Technetium(V) and rhenium(V) complexes with N-(2-mercaptophenyl)salicylideneiminate. Crystal structure of chloro(oxo)[N-(2-sulphidophenyl)salicylideneiminato-NOS]technetium(V)

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Abstract
The reactions of the tridentate Schiff-base ligand derived from salicylaldehyde and o-aminothio-phenol (H2L1) with [MOCl4]–(M = Tc or Re) have been investigated. The complexes [MOCl(L1)], [ReOCl2(L1)]–, and [ReOCl(X)(L1)](X = MeOH or EtOH) were synthesized and characterized by elemental analysis, i.r., 1H n.m.r., and u.v.–visible spectroscopy, mass spectrometry, magnetic susceptibility, conductivity, and thermogravimetric measurements and the complete configurations of the complexes were determined. X-Ray crystallographic investigation on [TcOCl(L1)] shows the molecular structure to be a distorted square pyramid having the ligand L1 in the equatorial plane with respect to TcO. The molecule is in the monoclinic space group P21/a, with a= 14.255(9)b= 12.495(7), c= 7.865(6)Å, β= 105.22(5)°, and Z= 4. The structure has been refined to R= 0.068 for 2 184 observed reflections. The reactions of [MOCl(L1)](M = Tc or Re) or [ReOCl(X)(L1)](X = MeOH or EtOH) with the bidentate Schiff-base ligands (HL) salicylideneimine (HL3), N-methylsalicylideneimine (HL4), N-phenylsalicylidene-imine (HL5), N-(2-hydroxyphenyl)-p-nitrobenzylideneimine (HL6), quinolin-8-ol (Hquin), quinoline-8-thiol (Htquin), and N-(2-mercaptophenyl)-p-nitrobenzylideneimine (HL7) lead to the ‘mixed’ compounds [MO(L1)(L)]. The products with L = tquin or L7 were obtained only for [ReOCl(X)(L1)](X = MeOH or EtOH). All these complexes were characterized by the physicochemical techniques listed above.

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