Rubidium potassium hexa­fluorido­zirconate(IV) bis­(hydrogen fluoride), Rb_2−xK_xZrF₆·2HF (x = 0.4171)

The title compound is built from edge-sharing centrosymmetric dimeric [Zr₂F₁₂]⁴⁻ complexes, HF mol­ecules, Rb⁺ and K⁺ cations. Rubidium and potassium ions are statistically disordered on one of the metal positions. The Zr^IV coordination polyhedron is a monocapped trigonal prism. The two crystallographically independent Rb(K) ions are coordinated by F atoms and HF mol­ecules with coordination numbers 7 and 9, respectively, for the two sites. In addition, the structure is stabilized by strong F—H...F hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](r-F) = 0.001 Å
• Disorder in main residue
• R factor = 0.026
• wR factor = 0.061
• Data-to-parameter ratio = 20.5

checkCIF/PLATON results

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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
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..          ?
PLAT301_ALERT_3_C Main Residue  Disorder .........................      14.00 Perc.

Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          1

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   1 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
   2 ALERT type 3 Indicator that the structure quality may be low
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S1. Comment

This work is a continuation of the study of the structure and physicochemical properties of zirconium fluoride complexes with homo- and heteroatomic cations (Gerasimenko et al., 2006, 2007a, 2007b; Kavun et al., 2006) and deals with synthesis and crystal structure of rubidium–potassium hexafluoridozirconate(IV) di(hydrogen fluoride), Rb_{2 - x}K_xZrF₆·2HF (I) where x=0.4171. The asymmetric unit contains one Zr atom, six fluorine atoms, two sites of rubidium and potassium cations and two hydrogen fluoride molecules. The Zr atoms are coordinated by seven F atoms in a slightly distorted monocapped trigonal prism 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 3.6579 (4) Å. Along to the c direction, Zr- polyhedra pack up in columns (Fig. 2).

In this structure, there are two sites in which the outer-sphere rubidium and potassium cations are located. In each site the rubidium cations are statistically substituted by the potassium cations. According to the performed refinement, Rb/K site occupancy factors are equal to 0.8742 (7)/0.1258 for the Rb1/K1 site and 0.7087 (7)/0.2913 for the Rb2/K2 site. The coordination numbers (CN) of these sites were calculated by the method of intersecting spheres (Serezhkin et al., 1997) with use of the program package TOPOS (Blatov, 2004). For the first site (Fig. 3a), the CN is 9 (Rb1(K1)–F, 2.7609 (14) – 3.1054 (13) Å) and for the second site (Fig. 3 b), the CN is 7 (Rb2(K2)–F, 2.7584 (14) – 2.9094 (14) Å).

The HF molecules are involved as donors in strong hydrogen bonds (2.326 (2), 2.402 (2) and 2.326 (8) Å) with the F6ⁱⁱ and F4 atoms (Fig. 2). The F8 atom of HF molecule is split on two sites: F8a and F8b (Fig. 2, 3). The refined occupancy of the F8a and F8b sites are 0.790 (4) and 0.210 (4), respectively. Unfortunately, we did not manage to split the position of H2 atom, therefore, the angle of the hydrogen bond F8b–H2···F4 equal to139(4)° is unusual for strong hydrogen bonds.

Related literature

For related literature, see: Blatov (2004); Gerasimenko et al. (2006), Gerasimenko, Didenko & Kavun (2007); Gerasimenko, Kavun et al. (2007); Kavun et al. (2006); Serezhkin et al. (1997).

S2. Experimental

ZrO₂ (6.2 g, 0.05 mol; Reachem(Russia), 99.99% purity) was reacted with RbF (7.8 g, 0.075 mol; Alfa Aesar, 99.7% purity) and KF·2H₂O (2.4 g, 0.025 mol; Reachem(Russia), 99.99% purity) in a solution of hydrofluoric acid (40%, 30 ml; Reachem(Russia), 99.99% purity). Upon slow evaporation at room temperature, crystals of Rb_{5 - x}K_xZr₃F₁₇·0.5H₂O (x =2.0 and 2.25) precipitated first (later we will report about their crystal structures), and after they were separated, crystals of (I) precipitated next.

