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Acta Crystallogr Sect E Struct Rep Online. 2008 June 1; 64(Pt 6): i32.
Published online 2008 May 7. doi:  10.1107/S1600536808012865
PMCID: PMC2961491

Tetra­potassium dianti­mony(III) tin(IV) tetra­deca­fluoride

Abstract

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 [triangle]); Davidovich & Zemnukhova (1975 [triangle]); Gillespie (1970 [triangle]); Kriegsmann & Kessler (1962 [triangle]); Serezhkin et al. (1997 [triangle]).

Experimental

Crystal data

  • K4Sb2SnF14
  • M r = 784.59
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-00i32-efi1.jpg
  • 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 [triangle]) 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[F 2 > 2σ(F 2)] = 0.037
  • wR(F 2) = 0.090
  • S = 1.30
  • 4635 reflections
  • 98 parameters
  • Δρmax = 1.91 e Å−3
  • Δρmin = −3.69 e Å−3

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

Table 1
Selected bond lengths (Å)

Supplementary Material

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

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

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

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

supplementary crystallographic information

Comment

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].

Experimental

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).

Refinement

The maximum peak and deepest hole are located 0.70 Å and 0.96 Å, respectively, from Sn.

Figures

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.

Crystal data

K4Sb2SnF14Z = 1
Mr = 784.59F000 = 354
Triclinic, P1Dx = 3.760 Mg m3
a = 6.7356 (2) ÅMo Kα radiation λ = 0.71073 Å
b = 7.4704 (2) ÅCell parameters from 2472 reflections
c = 7.6370 (2) Åθ = 3.4–46.9º
α = 92.691 (1)ºµ = 7.00 mm1
β = 91.461 (1)ºT = 298 (2) K
γ = 115.323 (1)ºPrism, colourless
V = 346.526 (17) Å30.4 × 0.35 × 0.28 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer4635 independent reflections
Radiation source: fine-focus sealed tube4250 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.024
Detector resolution: 8.33 pixels mm-1θmax = 47.0º
T = 298(2) Kθmin = 3.4º
[var phi] and ω scansh = −9→13
Absorption correction: gaussian(XPREP and SADABS; Bruker, 2003)k = −15→9
Tmin = 0.136, Tmax = 0.291l = −15→11
7147 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full  w = 1/[σ2(Fo2) + (0.0258P)2 + 0.7101P] where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.037(Δ/σ)max = 0.003
wR(F2) = 0.090Δρmax = 1.91 e Å3
S = 1.30Δρmin = −3.69 e Å3
4635 reflectionsExtinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
98 parametersExtinction coefficient: 0.0782 (13)
Primary atom site location: structure-invariant direct methods

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 (Å2)

xyzUiso*/Ueq
Sb0.611210 (19)0.191057 (16)0.312309 (15)0.01531 (2)
Sn1.00000.00000.00000.01467 (3)
K10.85162 (7)0.73682 (7)0.41457 (6)0.02301 (9)
K20.71347 (7)0.44513 (8)0.85599 (6)0.02309 (8)
F10.5699 (2)0.3363 (2)0.51424 (18)0.0247 (3)
F20.5990 (2)0.4270 (2)0.18860 (19)0.0237 (3)
F30.9214 (2)0.3796 (2)0.3294 (2)0.0252 (3)
F40.7266 (2)0.0671 (2)0.5021 (2)0.0300 (3)
F51.1417 (3)0.1313 (2)0.22704 (19)0.0297 (3)
F60.7209 (3)−0.1279 (3)0.1151 (2)0.0332 (4)
F71.0620 (3)−0.2265 (2)0.0506 (2)0.0322 (3)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Sb0.01754 (4)0.01469 (4)0.01477 (4)0.00794 (3)0.00034 (3)0.00109 (3)
Sn0.01815 (5)0.01411 (5)0.01377 (5)0.00878 (4)0.00109 (4)0.00153 (4)
K10.01943 (14)0.02305 (16)0.02459 (16)0.00756 (12)−0.00196 (13)0.00015 (13)
K20.02202 (15)0.02791 (16)0.02086 (15)0.01186 (12)0.00175 (13)0.00452 (13)
F10.0254 (5)0.0286 (5)0.0191 (5)0.0108 (4)0.0045 (4)−0.0032 (4)
F20.0302 (5)0.0201 (4)0.0233 (5)0.0131 (4)−0.0020 (5)0.0048 (4)
F30.0174 (4)0.0274 (6)0.0294 (6)0.0079 (4)0.0038 (4)0.0046 (5)
F40.0215 (5)0.0312 (6)0.0363 (7)0.0093 (5)−0.0031 (5)0.0159 (5)
F50.0381 (6)0.0344 (6)0.0195 (5)0.0197 (5)−0.0083 (5)−0.0074 (5)
F60.0254 (6)0.0395 (8)0.0323 (7)0.0105 (5)0.0098 (5)0.0086 (6)
F70.0449 (7)0.0240 (5)0.0353 (7)0.0226 (5)−0.0084 (6)0.0009 (5)

