Tetra­potassium dianti­mony(III) tin(IV) tetra­deca­fluoride

Gerasimenko, A.V.; Merkulov, E.B.; Usol'tseva, T.I.

doi:10.1107/S1600536808012865

inorganic compounds

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Volume 64| Part 6| June 2008| Page i32

doi:10.1107/S1600536808012865

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Tetrapotassium diantimony(III) tin(IV) tetradecafluoride

A. V. Gerasimenko,^a ^* E. B. Merkulov ^a and T. I. Usol'tseva ^a

^aInstitute of Chemistry FEB RAS, 159 prospekt 100-letiya Vladivostoka, Vladivostok 690022, Russian Federation
^*Correspondence e-mail: gerasimenko@ich.dvo.ru

(Received 28 April 2008; accepted 1 May 2008; online 7 May 2008)

The title compound, K₄Sb₂SnF₁₄, is built from anionic layers, with an overall composition of [Sb₂SnF₁₄]⁴⁻ extending parallel to the ac plane, and K⁺ cations. The layers are made up from vertex-sharing centrosymmetric SnF₆ octahedra and Sb₂F₁₂ dimers. The Sn—F distances are in the range 1.9581 (14)–1.9611 (17) Å. The Sb polyhedra contain three short terminal Sb—F bonds [1.9380 (14)–2.0696 (15) Å], one short bridging bond [2.0609 (17) Å], one bridging bond of medium length [2.7516 (15) Å], and two longer bridging bonds [3.0471 (18) and 3.117 (2) Å]. The K⁺ ions are coordinated by F atoms with coordination numbers 10 and 8, and K—F bond lengths are in the range 2.6235 (16)–3.122 (2) Å.

Related literature

For related literature, see: Blatov (2004 ); Davidovich & Zemnukhova (1975 ); Gillespie (1970 ); Kriegsmann & Kessler (1962 ); Serezhkin et al. (1997 ).

Experimental

Crystal data

K₄Sb₂SnF₁₄
M_r = 784.59
Triclinic, $[P \overline 1]$
a = 6.7356 (2) Å
b = 7.4704 (2) Å
c = 7.6370 (2) Å
α = 92.691 (1)°
β = 91.461 (1)°
γ = 115.323 (1)°
V = 346.53 (2) Å³
Z = 1
Mo Kα radiation
μ = 7.00 mm⁻¹
T = 298 (2) K
0.4 × 0.35 × 0.28 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer
Absorption correction: Gaussian (XPREP and SADABS; Bruker, 2003 ) T_min = 0.136, T_max = 0.291
7147 measured reflections
4635 independent reflections
4250 reflections with I > 2σ(I)
R_int = 0.024

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.090
S = 1.30
4635 reflections
98 parameters
Δρ_max = 1.91 e Å⁻³
Δρ_min = −3.69 e Å⁻³

Table 1
Selected bond lengths (Å)

Sb—F1	1.9380 (14)
Sb—F3	1.9539 (13)
Sb—F4	2.0609 (17)
Sb—F2	2.0696 (15)
Sb—F4ⁱ	2.7516 (15)
Sb—F5ⁱⁱ	3.0471 (18)
Sb—F6	3.117 (2)
Sn—F5	1.9581 (14)
Sn—F7	1.9611 (17)
Sn—F6	1.9611 (16)
K1—F4^iv	2.6235 (16)
K1—F2	2.7086 (14)
K1—F1^v	2.7268 (16)
K1—F6^vi	2.811 (2)
K1—F3^iv	2.8390 (18)
K1—F5^iv	2.8578 (16)
K1—F1	2.9262 (15)
K1—F3	2.9485 (18)
K1—F4^vi	2.982 (2)
K1—F7^vi	3.122 (2)
K2—F2^vii	2.6662 (15)
K2—F2^v	2.6777 (18)
K2—F3^iv	2.7136 (15)
K2—F1	2.7216 (15)
K2—F7^viii	2.7620 (19)
K2—F7^ix	2.8795 (17)
K2—F6ⁱ	2.8943 (16)
K2—F5^iv	2.9912 (18)
Symmetry codes: (i) -x+1, -y, -z+1; (ii) x-1, y, z; (iii) -x+2, -y, -z; (iv) -x+2, -y+1, -z+1; (v) -x+1, -y+1, -z+1; (vi) x, y+1, z; (vii) x, y, z+1; (viii) -x+2, -y, -z+1; (ix) x, y+1, z+1.

Data collection: SMART (Bruker, 1998 ); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: publCIF (Westrip, 2008 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808012865/fi2062sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808012865/fi2062Isup2.hkl

checkCIF report

Comment top

The asymmetric unit of the title compound, K₄Sb₂SnF₁₄, (I), contains one crystallographically independent Sb atom, one Sn atom on a special position (Wyckoff position 1a), seven fluorine atoms and two potassium cations. The Sn atoms are coordinated by six F atoms in a centrosymmetric, slightly distorted octahedral environment (Fig. 1a), with Sn—F distances ranging from 1.9581 (14) to 1.9611 (17) Å (Table 1). The nearest environment of the Sb atom is formed by four fluorine atoms with Sb—F bond distances ranging from 1.9380 (14) to 2.0696 (15) Å. Taking into account a lone electron pair (E), the coordination polyhedron of Sb(III) can be described as a trigonal bipyramid (Gillespie, 1970). Three fluorine atoms, F4ⁱ, F5ⁱⁱ and F6, are involved in the second coordination sphere of Sb with Sb—F bond distances of 2.7516 (15), 3.0471 (18) and 3.117 (2) Å, respectively. Two Sb polyhedra are linked by double fluorine bridges (F4 and F4ⁱ) to form a centrosymmetric dimer (Fig. 1 b), with an Sb···Sbⁱ distance of 3.9925 (2) Å.

The Sn(IV) and Sb(III) complexes are bound via fluorine bridges yielding the anionic layers [Sb₂SnF₁₄]^4- parallel to the ac plane (Fig. 2), with Sn···Sb distances of 4.21660 (15) and 4.33908 (16) Å. Such layers alternate with layers of potassium cations (Fig.3).

The coordination numbers (CN) of the potassium cations were calculated by the method of intersecting spheres (Serezhkin et al., 1997) with use of the program package TOPOS (Blatov, 2004). For the K1 (Fig. 4a), the CN is 10 [K1—F, 2.6235 (16) – 3.122 (2) Å] and for the K2 (Fig. 4 b), the CN is 8 [K2—F, 2.6662 (15) – 2.9912 (18) Å].

Related literature top

For related literature, see: Blatov (2004); Davidovich & Zemnukhova (1975); Gillespie (1970); Kriegsmann & Kessler (1962); Serezhkin et al. (1997).

Experimental top

KSbF₄ (5.94 g, 0.025 mol) was reacted with K₂SnF₆.H₂O (8.21 g, 0.025 mol) in a solution of hydrofluoric acid (10%, 200 ml; Reachem(Russia), 99.99% purity). The solution obtained was evaporated in air at room temperature down to 1/3 of the initial volume. Then the precipitate was separated from solution and dried to constant weight (1.98 g). The complexes KSbF₄ and K₂SnF₆.H₂O were prepared according to (Davidovich & Zemnukhova, 1975; Kriegsmann & Kessler, 1962).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top

	Fig. 1. (a) the Sn and (b) Sb coordination polyhedra, with displacement ellipsoids drawn at the 50% probability level. Symmetry codes are given in Table 1.
	Fig. 2. Fragment of the anionic layer [Sb₂SnF₁₄]^4- viewed along the b axis.
	Fig. 3. The structure of (I), viewed along the a axis. Sn octahedra are shown as dotted, Sb dimers as parallel lines and K atoms as white spheres.
	Fig. 4. (a) the K1 and (b) K2 coordination polyhedra, with displacement ellipsoids drawn at the 50% probability level. Symmetry codes are given in Table 1.

