Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103025691/fa1034sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270103025691/fa1034Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270103025691/fa1034IIsup3.hkl |
CCDC references: 229089; 229090
A suspension of FeNH4(SO4)2.12(H2O) (0.48 g, 1.0 mmol), 2,2'-bipyridine (0.16 g, 1.0 mmol), and NaO2CCF3 (0.82 g, 6.0 mmol) in acetone (50 ml) was stirred for 24 h at room temperature under an atmosphere of dry air, resulting in an orange solution and a precipitate of NaCl. The precipitate was removed by filtration and the solvent was evaporated. The product was dissolved in acetone (20 ml), the solution was filtered and excess diethyl ether was added to the filtrate to give a red-brown crystalline solid. The solid was extracted with tetrahydrofuran and layered with hexanes. Green crystals of (I) suitable for X-ray analysis were obtained after two or three days. A solution of (I) (0.10 g) dissolved in CF3COOH (5 ml) was stirred for 12 h, yielding a green–brown solution and an off-white precipitate. The precipitate was removed by filtration and the filtrate was evaporated slowly at room temperature. Red block-shaped crystals of (II) were collected by filtration, washed with hexanes and dried under vacuum.
Difference electron-density syntheses revealed disorder for CF3 groups belonging to non-bridging trifluoroacetate ions in (I) and for all trifluoroacetate ions in (II). This disorder was modeled with the following approach: Initially, the C—F and F···F distances were restrained to typical values [1.33 (1) and 2.14 (1) Å] for CF3 groups obtained from a limited search of the Cambridge Structural Database (Allen, 2002). These values were refined once the disorder model was complete. Refinement of the model with these restraints and site occupancies of 0.5 gave CF3 groups with sensible geometries. However, large peaks (1.55–4.53 e Å−3) in the difference syntheses indicated that each disordered CF3 group occupies two or more positions. Initially, these peaks were used to add F atoms belonging to a second component to each disordered CF3 group. The C atom of the ideal CF3 group was duplicated, and the thermal parameters of both components were constrained to equality. After refinement, there were two separate CF3 groups, rotated (and displaced slightly) about the first, with refined site occupancies of 0.5 (1). Large peaks (the highest being 2.48 e Å−3) seemingly belonging to third components were present. Three components were added to all bridging CF3 groups in (I) and to seven of the nine CF3 groups in (II). The C—F and F···F distances were restrained to be equal to one another and these values were refined. The maximum residual electron density in the regions of the CF3 groups was approximately equal to the largest peaks found elsewhere in the structure after isotropic refinement with this model, but anisotropic refinement resulted in prolate ellipsoids for these F atoms. Therefore, this disorder may be better represented by a large number of components or a torus of electron density about the C—C bond axis, with total occupancy equal to three F atoms. Because of the large number of disordered groups, the high number of parameters and free variables, and the weak scattering by each component, the maximum number of components in the disorder model was limited to three (with site occupancies refined and prolate ellipsoids representing the diffuse electron density). It was necessary to restrain the C—C bond distances in each component to be equal to one another. Introducing the disorder model reduced the values of R1 appreciably [from above 0.10 to 0.0431 for (I) and from above 0.12 to 0.0603 for (II)]. Refinement with the disorder model accounted for most of the electron density, with the highest peaks being similar in magnitude to the deepest holes. In (I), the highest residual peak (0.65 e Å−3) is located 0.58 Å from F28B, and in (II) the highest peak (0.85 e Å−3) is located 0.68 Å from F24B. The H atom belonging to the carboxyl group in (II) was placed at a position where it could donate a hydrogen bond to O15 and with the C—O—H angle restrained to be tetrahedral.
For both compounds, data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000).
[Fe2O(C2F3O2)4(C10H8N2)2] | F(000) = 1776 |
Mr = 892.15 | Dx = 1.814 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 1562 reflections |
a = 10.3902 (16) Å | θ = 2.3–25.3° |
b = 16.751 (3) Å | µ = 1.02 mm−1 |
c = 18.960 (3) Å | T = 110 K |
β = 98.046 (4)° | Rectangular plate, light green |
V = 3267.4 (9) Å3 | 0.40 × 0.28 × 0.06 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 6984 independent reflections |
Radiation source: fine-focus sealed tube | 5087 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 27.5°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −13→13 |
Tmin = 0.627, Tmax = 0.942 | k = −20→19 |
23339 measured reflections | l = −24→23 |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.118 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0535P)2 + 2.838P] where P = (Fo2 + 2Fc2)/3 |
6984 reflections | (Δ/σ)max = 0.001 |
529 parameters | Δρmax = 0.65 e Å−3 |
53 restraints | Δρmin = −0.58 e Å−3 |
[Fe2O(C2F3O2)4(C10H8N2)2] | V = 3267.4 (9) Å3 |
Mr = 892.15 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.3902 (16) Å | µ = 1.02 mm−1 |
b = 16.751 (3) Å | T = 110 K |
c = 18.960 (3) Å | 0.40 × 0.28 × 0.06 mm |
β = 98.046 (4)° |
Bruker SMART APEX CCD area-detector diffractometer | 6984 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 5087 reflections with I > 2σ(I) |
Tmin = 0.627, Tmax = 0.942 | Rint = 0.037 |
23339 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 53 restraints |
wR(F2) = 0.118 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.65 e Å−3 |
6984 reflections | Δρmin = −0.58 e Å−3 |
529 parameters |
