Synthesis and structure of the two-dimensional bimetallic oxide [H 4tphz]3[{Zn(2)(tphz)(H(2)O) 4}{Mo5O15(O(3)PCH(2)CH 2PO3)}4]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz)

Eric Burkholder; Jon Zubieta

doi:10.1016/j.ica.2003.09.005

Synthesis and structure of the two-dimensional bimetallic oxide [H ₄tphz]₃[{Zn(2)(tphz)(H(2)O) ₄}{Mo₅O₁₅(O(3)PCH(2)CH ₂PO₃)}₄]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz)

Eric Burkholder, Jon Zubieta

Department of Chemistry

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

21 Scopus citations

Abstract

The hydrothermal reaction of (NH₄)₆Mo ₇O₂₄·4H₂O, ZnSO₄·7H₂O, tetra-2-pyridylpyrazine, ethylenediphosphonic acid, H₂O and HF at 170°C for 96 h yields yellow crystals of [H ₄tphz]₃[{Zn₂(tphz)(H₂O) ₄}{Mo₅O₁₅(O₃PCH₂CH ₂PO₃)}₄]·14H₂O (1·14H₂O) (tphz = tetrapyrido[2,3-a:3′,2′-c: 2″,13″-h:3‴,2‴-j]phenazine (tphz)). The structure of 1 consists of two-dimensional networks constructed from chains of {Mo ₅O₁₅(O₃PR)₂}^4- clusters tethered through the ethylene bridges of the diphosphonate ligands, which are in turn crosslinked through the {Zn₂(tphz)(H₂O) ₄}⁴⁺ subunits. This connectivity generates intralamellar cavities which are occupied by the tetraprotonated H₄tphz ⁴⁺ cations. A curious feature of the chemistry is the hydrothermal conversion of the tetra-2-pyridylpyrazine starting material to tphz.

Original language	English (US)
Pages (from-to)	1229-1235
Number of pages	7
Journal	Inorganica Chimica Acta
Volume	357
Issue number	4
DOIs	https://doi.org/10.1016/j.ica.2003.09.005
State	Published - Mar 10 2004

Keywords

Bimetallic oxide
Hydrothermal synthesis
Molybdophosphonate cluster
Network oxide

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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Burkholder, E., & Zubieta, J. (2004). Synthesis and structure of the two-dimensional bimetallic oxide [H ₄tphz]₃[{Zn(2)(tphz)(H(2)O) ₄}{Mo₅O₁₅(O(3)PCH(2)CH ₂PO₃)}₄]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz). Inorganica Chimica Acta, 357(4), 1229-1235. https://doi.org/10.1016/j.ica.2003.09.005

Synthesis and structure of the two-dimensional bimetallic oxide [H ₄tphz]₃[{Zn(2)(tphz)(H(2)O) ₄}{Mo₅O₁₅(O(3)PCH(2)CH ₂PO₃)}₄]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz). / Burkholder, Eric; Zubieta, Jon.
In: Inorganica Chimica Acta, Vol. 357, No. 4, 10.03.2004, p. 1229-1235.

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

Burkholder, E & Zubieta, J 2004, 'Synthesis and structure of the two-dimensional bimetallic oxide [H ₄tphz]₃[{Zn(2)(tphz)(H(2)O) ₄}{Mo₅O₁₅(O(3)PCH(2)CH ₂PO₃)}₄]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz)', Inorganica Chimica Acta, vol. 357, no. 4, pp. 1229-1235. https://doi.org/10.1016/j.ica.2003.09.005

Burkholder E, Zubieta J. Synthesis and structure of the two-dimensional bimetallic oxide [H ₄tphz]₃[{Zn(2)(tphz)(H(2)O) ₄}{Mo₅O₁₅(O(3)PCH(2)CH ₂PO₃)}₄]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz). Inorganica Chimica Acta. 2004 Mar 10;357(4):1229-1235. doi: 10.1016/j.ica.2003.09.005

Burkholder, Eric ; Zubieta, Jon. / Synthesis and structure of the two-dimensional bimetallic oxide [H ₄tphz]₃[{Zn(2)(tphz)(H(2)O) ₄}{Mo₅O₁₅(O(3)PCH(2)CH ₂PO₃)}₄]·14H(2)O : The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz). In: Inorganica Chimica Acta. 2004 ; Vol. 357, No. 4. pp. 1229-1235.

