Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010876810402333X/bk0147sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810402333X/bk01471sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S010876810402333X/bk01472sup3.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S010876810402333X/bk0147sup4.pdf |
The intensity data from Crystal 1 and, separately, Crystal 2 were each corrected for absorption with DIFABS following isotropic refinement (Walker & Stuart, 1983). Corrections based on azimuthal scans did not lead to significant reduction in residuals or standard uncertainties (s.u.s) and analytical corrections were precluded by the irregular crystal form. We found the results of corrections made with DIFABS for µ < 5 mm−1 are comparable with those made analytically, a conclusion supported by the minor residual systematic error detected in atomic coordinates The intensies of three control reflections showed no significant variation for either crystal. Structure solution: SIR92 E-map (Altomare et al., 1994), confirmed by Patterson solution. The refined site occupancy factors for the K and Cr atoms were not significantly different from unity. The value of a secondary extinction parameter was also refined. The structure of K2Cr2O7 has been reported both by Brandon & Brown (1968) who used a non-standard triclinic cell (a = 13.367, b = 7.376, c = 7.445 Å) and by Brunton (1973).
Data collection: CAD-4-PC (Enraf-Nonius, 1993) for (1). Cell refinement: CAD-4-PC (Enraf-Nonius, 1993) for (1). Data reduction: TEXSAN (Molecular Structure Corp., 1997) for (1). Program(s) used to solve structure: TEXSAN (Molecular Structure Corp., 1997) for (1). Program(s) used to refine structure: TEXSAN (Molecular Structure Corp., 1997) for (1). Software used to prepare material for publication: TEXSAN (Molecular Structure Corp., 1997) for (1).
K2Cr2O7 | Z = 4 |
Mr = 294.18 | F(000) = 568 |
Triclinic, P1 | Dx = 2.694 Mg m−3 Dm = 2.676 Mg m−3 Dm measured by ? |
Hall symbol: -P 1 | Melting point: 659 K |
a = 7.3807 (9) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 7.4593 (11) Å | Cell parameters from 25 reflections |
c = 13.3910 (16) Å | θ = 14.0–15.0° |
α = 96.205 (11)° | µ = 4.13 mm−1 |
β = 98.033 (10)° | T = 296 K |
γ = 90.914 (12)° | Block, intense-orange |
V = 725.37 (16) Å3 | 0.27 × 0.20 × 0.14 mm |
Nonius CAD-4 serial diffractometer | 4096 reflections with I > 1.00σ(I) |
Radiation source: sealed X-ray tube | Rint = 0.011 |
Graphite monochromator | θmax = 30.0°, θmin = 1.5° |
ω–2θ scans | h = 0→10 |
Absorption correction: part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983) | k = −10→10 |
Tmin = 0.382, Tmax = 0.560 | l = −18→18 |
4533 measured reflections | 3 standard reflections every 300 reflections |
4227 independent reflections | intensity decay: 0.0% |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 4Fo2/[σ2(I) + (0.025I)2] |
R[F2 > 2σ(F2)] = 0.025 | (Δ/σ)max = 0.020 |
wR(F2) = 0.040 | Δρmax = 0.49 e Å−3 |
S = 1.58 | Δρmin = −0.40 e Å−3 |
4227 reflections | Extinction correction: Zachariasen (1967), equ(3) Acta Cryst.(1968) A24, p213. |
200 parameters | Extinction coefficient: 1.27 x 10-6 |
0 restraints |
K2Cr2O7 | γ = 90.914 (12)° |
Mr = 294.18 | V = 725.37 (16) Å3 |
Triclinic, P1 | Z = 4 |
a = 7.3807 (9) Å | Mo Kα radiation |
b = 7.4593 (11) Å | µ = 4.13 mm−1 |
c = 13.3910 (16) Å | T = 296 K |
α = 96.205 (11)° | 0.27 × 0.20 × 0.14 mm |
β = 98.033 (10)° |
Nonius CAD-4 serial diffractometer | 4096 reflections with I > 1.00σ(I) |
Absorption correction: part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983) | Rint = 0.011 |
Tmin = 0.382, Tmax = 0.560 | 3 standard reflections every 300 reflections |
4533 measured reflections | intensity decay: 0.0% |
4227 independent reflections |
R[F2 > 2σ(F2)] = 0.025 | 200 parameters |
wR(F2) = 0.040 | 0 restraints |
S = 1.58 | Δρmax = 0.49 e Å−3 |
4227 reflections | Δρmin = −0.40 e Å−3 |
x | y | z | Uiso*/Ueq | ||
Cr(1) | 0.59179 (4) | 0.76891 (5) | 0.60724 (2) | 0.01925 (8) | |
Cr(2) | 0.79289 (4) | 0.80674 (5) | 0.41375 (2) | 0.01880 (8) | |
Cr(3) | 0.81711 (4) | 0.42584 (5) | 0.11354 (2) | 0.01890 (8) | |
Cr(4) | 0.81344 (4) | 0.15250 (4) | −0.08323 (2) | 0.01835 (8) | |
K(1) | 1.10341 (8) | 0.66917 (7) | 0.64038 (4) | 0.03104 (13) | |
K(2) | 0.25001 (7) | 0.76710 (7) | 0.34950 (4) | 0.02929 (12) | |
K(3) | 0.66252 (6) | −0.08518 (7) | 0.15847 (4) | 0.02480 (11) | |
K(4) | 0.69509 (8) | 0.65240 (7) | −0.13583 (4) | 0.03184 (13) | |
O(1) | 0.7201 (3) | 0.6124 (3) | 0.64937 (14) | 0.0342 (5) | |
O(2) | 0.5550 (3) | 0.9102 (3) | 0.70198 (13) | 0.0349 (5) | |
O(3) | 0.4024 (2) | 0.6849 (3) | 0.54525 (14) | 0.0361 (5) | |
O(4) | 0.7076 (2) | 0.8937 (2) | 0.52700 (13) | 0.0296 (4) | |
O(5) | 0.9595 (2) | 0.6749 (2) | 0.44295 (12) | 0.0288 (4) | |
O(6) | 0.8687 (3) | 0.9709 (2) | 0.36065 (13) | 0.0331 (5) | |
O(7) | 0.6345 (2) | 0.6952 (3) | 0.33667 (14) | 0.0362 (5) | |
O(8) | 0.6891 (2) | 0.2927 (2) | 0.16402 (13) | 0.0306 (4) | |
O(9) | 0.9757 (2) | 0.5181 (3) | 0.19989 (12) | 0.0304 (4) | |
O(10) | 0.6948 (3) | 0.5751 (3) | 0.06114 (13) | 0.0345 (5) | |
O(11) | 0.9299 (2) | 0.2957 (2) | 0.02274 (12) | 0.0246 (4) | |
O(12) | 0.6919 (2) | −0.0006 (2) | −0.04330 (13) | 0.0296 (4) | |
O(13) | 0.9600 (2) | 0.0608 (3) | −0.14886 (15) | 0.0373 (5) | |
O(14) | 0.6770 (2) | 0.2738 (2) | −0.15168 (12) | 0.0270 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr(1) | 0.0190 (2) | 0.0207 (2) | 0.0186 (2) | 0.00273 (12) | 0.00384 (12) | 0.00238 (12) |
Cr(2) | 0.0181 (2) | 0.0203 (2) | 0.0188 (2) | 0.00215 (12) | 0.00358 (11) | 0.00476 (12) |
Cr(3) | 0.0192 (2) | 0.0183 (2) | 0.0185 (2) | −0.00111 (11) | 0.00035 (11) | 0.00206 (12) |
Cr(4) | 0.0171 (2) | 0.0182 (2) | 0.0197 (2) | 0.00068 (11) | 0.00301 (11) | 0.00111 (12) |
K(1) | 0.0375 (3) | 0.0315 (3) | 0.0237 (2) | −0.0073 (2) | 0.0020 (2) | 0.0055 (2) |
K(2) | 0.0327 (3) | 0.0273 (2) | 0.0290 (2) | −0.0025 (2) | 0.0094 (2) | 0.00208 (19) |
K(3) | 0.0236 (2) | 0.0243 (2) | 0.0261 (2) | −0.00002 (17) | 0.00360 (17) | 0.009 (2) |
K(4) | 0.0373 (3) | 0.0302 (3) | 0.0278 (2) | 0.0102 (2) | 0.0035 (2) | 0.0023 (2) |
O(1) | 0.0328 (9) | 0.0319 (9) | 0.0380 (10) | 0.0093 (7) | −0.0001 (7) | 0.0100 (8) |
O(2) | 0.0434 (10) | 0.0336 (9) | 0.0294 (9) | 0.0031 (8) | 0.0162 (8) | −0.0029 (7) |
O(3) | 0.0264 (8) | 0.0461 (11) | 0.0338 (9) | −0.0043 (8) | −0.0020 (7) | 0.0044 (8) |
O(4) | 0.0381 (9) | 0.0248 (8) | 0.0294 (8) | 0.0010 (7) | 0.0168 (7) | 0.0027 (6) |
O(5) | 0.0272 (8) | 0.0328 (9) | 0.0274 (8) | 0.0107 (7) | 0.0032 (6) | 0.0068 (7) |
O(6) | 0.0423 (10) | 0.0280 (9) | 0.0324 (9) | −0.0014 (7) | 0.0109 (7) | 0.0117 (7) |
O(7) | 0.0273 (8) | 0.0438 (11) | 0.0344 (9) | −0.0053 (8) | −0.0018 (7) | −0.0003 (8) |
O(8) | 0.0302 (8) | 0.0290 (9) | 0.0336 (9) | −0.0070 (7) | 0.0084 (7) | 0.0045 (7) |
O(9) | 0.0301 (8) | 0.0366 (9) | 0.0220 (7) | −0.0105 (7) | 0.0000 (6) | −0.0010 (7) |
O(10) | 0.0407 (10) | 0.0317 (9) | 0.0310 (9) | 0.0140 (8) | 0.0024 (7) | 0.0053 (7) |
O(11) | 0.0195 (7) | 0.0269 (8) | 0.0254 (7) | 0.0000 (6) | 0.0004 (6) | −0.0026 (6) |
O(12) | 0.0368 (9) | 0.0245 (8) | 0.0278 (8) | −0.0078 (7) | 0.0055 (7) | 0.0046 (6) |
O(13) | 0.0290 (9) | 0.0431 (11) | 0.0396 (10) | 0.0067 (8) | 0.0123 (7) | −0.0068 (8) |
O(14) | 0.0269 (8) | 0.0249 (8) | 0.0286 (8) | 0.0022 (6) | −0.0016 (6) | 0.0065 (6) |
Cr(1)—O(1) | 1.6144 (17) | K(2)—O(3) | 2.8386 (19) |
Cr(1)—O(2) | 1.6158 (17) | K(2)—O(4)v | 2.8569 (17) |
Cr(1)—O(3) | 1.6036 (17) | K(2)—O(5)vi | 2.7434 (17) |
Cr(1)—O(4) | 1.7884 (16) | K(2)—O(6)vi | 3.234 (2) |
Cr(2)—O(4) | 1.7844 (16) | K(2)—O(7) | 2.9212 (19) |
Cr(2)—O(5) | 1.6181 (16) | K(2)—O(9)vi | 3.0827 (17) |
Cr(2)—O(6) | 1.6110 (17) | K(2)—O(13)vii | 3.303 (2) |
Cr(2)—O(7) | 1.6035 (17) | K(2)—O(14)vii | 2.7621 (17) |
Cr(3)—O(8) | 1.6216 (16) | K(3)—O(2)iv | 2.8547 (17) |
Cr(3)—O(9) | 1.6141 (16) | K(3)—O(6)viii | 2.8990 (19) |
Cr(3)—O(10) | 1.6034 (17) | K(3)—O(7)viii | 3.065 (2) |
Cr(3)—O(11) | 1.7795 (16) | K(3)—O(8) | 2.8146 (18) |
Cr(4)—O(11) | 1.7877 (15) | K(3)—O(10)viii | 2.7511 (18) |
Cr(4)—O(12) | 1.6213 (16) | K(3)—O(12) | 2.8764 (17) |
Cr(4)—O(13) | 1.6030 (17) | K(3)—O(12)ix | 2.9610 (19) |
Cr(4)—O(14) | 1.6195 (16) | K(3)—O(13)x | 2.8108 (18) |
K(1)—O(1) | 2.8753 (19) | K(3)—O(14)ix | 2.8397 (17) |
K(1)—O(3)i | 2.7046 (19) | K(4)—O(1)xi | 2.892 (2) |
K(1)—O(5) | 2.7131 (17) | K(4)—O(2)xi | 3.134 (2) |
K(1)—O(5)ii | 2.6920 (18) | K(4)—O(8)vii | 2.8501 (18) |
K(1)—O(6)iii | 2.6912 (18) | K(4)—O(9)xii | 2.9498 (19) |
K(1)—O(8)ii | 2.8267 (18) | K(4)—O(10) | 2.7604 (19) |
K(1)—O(9)ii | 2.7995 (18) | K(4)—O(11)xii | 2.9618 (16) |
K(2)—O(1)iv | 2.8442 (19) | K(4)—O(12)xiii | 2.7483 (18) |
K(2)—O(2)v | 2.9778 (19) | K(4)—O(14) | 2.8088 (17) |
Cr(1)···K(2)v | 3.5954 (6) | K(4)···O(14) | 2.8088 (17) |
Cr(3)···K(1)ii | 3.4180 (6) | K(4)···O(8)vii | 2.8501 (18) |
Cr(3)···O(11)xii | 3.5748 (17) | K(4)···O(1)xi | 2.892 (2) |
Cr(4)···O(9)xii | 3.5050 (17) | K(4)···O(9)xii | 2.9498 (19) |
Cr(4)···O(2)xiv | 3.5230 (19) | K(4)···O(11)xii | 2.9618 (16) |
Cr(4)···K(3)ix | 3.5289 (7) | K(4)···O(2)xi | 3.134 (2) |
K(1)···O(6)iii | 2.6912 (18) | O(1)···O(9)ii | 3.048 (3) |
K(1)···O(5)ii | 2.6920 (18) | O(1)···O(3)iv | 3.249 (3) |
K(1)···O(3)i | 2.7046 (19) | O(1)···O(5)ii | 3.482 (2) |
K(1)···O(5) | 2.7131 (17) | O(1)···O(7)iv | 3.490 (3) |
K(1)···O(9)ii | 2.7995 (18) | O(2)···O(8)iv | 3.187 (2) |
K(1)···O(8)ii | 2.8267 (18) | O(2)···O(14)xv | 3.207 (2) |
K(1)···O(1) | 2.8753 (19) | O(2)···O(12)xv | 3.409 (2) |
K(1)···O(7)ii | 3.377 (2) | O(2)···O(13)xv | 3.454 (3) |
K(2)···O(5)vi | 2.7434 (17) | O(3)···O(3)iv | 3.324 (4) |
K(2)···O(14)vii | 2.7621 (17) | O(3)···O(5)vi | 3.360 (2) |
K(2)···O(3) | 2.8386 (19) | O(3)···O(7)iv | 3.417 (3) |
K(2)···O(1)iv | 2.8442 (19) | O(4)···O(6)iii | 3.365 (3) |
K(2)···O(4)v | 2.8569 (17) | O(5)···O(5)ii | 3.187 (3) |
K(2)···O(7) | 2.9212 (19) | O(5)···O(9) | 3.357 (2) |
K(2)···O(2)v | 2.9778 (19) | O(6)···O(13)xii | 3.250 (3) |
K(2)···O(9)vi | 3.0827 (17) | O(7)···O(14)vii | 3.166 (2) |
K(2)···O(6)vi | 3.234 (2) | O(7)···O(9) | 3.510 (3) |
K(2)···O(13)vii | 3.303 (2) | O(9)···O(14)xii | 3.154 (2) |
K(3)···O(10)viii | 2.7511 (18) | O(9)···O(13)xii | 3.326 (3) |
K(3)···O(13)x | 2.8108 (18) | O(9)···O(11)xii | 3.570 (2) |
K(3)···O(8) | 2.8146 (18) | O(10)···O(10)vii | 3.223 (4) |
K(3)···O(14)ix | 2.8397 (17) | O(10)···O(11)xii | 3.299 (3) |
K(3)···O(2)iv | 2.8547 (17) | O(10)···O(14)vii | 3.317 (3) |
K(3)···O(12) | 2.8764 (17) | O(10)···O(12)xiii | 3.595 (3) |
K(3)···O(6)viii | 2.8990 (19) | O(11)···O(11)xii | 3.348 (3) |
K(3)···O(12)ix | 2.9610 (19) | O(11)···O(13)x | 3.353 (3) |
