Dipotassium hexa­fluoridozirconate(IV) hydrogen fluoride, K2ZrF6·HF

Gerasimenko, A.V.; Didenko, N.A.; Kavun, V.Y.

doi:10.1107/S160053680703615X

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Dipotassium hexafluoridozirconate(IV) hydrogen fluoride, K₂ZrF₆·HF

A. V. Gerasimenko, N. A. Didenko and V. Y. Kavun

The title compound is built from edge-sharing centrosymmetric dimeric [Zr₂F₁₂]⁴⁻ complexes, K⁺ cations and HF molecules. The Zr^IV coordination polyhedron is a distorted monocapped octahedron. The K⁺ ions are coordinated by F atoms and HF molecules with potassium coordination numbers of 7 and 8. In addition, the structure is stabilized by strong F—H

F hydrogen bonds.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680703615X/mg2031sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680703615X/mg2031Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 203 K
Mean (r-F) = 0.001 Å
R factor = 0.030
wR factor = 0.071
Data-to-parameter ratio = 55.5

checkCIF/PLATON results

No syntax errors found





Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.443     0.535
            Tmin and Tmax expected:      0.277     0.442
            RR =      1.321
            Please check that your absorption correction is appropriate.
PLAT794_ALERT_5_G Check Predicted Bond Valency for Zr          (4)       3.93

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

Comment top

The title compound, (I), is isostructural to K₂Rb₂(ZrF₆)₂^.2H₂O, (II), if hydrogen atoms are neglected (Tkachev et al., 1993). The asymmetric unit contains one crystallographically independent Zr atom, six fluorine atoms, two potassium cations and one hydrogen fluoride molecule. The Zr atoms are coordinated by seven F atoms in a distorted monocapped octahedral geometry. Two Zr-centred polyhedra are linked by double F bridges to form a centrosymmetric dimeric [Zr₂F₁₂]^4- complex (Fig. 1) with a Zr···Zrⁱ distance of 3.6810 (2) Å. Parallel to the ac plane, layers of K1 atoms and HF molecules alternate with layers of K2 atoms and [Zr₂F₁₂]^4- complexes (Fig. 2).

The coordination numbers (CN) of potassium atoms were calculated by the method of intersecting spheres (Serezhkin et al., 1997) with use of the program package TOPOS (Blatov, 2004). For K1, the CN is 8 (K1–F, 2.6214 (6)–2.9848 (9) Å) and for K2, the CN is 7 (K2–F, 2.6365 (6)–2.8774 (9) Å).

The HF molecule is coordinated to both potassium atoms and is involved as a donor in the strong hydrogen bond (2.3865 (10) Å) with the F6 atom (Fig. 2). Unlike the structure of (II), where the water molecule forms two hydrogen bonds with an F6 atom (2.88 Å) and a bridging F3 atom (2.74 Å) (Tkachev et al., 1993), in (I) there is only one hydrogen bond, resulting in a lengthened Zr–F6 bond (2.0790 (6) Å) and nearly equal Zr–F3 and Zr–F3ⁱ bridging bonds (2.1696 (6) and 2.1833 (6) Å). In (II), the corresponding bonds are 2.046, 2.188, and 2.199 Å, respectively (Tkachev et al., 1993).

Related literature top

For related literature, see: Blatov (2004); Serezhkin et al. (1997); Tkachev et al. (1993).

Experimental top

ZrO₂ (6.2 g, 0.05 mol) was reacted with KHF₂ (7.9 g, 0.1 mol) in a solution of hydrofluoric acid (40%, 30 ml). Upon slow evaporation at room temperature, crystals of K₂ZrF₆ precipitated first, and after they were separated, crystals of (I) precipitated next.

Structure description top

For related literature, see: Blatov (2004); Serezhkin et al. (1997); Tkachev et al. (1993).

Computing details top

Data collection: SMART (Bruker, 1998a); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1998b); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top

	Fig. 1. A view of the centrosymmetric dimeric [Zr₂F₁₂]^4- complex, with displacement ellipsoids drawn at the 50% probability level.
	Fig. 2. The structure of (I), viewed along the c axis.