Tetrapotassium diantimony(III) tin(IV) tetradecafluoride top

Crystal data top

K₄Sb₂SnF₁₄	Z = 1
M_r = 784.59	F(000) = 354
Triclinic, P1	D_x = 3.760 Mg m⁻³
a = 6.7356 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 7.4704 (2) Å	Cell parameters from 2472 reflections
c = 7.6370 (2) Å	θ = 3.4–46.9°
α = 92.691 (1)°	µ = 7.00 mm⁻¹
β = 91.461 (1)°	T = 298 K
γ = 115.323 (1)°	Prism, colourless
V = 346.53 (2) Å³	0.4 × 0.35 × 0.28 mm

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	4635 independent reflections
Radiation source: fine-focus sealed tube	4250 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
Detector resolution: 8.33 pixels mm^-1	θ_max = 47.0°, θ_min = 3.4°
ϕ and ω scans	h = −9→13
Absorption correction: gaussian (XPREP and SADABS; Bruker, 2003)	k = −15→9
T_min = 0.136, T_max = 0.291	l = −15→11
7147 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.037	w = 1/[σ²(F_o²) + (0.0258P)² + 0.7101P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.090	(Δ/σ)_max = 0.003
S = 1.30	Δρ_max = 1.91 e Å⁻³
4635 reflections	Δρ_min = −3.69 e Å⁻³
98 parameters	Extinction correction: SHELXTL (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0782 (13)

Crystal data top

K₄Sb₂SnF₁₄	γ = 115.323 (1)°
M_r = 784.59	V = 346.53 (2) Å³
Triclinic, P1	Z = 1
a = 6.7356 (2) Å	Mo Kα radiation
b = 7.4704 (2) Å	µ = 7.00 mm⁻¹
c = 7.6370 (2) Å	T = 298 K
α = 92.691 (1)°	0.4 × 0.35 × 0.28 mm
β = 91.461 (1)°

Data collection top

Bruker SMART 1000 CCD area-detector diffractometer	4635 independent reflections
Absorption correction: gaussian (XPREP and SADABS; Bruker, 2003)	4250 reflections with I > 2σ(I)
T_min = 0.136, T_max = 0.291	R_int = 0.024
7147 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	98 parameters
wR(F²) = 0.090	0 restraints
S = 1.30	Δρ_max = 1.91 e Å⁻³
4635 reflections	Δρ_min = −3.69 e Å⁻³

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
Sb	0.611210 (19)	0.191057 (16)	0.312309 (15)	0.01531 (2)
Sn	1.0000	0.0000	0.0000	0.01467 (3)
K1	0.85162 (7)	0.73682 (7)	0.41457 (6)	0.02301 (9)
K2	0.71347 (7)	0.44513 (8)	0.85599 (6)	0.02309 (8)
F1	0.5699 (2)	0.3363 (2)	0.51424 (18)	0.0247 (3)
F2	0.5990 (2)	0.4270 (2)	0.18860 (19)	0.0237 (3)
F3	0.9214 (2)	0.3796 (2)	0.3294 (2)	0.0252 (3)
F4	0.7266 (2)	0.0671 (2)	0.5021 (2)	0.0300 (3)
F5	1.1417 (3)	0.1313 (2)	0.22704 (19)	0.0297 (3)
F6	0.7209 (3)	−0.1279 (3)	0.1151 (2)	0.0332 (4)
F7	1.0620 (3)	−0.2265 (2)	0.0506 (2)	0.0322 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sb	0.01754 (4)	0.01469 (4)	0.01477 (4)	0.00794 (3)	0.00034 (3)	0.00109 (3)
Sn	0.01815 (5)	0.01411 (5)	0.01377 (5)	0.00878 (4)	0.00109 (4)	0.00153 (4)
K1	0.01943 (14)	0.02305 (16)	0.02459 (16)	0.00756 (12)	−0.00196 (13)	0.00015 (13)
K2	0.02202 (15)	0.02791 (16)	0.02086 (15)	0.01186 (12)	0.00175 (13)	0.00452 (13)
F1	0.0254 (5)	0.0286 (5)	0.0191 (5)	0.0108 (4)	0.0045 (4)	−0.0032 (4)
F2	0.0302 (5)	0.0201 (4)	0.0233 (5)	0.0131 (4)	−0.0020 (5)	0.0048 (4)
F3	0.0174 (4)	0.0274 (6)	0.0294 (6)	0.0079 (4)	0.0038 (4)	0.0046 (5)
F4	0.0215 (5)	0.0312 (6)	0.0363 (7)	0.0093 (5)	−0.0031 (5)	0.0159 (5)
F5	0.0381 (6)	0.0344 (6)	0.0195 (5)	0.0197 (5)	−0.0083 (5)	−0.0074 (5)
F6	0.0254 (6)	0.0395 (8)	0.0323 (7)	0.0105 (5)	0.0098 (5)	0.0086 (6)
F7	0.0449 (7)	0.0240 (5)	0.0353 (7)	0.0226 (5)	−0.0084 (6)	0.0009 (5)

