Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806029898/ez2017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806029898/ez2017Isup2.hkl |
CCDC reference: 620958
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- Disorder in solvent or counterion
- R factor = 0.032
- wR factor = 0.085
- Data-to-parameter ratio = 13.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT395_ALERT_2_B Deviating X-O-Y Angle from 120 Deg for O3W 166.50 Deg. PLAT415_ALERT_2_B Short Inter D-H..H-X H12B .. H51 .. 2.04 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H22 .. H32 .. 1.46 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H31 .. H42 .. 1.66 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.10 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 33.00 Perc. PLAT417_ALERT_2_C Short Inter D-H..H-D H22 .. H31 .. 2.11 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact C31 .. O5W .. 2.97 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H51 .. F11 .. 2.61 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H52 .. O31 .. 2.64 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C14 H18 F7 Fe3 O17 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 H2 O
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.
[Fe3(C2H2FO2)7O(H2O)2]·2H2O | F(000) = 1596 |
Mr = 794.87 | Dx = 1.898 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8000 reflections |
a = 17.9617 (15) Å | θ = 2.3–26° |
b = 10.6921 (5) Å | µ = 1.67 mm−1 |
c = 15.5496 (13) Å | T = 293 K |
β = 111.329 (9)° | Block, red |
V = 2781.7 (4) Å3 | 0.48 × 0.35 × 0.30 mm |
Z = 4 |
Stoe IPDS area-detector diffractometer | 5450 independent reflections |
Radiation source: fine-focus sealed tube | 4281 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
φ scans | θmax = 26.1°, θmin = 2.3° |
Absorption correction: multi-scan (Blessing, 1995) | h = −22→22 |
Tmin = 0.552, Tmax = 0.606 | k = −13→13 |
38802 measured reflections | l = −19→19 |
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0589P)2] where P = (Fo2 + 2Fc2)/3 |
5450 reflections | (Δ/σ)max = 0.001 |
410 parameters | Δρmax = 0.66 e Å−3 |
6 restraints | Δρmin = −0.52 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.20796 (2) | −0.40836 (3) | 0.53695 (2) | 0.02400 (10) | |
Fe2 | 0.28430 (2) | −0.31814 (3) | 0.38537 (2) | 0.02420 (10) | |
Fe3 | 0.24172 (2) | −0.61838 (3) | 0.39772 (2) | 0.02451 (10) | |
F11 | 0.14541 (16) | −0.5973 (2) | 0.08229 (14) | 0.0685 (7) | |
