Characterization by crystallography

While a number of SbPh3 complexes of copper(I) have been prepared,23 335 356 only [(Ph3Sb)3CuCl]CHCl385 has been characterized by crystallography. 

Irradiation of Tc(CO)3(Cp ) by a low pressure mercury lamp in dry cyclohexane in the absence of air produces two carbonyl-bridged dimers, (Cp )Tc(/t-CO)3Tc(Cp ) which was characterized by crystallography and (Cp )(CO)2Tc(/t-CO)Tc(Cp )(CO)2 whose structure was suggested by spectroscopic comparison with the structurally characterized Re analogue. These two compounds can be separated by colunm chromatography. The IR spectrum of the former compound showed only one carbonyl stretching at 1785 cm and its stmcture is shown in Figure 7. 

As with bipy, a considerable number of chloride complexes have been examined in detail. Compounds characterized by crystallography include [(phen)2La(0H2)5]Cl3 phen 4H20, [(phen)2-La(0H2)5]Cl3-Me0H-H20, [(bipy)2Ln(0H2)4Cl]Cl2-2H20, [(phen)2Lu(0H2)4]Cl3 2H20,... 

A single Au1 complex, [AuL(PPh3)], where L - 2-cyanamidofluoren-9-one, has been synthesized and characterized by crystallography.63... 

A related intramolecular cyclization occurs to give the cyclobutadiene complex 41, which on treatment with lithium gave the dilithium species 42 (Scheme 16). The latter could be isolated and characterized by crystallography <2000CL896>. 

The next step in the catalytic cycle, ionic hydrogenation of ketones from cationic dihydrides, was separately shown to occur under stoichiometric conditions, as shown in Equation 3.17. Alcohol complexes have been synthesized and isolated, and some were characterized by crystallography [43]. Analogous alcohol complexes were observed spectroscopically during the catalytic reaction, so displacement of the alcohol by H2 regenerates the dihydride and completes the catalytic cycle. 

Two new protocols for a-silylation of aldehydes employ copper(I)-catalysed 1,2-additon of nucleophilic silicon to the aldehydes. Starting from an Si-B reagent, activation by copper is achieved either with a sophisticated NHC/CuOBu-t catalyst or with a CuCN/NaOMe system, the latter working well at low temperature. Investigation of both catalysts has been studied kinetically by NMR, and key intermediates have been characterized by crystallography. ... 

Ferritin is a protein that is 17-20% iron, all in the ferric state. It has been characterized by crystallography, ultracentrifugation, and isoelectric and electrophoretic methods, and the molecule has been seen with the aid of the electron microscope. Ferritin is an ellipsoid molecule. The inorganic core is coated by the protein shell. The inorganic component of ferritin can be dissociated from the protein moiety by reduction of the metalloprotein with cysteine, ascorbic acid, or sodium dithionite. 

---