4-Bromophenylboronate Derivatives of Ring and Cage Borosilicates

2002 ◽  
Vol 67 (7) ◽  
pp. 1051-1060 ◽  
Author(s):  
Anthony G. Avent ◽  
Simon E. Lawrence ◽  
Margaret M. Meehan ◽  
Tom G. Russell ◽  
Trevor R. Spalding
Keyword(s):  
Single Crystal ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Work Up ◽  
Derivatives Of

The reactions between equimolecular amounts of 4-bromophenylboronic acid and di-tert-butylsilanediol or tert-butylsilanetriol in toluene solutions at reflux temperatures afforded the borosilicate ring compound [(4-BrC6H4B)O2Si(t-Bu)2]2 (1), and the cube-based species [(t-BuSi)4(4-BrC6H4B)4O10] (2), in medium (62%) and low (13%) yields, respectively. These compounds were characterised by microanalysis, IR and NMR (1H, 11B, 13C and 29Si) spectroscopy and single crystal X-ray crystallography. During the work-up of 2, a sample of the boroxine, [(4-BrC6H4BO)3] (3), was isolated and was characterised by single crystal diffraction.

The Conformation of Some 1,6-Disulfide-Bridged D-Hexopyranoses

2005 ◽  
Vol 58 (3) ◽  
pp. 199 ◽  
Author(s):  
Ethan D. Goddard-Borger ◽  
Brian W. Skelton ◽  
Robert V. Stick ◽  
Allan H. White
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Similar Investigation ◽  
X Ray ◽  
X Ray Crystallography ◽  
Structure Determinations ◽  
Derivatives Of

The use of 1H NMR spectroscopy, in tandem with X-ray crystallography, has cast light on the conformation of the 1,6-disulfide-bridged derivatives of d-gluco-, d-manno-, d-allo-, d-galacto-, and d-talo-pyranose. A similar investigation was performed on the thiosulfinate derived from the d-gluco disulfide. Single-crystal X-ray structure determinations are reported for (1S,5S,6S,7S,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, (1S,5S,6S,7R,8R)-6,7,8-tribenzoyloxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane, and (1S,2S,5S,6S,7S,8R)-6,7,8-triacetoxy-9-oxa-2,3-dithiabicyclo[3.3.1]nonane 2-oxide.

Synthesis, Spectroscopic Characterization, and Structure of closo-1,10-B10H8F22- and Related Fluorinated Derivatives of B10H102-

1997 ◽  
Vol 62 (8) ◽  
pp. 1310-1324 ◽  
Author(s):  
Sergei V. Ivanov ◽  
Svetlana M. Ivanova ◽  
Susie M. Miller ◽  
Oren P. Anderson ◽  
Nikolai T. Kuznetsov ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Single Crystal ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
X Ray Crystallography ◽  
Fluorinated Derivatives ◽  
Derivatives Of

The treatment of salts of the B10H102- anion with the commercially available N-fluoro reagent 1-chloromethyl-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate) (F-TEDA) resulted in the formation of fluorinated derivatives of this ten-vertex borane dianion. The effects of changing the solvent, temperature, and reagent stoichiometry were studied. The derivatives 1-B10H9F2-, 2-B10H9F2-, 1,2-B10H8F22-, 1,6-B10H8F22-, 1,10-B10H8F22-, and 1,2,10-B10H7F32- were examined by a combination of 11B and 19F NMR spectroscopy and by IR spectroscopy. The salt [Ph4P]2[1,10-B10H8F2] . 3 CH2Cl2 was structurally characterized by single-crystal X-ray crystallography: C51H48B10Cl6F2P2, monoclinic, C2/c, a = 13.8134(9), b = 19.141(1), c = 21.136(1) Å, β = 91.546(1)°, Z = 4, T = -100 °C, R = 0.077.

Pentafluorophenyl and phenyl substituted azidoborates

2002 ◽  
Vol 80 (11) ◽  
pp. 1444-1450 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Thomas M Klapötke ◽  
Burkhard Krumm ◽  
Heinrich Nöth ◽  
Max Suter ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Boron Atom ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
X Ray Crystallography ◽  
Multinuclear Nmr Spectroscopy

The azidoborates [(C6F5)4–nB(N3)n]– (n = 1–3) (1–3) were synthesized by reacting the corresponding borane with [R]N3 (R = Me4N, Ph4P). To study the influence of the electron withdrawing C6F5-substituent on the boron atom, [Me4N][(C6H5)3BN3] (4) was also prepared. All compounds were fully characterized by IR, Raman, and multinuclear NMR spectroscopy in addition to characterization by single crystal diffraction analyses.Key words: azidoborate, pentafluorophenyl, multinuclear NMR spectroscopy, X-ray crystallography.

scholarly journals Environmentally Friendly Nafion-Catalyzed Synthesis of Substituted 2-Ethyl-3-Methylquinolines from Aniline and Propionaldehyde under Microwave Irradiation