Geometric parameters (Å, °)

Sb—F11.9380 (14)K2—F2xi2.6777 (18)
Sb—F31.9539 (13)K2—F3v2.7136 (15)
Sb—F42.0609 (17)K2—F12.7216 (15)
Sb—F22.0696 (15)K2—F7xv2.7620 (19)
Sb—F4i2.7516 (15)K2—F7xvi2.8795 (17)
Sb—F5ii3.0471 (18)K2—F6i2.8943 (16)
Sb—F63.117 (2)K2—F5v2.9912 (18)
Sb—F7iii3.5325 (19)K2—F6xvi3.655 (2)
Sb—K13.7207 (5)K2—Snxvi3.8388 (5)
Sb—F6iv3.8032 (18)K2—F43.847 (2)
Sb—F53.8531 (19)K2—K1xi3.9388 (7)
Sb—F1i3.9018 (16)K2—F3xiv3.9710 (17)
Sb—K1v3.9464 (5)K2—Sbxiv3.9808 (5)
Sb—K2vi3.9808 (5)K2—K2xvii3.9938 (10)
Sb—Sbi3.9925 (2)K2—K2xviii4.1352 (10)
Sn—F51.9581 (14)K2—F1xi4.1386 (18)
Sn—F5iii1.9581 (14)K2—K1v4.2602 (8)
Sn—F7iii1.9611 (17)K2—Sbxi4.3692 (6)
Sn—F71.9611 (17)F1—K1xi2.7268 (16)
Sn—F6iii1.9611 (16)F1—Sbi3.9018 (16)
Sn—F61.9611 (16)F1—K2xi4.1386 (18)
Sn—K1vii3.7354 (5)F1—Sbxi4.3632 (17)
Sn—K1viii3.7354 (5)F2—K2vi2.6662 (15)
Sn—K2ix3.8388 (5)F2—K2xi2.6777 (18)
Sn—K2v3.8388 (5)F3—K2v2.7136 (14)
Sb—Sn4.21660 (15)F3—K1v2.8390 (18)
Sn—Sbiii4.21661 (15)F3—K2vi3.9710 (17)
Sn—Sbiv4.33908 (16)F3—Sbv4.2172 (14)
Sn—Sbx4.33908 (16)F4—K1v2.6235 (15)
K1—F4v2.6235 (16)F4—Sbi2.7516 (15)
K1—F22.7086 (14)F4—K1viii2.982 (2)
K1—F1xi2.7268 (16)F5—K1v2.8578 (16)
K1—F6xii2.811 (2)F5—K2v2.9912 (18)
K1—F3v2.8390 (18)F5—Sbx3.0471 (18)
K1—F5v2.8578 (16)F5—K1viii3.1882 (17)
K1—F12.9262 (15)F5—Sbxv4.9869 (18)
K1—F32.9485 (18)F6—K1viii2.811 (2)
K1—F4xii2.982 (2)F6—K2i2.8943 (16)
K1—F7xii3.122 (2)F6—K2ix3.655 (2)
K1—F5xii3.1882 (17)F6—Sbiv3.8032 (18)
K1—K1xiii3.7178 (9)F6—Sbi4.9129 (17)
K1—Snxii3.7354 (5)F6—Sbviii5.124 (2)
K1—K2xi3.9388 (7)F7—K2xv2.7620 (19)
K1—Sbv3.9464 (5)F7—K2ix2.8795 (16)
K1—Sbxi4.0028 (5)F7—K1viii3.1222 (19)
K1—K24.0117 (7)F7—Sbiii3.5325 (19)
K1—K2v4.2602 (8)F7—Sbx4.0712 (16)
K1—Sbxii4.4308 (6)F7—Sbviii4.6870 (16)
K2—F2xiv2.6662 (15)
F1—Sb—F387.64 (6)Snxii—K1—K2v70.956 (11)
F1—Sb—F482.57 (7)K2xi—K1—K2v110.414 (15)
F3—Sb—F480.01 (6)Sbv—K1—K2v64.623 (11)
F1—Sb—F280.77 (6)Sbxi—K1—K2v170.056 (15)
F3—Sb—F279.13 (6)K2—K1—K2v106.442 (15)
F4—Sb—F2153.71 (6)F4v—K1—Sbxii105.98 (4)
F1—Sb—F4i71.19 (6)F2—K1—Sbxii103.48 (4)
F3—Sb—F4i143.84 (6)F1xi—K1—Sbxii60.65 (4)
F4—Sb—F4i68.69 (6)F6xii—K1—Sbxii44.34 (4)
F2—Sb—F4i123.67 (6)F3v—K1—Sbxii142.69 (4)
F1—Sb—F5ii80.34 (5)F5v—K1—Sbxii83.36 (4)
F3—Sb—F5ii145.85 (6)F1—K1—Sbxii123.89 (4)
F4—Sb—F5ii129.10 (5)F3—K1—Sbxii155.13 (3)