S3. Refinement

The Rb and K site occupancies were refined together with the refinement of the structural parameters of these atoms, assuming that their positional and thermal parameters were the same. The site-occupancy factors of F8a and F8b atoms were refined by restraining the sum of occupancies to 1.0. Their displacement parameters were constrained to be identical using the EADP instructions. The H atoms were found in a difference Fourier map and refined with U_iso(H) = 1.5U_eq(F). The maximum peak and deepest hole are located 0.79 Å and 0.72 Å, respectively, from Zr and F6.

Computing details

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

Figures

	Fig. 1. A view of the centrosymmetric dimeric [Zr2F12]^4- complex, with displacement ellipsoids drawn at the 50% probability level. Symmetry code as in Table 1.
	Fig. 2. The structure of (I), viewed along the c axis.
	Fig. 3. (a) The Rb1(K1) and (b) Rb2(K2) coordination polyhedra, with displacement ellipsoids drawn at the 50% probability level. Symmetry codes: ii: 1 - x, 1/2 + y, 1/2 - z; iv: 1 - x, 2 - y, -z; v: 1 - x, -1/2 + y, 1/2 - z; vi: 1 + x, 3/2 - y, -1/2 + z; vii: 1 + x, y, z; ix: x, -1 + y, z; x: 1 + x, -1 + y, z; xii: 1 - x, 1 - y, z.

Rubidium potassium hexafluoridozirconate(IV) bis(hydrogen fluoride)

Crystal data

Rb1.58K0.42ZrF6·2HF	F(000) = 722
Mr = 396.84	Dx = 3.425 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1764 reflections
a = 7.2427 (5) Å	θ = 2.8–31.3°
b = 11.7111 (8) Å	µ = 11.68 mm^−1
c = 9.0742 (6) Å	T = 173 K
β = 90.413 (2)°	Prism, colourless
V = 769.65 (9) Å^3	0.27 × 0.22 × 0.17 mm
Z = 4

Data collection

Bruker SMART 1000 CCD area-detector diffractometer	2437 independent reflections
Radiation source: fine-focus sealed tube	2223 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 8.33 pixels mm^-1	θmax = 31.5°, θmin = 2.8°
ω scans	h = −10→10
Absorption correction: gaussian (SADABS and XPREP; Bruker, 2003)	k = −17→16
Tmin = 0.176, Tmax = 0.444	l = −13→7
6082 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.026	Only H-atom coordinates refined
wR(F^2) = 0.061	w = 1/[σ^2(Fo^2) + (0.0216P)^2 + 0.8571P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.026
2437 reflections	Δρmax = 0.68 e Å^−3
119 parameters	Δρmin = −0.62 e Å^−3
1 restraint	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0034 (3)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Zr	0.13506 (2)	0.979721 (14)	0.169058 (18)	0.01248 (4)
Rb1	0.85934 (3)	0.681632 (16)	−0.00920 (2)	0.01949 (5)	0.8742 (7)
K1	0.85934 (3)	0.681632 (16)	−0.00920 (2)	0.01949 (5)	0.1258
Rb2	0.63267 (3)	0.14738 (2)	0.22385 (2)	0.02009 (6)	0.7087 (7)
K2	0.63267 (3)	0.14738 (2)	0.22385 (2)	0.02009 (6)	0.2913
F2	−0.05205 (17)	1.02431 (10)	0.31821 (13)	0.0210 (3)
F1	0.05701 (15)	0.91307 (9)	−0.04199 (12)	0.0172 (2)
F5	0.08382 (18)	0.81754 (10)	0.22501 (13)	0.0232 (3)
F6	0.2991 (2)	0.97382 (11)	0.36010 (14)	0.0300 (3)
F3	0.25829 (19)	1.13146 (11)	0.16978 (18)	0.0335 (3)
F4	0.37882 (18)	0.92093 (14)	0.08435 (16)	0.0360 (4)
F7	0.5434 (2)	0.17326 (12)	0.52128 (18)	0.0402 (4)
H1	0.593 (5)	0.121 (3)	0.560 (4)	0.060*
F8a	0.6904 (3)	0.8804 (2)	0.1602 (3)	0.0417 (6)	0.790 (4)
F8b	0.6467 (11)	0.8442 (8)	0.1869 (10)	0.040 (2)	0.210 (4)
H2	0.586 (5)	0.897 (3)	0.147 (4)	0.060*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zr	0.01345 (7)	0.01337 (7)	0.01059 (7)	0.00168 (6)	−0.00099 (6)	−0.00001 (6)
Rb1	0.02571 (10)	0.01514 (8)	0.01765 (9)	0.00183 (7)	0.00263 (7)	0.00237 (6)
K1	0.02571 (10)	0.01514 (8)	0.01765 (9)	0.00183 (7)	0.00263 (7)	0.00237 (6)
Rb2	0.01561 (10)	0.02453 (11)	0.02013 (11)	0.00128 (8)	0.00099 (8)	−0.00070 (8)
K2	0.01561 (10)	0.02453 (11)	0.02013 (11)	0.00128 (8)	0.00099 (8)	−0.00070 (8)
F2	0.0253 (6)	0.0220 (5)	0.0156 (5)	0.0044 (4)	0.0042 (4)	0.0006 (4)
F1	0.0210 (5)	0.0169 (5)	0.0138 (5)	0.0053 (4)	−0.0029 (4)	−0.0029 (4)
F5	0.0330 (6)	0.0160 (5)	0.0207 (6)	0.0031 (4)	0.0029 (5)	0.0033 (4)
F6	0.0370 (7)	0.0303 (6)	0.0226 (6)	0.0114 (5)	−0.0128 (5)	−0.0042 (5)
F3	0.0259 (6)	0.0244 (6)	0.0501 (8)	−0.0088 (5)	−0.0119 (6)	0.0105 (6)
F4	0.0154 (5)	0.0602 (9)	0.0324 (7)	0.0094 (6)	−0.0016 (5)	−0.0153 (6)
F7	0.0547 (9)	0.0300 (7)	0.0359 (8)	0.0137 (6)	−0.0158 (7)	0.0032 (6)
F8a	0.0205 (8)	0.0497 (12)	0.0547 (13)	0.0074 (8)	−0.0132 (8)	−0.0072 (10)
F8b	0.027 (4)	0.052 (5)	0.040 (4)	0.015 (3)	−0.012 (3)	−0.002 (3)

