Difluorophosphate

From Wikipedia, the free encyclopedia
Difluorophosphate
Ball-and-stick model of the difluorophosphate ion
Spacefill model of difluorophosphate
Names
Systematic IUPAC name
Difluorophosphate[1]
Identifiers
  • 7238-93-9
3D model (JSmol)
ChemSpider
  • InChI=1S/F2HO2P/c1-5(2,3)4/h(H,3,4)/p-1
    Key: DGTVXEHQMSJRPE-UHFFFAOYSA-M
  • InChI=1/F2HO2P/c1-5(2,3)4/h(H,3,4)/p-1
    Key: DGTVXEHQMSJRPE-REWHXWOFAH
  • [O-]P(=O)(F)F
Properties
PO
2F−
2
Molar mass 100.97 g mol−1
Except where otherwise noted, data are given for materials in their standard state (at 25 °C [77 °F], 100 kPa).
☒N (what is checkY☒N ?)
Infobox references

Difluorophosphate or difluorodioxophosphate or phosphorodifluoridate is an anion with formula PO
2F−
2. It has a single negative charge and resembles perchlorate (ClO−
4) and monofluorosulfonate (SO3F−) in shape and compounds.[2] These ions are isoelectronic, along with tetrafluoroaluminate, phosphate, orthosilicate, and sulfate.[2][3] 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.[2]

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.[4] It may be covalently bound to a non metal or an organic moiety to make an ester or an amide.

Formation[]

The ammonium salt of difluorophosphate is formed from treating phosphorus pentoxide with ammonium fluoride.[2] This was how the ion was first made by its discoverer, Willy Lange, in 1929.[3][5]

Alkali chlorides can react with dry difluorophosphoric acid to form alkali metal salts.[6]

NaCl + HPO2F2 → NaPO2F2 + HCl(g)

Fluoridation of dichlorophosphates can produce difluorophosphates.[7] Another method is fluorination of phosphates or polyphosphates.[5]

Trimethylsilyl difluorophosphate reacts with metal chlorides to give difluorophosphates.[8]

The anhydride phosphoryl difluoride oxide (P2O3F4) reacts with oxides such as UO3 to yield difuorophosphates.[9] Phosphoryl difluoride oxide also reacts with alkali fluorides to yield difluorophosphates.[10]

Properties[]

In ammonium difluorophosphate the difluorophosphate ion has these interatomic dimensions: P–O length 1.457 Å, P–F length 1.541 Å, O–P–O angle 118.7°, F–P–O 109.4° and F–P–F angle 98.6°. Hydrogen bonding from ammonium to oxygen atoms causes a change to the difluorophosphate ion in the ammonium salt. In potassium difluorophosphate the ion has dimensions: P–O length 1.470 Å, P–F length 1.575 Å, O–P–O angle 122.4°, F–P–O 108.6° and F–P–F angle 97.1°.[11]

On heating the salts that are not of alkali or alkaline earths, difluorophosphates decompose firstly by giving off POF3 forming a monofluorophosphate (PO3F2−) compound, and then this in turn decomposes to an orthophosphate PO3−
4 compound.[12][13]

Difluorophosphate salts are normally soluble and stable in water. However, in acidic or alkaline conditions they can be hydrolyzed to monofluorophosphates and hydrofluoric acid.[14] The caesium and potassium salts are the least soluble.[14]

Irradiating potassium difluorophosphate with gamma rays can make the free radicals PO2F•−, PO3F•− and PO
2F•
2.[15][16]

Compounds[]