Catalysts ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 877
Author(s):  
Chieh-Kai Chan ◽  
Chien-Yu Lai ◽  
Cheng-Chung Wang
Keyword(s):  
Reaction Mechanism ◽  
Microwave Irradiation ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Environmentally Friendly ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Related Data ◽  
Heating Source ◽  
Chemical Structures

Herein, we report a facile synthetic methodology for the preparation of 2,3-dialkylquinolines from anilines and propionaldehydes. This cyclization involved environmentally friendly Nafion® NR50 as an acidic catalyst with microwave irradiation as the heating source. A series of substituted 2-ethyl-3-methylquinolines were prepared from various anilines and propionaldehyde derivatives through this protocol with good to excellent yields. Some new chemical structures were confirmed by X-ray single-crystal diffraction analysis and the related data were provided. The plausible reaction mechanism studies are also discussed.

Verfeinerung der Kristallstruktur von Tripalladium-di-tetrathiophospliat Pd3(PS4)2 Refinement of the Crystal Structure of Tripalladium-di-tetrathiophosphate Pda3(PS4)2

1983 ◽  
Vol 38 (4) ◽  
pp. 426-427 ◽  
Author(s):  
Arndt Simon ◽  
Karl Peters ◽  
Harry Hahn
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Type Structure ◽  
Tetrahedral Symmetry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Planar Environment

Abstract The structure of the title compound has been determined by X-ray crystallography. The title compound is synthesized from the elements at 600 °C. Its crystal structure, derived from powder data [3] is refined by single crystal diffractometer data. The structure is trigonal (P3̅ml, α = 684.1(1), c = 724.4(1) pm); Pd2+ cations and PS43- anions form a network with an anti-Claudetite (AS2O3) type structure. The PS4 units are distinctly distorted from ideal tetrahedral symmetry. The Pd atoms have a planar environment of 4 S atoms.

scholarly journals Synthesis, Structure, and Antiproliferative Activity of Three Gallium(III) Azole Complexes

2010 ◽  
Vol 2010 ◽  
pp. 1-10 ◽  
Author(s):  
Stergios Zanias ◽  
Giannis S. Papaefstathiou ◽  
Catherine P. Raptopoulou ◽  
Konstantinos T. Papazisis ◽  
Vasiliki Vala ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Antiproliferative Activity ◽  
Bioinorganic Chemistry ◽  
Anionic Complex ◽  
X Ray ◽  
X Ray Crystallography ◽  
Mononuclear Complexes ◽  
Human And Mouse ◽  
Antiproliferative Activities

As part of our interest into the bioinorganic chemistry of gallium, gallium(III) complexes of the azole ligands 2,1,3-benzothiadiazole (btd), 1,2,3-benzotriazole (btaH), and 1-methyl-4,5-diphenylimidazole (L) have been isolated. Reaction of btaH or btd withGaBr3orGaCl3resulted in the mononuclear complexes[GaBr3(btaH)2](1) and[GaCl3(btd)2](2), respectively, while treatment ofGaCl3with L resulted in the anionic complex(LH)2[GaCl4](3). All three complexes were characterized by single-crystal X-ray crystallography and IR spectroscopy, while their antiproliferative activities were investigated against a series of human and mouse cancer cell lines.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

The direct electrochemical synthesis of some metal derivatives of lapachol

1997 ◽  
Vol 75 (5) ◽  
pp. 499-506 ◽  
Author(s):  
E.H. De Oliveira ◽  
G.E.A. Medeiros ◽  
C. Peppe ◽  
Martyn A. Brown ◽  
Dennis G. Tuck
Keyword(s):  
Electrochemical Oxidation ◽  
Copper Atom ◽  
Electrochemical Synthesis ◽  
Acetonitrile Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Anode ◽  
X Ray Crystallography ◽  
Metal Derivatives ◽  
Derivatives Of

The electrochemical oxidation of a sacrificial metal anode (M = Zn, Cd, Cu) in an acetonitrile solution of 2-hydroxy-3-(3-methyl-2-butenyl)-1,4-naphthoquinone, lapachol, C15H14O3 (=HL) gives ML2. The results are in keeping with earlier work on direct electrochemical synthesis in related systems. Adducts with 2,2′-bipyridine (bpy) and N,N,N′,N′-tetramethylethanediamine (tmen) have also been prepared. The structure of the 2,2′-bipyridine adduct of Cu(lapacholate)2 has been established by X-ray crystallography. The parameters are triclinic, space group [Formula: see text], a = 12.748(59) Å, b = 13.859(49) Å, c = 11.770(59) Å, α = 108.30(4)°, β = 108.08(3)°, γ = 68.94(3)°, Z = 2, R = 0.059 for 2256 unique reflections. The copper atom is in a distorted CuN2O2O2′ environment. The mechanism of the formation of this Cu(lapacholate)2 is discussed. Keywords: electrochemical synthesis, lapachol, X-ray crystallography, copper(II) complex.

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