Geometric parameters (Å, º)

Zr—F3	1.9886 (13)	F1—Zr^i	2.1950 (11)
Zr—F2	1.9919 (12)	F1—K2^xii	2.8860 (11)
Zr—F5	2.0014 (11)	F1—Rb2^xii	2.8860 (11)
Zr—F4	2.0497 (13)	F1—Rb1^xiv	3.0806 (11)
Zr—F6	2.0958 (13)	F1—K1^xiv	3.0806 (11)
Zr—F1	2.1403 (11)	F5—K2^ii	2.8964 (12)
Zr—F1^i	2.1950 (11)	F5—Rb2^ii	2.8964 (12)
Zr—Zr^i	3.6579 (4)	F5—Rb1^iii	2.9183 (12)
Zr—K1^ii	3.8882 (3)	F5—K1^iii	2.9183 (12)
Zr—Rb1^ii	3.8882 (3)	F5—Rb1^xiv	3.1054 (13)
Zr—K1^iii	4.0207 (3)	F5—K1^xiv	3.1054 (13)
Zr—Rb1^iii	4.0207 (3)	F6—K1^ii	3.0156 (13)
Rb1—F3^iv	2.7609 (14)	F6—Rb1^ii	3.0156 (13)
Rb1—F2^v	2.8829 (12)	F6—K2^xv	3.3969 (15)
Rb1—F5^vi	2.9183 (13)	F6—Rb2^xv	3.3969 (15)
Rb1—F7^ii	2.9197 (18)	F3—K2^xv	2.7584 (14)
Rb1—F2^vi	2.9489 (12)	F3—Rb2^xv	2.7584 (14)
Rb1—F6^v	3.0156 (13)	F3—Rb1^iv	2.7609 (14)
Rb1—F8b	3.033 (9)	F3—K1^iv	2.7609 (14)
Rb1—F8a	3.051 (2)	F3—K1^ii	3.2550 (16)
Rb1—F1^vii	3.0806 (11)	F3—Rb1^ii	3.2550 (16)
Rb1—F5^vii	3.1054 (13)	F4—K2^xii	2.9094 (14)
Rb1—F8b^viii	3.164 (9)	F4—Rb2^xii	2.9094 (14)
Rb1—F3^v	3.2550 (16)	F4—Rb2^xv	3.4615 (16)
Rb2—F3^ix	2.7584 (14)	F7—K2^xvi	2.8621 (16)
Rb2—F7	2.7964 (17)	F7—Rb2^xvi	2.8621 (16)
Rb2—F2^x	2.8278 (12)	F7—Rb1^v	2.9197 (18)
Rb2—F7^xi	2.8621 (16)	F7—K1^v	2.9197 (18)
Rb2—F1^xii	2.8860 (11)	F7—H1	0.79 (4)
Rb2—F5^v	2.8964 (12)	F8a—F8b	0.583 (9)
Rb2—F4^xii	2.9094 (14)	F8a—K2^xv	3.207 (2)
Rb2—F8b^v	3.176 (9)	F8a—Rb2^xv	3.207 (2)
Rb2—F8a^ix	3.207 (2)	F8a—Rb1^xvii	3.313 (2)
Rb2—F6^ix	3.3969 (15)	F8a—K1^xvii	3.313 (2)
Rb2—F4^ix	3.4615 (16)	F8a—H2	0.79 (4)
Rb2—F8b^ix	3.568 (9)	F8b—K1^xvii	3.164 (9)
F2—K2^xiii	2.8278 (12)	F8b—Rb1^xvii	3.164 (9)
F2—Rb2^xiii	2.8278 (12)	F8b—K2^ii	3.176 (9)
F2—Rb1^ii	2.8829 (12)	F8b—Rb2^ii	3.176 (9)
F2—K1^ii	2.8829 (12)	F8b—Rb2^xv	3.568 (9)
F2—K1^iii	2.9489 (12)	F8b—H2	0.84 (4)
F2—Rb1^iii	2.9489 (12)
