The structures and optoelectronic properties of tricarbonylrhenium(I) complexes of di(2-pyrazolyl-p-tolyl)amine in its neutral and deprotonated (uninegative amido) form were investigated. Reactions of the complexes with Brønsted acids or bases result in distinctive changes of colour and electrochemical activity owing to the non-innocent nature of the ligand.
Two new redox active ligands based on di(2-(3-organopyrazolyl)-p-tolyl)amine have been prepared in order to investigate potential effects of steric bulk on the structures, electronic properties, or reactivity of tricarbonylrhenium(I) complexes. Replacing the hydrogens at the 3-pyrazolyl positions with alkyl groups causes significant distortion to the ligand framework due to potential interactions between these groups when bound to a fac-Re(CO)(3) moiety. The distortions effectively increase the nucleophilic character of the central amino nitrogen and ligand-centered reactivity of the metal complexes.
Tetrathiotetracene crystals belong to space group P1 with a= 9"890, b= 18.226, c= 3.968 A, 0~ = 87 ° 38', fl= 79°44 ', y=96°29 ' and two molecules per cell. The crystal structure has been determined by a threedimensional X-ray diffraction analysis. Intensity data were collected on photographic film and a Stoe diffractometer. The structure was solved from the Patterson functions (001) and (100) with the help of the Fourier technique and packing considerations. Refinement by a full-matrix, least-squares method gave a final R value of 0.13 for 1100 reflexions. The S-S bond length is 2"100 A, and the average S-C distance is 1.781 A. The molecule is nearly planar; only the S atoms are slightly out of the plane (0.021 to 0"056 ,~). The C-C bond lengths are almost the same as those in the tetracene molecule.
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