F21 | 0.52501 (12) | −0.4647 (2) | 0.3888 (2) | 0.0789 (8) | |
F31 | 0.47367 (14) | −0.1344 (3) | 0.64504 (18) | 0.0791 (7) | |
F41 | −0.00352 (13) | −0.7677 (2) | 0.37202 (17) | 0.0716 (7) | |
F51 | 0.01433 (12) | −0.1123 (2) | 0.39736 (18) | 0.0675 (6) | |
F61 | 0.3612 (2) | −0.8336 (3) | 0.67073 (17) | 0.1089 (12) | |
F71 | 0.07085 (13) | −0.9228 (2) | 0.18091 (14) | 0.0587 (5) | |
O1 | 0.24455 (10) | −0.44816 (16) | 0.43900 (11) | 0.0242 (4) | |
O1W | 0.17124 (11) | −0.36300 (18) | 0.64477 (12) | 0.0285 (4) | |
H11 | 0.1922 (19) | −0.290 (2) | 0.675 (2) | 0.043* | |
H12 | 0.1774 (19) | −0.430 (2) | 0.6867 (19) | 0.043* | |
O2W | 0.32448 (12) | −0.1700 (2) | 0.33012 (14) | 0.0370 (5) | |
H21 | 0.2976 (18) | −0.091 (2) | 0.321 (3) | 0.056* | |
H22 | 0.3786 (11) | −0.149 (3) | 0.351 (2) | 0.056* | |
O11 | 0.19937 (13) | −0.56971 (19) | 0.26202 (13) | 0.0379 (5) | |
O12 | 0.21965 (12) | −0.36533 (19) | 0.25133 (12) | 0.0350 (4) | |
O21 | 0.35389 (12) | −0.61340 (19) | 0.39521 (15) | 0.0396 (5) | |
O22 | 0.37895 (12) | −0.41239 (19) | 0.37750 (15) | 0.0374 (5) | |
O31 | 0.36141 (11) | −0.2514 (2) | 0.50832 (13) | 0.0364 (5) | |
O32 | 0.28509 (12) | −0.2682 (2) | 0.59271 (14) | 0.0399 (5) | |
O41 | 0.11983 (12) | −0.53240 (19) | 0.50783 (14) | 0.0360 (5) | |
O42 | 0.12902 (12) | −0.6473 (2) | 0.39246 (14) | 0.0369 (5) | |
O51 | 0.19513 (12) | −0.20114 (19) | 0.37805 (14) | 0.0370 (5) | |
O52 | 0.12815 (11) | −0.27883 (19) | 0.46199 (13) | 0.0345 (4) | |
O61 | 0.28734 (13) | −0.68758 (19) | 0.52769 (13) | 0.0391 (5) | |
O62 | 0.28392 (13) | −0.5315 (2) | 0.62217 (13) | 0.0422 (5) | |
O71 | 0.24056 (12) | −0.79348 (18) | 0.35490 (13) | 0.0347 (4) | |
O72 | 0.21917 (14) | −0.97388 (19) | 0.28278 (15) | 0.0435 (5) | |
C11 | 0.19478 (15) | −0.4715 (3) | 0.21792 (17) | 0.0295 (6) | |
C12 | 0.1567 (2) | −0.4769 (3) | 0.1149 (2) | 0.0490 (8) | |
H12A | 0.1055 | −0.4345 | 0.0954 | 0.059* | |
H12B | 0.1903 | −0.4330 | 0.0881 | 0.059* | |
C21 | 0.39627 (15) | −0.5254 (3) | 0.38618 (18) | 0.0306 (6) | |
C22 | 0.47651 (17) | −0.5649 (3) | 0.3846 (2) | 0.0457 (8) | |
H22A | 0.5025 | −0.6197 | 0.4366 | 0.055* | |
H22B | 0.4685 | −0.6115 | 0.3285 | 0.055* | |
C31 | 0.34655 (16) | −0.2322 (3) | 0.57944 (18) | 0.0315 (6) | |
C32 | 0.4042 (2) | −0.1605 (4) | 0.6584 (3) | 0.0565 (10) | |
H32A | 0.3795 | −0.0828 | 0.6661 | 0.068* | |
H32B | 0.4163 | −0.2088 | 0.7147 | 0.068* | |
C41 | 0.09564 (15) | −0.6148 (2) | 0.44653 (18) | 0.0276 (5) | |