Dipotassium hexafluoridozirconate(IV) hydrogen fluoride top

Crystal data top

K₂ZrF₆·HF	F(000) = 1136
M_r = 303.43	D_x = 3.093 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 1939 reflections
a = 13.3641 (5) Å	θ = 3.6–45.0°
b = 11.4457 (4) Å	µ = 3.03 mm⁻¹
c = 8.5211 (3) Å	T = 203 K
V = 1303.40 (8) Å³	Prism, colourless
Z = 8	0.44 × 0.37 × 0.27 mm

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	5275 independent reflections
Radiation source: fine-focus sealed tube	4834 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
Detector resolution: 8.33 pixels mm^-1	θ_max = 45.0°, θ_min = 3.1°
ω scans	h = −26→23
Absorption correction: gaussian (SADABS in XPREP; Bruker, 2003)	k = −20→22
T_min = 0.443, T_max = 0.535	l = −16→16
23595 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.030	Only H-atom coordinates refined
wR(F²) = 0.071	w = 1/[σ²(F_o²) + (0.0278P)² + 0.8258P] where P = (F_o² + 2F_c²)/3
S = 1.21	(Δ/σ)_max = 0.003
5275 reflections	Δρ_max = 1.58 e Å⁻³
95 parameters	Δρ_min = −1.30 e Å⁻³
0 restraints	Extinction correction: SHELXTL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0049 (2)

Crystal data top

K₂ZrF₆·HF	V = 1303.40 (8) Å³
M_r = 303.43	Z = 8
Orthorhombic, Pbca	Mo Kα radiation
a = 13.3641 (5) Å	µ = 3.03 mm⁻¹
b = 11.4457 (4) Å	T = 203 K
c = 8.5211 (3) Å	0.44 × 0.37 × 0.27 mm

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	5275 independent reflections
Absorption correction: gaussian (SADABS in XPREP; Bruker, 2003)	4834 reflections with I > 2σ(I)
T_min = 0.443, T_max = 0.535	R_int = 0.030
23595 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.030	0 restraints
wR(F²) = 0.071	Only H-atom coordinates refined
S = 1.21	Δρ_max = 1.58 e Å⁻³
5275 reflections	Δρ_min = −1.30 e Å⁻³
95 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Zr	0.118901 (5)	0.040452 (6)	0.094477 (8)	0.00846 (1)
K1	0.170769 (16)	0.740441 (15)	0.84850 (2)	0.01749 (3)
K2	0.106835 (15)	0.06846 (2)	0.61088 (3)	0.01853 (3)
F1	0.08118 (5)	−0.02918 (5)	0.30531 (7)	0.01728 (10)
F2	0.20020 (4)	−0.10800 (5)	0.07447 (7)	0.01528 (9)
F3	0.04308 (4)	−0.06348 (6)	−0.08217 (8)	0.02043 (11)
F4	0.25374 (5)	0.09337 (6)	0.16899 (10)	0.02846 (15)
F5	0.15406 (7)	0.12846 (7)	−0.09782 (8)	0.02574 (14)
F6	0.08494 (5)	0.19919 (5)	0.20043 (8)	0.02147 (12)
F7	−0.03330 (6)	0.18673 (8)	0.40966 (9)	0.02981 (17)
H1	0.0108 (18)	0.198 (2)	0.335 (3)	0.045*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zr	0.00841 (2)	0.00835 (2)	0.00861 (3)	−0.00061 (2)	−0.00108 (2)	0.00001 (2)
K1	0.02166 (7)	0.01343 (5)	0.01738 (7)	−0.00241 (5)	0.00038 (5)	−0.00296 (5)
K2	0.01207 (6)	0.02388 (7)	0.01963 (7)	0.00100 (5)	−0.00039 (5)	−0.00405 (6)
F1	0.0187 (2)	0.0189 (2)	0.0143 (2)	0.00307 (17)	0.00298 (17)	0.00444 (16)
F2	0.01427 (19)	0.01355 (17)	0.0180 (2)	0.00254 (15)	−0.00253 (16)	−0.00328 (15)
F3	0.01218 (19)	0.0261 (2)	0.0230 (2)	0.00429 (18)	−0.00479 (17)	−0.01411 (19)
F4	0.0159 (2)	0.0211 (2)	0.0483 (4)	−0.00098 (19)	−0.0129 (3)	−0.0108 (3)
F5	0.0333 (3)	0.0260 (3)	0.0179 (3)	−0.0053 (3)	0.0052 (2)	0.0075 (2)
F6	0.0268 (3)	0.01294 (18)	0.0247 (3)	−0.00303 (18)	0.0042 (2)	−0.00626 (18)
F7	0.0254 (3)	0.0383 (4)	0.0258 (3)	0.0039 (3)	0.0074 (2)	−0.0036 (3)

