Studies of Technetium Complexes. Part 6. The Preparation, Characterisation, and Electron Spin Resonance Spectra of Salts of Tetrachloro- and Tetrabromo-nitridotechnetate(VI): Crystal Structure of Tetraphenylarsonium Tetrachloronitridotechnetate(VI)

Article abstract of DOI:10.1039/DT9840002395

The air-stable compounds R and R (R=(1+) or n4>(1+)) have been prepared by the reaction of with NaN3 in the presence of concentrated HCl or of HBr.The e.s.r spectra of (1-) and (1-) are typical of ions with a 4d¹ electronic configuration and the unpaired electron in an orbital with substantial 4d_xy character.The crystal structure of has been determined by single crystal X-ray diffraction methods at 21 deg C.Crystals are tetragonal, space group P4/n with a=12.707(2), c=7.793(1) Angstroem, and Z=2.Full-matrix least-squares refinement gave a final R value of 0.031 for 1 079 independent reflections.The compound is isostructural with the series (M= Mo, W, Re, Ru, or Os) and with (M= Mo or Re).The (1-) anion in possesses C_4v symmetry with Cl-Tc-Cl bond angles of 86.95(1) and 153.33(6) deg and N<*>Tc-Cl bond angles of 103.34(3) deg.The Tc<*>N bond distance is 1.581(5) Angstroem and Tc-Cl distances are 2.3220(9) Angstroem.

Full text of DOI:10.1039/DT9840002395

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