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Difluorophosphate

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Difluorophosphate
Structure of difluorophosphate ion
Ball-and-stick model of the difluorophosphate ion
Ball-and-stick model of the difluorophosphate ion
Spacefill model of difluorophosphate
Spacefill model of difluorophosphate
Names
Systematic IUPAC name Difluorophosphate
Identifiers
CAS Number
3D model (JSmol)
ChemSpider
PubChem CID
CompTox Dashboard (EPA)
InChI
  • InChI=1S/F2HO2P/c1-5(2,3)4/h(H,3,4)/p-1Key: DGTVXEHQMSJRPE-UHFFFAOYSA-M
  • InChI=1/F2HO2P/c1-5(2,3)4/h(H,3,4)/p-1Key: DGTVXEHQMSJRPE-REWHXWOFAH
SMILES
  • P(=O)(F)F
Properties
Chemical formula PO2F−2
Molar mass 100.97 g mol
Structure
Coordination geometry Tetracoordinated at phosphorus atom
Molecular shape Tetrahedral at phosphorus atom
Except where otherwise noted, data are given for materials in their standard state (at 25 °C , 100 kPa). ☒N (what is  ?) Infobox references
Chemical compound

Difluorophosphate or difluorodioxophosphate or phosphorodifluoridate is an anion with formula PO2F−2. It has a single negative charge and resembles perchlorate (ClO−4) and monofluorosulfonate (SO3F) in shape and compounds. These ions are isoelectronic, along with tetrafluoroaluminate, phosphate, orthosilicate, and sulfate. It forms a series of compounds. The ion is toxic to mammals as it causes blockage to iodine uptake in the thyroid. However it is degraded in the body over several hours.

Compounds containing difluorophosphate may have it as a simple uninegative ion, it may function as a difluorophosphato ligand where it is covalently bound to one or two metal atoms, or go on to form a networked solid. It may be covalently bound to a non metal or an organic moiety to make an ester or an amide.

Formation

Ammonium difluorophosphate ([NH4]PO2F2) is formed from treating phosphorus pentoxide with ammonium fluoride. This was how the ion was first made by its discoverer, Willy Lange, in 1929.

Alkali metal chlorides can react with dry difluorophosphoric acid to form alkali metal salts.

NaCl + HPO2F2 → NaPO2F2 + HCl(g)

Fluorination of dichlorophosphates can produce difluorophosphates. Another method is fluorination of phosphates or polyphosphates.

Trimethylsilyl difluorophosphate ((CH3)3Si−O−P(=O)F2) reacts with metal chlorides to give difluorophosphates.

The anhydride of difluorophosphoric acid (HPO2F2), phosphoryl difluoride oxide (P2O3F4) reacts with oxides such as UO3 to yield difuorophosphates. Phosphoryl difluoride oxide also reacts with alkali metal fluorides to yield difluorophosphates.

Properties

The difluorophosphate ion in ammonium difluorophosphate and potassium difluorophosphate has these interatomic dimensions:

Difluorophosphate salt P–O length P–F length O–P–O angle F–P–O angle F–P–F angle
Ammonium difluorophosphate 1.457 Å 1.541 Å 118.7° 109.4° 98.6°
Potassium difluorophosphate 1.470 Å 1.575 Å 122.4° 108.6° 97.1°

Hydrogen bonding from ammonium ion to oxygen atoms causes a change to the difluorophosphate ion in the ammonium salt.

On heating the salts that are not of alkali metals or alkaline earth metals, difluorophosphates decompose firstly by giving off POF3 forming a monofluorophosphate (PO3F) compound, and then this in turn decomposes to an orthophosphate PO3−4 compound.

Difluorophosphate salts are normally soluble and stable in water. However, in acidic or alkaline conditions they can be hydrolyzed to monofluorophosphates and hydrofluoric acid. The caesium and potassium salts are the least soluble.

Irradiating potassium difluorophosphate with gamma rays can make the free radicals •PO2F, •PO3F and •PO2F2.