Geometric parameters (Å, º) top

Zr—F5	1.9799 (7)	K2—F4^xiv	2.6735 (7)
Zr—F4	2.0043 (7)	K2—F6^x	2.7822 (7)
Zr—F2	2.0241 (5)	K2—F1	2.8541 (6)
Zr—F1	2.0290 (6)	K2—F7	2.8774 (9)
Zr—F6	2.0790 (6)	K2—F7^v	3.0867 (10)
Zr—F3	2.1696 (6)	K2—F3^xv	3.1381 (7)
Zr—F3ⁱ	2.1833 (6)	K2—K2^v	3.7657 (4)
Zr—K2ⁱⁱ	3.8740 (2)	K2—Zr^xiv	3.8740 (2)
Zr—K1ⁱⁱⁱ	3.9373 (2)	K2—K1^xvi	4.0997 (3)
Zr—K1^iv	4.0823 (2)	F1—K2^v	2.6506 (7)
Zr—K2^v	4.1180 (2)	F1—K1ⁱⁱⁱ	2.7232 (6)
Zr—K2^vi	4.1364 (3)	F2—K1^iv	2.6214 (6)
K1—F2^vii	2.6214 (6)	F2—K2ⁱⁱ	2.6365 (6)
K1—F4^viii	2.6411 (7)	F2—K1ⁱⁱⁱ	2.8115 (6)
K1—F5^ix	2.7079 (8)	F3—Zrⁱ	2.1833 (6)
K1—F1^x	2.7232 (6)	F3—K1^iv	2.8805 (7)
K1—F2^x	2.8115 (6)	F3—K2^vi	3.1381 (7)
K1—F7^xi	2.8284 (8)	F4—K1^xvii	2.6411 (7)
K1—F3^vii	2.8805 (7)	F4—K2ⁱⁱ	2.6735 (7)
K1—F7^xii	2.9848 (9)	F4—K1^xviii	3.3629 (9)
K1—F4^ix	3.3629 (9)	F5—K2^vi	2.6517 (7)
K1—Zr^x	3.9373 (2)	F5—K1^xviii	2.7079 (8)
K1—Zr^vii	4.0823 (2)	F6—K2ⁱⁱⁱ	2.7822 (6)
K1—K2^xiii	4.0997 (3)	F7—K1^xix	2.8284 (8)
K2—F2^xiv	2.6365 (6)	F7—K1^xii	2.9848 (9)
K2—F1^v	2.6506 (7)	F7—K2^v	3.0867 (10)
K2—F5^xv	2.6517 (7)