F2—Sb—F5ii67.49 (5)F4xii—K1—Sbxii23.27 (3)
F4i—Sb—F5ii60.42 (5)F7xii—K1—Sbxii92.88 (4)
F1—Sb—F6156.26 (6)F5xii—K1—Sbxii58.05 (4)
F3—Sb—F691.23 (6)K1xiii—K1—Sbxii57.132 (15)
F4—Sb—F673.89 (6)Sb—K1—Sbxii132.635 (13)
F2—Sb—F6122.29 (5)Snxii—K1—Sbxii61.479 (8)
F4i—Sb—F696.84 (5)K2xi—K1—Sbxii63.210 (12)
F5ii—Sb—F6112.19 (4)Sbv—K1—Sbxii127.696 (11)
F1—Sb—F7iii144.50 (5)Sbxi—K1—Sbxii56.236 (8)
F3—Sb—F7iii60.78 (5)K2—K1—Sbxii121.076 (15)
F4—Sb—F7iii105.41 (6)K2v—K1—Sbxii132.216 (14)
F2—Sb—F7iii77.82 (5)F2xiv—K2—F2xi83.28 (5)
F4i—Sb—F7iii144.19 (5)F2xiv—K2—F3v138.86 (5)
F5ii—Sb—F7iii116.08 (4)F2xi—K2—F3v116.46 (5)
F6—Sb—F7iii49.35 (4)F2xiv—K2—F1145.86 (5)
F1—Sb—K151.20 (4)F2xi—K2—F175.98 (5)
F3—Sb—K151.92 (5)F3v—K2—F175.22 (4)
F4—Sb—K1108.38 (5)F2xiv—K2—F7xv85.87 (5)
F2—Sb—K145.52 (4)F2xi—K2—F7xv163.17 (5)
F4i—Sb—K1121.51 (4)F3v—K2—F7xv80.02 (5)
F5ii—Sb—K197.07 (3)F1—K2—F7xv107.02 (6)
F6—Sb—K1140.19 (3)F2xiv—K2—F7xvi73.56 (5)
F7iii—Sb—K194.15 (3)F2xi—K2—F7xvi103.37 (5)
F1—Sb—F6iv119.92 (6)F3v—K2—F7xvi67.03 (5)
F3—Sb—F6iv118.94 (5)F1—K2—F7xvi137.34 (5)
F4—Sb—F6iv149.10 (6)F7xv—K2—F7xvi85.75 (5)
F2—Sb—F6iv56.92 (5)F2xiv—K2—F6i69.80 (5)
F4i—Sb—F6iv97.15 (4)F2xi—K2—F6i68.66 (5)
F5ii—Sb—F6iv46.60 (4)F3v—K2—F6i149.54 (5)
F6—Sb—F6iv81.11 (5)F1—K2—F6i77.45 (5)
F7iii—Sb—F6iv69.52 (4)F7xv—K2—F6i95.51 (6)
K1—Sb—F6iv102.43 (3)F7xvi—K2—F6i143.13 (5)
F1—Sb—F5124.91 (5)F2xiv—K2—F5v105.63 (5)
F3—Sb—F547.69 (6)F2xi—K2—F5v62.58 (5)
F4—Sb—F562.29 (5)F3v—K2—F5v61.36 (5)
F2—Sb—F5112.55 (5)F1—K2—F5v88.59 (5)
F4i—Sb—F5123.65 (5)F7xv—K2—F5v133.22 (5)
F5ii—Sb—F5154.74 (5)F7xvi—K2—F5v56.44 (5)
F6—Sb—F544.86 (4)F6i—K2—F5v131.19 (6)
F7iii—Sb—F543.91 (4)F2xiv—K2—F6xvi57.19 (4)
K1—Sb—F599.51 (3)F2xi—K2—F6xvi58.00 (4)
F6iv—Sb—F5110.73 (4)F3v—K2—F6xvi101.14 (4)
F1—Sb—F1i101.60 (5)F1—K2—F6xvi126.75 (5)
F3—Sb—F1i119.88 (6)F7xv—K2—F6xvi124.94 (5)
F4—Sb—F1i43.93 (5)F7xvi—K2—F6xvi47.89 (5)
F2—Sb—F1i160.78 (5)F6i—K2—F6xvi105.87 (4)
F4i—Sb—F1i42.52 (5)F5v—K2—F6xvi48.52 (4)
F5ii—Sb—F1i93.92 (4)F2xiv—K2—Snxvi80.82 (3)
F6—Sb—F1i58.86 (4)F2xi—K2—Snxvi75.59 (3)
F7iii—Sb—F1i107.93 (3)F3v—K2—Snxvi71.04 (4)
K1—Sb—F1i147.81 (2)F1—K2—Snxvi118.69 (4)
F6iv—Sb—F1i107.05 (3)F7xv—K2—Snxvi115.30 (4)
F5—Sb—F1i82.00 (3)F7xvi—K2—Snxvi29.81 (4)
F1—Sb—K1v83.19 (5)F6i—K2—Snxvi135.57 (4)
F3—Sb—K1v42.71 (5)F5v—K2—Snxvi30.19 (3)
F4—Sb—K1v37.30 (4)F6xvi—K2—Snxvi30.21 (2)