Compounds

Formula Name Structure Infrared spectrum Melting point Comments Reference
LiPO2F2 Lithium difluorophosphate 360 °C
Be(PO2F2)2 Beryllium difluorophosphate >400 °C d prepared from BeCl2 and acid
CH3CH2−O−P(=O)F2 Ethyl difluorophosphate
[NH4]PO2F−2 Ammonium difluorophosphate orthorhombic: a = 8.13 Å, b = 6.43 Å, c = 7·86 Å, Z = 4 space group Pnma P–F stretching 842 and 860 cm; P–O stretching 1138 and 1292 cm 213 °C
[NO2]PO2F−2 Nitronium difluorophosphate 515, 530, 550, 560, 575, 845, 880, 1145, 1300, 2390, 3760 cm nitronium formed from anhydride and N2O5
[NO]PO2F−2 Nitrosonium difluorophosphate 500, 840, 880, 1130, 1272, 1315, 2278 cm nitrosonium formed from anhydride and N2O3
NaPO2F2 Sodium difluorophosphate 210 °C
Mg(PO2F2)2 Magnesium difluorophosphate 200 °C
[NH4]Mg(PO2F−2)3 Ammonium magnesium difluorophosphate Cmcm a=5.411 b=15.20 c=12.68
Al(PO2F2)3 Aluminium difluorophosphate polymeric 505, 541, 582, 642, 918, 971, 1200, 1290 cm (with 355 cm impurity) formed from Al(CH2CH3)3 and acid; colourless insoluble powder
Si(−O−P(=O)F2)4 Silicon(IV) difluorophosphate formed from SiCl4 and anhydride
(CH3)3Si−O−P(=O)F2 Trimethylsilyl difluorophosphate formed from anhydride and [(CH3)3Si]2O
KPO2F2 Potassium difluorophosphate orthorhombic: a = 8.03 Å, b = 6.205 Å, c = 7.633 Å, Z = 4, V=380.9 Å, density = 2.44 g/cm 510, 525, 570, 835, 880, 1145, 1320, 1340 cm 263 °C colourless elongated prisms
(K)4(PO2F−2)2(S2O2−7) Tetrapotassium difluorophosphate pyrosulfate C2/c: a = 13.00 Å, b = 7.543 Å, c = 19.01 Å, β = 130.07°, Z = 4
Ca(PO2F2)2·CH3COOCH2CH3 Calcium difluorophosphate - ethyl acetate 1:1 solvate
Ca(PO2F2)2 Calcium difluorophosphate >345 °C d
[VO2]PO2F−2 Pervanadyl difluorophosphate
CrO2(PO2F2)2 Chromyl difluorophosphate formed from anhydride; red-brown
Cr(PO2F2)3 Chromium(III) difluorophosphate 320, 385, 490, 575, 905, 955, 1165, 1255 cm formed from excess anhydride, green
Mn(CO)5PO2F2 184 °C
HMn(PO2F2)3 dissolve manganese in acid; white
[NH+4](Mn)3(PO2F−2)(PO3F)2(F)2
Fe(PO2F2)2 Iron(II) difluorophosphate 463, 496, 668 (weak), 869 (double), 1139, 1290 cm 180 °C d colour blue green, hygroscopic, melts 250 °C, above 300 °C starts decomposing to Fe3(PO4)2
Fe(PO2F2)3 Iron(III) difluorophosphate 262, 493, 528, 570, 914, 965, 1173, 1242 cm >400 °C decomposes at 230 °C yielding FeF3; dissolve iron in acid in presence of oxygen
K(Fe)3(PO2F−2)(PO3F)2(F)2
Co(PO2F2)2 Cobalt(II) difluorophosphate 173 °C prepared from CoCl2 and acid; pink or blue; blue formed by heating pink to 140 °C
HCo(PO2F2)3 dissolve cobalt in acid; red-purple
Co(PO2F2)2·2CH3CN Cobalt(II) difluorophosphate - methyl cyanide solvate 1:2 orthorhombic: a = 9.227 Å, b = 13.871 Å, c = 9.471 Å, V = 1212 Å, Z = 4, density = 1.88 g/cm treat HCo(PO2F2)3 with CH3CN for a few weeks; red crystals
[NH+4](Co)3(PO2F−2)(PO3F)2(F)2