Formula Structure Infrared spectrum Melting point Reference Comments
LiPO2F2 360 °C [5][6]
Be(PO2F2)2 >400 °C d [17] prepared from BeCl2 and acid
C2H5OPOF2 [18]
NH4PO2F2 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−1; P–O stretching 1138 and 1292 cm−1 213 °C [6][11]
NO2PO2F2 515, 530, 550, 560, 575, 845, 880, 1145, 1300, 2390, 3760 cm−1 [19] nitronium formed from anhydride and N2O5
NOPO2F2 500, 840, 880, 1130, 1272, 1315, 2278 cm−1 [19] nitrosonium formed from anhydride and N2O3
NaPO2F2 210 °C [6]
Mg(PO2F2)2 200 °C [5]
Al(PO2F2)3 polymeric[4] 505, 541, 582, 642, 918, 971, 1200, 1290 cm−1 (with 355 cm–1 impurity) [7][8] formed from AlEt3 and acid; colourless insoluble powder[4]
Si(OPOF2)4 [18] formed from SiCl4 and anhydride
(CH3)Si3OPOF2 [4][18] formed from anhydride and [(CH3)3Si]2O
KPO2F2 orthorhombic: a = 8.03 Å, b = 6.205 Å, c = 7.633 Å, Z = 4, V=380.9 Å3, density = 2.44 g/cm3 510, 525, 570, 835, 880, 1145, 1320, 1340 cm−1 263 °C [6][11][19][20][21] colourless elongated prisms
K4(PO2F2)2(S2O7) C2/c: a = 13.00 Å, b = 7.543 Å, c = 19.01 Å, β = 130.07°, Z = 4 [22]
Ca(PO2F2)2 · CH3COOCH2CH3 [23]
Ca(PO2F2)2 >345 °C d [5]
VO2PO2F2 [9]
CrO2(PO2F2)2 [24] formed from anhydride; red-brown
Cr(PO2F2)3 320, 385, 490, 575, 905, 955, 1165, 1255 cm−1 [24] formed from excess anhydride, green
Mn(CO)5PO2F2 184 °C [25]
HMn(PO2F2)3 [26] dissolve manganese in acid; white
(NH4)Mn3(PO2F2)(PO3F)2F2 [27]
Fe(PO2F2)2 463, 496, 668 (weak), 869 (double), 1139, 1290 cm−1 180 °C d [12] colour blue green, hygroscopic, melts 250 °C, above 300 °C starts decomposing to Fe3(PO4)2
Fe(PO2F2)3 262, 493, 528, 570, 914, 965, 1173, 1242 cm−1 >400 °C [7] decomposes at 230 °C yielding FeF3; dissolve iron in acid in presence of oxygen
KFe2(PO2F2)(PO3F)2F2 [27]
Co(PO2F2)2 173 °C [17] prepared from CoCl2 and acid; pink or blue; blue formed by heating pink to 140 °C
HCo(PO2F2)3 [26] dissolve cobalt in acid; red-purple
Co(PO2F2)2 · 2CH3CN orthorhombic: a = 9.227 Å, b = 13.871 Å, c = 9.471 Å, V = 1212 Å3, Z = 4, density = 1.88 g/cm3 [28] treat HCo(PO2F2)3 with MeCN for a few weeks; red crystals
(NH4)Co3(PO2F2)(PO3F)2F2 [27]
Ni(PO2F2)2 255 °C d [17] slowly prepared from NiCl2 and acid; yellow
HNi(PO2F2)3 [26] dissolve nickel in acid; yellow
Cu(PO2F2)2 orthorhombic Fddd: a = 10.134 Å, b = 24.49 Å, c = 34.06 Å, Z = 48, V = 8454.3 Å3, density = 2.50 g/cm3 265 °C d [5][28] 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 Å3 [29] colourless
Zn(PO2F2)2 c. 25 °C? [5] glassy
ZnH2(PO2F2)4 [8]
Ga(PO2F2)3 [30]
[(CH3)2GaPO2F2]2 dimeric 380, 492, 520, 551, 616, 709, 750, 899, 949, 1171, 1218, 1262, 1295, 1404, 2922, 2982 cm−1 [4][31]
RbPO2F2 orthorhombic: a = 8.15 Å, b = 6.45 Å, c = 7.79 Å, Z = 4, V = 409.5 Å3 density = 3.02 g/cm3 P–F stretching 827 and 946 cm−1; P–O stretching 1145 and 1320 cm−1 160 °C [6][11][20] white
Sr(PO2F2)2 250 °C d [17] prepared from SrCl2 and acid
AgPO2F2 [32]
Ag9(PO2F2)14 [27]
Ag(1-methyl-2-alkylthiomethyl-1H-benzimidazole)PO2F2 [32]
Ag(2,6-bis-[(2-methylthiophenyl)-2-azaethenyl]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 Å3, density = 1.81 g/cm3 [33]
Ag(4,4′-dicyanodiphenylacetylene)PO2F2
Cd(PO2F2)2 245 °C d [5]
In(PO2F2)3 269, 492, 528, 567, 910, 962, 1179, 1269 cm−1 [7] white, decomposes at 260 °C yielding InF3
[(CH3)2InPO2F2]2 dimeric 373, 490, 500, 535, 559, 735, 878, 925, 1128, 1179, 1275, 1435, 2928, 3000 cm−1 [31]
SnCl2(PO2F2)2 [34]
(CH3)2Sn(PO2F2)2 204 °C d [17] prepared from (CH3)2SnCl2 and acid; yellow
(C2H5)2Sn(PO2F2)2 262 °C d [17] prepared from (C2H5)2SnCl2 and acid; yellow
(n-C3H7)2Sn(PO2F2)2 245 °C d [17] prepared from (n-C3H7)2SnCl2 and acid; yellow
(n-C4H9)2Sn(PO2F2)2 235 °C d [17] prepared from (n-C4H9)2SnCl2 and acid; yellow
(n-C8H17)2Sn(PO2F2)2 114 °C [17] prepared from (n-C8H17)2SnCl2 and acid; yellow
SbCl4PO2F2 [34]
SbF4PO2F2 [34]
(2,2-dipyradyl)2Re(CO)2PO2F2 [35]
Au[bis(triphenylphosphine sulfide-S)]PO2F2 [36]
IO2PO2F2 Raman: 130, 163, 191, 219, 295, 323, 329, 378, 637, 713, 737, 781, 799, 839, 918, 1163cm−1 [37] yellowish colour, produced from , decomposed by water
IO3PO2F2 Raman: 217, 247, 269, 305, 343, 367, 395, 473, 569, 643, 671, 717, 797, 891, 1123cm−1 [37] yellowish colour, produced from H5IO6, decomposed by water
FXePO2F2 [38]
Xe(PO2F2)2 [38]
CsPO2F2 orthorhombic: a = 8.437 Å, b = 6.796 Å, c = 8.06 Å, Z = 4, V = 462.1 Å3, density = 3.36 g/cm3 286 °C [6][11][20]
Cs2Fe2(PO2F2)(PO2F)2F3 [27]
Ba(PO2F2)2 >400 °C [5]
Re(CO)5PO2F2 [35]
Hg(PO2F2)2 [5]
Hg2(PO2F2)2 Raman: 220 cm−1 [5] produced from anhydride
TlPO2F2 [5] produced from anhydride, or acid on TlCl
[(CH3)2TlPO2F2]2 dimeric 360, 374, 500, 505, 520, 559, 850, 880, 1120, 1140, 1195, 1250, 1285, 2932, 3020 cm−1 [31]
Pb(PO2F2)2 189 °C d [5]
UO2(PO2F2)2 260, 498, 854, 924, 980, 1124 cm−1 [9] IR spectrum due to UO2+
2
(C2H5)4NPO2F2 [39]
1-ethyl-3-methylimidazolium difluorophosphate [40] ionic liquid
1-butyl-3-methylimidazolium difluorophosphate [40] ionic liquid
1-butyl-1-methylpyrrolidinium difluorophosphate [40] ionic liquid
1-butyl-1-methylpiperidinium difluorophosphate [40] ionic liquid
di(3,3′,4,4′-tetramethyl-2,2′,5,5′-tetraselenafulvalenium)difluorophosphate [41] 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 Å3, Z = 4 [2][27] insoluble; yellow-brown
Strychnine PO2F2 [3]
Cocaine PO2F2 [3]
Brucine PO2F2 [3]
Morphine PO2F2 [3]
N(CH3)4PO2F2 [3]
HB(PO2F2)4 469, 502, 552, 647, 836, 940, 994, 1093, 1348, 1567 cm−1 [4] formed from BBr3 and acid; liquid
LiB(PO2F2)4 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−1 [4] formed from HB(PO2F2)4 and butyllithium; colourless
HS(CH3)2B(PO2F2)4 472, 511, 555, 648, 832, 933, 993, 1082, 1337, 1436, 2851, 2921, 3042 cm−1 [4] formed from BH3 · S(CH3)2 and acid; ionic liquid
[LiEtOEt]3Al(PO2F2)6 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−1 [4] formed from butyllithium and triethylaluminium and the acid; white
K2CrO2(PO2F2)4 305, 370, 485, 550, 870, 920, 1050, 1130, 1250 cm−1 145 °C d [24] formed from anhydride and K2CrO4; brown
Na2MoO2(PO2F2)4 amorphous 280, 490, 620, 880, 915, 950, 1020, 1070, 1140, 1280 cm−1 125 °C d [24] formed from anhydride and ; white
Na2WO2(PO2F2)4 amorphous 280, 474, 620, 930, 1030, 1130, 1230 cm−1 109 °C d [24] formed from anhydride and ; white