F2—Sb—K1v120.02 (4)F2xiv—K2—F4134.72 (4)
F4i—Sb—K1v104.20 (4)F2xi—K2—F4116.59 (4)
F5ii—Sb—K1v160.47 (3)F3v—K2—F470.89 (4)
F6—Sb—K1v79.99 (3)F1—K2—F443.32 (5)
F7iii—Sb—K1v83.45 (3)F7xv—K2—F463.76 (5)
K1—Sb—K1v80.495 (13)F7xvi—K2—F4131.42 (5)
F6iv—Sb—K1v152.92 (3)F6i—K2—F480.07 (5)
F5—Sb—K1v42.97 (2)F5v—K2—F4119.65 (4)
F1i—Sb—K1v79.15 (2)F6xvi—K2—F4167.89 (4)
F1—Sb—K2vi117.92 (5)Snxvi—K2—F4141.35 (3)
F3—Sb—K2vi75.50 (5)F2xiv—K2—K1xi103.45 (4)
F4—Sb—K2vi146.86 (5)F2xi—K2—K1xi43.32 (3)
F2—Sb—K2vi37.79 (4)F3v—K2—K1xi115.64 (4)
F4i—Sb—K2vi140.23 (4)F1—K2—K1xi43.76 (3)
F5ii—Sb—K2vi82.15 (3)F7xv—K2—K1xi128.37 (4)
F6—Sb—K2vi84.58 (3)F7xvi—K2—K1xi145.82 (4)
F7iii—Sb—K2vi42.62 (3)F6i—K2—K1xi45.47 (4)
K1—Sb—K2vi72.944 (11)F5v—K2—K1xi93.55 (3)
F6iv—Sb—K2vi43.58 (2)F6xvi—K2—K1xi101.07 (3)
F5—Sb—K2vi84.66 (3)Snxvi—K2—K1xi116.309 (16)
F1i—Sb—K2vi138.75 (2)F4—K2—K1xi75.33 (3)
K1v—Sb—K2vi115.096 (10)F2xiv—K2—F3xiv39.66 (4)
F1—Sb—Sbi73.20 (5)F2xi—K2—F3xiv121.93 (4)
F3—Sb—Sbi117.83 (5)F3v—K2—F3xiv106.25 (4)
F4—Sb—Sbi39.94 (4)F1—K2—F3xiv155.67 (5)
F2—Sb—Sbi147.66 (4)F7xv—K2—F3xiv50.88 (5)
F4i—Sb—Sbi28.74 (4)F7xvi—K2—F3xiv59.33 (4)
F5ii—Sb—Sbi89.16 (3)F6i—K2—F3xiv93.31 (4)
F6—Sb—Sbi86.50 (3)F5v—K2—F3xiv113.77 (4)
F7iii—Sb—Sbi134.11 (3)F6xvi—K2—F3xiv77.30 (4)
K1—Sb—Sbi121.530 (9)Snxvi—K2—F3xiv83.69 (2)
F6iv—Sb—Sbi121.92 (2)F4—K2—F3xiv113.32 (4)
F5—Sb—Sbi98.15 (3)K1xi—K2—F3xiv137.39 (2)
F1i—Sb—Sbi28.39 (2)F2xiv—K2—Sbxiv28.40 (3)
K1v—Sb—Sbi76.021 (8)F2xi—K2—Sbxiv106.25 (3)
K2vi—Sb—Sbi164.150 (8)F3v—K2—Sbxiv132.62 (4)
F5—Sn—F5iii180.00 (5)F1—K2—Sbxiv137.36 (3)
F5—Sn—F7iii90.26 (7)F7xv—K2—Sbxiv59.99 (4)
F5iii—Sn—F7iii89.74 (7)F7xvi—K2—Sbxiv84.57 (4)
F5—Sn—F789.74 (7)F6i—K2—Sbxiv64.94 (4)
F5iii—Sn—F790.26 (7)F5v—K2—Sbxiv131.15 (3)
F7iii—Sn—F7180.00 (14)F6xvi—K2—Sbxiv84.19 (3)
F5—Sn—F6iii91.07 (7)Snxvi—K2—Sbxiv102.504 (11)
F5iii—Sn—F6iii88.93 (7)F4—K2—Sbxiv107.92 (3)
F7iii—Sn—F6iii88.84 (8)K1xi—K2—Sbxiv109.172 (12)
F7—Sn—F6iii91.16 (8)F3xiv—K2—Sbxiv28.449 (19)
F5—Sn—F688.93 (7)F2xiv—K2—K2xvii41.75 (4)
F5iii—Sn—F691.07 (7)F2xi—K2—K2xvii41.53 (3)
F7iii—Sn—F691.16 (8)F3v—K2—K2xvii143.27 (4)
F7—Sn—F688.84 (8)F1—K2—K2xvii112.96 (4)
F6iii—Sn—F6180.00 (16)F7xv—K2—K2xvii126.42 (4)
F5—Sn—K1vii121.41 (5)F7xvi—K2—K2xvii88.06 (4)
F5iii—Sn—K1vii58.59 (5)F6i—K2—K2xvii61.68 (4)
F7iii—Sn—K1vii56.67 (6)F5v—K2—K2xvii82.59 (4)