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title = "Synthesis and structure of the two-dimensional bimetallic oxide [H 4tphz]3[{Zn(2)(tphz)(H(2)O) 4}{Mo5O15(O(3)PCH(2)CH 2PO3)}4]·14H(2)O: The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz)",

abstract = "The hydrothermal reaction of (NH4)6Mo 7O24·4H2O, ZnSO4·7H2O, tetra-2-pyridylpyrazine, ethylenediphosphonic acid, H2O and HF at 170°C for 96 h yields yellow crystals of [H 4tphz]3[{Zn2(tphz)(H2O) 4}{Mo5O15(O3PCH2CH 2PO3)}4]·14H2O (1·14H2O) (tphz = tetrapyrido[2,3-a:3′,2′-c: 2″,13″-h:3‴,2‴-j]phenazine (tphz)). The structure of 1 consists of two-dimensional networks constructed from chains of {Mo 5O15(O3PR)2}4- clusters tethered through the ethylene bridges of the diphosphonate ligands, which are in turn crosslinked through the {Zn2(tphz)(H2O) 4}4+ subunits. This connectivity generates intralamellar cavities which are occupied by the tetraprotonated H4tphz 4+ cations. A curious feature of the chemistry is the hydrothermal conversion of the tetra-2-pyridylpyrazine starting material to tphz.",

keywords = "Bimetallic oxide, Hydrothermal synthesis, Molybdophosphonate cluster, Network oxide",

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/j.ica.2003.09.005",

language = "English (US)",

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T1 - Synthesis and structure of the two-dimensional bimetallic oxide [H 4tphz]3[{Zn(2)(tphz)(H(2)O) 4}{Mo5O15(O(3)PCH(2)CH 2PO3)}4]·14H(2)O

T2 - The hydrothermal conversion of tetra-2-pyridylpyrazine to tetrapyrido [2,3-a:3′,2′-c:2″,3″-h:3‴,2‴-j]phenazine (tphz)

AU - Burkholder, Eric

AU - Zubieta, Jon

N1 - Funding Information: This work was supported by a grant from the National Science Foundation, CHE-0242153.

PY - 2004/3/10

Y1 - 2004/3/10

N2 - The hydrothermal reaction of (NH4)6Mo 7O24·4H2O, ZnSO4·7H2O, tetra-2-pyridylpyrazine, ethylenediphosphonic acid, H2O and HF at 170°C for 96 h yields yellow crystals of [H 4tphz]3[{Zn2(tphz)(H2O) 4}{Mo5O15(O3PCH2CH 2PO3)}4]·14H2O (1·14H2O) (tphz = tetrapyrido[2,3-a:3′,2′-c: 2″,13″-h:3‴,2‴-j]phenazine (tphz)). The structure of 1 consists of two-dimensional networks constructed from chains of {Mo 5O15(O3PR)2}4- clusters tethered through the ethylene bridges of the diphosphonate ligands, which are in turn crosslinked through the {Zn2(tphz)(H2O) 4}4+ subunits. This connectivity generates intralamellar cavities which are occupied by the tetraprotonated H4tphz 4+ cations. A curious feature of the chemistry is the hydrothermal conversion of the tetra-2-pyridylpyrazine starting material to tphz.

AB - The hydrothermal reaction of (NH4)6Mo 7O24·4H2O, ZnSO4·7H2O, tetra-2-pyridylpyrazine, ethylenediphosphonic acid, H2O and HF at 170°C for 96 h yields yellow crystals of [H 4tphz]3[{Zn2(tphz)(H2O) 4}{Mo5O15(O3PCH2CH 2PO3)}4]·14H2O (1·14H2O) (tphz = tetrapyrido[2,3-a:3′,2′-c: 2″,13″-h:3‴,2‴-j]phenazine (tphz)). The structure of 1 consists of two-dimensional networks constructed from chains of {Mo 5O15(O3PR)2}4- clusters tethered through the ethylene bridges of the diphosphonate ligands, which are in turn crosslinked through the {Zn2(tphz)(H2O) 4}4+ subunits. This connectivity generates intralamellar cavities which are occupied by the tetraprotonated H4tphz 4+ cations. A curious feature of the chemistry is the hydrothermal conversion of the tetra-2-pyridylpyrazine starting material to tphz.

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KW - Hydrothermal synthesis

KW - Molybdophosphonate cluster

KW - Network oxide

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