Acta Cryst. (2008). E64, i32 [ doi:10.1107/S1600536808012865 ]
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.
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).
The maximum peak and deepest hole are located 0.70 Å and 0.96 Å, respectively, from Sn.
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).
| K4Sb2SnF14 | Z = 1 |
| Mr = 784.59 | F000 = 354 |
| Triclinic, P1 | Dx = 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 = 3.4–46.9º |
| α = 92.691 (1)º | µ = 7.00 mm−1 |
| β = 91.461 (1)º | T = 298 (2) K |
| γ = 115.323 (1)º | Prism, colourless |
| V = 346.526 (17) Å3 | 0.4 × 0.35 × 0.28 mm |
| Bruker SMART 1000 CCD area-detector diffractometer | 4635 independent reflections |
| Radiation source: fine-focus sealed tube | 4250 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.024 |
| Detector resolution: 8.33 pixels mm-1 | θmax = 47.0º |
| T = 298(2) K | θmin = 3.4º |
| φ and ω scans | h = −9→13 |
| Absorption correction: gaussian (XPREP and SADABS; Bruker, 2003) | k = −15→9 |
| Tmin = 0.136, Tmax = 0.291 | l = −15→11 |
| 7147 measured reflections |
| Refinement on F2 | Secondary 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) = 0.090 | Δρmax = 1.91 e Å−3 |
| S = 1.30 | Δρmin = −3.69 e Å−3 |
| 4635 reflections | Extinction correction: SHELXTL (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 98 parameters | Extinction coefficient: 0.0782 (13) |
| Primary atom site location: structure-invariant direct methods |
| K4Sb2SnF14 | γ = 115.323 (1)º |
| Mr = 784.59 | V = 346.526 (17) Å3 |
| Triclinic, P1 | Z = 1 |
| a = 6.7356 (2) Å | Mo Kα |
| b = 7.4704 (2) Å | µ = 7.00 mm−1 |
| c = 7.6370 (2) Å | T = 298 (2) K |
| α = 92.691 (1)º | 0.4 × 0.35 × 0.28 mm |
| β = 91.461 (1)º |
| Bruker SMART 1000 CCD area-detector diffractometer | 4635 independent reflections |
| Absorption correction: gaussian (XPREP and SADABS; Bruker, 2003) | 4250 reflections with I > 2σ(I) |
| Tmin = 0.136, Tmax = 0.291 | Rint = 0.024 |
| 7147 measured reflections |
| R[F2 > 2σ(F2)] = 0.037 | 98 parameters |
| wR(F2) = 0.090 | Δρmax = 1.91 e Å−3 |
| S = 1.30 | Δρmin = −3.69 e Å−3 |
| 4635 reflections |
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. |
| x | y | z | Uiso*/Ueq | ||
| 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) |
| 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) |
| Sb—F1 | 1.9380 (14) | K2—F2xi | 2.6777 (18) |
| Sb—F3 | 1.9539 (13) | K2—F3v | 2.7136 (15) |
| Sb—F4 | 2.0609 (17) | K2—F1 | 2.7216 (15) |
| Sb—F2 | 2.0696 (15) | K2—F7xv | 2.7620 (19) |
| Sb—F4i | 2.7516 (15) | K2—F7xvi | 2.8795 (17) |
| Sb—F5ii | 3.0471 (18) | K2—F6i | 2.8943 (16) |
| Sb—F6 | 3.117 (2) | K2—F5v | 2.9912 (18) |
| Sb—F7iii | 3.5325 (19) | K2—F6xvi | 3.655 (2) |