F3—Zr—F2	94.07 (6)	F8b^v—Rb2—F6^ix	83.42 (16)
F3—Zr—F5	158.63 (6)	F8a^ix—Rb2—F6^ix	64.92 (4)
F2—Zr—F5	87.03 (5)	F3^ix—Rb2—F4^ix	50.53 (4)
F3—Zr—F4	85.05 (6)	F7—Rb2—F4^ix	108.06 (4)
F2—Zr—F4	159.22 (5)	F2^x—Rb2—F4^ix	98.39 (3)
F5—Zr—F4	86.46 (6)	F7^xi—Rb2—F4^ix	102.15 (4)
F3—Zr—F6	77.00 (6)	F1^xii—Rb2—F4^ix	90.96 (3)
F2—Zr—F6	80.28 (5)	F5^v—Rb2—F4^ix	163.69 (3)
F5—Zr—F6	82.18 (5)	F4^xii—Rb2—F4^ix	55.00 (5)
F4—Zr—F6	79.30 (6)	F8b^v—Rb2—F4^ix	108.15 (15)
F3—Zr—F1	116.39 (6)	F8a^ix—Rb2—F4^ix	42.00 (4)
F2—Zr—F1	121.80 (5)	F6^ix—Rb2—F4^ix	45.37 (3)
F5—Zr—F1	80.36 (5)	F3^ix—Rb2—F8b^ix	86.82 (13)
F4—Zr—F1	76.38 (5)	F7—Rb2—F8b^ix	101.86 (15)
F6—Zr—F1	150.76 (5)	F2^x—Rb2—F8b^ix	59.86 (13)
F3—Zr—F1^i	76.90 (5)	F7^xi—Rb2—F8b^ix	132.56 (15)
F2—Zr—F1^i	77.01 (4)	F1^xii—Rb2—F8b^ix	71.30 (14)
F5—Zr—F1^i	123.92 (5)	F5^v—Rb2—F8b^ix	132.78 (13)
F4—Zr—F1^i	122.65 (5)	F4^xii—Rb2—F8b^ix	68.69 (15)
F6—Zr—F1^i	143.78 (5)	F8b^v—Rb2—F8b^ix	139.89 (13)
F1—Zr—F1^i	64.93 (5)	F8a^ix—Rb2—F8b^ix	7.76 (14)
F3—Zr—Zr^i	97.13 (4)	F6^ix—Rb2—F8b^ix	57.28 (14)
F2—Zr—Zr^i	99.99 (4)	F4^ix—Rb2—F8b^ix	38.61 (13)
F5—Zr—Zr^i	103.71 (4)	F3^ix—Rb2—H1	94.1 (7)
F4—Zr—Zr^i	100.72 (4)	F7—Rb2—H1	14.4 (7)
F6—Zr—Zr^i	174.11 (4)	F2^x—Rb2—H1	74.3 (7)
F1—Zr—Zr^i	32.93 (3)	F7^xi—Rb2—H1	133.4 (7)
F1^i—Zr—Zr^i	32.00 (3)	F1^xii—Rb2—H1	128.3 (7)
F3—Zr—K1^ii	56.76 (5)	F5^v—Rb2—H1	88.8 (7)
F2—Zr—K1^ii	45.93 (4)	F4^xii—Rb2—H1	157.3 (7)
F5—Zr—K1^ii	112.13 (4)	F8b^v—Rb2—H1	75.9 (7)
F4—Zr—K1^ii	119.86 (4)	F8a^ix—Rb2—H1	95.5 (7)
F6—Zr—K1^ii	50.27 (4)	F6^ix—Rb2—H1	60.6 (7)
F1—Zr—K1^ii	158.95 (3)	F4^ix—Rb2—H1	103.5 (7)
F1^i—Zr—K1^ii	94.13 (3)	F8b^ix—Rb2—H1	89.9 (7)
Zr^i—Zr—K1^ii	126.108 (8)	Zr—F2—K2^xiii	118.67 (5)
F3—Zr—Rb1^ii	56.76 (5)	Zr—F2—Rb2^xiii	118.67 (5)
F2—Zr—Rb1^ii	45.93 (4)	Zr—F2—Rb1^ii	104.31 (5)
F5—Zr—Rb1^ii	112.13 (4)	K2^xiii—F2—Rb1^ii	104.05 (4)
