Hydrogen-bonded lamellar network of pyromellitic acid pillared by 8-hydroxyquinoline

8-Hydroxyquinoline (8-q) salt of pyromellitic acid (benzene-1,2,4,5-tetracarboxylic acid, H(4)bta) forms robust lamellar structure where [H(2)bta](2-) anions build up sheets through strong hydrogen bonds in two dimensions and [H-8-q](+) cations act as pillars to afford an extended three dimensional network.

Crystal structure of 11-{[(4 '-heptoxy-4-biphenylyl) carbonyl]oxy}-1-undecyne

The crystal structure of 11-{[(4'-heptoxy-4-biphenylyl) carbonyl] oxy}-1-undecyne (A9EO7), an acetylene with a biphenyl mesogenic moiety, was studied by combination of electron diffraction (ED), wide-angle X-ray diffraction (WAXD), and molecular simulation of ED pattern and molecular packing. A9EO7 was found to adopt an orthorhombic P2(1)2(1)2 space group with cell parameters of a = 5.78 Angstrom, b = 7.46 Angstrom, and c = 63.26 Angstrom, for which molecular packing calculations were conducted to elucidate the molecular conformation. Its crystal morphology was observed using a transmission electron microscope (TEM) and an atom force microscope (AFM). A9EO7 crystal grew to form step like morphology. Crystallization behavior of A9EO7 in magnetic field was examined. Induced by magnetic field A9EO7 could crystallize in such a way that its molecular long axis was parallel to the substrate.

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.

Synthesis, structure characterization of the complexes of beta-alkoxycarbonylethyltin trichlorides with Schiff base ligands

Thirty - two title complexes (ROCOCHRCH2SnCl3)-C-1 . (2 - HOC6H4CH = NC6H4 - X) (R = Me, Et, n - Bu; R-1 = H, Me; X = H,4' - Cl, 3' - Pr, 3' - OH, 3', 4' - Cl-2, 4' - OMe) were synthesized and characterized by elemental analysis,UV - vis, IR, H-1 NMR. The crystal structure of n - BuOCOCH2CH2SnCl3 . (2 - HOC6H4CH - NC6H4OMe - 4') were determined by the X - ray diffraction analysis, The crystal belongs to monoclinic system, with a = 1.4661 (3)nm, b = 0.9307 (2)nm, c = 1.7888 (4)nm, beta = 94.04 (3)degrees, V = 2.4348nm(3), D-c = 1.581mg/m(3), Z = 4, F(000) = 1160, mu = 1.405mm(-1), R = 0.0354, R-w = 0,0486, space group: P2(1)/c. The complexes exist as a discrete monomer. The tin atom has a distorted octahedral geometry due to intramolecular coordination of the carbonyl oxygen and the phenolic oxygen of the Schiff base ligands, The coordination number of tin atom is 6.

Synthesis, crystal structure and properties of (Z)-3-triphenylstannyl-1,1-diphenyl propenol

Five new organotin compounds were synthesized and characterized, X-ray crystal structure analysis of (Z)-3-triphenylstannyl-1,1-diphenyl propenol was performed, The crystal belongs to space group P2(1)/n. The cell parameters are: a = 1.235 7(2) nm, b = 0.987 4(2) nm, c = 2.208 1(4) nm, beta = 95.23(3)degrees, V = 2.683 0(9) nm(3), Z = 4, R = 0.027 9, R-w = 0.064 5. The tin atom of the molecule exists in a distorted tetrahedron, Z isomer of double bond is obtained.

Crystal structure and mechanism of (Z)-1-[2-(phenyl-bromide-chloride)vinyl]-1-cyclohexanol

The crystal structure and mechanism of the title molecule are described. This crystal is orthorhombic, belonging to space group PC21/B with a=1,002 1(2) nm, b=1.483 0(3) nm, c=2.173 6(4) nm, V=3.230 39(2) nm(3), Z=2, D-c=1.80 g/cm(3), R=0.069 3. The structure was solved by direct method. The tin atom of the title compound exists in two distorted-trigonal-bipyramidal geometry, defined by two carbon, one bromide, one chloride and one oxygen atoms leading to a five-membered chelate ring. In the structure, the five-membered ring containing the intermolecular O-->Sn has a half chair conformation.