| Sb—K1 | 3.7207 (5) | K2—Snxvi | 3.8388 (5) |
| Sb—F6iv | 3.8032 (18) | K2—F4 | 3.847 (2) |
| Sb—F5 | 3.8531 (19) | K2—K1xi | 3.9388 (7) |
| Sb—F1i | 3.9018 (16) | K2—F3xiv | 3.9710 (17) |
| Sb—K1v | 3.9464 (5) | K2—Sbxiv | 3.9808 (5) |
| Sb—K2vi | 3.9808 (5) | K2—K2xvii | 3.9938 (10) |
| Sb—Sbi | 3.9925 (2) | K2—K2xviii | 4.1352 (10) |
| Sn—F5 | 1.9581 (14) | K2—F1xi | 4.1386 (18) |
| Sn—F5iii | 1.9581 (14) | K2—K1v | 4.2602 (8) |
| Sn—F7iii | 1.9611 (17) | K2—Sbxi | 4.3692 (6) |
| Sn—F7 | 1.9611 (17) | F1—K1xi | 2.7268 (16) |
| Sn—F6iii | 1.9611 (16) | F1—Sbi | 3.9018 (16) |
| Sn—F6 | 1.9611 (16) | F1—K2xi | 4.1386 (18) |
| Sn—K1vii | 3.7354 (5) | F1—Sbxi | 4.3632 (17) |
| Sn—K1viii | 3.7354 (5) | F2—K2vi | 2.6662 (15) |
| Sn—K2ix | 3.8388 (5) | F2—K2xi | 2.6777 (18) |
| Sn—K2v | 3.8388 (5) | F3—K2v | 2.7136 (14) |
| Sb—Sn | 4.21660 (15) | F3—K1v | 2.8390 (18) |
| Sn—Sbiii | 4.21661 (15) | F3—K2vi | 3.9710 (17) |
| Sn—Sbiv | 4.33908 (16) | F3—Sbv | 4.2172 (14) |
| Sn—Sbx | 4.33908 (16) | F4—K1v | 2.6235 (15) |
| K1—F4v | 2.6235 (16) | F4—Sbi | 2.7516 (15) |
| K1—F2 | 2.7086 (14) | F4—K1viii | 2.982 (2) |
| K1—F1xi | 2.7268 (16) | F5—K1v | 2.8578 (16) |
| K1—F6xii | 2.811 (2) | F5—K2v | 2.9912 (18) |
| K1—F3v | 2.8390 (18) | F5—Sbx | 3.0471 (18) |
| K1—F5v | 2.8578 (16) | F5—K1viii | 3.1882 (17) |
| K1—F1 | 2.9262 (15) | F5—Sbxv | 4.9869 (18) |
| K1—F3 | 2.9485 (18) | F6—K1viii | 2.811 (2) |
| K1—F4xii | 2.982 (2) | F6—K2i | 2.8943 (16) |
| K1—F7xii | 3.122 (2) | F6—K2ix | 3.655 (2) |
| K1—F5xii | 3.1882 (17) | F6—Sbiv | 3.8032 (18) |
| K1—K1xiii | 3.7178 (9) | F6—Sbi | 4.9129 (17) |
| K1—Snxii | 3.7354 (5) | F6—Sbviii | 5.124 (2) |
| K1—K2xi | 3.9388 (7) | F7—K2xv | 2.7620 (19) |
| K1—Sbv | 3.9464 (5) | F7—K2ix | 2.8795 (16) |
| K1—Sbxi | 4.0028 (5) | F7—K1viii | 3.1222 (19) |
| K1—K2 | 4.0117 (7) | F7—Sbiii | 3.5325 (19) |
| K1—K2v | 4.2602 (8) | F7—Sbx | 4.0712 (16) |
| K1—Sbxii | 4.4308 (6) | F7—Sbviii | 4.6870 (16) |
| K2—F2xiv | 2.6662 (15) | ||
| F1—Sb—F3 | 87.64 (6) | Snxii—K1—K2v | 70.956 (11) |
| F1—Sb—F4 | 82.57 (7) | K2xi—K1—K2v | 110.414 (15) |
| F3—Sb—F4 | 80.01 (6) | Sbv—K1—K2v | 64.623 (11) |
| F1—Sb—F2 | 80.77 (6) | Sbxi—K1—K2v | 170.056 (15) |
| F3—Sb—F2 | 79.13 (6) | K2—K1—K2v | 106.442 (15) |
| F4—Sb—F2 | 153.71 (6) | F4v—K1—Sbxii | 105.98 (4) |
| F1—Sb—F4i | 71.19 (6) | F2—K1—Sbxii | 103.48 (4) |
| F3—Sb—F4i | 143.84 (6) | F1xi—K1—Sbxii | 60.65 (4) |
| F4—Sb—F4i | 68.69 (6) | F6xii—K1—Sbxii | 44.34 (4) |
| F2—Sb—F4i | 123.67 (6) | F3v—K1—Sbxii | 142.69 (4) |
| F1—Sb—F5ii | 80.34 (5) | F5v—K1—Sbxii | 83.36 (4) |
| F3—Sb—F5ii | 145.85 (6) | F1—K1—Sbxii | 123.89 (4) |
| F4—Sb—F5ii | 129.10 (5) | F3—K1—Sbxii | 155.13 (3) |
| F2—Sb—F5ii | 67.49 (5) | F4xii—K1—Sbxii | 23.27 (3) |