F7—Sn—K1vii123.33 (6)F6xvi—K2—K2xvii44.19 (3)
F6iii—Sn—K1vii47.50 (6)Snxvi—K2—K2xvii74.136 (15)
F6—Sn—K1vii132.50 (6)F4—K2—K2xvii140.33 (3)
F5—Sn—K1viii58.59 (5)K1xi—K2—K2xvii70.576 (15)
F5iii—Sn—K1viii121.41 (5)F3xiv—K2—K2xvii80.83 (3)
F7iii—Sn—K1viii123.33 (6)Sbxiv—K2—K2xvii66.445 (12)
F7—Sn—K1viii56.67 (6)F2xiv—K2—K1149.45 (4)
F6iii—Sn—K1viii132.50 (6)F2xi—K2—K174.53 (3)
F6—Sn—K1viii47.50 (6)F3v—K2—K144.99 (4)
K1vii—Sn—K1viii180.000 (14)F1—K2—K146.84 (3)
F5—Sn—K2ix129.80 (5)F7xv—K2—K1119.96 (4)
F5iii—Sn—K2ix50.20 (5)F7xvi—K2—K191.21 (4)
F7iii—Sn—K2ix133.12 (5)F6i—K2—K1118.92 (4)
F7—Sn—K2ix46.88 (5)F5v—K2—K145.32 (3)
F6iii—Sn—K2ix110.30 (6)F6xvi—K2—K192.86 (3)
F6—Sn—K2ix69.70 (6)Snxvi—K2—K173.573 (11)
K1vii—Sn—K2ix105.549 (10)F4—K2—K175.05 (3)
K1viii—Sn—K2ix74.451 (10)K1xi—K2—K174.327 (13)
F5—Sn—K2v50.20 (5)F3xiv—K2—K1147.77 (2)
F5iii—Sn—K2v129.80 (5)Sbxiv—K2—K1175.774 (15)
F7iii—Sn—K2v46.88 (5)K2xvii—K2—K1113.33 (2)
F7—Sn—K2v133.12 (5)F2xiv—K2—K2xviii75.81 (4)
F6iii—Sn—K2v69.70 (6)F2xi—K2—K2xviii143.16 (4)
F6—Sn—K2v110.30 (6)F3v—K2—K2xviii67.21 (4)
K1vii—Sn—K2v74.451 (10)F1—K2—K2xviii135.04 (4)
K1viii—Sn—K2v105.549 (10)F7xv—K2—K2xviii43.98 (3)
K2ix—Sn—K2v180.000 (9)F7xvi—K2—K2xviii41.77 (4)
F5—Sn—Sb65.81 (5)F6i—K2—K2xviii128.40 (5)
F5iii—Sn—Sb114.19 (5)F5v—K2—K2xviii94.15 (4)
F7iii—Sn—Sb56.42 (6)F6xvi—K2—K2xviii85.16 (3)
F7—Sn—Sb123.58 (6)Snxvi—K2—K2xviii71.414 (13)
F6iii—Sn—Sb136.06 (6)F4—K2—K2xviii99.52 (3)
F6—Sn—Sb43.94 (6)K1xi—K2—K2xviii172.16 (2)
K1vii—Sn—Sb112.591 (9)F3xiv—K2—K2xviii39.05 (2)
K1viii—Sn—Sb67.409 (9)Sbxiv—K2—K2xviii66.425 (12)
K2ix—Sn—Sb113.168 (8)K2xvii—K2—K2xviii111.90 (2)
K2v—Sn—Sb66.832 (8)K1—K2—K2xviii110.379 (17)
F5—Sn—Sbiii114.19 (5)F2xiv—K2—F1xi120.78 (4)
F5iii—Sn—Sbiii65.81 (5)F2xi—K2—F1xi37.66 (4)
F7iii—Sn—Sbiii123.58 (6)F3v—K2—F1xi83.92 (4)
F7—Sn—Sbiii56.42 (6)F1—K2—F1xi46.14 (5)
F6iii—Sn—Sbiii43.94 (6)F7xv—K2—F1xi151.93 (5)
F6—Sn—Sbiii136.06 (6)F7xvi—K2—F1xi108.92 (4)
K1vii—Sn—Sbiii67.409 (9)F6i—K2—F1xi86.80 (5)
K1viii—Sn—Sbiii112.591 (9)F5v—K2—F1xi52.66 (4)
K2ix—Sn—Sbiii66.832 (8)F6xvi—K2—F1xi80.65 (4)
K2v—Sn—Sbiii113.168 (8)Snxvi—K2—F1xi80.33 (2)
Sb—Sn—Sbiii180.0F4—K2—F1xi89.28 (3)
F4v—K1—F2135.92 (6)K1xi—K2—F1xi42.39 (2)
F4v—K1—F1xi148.39 (5)F3xiv—K2—F1xi157.10 (4)
F2—K1—F1xi75.39 (5)Sbxiv—K2—F1xi142.70 (2)
F4v—K1—F6xii112.69 (5)K2xvii—K2—F1xi79.10 (3)
