Conformations of saturated six-membered-ring phosphorus heterocycles. Axial, nonplanar dimethylamino group of 5,5-dimethyl-2-(dimethylamino)-2-oxo-1,3,2-oxazaphosphorinane as determined by x-ray crystallography. Proton NMR and IR spectroscopic analysis of conformation in solution

1984 ◽  
Vol 106 (8) ◽  
pp. 2353-2358 ◽  
Author(s):  
Robert R. Holmes ◽  
Roberta O. Day ◽  
William N. Setzer ◽  
Alan E. Sopchik ◽  
Wesley G. Bentrude
Keyword(s):  
Spectroscopic Analysis ◽  
Proton Nmr ◽  
Membered Ring ◽  
Dimethylamino Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Phosphorus Heterocycles ◽  
Ir Spectroscopic

scholarly journals Silylated gallium and indium chalcogenide ring systems as potential precursors to ME (E=O, S) materials

2013 ◽  
Vol 11 (7) ◽  
pp. 1225-1238
Author(s):  
Iliana Medina-Ramírez ◽  
Cynthia Floyd ◽  
Joel Mague ◽  
Mark Fink
Keyword(s):  
Thermal Decomposition ◽  
Room Temperature ◽  
Membered Ring ◽  
Molecular Structures ◽  
Nmr Studies ◽  
X Ray ◽  
X Ray Crystallography ◽  
High Yields ◽  
Vt Nmr ◽  
State 1

AbstractThe reaction of R3M (M=Ga, In) with HESiR′3 (E=O, S; R′3=Ph3, iPr3, Et3, tBuMe2) leads to the formation of (Me2GaOSiPh3)2(1); (Me2GaOSitBuMe2)2(2); (Me2GaOSiEt3)2(3); (Me2InOSiPh3)2(4); (Me2InOSitBuMe2)2(5); (Me2InOSiEt3)2(6); (Me2GaSSiPh3)2(7); (Et2GaSSiPh3)2(8); (Me2GaSSiiPr3)2(9); (Et2GaSSiiPr3)2(10); (Me2InSSiPh3)3(11); (Me2InSSiiPr3)n(12), in high yields at room temperature. The compounds have been characterized by multinuclear NMR and in most cases by X-ray crystallography. The molecular structures of (1), (4), (7) and (8) have been determined. Compounds (3), (6) and (10) are liquids at room temperature. In the solid state, (1), (4), (7) and (9) are dimers with central core of the dimer being composed of a M2E2 four-membered ring. VT-NMR studies of (7) show facile redistribution between four- and six-membered rings in solution. The thermal decomposition of (1)–(12) was examined by TGA and range from 200 to 350°C. Bulk pyrolysis of (1) and (2) led to the formation of Ga2O3; (4) and (5) In metal; (7)–(10) GaS and (11)–(12) InS powders, respectively.

scholarly journals Reactions and interactions between peri-groups in 1-dimethylamino-naphthalene salts: an example of a “through space” amide

2016 ◽  
Vol 88 (4) ◽  
pp. 317-331
Author(s):  
Amélie Wannebroucq ◽  
Andrew P. Jarmyn ◽  
Mateusz B. Pitak ◽  
Simon J. Coles ◽  
John D. Wallis
Keyword(s):  
Hydrogen Bond ◽  
Methyl Ester ◽  
Carbonyl Group ◽  
Dimethylamino Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Electron Donation ◽  
Protonated Cation

Abstract8-Dimethylaminonaphthalene-1-carbaldehyde reacts readily at 0°C with benzoyl or pivaloyl chloride by O-acylation and formation of a N–C bond (1.566(2)–1.568(3) Å) between the peri-substituents to give a salt. The reaction is promoted by electron donation from the dimethylamino group to the carbonyl group, akin to the properties of an amide. In contrast, the corresponding methyl ester and N,N-diisopropylamide react with acid in ether by protonation of the dimethylamino group and formation of a hydrogen bond to the carbonyl group, while under similar conditions the N,N-dimethylamide undergoes ready hydrolysis to the acid. The structures of products are determined by X-ray crystallography, and from the latter hydrolysis crystals containing zwitterionic 1-dimethylammonium-naphthalene-8-carboxylate and the corresponding O-protonated cation along with dimethylammonium and triflate ions were obtained.

Conformation of two 4'-thio-2'-deoxynucleoside analogs studied by 5000-MHz proton NMR spectroscopy and x-ray crystallography.

1992 ◽  
Vol 114 (25) ◽  
pp. 9936-9943 ◽  
Author(s):  
Leo H. Koole ◽  
Janez Plavec ◽  
Hongying Liu ◽  
Beverly R. Vincent ◽  
Michael R. Dyson ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Proton Nmr ◽  
Proton Nmr Spectroscopy ◽  
X Ray ◽  
X Ray Crystallography

Mononuclear and Binuclear Complexes of Platinum(0) Containing (Alkynyl)phenylsilanes

1999 ◽  
Vol 52 (1) ◽  
pp. 51 ◽  
Author(s):  
Martin A. Bennett ◽  
Christopher J. Cobley ◽  
David C. R. Hockless ◽  
Thomas Klettke
Keyword(s):  
Spectroscopic Data ◽  
Chair Conformation ◽  
Membered Ring ◽  
Binuclear Complexes ◽  
Nickel Compound ◽  
X Ray ◽  
X Ray Crystallography

Reaction of bis(cycloocta-1,5-diene)platinum(0) with the (alkynyl)phenylsilanes Ph3SiC2But, Ph2Si(C2But)2 and PhSi(C2But)3 gives, respectively, [Pt (Ph3SiC2But)2] (1b), [Pt {Ph2Si(C2But)}]2 (2b), and [Pt {PhSi(C2But)3}]2 (4b), which contain zerovalent platinum atoms coordinated by two alkyne units. Spectroscopic data indicate that (2b) and (4b) contain two PtC4 and two SiC4 tetrahedra joined at the corners. X-Ray crystallography shows that complex (4b) is isostructural and isomorphous with the known nickel analogue, two of the alkyne units being uncoordinated; the central eight-membered ring comprising two silicon, four alkyne carbon and two platinum atoms has an approximate chair conformation. In contrast, the monomer (1b) is isostructural but not isomorphous with the analogous nickel compound (1a); in the crystal there is evidence for a weak intramolecular phenyl-phenyl interaction.

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