| F4i—Sb—F5ii | 60.42 (5) | F7xii—K1—Sbxii | 92.88 (4) |
| F1—Sb—F6 | 156.26 (6) | F5xii—K1—Sbxii | 58.05 (4) |
| F3—Sb—F6 | 91.23 (6) | K1xiii—K1—Sbxii | 57.132 (15) |
| F4—Sb—F6 | 73.89 (6) | Sb—K1—Sbxii | 132.635 (13) |
| F2—Sb—F6 | 122.29 (5) | Snxii—K1—Sbxii | 61.479 (8) |
| F4i—Sb—F6 | 96.84 (5) | K2xi—K1—Sbxii | 63.210 (12) |
| F5ii—Sb—F6 | 112.19 (4) | Sbv—K1—Sbxii | 127.696 (11) |
| F1—Sb—F7iii | 144.50 (5) | Sbxi—K1—Sbxii | 56.236 (8) |
| F3—Sb—F7iii | 60.78 (5) | K2—K1—Sbxii | 121.076 (15) |
| F4—Sb—F7iii | 105.41 (6) | K2v—K1—Sbxii | 132.216 (14) |
| F2—Sb—F7iii | 77.82 (5) | F2xiv—K2—F2xi | 83.28 (5) |
| F4i—Sb—F7iii | 144.19 (5) | F2xiv—K2—F3v | 138.86 (5) |
| F5ii—Sb—F7iii | 116.08 (4) | F2xi—K2—F3v | 116.46 (5) |
| F6—Sb—F7iii | 49.35 (4) | F2xiv—K2—F1 | 145.86 (5) |
| F1—Sb—K1 | 51.20 (4) | F2xi—K2—F1 | 75.98 (5) |
| F3—Sb—K1 | 51.92 (5) | F3v—K2—F1 | 75.22 (4) |
| F4—Sb—K1 | 108.38 (5) | F2xiv—K2—F7xv | 85.87 (5) |
| F2—Sb—K1 | 45.52 (4) | F2xi—K2—F7xv | 163.17 (5) |
| F4i—Sb—K1 | 121.51 (4) | F3v—K2—F7xv | 80.02 (5) |
| F5ii—Sb—K1 | 97.07 (3) | F1—K2—F7xv | 107.02 (6) |
| F6—Sb—K1 | 140.19 (3) | F2xiv—K2—F7xvi | 73.56 (5) |
| F7iii—Sb—K1 | 94.15 (3) | F2xi—K2—F7xvi | 103.37 (5) |
| F1—Sb—F6iv | 119.92 (6) | F3v—K2—F7xvi | 67.03 (5) |
| F3—Sb—F6iv | 118.94 (5) | F1—K2—F7xvi | 137.34 (5) |
| F4—Sb—F6iv | 149.10 (6) | F7xv—K2—F7xvi | 85.75 (5) |
| F2—Sb—F6iv | 56.92 (5) | F2xiv—K2—F6i | 69.80 (5) |
| F4i—Sb—F6iv | 97.15 (4) | F2xi—K2—F6i | 68.66 (5) |
| F5ii—Sb—F6iv | 46.60 (4) | F3v—K2—F6i | 149.54 (5) |
| F6—Sb—F6iv | 81.11 (5) | F1—K2—F6i | 77.45 (5) |
| F7iii—Sb—F6iv | 69.52 (4) | F7xv—K2—F6i | 95.51 (6) |
| K1—Sb—F6iv | 102.43 (3) | F7xvi—K2—F6i | 143.13 (5) |
| F1—Sb—F5 | 124.91 (5) | F2xiv—K2—F5v | 105.63 (5) |
| F3—Sb—F5 | 47.69 (6) | F2xi—K2—F5v | 62.58 (5) |
| F4—Sb—F5 | 62.29 (5) | F3v—K2—F5v | 61.36 (5) |
| F2—Sb—F5 | 112.55 (5) | F1—K2—F5v | 88.59 (5) |
| F4i—Sb—F5 | 123.65 (5) | F7xv—K2—F5v | 133.22 (5) |
| F5ii—Sb—F5 | 154.74 (5) | F7xvi—K2—F5v | 56.44 (5) |
| F6—Sb—F5 | 44.86 (4) | F6i—K2—F5v | 131.19 (6) |
| F7iii—Sb—F5 | 43.91 (4) | F2xiv—K2—F6xvi | 57.19 (4) |
| K1—Sb—F5 | 99.51 (3) | F2xi—K2—F6xvi | 58.00 (4) |
| F6iv—Sb—F5 | 110.73 (4) | F3v—K2—F6xvi | 101.14 (4) |
| F1—Sb—F1i | 101.60 (5) | F1—K2—F6xvi | 126.75 (5) |
| F3—Sb—F1i | 119.88 (6) | F7xv—K2—F6xvi | 124.94 (5) |
| F4—Sb—F1i | 43.93 (5) | F7xvi—K2—F6xvi | 47.89 (5) |
| F2—Sb—F1i | 160.78 (5) | F6i—K2—F6xvi | 105.87 (4) |
| F4i—Sb—F1i | 42.52 (5) | F5v—K2—F6xvi | 48.52 (4) |
| F5ii—Sb—F1i | 93.92 (4) | F2xiv—K2—Snxvi | 80.82 (3) |
| F6—Sb—F1i | 58.86 (4) | F2xi—K2—Snxvi | 75.59 (3) |
| F7iii—Sb—F1i | 107.93 (3) | F3v—K2—Snxvi | 71.04 (4) |
| K1—Sb—F1i | 147.81 (2) | F1—K2—Snxvi | 118.69 (4) |
