Baeyer-Villiger Oxidation of 10-Methyl-9-Anthraldehyde: Formation and Photochemical Dimerization of 9-Formyloxy-10-methylanthracene

1988 ◽  
Vol 41 (12) ◽  
pp. 1977 ◽  
Author(s):  
HD Becker ◽  
BW Skelton ◽  
AB Turner ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Hydrogen Peroxide ◽  
Acetic Acid ◽  
Sulfuric Acid ◽  
Diffraction Study ◽  
Crystalline State ◽  
X Ray Diffraction ◽  
X Ray ◽  
Tail Structure ◽  
Villiger Oxidation

Oxidation of 10-methyl-9-anthraldehyde with hydrogen peroxide in acetic acid in the presence of sulfuric acid gives 9-formyloxy-10-methylanthracene which dimerizes in solution upon exposure to light. The head-to-tail structure of the 4π+4π photodimer was established by a single-crystal X-ray diffraction study. In the crystalline state, the molecular structure is centrosymmetric, and the length of the photochemically formed bonds 1.646(4)Ǻ. Crystals are monoclinic, P21/c, a 7.980(5), b 16.143(7), c 9.571(3)Ǻ, β 114.38(3)°, Z=2 dimers; R was 0.041 for 1362 'observed' diffractometer reflections.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

A Novel Methylene Dithioether as a Ligand: Synthesis and Molecular Structure of a Zinc(II) Complex with N4S2 Coordination Environment

2003 ◽  
Vol 58 (10) ◽  
pp. 1027-1029 ◽  
Author(s):  
F. Ekkehardt Hahn ◽  
Christoph Jocher ◽  
Henning Schröder
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Aluminum Hydroxide ◽  
Zinc Atom ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Octadentate Ligand ◽  
Ligand Synthesis ◽  
Perchlorate Hexahydrate

The octadentate ligand [N(CH2CH2NH2)(CH2CH2CH2OH)(CH2CH2S)]2CH2, (NNOS-232)2CH2, was synthesized accidentally by the reaction of the unsymmetrically substituted tripod [N(CH2CH2NH2)(CH2CH2CH2OH)(CH2CH2SH)], NNOS-232, with dichloromethane in the presence of aluminum hydroxide. Ligand (NNOS-232)2CH2 was reacted with zinc bis(perchlorate) hexahydrate to yield the complex [Zn((NNOS-232)2CH2)](ClO4)2 1 exhibiting a distorted octahedrally coordinated zinc atom in an N4S2 coordination environment, as shown by an X-ray diffraction study.

scholarly journals Synthesis and Characterization of New Diiron and Diruthenium μ-Aminocarbyne Complexes Containing Terminal S-, P- and C-Ligands

2007 ◽  
Vol 62 (3) ◽  
pp. 427-438 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Luigi Busetto ◽  
Fabio Marchetti ◽  
Magda Monari ◽  
Stefano Zacchini ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Coordination Mode ◽  
Bond Cleavage ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dithiocarbamate Ligand ◽  
High Yields

The diiron aminocarbyne complexes [Fe2{μ-CN(Me)(R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (R = Xy1, 1a; R = Me, 1b; R = CH2Ph, 1c; Xy1 = 2,6-Me2C6H3) undergo replacement of the coordinated nitrile by halides, diethyldithiocarbamate, and dicyanomethanide to give [Fe2{μ-CN(Me) (R)}(μ-CO)(CO)(X)(Cp)2] complexes (R = Me, X = Br, 4a; R = Me, X = I, 4b; R = CH2Ph, X = Cl, 4c; R = CH2Ph, X = Br, 4d; R = CH2Ph, X = I, 4e; R = Xy1, X = SC(S)NEt2, 5a; R = Me, X = SC(S)NEt2, 5b; R = Xy1, X = CH(CN)2, 7), in good yields. The molecular structure of 5a shows an unusual η1 coordination mode of the dithiocarbamate ligand. Similarly, treatment of [M2{μ-CN(Me) (R)}(μ-CO)(CO)(NCMe)(Cp)2][SO3CF3] (M = Fe, R = Xy1, 1a; M = Fe, R = Me, 1b; M = Ru, R = Xy1, 2a; M = Ru, R = Me, 2b) with a series of phosphanes generates the cationic complexes [M2{μ- CN(Me)(R)}(μ-CO)(CO)(P)(Cp)2][SO3CF3] (M = Fe, R = Xy1, P = PPh2H, 6a; M = Fe, R = Xy1, P = PPh3, 6b; M = Fe, R = Xy1, P = PMe3, 6c; M = Fe, R = Me, P = PMe2Ph, 6d; M = Fe, R = Me, P = PPh3, 6e; M = Fe, R = Me, P = PMePh2, 6f; M = Ru, R = Xy1, P = PPh2H, 6g; M = Ru, R = Me, P = PPh2H, 6h), in high yields. The molecular structure of 6a has been elucidated by an X-ray diffraction study. The reactions of [Fe2{μ-CN(Me)(Xyl)}(μ-CO)(CO)(NCR′)(Cp)2][SO3CF3] [R′ = Me, 1a; R′ = tBu, 3] with PhLi and PPh2Li yield [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(Ph)(Cp)2] (8) and [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(PPh2)(Cp)2] (9), respectively. The molecular structure of 8 has been ascertained by X-ray diffraction. Conversely, the reaction of 1a with MeLi generates the aminoalkylidene compound [Fe2{C(Me)N(Me)(Xy1)}(μ-CO)2(CO)(Cp)2] (10).Finally, the acetone complex [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(OCMe2)(Cp)2][SO3CF3] (12) reacts with lithium acetylides to give complexes [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO)(C≡CR)(Cp)2] (R = p-C6H4Me, 11a; R = Ph, 11b; R = SiMe3, 11c), in high yields. Filtration through alumina of a solution of 11a in CH2Cl2 results in hydration of the acetylide group and C-Si bond cleavage, affording [Fe2{μ-CN(Me)(Xy1)}(μ-CO)(CO){C(O)Me}(Cp)2] (12).