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 | 0.43527 (3) | 0.74658 (2) | 0.222850 (19) | 0.01535 (11) | |
O1 | 0.29403 (16) | 0.79834 (11) | 0.18299 (9) | 0.0182 (4) | |
N1 | 0.6074 (2) | 0.69739 (14) | 0.28681 (11) | 0.0185 (5) | |
C1 | 0.6695 (3) | 0.63179 (18) | 0.26983 (16) | 0.0248 (6) | |
H1 | 0.6328 | 0.6011 | 0.2299 | 0.030* | |
Fe2 | 0.14903 (3) | 0.75136 (2) | 0.142185 (19) | 0.01513 (11) | |
O3 | 0.14830 (16) | 0.65214 (11) | 0.20689 (9) | 0.0191 (4) | |
N2 | 0.4754 (2) | 0.82587 (14) | 0.31046 (11) | 0.0180 (5) | |
C2 | 0.7856 (3) | 0.6071 (2) | 0.30852 (17) | 0.0320 (7) | |
H2 | 0.8275 | 0.5600 | 0.2956 | 0.038* | |
O2 | 0.33033 (16) | 0.67154 (11) | 0.28610 (9) | 0.0191 (4) | |
N3 | −0.02584 (19) | 0.71101 (14) | 0.07478 (11) | 0.0178 (5) | |
C3 | 0.8393 (3) | 0.6522 (2) | 0.36616 (17) | 0.0328 (8) | |
H3 | 0.9195 | 0.6367 | 0.3931 | 0.039* | |
O5 | 0.24614 (16) | 0.67015 (11) | 0.07990 (9) | 0.0181 (4) | |
N4 | 0.1236 (2) | 0.83200 (14) | 0.05422 (11) | 0.0175 (5) | |
C4 | 0.7757 (3) | 0.71981 (19) | 0.38425 (16) | 0.0275 (7) | |
H4 | 0.8110 | 0.7514 | 0.4239 | 0.033* | |
O4 | 0.42724 (16) | 0.64824 (11) | 0.15889 (10) | 0.0185 (4) | |
C5 | 0.6589 (2) | 0.74102 (17) | 0.34350 (15) | 0.0209 (6) | |
O6 | 0.55953 (16) | 0.80036 (12) | 0.16675 (10) | 0.0220 (4) | |
C6 | 0.5830 (2) | 0.81208 (17) | 0.35773 (14) | 0.0196 (6) | |
O7 | 0.4741 (2) | 0.77517 (15) | 0.05275 (11) | 0.0345 (5) | |
C7 | 0.4017 (3) | 0.88894 (18) | 0.31873 (15) | 0.0235 (6) | |
H7 | 0.3260 | 0.8975 | 0.2853 | 0.028* | |
O8 | 0.02617 (17) | 0.80909 (12) | 0.19572 (10) | 0.0235 (4) | |
C8 | 0.4308 (3) | 0.94260 (19) | 0.37395 (16) | 0.0279 (7) | |
H8 | 0.3774 | 0.9879 | 0.3781 | 0.033* | |
O9 | 0.1043 (2) | 0.78789 (16) | 0.31131 (11) | 0.0406 (6) | |
C9 | 0.5399 (3) | 0.9283 (2) | 0.42299 (16) | 0.0311 (7) | |
H9 | 0.5624 | 0.9638 | 0.4619 | 0.037* | |
C10 | 0.6156 (3) | 0.86229 (19) | 0.41501 (15) | 0.0272 (7) | |
H10 | 0.6900 | 0.8515 | 0.4488 | 0.033* | |
C11 | −0.1004 (3) | 0.65146 (18) | 0.09136 (15) | 0.0231 (6) | |
H11 | −0.0736 | 0.6220 | 0.1337 | 0.028* | |
C12 | −0.2153 (3) | 0.63058 (19) | 0.04973 (17) | 0.0285 (7) | |
H12 | −0.2671 | 0.5882 | 0.0636 | 0.034* | |
C13 | −0.2536 (3) | 0.67242 (19) | −0.01249 (16) | 0.0290 (7) | |
H13 | −0.3313 | 0.6584 | −0.0426 | 0.035* | |
C14 | −0.1775 (3) | 0.73495 (18) | −0.03045 (16) | 0.0239 (6) | |
H14 | −0.2022 | 0.7646 | −0.0729 | 0.029* | |
C15 | −0.0641 (2) | 0.75357 (17) | 0.01486 (15) | 0.0192 (6) | |
C16 | 0.0202 (2) | 0.82160 (17) | 0.00319 (14) | 0.0177 (6) | |
C17 | −0.0025 (3) | 0.87369 (18) | −0.05423 (14) | 0.0232 (6) | |
H17 | −0.0740 | 0.8652 | −0.0905 | 0.028* | |
C18 | 0.0791 (3) | 0.93755 (19) | −0.05834 (15) | 0.0266 (7) | |
H18 | 0.0636 | 0.9740 | −0.0969 | 0.032* | |
C19 | 0.1845 (3) | 0.94819 (18) | −0.00547 (16) | 0.0254 (6) | |
H19 | 0.2420 | 0.9921 | −0.0070 | 0.030* | |
C20 | 0.2037 (2) | 0.89333 (17) | 0.04935 (14) | 0.0206 (6) | |
H20 | 0.2769 | 0.8995 | 0.0850 | 0.025* | |
C21 | 0.2243 (2) | 0.63977 (17) | 0.26316 (14) | 0.0178 (6) | |
C22 | 0.1846 (2) | 0.57195 (19) | 0.31018 (15) | 0.0231 (6) | |
F22A | 0.27309 (17) | 0.51358 (11) | 0.31489 (11) | 0.0388 (5) | |
F22C | 0.07078 (16) | 0.53975 (12) | 0.28551 (9) | 0.0346 (5) | |
C23 | 0.3540 (2) | 0.63930 (16) | 0.10127 (14) | 0.0163 (5) | |
C24 | 0.4007 (2) | 0.57825 (17) | 0.05008 (15) | 0.0210 (6) | |
F24A | 0.31283 (15) | 0.52004 (11) | 0.03609 (10) | 0.0352 (5) | |
F22B | 0.17834 (18) | 0.59716 (12) | 0.37621 (9) | 0.0374 (5) | |
F24B | 0.51217 (15) | 0.54390 (11) | 0.07640 (9) | 0.0295 (4) | |
F24C | 0.41675 (17) | 0.61134 (11) | −0.01170 (9) | 0.0332 (4) | |
C25 | 0.5417 (2) | 0.81094 (17) | 0.09976 (15) | 0.0215 (6) | |
C27 | 0.0384 (3) | 0.82197 (18) | 0.26243 (16) | 0.0261 (7) | |
C26A | 0.6152 (8) | 0.8836 (4) | 0.0769 (5) | 0.0305 (9) | 0.36 |
F26A | 0.5795 (6) | 0.9041 (4) | 0.0090 (3) | 0.0381 (6) | 0.36 |
F26B | 0.7448 (7) | 0.8738 (5) | 0.0862 (3) | 0.0381 (6) | 0.36 |
F26C | 0.5847 (6) | 0.9463 (4) | 0.1146 (4) | 0.0381 (6) | 0.36 |
C26B | 0.6300 (10) | 0.8777 (5) | 0.0790 (7) | 0.0305 (9) | 0.28 |
F26D | 0.6301 (11) | 0.8915 (8) | 0.0085 (5) | 0.0381 (6) | 0.28 |
F26E | 0.7551 (10) | 0.8569 (5) | 0.1032 (5) | 0.0381 (6) | 0.28 |
F26F | 0.6180 (8) | 0.9510 (6) | 0.1078 (5) | 0.0381 (6) | 0.28 |
C26C | 0.6134 (8) | 0.8846 (4) | 0.0773 (5) | 0.0305 (9) | 0.36 |
F26G | 0.6174 (9) | 0.8808 (6) | 0.0069 (4) | 0.0381 (6) | 0.36 |
F26H | 0.7366 (6) | 0.8932 (4) | 0.1098 (3) | 0.0381 (6) | 0.36 |
F26I | 0.5504 (6) | 0.9514 (4) | 0.0902 (3) | 0.0381 (6) | 0.36 |
C28A | −0.0159 (8) | 0.9021 (3) | 0.2839 (5) | 0.0322 (17) | 0.36 |
F28A | 0.0788 (5) | 0.9521 (4) | 0.3117 (3) | 0.0476 (7) | 0.36 |
F28B | −0.0891 (6) | 0.9421 (4) | 0.2295 (3) | 0.0476 (7) | 0.36 |
F28C | −0.0999 (6) | 0.8951 (5) | 0.3328 (4) | 0.0476 (7) | 0.36 |
C28B | −0.0629 (6) | 0.8836 (4) | 0.2780 (5) | 0.0322 (17) | 0.43 |
F28D | −0.0393 (5) | 0.9535 (3) | 0.2465 (3) | 0.0476 (7) | 0.43 |
F28E | −0.0546 (8) | 0.8979 (5) | 0.3488 (3) | 0.0476 (7) | 0.43 |
F28F | −0.1852 (4) | 0.8628 (3) | 0.2567 (3) | 0.0476 (7) | 0.43 |
C28C | −0.0400 (9) | 0.8932 (5) | 0.2840 (6) | 0.0322 (17) | 0.21 |
F28G | 0.0261 (10) | 0.9613 (6) | 0.2811 (6) | 0.0476 (7) | 0.21 |
F28H | −0.0654 (16) | 0.8808 (9) | 0.3504 (6) | 0.0476 (7) | 0.21 |
F28I | −0.1553 (9) | 0.9041 (7) | 0.2429 (5) | 0.0476 (7) | 0.21 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.01452 (18) | 0.0184 (2) | 0.01215 (19) | −0.00205 (14) | −0.00165 (14) | 0.00017 (16) |
O1 | 0.0196 (9) | 0.0174 (11) | 0.0162 (9) | −0.0003 (7) | −0.0022 (7) | 0.0000 (8) |
N1 | 0.0178 (10) | 0.0223 (13) | 0.0146 (11) | −0.0022 (9) | −0.0005 (8) | 0.0032 (10) |
C1 | 0.0224 (13) | 0.0270 (18) | 0.0240 (15) | 0.0032 (11) | −0.0008 (11) | 0.0017 (13) |
Fe2 | 0.01449 (18) | 0.0181 (2) | 0.01193 (19) | 0.00015 (14) | −0.00136 (14) | −0.00065 (16) |
