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The crystal structure of tripotassium sodium hexa­chloro­ferrate(II) has been determined by X-ray diffraction at 293, 84 and 9.5 K. The accurate and extensive data sets collected should be suitable for charge-density analysis studies.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100006053/qb0210sup1.cif
Contains datablocks 293K, 84K, 10K, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006053/qb0210293Ksup2.hkl
Contains datablock 293K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006053/qb021084Ksup3.hkl
Contains datablock 84K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006053/qb021010Ksup4.hkl
Contains datablock 10K

Computing details top

Data collection: local software for 293K, (10K); P3/P4-PC Software (Siemens, 1991) for (84K). Cell refinement: local software for 293K, (10K); P3/P4-PC Software for (84K). For all compounds, data reduction: PROFIT (Streltsov & Zavodnik, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1983); software used to prepare material for publication: SHELXL97.

(293K) tripotassium sodium hexachloroferrate(II) top
Crystal data top
K3Na[FeCl6]Dx = 2.343 Mg m3
Mr = 408.84Melting point: not measured K
Trigonal, R3cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -R 3 2"cCell parameters from 12 reflections
a = 12.033 (2) Åθ = 15.5–15.5°
c = 13.863 (4) ŵ = 3.74 mm1
V = 1738.3 (6) Å3T = 293 K
Z = 6Cube, very pale yellow
F(000) = 11760.40 × 0.40 × 0.40 mm
Data collection top
Huber 512 goniometer
diffractometer
347 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tubeRint = 0.044
None monochromatorθmax = 25.1°, θmin = 3.4°
ω–2θ scansh = 1414
Absorption correction: for a sphere
(Xtal3.4; Hall et al., 1994)
k = 1414
Tmin = 0.268, Tmax = 0.282l = 1616
3808 measured reflections3 standard reflections every 100 reflections
347 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017 w = 1/[σ2(Fo2) + (0.0099P)2 + 0.5551P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.031(Δ/σ)max < 0.001
S = 1.62Δρmax = 0.38 e Å3
347 reflectionsΔρmin = 0.37 e Å3
20 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0146 (6)
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
xyzUiso*/Ueq
Fe0.00000.00000.00000.01592 (16)
K0.29056 (3)0.33330.08330.02606 (17)
Na0.00000.00000.25000.0282 (3)
Cl0.17995 (3)0.02704 (3)0.10753 (2)0.02232 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.01657 (19)0.01657 (19)0.0146 (2)0.00828 (9)0.0000.000
K0.0256 (2)0.0244 (2)0.0277 (3)0.01222 (12)0.00264 (8)0.00529 (16)
Na0.0334 (4)0.0334 (4)0.0176 (6)0.0167 (2)0.0000.000
Cl0.0203 (2)0.0277 (2)0.0208 (2)0.01338 (14)0.00256 (11)0.00041 (12)
Geometric parameters (Å, º) top
Fe—Cli2.5124 (5)K—Clx3.3368 (7)
Fe—Cl2.5124 (5)K—Clii3.3368 (7)
Fe—Clii2.5124 (5)K—Fexi3.9526 (6)