F5—Zr—F4	83.98 (4)	F7^xi—K1—Zr^vii	72.45 (2)
F5—Zr—F2	103.30 (3)	F3^vii—K1—Zr^vii	30.543 (12)
F4—Zr—F2	78.33 (3)	F7^xii—K1—Zr^vii	92.234 (18)
F5—Zr—F1	172.54 (3)	F4^ix—K1—Zr^vii	93.154 (13)
F4—Zr—F1	93.53 (3)	Zr^x—K1—Zr^vii	159.923 (6)
F2—Zr—F1	83.00 (2)	F2^vii—K1—K2^xiii	124.870 (15)
F5—Zr—F6	88.09 (3)	F4^viii—K1—K2^xiii	77.459 (17)
F4—Zr—F6	78.15 (3)	F5^ix—K1—K2^xiii	39.595 (15)
F2—Zr—F6	152.55 (3)	F1^x—K1—K2^xiii	79.959 (14)
F1—Zr—F6	84.52 (3)	F2^x—K1—K2^xiii	39.604 (12)
F5—Zr—F3	79.37 (3)	F7^xi—K1—K2^xiii	136.58 (2)
F4—Zr—F3	143.64 (3)	F3^vii—K1—K2^xiii	154.800 (16)
F2—Zr—F3	74.45 (2)	F7^xii—K1—K2^xiii	102.494 (16)
F1—Zr—F3	106.43 (3)	F4^ix—K1—K2^xiii	86.747 (13)
F6—Zr—F3	132.73 (3)	Zr^x—K1—K2^xiii	57.592 (4)
F5—Zr—F3ⁱ	97.71 (3)	Zr^vii—K1—K2^xiii	141.310 (6)
F4—Zr—F3ⁱ	150.48 (3)	F2^xiv—K2—F1^v	171.13 (2)
F2—Zr—F3ⁱ	129.02 (2)	F2^xiv—K2—F5^xv	80.38 (2)
F1—Zr—F3ⁱ	81.00 (3)	F1^v—K2—F5^xv	90.99 (2)
F6—Zr—F3ⁱ	72.48 (3)	F2^xiv—K2—F4^xiv	57.253 (19)
F3—Zr—F3ⁱ	64.52 (3)	F1^v—K2—F4^xiv	119.55 (2)
F5—Zr—K2ⁱⁱ	88.23 (3)	F5^xv—K2—F4^xiv	80.80 (3)
F4—Zr—K2ⁱⁱ	40.11 (2)	F2^xiv—K2—F6^x	88.34 (2)
F2—Zr—K2ⁱⁱ	39.196 (16)	F1^v—K2—F6^x	89.34 (2)
F1—Zr—K2ⁱⁱ	94.399 (18)	F5^xv—K2—F6^x	61.36 (2)
F6—Zr—K2ⁱⁱ	118.17 (2)	F4^xiv—K2—F6^x	133.22 (2)
F3—Zr—K2ⁱⁱ	106.885 (17)	F2^xiv—K2—F1	94.437 (19)
F3ⁱ—Zr—K2ⁱⁱ	168.149 (19)	F1^v—K2—F1	93.756 (18)
F5—Zr—K1ⁱⁱⁱ	145.96 (2)	F5^xv—K2—F1	169.73 (2)
F4—Zr—K1ⁱⁱⁱ	85.09 (2)	F4^xiv—K2—F1	88.93 (2)
F2—Zr—K1ⁱⁱⁱ	42.802 (17)	F6^x—K2—F1	127.72 (2)
F1—Zr—K1ⁱⁱⁱ	40.202 (17)	F2^xiv—K2—F7	119.06 (2)
F6—Zr—K1ⁱⁱⁱ	120.88 (2)	F1^v—K2—F7	67.88 (2)
F3—Zr—K1ⁱⁱⁱ	90.912 (19)	F5^xv—K2—F7	126.22 (3)
F3ⁱ—Zr—K1ⁱⁱⁱ	107.430 (19)	F4^xiv—K2—F7	152.86 (3)
K2ⁱⁱ—Zr—K1ⁱⁱⁱ	63.310 (5)	F6^x—K2—F7	69.22 (2)
F5—Zr—K1^iv	87.86 (2)	F1—K2—F7	64.05 (2)
F4—Zr—K1^iv	105.32 (2)	F2^xiv—K2—F7^v	117.85 (2)
F2—Zr—K1^iv	32.804 (16)	F1^v—K2—F7^v	63.44 (2)
F1—Zr—K1^iv	99.579 (17)	F5^xv—K2—F7^v	111.96 (2)
F6—Zr—K1^iv	174.36 (2)	F4^xiv—K2—F7^v	64.96 (2)
