Reactions of polyoxomolybdates with oximes. The crystal and molecular               structures of...

Shuncheng Liu; Huizhe Zhu; Jon Zubieta

doi:10.1016/S0277-5387(89)80013-0

Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of...

Shuncheng Liu, Huizhe Zhu, Jon Zubieta

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Abstract

Title full: Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of [(C₄H₉)₄N]₂[Mo₂O ₅C₆H₄(O)CHNO₂] · CH₂Cl₂ and [(C₄H₉)₄N]₂[Mo₂O ₅C₆H₅CH(O)C(NO)C₆H₅₂]. The reactions of [(C₄H₉)₄N]₂[Mo₂O ₇] with the oximes benzoinoxime and salicylaldoxime yielded the complexes [(C₄H₉)₄N]₂[Mo₂O ₅C₆H₄(O)CHNO₂] · CH₂CI₂(7) and [(C₄H₉)₄N]₂[Mo₂O ₅C₆H₅CH(O)C(NO)C₆H_{5 2}] (8). The structures of 7 and 8 exhibit the [Mo₂O₅]₂₊ core with the oximato moieties of the ligands functioning as μ₂-O,N bridging donors. The metrical parameters are consistent with the sp² hybridization of the oximato nitrogen with double bond character localized on the C{single bond}N bond. Crystal data: Compound 7, monoclinic space group, P2₁/c, a = 16.271(6), b = 14.010(4), c = 25.390(8) Å, β = 101.34(2)°, V = 5672.9(19) Å³, D_calc = 1.30 g cm^-3 for Z = 4. Structure solution and refinement based on 4718 reflections with F_o ≥ 6σ(F_o)(Mo-K_α, λ = 0.71073 Å) converged at a conventional residual of 0.064. Compound 8, rhombohedral space group (hexagonal setting) R over(3, -), a = b = 47.188(14), c = 15.766(3) Å, V = 30403.4(27) Å³, D_calc = 1.19 g cm^-3 for Z = 18. Structure solution and refinement based on 3015 reflections with F_o ≥ 6σ(F_o) converged at a value of 0.069 for the conventional R factor. Reaction of the related salicylhydroxamic acid with [(C₄H₉)₄N]₂[Mo₂O ₇] in methanol yielded the complex [(C₄H₉)₄N][MoO₂C₆ H₄(OH)C(O)NOC₆H₄(OH)C(O)NHO] (11), a species exhibiting both hydroximato(2-) and hydroxamato(1-) forms of the ligand. Crystal data: Compound 11, monoclinic space group P2₁/c, a = 10.261(2), b = 17.864(4), c = 18.270(3) Å, β = 91.98(1)°, V = 3347.0(10) Å³, D_calc = 1.34 g cm^-3 for Z = 4. Structure solution and refinement based on 3406 reflections converged at a value of 0.049 for the conventional R factor.

Original language	English (US)
Pages (from-to)	2473-2480
Number of pages	8
Journal	Polyhedron
Volume	8
Issue number	20
DOIs	https://doi.org/10.1016/S0277-5387(89)80013-0
State	Published - 1989
Externally published	Yes

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Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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Liu, S., Zhu, H., & Zubieta, J. (1989). Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of... Polyhedron, 8(20), 2473-2480. https://doi.org/10.1016/S0277-5387(89)80013-0

@article{d16051d1103649e0a84793ee16b1efdb,

title = "Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of...",

abstract = "Title full: Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2Cl2 and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H 52]. The reactions of [(C4H9)4N]2[Mo2O 7] with the oximes benzoinoxime and salicylaldoxime yielded the complexes [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2CI2(7) and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H5 2] (8). The structures of 7 and 8 exhibit the [Mo2O5]2+ core with the oximato moieties of the ligands functioning as μ2-O,N bridging donors. The metrical parameters are consistent with the sp2 hybridization of the oximato nitrogen with double bond character localized on the C{single bond}N bond. Crystal data: Compound 7, monoclinic space group, P21/c, a = 16.271(6), b = 14.010(4), c = 25.390(8) {\AA}, β = 101.34(2)°, V = 5672.9(19) {\AA}3, Dcalc = 1.30 g cm-3 for Z = 4. Structure solution and refinement based on 4718 reflections with Fo ≥ 6σ(Fo)(Mo-Kα, λ = 0.71073 {\AA}) converged at a conventional residual of 0.064. Compound 8, rhombohedral space group (hexagonal setting) R over(3, -), a = b = 47.188(14), c = 15.766(3) {\AA}, V = 30403.4(27) {\AA}3, Dcalc = 1.19 g cm-3 for Z = 18. Structure solution and refinement based on 3015 reflections with Fo ≥ 6σ(Fo) converged at a value of 0.069 for the conventional R factor. Reaction of the related salicylhydroxamic acid with [(C4H9)4N]2[Mo2O 7] in methanol yielded the complex [(C4H9)4N][MoO2C6 H4(OH)C(O)NOC6H4(OH)C(O)NHO] (11), a species exhibiting both hydroximato(2-) and hydroxamato(1-) forms of the ligand. Crystal data: Compound 11, monoclinic space group P21/c, a = 10.261(2), b = 17.864(4), c = 18.270(3) {\AA}, β = 91.98(1)°, V = 3347.0(10) {\AA}3, Dcalc = 1.34 g cm-3 for Z = 4. Structure solution and refinement based on 3406 reflections converged at a value of 0.049 for the conventional R factor.",

