The OsO3F+and μ-F(OsO3F)2+Cations:  Their Syntheses and Study by Raman and19F NMR Spectroscopy and Electron Structure Calculations and X-ray Crystal Structures of [OsO3F][PnF6] (Pn = As, Sb), [OsO3F][HF]2[AsF6], [OsO3F][HF][SbF6], and [OsO3F][Sb3F16]†

2002 ◽  
Vol 41 (2) ◽  
pp. 259-277 ◽  
Author(s):  
Michael Gerken ◽  
David A. Dixon ◽  
Gary J. Schrobilgen
Keyword(s):  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Electron Structure ◽  
X Ray ◽  
Structure Calculations

Synthesis and crystal structures of three novel benzimidazole/benzoindolizine hybrids

2016 ◽  
Vol 71 (3) ◽  
pp. 231-239 ◽  
Author(s):  
Roumaissa Belguedj ◽  
Sofiane Bouacida ◽  
Hocine Merazig ◽  
Ali Belfaitah ◽  
Aissa Chibani ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Dipolar Cycloaddition ◽  
Dimethyl Acetylenedicarboxylate ◽  
X Ray ◽  
X Ray Crystallography ◽  
Dimethyl Maleate

AbstractThree benzoindolizine derivatives, 1, 2, and 3, were obtained via 1,3-dipolar cycloaddition. The reaction of 1-(2′-benzimidazolylmethyl)isoquinolinium ylides with dimethyl acetylenedicarboxylate gave a mixture of pyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (1) and 1,10b-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (2) derivatives containing a benzimidazole moiety. The reaction of this isoquinolinium N-ylide with dimethyl maleate gave an unexpected 2,3-dihydropyrrolo[2,1-a]isoquinoline-1,2-dicarboxylate (3). The structures of all reported compounds have been examined by X-ray crystallography, mass spectrometry, and NMR spectroscopy.

Structures of two new high-pressure forms of AlPO4 by X-ray powder diffraction and NMR spectroscopy

2011 ◽  
Vol 67 (1) ◽  
pp. 30-40 ◽  
Author(s):  
Masami Kanzaki ◽  
Xianyu Xue ◽  
Sindy Reibstein ◽  
Eleanor Berryman ◽  
Seonyi Namgung
Keyword(s):  
High Pressure ◽  
Nmr Spectroscopy ◽  
Ab Initio ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Structure Determination ◽  
Rietveld Method ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
X Ray

The crystal structures of two new high-pressure AlPO4 phases are reported. One phase synthesized at 6 GPa and 1523 K is triclinic (P\bar 1) whilst the other phase synthesized at 7 GPa and 1773 K is monoclinic (P2_1/c). 31P MAS (magic-angle spinning) NMR suggests three tetrahedral P sites with equal abundance in both phases. 27Al 3Q MAS NMR spectra provided evidence for two octahedral sites and one five-coordinated Al site in each phase. The crystal structures were solved using an ab initio structure determination technique from synchrotron powder X-ray diffraction data utilizing the local structural information from NMR, and were further refined by the Rietveld method. Both phases contain doubly bent chains made of six edge-shared Al polyhedra (including five-coordinated Al), which are joined by PO4 tetrahedra. The P\bar{1} phase is isostructural with FeVO4 and AlVO4. The two phases differ in the packing manner of the chains. This study has demonstrated that the combined application of ab initio structure determination via X-ray powder diffraction and solid-state NMR spectroscopy is a powerful approach to the rapid solution of complex inorganic crystal structures.

Synthesis, Crystal Structures, and Reactions of 2-Oxomalonylbis(arylimidoyl) Chlorides and Hydroxymethane Tris(arylimidoyl) Chlorides

2005 ◽  
Vol 58 (7) ◽  
pp. 522
Author(s):  
Richard J. Bowen ◽  
Judy Caddy ◽  
Mabel E. Coyanis ◽  
Manuel A. Fernandes ◽  
Marcus Layh ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Hydrolysis Of

The 2-oxomalonylbis(arylimidoyl) chlorides [C6H3(R2-2,6)N=CCl]2CO (R = Me, 3a; Pri, 3b; H, 3c) were synthesized from C6H3(R2-2,6)NHCHO and an excess of (COCl2)3 and their reaction with various nucleophiles was studied. Successive hydrolysis of 3a led to the formation of [C6H3(Me2-2,6)N=CCl]3COH 4a and [C6H3(Me2-2,6)NHCO]3COH 5a, while treatment of 3a with HAuCl4(H2O)x gave {[C6H3(Me2-2,6)N(H)=CCl][C6H3(Me2-2,6)NHCO]2COH}AuCl4 6a. All compounds were fully characterized by microanalysis, NMR spectroscopy, mass spectrometry, and, in the case of 3a, 4a, 5a, and 6a, by X-ray crystallography.

