Vibrational spectra of the layered monofluorophosphate (V), NH4Ag3(PO3F)2

Baran, Enrique J.; Weil, Mat­thias

doi:10.1002/jrs.2461

Cited by 10 publications

(9 citation statements)

References 13 publications

(12 reference statements)

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“…The spectrum of 1 also shows some additional bands characteristic for the NH 4 + group. A broad band at 3217 cm –1 is attributed to the N–H stretching vibrations, while the band at 1406 cm –1 is ascribed to the N–H deformation vibrations. , The spectrum of 3 differs from those of 1 and 2 because this compound contains the PO 3 F group instead of the PO 3 (OH) group. A band at 1109 cm –1 , having a shoulder at the higher energy side of the band, is assigned to the asymmetric P–O stretching vibrations of the PO 3 F group.…”

Section: Results and Discussionsupporting

confidence: 79%

“…A band at 835 cm –1 is ascribed to the P–F stretching vibration. In the spectra of other monofluorophoshate compounds, the P–F stretching vibration band is found at 824 cm –1 for Hg 2 PO 3 F, 792 cm –1 for Ag 2 PO 3 F, and 776 cm –1 for NH 4 Ag 3 (PO 3 F) 2 . − These results are in agreement with the structural features of the above-mentioned compounds, as the P–F bond length increases from 1.568(8) Å for Hg 2 PO 3 F through 1.575(2) Å for Ag 2 PO 3 F to 1.590 Å for NH 4 Ag 3 (PO 3 F) 2 . From the data provided, it can be concluded that the band shifts to the lower wavenumber with the P–F bond elongation.…”

Section: Results and Discussionsupporting

confidence: 79%

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Ionothermal Synthesis, Structures, and Magnetism of Three New Open Framework Iron Halide-Phosphates

et al. 2019

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A set of different open framework iron phosphates have been synthesized ionothermally using a task-specific ionic liquid, 1-butyl-4-methylpyridinium hexafluorophosphate, that acts in the synthesis as the reaction medium and mineralizer: (NH4)2Fe2(HPO4)(PO4)Cl2F (1) and K2Fe2(HPO4)(PO4)Cl2F (2) exhibit similar composition and closely related structural features. Both structures consist of {Fe2(HPO4)(PO4)Cl2F}2– macroanions and charge balancing ammonium or potassium cations. Their open framework structure contains layers and chains of corner-linked {Fe(1)O2Cl4} and {Fe(2)F2O4} octahedra, respectively, interconnected by PO4 tetrahedra forming 10-ring channels. KFe(PO3F)F2 (3) is built up by {Fe[(PO3F)4/3F2/2]}{Fe(PO3F)2/3F2/2F2} layers separated by K+ cations. Chains of alternating {FeF2O4} and {FeO2F4} octahedra, which are linear for 1 but undulated for 2, are linked to each other via corner-sharing {PO3F} tetrahedra with the fluorine pointing into the interlayer space. The compounds were characterized by means of single crystal and powder X-ray diffraction, infrared spectroscopy, and magnetic measurements. 1 reveals a strong ground state spin anisotropy with a spin 5/2 state and a magnetic moment of 5.3 μB/Fe3+. Specific heat and magnetic data unveil three magnetic transitions at 95, 50, and 3.6 K. Compound 2 has a very similar crystal structure as compared to 1 but exhibits a different magnetic behavior: a slightly lower magnetic moment of 4.7 μB/Fe3+ and a magnetic transition to a canted antiferromagnetic state below 90 K. Compound 3 exhibits typical paramagnetic behavior close to room-temperature (5.71 μB/Fe3+). There are no clear indications for a phase transition down to 2 K despite strong antiferromagnetic spin–spin interactions; only a magnetic anomaly appears at 50 K in the zero-field cooled data.

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Section: Results and Discussionsupporting

confidence: 79%

Section: Results and Discussionsupporting

confidence: 79%

Ionothermal Synthesis, Structures, and Magnetism of Three New Open Framework Iron Halide-Phosphates

et al. 2019

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“…The IR spectra (Figure SI-2) of the title compounds 1 – 4 were recorded in the region of 4000–400 cm –1 . For the ammonia containing manganese phosphates ( 2 , 4 ), the vibration modes of the N–H bonds of the (NH 4 ) + ions range between 1384 and 1546 cm –1 (deformation vibrations) and 2784 and 3385 cm –1 (stretching vibrations). − The broad band observed around 3225 cm –1 can be attributed to the stretching vibration of hydroxyl groups of the phosphate tetrahedra in all title compounds 1 – 4 . At lower wavenumbers, all IR spectra are quite similar because the vibrational modes for the P–OH, P–O, and P–F bonds of the various tetrahedral phosphate units (PO 2 (OH) 2 , PO 3 (OH), PO 3 F) arise between 400 and 1300 cm –1 . − The band at 1260 cm –1 , which is for compound 2 notably intense, can be assigned to the P–O–H deformation vibration .…”