C42 | 0.01969 (18) | −0.6787 (3) | 0.4409 (2) | 0.0396 (7) | |
H42A | 0.0273 | −0.7182 | 0.4996 | 0.048* | |
H42B | −0.0223 | −0.6168 | 0.4292 | 0.048* | |
C51 | 0.13732 (15) | −0.2053 (3) | 0.40499 (18) | 0.0290 (6) | |
C52 | 0.0747 (2) | −0.1072 (4) | 0.3632 (3) | 0.0507 (9) | |
H52A | 0.0994 | −0.0252 | 0.3756 | 0.061* | |
H52B | 0.0523 | −0.1185 | 0.2967 | 0.061* | |
C61 | 0.30238 (16) | −0.6389 (3) | 0.60550 (18) | 0.0327 (6) | |
C62 | 0.3471 (2) | −0.7146 (4) | 0.6904 (2) | 0.0568 (10) | |
H62A | 0.3978 | −0.6740 | 0.7237 | 0.068* | |
H62B | 0.3165 | −0.7161 | 0.7305 | 0.068* | |
C71 | 0.19669 (18) | −0.8694 (3) | 0.29435 (18) | 0.0313 (6) | |
C72 | 0.1141 (2) | −0.8270 (3) | 0.2345 (2) | 0.0481 (8) | |
H72A | 0.0864 | −0.7957 | 0.2733 | 0.058* | |
H72B | 0.1182 | −0.7592 | 0.1950 | 0.058* | |
O3W | 0.4788 (3) | −0.1488 (9) | 0.3750 (8) | 0.294 (6) | |
H31 | 0.4924 | −0.0735 | 0.3710 | 0.441* | |
H32 | 0.4546 | −0.2164 | 0.3770 | 0.441* | |
O4W | 0.6078 (7) | −0.0879 (9) | 0.5150 (7) | 0.274 (10) | 0.748 (10) |
H41 | 0.6360 | −0.1445 | 0.5504 | 0.411* | 0.748 (10) |
H42 | 0.5653 | −0.1069 | 0.4703 | 0.411* | 0.748 (10) |
O5W | 0.2875 (10) | −0.5207 (10) | 0.0067 (8) | 0.084 (6) | 0.252 (10) |
H51 | 0.2736 | −0.5288 | 0.0531 | 0.126* | 0.252 (10) |
H52 | 0.2707 | −0.4501 | −0.0178 | 0.126* | 0.252 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.02859 (19) | 0.0218 (2) | 0.02261 (18) | 0.00050 (14) | 0.01054 (14) | −0.00161 (14) |
Fe2 | 0.02598 (18) | 0.0219 (2) | 0.02622 (19) | 0.00019 (14) | 0.01132 (14) | 0.00046 (14) |
Fe3 | 0.03087 (19) | 0.01914 (19) | 0.02415 (18) | 0.00116 (14) | 0.01076 (14) | −0.00168 (14) |
F11 | 0.0996 (18) | 0.0566 (14) | 0.0391 (11) | −0.0211 (12) | 0.0132 (11) | −0.0155 (9) |
F21 | 0.0411 (11) | 0.0734 (17) | 0.133 (2) | −0.0095 (11) | 0.0440 (13) | −0.0133 (15) |
F31 | 0.0511 (13) | 0.100 (2) | 0.0768 (16) | −0.0307 (13) | 0.0119 (11) | −0.0226 (14) |
F41 | 0.0603 (13) | 0.0760 (17) | 0.0864 (16) | −0.0381 (12) | 0.0363 (12) | −0.0419 (13) |
F51 | 0.0453 (11) | 0.0733 (16) | 0.0961 (17) | 0.0262 (10) | 0.0403 (11) | 0.0293 (13) |
F61 | 0.180 (3) | 0.0788 (19) | 0.0585 (15) | 0.080 (2) | 0.0322 (17) | 0.0249 (13) |
F71 | 0.0620 (12) | 0.0468 (12) | 0.0547 (12) | −0.0077 (10) | 0.0064 (10) | −0.0193 (9) |
O1 | 0.0284 (9) | 0.0206 (9) | 0.0244 (8) | 0.0005 (7) | 0.0106 (7) | −0.0012 (7) |
O1W | 0.0382 (10) | 0.0234 (10) | 0.0251 (9) | −0.0012 (8) | 0.0128 (8) | −0.0011 (7) |