Komplexe des Typs [MCl4(SEt2)2] mit M = Mo und W. Kristallstrukturen, NMR-Spektren und magnetisches Verhalten/[MCl4(SEt2)2] Complexes with M = Mo and W. Crystal Structures, NMR Spectra, and Magnetic Behaviour

1995 ◽  
Vol 50 (2) ◽  
pp. 159-167 ◽  
Author(s):  
Peter Dierkes ◽  
Gerlinde Frenzen ◽  
Sigrid Wocadlo ◽  
Werner Massa ◽  
Stefan Berger ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Nmr Spectra ◽  
Magnetic Behaviour ◽  
Triclinic Space Group ◽  
Magnetic Susceptibilities ◽  
X Ray ◽  
Metal Atoms ◽  
Ray Methods ◽  
C Nmr

The crystal structures of the thioether complexes [MCl4(SEt2)2] with M = Mo and W have been solved by X-ray methods. Both compounds crystallize isotypically in the triclinic space group P1̄ with two formula units per cell unit. The metal atoms are octahedrally coordinated by four chlorine atoms and by the two sulfur atoms of the thioether molecules in transposition (symmetry Ci) with bond lengths (average): Mo-Cl 233.1, Mo-S 253.4, W-Cl 233.1, and W-S 251.7 pm. Both complexes were also characterized by 1H and 13C NMR spectroscopy as well as by measurement of the magnetic susceptibilities in the temperature range from 1.8 to 350 K.

Crystal structures and cation ordering in Cs2MgSi5O12, Rb2MgSi5O12 and Cs2ZnSi5O12 leucites

2009 ◽  
Vol 65 (4) ◽  
pp. 435-444 ◽  
Author(s):  
A. M. T. Bell ◽  
C. M. B. Henderson
Keyword(s):  
Nmr Spectroscopy ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Divalent Cation ◽  
Mas Nmr ◽  
Cation Ordering ◽  
X Ray ◽  
Tetrahedral Sites ◽  
Starting Model ◽  
Leucite Structure

The crystal structures of the leucite analogues Cs2MgSi5O12, Cs2ZnSi5O12 and Rb2MgSi5O12 have been determined by synchrotron X-ray powder diffraction using Rietveld refinement in conjunction with 29Si MAS NMR spectroscopy. These leucites are framework structures with distinct tetrahedral sites (T sites) occupied by Si and a divalent cation (either Mg or Zn in these samples); there is also a monovalent extra-framework cation (either Cs or Rb in these samples). The refined crystal structures were based on the Pbca leucite structure of Cs2CdSi5O12, thus a framework with five ordered Si T sites and one ordered Cd T site was used as the starting model for refinement. 29Si MAS NMR shows five distinct Si T sites for Cs2MgSi5O12 and Rb2MgSi5O12, but six Si T sites for Cs2ZnSi5O12. The refined structures for Cs2MgSi5O12 and Rb2MgSi5O12 were determined with complete T-site ordering, but the refined structure for Cs2ZnSi5O12 was determined with partial disorder of Mg and Si over two of the T sites.

Synthesis of new platinum(II) complexes containing hybrid thioether–pyrazole ligands: Structural analysis by 1H and 13C{1H} NMR spectroscopy and X-ray crystal structures

2007 ◽  
Vol 360 (6) ◽  
pp. 2071-2082 ◽  
Author(s):  
Antonio de Leon ◽  
Josefina Pons ◽  
Jordi García-Antón ◽  
Xavier Solans ◽  
Mercè Font-Bardia ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Crystal Structures ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
X Ray ◽  
Pyrazole Ligands
Sign in / Sign up

Export Citation Format

Share Document