Silver vanadyl(IV) ortho-pyrophosphate: Synthesis, crystal structure, and characterization of the (V≡O)2+ group

Knut Wittich; Yaser Nejatyjahromy; Dinar Abdullin; Olav Schiemann; Andrey Karpov; Katharina Dobner; Frank Rosowski; Robert Glaum

doi:10.1002/zaac.201800033

Silver vanadyl(IV) ortho-pyrophosphate: Synthesis, crystal structure, and characterization of the (V≡O)²⁺ group

Knut Wittich, Yaser Nejatyjahromy, Dinar Abdullin, Olav Schiemann, Andrey Karpov, Katharina Dobner, Frank Rosowski, Robert Glaum

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

1 Scopus citations

Abstract

Ag₆(V^IVO)₂(PO₄)₂(P₂O₇) was obtained by reaction of Ag₃PO₄ and (VO)₂P₂O₇ (sealed ampoule, 550 °C, 3 d). The crystal structure of the new mixed ortho-pyrophosphate was determined from X-ray single-crystal data [Pnma, Z = 4, a = 12.759(3) Å, b = 17.340(4) Å, c = 6.418(1) Å, R₁ = 0.071, wR₂ = 0.184 for 3174 unique reflections with F_o > 4σ(F_o), 141 variables]. Ag⁺ ions are located in between layers [(V^IVO)₂(PO₄)₂(P₂O₇)]^6–. Equilibrium relations of the new phosphate to neighboring phases were determined. The electronic structure of the (V^IV≡O)²⁺ group was investigated by polarized electronic absorption spectroscopy (ṽ_1a = 9450 cm^–1, ṽ_1b = 9950 cm^–1, ṽ₂ = 14750 cm^–1), EPR spectroscopy [X- and Q-band, powder and single crystal, orthorhombic crystal g-tensor with g₁ = 1.9445(3), g₂ = 1.9521(3), g₃ = 1.9695(3)], and magnetic measurements (powder, μ_exp/μ_B = 1.71, Θ_p = –1.7 K).

Original language	English
Pages (from-to)	424-429
Number of pages	6
Journal	Zeitschrift fur Anorganische und Allgemeine Chemie
Volume	644
Issue number	8-9
DOIs	https://doi.org/10.1002/zaac.201800033
State	Published - 17 May 2018
Externally published	Yes

Keywords

Heterogeneous catalysis
Selective oxidation
Solid-state chemistry
Solid-state structures
Vanadyl phosphate

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10.1002/zaac.201800033

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@article{52f62f59463045bd88d80fc18b3d4bdb,

title = "Silver vanadyl(IV) ortho-pyrophosphate: Synthesis, crystal structure, and characterization of the (V≡O)2+ group",

abstract = "Ag6(VIVO)2(PO4)2(P2O7) was obtained by reaction of Ag3PO4 and (VO)2P2O7 (sealed ampoule, 550 °C, 3 d). The crystal structure of the new mixed ortho-pyrophosphate was determined from X-ray single-crystal data [Pnma, Z = 4, a = 12.759(3) {\AA}, b = 17.340(4) {\AA}, c = 6.418(1) {\AA}, R1 = 0.071, wR2 = 0.184 for 3174 unique reflections with Fo > 4σ(Fo), 141 variables]. Ag+ ions are located in between layers [(VIVO)2(PO4)2(P2O7)]6–. Equilibrium relations of the new phosphate to neighboring phases were determined. The electronic structure of the (VIV≡O)2+ group was investigated by polarized electronic absorption spectroscopy (ṽ1a = 9450 cm–1, ṽ1b = 9950 cm–1, ṽ2 = 14750 cm–1), EPR spectroscopy [X- and Q-band, powder and single crystal, orthorhombic crystal g-tensor with g1 = 1.9445(3), g2 = 1.9521(3), g3 = 1.9695(3)], and magnetic measurements (powder, μexp/μB = 1.71, Θp = –1.7 K).",

keywords = "Heterogeneous catalysis, Selective oxidation, Solid-state chemistry, Solid-state structures, Vanadyl phosphate",

