Structural determination and characterization of copper and zinc bis-glycinates with X-ray crystallography and mass spectrometry

2010 ◽  
Vol 63 (19) ◽  
pp. 3335-3347 ◽  
Author(s):  
Sanjit Konar ◽  
Kevin Gagnon ◽  
Abraham Clearfield ◽  
Charles Thompson ◽  
Jennifer Hartle ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Copper And Zinc

scholarly journals Characterization of reactive organometallic species via MicroED

2019 ◽  
Author(s):  
Christopher Jones ◽  
Matthew Asay ◽  
Lee Joon Kim ◽  
Jack Kleinsasser ◽  
Ambarneil Saha ◽  
...  
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Cryogenic Cooling ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diamagnetic Transition

Here we apply microcrystal electron diffraction (MicroED) to the structural determination of transition metal complexes. We find that the simultaneous use of 300 keV electrons, very low electron doses, and an ultra-sensitive camera allows for the collection of data without cryogenic cooling of the stage. This technique reveals the first crystal structures of the classic zirconocene hydride, colloquially known as “Schwartz’s reagent”, a novel Pd(II) complex not amenable to solution-state NMR or X-ray crystallography, and five other paramagnetic or diamagnetic transition metal complexes.

scholarly journals Characterization of reactive organometallic species via MicroED

2019 ◽  
Author(s):  
Christopher Jones ◽  
Matthew Asay ◽  
Lee Joon Kim ◽  
Jack Kleinsasser ◽  
Ambarneil Saha ◽  
...  
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Cryogenic Cooling ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diamagnetic Transition

Here we apply microcrystal electron diffraction (MicroED) to the structural determination of transition metal complexes. We find that the simultaneous use of 300 keV electrons, very low electron doses, and an ultra-sensitive camera allows for the collection of data without cryogenic cooling of the stage. This technique reveals the first crystal structures of the classic zirconocene hydride, colloquially known as “Schwartz’s reagent”, a novel Pd(II) complex not amenable to solution-state NMR or X-ray crystallography, and five other paramagnetic or diamagnetic transition metal complexes.

scholarly journals Characterization of reactive organometallic species via MicroED

2019 ◽  
Author(s):  
Christopher Jones ◽  
Matthew Asay ◽  
Lee Joon Kim ◽  
Jack Kleinsasser ◽  
Ambarneil Saha ◽  
...  
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Cryogenic Cooling ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diamagnetic Transition

Here we apply microcrystal electron diffraction (MicroED) to the structural determination of transition metal complexes. We find that the simultaneous use of 300 keV electrons, very low electron doses, and an ultra-sensitive camera allows for the collection of data without cryogenic cooling of the stage. This technique reveals the first crystal structures of the classic zirconocene hydride, colloquially known as “Schwartz’s reagent”, a novel Pd(II) complex not amenable to solution-state NMR or X-ray crystallography, and five other paramagnetic or diamagnetic transition metal complexes.

A twist on Hellwinkel’s salt, [P(2,2′-biphenyl)2]+[P(2,2′-biphenyl)3]–

2018 ◽  
Vol 96 (6) ◽  
pp. 526-533 ◽  
Author(s):  
Khatera Hazin ◽  
Derek P. Gates
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Spiro Compound ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Isolation And Characterization

Treating PCl5 with C12H8Li2, generated from either C12H10, C12H8Br2, or C12H8I2, affords three products in different ratios depending on the source of the lithiated biphenyl. Hellwinkel’s salt [P(C12H8)2][P(C12H8)3] ([1][2]) and another product [P(C12H8)(C24H16)][P(C12H8)3] ([1′][2]) were obtained by reacting PCl5 with 2,2′-dilithiobiphenyl [Route A: 2.5 equiv.; obtained from biphenyl, n-BuLi, and TMEDA; Route B: 3.0 equiv.; obtained from 2,2′-diiodobiphenyl and n-BuLi; Route C: 4.0 equiv.; obtained from 2,2′-dibromobiphenyl and n-BuLi]. The synthesis, isolation, and characterization of the chiral spiro-compound [1′][2] and the characterization of the pentavalent phosphorane [P(C12H8)2(C12H9)] (3) are reported. The complex [1′][2] was characterized by 31P{1H} NMR spectroscopy, X-ray crystallography, and mass spectrometry. The pentavalent compound (3) was characterized by 31P{1H} NMR spectroscopy and X-ray crystallography.

scholarly journals 4-vinylpyridine derivatives: Protonation, methylation and silver(I) coordination chemistry

2021 ◽  
pp. 174751982198965
Author(s):  
Guoqi Zhang
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Coordination Chemistry ◽  
Elemental Analysis ◽  
Silver Complex ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Moiety ◽  
New Compounds

( E)-4-[2-(Pyridin-4-yl)vinyl]benzaldehyde, containing both a 4-vinylpyridine and an aldehyde functionality, is utilized to develop new, highly conjugated chalcone compounds and a bis-Schiff base azine compound. The chalcone-containing compounds are further explored for their protonation, methylation and silver(I) coordination chemistry using the pyridine moiety. In parallel, a cyano-containing analogue, ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile is also synthesized and studied for its silver(I) coordination chemistry. These new compounds are fully characterized by mass spectrometry, elemental analysis and spectroscopic techniques. The methylated product of ( E)-1-(9-anthryl)-3-{4-[2-(pyridin-4-yl)vinyl]phenyl}prop-2-en-1-one and a silver complex of ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile are structurally determined by X-ray crystallography.

scholarly journals Structural Characterization of Heterodinuclear ZnII-LnIII Complexes (Ln = Pr, Nd) with a Ring-Contracted H2valdien-Derived Schiff Base Ligand

2021 ◽  
Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel
Keyword(s):  
Molecular Structure ◽  
Schiff Base ◽  
Structural Characterization ◽  
Schiff Base Ligand ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Imidazoline Ring

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.

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