Interactions of thiamine monophosphate (TMP) with one- and two-dimensional polymeric halogenomercurate anions. Crystal structures of (TMP)(Hg2Br5)center dot 0.5H(2)O and (TMP)(2)(Hg3I8)

An investigation into the interactions between thiamine monophosphate (TMP) and anions has resulted in the preparation and X-ray characterization of the compounds (TMP)(Hg2Br5).0.5H(2)O (1) and (TMP)(2)(Hg3I8) (2). In each compound the TMP molecule exists as a monovalent cation in the usual F conformation. The halogenomercurate anions occur in two-dimensional (2-D) network in 1 or one-dimensional (1-D) chain in 2. In both 1 and 2, the structures consist of alternating cationic sheets of the hydrogen-bonded TMP molecules and anionic sheets of the polymeric halogenomercurate anions. The TMP molecule binds to the polymeric anions through the characteristic 'anion bridge I', C(2)-H..X...pyrimidinium (X = Br in 1 and 1 in 2), and electrostatic interactions between electropositive S(1) and halogen atoms. The 'anion bridge II' of the type N(4'1)-H...X...thiazolium (X = phosphate group) plays a role in stabilizing the molecular conformation. The biological implication of the host-guest-like complexation between TMP and polymeric anions is discussed.

Hydrothermal synthesis and X-ray single crystal structure of bimetallic cluster complex [{Co(phen)(2)}(2)V4O12]center dot H2O

A new bimetallic cluster complex with the formula [{Co(phen)(2)}(2)V4O12](H2O)-H-. was synthesized from the hydrothermal reaction of V2O5, H2C2O4, Co(NO3)(2), 1,10-phenanthroline (phen), (C4H9)(4)NOH and water. The compound crystallizes in an orthorhombic system with space group Pbcn and unit cell parameters a = 19.106(3) Angstrom, b = 15.250(3) Angstrom, c = 16.321(2) Angstrom, V = 4755.4(13) Angstrom(3), Z = 4 and R = 0.0318. The bimetallic cluster complex [{Co(phen)(2)}(2)V4O12](H2O)-H-. is composed of a discrete V4O124- cluster eovalently attached to two [Co(phen)(2)](2+) fragments and the discrete hexanuclear bimetallic clusters of [{Co(phen)(2)}(V4O12)-V-2](H2O)-H-. are further extended into interesting three-dimensional supermolecular arrays via pi-pi stacking interactions of phen groups. Other characterizations by elemental analysis, IR, and thermal analysis are also described.

SeGPX activity of three organoselenium-containing cyclodextrins and their scavenging effects on HO center dot

Three organoselenium-containing derivatives of beta-cyclodextrins (beta-CD), mono-6-benzylseleno-6-deoxy-beta-cyclodextrin (compound 1), 6,6'-trimethylenediseleno bridged beta-cyclodextrin dimer(compound 2) and 6,6'- (o-phenylene)diseleno bridged beta-cyclodextrin dimer (compound 3) functioned as mimics of selenium-containing glutathione peroxidase(SeGPX). Acting on H2O2 and GSH, the SeGPX activities of these compounds were 0.83-, 0.26-, and 1. 23-fold of that of Ebselen (0.99 U/mu mol), respectively. The relationship between the structure and the function of these compounds was studied. The results suggested that the hydrophobicity and rigidity of phenyl group is the main reason that accounted for the higher activity of compounds 3 and 1. Phenyl group not only provided the hydrophobic circumstance which is necessary for the catalytic function of selenium, but also make it possible that the cyclodextrin unit of compounds 1 and 3 combines the substrate with a more effective direction. Fluorometric techniques were utilized to determine the yields of the hydroxyl radical produced by Fenton reactions through the formation of hydroxy benzoic acids from benzoate. Compared with Ebselen which showed a significant inhibition effect on the formation of HO., these organoselenium-containing cyclodextrins showed a little scavenging effect on the formation of HO. throughout the whole process.

Synthesis, structure and properties of alpha-Keggin-type of K6H3[ZnW11O40Al]center dot 9.5H(2)O

A new heteropolycomplex, K6H3[ZnW11O40Al] . 9.5H(2)O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, Al-27 NMR, electrochemistry and X-ray crystallography. The crystal of K6H3[ZnW11O40Al] . 9.5H(2)O is cubic, space group Fm-3m, with lattice constants a=b=c=2. 144 8(2) nm, V = 9.866(2) nm(3), Mo radiation, R = 0.057 8 for 497 independent data with [I>2 delta(I)]. The anion is of alpha-type Keggin structure with C-s symmetry.

