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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
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 m−3 |
Mr = 408.84 | Melting point: not measured K |
Trigonal, R3c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -R 3 2"c | Cell parameters from 12 reflections |
a = 12.033 (2) Å | θ = 15.5–15.5° |
c = 13.863 (4) Å | µ = 3.74 mm−1 |
V = 1738.3 (6) Å3 | T = 293 K |
Z = 6 | Cube, very pale yellow |
F(000) = 1176 | 0.40 × 0.40 × 0.40 mm |
Data collection top
Huber 512 goniometer diffractometer | 347 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.044 |
None monochromator | θmax = 25.1°, θmin = 3.4° |
ω–2θ scans | h = −14→14 |
Absorption correction: for a sphere (Xtal3.4; Hall et al., 1994) | k = −14→14 |
Tmin = 0.268, Tmax = 0.282 | l = −16→16 |
3808 measured reflections | 3 standard reflections every 100 reflections |
347 independent reflections | intensity decay: 1% |
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)] = 0.017 | w = 1/[σ2(Fo2) + (0.0099P)2 + 0.5551P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.031 | (Δ/σ)max < 0.001 |
S = 1.62 | Δρmax = 0.38 e Å−3 |
347 reflections | Δρmin = −0.37 e Å−3 |
20 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction 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 | x | y | z | Uiso*/Ueq | |
Fe | 0.0000 | 0.0000 | 0.0000 | 0.01592 (16) | |
K | 0.29056 (3) | 0.3333 | 0.0833 | 0.02606 (17) | |
Na | 0.0000 | 0.0000 | 0.2500 | 0.0282 (3) | |
Cl | 0.17995 (3) | 0.02704 (3) | 0.10753 (2) | 0.02232 (16) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe | 0.01657 (19) | 0.01657 (19) | 0.0146 (2) | 0.00828 (9) | 0.000 | 0.000 |
K | 0.0256 (2) | 0.0244 (2) | 0.0277 (3) | 0.01222 (12) | −0.00264 (8) | −0.00529 (16) |
Na | 0.0334 (4) | 0.0334 (4) | 0.0176 (6) | 0.0167 (2) | 0.000 | 0.000 |
Cl | 0.0203 (2) | 0.0277 (2) | 0.0208 (2) | 0.01338 (14) | −0.00256 (11) | −0.00041 (12) |
Geometric parameters (Å, º) top
Fe—Cli | 2.5124 (5) | K—Clx | 3.3368 (7) |
Fe—Cl | 2.5124 (5) | K—Clii | 3.3368 (7) |
Fe—Clii | 2.5124 (5) | K—Fexi | 3.9526 (6) |
Fe—Cliii | 2.5124 (5) | K—Naxii | 4.4302 (7) |
Fe—Cliv | 2.5124 (5) | K—Kiv | 4.4302 (6) |
Fe—Clv | 2.5124 (5) | Na—Cliii | 2.8268 (5) |
Fe—Na | 3.466 (1) | Na—Clxiii | 2.8268 (6) |
Fe—Nai | 3.466 (1) | Na—Clxiv | 2.8268 (6) |
Fe—Ki | 3.9526 (6) | Na—Clxv | 2.8268 (6) |
Fe—K | 3.9526 (6) | Na—Clii | 2.8268 (6) |
Fe—Kiii | 3.9526 (6) | Na—Cl | 2.8268 (6) |
Fe—Kii | 3.9526 (6) | Na—Fexiii | 3.466 (1) |
K—Clvi | 3.1770 (7) | Na—Kxvi | 4.4302 (7) |
K—Cliv | 3.1771 (7) | Na—Kii | 4.4302 (7) |
K—Clvii | 3.2165 (6) | Na—Kiii | 4.4302 (7) |
K—Clviii | 3.2165 (6) | Cl—Kv | 3.1771 (7) |
K—Clix | 3.2499 (6) | Cl—Kviii | 3.2165 (6) |
K—Cl | 3.2499 (6) | Cl—Kiii | 3.3368 (7) |
| | | |
Cli—Fe—Cl | 180.000 (17) | Cl—K—Fe | 39.329 (7) |
Cli—Fe—Clii | 91.61 (2) | Clx—K—Fe | 99.005 (10) |
Cl—Fe—Clii | 88.39 (2) | Clii—K—Fe | 39.188 (7) |
Cli—Fe—Cliii | 91.61 (2) | Fexi—K—Fe | 135.684 (11) |
Cl—Fe—Cliii | 88.39 (2) | Clvi—K—Naxii | 87.834 (18) |
Clii—Fe—Cliii | 88.39 (2) | Cliv—K—Naxii | 83.247 (16) |
Cli—Fe—Cliv | 88.39 (2) | Clvii—K—Naxii | 82.819 (12) |
Cl—Fe—Cliv | 91.61 (2) | Clviii—K—Naxii | 130.759 (9) |
Clii—Fe—Cliv | 91.61 (2) | Clix—K—Naxii | 39.567 (6) |
Cliii—Fe—Cliv | 180.000 (11) | Cl—K—Naxii | 151.268 (9) |
Cli—Fe—Clv | 88.39 (2) | Clx—K—Naxii | 39.632 (6) |