| F6iv—Sb—F1i | 107.05 (3) | F7xv—K2—Snxvi | 115.30 (4) |
| F5—Sb—F1i | 82.00 (3) | F7xvi—K2—Snxvi | 29.81 (4) |
| F1—Sb—K1v | 83.19 (5) | F6i—K2—Snxvi | 135.57 (4) |
| F3—Sb—K1v | 42.71 (5) | F5v—K2—Snxvi | 30.19 (3) |
| F4—Sb—K1v | 37.30 (4) | F6xvi—K2—Snxvi | 30.21 (2) |
| F2—Sb—K1v | 120.02 (4) | F2xiv—K2—F4 | 134.72 (4) |
| F4i—Sb—K1v | 104.20 (4) | F2xi—K2—F4 | 116.59 (4) |
| F5ii—Sb—K1v | 160.47 (3) | F3v—K2—F4 | 70.89 (4) |
| F6—Sb—K1v | 79.99 (3) | F1—K2—F4 | 43.32 (5) |
| F7iii—Sb—K1v | 83.45 (3) | F7xv—K2—F4 | 63.76 (5) |
| K1—Sb—K1v | 80.495 (13) | F7xvi—K2—F4 | 131.42 (5) |
| F6iv—Sb—K1v | 152.92 (3) | F6i—K2—F4 | 80.07 (5) |
| F5—Sb—K1v | 42.97 (2) | F5v—K2—F4 | 119.65 (4) |
| F1i—Sb—K1v | 79.15 (2) | F6xvi—K2—F4 | 167.89 (4) |
| F1—Sb—K2vi | 117.92 (5) | Snxvi—K2—F4 | 141.35 (3) |
| F3—Sb—K2vi | 75.50 (5) | F2xiv—K2—K1xi | 103.45 (4) |
| F4—Sb—K2vi | 146.86 (5) | F2xi—K2—K1xi | 43.32 (3) |
| F2—Sb—K2vi | 37.79 (4) | F3v—K2—K1xi | 115.64 (4) |
| F4i—Sb—K2vi | 140.23 (4) | F1—K2—K1xi | 43.76 (3) |
| F5ii—Sb—K2vi | 82.15 (3) | F7xv—K2—K1xi | 128.37 (4) |
| F6—Sb—K2vi | 84.58 (3) | F7xvi—K2—K1xi | 145.82 (4) |
| F7iii—Sb—K2vi | 42.62 (3) | F6i—K2—K1xi | 45.47 (4) |
| K1—Sb—K2vi | 72.944 (11) | F5v—K2—K1xi | 93.55 (3) |
| F6iv—Sb—K2vi | 43.58 (2) | F6xvi—K2—K1xi | 101.07 (3) |
| F5—Sb—K2vi | 84.66 (3) | Snxvi—K2—K1xi | 116.309 (16) |
| F1i—Sb—K2vi | 138.75 (2) | F4—K2—K1xi | 75.33 (3) |
| K1v—Sb—K2vi | 115.096 (10) | F2xiv—K2—F3xiv | 39.66 (4) |
| F1—Sb—Sbi | 73.20 (5) | F2xi—K2—F3xiv | 121.93 (4) |
| F3—Sb—Sbi | 117.83 (5) | F3v—K2—F3xiv | 106.25 (4) |
| F4—Sb—Sbi | 39.94 (4) | F1—K2—F3xiv | 155.67 (5) |
| F2—Sb—Sbi | 147.66 (4) | F7xv—K2—F3xiv | 50.88 (5) |
| F4i—Sb—Sbi | 28.74 (4) | F7xvi—K2—F3xiv | 59.33 (4) |
| F5ii—Sb—Sbi | 89.16 (3) | F6i—K2—F3xiv | 93.31 (4) |
| F6—Sb—Sbi | 86.50 (3) | F5v—K2—F3xiv | 113.77 (4) |
| F7iii—Sb—Sbi | 134.11 (3) | F6xvi—K2—F3xiv | 77.30 (4) |
| K1—Sb—Sbi | 121.530 (9) | Snxvi—K2—F3xiv | 83.69 (2) |
| F6iv—Sb—Sbi | 121.92 (2) | F4—K2—F3xiv | 113.32 (4) |
| F5—Sb—Sbi | 98.15 (3) | K1xi—K2—F3xiv | 137.39 (2) |
| F1i—Sb—Sbi | 28.39 (2) | F2xiv—K2—Sbxiv | 28.40 (3) |
| K1v—Sb—Sbi | 76.021 (8) | F2xi—K2—Sbxiv | 106.25 (3) |
| K2vi—Sb—Sbi | 164.150 (8) | F3v—K2—Sbxiv | 132.62 (4) |
| F5—Sn—F5iii | 180.00 (5) | F1—K2—Sbxiv | 137.36 (3) |
| F5—Sn—F7iii | 90.26 (7) | F7xv—K2—Sbxiv | 59.99 (4) |
| F5iii—Sn—F7iii | 89.74 (7) | F7xvi—K2—Sbxiv | 84.57 (4) |
| F5—Sn—F7 | 89.74 (7) | F6i—K2—Sbxiv | 64.94 (4) |
| F5iii—Sn—F7 | 90.26 (7) | F5v—K2—Sbxiv | 131.15 (3) |
| F7iii—Sn—F7 | 180.00 (14) | F6xvi—K2—Sbxiv | 84.19 (3) |
| F5—Sn—F6iii | 91.07 (7) | Snxvi—K2—Sbxiv | 102.504 (11) |
| F5iii—Sn—F6iii | 88.93 (7) | F4—K2—Sbxiv | 107.92 (3) |