O3 | 0.0180 (8) | 0.0216 (11) | 0.0165 (9) | −0.0018 (7) | −0.0014 (7) | 0.0015 (8) |
N2 | 0.0193 (10) | 0.0200 (13) | 0.0139 (11) | −0.0041 (9) | −0.0003 (9) | 0.0011 (10) |
C2 | 0.0228 (14) | 0.035 (2) | 0.0376 (18) | 0.0075 (12) | 0.0008 (13) | 0.0026 (15) |
O2 | 0.0167 (8) | 0.0236 (11) | 0.0160 (9) | −0.0028 (7) | −0.0014 (7) | 0.0024 (8) |
N3 | 0.0170 (10) | 0.0195 (13) | 0.0165 (11) | 0.0001 (9) | 0.0012 (8) | −0.0031 (10) |
C3 | 0.0204 (13) | 0.040 (2) | 0.0343 (17) | 0.0018 (13) | −0.0081 (12) | 0.0087 (15) |
O5 | 0.0155 (8) | 0.0218 (11) | 0.0162 (9) | 0.0025 (7) | −0.0009 (7) | −0.0029 (8) |
N4 | 0.0183 (10) | 0.0190 (13) | 0.0147 (11) | −0.0001 (9) | 0.0006 (8) | −0.0030 (9) |
C4 | 0.0241 (14) | 0.0317 (18) | 0.0236 (15) | −0.0056 (12) | −0.0078 (12) | 0.0053 (14) |
O4 | 0.0174 (8) | 0.0199 (11) | 0.0169 (9) | 0.0002 (7) | −0.0023 (7) | −0.0003 (8) |
C5 | 0.0189 (12) | 0.0231 (17) | 0.0193 (14) | −0.0061 (10) | −0.0016 (11) | 0.0036 (12) |
O6 | 0.0202 (9) | 0.0283 (12) | 0.0172 (10) | −0.0067 (8) | 0.0013 (7) | 0.0027 (9) |
C6 | 0.0211 (12) | 0.0227 (16) | 0.0144 (13) | −0.0060 (11) | 0.0005 (10) | 0.0048 (12) |
O7 | 0.0369 (12) | 0.0433 (14) | 0.0219 (11) | −0.0160 (10) | −0.0006 (9) | 0.0001 (10) |
C7 | 0.0236 (13) | 0.0260 (17) | 0.0203 (14) | −0.0028 (11) | 0.0014 (11) | 0.0017 (12) |
O8 | 0.0207 (9) | 0.0327 (13) | 0.0164 (10) | 0.0046 (8) | 0.0002 (7) | −0.0047 (9) |
C8 | 0.0280 (14) | 0.0280 (18) | 0.0285 (16) | −0.0013 (12) | 0.0072 (12) | −0.0064 (14) |
O9 | 0.0427 (13) | 0.0572 (17) | 0.0206 (11) | 0.0162 (12) | −0.0003 (10) | −0.0034 (11) |
C9 | 0.0368 (16) | 0.035 (2) | 0.0213 (15) | −0.0106 (14) | 0.0047 (13) | −0.0115 (14) |
C10 | 0.0262 (14) | 0.0365 (19) | 0.0169 (14) | −0.0077 (12) | −0.0042 (11) | −0.0002 (13) |
C11 | 0.0220 (13) | 0.0236 (17) | 0.0234 (15) | −0.0032 (11) | 0.0018 (11) | −0.0015 (13) |
C12 | 0.0216 (13) | 0.0296 (18) | 0.0336 (17) | −0.0089 (12) | 0.0017 (12) | −0.0071 (14) |
C13 | 0.0194 (13) | 0.0345 (19) | 0.0306 (17) | −0.0018 (12) | −0.0056 (12) | −0.0061 (14) |
C14 | 0.0213 (13) | 0.0262 (17) | 0.0218 (14) | 0.0037 (11) | −0.0057 (11) | −0.0039 (12) |
C15 | 0.0163 (12) | 0.0217 (16) | 0.0187 (13) | 0.0041 (10) | −0.0001 (10) | −0.0058 (12) |
C16 | 0.0178 (12) | 0.0202 (15) | 0.0148 (13) | 0.0041 (10) | 0.0012 (10) | −0.0040 (11) |
C17 | 0.0245 (13) | 0.0295 (18) | 0.0142 (13) | 0.0044 (11) | −0.0016 (11) | −0.0016 (12) |
C18 | 0.0344 (15) | 0.0281 (18) | 0.0175 (14) | 0.0048 (13) | 0.0048 (12) | 0.0047 (13) |
C19 | 0.0302 (14) | 0.0218 (17) | 0.0245 (15) | −0.0023 (12) | 0.0049 (12) | 0.0019 (13) |
C20 | 0.0208 (13) | 0.0240 (17) | 0.0167 (13) | −0.0020 (11) | 0.0020 (10) | −0.0008 (12) |
C21 | 0.0183 (12) | 0.0191 (15) | 0.0165 (13) | 0.0014 (10) | 0.0040 (10) | −0.0016 (11) |
C22 | 0.0217 (13) | 0.0290 (18) | 0.0183 (14) | −0.0048 (11) | 0.0021 (11) | 0.0009 (13) |
F22A | 0.0353 (10) | 0.0291 (11) | 0.0523 (12) | 0.0034 (8) | 0.0077 (9) | 0.0177 (9) |
F22C | 0.0281 (9) | 0.0431 (12) | 0.0315 (10) | −0.0171 (8) | −0.0001 (7) | 0.0069 (9) |
C23 | 0.0166 (11) | 0.0178 (15) | 0.0144 (13) | −0.0037 (10) | 0.0018 (10) | 0.0005 (11) |
C24 | 0.0189 (12) | 0.0224 (16) | 0.0210 (14) | 0.0007 (10) | 0.0010 (11) | −0.0030 (12) |
F24A | 0.0277 (9) | 0.0293 (11) | 0.0498 (12) | −0.0070 (7) | 0.0092 (8) | −0.0196 (9) |
F22B | 0.0467 (11) | 0.0500 (13) | 0.0169 (9) | −0.0160 (9) | 0.0091 (8) | 0.0004 (8) |
F24B | 0.0240 (8) | 0.0342 (11) | 0.0291 (9) | 0.0109 (7) | −0.0002 (7) | −0.0055 (8) |
F24C | 0.0424 (10) | 0.0380 (11) | 0.0208 (9) | 0.0096 (8) | 0.0105 (8) | −0.0005 (8) |
C25 | 0.0198 (12) | 0.0244 (17) | 0.0207 (14) | −0.0013 (11) | 0.0042 (11) | 0.0027 (12) |
C27 | 0.0261 (14) | 0.0301 (18) | 0.0227 (15) | −0.0020 (12) | 0.0057 (12) | −0.0036 (13) |
C26A | 0.036 (2) | 0.035 (2) | 0.0201 (15) | −0.0106 (16) | 0.0051 (14) | −0.0006 (15) |
F26A | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
F26B | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
F26C | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
C26B | 0.036 (2) | 0.035 (2) | 0.0201 (15) | −0.0106 (16) | 0.0051 (14) | −0.0006 (15) |
F26D | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
F26E | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
F26F | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
C26C | 0.036 (2) | 0.035 (2) | 0.0201 (15) | −0.0106 (16) | 0.0051 (14) | −0.0006 (15) |
F26G | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
F26H | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
F26I | 0.0464 (13) | 0.0376 (14) | 0.0322 (10) | −0.0207 (13) | 0.0120 (12) | 0.0013 (9) |
C28A | 0.039 (4) | 0.041 (3) | 0.016 (2) | 0.008 (3) | 0.003 (3) | −0.009 (2) |
F28A | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
F28B | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
F28C | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
C28B | 0.039 (4) | 0.041 (3) | 0.016 (2) | 0.008 (3) | 0.003 (3) | −0.009 (2) |
F28D | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
F28E | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
F28F | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
C28C | 0.039 (4) | 0.041 (3) | 0.016 (2) | 0.008 (3) | 0.003 (3) | −0.009 (2) |
F28G | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
F28H | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
F28I | 0.0485 (18) | 0.0411 (14) | 0.0552 (16) | 0.0100 (14) | 0.0147 (12) | −0.0062 (12) |
Fe1—O1 | 1.7793 (17) | C12—C13 | 1.382 (4) |
Fe1—O6 | 1.9987 (18) | C12—H12 | 0.9500 |
Fe1—O4 | 2.0403 (19) | C13—C14 | 1.383 (4) |
Fe1—N2 | 2.122 (2) | C13—H13 | 0.9500 |
Fe1—O2 | 2.1384 (19) | C14—C15 | 1.393 (4) |
Fe1—N1 | 2.177 (2) | C14—H14 | 0.9500 |
Fe1—Fe2 | 3.1492 (6) | C15—C16 | 1.473 (4) |
O1—Fe2 | 1.7780 (17) | C16—C17 | 1.389 (4) |
N1—C1 | 1.336 (4) | C17—C18 | 1.374 (4) |
N1—C5 | 1.347 (3) | C17—H17 | 0.9500 |
C1—C2 | 1.384 (4) | C18—C19 | 1.389 (4) |
