The NMR study of inversion at the metal centre and ligand exchange processes of HgII bis-chelates: X-ray crystal structure of [pyr(NC6H11-c)S]2Hg

Polyhedron ◽  
1989 ◽  
Vol 8 (5) ◽  
pp. 569-575 ◽  
Author(s):  
A.L. Nivorozhkin ◽  
E.V. Sukholenko ◽  
L.E. Nivorozhkin ◽  
N.I. Borisenko ◽  
V.I. Minkin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ligand Exchange ◽  
Metal Centre ◽  
X Ray ◽  
Nmr Study ◽  
Exchange Processes

Synthesis, X-ray crystal structure, and solid-state 13C NMR study of tris(9-crown-3)triphenylene

2001 ◽  
Vol 79 (2) ◽  
pp. 195-200 ◽  
Author(s):  
Gerald W Buchanan ◽  
Majid F Rastegar ◽  
Glenn PA Yap
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crown Ether ◽  
Chemical Shifts ◽  
Aromatic Rings ◽  
X Ray ◽  
Nmr Study ◽  
Group A ◽  
C Nmr ◽  
Solid State 13C Nmr

Benzo-9-crown-3 ether trimerizes in the presence of FeCl3 and aqueous H2SO4 to produce tris(9-crown-3)triphenylene in 25.4% yield. This compound crystallizes in the monoclinic P21/c space group: a = 13.759(2) Å, b = 13.318(2) Å, c = 13.399(2) Å, β = 96.883(2)°, with Z = 4. The three 9-crown-3 ether units of the trimer possess different geometries and there is substantial deviation from coplanarity in the three aromatic rings. 13C NMR chemical shifts in the solid state are consistent with this lack of symmetry and are discussed in terms of the X-ray crystal-structure data.Key words: crown ether, trimerization, stereochemistry.

Synthesis, NMR Study, and Reactivity of Isomeric Early−Late Heterobimetallic Dihydrides. X-ray Crystal Structure of (PPh3)HRu(μ-H)(μ-PMe2C5Me4)2(μ-Cl)ZrCl

1996 ◽  
Vol 35 (25) ◽  
pp. 7316-7324 ◽  
Author(s):  
Vladimir I. Bakhmutov ◽  
Marc Visseaux ◽  
Denise Baudry ◽  
Alain Dormond ◽  
Philippe Richard
Keyword(s):  
Crystal Structure ◽  
X Ray ◽  
Nmr Study ◽  
Early Late

Metal polypyrazolylborates XIII. Solution and solid state NMR study of cyano—mercury(II) polypyrazolylborates. X-ray crystal structure of [HB(3,5-Me2pz)3]HgCN

1997 ◽  
Vol 539 (1-2) ◽  
pp. 9-17 ◽  
Author(s):  
Giancarlo Gioia Lobbia ◽  
Patrizio Cecchi ◽  
Roberto Gobetto ◽  
Giuseppe Digilio ◽  
Riccardo Spagna ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Solid State Nmr ◽  
X Ray ◽  
Nmr Study

scholarly journals Linear dicoordinate beryllium: a 9Be solid-state NMR study of a discrete zero-valent s-block beryllium complex

2018 ◽  
Vol 96 (7) ◽  
pp. 646-652 ◽  
Author(s):  
C. Leroy ◽  
J.K. Schuster ◽  
T. Schaefer ◽  
K. Müller-Buschbaum ◽  
H. Braunschweig ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Chemical Shift Tensor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Quadrupolar Coupling ◽  
Nmr Study ◽  
Tensor Data

Beryllium-9 (9Be) quadrupolar coupling and chemical shift tensor data are reported for bis(1-(2,6-diisopropylphenyl)-3,3,5,5-tetramethylpyrrolidine-2-ylidene)beryllium (Be(CAAC)2). These are the first such data for beryllium in a linear dicoordinate environment. The 9Be quadrupolar coupling constant, 2.36(0.02) MHz, is the largest recorded in the solid state to date for this isotope. The span of the beryllium chemical shift tensor, 22(2) ppm, covers about half of the known 9Be chemical shift range, and the isotropic 9Be chemical shift, 32.0(0.3) ppm, is the largest reported in the solid state to our knowledge. DFT calculations reproduce the experimental data well. A natural localized molecular orbital approach has been used to explain the origins and orientation of the beryllium electric field gradient tensor. The single-crystal X-ray structure of a second polymorph of Be(CAAC)2 is also reported. Inspection of the powder X-ray diffraction data shows that the new crystal structure is part of the bulk product next to another crystalline phase. Therefore, experimental X-ray powder data for the microcrystalline powder sample and the SSNMR data do not fully match either the originally reported crystal structure (Arrowsmith et al. Nat. Chem. 2016, 8, 890–894) or the new polymorph. The ability of solid-state NMR and powder X-ray diffraction to characterize powdered samples was thus particularly useful in this work.