Cl—Fe—Clv | 91.61 (2) | Clii—K—Naxii | 102.610 (10) |
Clii—Fe—Clv | 180.000 (16) | Fexi—K—Naxii | 48.430 (14) |
Cliii—Fe—Clv | 91.61 (2) | Fe—K—Naxii | 114.187 (11) |
Cliv—Fe—Clv | 88.39 (2) | Clvi—K—Kiv | 106.820 (16) |
Cli—Fe—Na | 126.394 (11) | Cliv—K—Kiv | 47.111 (8) |
Cl—Fe—Na | 53.606 (11) | Clvii—K—Kiv | 110.683 (19) |
Clii—Fe—Na | 53.606 (11) | Clviii—K—Kiv | 167.429 (6) |
Cliii—Fe—Na | 53.606 (11) | Clix—K—Kiv | 100.279 (12) |
Cliv—Fe—Na | 126.394 (11) | Cl—K—Kiv | 95.075 (6) |
Clv—Fe—Na | 126.394 (11) | Clx—K—Kiv | 46.330 (9) |
Cli—Fe—Nai | 53.606 (11) | Clii—K—Kiv | 45.651 (10) |
Cl—Fe—Nai | 126.394 (11) | Fexi—K—Kiv | 85.486 (11) |
Clii—Fe—Nai | 126.394 (11) | Fe—K—Kiv | 55.915 (2) |
Cliii—Fe—Nai | 126.394 (11) | Naxii—K—Kiv | 61.431 (10) |
Cliv—Fe—Nai | 53.606 (11) | Cliii—Na—Clxiii | 148.923 (13) |
Clv—Fe—Nai | 53.606 (11) | Cliii—Na—Clxiv | 127.720 (15) |
Na—Fe—Nai | 180.0 | Clxiii—Na—Clxiv | 76.571 (17) |
Cli—Fe—Ki | 55.066 (8) | Cliii—Na—Clxv | 89.78 (2) |
Cl—Fe—Ki | 124.934 (8) | Clxiii—Na—Clxv | 76.572 (17) |
Clii—Fe—Ki | 122.945 (8) | Clxiv—Na—Clxv | 76.571 (17) |
Cliii—Fe—Ki | 53.401 (16) | Cliii—Na—Clii | 76.571 (17) |
Cliv—Fe—Ki | 126.599 (16) | Clxiii—Na—Clii | 89.78 (2) |
Clv—Fe—Ki | 57.055 (8) | Clxiv—Na—Clii | 148.923 (13) |
Na—Fe—Ki | 106.994 (5) | Clxv—Na—Clii | 127.720 (16) |
Nai—Fe—Ki | 73.006 (5) | Cliii—Na—Cl | 76.572 (17) |
Cli—Fe—K | 124.934 (8) | Clxiii—Na—Cl | 127.720 (16) |
Cl—Fe—K | 55.066 (8) | Clxiv—Na—Cl | 89.78 (2) |
Clii—Fe—K | 57.055 (8) | Clxv—Na—Cl | 148.923 (13) |
Cliii—Fe—K | 126.599 (16) | Clii—Na—Cl | 76.571 (17) |
Cliv—Fe—K | 53.401 (16) | Cliii—Na—Fexiii | 134.321 (11) |
Clv—Fe—K | 122.945 (8) | Clxiii—Na—Fexiii | 45.679 (11) |
Na—Fe—K | 73.006 (5) | Clxiv—Na—Fexiii | 45.679 (11) |
Nai—Fe—K | 106.994 (5) | Clxv—Na—Fexiii | 45.679 (11) |
Ki—Fe—K | 180.000 (11) | Clii—Na—Fexiii | 134.321 (11) |
Cli—Fe—Kiii | 122.945 (8) | Cl—Na—Fexiii | 134.321 (11) |
Cl—Fe—Kiii | 57.055 (8) | Cliii—Na—Fe | 45.679 (11) |
Clii—Fe—Kiii | 126.599 (16) | Clxiii—Na—Fe | 134.321 (11) |
Cliii—Fe—Kiii | 55.066 (8) | Clxiv—Na—Fe | 134.321 (11) |
Cliv—Fe—Kiii | 124.934 (8) | Clxv—Na—Fe | 134.321 (11) |
Clv—Fe—Kiii | 53.401 (16) | Clii—Na—Fe | 45.679 (11) |
Na—Fe—Kiii | 73.006 (5) | Cl—Na—Fe | 45.679 (11) |
Nai—Fe—Kiii | 106.994 (5) | Fexiii—Na—Fe | 180.0 |
Ki—Fe—Kiii | 68.169 (5) | Cliii—Na—Kxvi | 86.238 (16) |
K—Fe—Kiii | 111.831 (5) | Clxiii—Na—Kxvi | 104.235 (19) |
Cli—Fe—Kii | 53.401 (16) | Clxiv—Na—Kxvi | 47.082 (9) |
Cl—Fe—Kii | 126.599 (16) | Clxv—Na—Kxvi | 48.844 (9) |
Clii—Fe—Kii | 55.066 (8) | Clii—Na—Kxvi | 162.671 (6) |
Cliii—Fe—Kii | 57.055 (8) | Cl—Na—Kxvi | 101.781 (14) |
Cliv—Fe—Kii | 122.945 (8) | Fexiii—Na—Kxvi | 58.564 (9) |
Clv—Fe—Kii | 124.934 (8) | Fe—Na—Kxvi | 121.436 (9) |
Na—Fe—Kii | 73.006 (5) | Cliii—Na—Kii | 48.844 (9) |
Nai—Fe—Kii | 106.994 (5) | Clxiii—Na—Kii | 101.780 (14) |
Ki—Fe—Kii | 68.169 (5) | Clxiv—Na—Kii | 162.671 (6) |
K—Fe—Kii | 111.831 (5) | Clxv—Na—Kii | 86.238 (16) |
Kiii—Fe—Kii | 111.831 (5) | Clii—Na—Kii | 47.082 (9) |
Clvi—K—Cliv | 153.303 (18) | Cl—Na—Kii | 104.235 (19) |
Clvi—K—Clvii | 130.420 (12) | Fexiii—Na—Kii | 121.435 (9) |
Cliv—K—Clvii | 73.370 (17) | Fe—Na—Kii | 58.565 (9) |
Clvi—K—Clviii | 73.368 (17) | Kxvi—Na—Kii | 118.569 (10) |
Cliv—K—Clviii | 130.422 (12) | Cliii—Na—Kiii | 47.082 (9) |
