Rhenium(V)‐oxidepyrophosphate Re2O3(P2O7)‡

Islam, Saiful M.; Glaum, Robert

doi:10.1002/zaac.200900448

Cited by 6 publications

(5 citation statements)

References 46 publications

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“…In the infrared spectrum of ReO 2 (PO 4 ) (Table 4) bands at about 1190 cm –1 , 1155 cm –1 , 1082 cm –1 , and 1024 cm –1 are attributed to the P–O symmetric and asymmetric stretching vibrations of [PO 4 ] group 9,43. In agreement with the IR spectrum of Re 2 O 7 44 two bands at about 968 cm –1 and 942 cm –1 are assigned to the stretching vibrations (O=Re=O).…”

Section: Resultssupporting

confidence: 77%

“…We tend to correlate the broad band of ReO 2 (PO 4 ) centered at 874 cm –1 to the antisymmetric stretching vibration ν as (Re–O–P). This assignment is backed by ν as (Re–O–Re) ≈ 850 cm –1 observed for Re 2 O 7 45,44 and ν as (P–O–P) ≈ 950 cm –1 as it is observed for many pyrophosphates 9,43,46. Bands in between 600 and 400 cm –1 can be assigned to deformation vibrations δ (O–P–O).…”

Section: Resultsmentioning

confidence: 58%

“…Obviously, even phosphates of the non‐existing binary oxides “CrO” and “Mo 2 O 3 ” can be obtained. By the recent characterization of Re VI 2 O 3 (PO 4 ) 2 8 and Re V 2 O 3 (P 2 O 7 )9 in addition to the long known pyrophosphate Re IV P 2 O 7 10 our attention was attracted to the thermodynamic stability of phosphates containing rhenium in its various oxidation states. Eventually, the question arose whether phosphates of Re 2 O 7 or even OsO 4 might exist.…”

Section: Introductionmentioning

confidence: 99%

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The First Phosphates of Heptavalent Rhenium

Islam

Glaum

Pelka

et al. 2013

Zeitschrift anorg allge chemie

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ReVIIO2(PO4) and (ReVII2O5)Sio2[Sit2O(PO4)6] were obtained from Re2O7 and P4O10 in sealed silica tubes (250 ≤ ϑ ≤ 400 °C). The crystal structures were solved and refined from X‐ray single crystal data (ReVIIO2(PO4): C2/c, Z = 24, a = 14.403(1) Å, b = 8.414(1) Å, c = 20.647(3) Å, β = 93.165(8)°, T = 123 K, 10352 ind. refl., 218 variables, 24 atoms in asymmetric unit, R1 = 0.041, wR2 = 0.106; (ReVII2O5)Sio2[Sit2O(PO4)6]: P$\bar{1}$, Z = 1, a = 7.8589(3) Å, b = 7.8609(3) Å, c = 10.8311(4) Å, α = 85.312(2)°, β = 73.078(2)°, γ = 60.075(2)°, T = 298 K, 2551 ind. reflections, 174 variables, 22 atoms in asymmetric unit, R1 = 0.078, wR2 = 0.208). The complex crystal structure of ReO2(PO4) can be derived from the ReO3 structure type. The crystal structure of the silicophosphate consists of distorted [Re2O11] dioctahedra (1.69 Å ≤ d(Re–O) ≤ 2.08 Å), [SiIVO6] octahedra, and [Sit2O(PO4)6]12– heteropolyanions. In ReO2(PO4) monomeric perrhenyl ions (ReO2)3+ (∠(Ot,Re, Ot) ≈ 101.5°) are formed. The silicophosphate (Re2O5)Sio2[Sit2O(PO4)6] contains dinuclear (Re2O5)4+ cations. 31P‐MAS‐NMR studies on ReO2(PO4) are in accordance with three independent sites of phosphorus. The results of 31P‐ and 29Si‐MAS‐NMR studies on (Re2O5)Sio2[Sit2O(PO4)6] are in agreement with three crystallographically independent sites for phosphorus and two sites for silicon.

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Section: Resultssupporting

confidence: 77%

Section: Resultsmentioning

confidence: 58%

Section: Introductionmentioning

confidence: 99%

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The First Phosphates of Heptavalent Rhenium

Islam

Glaum

Pelka

et al. 2013

Zeitschrift anorg allge chemie

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“…There is even evidence for polymorphism in Re VII O 2 (PO 4 ) as it was observed for Mo VI O 2 (SO 4 ) 24. Phosphates of rhenium in the lower oxidation states 4+, 5+, and 6+ (ReP 2 O 7 ,10 Re 2 O 3 (P 2 O 7 ),9 Re 2 O 3 (PO 4 ) 2 8) are closely related to the corresponding tungsten compounds W IV P 2 O 7 ,48 W V 2 O 3 (P 2 O 7 ),49 and W VI 2 O 3 (PO 4 ) 2 50,51…”

Section: Discussionmentioning

confidence: 83%

Palladium‐Catalyzed C–H Bond Acylation of Acetanilides with Benzylic Alcohols under Aqueous Conditions