K(3)···O(7)viii | 3.065 (2) | O(11)···O(12)x | 3.582 (2) |
K(4)···O(12)xiii | 2.7483 (18) | O(12)···O(13)x | 3.445 (3) |
K(4)···O(10) | 2.7604 (19) | ||
O(1)—Cr(1)—O(2) | 108.87 (10) | O(7)viii—K(3)—O(14)ix | 64.72 (5) |
O(1)—Cr(1)—O(3) | 110.89 (10) | O(8)—K(3)—O(10)viii | 150.58 (6) |
O(1)—Cr(1)—O(4) | 110.25 (9) | O(8)—K(3)—O(12) | 72.02 (5) |
O(2)—Cr(1)—O(3) | 110.70 (10) | O(8)—K(3)—O(12)ix | 77.35 (5) |
O(2)—Cr(1)—O(4) | 106.54 (9) | O(8)—K(3)—O(13)x | 83.21 (5) |
O(3)—Cr(1)—O(4) | 109.49 (9) | O(8)—K(3)—O(14)ix | 122.38 (5) |
O(4)—Cr(2)—O(5) | 108.86 (8) | O(10)viii—K(3)—O(12) | 79.38 (5) |
O(4)—Cr(2)—O(6) | 109.55 (9) | O(10)viii—K(3)—O(12)ix | 97.76 (5) |
O(4)—Cr(2)—O(7) | 110.43 (9) | O(10)viii—K(3)—O(13)x | 82.68 (6) |
O(5)—Cr(2)—O(6) | 108.92 (9) | O(10)viii—K(3)—O(14)ix | 72.77 (5) |
O(5)—Cr(2)—O(7) | 109.32 (10) | O(12)—K(3)—O(12)ix | 66.62 (6) |
O(6)—Cr(2)—O(7) | 109.72 (10) | O(12)—K(3)—O(13)x | 74.55 (6) |
O(8)—Cr(3)—O(9) | 109.26 (9) | O(12)—K(3)—O(14)ix | 107.84 (5) |
O(8)—Cr(3)—O(10) | 109.99 (10) | O(12)ix—K(3)—O(13)x | 140.27 (6) |
O(8)—Cr(3)—O(11) | 109.11 (8) | O(12)ix—K(3)—O(14)ix | 53.85 (5) |
O(9)—Cr(3)—O(10) | 111.28 (10) | O(13)x—K(3)—O(14)ix | 154.15 (6) |
O(9)—Cr(3)—O(11) | 106.47 (8) | O(1)xi—K(4)—O(2)xi | 51.52 (5) |
O(10)—Cr(3)—O(11) | 110.66 (8) | O(1)xi—K(4)—O(8)vii | 94.10 (5) |
O(11)—Cr(4)—O(12) | 109.64 (8) | O(1)xi—K(4)—O(9)xii | 62.90 (5) |
O(11)—Cr(4)—O(13) | 109.56 (8) | O(1)xi—K(4)—O(10) | 161.66 (6) |
O(11)—Cr(4)—O(14) | 108.49 (8) | O(1)xi—K(4)—O(11)xii | 108.42 (5) |
O(12)—Cr(4)—O(13) | 110.50 (10) | O(1)xi—K(4)—O(12)xiii | 116.50 (5) |
O(12)—Cr(4)—O(14) | 108.43 (9) | O(1)xi—K(4)—O(14) | 86.44 (5) |
O(13)—Cr(4)—O(14) | 110.18 (10) | O(2)xi—K(4)—O(8)vii | 64.16 (5) |
O(1)—K(1)—O(3)i | 154.63 (6) | O(2)xi—K(4)—O(9)xii | 106.97 (5) |
O(1)—K(1)—O(5) | 78.80 (5) | O(2)xi—K(4)—O(10) | 145.70 (5) |
O(1)—K(1)—O(5)ii | 77.34 (5) | O(2)xi—K(4)—O(11)xii | 120.07 (5) |
O(1)—K(1)—O(6)iii | 102.26 (6) | O(2)xi—K(4)—O(12)xiii | 70.49 (5) |
O(1)—K(1)—O(8)ii | 111.58 (5) | O(2)xi—K(4)—O(14) | 129.20 (5) |
O(1)—K(1)—O(9)ii | 64.96 (5) | O(8)vii—K(4)—O(9)xii | 151.46 (5) |
O(3)i—K(1)—O(5) | 76.65 (5) | O(8)vii—K(4)—O(10) | 92.53 (5) |
O(3)i—K(1)—O(5)ii | 89.13 (6) | O(8)vii—K(4)—O(11)xii | 153.71 (5) |
O(3)i—K(1)—O(6)iii | 81.29 (6) | O(8)vii—K(4)—O(12)xiii | 80.31 (5) |
O(3)i—K(1)—O(8)ii | 93.50 (5) | O(8)vii—K(4)—O(14) | 97.34 (5) |
O(3)i—K(1)—O(9)ii | 132.45 (6) | O(9)xii—K(4)—O(10) | 104.94 (5) |
O(5)—K(1)—O(5)ii | 72.27 (6) | O(9)xii—K(4)—O(11)xii | 54.80 (4) |
O(5)—K(1)—O(6)iii | 83.55 (6) | O(9)xii—K(4)—O(12)xiii | 123.95 (5) |
O(5)—K(1)—O(8)ii | 168.37 (5) | O(9)xii—K(4)—O(14) | 66.36 (5) |
O(5)—K(1)—O(9)ii | 135.58 (5) | O(10)—K(4)—O(11)xii | 70.31 (5) |
O(5)ii—K(1)—O(6)iii | 155.49 (5) | O(10)—K(4)—O(12)xiii | 81.48 (5) |
O(5)ii—K(1)—O(8)ii | 114.28 (5) | O(10)—K(4)—O(14) | 75.75 (5) |
O(5)ii—K(1)—O(9)ii | 75.33 (5) | O(11)xii—K(4)—O(12)xiii | 77.60 (5) |
O(6)iii—K(1)—O(8)ii | 88.91 (6) | O(11)xii—K(4)—O(14) | 97.43 (5) |
O(6)iii—K(1)—O(9)ii | 127.21 (6) | O(12)xiii—K(4)—O(14) | 157.00 (5) |
O(8)ii—K(1)—O(9)ii | 55.93 (5) | Cr(1)—O(1)—K(1) | 114.36 (9) |
O(1)iv—K(2)—O(2)v | 141.70 (5) | Cr(1)—O(1)—K(2)iv | 144.21 (10) |
O(1)iv—K(2)—O(3) | 69.73 (6) | Cr(1)—O(1)—K(4)xvi | 103.26 (8) |
O(1)iv—K(2)—O(4)v | 144.47 (5) | K(1)—O(1)—K(2)iv | 93.43 (5) |
O(1)iv—K(2)—O(5)vi | 77.06 (5) | K(1)—O(1)—K(4)xvi | 104.07 (6) |
O(1)iv—K(2)—O(6)vi | 123.00 (5) | K(2)iv—O(1)—K(4)xvi | 90.42 (5) |
O(1)iv—K(2)—O(7) | 74.50 (6) | Cr(1)—O(2)—K(2)v | 98.66 (8) |
O(1)iv—K(2)—O(9)vi | 61.74 (5) | Cr(1)—O(2)—K(3)iv | 154.96 (10) |
O(1)iv—K(2)—O(13)vii | 120.92 (5) | Cr(1)—O(2)—K(4)xvi | 93.82 (8) |
O(1)iv—K(2)—O(14)vii | 88.26 (5) | K(2)v—O(2)—K(3)iv | 99.10 (6) |
O(2)v—K(2)—O(3) | 109.63 (5) | K(2)v—O(2)—K(4)xvi | 127.47 (7) |
O(2)v—K(2)—O(4)v | 55.75 (5) | K(3)iv—O(2)—K(4)xvi | 89.25 (5) |
O(2)v—K(2)—O(5)vi | 140.92 (5) | Cr(1)—O(3)—K(1)vi | 119.64 (9) |
O(2)v—K(2)—O(6)vi | 93.86 (5) | Cr(1)—O(3)—K(2) | 124.85 (10) |
O(2)v—K(2)—O(7) | 68.92 (5) | K(1)vi—O(3)—K(2) | 102.31 (6) |
O(2)v—K(2)—O(9)vi | 125.21 (5) | Cr(1)—O(4)—Cr(2) | 126.91 (10) |
O(2)v—K(2)—O(13)vii | 66.48 (5) | Cr(1)—O(4)—K(2)v | 98.82 (7) |
O(2)v—K(2)—O(14)vii | 67.82 (5) | Cr(2)—O(4)—K(2)v | 133.71 (8) |
O(3)—K(2)—O(4)v | 74.91 (6) | Cr(2)—O(5)—K(1) | 119.63 (8) |
O(3)—K(2)—O(5)vi | 73.98 (5) | Cr(2)—O(5)—K(1)ii | 113.93 (8) |
O(3)—K(2)—O(6)vi | 110.23 (5) | Cr(2)—O(5)—K(2)i | 108.75 (8) |
O(3)—K(2)—O(7) | 74.36 (5) | K(1)—O(5)—K(1)ii | 107.73 (6) |
O(3)—K(2)—O(9)vi | 124.26 (5) | K(1)—O(5)—K(2)i | 104.62 (6) |
O(3)—K(2)—O(13)vii | 167.72 (5) | K(1)ii—O(5)—K(2)i | 99.99 (5) |
O(3)—K(2)—O(14)vii | 140.05 (5) | Cr(2)—O(6)—K(1)iii | 146.48 (10) |
O(4)v—K(2)—O(5)vi | 90.22 (5) | Cr(2)—O(6)—K(2)i | 89.69 (8) |
O(4)v—K(2)—O(6)vi | 66.73 (5) | Cr(2)—O(6)—K(3)xiii | 102.13 (8) |
O(4)v—K(2)—O(7) | 99.45 (5) | K(1)iii—O(6)—K(2)i | 114.18 (6) |
O(4)v—K(2)—O(9)vi | 143.95 (5) | K(1)iii—O(6)—K(3)xiii | 93.47 (5) |
O(4)v—K(2)—O(13)vii | 93.91 (5) | K(2)i—O(6)—K(3)xiii | 106.60 (6) |
O(4)v—K(2)—O(14)vii | 122.45 (5) | Cr(2)—O(7)—K(2) | 120.27 (10) |
O(5)vi—K(2)—O(6)vi | 51.36 (5) | Cr(2)—O(7)—K(3)xiii | 95.83 (8) |
O(5)vi—K(2)—O(7) | 143.07 (6) | K(2)—O(7)—K(3)xiii | 95.70 (6) |
O(5)vi—K(2)—O(9)vi | 70.08 (5) | Cr(3)—O(8)—K(1)ii | 96.66 (7) |
O(5)vi—K(2)—O(13)vii | 101.46 (5) | Cr(3)—O(8)—K(3) | 132.71 (9) |
O(5)vi—K(2)—O(14)vii | 134.47 (5) | Cr(3)—O(8)—K(4)vii | 117.38 (9) |
O(6)vi—K(2)—O(7) | 162.49 (5) | K(1)ii—O(8)—K(3) | 92.44 (5) |
O(6)vi—K(2)—O(9)vi | 77.52 (5) | K(1)ii—O(8)—K(4)vii | 121.40 (6) |
O(6)vi—K(2)—O(13)vii | 59.61 (4) | K(3)—O(8)—K(4)vii | 96.06 (5) |
O(6)vi—K(2)—O(14)vii | 109.72 (5) | Cr(3)—O(9)—K(1)ii | 97.89 (7) |
O(7)—K(2)—O(9)vi | 114.55 (5) | Cr(3)—O(9)—K(2)i | 168.27 (10) |
O(7)—K(2)—O(13)vii | 113.19 (5) | Cr(3)—O(9)—K(4)xii | 101.45 (8) |
O(7)—K(2)—O(14)vii | 67.64 (5) | K(1)ii—O(9)—K(2)i | 89.99 (5) |
O(9)vi—K(2)—O(13)vii | 62.66 (5) | K(1)ii—O(9)—K(4)xii | 104.49 (6) |
O(9)vi—K(2)—O(14)vii | 65.04 (5) | K(2)i—O(9)—K(4)xii | 84.85 (5) |
O(13)vii—K(2)—O(14)vii | 50.70 (5) | Cr(3)—O(10)—K(3)xiii | 122.02 (9) |
O(2)iv—K(3)—O(6)viii | 69.60 (5) | Cr(3)—O(10)—K(4) | 124.82 (9) |
O(2)iv—K(3)—O(7)viii | 68.55 (5) | K(3)xiii—O(10)—K(4) | 100.79 (6) |
O(2)iv—K(3)—O(8) | 68.41 (5) | Cr(3)—O(11)—Cr(4) | 123.97 (8) |
O(2)iv—K(3)—O(10)viii | 138.19 (6) | Cr(3)—O(11)—K(4)xii | 96.85 (6) |
O(2)iv—K(3)—O(12) | 127.25 (6) | Cr(4)—O(11)—K(4)xii | 137.82 (8) |
O(2)iv—K(3)—O(12)ix | 71.75 (5) | Cr(4)—O(12)—K(3) | 131.20 (9) |
O(2)iv—K(3)—O(13)x | 131.37 (5) | Cr(4)—O(12)—K(3)ix | 96.32 (8) |
O(2)iv—K(3)—O(14)ix | 68.56 (5) | Cr(4)—O(12)—K(4)viii | 117.75 (9) |
O(6)viii—K(3)—O(7)viii | 52.22 (5) | K(3)—O(12)—K(3)ix | 113.38 (6) |
O(6)viii—K(3)—O(8) | 85.14 (5) | K(3)—O(12)—K(4)viii | 98.02 (5) |
O(6)viii—K(3)—O(10)viii | 113.49 (5) | K(3)ix—O(12)—K(4)viii | 95.00 (5) |
O(6)viii—K(3)—O(12) | 139.16 (5) | Cr(4)—O(13)—K(2)vii | 88.99 (8) |
O(6)viii—K(3)—O(12)ix | 141.16 (5) | Cr(4)—O(13)—K(3)x | 138.98 (10) |
O(6)viii—K(3)—O(13)x | 69.38 (5) | K(2)vii—O(13)—K(3)x | 106.93 (6) |
O(6)viii—K(3)—O(14)ix | 112.98 (5) | Cr(4)—O(14)—K(2)vii | 109.90 (8) |
O(7)viii—K(3)—O(8) | 127.44 (5) | Cr(4)—O(14)—K(3)ix | 101.07 (7) |
O(7)viii—K(3)—O(10)viii | 81.16 (5) | Cr(4)—O(14)—K(4) | 124.48 (8) |
O(7)viii—K(3)—O(12) | 160.50 (5) | K(2)vii—O(14)—K(3)ix | 104.82 (5) |
O(7)viii—K(3)—O(12)ix | 115.19 (5) | K(2)vii—O(14)—K(4) | 93.89 (5) |
O(7)viii—K(3)—O(13)x | 104.18 (6) | K(3)ix—O(14)—K(4) | 120.72 (6) |
Cr(1)—O(1)—K(1)—O(3)i | −71.97 (17) | Cr(4)—O(14)—K(4)—O(10) | −50.59 (10) |
Cr(1)—O(1)—K(1)—O(5) | −57.21 (10) | Cr(4)—O(14)—K(4)—O(11)xii | 16.85 (11) |
Cr(1)—O(1)—K(1)—O(5)ii | −131.32 (10) | Cr(4)—O(14)—K(4)—O(12)xiii | −58.86 (19) |
Cr(1)—O(1)—K(1)—O(6)iii | 23.57 (11) | K(1)—O(1)—Cr(1)—O(2) | −96.48 (10) |
Cr(1)—O(1)—K(1)—O(8)ii | 117.30 (9) | K(1)—O(1)—Cr(1)—O(3) | 141.49 (9) |
Cr(1)—O(1)—K(1)—O(9)ii | 149.13 (11) | K(1)—O(1)—Cr(1)—O(4) | 20.06 (11) |
Cr(1)—O(1)—K(2)iv—O(2)viii | −56.7 (2) | K(1)—O(1)—K(2)iv—O(2)viii | 161.19 (7) |
Cr(1)—O(1)—K(2)iv—O(3)iv | 39.68 (16) | K(1)—O(1)—K(2)iv—O(3)iv | −102.47 (6) |
Cr(1)—O(1)—K(2)iv—O(4)viii | 45.5 (2) | K(1)—O(1)—K(2)iv—O(4)viii | −96.64 (9) |
Cr(1)—O(1)—K(2)iv—O(5)ii | 117.16 (17) | K(1)—O(1)—K(2)iv—O(5)ii | −25.00 (5) |
Cr(1)—O(1)—K(2)iv—O(6)ii | 141.20 (15) | K(1)—O(1)—K(2)iv—O(6)ii | −0.96 (8) |
Cr(1)—O(1)—K(2)iv—O(7)iv | −39.03 (17) | K(1)—O(1)—K(2)iv—O(7)iv | 178.82 (6) |
Cr(1)—O(1)—K(2)iv—O(9)ii | −168.71 (19) | K(1)—O(1)—K(2)iv—O(9)ii | 49.14 (5) |
Cr(1)—O(1)—K(4)xvi—O(2) | −9.84 (7) | K(1)—O(1)—K(4)xvi—O(2) | 109.89 (8) |
Cr(1)—O(2)—K(2)v—O(3)v | 57.90 (9) | K(1)—O(5)—Cr(2)—O(4) | −11.38 (12) |
Cr(1)—O(2)—K(2)v—O(4) | 3.15 (7) | K(1)—O(5)—Cr(2)—O(6) | 108.02 (10) |
Cr(1)—O(2)—K(2)v—O(5)iii | −30.65 (13) | K(1)—O(5)—Cr(2)—O(7) | −132.09 (10) |
Cr(1)—O(2)—K(2)v—O(6)iii | −55.18 (8) | K(1)—O(5)—K(1)ii—O(1)ii | −82.11 (6) |
Cr(1)—O(2)—K(2)v—O(7)v | 121.53 (9) | K(1)—O(5)—K(1)ii—O(5)ii | 0.0000 |
Cr(1)—O(2)—K(2)v—O(9)iii | −132.63 (8) | K(1)—O(5)—K(1)ii—O(6)viii | 9.74 (16) |
Cr(1)—O(2)—K(3)iv—O(6)v | −39.9 (2) | K(1)—O(5)—K(1)ii—O(8) | 169.70 (5) |
Cr(1)—O(2)—K(3)iv—O(7)v | −96.1 (3) | K(1)—O(5)—K(1)ii—O(9) | −149.18 (7) |
Cr(1)—O(2)—K(3)iv—O(8)iv | 53.0 (2) | K(1)—O(5)—K(2)i—O(1)ii | 84.21 (6) |
Cr(1)—O(2)—K(3)iv—O(10)v | −142.7 (2) | K(1)—O(5)—K(2)i—O(2)iii | −89.70 (9) |
Cr(1)—O(2)—K(3)iv—O(12)iv | 97.1 (2) | K(1)—O(5)—K(2)i—O(4)iii | −62.32 (6) |
Cr(1)—O(2)—K(4)xvi—O(1) | 9.59 (6) | K(1)—O(5)—K(2)i—O(6) | −121.73 (8) |
Cr(1)—O(3)—K(2)—O(1)iv | 126.12 (13) | K(1)—O(5)—K(2)i—O(9) | 148.53 (7) |
Cr(1)—O(3)—K(2)—O(2)v | −13.03 (13) | K(1)—O(5)—K(2)i—O(13)xii | −156.35 (5) |
Cr(1)—O(3)—K(2)—O(4)v | −57.38 (12) | K(1)—O(5)—K(2)i—O(14)xii | 158.61 (6) |
Cr(1)—O(3)—K(2)—O(5)vi | −152.06 (13) | K(1)—O(5)ii—Cr(2)ii—O(4)ii | −118.09 (8) |
Cr(1)—O(3)—K(2)—O(6)vi | −115.01 (11) | K(1)—O(5)ii—Cr(2)ii—O(6)ii | 122.51 (9) |
Cr(1)—O(3)—K(2)—O(7) | 47.22 (11) | K(1)—O(5)ii—Cr(2)ii—O(7)ii | 2.62 (11) |
Cr(1)—O(3)—K(2)—O(9)vi | 156.57 (10) | K(1)—O(5)ii—K(1)ii—O(1)ii | 80.14 (6) |
Cr(1)—O(3)—K(2)—O(13)vii | −82.3 (3) | K(1)—O(5)ii—K(1)ii—O(5) | 0.0000 |
Cr(1)—O(3)—K(2)—O(14)vii | 65.54 (16) | K(1)—O(5)ii—K(1)ii—O(6)viii | −175.95 (7) |
Cr(1)—O(4)—Cr(2)—O(5) | −66.67 (14) | K(1)—O(5)ii—K(1)ii—O(8) | −126.0 (3) |
Cr(1)—O(4)—Cr(2)—O(6) | 174.32 (12) | K(1)—O(5)ii—K(1)ii—O(9) | 45.08 (9) |
Cr(1)—O(4)—Cr(2)—O(7) | 53.35 (15) | K(1)—O(6)iii—Cr(2)iii—O(4)iii | 8.6 (2) |
Cr(1)—O(4)—K(2)v—O(2) | −2.85 (6) | K(1)—O(6)iii—Cr(2)iii—O(5)iii | 127.60 (18) |
Cr(1)—O(4)—K(2)v—O(3)v | −130.05 (8) | K(1)—O(6)iii—Cr(2)iii—O(7)iii | −112.76 (18) |
Cr(1)—O(4)—K(2)v—O(5)iii | 156.62 (7) | K(1)—O(8)ii—Cr(3)ii—O(9)ii | 4.82 (10) |