F2—K1—F6xii69.51 (5)K1—K2—F1xi39.05 (2)
F1xi—K1—F6xii78.81 (5)K2xviii—K2—F1xi144.60 (3)
F4v—K1—F3v56.26 (5)F2xiv—K2—K1v132.57 (4)
F2—K1—F3v111.27 (5)F2xi—K2—K1v143.70 (4)
F1xi—K1—F3v115.30 (5)F3v—K2—K1v43.33 (4)
F6xii—K1—F3v165.82 (5)F1—K2—K1v69.71 (4)
F4v—K1—F5v77.12 (5)F7xv—K2—K1v47.07 (4)
F2—K1—F5v138.76 (5)F7xvi—K2—K1v94.17 (4)
F1xi—K1—F5v73.05 (5)F6i—K2—K1v113.54 (4)
F6xii—K1—F5v127.69 (6)F5v—K2—K1v104.38 (4)
F3v—K1—F5v61.68 (5)F6xvi—K2—K1v140.15 (3)
F4v—K1—F1125.45 (5)Snxvi—K2—K1v110.896 (12)
F2—K1—F154.76 (4)F4—K2—K1v37.32 (2)
F1xi—K1—F163.69 (6)K1xi—K2—K1v110.414 (15)
F6xii—K1—F1117.92 (5)F3xiv—K2—K1v94.36 (3)
F3v—K1—F170.23 (4)Sbxiv—K2—K1v106.861 (15)
F5v—K1—F187.34 (4)K2xvii—K2—K1v172.75 (2)
F4v—K1—F389.08 (5)K1—K2—K1v73.558 (15)
F2—K1—F353.71 (5)K2xviii—K2—K1v66.149 (15)
F1xi—K1—F3114.74 (4)F1xi—K2—K1v106.60 (2)
F6xii—K1—F3111.78 (5)F2xiv—K2—Sbxi96.86 (4)
F3v—K1—F362.17 (5)F2xi—K2—Sbxi20.08 (3)
F5v—K1—F3119.86 (5)F3v—K2—Sbxi96.64 (4)
F1—K1—F354.61 (4)F1—K2—Sbxi71.72 (4)
F4v—K1—F4xii97.18 (5)F7xv—K2—Sbxi176.66 (4)
F2—K1—F4xii121.36 (5)F7xvi—K2—Sbxi93.17 (4)
F1xi—K1—F4xii58.73 (4)F6i—K2—Sbxi87.26 (4)
F6xii—K1—F4xii67.58 (5)F5v—K2—Sbxi44.16 (3)
F3v—K1—F4xii120.01 (5)F6xvi—K2—Sbxi55.73 (3)
F5v—K1—F4xii60.16 (5)Snxvi—K2—Sbxi63.440 (9)
F1—K1—F4xii119.49 (5)F4—K2—Sbxi115.04 (3)
F3—K1—F4xii173.45 (4)K1xi—K2—Sbxi52.902 (10)
F4v—K1—F7xii77.31 (5)F3xiv—K2—Sbxi130.95 (3)
F2—K1—F7xii69.12 (4)Sbxiv—K2—Sbxi123.080 (12)
F1xi—K1—F7xii128.67 (5)K2xvii—K2—Sbxi56.635 (14)
F6xii—K1—F7xii54.82 (5)K1—K2—Sbxi56.866 (11)
F3v—K1—F7xii111.57 (5)K2xviii—K2—Sbxi134.85 (2)
F5v—K1—F7xii152.00 (5)F1xi—K2—Sbxi26.15 (2)
F1—K1—F7xii117.02 (4)K1v—K2—Sbxi129.978 (13)
F3—K1—F7xii70.83 (4)Sb—F1—K2140.58 (8)
F4xii—K1—F7xii112.37 (5)Sb—F1—K1xi117.20 (6)
F4v—K1—F5xii59.59 (5)K2—F1—K1xi92.59 (5)
F2—K1—F5xii113.82 (4)Sb—F1—K197.72 (5)
F1xi—K1—F5xii118.46 (5)K2—F1—K190.44 (4)
F6xii—K1—F5xii54.02 (4)K1xi—F1—K1116.31 (6)
F3v—K1—F5xii115.85 (4)Sb—F1—Sbi78.40 (5)
F5v—K1—F5xii104.33 (4)K2—F1—Sbi81.29 (4)
F1—K1—F5xii168.30 (4)K1xi—F1—Sbi81.82 (3)
F3—K1—F5xii118.02 (5)K1—F1—Sbi160.56 (6)
F4xii—K1—F5xii67.26 (5)Sb—F1—K2xi83.58 (5)
F7xii—K1—F5xii51.96 (4)K2—F1—K2xi133.86 (5)
F4v—K1—K1xiii52.74 (4)K1xi—F1—K2xi67.96 (4)
F2—K1—K1xiii157.57 (4)K1—F1—K2xi65.15 (3)
F1xi—K1—K1xiii100.64 (4)Sbi—F1—K2xi132.27 (4)