Ni(PO2F2)2 Nickel(II) difluorophosphate 255 °C d slowly prepared from NiCl2 and acid; yellow
HNi(PO2F2)3 dissolve nickel in acid; yellow
Cu(PO2F2)2 Copper(II) difluorophosphate orthorhombic Fddd: a = 10.134 Å, b = 24.49 Å, c = 34.06 Å, Z = 48, V = 8454.3 Å, density = 2.50 g/cm 265 °C d pale blue needles
CuI(xantphos)2(μ-PO2F2) polymeric; monoclinic: a = 12.435 Å, b = 10.887 Å, c = 25.682 Å, β = 100.220°, V = 3421 Å colourless
Zn(PO2F2)2 Zinc(II) difluorophosphate c. 25 °C? glassy
H2[Zn(PO2F2)4] Tetra(difluorophosphato)zincic(II) acid
Ga(PO2F2)3 Gallium(III) difluorophosphate
[(CH3)2GaPO2F2]2 Dimethylgallium(III) difluorophosphate dimeric 380, 492, 520, 551, 616, 709, 750, 899, 949, 1171, 1218, 1262, 1295, 1404, 2922, 2982 cm
RbPO2F2 Rubidium difluorophosphate orthorhombic: a = 8.15 Å, b = 6.45 Å, c = 7.79 Å, Z = 4, V = 409.5 Å density = 3.02 g/cm P–F stretching 827 and 946 cm; P–O stretching 1145 and 1320 cm 160 °C white
Sr(PO2F2)2 Strontium difluorophosphate 250 °C d prepared from SrCl2 and acid
[NH4]Sr(PO2F2)3 Ammonium strontium difluorophosphate Triclinic P1 a=7.370 b=11.054 c=13.645 α=88.861 β=87.435° γ=89.323°
AgPO2F2 Silver(I) difluorophosphate
Ag9(PO2F2)14
Ag(1-methyl-2-alkylthiomethyl-1H-benzimidazole)PO2F2
Ag(2,6-bis-pyridine)PO2F2 Triclinic P1: a = 7.687 Å, b = 10.740 Å, c = 13.568 Å, α = 99.52°, β = 96.83°, γ = 99.83°, Z = 2, V = 1076 Å, density = 1.81 g/cm
Ag(4,4′-dicyanodiphenylacetylene)PO2F2
Cd(PO2F2)2 Cadmium(II) difluorophosphate 245 °C d
In(PO2F2)3 Indium(III) difluorophosphate 269, 492, 528, 567, 910, 962, 1179, 1269 cm white, decomposes at 260 °C yielding InF3
[(CH3)2InPO2F2]2 Dimethylindium(III) difluorophosphate dimeric 373, 490, 500, 535, 559, 735, 878, 925, 1128, 1179, 1275, 1435, 2928, 3000 cm
SnCl2(PO2F2)2 Tin(IV) dichloride difluorophosphate
(CH3)2Sn(PO2F2)2 Dimethyltin(IV) difluorophosphate 204 °C d prepared from (CH3)2SnCl2 and acid; yellow
(CH3CH2)2Sn(PO2F2)2 Diethyltin(IV) difluorophosphate 262 °C d prepared from (CH3CH2)2SnCl2 and acid; yellow
(CH3CH2CH2)2Sn(PO2F2)2 Dipropyltin(IV) difluorophosphate 245 °C d prepared from (CH3CH2CH2)2SnCl2 and acid; yellow
(CH3(CH2)3)2Sn(PO2F2)2 Dibutyltin(IV) difluorophosphate 235 °C d prepared from (CH3(CH2)7)2SnCl2 and acid; yellow
(CH3(CH2)7)2Sn(PO2F2)2 Dioctyltin(IV) difluorophosphate 114 °C prepared from (CH3(CH2)7)2SnCl2 and acid; yellow
SbCl4PO2F2 Antimony(V) tetrachloride difluorophosphate
SbF4PO2F2 Antimony(V) tetrafluoride difluorophosphate
(2,2-dipyradyl)2Re(CO)2PO2F2
AuPO2F2
IO2PO2F2 Raman: 130, 163, 191, 219, 295, 323, 329, 378, 637, 713, 737, 781, 799, 839, 918, 1163 cm yellowish colour, produced from IO3, decomposed by water
IO3PO2F2 Raman: 217, 247, 269, 305, 343, 367, 395, 473, 569, 643, 671, 717, 797, 891, 1123 cm yellowish colour, produced from H5IO6, decomposed by water
FXePO2F2 Xenon(II) fluoride difluorophosphate