Related substances[]

Difluorphosphoric acid[]

Difluorphosphoric 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:[42]

POF3 + H2PO3F → 2HPO2F2

Difluorophosphoric acid can also be produced by fluorinating phosphorus oxychlorides. P2O3Cl4 and POCl3 react with hydrogen fluoride solution to yield HPO2Cl2 and then HPO2F2.[43] Yet another way is to treat orthophosphate (PO3−
4) with fluorosulfuric acid (HSO3F).[44]

Difluorphosphoric acid melts at −96.5 °C and boils at 115.9 °C. Its density at 25 °C is 1.583 g/cm3.[14]

Phosphoryl difluoride oxide[]

Difluorophosphoric acid anhydride also known as phosphoryl difluoride oxide or diphosphoryl tetrafluoride (F2OPOPOF2 or P2O3F4) is an anhydride of difluorphosphoric acid. It crystallises in the orthorhombic system, with space group Pcca and Z = 4.[45] P2O3F4 can be made by refluxing difluorophosphoric acid with phosphorus pentoxide. P2O3F4 boils at 71 °C.[46]

Substitution[]

In addition to the isoelectronic series, ions related by substituting fluorine or oxygen by other elements include monofluorophosphate, , , , , , , and .[47]

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.[48]

Amines can react with phosphoryl fluoride to make substances with a formula RR′N–POF2. 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 (RN=POF).[49]

References[]

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