Clvii—K—Clviii | 76.67 (2) | Clxiii—Na—Kiii | 162.671 (6) |
Clvi—K—Clix | 68.177 (13) | Clxiv—Na—Kiii | 86.238 (16) |
Cliv—K—Clix | 116.390 (14) | Clxv—Na—Kiii | 101.780 (13) |
Clvii—K—Clix | 74.157 (10) | Clii—Na—Kiii | 104.235 (19) |
Clviii—K—Clix | 91.483 (9) | Cl—Na—Kiii | 48.844 (9) |
Clvi—K—Cl | 116.390 (14) | Fexiii—Na—Kiii | 121.435 (9) |
Cliv—K—Cl | 68.176 (13) | Fe—Na—Kiii | 58.565 (9) |
Clvii—K—Cl | 91.484 (9) | Kxvi—Na—Kiii | 64.167 (17) |
Clviii—K—Cl | 74.159 (10) | Kii—Na—Kiii | 95.279 (11) |
Clix—K—Cl | 161.875 (17) | Cliii—Na—K | 104.235 (19) |
Clvi—K—Clx | 67.105 (14) | Clxiii—Na—K | 86.238 (16) |
Cliv—K—Clx | 90.597 (11) | Clxiv—Na—K | 101.780 (14) |
Clvii—K—Clx | 122.147 (8) | Clxv—Na—K | 162.671 (6) |
Clviii—K—Clx | 138.965 (10) | Clii—Na—K | 48.844 (9) |
Clix—K—Clx | 64.240 (11) | Cl—Na—K | 47.082 (9) |
Cl—K—Clx | 133.862 (11) | Fexiii—Na—K | 121.435 (9) |
Clvi—K—Clii | 90.598 (11) | Fe—Na—K | 58.565 (9) |
Cliv—K—Clii | 67.104 (14) | Kxvi—Na—K | 140.673 (10) |
Clvii—K—Clii | 138.966 (10) | Kii—Na—K | 95.279 (12) |
Clviii—K—Clii | 122.148 (8) | Kiii—Na—K | 95.279 (11) |
Clix—K—Clii | 133.863 (11) | Fe—Cl—Na | 80.72 (2) |
Cl—K—Clii | 64.239 (11) | Fe—Cl—Kv | 87.19 (2) |
Clx—K—Clii | 69.831 (13) | Na—Cl—Kv | 167.815 (11) |
Clvi—K—Fexi | 39.411 (7) | Fe—Cl—Kviii | 168.449 (13) |
Cliv—K—Fexi | 126.760 (9) | Na—Cl—Kviii | 96.77 (2) |
Clvii—K—Fexi | 113.472 (8) | Kv—Cl—Kviii | 94.796 (19) |
Clviii—K—Fexi | 101.149 (10) | Fe—Cl—K | 85.605 (10) |
Clix—K—Fexi | 39.329 (7) | Na—Cl—K | 93.351 (9) |
Cl—K—Fexi | 153.168 (10) | Kv—Cl—K | 87.143 (8) |
Clx—K—Fexi | 39.189 (7) | Kviii—Cl—K | 105.841 (10) |
Clii—K—Fexi | 99.006 (10) | Fe—Cl—Kiii | 83.756 (9) |
Clvi—K—Fe | 126.760 (9) | Na—Cl—Kiii | 91.524 (9) |
Cliv—K—Fe | 39.411 (7) | Kv—Cl—Kiii | 85.669 (8) |
Clvii—K—Fe | 101.151 (10) | Kviii—Cl—Kiii | 85.047 (8) |
Clviii—K—Fe | 113.473 (8) | K—Cl—Kiii | 167.430 (11) |
Clix—K—Fe | 153.168 (10) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −y, x−y, z; (iii) −x+y, −x, z; (iv) x−y, 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, z−1/6; (viii) −x+2/3, −y+1/3, −z+1/3; (ix) x−y+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, z−1/3; (xiii) y, x, −z+1/2; (xiv) x−y, −y, −z+1/2; (xv) −x, −x+y, −z+1/2; (xvi) x−1/3, y−2/3, z+1/3. |
(84K) tripotassium sodium hexachloroferrate(II)
top
Crystal data top
K3Na[FeCl6] | Dx = 2.405 Mg m−3 |
Mr = 408.84 | Melting point: not measured K |
Trigonal, R3c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -R 3 2"c | Cell parameters from 14 reflections |
a = 11.922 (1) Å | θ = 17.0–20.5° |
c = 13.761 (2) Å | µ = 3.83 mm−1 |
V = 1693.9 (3) Å3 | T = 84 K |
Z = 6 | Prism, very pale yellow |
F(000) = 1176 | 0.49 × 0.35 × 0.33 mm |
Data collection top
Syntex P21 diffractometer | 1930 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 50.1°, θmin = 3.4° |
ω–2θ scans | h = −25→25 |
Absorption correction: gaussian (Xtal 3.4; Hall et al., 1994) | k = −25→25 |
Tmin = 0.279, Tmax = 0.377 | l = −29→29 |
37086 measured reflections | 6 standard reflections every 100 reflections |
1991 independent reflections | intensity decay: 2% |
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)] = 0.018 | w = 1/[σ2(Fo2) + (0.0106P)2 + 0.791P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.036 | (Δ/σ)max = 0.001 |
S = 1.40 | Δρmax = 0.44 e Å−3 |
1991 reflections | Δρmin = −0.37 e Å−3 |