Fe—Cliii2.5124 (5)K—Naxii4.4302 (7)
Fe—Cliv2.5124 (5)K—Kiv4.4302 (6)
Fe—Clv2.5124 (5)Na—Cliii2.8268 (5)
Fe—Na3.466 (1)Na—Clxiii2.8268 (6)
Fe—Nai3.466 (1)Na—Clxiv2.8268 (6)
Fe—Ki3.9526 (6)Na—Clxv2.8268 (6)
Fe—K3.9526 (6)Na—Clii2.8268 (6)
Fe—Kiii3.9526 (6)Na—Cl2.8268 (6)
Fe—Kii3.9526 (6)Na—Fexiii3.466 (1)
K—Clvi3.1770 (7)Na—Kxvi4.4302 (7)
K—Cliv3.1771 (7)Na—Kii4.4302 (7)
K—Clvii3.2165 (6)Na—Kiii4.4302 (7)
K—Clviii3.2165 (6)Cl—Kv3.1771 (7)
K—Clix3.2499 (6)Cl—Kviii3.2165 (6)
K—Cl3.2499 (6)Cl—Kiii3.3368 (7)
Cli—Fe—Cl180.000 (17)Cl—K—Fe39.329 (7)
Cli—Fe—Clii91.61 (2)Clx—K—Fe99.005 (10)
Cl—Fe—Clii88.39 (2)Clii—K—Fe39.188 (7)
Cli—Fe—Cliii91.61 (2)Fexi—K—Fe135.684 (11)
Cl—Fe—Cliii88.39 (2)Clvi—K—Naxii87.834 (18)
Clii—Fe—Cliii88.39 (2)Cliv—K—Naxii83.247 (16)
Cli—Fe—Cliv88.39 (2)Clvii—K—Naxii82.819 (12)
Cl—Fe—Cliv91.61 (2)Clviii—K—Naxii130.759 (9)
Clii—Fe—Cliv91.61 (2)Clix—K—Naxii39.567 (6)
Cliii—Fe—Cliv180.000 (11)Cl—K—Naxii151.268 (9)
Cli—Fe—Clv88.39 (2)Clx—K—Naxii39.632 (6)
Cl—Fe—Clv91.61 (2)Clii—K—Naxii102.610 (10)
Clii—Fe—Clv180.000 (16)Fexi—K—Naxii48.430 (14)
Cliii—Fe—Clv91.61 (2)Fe—K—Naxii114.187 (11)
Cliv—Fe—Clv88.39 (2)Clvi—K—Kiv106.820 (16)
Cli—Fe—Na126.394 (11)Cliv—K—Kiv47.111 (8)
Cl—Fe—Na53.606 (11)Clvii—K—Kiv110.683 (19)
Clii—Fe—Na53.606 (11)Clviii—K—Kiv167.429 (6)
Cliii—Fe—Na53.606 (11)Clix—K—Kiv100.279 (12)
Cliv—Fe—Na126.394 (11)Cl—K—Kiv95.075 (6)
Clv—Fe—Na126.394 (11)Clx—K—Kiv46.330 (9)
Cli—Fe—Nai53.606 (11)Clii—K—Kiv45.651 (10)
Cl—Fe—Nai126.394 (11)Fexi—K—Kiv85.486 (11)
Clii—Fe—Nai126.394 (11)Fe—K—Kiv55.915 (2)
Cliii—Fe—Nai126.394 (11)Naxii—K—Kiv61.431 (10)
Cliv—Fe—Nai53.606 (11)Cliii—Na—Clxiii148.923 (13)
Clv—Fe—Nai53.606 (11)Cliii—Na—Clxiv127.720 (15)
Na—Fe—Nai180.0Clxiii—Na—Clxiv76.571 (17)
Cli—Fe—Ki55.066 (8)Cliii—Na—Clxv89.78 (2)
Cl—Fe—Ki124.934 (8)Clxiii—Na—Clxv76.572 (17)
Clii—Fe—Ki122.945 (8)Clxiv—Na—Clxv76.571 (17)
Cliii—Fe—Ki53.401 (16)Cliii—Na—Clii76.571 (17)
Cliv—Fe—Ki126.599 (16)Clxiii—Na—Clii89.78 (2)
Clv—Fe—Ki57.055 (8)Clxiv—Na—Clii148.923 (13)
Na—Fe—Ki106.994 (5)Clxv—Na—Clii127.720 (16)
Nai—Fe—Ki73.006 (5)Cliii—Na—Cl76.572 (17)
Cli—Fe—K124.934 (8)Clxiii—Na—Cl127.720 (16)
Cl—Fe—K55.066 (8)Clxiv—Na—Cl89.78 (2)
Clii—Fe—K57.055 (8)Clxv—Na—Cl148.923 (13)
Cliii—Fe—K126.599 (16)Clii—Na—Cl76.571 (17)
Cliv—Fe—K53.401 (16)Cliii—Na—Fexiii134.321 (11)
Clv—Fe—K122.945 (8)Clxiii—Na—Fexiii45.679 (11)
Na—Fe—K73.006 (5)Clxiv—Na—Fexiii45.679 (11)
Nai—Fe—K106.994 (5)Clxv—Na—Fexiii45.679 (11)
Ki—Fe—K180.000 (11)Clii—Na—Fexiii134.321 (11)
Cli—Fe—Kiii122.945 (8)Cl—Na—Fexiii134.321 (11)
Cl—Fe—Kiii57.055 (8)Cliii—Na—Fe45.679 (11)
Clii—Fe—Kiii126.599 (16)Clxiii—Na—Fe134.321 (11)
Cliii—Fe—Kiii55.066 (8)Clxiv—Na—Fe134.321 (11)
Cliv—Fe—Kiii124.934 (8)Clxv—Na—Fe134.321 (11)
Clv—Fe—Kiii53.401 (16)Clii—Na—Fe45.679 (11)