O2W | 0.0374 (11) | 0.0312 (11) | 0.0449 (11) | −0.0030 (9) | 0.0179 (9) | 0.0064 (9) |
O11 | 0.0577 (13) | 0.0263 (11) | 0.0274 (9) | −0.0038 (9) | 0.0126 (9) | 0.0001 (8) |
O12 | 0.0473 (11) | 0.0286 (11) | 0.0260 (9) | −0.0076 (9) | 0.0096 (8) | 0.0009 (8) |
O21 | 0.0351 (11) | 0.0320 (12) | 0.0558 (13) | 0.0027 (9) | 0.0216 (10) | −0.0050 (9) |
O22 | 0.0365 (10) | 0.0333 (12) | 0.0499 (12) | 0.0042 (9) | 0.0246 (9) | 0.0027 (9) |
O31 | 0.0316 (10) | 0.0426 (12) | 0.0357 (11) | −0.0067 (9) | 0.0132 (8) | −0.0071 (9) |
O32 | 0.0431 (11) | 0.0417 (13) | 0.0405 (11) | −0.0138 (10) | 0.0217 (9) | −0.0160 (9) |
O41 | 0.0426 (11) | 0.0332 (12) | 0.0396 (11) | −0.0120 (9) | 0.0240 (9) | −0.0117 (9) |
O42 | 0.0367 (10) | 0.0382 (12) | 0.0399 (11) | −0.0087 (9) | 0.0188 (9) | −0.0144 (9) |
O51 | 0.0374 (11) | 0.0309 (11) | 0.0486 (12) | 0.0077 (8) | 0.0227 (9) | 0.0127 (9) |
O52 | 0.0364 (10) | 0.0347 (11) | 0.0355 (10) | 0.0081 (8) | 0.0169 (8) | 0.0087 (9) |
O61 | 0.0570 (13) | 0.0288 (11) | 0.0283 (10) | 0.0084 (9) | 0.0116 (9) | 0.0033 (8) |
O62 | 0.0531 (13) | 0.0414 (13) | 0.0284 (10) | 0.0187 (10) | 0.0104 (9) | 0.0010 (9) |
O71 | 0.0436 (11) | 0.0224 (10) | 0.0349 (10) | 0.0020 (8) | 0.0105 (9) | −0.0048 (8) |
O72 | 0.0601 (13) | 0.0216 (11) | 0.0462 (12) | 0.0060 (10) | 0.0163 (10) | −0.0074 (9) |
C11 | 0.0310 (13) | 0.0318 (16) | 0.0254 (13) | −0.0019 (11) | 0.0101 (11) | 0.0006 (11) |
C12 | 0.066 (2) | 0.046 (2) | 0.0275 (15) | −0.0148 (17) | 0.0076 (14) | −0.0011 (13) |
C21 | 0.0267 (13) | 0.0366 (17) | 0.0272 (13) | 0.0027 (11) | 0.0085 (10) | −0.0071 (11) |
C22 | 0.0311 (15) | 0.052 (2) | 0.0535 (19) | 0.0041 (14) | 0.0151 (14) | −0.0134 (16) |
C31 | 0.0295 (13) | 0.0286 (15) | 0.0325 (14) | −0.0002 (11) | 0.0065 (11) | −0.0055 (11) |
C32 | 0.0441 (18) | 0.070 (3) | 0.052 (2) | −0.0171 (17) | 0.0134 (15) | −0.0241 (18) |
C41 | 0.0291 (13) | 0.0235 (14) | 0.0296 (13) | 0.0004 (11) | 0.0101 (10) | 0.0016 (10) |
C42 | 0.0376 (15) | 0.0397 (18) | 0.0440 (16) | −0.0117 (13) | 0.0177 (13) | −0.0107 (13) |
C51 | 0.0293 (13) | 0.0275 (14) | 0.0300 (13) | 0.0045 (11) | 0.0106 (11) | 0.0005 (11) |
C52 | 0.0432 (17) | 0.057 (2) | 0.060 (2) | 0.0213 (16) | 0.0278 (16) | 0.0260 (17) |
C61 | 0.0322 (14) | 0.0374 (17) | 0.0275 (14) | 0.0069 (12) | 0.0099 (11) | 0.0040 (12) |
C62 | 0.071 (2) | 0.059 (2) | 0.0353 (17) | 0.034 (2) | 0.0128 (16) | 0.0101 (16) |
C71 | 0.0469 (16) | 0.0239 (15) | 0.0285 (13) | −0.0003 (12) | 0.0202 (12) | −0.0016 (11) |