20 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction 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 | x | y | z | Uiso*/Ueq | |
Fe | 0.0000 | 0.0000 | 0.0000 | 0.00521 (2) | |
K | 0.289724 (12) | 0.3333 | 0.0833 | 0.00863 (2) | |
Na | 0.0000 | 0.0000 | 0.2500 | 0.00987 (8) | |
Cl | 0.180781 (10) | 0.027362 (11) | 0.107931 (8) | 0.00760 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe | 0.00549 (3) | 0.00549 (3) | 0.00464 (5) | 0.00275 (2) | 0.000 | 0.000 |
K | 0.00862 (3) | 0.00826 (4) | 0.00890 (5) | 0.00413 (2) | −0.00083 (2) | −0.00165 (3) |
Na | 0.01173 (12) | 0.01173 (12) | 0.00614 (17) | 0.00587 (6) | 0.000 | 0.000 |
Cl | 0.00706 (4) | 0.00934 (4) | 0.00697 (4) | 0.00453 (3) | −0.00078 (2) | −0.00015 (3) |
Geometric parameters (Å, º) top
Fe—Cli | 2.5009 (2) | K—Clx | 3.3011 (3) |
Fe—Cl | 2.5009 (2) | K—Cliv | 3.3011 (3) |
Fe—Clii | 2.5009 (2) | K—Fexi | 3.9130 (3) |
Fe—Cliii | 2.5009 (2) | K—Naxii | 4.3883 (3) |
Fe—Cliv | 2.5009 (2) | K—Kii | 4.3883 (3) |
Fe—Clv | 2.5009 (2) | Na—Clv | 2.8055 (3) |
Fe—Na | 3.4402 (5) | Na—Clxiii | 2.8055 (3) |
Fe—Nai | 3.4402 (5) | Na—Clxiv | 2.8055 (3) |
Fe—K | 3.9130 (3) | Na—Clxv | 2.8055 (3) |
Fe—Ki | 3.9130 (3) | Na—Cl | 2.8055 (3) |
Fe—Kii | 3.9130 (3) | Na—Cliv | 2.8055 (3) |
Fe—Kiv | 3.9130 (3) | Na—Fexiii | 3.4402 (5) |
K—Clvi | 3.1496 (3) | Na—Kxvi | 4.3883 (3) |
K—Cliii | 3.1497 (4) | Na—Kiv | 4.3883 (3) |
K—Clvii | 3.1875 (3) | Na—Kv | 4.3883 (3) |
K—Clviii | 3.1876 (3) | Cl—Kii | 3.1497 (3) |
K—Clix | 3.2202 (3) | Cl—Kviii | 3.1876 (3) |
K—Cl | 3.2203 (3) | Cl—Kv | 3.3011 (3) |
| | | |
Cli—Fe—Cl | 180.000 (6) | Cl—K—Fe | 39.568 (3) |
Cli—Fe—Clii | 88.336 (8) | Clx—K—Fe | 99.051 (4) |
Cl—Fe—Clii | 91.664 (7) | Cliv—K—Fe | 39.430 (3) |
Cli—Fe—Cliii | 88.336 (8) | Fexi—K—Fe | 135.961 (4) |
Cl—Fe—Cliii | 91.664 (8) | Clvi—K—Naxii | 88.201 (9) |
Clii—Fe—Cliii | 88.336 (8) | Cliii—K—Naxii | 83.078 (8) |
Cli—Fe—Cliv | 91.664 (8) | Clvii—K—Naxii | 82.664 (6) |
Cl—Fe—Cliv | 88.336 (8) | Clviii—K—Naxii | 130.726 (4) |
Clii—Fe—Cliv | 180.000 (6) | Clix—K—Naxii | 39.665 (3) |
Cliii—Fe—Cliv | 91.664 (7) | Cl—K—Naxii | 151.500 (4) |
Cli—Fe—Clv | 91.664 (8) | Clx—K—Naxii | 39.724 (3) |
Cl—Fe—Clv | 88.336 (8) | Cliv—K—Naxii | 102.749 (4) |
Clii—Fe—Clv | 91.664 (8) | Fexi—K—Naxii | 48.551 (7) |
Cliii—Fe—Clv | 180.000 (10) | Fe—K—Naxii | 114.284 (5) |
Clv—Fe—Cliv | 88.336 (8) | Clvi—K—Kii | 153.376 (3) |
Cli—Fe—Na | 126.433 (5) | Cliii—K—Kii | 48.602 (4) |
Cl—Fe—Na | 53.567 (5) | Clvii—K—Kii | 48.548 (4) |
Clii—Fe—Na | 126.433 (5) | Clviii—K—Kii | 81.853 (8) |
Cliii—Fe—Na | 126.433 (5) | Clix—K—Kii | 122.024 (5) |
Clv—Fe—Na | 53.567 (5) | Cl—K—Kii | 45.792 (5) |
Cliv—Fe—Na | 53.567 (5) | Clx—K—Kii | 138.589 (5) |
Cli—Fe—Nai | 53.567 (5) | Cliv—K—Kii | 95.165 (2) |
Cl—Fe—Nai | 126.433 (5) | Fexi—K—Kii | 160.851 (3) |
Clii—Fe—Nai | 53.567 (5) | Fe—K—Kii | 55.894 (1) |
Cliii—Fe—Nai | 53.567 (5) | Naxii—K—Kii | 115.634 (9) |
Clv—Fe—Nai | 126.433 (5) | Clv—Na—Clxiii | 148.928 (5) |
Cliv—Fe—Nai | 126.433 (5) | Clv—Na—Clxiv | 89.514 (10) |
Na—Fe—Nai | 180.0 | Clxiii—Na—Clxiv | 76.796 (8) |
Cli—Fe—Ki | 55.107 (3) | Clv—Na—Clxv | 127.504 (7) |
Cl—Fe—Ki | 124.893 (3) | Clxiii—Na—Clxv | 76.796 (8) |
Clii—Fe—Ki | 56.968 (3) | Clxiv—Na—Clxv | 76.796 (8) |
Cliii—Fe—Ki | 126.515 (8) | Clv—Na—Cl | 76.796 (8) |
Clv—Fe—Ki | 53.485 (8) | Clxiii—Na—Cl | 127.504 (7) |