Geometric parameters (Å, º) top

Sb—F1	1.9380 (14)	K2—F2^xi	2.6777 (18)
Sb—F3	1.9539 (13)	K2—F3^v	2.7136 (15)
Sb—F4	2.0609 (17)	K2—F1	2.7216 (15)
Sb—F2	2.0696 (15)	K2—F7^xv	2.7620 (19)
Sb—F4ⁱ	2.7516 (15)	K2—F7^xvi	2.8795 (17)
Sb—F5ⁱⁱ	3.0471 (18)	K2—F6ⁱ	2.8943 (16)
Sb—F6	3.117 (2)	K2—F5^v	2.9912 (18)
Sb—F7ⁱⁱⁱ	3.5325 (19)	K2—F6^xvi	3.655 (2)
Sb—K1	3.7207 (5)	K2—Sn^xvi	3.8388 (5)
Sb—F6^iv	3.8032 (18)	K2—F4	3.847 (2)
Sb—F5	3.8531 (19)	K2—K1^xi	3.9388 (7)
Sb—F1ⁱ	3.9018 (16)	K2—F3^xiv	3.9710 (17)
Sb—K1^v	3.9464 (5)	K2—Sb^xiv	3.9808 (5)
Sb—K2^vi	3.9808 (5)	K2—K2^xvii	3.9938 (10)
Sb—Sbⁱ	3.9925 (2)	K2—K2^xviii	4.1352 (10)
Sn—F5	1.9581 (14)	K2—F1^xi	4.1386 (18)
Sn—F5ⁱⁱⁱ	1.9581 (14)	K2—K1^v	4.2602 (8)
Sn—F7ⁱⁱⁱ	1.9611 (17)	K2—Sb^xi	4.3692 (6)
Sn—F7	1.9611 (17)	F1—K1^xi	2.7268 (16)
Sn—F6ⁱⁱⁱ	1.9611 (16)	F1—Sbⁱ	3.9018 (16)
Sn—F6	1.9611 (16)	F1—K2^xi	4.1386 (18)
Sn—K1^vii	3.7354 (5)	F1—Sb^xi	4.3632 (17)
Sn—K1^viii	3.7354 (5)	F2—K2^vi	2.6662 (15)
Sn—K2^ix	3.8388 (5)	F2—K2^xi	2.6777 (18)
Sn—K2^v	3.8388 (5)	F3—K2^v	2.7136 (14)
Sb—Sn	4.2166 (2)	F3—K1^v	2.8390 (18)
Sn—Sbⁱⁱⁱ	4.2166 (2)	F3—K2^vi	3.9710 (17)
Sn—Sb^iv	4.3391 (2)	F3—Sb^v	4.2172 (14)
Sn—Sb^x	4.3391 (2)	F4—K1^v	2.6235 (15)
K1—F4^v	2.6235 (16)	F4—Sbⁱ	2.7516 (15)
K1—F2	2.7086 (14)	F4—K1^viii	2.982 (2)
K1—F1^xi	2.7268 (16)	F5—K1^v	2.8578 (16)
K1—F6^xii	2.811 (2)	F5—K2^v	2.9912 (18)
K1—F3^v	2.8390 (18)	F5—Sb^x	3.0471 (18)
K1—F5^v	2.8578 (16)	F5—K1^viii	3.1882 (17)
K1—F1	2.9262 (15)	F5—Sb^xv	4.9869 (18)
K1—F3	2.9485 (18)	F6—K1^viii	2.811 (2)
K1—F4^xii	2.982 (2)	F6—K2ⁱ	2.8943 (16)
K1—F7^xii	3.122 (2)	F6—K2^ix	3.655 (2)
K1—F5^xii	3.1882 (17)	F6—Sb^iv	3.8032 (18)
K1—K1^xiii	3.7178 (9)	F6—Sbⁱ	4.9129 (17)
K1—Sn^xii	3.7354 (5)	F6—Sb^viii	5.124 (2)
K1—K2^xi	3.9388 (7)	F7—K2^xv	2.7620 (19)
K1—Sb^v	3.9464 (5)	F7—K2^ix	2.8795 (16)
K1—Sb^xi	4.0028 (5)	F7—K1^viii	3.1222 (19)
K1—K2	4.0117 (7)	F7—Sbⁱⁱⁱ	3.5325 (19)
K1—K2^v	4.2602 (8)	F7—Sb^x	4.0712 (16)
K1—Sb^xii	4.4308 (6)	F7—Sb^viii	4.6870 (16)
K2—F2^xiv	2.6662 (15)