Cr(1)—O(4)—K(2)v—O(6)iii | 109.57 (8) | K(1)—O(8)ii—Cr(3)ii—O(10)ii | 127.24 (8) |
Cr(1)—O(4)—K(2)v—O(7)v | −59.19 (8) | K(1)—O(8)ii—Cr(3)ii—O(11)ii | −111.21 (7) |
Cr(1)—O(4)—K(2)v—O(9)iii | 101.62 (9) | K(1)—O(8)ii—K(3)ii—O(2)i | −71.19 (6) |
Cr(2)—O(4)—Cr(1)—O(1) | 58.87 (15) | K(1)—O(8)ii—K(3)ii—O(6)iii | −1.23 (5) |
Cr(2)—O(4)—Cr(1)—O(2) | 176.85 (12) | K(1)—O(8)ii—K(3)ii—O(7)iii | −34.14 (8) |
Cr(2)—O(4)—Cr(1)—O(3) | −63.40 (15) | K(1)—O(8)ii—K(3)ii—O(10)iii | 130.35 (10) |
Cr(2)—O(4)—K(2)v—O(2) | −174.35 (15) | K(1)—O(8)ii—K(3)ii—O(12)ii | 144.45 (6) |
Cr(2)—O(4)—K(2)v—O(3)v | 58.45 (12) | K(1)—O(9)ii—Cr(3)ii—O(8)ii | −4.88 (10) |
Cr(2)—O(4)—K(2)v—O(5)iii | −14.88 (12) | K(1)—O(9)ii—Cr(3)ii—O(10)ii | −126.52 (8) |
Cr(2)—O(4)—K(2)v—O(6)iii | −61.93 (11) | K(1)—O(9)ii—Cr(3)ii—O(11)ii | 112.82 (7) |
Cr(2)—O(4)—K(2)v—O(7)v | 129.31 (12) | K(2)—O(1)iv—Cr(1)iv—O(2)iv | −125.76 (16) |
Cr(2)—O(4)—K(2)v—O(9)iii | −69.88 (15) | K(2)—O(1)iv—Cr(1)iv—O(3)iv | −3.7 (2) |
Cr(2)—O(5)—K(1)—O(1) | 52.06 (10) | K(2)—O(1)iv—Cr(1)iv—O(4)iv | 117.70 (16) |
Cr(2)—O(5)—K(1)—O(3)i | −134.38 (11) | K(2)—O(1)iv—K(1)iv—O(3)xvii | −84.84 (14) |
Cr(2)—O(5)—K(1)—O(5)ii | 132.20 (13) | K(2)—O(1)iv—K(1)iv—O(5)vi | −25.48 (5) |
Cr(2)—O(5)—K(1)—O(6)iii | −51.85 (10) | K(2)—O(1)iv—K(1)iv—O(5)iv | −99.59 (6) |
Cr(2)—O(5)—K(1)—O(8)ii | −101.8 (3) | K(2)—O(1)iv—K(1)iv—O(6)xviii | 179.62 (5) |
Cr(2)—O(5)—K(1)—O(9)ii | 87.12 (12) | K(2)—O(1)iv—K(1)iv—O(8)vi | 85.89 (6) |
Cr(2)—O(5)—K(1)ii—O(1)ii | 142.68 (9) | K(2)—O(1)iv—K(1)iv—O(9)vi | 54.06 (5) |
Cr(2)—O(5)—K(1)ii—O(5)ii | −135.21 (12) | K(2)—O(2)v—Cr(1)v—O(1)v | −114.54 (8) |
Cr(2)—O(5)—K(1)ii—O(6)viii | −125.48 (13) | K(2)—O(2)v—Cr(1)v—O(3)v | 123.31 (9) |
Cr(2)—O(5)—K(1)ii—O(8) | 34.49 (10) | K(2)—O(2)v—Cr(1)v—O(4)v | 4.35 (9) |
Cr(2)—O(5)—K(1)ii—O(9) | 75.61 (9) | K(2)—O(3)—Cr(1)—O(1) | −130.64 (11) |
Cr(2)—O(5)—K(2)i—O(1)ii | −146.88 (9) | K(2)—O(3)—Cr(1)—O(2) | 108.40 (12) |
Cr(2)—O(5)—K(2)i—O(2)iii | 39.21 (13) | K(2)—O(3)—Cr(1)—O(4) | −8.76 (14) |
Cr(2)—O(5)—K(2)i—O(4)iii | 66.59 (9) | K(2)—O(4)v—Cr(1)v—O(1)v | 113.45 (8) |
Cr(2)—O(5)—K(2)i—O(6) | 7.18 (7) | K(2)—O(4)v—Cr(1)v—O(2)v | −4.53 (10) |
Cr(2)—O(5)—K(2)i—O(9) | −82.56 (9) | K(2)—O(4)v—Cr(1)v—O(3)v | −124.28 (9) |
Cr(2)—O(5)—K(2)i—O(13)xii | −27.44 (9) | K(2)—O(4)v—Cr(2)v—O(5)v | −102.80 (12) |
Cr(2)—O(5)—K(2)i—O(14)xii | −72.49 (11) | K(2)—O(4)v—Cr(2)v—O(6)v | 16.21 (15) |
Cr(2)—O(6)—K(1)iii—O(1)iii | 131.21 (18) | K(2)—O(4)v—Cr(2)v—O(7)v | 137.17 (12) |
Cr(2)—O(6)—K(1)iii—O(5)iii | 54.19 (19) | K(2)—O(7)—Cr(2)—O(4) | 23.68 (13) |
Cr(2)—O(6)—K(2)i—O(1)ii | 23.73 (10) | K(2)—O(7)—Cr(2)—O(5) | 143.43 (9) |
Cr(2)—O(6)—K(2)i—O(2)iii | −167.25 (7) | K(2)—O(7)—Cr(2)—O(6) | −97.18 (11) |
Cr(2)—O(6)—K(2)i—O(4)iii | −117.26 (8) | K(2)—O(7)—K(3)xiii—O(2)v | 39.12 (5) |
Cr(2)—O(6)—K(2)i—O(5) | −6.83 (6) | K(2)—O(7)—K(3)xiii—O(6) | 119.36 (8) |
Cr(2)—O(6)—K(2)i—O(9) | 67.52 (7) | K(2)—O(7)—K(3)xiii—O(10) | −111.52 (6) |
Cr(2)—O(6)—K(2)i—O(13)xii | 132.97 (9) | K(2)—O(13)vii—Cr(4)vii—O(11)vii | 123.32 (7) |
Cr(2)—O(6)—K(2)i—O(14)xii | 124.95 (7) | K(2)—O(13)vii—Cr(4)vii—O(12)vii | −115.77 (8) |
Cr(2)—O(6)—K(3)xiii—O(2)v | 80.10 (9) | K(2)—O(13)vii—Cr(4)vii—O(14)vii | 4.03 (9) |
Cr(2)—O(6)—K(3)xiii—O(7) | 1.95 (7) | K(2)—O(13)vii—K(3)xix—O(2)xx | 66.63 (9) |
Cr(2)—O(6)—K(3)xiii—O(10) | −54.76 (10) | K(2)—O(13)vii—K(3)xix—O(6)vi | 32.51 (5) |
Cr(2)—O(7)—K(2)—O(1)iv | −128.55 (12) | K(2)—O(13)vii—K(3)xix—O(7)vi | −7.11 (7) |
Cr(2)—O(7)—K(2)—O(2)v | 63.05 (11) | K(2)—O(13)vii—K(3)xix—O(10)vi | −86.02 (6) |
Cr(2)—O(7)—K(2)—O(3) | −55.75 (11) | K(2)—O(14)vii—Cr(4)vii—O(11)vii | −125.07 (7) |
Cr(2)—O(7)—K(2)—O(4)v | 15.55 (12) | K(2)—O(14)vii—Cr(4)vii—O(12)vii | 115.92 (8) |
Cr(2)—O(7)—K(2)—O(5)vi | −87.63 (14) | K(2)—O(14)vii—Cr(4)vii—O(13)vii | −5.13 (11) |
Cr(2)—O(7)—K(2)—O(6)vi | 52.1 (2) | K(2)—O(14)vii—K(3)xiii—O(2)v | −35.26 (6) |
Cr(2)—O(7)—K(2)—O(9)vi | −176.73 (10) | K(2)—O(14)vii—K(3)xiii—O(6) | 19.76 (7) |
Cr(2)—O(7)—K(2)—O(13)vii | 113.97 (11) | K(2)—O(14)vii—K(3)xiii—O(7) | 40.33 (5) |
Cr(2)—O(7)—K(2)—O(14)vii | 136.85 (12) | K(2)—O(14)vii—K(3)xiii—O(10) | 128.52 (6) |
Cr(2)—O(7)—K(3)xiii—O(2)v | −82.17 (8) | K(2)—O(14)vii—K(4)vii—O(8) | −101.24 (5) |
Cr(2)—O(7)—K(3)xiii—O(6) | −1.92 (6) | K(2)—O(14)vii—K(4)vii—O(9)vi | 54.34 (5) |
Cr(2)—O(7)—K(3)xiii—O(10) | 127.19 (9) | K(2)—O(14)vii—K(4)vii—O(10)vii | 168.01 (6) |
Cr(3)—O(8)—K(1)ii—O(1)ii | −32.06 (9) | K(2)—O(14)vii—K(4)vii—O(11)vi | 100.58 (5) |
Cr(3)—O(8)—K(1)ii—O(5) | 53.34 (9) | K(2)—O(14)vii—K(4)vii—O(12)ix | 176.29 (12) |
Cr(3)—O(8)—K(1)ii—O(5)ii | 175.7 (2) | K(3)—O(2)iv—Cr(1)iv—O(1)iv | 110.7 (2) |
Cr(3)—O(8)—K(1)ii—O(6)viii | −134.83 (8) | K(3)—O(2)iv—Cr(1)iv—O(3)iv | −11.4 (3) |
Cr(3)—O(8)—K(1)ii—O(9) | 3.16 (7) | K(3)—O(2)iv—Cr(1)iv—O(4)iv | −130.4 (2) |
Cr(3)—O(8)—K(3)—O(2)iv | 172.57 (14) | K(3)—O(2)iv—K(2)viii—O(1)xxi | 22.53 (11) |
Cr(3)—O(8)—K(3)—O(6)viii | 102.61 (12) | K(3)—O(2)iv—K(2)viii—O(13)ix | −88.15 (6) |
Cr(3)—O(8)—K(3)—O(7)viii | 135.53 (11) | K(3)—O(2)iv—K(2)viii—O(14)ix | −32.80 (5) |
Cr(3)—O(8)—K(3)—O(10)viii | −29.0 (2) | K(3)—O(8)—Cr(3)—O(9) | −104.39 (13) |
Cr(3)—O(8)—K(3)—O(12) | −43.06 (12) | K(3)—O(8)—Cr(3)—O(10) | 133.20 (12) |
Cr(3)—O(8)—K(3)—O(12)ix | −112.29 (13) | K(3)—O(8)—Cr(3)—O(11) | 11.64 (14) |
Cr(3)—O(8)—K(3)—O(13)x | 32.84 (12) | K(3)—O(8)—K(1)ii—O(1)ii | 101.45 (5) |
Cr(3)—O(8)—K(3)—O(14)ix | −143.18 (11) | K(3)—O(8)—K(1)ii—O(5) | −173.15 (5) |
Cr(3)—O(8)—K(4)vii—O(9)vi | −90.04 (13) | K(3)—O(8)—K(1)ii—O(5)ii | −50.8 (3) |
Cr(3)—O(8)—K(4)vii—O(10)vii | 38.36 (10) | K(3)—O(8)—K(1)ii—O(6)viii | −1.32 (5) |
Cr(3)—O(8)—K(4)vii—O(11)vi | 86.13 (15) | K(3)—O(8)—K(1)ii—O(9) | 136.68 (7) |
Cr(3)—O(8)—K(4)vii—O(12)ix | 119.27 (10) | K(3)—O(8)—K(4)vii—O(9)vi | 124.55 (10) |
Cr(3)—O(8)—K(4)vii—O(14)vii | −37.59 (10) | K(3)—O(8)—K(4)vii—O(10)vii | −107.05 (6) |
Cr(3)—O(9)—K(1)ii—O(1)ii | 140.51 (10) | K(3)—O(8)—K(4)vii—O(11)vi | −59.28 (13) |
Cr(3)—O(9)—K(1)ii—O(5) | −136.83 (9) | K(3)—O(8)—K(4)vii—O(12)ix | −26.14 (5) |
Cr(3)—O(9)—K(1)ii—O(5)ii | 178.97 (7) | K(3)—O(8)—K(4)vii—O(14)vii | 177.00 (5) |
Cr(3)—O(9)—K(1)ii—O(6)viii | 53.97 (11) | K(3)—O(10)viii—Cr(3)viii—O(8)viii | 96.76 (12) |
Cr(3)—O(9)—K(1)ii—O(8) | −3.19 (7) | K(3)—O(10)viii—Cr(3)viii—O(9)viii | −24.46 (14) |
Cr(3)—O(9)—K(2)i—O(1)ii | −176.8 (5) | K(3)—O(10)viii—Cr(3)viii—O(11)viii | −142.62 (9) |
Cr(3)—O(9)—K(2)i—O(2)iii | −41.5 (5) | K(3)—O(10)viii—K(4)viii—O(8)ix | −75.31 (6) |
Cr(3)—O(9)—K(2)i—O(4)iii | 36.9 (5) | K(3)—O(10)viii—K(4)viii—O(9)x | 127.49 (6) |
Cr(3)—O(9)—K(2)i—O(5) | 97.5 (4) | K(3)—O(10)viii—K(4)viii—O(11)x | 84.31 (6) |
Cr(3)—O(9)—K(2)i—O(6) | 44.4 (4) | K(3)—O(10)viii—K(4)viii—O(12) | 4.50 (6) |
Cr(3)—O(9)—K(2)i—O(13)xii | −17.6 (4) | K(3)—O(12)—Cr(4)—O(11) | −5.33 (14) |
Cr(3)—O(9)—K(2)i—O(14)xii | −74.6 (4) | K(3)—O(12)—Cr(4)—O(13) | 115.53 (12) |
Cr(3)—O(9)—K(4)xii—O(8)i | −177.70 (8) | K(3)—O(12)—Cr(4)—O(14) | −123.61 (11) |
Cr(3)—O(9)—K(4)xii—O(10)xii | 56.42 (9) | K(3)—O(12)—K(3)ix—O(8)ix | −75.66 (6) |
Cr(3)—O(9)—K(4)xii—O(11) | 4.37 (6) | K(3)—O(12)—K(3)ix—O(12)ix | 0.0000 |
Cr(3)—O(9)—K(4)xii—O(12)x | −33.28 (10) | K(3)—O(12)—K(3)ix—O(13)vi | −13.02 (11) |
Cr(3)—O(9)—K(4)xii—O(14)xii | 123.17 (9) | K(3)—O(12)—K(3)ix—O(14) | 136.82 (8) |
Cr(3)—O(10)—K(3)xiii—O(2)v | −85.16 (14) | K(3)—O(12)—K(4)viii—O(8)ix | 89.79 (6) |
Cr(3)—O(10)—K(3)xiii—O(6) | 0.00 (14) | K(3)—O(12)—K(4)viii—O(9)x | −106.59 (6) |
Cr(3)—O(10)—K(3)xiii—O(7) | −41.96 (11) | K(3)—O(12)—K(4)viii—O(11)x | −75.86 (5) |
Cr(3)—O(10)—K(4)—O(1)xi | 31.4 (3) | K(3)—O(12)ix—Cr(4)ix—O(11)ix | −123.54 (6) |
Cr(3)—O(10)—K(4)—O(2)xi | −172.71 (9) | K(3)—O(12)ix—Cr(4)ix—O(13)ix | 115.60 (9) |
Cr(3)—O(10)—K(4)—O(8)vii | 142.49 (12) | K(3)—O(12)ix—Cr(4)ix—O(14)ix | −5.25 (9) |
Cr(3)—O(10)—K(4)—O(9)xii | −14.71 (13) | K(3)—O(12)ix—K(3)ix—O(8)ix | 83.66 (6) |
Cr(3)—O(10)—K(4)—O(11)xii | −57.89 (12) | K(3)—O(12)ix—K(3)ix—O(12) | 0.0000 |
Cr(3)—O(10)—K(4)—O(12)xiii | −137.70 (13) | K(3)—O(12)ix—K(3)ix—O(13)vi | 171.40 (7) |
Cr(3)—O(10)—K(4)—O(14) | 45.56 (12) | K(3)—O(12)ix—K(3)ix—O(14) | −35.48 (7) |
Cr(3)—O(11)—Cr(4)—O(12) | −59.66 (13) | K(3)—O(13)x—Cr(4)x—O(11)x | 8.26 (19) |
Cr(3)—O(11)—Cr(4)—O(13) | 178.91 (12) | K(3)—O(13)x—Cr(4)x—O(12)x | 129.17 (15) |
Cr(3)—O(11)—Cr(4)—O(14) | 58.59 (13) | K(3)—O(13)x—Cr(4)x—O(14)x | −111.02 (16) |
Cr(3)—O(11)—K(4)xii—O(8)i | 178.32 (9) | K(3)—O(14)ix—Cr(4)ix—O(11)ix | 124.56 (7) |
Cr(3)—O(11)—K(4)xii—O(9) | −3.92 (6) | K(3)—O(14)ix—Cr(4)ix—O(12)ix | 5.55 (9) |
Cr(3)—O(11)—K(4)xii—O(10)xii | −129.90 (8) | K(3)—O(14)ix—Cr(4)ix—O(13)ix | −115.50 (9) |
Cr(3)—O(11)—K(4)xii—O(12)x | 144.83 (7) | K(3)—O(14)ix—K(2)viii—O(1)xxi | −115.54 (6) |
Cr(3)—O(11)—K(4)xii—O(14)xii | −57.98 (7) | K(3)—O(14)ix—K(2)viii—O(13)ix | 110.90 (7) |
Cr(4)—O(11)—Cr(3)—O(8) | 57.10 (13) | K(3)—O(14)ix—K(4)ix—O(8)viii | 8.56 (8) |
Cr(4)—O(11)—Cr(3)—O(9) | 174.90 (11) | K(3)—O(14)ix—K(4)ix—O(9)xviii | 164.14 (8) |
Cr(4)—O(11)—Cr(3)—O(10) | −64.05 (14) | K(3)—O(14)ix—K(4)ix—O(10)ix | −82.19 (7) |
Cr(4)—O(11)—K(4)xii—O(8)i | 12.2 (2) | K(3)—O(14)ix—K(4)ix—O(11)xviii | −149.63 (6) |
Cr(4)—O(11)—K(4)xii—O(9) | −170.03 (14) | K(3)—O(14)ix—K(4)ix—O(12)xxii | −73.92 (15) |
Cr(4)—O(11)—K(4)xii—O(10)xii | 63.98 (12) | K(4)—O(8)vii—Cr(3)vii—O(9)vii | −125.81 (10) |
Cr(4)—O(11)—K(4)xii—O(12)x | −21.29 (12) | K(4)—O(8)vii—Cr(3)vii—O(10)vii | −3.40 (12) |
Cr(4)—O(11)—K(4)xii—O(14)xii | 135.91 (12) | K(4)—O(8)vii—Cr(3)vii—O(11)vii | 118.16 (9) |
Cr(4)—O(12)—K(3)—O(2)iv | 81.76 (14) | K(4)—O(8)vii—K(3)vii—O(6)xxiii | 120.71 (6) |
Cr(4)—O(12)—K(3)—O(6)viii | −20.36 (17) | K(4)—O(8)vii—K(3)vii—O(7)xxiii | 87.79 (7) |
Cr(4)—O(12)—K(3)—O(7)viii | −137.77 (13) | K(4)—O(8)vii—K(3)vii—O(10)xxiii | −107.72 (10) |
Cr(4)—O(12)—K(3)—O(8) | 38.87 (12) | K(4)—O(8)vii—K(3)vii—O(12)xiii | −24.40 (5) |
Cr(4)—O(12)—K(3)—O(10)viii | −134.13 (13) | K(4)—O(8)vii—K(3)vii—O(12)vii | −93.62 (6) |
Cr(4)—O(12)—K(3)—O(12)ix | 122.53 (15) | K(4)—O(8)vii—K(3)vii—O(13)xix | −169.53 (6) |
Cr(4)—O(12)—K(3)—O(13)x | −48.88 (12) | K(4)—O(8)vii—K(3)vii—O(14)xiii | 6.50 (8) |
Cr(4)—O(12)—K(3)—O(14)ix | 158.01 (11) | K(4)—O(9)xii—Cr(3)xii—O(8)xii | −111.49 (8) |
Cr(4)—O(12)—K(3)ix—O(8)ix | 144.00 (8) | K(4)—O(9)xii—Cr(3)xii—O(10)xii | 126.87 (9) |
Cr(4)—O(12)—K(3)ix—O(12)ix | −140.34 (11) | K(4)—O(9)xii—Cr(3)xii—O(11)xii | 6.21 (9) |
Cr(4)—O(12)—K(3)ix—O(13)vi | −153.36 (7) | K(4)—O(10)—Cr(3)—O(8) | −128.48 (11) |
Cr(4)—O(12)—K(3)ix—O(14) | −3.52 (6) | K(4)—O(10)—Cr(3)—O(9) | 110.30 (11) |
Cr(4)—O(12)—K(4)viii—O(8)ix | −124.54 (10) | K(4)—O(10)—Cr(3)—O(11) | −7.86 (14) |
Cr(4)—O(12)—K(4)viii—O(9)x | 39.08 (12) | K(4)—O(10)—K(3)xiii—O(2)v | 131.24 (7) |