C1—H1 | 0.9500 | C18—H18 | 0.9500 |
Fe2—O8 | 1.9894 (19) | C19—C20 | 1.381 (4) |
Fe2—O3 | 2.0664 (19) | C19—H19 | 0.9500 |
Fe2—N4 | 2.134 (2) | C20—H20 | 0.9500 |
Fe2—O5 | 2.1440 (18) | C21—C22 | 1.535 (4) |
Fe2—N3 | 2.177 (2) | C22—F22C | 1.325 (3) |
O3—C21 | 1.252 (3) | C22—F22B | 1.332 (3) |
N2—C7 | 1.326 (4) | C22—F22A | 1.336 (3) |
N2—C6 | 1.352 (3) | C23—C24 | 1.535 (4) |
C2—C3 | 1.380 (5) | C24—F24B | 1.326 (3) |
C2—H2 | 0.9500 | C24—F24C | 1.327 (3) |
O2—C21 | 1.246 (3) | C24—F24A | 1.337 (3) |
N3—C11 | 1.327 (3) | C25—C26A | 1.532 (3) |
N3—C15 | 1.353 (4) | C25—C26C | 1.532 (3) |
C3—C4 | 1.379 (5) | C25—C26B | 1.532 (3) |
C3—H3 | 0.9500 | C27—C28C | 1.532 (3) |
O5—C23 | 1.249 (3) | C27—C28B | 1.532 (3) |
N4—C20 | 1.334 (3) | C27—C28A | 1.533 (3) |
N4—C16 | 1.353 (3) | C26A—F26C | 1.333 (8) |
C4—C5 | 1.390 (4) | C26A—F26A | 1.334 (8) |
C4—H4 | 0.9500 | C26A—F26B | 1.343 (7) |
O4—C23 | 1.250 (3) | C26B—F26F | 1.357 (8) |
C5—C6 | 1.474 (4) | C26B—F26D | 1.357 (8) |
O6—C25 | 1.270 (3) | C26B—F26E | 1.362 (9) |
C6—C10 | 1.378 (4) | C26C—F26I | 1.337 (8) |
O7—C25 | 1.213 (3) | C26C—F26G | 1.343 (8) |
C7—C8 | 1.381 (4) | C26C—F26H | 1.349 (8) |
C7—H7 | 0.9500 | C28A—F28A | 1.343 (8) |
O8—C27 | 1.272 (3) | C28A—F28C | 1.366 (8) |
C8—C9 | 1.383 (4) | C28A—F28B | 1.367 (8) |
C8—H8 | 0.9500 | C28B—F28F | 1.325 (7) |
O9—C27 | 1.215 (4) | C28B—F28D | 1.352 (7) |
C9—C10 | 1.378 (4) | C28B—F28E | 1.355 (7) |
C9—H9 | 0.9500 | C28C—F28H | 1.337 (9) |
C10—H10 | 0.9500 | C28C—F28G | 1.338 (9) |
C11—C12 | 1.381 (4) | C28C—F28I | 1.347 (9) |
C11—H11 | 0.9500 | ||
O1—Fe1—O6 | 96.32 (8) | C13—C14—H14 | 120.6 |
O1—Fe1—O4 | 100.27 (8) | C15—C14—H14 | 120.6 |
O6—Fe1—O4 | 91.34 (8) | N3—C15—C14 | 121.6 (3) |
O1—Fe1—N2 | 95.02 (8) | N3—C15—C16 | 115.0 (2) |
O6—Fe1—N2 | 93.65 (8) | C14—C15—C16 | 123.4 (3) |
O4—Fe1—N2 | 163.30 (8) | N4—C16—C17 | 120.7 (3) |
O1—Fe1—O2 | 94.00 (8) | N4—C16—C15 | 114.9 (2) |
O6—Fe1—O2 | 168.96 (8) | C17—C16—C15 | 124.4 (2) |
O4—Fe1—O2 | 82.94 (8) | C18—C17—C16 | 119.7 (2) |
N2—Fe1—O2 | 89.35 (8) | C18—C17—H17 | 120.2 |
O1—Fe1—N1 | 170.16 (9) | C16—C17—H17 | 120.2 |
O6—Fe1—N1 | 85.73 (8) | C17—C18—C19 | 119.3 (3) |
O4—Fe1—N1 | 89.29 (8) | C17—C18—H18 | 120.3 |
N2—Fe1—N1 | 75.22 (9) | C19—C18—H18 | 120.3 |
O2—Fe1—N1 | 84.77 (7) | C20—C19—C18 | 118.3 (3) |
Fe2—O1—Fe1 | 124.57 (11) | C20—C19—H19 | 120.8 |
C1—N1—C5 | 119.1 (2) | C18—C19—H19 | 120.8 |
C1—N1—Fe1 | 124.31 (18) | N4—C20—C19 | 122.6 (3) |
C5—N1—Fe1 | 116.29 (18) | N4—C20—H20 | 118.7 |
N1—C1—C2 | 122.1 (3) | C19—C20—H20 | 118.7 |
N1—C1—H1 | 118.9 | O2—C21—O3 | 130.4 (3) |
C2—C1—H1 | 118.9 | O2—C21—C22 | 114.2 (2) |
O1—Fe2—O8 | 97.35 (8) | O3—C21—C22 | 115.4 (2) |
O1—Fe2—O3 | 99.84 (8) | F22C—C22—F22B | 107.6 (2) |
O8—Fe2—O3 | 91.84 (8) | F22C—C22—F22A | 107.3 (2) |
O1—Fe2—N4 | 93.70 (8) | F22B—C22—F22A | 107.0 (2) |
O8—Fe2—N4 | 94.18 (8) | F22C—C22—C21 | 113.3 (2) |
O3—Fe2—N4 | 164.35 (8) | F22B—C22—C21 | 111.3 (2) |
O1—Fe2—O5 | 94.88 (8) | F22A—C22—C21 | 110.0 (2) |
O8—Fe2—O5 | 167.04 (8) | O5—C23—O4 | 130.0 (3) |
O3—Fe2—O5 | 81.83 (7) | O5—C23—C24 | 114.8 (2) |
N4—Fe2—O5 | 89.28 (8) | O4—C23—C24 | 115.1 (2) |
O1—Fe2—N3 | 168.34 (9) | F24B—C24—F24C | 107.6 (2) |
O8—Fe2—N3 | 84.72 (8) | F24B—C24—F24A | 107.1 (2) |
O3—Fe2—N3 | 91.53 (8) | F24C—C24—F24A | 107.2 (2) |
N4—Fe2—N3 | 74.68 (8) | F24B—C24—C23 | 112.8 (2) |
O5—Fe2—N3 | 84.15 (7) | F24C—C24—C23 | 111.7 (2) |
C21—O3—Fe2 | 125.77 (18) | F24A—C24—C23 | 110.1 (2) |
C7—N2—C6 | 119.7 (2) | O7—C25—O6 | 130.9 (3) |
C7—N2—Fe1 | 122.53 (18) | O7—C25—C26A | 116.4 (4) |
C6—N2—Fe1 | 117.75 (19) | O6—C25—C26A | 112.7 (4) |
C3—C2—C1 | 118.8 (3) | O7—C25—C26C | 116.6 (4) |
C3—C2—H2 | 120.6 | O6—C25—C26C | 112.5 (4) |
C1—C2—H2 | 120.6 | O7—C25—C26B | 118.5 (5) |
C21—O2—Fe1 | 123.42 (17) | O6—C25—C26B | 110.5 (5) |
C11—N3—C15 | 118.8 (2) | O9—C27—O8 | 130.3 (3) |
C11—N3—Fe2 | 124.12 (18) | O9—C27—C28C | 115.2 (5) |
C15—N3—Fe2 | 116.89 (18) | O8—C27—C28C | 114.5 (5) |
C4—C3—C2 | 119.4 (3) | O9—C27—C28B | 119.9 (4) |
C4—C3—H3 | 120.3 | O8—C27—C28B | 109.3 (4) |
C2—C3—H3 | 120.3 | O9—C27—C28A | 113.5 (4) |
C23—O5—Fe2 | 123.63 (17) | O8—C27—C28A | 115.0 (4) |
C20—N4—C16 | 119.4 (2) | F26C—C26A—F26A | 105.1 (6) |
C20—N4—Fe2 | 122.12 (17) | F26C—C26A—F26B | 109.6 (6) |
C16—N4—Fe2 | 118.47 (18) | F26A—C26A—F26B | 107.3 (6) |
C3—C4—C5 | 118.9 (3) | F26C—C26A—C25 | 107.9 (6) |
C3—C4—H4 | 120.6 | F26A—C26A—C25 | 113.3 (6) |
C5—C4—H4 | 120.6 | F26B—C26A—C25 | 113.3 (6) |
C23—O4—Fe1 | 125.84 (18) | F26F—C26B—F26D | 104.8 (6) |
N1—C5—C4 | 121.6 (3) | F26F—C26B—F26E | 103.4 (7) |
N1—C5—C6 | 114.9 (2) | F26D—C26B—F26E | 104.1 (7) |
C4—C5—C6 | 123.5 (3) | F26F—C26B—C25 | 117.7 (8) |
C25—O6—Fe1 | 125.49 (16) | F26D—C26B—C25 | 117.4 (9) |
N2—C6—C10 | 120.5 (3) | F26E—C26B—C25 | 107.7 (8) |
N2—C6—C5 | 115.5 (2) | F26I—C26C—F26G | 107.9 (6) |
C10—C6—C5 | 123.9 (2) | F26I—C26C—F26H | 106.6 (6) |
N2—C7—C8 | 122.7 (3) | F26G—C26C—F26H | 107.4 (6) |
N2—C7—H7 | 118.7 | F26I—C26C—C25 | 110.7 (6) |
C8—C7—H7 | 118.7 | F26G—C26C—C25 | 108.8 (7) |
C27—O8—Fe2 | 127.44 (17) | F26H—C26C—C25 | 115.2 (6) |
C7—C8—C9 | 118.0 (3) | F28A—C28A—F28C | 106.8 (6) |
C7—C8—H8 | 121.0 | F28A—C28A—F28B | 106.9 (6) |
C9—C8—H8 | 121.0 | F28C—C28A—F28B | 102.3 (5) |
C10—C9—C8 | 119.5 (3) | F28A—C28A—C27 | 112.0 (5) |
C10—C9—H9 | 120.3 | F28C—C28A—C27 | 113.5 (7) |
C8—C9—H9 | 120.3 | F28B—C28A—C27 | 114.6 (6) |
C6—C10—C9 | 119.7 (3) | F28F—C28B—F28D | 108.6 (6) |
C6—C10—H10 | 120.2 | F28F—C28B—F28E | 105.9 (5) |
C9—C10—H10 | 120.2 | F28D—C28B—F28E | 107.1 (6) |
N3—C11—C12 | 122.8 (3) | F28F—C28B—C27 | 114.8 (5) |
N3—C11—H11 | 118.6 | F28D—C28B—C27 | 109.0 (5) |
C12—C11—H11 | 118.6 | F28E—C28B—C27 | 111.1 (7) |
C11—C12—C13 | 118.8 (3) | F28H—C28C—F28G | 109.9 (8) |
C11—C12—H12 | 120.6 | F28H—C28C—F28I | 106.9 (8) |
C13—C12—H12 | 120.6 | F28G—C28C—F28I | 106.3 (7) |
C12—C13—C14 | 119.2 (3) | F28H—C28C—C27 | 108.2 (11) |