author = "Knut Wittich and Yaser Nejatyjahromy and Dinar Abdullin and Olav Schiemann and Andrey Karpov and Katharina Dobner and Frank Rosowski and Robert Glaum",

note = "Publisher Copyright: {\textcopyright} 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.",

year = "2018",

month = may,

day = "17",

doi = "10.1002/zaac.201800033",

language = "English",

volume = "644",

pages = "424--429",

journal = "Zeitschrift fur Anorganische und Allgemeine Chemie",

issn = "0044-2313",

publisher = "Wiley-VCH Verlag",

number = "8-9",

}

TY - JOUR

T1 - Silver vanadyl(IV) ortho-pyrophosphate

T2 - Synthesis, crystal structure, and characterization of the (V≡O)2+ group

AU - Wittich, Knut

AU - Nejatyjahromy, Yaser

AU - Abdullin, Dinar

AU - Schiemann, Olav

AU - Karpov, Andrey

AU - Dobner, Katharina

AU - Rosowski, Frank

AU - Glaum, Robert

PY - 2018/5/17

Y1 - 2018/5/17

N2 - Ag6(VIVO)2(PO4)2(P2O7) was obtained by reaction of Ag3PO4 and (VO)2P2O7 (sealed ampoule, 550 °C, 3 d). The crystal structure of the new mixed ortho-pyrophosphate was determined from X-ray single-crystal data [Pnma, Z = 4, a = 12.759(3) Å, b = 17.340(4) Å, c = 6.418(1) Å, R1 = 0.071, wR2 = 0.184 for 3174 unique reflections with Fo > 4σ(Fo), 141 variables]. Ag+ ions are located in between layers [(VIVO)2(PO4)2(P2O7)]6–. Equilibrium relations of the new phosphate to neighboring phases were determined. The electronic structure of the (VIV≡O)2+ group was investigated by polarized electronic absorption spectroscopy (ṽ1a = 9450 cm–1, ṽ1b = 9950 cm–1, ṽ2 = 14750 cm–1), EPR spectroscopy [X- and Q-band, powder and single crystal, orthorhombic crystal g-tensor with g1 = 1.9445(3), g2 = 1.9521(3), g3 = 1.9695(3)], and magnetic measurements (powder, μexp/μB = 1.71, Θp = –1.7 K).

AB - Ag6(VIVO)2(PO4)2(P2O7) was obtained by reaction of Ag3PO4 and (VO)2P2O7 (sealed ampoule, 550 °C, 3 d). The crystal structure of the new mixed ortho-pyrophosphate was determined from X-ray single-crystal data [Pnma, Z = 4, a = 12.759(3) Å, b = 17.340(4) Å, c = 6.418(1) Å, R1 = 0.071, wR2 = 0.184 for 3174 unique reflections with Fo > 4σ(Fo), 141 variables]. Ag+ ions are located in between layers [(VIVO)2(PO4)2(P2O7)]6–. Equilibrium relations of the new phosphate to neighboring phases were determined. The electronic structure of the (VIV≡O)2+ group was investigated by polarized electronic absorption spectroscopy (ṽ1a = 9450 cm–1, ṽ1b = 9950 cm–1, ṽ2 = 14750 cm–1), EPR spectroscopy [X- and Q-band, powder and single crystal, orthorhombic crystal g-tensor with g1 = 1.9445(3), g2 = 1.9521(3), g3 = 1.9695(3)], and magnetic measurements (powder, μexp/μB = 1.71, Θp = –1.7 K).

KW - Heterogeneous catalysis

KW - Selective oxidation

KW - Solid-state chemistry

KW - Solid-state structures

KW - Vanadyl phosphate

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U2 - 10.1002/zaac.201800033

DO - 10.1002/zaac.201800033

M3 - Article

AN - SCOPUS:85054730616

SN - 0044-2313

VL - 644

SP - 424

EP - 429

JO - Zeitschrift fur Anorganische und Allgemeine Chemie

JF - Zeitschrift fur Anorganische und Allgemeine Chemie

IS - 8-9

ER -

Silver vanadyl(IV) ortho-pyrophosphate: Synthesis, crystal structure, and characterization of the (V≡O)²⁺ group

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Keywords

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