F1—Sb—F3	87.64 (6)	Sn^xii—K1—K2^v	70.956 (11)
F1—Sb—F4	82.57 (7)	K2^xi—K1—K2^v	110.414 (15)
F3—Sb—F4	80.01 (6)	Sb^v—K1—K2^v	64.623 (11)
F1—Sb—F2	80.77 (6)	Sb^xi—K1—K2^v	170.056 (15)
F3—Sb—F2	79.13 (6)	K2—K1—K2^v	106.442 (15)
F4—Sb—F2	153.71 (6)	F4^v—K1—Sb^xii	105.98 (4)
F1—Sb—F4ⁱ	71.19 (6)	F2—K1—Sb^xii	103.48 (4)
F3—Sb—F4ⁱ	143.84 (6)	F1^xi—K1—Sb^xii	60.65 (4)
F4—Sb—F4ⁱ	68.69 (6)	F6^xii—K1—Sb^xii	44.34 (4)
F2—Sb—F4ⁱ	123.67 (6)	F3^v—K1—Sb^xii	142.69 (4)
F1—Sb—F5ⁱⁱ	80.34 (5)	F5^v—K1—Sb^xii	83.36 (4)
F3—Sb—F5ⁱⁱ	145.85 (6)	F1—K1—Sb^xii	123.89 (4)
F4—Sb—F5ⁱⁱ	129.10 (5)	F3—K1—Sb^xii	155.13 (3)
F2—Sb—F5ⁱⁱ	67.49 (5)	F4^xii—K1—Sb^xii	23.27 (3)
F4ⁱ—Sb—F5ⁱⁱ	60.42 (5)	F7^xii—K1—Sb^xii	92.88 (4)
F1—Sb—F6	156.26 (6)	F5^xii—K1—Sb^xii	58.05 (4)
F3—Sb—F6	91.23 (6)	K1^xiii—K1—Sb^xii	57.132 (15)
F4—Sb—F6	73.89 (6)	Sb—K1—Sb^xii	132.635 (13)
F2—Sb—F6	122.29 (5)	Sn^xii—K1—Sb^xii	61.479 (8)
F4ⁱ—Sb—F6	96.84 (5)	K2^xi—K1—Sb^xii	63.210 (12)
F5ⁱⁱ—Sb—F6	112.19 (4)	Sb^v—K1—Sb^xii	127.696 (11)
F1—Sb—F7ⁱⁱⁱ	144.50 (5)	Sb^xi—K1—Sb^xii	56.236 (8)
F3—Sb—F7ⁱⁱⁱ	60.78 (5)	K2—K1—Sb^xii	121.076 (15)
F4—Sb—F7ⁱⁱⁱ	105.41 (6)	K2^v—K1—Sb^xii	132.216 (14)
F2—Sb—F7ⁱⁱⁱ	77.82 (5)	F2^xiv—K2—F2^xi	83.28 (5)
F4ⁱ—Sb—F7ⁱⁱⁱ	144.19 (5)	F2^xiv—K2—F3^v	138.86 (5)
F5ⁱⁱ—Sb—F7ⁱⁱⁱ	116.08 (4)	F2^xi—K2—F3^v	116.46 (5)
F6—Sb—F7ⁱⁱⁱ	49.35 (4)	F2^xiv—K2—F1	145.86 (5)
F1—Sb—K1	51.20 (4)	F2^xi—K2—F1	75.98 (5)
F3—Sb—K1	51.92 (5)	F3^v—K2—F1	75.22 (4)
F4—Sb—K1	108.38 (5)	F2^xiv—K2—F7^xv	85.87 (5)
F2—Sb—K1	45.52 (4)	F2^xi—K2—F7^xv	163.17 (5)
F4ⁱ—Sb—K1	121.51 (4)	F3^v—K2—F7^xv	80.02 (5)
F5ⁱⁱ—Sb—K1	97.07 (3)	F1—K2—F7^xv	107.02 (6)
F6—Sb—K1	140.19 (3)	F2^xiv—K2—F7^xvi	73.56 (5)
F7ⁱⁱⁱ—Sb—K1	94.15 (3)	F2^xi—K2—F7^xvi	103.37 (5)
F1—Sb—F6^iv	119.92 (6)	F3^v—K2—F7^xvi	67.03 (5)
F3—Sb—F6^iv	118.94 (5)	F1—K2—F7^xvi	137.34 (5)
F4—Sb—F6^iv	149.10 (6)	F7^xv—K2—F7^xvi	85.75 (5)
F2—Sb—F6^iv	56.92 (5)	F2^xiv—K2—F6ⁱ	69.80 (5)
F4ⁱ—Sb—F6^iv	97.15 (4)	F2^xi—K2—F6ⁱ	68.66 (5)
F5ⁱⁱ—Sb—F6^iv	46.60 (4)	F3^v—K2—F6ⁱ	149.54 (5)
F6—Sb—F6^iv	81.11 (5)	F1—K2—F6ⁱ	77.45 (5)
F7ⁱⁱⁱ—Sb—F6^iv	69.52 (4)	F7^xv—K2—F6ⁱ	95.51 (6)
K1—Sb—F6^iv	102.43 (3)	F7^xvi—K2—F6ⁱ	143.13 (5)
F1—Sb—F5	124.91 (5)	F2^xiv—K2—F5^v	105.63 (5)
F3—Sb—F5	47.69 (6)	F2^xi—K2—F5^v	62.58 (5)
F4—Sb—F5	62.29 (5)	F3^v—K2—F5^v	61.36 (5)
F2—Sb—F5	112.55 (5)	F1—K2—F5^v	88.59 (5)
F4ⁱ—Sb—F5	123.65 (5)	F7^xv—K2—F5^v	133.22 (5)
F5ⁱⁱ—Sb—F5	154.74 (5)	F7^xvi—K2—F5^v	56.44 (5)
F6—Sb—F5	44.86 (4)	F6ⁱ—K2—F5^v	131.19 (6)
F7ⁱⁱⁱ—Sb—F5	43.91 (4)	F2^xiv—K2—F6^xvi	57.19 (4)
K1—Sb—F5	99.51 (3)	F2^xi—K2—F6^xvi	58.00 (4)
F6^iv—Sb—F5	110.73 (4)	F3^v—K2—F6^xvi	101.14 (4)
F1—Sb—F1ⁱ	101.60 (5)	F1—K2—F6^xvi	126.75 (5)
F3—Sb—F1ⁱ	119.88 (6)	F7^xv—K2—F6^xvi	124.94 (5)
F4—Sb—F1ⁱ	43.93 (5)	F7^xvi—K2—F6^xvi	47.89 (5)
F2—Sb—F1ⁱ	160.78 (5)	F6ⁱ—K2—F6^xvi	105.87 (4)
F4ⁱ—Sb—F1ⁱ	42.52 (5)	F5^v—K2—F6^xvi	48.52 (4)
F5ⁱⁱ—Sb—F1ⁱ	93.92 (4)	F2^xiv—K2—Sn^xvi	80.82 (3)
F6—Sb—F1ⁱ	58.86 (4)	F2^xi—K2—Sn^xvi	75.59 (3)
F7ⁱⁱⁱ—Sb—F1ⁱ	107.93 (3)	F3^v—K2—Sn^xvi	71.04 (4)
K1—Sb—F1ⁱ	147.81 (2)	F1—K2—Sn^xvi	118.69 (4)
F6^iv—Sb—F1ⁱ	107.05 (3)	F7^xv—K2—Sn^xvi	115.30 (4)
F5—Sb—F1ⁱ	82.00 (3)	F7^xvi—K2—Sn^xvi	29.81 (4)
F1—Sb—K1^v	83.19 (5)	F6ⁱ—K2—Sn^xvi	135.57 (4)
F3—Sb—K1^v	42.71 (5)	F5^v—K2—Sn^xvi	30.19 (3)
F4—Sb—K1^v	37.30 (4)	F6^xvi—K2—Sn^xvi	30.21 (2)
F2—Sb—K1^v	120.02 (4)	F2^xiv—K2—F4	134.72 (4)
F4ⁱ—Sb—K1^v	104.20 (4)	F2^xi—K2—F4	116.59 (4)
F5ⁱⁱ—Sb—K1^v	160.47 (3)	F3^v—K2—F4	70.89 (4)
F6—Sb—K1^v	79.99 (3)	F1—K2—F4	43.32 (5)
F7ⁱⁱⁱ—Sb—K1^v	83.45 (3)	F7^xv—K2—F4	63.76 (5)
K1—Sb—K1^v	80.495 (13)	F7^xvi—K2—F4	131.42 (5)
F6^iv—Sb—K1^v	152.92 (3)	F6ⁱ—K2—F4	80.07 (5)
F5—Sb—K1^v	42.97 (2)	F5^v—K2—F4	119.65 (4)
F1ⁱ—Sb—K1^v	79.15 (2)	F6^xvi—K2—F4	167.89 (4)
F1—Sb—K2^vi	117.92 (5)	Sn^xvi—K2—F4	141.35 (3)
F3—Sb—K2^vi	75.50 (5)	F2^xiv—K2—K1^xi	103.45 (4)
F4—Sb—K2^vi	146.86 (5)	F2^xi—K2—K1^xi	43.32 (3)
F2—Sb—K2^vi	37.79 (4)	F3^v—K2—K1^xi	115.64 (4)
F4ⁱ—Sb—K2^vi	140.23 (4)	F1—K2—K1^xi	43.76 (3)
F5ⁱⁱ—Sb—K2^vi	82.15 (3)	F7^xv—K2—K1^xi	128.37 (4)
F6—Sb—K2^vi	84.58 (3)	F7^xvi—K2—K1^xi	145.82 (4)
F7ⁱⁱⁱ—Sb—K2^vi	42.62 (3)	F6ⁱ—K2—K1^xi	45.47 (4)
K1—Sb—K2^vi	72.944 (11)	F5^v—K2—K1^xi	93.55 (3)