C12—C13—H13 | 120.4 | F28G—C28C—C27 | 111.0 (7) |
C14—C13—H13 | 120.4 | F28I—C28C—C27 | 114.4 (8) |
C13—C14—C15 | 118.8 (3) | ||
O6—Fe1—O1—Fe2 | 125.62 (12) | N3—Fe2—O8—C27 | 145.5 (2) |
O4—Fe1—O1—Fe2 | 33.11 (13) | N2—C7—C8—C9 | −1.3 (5) |
N2—Fe1—O1—Fe2 | −140.13 (12) | C7—C8—C9—C10 | 0.5 (5) |
O2—Fe1—O1—Fe2 | −50.43 (12) | N2—C6—C10—C9 | −1.8 (4) |
O6—Fe1—N1—C1 | −84.1 (2) | C5—C6—C10—C9 | 178.6 (3) |
O4—Fe1—N1—C1 | 7.3 (2) | C8—C9—C10—C6 | 1.0 (5) |
N2—Fe1—N1—C1 | −179.0 (2) | C15—N3—C11—C12 | 0.5 (4) |
O2—Fe1—N1—C1 | 90.3 (2) | Fe2—N3—C11—C12 | 175.7 (2) |
O6—Fe1—N1—C5 | 89.9 (2) | N3—C11—C12—C13 | 1.1 (5) |
O4—Fe1—N1—C5 | −178.7 (2) | C11—C12—C13—C14 | −1.4 (5) |
N2—Fe1—N1—C5 | −5.00 (19) | C12—C13—C14—C15 | 0.2 (4) |
O2—Fe1—N1—C5 | −95.7 (2) | C11—N3—C15—C14 | −1.7 (4) |
Fe1—N1—C1—C2 | 173.7 (2) | Fe2—N3—C15—C14 | −177.3 (2) |
Fe1—O1—Fe2—O8 | 127.53 (12) | C11—N3—C15—C16 | 176.2 (2) |
Fe1—O1—Fe2—O3 | 34.36 (13) | Fe2—N3—C15—C16 | 0.7 (3) |
Fe1—O1—Fe2—N4 | −137.77 (12) | C13—C14—C15—N3 | 1.4 (4) |
Fe1—O1—Fe2—O5 | −48.17 (12) | C13—C14—C15—C16 | −176.4 (3) |
Fe1—O1—Fe2—N3 | −132.9 (4) | C20—N4—C16—C17 | 0.5 (4) |
O1—Fe2—O3—C21 | 7.8 (2) | Fe2—N4—C16—C17 | 178.4 (2) |
O8—Fe2—O3—C21 | −90.0 (2) | C20—N4—C16—C15 | −178.2 (2) |
N4—Fe2—O3—C21 | 157.4 (3) | Fe2—N4—C16—C15 | −0.3 (3) |
O5—Fe2—O3—C21 | 101.4 (2) | N3—C15—C16—N4 | −0.2 (3) |
N3—Fe2—O3—C21 | −174.8 (2) | C14—C15—C16—N4 | 177.7 (3) |
O1—Fe1—N2—C7 | −0.1 (2) | N3—C15—C16—C17 | −178.9 (2) |
O6—Fe1—N2—C7 | 96.5 (2) | C14—C15—C16—C17 | −1.0 (4) |
O4—Fe1—N2—C7 | −156.4 (2) | N4—C16—C17—C18 | −1.6 (4) |
O2—Fe1—N2—C7 | −94.1 (2) | C15—C16—C17—C18 | 177.0 (3) |
N1—Fe1—N2—C7 | −178.9 (2) | C16—C17—C18—C19 | 1.1 (4) |
O1—Fe1—N2—C6 | −177.83 (19) | C17—C18—C19—C20 | 0.4 (4) |
O6—Fe1—N2—C6 | −81.15 (19) | C16—N4—C20—C19 | 1.1 (4) |
O4—Fe1—N2—C6 | 26.0 (4) | Fe2—N4—C20—C19 | −176.7 (2) |
O2—Fe1—N2—C6 | 88.22 (19) | C18—C19—C20—N4 | −1.6 (4) |
N1—Fe1—N2—C6 | 3.46 (18) | Fe1—O2—C21—O3 | −12.1 (4) |
N1—C1—C2—C3 | −0.5 (5) | Fe1—O2—C21—C22 | 164.62 (17) |
O1—Fe1—O2—C21 | 42.4 (2) | Fe2—O3—C21—O2 | −16.8 (4) |
O6—Fe1—O2—C21 | −116.7 (4) | Fe2—O3—C21—C22 | 166.49 (17) |
O4—Fe1—O2—C21 | −57.5 (2) | O2—C21—C22—F22C | 179.0 (2) |
N2—Fe1—O2—C21 | 137.4 (2) | O3—C21—C22—F22C | −3.7 (4) |
N1—Fe1—O2—C21 | −147.4 (2) | O2—C21—C22—F22B | 57.6 (3) |
O1—Fe2—N3—C11 | 179.0 (4) | O3—C21—C22—F22B | −125.1 (3) |
O8—Fe2—N3—C11 | −80.1 (2) | O2—C21—C22—F22A | −60.9 (3) |
O3—Fe2—N3—C11 | 11.6 (2) | O3—C21—C22—F22A | 116.4 (3) |
N4—Fe2—N3—C11 | −175.9 (2) | Fe2—O5—C23—O4 | −1.3 (4) |
O5—Fe2—N3—C11 | 93.2 (2) | Fe2—O5—C23—C24 | 175.72 (16) |
O1—Fe2—N3—C15 | −5.7 (5) | Fe1—O4—C23—O5 | −26.2 (4) |
O8—Fe2—N3—C15 | 95.15 (19) | Fe1—O4—C23—C24 | 156.87 (17) |
O3—Fe2—N3—C15 | −173.14 (19) | O5—C23—C24—F24B | −176.7 (2) |
N4—Fe2—N3—C15 | −0.66 (18) | O4—C23—C24—F24B | 0.8 (3) |
O5—Fe2—N3—C15 | −91.52 (19) | O5—C23—C24—F24C | 62.0 (3) |
C1—C2—C3—C4 | 0.8 (5) | O4—C23—C24—F24C | −120.6 (3) |
O1—Fe2—O5—C23 | 35.9 (2) | O5—C23—C24—F24A | −57.0 (3) |
O8—Fe2—O5—C23 | −124.8 (3) | O4—C23—C24—F24A | 120.4 (3) |
O3—Fe2—O5—C23 | −63.4 (2) | Fe1—O6—C25—O7 | −24.1 (5) |
N4—Fe2—O5—C23 | 129.5 (2) | Fe1—O6—C25—C26A | 153.1 (4) |
N3—Fe2—O5—C23 | −155.8 (2) | Fe1—O6—C25—C26C | 152.0 (4) |
O1—Fe2—N4—C20 | −2.7 (2) | Fe1—O6—C25—C26B | 160.1 (5) |
O8—Fe2—N4—C20 | 95.0 (2) | Fe2—O8—C27—O9 | −21.1 (5) |
O3—Fe2—N4—C20 | −152.7 (3) | Fe2—O8—C27—C28C | 157.2 (5) |
O5—Fe2—N4—C20 | −97.5 (2) | Fe2—O8—C27—C28B | 167.7 (3) |
N3—Fe2—N4—C20 | 178.3 (2) | Fe2—O8—C27—C28A | 145.1 (4) |
O1—Fe2—N4—C16 | 179.50 (19) | O7—C25—C26A—F26C | 125.0 (6) |
O8—Fe2—N4—C16 | −82.8 (2) | O6—C25—C26A—F26A | −168.5 (5) |
O3—Fe2—N4—C16 | 29.5 (4) | O7—C25—C26A—F26B | −113.4 (6) |
O5—Fe2—N4—C16 | 84.66 (19) | O7—C25—C26B—F26F | 124.9 (8) |
N3—Fe2—N4—C16 | 0.53 (18) | O6—C25—C26B—F26F | −58.7 (10) |
C2—C3—C4—C5 | −0.3 (5) | O7—C25—C26B—F26D | −1.8 (11) |
O1—Fe1—O4—C23 | 11.3 (2) | O6—C25—C26B—F26D | 174.6 (8) |
O6—Fe1—O4—C23 | −85.4 (2) | O7—C25—C26B—F26E | −118.8 (7) |
N2—Fe1—O4—C23 | 167.2 (3) | O6—C25—C26B—F26E | 57.6 (8) |
O2—Fe1—O4—C23 | 104.1 (2) | O7—C25—C26C—F26I | 99.8 (7) |
N1—Fe1—O4—C23 | −171.1 (2) | O6—C25—C26C—F26I | −76.9 (7) |
C1—N1—C5—C4 | 0.6 (4) | O7—C25—C26C—F26G | −18.6 (8) |
Fe1—N1—C5—C4 | −173.7 (2) | O6—C25—C26C—F26G | 164.7 (6) |
C1—N1—C5—C6 | −180.0 (2) | O7—C25—C26C—F26H | −139.2 (6) |
Fe1—N1—C5—C6 | 5.7 (3) | O6—C25—C26C—F26H | 44.1 (8) |
C3—C4—C5—N1 | −0.4 (4) | O9—C27—C28A—F28A | 57.3 (8) |
C3—C4—C5—C6 | −179.7 (3) | O8—C27—C28A—F28A | −111.2 (6) |
O1—Fe1—O6—C25 | −46.9 (2) | O9—C27—C28A—F28C | −63.7 (7) |
O4—Fe1—O6—C25 | 53.6 (2) | O8—C27—C28A—F28C | 127.8 (6) |
N2—Fe1—O6—C25 | −142.4 (2) | O9—C27—C28A—F28B | 179.3 (5) |
O2—Fe1—O6—C25 | 112.1 (4) | O8—C27—C28A—F28B | 10.7 (8) |
N1—Fe1—O6—C25 | 142.8 (2) | O9—C27—C28B—F28F | −113.5 (6) |
C7—N2—C6—C10 | 1.0 (4) | O8—C27—C28B—F28F | 58.8 (7) |
Fe1—N2—C6—C10 | 178.8 (2) | O9—C27—C28B—F28D | 124.4 (5) |
C7—N2—C6—C5 | −179.4 (2) | O8—C27—C28B—F28D | −63.3 (6) |
Fe1—N2—C6—C5 | −1.6 (3) | O9—C27—C28B—F28E | 6.6 (7) |
N1—C5—C6—N2 | −2.8 (4) | O8—C27—C28B—F28E | 178.9 (5) |
C4—C5—C6—N2 | 176.6 (3) | O9—C27—C28C—F28H | −27.8 (9) |
N1—C5—C6—C10 | 176.8 (3) | O8—C27—C28C—F28H | 153.6 (7) |
C4—C5—C6—C10 | −3.8 (4) | O9—C27—C28C—F28G | 92.8 (9) |
C6—N2—C7—C8 | 0.6 (4) | O8—C27—C28C—F28G | −85.7 (9) |
Fe1—N2—C7—C8 | −177.1 (2) | O9—C27—C28C—F28I | −146.8 (8) |
O1—Fe2—O8—C27 | −46.1 (2) | O8—C27—C28C—F28I | 34.6 (10) |
O3—Fe2—O8—C27 | 54.1 (2) | O2—Fe1—Fe2—O3 | −17.45 (8) |
N4—Fe2—O8—C27 | −140.4 (2) | O4—Fe1—Fe2—O5 | −16.31 (8) |
O5—Fe2—O8—C27 | 114.5 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···O4 | 0.95 | 2.49 | 3.059 (3) | 119 |
C7—H7···O1 | 0.95 | 2.54 | 3.062 (3) | 115 |
C20—H20···O1 | 0.95 | 2.50 | 3.028 (3) | 115 |
C11—H11···O3 | 0.95 | 2.57 | 3.145 (3) | 119 |
C20—H20···F22Ai | 0.95 | 2.79 | 3.251 (3) | 111 |