F4—Zr—Rb1^ii	119.86 (4)	Rb2^xiii—F2—Rb1^ii	104.05 (4)
F6—Zr—Rb1^ii	50.27 (4)	Zr—F2—K1^ii	104.31 (5)
F1—Zr—Rb1^ii	158.95 (3)	K2^xiii—F2—K1^ii	104.05 (4)
F1^i—Zr—Rb1^ii	94.13 (3)	Rb2^xiii—F2—K1^ii	104.05 (4)
Zr^i—Zr—Rb1^ii	126.108 (8)	Zr—F2—K1^iii	107.35 (5)
K1^ii—Zr—Rb1^ii	0.000 (4)	K2^xiii—F2—K1^iii	113.54 (4)
F3—Zr—K1^iii	130.00 (5)	Rb2^xiii—F2—K1^iii	113.54 (4)
F2—Zr—K1^iii	44.43 (3)	Rb1^ii—F2—K1^iii	108.04 (4)
F5—Zr—K1^iii	43.60 (4)	K1^ii—F2—K1^iii	108.04 (4)
F4—Zr—K1^iii	123.24 (5)	Zr—F2—Rb1^iii	107.35 (5)
F6—Zr—K1^iii	70.46 (4)	K2^xiii—F2—Rb1^iii	113.54 (4)
F1—Zr—K1^iii	110.42 (3)	Rb2^xiii—F2—Rb1^iii	113.54 (4)
F1^i—Zr—K1^iii	109.51 (3)	Rb1^ii—F2—Rb1^iii	108.04 (4)
Zr^i—Zr—K1^iii	113.868 (8)	K1^ii—F2—Rb1^iii	108.04 (4)
K1^ii—Zr—K1^iii	73.249 (7)	Zr—F1—Zr^i	115.07 (5)
Rb1^ii—Zr—K1^iii	73.249 (7)	Zr—F1—K2^xii	113.54 (4)
F3—Zr—Rb1^iii	130.00 (5)	Zr^i—F1—K2^xii	109.46 (4)
F2—Zr—Rb1^iii	44.43 (3)	Zr—F1—Rb2^xii	113.54 (4)
F5—Zr—Rb1^iii	43.60 (4)	Zr^i—F1—Rb2^xii	109.46 (4)
F4—Zr—Rb1^iii	123.24 (5)	Zr—F1—Rb1^xiv	110.76 (4)
F6—Zr—Rb1^iii	70.46 (4)	Zr^i—F1—Rb1^xiv	105.12 (4)
F1—Zr—Rb1^iii	110.42 (3)	K2^xii—F1—Rb1^xiv	101.76 (3)
F1^i—Zr—Rb1^iii	109.51 (3)	Rb2^xii—F1—Rb1^xiv	101.76 (3)
Zr^i—Zr—Rb1^iii	113.868 (8)	Zr—F1—K1^xiv	110.76 (4)
K1^ii—Zr—Rb1^iii	73.249 (7)	Zr^i—F1—K1^xiv	105.12 (4)
Rb1^ii—Zr—Rb1^iii	73.249 (7)	K2^xii—F1—K1^xiv	101.76 (3)
F3^iv—Rb1—F2^v	165.97 (4)	Rb2^xii—F1—K1^xiv	101.76 (3)
F3^iv—Rb1—F5^vi	74.50 (4)	Zr—F5—K2^ii	124.13 (6)
F2^v—Rb1—F5^vi	103.22 (3)	Zr—F5—Rb2^ii	124.13 (6)
F3^iv—Rb1—F7^ii	72.69 (4)	Zr—F5—Rb1^iii	108.18 (5)
F2^v—Rb1—F7^ii	118.71 (4)	K2^ii—F5—Rb1^iii	105.57 (4)
F5^vi—Rb1—F7^ii	122.10 (4)	Rb2^ii—F5—Rb1^iii	105.57 (4)
F3^iv—Rb1—F2^vi	115.83 (4)	Zr—F5—K1^iii	108.18 (5)
F2^v—Rb1—F2^vi	71.96 (4)	K2^ii—F5—K1^iii	105.57 (4)
