hemidirected coordination geometries. To the best of our knowledge, these 1D coordination polymers are the novel Pb₂-(μ-N₃)₂ units of lead(II) compounds and interact with each other via π–π stacking and weak Pb⋯N interactions to create 3D and 2D frameworks.     

Two types of tetrasubstitution in [H4Ru4(CO)12]: spectroscopic characterization and crystal structure determination of [H4Ru4(CO)8(PMe2Ph)4] and [H2Ru4(CO)9(PMe2Ph)4]

Two tetrasubstituted tetranuclear ruthenium clusters containing dimethylphenylphosphine [H₄Ru₄(CO)₈(PMe₂Ph)₄] and [H₂Ru₄(CO)₉(PMe₂Ph)₄] were prepared and characterized spectroscopically as well as by X-ray crystallography. Both compounds show a structure based on the usual 60-electron tetrahedral framework with each ruthenium atom being bonded to one phosphine ligand. In the case of the nonacarbonyl derivative, one of the ruthenium atoms has one terminal carbonyl group and is also bonded to two semibridging carbonyl groups; two other metal–metal bonds are bridged by the hydride groups. In the case of the octacarbonyl compound all the ruthenium atoms are bonded to two terminal carbonyls and to two bridging hydrides. NMR spectroscopical information of [H₄Ru₄(CO)₈(PMe₂Ph)₄] suggests the presence of two isomers in solution which we propose to have D_2d and C_s symmetries. The observation of the NMR properties gives some observations about conditions that favour coupling between substituents in different ruthenium atoms.