Cr(4)—O(12)—K(4)viii—O(11)x | 69.81 (10) | K(4)—O(10)—K(3)xiii—O(6) | −143.60 (5) |
Cr(4)—O(13)—K(2)vii—O(3)vii | −150.9 (2) | K(4)—O(10)—K(3)xiii—O(7) | 174.44 (6) |
Cr(4)—O(13)—K(2)vii—O(5)xii | 142.13 (8) | K(4)—O(11)xii—Cr(3)xii—O(8)xii | 111.69 (8) |
Cr(4)—O(13)—K(2)vii—O(6)xii | 173.09 (10) | K(4)—O(11)xii—Cr(3)xii—O(9)xii | −6.10 (9) |
Cr(4)—O(13)—K(2)vii—O(7)vii | −24.82 (9) | K(4)—O(11)xii—Cr(3)xii—O(10)xii | −127.16 (8) |
Cr(4)—O(13)—K(2)vii—O(9)xii | 81.88 (8) | K(4)—O(11)xii—Cr(4)xii—O(12)xii | −103.64 (12) |
Cr(4)—O(13)—K(2)vii—O(14) | 2.87 (6) | K(4)—O(11)xii—Cr(4)xii—O(13)xii | 17.79 (15) |
Cr(4)—O(13)—K(3)x—O(8)x | 131.36 (17) | K(4)—O(11)xii—Cr(4)xii—O(14)xii | 138.11 (11) |
Cr(4)—O(13)—K(3)x—O(12)i | 70.6 (2) | K(4)—O(14)—Cr(4)—O(11) | 15.43 (12) |
Cr(4)—O(13)—K(3)x—O(12)x | 58.19 (16) | K(4)—O(14)—Cr(4)—O(12) | 134.44 (10) |
Cr(4)—O(13)—K(3)x—O(14)i | −40.9 (3) | K(4)—O(14)—Cr(4)—O(13) | −104.51 (11) |
Cr(4)—O(14)—K(2)vii—O(3)vii | 168.58 (7) | K(4)—O(14)—K(2)vii—O(3)vii | −62.51 (9) |
Cr(4)—O(14)—K(2)vii—O(5)xii | −66.68 (11) | K(4)—O(14)—K(2)vii—O(5)xii | 62.23 (8) |
Cr(4)—O(14)—K(2)vii—O(6)xii | −11.97 (9) | K(4)—O(14)—K(2)vii—O(6)xii | 116.94 (5) |
Cr(4)—O(14)—K(2)vii—O(7)vii | 149.47 (10) | K(4)—O(14)—K(2)vii—O(7)vii | −81.61 (6) |
Cr(4)—O(14)—K(2)vii—O(9)xii | −77.14 (8) | K(4)—O(14)—K(2)vii—O(9)xii | 51.78 (5) |
Cr(4)—O(14)—K(2)vii—O(13) | −3.02 (6) | K(4)—O(14)—K(2)vii—O(13) | 125.89 (7) |
Cr(4)—O(14)—K(3)ix—O(8)ix | −34.79 (10) | K(4)—O(14)—K(3)ix—O(8)ix | −176.73 (6) |
Cr(4)—O(14)—K(3)ix—O(12) | 3.57 (6) | K(4)—O(14)—K(3)ix—O(12) | −138.38 (9) |
Cr(4)—O(14)—K(3)ix—O(12)ix | 44.85 (9) | K(4)—O(14)—K(3)ix—O(12)ix | −97.09 (7) |
Cr(4)—O(14)—K(3)ix—O(13)vi | 136.14 (11) | K(4)—O(14)—K(3)ix—O(13)vi | −5.81 (17) |
Cr(4)—O(14)—K(4)—O(1)xi | 124.98 (10) | O(5)—K(1)—O(5)ii—K(1)ii | 0.0000 |
Cr(4)—O(14)—K(4)—O(2)xi | 156.18 (8) | O(5)—K(1)ii—O(5)ii—K(1) | 0.0000 |
Cr(4)—O(14)—K(4)—O(8)vii | −141.34 (10) | O(12)—K(3)—O(12)ix—K(3)ix | 0.0000 |
Cr(4)—O(14)—K(4)—O(9)xii | 63.08 (10) | O(12)—K(3)ix—O(12)ix—K(3) | 0.0000 |
Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x+2, −y+2, −z+1; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+2, −z+1; (vi) x−1, y, z; (vii) −x+1, −y+1, −z; (viii) x, y−1, z; (ix) −x+1, −y, −z; (x) −x+2, −y, −z; (xi) x, y, z−1; (xii) −x+2, −y+1, −z; (xiii) x, y+1, z; (xiv) x, y−1, z−1; (xv) x, y+1, z+1; (xvi) x, y, z+1; (xvii) −x, −y+1, −z+1; (xviii) x−1, y−1, z; (xix) x−1, y+1, z; (xx) −x, −y+2, −z+1; (xxi) −x+1, −y, −z+1; (xxii) −x+1, −y−1, −z; (xxiii) −x+1, −y+2, −z. |
2KCr2O7 | Z = 4 |
Mr = 294.18 | F(000) = 568.00 |
Triclinic, P1 | Dx = 2.691 Mg m−3 Dm = 2.676 Mg m−3 Dm measured by ? |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.3837 (8) Å | Cell parameters from 25 reflections |
b = 7.4622 (6) Å | θ = 14.0–14.7° |
c = 13.3949 (12) Å | µ = 4.13 mm−1 |
α = 96.204 (7)° | T = 296 K |
β = 98.046 (8)° | Block, intense-orange |
γ = 90.943 (8)° | 0.25 × 0.20 × 0.15 mm |
V = 726.12 (12) Å3 |
Nonius CAD-4 serial deiffractometer | 2253 reflections with I > 1.00σ(I) |
Radiation source: sealed X-ray tube | Rint = 0.020 |
Graphite monochromator | θmax = 25.0°, θmin = 1.5° |
ω–2θ scans | h = 0→8 |
Absorption correction: part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983) | k = −8→8 |
Tmin = 0.386, Tmax = 0.538 | l = −15→15 |
2759 measured reflections | 3 standard reflections every 300 reflections |
2544 independent reflections | intensity decay: 0.0% |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 4Fo2/[σ2(I) + (0.020I)2] |
R[F2 > 2σ(F2)] = 0.029 | (Δ/σ)max = 0.008 |
wR(F2) = 0.042 | Δρmax = 0.61 e Å−3 |
S = 1.86 | Δρmin = −0.45 e Å−3 |
2544 reflections | Extinction correction: Zachariasen (1967), equ(3) Acta Cryst.(1968) A24, p213. |
200 parameters | Extinction coefficient: 3.6 x 10-7 |
0 restraints |
2KCr2O7 | γ = 90.943 (8)° |
Mr = 294.18 | V = 726.12 (12) Å3 |
Triclinic, P1 | Z = 4 |
a = 7.3837 (8) Å | Mo Kα radiation |
b = 7.4622 (6) Å | µ = 4.13 mm−1 |
c = 13.3949 (12) Å | T = 296 K |
α = 96.204 (7)° | 0.25 × 0.20 × 0.15 mm |
β = 98.046 (8)° |
Nonius CAD-4 serial deiffractometer | 2253 reflections with I > 1.00σ(I) |
Absorption correction: part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983) | Rint = 0.020 |
Tmin = 0.386, Tmax = 0.538 | 3 standard reflections every 300 reflections |
2759 measured reflections | intensity decay: 0.0% |
2544 independent reflections |
R[F2 > 2σ(F2)] = 0.029 | 200 parameters |
wR(F2) = 0.042 | 0 restraints |
S = 1.86 | Δρmax = 0.61 e Å−3 |
2544 reflections | Δρmin = −0.45 e Å−3 |
x | y | z | Uiso*/Ueq | ||
Cr(1) | 0.59177 (7) | 0.76886 (7) | 0.60724 (4) | 0.01927 (15) | |
Cr(2) | 0.79290 (7) | 0.80680 (7) | 0.41370 (4) | 0.01877 (15) | |
Cr(3) | 0.81703 (7) | 0.42577 (7) | 0.11362 (4) | 0.01890 (15) | |
Cr(4) | 0.81338 (7) | 0.15247 (7) | −0.08318 (4) | 0.01837 (15) | |
K(1) | 1.10346 (12) | 0.66920 (11) | 0.64034 (6) | 0.0309 (2) | |
K(2) | 0.25016 (11) | 0.76715 (10) | 0.34962 (6) | 0.0289 (2) | |
K(3) | 0.66245 (10) | −0.08530 (10) | 0.15847 (6) | 0.0247 (2) | |
K(4) | 0.69492 (12) | 0.65228 (11) | −0.13585 (6) | 0.0316 (2) | |
O(1) | 0.7196 (4) | 0.6125 (4) | 0.6490 (2) | 0.0343 (8) | |
O(2) | 0.5547 (4) | 0.9100 (4) | 0.7017 (2) | 0.0351 (8) | |
O(3) | 0.4024 (4) | 0.6852 (4) | 0.5451 (2) | 0.0359 (8) | |
O(4) | 0.7076 (4) | 0.8928 (3) | 0.52682 (19) | 0.0301 (7) | |
O(5) | 0.9591 (3) | 0.6753 (3) | 0.44298 (19) | 0.0289 (7) | |
O(6) | 0.8688 (4) | 0.9716 (3) | 0.3608 (2) | 0.0325 (7) | |
O(7) | 0.6344 (4) | 0.6951 (4) | 0.3365 (2) | 0.0358 (8) | |
O(8) | 0.6890 (4) | 0.2929 (3) | 0.1638 (2) | 0.0300 (7) | |
O(9) | 0.9756 (4) | 0.5180 (4) | 0.20002 (18) | 0.0302 (7) | |
O(10) | 0.6949 (4) | 0.5755 (4) | 0.0612 (2) | 0.0340 (7) | |
O(11) | 0.9293 (3) | 0.2959 (3) | 0.02274 (18) | 0.0242 (6) | |
O(12) | 0.6919 (4) | −0.0003 (3) | −0.04335 (19) | 0.0293 (7) | |
O(13) | 0.9604 (4) | 0.0612 (4) | −0.1486 (2) | 0.0363 (8) | |
O(14) | 0.6774 (3) | 0.2736 (3) | −0.15180 (19) | 0.0274 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr(1) | 0.0186 (3) | 0.0208 (3) | 0.0189 (3) | 0.0025 (2) | 0.0038 (2) | 0.0025 (2) |
Cr(2) | 0.0179 (3) | 0.0206 (3) | 0.0188 (3) | 0.0021 (2) | 0.0039 (2) | 0.0048 (2) |
Cr(3) | 0.0187 (3) | 0.0184 (3) | 0.0188 (3) | −0.0013 (2) | 0.0003 (2) | 0.0019 (2) |
Cr(4) | 0.0167 (3) | 0.0183 (3) | 0.0200 (3) | 0.0003 (2) | 0.0030 (2) | 0.0010 (2) |
K(1) | 0.0371 (5) | 0.0311 (5) | 0.0243 (4) | −0.0073 (4) | 0.0021 (3) | 0.0055 (3) |
K(2) | 0.0322 (5) | 0.0268 (4) | 0.0291 (4) | −0.0030 (3) | 0.0099 (3) | 0.0020 (3) |
K(3) | 0.0234 (4) | 0.0244 (4) | 0.0259 (4) | −0.0003 (3) | 0.0036 (3) | 0.0008 (3) |
K(4) | 0.0374 (5) | 0.0296 (4) | 0.0278 (4) | 0.0103 (4) | 0.0039 (4) | 0.0022 (3) |
O(1) | 0.0320 (14) | 0.0309 (14) | 0.040 (2) | 0.0097 (12) | −0.0003 (12) | 0.0100 (12) |
O(2) | 0.042 (2) | 0.0346 (15) | 0.0304 (15) | 0.0037 (12) | 0.0152 (12) | −0.0026 (12) |
O(3) | 0.0274 (14) | 0.045 (2) | 0.0334 (15) | −0.0046 (12) | −0.0022 (12) | 0.0064 (13) |
O(4) | 0.0368 (15) | 0.0248 (13) | 0.0320 (14) | 0.0016 (11) | 0.0165 (12) | 0.0028 (11) |
O(5) | 0.0276 (13) | 0.0316 (14) | 0.0285 (14) | 0.0115 (11) | 0.0034 (11) | 0.0064 (11) |
O(6) | 0.041 (2) | 0.0273 (14) | 0.0318 (14) | −0.0026 (11) | 0.0097 (12) | 0.0098 (11) |
O(7) | 0.0287 (14) | 0.043 (2) | 0.0331 (15) | −0.0042 (12) | −0.0020 (12) | 0.0007 (12) |
O(8) | 0.0298 (14) | 0.0291 (14) | 0.032 (2) | −0.0064 (11) | 0.0081 (11) | 0.0036 (11) |
O(9) | 0.030 (2) | 0.0358 (14) | 0.0221 (13) | −0.0102 (11) | 0.0000 (11) | −0.0012 (11) |
O(10) | 0.0416 (16) | 0.0291 (14) | 0.0313 (15) | 0.0130 (12) | 0.0024 (12) | 0.0048 (11) |
O(11) | 0.0182 (12) | 0.027 (2) | 0.026 (2) | −0.0010 (10) | −0.0002 (10) | −0.0014 (10) |
O(12) | 0.036 (2) | 0.0245 (13) | 0.0276 (14) | −0.0072 (11) | 0.0047 (11) | 0.0036 (11) |
O(13) | 0.0291 (15) | 0.0411 (16) | 0.039 (2) | 0.0070 (12) | 0.0130 (12) | −0.0064 (13) |
O(14) | 0.0263 (13) | 0.0250 (13) | 0.030 (2) | 0.0020 (10) | −0.0017 (11) | 0.0047 (10) |
Cr(1)—O(1) | 1.611 (2) | K(2)—O(3) | 2.835 (3) |
Cr(1)—O(2) | 1.613 (3) | K(2)—O(4)v | 2.863 (3) |
Cr(1)—O(3) | 1.604 (3) | K(2)—O(5)vi | 2.746 (3) |
Cr(1)—O(4) | 1.788 (3) | K(2)—O(6)vi | 3.239 (3) |
Cr(2)—O(4) | 1.782 (2) | K(2)—O(7) | 2.922 (3) |
Cr(2)—O(5) | 1.615 (2) | K(2)—O(9)vi | 3.085 (3) |
Cr(2)—O(6) | 1.614 (3) | K(2)—O(13)vii | 3.308 (3) |
Cr(2)—O(7) | 1.605 (3) | K(2)—O(14)vii | 2.762 (3) |
Cr(3)—O(8) | 1.618 (3) | K(3)—O(2)iv | 2.859 (3) |
Cr(3)—O(9) | 1.615 (2) | K(3)—O(6)viii | 2.902 (3) |
Cr(3)—O(10) | 1.606 (3) | K(3)—O(7)viii | 3.064 (3) |
Cr(3)—O(11) | 1.778 (2) | K(3)—O(8) | 2.818 (3) |
Cr(4)—O(11) | 1.787 (2) | K(3)—O(10)viii | 2.749 (3) |
Cr(4)—O(12) | 1.619 (3) | K(3)—O(12) | 2.879 (3) |
Cr(4)—O(13) | 1.604 (3) | K(3)—O(12)ix | 2.961 (3) |
Cr(4)—O(14) | 1.619 (2) | K(3)—O(13)x | 2.810 (3) |
K(1)—O(1) | 2.879 (3) | K(3)—O(14)ix | 2.842 (3) |
K(1)—O(3)i | 2.707 (3) | K(4)—O(1)xi | 2.896 (3) |
K(1)—O(5) | 2.714 (3) | K(4)—O(2)xi | 3.138 (3) |
K(1)—O(5)ii | 2.695 (3) | K(4)—O(8)vii | 2.849 (3) |
K(1)—O(6)iii | 2.687 (3) | K(4)—O(9)xii | 2.953 (3) |
K(1)—O(8)ii | 2.831 (3) | K(4)—O(10) | 2.761 (3) |
K(1)—O(9)ii | 2.799 (3) | K(4)—O(11)xii | 2.967 (2) |
K(2)—O(1)iv | 2.847 (3) | K(4)—O(12)xiii | 2.752 (3) |
K(2)—O(2)v | 2.979 (3) | K(4)—O(14) | 2.810 (3) |
Cr(3)···O(11)xii | 3.579 (3) | K(4)···O(1)xi | 2.896 (3) |
Cr(4)···O(9)xii | 3.509 (3) | K(4)···O(9)xii | 2.953 (3) |
Cr(4)···O(2)xiv | 3.528 (3) | K(4)···O(11)xii | 2.967 (2) |
K(1)···O(6)iii | 2.687 (3) | K(4)···O(2)xi | 3.138 (3) |
K(1)···O(5)ii | 2.695 (3) | O(1)···O(9)ii | 3.053 (4) |
K(1)···O(3)i | 2.707 (3) | O(1)···O(3)iv | 3.246 (4) |
K(1)···O(5) | 2.714 (3) | O(1)···O(5)ii | 3.489 (4) |
K(1)···O(9)ii | 2.799 (3) | O(1)···O(7)iv | 3.490 (4) |
K(1)···O(8)ii | 2.831 (3) | O(2)···O(8)iv | 3.192 (4) |
K(1)···O(1) | 2.879 (3) | O(2)···O(14)xv | 3.210 (4) |
K(1)···O(7)ii | 3.379 (3) | O(2)···O(12)xv | 3.414 (4) |
K(2)···O(5)vi | 2.746 (3) | O(2)···O(13)xv | 3.462 (4) |
K(2)···O(14)vii | 2.762 (3) | O(3)···O(3)iv | 3.328 (6) |
K(2)···O(3) | 2.835 (3) | O(3)···O(5)vi | 3.362 (4) |
K(2)···O(1)iv | 2.847 (3) | O(3)···O(7)iv | 3.422 (4) |
K(2)···O(4)v | 2.863 (3) | O(4)···O(6)iii | 3.365 (4) |
K(2)···O(7) | 2.922 (3) | O(5)···O(5)ii | 3.194 (5) |
K(2)···O(2)v | 2.979 (3) | O(5)···O(9) | 3.358 (4) |
K(2)···O(9)vi | 3.085 (3) | O(5)···O(6)iii | 3.595 (4) |
K(2)···O(6)vi | 3.239 (3) | O(6)···O(13)xii | 3.254 (4) |
K(2)···O(13)vii | 3.308 (3) | O(7)···O(14)vii | 3.166 (4) |
K(3)···O(10)viii | 2.749 (3) | O(7)···O(9) | 3.509 (4) |
K(3)···O(13)x | 2.810 (3) | O(9)···O(14)xii | 3.154 (4) |