F6^iv—Sb—K2^vi	43.58 (2)	F6^xvi—K2—K1^xi	101.07 (3)
F5—Sb—K2^vi	84.66 (3)	Sn^xvi—K2—K1^xi	116.309 (16)
F1ⁱ—Sb—K2^vi	138.75 (2)	F4—K2—K1^xi	75.33 (3)
K1^v—Sb—K2^vi	115.096 (10)	F2^xiv—K2—F3^xiv	39.66 (4)
F1—Sb—Sbⁱ	73.20 (5)	F2^xi—K2—F3^xiv	121.93 (4)
F3—Sb—Sbⁱ	117.83 (5)	F3^v—K2—F3^xiv	106.25 (4)
F4—Sb—Sbⁱ	39.94 (4)	F1—K2—F3^xiv	155.67 (5)
F2—Sb—Sbⁱ	147.66 (4)	F7^xv—K2—F3^xiv	50.88 (5)
F4ⁱ—Sb—Sbⁱ	28.74 (4)	F7^xvi—K2—F3^xiv	59.33 (4)
F5ⁱⁱ—Sb—Sbⁱ	89.16 (3)	F6ⁱ—K2—F3^xiv	93.31 (4)
F6—Sb—Sbⁱ	86.50 (3)	F5^v—K2—F3^xiv	113.77 (4)
F7ⁱⁱⁱ—Sb—Sbⁱ	134.11 (3)	F6^xvi—K2—F3^xiv	77.30 (4)
K1—Sb—Sbⁱ	121.530 (9)	Sn^xvi—K2—F3^xiv	83.69 (2)
F6^iv—Sb—Sbⁱ	121.92 (2)	F4—K2—F3^xiv	113.32 (4)
F5—Sb—Sbⁱ	98.15 (3)	K1^xi—K2—F3^xiv	137.39 (2)
F1ⁱ—Sb—Sbⁱ	28.39 (2)	F2^xiv—K2—Sb^xiv	28.40 (3)
K1^v—Sb—Sbⁱ	76.021 (8)	F2^xi—K2—Sb^xiv	106.25 (3)
K2^vi—Sb—Sbⁱ	164.150 (8)	F3^v—K2—Sb^xiv	132.62 (4)
F5—Sn—F5ⁱⁱⁱ	180.00 (5)	F1—K2—Sb^xiv	137.36 (3)
F5—Sn—F7ⁱⁱⁱ	90.26 (7)	F7^xv—K2—Sb^xiv	59.99 (4)
F5ⁱⁱⁱ—Sn—F7ⁱⁱⁱ	89.74 (7)	F7^xvi—K2—Sb^xiv	84.57 (4)
F5—Sn—F7	89.74 (7)	F6ⁱ—K2—Sb^xiv	64.94 (4)
F5ⁱⁱⁱ—Sn—F7	90.26 (7)	F5^v—K2—Sb^xiv	131.15 (3)
F7ⁱⁱⁱ—Sn—F7	180.00 (14)	F6^xvi—K2—Sb^xiv	84.19 (3)
F5—Sn—F6ⁱⁱⁱ	91.07 (7)	Sn^xvi—K2—Sb^xiv	102.504 (11)
F5ⁱⁱⁱ—Sn—F6ⁱⁱⁱ	88.93 (7)	F4—K2—Sb^xiv	107.92 (3)
F7ⁱⁱⁱ—Sn—F6ⁱⁱⁱ	88.84 (8)	K1^xi—K2—Sb^xiv	109.172 (12)
F7—Sn—F6ⁱⁱⁱ	91.16 (8)	F3^xiv—K2—Sb^xiv	28.449 (19)
F5—Sn—F6	88.93 (7)	F2^xiv—K2—K2^xvii	41.75 (4)
F5ⁱⁱⁱ—Sn—F6	91.07 (7)	F2^xi—K2—K2^xvii	41.53 (3)
F7ⁱⁱⁱ—Sn—F6	91.16 (8)	F3^v—K2—K2^xvii	143.27 (4)
F7—Sn—F6	88.84 (8)	F1—K2—K2^xvii	112.96 (4)
F6ⁱⁱⁱ—Sn—F6	180.00 (16)	F7^xv—K2—K2^xvii	126.42 (4)
F5—Sn—K1^vii	121.41 (5)	F7^xvi—K2—K2^xvii	88.06 (4)
F5ⁱⁱⁱ—Sn—K1^vii	58.59 (5)	F6ⁱ—K2—K2^xvii	61.68 (4)
F7ⁱⁱⁱ—Sn—K1^vii	56.67 (6)	F5^v—K2—K2^xvii	82.59 (4)
F7—Sn—K1^vii	123.33 (6)	F6^xvi—K2—K2^xvii	44.19 (3)
F6ⁱⁱⁱ—Sn—K1^vii	47.50 (6)	Sn^xvi—K2—K2^xvii	74.136 (15)
F6—Sn—K1^vii	132.50 (6)	F4—K2—K2^xvii	140.33 (3)
F5—Sn—K1^viii	58.59 (5)	K1^xi—K2—K2^xvii	70.576 (15)
F5ⁱⁱⁱ—Sn—K1^viii	121.41 (5)	F3^xiv—K2—K2^xvii	80.83 (3)
F7ⁱⁱⁱ—Sn—K1^viii	123.33 (6)	Sb^xiv—K2—K2^xvii	66.445 (12)
F7—Sn—K1^viii	56.67 (6)	F2^xiv—K2—K1	149.45 (4)
F6ⁱⁱⁱ—Sn—K1^viii	132.50 (6)	F2^xi—K2—K1	74.53 (3)
F6—Sn—K1^viii	47.50 (6)	F3^v—K2—K1	44.99 (4)
K1^vii—Sn—K1^viii	180.000 (14)	F1—K2—K1	46.84 (3)
F5—Sn—K2^ix	129.80 (5)	F7^xv—K2—K1	119.96 (4)
F5ⁱⁱⁱ—Sn—K2^ix	50.20 (5)	F7^xvi—K2—K1	91.21 (4)
F7ⁱⁱⁱ—Sn—K2^ix	133.12 (5)	F6ⁱ—K2—K1	118.92 (4)
F7—Sn—K2^ix	46.88 (5)	F5^v—K2—K1	45.32 (3)
F6ⁱⁱⁱ—Sn—K2^ix	110.30 (6)	F6^xvi—K2—K1	92.86 (3)
F6—Sn—K2^ix	69.70 (6)	Sn^xvi—K2—K1	73.573 (11)
K1^vii—Sn—K2^ix	105.549 (10)	F4—K2—K1	75.05 (3)
K1^viii—Sn—K2^ix	74.451 (10)	K1^xi—K2—K1	74.327 (13)
F5—Sn—K2^v	50.20 (5)	F3^xiv—K2—K1	147.77 (2)
F5ⁱⁱⁱ—Sn—K2^v	129.80 (5)	Sb^xiv—K2—K1	175.774 (15)
F7ⁱⁱⁱ—Sn—K2^v	46.88 (5)	K2^xvii—K2—K1	113.33 (2)
F7—Sn—K2^v	133.12 (5)	F2^xiv—K2—K2^xviii	75.81 (4)
F6ⁱⁱⁱ—Sn—K2^v	69.70 (6)	F2^xi—K2—K2^xviii	143.16 (4)
F6—Sn—K2^v	110.30 (6)	F3^v—K2—K2^xviii	67.21 (4)
K1^vii—Sn—K2^v	74.451 (10)	F1—K2—K2^xviii	135.04 (4)
K1^viii—Sn—K2^v	105.549 (10)	F7^xv—K2—K2^xviii	43.98 (3)
K2^ix—Sn—K2^v	180.000 (9)	F7^xvi—K2—K2^xviii	41.77 (4)
F5—Sn—Sb	65.81 (5)	F6ⁱ—K2—K2^xviii	128.40 (5)
F5ⁱⁱⁱ—Sn—Sb	114.19 (5)	F5^v—K2—K2^xviii	94.15 (4)
F7ⁱⁱⁱ—Sn—Sb	56.42 (6)	F6^xvi—K2—K2^xviii	85.16 (3)
F7—Sn—Sb	123.58 (6)	Sn^xvi—K2—K2^xviii	71.414 (13)
F6ⁱⁱⁱ—Sn—Sb	136.06 (6)	F4—K2—K2^xviii	99.52 (3)
F6—Sn—Sb	43.94 (6)	K1^xi—K2—K2^xviii	172.16 (2)
K1^vii—Sn—Sb	112.591 (9)	F3^xiv—K2—K2^xviii	39.05 (2)
K1^viii—Sn—Sb	67.409 (9)	Sb^xiv—K2—K2^xviii	66.425 (12)
K2^ix—Sn—Sb	113.168 (8)	K2^xvii—K2—K2^xviii	111.90 (2)
K2^v—Sn—Sb	66.832 (8)	K1—K2—K2^xviii	110.379 (17)
F5—Sn—Sbⁱⁱⁱ	114.19 (5)	F2^xiv—K2—F1^xi	120.78 (4)
F5ⁱⁱⁱ—Sn—Sbⁱⁱⁱ	65.81 (5)	F2^xi—K2—F1^xi	37.66 (4)
F7ⁱⁱⁱ—Sn—Sbⁱⁱⁱ	123.58 (6)	F3^v—K2—F1^xi	83.92 (4)
F7—Sn—Sbⁱⁱⁱ	56.42 (6)	F1—K2—F1^xi	46.14 (5)
F6ⁱⁱⁱ—Sn—Sbⁱⁱⁱ	43.94 (6)	F7^xv—K2—F1^xi	151.93 (5)
F6—Sn—Sbⁱⁱⁱ	136.06 (6)	F7^xvi—K2—F1^xi	108.92 (4)
K1^vii—Sn—Sbⁱⁱⁱ	67.409 (9)	F6ⁱ—K2—F1^xi	86.80 (5)
K1^viii—Sn—Sbⁱⁱⁱ	112.591 (9)	F5^v—K2—F1^xi	52.66 (4)
K2^ix—Sn—Sbⁱⁱⁱ	66.832 (8)	F6^xvi—K2—F1^xi	80.65 (4)