Cliv—Fe—Ki | 123.032 (3) | Clxiv—Na—Cl | 148.928 (5) |
Na—Fe—Ki | 107.041 (3) | Clxv—Na—Cl | 89.514 (10) |
Nai—Fe—Ki | 72.959 (3) | Clv—Na—Cliv | 76.796 (8) |
Cli—Fe—K | 124.893 (3) | Clxiii—Na—Cliv | 89.514 (10) |
Cl—Fe—K | 55.107 (3) | Clxiv—Na—Cliv | 127.504 (6) |
Clii—Fe—K | 123.032 (3) | Clxv—Na—Cliv | 148.928 (5) |
Cliii—Fe—K | 53.485 (8) | Cl—Na—Cliv | 76.796 (8) |
Clv—Fe—K | 126.515 (8) | Clv—Na—Fexiii | 134.176 (5) |
Cliv—Fe—K | 56.968 (3) | Clxiii—Na—Fexiii | 45.824 (5) |
Na—Fe—K | 72.959 (3) | Clxiv—Na—Fexiii | 45.824 (5) |
Nai—Fe—K | 107.041 (3) | Clxv—Na—Fexiii | 45.824 (5) |
Ki—Fe—K | 180.000 (4) | Cl—Na—Fexiii | 134.176 (5) |
Cli—Fe—Kv | 123.032 (3) | Cliv—Na—Fexiii | 134.176 (5) |
Cl—Fe—Kv | 56.968 (3) | Clv—Na—Fe | 45.824 (5) |
Clii—Fe—Kv | 53.485 (8) | Clxiii—Na—Fe | 134.176 (5) |
Cliii—Fe—Kv | 124.893 (3) | Clxiv—Na—Fe | 134.176 (5) |
Clv—Fe—Kv | 55.107 (3) | Clxv—Na—Fe | 134.176 (5) |
Cliv—Fe—Kv | 126.515 (8) | Cl—Na—Fe | 45.824 (5) |
Na—Fe—Kv | 72.959 (3) | Cliv—Na—Fe | 45.824 (5) |
Nai—Fe—Kv | 107.041 (3) | Fexiii—Na—Fe | 180.0 |
Ki—Fe—Kv | 68.212 (2) | Clv—Na—Kxvi | 86.099 (8) |
K—Fe—Kv | 111.788 (3) | Clxiii—Na—Kxvi | 104.307 (9) |
Cli—Fe—Kiv | 53.485 (8) | Clxiv—Na—Kxvi | 48.763 (4) |
Cl—Fe—Kiv | 126.515 (8) | Clxv—Na—Kxvi | 47.111 (4) |
Clii—Fe—Kiv | 124.893 (3) | Cl—Na—Kxvi | 101.876 (6) |
Cliii—Fe—Kiv | 123.032 (3) | Cliv—Na—Kxvi | 162.722 (2) |
Clv—Fe—Kiv | 56.968 (3) | Fexiii—Na—Kxvi | 58.490 (4) |
Cliv—Fe—Kiv | 55.107 (3) | Fe—Na—Kxvi | 121.510 (4) |
Na—Fe—Kiv | 72.959 (3) | Clv—Na—Kiv | 48.764 (4) |
Nai—Fe—Kiv | 107.041 (3) | Clxiii—Na—Kiv | 101.875 (6) |
Ki—Fe—Kiv | 68.212 (2) | Clxiv—Na—Kiv | 86.099 (8) |
K—Fe—Kiv | 111.788 (2) | Clxv—Na—Kiv | 162.722 (2) |
Kv—Fe—Kiv | 111.788 (2) | Cl—Na—Kiv | 104.307 (9) |
Clvi—K—Cliii | 153.734 (7) | Cliv—Na—Kiv | 47.111 (4) |
Clvi—K—Clvii | 130.279 (5) | Fexiii—Na—Kiv | 121.510 (4) |
Cliii—K—Clvii | 73.150 (8) | Fe—Na—Kiv | 58.490 (4) |
Clvi—K—Clviii | 73.148 (8) | Kxvi—Na—Kiv | 118.401 (4) |
Cliii—K—Clviii | 130.281 (5) | Clv—Na—Kv | 47.111 (4) |
Clvii—K—Clviii | 76.588 (10) | Clxiii—Na—Kv | 162.722 (2) |
Clvi—K—Clix | 68.551 (6) | Clxiv—Na—Kv | 101.875 (6) |
Cliii—K—Clix | 116.090 (6) | Clxv—Na—Kv | 86.099 (8) |
Clvii—K—Clix | 73.775 (4) | Cl—Na—Kv | 48.764 (4) |
Clviii—K—Clix | 91.342 (4) | Cliv—Na—Kv | 104.307 (9) |
Clvi—K—Cl | 116.090 (6) | Fexiii—Na—Kv | 121.510 (4) |
Cliii—K—Cl | 68.550 (6) | Fe—Na—Kv | 58.490 (4) |
Clvii—K—Cl | 91.344 (4) | Kxvi—Na—Kv | 64.366 (8) |
Clviii—K—Cl | 73.777 (4) | Kiv—Na—Kv | 95.179 (6) |
Clix—K—Cl | 161.231 (6) | Clv—Na—K | 104.307 (9) |
Clvi—K—Clx | 67.538 (6) | Clxiii—Na—K | 86.099 (8) |
Cliii—K—Clx | 90.534 (4) | Clxiv—Na—K | 162.722 (2) |
Clvii—K—Clx | 122.074 (4) | Clxv—Na—K | 101.875 (6) |
Clviii—K—Clx | 139.160 (4) | Cl—Na—K | 47.111 (4) |
Clix—K—Clx | 64.594 (4) | Cliv—Na—K | 48.764 (4) |
Cl—K—Clx | 134.151 (4) | Fexiii—Na—K | 121.510 (4) |
Clvi—K—Cliv | 90.535 (4) | Fe—Na—K | 58.490 (4) |
Cliii—K—Cliv | 67.537 (6) | Kxvi—Na—K | 140.938 (4) |
Clvii—K—Cliv | 139.161 (4) | Kiv—Na—K | 95.179 (6) |
Clviii—K—Cliv | 122.074 (4) | Kv—Na—K | 95.179 (6) |
Clix—K—Cliv | 134.151 (4) | Fe—Cl—Na | 80.609 (10) |
Cl—K—Cliv | 64.593 (4) | Fe—Cl—Kii | 86.860 (10) |
Clx—K—Cliv | 69.776 (5) | Na—Cl—Kii | 167.394 (4) |
Clvi—K—Fexi | 39.655 (3) | Fe—Cl—Kviii | 168.357 (5) |