K(3)···O(8) | 2.818 (3) | O(9)···O(13)xii | 3.326 (4) |
K(3)···O(14)ix | 2.842 (3) | O(9)···O(11)xii | 3.574 (4) |
K(3)···O(2)iv | 2.859 (3) | O(10)···O(10)vii | 3.227 (6) |
K(3)···O(12) | 2.879 (3) | O(10)···O(11)xii | 3.303 (4) |
K(3)···O(6)viii | 2.902 (3) | O(10)···O(14)vii | 3.322 (4) |
K(3)···O(12)ix | 2.961 (3) | O(10)···O(12)xiii | 3.597 (4) |
K(3)···O(7)viii | 3.064 (3) | O(11)···O(11)xii | 3.349 (5) |
K(4)···O(12)xiii | 2.752 (3) | O(11)···O(13)x | 3.357 (4) |
K(4)···O(10) | 2.761 (3) | O(11)···O(12)x | 3.590 (3) |
K(4)···O(14) | 2.810 (3) | O(12)···O(13)x | 3.443 (4) |
K(4)···O(8)vii | 2.849 (3) | ||
O(1)—Cr(1)—O(2) | 109.10 (14) | O(8)—K(3)—O(10)viii | 150.49 (8) |
O(1)—Cr(1)—O(3) | 110.92 (14) | O(8)—K(3)—O(12) | 71.89 (7) |
O(1)—Cr(1)—O(4) | 110.10 (13) | O(8)—K(3)—O(12)ix | 77.32 (7) |
O(2)—Cr(1)—O(3) | 110.61 (14) | O(8)—K(3)—O(13)x | 83.26 (8) |
O(2)—Cr(1)—O(4) | 106.72 (13) | O(8)—K(3)—O(14)ix | 122.29 (8) |
O(3)—Cr(1)—O(4) | 109.31 (13) | O(10)viii—K(3)—O(12) | 79.42 (8) |
O(4)—Cr(2)—O(5) | 108.71 (13) | O(10)viii—K(3)—O(12)ix | 97.79 (8) |
O(4)—Cr(2)—O(6) | 109.59 (13) | O(10)viii—K(3)—O(13)x | 82.56 (8) |
O(4)—Cr(2)—O(7) | 110.38 (13) | O(10)viii—K(3)—O(14)ix | 72.90 (8) |
O(5)—Cr(2)—O(6) | 109.00 (14) | O(12)—K(3)—O(12)ix | 66.64 (9) |
O(5)—Cr(2)—O(7) | 109.32 (14) | O(12)—K(3)—O(14)ix | 107.91 (8) |
O(6)—Cr(2)—O(7) | 109.81 (14) | O(12)ix—K(3)—O(13)x | 140.25 (8) |
O(8)—Cr(3)—O(9) | 109.34 (13) | O(12)ix—K(3)—O(14)ix | 53.80 (7) |
O(8)—Cr(3)—O(10) | 109.99 (14) | O(13)x—K(3)—O(14)ix | 154.17 (8) |
O(8)—Cr(3)—O(11) | 109.07 (12) | O(1)xi—K(4)—O(2)xi | 51.42 (7) |
O(9)—Cr(3)—O(10) | 111.19 (14) | O(1)xi—K(4)—O(8)vii | 94.13 (8) |
O(9)—Cr(3)—O(11) | 106.57 (12) | O(1)xi—K(4)—O(9)xii | 62.92 (7) |
O(10)—Cr(3)—O(11) | 110.59 (12) | O(1)xi—K(4)—O(10) | 161.77 (8) |
O(11)—Cr(4)—O(12) | 109.63 (12) | O(1)xi—K(4)—O(11)xii | 108.39 (8) |
O(11)—Cr(4)—O(13) | 109.52 (13) | O(1)xi—K(4)—O(12)xiii | 116.42 (8) |
O(11)—Cr(4)—O(14) | 108.40 (12) | O(1)xi—K(4)—O(14) | 86.43 (8) |
O(12)—Cr(4)—O(13) | 110.65 (14) | O(2)xi—K(4)—O(8)vii | 64.22 (7) |
O(12)—Cr(4)—O(14) | 108.50 (13) | O(2)xi—K(4)—O(9)xii | 106.90 (7) |
O(13)—Cr(4)—O(14) | 110.10 (14) | O(2)xi—K(4)—O(10) | 145.71 (7) |
O(1)—K(1)—O(3)i | 154.54 (8) | O(2)xi—K(4)—O(11)xii | 120.08 (8) |
O(1)—K(1)—O(5) | 78.67 (8) | O(2)xi—K(4)—O(12)xiii | 70.50 (7) |
O(1)—K(1)—O(5)ii | 77.42 (8) | O(2)xi—K(4)—O(14) | 129.17 (8) |
O(1)—K(1)—O(6)iii | 102.20 (8) | O(8)vii—K(4)—O(9)xii | 151.53 (8) |
O(1)—K(1)—O(8)ii | 111.60 (8) | O(8)vii—K(4)—O(10) | 92.48 (8) |
O(1)—K(1)—O(9)ii | 65.04 (8) | O(8)vii—K(4)—O(11)xii | 153.70 (8) |
O(3)i—K(1)—O(5) | 76.68 (8) | O(8)vii—K(4)—O(12)xiii | 80.28 (8) |
O(3)i—K(1)—O(5)ii | 89.10 (8) | O(8)vii—K(4)—O(14) | 97.45 (8) |
O(3)i—K(1)—O(6)iii | 81.26 (8) | O(9)xii—K(4)—O(10) | 104.98 (8) |
O(3)i—K(1)—O(8)ii | 93.58 (8) | O(9)xii—K(4)—O(11)xii | 54.73 (7) |
O(3)i—K(1)—O(9)ii | 132.50 (9) | O(9)xii—K(4)—O(12)xiii | 123.90 (8) |
O(5)—K(1)—O(5)ii | 72.39 (9) | O(9)xii—K(4)—O(14) | 66.29 (7) |
O(5)—K(1)—O(6)iii | 83.46 (8) | O(10)—K(4)—O(11)xii | 70.30 (8) |
O(5)—K(1)—O(8)ii | 168.45 (8) | O(10)—K(4)—O(12)xiii | 81.45 (8) |
O(5)—K(1)—O(9)ii | 135.57 (8) | O(10)—K(4)—O(14) | 75.86 (8) |
O(5)ii—K(1)—O(6)iii | 155.50 (8) | O(11)xii—K(4)—O(12)xiii | 77.66 (7) |
O(5)ii—K(1)—O(8)ii | 114.18 (8) | O(11)xii—K(4)—O(14) | 97.32 (7) |
O(5)ii—K(1)—O(9)ii | 75.32 (8) | O(12)xiii—K(4)—O(14) | 157.10 (8) |
O(6)iii—K(1)—O(8)ii | 89.00 (8) | Cr(1)—O(1)—K(1) | 114.41 (13) |
O(6)iii—K(1)—O(9)ii | 127.24 (8) | Cr(1)—O(1)—K(2)iv | 144.37 (15) |
O(8)ii—K(1)—O(9)ii | 55.87 (7) | Cr(1)—O(1)—K(4)xvi | 103.20 (12) |
O(1)iv—K(2)—O(2)v | 141.69 (8) | K(1)—O(1)—K(2)iv | 93.35 (8) |
O(1)iv—K(2)—O(3) | 69.68 (8) | K(1)—O(1)—K(4)xvi | 103.98 (9) |
O(1)iv—K(2)—O(4)v | 144.48 (8) | K(2)iv—O(1)—K(4)xvi | 90.34 (8) |
O(1)iv—K(2)—O(5)vi | 77.17 (8) | Cr(1)—O(2)—K(2)v | 98.71 (12) |
O(1)iv—K(2)—O(6)vi | 123.12 (8) | Cr(1)—O(2)—K(3)iv | 155.11 (15) |
O(1)iv—K(2)—O(7) | 74.43 (8) | Cr(1)—O(2)—K(4)xvi | 93.77 (11) |
O(1)iv—K(2)—O(9)vi | 61.81 (8) | K(2)v—O(2)—K(3)iv | 99.02 (8) |
O(1)iv—K(2)—O(13)vii | 120.91 (8) | K(2)v—O(2)—K(4)xvi | 127.43 (10) |
O(1)iv—K(2)—O(14)vii | 88.32 (8) | K(3)iv—O(2)—K(4)xvi | 89.19 (7) |
O(2)v—K(2)—O(3) | 109.58 (8) | Cr(1)—O(3)—K(1)vi | 119.56 (14) |
O(2)v—K(2)—O(4)v | 55.70 (7) | Cr(1)—O(3)—K(2) | 124.99 (14) |
O(2)v—K(2)—O(5)vi | 140.81 (8) | K(1)vi—O(3)—K(2) | 102.34 (9) |
O(2)v—K(2)—O(6)vi | 93.78 (7) | Cr(1)—O(4)—Cr(2) | 127.29 (14) |
O(2)v—K(2)—O(7) | 68.95 (8) | Cr(1)—O(4)—K(2)v | 98.65 (10) |
O(2)v—K(2)—O(9)vi | 125.27 (8) | Cr(2)—O(4)—K(2)v | 133.52 (12) |
O(2)v—K(2)—O(13)vii | 66.59 (8) | Cr(2)—O(5)—K(1) | 119.78 (12) |
O(2)v—K(2)—O(14)vii | 67.89 (7) | Cr(2)—O(5)—K(1)ii | 113.98 (13) |
O(3)—K(2)—O(4)v | 74.97 (8) | Cr(2)—O(5)—K(2)i | 108.81 (12) |
O(3)—K(2)—O(5)vi | 74.07 (8) | K(1)—O(5)—K(1)ii | 107.61 (9) |
O(3)—K(2)—O(6)vi | 110.23 (8) | K(1)—O(5)—K(2)i | 104.51 (9) |
O(3)—K(2)—O(7) | 74.43 (8) | K(1)ii—O(5)—K(2)i | 99.89 (8) |
O(3)—K(2)—O(9)vi | 124.25 (8) | Cr(2)—O(6)—K(1)iii | 146.63 (15) |
O(3)—K(2)—O(13)vii | 167.76 (8) | Cr(2)—O(6)—K(2)i | 89.56 (11) |
O(3)—K(2)—O(14)vii | 140.12 (8) | Cr(2)—O(6)—K(3)xiii | 101.94 (12) |
O(4)v—K(2)—O(5)vi | 90.16 (8) | K(1)iii—O(6)—K(2)i | 114.28 (9) |
O(4)v—K(2)—O(6)vi | 66.60 (7) | K(1)iii—O(6)—K(3)xiii | 93.54 (8) |
O(4)v—K(2)—O(7) | 99.58 (8) | K(2)i—O(6)—K(3)xiii | 106.53 (8) |
O(4)v—K(2)—O(9)vi | 143.87 (8) | Cr(2)—O(7)—K(2) | 120.15 (14) |
O(4)v—K(2)—O(13)vii | 93.91 (7) | Cr(2)—O(7)—K(3)xiii | 95.82 (12) |
O(4)v—K(2)—O(14)vii | 122.42 (8) | K(2)—O(7)—K(3)xiii | 95.73 (8) |
O(5)vi—K(2)—O(7) | 143.20 (8) | Cr(3)—O(8)—K(1)ii | 96.60 (11) |
O(5)vi—K(2)—O(9)vi | 70.05 (7) | Cr(3)—O(8)—K(3) | 132.76 (13) |
O(5)vi—K(2)—O(13)vii | 101.33 (7) | Cr(3)—O(8)—K(4)vii | 117.50 (13) |
O(5)vi—K(2)—O(14)vii | 134.38 (8) | K(1)ii—O(8)—K(3) | 92.33 (8) |
O(6)vi—K(2)—O(9)vi | 77.57 (7) | K(1)ii—O(8)—K(4)vii | 121.29 (9) |
O(6)vi—K(2)—O(13)vii | 59.60 (6) | K(3)—O(8)—K(4)vii | 96.09 (8) |
O(6)vi—K(2)—O(14)vii | 109.65 (7) | Cr(3)—O(9)—K(1)ii | 97.92 (11) |
O(7)—K(2)—O(9)vi | 114.49 (8) | Cr(3)—O(9)—K(2)i | 168.24 (14) |
O(7)—K(2)—O(13)vii | 113.16 (7) | Cr(3)—O(9)—K(4)xii | 101.45 (11) |
O(7)—K(2)—O(14)vii | 67.64 (8) | K(1)ii—O(9)—K(2)i | 90.01 (7) |
O(9)vi—K(2)—O(13)vii | 62.59 (7) | K(1)ii—O(9)—K(4)xii | 104.54 (9) |
O(9)vi—K(2)—O(14)vii | 65.01 (7) | K(2)i—O(9)—K(4)xii | 84.82 (7) |
O(13)vii—K(2)—O(14)vii | 50.62 (7) | Cr(3)—O(10)—K(3)xiii | 122.12 (14) |
O(2)iv—K(3)—O(7)viii | 68.57 (8) | Cr(3)—O(10)—K(4) | 124.79 (13) |
O(2)iv—K(3)—O(8) | 68.42 (8) | K(3)xiii—O(10)—K(4) | 100.88 (9) |
O(2)iv—K(3)—O(10)viii | 138.29 (9) | Cr(3)—O(11)—Cr(4) | 124.19 (13) |
O(2)iv—K(3)—O(12) | 127.24 (8) | Cr(3)—O(11)—K(4)xii | 96.82 (9) |
O(2)iv—K(3)—O(12)ix | 71.80 (8) | Cr(4)—O(11)—K(4)xii | 137.61 (11) |
O(2)iv—K(3)—O(13)x | 131.38 (8) | Cr(4)—O(12)—K(3) | 131.24 (13) |
O(2)iv—K(3)—O(14)ix | 68.55 (8) | Cr(4)—O(12)—K(3)ix | 96.38 (11) |
O(6)viii—K(3)—O(7)viii | 52.32 (7) | Cr(4)—O(12)—K(4)viii | 117.77 (13) |
O(6)viii—K(3)—O(8) | 85.11 (8) | K(3)—O(12)—K(3)ix | 113.36 (9) |
O(6)viii—K(3)—O(10)viii | 113.57 (8) | K(3)—O(12)—K(4)viii | 97.92 (8) |
O(6)viii—K(3)—O(12) | 139.07 (8) | K(3)ix—O(12)—K(4)viii | 95.01 (8) |
O(6)viii—K(3)—O(12)ix | 141.10 (8) | Cr(4)—O(13)—K(2)vii | 88.94 (11) |
O(6)viii—K(3)—O(13)x | 69.44 (8) | Cr(4)—O(13)—K(3)x | 139.24 (15) |
O(6)viii—K(3)—O(14)ix | 113.01 (8) | K(2)vii—O(13)—K(3)x | 106.93 (9) |
O(7)viii—K(3)—O(8) | 127.53 (8) | Cr(4)—O(14)—K(2)vii | 110.09 (12) |
O(7)viii—K(3)—O(10)viii | 81.16 (8) | Cr(4)—O(14)—K(3)ix | 101.01 (11) |
O(7)viii—K(3)—O(12) | 160.54 (7) | Cr(4)—O(14)—K(4) | 124.55 (12) |
O(7)viii—K(3)—O(12)ix | 115.18 (7) | K(2)vii—O(14)—K(3)ix | 104.82 (8) |
O(7)viii—K(3)—O(13)x | 104.20 (8) | K(2)vii—O(14)—K(4) | 93.94 (8) |
O(7)viii—K(3)—O(14)ix | 64.72 (7) | K(3)ix—O(14)—K(4) | 120.54 (9) |
Cr(1)—O(1)—K(1)—O(3)i | −71.9 (3) | Cr(4)—O(14)—K(4)—O(9)xii | 63.35 (15) |
Cr(1)—O(1)—K(1)—O(5) | −57.30 (14) | Cr(4)—O(14)—K(4)—O(10) | −50.34 (15) |
Cr(1)—O(1)—K(1)—O(5)ii | −131.54 (15) | Cr(4)—O(14)—K(4)—O(11)xii | 17.16 (16) |
Cr(1)—O(1)—K(1)—O(6)iii | 23.37 (16) | Cr(4)—O(14)—K(4)—O(12)xiii | −58.4 (3) |
Cr(1)—O(1)—K(1)—O(8)ii | 117.17 (14) | K(1)—O(1)—Cr(1)—O(2) | −96.42 (15) |
Cr(1)—O(1)—K(1)—O(9)ii | 148.98 (17) | K(1)—O(1)—Cr(1)—O(3) | 141.49 (14) |
Cr(1)—O(1)—K(2)iv—O(2)viii | −56.3 (3) | K(1)—O(1)—Cr(1)—O(4) | 20.38 (17) |
Cr(1)—O(1)—K(2)iv—O(3)iv | 39.9 (2) | K(1)—O(1)—K(2)iv—O(2)viii | 161.27 (10) |
Cr(1)—O(1)—K(2)iv—O(4)viii | 45.7 (3) | K(1)—O(1)—K(2)iv—O(3)iv | −102.54 (9) |
Cr(1)—O(1)—K(2)iv—O(5)ii | 117.4 (3) | K(1)—O(1)—K(2)iv—O(4)viii | −96.69 (13) |
Cr(1)—O(1)—K(2)iv—O(6)ii | 141.3 (2) | K(1)—O(1)—K(2)iv—O(5)ii | −25.00 (7) |
Cr(1)—O(1)—K(2)iv—O(7)iv | −39.0 (3) | K(1)—O(1)—K(2)iv—O(6)ii | −1.07 (11) |
Cr(1)—O(1)—K(2)iv—O(9)ii | −168.6 (3) | K(1)—O(1)—K(2)iv—O(7)iv | 178.65 (9) |
Cr(1)—O(1)—K(4)xvi—K(1) | −119.72 (16) | K(1)—O(1)—K(2)iv—O(9)ii | 49.04 (7) |
Cr(1)—O(1)—K(4)xvi—O(2) | −9.77 (10) | K(1)—O(1)—K(4)xvi—O(2) | 109.96 (11) |
Cr(1)—O(2)—K(2)v—O(3)v | 58.00 (14) | K(1)—O(5)—Cr(2)—O(4) | −11.56 (17) |
Cr(1)—O(2)—K(2)v—O(4) | 3.17 (10) | K(1)—O(5)—Cr(2)—O(6) | 107.85 (15) |
Cr(1)—O(2)—K(2)v—O(5)iii | −30.59 (19) | K(1)—O(5)—Cr(2)—O(7) | −132.11 (15) |
Cr(1)—O(2)—K(2)v—O(6)iii | −55.04 (12) | K(1)—O(5)—K(1)ii—O(1)ii | −81.93 (9) |
Cr(1)—O(2)—K(2)v—O(7)v | 121.75 (13) | K(1)—O(5)—K(1)ii—O(5)ii | 0.0000 |
Cr(1)—O(2)—K(2)v—O(9)iii | −132.48 (11) | K(1)—O(5)—K(1)ii—O(6)viii | 9.9 (2) |
Cr(1)—O(2)—K(3)iv—O(6)v | −40.0 (3) | K(1)—O(5)—K(1)ii—O(8) | 169.82 (8) |
Cr(1)—O(2)—K(3)iv—O(7)v | −96.4 (4) | K(1)—O(5)—K(1)ii—O(9) | −149.07 (10) |
Cr(1)—O(2)—K(3)iv—O(8)iv | 52.8 (3) | K(1)—O(5)—K(2)i—O(1)ii | 84.03 (9) |
Cr(1)—O(2)—K(3)iv—O(10)v | −142.8 (3) | K(1)—O(5)—K(2)i—O(2)iii | −89.82 (13) |
Cr(1)—O(2)—K(3)iv—O(12)iv | 96.8 (4) | K(1)—O(5)—K(2)i—O(4)iii | −62.50 (9) |
Cr(1)—O(2)—K(4)xvi—O(1) | 9.52 (10) | K(1)—O(5)—K(2)i—O(6) | −121.77 (12) |
Cr(1)—O(3)—K(2)—O(1)iv | 126.04 (18) | K(1)—O(5)—K(2)i—O(9) | 148.38 (10) |
Cr(1)—O(3)—K(2)—O(2)v | −13.11 (19) | K(1)—O(5)—K(2)i—O(13)xii | −156.52 (8) |
Cr(1)—O(3)—K(2)—O(4)v | −57.47 (16) | K(1)—O(5)—K(2)i—O(14)xii | 158.66 (9) |
Cr(1)—O(3)—K(2)—O(5)vi | −152.04 (19) | K(1)—O(5)ii—Cr(2)ii—O(4)ii | −117.96 (13) |
Cr(1)—O(3)—K(2)—O(6)vi | −114.98 (16) | K(1)—O(5)ii—Cr(2)ii—O(6)ii | 122.64 (14) |
Cr(1)—O(3)—K(2)—O(7) | 47.22 (16) | K(1)—O(5)ii—Cr(2)ii—O(7)ii | 2.60 (17) |
Cr(1)—O(3)—K(2)—O(9)vi | 156.54 (14) | K(1)—O(5)ii—K(1)ii—O(1)ii | 80.25 (9) |
Cr(1)—O(3)—K(2)—O(13)vii | −82.7 (4) | K(1)—O(5)ii—K(1)ii—O(5) | 0.0000 |
Cr(1)—O(3)—K(2)—O(14)vii | 65.5 (2) | K(1)—O(5)ii—K(1)ii—O(6)viii | −175.87 (10) |