F6xii—K1—K1xiii88.06 (4)Sb—F1—Sbxi145.08 (7)
F3v—K1—K1xiii90.53 (3)K2—F1—Sbxi71.96 (3)
F5v—K1—K1xiii56.19 (4)K1xi—F1—Sbxi57.94 (3)
F1—K1—K1xiii143.52 (4)K1—F1—Sbxi63.04 (3)
F3—K1—K1xiii141.78 (4)Sbi—F1—Sbxi129.25 (3)
F4xii—K1—K1xiii44.44 (3)K2xi—F1—Sbxi62.18 (3)
F7xii—K1—K1xiii98.64 (3)Sb—F2—K2vi113.81 (7)
F5xii—K1—K1xiii48.14 (3)Sb—F2—K2xi133.55 (7)
F4v—K1—Sb119.75 (5)K2vi—F2—K2xi96.72 (5)
F2—K1—Sb33.04 (3)Sb—F2—K1101.44 (6)
F1xi—K1—Sb83.66 (3)K2vi—F2—K1117.00 (5)
F6xii—K1—Sb102.46 (4)K2xi—F2—K193.98 (5)
F3v—K1—Sb78.76 (3)Sb—F3—K2v144.17 (8)
F5v—K1—Sb116.80 (4)Sb—F3—K1v109.46 (6)
F1—K1—Sb31.07 (3)K2v—F3—K1v92.49 (5)
F3—K1—Sb31.44 (3)Sb—F3—K196.64 (6)
F4xii—K1—Sb142.03 (3)K2v—F3—K197.51 (5)
F7xii—K1—Sb85.99 (3)K1v—F3—K1117.83 (5)
F5xii—K1—Sb137.87 (3)Sb—F3—K2vi76.06 (5)
K1xiii—K1—Sb169.27 (2)K2v—F3—K2vi73.75 (4)
F4v—K1—Snxii83.78 (4)K1v—F3—K2vi158.09 (6)
F2—K1—Snxii82.30 (3)K1—F3—K2vi81.50 (4)
F1xi—K1—Snxii109.42 (4)Sb—F3—Sbv140.22 (6)
F6xii—K1—Snxii30.96 (3)K2v—F3—Sbv75.23 (3)
F3v—K1—Snxii135.18 (3)K1v—F3—Sbv59.92 (3)
F5v—K1—Snxii133.25 (4)K1—F3—Sbv63.99 (3)
F1—K1—Snxii137.06 (3)K2vi—F3—Sbv129.27 (4)
F3—K1—Snxii101.81 (3)Sb—F4—K1v114.26 (6)
F4xii—K1—Snxii80.88 (3)Sb—F4—Sbi111.31 (6)
F7xii—K1—Snxii31.65 (3)K1v—F4—Sbi130.88 (7)
F5xii—K1—Snxii31.61 (3)Sb—F4—K1viii121.86 (8)
K1xiii—K1—Snxii78.252 (16)K1v—F4—K1viii82.82 (5)
Sb—K1—Snxii109.774 (12)Sbi—F4—K1viii88.45 (5)
F4v—K1—K2xi159.66 (4)Sb—F4—K290.97 (6)
F2—K1—K2xi42.70 (4)K1v—F4—K279.93 (4)
F1xi—K1—K2xi43.65 (3)Sbi—F4—K281.98 (4)
F6xii—K1—K2xi47.22 (3)K1viii—F4—K2146.97 (6)
F3v—K1—K2xi142.68 (3)Sn—F5—K1v154.71 (8)
F5v—K1—K2xi116.36 (4)Sn—F5—K2v99.61 (6)
F1—K1—K2xi72.46 (3)K1v—F5—K2v86.58 (5)
F3—K1—K2xi96.07 (3)Sn—F5—Sbx118.58 (7)
F4xii—K1—K2xi78.71 (3)K1v—F5—Sbx85.29 (4)
F7xii—K1—K2xi85.80 (4)K2v—F5—Sbx92.70 (4)
F5xii—K1—K2xi100.98 (3)Sn—F5—K1viii89.79 (5)
K1xiii—K1—K2xi120.30 (2)K1v—F5—K1viii75.67 (4)
Sb—K1—K2xi69.495 (11)K2v—F5—K1viii154.85 (7)
Snxii—K1—K2xi75.912 (12)Sbx—F5—K1viii103.25 (5)
F4v—K1—Sbv28.43 (4)Sn—F5—Sb86.58 (6)
F2—K1—Sbv127.52 (4)K1v—F5—Sb70.26 (4)
F1xi—K1—Sbv136.40 (3)K2v—F5—Sb79.97 (4)
F6xii—K1—Sbv140.46 (3)Sbx—F5—Sb154.74 (5)
F3v—K1—Sbv27.83 (3)K1viii—F5—Sb77.35 (4)
F5v—K1—Sbv66.77 (4)Sn—F5—Sbxv124.19 (7)
F1—K1—Sbv97.55 (3)K1v—F5—Sbxv61.95 (3)
F3—K1—Sbv73.82 (3)K2v—F5—Sbxv132.77 (4)
F4xii—K1—Sbv111.02 (3)Sbx—F5—Sbxv53.18 (3)
