Hydrothermal synthesis and structure of [Ni(tpyrpyz)2] 2[Mo4O12F2][Mo6O 19]·2H2O, a material exhibiting an unusual tetranuclear polyoxofluoromolybdate cluster [Mo4O12F 2]2-

Eric Burkholder; Jon Zubieta

doi:10.1016/S0020-1693(03)00480-8

Hydrothermal synthesis and structure of [Ni(tpyrpyz)₂] ₂[Mo₄O₁₂F₂][Mo₆O ₁₉]·2H₂O, a material exhibiting an unusual tetranuclear polyoxofluoromolybdate cluster [Mo₄O₁₂F ₂]^2-

Eric Burkholder, Jon Zubieta

Department of Chemistry

Research output: Contribution to journal › Article › peer-review

37 Scopus citations

Abstract

The hydrothermal reaction of a solution of Ni(CH₃CO ₂)₂·4H₂O, MoO₃, tetra-4-pyridylpyrazine, H₂O₃PCH₃, and HF at 200 °C for 96 h yields orange crystals of [Ni(tpyrpyz)₂] ₂[Mo₄O₁₂F₂][Mo₆O ₁₇]·2H₂O (1·2H₂O). The structure consists of discrete {Ni(tpyrpyz)₂}²⁺ cations and {Mo ₆O₁₉}^2- and {Mo₄O₁₂F ₂}^2- anionic clusters. The hexamolybdate is the well-documented octahedron of octahedra, that is, six {MoO₆} octahedra in a compact edge-sharing arrangement. The novel oxyfluoride cluster {Mo₄O₁₂F₂}^2- features two {MoO ₄F₂} octahedra, sharing the edge defined by the fluoride ligands; the octahedral Mo sites corner-share to two {MoO₄} tetrahedra in the μ₂-O, O^′ bridging mode.

Original language	English (US)
Pages (from-to)	279-284
Number of pages	6
Journal	Inorganica Chimica Acta
Volume	357
Issue number	1
DOIs	https://doi.org/10.1016/S0020-1693(03)00480-8
State	Published - Jan 9 2004

Keywords

Hydrothermal synthesis
Molybdenum oxides
Oxyfluoromolybdates
Polyoxoanions

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

Access to Document

10.1016/S0020-1693(03)00480-8

Cite this

@article{81cbe475061749cb98cc8dc5a2436467,

title = "Hydrothermal synthesis and structure of [Ni(tpyrpyz)2] 2[Mo4O12F2][Mo6O 19]·2H2O, a material exhibiting an unusual tetranuclear polyoxofluoromolybdate cluster [Mo4O12F 2]2-",

abstract = "The hydrothermal reaction of a solution of Ni(CH3CO 2)2·4H2O, MoO3, tetra-4-pyridylpyrazine, H2O3PCH3, and HF at 200 °C for 96 h yields orange crystals of [Ni(tpyrpyz)2] 2[Mo4O12F2][Mo6O 17]·2H2O (1·2H2O). The structure consists of discrete {Ni(tpyrpyz)2}2+ cations and {Mo 6O19}2- and {Mo4O12F 2}2- anionic clusters. The hexamolybdate is the well-documented octahedron of octahedra, that is, six {MoO6} octahedra in a compact edge-sharing arrangement. The novel oxyfluoride cluster {Mo4O12F2}2- features two {MoO 4F2} octahedra, sharing the edge defined by the fluoride ligands; the octahedral Mo sites corner-share to two {MoO4} tetrahedra in the μ2-O, O′ bridging mode.",

keywords = "Hydrothermal synthesis, Molybdenum oxides, Oxyfluoromolybdates, Polyoxoanions",

author = "Eric Burkholder and Jon Zubieta",

note = "Funding Information: This work was supported by a grant from the National Science Foundation, CHE-0242153. ",

year = "2004",

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doi = "10.1016/S0020-1693(03)00480-8",

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AU - Zubieta, Jon

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N2 - The hydrothermal reaction of a solution of Ni(CH3CO 2)2·4H2O, MoO3, tetra-4-pyridylpyrazine, H2O3PCH3, and HF at 200 °C for 96 h yields orange crystals of [Ni(tpyrpyz)2] 2[Mo4O12F2][Mo6O 17]·2H2O (1·2H2O). The structure consists of discrete {Ni(tpyrpyz)2}2+ cations and {Mo 6O19}2- and {Mo4O12F 2}2- anionic clusters. The hexamolybdate is the well-documented octahedron of octahedra, that is, six {MoO6} octahedra in a compact edge-sharing arrangement. The novel oxyfluoride cluster {Mo4O12F2}2- features two {MoO 4F2} octahedra, sharing the edge defined by the fluoride ligands; the octahedral Mo sites corner-share to two {MoO4} tetrahedra in the μ2-O, O′ bridging mode.

AB - The hydrothermal reaction of a solution of Ni(CH3CO 2)2·4H2O, MoO3, tetra-4-pyridylpyrazine, H2O3PCH3, and HF at 200 °C for 96 h yields orange crystals of [Ni(tpyrpyz)2] 2[Mo4O12F2][Mo6O 17]·2H2O (1·2H2O). The structure consists of discrete {Ni(tpyrpyz)2}2+ cations and {Mo 6O19}2- and {Mo4O12F 2}2- anionic clusters. The hexamolybdate is the well-documented octahedron of octahedra, that is, six {MoO6} octahedra in a compact edge-sharing arrangement. The novel oxyfluoride cluster {Mo4O12F2}2- features two {MoO 4F2} octahedra, sharing the edge defined by the fluoride ligands; the octahedral Mo sites corner-share to two {MoO4} tetrahedra in the μ2-O, O′ bridging mode.

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