Na—Fe—Kiii73.006 (5)Cl—Na—Fe45.679 (11)
Nai—Fe—Kiii106.994 (5)Fexiii—Na—Fe180.0
Ki—Fe—Kiii68.169 (5)Cliii—Na—Kxvi86.238 (16)
K—Fe—Kiii111.831 (5)Clxiii—Na—Kxvi104.235 (19)
Cli—Fe—Kii53.401 (16)Clxiv—Na—Kxvi47.082 (9)
Cl—Fe—Kii126.599 (16)Clxv—Na—Kxvi48.844 (9)
Clii—Fe—Kii55.066 (8)Clii—Na—Kxvi162.671 (6)
Cliii—Fe—Kii57.055 (8)Cl—Na—Kxvi101.781 (14)
Cliv—Fe—Kii122.945 (8)Fexiii—Na—Kxvi58.564 (9)
Clv—Fe—Kii124.934 (8)Fe—Na—Kxvi121.436 (9)
Na—Fe—Kii73.006 (5)Cliii—Na—Kii48.844 (9)
Nai—Fe—Kii106.994 (5)Clxiii—Na—Kii101.780 (14)
Ki—Fe—Kii68.169 (5)Clxiv—Na—Kii162.671 (6)
K—Fe—Kii111.831 (5)Clxv—Na—Kii86.238 (16)
Kiii—Fe—Kii111.831 (5)Clii—Na—Kii47.082 (9)
Clvi—K—Cliv153.303 (18)Cl—Na—Kii104.235 (19)
Clvi—K—Clvii130.420 (12)Fexiii—Na—Kii121.435 (9)
Cliv—K—Clvii73.370 (17)Fe—Na—Kii58.565 (9)
Clvi—K—Clviii73.368 (17)Kxvi—Na—Kii118.569 (10)
Cliv—K—Clviii130.422 (12)Cliii—Na—Kiii47.082 (9)
Clvii—K—Clviii76.67 (2)Clxiii—Na—Kiii162.671 (6)
Clvi—K—Clix68.177 (13)Clxiv—Na—Kiii86.238 (16)
Cliv—K—Clix116.390 (14)Clxv—Na—Kiii101.780 (13)
Clvii—K—Clix74.157 (10)Clii—Na—Kiii104.235 (19)
Clviii—K—Clix91.483 (9)Cl—Na—Kiii48.844 (9)
Clvi—K—Cl116.390 (14)Fexiii—Na—Kiii121.435 (9)
Cliv—K—Cl68.176 (13)Fe—Na—Kiii58.565 (9)
Clvii—K—Cl91.484 (9)Kxvi—Na—Kiii64.167 (17)
Clviii—K—Cl74.159 (10)Kii—Na—Kiii95.279 (11)
Clix—K—Cl161.875 (17)Cliii—Na—K104.235 (19)
Clvi—K—Clx67.105 (14)Clxiii—Na—K86.238 (16)
Cliv—K—Clx90.597 (11)Clxiv—Na—K101.780 (14)
Clvii—K—Clx122.147 (8)Clxv—Na—K162.671 (6)
Clviii—K—Clx138.965 (10)Clii—Na—K48.844 (9)
Clix—K—Clx64.240 (11)Cl—Na—K47.082 (9)
Cl—K—Clx133.862 (11)Fexiii—Na—K121.435 (9)
Clvi—K—Clii90.598 (11)Fe—Na—K58.565 (9)
Cliv—K—Clii67.104 (14)Kxvi—Na—K140.673 (10)
Clvii—K—Clii138.966 (10)Kii—Na—K95.279 (12)
Clviii—K—Clii122.148 (8)Kiii—Na—K95.279 (11)
Clix—K—Clii133.863 (11)Fe—Cl—Na80.72 (2)
Cl—K—Clii64.239 (11)Fe—Cl—Kv87.19 (2)
Clx—K—Clii69.831 (13)Na—Cl—Kv167.815 (11)
Clvi—K—Fexi39.411 (7)Fe—Cl—Kviii168.449 (13)
Cliv—K—Fexi126.760 (9)Na—Cl—Kviii96.77 (2)
Clvii—K—Fexi113.472 (8)Kv—Cl—Kviii94.796 (19)
Clviii—K—Fexi101.149 (10)Fe—Cl—K85.605 (10)
Clix—K—Fexi39.329 (7)Na—Cl—K93.351 (9)
Cl—K—Fexi153.168 (10)Kv—Cl—K87.143 (8)
Clx—K—Fexi39.189 (7)Kviii—Cl—K105.841 (10)
Clii—K—Fexi99.006 (10)Fe—Cl—Kiii83.756 (9)
Clvi—K—Fe126.760 (9)Na—Cl—Kiii91.524 (9)
Cliv—K—Fe39.411 (7)Kv—Cl—Kiii85.669 (8)
Clvii—K—Fe101.151 (10)Kviii—Cl—Kiii85.047 (8)
Clviii—K—Fe113.473 (8)K—Cl—Kiii167.430 (11)
Clix—K—Fe153.168 (10)
Symmetry codes: (i) x, y, z; (ii) y, xy, z; (iii) x+y, x, z; (iv) xy, x, z; (v) y, x+y, z; (vi) y+1/3, x+2/3, z+1/6; (vii) x+y+2/3, y+1/3, z1/6; (viii) x+2/3, y+1/3, z+1/3; (ix) xy+1/3, y+2/3, z+1/6; (x) x+1/3, x+y+2/3, z+1/6; (xi) y+1/3, x+2/3, z+1/6; (xii) x+1/3, y+2/3, z1/3; (xiii) y, x, z+1/2; (xiv) xy, y, z+1/2; (xv) x, x+y, z+1/2; (xvi) x1/3, y2/3, z+1/3.