The molecular structure of N,N′-disulfinyl-3,4,5,6-tetrafluoro-1,2-diaminobenzene: A computational and X-ray diffraction study

2010 ◽  
Vol 978 (1-3) ◽  
pp. 158-162 ◽  
Author(s):  
Arkady G. Makarov ◽  
Irina Yu. Bagryanskaya ◽  
Yuri V. Gatilov ◽  
Alexander Yu. Makarov ◽  
Karla Tersago ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
X Ray Diffraction ◽  
X Ray

Reactions of Transition-Metal Sigma-Acetylides. V. Synthesis and X-Ray Structure of Co2(µ-η2-PhC2Fe(Co)2(η-C5h5))(Co)6

1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Diffraction Study ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.

X-ray diffraction study of copper(I) thiourea complexes formed in sulfate-containing acid solutions

2000 ◽  
Vol 56 (6) ◽  
pp. 993-997 ◽  
Author(s):  
O. E. Piro ◽  
R. C. V. Piatti ◽  
A. E. Bolzán ◽  
R. C. Salvarezza ◽  
A. J. Arvia
Keyword(s):  
Molecular Structure ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
Copper Ions ◽  
Acid Solutions ◽  
Inversion Center ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thiourea Complex

The formation of three different copper(I) thiourea complexes in sulfate-containing acid solutions was observed. The ratio between CuI and thiourea (tu) in these complexes depends on the amount of thiourea and copper sulfate in the solution. The crystal and molecular structure of a new complex, [Cu_2(tu)_6](SO_4)\cdotH_2O, was determined, and the formation and structures of [Cu_2(tu)_5](SO_4)\cdot3H_2O and [Cu_4(tu)_7](SO_4)_2\cdotH_2O were confirmed. The compound [Cu_2(tu)_6](SO_4)\cdotH_2O crystallizes in the P\overline 1 space group, with a = 11.079 (2), b = 11.262 (1), c = 12.195 (2) Å, \alpha = 64.84 (1), \beta = 76.12 (1), \gamma = 66.06 (1)°, and Z = 2. The Cu-thiourea complex is arranged as a CuI tetranuclear ion, [Cu_4(tu)_{12}]^{4+}, sited on a crystallographic inversion center. All copper ions are in a tetrahedral coordination with thiourea ligands and located at alternate sites on an eight-membered, crown-like ring.

scholarly journals Synthesis, reactivity, and antimicrobial properties of boron-containing 4-ethyl-3-thiosemicarbazide derivatives

2018 ◽  
Vol 96 (10) ◽  
pp. 906-911 ◽  
Author(s):  
Ryan S. Scott ◽  
Alex J. Veinot ◽  
Darcie L. Stack ◽  
Patrick T. Gormley ◽  
B. Ninh Khuong ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Saccharomyces Cerevisiae ◽  
Pseudomonas Aeruginosa ◽  
Aspergillus Niger ◽  
Diffraction Study ◽  
Boronic Acid ◽  
Antimicrobial Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thiosemicarbazide Derivatives

The addition of 4-ethyl-3-thiosemicarbazide to benzaldehyde and boronic acid containing derivatives afforded the corresponding thiosemicarbazones (1–3) or benzodiazaborines (4–6) depending on the position of the boronic acid within the ring. All compounds have been characterized fully including an X-ray diffraction study of the methoxy-containing benzodiazaborine 6. Attempts to coordinate thiosemicarbazones 2 and 3 to palladium(II) acetate were unsuccessful; however, addition of the non-boron-containing derivative 1 to palladium afforded complex 7 whose molecular structure was determined by an X-ray diffraction study. The initial bioactivities of compounds 1–7 were examined against two fungi, Aspergillus niger and Saccharomyces cerevisiae, and two bacteria, Bacillus cereus and Pseudomonas aeruginosa.

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