Section: Resultsmentioning

confidence: 99%

Ionothermal Synthesis Enables Access to 3D Open Framework Manganese Phosphates Containing Extra-Large 18-Ring Channels

et al. 2019

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An ionothermal synthesis study of transition metal phosphates using the ionic liquid 1-butyl-4-methylpyridinium hexafluorophosphate [C4mpy][PF6] yielded four new, different open framework manganese compounds, that is, K2Mn3(HPO4)2(PO3F)F2 (1), (NH4)2Mn3(HPO4)2(PO3F)F2 (2), KMn3(H2PO4)(HPO4)2F2 (3), and (NH4)Mn3(H2PO4)(PO3F)2F2 (4). The obtained products not only feature new framework topologies unprecedented in the family of phosphates but also interesting properties as the transition metal gives rise to both luminescent (rendering them potential nonrare earth containing red emitting phosphors) and unconventional magnetic properties governed by geometric frustrations. Aside from the structural analysis (powder and single-crystal X-ray diffraction, infrared spectroscopy), a variety of characterization methods (photoluminescence spectroscopy and magnetic measurements) were applied to study the material’s properties. Single crystal X-ray studies reveal that 1 (P21/c with a = 5.501(1), b = 14.203(3), c = 16.905(4) Å, β = 108.65(3)°, V = 1251.4 Å3, and Z = 4) and 2 (P2 1 /c with a = 5.587(1), b = 14.507(3), c = 17.364(3) Å, β = 108.75(3)°, V = 1332.6(5) Å3, and Z = 4) feature S-shaped 18-ring channels along [100], which are formed by trimer-Mn3O9F2 chains parallel to [100] and interconnecting PO3(OH) and PO3F tetrahedra. The structure of compounds 3 (C2/c with a = 20.307(4), b = 7.635(1), c = 7.834(2) Å, β = 103.26(3)°, V = 1182.2(4) Å3, and Z = 4) and 4 (C2/c with a = 20.402(4), b = 7.673(1), c = 7.845(2) Å, β = 103.56(3)°, V = 1193.8(4) Å3, and Z = 4) are characterized by layers, which are built of Mn3O8F4 octahedra trimers, with Kagomé topology parallel to the bc plane featuring 3,6-ring channels. The layers are stacked according to a sequence of AA i along the a axis. Taking into account the [P(2)O3(OH)/P(2)O3F] tetrahedra, the Kagomé layers are replenished to a Mn3O2(HPO4)/Mn3O2(PO3F) composition, which are interlinked by [P(1)O2(OH)2] forming 10-ring channels parallel to [001]. Charge compensation of the macroanions is achieved by K+ (1 and 3) and (NH4)+ (2 and 4) cations. At room temperature, compounds 1–4 demonstrate a reddish orange emission ascribed to the spin-forbidden 4T1g(4G) → 6A1g(6S) transition of the Mn2+ ions. Upon lowering the temperature to 77 K, the emission of each compound is red-shifted and becomes pure red. Compounds 1 and 2 contain spin trimers with a presumable doubled ground state. The intertrimer magnetic coupling is relatively weak, and small ferrimagnetic domains are possible in 1. The magnetic behavior of 3 and 4 can be considered as antiferromagnetic. This can be understood as their staircase Kagomé lattices are distorted, meaning that the intrinsic geometrical frustration is lifted.

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“…9). [31][32][33] Additional vibrations in the region of 1100-1200cm -1 also suggest a reduction in symmetry of the oxoanion unit. For M=Co and Cu, the spectra resulting from the fluorophosphates doped materials matched that which was obtained for the undoped Na 2 Ni(SO 4 ) 2 •2H 2 O material which naturally adopts the triclinic structure (Fig.…”

Section: Raman Data For Na 2 M(so 4 ) 2-x (Po 3 F) X •2h 2 O (M= Fe mentioning

confidence: 99%

Investigation into the effect on structure of oxoanion doping in Na2M(SO4)2·2H2O

Driscoll

Kendrick

Wright

et al. 2016

Journal of Solid State Chemistry

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Vibrational spectra of the layered monofluorophosphate (V), NH₄Ag₃(PO₃F)₂

Cited by 10 publications

References 13 publications

Ionothermal Synthesis, Structures, and Magnetism of Three New Open Framework Iron Halide-Phosphates

Ionothermal Synthesis, Structures, and Magnetism of Three New Open Framework Iron Halide-Phosphates

Ionothermal Synthesis Enables Access to 3D Open Framework Manganese Phosphates Containing Extra-Large 18-Ring Channels

Investigation into the effect on structure of oxoanion doping in Na2M(SO4)2·2H2O

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