Cr(1)—O(4)—Cr(2)—O(5) | −66.7 (2) | K(1)—O(5)ii—K(1)ii—O(8) | −126.3 (4) |
Cr(1)—O(4)—Cr(2)—O(6) | 174.30 (17) | K(1)—O(5)ii—K(1)ii—O(9) | 45.27 (14) |
Cr(1)—O(4)—Cr(2)—O(7) | 53.2 (2) | K(1)—O(6)iii—Cr(2)iii—O(4)iii | 8.8 (3) |
Cr(1)—O(4)—K(2)v—O(2) | −2.86 (9) | K(1)—O(6)iii—Cr(2)iii—O(5)iii | 127.6 (3) |
Cr(1)—O(4)—K(2)v—O(3)v | −129.96 (12) | K(1)—O(6)iii—Cr(2)iii—O(7)iii | −112.6 (3) |
Cr(1)—O(4)—K(2)v—O(5)iii | 156.59 (11) | K(1)—O(8)ii—Cr(3)ii—K(3)xvii | 87.54 (8) |
Cr(1)—O(4)—K(2)v—O(6)iii | 109.61 (12) | K(1)—O(8)ii—Cr(3)ii—O(9)ii | 4.83 (14) |
Cr(1)—O(4)—K(2)v—O(7)v | −59.07 (11) | K(1)—O(8)ii—Cr(3)ii—O(10)ii | 127.20 (11) |
Cr(1)—O(4)—K(2)v—O(9)iii | 101.67 (14) | K(1)—O(8)ii—Cr(3)ii—O(11)ii | −111.35 (10) |
Cr(2)—O(4)—Cr(1)—O(1) | 58.7 (2) | K(1)—O(8)ii—K(3)ii—O(2)i | −71.05 (8) |
Cr(2)—O(4)—Cr(1)—O(2) | 177.00 (18) | K(1)—O(8)ii—K(3)ii—O(6)iii | −1.19 (8) |
Cr(2)—O(4)—Cr(1)—O(3) | −63.3 (2) | K(1)—O(8)ii—K(3)ii—O(7)iii | −34.12 (11) |
Cr(2)—O(4)—K(2)v—O(2) | −174.6 (2) | K(1)—O(8)ii—K(3)ii—O(10)iii | 130.38 (15) |
Cr(2)—O(4)—K(2)v—O(3)v | 58.32 (17) | K(1)—O(8)ii—K(3)ii—O(12)ii | 144.47 (9) |
Cr(2)—O(4)—K(2)v—O(5)iii | −15.13 (18) | K(1)—O(9)ii—Cr(3)ii—O(8)ii | −4.90 (14) |
Cr(2)—O(4)—K(2)v—O(6)iii | −62.10 (17) | K(1)—O(9)ii—Cr(3)ii—O(10)ii | −126.55 (12) |
Cr(2)—O(4)—K(2)v—O(7)v | 129.22 (17) | K(1)—O(9)ii—Cr(3)ii—O(11)ii | 112.86 (11) |
Cr(2)—O(4)—K(2)v—O(9)iii | −70.0 (2) | K(2)—O(1)iv—Cr(1)iv—O(2)iv | −125.6 (2) |
Cr(2)—O(5)—K(1)—O(1) | 52.06 (15) | K(2)—O(1)iv—Cr(1)iv—O(3)iv | −3.5 (3) |
Cr(2)—O(5)—K(1)—O(3)i | −134.36 (16) | K(2)—O(1)iv—Cr(1)iv—O(4)iv | 117.6 (2) |
Cr(2)—O(5)—K(1)—O(5)ii | 132.3 (2) | K(2)—O(1)iv—K(1)iv—O(3)xviii | −85.1 (2) |
Cr(2)—O(5)—K(1)—O(6)iii | −51.82 (15) | K(2)—O(1)iv—K(1)iv—O(5)vi | −25.48 (7) |
Cr(2)—O(5)—K(1)—O(8)ii | −101.4 (4) | K(2)—O(1)iv—K(1)iv—O(5)iv | −99.73 (8) |
Cr(2)—O(5)—K(1)—O(9)ii | 87.04 (18) | K(2)—O(1)iv—K(1)iv—O(6)xix | 179.61 (8) |
Cr(2)—O(5)—K(1)ii—O(1)ii | 142.70 (14) | K(2)—O(1)iv—K(1)iv—O(8)vi | 85.81 (9) |
Cr(2)—O(5)—K(1)ii—O(5)ii | −135.37 (18) | K(2)—O(1)iv—K(1)iv—O(9)vi | 54.00 (8) |
Cr(2)—O(5)—K(1)ii—O(6)viii | −125.43 (19) | K(2)—O(2)v—Cr(1)v—O(1)v | −114.55 (12) |
Cr(2)—O(5)—K(1)ii—O(8) | 34.45 (16) | K(2)—O(2)v—Cr(1)v—O(3)v | 123.18 (12) |
Cr(2)—O(5)—K(1)ii—O(9) | 75.56 (13) | K(2)—O(2)v—Cr(1)v—O(4)v | 4.37 (14) |
Cr(2)—O(5)—K(2)i—O(1)ii | −146.91 (14) | K(2)—O(3)—Cr(1)—O(1) | −130.49 (16) |
Cr(2)—O(5)—K(2)i—O(2)iii | 39.2 (2) | K(2)—O(3)—Cr(1)—O(2) | 108.31 (17) |
Cr(2)—O(5)—K(2)i—O(4)iii | 66.56 (13) | K(2)—O(3)—Cr(1)—O(4) | −8.9 (2) |
Cr(2)—O(5)—K(2)i—O(6) | 7.29 (10) | K(2)—O(4)v—Cr(1)v—O(1)v | 113.72 (12) |
Cr(2)—O(5)—K(2)i—O(9) | −82.56 (13) | K(2)—O(4)v—Cr(1)v—O(2)v | −4.55 (14) |
Cr(2)—O(5)—K(2)i—O(13)xii | −27.46 (14) | K(2)—O(4)v—Cr(1)v—O(3)v | −124.20 (12) |
Cr(2)—O(5)—K(2)i—O(14)xii | −72.28 (16) | K(2)—O(4)v—Cr(2)v—O(5)v | −103.02 (18) |
Cr(2)—O(6)—K(1)iii—O(1)iii | 131.3 (3) | K(2)—O(4)v—Cr(2)v—O(6)v | 16.0 (2) |
Cr(2)—O(6)—K(1)iii—O(5)iii | 54.4 (3) | K(2)—O(4)v—Cr(2)v—O(7)v | 137.08 (17) |
Cr(2)—O(6)—K(2)i—O(1)ii | 23.53 (15) | K(2)—O(7)—Cr(2)—O(4) | 23.82 (18) |
Cr(2)—O(6)—K(2)i—O(2)iii | −167.33 (11) | K(2)—O(7)—Cr(2)—O(5) | 143.35 (14) |
Cr(2)—O(6)—K(2)i—O(4)iii | −117.42 (12) | K(2)—O(7)—Cr(2)—O(6) | −97.11 (16) |
Cr(2)—O(6)—K(2)i—O(5) | −6.91 (9) | K(2)—O(7)—K(3)xiii—O(2)v | 39.13 (8) |
Cr(2)—O(6)—K(2)i—O(9) | 67.36 (11) | K(2)—O(7)—K(3)xiii—O(6) | 119.19 (11) |
Cr(2)—O(6)—K(2)i—O(13)xii | 132.70 (13) | K(2)—O(7)—K(3)xiii—O(10) | −111.64 (9) |
Cr(2)—O(6)—K(2)i—O(14)xii | 124.82 (11) | K(2)—O(13)vii—Cr(4)vii—O(11)vii | 123.32 (10) |
Cr(2)—O(6)—K(3)xiii—O(2)v | 80.23 (13) | K(2)—O(13)vii—Cr(4)vii—O(12)vii | −115.71 (11) |
Cr(2)—O(6)—K(3)xiii—O(7) | 2.00 (9) | K(2)—O(13)vii—Cr(4)vii—O(14)vii | 4.22 (13) |
Cr(2)—O(6)—K(3)xiii—O(10) | −54.71 (15) | K(2)—O(13)vii—K(3)xx—O(2)xxi | 66.53 (13) |
Cr(2)—O(7)—K(2)—O(1)iv | −128.45 (17) | K(2)—O(13)vii—K(3)xx—O(6)vi | 32.54 (7) |
Cr(2)—O(7)—K(2)—O(2)v | 62.99 (15) | K(2)—O(13)vii—K(3)xx—O(7)vi | −7.25 (9) |
Cr(2)—O(7)—K(2)—O(3) | −55.70 (15) | K(2)—O(13)vii—K(3)xx—O(10)vi | −86.12 (9) |
Cr(2)—O(7)—K(2)—O(4)v | 15.63 (17) | K(2)—O(14)vii—Cr(4)vii—O(11)vii | −125.17 (11) |
Cr(2)—O(7)—K(2)—O(5)vi | −87.7 (2) | K(2)—O(14)vii—Cr(4)vii—O(12)vii | 115.83 (12) |
Cr(2)—O(7)—K(2)—O(6)vi | 52.3 (3) | K(2)—O(14)vii—Cr(4)vii—O(13)vii | −5.39 (16) |
Cr(2)—O(7)—K(2)—O(9)vi | −176.71 (14) | K(2)—O(14)vii—K(3)xiii—O(2)v | −35.28 (8) |
Cr(2)—O(7)—K(2)—O(13)vii | 114.11 (15) | K(2)—O(14)vii—K(3)xiii—O(6) | 19.56 (10) |
Cr(2)—O(7)—K(2)—O(14)vii | 136.86 (18) | K(2)—O(14)vii—K(3)xiii—O(7) | 40.32 (8) |
Cr(2)—O(7)—K(3)xiii—O(2)v | −82.04 (12) | K(2)—O(14)vii—K(3)xiii—O(10) | 128.46 (9) |
Cr(2)—O(7)—K(3)xiii—O(6) | −1.98 (9) | K(2)—O(14)vii—K(4)vii—O(8) | −101.23 (8) |
Cr(2)—O(7)—K(3)xiii—O(10) | 127.19 (12) | K(2)—O(14)vii—K(4)vii—O(9)vi | 54.40 (7) |
Cr(3)—O(8)—K(1)ii—O(1)ii | −32.08 (13) | K(2)—O(14)vii—K(4)vii—O(10)vii | 168.08 (9) |
Cr(3)—O(8)—K(1)ii—O(5) | 53.39 (13) | K(2)—O(14)vii—K(4)vii—O(11)vi | 100.59 (8) |
Cr(3)—O(8)—K(1)ii—O(5)ii | 176.1 (3) | K(2)—O(14)vii—K(4)vii—O(12)ix | 176.12 (18) |
Cr(3)—O(8)—K(1)ii—O(6)viii | −134.81 (11) | K(3)—O(2)iv—Cr(1)iv—O(1)iv | 110.5 (4) |
Cr(3)—O(8)—K(1)ii—O(9) | 3.17 (9) | K(3)—O(2)iv—Cr(1)iv—O(3)iv | −11.8 (4) |
Cr(3)—O(8)—K(3)—O(2)iv | 172.3 (2) | K(3)—O(2)iv—Cr(1)iv—O(4)iv | −130.6 (3) |
Cr(3)—O(8)—K(3)—O(6)viii | 102.40 (19) | K(3)—O(2)iv—K(2)viii—O(1)xxii | 22.75 (17) |
Cr(3)—O(8)—K(3)—O(7)viii | 135.32 (16) | K(3)—O(2)iv—K(2)viii—O(13)ix | −88.04 (8) |
Cr(3)—O(8)—K(3)—O(10)viii | −29.2 (3) | K(3)—O(2)iv—K(2)viii—O(14)ix | −32.81 (7) |
Cr(3)—O(8)—K(3)—O(12) | −43.26 (18) | K(3)—O(8)—Cr(3)—O(9) | −104.19 (19) |
Cr(3)—O(8)—K(3)—O(12)ix | −112.53 (19) | K(3)—O(8)—Cr(3)—O(10) | 133.43 (17) |
Cr(3)—O(8)—K(3)—O(13)x | 32.57 (18) | K(3)—O(8)—Cr(3)—O(11) | 12.0 (2) |
Cr(3)—O(8)—K(3)—O(14)ix | −143.40 (16) | K(3)—O(8)—K(1)ii—O(1)ii | 101.45 (8) |
Cr(3)—O(8)—K(4)vii—O(9)vi | −89.9 (2) | K(3)—O(8)—K(1)ii—O(5) | −173.08 (7) |
Cr(3)—O(8)—K(4)vii—O(10)vii | 38.57 (14) | K(3)—O(8)—K(1)ii—O(5)ii | −50.4 (4) |
Cr(3)—O(8)—K(4)vii—O(11)vi | 86.2 (2) | K(3)—O(8)—K(1)ii—O(6)viii | −1.28 (8) |
Cr(3)—O(8)—K(4)vii—O(12)ix | 119.46 (15) | K(3)—O(8)—K(1)ii—O(9) | 136.70 (11) |
Cr(3)—O(8)—K(4)vii—O(14)vii | −37.49 (15) | K(3)—O(8)—K(4)vii—O(9)vi | 124.44 (15) |
Cr(3)—O(9)—K(1)ii—O(1)ii | 140.51 (14) | K(3)—O(8)—K(4)vii—O(10)vii | −107.05 (8) |
Cr(3)—O(9)—K(1)ii—O(5) | −136.75 (13) | K(3)—O(8)—K(4)vii—O(11)vi | −59.42 (19) |
Cr(3)—O(9)—K(1)ii—O(5)ii | 178.83 (10) | K(3)—O(8)—K(4)vii—O(12)ix | −26.16 (8) |
Cr(3)—O(9)—K(1)ii—O(6)viii | 54.01 (16) | K(3)—O(8)—K(4)vii—O(14)vii | 176.89 (7) |
Cr(3)—O(9)—K(1)ii—O(8) | −3.19 (9) | K(3)—O(10)viii—Cr(3)viii—O(8)viii | 96.73 (17) |
Cr(3)—O(9)—K(2)i—O(1)ii | −176.6 (7) | K(3)—O(10)viii—Cr(3)viii—O(9)viii | −24.5 (2) |
Cr(3)—O(9)—K(2)i—O(2)iii | −41.2 (7) | K(3)—O(10)viii—Cr(3)viii—O(11)viii | −142.73 (13) |
Cr(3)—O(9)—K(2)i—O(4)iii | 37.1 (7) | K(3)—O(10)viii—K(4)viii—O(8)ix | −75.22 (9) |
Cr(3)—O(9)—K(2)i—O(5) | 97.6 (7) | K(3)—O(10)viii—K(4)viii—O(9)x | 127.49 (8) |
Cr(3)—O(9)—K(2)i—O(6) | 44.6 (7) | K(3)—O(10)viii—K(4)viii—O(11)x | 84.44 (9) |
Cr(3)—O(9)—K(2)i—O(13)xii | −17.4 (7) | K(3)—O(10)viii—K(4)viii—O(12) | 4.56 (8) |
Cr(3)—O(9)—K(2)i—O(14)xii | −74.3 (7) | K(3)—O(12)—Cr(4)—O(11) | −5.6 (2) |
Cr(3)—O(9)—K(4)xii—O(8)i | −177.73 (13) | K(3)—O(12)—Cr(4)—O(13) | 115.33 (18) |
Cr(3)—O(9)—K(4)xii—O(10)xii | 56.29 (13) | K(3)—O(12)—Cr(4)—O(14) | −123.79 (17) |
Cr(3)—O(9)—K(4)xii—O(11) | 4.36 (9) | K(3)—O(12)—K(3)ix—O(8)ix | −75.54 (9) |
Cr(3)—O(9)—K(4)xii—O(12)x | −33.39 (15) | K(3)—O(12)—K(3)ix—O(12)ix | 0.0000 |
Cr(3)—O(9)—K(4)xii—O(14)xii | 123.11 (13) | K(3)—O(12)—K(3)ix—O(13)vi | −12.84 (16) |
Cr(3)—O(10)—K(3)xiii—O(2)v | −84.9 (2) | K(3)—O(12)—K(3)ix—O(14) | 136.97 (12) |
Cr(3)—O(10)—K(3)xiii—O(6) | 0.2 (2) | K(3)—O(12)—K(4)viii—O(8)ix | 89.70 (8) |
Cr(3)—O(10)—K(3)xiii—O(7) | −41.85 (16) | K(3)—O(12)—K(4)viii—O(9)x | −106.67 (9) |
Cr(3)—O(10)—K(4)—O(1)xi | 31.1 (4) | K(3)—O(12)—K(4)viii—O(11)x | −75.90 (8) |
Cr(3)—O(10)—K(4)—O(2)xi | −172.83 (13) | K(3)—O(12)ix—Cr(4)ix—O(11)ix | −123.36 (9) |
Cr(3)—O(10)—K(4)—O(8)vii | 142.34 (17) | K(3)—O(12)ix—Cr(4)ix—O(13)ix | 115.73 (13) |
Cr(3)—O(10)—K(4)—O(9)xii | −14.95 (19) | K(3)—O(12)ix—Cr(4)ix—O(14)ix | −5.15 (13) |
Cr(3)—O(10)—K(4)—O(11)xii | −58.00 (17) | K(3)—O(12)ix—K(3)ix—O(8)ix | 83.66 (9) |
Cr(3)—O(10)—K(4)—O(12)xiii | −137.87 (19) | K(3)—O(12)ix—K(3)ix—O(12) | 0.0000 |
Cr(3)—O(10)—K(4)—O(14) | 45.28 (17) | K(3)—O(12)ix—K(3)ix—O(13)vi | 171.52 (10) |
Cr(3)—O(11)—Cr(4)—O(12) | −59.45 (19) | K(3)—O(12)ix—K(3)ix—O(14) | −35.36 (10) |
Cr(3)—O(11)—Cr(4)—O(13) | 178.96 (17) | K(3)—O(13)x—Cr(4)x—O(11)x | 8.2 (3) |
Cr(3)—O(11)—Cr(4)—O(14) | 58.82 (19) | K(3)—O(13)x—Cr(4)x—O(12)x | 129.2 (2) |
Cr(3)—O(11)—K(4)xii—O(8)i | 178.35 (14) | K(3)—O(13)x—Cr(4)x—O(14)x | −110.9 (2) |
Cr(3)—O(11)—K(4)xii—O(9) | −3.91 (8) | K(3)—O(14)ix—Cr(4)ix—O(11)ix | 124.43 (10) |
Cr(3)—O(11)—K(4)xii—O(10)xii | −130.03 (11) | K(3)—O(14)ix—Cr(4)ix—O(12)ix | 5.43 (14) |
Cr(3)—O(11)—K(4)xii—O(12)x | 144.75 (11) | K(3)—O(14)ix—Cr(4)ix—O(13)ix | −115.79 (13) |
Cr(3)—O(11)—K(4)xii—O(14)xii | −57.94 (11) | K(3)—O(14)ix—K(2)viii—O(1)xxii | −115.40 (8) |
Cr(4)—O(11)—Cr(3)—O(8) | 56.84 (19) | K(3)—O(14)ix—K(2)viii—O(13)ix | 111.05 (11) |
Cr(4)—O(11)—Cr(3)—O(9) | 174.78 (16) | K(3)—O(14)ix—K(4)ix—O(8)viii | 8.55 (12) |
Cr(4)—O(11)—Cr(3)—O(10) | −64.2 (2) | K(3)—O(14)ix—K(4)ix—O(9)xix | 164.17 (12) |
Cr(4)—O(11)—K(4)xii—O(8)i | 12.3 (3) | K(3)—O(14)ix—K(4)ix—O(10)ix | −82.14 (11) |
Cr(4)—O(11)—K(4)xii—O(9) | −170.0 (2) | K(3)—O(14)ix—K(4)ix—O(11)xix | −149.64 (10) |
Cr(4)—O(11)—K(4)xii—O(10)xii | 63.90 (17) | K(3)—O(14)ix—K(4)ix—O(12)xxiii | −74.1 (2) |
Cr(4)—O(11)—K(4)xii—O(12)x | −21.32 (17) | K(4)—O(8)vii—Cr(3)vii—O(9)vii | −125.69 (14) |
Cr(4)—O(11)—K(4)xii—O(14)xii | 135.99 (17) | K(4)—O(8)vii—Cr(3)vii—O(10)vii | −3.32 (18) |
Cr(4)—O(12)—K(3)—O(2)iv | 81.7 (2) | K(4)—O(8)vii—Cr(3)vii—O(11)vii | 118.13 (13) |
Cr(4)—O(12)—K(3)—O(6)viii | −20.1 (2) | K(4)—O(8)vii—K(3)vii—O(6)xxiv | 120.62 (8) |
Cr(4)—O(12)—K(3)—O(7)viii | −137.6 (2) | K(4)—O(8)vii—K(3)vii—O(7)xxiv | 87.69 (10) |
Cr(4)—O(12)—K(3)—O(8) | 38.99 (17) | K(4)—O(8)vii—K(3)vii—O(10)xxiv | −107.81 (16) |
Cr(4)—O(12)—K(3)—O(10)viii | −134.01 (19) | K(4)—O(8)vii—K(3)vii—O(12)xiii | −24.45 (7) |
Cr(4)—O(12)—K(3)—O(12)ix | 122.6 (2) | K(4)—O(8)vii—K(3)vii—O(12)vii | −93.72 (9) |
Cr(4)—O(12)—K(3)—O(13)x | −48.88 (17) | K(4)—O(8)vii—K(3)vii—O(13)xx | −169.55 (9) |
Cr(4)—O(12)—K(3)—O(14)ix | 158.00 (16) | K(4)—O(8)vii—K(3)vii—O(14)xiii | 6.42 (12) |