C72 | 0.0515 (19) | 0.0331 (18) | 0.0483 (18) | 0.0007 (15) | 0.0045 (15) | −0.0124 (14) |
O3W | 0.098 (4) | 0.298 (11) | 0.497 (16) | −0.082 (5) | 0.121 (7) | 0.010 (10) |
O4W | 0.293 (15) | 0.180 (9) | 0.191 (9) | 0.162 (10) | −0.101 (9) | −0.050 (7) |
O5W | 0.163 (16) | 0.032 (6) | 0.053 (7) | −0.034 (7) | 0.035 (8) | −0.006 (5) |
Fe1—O1 | 1.9134 (17) | O41—C41 | 1.254 (3) |
Fe1—O41 | 1.9871 (19) | O42—C41 | 1.247 (3) |
Fe1—O62 | 2.009 (2) | O51—C51 | 1.254 (3) |
Fe1—O32 | 2.011 (2) | O52—C51 | 1.240 (3) |
Fe1—O52 | 2.0288 (19) | O61—C61 | 1.253 (3) |
Fe1—O1W | 2.0702 (18) | O62—C61 | 1.248 (4) |
Fe2—O1 | 1.8896 (17) | O71—C71 | 1.275 (3) |
Fe2—O51 | 2.003 (2) | O72—C71 | 1.223 (3) |
Fe2—O22 | 2.018 (2) | C11—C12 | 1.497 (4) |
Fe2—O31 | 2.0386 (19) | C12—H12A | 0.9700 |
Fe2—O12 | 2.0461 (19) | C12—H12B | 0.9700 |
Fe2—O2W | 2.054 (2) | C21—C22 | 1.510 (4) |
Fe3—O1 | 1.9244 (17) | C22—H22A | 0.9700 |
Fe3—O71 | 1.9847 (19) | C22—H22B | 0.9700 |
Fe3—O42 | 2.0199 (19) | C31—C32 | 1.498 (4) |
Fe3—O61 | 2.0245 (19) | C32—H32A | 0.9700 |
Fe3—O21 | 2.030 (2) | C32—H32B | 0.9700 |
Fe3—O11 | 2.033 (2) | C41—C42 | 1.499 (4) |
F11—C12 | 1.371 (4) | C42—H42A | 0.9700 |
F21—C22 | 1.367 (4) | C42—H42B | 0.9700 |
F31—C32 | 1.366 (4) | C51—C52 | 1.502 (4) |
F41—C42 | 1.379 (4) | C52—H52A | 0.9700 |
F51—C52 | 1.371 (4) | C52—H52B | 0.9700 |
F61—C62 | 1.354 (5) | C61—C62 | 1.507 (4) |
F71—C72 | 1.369 (4) | C62—H62A | 0.9700 |
O1W—H11 | 0.922 (18) | C62—H62B | 0.9700 |
O1W—H12 | 0.946 (17) | C71—C72 | 1.506 (4) |
O2W—H21 | 0.959 (18) | C72—H72A | 0.9700 |
O2W—H22 | 0.935 (18) | C72—H72B | 0.9700 |
O11—C11 | 1.241 (3) | O3W—H31 | 0.8499 |
O12—C11 | 1.260 (3) | O3W—H32 | 0.8502 |
O21—C21 | 1.250 (4) | O4W—H41 | 0.8500 |
O22—C21 | 1.243 (4) | O4W—H42 | 0.8494 |
O31—C31 | 1.245 (3) | O5W—H51 | 0.8500 |
O32—C31 | 1.255 (3) | O5W—H52 | 0.8500 |
O1—Fe1—O41 | 98.39 (8) | O11—C11—O12 | 126.3 (2) |
O1—Fe1—O62 | 91.82 (8) | O11—C11—C12 | 118.1 (3) |
O41—Fe1—O62 | 90.37 (10) | O12—C11—C12 | 115.6 (2) |
O1—Fe1—O32 | 97.29 (8) | F11—C12—C11 | 112.4 (3) |
O41—Fe1—O32 | 164.27 (8) | F11—C12—H12A | 109.1 |
O62—Fe1—O32 | 90.47 (10) | C11—C12—H12A | 109.1 |
O1—Fe1—O52 | 94.01 (8) | F11—C12—H12B | 109.1 |
O41—Fe1—O52 | 89.25 (9) | C11—C12—H12B | 109.1 |
O62—Fe1—O52 | 174.15 (8) | H12A—C12—H12B | 107.9 |
O32—Fe1—O52 | 88.33 (9) | O22—C21—O21 | 127.3 (2) |
O1—Fe1—O1W | 178.49 (8) | O22—C21—C22 | 118.2 (3) |
O41—Fe1—O1W | 83.04 (8) | O21—C21—C22 | 114.5 (3) |