K2^v—Sn—Sbⁱⁱⁱ	113.168 (8)	Sn^xvi—K2—F1^xi	80.33 (2)
Sb—Sn—Sbⁱⁱⁱ	180.0	F4—K2—F1^xi	89.28 (3)
F4^v—K1—F2	135.92 (6)	K1^xi—K2—F1^xi	42.39 (2)
F4^v—K1—F1^xi	148.39 (5)	F3^xiv—K2—F1^xi	157.10 (4)
F2—K1—F1^xi	75.39 (5)	Sb^xiv—K2—F1^xi	142.70 (2)
F4^v—K1—F6^xii	112.69 (5)	K2^xvii—K2—F1^xi	79.10 (3)
F2—K1—F6^xii	69.51 (5)	K1—K2—F1^xi	39.05 (2)
F1^xi—K1—F6^xii	78.81 (5)	K2^xviii—K2—F1^xi	144.60 (3)
F4^v—K1—F3^v	56.26 (5)	F2^xiv—K2—K1^v	132.57 (4)
F2—K1—F3^v	111.27 (5)	F2^xi—K2—K1^v	143.70 (4)
F1^xi—K1—F3^v	115.30 (5)	F3^v—K2—K1^v	43.33 (4)
F6^xii—K1—F3^v	165.82 (5)	F1—K2—K1^v	69.71 (4)
F4^v—K1—F5^v	77.12 (5)	F7^xv—K2—K1^v	47.07 (4)
F2—K1—F5^v	138.76 (5)	F7^xvi—K2—K1^v	94.17 (4)
F1^xi—K1—F5^v	73.05 (5)	F6ⁱ—K2—K1^v	113.54 (4)
F6^xii—K1—F5^v	127.69 (6)	F5^v—K2—K1^v	104.38 (4)
F3^v—K1—F5^v	61.68 (5)	F6^xvi—K2—K1^v	140.15 (3)
F4^v—K1—F1	125.45 (5)	Sn^xvi—K2—K1^v	110.896 (12)
F2—K1—F1	54.76 (4)	F4—K2—K1^v	37.32 (2)
F1^xi—K1—F1	63.69 (6)	K1^xi—K2—K1^v	110.414 (15)
F6^xii—K1—F1	117.92 (5)	F3^xiv—K2—K1^v	94.36 (3)
F3^v—K1—F1	70.23 (4)	Sb^xiv—K2—K1^v	106.861 (15)
F5^v—K1—F1	87.34 (4)	K2^xvii—K2—K1^v	172.75 (2)
F4^v—K1—F3	89.08 (5)	K1—K2—K1^v	73.558 (15)
F2—K1—F3	53.71 (5)	K2^xviii—K2—K1^v	66.149 (15)
F1^xi—K1—F3	114.74 (4)	F1^xi—K2—K1^v	106.60 (2)
F6^xii—K1—F3	111.78 (5)	F2^xiv—K2—Sb^xi	96.86 (4)
F3^v—K1—F3	62.17 (5)	F2^xi—K2—Sb^xi	20.08 (3)
F5^v—K1—F3	119.86 (5)	F3^v—K2—Sb^xi	96.64 (4)
F1—K1—F3	54.61 (4)	F1—K2—Sb^xi	71.72 (4)
F4^v—K1—F4^xii	97.18 (5)	F7^xv—K2—Sb^xi	176.66 (4)
F2—K1—F4^xii	121.36 (5)	F7^xvi—K2—Sb^xi	93.17 (4)
F1^xi—K1—F4^xii	58.73 (4)	F6ⁱ—K2—Sb^xi	87.26 (4)
F6^xii—K1—F4^xii	67.58 (5)	F5^v—K2—Sb^xi	44.16 (3)
F3^v—K1—F4^xii	120.01 (5)	F6^xvi—K2—Sb^xi	55.73 (3)
F5^v—K1—F4^xii	60.16 (5)	Sn^xvi—K2—Sb^xi	63.440 (9)
F1—K1—F4^xii	119.49 (5)	F4—K2—Sb^xi	115.04 (3)
F3—K1—F4^xii	173.45 (4)	K1^xi—K2—Sb^xi	52.902 (10)
F4^v—K1—F7^xii	77.31 (5)	F3^xiv—K2—Sb^xi	130.95 (3)
F2—K1—F7^xii	69.12 (4)	Sb^xiv—K2—Sb^xi	123.080 (12)
F1^xi—K1—F7^xii	128.67 (5)	K2^xvii—K2—Sb^xi	56.635 (14)
F6^xii—K1—F7^xii	54.82 (5)	K1—K2—Sb^xi	56.866 (11)
F3^v—K1—F7^xii	111.57 (5)	K2^xviii—K2—Sb^xi	134.85 (2)
F5^v—K1—F7^xii	152.00 (5)	F1^xi—K2—Sb^xi	26.15 (2)
F1—K1—F7^xii	117.02 (4)	K1^v—K2—Sb^xi	129.978 (13)
F3—K1—F7^xii	70.83 (4)	Sb—F1—K2	140.58 (8)
F4^xii—K1—F7^xii	112.37 (5)	Sb—F1—K1^xi	117.20 (6)
F4^v—K1—F5^xii	59.59 (5)	K2—F1—K1^xi	92.59 (5)
F2—K1—F5^xii	113.82 (4)	Sb—F1—K1	97.72 (5)
F1^xi—K1—F5^xii	118.46 (5)	K2—F1—K1	90.44 (4)
F6^xii—K1—F5^xii	54.02 (4)	K1^xi—F1—K1	116.31 (6)
F3^v—K1—F5^xii	115.85 (4)	Sb—F1—Sbⁱ	78.40 (5)
F5^v—K1—F5^xii	104.33 (4)	K2—F1—Sbⁱ	81.29 (4)
F1—K1—F5^xii	168.30 (4)	K1^xi—F1—Sbⁱ	81.82 (3)
F3—K1—F5^xii	118.02 (5)	K1—F1—Sbⁱ	160.56 (6)
F4^xii—K1—F5^xii	67.26 (5)	Sb—F1—K2^xi	83.58 (5)
F7^xii—K1—F5^xii	51.96 (4)	K2—F1—K2^xi	133.86 (5)
F4^v—K1—K1^xiii	52.74 (4)	K1^xi—F1—K2^xi	67.96 (4)
F2—K1—K1^xiii	157.57 (4)	K1—F1—K2^xi	65.15 (3)
F1^xi—K1—K1^xiii	100.64 (4)	Sbⁱ—F1—K2^xi	132.27 (4)
F6^xii—K1—K1^xiii	88.06 (4)	Sb—F1—Sb^xi	145.08 (7)
F3^v—K1—K1^xiii	90.53 (3)	K2—F1—Sb^xi	71.96 (3)
F5^v—K1—K1^xiii	56.19 (4)	K1^xi—F1—Sb^xi	57.94 (3)
F1—K1—K1^xiii	143.52 (4)	K1—F1—Sb^xi	63.04 (3)
F3—K1—K1^xiii	141.78 (4)	Sbⁱ—F1—Sb^xi	129.25 (3)
F4^xii—K1—K1^xiii	44.44 (3)	K2^xi—F1—Sb^xi	62.18 (3)
F7^xii—K1—K1^xiii	98.64 (3)	Sb—F2—K2^vi	113.81 (7)
F5^xii—K1—K1^xiii	48.14 (3)	Sb—F2—K2^xi	133.55 (7)
F4^v—K1—Sb	119.75 (5)	K2^vi—F2—K2^xi	96.72 (5)
F2—K1—Sb	33.04 (3)	Sb—F2—K1	101.44 (6)
F1^xi—K1—Sb	83.66 (3)	K2^vi—F2—K1	117.00 (5)
F6^xii—K1—Sb	102.46 (4)	K2^xi—F2—K1	93.98 (5)
F3^v—K1—Sb	78.76 (3)	Sb—F3—K2^v	144.17 (8)
F5^v—K1—Sb	116.80 (4)	Sb—F3—K1^v	109.46 (6)
F1—K1—Sb	31.07 (3)	K2^v—F3—K1^v	92.49 (5)
F3—K1—Sb	31.44 (3)	Sb—F3—K1	96.64 (6)
F4^xii—K1—Sb	142.03 (3)	K2^v—F3—K1	97.51 (5)
F7^xii—K1—Sb	85.99 (3)	K1^v—F3—K1	117.83 (5)
F5^xii—K1—Sb	137.87 (3)	Sb—F3—K2^vi	76.06 (5)
K1^xiii—K1—Sb	169.27 (2)	K2^v—F3—K2^vi	73.75 (4)
F4^v—K1—Sn^xii	83.78 (4)	K1^v—F3—K2^vi	158.09 (6)
F2—K1—Sn^xii	82.30 (3)	K1—F3—K2^vi	81.50 (4)
F1^xi—K1—Sn^xii	109.42 (4)	Sb—F3—Sb^v	140.22 (6)
F6^xii—K1—Sn^xii	30.96 (3)	K2^v—F3—Sb^v	75.23 (3)