Xe(PO2F2)2 Xenon(II) difluorophosphate
CsPO2F2 Caesium difluorophosphate orthorhombic: a = 8.437 Å, b = 6.796 Å, c = 8.06 Å, Z = 4, V = 462.1 Å, density = 3.36 g/cm 286 °C
(Cs)2(Fe)2(PO2F−2)(PO3F)2(F)3
Ba(PO2F2)2 Barium difluorophosphate orthorhombic I42d a =10.4935 b =10.4935 c =26.030 >400 °C
[NH4]2Ba(PO2F2)4 Diammonium barium difluorophosphate P2/n a=14.285 b=5.472 c=19.474 β=97.607°
Re(CO)5PO2F2
Hg(PO2F2)2 Mercury(II) difluorophosphate
Hg2(PO2F2)2 Mercury(I) difluorophosphate or di(difluorophosphato)dimercurane Raman: 220 cm produced from anhydride
TlPO2F2 Thallium(I) difluorophosphate produced from anhydride, or acid on TlCl
[(CH3)2TlPO2F2]2 Dimethylthallium(III) difluorophosphate dimeric 360, 374, 500, 505, 520, 559, 850, 880, 1120, 1140, 1195, 1250, 1285, 2932, 3020 cm
Pb(PO2F2)2 Lead(II) difluorophosphate 189 °C d
UO2(PO2F2)2 Uranyl difluorophosphate 260, 498, 854, 924, 980, 1124 cm IR spectrum due to UO2+2
[(CH3CH2)4N]PO2F−2 Tetraethylammonium difluorophosphate
1-ethyl-3-methylimidazolium difluorophosphate ionic liquid
1-butyl-3-methylimidazolium difluorophosphate ionic liquid
1-butyl-1-methylpyrrolidinium difluorophosphate ionic liquid
1-butyl-1-methylpiperidinium difluorophosphate ionic liquid
di(3,3′,4,4′-tetramethyl-2,2′,5,5′-tetraselenafulvalenium)difluorophosphate Transitions to a metallic state below 137 K (−136 °C)
1,4-diphenyl-3,5-enanilo-4,5-dihydro-1,2,4-triazole (nitron) monoclinic P21/n: a = 7.3811 Å, b = 14.9963 Å, c = 16.922 Å, β = 102.138°, V = 1361.2 Å, Z = 4 insoluble; yellow-brown
Strychnine PO2F2
Cocaine PO2F2
Brucine PO2F2
Morphine PO2F2
[N(CH3)4]PO2F−2 Tetramethylammonium difluorophosphate
H[B(PO2F2)4] Tetra(difluorophosphato)boric acid 469, 502, 552, 647, 836, 940, 994, 1093, 1348, 1567 cm formed from BBr3 and acid; liquid
Li[B(PO2F2)4] Lithium tetra(difluorophosphato)borate monoclinic P21/c: a=7.9074 Å, b = 14.00602 Å, c = 13.7851 Å, β = 121.913°, Z = 4 479, 502, 568, 833, 945, 1002, 1080, 1334 cm formed from HB(PO2F2)4 and butyllithium; colourless
[HS(CH3)2][B(PO2F2)4] Dimethylsulfonium tetra(difluorophosphato)borate 472, 511, 555, 648, 832, 933, 993, 1082, 1337, 1436, 2851, 2921, 3042 cm formed from BH3·S(CH3)2 and acid; ionic liquid
[Li((CH3CH2)2O)]3[Al(PO2F2)6] (Diethyl ether)lithium hexa(difluorophosphato)aluminate trigonal R3: a = 17.4058 Å, b = 17.4058 Å, c = 21.4947 Å, γ = 120°, Z = 6 417, 503, 536, 624, 723, 891, 922, 964, 1174, 1204, 1283 cm formed from butyllithium and triethylaluminium and the acid; white
K2CrO2(PO2F2)4 305, 370, 485, 550, 870, 920, 1050, 1130, 1250 cm 145 °C d formed from anhydride and K2CrO4; brown
Na2MoO2(PO2F2)4 amorphous 280, 490, 620, 880, 915, 950, 1020, 1070, 1140, 1280 cm 125 °C d formed from anhydride and K2MoO4; white
Na2WO2(PO2F2)4 amorphous 280, 474, 620, 930, 1030, 1130, 1230 cm 109 °C d formed from anhydride and K2WO4; white