C17—H17···F22Bii | 0.95 | 2.64 | 3.428 (3) | 141 |
C2—H2···F22Ciii | 0.95 | 2.58 | 3.257 (3) | 128 |
C12—H12···F24Aiv | 0.95 | 2.61 | 3.095 (3) | 112 |
C12—H12···F24Bv | 0.95 | 2.45 | 3.284 (3) | 146 |
C10—H10···F24Cvi | 0.95 | 2.45 | 3.271 (3) | 144 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+3/2, z−1/2; (iii) x+1, y, z; (iv) −x, −y+1, −z; (v) x−1, y, z; (vi) x+1/2, −y+3/2, z+1/2. |
[Fe4O2(C2F3O2)8(C10H8N2)2]·C2HF3O2 | F(000) = 3120 |
Mr = 1585.96 | Dx = 1.959 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 2413 reflections |
a = 12.733 (3) Å | θ = 2.3–26.6° |
b = 19.015 (4) Å | µ = 1.23 mm−1 |
c = 22.222 (4) Å | T = 173 K |
β = 91.63 (3)° | Block, red brown |
V = 5378 (2) Å3 | 0.35 × 0.27 × 0.19 mm |
Z = 4 |
Bruker SMART 1000 CCD area-detector diffractometer | 10470 independent reflections |
Radiation source: fine-focus sealed tube | 7787 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
ω scans | θmax = 26.9°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −14→16 |
Tmin = 0.670, Tmax = 0.803 | k = −24→21 |
24224 measured reflections | l = −25→28 |
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)] = 0.060 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0406P)2 + 19.8269P] where P = (Fo2 + 2Fc2)/3 |
10470 reflections | (Δ/σ)max = 0.001 |
972 parameters | Δρmax = 0.85 e Å−3 |
190 restraints | Δρmin = −0.60 e Å−3 |
[Fe4O2(C2F3O2)8(C10H8N2)2]·C2HF3O2 | V = 5378 (2) Å3 |
Mr = 1585.96 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 12.733 (3) Å | µ = 1.23 mm−1 |
b = 19.015 (4) Å | T = 173 K |
c = 22.222 (4) Å | 0.35 × 0.27 × 0.19 mm |
β = 91.63 (3)° |
Bruker SMART 1000 CCD area-detector diffractometer | 10470 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 7787 reflections with I > 2σ(I) |
Tmin = 0.670, Tmax = 0.803 | Rint = 0.040 |
24224 measured reflections |
R[F2 > 2σ(F2)] = 0.060 | 190 restraints |
wR(F2) = 0.136 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0406P)2 + 19.8269P] where P = (Fo2 + 2Fc2)/3 |
10470 reflections | Δρmax = 0.85 e Å−3 |
972 parameters | Δρmin = −0.60 e Å−3 |
Experimental. The structure shows considerable disorder and this contributes to diffuse scattering. The data collection nominally covered a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different ϕ angle for the crystal and each exposure covered 0.3° in ω. The crystal-to-detector distance was 4.97 cm. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analyzing the duplicate reflections. Decay was found to be less than 1%, and no decay correction was therefore applied. |
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. The slightly large R-factor is a consequence of residual disorder which was not treated by the disorder model. 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 | 0.74755 (5) | 0.86143 (4) | 0.02426 (3) | 0.02201 (17) | |
N1 | 0.6257 (3) | 0.9266 (2) | 0.05406 (19) | 0.0271 (9) | |
C1 | 0.5431 (4) | 0.9022 (3) | 0.0847 (2) | 0.0302 (12) | |
H1 | 0.5372 | 0.8531 | 0.0912 | 0.036* | |
Fe2 | 0.77697 (5) | 0.57498 (3) | 0.12922 (3) | 0.01729 (15) | |
O2 | 0.8396 (2) | 0.89221 (17) | 0.09778 (15) | 0.0239 (7) | |
N2 | 0.7882 (3) | 0.9642 (2) | −0.00781 (19) | 0.0321 (10) | |
C2 | 0.4669 (5) | 0.9460 (3) | 0.1067 (3) | 0.0370 (13) | |
H2 | 0.4101 | 0.9274 | 0.1285 | 0.044* | |
Fe3 | 0.71594 (5) | 0.74359 (3) | 0.14182 (3) | 0.01720 (15) | |
O3 | 0.7534 (2) | 0.84080 (16) | 0.17338 (14) | 0.0216 (7) | |
N3 | 0.6472 (3) | 0.5079 (2) | 0.11824 (17) | 0.0202 (8) | |
C3 | 0.4745 (5) | 1.0167 (3) | 0.0967 (3) | 0.0445 (15) | |
H3 | 0.4225 | 1.0478 | 0.1111 | 0.053* | |
Fe4 | 0.69063 (5) | 0.69184 (3) | 0.01983 (3) | 0.01874 (16) | |
O4 | 0.6751 (3) | 0.84766 (17) | −0.05909 (15) | 0.0256 (8) | |
N4 | 0.8367 (3) | 0.4771 (2) | 0.16003 (17) | 0.0203 (8) | |
C4 | 0.5579 (5) | 1.0426 (3) | 0.0655 (3) | 0.0410 (14) | |
H4 | 0.5640 | 1.0917 | 0.0584 | 0.049* | |
O5 | 0.6746 (3) | 0.72999 (16) | −0.06602 (14) | 0.0235 (7) | |
C5 | 0.6332 (4) | 0.9966 (3) | 0.0446 (2) | 0.0328 (12) | |
O6 | 0.8775 (3) | 0.81746 (18) | −0.01111 (15) | 0.0273 (8) | |
C6 | 0.7252 (5) | 1.0175 (3) | 0.0096 (2) | 0.0344 (13) | |
O7 | 0.8532 (2) | 0.70132 (17) | 0.00328 (15) | 0.0240 (7) | |
C7 | 0.7468 (5) | 1.0863 (3) | −0.0053 (3) | 0.0456 (16) | |
H7 | 0.7022 | 1.1234 | 0.0070 | 0.055* | |
O8 | 0.9178 (2) | 0.62230 (17) | 0.14564 (15) | 0.0231 (7) | |
C8 | 0.8344 (6) | 1.1002 (4) | −0.0383 (3) | 0.0558 (19) | |
H8 | 0.8499 | 1.1471 | −0.0496 | 0.067* | |
O9 | 0.8806 (2) | 0.73750 (16) | 0.13930 (14) | 0.0197 (7) | |
C9 | 0.8986 (5) | 1.0470 (4) | −0.0548 (3) | 0.0472 (17) | |
H9 | 0.9600 | 1.0566 | −0.0767 | 0.057* | |
O10 | 0.8316 (2) | 0.54415 (17) | 0.04785 (15) | 0.0241 (7) | |
C10 | 0.8734 (5) | 0.9781 (3) | −0.0393 (3) | 0.0432 (15) | |
H10 | 0.9174 | 0.9406 | −0.0513 | 0.052* | |
O11 | 0.7180 (2) | 0.59633 (16) | −0.01766 (14) | 0.0220 (7) | |
C11 | 0.5530 (4) | 0.5292 (3) | 0.0967 (2) | 0.0258 (11) | |
H11 | 0.5445 | 0.5768 | 0.0845 | 0.031* | |
O12 | 0.7448 (2) | 0.58945 (17) | 0.21833 (14) | 0.0233 (7) | |
C12 | 0.4686 (4) | 0.4845 (3) | 0.0916 (2) | 0.0303 (12) | |
H12 | 0.4028 | 0.5007 | 0.0758 | 0.036* | |
O13 | 0.7328 (2) | 0.70677 (16) | 0.22822 (14) | 0.0215 (7) | |
C13 | 0.4813 (4) | 0.4160 (3) | 0.1098 (2) | 0.0309 (12) | |
H13 | 0.4236 | 0.3844 | 0.1078 | 0.037* | |
O14 | 0.5644 (2) | 0.75827 (17) | 0.16000 (15) | 0.0238 (7) | |
C14 | 0.5782 (4) | 0.3935 (3) | 0.1311 (2) | 0.0288 (11) | |
H14 | 0.5882 | 0.3460 | 0.1430 | 0.035* | |
O15 | 0.5163 (3) | 0.65303 (19) | 0.19439 (17) | 0.0352 (9) | |
C15 | 0.6608 (4) | 0.4407 (2) | 0.1349 (2) | 0.0212 (10) | |
O16 | 0.5370 (2) | 0.67776 (17) | 0.01894 (15) | 0.0240 (7) | |
C16 | 0.7685 (4) | 0.4233 (2) | 0.1577 (2) | 0.0237 (10) | |
O17 | 0.4680 (3) | 0.7795 (2) | −0.01451 (19) | 0.0430 (10) | |
C17 | 0.7967 (4) | 0.3572 (3) | 0.1782 (2) | 0.0277 (11) | |
H17 | 0.7471 | 0.3199 | 0.1772 | 0.033* | |