Synthesis and crystal structure of (eta(8)-C8H8)Gd(eta(5)-C6H5CH2C5H4)center dot DME

LnCl(3) reacted with C6H5CH2C5H4Na in THF (tetrahydrofuran) in the ratio 1.1 at room temperature for 1 h giving C(6)H(5)CH(2)C(6)H(4)LnCl(2) . nTHF, which reacted with C8H8K2/THF and the crystals obtained were recrystallized in DME to yield the title complex. The crystal structure of (C8H8) Ln (C6H5CH2C5H4). DME was determined revealing that the Gd complex has one conformation. One benzylcyclopentadienyl (eta(5)), one cyclooctatetraenyl (eta(8)) and the two oxygen atoms of DME (dimethoxyethane) are coordinated to Gd with the effective coordination number of 10.

Preparation and crystal structures of LaCl3(15-crown-5) and [LaCl2(phen)(H2O)(2)(mu-Cl)](2)center dot(15-crown-5)center dot MeCN

LaCl3(15-crown-5), I was prepared by the reaction of LaCl(3)nH(2)O with 15-crown-5 and bipy (2,2'-bipyridyl). [LaCl2(phen)(H2O)(2)(mu-Cl)](2) .(15-crown-5). MeCN, II, was crystallized from a mixture of LaC1(3) . nH(2)O, phen (1,10-phenanthroline) and 15-crown-5 in MeOH/MeCN, Crystal structures of these two complexes have been determined by X-ray methods. The La(III) ion in I is coordinated by three Cl anions and five oxygen atoms of a crown ether. The two metal ions in II are bridged by two Cl anions and the crown ligand is hydrogen-bonded to the coordinated water molecules to form polymeric... crown/cation/cation/crown... chains.

A BINUCLEAR NICKEL(II) COMPLEX CONTAINING AN OXAMIDO-BRIDGE - SYNTHESIS, PROPERTIES AND X-RAY CRYSTAL-STRUCTURE OF [NI(OXAE)NI(PHEN)(2)](CLO4)(2)CENTER-DOT-3H2O

The binuclear complex [Ni(oxae)Ni(phen)2](ClO4)(2) . H2O (oxae=N,N'bis(2-aminoethyl) oxamido dianion, phen = 1, 10-phenanthroline) was prepared from the planar monomeric complex Ni(oxae) and characterized through analytical and spectroscopic measurements. The structure of [Ni(oxae)Ni(phen)(2)] (ClO4)2 . 3H(2)O was investigated by single-crystal X-ray analysis. The complex has an extended oxamido-bridged structure and consists of two nickel(II) ions, one of them in a square planar environment and another in a distorted octahedral environment. The Ni-Ni distance is 5.267 Angstrom.

SYNTHESIS AND STRUCTURE CHARACTERIZATION OF LANTHANUM [2,2,2]CRYPTATES, [LACL[2,2,2](H2O)]CL-2-CENTER-DOT-H2O AND [LA(CF3SO3)[2,2,2]1(DMF)](CF3SO3)(2)

Two lanthanum(III) [2,2,2]cryptates, [LaCl[2,2,2](H2O)]Cl-2.H2O (1) and [La(CF3SO3)[2,2,2](DMF)] (CF3SO3)(2) (2) have been prepared by the reaction of LaCl3 and La(CF3SO3)(3) with [2,2,2]cryptand, respectively and their crystal structures have been determ

Crystal structure of (5R,10R)-2,7-dibromo-3,8-dihydroxy-5,10-dimethoxy-5,10-dihydrochromeno[5,4,3-cde]chromene sesquihydrate, C16H12Br2O6 center dot 1.5H(2)O

C16H15Br2O7.5, orthorhombic, P2(1)2(1)2 (no. 18), a = 18.483(2) angstrom, b = 9.413(1) angstrom, c = 10.072(1) angstrom, V = 1752.3 angstrom(3), Z = 4, R-gt(F) = 0.083, wR(ref)(F-2) = 0.202, T= 293 K.

Morphological Evolution During Synthesis of New AlPO4 Center dot H2O Crystal

A new crystal of aluminophosphate, AIPO(4)(.)H(2)O, is synthesized from two-batch aqueous solution under hydrothermal conditions. Three types of the crystal habits, i.e. the tetragonal double pyramid, the tetragonal prism and the plate-type tetragonal prism, are found from batch-A solution. Two types of the crystal habits, i.e. the hexagonal pyramid and the strip-type tetragonal prism, are found from batch-B solution. The change of crystal morphology is originated from the fluctuation of the synthesis conditions, such as the supersaturation, the temperature and the impurity content. It causes change of the step energies, the defect density and the step roughness, and further, change of the growth rates. Since the crystal morphology is sensitive to the mass transport mechanism, the crystal habits could be changed under the microgravity.

