Synthesis and crystal structure of 3-methoxycarbonylethyltin tetrachlorides anion

The anion of MeO2CCH2CH2SnCl4 - was obtained by decomposing the yellow solution of MeO2CCH2CH2SnCl3.(2-OHC6H4CH=NC6H5) by standing for 15 days, which is the product of 3-methoxy-carbonylethyltin trichlorides with Schiff base (2-OHC6H4CH=NC6H5). The title compound was characterized by elemental analysis, IR. H-1 NMR,C-13 NMR and X-ray diffraction analysis. The crystal of the title compound belongs to orthorhombic system, space group P2cn, a=7.852(2), b=12.236(1),c=16.952(4)Adegrees, V=1628.7 Angstrom(3), Z=4, D-c=1.79g/cm(3) F(000)=860, mu=22.2cm(-1), R=0.0449, Rw=0.0382. The title compound exists as a discrete molecule, and the tin atom attains a distorted octahedral geometry via the coordination of intramolecular carbonyl oxygen and chloride ion. The coordination number of tin atom is 6.

Single-crystal X-ray structure and properties of K-10[Ni-4(H2O)(2)(AsW9O34)(2)]center dot 4H(2)O

The rational synthesis and the structural and magnetic characterization of a nickel cluster are presented. The compound comprises a rhomblike Ni4O16 group encapsulated between two-heptadentate tungstoarsenate ligands [AsW9O34](9-). The crystal structure of K-10[Ni-4(H2O)(2)(AsW9O34)(2)](.)4H(2)O was solved in monoclinic, P2(1)/n symmetry, with a = 12.258(3) Angstrom, b = 21.232(4) Angstrom, c = 15.837(3) Angstrom, beta = 92.05(3)degrees, V = 4119.1(14) Angstrom(3), Z = 2, and R = 0.0862. The crystal structure of the Ni(II) derivative was compared with that of the Cu(II), Zn(II), Co(II) and Mn(II) derivatives. The Ni4O14(H2O)(2) unit in the compound shows no Jahn-Teller distortion. On the other hand, the Ni(II) derivative shows ferromagnetic exchange interactions within the Ni4O16 group (J = 7.8 cm(-1), J' = 13.7 cm(-1)) and an S = 4 ground state, the highest spin state reported in a heteropoly complex. Its redox electrochemistry has been studied in acid buffer solutions using cyclic voltammetry. It exhibited two steps of one-electron redox waves attributed to redox processes of the tungsten-oxo framework. The new catalyst showed an electrocatalytic effect on the reduction of NO2-.

Crystal structure of a noval poly(aryl ether ketone) containing meta-phenyl linkage

Crystal structure of a novel aryl ether ketone polymer poly(aryl ether ketone ether ketone ketone containing meta-phenyl linkage)(PEKEKmK) was determined by means of WAXD and ED. An orthorhombic unit cell is proposed containing two chains with a=0.772 nm, b=0.604 nm and c=2.572 nm. According to the orthorhombic system, the 10 reflections of this polymer were indexed.

Crystal structure and variation in unit cell parameters with crystallization temperatures of poly (ether ketone ether ketone ketone)s containing meta-phenyl links (PEKEKmK)

The X-ray diffraction patterns of the crystalline aromatic ketone polymer PEKEKmK (aryl ether ketone ether ketone ketone polymer containing meta-phenyl links) have been investigated (for the chemical structure, see Formula). An orthorhombic unit cell is proposed to contain two chains with a = 0.772 nm, b = 0.604 nm and c = 2.572 nm. According to the orthorhombic system, the 11 reflections of this polymer were indexed. Meanwhile, variation in unit cell parameters with crystallization temperatures of PEKEKmK was also investigated. [GRAPHICS]

Synthesis, characterization and crystal structure of a charge transfer salt based on 1.3-cyclopentadiene tetrabutylammoniumdodecamolybdosilicoate