Luo

Yang

et al. 2015

Eur J Org Chem

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“…For all transition metals, but technetium and osmium, anhydrous phosphates have been known and crystallographically characterized [1][2][3][4][5] for some years. Remarkably, The wide variability of oxidation states of the metal and of the P/M ratio observed for anhydrous rhenium phosphates appears to be particularly noteworthy (Re IV P 2 O 7 , [6] Re V 2 O 3 (P 2 O 7 ), [7] Re VI 2 O 3 (PO 4 ) 2 , [8] Re VII O 2 (PO 4 ) [9] ). In stark contrast, for the neighbouring platinum group metals (PGM) ruthenium, rhodium and iridium anhydrous phosphates are well established only of the trivalent cations (Ru(PO 3 ) 3 , [10,11] RhPO 4 and (Rh(PO 3 ) 3 , [12] Ir(PO 3 ) 3 [13] ).…”

Section: Introductionmentioning

confidence: 99%

Osmium(IV) pyrophosphate: Synthesis, Crystallization, and Ligand‐Field Analysis of the [Os^IVO₆] Chromophore

Glaum

Rössel²,

Daniels³

et al. 2022

Zeitschrift anorg allge chemie

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Dedicated to Professor Caroline Röhr on her anniversaryTwo polymorphs of burgundy-red OsP 2 O 7 , with cubic (ZrP 2 O 7 structure type, Z = 4, a = 7.8276(4) Å, 3 × 3 × 3 superstructure with a' = 3a = 23.484(2) Å) and triclinic symmetry (ruby-red crystals, single-crystal X-ray structure determination, GeP 2 O 7 structure type, P � 1 (no. 2), Z = 2, a = 4.8072(7) Å, b = 6.8993(13) Å, c = 8.050(1) Å, α = 91.82(2)°, β = 92.92(1)°, γ = 107.42(2)°, 98 parameters, R 1 = 0.045, wR 2 = 0.144, 3006 unique reflections with j F o j > 4σ(F o )) have been obtained reducing OsO 4 by phosphorus in sealed silica ampoules followed by subsequent chemical vapour transport. Reaction with the wall led to mixed Si IV /Os IV silicophosphates (Os 1À x Si x ) 3 [Si 2 O(PO 4 ) 6 ] {x = 0.84, pale orange, Si IV 3 [Si 2 O(PO 4 ) 6 ] structure type, R � 3, Z = 3, a = 7.893(1) Å, c = 24.409(5) Å, 59 parameters, R 1 = 0.058, wR 2 = 0.160, 1311 unique reflections with 1033 j F o j > 4σ(F o ); x = 0.47, orange, Ge IV 3 [Si 2 O(PO 4 ) 6 ] structure type, P � 31c, Z = 2, a = 7.9979(3) Å, c = 16.4625(5) Å, 59 parameters, R 1 = 0.040, wR 2 = 0.094, 902 unique reflections with 749 j F o j > 4σ(F o )}. Both structures were refined from single-crystal data. Above 25 K triclinic OsP 2 O 7 shows temperature independent paramagnetism with a strong temperature dependence of m=m B pointing to 3 T 1g as electronic ground state for Os 4 + (d 4 ) with strong spin-orbit coupling leading to J = 0 and the nonmagnetic ground state of the octahedral [Os IV O 6 ] chromophore.. Optical spectra of both polymorphs of OsP 2 O 7 show similar combinations of intense sharp and broad absorption bands typical for d n electronic systems systems with both, spin-orbit coupling and ligand field splitting, being strong. The observations are consistent with the ligand-field parameters Δ o = 20000 cm À 1 , B = 704 cm À 1 , and ζ = 3454 cm À 1 for the octahedral [Os IV O 6 ] chromophore.

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Rhenium(V)‐oxidepyrophosphate Re₂O₃(P₂O₇)‡

Cited by 6 publications

References 46 publications

The First Phosphates of Heptavalent Rhenium

The First Phosphates of Heptavalent Rhenium

Palladium‐Catalyzed C–H Bond Acylation of Acetanilides with Benzylic Alcohols under Aqueous Conditions

Osmium(IV) pyrophosphate: Synthesis, Crystallization, and Ligand‐Field Analysis of the [Os^IVO₆] Chromophore

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Rhenium(V)‐oxidepyrophosphate Re2O3(P2O7)‡

Cited by 6 publications

References 46 publications

The First Phosphates of Heptavalent Rhenium

The First Phosphates of Heptavalent Rhenium

Palladium‐Catalyzed C–H Bond Acylation of Acetanilides with Benzylic Alcohols under Aqueous Conditions

Osmium(IV) pyrophosphate: Synthesis, Crystallization, and Ligand‐Field Analysis of the [OsIVO6] Chromophore

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About

Rhenium(V)‐oxidepyrophosphate Re₂O₃(P₂O₇)‡

Osmium(IV) pyrophosphate: Synthesis, Crystallization, and Ligand‐Field Analysis of the [Os^IVO₆] Chromophore