Synthesis, structure characterization and transesterification of the complexes of beta-alkoxycarbonylethyltin trichlorides

Thirteen title complexes ROCOCH2CH2SnCl3 . L(R = C(1 similar to 5)alkyl;L = DBSO,HMPA) were synthesized and characterized by elemental analysis, IR,H-1 NMR. The crystal structure of n -PrOCOCH2CH2SnCl3 . DBSO was determined by the X-ray diffraction analysis. The crystal belongs to orthorhombic system,space group P2(1)2(1)2(1) with a = 1.062, b = 1.427, c = 1.635nm; Z = 4. The complex exists as a discrete molecule, and the tin atom attains a distorted octahedral geometry via the coordination of intramolecular carbonyl oxygen and the Lewis base donor atom. The transesterification of CH3OCOCH2CH2SnCl3 . L with alcohol was studied, and the intramolecular Lewis acid catalytic mechanism was suggested.

Synthesis and chemical properties of [Z]-1-[2-(triaryl stannyl)vinyl]cyclooctanol

The compounds of [Z]-1-[2-(triphenyl stannyl) vinyl] cyclooctanol (1) and [Z]-1-[2-(tri-p-tolyl stannyl) vinyl] cyclooctanol (2) were synthesized by the reactions of triphenyltin hydride and tri-p-tolyltin hydride with 1-ethynyl cyclooctanol. The crystal structure of compound 1 was determined. The reactions of compound 1 and 2 with IC1, Br-2, I-2 formed nine organotin halides. The organotin oxide or hydroxide were prepared by the reactions of [Z]-1-[2-(phenyl dibromo stannyl) vinyl] cyclooctanol (6) and [Z]-1-[2-(diphenyl monobromo stannyl) vinyl] cyclooctanol (5) with KOH. Three complexes were obtained by the reactions of [Z]-1-[2-(phenyl diiodide stannyl) vinyl] cyclooctanol (8) with three ligands (2,2'-bipyridyl,5-nitro-1,10-phenanthroline,8-Hydroxyquinoline). The sixteen new compounds synthesized in this paper were characterized by means of elemental analysis, IR, H-1 NMR. The reaction mechanism of triphenyltin hydride and tri-p-tolyltin hydride with 1-ethynyl cyclooctanol were also proposed.

A study of the radical reaction of C-60 with n-Bu(3)SnH

The reaction of buckministerfullerene (C-60) with tri-n-blltyltin hydride(n-Bu(3)SnH) in toluene solution has been investigated. According to mass spectrometry analysis, the products of above reaction are C-60(BuH)(n)(n = 1 similar to 3) and Bu(x)Sn(y)H(x) (x = 3 similar to 8, y = 1 similar to 4,approximate to = 0 similar to 3). The reaction maybe provide a new method for the synthesis of alkylated fullerene derivatives. Where C-60 also takes a role of a catalysis of organtic-tin polymerization. The radical reaction mechanism has been discussed.

Crystal and molecular structure of the complex of methoxycarbonylethyltin trichloride with salicylidene-m-toluidine

The synthesis and properties of the title complex CH3OCOCH2CH2SnCl3.2-HOC6H4CH=NC6H4-3'-CH3 are described. It crystallizes from benzene in the monoclinic space group P2(1/n) with unit cell dimensions a=10.326 (C),b=6.815(8), c=12.931(6) Angstrom, beta =111.52(3,)degrees, V=2088.7(1) Angstrom (3), Z=4, F(000) =1040, mu =16.31 cm(-1), Dc=1. 67g/cm(3) final R factor is 0.037 for 3177 observed reflections, 1 greater than or equal to3 sigma (1(0)). The tin atom in the structure of the complex exists in a distored octahedral geometry defined by three Cl atoms, the C and O atoms of a chelating methoxycarbonylethyl. group as well as an O atom derived from the Schiff base ligand.

SYNTHESIS AND CRYSTAL-STRUCTURE OF (C9H7GDCL2.3THF)THF

The indenylpdolinium dichloride tristetrahydrofuranate (C9H7GdCl2.3THF)THF was prepared and its crystal structure (monoclinic space group P2(1)) determined by X-ray diffraction. In C9H7GdCl2.3THF, Gd, O(1), O(2), O(3) and the centroid of the five-membered indenyl ring form a plane, and Cl(1) and Cl(2) are located at two opposite sides of the plane to give a pseudo-octahedron. The coordination number of Gd is eight.

核磁共振波谱仪MLEV-16宽带去耦系统

在FX-100核磁共振波谱仪上建立了MLEV-16宽带去耦系统.对去耦电路的各级信号进行了分析,说明了MLEV-16去耦电略的控制关系.利用去耦电路实现了由计算机和可编程序器控制的宽带去耦,用波谱仪原有去耦功率作了~(13)C{F~(19)}氟宽带去耦的碳-13谱的观测,去耦范围达12.4kHz,可以满足大部分有机氟化物的~(13)C核磁共振研究。