Synthesis and characterisation of first row transition metal complexes of functionalized 1,2,4-benzothiadiazines

Ewan R. Clark; Muhammad U. Anwar; Bryce J. Leontowicz; Yassine Beldjoudi; John J. Hayward; Wesley T. K. Chan; Emma L. Gavey; Melanie Pilkington; Eli Zysman-Colman; Jeremy M. Rawson

doi:10.1039/C4DT01413H

Synthesis and characterisation of first row transition metal complexes of functionalized 1,2,4-benzothiadiazines†

Ewan R. Clark,*^a Muhammad U. Anwar,^b Bryce J. Leontowicz,^b Yassine Beldjoudi,^b John J. Hayward,^b Wesley T. K. Chan,^c Emma L. Gavey,^d Melanie Pilkington,^d Eli Zysman-Colman^e and Jeremy M. Rawson*^ab

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* Corresponding authors

^a Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK
E-mail: erc@cantab.net

^b Department of Chemistry and Biochemistry, University of Windsor, 401 Sunset Avenue, Windsor, ON, Canada
E-mail: jmrawson@uwindsor.ca

^c Laboratory of X-Ray Crystal Structure Analysis, Department of Applied Biology and Chemical Technology, Hong Kong Polytechnic University, Hung Hom, Kowloon, Hong Kong SAR

^d Department of Chemistry, Brock University, 500 Glenridge Avenue, St Catharines, Ontario, Canada

^e EastChem School of Chemistry, University of St Andrews, North Haugh, St. Andrews, Fife, KY16 9ST UK

Abstract

Reaction of the novel ligand 3-(2′-pyridyl)-benzo-1,2,4-thiadiazine (L) with the transition metal chloride salts MCl₂·xH₂O (M^II = Mn, Fe, Co, Cu and Zn) in a 2 : 1 mole ratio afforded the mononuclear octahedral (high spin) complexes L₂MCl₂ (1a–1e respectively) in which L binds in a chelate fashion via N(2) and the pyridyl N atoms. In the case of CuCl₂ the intermediate 1 : 1 four-coordinate complex LCuCl₂ (2) was also isolated which adopts a polymeric structure with pseudo-square planar molecules linked via long Cu⋯S contacts (d_Cu⋯S = 2.938(1) Å) in the apical position. In the presence of non-interacting ions, 3 : 1 complexes are isolated, exemplified by the reaction of L with Fe(CF₃SO₃)₂ in a 3 : 1 ratio which affords the low spin complex [L₃Fe][CF₃SO₃]₂ (3). Reaction of L with VCl₃ in a 2 : 1 mole ratio under aerobic conditions afforded the vanadyl complex [L₂V( [double bond, length as m-dash] O)Cl][Cl] (4).

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Synthesis and characterisation of first row transition metal complexes of functionalized 1,2,4-benzothiadiazines†

Abstract

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Synthesis and characterisation of first row transition metal complexes of functionalized 1,2,4-benzothiadiazines

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