(84K) tripotassium sodium hexachloroferrate(II) top
Crystal data top
K3Na[FeCl6]Dx = 2.405 Mg m3
Mr = 408.84Melting point: not measured K
Trigonal, R3cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -R 3 2"cCell parameters from 14 reflections
a = 11.922 (1) Åθ = 17.0–20.5°
c = 13.761 (2) ŵ = 3.83 mm1
V = 1693.9 (3) Å3T = 84 K
Z = 6Prism, very pale yellow
F(000) = 11760.49 × 0.35 × 0.33 mm
Data collection top
Syntex P21
diffractometer
1930 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.028
Graphite monochromatorθmax = 50.1°, θmin = 3.4°
ω–2θ scansh = 2525
Absorption correction: gaussian
(Xtal 3.4; Hall et al., 1994)
k = 2525
Tmin = 0.279, Tmax = 0.377l = 2929
37086 measured reflections6 standard reflections every 100 reflections
1991 independent reflections intensity decay: 2%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.018 w = 1/[σ2(Fo2) + (0.0106P)2 + 0.791P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.036(Δ/σ)max = 0.001
S = 1.40Δρmax = 0.44 e Å3
1991 reflectionsΔρmin = 0.37 e Å3
20 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0047 (2)
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
xyzUiso*/Ueq
Fe0.00000.00000.00000.00521 (2)
K0.289724 (12)0.33330.08330.00863 (2)
Na0.00000.00000.25000.00987 (8)
Cl0.180781 (10)0.027362 (11)0.107931 (8)0.00760 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.00549 (3)0.00549 (3)0.00464 (5)0.00275 (2)0.0000.000
K0.00862 (3)0.00826 (4)0.00890 (5)0.00413 (2)0.00083 (2)0.00165 (3)
Na0.01173 (12)0.01173 (12)0.00614 (17)0.00587 (6)0.0000.000
Cl0.00706 (4)0.00934 (4)0.00697 (4)0.00453 (3)0.00078 (2)0.00015 (3)
Geometric parameters (Å, º) top
Fe—Cli2.5009 (2)K—Clx3.3011 (3)
Fe—Cl2.5009 (2)K—Cliv3.3011 (3)
Fe—Clii2.5009 (2)K—Fexi3.9130 (3)
Fe—Cliii2.5009 (2)K—Naxii4.3883 (3)
Fe—Cliv2.5009 (2)K—Kii4.3883 (3)
Fe—Clv2.5009 (2)Na—Clv2.8055 (3)
Fe—Na3.4402 (5)Na—Clxiii2.8055 (3)
Fe—Nai3.4402 (5)Na—Clxiv2.8055 (3)
Fe—K3.9130 (3)Na—Clxv2.8055 (3)
Fe—Ki3.9130 (3)Na—Cl2.8055 (3)
Fe—Kii3.9130 (3)Na—Cliv2.8055 (3)
Fe—Kiv3.9130 (3)Na—Fexiii3.4402 (5)
K—Clvi3.1496 (3)Na—Kxvi4.3883 (3)
K—Cliii3.1497 (4)Na—Kiv4.3883 (3)
K—Clvii3.1875 (3)Na—Kv4.3883 (3)
K—Clviii3.1876 (3)Cl—Kii3.1497 (3)
K—Clix3.2202 (3)Cl—Kviii3.1876 (3)
K—Cl3.2203 (3)Cl—Kv3.3011 (3)
Cli—Fe—Cl180.000 (6)Cl—K—Fe39.568 (3)
Cli—Fe—Clii88.336 (8)Clx—K—Fe99.051 (4)
Cl—Fe—Clii91.664 (7)Cliv—K—Fe39.430 (3)
Cli—Fe—Cliii88.336 (8)Fexi—K—Fe135.961 (4)
Cl—Fe—Cliii91.664 (8)Clvi—K—Naxii88.201 (9)
Clii—Fe—Cliii88.336 (8)Cliii—K—Naxii83.078 (8)
Cli—Fe—Cliv91.664 (8)Clvii—K—Naxii82.664 (6)
Cl—Fe—Cliv88.336 (8)Clviii—K—Naxii130.726 (4)
Clii—Fe—Cliv180.000 (6)Clix—K—Naxii39.665 (3)
Cliii—Fe—Cliv91.664 (7)Cl—K—Naxii151.500 (4)
Cli—Fe—Clv91.664 (8)Clx—K—Naxii39.724 (3)
Cl—Fe—Clv88.336 (8)Cliv—K—Naxii102.749 (4)
Clii—Fe—Clv91.664 (8)Fexi—K—Naxii48.551 (7)
Cliii—Fe—Clv180.000 (10)Fe—K—Naxii114.284 (5)
Clv—Fe—Cliv88.336 (8)Clvi—K—Kii153.376 (3)