| F7iii—Sn—F6iii | 88.84 (8) | K1xi—K2—Sbxiv | 109.172 (12) |
| F7—Sn—F6iii | 91.16 (8) | F3xiv—K2—Sbxiv | 28.449 (19) |
| F5—Sn—F6 | 88.93 (7) | F2xiv—K2—K2xvii | 41.75 (4) |
| F5iii—Sn—F6 | 91.07 (7) | F2xi—K2—K2xvii | 41.53 (3) |
| F7iii—Sn—F6 | 91.16 (8) | F3v—K2—K2xvii | 143.27 (4) |
| F7—Sn—F6 | 88.84 (8) | F1—K2—K2xvii | 112.96 (4) |
| F6iii—Sn—F6 | 180.00 (16) | F7xv—K2—K2xvii | 126.42 (4) |
| F5—Sn—K1vii | 121.41 (5) | F7xvi—K2—K2xvii | 88.06 (4) |
| F5iii—Sn—K1vii | 58.59 (5) | F6i—K2—K2xvii | 61.68 (4) |
| F7iii—Sn—K1vii | 56.67 (6) | F5v—K2—K2xvii | 82.59 (4) |
| F7—Sn—K1vii | 123.33 (6) | F6xvi—K2—K2xvii | 44.19 (3) |
| F6iii—Sn—K1vii | 47.50 (6) | Snxvi—K2—K2xvii | 74.136 (15) |
| F6—Sn—K1vii | 132.50 (6) | F4—K2—K2xvii | 140.33 (3) |
| F5—Sn—K1viii | 58.59 (5) | K1xi—K2—K2xvii | 70.576 (15) |
| F5iii—Sn—K1viii | 121.41 (5) | F3xiv—K2—K2xvii | 80.83 (3) |
| F7iii—Sn—K1viii | 123.33 (6) | Sbxiv—K2—K2xvii | 66.445 (12) |
| F7—Sn—K1viii | 56.67 (6) | F2xiv—K2—K1 | 149.45 (4) |
| F6iii—Sn—K1viii | 132.50 (6) | F2xi—K2—K1 | 74.53 (3) |
| F6—Sn—K1viii | 47.50 (6) | F3v—K2—K1 | 44.99 (4) |
| K1vii—Sn—K1viii | 180.000 (14) | F1—K2—K1 | 46.84 (3) |
| F5—Sn—K2ix | 129.80 (5) | F7xv—K2—K1 | 119.96 (4) |
| F5iii—Sn—K2ix | 50.20 (5) | F7xvi—K2—K1 | 91.21 (4) |
| F7iii—Sn—K2ix | 133.12 (5) | F6i—K2—K1 | 118.92 (4) |
| F7—Sn—K2ix | 46.88 (5) | F5v—K2—K1 | 45.32 (3) |
| F6iii—Sn—K2ix | 110.30 (6) | F6xvi—K2—K1 | 92.86 (3) |
| F6—Sn—K2ix | 69.70 (6) | Snxvi—K2—K1 | 73.573 (11) |
| K1vii—Sn—K2ix | 105.549 (10) | F4—K2—K1 | 75.05 (3) |
| K1viii—Sn—K2ix | 74.451 (10) | K1xi—K2—K1 | 74.327 (13) |
| F5—Sn—K2v | 50.20 (5) | F3xiv—K2—K1 | 147.77 (2) |
| F5iii—Sn—K2v | 129.80 (5) | Sbxiv—K2—K1 | 175.774 (15) |
| F7iii—Sn—K2v | 46.88 (5) | K2xvii—K2—K1 | 113.33 (2) |
| F7—Sn—K2v | 133.12 (5) | F2xiv—K2—K2xviii | 75.81 (4) |
| F6iii—Sn—K2v | 69.70 (6) | F2xi—K2—K2xviii | 143.16 (4) |
| F6—Sn—K2v | 110.30 (6) | F3v—K2—K2xviii | 67.21 (4) |
| K1vii—Sn—K2v | 74.451 (10) | F1—K2—K2xviii | 135.04 (4) |
| K1viii—Sn—K2v | 105.549 (10) | F7xv—K2—K2xviii | 43.98 (3) |
| K2ix—Sn—K2v | 180.000 (9) | F7xvi—K2—K2xviii | 41.77 (4) |
| F5—Sn—Sb | 65.81 (5) | F6i—K2—K2xviii | 128.40 (5) |
| F5iii—Sn—Sb | 114.19 (5) | F5v—K2—K2xviii | 94.15 (4) |
| F7iii—Sn—Sb | 56.42 (6) | F6xvi—K2—K2xviii | 85.16 (3) |
| F7—Sn—Sb | 123.58 (6) | Snxvi—K2—K2xviii | 71.414 (13) |
| F6iii—Sn—Sb | 136.06 (6) | F4—K2—K2xviii | 99.52 (3) |
| F6—Sn—Sb | 43.94 (6) | K1xi—K2—K2xviii | 172.16 (2) |
| K1vii—Sn—Sb | 112.591 (9) | F3xiv—K2—K2xviii | 39.05 (2) |
| K1viii—Sn—Sb | 67.409 (9) | Sbxiv—K2—K2xviii | 66.425 (12) |
| K2ix—Sn—Sb | 113.168 (8) | K2xvii—K2—K2xviii | 111.90 (2) |
| K2v—Sn—Sb | 66.832 (8) | K1—K2—K2xviii | 110.379 (17) |