Cliii—K—Fexi | 126.836 (3) | Na—Cl—Kviii | 96.949 (10) |
Clvii—K—Fexi | 113.330 (3) | Kii—Cl—Kviii | 95.060 (9) |
Clviii—K—Fexi | 101.096 (5) | Fe—Cl—K | 85.326 (4) |
Clix—K—Fexi | 39.568 (3) | Na—Cl—K | 93.225 (4) |
Cl—K—Fexi | 153.271 (4) | Kii—Cl—K | 87.080 (3) |
Clx—K—Fexi | 39.431 (3) | Kviii—Cl—K | 106.223 (4) |
Cliv—K—Fexi | 99.052 (4) | Fe—Cl—Kv | 83.602 (3) |
Clvi—K—Fe | 126.836 (3) | Na—Cl—Kv | 91.513 (3) |
Cliii—K—Fe | 39.655 (3) | Kii—Cl—Kv | 85.695 (3) |
Clvii—K—Fe | 101.097 (5) | Kviii—Cl—Kv | 85.091 (3) |
Clviii—K—Fe | 113.332 (3) | K—Cl—Kv | 167.083 (4) |
Clix—K—Fe | 153.270 (4) | | |
Symmetry codes: (i) −x, −y, −z; (ii) y, −x+y, −z; (iii) x−y, x, −z; (iv) −y, x−y, z; (v) −x+y, −x, z; (vi) −y+1/3, −x+2/3, z+1/6; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) −x+2/3, −y+1/3, −z+1/3; (ix) x−y+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, z−1/3; (xiii) y, x, −z+1/2; (xiv) −x, −x+y, −z+1/2; (xv) x−y, −y, −z+1/2; (xvi) x−1/3, y−2/3, z+1/3. |
(10K) tripotassium sodium hexachloroferrate(II)
top
Crystal data top
K3Na[FeCl6] | Dx = 2.421 Mg m−3 |
Mr = 408.84 | Melting point: not measured K |
Trigonal, R3c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -R 3 2"c | Cell parameters from 24 reflections |
a = 11.893 (1) Å | θ = 24.4–29.9° |
c = 13.735 (2) Å | µ = 3.86 mm−1 |
V = 1682.4 (3) Å3 | T = 10 K |
Z = 6 | Cube, very pale yellow |
F(000) = 1176 | 0.40 × 0.40 × 0.40 mm |
Data collection top
Huber 512 goniometer diffractometer | 1981 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.035 |
None monochromator | θmax = 50.2°, θmin = 3.4° |
ω–2θ scans | h = −25→25 |
Absorption correction: for a sphere (Xtal 3.4; Hall et al., 1994) | k = −25→25 |
Tmin = 0.257, Tmax = 0.306 | l = −29→29 |
28510 measured reflections | 3 standard reflections every 100 reflections |
1983 independent reflections | intensity decay: 1% |
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)] = 0.020 | w = 1/[σ2(Fo2) + (0.0109P)2 + 3.4848P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.050 | (Δ/σ)max = 0.001 |
S = 1.46 | Δρmax = 0.52 e Å−3 |
1983 reflections | Δρmin = −0.93 e Å−3 |
20 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction 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 | x | y | z | Uiso*/Ueq | |
Fe | 0.0000 | 0.0000 | 0.0000 | 0.00351 (3) | |
K | 0.289535 (16) | 0.3333 | 0.0833 | 0.00540 (3) | |
Na | 0.0000 | 0.0000 | 0.2500 | 0.00655 (10) | |
Cl | 0.180955 (14) | 0.027399 (15) | 0.107988 (11) | 0.00503 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe | 0.00347 (4) | 0.00347 (4) | 0.00360 (6) | 0.00174 (2) | 0.000 | 0.000 |
K | 0.00528 (4) | 0.00514 (6) | 0.00572 (6) | 0.00257 (3) | −0.00023 (2) | −0.00047 (4) |
Na | 0.00724 (16) | 0.00724 (16) | 0.0052 (2) | 0.00362 (8) | 0.000 | 0.000 |
Cl | 0.00461 (5) | 0.00553 (5) | 0.00517 (5) | 0.00271 (4) | −0.00032 (3) | −0.00004 (3) |
Geometric parameters (Å, º) top
Fe—Cli | 2.4973 (2) | K—Clx | 3.2915 (4) |
Fe—Cl | 2.4973 (2) | K—Cliv | 3.2916 (3) |
Fe—Clii | 2.4973 (2) | K—Fexi | 3.9028 (3) |
Fe—Cliii | 2.4973 (2) | K—Naxii | 4.3775 (3) |
Fe—Cliv | 2.4973 (2) | K—Kiii | 4.3775 (3) |
Fe—Clv | 2.4973 (2) | Na—Clv | 2.8002 (3) |
Fe—Na | 3.4337 (5) | Na—Clxiii | 2.8002 (3) |
Fe—Nai | 3.4337 (5) | Na—Clxiv | 2.8002 (3) |
Fe—K | 3.9029 (3) | Na—Clxv | 2.8002 (3) |
Fe—Ki | 3.9029 (3) | Na—Cl | 2.8002 (3) |
Fe—Kii | 3.9029 (3) | Na—Cliv | 2.8002 (3) |
