Synthesis and Structures of the Capped and Sandwiched Cobalt Heptamolybdate Polyoxometalate (NH4)6{[Co(H2O)5][Mo7O24][Co(H2O)2][Mo7O24][Co(H2O)5]} · 6 H2O and Its Extended Structure (NH4)6{[Co(H2O)2]3[Mo7O24]2}

Matthieu R. Spriet; Matthew J. Polinski; Brandon Q. Mercado; Eric M. Villa

doi:10.3390/cryst12091201

Synthesis and Structures of the Capped and Sandwiched Cobalt Heptamolybdate Polyoxometalate (NH₄)₆{[Co(H₂O)₅][Mo₇O₂₄][Co(H₂O)₂][Mo₇O₂₄][Co(H₂O)₅]} · 6 H₂O and Its Extended Structure (NH₄)₆{[Co(H₂O)₂]₃[Mo₇O₂₄]₂}

Matthieu R. Spriet, Matthew J. Polinski, Brandon Q. Mercado, Eric M. Villa

Department of Chemistry

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

Abstract

Two polyoxometalate-based compounds containing the heptamolybdate anion and cobalt(II) have been synthesized, structurally characterized via single-crystal X-ray diffraction and spectroscopically analyzed with solid-state UV–Vis–NIR. The first crystal structure presented is a capped- and sandwich-style polyoxometalate (NH₄)₆{[Co(H₂O)₅][Mo₇O₂₄] [Co(H₂O)₂][Mo₇O₂₄][Co(H₂O)₅]} · 6 H₂O (Co₃Mo₁₄-POM). This orange product crystallizes in the P-1 space group and has an interesting structure for polyoxometalates (POMs). Here, the cobalt(II) groups are functioning both as a bridge between two heptamolybdate units and also capping units at the top and the bottom of the polyoxometalate. The second structure, another product within the same reaction, is constructed on a similar bonding motif but now forms an extended structure: (NH₄)₆{[Co(H₂O)₂]₃[Mo₇O₂₄]₂} (Co₃Mo₁₄-ES). This compound also crystallizes in the space group P-1 but is easily separated due to its much darker red-violet color. These structures present themselves as a noteworthy compounds within POM-based crystal structures. Herein, the syntheses, crystal structures and characterization of these compounds are presented.

Original language	English (US)
Article number	1201
Journal	Crystals
Volume	12
Issue number	9
DOIs	https://doi.org/10.3390/cryst12091201
State	Published - Sep 2022

All Science Journal Classification (ASJC) codes

Chemical Engineering(all)
Materials Science(all)
Condensed Matter Physics
Inorganic Chemistry

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10.3390/cryst12091201

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Synthesis and Structures of the Capped and Sandwiched Cobalt Heptamolybdate Polyoxometalate (NH₄)₆{[Co(H₂O)₅][Mo₇O₂₄][Co(H₂O)₂][Mo₇O₂₄][Co(H₂O)₅]} · 6 H₂O and Its Extended Structure (NH₄)₆{[Co(H₂O)₂]₃[Mo₇O₂₄]₂}. / Spriet, Matthieu R.; Polinski, Matthew J.; Mercado, Brandon Q. et al.

In: Crystals, Vol. 12, No. 9, 1201, 09.2022.

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

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title = "Synthesis and Structures of the Capped and Sandwiched Cobalt Heptamolybdate Polyoxometalate (NH4)6{[Co(H2O)5][Mo7O24][Co(H2O)2][Mo7O24][Co(H2O)5]} · 6 H2O and Its Extended Structure (NH4)6{[Co(H2O)2]3[Mo7O24]2}",

abstract = "Two polyoxometalate-based compounds containing the heptamolybdate anion and cobalt(II) have been synthesized, structurally characterized via single-crystal X-ray diffraction and spectroscopically analyzed with solid-state UV–Vis–NIR. The first crystal structure presented is a capped- and sandwich-style polyoxometalate (NH4)6{[Co(H2O)5][Mo7O24] [Co(H2O)2][Mo7O24][Co(H2O)5]} · 6 H2O (Co3Mo14-POM). This orange product crystallizes in the P-1 space group and has an interesting structure for polyoxometalates (POMs). Here, the cobalt(II) groups are functioning both as a bridge between two heptamolybdate units and also capping units at the top and the bottom of the polyoxometalate. The second structure, another product within the same reaction, is constructed on a similar bonding motif but now forms an extended structure: (NH4)6{[Co(H2O)2]3[Mo7O24]2} (Co3Mo14-ES). This compound also crystallizes in the space group P-1 but is easily separated due to its much darker red-violet color. These structures present themselves as a noteworthy compounds within POM-based crystal structures. Herein, the syntheses, crystal structures and characterization of these compounds are presented.",