| F5—Sn—Sbiii | 114.19 (5) | F2xiv—K2—F1xi | 120.78 (4) |
| F5iii—Sn—Sbiii | 65.81 (5) | F2xi—K2—F1xi | 37.66 (4) |
| F7iii—Sn—Sbiii | 123.58 (6) | F3v—K2—F1xi | 83.92 (4) |
| F7—Sn—Sbiii | 56.42 (6) | F1—K2—F1xi | 46.14 (5) |
| F6iii—Sn—Sbiii | 43.94 (6) | F7xv—K2—F1xi | 151.93 (5) |
| F6—Sn—Sbiii | 136.06 (6) | F7xvi—K2—F1xi | 108.92 (4) |
| K1vii—Sn—Sbiii | 67.409 (9) | F6i—K2—F1xi | 86.80 (5) |
| K1viii—Sn—Sbiii | 112.591 (9) | F5v—K2—F1xi | 52.66 (4) |
| K2ix—Sn—Sbiii | 66.832 (8) | F6xvi—K2—F1xi | 80.65 (4) |
| K2v—Sn—Sbiii | 113.168 (8) | Snxvi—K2—F1xi | 80.33 (2) |
| Sb—Sn—Sbiii | 180.0 | F4—K2—F1xi | 89.28 (3) |
| F4v—K1—F2 | 135.92 (6) | K1xi—K2—F1xi | 42.39 (2) |
| F4v—K1—F1xi | 148.39 (5) | F3xiv—K2—F1xi | 157.10 (4) |
| F2—K1—F1xi | 75.39 (5) | Sbxiv—K2—F1xi | 142.70 (2) |
| F4v—K1—F6xii | 112.69 (5) | K2xvii—K2—F1xi | 79.10 (3) |
| F2—K1—F6xii | 69.51 (5) | K1—K2—F1xi | 39.05 (2) |
| F1xi—K1—F6xii | 78.81 (5) | K2xviii—K2—F1xi | 144.60 (3) |
| F4v—K1—F3v | 56.26 (5) | F2xiv—K2—K1v | 132.57 (4) |
| F2—K1—F3v | 111.27 (5) | F2xi—K2—K1v | 143.70 (4) |
| F1xi—K1—F3v | 115.30 (5) | F3v—K2—K1v | 43.33 (4) |
| F6xii—K1—F3v | 165.82 (5) | F1—K2—K1v | 69.71 (4) |
| F4v—K1—F5v | 77.12 (5) | F7xv—K2—K1v | 47.07 (4) |
| F2—K1—F5v | 138.76 (5) | F7xvi—K2—K1v | 94.17 (4) |
| F1xi—K1—F5v | 73.05 (5) | F6i—K2—K1v | 113.54 (4) |
| F6xii—K1—F5v | 127.69 (6) | F5v—K2—K1v | 104.38 (4) |
| F3v—K1—F5v | 61.68 (5) | F6xvi—K2—K1v | 140.15 (3) |
| F4v—K1—F1 | 125.45 (5) | Snxvi—K2—K1v | 110.896 (12) |
| F2—K1—F1 | 54.76 (4) | F4—K2—K1v | 37.32 (2) |
| F1xi—K1—F1 | 63.69 (6) | K1xi—K2—K1v | 110.414 (15) |
| F6xii—K1—F1 | 117.92 (5) | F3xiv—K2—K1v | 94.36 (3) |
| F3v—K1—F1 | 70.23 (4) | Sbxiv—K2—K1v | 106.861 (15) |
| F5v—K1—F1 | 87.34 (4) | K2xvii—K2—K1v | 172.75 (2) |
| F4v—K1—F3 | 89.08 (5) | K1—K2—K1v | 73.558 (15) |
| F2—K1—F3 | 53.71 (5) | K2xviii—K2—K1v | 66.149 (15) |
| F1xi—K1—F3 | 114.74 (4) | F1xi—K2—K1v | 106.60 (2) |
| F6xii—K1—F3 | 111.78 (5) | F2xiv—K2—Sbxi | 96.86 (4) |
| F3v—K1—F3 | 62.17 (5) | F2xi—K2—Sbxi | 20.08 (3) |
| F5v—K1—F3 | 119.86 (5) | F3v—K2—Sbxi | 96.64 (4) |
| F1—K1—F3 | 54.61 (4) | F1—K2—Sbxi | 71.72 (4) |
| F4v—K1—F4xii | 97.18 (5) | F7xv—K2—Sbxi | 176.66 (4) |
| F2—K1—F4xii | 121.36 (5) | F7xvi—K2—Sbxi | 93.17 (4) |
| F1xi—K1—F4xii | 58.73 (4) | F6i—K2—Sbxi | 87.26 (4) |
| F6xii—K1—F4xii | 67.58 (5) | F5v—K2—Sbxi | 44.16 (3) |
| F3v—K1—F4xii | 120.01 (5) | F6xvi—K2—Sbxi | 55.73 (3) |
| F5v—K1—F4xii | 60.16 (5) | Snxvi—K2—Sbxi | 63.440 (9) |
| F1—K1—F4xii | 119.49 (5) | F4—K2—Sbxi | 115.04 (3) |
| F3—K1—F4xii | 173.45 (4) | K1xi—K2—Sbxi | 52.902 (10) |
| F4v—K1—F7xii | 77.31 (5) | F3xiv—K2—Sbxi | 130.95 (3) |
| F2—K1—F7xii | 69.12 (4) | Sbxiv—K2—Sbxi | 123.080 (12) |
