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The synthesis and characterization of tri- and tetrametaphosphate titanium(IV) oxo and peroxo complexes is described. Addition of 0.5 equiv of [OTi(acac) 2 ] 2 o dihydrogen tetrametaphosphate ([P 4 O 12 H 2 ] 2- ) and monohydrogen trimetaphosphate ([P 3 O 9 H] 2- ) provided a bis(μ 2 ,κ 2 ,κ 2 ) tetrametaphosphate titanyl dimer, [OTiP 4 O 12 ] 2  4- (1; 70% yield), and a trimetaphosphate titanyl acetylacetonate complex, [OTiP 3 O 9 (acac)] 2- (2; 59% yield). Both 1 and 2 have been structurally characterized, crystallizing in the triclinic P1̅ and monoclinic P2 1 space groups, respectively. These complexes contain Ti≡O units with distances of 1.624(7) and 1.644(2) Å, respectively, and represent rare examples of structurally characterized terminal titanyls within an all-oxygen coordination environment. Complexes 1 and 2 react with hydrogen peroxide to produce the corresponding peroxotitanium(IV) metaphosphate complexes [O 2 TiP 4 O 12 ] 2  4- (3; 61% yield) and [O 2 TiP 3 O 9 (acac)] 2- (4; 65% yield), respectively. Both 3 and 4 have been characterized by single-crystal X-ray diffraction studies, and their solid-state structures are presented. Complex 3 functions as an oxygen atom transfer (OAT) reagent capable of oxidizing phosphorus(III) compounds (P(OMe) 3 , PPh 3 ) and SMe 2 at ambient temperature to result in the corresponding organic oxide with regeneration of dimer 1.

Terminal Titanyl Complexes of Tri- and Tetrametaphosphate: Synthesis, Structures, and Reactivity with Hydrogen Peroxide