A charge transfer salt, (Bu4N)(4) (C5H6)[(HSiMo11MoO40)-Mo-VI-O-V] has been photochemically synthesized from (Bu4N)(4)SiMo12O40 and 1.3-cyclopentadiene and Characterized, by elemental analysis, IR spectra, solid diffusion reflectance electronic spectra, CV and ESR. The X-ray crystal structure revealed that the title complex crystal data are as follows: triclinic, space group P (1) over bar, a = 14.347(3), b = 14.423(3), c = 27.158(5) Angstrom, alpha = 96.90(3), beta = 104.18(3), gamma = 98.20(3)degrees, V = 5322(2) Angstrom (3), Z = 2, M-r = 2855. 30, D-c = 1.782g.cm(-3), F(000) = 2860, R = 0.0719, wR = 0.198. The title compound is composed of 1.3-cyclopentadiene, four tetrabutylammonium and [(SiMo11MoO40)-Mo-VI-O-V](4-) anion.

Self-assembled monolayer of polyoxometalate on gold surfaces: Quartz crystal microbalance, electrochemistry, and in-situ scanning tunneling microscopy study

A new kind of inorganic self-assembled monolayer (SAM) was prepared by spontaneous adsorption of polyoxometalate anion, AsMo11VO404-, onto a gold surface from acidic aqueous solution. The adsorption process, structure, and electrochemical properties of the AsMo11VO404- SAM were investigated by quartz crystal microbalance (QCM), electrochemistry, and scanning tunneling microscopy (STM). The QCM data suggested that the self-assembling process could be described in terms of the Langmuir adsorption model, providing the value of the free energy of adsorption at -20 KJ mol(-1). The maximum surface coverage of the AsMo11VO404- SAM on gold surface was determined from the QCM data to be 1.7 x 10(-10) mol cm(-2), corresponding to a close-packed monolayer of AsMo11VO404- anion. The analysis of the voltammograms of the AsMo11VO404- SAM on gold electrode showed three pairs of reversible peaks with an equal surface coverage of 1.78 x 10(-10) mol cm(-2) for each of the peaks, and the value was agreed well with the QCM data. In-situ STM image demonstrated that the AsMo11VO404- SAM was very uniform and no aggregates or multilayer could be observed. Furthermore, the high-resolution STM images revealed that the AsMo11VO404- SAM on Au(lll) surface was composed of square unit cells with a lattice space of 10-11 Angstrom at +0.7 V (vs Ag\AgCl). The value was quite close to the diameter of AsMo11VO404- anion obtained from X-ray crystallographic study. The surface coverage of the AsMo11VO404- SAM on gold electrode estimated from the STM image was around 1.8 x 10(-10) mol cm(-2), which was consistent with the QCM and electrochemical results.

X-ray crystal structure and molecular mechanics calculations of (2,6-iso-dipropyl-phenylamide) dimethyl (tetra-methylcyclopenta-dienyl) silane titanium dichloride

Crystal and molecular structure of (2.6-dipropylphenylamide) dimethyl (tetra-methyl cyclopentadienyl) silane titanium dichloride (I) was fully characterized by X-ray diffraction. The crystal is obtained from a mixture of ether/hexane as orthorhombic. with a = 12.658 (3) Angstrom. b = 16.62 (3) Angstrom. c = 11.760 (2) Angstrom. V = 2474.2 (9) Angstrom(3). Z = 4, space group Pnma. R = 0.0399; Componud I compose of the pi-bounded ring with its dimethylsilyl-dipropyl phenyl amido group and the two terminal chloride atoms coordinated to central metal to form a so-called constrained geometry catalyst (CGC) structure. The result of molecular mechanics (MM) calculations on compound I shows that bond lengths and bond angles from the MM calculation are comparable to the data obtained from the X-ray diffraction study. The relation of the structure of CGCs and their catalytic activity by MM calculations is also discussed.