author = "Shuncheng Liu and Huizhe Zhu and Jon Zubieta",

year = "1989",

doi = "10.1016/S0277-5387(89)80013-0",

language = "English (US)",

volume = "8",

pages = "2473--2480",

journal = "Polyhedron",

issn = "0277-5387",

publisher = "Elsevier",

number = "20",

}

TY - JOUR

T1 - Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of...

AU - Liu, Shuncheng

AU - Zhu, Huizhe

AU - Zubieta, Jon

PY - 1989

Y1 - 1989

N2 - Title full: Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2Cl2 and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H 52]. The reactions of [(C4H9)4N]2[Mo2O 7] with the oximes benzoinoxime and salicylaldoxime yielded the complexes [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2CI2(7) and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H5 2] (8). The structures of 7 and 8 exhibit the [Mo2O5]2+ core with the oximato moieties of the ligands functioning as μ2-O,N bridging donors. The metrical parameters are consistent with the sp2 hybridization of the oximato nitrogen with double bond character localized on the C{single bond}N bond. Crystal data: Compound 7, monoclinic space group, P21/c, a = 16.271(6), b = 14.010(4), c = 25.390(8) Å, β = 101.34(2)°, V = 5672.9(19) Å3, Dcalc = 1.30 g cm-3 for Z = 4. Structure solution and refinement based on 4718 reflections with Fo ≥ 6σ(Fo)(Mo-Kα, λ = 0.71073 Å) converged at a conventional residual of 0.064. Compound 8, rhombohedral space group (hexagonal setting) R over(3, -), a = b = 47.188(14), c = 15.766(3) Å, V = 30403.4(27) Å3, Dcalc = 1.19 g cm-3 for Z = 18. Structure solution and refinement based on 3015 reflections with Fo ≥ 6σ(Fo) converged at a value of 0.069 for the conventional R factor. Reaction of the related salicylhydroxamic acid with [(C4H9)4N]2[Mo2O 7] in methanol yielded the complex [(C4H9)4N][MoO2C6 H4(OH)C(O)NOC6H4(OH)C(O)NHO] (11), a species exhibiting both hydroximato(2-) and hydroxamato(1-) forms of the ligand. Crystal data: Compound 11, monoclinic space group P21/c, a = 10.261(2), b = 17.864(4), c = 18.270(3) Å, β = 91.98(1)°, V = 3347.0(10) Å3, Dcalc = 1.34 g cm-3 for Z = 4. Structure solution and refinement based on 3406 reflections converged at a value of 0.049 for the conventional R factor.

AB - Title full: Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2Cl2 and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H 52]. The reactions of [(C4H9)4N]2[Mo2O 7] with the oximes benzoinoxime and salicylaldoxime yielded the complexes [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2CI2(7) and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H5 2] (8). The structures of 7 and 8 exhibit the [Mo2O5]2+ core with the oximato moieties of the ligands functioning as μ2-O,N bridging donors. The metrical parameters are consistent with the sp2 hybridization of the oximato nitrogen with double bond character localized on the C{single bond}N bond. Crystal data: Compound 7, monoclinic space group, P21/c, a = 16.271(6), b = 14.010(4), c = 25.390(8) Å, β = 101.34(2)°, V = 5672.9(19) Å3, Dcalc = 1.30 g cm-3 for Z = 4. Structure solution and refinement based on 4718 reflections with Fo ≥ 6σ(Fo)(Mo-Kα, λ = 0.71073 Å) converged at a conventional residual of 0.064. Compound 8, rhombohedral space group (hexagonal setting) R over(3, -), a = b = 47.188(14), c = 15.766(3) Å, V = 30403.4(27) Å3, Dcalc = 1.19 g cm-3 for Z = 18. Structure solution and refinement based on 3015 reflections with Fo ≥ 6σ(Fo) converged at a value of 0.069 for the conventional R factor. Reaction of the related salicylhydroxamic acid with [(C4H9)4N]2[Mo2O 7] in methanol yielded the complex [(C4H9)4N][MoO2C6 H4(OH)C(O)NOC6H4(OH)C(O)NHO] (11), a species exhibiting both hydroximato(2-) and hydroxamato(1-) forms of the ligand. Crystal data: Compound 11, monoclinic space group P21/c, a = 10.261(2), b = 17.864(4), c = 18.270(3) Å, β = 91.98(1)°, V = 3347.0(10) Å3, Dcalc = 1.34 g cm-3 for Z = 4. Structure solution and refinement based on 3406 reflections converged at a value of 0.049 for the conventional R factor.

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