F3—Zr—K1^iv	42.430 (17)	F6^x—K2—F7^v	152.45 (2)
F3ⁱ—Zr—K1^iv	104.196 (17)	F1—K2—F7^v	62.582 (19)
K2ⁱⁱ—Zr—K1^iv	65.620 (5)	F7—K2—F7^v	101.78 (2)
K1ⁱⁱⁱ—Zr—K1^iv	64.248 (3)	F2^xiv—K2—F3^xv	116.502 (18)
F5—Zr—K2^v	146.34 (3)	F1^v—K2—F3^xv	55.698 (17)
F4—Zr—K2^v	123.85 (3)	F5^xv—K2—F3^xv	53.77 (2)
F2—Zr—K2^v	100.980 (17)	F4^xiv—K2—F3^xv	72.63 (2)
F1—Zr—K2^v	32.783 (18)	F6^x—K2—F3^xv	101.703 (19)
F6—Zr—K2^v	80.783 (19)	F1—K2—F3^xv	122.639 (18)
F3—Zr—K2^v	85.118 (18)	F7—K2—F3^xv	123.12 (2)
F3ⁱ—Zr—K2^v	48.660 (19)	F7^v—K2—F3^xv	60.360 (19)
K2ⁱⁱ—Zr—K2^v	125.009 (5)	F2^xiv—K2—K2^v	138.945 (17)
K1ⁱⁱⁱ—Zr—K2^v	63.039 (5)	F1^v—K2—K2^v	49.139 (14)
K1^iv—Zr—K2^v	100.533 (5)	F5^xv—K2—K2^v	139.29 (2)
F5—Zr—K2^vi	31.28 (2)	F4^xiv—K2—K2^v	109.46 (2)
F4—Zr—K2^vi	109.10 (3)	F6^x—K2—K2^v	117.109 (18)
F2—Zr—K2^vi	90.120 (17)	F1—K2—K2^v	44.617 (13)
F1—Zr—K2^vi	154.536 (18)	F7—K2—K2^v	53.362 (19)
F6—Zr—K2^vi	110.88 (2)	F7^v—K2—K2^v	48.418 (16)
F3—Zr—K2^vi	48.175 (19)	F3^xv—K2—K2^v	90.694 (14)
F3ⁱ—Zr—K2^vi	84.499 (17)	F2^xiv—K2—Zr^xiv	29.024 (12)
K2ⁱⁱ—Zr—K2^vi	95.611 (5)	F1^v—K2—Zr^xiv	148.434 (15)
K1ⁱⁱⁱ—Zr—K2^vi	128.158 (5)	F5^xv—K2—Zr^xiv	83.797 (19)
K1^iv—Zr—K2^vi	63.915 (5)	F4^xiv—K2—Zr^xiv	28.880 (14)
K2^v—Zr—K2^vi	127.033 (4)	F6^x—K2—Zr^xiv	114.644 (16)
F2^vii—K1—F4^viii	83.77 (2)	F1—K2—Zr^xiv	87.405 (13)
F2^vii—K1—F5^ix	93.40 (2)	F7—K2—Zr^xiv	138.215 (17)
F4^viii—K1—F5^ix	96.23 (2)	F7^v—K2—Zr^xiv	89.697 (17)
F2^vii—K1—F1^x	138.84 (2)	F3^xv—K2—Zr^xiv	97.590 (12)
F4^viii—K1—F1^x	136.82 (2)	K2^v—K2—Zr^xiv	124.431 (9)
F5^ix—K1—F1^x	89.00 (2)	F2^xiv—K2—K1^xvi	42.828 (13)
F2^vii—K1—F2^x	161.06 (2)	F1^v—K2—K1^xvi	129.466 (15)
F4^viii—K1—F2^x	81.60 (2)	F5^xv—K2—K1^xvi	40.607 (18)
F5^ix—K1—F2^x	76.358 (19)	F4^xiv—K2—K1^xvi	74.689 (18)
F1^x—K1—F2^x	58.032 (17)	F6^x—K2—K1^xvi	58.790 (16)
F2^vii—K1—F7^xi	72.91 (2)	F1—K2—K1^xvi	136.521 (14)
F4^viii—K1—F7^xi	145.75 (3)	F7—K2—K1^xvi	122.70 (2)
F5^ix—K1—F7^xi	109.61 (2)	F7^v—K2—K1^xvi	135.492 (17)