Cli—Fe—Na126.433 (5)Cliii—K—Kii48.602 (4)
Cl—Fe—Na53.567 (5)Clvii—K—Kii48.548 (4)
Clii—Fe—Na126.433 (5)Clviii—K—Kii81.853 (8)
Cliii—Fe—Na126.433 (5)Clix—K—Kii122.024 (5)
Clv—Fe—Na53.567 (5)Cl—K—Kii45.792 (5)
Cliv—Fe—Na53.567 (5)Clx—K—Kii138.589 (5)
Cli—Fe—Nai53.567 (5)Cliv—K—Kii95.165 (2)
Cl—Fe—Nai126.433 (5)Fexi—K—Kii160.851 (3)
Clii—Fe—Nai53.567 (5)Fe—K—Kii55.894 (1)
Cliii—Fe—Nai53.567 (5)Naxii—K—Kii115.634 (9)
Clv—Fe—Nai126.433 (5)Clv—Na—Clxiii148.928 (5)
Cliv—Fe—Nai126.433 (5)Clv—Na—Clxiv89.514 (10)
Na—Fe—Nai180.0Clxiii—Na—Clxiv76.796 (8)
Cli—Fe—Ki55.107 (3)Clv—Na—Clxv127.504 (7)
Cl—Fe—Ki124.893 (3)Clxiii—Na—Clxv76.796 (8)
Clii—Fe—Ki56.968 (3)Clxiv—Na—Clxv76.796 (8)
Cliii—Fe—Ki126.515 (8)Clv—Na—Cl76.796 (8)
Clv—Fe—Ki53.485 (8)Clxiii—Na—Cl127.504 (7)
Cliv—Fe—Ki123.032 (3)Clxiv—Na—Cl148.928 (5)
Na—Fe—Ki107.041 (3)Clxv—Na—Cl89.514 (10)
Nai—Fe—Ki72.959 (3)Clv—Na—Cliv76.796 (8)
Cli—Fe—K124.893 (3)Clxiii—Na—Cliv89.514 (10)
Cl—Fe—K55.107 (3)Clxiv—Na—Cliv127.504 (6)
Clii—Fe—K123.032 (3)Clxv—Na—Cliv148.928 (5)
Cliii—Fe—K53.485 (8)Cl—Na—Cliv76.796 (8)
Clv—Fe—K126.515 (8)Clv—Na—Fexiii134.176 (5)
Cliv—Fe—K56.968 (3)Clxiii—Na—Fexiii45.824 (5)
Na—Fe—K72.959 (3)Clxiv—Na—Fexiii45.824 (5)
Nai—Fe—K107.041 (3)Clxv—Na—Fexiii45.824 (5)
Ki—Fe—K180.000 (4)Cl—Na—Fexiii134.176 (5)
Cli—Fe—Kv123.032 (3)Cliv—Na—Fexiii134.176 (5)
Cl—Fe—Kv56.968 (3)Clv—Na—Fe45.824 (5)
Clii—Fe—Kv53.485 (8)Clxiii—Na—Fe134.176 (5)
Cliii—Fe—Kv124.893 (3)Clxiv—Na—Fe134.176 (5)
Clv—Fe—Kv55.107 (3)Clxv—Na—Fe134.176 (5)
Cliv—Fe—Kv126.515 (8)Cl—Na—Fe45.824 (5)
Na—Fe—Kv72.959 (3)Cliv—Na—Fe45.824 (5)
Nai—Fe—Kv107.041 (3)Fexiii—Na—Fe180.0
Ki—Fe—Kv68.212 (2)Clv—Na—Kxvi86.099 (8)
K—Fe—Kv111.788 (3)Clxiii—Na—Kxvi104.307 (9)
Cli—Fe—Kiv53.485 (8)Clxiv—Na—Kxvi48.763 (4)
Cl—Fe—Kiv126.515 (8)Clxv—Na—Kxvi47.111 (4)
Clii—Fe—Kiv124.893 (3)Cl—Na—Kxvi101.876 (6)
Cliii—Fe—Kiv123.032 (3)Cliv—Na—Kxvi162.722 (2)
Clv—Fe—Kiv56.968 (3)Fexiii—Na—Kxvi58.490 (4)
Cliv—Fe—Kiv55.107 (3)Fe—Na—Kxvi121.510 (4)
Na—Fe—Kiv72.959 (3)Clv—Na—Kiv48.764 (4)
Nai—Fe—Kiv107.041 (3)Clxiii—Na—Kiv101.875 (6)
Ki—Fe—Kiv68.212 (2)Clxiv—Na—Kiv86.099 (8)
K—Fe—Kiv111.788 (2)Clxv—Na—Kiv162.722 (2)
Kv—Fe—Kiv111.788 (2)Cl—Na—Kiv104.307 (9)
Clvi—K—Cliii153.734 (7)Cliv—Na—Kiv47.111 (4)
Clvi—K—Clvii130.279 (5)Fexiii—Na—Kiv121.510 (4)
Cliii—K—Clvii73.150 (8)Fe—Na—Kiv58.490 (4)
Clvi—K—Clviii73.148 (8)Kxvi—Na—Kiv118.401 (4)
Cliii—K—Clviii130.281 (5)Clv—Na—Kv47.111 (4)
Clvii—K—Clviii76.588 (10)Clxiii—Na—Kv162.722 (2)
Clvi—K—Clix68.551 (6)Clxiv—Na—Kv101.875 (6)
Cliii—K—Clix116.090 (6)Clxv—Na—Kv86.099 (8)
Clvii—K—Clix73.775 (4)Cl—Na—Kv48.764 (4)
Clviii—K—Clix91.342 (4)Cliv—Na—Kv104.307 (9)
Clvi—K—Cl116.090 (6)Fexiii—Na—Kv121.510 (4)
Cliii—K—Cl68.550 (6)Fe—Na—Kv58.490 (4)
Clvii—K—Cl91.344 (4)Kxvi—Na—Kv64.366 (8)
Clviii—K—Cl73.777 (4)Kiv—Na—Kv95.179 (6)
Clix—K—Cl161.231 (6)Clv—Na—K104.307 (9)
Clvi—K—Clx67.538 (6)Clxiii—Na—K86.099 (8)
Cliii—K—Clx90.534 (4)Clxiv—Na—K162.722 (2)
Clvii—K—Clx122.074 (4)Clxv—Na—K101.875 (6)