Cr(4)—O(12)—K(3)ix—O(8)ix | 144.04 (12) | K(4)—O(9)xii—Cr(3)xii—O(8)xii | −111.56 (12) |
Cr(4)—O(12)—K(3)ix—O(12)ix | −140.42 (16) | K(4)—O(9)xii—Cr(3)xii—O(10)xii | 126.79 (13) |
Cr(4)—O(12)—K(3)ix—O(13)vi | −153.26 (11) | K(4)—O(9)xii—Cr(3)xii—O(11)xii | 6.20 (13) |
Cr(4)—O(12)—K(3)ix—O(14) | −3.45 (9) | K(4)—O(10)—Cr(3)—O(8) | −128.25 (16) |
Cr(4)—O(12)—K(4)viii—O(8)ix | −124.67 (15) | K(4)—O(10)—Cr(3)—O(9) | 110.48 (16) |
Cr(4)—O(12)—K(4)viii—O(9)x | 38.95 (18) | K(4)—O(10)—Cr(3)—O(11) | −7.7 (2) |
Cr(4)—O(12)—K(4)viii—O(11)x | 69.73 (14) | K(4)—O(10)—K(3)xiii—O(2)v | 131.30 (11) |
Cr(4)—O(13)—K(2)vii—O(3)vii | −151.0 (3) | K(4)—O(10)—K(3)xiii—O(6) | −143.59 (8) |
Cr(4)—O(13)—K(2)vii—O(5)xii | 142.33 (11) | K(4)—O(10)—K(3)xiii—O(7) | 174.39 (10) |
Cr(4)—O(13)—K(2)vii—O(6)xii | 173.39 (14) | K(4)—O(11)xii—Cr(3)xii—O(8)xii | 111.84 (11) |
Cr(4)—O(13)—K(2)vii—O(7)vii | −24.56 (13) | K(4)—O(11)xii—Cr(3)xii—O(9)xii | −6.09 (13) |
Cr(4)—O(13)—K(2)vii—O(9)xii | 82.06 (11) | K(4)—O(11)xii—Cr(3)xii—O(10)xii | −127.07 (12) |
Cr(4)—O(13)—K(2)vii—O(14) | 3.01 (9) | K(4)—O(11)xii—Cr(4)xii—O(12)xii | −103.75 (18) |
Cr(4)—O(13)—K(3)x—O(8)x | 131.3 (2) | K(4)—O(11)xii—Cr(4)xii—O(13)xii | 17.8 (2) |
Cr(4)—O(13)—K(3)x—O(12)i | 70.5 (3) | K(4)—O(11)xii—Cr(4)xii—O(14)xii | 137.98 (17) |
Cr(4)—O(13)—K(3)x—O(12)x | 58.3 (2) | K(4)—O(14)—Cr(4)—O(11) | 15.25 (18) |
Cr(4)—O(13)—K(3)x—O(14)i | −40.9 (4) | K(4)—O(14)—Cr(4)—O(12) | 134.24 (14) |
Cr(4)—O(14)—K(2)vii—K(1)xii | −118.96 (18) | K(4)—O(14)—Cr(4)—O(13) | −104.53 (16) |
Cr(4)—O(14)—K(2)vii—K(3)ix | 107.88 (15) | K(4)—O(14)—K(2)vii—O(3)vii | −62.40 (14) |
Cr(4)—O(14)—K(2)vii—O(3)vii | 168.51 (11) | K(4)—O(14)—K(2)vii—O(5)xii | 62.51 (12) |
Cr(4)—O(14)—K(2)vii—O(5)xii | −66.58 (16) | K(4)—O(14)—K(2)vii—O(6)xii | 117.11 (7) |
Cr(4)—O(14)—K(2)vii—O(6)xii | −11.97 (14) | K(4)—O(14)—K(2)vii—O(7)vii | −81.48 (8) |
Cr(4)—O(14)—K(2)vii—O(7)vii | 149.44 (14) | K(4)—O(14)—K(2)vii—O(9)xii | 51.85 (7) |
Cr(4)—O(14)—K(2)vii—O(9)xii | −77.24 (12) | K(4)—O(14)—K(2)vii—O(13) | 125.92 (11) |
Cr(4)—O(14)—K(2)vii—O(13) | −3.17 (10) | K(4)—O(14)—K(3)ix—O(8)ix | −176.62 (9) |
Cr(4)—O(14)—K(3)ix—O(8)ix | −34.85 (15) | K(4)—O(14)—K(3)ix—O(12) | −138.28 (13) |
Cr(4)—O(14)—K(3)ix—O(12) | 3.49 (9) | K(4)—O(14)—K(3)ix—O(12)ix | −97.11 (11) |
Cr(4)—O(14)—K(3)ix—O(12)ix | 44.66 (12) | K(4)—O(14)—K(3)ix—O(13)vi | −5.8 (3) |
Cr(4)—O(14)—K(3)ix—O(13)vi | 135.92 (17) | O(5)—K(1)ii—O(5)ii—K(1) | 0.0000 |
Cr(4)—O(14)—K(4)—O(1)xi | 125.26 (16) | O(12)—K(3)—O(12)ix—K(3)ix | 0.0000 |
Cr(4)—O(14)—K(4)—O(2)xi | 156.31 (13) | O(12)—K(3)ix—O(12)ix—K(3) | 0.0000 |
Cr(4)—O(14)—K(4)—O(8)vii | −141.03 (15) |
Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x+2, −y+2, −z+1; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+2, −z+1; (vi) x−1, y, z; (vii) −x+1, −y+1, −z; (viii) x, y−1, z; (ix) −x+1, −y, −z; (x) −x+2, −y, −z; (xi) x, y, z−1; (xii) −x+2, −y+1, −z; (xiii) x, y+1, z; (xiv) x, y−1, z−1; (xv) x, y+1, z+1; (xvi) x, y, z+1; (xvii) −x+2, −y, −z+1; (xviii) −x, −y+1, −z+1; (xix) x−1, y−1, z; (xx) x−1, y+1, z; (xxi) −x, −y+2, −z+1; (xxii) −x+1, −y, −z+1; (xxiii) −x+1, −y−1, −z; (xxiv) −x+1, −y+2, −z. |
Experimental details
(1) | (2) | |
Crystal data | ||
Chemical formula | K2Cr2O7 | 2KCr2O7 |
Mr | 294.18 | 294.18 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 296 | 296 |
a, b, c (Å) | 7.3807 (9), 7.4593 (11), 13.3910 (16) | 7.3837 (8), 7.4622 (6), 13.3949 (12) |
α, β, γ (°) | 96.205 (11), 98.033 (10), 90.914 (12) | 96.204 (7), 98.046 (8), 90.943 (8) |
V (Å3) | 725.37 (16) | 726.12 (12) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 4.13 | 4.13 |
Crystal size (mm) | 0.27 × 0.20 × 0.14 | 0.25 × 0.20 × 0.15 |
Data collection | ||
Diffractometer | Nonius CAD-4 serial diffractometer | Nonius CAD-4 serial deiffractometer |
Absorption correction | Part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983) | Part of the refinement model (ΔF) DIFABS (Walker & Stuart, 1983) |
Tmin, Tmax | 0.382, 0.560 | 0.386, 0.538 |
No. of measured, independent and observed [I > 1.00σ(I)] reflections | 4533, 4227, 4096 | 2759, 2544, 2253 |
Rint | 0.011 | 0.020 |
(sin θ/λ)max (Å−1) | 0.703 | 0.595 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.040, 1.58 | 0.029, 0.042, 1.86 |
No. of reflections | 4227 | 2544 |
No. of parameters | 200 | 200 |
Δρmax, Δρmin (e Å−3) | 0.49, −0.40 | 0.61, −0.45 |
Computer programs: CAD-4-PC (Enraf-Nonius, 1993), TEXSAN (Molecular Structure Corp., 1997).
Cr(1)—O(1) | 1.6144 (17) | K(2)—O(3) | 2.8386 (19) |
Cr(1)—O(2) | 1.6158 (17) | K(2)—O(4)v | 2.8569 (17) |
Cr(1)—O(3) | 1.6036 (17) | K(2)—O(5)vi | 2.7434 (17) |
Cr(1)—O(4) | 1.7884 (16) | K(2)—O(6)vi | 3.234 (2) |
Cr(2)—O(4) | 1.7844 (16) | K(2)—O(7) | 2.9212 (19) |
Cr(2)—O(5) | 1.6181 (16) | K(2)—O(9)vi | 3.0827 (17) |
Cr(2)—O(6) | 1.6110 (17) | K(2)—O(13)vii | 3.303 (2) |
Cr(2)—O(7) | 1.6035 (17) | K(2)—O(14)vii | 2.7621 (17) |
Cr(3)—O(8) | 1.6216 (16) | K(3)—O(2)iv | 2.8547 (17) |
Cr(3)—O(9) | 1.6141 (16) | K(3)—O(6)viii | 2.8990 (19) |
Cr(3)—O(10) | 1.6034 (17) | K(3)—O(7)viii | 3.065 (2) |
Cr(3)—O(11) | 1.7795 (16) | K(3)—O(8) | 2.8146 (18) |
Cr(4)—O(11) | 1.7877 (15) | K(3)—O(10)viii | 2.7511 (18) |
Cr(4)—O(12) | 1.6213 (16) | K(3)—O(12) | 2.8764 (17) |
Cr(4)—O(13) | 1.6030 (17) | K(3)—O(12)ix | 2.9610 (19) |
Cr(4)—O(14) | 1.6195 (16) | K(3)—O(13)x | 2.8108 (18) |
K(1)—O(1) | 2.8753 (19) | K(3)—O(14)ix | 2.8397 (17) |
K(1)—O(3)i | 2.7046 (19) | K(4)—O(1)xi | 2.892 (2) |
K(1)—O(5) | 2.7131 (17) | K(4)—O(2)xi | 3.134 (2) |
K(1)—O(5)ii | 2.6920 (18) | K(4)—O(8)vii | 2.8501 (18) |
K(1)—O(6)iii | 2.6912 (18) | K(4)—O(9)xii | 2.9498 (19) |
K(1)—O(8)ii | 2.8267 (18) | K(4)—O(10) | 2.7604 (19) |
K(1)—O(9)ii | 2.7995 (18) | K(4)—O(11)xii | 2.9618 (16) |
K(2)—O(1)iv | 2.8442 (19) | K(4)—O(12)xiii | 2.7483 (18) |
K(2)—O(2)v | 2.9778 (19) | K(4)—O(14) | 2.8088 (17) |
O(1)—Cr(1)—O(2) | 108.87 (10) | O(7)viii—K(3)—O(14)ix | 64.72 (5) |
O(1)—Cr(1)—O(3) | 110.89 (10) | O(8)—K(3)—O(10)viii | 150.58 (6) |
O(1)—Cr(1)—O(4) | 110.25 (9) | O(8)—K(3)—O(12) | 72.02 (5) |
O(2)—Cr(1)—O(3) | 110.70 (10) | O(8)—K(3)—O(12)ix | 77.35 (5) |
O(2)—Cr(1)—O(4) | 106.54 (9) | O(8)—K(3)—O(13)x | 83.21 (5) |
O(3)—Cr(1)—O(4) | 109.49 (9) | O(8)—K(3)—O(14)ix | 122.38 (5) |
O(4)—Cr(2)—O(5) | 108.86 (8) | O(10)viii—K(3)—O(12) | 79.38 (5) |
O(4)—Cr(2)—O(6) | 109.55 (9) | O(10)viii—K(3)—O(12)ix | 97.76 (5) |
O(4)—Cr(2)—O(7) | 110.43 (9) | O(10)viii—K(3)—O(13)x | 82.68 (6) |
O(5)—Cr(2)—O(6) | 108.92 (9) | O(10)viii—K(3)—O(14)ix | 72.77 (5) |
O(5)—Cr(2)—O(7) | 109.32 (10) | O(12)—K(3)—O(12)ix | 66.62 (6) |
O(6)—Cr(2)—O(7) | 109.72 (10) | O(12)—K(3)—O(13)x | 74.55 (6) |
O(8)—Cr(3)—O(9) | 109.26 (9) | O(12)—K(3)—O(14)ix | 107.84 (5) |
O(8)—Cr(3)—O(10) | 109.99 (10) | O(12)ix—K(3)—O(13)x | 140.27 (6) |
O(8)—Cr(3)—O(11) | 109.11 (8) | O(12)ix—K(3)—O(14)ix | 53.85 (5) |
O(9)—Cr(3)—O(10) | 111.28 (10) | O(13)x—K(3)—O(14)ix | 154.15 (6) |
O(9)—Cr(3)—O(11) | 106.47 (8) | O(1)xi—K(4)—O(2)xi | 51.52 (5) |
O(10)—Cr(3)—O(11) | 110.66 (8) | O(1)xi—K(4)—O(8)vii | 94.10 (5) |
O(11)—Cr(4)—O(12) | 109.64 (8) | O(1)xi—K(4)—O(9)xii | 62.90 (5) |
O(11)—Cr(4)—O(13) | 109.56 (8) | O(1)xi—K(4)—O(10) | 161.66 (6) |
O(11)—Cr(4)—O(14) | 108.49 (8) | O(1)xi—K(4)—O(11)xii | 108.42 (5) |
O(12)—Cr(4)—O(13) | 110.50 (10) | O(1)xi—K(4)—O(12)xiii | 116.50 (5) |
O(12)—Cr(4)—O(14) | 108.43 (9) | O(1)xi—K(4)—O(14) | 86.44 (5) |
O(13)—Cr(4)—O(14) | 110.18 (10) | O(2)xi—K(4)—O(8)vii | 64.16 (5) |
O(1)—K(1)—O(3)i | 154.63 (6) | O(2)xi—K(4)—O(9)xii | 106.97 (5) |
O(1)—K(1)—O(5) | 78.80 (5) | O(2)xi—K(4)—O(10) | 145.70 (5) |
O(1)—K(1)—O(5)ii | 77.34 (5) | O(2)xi—K(4)—O(11)xii | 120.07 (5) |
O(1)—K(1)—O(6)iii | 102.26 (6) | O(2)xi—K(4)—O(12)xiii | 70.49 (5) |
O(1)—K(1)—O(8)ii | 111.58 (5) | O(2)xi—K(4)—O(14) | 129.20 (5) |
O(1)—K(1)—O(9)ii | 64.96 (5) | O(8)vii—K(4)—O(9)xii | 151.46 (5) |
O(3)i—K(1)—O(5) | 76.65 (5) | O(8)vii—K(4)—O(10) | 92.53 (5) |
O(3)i—K(1)—O(5)ii | 89.13 (6) | O(8)vii—K(4)—O(11)xii | 153.71 (5) |
O(3)i—K(1)—O(6)iii | 81.29 (6) | O(8)vii—K(4)—O(12)xiii | 80.31 (5) |
O(3)i—K(1)—O(8)ii | 93.50 (5) | O(8)vii—K(4)—O(14) | 97.34 (5) |
O(3)i—K(1)—O(9)ii | 132.45 (6) | O(9)xii—K(4)—O(10) | 104.94 (5) |
O(5)—K(1)—O(5)ii | 72.27 (6) | O(9)xii—K(4)—O(11)xii | 54.80 (4) |
O(5)—K(1)—O(6)iii | 83.55 (6) | O(9)xii—K(4)—O(12)xiii | 123.95 (5) |
O(5)—K(1)—O(8)ii | 168.37 (5) | O(9)xii—K(4)—O(14) | 66.36 (5) |
O(5)—K(1)—O(9)ii | 135.58 (5) | O(10)—K(4)—O(11)xii | 70.31 (5) |
O(5)ii—K(1)—O(6)iii | 155.49 (5) | O(10)—K(4)—O(12)xiii | 81.48 (5) |
O(5)ii—K(1)—O(8)ii | 114.28 (5) | O(10)—K(4)—O(14) | 75.75 (5) |
O(5)ii—K(1)—O(9)ii | 75.33 (5) | O(11)xii—K(4)—O(12)xiii | 77.60 (5) |
O(6)iii—K(1)—O(8)ii | 88.91 (6) | O(11)xii—K(4)—O(14) | 97.43 (5) |
O(6)iii—K(1)—O(9)ii | 127.21 (6) | O(12)xiii—K(4)—O(14) | 157.00 (5) |
O(8)ii—K(1)—O(9)ii | 55.93 (5) | Cr(1)—O(1)—K(1) | 114.36 (9) |
O(1)iv—K(2)—O(2)v | 141.70 (5) | Cr(1)—O(1)—K(2)iv | 144.21 (10) |
O(1)iv—K(2)—O(3) | 69.73 (6) | Cr(1)—O(1)—K(4)xiv | 103.26 (8) |
O(1)iv—K(2)—O(4)v | 144.47 (5) | K(1)—O(1)—K(2)iv | 93.43 (5) |
O(1)iv—K(2)—O(5)vi | 77.06 (5) | K(1)—O(1)—K(4)xiv | 104.07 (6) |
O(1)iv—K(2)—O(6)vi | 123.00 (5) | K(2)iv—O(1)—K(4)xiv | 90.42 (5) |
O(1)iv—K(2)—O(7) | 74.50 (6) | Cr(1)—O(2)—K(2)v | 98.66 (8) |
O(1)iv—K(2)—O(9)vi | 61.74 (5) | Cr(1)—O(2)—K(3)iv | 154.96 (10) |
O(1)iv—K(2)—O(13)vii | 120.92 (5) | Cr(1)—O(2)—K(4)xiv | 93.82 (8) |
O(1)iv—K(2)—O(14)vii | 88.26 (5) | K(2)v—O(2)—K(3)iv | 99.10 (6) |
O(2)v—K(2)—O(3) | 109.63 (5) | K(2)v—O(2)—K(4)xiv | 127.47 (7) |
O(2)v—K(2)—O(4)v | 55.75 (5) | K(3)iv—O(2)—K(4)xiv | 89.25 (5) |
O(2)v—K(2)—O(5)vi | 140.92 (5) | Cr(1)—O(3)—K(1)vi | 119.64 (9) |
O(2)v—K(2)—O(6)vi | 93.86 (5) | Cr(1)—O(3)—K(2) | 124.85 (10) |
O(2)v—K(2)—O(7) | 68.92 (5) | K(1)vi—O(3)—K(2) | 102.31 (6) |
O(2)v—K(2)—O(9)vi | 125.21 (5) | Cr(1)—O(4)—Cr(2) | 126.91 (10) |
O(2)v—K(2)—O(13)vii | 66.48 (5) | Cr(1)—O(4)—K(2)v | 98.82 (7) |
O(2)v—K(2)—O(14)vii | 67.82 (5) | Cr(2)—O(4)—K(2)v | 133.71 (8) |
O(3)—K(2)—O(4)v | 74.91 (6) | Cr(2)—O(5)—K(1) | 119.63 (8) |
O(3)—K(2)—O(5)vi | 73.98 (5) | Cr(2)—O(5)—K(1)ii | 113.93 (8) |
O(3)—K(2)—O(6)vi | 110.23 (5) | Cr(2)—O(5)—K(2)i | 108.75 (8) |
O(3)—K(2)—O(7) | 74.36 (5) | K(1)—O(5)—K(1)ii | 107.73 (6) |
O(3)—K(2)—O(9)vi | 124.26 (5) | K(1)—O(5)—K(2)i | 104.62 (6) |
O(3)—K(2)—O(13)vii | 167.72 (5) | K(1)ii—O(5)—K(2)i | 99.99 (5) |
O(3)—K(2)—O(14)vii | 140.05 (5) | Cr(2)—O(6)—K(1)iii | 146.48 (10) |
O(4)v—K(2)—O(5)vi | 90.22 (5) | Cr(2)—O(6)—K(2)i | 89.69 (8) |
O(4)v—K(2)—O(6)vi | 66.73 (5) | Cr(2)—O(6)—K(3)xiii | 102.13 (8) |
O(4)v—K(2)—O(7) | 99.45 (5) | K(1)iii—O(6)—K(2)i | 114.18 (6) |
O(4)v—K(2)—O(9)vi | 143.95 (5) | K(1)iii—O(6)—K(3)xiii | 93.47 (5) |