F3^v—K1—Sn^xii	135.18 (3)	K1^v—F3—Sb^v	59.92 (3)
F5^v—K1—Sn^xii	133.25 (4)	K1—F3—Sb^v	63.99 (3)
F1—K1—Sn^xii	137.06 (3)	K2^vi—F3—Sb^v	129.27 (4)
F3—K1—Sn^xii	101.81 (3)	Sb—F4—K1^v	114.26 (6)
F4^xii—K1—Sn^xii	80.88 (3)	Sb—F4—Sbⁱ	111.31 (6)
F7^xii—K1—Sn^xii	31.65 (3)	K1^v—F4—Sbⁱ	130.88 (7)
F5^xii—K1—Sn^xii	31.61 (3)	Sb—F4—K1^viii	121.86 (8)
K1^xiii—K1—Sn^xii	78.252 (16)	K1^v—F4—K1^viii	82.82 (5)
Sb—K1—Sn^xii	109.774 (12)	Sbⁱ—F4—K1^viii	88.45 (5)
F4^v—K1—K2^xi	159.66 (4)	Sb—F4—K2	90.97 (6)
F2—K1—K2^xi	42.70 (4)	K1^v—F4—K2	79.93 (4)
F1^xi—K1—K2^xi	43.65 (3)	Sbⁱ—F4—K2	81.98 (4)
F6^xii—K1—K2^xi	47.22 (3)	K1^viii—F4—K2	146.97 (6)
F3^v—K1—K2^xi	142.68 (3)	Sn—F5—K1^v	154.71 (8)
F5^v—K1—K2^xi	116.36 (4)	Sn—F5—K2^v	99.61 (6)
F1—K1—K2^xi	72.46 (3)	K1^v—F5—K2^v	86.58 (5)
F3—K1—K2^xi	96.07 (3)	Sn—F5—Sb^x	118.58 (7)
F4^xii—K1—K2^xi	78.71 (3)	K1^v—F5—Sb^x	85.29 (4)
F7^xii—K1—K2^xi	85.80 (4)	K2^v—F5—Sb^x	92.70 (4)
F5^xii—K1—K2^xi	100.98 (3)	Sn—F5—K1^viii	89.79 (5)
K1^xiii—K1—K2^xi	120.30 (2)	K1^v—F5—K1^viii	75.67 (4)
Sb—K1—K2^xi	69.495 (11)	K2^v—F5—K1^viii	154.85 (7)
Sn^xii—K1—K2^xi	75.912 (12)	Sb^x—F5—K1^viii	103.25 (5)
F4^v—K1—Sb^v	28.43 (4)	Sn—F5—Sb	86.58 (6)
F2—K1—Sb^v	127.52 (4)	K1^v—F5—Sb	70.26 (4)
F1^xi—K1—Sb^v	136.40 (3)	K2^v—F5—Sb	79.97 (4)
F6^xii—K1—Sb^v	140.46 (3)	Sb^x—F5—Sb	154.74 (5)
F3^v—K1—Sb^v	27.83 (3)	K1^viii—F5—Sb	77.35 (4)
F5^v—K1—Sb^v	66.77 (4)	Sn—F5—Sb^xv	124.19 (7)
F1—K1—Sb^v	97.55 (3)	K1^v—F5—Sb^xv	61.95 (3)
F3—K1—Sb^v	73.82 (3)	K2^v—F5—Sb^xv	132.77 (4)
F4^xii—K1—Sb^v	111.02 (3)	Sb^x—F5—Sb^xv	53.18 (3)
F7^xii—K1—Sb^v	94.88 (4)	K1^viii—F5—Sb^xv	52.27 (3)
F5^xii—K1—Sb^v	88.02 (3)	Sb—F5—Sb^xv	116.05 (4)
K1^xiii—K1—Sb^v	70.564 (14)	Sn—F6—K1^viii	101.55 (7)
Sb—K1—Sb^v	99.505 (13)	Sn—F6—K2ⁱ	152.63 (9)
Sn^xii—K1—Sb^v	110.137 (11)	K1^viii—F6—K2ⁱ	87.31 (5)
K2^xi—K1—Sb^v	168.929 (17)	Sn—F6—Sb	110.18 (7)
F4^v—K1—Sb^xi	122.89 (4)	K1^viii—F6—Sb	96.60 (5)
F2—K1—Sb^xi	100.69 (4)	K2ⁱ—F6—Sb	94.19 (5)
F1^xi—K1—Sb^xi	25.51 (3)	Sn—F6—K2^ix	80.09 (6)
F6^xii—K1—Sb^xi	90.54 (4)	K1^viii—F6—K2^ix	89.28 (6)
F3^v—K1—Sb^xi	103.00 (3)	K2ⁱ—F6—K2^ix	74.13 (4)
F5^v—K1—Sb^xi	49.35 (4)	Sb—F6—K2^ix	166.72 (6)
F1—K1—Sb^xi	76.30 (3)	Sn—F6—Sb^iv	91.99 (6)
F3—K1—Sb^xi	130.90 (3)	K1^viii—F6—Sb^iv	154.48 (6)
F4^xii—K1—Sb^xi	43.41 (3)	K2ⁱ—F6—Sb^iv	71.48 (4)
F7^xii—K1—Sb^xi	145.36 (4)	Sb—F6—Sb^iv	98.89 (5)
F5^xii—K1—Sb^xi	110.56 (4)	K2^ix—F6—Sb^iv	71.69 (3)
K1^xiii—K1—Sb^xi	78.484 (17)	Sn—F6—Sbⁱ	142.88 (7)
Sb—K1—Sb^xi	103.188 (10)	K1^viii—F6—Sbⁱ	54.56 (3)
Sn^xii—K1—Sb^xi	116.563 (15)	K2ⁱ—F6—Sbⁱ	62.34 (3)
K2^xi—K1—Sb^xi	67.191 (11)	Sb—F6—Sbⁱ	54.21 (3)
Sb^v—K1—Sb^xi	115.843 (12)	K2^ix—F6—Sbⁱ	122.30 (4)
F4^v—K1—K2	94.67 (4)	Sb^iv—F6—Sbⁱ	121.86 (4)
F2—K1—K2	97.42 (3)	Sn—F6—Sb^viii	110.68 (7)
F1^xi—K1—K2	72.99 (4)	K1^viii—F6—Sb^viii	45.15 (3)
F6^xii—K1—K2	151.21 (4)	K2ⁱ—F6—Sb^viii	58.40 (4)
F3^v—K1—K2	42.51 (3)	Sb—F6—Sb^viii	128.37 (5)
F5^v—K1—K2	48.10 (4)	K2^ix—F6—Sb^viii	50.61 (3)
F1—K1—K2	42.72 (3)	Sb^iv—F6—Sb^viii	109.80 (4)
F3—K1—K2	76.00 (3)	Sbⁱ—F6—Sb^viii	74.17 (2)
F4^xii—K1—K2	101.45 (4)	Sn—F7—K2^xv	160.99 (8)
F7^xii—K1—K2	145.89 (4)	Sn—F7—K2^ix	103.30 (7)
F5^xii—K1—K2	148.35 (3)	K2^xv—F7—K2^ix	94.25 (5)
K1^xiii—K1—K2	102.511 (19)	Sn—F7—K1^viii	91.68 (7)
Sb—K1—K2	69.152 (11)	K2^xv—F7—K1^viii	92.57 (5)
Sn^xii—K1—K2	177.363 (18)	K2^ix—F7—K1^viii	99.48 (5)
K2^xi—K1—K2	105.673 (13)	Sn—F7—Sbⁱⁱⁱ	96.03 (6)
Sb^v—K1—K2	67.947 (11)	K2^xv—F7—Sbⁱⁱⁱ	77.39 (5)
Sb^xi—K1—K2	66.072 (11)	K2^ix—F7—Sbⁱⁱⁱ	87.21 (5)
F4^v—K1—K2^v	62.75 (4)	K1^viii—F7—Sbⁱⁱⁱ	168.39 (6)
F2—K1—K2^v	73.17 (4)	Sn—F7—Sb^x	84.28 (5)
F1^xi—K1—K2^v	148.20 (3)	K2^xv—F7—Sb^x	77.70 (4)
F6^xii—K1—K2^v	94.45 (4)	K2^ix—F7—Sb^x	171.22 (6)
F3^v—K1—K2^v	72.82 (3)	K1^viii—F7—Sb^x	84.54 (4)
F5^v—K1—K2^v	131.10 (4)	Sbⁱⁱⁱ—F7—Sb^x	87.60 (4)
F1—K1—K2^v	93.76 (3)	Sn—F7—Sb^viii	128.27 (7)
F3—K1—K2^v	39.16 (3)	K2^xv—F7—Sb^viii	67.72 (3)
F4^xii—K1—K2^v	146.51 (3)	K2^ix—F7—Sb^viii	57.73 (3)
F7^xii—K1—K2^v	40.37 (4)	K1^viii—F7—Sb^viii	52.36 (3)
F5^xii—K1—K2^v	79.29 (4)	Sbⁱⁱⁱ—F7—Sb^viii	126.52 (4)
K1^xiii—K1—K2^v	110.234 (19)	Sb^x—F7—Sb^viii	120.88 (4)
Sb—K1—K2^v	67.341 (11)