F5^vi—Rb1—F2^vi	55.89 (3)	Rb2^ii—F5—K1^iii	105.57 (4)
F7^ii—Rb1—F2^vi	100.01 (4)	Zr—F5—Rb1^xiv	114.20 (5)
F3^iv—Rb1—F6^v	139.43 (4)	K2^ii—F5—Rb1^xiv	97.13 (3)
F2^v—Rb1—F6^v	53.04 (4)	Rb2^ii—F5—Rb1^xiv	97.13 (3)
F5^vi—Rb1—F6^v	126.13 (4)	Rb1^iii—F5—Rb1^xiv	105.98 (4)
F7^ii—Rb1—F6^v	66.82 (4)	K1^iii—F5—Rb1^xiv	105.98 (4)
F2^vi—Rb1—F6^v	70.32 (3)	Zr—F5—K1^xiv	114.20 (5)
F3^iv—Rb1—F8b	69.88 (18)	K2^ii—F5—K1^xiv	97.13 (3)
F2^v—Rb1—F8b	107.10 (17)	Rb2^ii—F5—K1^xiv	97.13 (3)
F5^vi—Rb1—F8b	140.44 (18)	Rb1^iii—F5—K1^xiv	105.98 (4)
F7^ii—Rb1—F8b	62.08 (17)	K1^iii—F5—K1^xiv	105.98 (4)
F2^vi—Rb1—F8b	159.74 (18)	Zr—F6—K1^ii	97.42 (5)
F6^v—Rb1—F8b	92.68 (18)	Zr—F6—Rb1^ii	97.42 (5)
F3^iv—Rb1—F8a	62.45 (6)	Zr—F6—K2^xv	94.57 (5)
F2^v—Rb1—F8a	112.27 (5)	K1^ii—F6—K2^xv	87.38 (3)
F5^vi—Rb1—F8a	129.92 (5)	Rb1^ii—F6—K2^xv	87.38 (3)
F7^ii—Rb1—F8a	68.92 (5)	Zr—F6—Rb2^xv	94.57 (5)
F2^vi—Rb1—F8a	168.91 (5)	K1^ii—F6—Rb2^xv	87.38 (3)
F6^v—Rb1—F8a	103.56 (5)	Rb1^ii—F6—Rb2^xv	87.38 (3)
F3^iv—Rb1—F1^vii	52.65 (3)	Zr—F3—K2^xv	120.10 (6)
F2^v—Rb1—F1^vii	113.39 (3)	Zr—F3—Rb2^xv	120.10 (6)
F5^vi—Rb1—F1^vii	69.83 (3)	Zr—F3—Rb1^iv	124.75 (6)
F7^ii—Rb1—F1^vii	119.39 (4)	K2^xv—F3—Rb1^iv	109.85 (4)
F2^vi—Rb1—F1^vii	124.42 (3)	Rb2^xv—F3—Rb1^iv	109.85 (4)
F6^v—Rb1—F1^vii	158.76 (3)	Zr—F3—K1^iv	124.75 (6)
F8b—Rb1—F1^vii	75.10 (18)	K2^xv—F3—K1^iv	109.85 (4)
F8a—Rb1—F1^vii	64.26 (5)	Rb2^xv—F3—K1^iv	109.85 (4)
F3^iv—Rb1—F5^vii	96.48 (4)	Zr—F3—K1^ii	92.52 (5)
F2^v—Rb1—F5^vii	70.57 (3)	K2^xv—F3—K1^ii	94.77 (4)
F5^vi—Rb1—F5^vii	105.77 (4)	Rb2^xv—F3—K1^ii	94.77 (4)
F7^ii—Rb1—F5^vii	124.11 (4)	Rb1^iv—F3—K1^ii	105.93 (4)
F2^vi—Rb1—F5^vii	131.90 (3)	K1^iv—F3—K1^ii	105.93 (4)
F6^v—Rb1—F5^vii	107.80 (3)	Zr—F3—Rb1^ii	92.52 (5)
F8b—Rb1—F5^vii	62.77 (16)	K2^xv—F3—Rb1^ii	94.77 (4)
F8a—Rb1—F5^vii	58.27 (4)	Rb2^xv—F3—Rb1^ii	94.77 (4)