O(4)v—K(2)—O(13)vii | 93.91 (5) | K(2)i—O(6)—K(3)xiii | 106.60 (6) |
O(4)v—K(2)—O(14)vii | 122.45 (5) | Cr(2)—O(7)—K(2) | 120.27 (10) |
O(5)vi—K(2)—O(6)vi | 51.36 (5) | Cr(2)—O(7)—K(3)xiii | 95.83 (8) |
O(5)vi—K(2)—O(7) | 143.07 (6) | K(2)—O(7)—K(3)xiii | 95.70 (6) |
O(5)vi—K(2)—O(9)vi | 70.08 (5) | Cr(3)—O(8)—K(1)ii | 96.66 (7) |
O(5)vi—K(2)—O(13)vii | 101.46 (5) | Cr(3)—O(8)—K(3) | 132.71 (9) |
O(5)vi—K(2)—O(14)vii | 134.47 (5) | Cr(3)—O(8)—K(4)vii | 117.38 (9) |
O(6)vi—K(2)—O(7) | 162.49 (5) | K(1)ii—O(8)—K(3) | 92.44 (5) |
O(6)vi—K(2)—O(9)vi | 77.52 (5) | K(1)ii—O(8)—K(4)vii | 121.40 (6) |
O(6)vi—K(2)—O(13)vii | 59.61 (4) | K(3)—O(8)—K(4)vii | 96.06 (5) |
O(6)vi—K(2)—O(14)vii | 109.72 (5) | Cr(3)—O(9)—K(1)ii | 97.89 (7) |
O(7)—K(2)—O(9)vi | 114.55 (5) | Cr(3)—O(9)—K(2)i | 168.27 (10) |
O(7)—K(2)—O(13)vii | 113.19 (5) | Cr(3)—O(9)—K(4)xii | 101.45 (8) |
O(7)—K(2)—O(14)vii | 67.64 (5) | K(1)ii—O(9)—K(2)i | 89.99 (5) |
O(9)vi—K(2)—O(13)vii | 62.66 (5) | K(1)ii—O(9)—K(4)xii | 104.49 (6) |
O(9)vi—K(2)—O(14)vii | 65.04 (5) | K(2)i—O(9)—K(4)xii | 84.85 (5) |
O(13)vii—K(2)—O(14)vii | 50.70 (5) | Cr(3)—O(10)—K(3)xiii | 122.02 (9) |
O(2)iv—K(3)—O(6)viii | 69.60 (5) | Cr(3)—O(10)—K(4) | 124.82 (9) |
O(2)iv—K(3)—O(7)viii | 68.55 (5) | K(3)xiii—O(10)—K(4) | 100.79 (6) |
O(2)iv—K(3)—O(8) | 68.41 (5) | Cr(3)—O(11)—Cr(4) | 123.97 (8) |
O(2)iv—K(3)—O(10)viii | 138.19 (6) | Cr(3)—O(11)—K(4)xii | 96.85 (6) |
O(2)iv—K(3)—O(12) | 127.25 (6) | Cr(4)—O(11)—K(4)xii | 137.82 (8) |
O(2)iv—K(3)—O(12)ix | 71.75 (5) | Cr(4)—O(12)—K(3) | 131.20 (9) |
O(2)iv—K(3)—O(13)x | 131.37 (5) | Cr(4)—O(12)—K(3)ix | 96.32 (8) |
O(2)iv—K(3)—O(14)ix | 68.56 (5) | Cr(4)—O(12)—K(4)viii | 117.75 (9) |
O(6)viii—K(3)—O(7)viii | 52.22 (5) | K(3)—O(12)—K(3)ix | 113.38 (6) |
O(6)viii—K(3)—O(8) | 85.14 (5) | K(3)—O(12)—K(4)viii | 98.02 (5) |
O(6)viii—K(3)—O(10)viii | 113.49 (5) | K(3)ix—O(12)—K(4)viii | 95.00 (5) |
O(6)viii—K(3)—O(12) | 139.16 (5) | Cr(4)—O(13)—K(2)vii | 88.99 (8) |
O(6)viii—K(3)—O(12)ix | 141.16 (5) | Cr(4)—O(13)—K(3)x | 138.98 (10) |
O(6)viii—K(3)—O(13)x | 69.38 (5) | K(2)vii—O(13)—K(3)x | 106.93 (6) |
O(6)viii—K(3)—O(14)ix | 112.98 (5) | Cr(4)—O(14)—K(2)vii | 109.90 (8) |
O(7)viii—K(3)—O(8) | 127.44 (5) | Cr(4)—O(14)—K(3)ix | 101.07 (7) |
O(7)viii—K(3)—O(10)viii | 81.16 (5) | Cr(4)—O(14)—K(4) | 124.48 (8) |
O(7)viii—K(3)—O(12) | 160.50 (5) | K(2)vii—O(14)—K(3)ix | 104.82 (5) |
O(7)viii—K(3)—O(12)ix | 115.19 (5) | K(2)vii—O(14)—K(4) | 93.89 (5) |
O(7)viii—K(3)—O(13)x | 104.18 (6) | K(3)ix—O(14)—K(4) | 120.72 (6) |
Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x+2, −y+2, −z+1; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+2, −z+1; (vi) x−1, y, z; (vii) −x+1, −y+1, −z; (viii) x, y−1, z; (ix) −x+1, −y, −z; (x) −x+2, −y, −z; (xi) x, y, z−1; (xii) −x+2, −y+1, −z; (xiii) x, y+1, z; (xiv) x, y, z+1. |
Cr(1)—O(1) | 1.611 (2) | K(2)—O(3) | 2.835 (3) |
Cr(1)—O(2) | 1.613 (3) | K(2)—O(4)v | 2.863 (3) |
Cr(1)—O(3) | 1.604 (3) | K(2)—O(5)vi | 2.746 (3) |
Cr(1)—O(4) | 1.788 (3) | K(2)—O(6)vi | 3.239 (3) |
Cr(2)—O(4) | 1.782 (2) | K(2)—O(7) | 2.922 (3) |
Cr(2)—O(5) | 1.615 (2) | K(2)—O(9)vi | 3.085 (3) |
Cr(2)—O(6) | 1.614 (3) | K(2)—O(13)vii | 3.308 (3) |
Cr(2)—O(7) | 1.605 (3) | K(2)—O(14)vii | 2.762 (3) |
Cr(3)—O(8) | 1.618 (3) | K(3)—O(2)iv | 2.859 (3) |
Cr(3)—O(9) | 1.615 (2) | K(3)—O(6)viii | 2.902 (3) |
Cr(3)—O(10) | 1.606 (3) | K(3)—O(7)viii | 3.064 (3) |
Cr(3)—O(11) | 1.778 (2) | K(3)—O(8) | 2.818 (3) |
Cr(4)—O(11) | 1.787 (2) | K(3)—O(10)viii | 2.749 (3) |
Cr(4)—O(12) | 1.619 (3) | K(3)—O(12) | 2.879 (3) |
Cr(4)—O(13) | 1.604 (3) | K(3)—O(12)ix | 2.961 (3) |
Cr(4)—O(14) | 1.619 (2) | K(3)—O(13)x | 2.810 (3) |
K(1)—O(1) | 2.879 (3) | K(3)—O(14)ix | 2.842 (3) |
K(1)—O(3)i | 2.707 (3) | K(4)—O(1)xi | 2.896 (3) |
K(1)—O(5) | 2.714 (3) | K(4)—O(2)xi | 3.138 (3) |
K(1)—O(5)ii | 2.695 (3) | K(4)—O(8)vii | 2.849 (3) |
K(1)—O(6)iii | 2.687 (3) | K(4)—O(9)xii | 2.953 (3) |
K(1)—O(8)ii | 2.831 (3) | K(4)—O(10) | 2.761 (3) |
K(1)—O(9)ii | 2.799 (3) | K(4)—O(11)xii | 2.967 (2) |
K(2)—O(1)iv | 2.847 (3) | K(4)—O(12)xiii | 2.752 (3) |
K(2)—O(2)v | 2.979 (3) | K(4)—O(14) | 2.810 (3) |
O(1)—Cr(1)—O(2) | 109.10 (14) | K(1)—O(5)—K(1)ii | 107.61 (9) |
O(1)—Cr(1)—O(3) | 110.92 (14) | K(1)—O(5)—K(2)i | 104.51 (9) |
O(1)—Cr(1)—O(4) | 110.10 (13) | K(1)ii—O(5)—K(2)i | 99.89 (8) |
O(2)—Cr(1)—O(3) | 110.61 (14) | Cr(2)—O(6)—K(1)iii | 146.63 (15) |
O(2)—Cr(1)—O(4) | 106.72 (13) | Cr(2)—O(6)—K(2)i | 89.56 (11) |
O(3)—Cr(1)—O(4) | 109.31 (13) | Cr(2)—O(6)—K(3)xiii | 101.94 (12) |
O(4)—Cr(2)—O(5) | 108.71 (13) | K(1)iii—O(6)—K(2)i | 114.28 (9) |
O(4)—Cr(2)—O(6) | 109.59 (13) | K(1)iii—O(6)—K(3)xiii | 93.54 (8) |
O(4)—Cr(2)—O(7) | 110.38 (13) | K(2)i—O(6)—K(3)xiii | 106.53 (8) |
O(5)—Cr(2)—O(6) | 109.00 (14) | Cr(2)—O(7)—K(2) | 120.15 (14) |
O(5)—Cr(2)—O(7) | 109.32 (14) | Cr(2)—O(7)—K(3)xiii | 95.82 (12) |
O(6)—Cr(2)—O(7) | 109.81 (14) | K(2)—O(7)—K(3)xiii | 95.73 (8) |
O(8)—Cr(3)—O(9) | 109.34 (13) | Cr(3)—O(8)—K(1)ii | 96.60 (11) |
O(8)—Cr(3)—O(10) | 109.99 (14) | Cr(3)—O(8)—K(3) | 132.76 (13) |
O(8)—Cr(3)—O(11) | 109.07 (12) | Cr(3)—O(8)—K(4)vii | 117.50 (13) |
O(9)—Cr(3)—O(10) | 111.19 (14) | K(1)ii—O(8)—K(3) | 92.33 (8) |
O(9)—Cr(3)—O(11) | 106.57 (12) | K(1)ii—O(8)—K(4)vii | 121.29 (9) |
O(10)—Cr(3)—O(11) | 110.59 (12) | K(3)—O(8)—K(4)vii | 96.09 (8) |
O(11)—Cr(4)—O(12) | 109.63 (12) | Cr(3)—O(9)—K(1)ii | 97.92 (11) |
O(11)—Cr(4)—O(13) | 109.52 (13) | Cr(3)—O(9)—K(2)i | 168.24 (14) |
O(11)—Cr(4)—O(14) | 108.40 (12) | Cr(3)—O(9)—K(4)xii | 101.45 (11) |
O(12)—Cr(4)—O(13) | 110.65 (14) | K(1)ii—O(9)—K(2)i | 90.01 (7) |
O(12)—Cr(4)—O(14) | 108.50 (13) | K(1)ii—O(9)—K(4)xii | 104.54 (9) |
O(13)—Cr(4)—O(14) | 110.10 (14) | K(2)i—O(9)—K(4)xii | 84.82 (7) |
O(12)xiii—K(4)—O(14) | 157.10 (8) | Cr(3)—O(10)—K(3)xiii | 122.12 (14) |
Cr(1)—O(1)—K(1) | 114.41 (13) | Cr(3)—O(10)—K(4) | 124.79 (13) |
Cr(1)—O(1)—K(2)iv | 144.37 (15) | K(3)xiii—O(10)—K(4) | 100.88 (9) |
Cr(1)—O(1)—K(4)xiv | 103.20 (12) | Cr(3)—O(11)—Cr(4) | 124.19 (13) |
K(1)—O(1)—K(2)iv | 93.35 (8) | Cr(3)—O(11)—K(4)xii | 96.82 (9) |
K(1)—O(1)—K(4)xiv | 103.98 (9) | Cr(4)—O(11)—K(4)xii | 137.61 (11) |
K(2)iv—O(1)—K(4)xiv | 90.34 (8) | Cr(4)—O(12)—K(3) | 131.24 (13) |
Cr(1)—O(2)—K(2)v | 98.71 (12) | Cr(4)—O(12)—K(3)ix | 96.38 (11) |
Cr(1)—O(2)—K(3)iv | 155.11 (15) | Cr(4)—O(12)—K(4)viii | 117.77 (13) |
Cr(1)—O(2)—K(4)xiv | 93.77 (11) | K(3)—O(12)—K(3)ix | 113.36 (9) |
K(2)v—O(2)—K(3)iv | 99.02 (8) | K(3)—O(12)—K(4)viii | 97.92 (8) |
K(2)v—O(2)—K(4)xiv | 127.43 (10) | K(3)ix—O(12)—K(4)viii | 95.01 (8) |
K(3)iv—O(2)—K(4)xiv | 89.19 (7) | Cr(4)—O(13)—K(2)vii | 88.94 (11) |
Cr(1)—O(3)—K(1)vi | 119.56 (14) | Cr(4)—O(13)—K(3)x | 139.24 (15) |
Cr(1)—O(3)—K(2) | 124.99 (14) | K(2)vii—O(13)—K(3)x | 106.93 (9) |
K(1)vi—O(3)—K(2) | 102.34 (9) | Cr(4)—O(14)—K(2)vii | 110.09 (12) |
Cr(1)—O(4)—Cr(2) | 127.29 (14) | Cr(4)—O(14)—K(3)ix | 101.01 (11) |
Cr(1)—O(4)—K(2)v | 98.65 (10) | Cr(4)—O(14)—K(4) | 124.55 (12) |
Cr(2)—O(4)—K(2)v | 133.52 (12) | K(2)vii—O(14)—K(3)ix | 104.82 (8) |
Cr(2)—O(5)—K(1) | 119.78 (12) | K(2)vii—O(14)—K(4) | 93.94 (8) |
Cr(2)—O(5)—K(1)ii | 113.98 (13) | K(3)ix—O(14)—K(4) | 120.54 (9) |
Cr(2)—O(5)—K(2)i | 108.81 (12) |
Symmetry codes: (i) x+1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x+2, −y+2, −z+1; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y+2, −z+1; (vi) x−1, y, z; (vii) −x+1, −y+1, −z; (viii) x, y−1, z; (ix) −x+1, −y, −z; (x) −x+2, −y, −z; (xi) x, y, z−1; (xii) −x+2, −y+1, −z; (xiii) x, y+1, z; (xiv) x, y, z+1. |
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Normal probability analysis shows the present coordinates do not differ significantly from the two earlier studies but that the latter systematically underestimate the uncertainties in these values by a factor \sim2. Measurement with a Perkin-Elmer Pyris-1 T GA reveals an insignificant loss of mass on first heating until TPT is reached. A sharp and reproducible mass loss of ~0.20%, based on several samples, occurs between TPT and 544 K. The thermal hysteresis and entropy change at TPT), measured with a Perkin-Elmer DSC-7 at heating rates ranging from 1 to 100 K min−1, agree with the values reported by Hess & Eysel (1989) except for the initial results on heating. A reproducible endothermic phase transition at 544 (2) K, on extrapolation to 0 K min−1 heating rate, is observed on solution-grown samples. The exothermic transition on cooling thereafter is reproducibly observed at 502 (2) K, the endothermic transition on second and subsequent heatings at 531 (2) K. The increase in TPT of 13 K is caused by the \sim5MPa pressure exerted by water at 531 K. The thermal hysteresis ranges from ~32 K at the lowest to ~80 K at the highest heating rate, isothermally extrapolating to ~29 K and is indicative of a first order phase transition. The averaged entropy change both at the initial and subsequent T(PT) is ΔS = 4.0 (1) J mol−1 K−1.
The component and total coordinate differences between phases II and IIb exceed the Δ(xyz)max < approx. 1.5 Å limit for reversible solid state phase transitions Corresponding angular changes are also unusually large, with Cr3O4 and Cr42O4 tetrahedral rotations of 67 and 81° around their respective Cr-Oshared-axes. Atomic position changes of such magnitude are highly unlikely, as is the possibility of a transition between phases II and IIb.
The unit cell and space group of monoclinic phase I determined at 573 K by Klement & Schwab (1960) has a supergroup-subgroup and unit cell relationship to phase II that allows a transition between the two phases. An inferred structure for phase I has been derived from phase II by assuming pairs of atoms related by the n glide plane in phase I undergo equal but opposite displacements at the transition. In the transition, the three terminal O atoms in each tetrahedron undergo a rotation of \sim60° about the Oshared-Cr- axis, with respect to the Cr—O—Cr plane. In consequence, the conformation of the Cr2O72− ion changes to that reported in one of the two independent ions in SrCr2O7 (Wilhelmi, 1967). No difference between corresponding atomic positions in phases I and II exceeds the Δ(xyz)max limit by more than 3 estimated uncertainties.
No atomic position in phase II differs from that inferred for the same atom in phase I by more than the Δ(xyz)max limit, the differences for K2 and O7 being without significance. The transition between phases I and II is, hence, probably of first order. If, however, TPT<<531 K, as suggested by Kozlova et al. (1978), then a new phase would be expected to intervene between phases IIb and I since a lower value for TPT would require phase I to be stable below its thermal limit.