Synthesis and crystal structure of a new supermolecular compound: [C12H24O6][H3PMo12O40]center dot 22H(2)O (C12H24O6=18-crown-6)

The title compound, [C12H24O6][H3PMo12O40]. 22H(2)O, was synthesized by the self-assembly of 18-crown-6 (abbreviated as C12H24O6 or 18C6) and H3PMo12O40 in the mixed solvent of CH3OH and CH3CN, and was characterized by IR, H-1 NMR and Xray diffraction for the first time. Crystal data: Triclinic, P (1) over bar, a = 13.428(3) Angstrom, b = 13.557(3)A, c = 14.642(3) Angstrom, a = 105.39(3)degrees, beta = 90.06(3)degrees, gamma = 119.56(5)degrees, V = 2207.5(8) Angstrom(3), Z = 1, R1 = 0.0719, wR2 = 0.1990. It has a disordered alpha-Keggin PMo12O403- anion, which contains the strong alternating short (mean 1.844 Angstrom) and long (mean 1.958 Angstrom) Mo-O-Mo bonds. In the unit cell, crown ethers and molybdophosphates are alternatively arranged in good order along c-axis. An oxonium ion is located at the center of a crown ether molecule., Oxonium ion interacts with 18C6 by the means of hydrogen bonds (mean 2.7771 Angstrom), which are electrostatic or resonant. The observations show the existence of [H3O(C12H24O6)](+) (C) 2000 Elsevier Science B.V. All rights reserved.

Synthesis and crystal structure of triphenyltin-2-(1,2-ethylenedithio) methylene-3-oxo-5-aryl-4-pentenicate

Nine triphenyltin - 2 - (1,2 - ethylenedithio) methylene - 3 - oxo - 5 - aryl - 4 - pentenicates were synthesized. The crystal structure of the title compound 3b (C33H28O3S2Sn) was determined by X - ray diffraction analysis. The crystal belongs to triclinic system, space group P(1)overbar with a = 0.9074 (2) nm, b = 1.6809(3)nm, c = 2.1834(4)nm, alpha =77.57(3)degrees, beta = 88.04(3)degrees, gamma = 89.47(3)degrees, V = 3.2503nm(3), Z = 2, R = 0.0592. In crystal of 3b, there exist intramolecular 0-Sn coordination bonds, with carboxylate group acting as a bidentate ligand: Sn(1)-0(1) = 0.2086(5) and Sn(1)-0(2) = 0.2594nm, having a deformed trigonal bipyramidal geometry.

Hydrothermal synthesis and crystal structure of [{Cu(2,2 '-bpy)(2)}(2)Mo8O26]: a beta-octamolybdate cluster covalently bonded to two {Cu(2,2 '-bpy)(2)}(2+) coordination complexes via bridging oxo groups

An organic-inorganic hybrid solid, (Cu(2,2'-bpy)(2))(2)Mo8O26, has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Dark green crystals crystallize in the orthorhombic system, space group Pna21, a = 24.164(5), b = 18.281(4), c = 11.877(2) Angstrom, alpha = 90 degrees, beta = 90 degrees, gamma = 90 degrees, V= 5247(2) Angstrom (3), Z = 4, lambda (MoK alpha) = 0.71073 Angstrom (R(F) = 0.0331 for 5353 reflections). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range 1.69 degrees < theta < 25.04 degrees using the omega -scan technique. The structure was solved by the direct method and refined by full-matrix least squares on F-2 using SHELXL-93. The structure of this compound consists of discrete (Cu(2,2'-bpy)(2))(2)Mo8O26 clusters, constructed from beta -octamolybdate subunits ((Mo8O26)(4-)) covalently bonded to two (Cu(2,2'-bpy)(2))(2+) coordination complexes via bridging oxo groups that connect two adjacent molybdenum sites. (C) 2001 Academic Press.