Clviii—K—Clx139.160 (4)Cl—Na—K47.111 (4)
Clix—K—Clx64.594 (4)Cliv—Na—K48.764 (4)
Cl—K—Clx134.151 (4)Fexiii—Na—K121.510 (4)
Clvi—K—Cliv90.535 (4)Fe—Na—K58.490 (4)
Cliii—K—Cliv67.537 (6)Kxvi—Na—K140.938 (4)
Clvii—K—Cliv139.161 (4)Kiv—Na—K95.179 (6)
Clviii—K—Cliv122.074 (4)Kv—Na—K95.179 (6)
Clix—K—Cliv134.151 (4)Fe—Cl—Na80.609 (10)
Cl—K—Cliv64.593 (4)Fe—Cl—Kii86.860 (10)
Clx—K—Cliv69.776 (5)Na—Cl—Kii167.394 (4)
Clvi—K—Fexi39.655 (3)Fe—Cl—Kviii168.357 (5)
Cliii—K—Fexi126.836 (3)Na—Cl—Kviii96.949 (10)
Clvii—K—Fexi113.330 (3)Kii—Cl—Kviii95.060 (9)
Clviii—K—Fexi101.096 (5)Fe—Cl—K85.326 (4)
Clix—K—Fexi39.568 (3)Na—Cl—K93.225 (4)
Cl—K—Fexi153.271 (4)Kii—Cl—K87.080 (3)
Clx—K—Fexi39.431 (3)Kviii—Cl—K106.223 (4)
Cliv—K—Fexi99.052 (4)Fe—Cl—Kv83.602 (3)
Clvi—K—Fe126.836 (3)Na—Cl—Kv91.513 (3)
Cliii—K—Fe39.655 (3)Kii—Cl—Kv85.695 (3)
Clvii—K—Fe101.097 (5)Kviii—Cl—Kv85.091 (3)
Clviii—K—Fe113.332 (3)K—Cl—Kv167.083 (4)
Clix—K—Fe153.270 (4)
Symmetry codes: (i) x, y, z; (ii) y, x+y, z; (iii) xy, x, z; (iv) y, xy, z; (v) x+y, x, z; (vi) y+1/3, x+2/3, z+1/6; (vii) x+y+2/3, y+1/3, z1/6; (viii) x+2/3, y+1/3, z+1/3; (ix) xy+1/3, y+2/3, z+1/6; (x) x+1/3, x+y+2/3, z+1/6; (xi) y+1/3, x+2/3, z+1/6; (xii) x+1/3, y+2/3, z1/3; (xiii) y, x, z+1/2; (xiv) x, x+y, z+1/2; (xv) xy, y, z+1/2; (xvi) x1/3, y2/3, z+1/3.
(10K) tripotassium sodium hexachloroferrate(II) top
Crystal data top
K3Na[FeCl6]Dx = 2.421 Mg m3
Mr = 408.84Melting point: not measured K
Trigonal, R3cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -R 3 2"cCell parameters from 24 reflections
a = 11.893 (1) Åθ = 24.4–29.9°
c = 13.735 (2) ŵ = 3.86 mm1
V = 1682.4 (3) Å3T = 10 K
Z = 6Cube, very pale yellow
F(000) = 11760.40 × 0.40 × 0.40 mm
Data collection top
Huber 512 goniometer
diffractometer
1981 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tubeRint = 0.035
None monochromatorθmax = 50.2°, θmin = 3.4°
ω–2θ scansh = 2525
Absorption correction: for a sphere
(Xtal 3.4; Hall et al., 1994)
k = 2525
Tmin = 0.257, Tmax = 0.306l = 2929
28510 measured reflections3 standard reflections every 100 reflections
1983 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020 w = 1/[σ2(Fo2) + (0.0109P)2 + 3.4848P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.050(Δ/σ)max = 0.001
S = 1.46Δρmax = 0.52 e Å3
1983 reflectionsΔρmin = 0.93 e Å3
20 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0071 (2)
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
xyzUiso*/Ueq
Fe0.00000.00000.00000.00351 (3)
K0.289535 (16)0.33330.08330.00540 (3)
Na0.00000.00000.25000.00655 (10)
Cl0.180955 (14)0.027399 (15)0.107988 (11)0.00503 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.00347 (4)0.00347 (4)0.00360 (6)0.00174 (2)0.0000.000
K0.00528 (4)0.00514 (6)0.00572 (6)0.00257 (3)0.00023 (2)0.00047 (4)
Na0.00724 (16)0.00724 (16)0.0052 (2)0.00362 (8)0.0000.000
Cl0.00461 (5)0.00553 (5)0.00517 (5)0.00271 (4)0.00032 (3)0.00004 (3)