O62—Fe1—O1W | 87.67 (8) | F21—C22—C21 | 112.1 (3) |
O32—Fe1—O1W | 81.29 (8) | F21—C22—H22A | 109.2 |
O52—Fe1—O1W | 86.48 (8) | C21—C22—H22A | 109.2 |
O1—Fe2—O51 | 93.55 (8) | F21—C22—H22B | 109.2 |
O1—Fe2—O22 | 96.97 (8) | C21—C22—H22B | 109.2 |
O51—Fe2—O22 | 169.27 (8) | H22A—C22—H22B | 107.9 |
O1—Fe2—O31 | 94.61 (8) | O31—C31—O32 | 125.5 (2) |
O51—Fe2—O31 | 95.23 (9) | O31—C31—C32 | 120.3 (3) |
O22—Fe2—O31 | 86.08 (8) | O32—C31—C32 | 114.2 (3) |
O1—Fe2—O12 | 95.89 (8) | F31—C32—C31 | 112.2 (3) |
O51—Fe2—O12 | 87.15 (9) | F31—C32—H32A | 109.2 |
O22—Fe2—O12 | 89.64 (9) | C31—C32—H32A | 109.2 |
O31—Fe2—O12 | 169.07 (8) | F31—C32—H32B | 109.2 |
O1—Fe2—O2W | 176.89 (8) | C31—C32—H32B | 109.2 |
O51—Fe2—O2W | 83.68 (8) | H32A—C32—H32B | 107.9 |
O22—Fe2—O2W | 85.86 (8) | O42—C41—O41 | 126.2 (2) |
O31—Fe2—O2W | 84.27 (8) | O42—C41—C42 | 119.0 (2) |
O12—Fe2—O2W | 85.40 (8) | O41—C41—C42 | 114.9 (2) |
O1—Fe3—O71 | 179.03 (8) | F41—C42—C41 | 111.8 (2) |
O1—Fe3—O42 | 93.61 (8) | F41—C42—H42A | 109.3 |
O71—Fe3—O42 | 87.34 (8) | C41—C42—H42A | 109.3 |
O1—Fe3—O61 | 93.48 (8) | F41—C42—H42B | 109.3 |
O71—Fe3—O61 | 86.63 (8) | C41—C42—H42B | 109.3 |
O42—Fe3—O61 | 91.15 (9) | H42A—C42—H42B | 107.9 |
O1—Fe3—O21 | 94.34 (8) | O52—C51—O51 | 127.1 (3) |
O71—Fe3—O21 | 84.70 (8) | O52—C51—C52 | 118.6 (2) |
O42—Fe3—O21 | 172.01 (8) | O51—C51—C52 | 114.3 (2) |
O61—Fe3—O21 | 89.12 (9) | F51—C52—C51 | 112.2 (3) |
O1—Fe3—O11 | 93.36 (8) | F51—C52—H52A | 109.2 |
O71—Fe3—O11 | 86.50 (8) | C51—C52—H52A | 109.2 |
O42—Fe3—O11 | 90.35 (9) | F51—C52—H52B | 109.2 |
O61—Fe3—O11 | 172.89 (8) | C51—C52—H52B | 109.2 |
O21—Fe3—O11 | 88.44 (9) | H52A—C52—H52B | 107.9 |
Fe2—O1—Fe1 | 118.82 (9) | O62—C61—O61 | 127.0 (3) |
Fe2—O1—Fe3 | 121.13 (9) | O62—C61—C62 | 114.1 (3) |
Fe1—O1—Fe3 | 120.05 (9) | O61—C61—C62 | 118.8 (3) |
Fe1—O1W—H11 | 115 (2) | F61—C62—C61 | 112.9 (3) |
Fe1—O1W—H12 | 113 (2) | F61—C62—H62A | 109.0 |
H11—O1W—H12 | 112 (3) | C61—C62—H62A | 109.0 |
Fe2—O2W—H21 | 121 (2) | F61—C62—H62B | 109.0 |
Fe2—O2W—H22 | 122 (2) | C61—C62—H62B | 109.0 |
H21—O2W—H22 | 104 (3) | H62A—C62—H62B | 107.8 |
C11—O11—Fe3 | 135.63 (18) | O72—C71—O71 | 122.8 (3) |
C11—O12—Fe2 | 128.80 (17) | O72—C71—C72 | 119.2 (3) |
C21—O21—Fe3 | 132.16 (18) | O71—C71—C72 | 118.1 (2) |
C21—O22—Fe2 | 131.46 (19) | F71—C72—C71 | 111.4 (3) |
C31—O31—Fe2 | 126.77 (17) | F71—C72—H72A | 109.4 |
C31—O32—Fe1 | 131.80 (18) | C71—C72—H72A | 109.4 |
C41—O41—Fe1 | 132.02 (17) | F71—C72—H72B | 109.4 |