| F1xi—K1—F7xii | 128.67 (5) | K2xvii—K2—Sbxi | 56.635 (14) |
| F6xii—K1—F7xii | 54.82 (5) | K1—K2—Sbxi | 56.866 (11) |
| F3v—K1—F7xii | 111.57 (5) | K2xviii—K2—Sbxi | 134.85 (2) |
| F5v—K1—F7xii | 152.00 (5) | F1xi—K2—Sbxi | 26.15 (2) |
| F1—K1—F7xii | 117.02 (4) | K1v—K2—Sbxi | 129.978 (13) |
| F3—K1—F7xii | 70.83 (4) | Sb—F1—K2 | 140.58 (8) |
| F4xii—K1—F7xii | 112.37 (5) | Sb—F1—K1xi | 117.20 (6) |
| F4v—K1—F5xii | 59.59 (5) | K2—F1—K1xi | 92.59 (5) |
| F2—K1—F5xii | 113.82 (4) | Sb—F1—K1 | 97.72 (5) |
| F1xi—K1—F5xii | 118.46 (5) | K2—F1—K1 | 90.44 (4) |
| F6xii—K1—F5xii | 54.02 (4) | K1xi—F1—K1 | 116.31 (6) |
| F3v—K1—F5xii | 115.85 (4) | Sb—F1—Sbi | 78.40 (5) |
| F5v—K1—F5xii | 104.33 (4) | K2—F1—Sbi | 81.29 (4) |
| F1—K1—F5xii | 168.30 (4) | K1xi—F1—Sbi | 81.82 (3) |
| F3—K1—F5xii | 118.02 (5) | K1—F1—Sbi | 160.56 (6) |
| F4xii—K1—F5xii | 67.26 (5) | Sb—F1—K2xi | 83.58 (5) |
| F7xii—K1—F5xii | 51.96 (4) | K2—F1—K2xi | 133.86 (5) |
| F4v—K1—K1xiii | 52.74 (4) | K1xi—F1—K2xi | 67.96 (4) |
| F2—K1—K1xiii | 157.57 (4) | K1—F1—K2xi | 65.15 (3) |
| F1xi—K1—K1xiii | 100.64 (4) | Sbi—F1—K2xi | 132.27 (4) |
| F6xii—K1—K1xiii | 88.06 (4) | Sb—F1—Sbxi | 145.08 (7) |
| F3v—K1—K1xiii | 90.53 (3) | K2—F1—Sbxi | 71.96 (3) |
| F5v—K1—K1xiii | 56.19 (4) | K1xi—F1—Sbxi | 57.94 (3) |
| F1—K1—K1xiii | 143.52 (4) | K1—F1—Sbxi | 63.04 (3) |
| F3—K1—K1xiii | 141.78 (4) | Sbi—F1—Sbxi | 129.25 (3) |
| F4xii—K1—K1xiii | 44.44 (3) | K2xi—F1—Sbxi | 62.18 (3) |
| F7xii—K1—K1xiii | 98.64 (3) | Sb—F2—K2vi | 113.81 (7) |
| F5xii—K1—K1xiii | 48.14 (3) | Sb—F2—K2xi | 133.55 (7) |
| F4v—K1—Sb | 119.75 (5) | K2vi—F2—K2xi | 96.72 (5) |
| F2—K1—Sb | 33.04 (3) | Sb—F2—K1 | 101.44 (6) |
| F1xi—K1—Sb | 83.66 (3) | K2vi—F2—K1 | 117.00 (5) |
| F6xii—K1—Sb | 102.46 (4) | K2xi—F2—K1 | 93.98 (5) |
| F3v—K1—Sb | 78.76 (3) | Sb—F3—K2v | 144.17 (8) |
| F5v—K1—Sb | 116.80 (4) | Sb—F3—K1v | 109.46 (6) |
| F1—K1—Sb | 31.07 (3) | K2v—F3—K1v | 92.49 (5) |
| F3—K1—Sb | 31.44 (3) | Sb—F3—K1 | 96.64 (6) |
| F4xii—K1—Sb | 142.03 (3) | K2v—F3—K1 | 97.51 (5) |
| F7xii—K1—Sb | 85.99 (3) | K1v—F3—K1 | 117.83 (5) |
| F5xii—K1—Sb | 137.87 (3) | Sb—F3—K2vi | 76.06 (5) |
| K1xiii—K1—Sb | 169.27 (2) | K2v—F3—K2vi | 73.75 (4) |
| F4v—K1—Snxii | 83.78 (4) | K1v—F3—K2vi | 158.09 (6) |
| F2—K1—Snxii | 82.30 (3) | K1—F3—K2vi | 81.50 (4) |
| F1xi—K1—Snxii | 109.42 (4) | Sb—F3—Sbv | 140.22 (6) |
| F6xii—K1—Snxii | 30.96 (3) | K2v—F3—Sbv | 75.23 (3) |
| F3v—K1—Snxii | 135.18 (3) | K1v—F3—Sbv | 59.92 (3) |
| F5v—K1—Snxii | 133.25 (4) | K1—F3—Sbv | 63.99 (3) |
| F1—K1—Snxii | 137.06 (3) | K2vi—F3—Sbv | 129.27 (4) |
| F3—K1—Snxii | 101.81 (3) | Sb—F4—K1v | 114.26 (6) |
| F4xii—K1—Snxii | 80.88 (3) | Sb—F4—Sbi | 111.31 (6) |