Geometric parameters (Å, º) top
Fe—Cli2.4973 (2)K—Clx3.2915 (4)
Fe—Cl2.4973 (2)K—Cliv3.2916 (3)
Fe—Clii2.4973 (2)K—Fexi3.9028 (3)
Fe—Cliii2.4973 (2)K—Naxii4.3775 (3)
Fe—Cliv2.4973 (2)K—Kiii4.3775 (3)
Fe—Clv2.4973 (2)Na—Clv2.8002 (3)
Fe—Na3.4337 (5)Na—Clxiii2.8002 (3)
Fe—Nai3.4337 (5)Na—Clxiv2.8002 (3)
Fe—K3.9029 (3)Na—Clxv2.8002 (3)
Fe—Ki3.9029 (3)Na—Cl2.8002 (3)
Fe—Kii3.9029 (3)Na—Cliv2.8002 (3)
Fe—Kiv3.9029 (3)Na—Fexiii3.4337 (5)
K—Clvi3.1423 (4)Na—Kxvi4.3775 (3)
K—Cliii3.1423 (4)Na—Kiv4.3775 (3)
K—Clvii3.1803 (3)Na—Kv4.3775 (3)
K—Clviii3.1803 (3)Cl—Kii3.1423 (4)
K—Clix3.2128 (3)Cl—Kviii3.1803 (3)
K—Cl3.2128 (3)Cl—Kv3.2916 (3)
Cli—Fe—Cl180.000 (9)Cl—K—Fe39.618 (3)
Cli—Fe—Clii88.330 (8)Clx—K—Fe99.063 (5)
Cl—Fe—Clii91.670 (8)Cliv—K—Fe39.482 (3)
Cli—Fe—Cliii88.330 (8)Fexi—K—Fe136.025 (5)
Cl—Fe—Cliii91.670 (8)Clvi—K—Naxii88.285 (9)
Clii—Fe—Cliii88.331 (8)Cliii—K—Naxii83.042 (8)
Cli—Fe—Cliv91.670 (8)Clvii—K—Naxii82.626 (6)
Cl—Fe—Cliv88.330 (8)Clviii—K—Naxii130.715 (5)
Clii—Fe—Cliv180.000 (9)Clix—K—Naxii39.694 (3)
Cliii—Fe—Cliv91.670 (8)Cl—K—Naxii151.541 (4)
Cli—Fe—Clv91.670 (8)Clx—K—Naxii39.751 (3)
Cl—Fe—Clv88.330 (8)Cliv—K—Naxii102.777 (5)
Clii—Fe—Clv91.670 (8)Fexi—K—Naxii48.584 (7)
Cliii—Fe—Clv180.000 (5)Fe—K—Naxii114.303 (6)
Cliv—Fe—Clv88.330 (8)Clvi—K—Kiii107.297 (8)
Cli—Fe—Na126.437 (6)Cliii—K—Kiii47.137 (4)
Cl—Fe—Na53.563 (6)Clvii—K—Kiii110.640 (9)
Clii—Fe—Na126.437 (6)Clviii—K—Kiii167.330 (3)
Cliii—Fe—Na126.437 (6)Clix—K—Kiii100.660 (6)
Cliv—Fe—Na53.563 (6)Cl—K—Kiii95.340 (3)
Clv—Fe—Na53.563 (6)Clx—K—Kiii46.374 (4)
Cli—Fe—Nai53.563 (6)Cliv—K—Kiii45.711 (5)
Cl—Fe—Nai126.437 (6)Fexi—K—Kiii85.826 (6)
Clii—Fe—Nai53.563 (6)Fe—K—Kiii55.888 (1)
Cliii—Fe—Nai53.563 (6)Naxii—K—Kiii61.635 (5)
Cliv—Fe—Nai126.437 (6)Clv—Na—Clxiii148.920 (7)
Clv—Fe—Nai126.437 (6)Clv—Na—Clxiv127.478 (8)
Na—Fe—Nai180.0Clxiii—Na—Clxiv76.831 (9)
Cli—Fe—K124.877 (4)Clv—Na—Clxv89.470 (11)
Cl—Fe—K55.123 (4)Clxiii—Na—Clxv76.831 (9)
Clii—Fe—K123.061 (4)Clxiv—Na—Clxv76.831 (9)
Cliii—Fe—K53.501 (8)Clv—Na—Cl76.831 (9)
Cliv—Fe—K56.939 (4)Clxiii—Na—Cl127.478 (8)
Clv—Fe—K126.499 (8)Clxiv—Na—Cl89.470 (11)
Na—Fe—K72.946 (3)Clxv—Na—Cl148.920 (7)
Nai—Fe—K107.054 (3)Clv—Na—Cliv76.831 (9)
Cli—Fe—Ki55.123 (4)Clxiii—Na—Cliv89.470 (11)
Cl—Fe—Ki124.877 (4)Clxiv—Na—Cliv148.920 (7)
Clii—Fe—Ki56.939 (4)Clxv—Na—Cliv127.478 (8)
Cliii—Fe—Ki126.499 (8)Cl—Na—Cliv76.831 (9)
Cliv—Fe—Ki123.061 (4)Clv—Na—Fexiii134.153 (6)
Clv—Fe—Ki53.501 (8)Clxiii—Na—Fexiii45.847 (6)
Na—Fe—Ki107.054 (3)Clxiv—Na—Fexiii45.847 (6)
Nai—Fe—Ki72.946 (3)Clxv—Na—Fexiii45.847 (6)
K—Fe—Ki180.0Cl—Na—Fexiii134.153 (6)
Cli—Fe—Kii126.499 (8)Cliv—Na—Fexiii134.153 (6)
Cl—Fe—Kii53.501 (8)Clv—Na—Fe45.847 (6)
Clii—Fe—Kii55.123 (4)Clxiii—Na—Fe134.153 (6)
Cliii—Fe—Kii56.939 (4)Clxiv—Na—Fe134.153 (6)
Cliv—Fe—Kii124.877 (4)Clxv—Na—Fe134.153 (6)
Clv—Fe—Kii123.061 (4)Cl—Na—Fe45.847 (6)
Na—Fe—Kii107.054 (3)Cliv—Na—Fe45.847 (6)
Nai—Fe—Kii72.946 (3)Fexiii—Na—Fe180.0