Related substances

Difluorphosphoric acid

Difluorophosphoric acid (HPO2F2) is one of the fluorophosphoric acids. It is produced when phosphoryl fluoride reacts with water:

POF3 + H2O → HPO2F2 + HF

This in turn is hydrolysed more to give monofluorophosphoric acid (H2PO3F), and a trace of hexafluorophosphoric acid (HPF6). HPO2F2 also is produced when HF reacts with phosphorus pentoxide. Yet another method involves making difluorphosphoric acid as a side product of calcium fluoride being heated with damp phosphorus pentoxide. A method to make pure difluorphosphoric acid involves heating phosphoryl fluoride with monofluorophosphoric acid and separating the product by distillation:

POF3 + H2PO3F → 2 HPO2F2

Difluorophosphoric acid can also be produced by fluorinating phosphorus oxychlorides. P2O3Cl4 and POCl3 react with hydrogen fluoride solution to yield HPO2Cl2 and then HPO2F2. Yet another way is to treat orthophosphate (PO3−4) with fluorosulfuric acid (HSO3F).

Difluorphosphoric acid is a colorless liquid. It melts at −96.5 °C (−141.7 °F) and boils at 115.9 °C (240.6 °F). Its density at 25 °C is 1.583 g/cm.

Phosphoryl difluoride oxide

Difluorophosphoric acid anhydride also known as phosphoryl difluoride oxide or diphosphoryl tetrafluoride (F2(O=)P−O−P(=O)F2 or P2O3F4) is an anhydride of difluorphosphoric acid. It crystallises in the orthorhombic system, with space group Pcca and Z = 4. P2O3F4 can be made by refluxing difluorophosphoric acid with phosphorus pentoxide. P2O3F4 boils at 71 °C.

Substitution

In addition to the isoelectronic series, ions related by substituting fluorine or oxygen by other elements include monofluorophosphate, difluorothiophosphate, dichlorothiophosphate, dichlorophosphate, chlorofluorothiophosphate, chlorofluorophosphate, dibromophosphate, and bromofluorophosphate.

Adducts

Difluorophosphate can form adducts with PF5 and AsF5. In these the oxygen atoms form a donor-acceptor link between the P and As (or P) atoms, linking the difluorides to the pentafluorides. Example salts include KPO2F2·2AsF5, KPO2F2·AsF5, KPO2F2·2PF5 and KPO2F2·PF5.

Amines can react with phosphoryl fluoride to make substances with a formula RR′N−P(=O)F2. The amines shown to do this include ethylamine, isopropylamine, n-butylamine, t-butylamine, dimethylamine, and diethylamine. The monoamines can further react to yield an alkyliminophosphoric fluoride (R−N=P(=O)F).

References

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