F1^vii—Rb1—F5^vii	51.23 (3)	Rb1^iv—F3—Rb1^ii	105.93 (4)
F3^iv—Rb1—F8b^viii	57.94 (17)	K1^iv—F3—Rb1^ii	105.93 (4)
F2^v—Rb1—F8b^viii	133.92 (18)	Zr—F4—K2^xii	115.73 (6)
F5^vi—Rb1—F8b^viii	63.29 (16)	Zr—F4—Rb2^xii	115.73 (6)
F7^ii—Rb1—F8b^viii	58.94 (16)	Zr—F4—Rb2^xv	93.56 (5)
F2^vi—Rb1—F8b^viii	64.24 (18)	K2^xii—F4—Rb2^xv	125.00 (5)
F6^v—Rb1—F8b^viii	97.44 (16)	Rb2^xii—F4—Rb2^xv	125.00 (5)
F8b—Rb1—F8b^viii	109.0 (2)	Rb2—F7—K2^xvi	130.29 (6)
F8a—Rb1—F8b^viii	108.51 (18)	Rb2—F7—Rb2^xvi	130.29 (6)
F1^vii—Rb1—F8b^viii	102.92 (16)	Rb2—F7—Rb1^v	101.85 (5)
F5^vii—Rb1—F8b^viii	153.48 (17)	K2^xvi—F7—Rb1^v	102.74 (5)
F3^iv—Rb1—F3^v	124.10 (4)	Rb2^xvi—F7—Rb1^v	102.74 (5)
F2^v—Rb1—F3^v	56.27 (3)	Rb2—F7—K1^v	101.85 (5)
F5^vi—Rb1—F3^v	159.03 (4)	K2^xvi—F7—K1^v	102.74 (5)
F7^ii—Rb1—F3^v	76.19 (4)	Rb2^xvi—F7—K1^v	102.74 (5)
F2^vi—Rb1—F3^v	114.48 (3)	Rb2—F7—H1	104 (3)
F6^v—Rb1—F3^v	47.68 (3)	K2^xvi—F7—H1	100 (3)
F8b—Rb1—F3^v	54.60 (18)	Rb2^xvi—F7—H1	100 (3)
F8a—Rb1—F3^v	63.41 (5)	Rb1^v—F7—H1	120 (3)
F1^vii—Rb1—F3^v	112.03 (3)	K1^v—F7—H1	120 (3)
F5^vii—Rb1—F3^v	65.43 (3)	F8b—F8a—Rb1	82.8 (9)
F8b^viii—Rb1—F3^v	132.73 (15)	F8b—F8a—K2^xv	124.3 (9)
F3^ix—Rb2—F7	86.85 (5)	Rb1—F8a—K2^xv	152.61 (8)
F3^ix—Rb2—F2^x	144.10 (4)	F8b—F8a—Rb2^xv	124.3 (9)
F7—Rb2—F2^x	87.41 (4)	Rb1—F8a—Rb2^xv	152.61 (8)
F3^ix—Rb2—F7^xi	73.63 (5)	F8b—F8a—Rb1^xvii	70.3 (9)
F7—Rb2—F7^xi	119.18 (4)	Rb1—F8a—Rb1^xvii	98.15 (6)
F2^x—Rb2—F7^xi	138.31 (4)	K2^xv—F8a—Rb1^xvii	95.66 (6)
F3^ix—Rb2—F1^xii	130.57 (4)	Rb2^xv—F8a—Rb1^xvii	95.66 (6)
F7—Rb2—F1^xii	139.90 (4)	F8b—F8a—K1^xvii	70.3 (9)
F2^x—Rb2—F1^xii	54.38 (3)	Rb1—F8a—K1^xvii	98.15 (6)
F7^xi—Rb2—F1^xii	89.20 (4)	K2^xv—F8a—K1^xvii	95.66 (6)
F3^ix—Rb2—F5^v	140.34 (4)	Rb2^xv—F8a—K1^xvii	95.66 (6)
F7—Rb2—F5^v	86.53 (4)	F8b—F8a—H2	74 (3)
F2^x—Rb2—F5^v	74.46 (4)	Rb1—F8a—H2	120 (3)