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

Experimental details

Crystal data
Chemical formula	K₄Sb₂SnF₁₄
M_r	784.59
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	6.7356 (2), 7.4704 (2), 7.6370 (2)
α, β, γ (°)	92.691 (1), 91.461 (1), 115.323 (1)
V (Å³)	346.53 (2)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	7.00
Crystal size (mm)	0.4 × 0.35 × 0.28

Data collection
Diffractometer	Bruker SMART 1000 CCD area-detector diffractometer
Absorption correction	Gaussian (XPREP and SADABS; Bruker, 2003)
T_min, T_max	0.136, 0.291
No. of measured, independent and observed [I > 2σ(I)] reflections	7147, 4635, 4250
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	1.029

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.090, 1.30
No. of reflections	4635
No. of parameters	98
Δρ_max, Δρ_min (e Å⁻³)	1.91, −3.69

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 2003), XP in SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2008).

Selected bond lengths (Å) top

Sb—F1	1.9380 (14)	K1—F6^vi	2.811 (2)
Sb—F3	1.9539 (13)	K1—F3^iv	2.8390 (18)
Sb—F4	2.0609 (17)	K1—F5^iv	2.8578 (16)
Sb—F2	2.0696 (15)	K1—F1	2.9262 (15)
Sb—F4ⁱ	2.7516 (15)	K1—F3	2.9485 (18)
Sb—F5ⁱⁱ	3.0471 (18)	K1—F4^vi	2.982 (2)
Sb—F6	3.117 (2)	K1—F7^vi	3.122 (2)
Sn—F5	1.9581 (14)	K2—F2^vii	2.6662 (15)
Sn—F5ⁱⁱⁱ	1.9581 (14)	K2—F2^v	2.6777 (18)
Sn—F7ⁱⁱⁱ	1.9611 (17)	K2—F3^iv	2.7136 (15)
Sn—F7	1.9611 (17)	K2—F1	2.7216 (15)
Sn—F6ⁱⁱⁱ	1.9611 (16)	K2—F7^viii	2.7620 (19)
Sn—F6	1.9611 (16)	K2—F7^ix	2.8795 (17)
K1—F4^iv	2.6235 (16)	K2—F6ⁱ	2.8943 (16)
K1—F2	2.7086 (14)	K2—F5^iv	2.9912 (18)
K1—F1^v	2.7268 (16)

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

Acknowledgements

The authors thank the Russian Foundation for Basic Research (project No. 08-03-00355) for financial support.

References

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