Synthesis and crystal structure of a novel compound: [H3PMo12O40][CO(NH2)(2)](3)center dot-5H(2)O

The title compound, [H3PMo12O40][CO(NH2)(2)](3). 5H(2)O, was synthesized and characterized by IR, C-13 NMR and X-ray diffraction. This is the first example of a urea-heteropoly acid species. Crystal data: monoclinic, C2/c, a = 17.790(4) Angstrom, b = 17.158(3) Angstrom, e = 25.512(5) Angstrom, beta = 100.65(3)degrees, V = 8514(3) Angstrom (3), Z = 6, R-1 = 0.0437, wR2 = 0. 1092. In the unit cell, the urea molecules occupy cavities in the polyoxometalate lattice ordered along b-axis. Water molecules occupy the space left by polyoxometalates, and urea. Polyoxometalate O atoms, the N atoms of urea and O atoms of water molecules are involved in hydrogen bonding. (C) 2001 Elsevier Science B.V. All rights reserved.

Hydrothermal synthesis and crystal structure of a novel layered compound [Ni(C10H8N2)(2)V3O8.5]

A novel layered compound, [Ni(C10H8N2)(2)V3O8.5], was hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 1.551 8(3) nm, b = 1.476 1(3) nm, c = 1.048 3(2) nm, beta = 92.02(3), V = 2.399 8(8) nm(3), Z = 4, R = 0. 046 7, wR(2) = 0. 085 9.

Synthesis and crystal structure of a novel compound constructed from tris-(2, 2 '-bipy)ruthenium(II) and decatungstate

Self-assembly of tris-[2,2 ' -bipyridine]ruthenium(II) chloride with decatunstate produced a novel cation radical salt, [Ru(bpy)(3)](2)[W10O32] . 3DMSO. This is the first product of 2,2 ' -bipyridineruthenium(II)-polyoxometalates species. Crystal data: Monoclinic, P2(1)/c, a = 12.902(3) Angstrom, b = 21.487(3) Angstrom, c = 15.854(5) Angstrom, beta = 93.46(2)degrees, V = 4387(2) Angstrom (3), Z = 2, R-1 = 0.0599, wR2 = 0.1183. X-ray crystallographic study showed that the crystal structure was constructed by electyrostatic attraction and C-H . . .O hydrogen bonds between tris-[2,2 ' -bipyridine]ruthenium(II) and decatungstate polyanion. The tris-[2,2 ' -bipyridine]ruthenium molecules occupy cavities in the polyoxometalate lattice ordered along b-axis. (C) 2001 Elsevier Science B.V. All rights reserved.

Single crystal structure of form I syndiotactic poly(butene-1)

The structures of single crystals of syndiotactic poly(butene-1) in form I, produced by thin-film growth, are studied by transmission electron microscopy and electron diffraction. Bright-field electron microscopy observation shows that the single crystal exhibits a regular rectangular shape with the long axis along its crystallographic b-axis. Electron diffraction results indicate an isochiral C-centered packing of a-fold helical chains in an orthorhombic unit cell corresponding to the C222(1) space group, according to the model proposed in the literature. The differences with the polymorphic behavior of syndiotactic polypropylene concerning the formation and the stability of the isochiral mode of packing are outlined.

Synthesis and crystal structure of [Nd(eta(6)-1,3,5-C6H3Me3)(AlCl4)(3)]( C6H6) and structural comparison of Ln(eta(6)-arene)(AlCl4)(3)

Reaction of NdCl3, with AlCl3 and mesitylene in benzene gives complex [Nd(eta (6)-1,3,5-C6H3Me3) (AlCl4)(3)] (C6H6) (1) which was characterized by elemental analysis, IR spectra, MS and X-lay diffractions. The X-ray determination indicates that 1 has a distorted pentagonal bipyramidal geometry and crystallizes in the monoclinic, space group P2(1)/n with a = 0.9586(2), b = 1.1717(5), c = 2.8966(7) nm, beta = 90.85 (2)degrees, V = 3.2529(6) nm(3), D-c = 1.573 g/cm(3), Z = 4. A comparison of bond parameters for all the reported Ln(eta (6)-Ar) (AlCl4)(3) complexes indicates that the bond distance of Ln-C is shortened with the increasing of methyl group on benzene and with the decreasing of radius of lanthanide ions.