Two novel molybdenum complexes containing [Mo2O2S2](2+) fragment: synthesis, crystal structures and catalytic studies

Mo2O2S2(HGly)(GlY)(2) 1 and K-6[Mo2O2S2(nta)(2)][Mo2O2S2(ntaH)(2)]center dot 4H(2)O 2 were synthesized by the reactions of (NH4)(2)MoS4 and amino acids L (L = glycine, nitrilotriacetic acid) in ethanol-water medium at ambient temperature. The two complexes were characterized by elemental analysis, infrared spectra, UV-visible spectra, TG-DTA and XPS.

Synthesis and structure of new low dimensional polymeric haloplumbate(II) complexes [Pb4Br12(C40H40N8)] and [Pb4Cl12(C40H40N8)]center dot H2O

New low dimensional polymeric haloplumbate(II) complexes of the dication of (4,4'-bis(imidazolyl-ylmethyl)biphenyl) were synthesised and their crystal structures determined. Complex 1, [Pb4Br12(C40H40N8)], has cis-edge-shared, octahedral, lead bromide double chains. In compound 2 [Pb4Cl12(C40H40N8)]center dot H2O, the inorganic chains are corner-shared, square pyramidal chains of lead chloride. In both compounds the organic ammoniums form regular layers that alternate with the inorganic chains.

Studies of the intermolecular DNA triplexes of C+center dot GC and T center dot AT triplets by electrospray ionization Fourier-transform ion cyclotron resonance mass spectrometry

Formation and stabilities of four 14-mer intermolecular DNA triplexes, consisting of third strands with repeating sequence CTCT, CCTT, CTT, or TTT, were studied by electrospray ionization Fourier-transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS) in the gas phase. The gas-phase stabilities of the triplexes were compared with their CD spectra and melting behaviors in solution, and parallel correlation between two phases were obtained. In the presence of 20 mm NH4+ (pH 5.5), the formation of the TTT triplex was not detected in both solution and the gas phase.

Hydrothermal Synthesis, Structures, and Luminescent Properties of Seven d(10) Metal-Organic Frameworks Based on 9,9-Dipropylfluorene-2,7-Dicarboxylic Acid (H(2)DFDA)

A series of Zn(II) and Cd(II) metal-organic frameworks, namely, [Zn(DFDA)] (1), [Cd(DFDA)(C2H5OH)] (2), [Zn-2(DFDA)(2)(L-1)(2)](2) center dot 3H(2)O (3), [Cd-2(DFDA)(2)(L-1)(2)] (4), [Zn(DFDA)(L-2)] (5), [Cd(DFDA)(L-2)(DMF)] (6), and [Zn(DFDA)(L-3)] (7) (where DFDA = 9,9-dipropylfluorene-2,7-dicarboxylate anion, L-1 = 1,4-bis(imidazol-1-ylmethyl)benzene, L-2 = 1,1'-(1,4-butanediyl) bis(imidazole), L-3 = 2,2'-bipyridine) have been synthesized under hydrothermal conditions and structurally characterized. Compound 1 exhibits a three-dimensional (3D framework containing one-dimensional (1D) Zn(II)-O clusters, with (4(8).6(7)) topology. Compound 2 contains hydrophobic channels built from infinite 1D Cd(II)-O clusters, with (4(8).5(4).6(3)) topology.

Assembly of Seven Supramolecular Compounds with p-Sulfonatocalix[6]arene

Seven supramolecular compounds comprising p-sulfonatocalix[6]arene and transition metals, {[Cu(Imz)-(phen)(H2O)](4)[C6AS]}center dot 10H(2)O (1), {[Cu(Imz)(2)(phen)](2)[Cu(Imz)(phen)(H2O)(2)](2)[C6AS]}center dot 13.3H(2)O (2), {[M(phen)(2)(H2O)]-[(M(phen)(2)](2)[C6AS]}center dot nH(2)O (3 and 4) (3: M = Co and n = 29.6; 4: M = Zn and n = 29.9), {[Cu(phen)(2)](4)[C6AS]}(2)center dot 13H(2)O (5), [H3O](2)[Co(phen)(3)](2)[C6AS]center dot 10.7H(2)O(6), and [Cu(phen)(2)(H2O)](2){[Cu(phen)(2)](2)[C6AS]}center dot 8H(2)O(7)(phen = 1,10-phenanthroline, C6AS = p-sulfonatocalix[6]arene, Imz = imidazole), have been synthesized by a hydrothermal method and structurally characterized by IR spectroscopy, thermogravimetric-differential thermal analysis (TG-DTA), and single crystal X-ray diffraction.