F1^x—K1—F7^xi	67.66 (2)	F3^xv—K2—K1^xvi	90.930 (13)
F2^x—K1—F7^xi	125.37 (2)	K2^v—K2—K1^xvi	175.841 (10)
F2^vii—K1—F3^vii	54.737 (17)	Zr^xiv—K2—K1^xvi	59.097 (4)
F4^viii—K1—F3^vii	77.52 (2)	Zr—F1—K2^v	122.73 (3)
F5^ix—K1—F3^vii	147.81 (2)	Zr—F1—K1ⁱⁱⁱ	111.05 (2)
F1^x—K1—F3^vii	117.33 (2)	K2^v—F1—K1ⁱⁱⁱ	103.28 (2)
F2^x—K1—F3^vii	132.321 (18)	Zr—F1—K2	128.62 (3)
F7^xi—K1—F3^vii	68.60 (2)	K2^v—F1—K2	86.244 (18)
F2^vii—K1—F7^xii	116.68 (2)	K1ⁱⁱⁱ—F1—K2	99.88 (2)
F4^viii—K1—F7^xii	66.87 (2)	Zr—F2—K1^iv	122.47 (3)
F5^ix—K1—F7^xii	142.08 (2)	Zr—F2—K2ⁱⁱ	111.78 (2)
F1^x—K1—F7^xii	82.98 (2)	K1^iv—F2—K2ⁱⁱ	110.29 (2)
F2^x—K1—F7^xii	67.95 (2)	Zr—F2—K1ⁱⁱⁱ	107.91 (2)
F7^xi—K1—F7^xii	101.41 (3)	K1^iv—F2—K1ⁱⁱⁱ	103.432 (19)
F3^vii—K1—F7^xii	64.47 (2)	K2ⁱⁱ—F2—K1ⁱⁱⁱ	97.567 (19)
F2^vii—K1—F4^ix	71.922 (18)	Zr—F3—Zrⁱ	115.48 (3)
F4^viii—K1—F4^ix	135.74 (3)	Zr—F3—K1^iv	107.03 (2)
F5^ix—K1—F4^ix	50.694 (19)	Zrⁱ—F3—K1^iv	132.19 (3)
F1^x—K1—F4^ix	78.296 (19)	Zr—F3—K2^vi	100.81 (2)
F2^x—K1—F4^ix	111.259 (18)	Zrⁱ—F3—K2^vi	99.85 (2)
F7^xi—K1—F4^ix	59.63 (2)	K1^iv—F3—K2^vi	92.473 (18)
F3^vii—K1—F4^ix	113.649 (19)	Zr—F4—K1^xvii	138.12 (3)
F7^xii—K1—F4^ix	157.36 (2)	Zr—F4—K2ⁱⁱ	111.01 (3)
F2^vii—K1—Zr^x	166.072 (14)	K1^xvii—F4—K2ⁱⁱ	109.88 (2)
F4^viii—K1—Zr^x	109.69 (2)	Zr—F4—K1^xviii	99.42 (3)
F5^ix—K1—Zr^x	81.870 (17)	K1^xvii—F4—K1^xviii	89.73 (2)
F1^x—K1—Zr^x	28.747 (13)	K2ⁱⁱ—F4—K1^xviii	89.27 (2)
F2^x—K1—Zr^x	29.286 (11)	Zr—F5—K2^vi	125.91 (4)
F7^xi—K1—Zr^x	96.241 (19)	Zr—F5—K1^xviii	125.86 (4)
F3^vii—K1—Zr^x	130.140 (14)	K2^vi—F5—K1^xviii	99.80 (2)
F7^xii—K1—Zr^x	73.412 (18)	Zr—F6—K2ⁱⁱⁱ	133.89 (3)
F4^ix—K1—Zr^x	95.194 (13)	K1^xix—F7—K2	95.21 (2)
F2^vii—K1—Zr^vii	24.729 (12)	K1^xix—F7—K1^xii	94.38 (3)
F4^viii—K1—Zr^vii	75.902 (18)	K2—F7—K1^xii	166.20 (3)
F5^ix—K1—Zr^vii	117.271 (17)	K1^xix—F7—K2^v	92.30 (2)
F1^x—K1—Zr^vii	137.870 (15)	K2—F7—K2^v	78.22 (2)
F2^x—K1—Zr^vii	154.647 (13)	K1^xii—F7—K2^v	91.52 (2)