F7^xi—Rb2—F5^v	75.80 (4)	K2^xv—F8a—H2	70 (3)
F1^xii—Rb2—F5^v	72.92 (3)	Rb2^xv—F8a—H2	70 (3)
F3^ix—Rb2—F4^xii	77.83 (4)	Rb1^xvii—F8a—H2	123 (3)
F7—Rb2—F4^xii	162.24 (5)	K1^xvii—F8a—H2	123 (3)
F2^x—Rb2—F4^xii	99.69 (4)	F8a—F8b—Rb1	86.2 (9)
F7^xi—Rb2—F4^xii	65.15 (4)	F8a—F8b—K1^xvii	99.7 (10)
F1^xii—Rb2—F4^xii	53.12 (3)	Rb1—F8b—K1^xvii	101.8 (2)
F5^v—Rb2—F4^xii	111.01 (4)	F8a—F8b—Rb1^xvii	99.7 (10)
F3^ix—Rb2—F8b^v	57.80 (15)	Rb1—F8b—Rb1^xvii	101.8 (2)
F7—Rb2—F8b^v	61.51 (17)	F8a—F8b—K2^ii	169.4 (11)
F2^x—Rb2—F8b^v	143.82 (16)	Rb1—F8b—K2^ii	91.2 (2)
F7^xi—Rb2—F8b^v	59.32 (17)	K1^xvii—F8b—K2^ii	90.9 (2)
F1^xii—Rb2—F8b^v	145.50 (16)	Rb1^xvii—F8b—K2^ii	90.9 (2)
F5^v—Rb2—F8b^v	84.96 (15)	F8a—F8b—Rb2^ii	169.4 (11)
F4^xii—Rb2—F8b^v	115.52 (16)	Rb1—F8b—Rb2^ii	91.2 (2)
F3^ix—Rb2—F8a^ix	91.79 (5)	K1^xvii—F8b—Rb2^ii	90.9 (2)
F7—Rb2—F8a^ix	108.11 (5)	Rb1^xvii—F8b—Rb2^ii	90.9 (2)
F2^x—Rb2—F8a^ix	56.75 (4)	F8a—F8b—Rb2^xv	47.9 (9)
F7^xi—Rb2—F8a^ix	128.97 (5)	Rb1—F8b—Rb2^xv	134.0 (3)
F1^xii—Rb2—F8a^ix	63.57 (4)	K1^xvii—F8b—Rb2^xv	91.6 (2)
F5^v—Rb2—F8a^ix	127.33 (4)	Rb1^xvii—F8b—Rb2^xv	91.6 (2)
F4^xii—Rb2—F8a^ix	64.00 (5)	K2^ii—F8b—Rb2^xv	132.8 (3)
F8b^v—Rb2—F8a^ix	146.87 (16)	Rb2^ii—F8b—Rb2^xv	132.8 (3)
F3^ix—Rb2—F6^ix	47.43 (4)	F8a—F8b—H2	65 (3)
F7—Rb2—F6^ix	62.84 (4)	Rb1—F8b—H2	118 (3)
F2^x—Rb2—F6^ix	99.19 (3)	K1^xvii—F8b—H2	134 (3)
F7^xi—Rb2—F6^ix	120.99 (4)	Rb1^xvii—F8b—H2	134 (3)
F1^xii—Rb2—F6^ix	128.33 (3)	K2^ii—F8b—H2	108 (3)
F5^v—Rb2—F6^ix	149.16 (3)	Rb2^ii—F8b—H2	108 (3)
F4^xii—Rb2—F6^ix	99.78 (4)	Rb2^xv—F8b—H2	45 (3)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
F7—H1···F6^xviii	0.79 (4)	1.54 (4)	2.326 (2)	176 (4)
F8a—H2···F4	0.79 (4)	1.62 (4)	2.402 (2)	168 (4)
F8b—H2···F4	0.84 (4)	1.62 (4)	2.326 (8)	139 (4)

Symmetry code: (xviii) −x+1, −y+1, −z+1.