High-field NMR study of vertex rotation in (C5HnMe5-n)MCo2(CO)8CR clusters (M = molybdenum, tungsten): x-ray crystal structure of (C5Me5)MoCo2(CO)8CCO2-iso-Pr

1991 ◽  
Vol 10 (7) ◽  
pp. 2362-2370 ◽  
Author(s):  
Karen A. Sutin ◽  
Lijuan. Li ◽  
Christopher S. Frampton ◽  
Brian G. Sayer ◽  
Michael J. McGlinchey
Keyword(s):  
Crystal Structure ◽  
High Field ◽  
X Ray ◽  
Nmr Study

Metal Tetrahydroborates and Tetrahydroborato Metalates, 15 [1]. An 11B and 113Cd NMR Study of MBH4–CdCl2 Systems in Dimethylformamide and the X-Ray Structure of CdCl2 · 2 DMF

1990 ◽  
Vol 45 (11) ◽  
pp. 1463-1471 ◽  
Author(s):  
Gerald Linti ◽  
Heinrich Nöth ◽  
Martina Thomann
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Coordination Polymer ◽  
Ambient Temperature ◽  
Nmr Spectra ◽  
Carbonyl Oxygen ◽  
X Ray ◽  
Rapid Exchange ◽  
Nmr Study ◽  
In Cis

CdCl2 dissociates in dimethylformamide into the species Cd(DMF)62+, CdCl(DMF)5+ and CdCl3- as determined by 113Cd NMR spectroscopy. 11B and 113Cd NMR spectra of MBH4/CdCl2 solutions in this solvent show the presence of complexes [CdCl2-n(BH4)n+1]- with rapid exchange of BH4- and Cl- at ambient temperature. There is no evidence that Cd(BH4)2 is formed in a metathetical reaction.The crystal structure of CdCl2 · 2 DMF has been determined. It is a coordination polymer containing hexacoordinated Cd atoms with the DMF molecules in cis-position. Coordination of DMF occurs via the carbonyl oxygen atoms.

Manganese(II) complexes derived from acyclic ligands having flexible alcohol arms: structural chracterization and SOD and catalase mimetic studies

2021 ◽  
Vol 77 (2) ◽  
pp. 100-110
Author(s):  
Vickie McKee ◽  
Muhammet Kose
Keyword(s):  
Crystal Structure ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Sod Activity ◽  
Potential Donor ◽  
X Ray ◽  
Flexible Ligands ◽  
Chloride Monohydrate ◽  
Acyclic Ligands

In this work, a series of seven MnII complexes of noncyclic flexible ligands derived from 2,6-diformylpyridine and ethanolamine or alkyl-substituted ethanolamines were prepared and characterized, six structurally by single-crystal X-ray diffraction studies. The complexes are dichlorido{2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]diethanol}manganese(II), [MnCl2(C11H15N3O2)] or [MnCl2(L1)], (2), bis{μ-2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]diethanol}bis[dithiocyanatomanganese(II)], [Mn2(NCS)4(C11H15N3O2)2] or [Mn2(NCS)4(L1)2], (3), chlorido{1,1′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-2-ol)}manganese(II) chloride monohydrate, [MnCl(C13H19N3O2)(H2O)]Cl·H2O or [MnCl(L2)(H2O)]Cl·H2O, (4), {1,1′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-2-ol)}dithiocyanatomanganese(II), [Mn(NCS)2(C13H19N3O2)] or [Mn(NCS)2(L2)], (5), aquadichlorido{2,2′-dimethyl-2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-1-ol)}manganese(II) 0.3-hydrate, [MnCl2(C15H23N3O2)(H2O)]·0.3H2O or [MnCl2(L3)(H2O)]·0.3H2O, (6), (dimethylformamide){2,2′-dimethyl-2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(propan-1-ol)}dithiocyanatomanganese(II), [Mn(NCS)2(C15H23N3O2)(C3H7NO)] or [Mn(NCS)2(L3)(DMF)], (7), and (dimethylformamide){2,2′-[(pyridine-2,6-diyl)bis(nitrilomethanylylidene)]bis(butan-1-ol)}dithiocyanatomanganese(II) dimethylformamide monosolvate, [Mn(NCS)2(C15H23N3O2)(C3H7NO)]·C3H7NO or [Mn(NCS)2(L4)(DMF)]·DMF, (8). The crystal structure of ligand L1 is also reported, but that of (5) is not. All four ligands (L1–L4) have five potential donor atoms in an N3O2 donor set, i.e. three N (pyridine/diimine donors) and two alcohol O atoms, to coordinate the MnII centre. The N3O2 donor set coordinates to the metal centre in a pentagonal planar arrangement; seven-coordinated MnII complexes were obtained via coordination of two auxiliary ligands (anions or water molecules) at the axial positions. However, in some cases, the alcohol O-atom donors remain uncoordinated, resulting in five- or six-coordinated MnII complexes. The structurally characterized complexes were tested for their catalytic scavenging of superoxide and peroxide. The results indicated that the complexes with coordinated exogenous water or chloride ligands showed higher SOD activity than those with exogenous thiocyanate ligands.

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