K—Fe—Kii68.223 (2)Clv—Na—Kxvi86.083 (8)
Ki—Fe—Kii111.777 (2)Clxiii—Na—Kxvi104.310 (10)
Cli—Fe—Kiv53.501 (8)Clxiv—Na—Kxvi47.122 (4)
Cl—Fe—Kiv126.499 (8)Clxv—Na—Kxvi48.735 (5)
Clii—Fe—Kiv124.877 (4)Cl—Na—Kxvi101.899 (7)
Cliii—Fe—Kiv123.061 (4)Cliv—Na—Kxvi162.735 (3)
Cliv—Fe—Kiv55.123 (4)Fexiii—Na—Kxvi58.470 (4)
Clv—Fe—Kiv56.939 (4)Fe—Na—Kxvi121.530 (4)
Na—Fe—Kiv72.946 (3)Clv—Na—Kiv48.735 (5)
Nai—Fe—Kiv107.054 (3)Clxiii—Na—Kiv101.898 (7)
K—Fe—Kiv111.777 (2)Clxiv—Na—Kiv162.734 (3)
Ki—Fe—Kiv68.223 (2)Clxv—Na—Kiv86.083 (8)
Kii—Fe—Kiv180.0Cl—Na—Kiv104.311 (10)
Clvi—K—Cliii153.843 (9)Cliv—Na—Kiv47.122 (4)
Clvi—K—Clvii130.253 (6)Fexiii—Na—Kiv121.530 (4)
Cliii—K—Clvii73.084 (9)Fe—Na—Kiv58.470 (4)
Clvi—K—Clviii73.082 (9)Kxvi—Na—Kiv118.365 (5)
Cliii—K—Clviii130.255 (6)Clv—Na—Kv47.122 (4)
Clvii—K—Clviii76.589 (11)Clxiii—Na—Kv162.734 (3)
Clvi—K—Clix68.623 (7)Clxiv—Na—Kv86.083 (8)
Cliii—K—Clix116.032 (7)Clxv—Na—Kv101.898 (7)
Clvii—K—Clix73.701 (5)Cl—Na—Kv48.735 (5)
Clviii—K—Clix91.301 (5)Cliv—Na—Kv104.311 (10)
Clvi—K—Cl116.033 (7)Fexiii—Na—Kv121.530 (4)
Cliii—K—Cl68.622 (7)Fe—Na—Kv58.470 (4)
Clvii—K—Cl91.302 (5)Kxvi—Na—Kv64.417 (9)
Clviii—K—Cl73.703 (5)Kiv—Na—Kv95.152 (6)
Clix—K—Cl161.085 (8)Clv—Na—K104.311 (10)
Clvi—K—Clx67.633 (7)Clxiii—Na—K86.083 (8)
Cliii—K—Clx90.532 (6)Clxiv—Na—K101.898 (7)
Clvii—K—Clx122.061 (4)Clxv—Na—K162.734 (3)
Clviii—K—Clx139.187 (5)Cl—Na—K47.122 (4)
Clix—K—Clx64.675 (5)Cliv—Na—K48.735 (5)
Cl—K—Clx134.215 (5)Fexiii—Na—K121.530 (4)
Clvi—K—Cliv90.533 (6)Fe—Na—K58.470 (4)
Cliii—K—Cliv67.631 (7)Kxvi—Na—K141.000 (5)
Clvii—K—Cliv139.188 (5)Kiv—Na—K95.152 (6)
Clviii—K—Cliv122.061 (4)Kv—Na—K95.152 (6)
Clix—K—Cliv134.216 (5)Fe—Cl—Na80.589 (10)
Cl—K—Cliv64.674 (5)Fe—Cl—Kii86.793 (10)
Clx—K—Cliv69.761 (6)Na—Cl—Kii167.311 (6)
Clvi—K—Fexi39.707 (3)Fe—Cl—Kviii168.349 (6)
Cliii—K—Fexi126.861 (5)Na—Cl—Kviii96.970 (10)
Clvii—K—Fexi113.306 (4)Kii—Cl—Kviii95.129 (10)
Clviii—K—Fexi101.071 (5)Fe—Cl—K85.259 (5)
Clix—K—Fexi39.619 (3)Na—Cl—K93.184 (5)
Cl—K—Fexi153.298 (5)Kii—Cl—K87.065 (4)
Clx—K—Fexi39.483 (3)Kviii—Cl—K106.297 (5)
Cliv—K—Fexi99.064 (5)Fe—Cl—Kv83.579 (4)
Clvi—K—Fe126.862 (5)Na—Cl—Kv91.514 (5)
Cliii—K—Fe39.706 (3)Kii—Cl—Kv85.714 (4)
Clvii—K—Fe101.072 (5)Kviii—Cl—Kv85.106 (4)
Clviii—K—Fe113.308 (4)K—Cl—Kv167.017 (6)
Clix—K—Fe153.297 (5)
Symmetry codes: (i) x, y, z; (ii) y, x+y, z; (iii) xy, x, z; (iv) y, xy, z; (v) x+y, x, z; (vi) y+1/3, x+2/3, z+1/6; (vii) x+y+2/3, y+1/3, z1/6; (viii) x+2/3, y+1/3, z+1/3; (ix) xy+1/3, y+2/3, z+1/6; (x) x+1/3, x+y+2/3, z+1/6; (xi) y+1/3, x+2/3, z+1/6; (xii) x+1/3, y+2/3, z1/3; (xiii) y, x, z+1/2; (xiv) xy, y, z+1/2; (xv) x, x+y, z+1/2; (xvi) x1/3, y2/3, z+1/3.
Bond lengths (A) and angles (°) in K3Na[FeCl6] at 293, 84 and 9.5 K top
293 K84 K9.5 K
Fe—Cl2.5124 (5)2.5009 (2)2.4973 (2)
Cl—Fe—Cl'180180180
Cl—Fe—Cl"88.39 (2)88.336 (8)88.330 (8)
Symmetry codes: (i) -x, -y, -z; (ii) -y, x-y, -z.
 

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