Fe—Kiv | 3.9029 (3) | Na—Fexiii | 3.4337 (5) |
K—Clvi | 3.1423 (4) | Na—Kxvi | 4.3775 (3) |
K—Cliii | 3.1423 (4) | Na—Kiv | 4.3775 (3) |
K—Clvii | 3.1803 (3) | Na—Kv | 4.3775 (3) |
K—Clviii | 3.1803 (3) | Cl—Kii | 3.1423 (4) |
K—Clix | 3.2128 (3) | Cl—Kviii | 3.1803 (3) |
K—Cl | 3.2128 (3) | Cl—Kv | 3.2916 (3) |
| | | |
Cli—Fe—Cl | 180.000 (9) | Cl—K—Fe | 39.618 (3) |
Cli—Fe—Clii | 88.330 (8) | Clx—K—Fe | 99.063 (5) |
Cl—Fe—Clii | 91.670 (8) | Cliv—K—Fe | 39.482 (3) |
Cli—Fe—Cliii | 88.330 (8) | Fexi—K—Fe | 136.025 (5) |
Cl—Fe—Cliii | 91.670 (8) | Clvi—K—Naxii | 88.285 (9) |
Clii—Fe—Cliii | 88.331 (8) | Cliii—K—Naxii | 83.042 (8) |
Cli—Fe—Cliv | 91.670 (8) | Clvii—K—Naxii | 82.626 (6) |
Cl—Fe—Cliv | 88.330 (8) | Clviii—K—Naxii | 130.715 (5) |
Clii—Fe—Cliv | 180.000 (9) | Clix—K—Naxii | 39.694 (3) |
Cliii—Fe—Cliv | 91.670 (8) | Cl—K—Naxii | 151.541 (4) |
Cli—Fe—Clv | 91.670 (8) | Clx—K—Naxii | 39.751 (3) |
Cl—Fe—Clv | 88.330 (8) | Cliv—K—Naxii | 102.777 (5) |
Clii—Fe—Clv | 91.670 (8) | Fexi—K—Naxii | 48.584 (7) |
Cliii—Fe—Clv | 180.000 (5) | Fe—K—Naxii | 114.303 (6) |
Cliv—Fe—Clv | 88.330 (8) | Clvi—K—Kiii | 107.297 (8) |
Cli—Fe—Na | 126.437 (6) | Cliii—K—Kiii | 47.137 (4) |
Cl—Fe—Na | 53.563 (6) | Clvii—K—Kiii | 110.640 (9) |
Clii—Fe—Na | 126.437 (6) | Clviii—K—Kiii | 167.330 (3) |
Cliii—Fe—Na | 126.437 (6) | Clix—K—Kiii | 100.660 (6) |
Cliv—Fe—Na | 53.563 (6) | Cl—K—Kiii | 95.340 (3) |
Clv—Fe—Na | 53.563 (6) | Clx—K—Kiii | 46.374 (4) |
Cli—Fe—Nai | 53.563 (6) | Cliv—K—Kiii | 45.711 (5) |
Cl—Fe—Nai | 126.437 (6) | Fexi—K—Kiii | 85.826 (6) |
Clii—Fe—Nai | 53.563 (6) | Fe—K—Kiii | 55.888 (1) |
Cliii—Fe—Nai | 53.563 (6) | Naxii—K—Kiii | 61.635 (5) |
Cliv—Fe—Nai | 126.437 (6) | Clv—Na—Clxiii | 148.920 (7) |
Clv—Fe—Nai | 126.437 (6) | Clv—Na—Clxiv | 127.478 (8) |
Na—Fe—Nai | 180.0 | Clxiii—Na—Clxiv | 76.831 (9) |
Cli—Fe—K | 124.877 (4) | Clv—Na—Clxv | 89.470 (11) |
Cl—Fe—K | 55.123 (4) | Clxiii—Na—Clxv | 76.831 (9) |
Clii—Fe—K | 123.061 (4) | Clxiv—Na—Clxv | 76.831 (9) |
Cliii—Fe—K | 53.501 (8) | Clv—Na—Cl | 76.831 (9) |
Cliv—Fe—K | 56.939 (4) | Clxiii—Na—Cl | 127.478 (8) |
Clv—Fe—K | 126.499 (8) | Clxiv—Na—Cl | 89.470 (11) |
Na—Fe—K | 72.946 (3) | Clxv—Na—Cl | 148.920 (7) |
Nai—Fe—K | 107.054 (3) | Clv—Na—Cliv | 76.831 (9) |
Cli—Fe—Ki | 55.123 (4) | Clxiii—Na—Cliv | 89.470 (11) |
Cl—Fe—Ki | 124.877 (4) | Clxiv—Na—Cliv | 148.920 (7) |
Clii—Fe—Ki | 56.939 (4) | Clxv—Na—Cliv | 127.478 (8) |
Cliii—Fe—Ki | 126.499 (8) | Cl—Na—Cliv | 76.831 (9) |
Cliv—Fe—Ki | 123.061 (4) | Clv—Na—Fexiii | 134.153 (6) |
Clv—Fe—Ki | 53.501 (8) | Clxiii—Na—Fexiii | 45.847 (6) |
Na—Fe—Ki | 107.054 (3) | Clxiv—Na—Fexiii | 45.847 (6) |
Nai—Fe—Ki | 72.946 (3) | Clxv—Na—Fexiii | 45.847 (6) |
K—Fe—Ki | 180.0 | Cl—Na—Fexiii | 134.153 (6) |
Cli—Fe—Kii | 126.499 (8) | Cliv—Na—Fexiii | 134.153 (6) |
Cl—Fe—Kii | 53.501 (8) | Clv—Na—Fe | 45.847 (6) |
Clii—Fe—Kii | 55.123 (4) | Clxiii—Na—Fe | 134.153 (6) |
Cliii—Fe—Kii | 56.939 (4) | Clxiv—Na—Fe | 134.153 (6) |
Cliv—Fe—Kii | 124.877 (4) | Clxv—Na—Fe | 134.153 (6) |
Clv—Fe—Kii | 123.061 (4) | Cl—Na—Fe | 45.847 (6) |
Na—Fe—Kii | 107.054 (3) | Cliv—Na—Fe | 45.847 (6) |
Nai—Fe—Kii | 72.946 (3) | Fexiii—Na—Fe | 180.0 |
K—Fe—Kii | 68.223 (2) | Clv—Na—Kxvi | 86.083 (8) |
Ki—Fe—Kii | 111.777 (2) | Clxiii—Na—Kxvi | 104.310 (10) |
Cli—Fe—Kiv | 53.501 (8) | Clxiv—Na—Kxvi | 47.122 (4) |