O18 | 0.3885 (4) | 0.5480 (2) | 0.21756 (19) | 0.0534 (12) | |
H18A | 0.4248 | 0.5848 | 0.2160 | 0.11 (4)* | |
C18 | 0.8975 (4) | 0.3461 (3) | 0.2003 (2) | 0.0310 (12) | |
H18 | 0.9187 | 0.3008 | 0.2138 | 0.037* | |
O19 | 0.3677 (4) | 0.5752 (3) | 0.3138 (2) | 0.0720 (15) | |
C19 | 0.9669 (4) | 0.4009 (3) | 0.2025 (2) | 0.0325 (12) | |
H19 | 1.0364 | 0.3944 | 0.2181 | 0.039* | |
C20 | 0.9342 (4) | 0.4660 (3) | 0.1816 (2) | 0.0275 (11) | |
H20 | 0.9827 | 0.5040 | 0.1826 | 0.033* | |
C21 | 0.8238 (4) | 0.8778 (3) | 0.1518 (2) | 0.0245 (11) | |
C22A | 0.9063 (7) | 0.8984 (6) | 0.2005 (4) | 0.0370 (2) | 0.33 |
F22A | 1.0011 (6) | 0.9099 (5) | 0.1784 (4) | 0.0370 (8) | 0.33 |
F22B | 0.9201 (9) | 0.8480 (5) | 0.2419 (5) | 0.0370 (8) | 0.33 |
F22C | 0.8784 (8) | 0.9563 (6) | 0.2299 (6) | 0.0370 (8) | 0.33 |
C22B | 0.8966 (8) | 0.9129 (5) | 0.1992 (4) | 0.037 (2) | 0.42 |
F22D | 0.9753 (6) | 0.9475 (4) | 0.1743 (3) | 0.0370 (8) | 0.42 |
F22E | 0.9378 (7) | 0.8649 (4) | 0.2367 (4) | 0.0370 (8) | 0.42 |
F22F | 0.8452 (7) | 0.9582 (7) | 0.2330 (6) | 0.0370 (8) | 0.42 |
C22C | 0.8933 (12) | 0.9249 (7) | 0.1926 (6) | 0.0370 (2) | 0.25 |
F22G | 0.9476 (10) | 0.9749 (7) | 0.1660 (6) | 0.0370 (8) | 0.25 |
F22H | 0.9597 (11) | 0.8831 (8) | 0.2231 (7) | 0.0370 (8) | 0.25 |
F22I | 0.8281 (14) | 0.9582 (12) | 0.2284 (10) | 0.0370 (8) | 0.25 |
C23 | 0.6602 (4) | 0.7904 (3) | −0.0852 (2) | 0.0245 (11) | |
C24A | 0.6109 (10) | 0.7954 (7) | −0.1489 (3) | 0.0321 (14) | 0.27 |
F24A | 0.5851 (12) | 0.7333 (5) | −0.1728 (6) | 0.0479 (11) | 0.27 |
F24B | 0.6819 (9) | 0.8244 (7) | −0.1837 (6) | 0.0479 (11) | 0.27 |
F24C | 0.5253 (9) | 0.8355 (6) | −0.1531 (5) | 0.0479 (11) | 0.27 |
C24B | 0.6134 (8) | 0.7948 (6) | −0.1495 (3) | 0.0321 (14) | 0.36 |
F24D | 0.6335 (9) | 0.7376 (5) | −0.1815 (4) | 0.0479 (11) | 0.36 |
F24E | 0.6508 (8) | 0.8501 (5) | −0.1783 (6) | 0.0479 (11) | 0.36 |
F24F | 0.5092 (6) | 0.8011 (6) | −0.1482 (4) | 0.0479 (11) | 0.36 |
C24C | 0.6259 (8) | 0.7934 (6) | −0.1519 (3) | 0.0321 (14) | 0.37 |
F24G | 0.6941 (7) | 0.7613 (5) | −0.1866 (4) | 0.0479 (11) | 0.37 |
F24H | 0.6122 (8) | 0.8573 (4) | −0.1749 (5) | 0.0479 (11) | 0.37 |
F24I | 0.5345 (7) | 0.7600 (6) | −0.1601 (4) | 0.0479 (11) | 0.37 |
C25 | 0.9014 (4) | 0.7537 (3) | −0.0148 (2) | 0.0247 (11) | |
C26A | 0.9978 (7) | 0.7399 (7) | −0.0522 (5) | 0.0353 (15) | 0.27 |
F26A | 1.0797 (14) | 0.7795 (7) | −0.0352 (7) | 0.0444 (11) | 0.27 |
F26B | 0.9781 (11) | 0.7540 (7) | −0.1106 (6) | 0.0444 (11) | 0.27 |
F26C | 1.0296 (13) | 0.6731 (6) | −0.0504 (7) | 0.0444 (11) | 0.27 |
C26B | 0.9974 (6) | 0.7382 (6) | −0.0520 (5) | 0.0353 (15) | 0.47 |
F26D | 1.0695 (11) | 0.7886 (6) | −0.0525 (5) | 0.0444 (11) | 0.47 |
F26E | 0.9607 (6) | 0.7327 (5) | −0.1090 (4) | 0.0444 (11) | 0.47 |
F26F | 1.0461 (8) | 0.6786 (5) | −0.0381 (4) | 0.0444 (11) | 0.47 |
C26C | 1.0058 (8) | 0.7391 (9) | −0.0442 (8) | 0.0353 (15) | 0.26 |
F26G | 1.0665 (19) | 0.7956 (8) | −0.0409 (10) | 0.0444 (11) | 0.26 |
F26H | 0.9951 (11) | 0.7206 (9) | −0.1018 (7) | 0.0444 (11) | 0.26 |
F26I | 1.0547 (12) | 0.6875 (9) | −0.0153 (6) | 0.0444 (11) | 0.26 |
C27 | 0.9400 (4) | 0.6856 (3) | 0.1423 (2) | 0.0205 (10) | |
C28A | 1.0573 (4) | 0.7049 (7) | 0.1451 (6) | 0.0272 (11) | 0.26 |
F28A | 1.0793 (9) | 0.7631 (6) | 0.1146 (6) | 0.0391 (9) | 0.26 |
F28B | 1.1202 (11) | 0.6550 (6) | 0.1251 (6) | 0.0391 (9) | 0.26 |
F28C | 1.0822 (9) | 0.7168 (6) | 0.2024 (5) | 0.0391 (9) | 0.26 |
C28B | 1.0580 (4) | 0.7028 (5) | 0.1430 (4) | 0.0272 (11) | 0.52 |
F28D | 1.0802 (5) | 0.7349 (3) | 0.0913 (3) | 0.0391 (9) | 0.52 |
F28E | 1.1174 (6) | 0.6460 (3) | 0.1471 (3) | 0.0391 (9) | 0.52 |
F28F | 1.0843 (5) | 0.7466 (3) | 0.1874 (3) | 0.0391 (9) | 0.52 |
C28C | 1.0581 (4) | 0.7020 (7) | 0.1411 (7) | 0.0272 (11) | 0.22 |
F28G | 1.0911 (11) | 0.7002 (8) | 0.0846 (5) | 0.0391 (9) | 0.22 |
F28H | 1.1126 (12) | 0.6538 (6) | 0.1719 (6) | 0.0391 (9) | 0.22 |
F28I | 1.0852 (11) | 0.7649 (6) | 0.1629 (7) | 0.0391 (9) | 0.22 |
C29 | 0.7929 (4) | 0.5565 (2) | −0.0030 (2) | 0.0224 (10) | |
C30A | 0.8453 (8) | 0.5211 (6) | −0.0568 (4) | 0.0331 (14) | 0.32 |
F30A | 0.9483 (7) | 0.5253 (7) | −0.0517 (6) | 0.0464 (10) | 0.32 |
F30B | 0.8131 (8) | 0.5461 (6) | −0.1095 (4) | 0.0464 (10) | 0.32 |
F30C | 0.8172 (9) | 0.4541 (5) | −0.0541 (5) | 0.0464 (10) | 0.32 |
C30B | 0.8419 (11) | 0.5212 (7) | −0.0579 (5) | 0.0331 (14) | 0.22 |
F30D | 0.9298 (12) | 0.4860 (9) | −0.0444 (6) | 0.0464 (10) | 0.22 |
F30E | 0.8655 (12) | 0.5686 (6) | −0.0993 (6) | 0.0464 (10) | 0.22 |
F30F | 0.7760 (11) | 0.4750 (8) | −0.0839 (8) | 0.0464 (10) | 0.22 |
C30C | 0.8468 (7) | 0.5135 (5) | −0.0521 (3) | 0.0331 (14) | 0.46 |
F30G | 0.8756 (6) | 0.4486 (4) | −0.0355 (3) | 0.0464 (10) | 0.46 |
F30H | 0.9339 (6) | 0.5457 (4) | −0.0680 (4) | 0.0464 (10) | 0.46 |
F30I | 0.7861 (5) | 0.5051 (5) | −0.1016 (3) | 0.0464 (10) | 0.46 |
C31 | 0.7335 (4) | 0.6453 (3) | 0.2466 (2) | 0.0230 (10) | |
C32A | 0.7182 (12) | 0.6403 (8) | 0.3148 (5) | 0.0326 (13) | 0.20 |
F32A | 0.6986 (13) | 0.5761 (7) | 0.3350 (9) | 0.0426 (10) | 0.20 |
F32B | 0.6407 (12) | 0.6816 (8) | 0.3328 (7) | 0.0426 (10) | 0.20 |
F32C | 0.8061 (10) | 0.6631 (8) | 0.3419 (8) | 0.0426 (10) | 0.20 |
C32B | 0.7152 (9) | 0.6334 (6) | 0.3139 (5) | 0.0326 (13) | 0.33 |
F32D | 0.7812 (7) | 0.5850 (5) | 0.3350 (5) | 0.0426 (10) | 0.33 |
F32E | 0.6182 (7) | 0.6113 (5) | 0.3234 (4) | 0.0426 (10) | 0.33 |
F32F | 0.7290 (9) | 0.6909 (4) | 0.3472 (5) | 0.0426 (10) | 0.33 |
C32C | 0.7175 (8) | 0.6371 (5) | 0.3156 (6) | 0.0326 (13) | 0.47 |
F32I | 0.7414 (6) | 0.5740 (3) | 0.3370 (4) | 0.0426 (10) | 0.47 |
F32H | 0.6176 (5) | 0.6503 (4) | 0.3277 (3) | 0.0426 (10) | 0.47 |
F32G | 0.7760 (5) | 0.6835 (4) | 0.3462 (4) | 0.0426 (10) | 0.47 |
C33 | 0.5002 (4) | 0.7141 (3) | 0.1816 (2) | 0.0255 (11) | |
C34A | 0.3934 (5) | 0.7460 (6) | 0.1976 (5) | 0.0328 (14) | 0.34 |