F7xii—K1—Sbv94.88 (4)K1viii—F5—Sbxv52.27 (3)
F5xii—K1—Sbv88.02 (3)Sb—F5—Sbxv116.05 (4)
K1xiii—K1—Sbv70.564 (14)Sn—F6—K1viii101.55 (7)
Sb—K1—Sbv99.505 (13)Sn—F6—K2i152.63 (9)
Snxii—K1—Sbv110.137 (11)K1viii—F6—K2i87.31 (5)
K2xi—K1—Sbv168.929 (17)Sn—F6—Sb110.18 (7)
F4v—K1—Sbxi122.89 (4)K1viii—F6—Sb96.60 (5)
F2—K1—Sbxi100.69 (4)K2i—F6—Sb94.19 (5)
F1xi—K1—Sbxi25.51 (3)Sn—F6—K2ix80.09 (6)
F6xii—K1—Sbxi90.54 (4)K1viii—F6—K2ix89.28 (6)
F3v—K1—Sbxi103.00 (3)K2i—F6—K2ix74.13 (4)
F5v—K1—Sbxi49.35 (4)Sb—F6—K2ix166.72 (6)
F1—K1—Sbxi76.30 (3)Sn—F6—Sbiv91.99 (6)
F3—K1—Sbxi130.90 (3)K1viii—F6—Sbiv154.48 (6)
F4xii—K1—Sbxi43.41 (3)K2i—F6—Sbiv71.48 (4)
F7xii—K1—Sbxi145.36 (4)Sb—F6—Sbiv98.89 (5)
F5xii—K1—Sbxi110.56 (4)K2ix—F6—Sbiv71.69 (3)
K1xiii—K1—Sbxi78.484 (17)Sn—F6—Sbi142.88 (7)
Sb—K1—Sbxi103.188 (10)K1i—F6—Sbi54.56 (3)
Snxii—K1—Sbxi116.563 (15)K2i—F6—Sbi62.34 (3)
K2xi—K1—Sbxi67.191 (11)Sb—F6—Sbi54.21 (3)
Sbv—K1—Sbxi115.843 (12)K2i—F6—Sbi122.30 (4)
F4v—K1—K294.67 (4)Sbi—F6—Sbi121.86 (4)
F2—K1—K297.42 (3)Sn—F6—Sbi110.68 (7)
F1xi—K1—K272.99 (4)K1i—F6—Sbi45.15 (3)
F6xii—K1—K2151.21 (4)K2i—F6—Sbi58.40 (4)
F3v—K1—K242.51 (3)Sb—F6—Sbi128.37 (5)
F5v—K1—K248.10 (4)K2i—F6—Sbi50.61 (3)
F1—K1—K242.72 (3)Sbi—F6—Sbi109.80 (4)
F3—K1—K276.00 (3)Sbi—F6—Sbi74.17 (2)
F4xii—K1—K2101.45 (4)Sn—F7—K2i160.99 (8)
F7xii—K1—K2145.89 (4)Sn—F7—K2i103.30 (7)
F5xii—K1—K2148.35 (3)K2i—F7—K2i94.25 (5)
K1xiii—K1—K2102.511 (19)Sn—F7—K1i91.68 (7)
Sb—K1—K269.152 (11)K2i—F7—K1i92.57 (5)
Snxii—K1—K2177.363 (18)K2i—F7—K1i99.48 (5)
K2xi—K1—K2105.673 (13)Sn—F7—Sbi96.03 (6)
Sbv—K1—K267.947 (11)K2i—F7—Sbi77.39 (5)
Sbxi—K1—K266.072 (11)K2i—F7—Sbi87.21 (5)
F4v—K1—K2v62.75 (4)K1i—F7—Sbi168.39 (6)
F2—K1—K2v73.17 (4)Sn—F7—Sbi84.28 (5)
F1xi—K1—K2v148.20 (3)K2i—F7—Sbi77.70 (4)
F6xii—K1—K2v94.45 (4)K2i—F7—Sbi171.22 (6)
F3v—K1—K2v72.82 (3)K1i—F7—Sbi84.54 (4)
F5v—K1—K2v131.10 (4)Sbi—F7—Sbi87.60 (4)
F1—K1—K2v93.76 (3)Sn—F7—Sbi128.27 (7)
F3—K1—K2v39.16 (3)K2i—F7—Sbi67.72 (3)
F4xii—K1—K2v146.51 (3)K2i—F7—Sbi57.73 (3)
F7xii—K1—K2v40.37 (4)K1i—F7—Sbi52.36 (3)
F5xii—K1—K2v79.29 (4)Sbi—F7—Sbi126.52 (4)
K1xiii—K1—K2v110.234 (19)Sbi—F7—Sbi120.88 (4)
Sb—K1—K2v67.341 (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.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FI2062).

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