Systematic synthesis, solution structural characterization of the square-pyramidal clusters MIr4(CO)7(.mu.-CO)2L(.eta.5-C5Me5)(.mu.4-PPh) (M = Rh, Ir; L = CO, PPh3), and x-ray structural determination of the iridium derivatives

1990 ◽  
Vol 9 (3) ◽  
pp. 645-656 ◽  
Author(s):  
Rajesh Khattar ◽  
Stephen Naylor ◽  
Maria D. Vargas ◽  
Dario Braga ◽  
Fabrizia Grepioni
Keyword(s):  
Structural Characterization ◽  
Structural Determination ◽  
X Ray ◽  
Systematic Synthesis ◽  
Synthesis Solution

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.

Synthesis, chemical, and electrochemical characterization of the [Ag13{?3-Fe(CO)4}] n? (n = 3, 4, 5) cluster anions: X-Ray structural determination of [N(PPh3)2]3 [Ag12(?12-Ag){?3Fe(CO)4}8]1

1995 ◽  
Vol 6 (1) ◽  
pp. 107-123 ◽  
Author(s):  
Vincenzo G. Albano ◽  
Francesca Calderoni ◽  
Maria Carmela Iapalucci ◽  
Giuliano Longoni ◽  
Magda Monari ◽  
...  
Keyword(s):  
Electrochemical Characterization ◽  
Structural Determination ◽  
Cluster Anions ◽  
X Ray

Single Crystal X-Ray Structural Characterization of [BiX2(S2CNEt2)]Infinity∞, X=Cl, Br

1994 ◽  
Vol 47 (2) ◽  
pp. 405 ◽  
Author(s):  
PK Bharadwaj ◽  
AM Lee ◽  
BW Skelton ◽  
BR Srinivasan ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Sulfur Atom ◽  
Structural Characterization ◽  
Structure Determination ◽  
Room Temperature ◽  
X Ray ◽  
Structure Determinations

Single-crystal room-temperature X-ray structure determinations of the title compounds have been carried out. The two compounds are isomorphous, and isomorphous with the previously determined iodide analogue, being monoclinic, P 21/c, a ≈ 10.0, b ≈ 14.9, c ≈ 7.8 Ǻ, β ≈ 92°, Z = 4 formula units; residuals were 0.037, 0.036 for 2197, 1654 'observed' reflections for X = Cl , Br respectively. As in the iodide, the complexes are infinite polymers, with successive bismuth atoms bridged by the two halides and one sulfur atom of the ligand , which also chelates each bismuth. The structure determination of C5H5NCONEt2]2 [Cl5Bi(NC5H5)], isostructural with its thiocarbamoyl analogue, is also recorded.

Lewis-Base Adducts of Lead(II) Compounds. III. Synthesis and Structural Characterization of Mononuclear (Nitrato-O,O′)bis(1,10-phenanthroline)-(thiocyanato-N)lead(II)

1989 ◽  
Vol 42 (2) ◽  
pp. 335 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Lone Pair ◽  
Lewis Base ◽  
Lead Atom ◽  
X Ray

The isolation and single-crystal X-ray structure determination of the title compound, [(phen)2Pb(NCS)(O2NO)] is described; crystals are triclinic, P1, a 15.554(7), b 9-670(4), c 8.429(3) α 72.53(3), β 81.90(3), γ 72.88(3)� Z = 2, yielding R 0.052 for 3405 independent 'observed' reflections. The lead atom is seven-coordinate [Pb-N 2.49(1)-2.60(1) (phen), 2.89(1) (NCS); Pb-O 2.75(1), 2.89(1) �] with a large vacancy in the coordination sphere, possibly indicative of a stereochemically active lone pair.

scholarly journals Glycoscience@Synchrotron: Synchrotron radiation applied to structural glycoscience

2017 ◽  
Vol 13 ◽  
pp. 1145-1167 ◽  
Author(s):  
Serge Pérez ◽  
Daniele de Sanctis
Keyword(s):  
Synchrotron Radiation ◽  
Structural Characterization ◽  
Crystalline State ◽  
Structural Diversity ◽  
Interacting Proteins ◽  
X Ray ◽  
Wide Range ◽  
Kinetics Of

Synchrotron radiation is the most versatile way to explore biological materials in different states: monocrystalline, polycrystalline, solution, colloids and multiscale architectures. Steady improvements in instrumentation have made synchrotrons the most flexible intense X-ray source. The wide range of applications of synchrotron radiation is commensurate with the structural diversity and complexity of the molecules and macromolecules that form the collection of substrates investigated by glycoscience. The present review illustrates how synchrotron-based experiments have contributed to our understanding in the field of structural glycobiology. Structural characterization of protein–carbohydrate interactions of the families of most glycan-interacting proteins (including glycosyl transferases and hydrolases, lectins, antibodies and GAG-binding proteins) are presented. Examples concerned with glycolipids and colloids are also covered as well as some dealing with the structures and multiscale architectures of polysaccharides. Insights into the kinetics of catalytic events observed in the crystalline state are also presented as well as some aspects of structure determination of protein in solution.

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.

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