119818-97-2Relevant academic research and scientific papers
Synthesis and characterization of technetium(III) complexes containing 2,2′-bipyridine and 1,10-phenanthroline. X-ray crystal structures of cis(Cl),trans(P)-[TcCl2(P(CH3)2C 6H5)2(bpy)]B(C6H5) 4, cis(Cl),trans(P)-[TcCl2(P(CH3)2C ...
Wilcox, Bruce E.,Ho, Douglas M.,Deutsch, Edward
, p. 1743 - 1751 (2008/10/08)
Full title: Synthesis and characterization of technetium(III) complexes containing 2,2′-bipyridine and 1,10-phenanthroline. X-ray crystal structures of cis(Cl),trans(P)-[TcCl2(P(CH3)2C 6H5)2(bpy)]B(C6H5) 4, cis(Cl),trans(P)-[TcCl2(P(CH3)2C 6H5)2(phen)]B(C6H5) 4, and cis(Cl),trans(P)-[TcCl2(P(CH3CH2)(C 6H5)2)2(bpy)]SO3CF 3. Technetium(III) complexes of the general formula cis(Cl),trans(P)-[TcCl2(P)2L]+, where (P) is dimethylphenylphosphine (PMe2Ph) or ethyldiphenylphosphine (PEtPh2) and L is 2,2′-bipyridine (bpy), 4,4′-dimethyl-2,2′-bipyridine (Me2bpy), or 1,10-phenanthroline (phen), have been synthesized and characterized. They are prepared by L substitution onto, with concomitant displacement of one chloride and one phosphine ligand from, the mer-TcCl3(P)3 starting material in refluxing ethanol. Analysis of these complexes by fast atom bombardment mass spectrometry (in the positive ion mode) provides "fingerprint" mass spectra that exhibit peaks assigned to the molecular ion M+ as well as peaks assigned to M+ minus one or more monodentate ligands. Single-crystal X-ray structure determinations of cis(Cl),trans(P)-[TcCl2(PMe2Ph)2(bpy)]BPh 4 (A), cis(Cl),trans(P)-[TcCl2-(PMe2Ph) 2(phen)]BPh4 (B), and cis(Cl),trans(P)-[TcCl2(PEtPh2)2(bpy)]SO 3CF3 (C), with formula weights of 921.62, 945.64, and 903.65, respectively, show that the technetium atoms reside in slightly distorted octahedral environments. Complex A crystallizes in the triclinic space group P1, with a = 10.700 (2) ?, b = 14.231 (2) ?, c = 16.018 (2) ?, α = 95.80 (1)°, β = 97.58 (1)°, γ = 108.34 (1)°, and V = 2268.5 (6) ?3, with Z = 2 for 3104 observed reflections with F > 6σ(F). Complex B crystallizes in the triclinic space group P1 with a = 10.668 (2) ?, b = 14.064 (2) ?, c = 16.529 (2) ?, α = 95.50 (1)°, β = 97.61 (1)°, γ = 108.67 (1)°, and V = 2309.3 (7) ?3, with Z = 2 for 4975 observed reflections with F> 3σ(F). Complex C crystallizes in the orthorhombic space group P212121 with a = 16.399 (2) ?, b = 21.869 (5) ?, c = 11.102 (2) ?, and V = 3982 (1) ?3, with Z = 4 for 3585 observed reflections with F > 6σ(F).