author = "Spriet, {Matthieu R.} and Polinski, {Matthew J.} and Mercado, {Brandon Q.} and Villa, {Eric M.}",

note = "Funding Information: The SEM-EDX was acquired through a Nebraska EPSCoR MRI award to Joel Destino (Creighton) and was wholly funded by Nebraska EPSCoR. The authors would like to thank Creighton University and the Creighton University Chemistry Department for continuing to support undergraduate research. Funding Information: This research was initially supported by Creighton University{\textquoteright}s Summer Faculty Research Fund from the Center for Undergraduate Research and Scholarship (Summer 2016) and then funded by Nebraska EPSCoR First Award (EPS-1004094; January–September 2016). Publisher Copyright: {\textcopyright} 2022 by the authors.",

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AU - Mercado, Brandon Q.

AU - Villa, Eric M.

N1 - Funding Information: The SEM-EDX was acquired through a Nebraska EPSCoR MRI award to Joel Destino (Creighton) and was wholly funded by Nebraska EPSCoR. The authors would like to thank Creighton University and the Creighton University Chemistry Department for continuing to support undergraduate research. Funding Information: This research was initially supported by Creighton University’s Summer Faculty Research Fund from the Center for Undergraduate Research and Scholarship (Summer 2016) and then funded by Nebraska EPSCoR First Award (EPS-1004094; January–September 2016). Publisher Copyright: © 2022 by the authors.

PY - 2022/9

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N2 - Two polyoxometalate-based compounds containing the heptamolybdate anion and cobalt(II) have been synthesized, structurally characterized via single-crystal X-ray diffraction and spectroscopically analyzed with solid-state UV–Vis–NIR. The first crystal structure presented is a capped- and sandwich-style polyoxometalate (NH4)6{[Co(H2O)5][Mo7O24] [Co(H2O)2][Mo7O24][Co(H2O)5]} · 6 H2O (Co3Mo14-POM). This orange product crystallizes in the P-1 space group and has an interesting structure for polyoxometalates (POMs). Here, the cobalt(II) groups are functioning both as a bridge between two heptamolybdate units and also capping units at the top and the bottom of the polyoxometalate. The second structure, another product within the same reaction, is constructed on a similar bonding motif but now forms an extended structure: (NH4)6{[Co(H2O)2]3[Mo7O24]2} (Co3Mo14-ES). This compound also crystallizes in the space group P-1 but is easily separated due to its much darker red-violet color. These structures present themselves as a noteworthy compounds within POM-based crystal structures. Herein, the syntheses, crystal structures and characterization of these compounds are presented.

AB - Two polyoxometalate-based compounds containing the heptamolybdate anion and cobalt(II) have been synthesized, structurally characterized via single-crystal X-ray diffraction and spectroscopically analyzed with solid-state UV–Vis–NIR. The first crystal structure presented is a capped- and sandwich-style polyoxometalate (NH4)6{[Co(H2O)5][Mo7O24] [Co(H2O)2][Mo7O24][Co(H2O)5]} · 6 H2O (Co3Mo14-POM). This orange product crystallizes in the P-1 space group and has an interesting structure for polyoxometalates (POMs). Here, the cobalt(II) groups are functioning both as a bridge between two heptamolybdate units and also capping units at the top and the bottom of the polyoxometalate. The second structure, another product within the same reaction, is constructed on a similar bonding motif but now forms an extended structure: (NH4)6{[Co(H2O)2]3[Mo7O24]2} (Co3Mo14-ES). This compound also crystallizes in the space group P-1 but is easily separated due to its much darker red-violet color. These structures present themselves as a noteworthy compounds within POM-based crystal structures. Herein, the syntheses, crystal structures and characterization of these compounds are presented.

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