C41—O42—Fe3 | 130.59 (17) | C71—C72—H72B | 109.4 |
C51—O51—Fe2 | 134.53 (18) | H72A—C72—H72B | 108.0 |
C51—O52—Fe1 | 126.43 (17) | H31—O3W—H32 | 166.5 |
C61—O61—Fe3 | 132.77 (19) | H41—O4W—H42 | 120.4 |
C61—O62—Fe1 | 129.34 (18) | H51—O5W—H52 | 107.7 |
C71—O71—Fe3 | 140.92 (19) | ||
O51—Fe2—O1—Fe1 | −44.60 (11) | O1—Fe2—O51—C51 | 5.1 (3) |
O22—Fe2—O1—Fe1 | 137.55 (10) | O22—Fe2—O51—C51 | 173.6 (4) |
O31—Fe2—O1—Fe1 | 50.95 (11) | O31—Fe2—O51—C51 | −89.8 (3) |
O12—Fe2—O1—Fe1 | −132.09 (10) | O12—Fe2—O51—C51 | 100.9 (3) |
O51—Fe2—O1—Fe3 | 136.17 (11) | O2W—Fe2—O51—C51 | −173.4 (3) |
O22—Fe2—O1—Fe3 | −41.68 (12) | O1—Fe1—O52—C51 | −36.8 (2) |
O31—Fe2—O1—Fe3 | −128.29 (10) | O41—Fe1—O52—C51 | −135.1 (2) |
O12—Fe2—O1—Fe3 | 48.67 (11) | O32—Fe1—O52—C51 | 60.4 (2) |
O41—Fe1—O1—Fe2 | 145.89 (10) | O1W—Fe1—O52—C51 | 141.8 (2) |
O62—Fe1—O1—Fe2 | −123.47 (11) | O1—Fe3—O61—C61 | 7.6 (3) |
O32—Fe1—O1—Fe2 | −32.77 (11) | O71—Fe3—O61—C61 | −173.4 (3) |
O52—Fe1—O1—Fe2 | 56.06 (11) | O42—Fe3—O61—C61 | −86.1 (3) |
O41—Fe1—O1—Fe3 | −34.87 (11) | O21—Fe3—O61—C61 | 101.9 (3) |
O62—Fe1—O1—Fe3 | 55.77 (11) | O1—Fe1—O62—C61 | −40.9 (3) |
O32—Fe1—O1—Fe3 | 146.48 (11) | O41—Fe1—O62—C61 | 57.5 (3) |
O52—Fe1—O1—Fe3 | −124.70 (10) | O32—Fe1—O62—C61 | −138.2 (3) |
O42—Fe3—O1—Fe2 | −134.27 (11) | O1W—Fe1—O62—C61 | 140.5 (3) |
O61—Fe3—O1—Fe2 | 134.35 (11) | O42—Fe3—O71—C71 | 46.6 (3) |
O21—Fe3—O1—Fe2 | 44.97 (11) | O61—Fe3—O71—C71 | 137.9 (3) |
O11—Fe3—O1—Fe2 | −43.71 (11) | O21—Fe3—O71—C71 | −132.7 (3) |
O42—Fe3—O1—Fe1 | 46.51 (11) | O11—Fe3—O71—C71 | −43.9 (3) |
O61—Fe3—O1—Fe1 | −44.87 (11) | Fe3—O11—C11—O12 | 1.3 (5) |
O21—Fe3—O1—Fe1 | −134.25 (11) | Fe3—O11—C11—C12 | −179.1 (2) |
O11—Fe3—O1—Fe1 | 137.07 (11) | Fe2—O12—C11—O11 | 6.2 (4) |
O1—Fe3—O11—C11 | 16.4 (3) | Fe2—O12—C11—C12 | −173.4 (2) |
O71—Fe3—O11—C11 | −162.7 (3) | O11—C11—C12—F11 | −11.6 (4) |
O42—Fe3—O11—C11 | 110.0 (3) | O12—C11—C12—F11 | 168.0 (3) |
O21—Fe3—O11—C11 | −77.9 (3) | Fe2—O22—C21—O21 | 6.4 (4) |
O1—Fe2—O12—C11 | −28.9 (2) | Fe2—O22—C21—C22 | −174.6 (2) |
O51—Fe2—O12—C11 | −122.1 (2) | Fe3—O21—C21—O22 | 1.3 (4) |
O22—Fe2—O12—C11 | 68.1 (2) | Fe3—O21—C21—C22 | −177.7 (2) |
O31—Fe2—O12—C11 | 134.9 (4) | O22—C21—C22—F21 | 10.1 (4) |
O2W—Fe2—O12—C11 | 154.0 (2) | O21—C21—C22—F21 | −170.7 (3) |
O1—Fe3—O21—C21 | −25.3 (3) | Fe2—O31—C31—O32 | 11.5 (4) |
O71—Fe3—O21—C21 | 154.6 (3) | Fe2—O31—C31—C32 | −168.3 (2) |
O61—Fe3—O21—C21 | −118.7 (3) | Fe1—O32—C31—O31 | 23.5 (5) |