Symmetry codes: (i) −x, −y, −z; (ii) −x+1/2, −y, z−1/2; (iii) x, −y+1/2, z−1/2; (iv) x, y−1, z−1; (v) −x, −y, −z+1; (vi) x, y, z−1; (vii) x, y+1, z+1; (viii) −x+1/2, −y+1, z+1/2; (ix) −x+1/2, y+1/2, z+1; (x) x, −y+1/2, z+1/2; (xi) −x, y+1/2, −z+3/2; (xii) −x, −y+1, −z+1; (xiii) −x+1/2, y+1/2, z; (xiv) −x+1/2, −y, z+1/2; (xv) x, y, z+1; (xvi) −x+1/2, y−1/2, z; (xvii) −x+1/2, −y+1, z−1/2; (xviii) −x+1/2, y−1/2, z−1; (xix) −x, y−1/2, −z+3/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
F7—H1···F6	0.87 (2)	1.52 (2)	2.3865 (10)	172 (2)

Experimental details

Crystal data
Chemical formula	K₂ZrF₆·HF
M_r	303.43
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	203
a, b, c (Å)	13.3641 (5), 11.4457 (4), 8.5211 (3)
V (Å³)	1303.40 (8)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	3.03
Crystal size (mm)	0.44 × 0.37 × 0.27

Data collection
Diffractometer	Bruker SMART 1000 CCD area-detector
Absorption correction	Gaussian (SADABS in XPREP; Bruker, 2003)
T_min, T_max	0.443, 0.535
No. of measured, independent and observed [I > 2σ(I)] reflections	23595, 5275, 4834
R_int	0.030
(sin θ/λ)_max (Å⁻¹)	0.995

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.030, 0.071, 1.21
No. of reflections	5275
No. of parameters	95
H-atom treatment	Only H-atom coordinates refined
Δρ_max, Δρ_min (e Å⁻³)	1.58, −1.30

Computer programs: SMART (Bruker, 1998a), SAINT (Bruker, 2003), SAINT, SHELXTL (Bruker, 1998b), SHELXTL.

Selected bond lengths (Å) top

Zr—F5	1.9799 (7)	K1—F2^v	2.8115 (6)
Zr—F4	2.0043 (7)	K1—F7^vi	2.8284 (8)
Zr—F2	2.0241 (5)	K1—F3ⁱⁱ	2.8805 (7)
Zr—F1	2.0290 (6)	K1—F7^vii	2.9848 (9)
Zr—F6	2.0790 (6)	K2—F2^viii	2.6365 (6)
Zr—F3	2.1696 (6)	K2—F1^ix	2.6506 (7)
Zr—F3ⁱ	2.1833 (6)	K2—F5^x	2.6517 (7)
K1—F2ⁱⁱ	2.6214 (6)	K2—F4^viii	2.6735 (7)
K1—F4ⁱⁱⁱ	2.6411 (7)	K2—F6^v	2.7822 (7)
K1—F5^iv	2.7079 (8)	K2—F1	2.8541 (6)
K1—F1^v	2.7232 (6)	K2—F7	2.8774 (9)

Symmetry codes: (i) −x, −y, −z; (ii) x, y+1, z+1; (iii) −x+1/2, −y+1, z+1/2; (iv) −x+1/2, y+1/2, z+1; (v) x, −y+1/2, z+1/2; (vi) −x, y+1/2, −z+3/2; (vii) −x, −y+1, −z+1; (viii) −x+1/2, −y, z+1/2; (ix) −x, −y, −z+1; (x) x, y, z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
F7—H1···F6	0.87 (2)	1.52 (2)	2.3865 (10)	172 (2)

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