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• W2316042309 abstract "Cobaltocene reduction of LMoVIO2(SPh) complexes yielded extremely dioxygen-sensitive cobaltocenium salts of the cis-dioxo-Mo(V) radical anions cis-[LMoVO2(SPh)]-, while sodium acenaphthalenide reduction of LaMoVIO2(SPh) yielded a complex sodium salt containing [LaMoVO2(SPh)]- [L = hydrotris(3,5-dimethylpyrazol-1-yl)borate (La), hydrotris(3-isopropylpyrazol-1-yl)borate (Lb), or hydrotris(3,5-dimethyl-1,2,4-triazol-1-yl)borate (Lc)]. Crystals of [CoCp2][LcMoVO2(SPh)]·toluene were orthorhombic, space group Pbca, with a = 17.695(3) Å, b = 19.490(3) Å, c = 21.925(4) Å, V = 7561(2) Å3 for Z = 8. The structure, refined using a full-matrix least-squares procedure and 2269 data, converged with R = 0.067 (Rw = 0.067). In the distorted octahedral anion, the metrical parameters of the cis-MoVO2 fragment [Mo−O = 1.742(9) Å, O−Mo−O = 112.1(4)°] are significantly larger than those of LcMoVIO2(SPh) [average Mo−O = 1.700(6) Å, O−Mo−O = 103.9(2)°]. 18O-Substitution of [CoCp2][La,bMoVO2(SPh)] permitted the assignment of bands at ca. 870 and 770 cm-1 to the νs and νas modes, respectively, of the cis-MoVO2 fragment. Freshly prepared solutions of [CoCp2][LMoVO2(SPh)] exhibited a broad EPR signal (g, 1.92; W1/2, 20 G) characteristic of a cis-[MoVO2]+ complex. The signal was stable when L = Lc but when L = La or Lb it was replaced by a proton-coupled signal characteristic of a cis-[MoVO(OH)]2+ center. The complex LaMoVO(OH)(SPh) was isolated as a coprecipitate with its conjugate base salt [CoCp2][LaMoVO2(SPh)]. It was characterized by infrared bands at 915 and 535 cm-1, assigned to ν(MoO) and ν(MoOH) modes, respectively. The anions were readily converted to air-stable LMoVO(OSiMe3)(SPh) upon reaction with Me3SiCl and reacted with dioxygen to regenerate LMoVIO2(SPh). The paper reports the first isolation in substance of compounds containing novel cis-[MoVO2]+ and cis-[MoVO(OH)]2+ centers and the first crystallographic characterization of a cis-dioxo-Mo(V) species." @default.
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• W2316042309 date "1996-01-01" @default.
• W2316042309 modified "2023-10-16" @default.
• W2316042309 title "Complexes Containing <i>cis-</i>[Mo^VO₂]⁺ and <i>cis</i>-[Mo^VO(OH)]²⁺ Centers" @default.
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• W2316042309 doi "https://doi.org/10.1021/ja952525a" @default.
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