O11—Fe3—O21—C21 | 68.0 (3) | Fe1—O32—C31—C32 | −156.7 (3) |
O1—Fe2—O22—C21 | 13.4 (3) | O31—C31—C32—F31 | −6.4 (5) |
O51—Fe2—O22—C21 | −155.0 (4) | O32—C31—C32—F31 | 173.7 (3) |
O31—Fe2—O22—C21 | 107.6 (3) | Fe3—O42—C41—O41 | 16.6 (4) |
O12—Fe2—O22—C21 | −82.5 (3) | Fe3—O42—C41—C42 | −162.7 (2) |
O2W—Fe2—O22—C21 | −167.9 (3) | Fe1—O41—C41—O42 | 8.3 (4) |
O1—Fe2—O31—C31 | −45.9 (2) | Fe1—O41—C41—C42 | −172.4 (2) |
O51—Fe2—O31—C31 | 48.1 (2) | O42—C41—C42—F41 | −0.8 (4) |
O22—Fe2—O31—C31 | −142.5 (2) | O41—C41—C42—F41 | 179.8 (3) |
O12—Fe2—O31—C31 | 150.3 (4) | Fe1—O52—C51—O51 | 4.7 (4) |
O2W—Fe2—O31—C31 | 131.2 (2) | Fe1—O52—C51—C52 | −173.9 (2) |
O1—Fe1—O32—C31 | −11.4 (3) | Fe2—O51—C51—O52 | 15.5 (5) |
O41—Fe1—O32—C31 | 173.5 (3) | Fe2—O51—C51—C52 | −165.8 (2) |
O62—Fe1—O32—C31 | 80.5 (3) | O52—C51—C52—F51 | 1.2 (5) |
O52—Fe1—O32—C31 | −105.2 (3) | O51—C51—C52—F51 | −177.6 (3) |
O1W—Fe1—O32—C31 | 168.1 (3) | Fe1—O62—C61—O61 | 12.5 (5) |
O1—Fe1—O41—C41 | 1.8 (3) | Fe1—O62—C61—C62 | −167.2 (2) |
O62—Fe1—O41—C41 | −90.1 (3) | Fe3—O61—C61—O62 | 8.6 (5) |
O32—Fe1—O41—C41 | 176.9 (3) | Fe3—O61—C61—C62 | −171.8 (2) |
O52—Fe1—O41—C41 | 95.8 (3) | O62—C61—C62—F61 | 175.3 (3) |
O1W—Fe1—O41—C41 | −177.7 (3) | O61—C61—C62—F61 | −4.4 (5) |
O1—Fe3—O42—C41 | −41.3 (3) | Fe3—O71—C71—O72 | 173.8 (2) |
O71—Fe3—O42—C41 | 138.8 (3) | Fe3—O71—C71—C72 | −5.7 (5) |
O61—Fe3—O42—C41 | 52.2 (3) | O72—C71—C72—F71 | 7.8 (4) |
O11—Fe3—O42—C41 | −134.7 (3) | O71—C71—C72—F71 | −172.7 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11···O12i | 0.92 (2) | 1.99 (2) | 2.901 (3) | 168 (3) |
O1W—H12···O72ii | 0.95 (2) | 1.74 (2) | 2.654 (3) | 160 (3) |
O1W—H12···F71ii | 0.95 (2) | 2.46 (3) | 3.091 (3) | 124 (2) |
O2W—H21···O72iii | 0.96 (2) | 1.81 (2) | 2.739 (3) | 161 (3) |
O2W—H22···O3W | 0.94 (2) | 1.70 (2) | 2.611 (6) | 164 (3) |
O3W—H31···F31iv | 0.85 | 2.34 | 3.192 (9) | 178 |
O3W—H32···O22 | 0.85 | 2.50 | 3.349 (8) | 178 |
O4W—H41···O71v | 0.85 | 2.27 | 3.018 (7) | 147 |
O4W—H42···O3W | 0.85 | 1.77 | 2.620 (12) | 178 |
O5W—H51···F61vi | 0.85 | 2.43 | 2.869 (13) | 113 |
O5W—H51···F11 | 0.85 | 2.61 | 3.279 (16) | 137 |
O5W—H52···O51vii | 0.85 | 2.34 | 3.157 (13) | 161 |
O5W—H52···O31vii | 0.85 | 2.64 | 3.195 (11) | 124 |
Symmetry codes: (i) x, −y−1/2, z+1/2; (ii) x, −y−3/2, z+1/2; (iii) x, y+1, z; (iv) −x+1, −y, −z+1; (v) −x+1, −y−1, −z+1; (vi) x, −y−3/2, z−1/2; (vii) x, −y−1/2, z−1/2. |
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