| F7xii—K1—Snxii | 31.65 (3) | K1v—F4—Sbi | 130.88 (7) |
| F5xii—K1—Snxii | 31.61 (3) | Sb—F4—K1viii | 121.86 (8) |
| K1xiii—K1—Snxii | 78.252 (16) | K1v—F4—K1viii | 82.82 (5) |
| Sb—K1—Snxii | 109.774 (12) | Sbi—F4—K1viii | 88.45 (5) |
| F4v—K1—K2xi | 159.66 (4) | Sb—F4—K2 | 90.97 (6) |
| F2—K1—K2xi | 42.70 (4) | K1v—F4—K2 | 79.93 (4) |
| F1xi—K1—K2xi | 43.65 (3) | Sbi—F4—K2 | 81.98 (4) |
| F6xii—K1—K2xi | 47.22 (3) | K1viii—F4—K2 | 146.97 (6) |
| F3v—K1—K2xi | 142.68 (3) | Sn—F5—K1v | 154.71 (8) |
| F5v—K1—K2xi | 116.36 (4) | Sn—F5—K2v | 99.61 (6) |
| F1—K1—K2xi | 72.46 (3) | K1v—F5—K2v | 86.58 (5) |
| F3—K1—K2xi | 96.07 (3) | Sn—F5—Sbx | 118.58 (7) |
| F4xii—K1—K2xi | 78.71 (3) | K1v—F5—Sbx | 85.29 (4) |
| F7xii—K1—K2xi | 85.80 (4) | K2v—F5—Sbx | 92.70 (4) |
| F5xii—K1—K2xi | 100.98 (3) | Sn—F5—K1viii | 89.79 (5) |
| K1xiii—K1—K2xi | 120.30 (2) | K1v—F5—K1viii | 75.67 (4) |
| Sb—K1—K2xi | 69.495 (11) | K2v—F5—K1viii | 154.85 (7) |
| Snxii—K1—K2xi | 75.912 (12) | Sbx—F5—K1viii | 103.25 (5) |
| F4v—K1—Sbv | 28.43 (4) | Sn—F5—Sb | 86.58 (6) |
| F2—K1—Sbv | 127.52 (4) | K1v—F5—Sb | 70.26 (4) |
| F1xi—K1—Sbv | 136.40 (3) | K2v—F5—Sb | 79.97 (4) |
| F6xii—K1—Sbv | 140.46 (3) | Sbx—F5—Sb | 154.74 (5) |
| F3v—K1—Sbv | 27.83 (3) | K1viii—F5—Sb | 77.35 (4) |
| F5v—K1—Sbv | 66.77 (4) | Sn—F5—Sbxv | 124.19 (7) |
| F1—K1—Sbv | 97.55 (3) | K1v—F5—Sbxv | 61.95 (3) |
| F3—K1—Sbv | 73.82 (3) | K2v—F5—Sbxv | 132.77 (4) |
| F4xii—K1—Sbv | 111.02 (3) | Sbx—F5—Sbxv | 53.18 (3) |
| F7xii—K1—Sbv | 94.88 (4) | K1viii—F5—Sbxv | 52.27 (3) |
| F5xii—K1—Sbv | 88.02 (3) | Sb—F5—Sbxv | 116.05 (4) |
| K1xiii—K1—Sbv | 70.564 (14) | Sn—F6—K1viii | 101.55 (7) |
| Sb—K1—Sbv | 99.505 (13) | Sn—F6—K2i | 152.63 (9) |
| Snxii—K1—Sbv | 110.137 (11) | K1viii—F6—K2i | 87.31 (5) |
| K2xi—K1—Sbv | 168.929 (17) | Sn—F6—Sb | 110.18 (7) |
| F4v—K1—Sbxi | 122.89 (4) | K1viii—F6—Sb | 96.60 (5) |
| F2—K1—Sbxi | 100.69 (4) | K2i—F6—Sb | 94.19 (5) |
| F1xi—K1—Sbxi | 25.51 (3) | Sn—F6—K2ix | 80.09 (6) |
| F6xii—K1—Sbxi | 90.54 (4) | K1viii—F6—K2ix | 89.28 (6) |
| F3v—K1—Sbxi | 103.00 (3) | K2i—F6—K2ix | 74.13 (4) |
| F5v—K1—Sbxi | 49.35 (4) | Sb—F6—K2ix | 166.72 (6) |
| F1—K1—Sbxi | 76.30 (3) | Sn—F6—Sbiv | 91.99 (6) |
| F3—K1—Sbxi | 130.90 (3) | K1viii—F6—Sbiv | 154.48 (6) |
| F4xii—K1—Sbxi | 43.41 (3) | K2i—F6—Sbiv | 71.48 (4) |
| F7xii—K1—Sbxi | 145.36 (4) | Sb—F6—Sbiv | 98.89 (5) |
| F5xii—K1—Sbxi | 110.56 (4) | K2ix—F6—Sbiv | 71.69 (3) |
| K1xiii—K1—Sbxi | 78.484 (17) | Sn—F6—Sbi | 142.88 (7) |
| Sb—K1—Sbxi | 103.188 (10) | K1i—F6—Sbi | 54.56 (3) |
| Snxii—K1—Sbxi | 116.563 (15) | K2i—F6—Sbi | 62.34 (3) |
| K2xi—K1—Sbxi | 67.191 (11) | Sb—F6—Sbi | 54.21 (3) |
| Sbv—K1—Sbxi |
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].