Cl—Fe—Kiv | 126.499 (8) | Clxv—Na—Kxvi | 48.735 (5) |
Clii—Fe—Kiv | 124.877 (4) | Cl—Na—Kxvi | 101.899 (7) |
Cliii—Fe—Kiv | 123.061 (4) | Cliv—Na—Kxvi | 162.735 (3) |
Cliv—Fe—Kiv | 55.123 (4) | Fexiii—Na—Kxvi | 58.470 (4) |
Clv—Fe—Kiv | 56.939 (4) | Fe—Na—Kxvi | 121.530 (4) |
Na—Fe—Kiv | 72.946 (3) | Clv—Na—Kiv | 48.735 (5) |
Nai—Fe—Kiv | 107.054 (3) | Clxiii—Na—Kiv | 101.898 (7) |
K—Fe—Kiv | 111.777 (2) | Clxiv—Na—Kiv | 162.734 (3) |
Ki—Fe—Kiv | 68.223 (2) | Clxv—Na—Kiv | 86.083 (8) |
Kii—Fe—Kiv | 180.0 | Cl—Na—Kiv | 104.311 (10) |
Clvi—K—Cliii | 153.843 (9) | Cliv—Na—Kiv | 47.122 (4) |
Clvi—K—Clvii | 130.253 (6) | Fexiii—Na—Kiv | 121.530 (4) |
Cliii—K—Clvii | 73.084 (9) | Fe—Na—Kiv | 58.470 (4) |
Clvi—K—Clviii | 73.082 (9) | Kxvi—Na—Kiv | 118.365 (5) |
Cliii—K—Clviii | 130.255 (6) | Clv—Na—Kv | 47.122 (4) |
Clvii—K—Clviii | 76.589 (11) | Clxiii—Na—Kv | 162.734 (3) |
Clvi—K—Clix | 68.623 (7) | Clxiv—Na—Kv | 86.083 (8) |
Cliii—K—Clix | 116.032 (7) | Clxv—Na—Kv | 101.898 (7) |
Clvii—K—Clix | 73.701 (5) | Cl—Na—Kv | 48.735 (5) |
Clviii—K—Clix | 91.301 (5) | Cliv—Na—Kv | 104.311 (10) |
Clvi—K—Cl | 116.033 (7) | Fexiii—Na—Kv | 121.530 (4) |
Cliii—K—Cl | 68.622 (7) | Fe—Na—Kv | 58.470 (4) |
Clvii—K—Cl | 91.302 (5) | Kxvi—Na—Kv | 64.417 (9) |
Clviii—K—Cl | 73.703 (5) | Kiv—Na—Kv | 95.152 (6) |
Clix—K—Cl | 161.085 (8) | Clv—Na—K | 104.311 (10) |
Clvi—K—Clx | 67.633 (7) | Clxiii—Na—K | 86.083 (8) |
Cliii—K—Clx | 90.532 (6) | Clxiv—Na—K | 101.898 (7) |
Clvii—K—Clx | 122.061 (4) | Clxv—Na—K | 162.734 (3) |
Clviii—K—Clx | 139.187 (5) | Cl—Na—K | 47.122 (4) |
Clix—K—Clx | 64.675 (5) | Cliv—Na—K | 48.735 (5) |
Cl—K—Clx | 134.215 (5) | Fexiii—Na—K | 121.530 (4) |
Clvi—K—Cliv | 90.533 (6) | Fe—Na—K | 58.470 (4) |
Cliii—K—Cliv | 67.631 (7) | Kxvi—Na—K | 141.000 (5) |
Clvii—K—Cliv | 139.188 (5) | Kiv—Na—K | 95.152 (6) |
Clviii—K—Cliv | 122.061 (4) | Kv—Na—K | 95.152 (6) |
Clix—K—Cliv | 134.216 (5) | Fe—Cl—Na | 80.589 (10) |
Cl—K—Cliv | 64.674 (5) | Fe—Cl—Kii | 86.793 (10) |
Clx—K—Cliv | 69.761 (6) | Na—Cl—Kii | 167.311 (6) |
Clvi—K—Fexi | 39.707 (3) | Fe—Cl—Kviii | 168.349 (6) |
Cliii—K—Fexi | 126.861 (5) | Na—Cl—Kviii | 96.970 (10) |
Clvii—K—Fexi | 113.306 (4) | Kii—Cl—Kviii | 95.129 (10) |
Clviii—K—Fexi | 101.071 (5) | Fe—Cl—K | 85.259 (5) |
Clix—K—Fexi | 39.619 (3) | Na—Cl—K | 93.184 (5) |
Cl—K—Fexi | 153.298 (5) | Kii—Cl—K | 87.065 (4) |
Clx—K—Fexi | 39.483 (3) | Kviii—Cl—K | 106.297 (5) |
Cliv—K—Fexi | 99.064 (5) | Fe—Cl—Kv | 83.579 (4) |
Clvi—K—Fe | 126.862 (5) | Na—Cl—Kv | 91.514 (5) |
Cliii—K—Fe | 39.706 (3) | Kii—Cl—Kv | 85.714 (4) |
Clvii—K—Fe | 101.072 (5) | Kviii—Cl—Kv | 85.106 (4) |
Clviii—K—Fe | 113.308 (4) | K—Cl—Kv | 167.017 (6) |
Clix—K—Fe | 153.297 (5) | | |
Symmetry codes: (i) −x, −y, −z; (ii) y, −x+y, −z; (iii) x−y, x, −z; (iv) −y, x−y, z; (v) −x+y, −x, z; (vi) −y+1/3, −x+2/3, z+1/6; (vii) −x+y+2/3, y+1/3, z−1/6; (viii) −x+2/3, −y+1/3, −z+1/3; (ix) x−y+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, z−1/3; (xiii) y, x, −z+1/2; (xiv) x−y, −y, −z+1/2; (xv) −x, −x+y, −z+1/2; (xvi) x−1/3, y−2/3, z+1/3. |
Bond lengths (A) and angles (°) in K3Na[FeCl6] at 293, 84 and 9.5 K top | 293 K | 84 K | 9.5 K |
Fe—Cl | 2.5124 (5) | 2.5009 (2) | 2.4973 (2) |
Cl—Fe—Cl' | 180 | 180 | 180 |
| | | |
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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