F34A | 0.4014 (9) | 0.7568 (5) | 0.2564 (4) | 0.0371 (9) | 0.34 |
F34B | 0.3127 (14) | 0.7035 (7) | 0.1867 (7) | 0.0371 (9) | 0.34 |
F34C | 0.3728 (8) | 0.8070 (5) | 0.1708 (4) | 0.0371 (9) | 0.34 |
C34B | 0.3912 (5) | 0.7443 (5) | 0.1952 (5) | 0.0328 (14) | 0.49 |
F34D | 0.3904 (7) | 0.7765 (3) | 0.2483 (3) | 0.0371 (9) | 0.49 |
F34E | 0.3217 (8) | 0.6922 (4) | 0.1958 (6) | 0.0371 (9) | 0.49 |
F34F | 0.3593 (7) | 0.7917 (4) | 0.1546 (3) | 0.0371 (9) | 0.49 |
C34C | 0.3922 (7) | 0.7491 (9) | 0.1891 (9) | 0.0328 (14) | 0.17 |
F34G | 0.3899 (14) | 0.8004 (9) | 0.2307 (8) | 0.0371 (9) | 0.17 |
F34H | 0.311 (2) | 0.7069 (11) | 0.2020 (11) | 0.0371 (9) | 0.17 |
F34I | 0.3646 (17) | 0.7808 (10) | 0.1370 (7) | 0.0371 (9) | 0.17 |
C35 | 0.4630 (4) | 0.7209 (3) | 0.0048 (2) | 0.0314 (12) | |
C36A | 0.3607 (7) | 0.6787 (7) | 0.0139 (6) | 0.036 (2) | 0.25 |
F36A | 0.3576 (11) | 0.6099 (6) | −0.0020 (6) | 0.0515 (10) | 0.25 |
F36B | 0.2797 (9) | 0.7064 (8) | −0.0184 (6) | 0.0515 (10) | 0.25 |
F36C | 0.3303 (10) | 0.6778 (8) | 0.0713 (5) | 0.0515 (10) | 0.25 |
C36B | 0.3540 (5) | 0.6928 (5) | 0.0223 (5) | 0.036 (2) | 0.40 |
F36D | 0.3568 (7) | 0.6561 (5) | 0.0738 (4) | 0.0515 (10) | 0.40 |
F36E | 0.3199 (6) | 0.6454 (5) | −0.0192 (4) | 0.0515 (10) | 0.40 |
F36F | 0.2785 (6) | 0.7404 (4) | 0.0244 (4) | 0.0515 (10) | 0.40 |
C36C | 0.3483 (5) | 0.6950 (6) | 0.0095 (5) | 0.036 (2) | 0.35 |
F36G | 0.3479 (8) | 0.6264 (5) | 0.0208 (5) | 0.0515 (10) | 0.35 |
F36H | 0.2975 (7) | 0.7039 (6) | −0.0425 (4) | 0.0515 (10) | 0.35 |
F36I | 0.3047 (7) | 0.7303 (6) | 0.0522 (4) | 0.0515 (10) | 0.35 |
C37 | 0.3510 (4) | 0.5419 (4) | 0.2698 (3) | 0.0452 (15) | |
C38A | 0.2785 (9) | 0.4768 (6) | 0.2684 (6) | 0.064 (3) | 0.34 |
F38A | 0.2770 (11) | 0.4365 (7) | 0.3186 (5) | 0.0668 (13) | 0.34 |
F38B | 0.2893 (11) | 0.4295 (8) | 0.2235 (5) | 0.0668 (13) | 0.34 |
F38C | 0.1785 (12) | 0.4998 (9) | 0.2604 (6) | 0.0668 (13) | 0.34 |
C38B | 0.2722 (7) | 0.4803 (5) | 0.2694 (5) | 0.064 (3) | 0.48 |
F38D | 0.2538 (8) | 0.4618 (5) | 0.3254 (4) | 0.0668 (13) | 0.48 |
F38E | 0.3077 (8) | 0.4252 (5) | 0.2404 (4) | 0.0668 (13) | 0.48 |
F38F | 0.1858 (7) | 0.5051 (6) | 0.2425 (5) | 0.0668 (13) | 0.48 |
C38C | 0.2617 (12) | 0.4886 (9) | 0.2794 (9) | 0.064 (3) | 0.18 |
F38G | 0.2354 (17) | 0.4970 (12) | 0.3359 (8) | 0.0668 (13) | 0.18 |
F38H | 0.3152 (15) | 0.4296 (11) | 0.2744 (11) | 0.0668 (13) | 0.18 |
F38I | 0.1753 (18) | 0.4833 (15) | 0.2456 (11) | 0.0668 (13) | 0.18 |
O1A | 0.6985 (2) | 0.78126 (15) | 0.06003 (13) | 0.0175 (7) | |
O1B | 0.7096 (2) | 0.65466 (15) | 0.10133 (13) | 0.0170 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0230 (4) | 0.0211 (4) | 0.0220 (4) | −0.0047 (3) | 0.0005 (3) | 0.0017 (3) |
N1 | 0.033 (2) | 0.021 (2) | 0.027 (2) | 0.0036 (18) | −0.0049 (18) | 0.0032 (17) |
C1 | 0.028 (3) | 0.029 (3) | 0.033 (3) | 0.003 (2) | 0.001 (2) | 0.010 (2) |
Fe2 | 0.0150 (3) | 0.0170 (3) | 0.0197 (4) | −0.0007 (3) | −0.0018 (2) | −0.0005 (3) |
O2 | 0.0229 (17) | 0.0236 (18) | 0.025 (2) | −0.0083 (14) | 0.0025 (14) | −0.0004 (14) |
N2 | 0.038 (3) | 0.034 (3) | 0.025 (2) | −0.017 (2) | −0.0064 (19) | 0.0063 (19) |
C2 | 0.041 (3) | 0.034 (3) | 0.037 (3) | 0.009 (3) | 0.006 (3) | 0.004 (2) |
Fe3 | 0.0156 (3) | 0.0172 (3) | 0.0188 (4) | 0.0000 (3) | 0.0008 (2) | −0.0001 (3) |
O3 | 0.0213 (17) | 0.0174 (17) | 0.0262 (19) | −0.0013 (13) | 0.0041 (14) | −0.0014 (13) |
N3 | 0.020 (2) | 0.019 (2) | 0.021 (2) | −0.0041 (16) | −0.0005 (16) | −0.0005 (16) |
C3 | 0.051 (4) | 0.036 (3) | 0.047 (4) | 0.014 (3) | −0.001 (3) | 0.000 (3) |
Fe4 | 0.0164 (3) | 0.0200 (4) | 0.0197 (4) | −0.0027 (3) | −0.0011 (3) | 0.0006 (3) |
O4 | 0.0326 (19) | 0.0202 (18) | 0.0240 (19) | −0.0044 (14) | −0.0025 (14) | 0.0004 (14) |
N4 | 0.022 (2) | 0.019 (2) | 0.020 (2) | −0.0005 (16) | 0.0015 (16) | −0.0002 (16) |
C4 | 0.059 (4) | 0.022 (3) | 0.042 (4) | 0.009 (3) | −0.015 (3) | −0.001 (2) |
O5 | 0.0282 (18) | 0.0202 (18) | 0.0220 (19) | −0.0028 (14) | −0.0027 (14) | 0.0044 (13) |
C5 | 0.042 (3) | 0.029 (3) | 0.027 (3) | −0.002 (2) | −0.011 (2) | 0.003 (2) |
O6 | 0.0235 (18) | 0.030 (2) | 0.029 (2) | −0.0049 (15) | 0.0062 (14) | 0.0010 (15) |
C6 | 0.051 (4) | 0.022 (3) | 0.029 (3) | −0.007 (2) | −0.012 (2) | 0.005 (2) |
O7 | 0.0208 (17) | 0.0246 (19) | 0.0266 (19) | −0.0033 (14) | 0.0039 (14) | −0.0028 (14) |
C7 | 0.063 (4) | 0.036 (3) | 0.037 (4) | −0.017 (3) | −0.007 (3) | 0.008 (3) |
O8 | 0.0166 (16) | 0.0218 (18) | 0.031 (2) | −0.0010 (13) | −0.0031 (13) | −0.0009 (14) |
C8 | 0.078 (5) | 0.039 (4) | 0.049 (4) | −0.022 (4) | −0.012 (4) | 0.012 (3) |
O9 | 0.0166 (16) | 0.0182 (17) | 0.0242 (18) | −0.0012 (13) | −0.0019 (13) | −0.0024 (13) |
C9 | 0.054 (4) | 0.059 (4) | 0.029 (3) | −0.027 (3) | 0.001 (3) | 0.014 (3) |
O10 | 0.0201 (17) | 0.0288 (19) | 0.0235 (19) | 0.0049 (14) | 0.0005 (14) | −0.0030 (14) |
C10 | 0.048 (4) | 0.048 (4) | 0.033 (3) | −0.019 (3) | −0.002 (3) | 0.002 (3) |
O11 | 0.0230 (17) | 0.0196 (17) | 0.0231 (19) | −0.0008 (14) | −0.0066 (13) | −0.0032 (13) |
C11 | 0.023 (3) | 0.028 (3) | 0.026 (3) | −0.004 (2) | 0.000 (2) | 0.001 (2) |
O12 | 0.0266 (18) | 0.0213 (18) | 0.0220 (19) | 0.0011 (14) | 0.0004 (14) | −0.0004 (14) |
C12 | 0.028 (3) | 0.031 (3) | 0.032 (3) | −0.007 (2) | −0.005 (2) | 0.001 (2) |
O13 | 0.0250 (17) | 0.0173 (17) | 0.0220 (18) | −0.0003 (13) | −0.0025 (13) | 0.0011 (13) |
C13 | 0.028 (3) | 0.033 (3) | 0.033 (3) | −0.017 (2) | 0.000 (2) | −0.002 (2) |
O14 | 0.0180 (16) | 0.0259 (18) | 0.0276 (19) | 0.0012 (14) | 0.0010 (14) | 0.0006 (14) |
C14 | 0.036 (3) | 0.025 (3) | 0.026 (3) | −0.007 (2) | −0.001 (2) | 0.004 (2) |
O15 | 0.0272 (19) | 0.032 (2) | 0.047 (2) | −0.0033 (16) | 0.0071 (17) | 0.0059 (17) |
C15 | 0.027 (3) | 0.022 (3) | 0.014 (2) | −0.005 (2) | 0.0018 (19) | −0.0044 (18) |
O16 | 0.0135 (16) | 0.0298 (19) | 0.0286 (19) | −0.0016 (14) | −0.0040 (13) | 0.0046 (15) |
C16 | 0.029 (3) | 0.022 (3) | 0.020 (3) | 0.000 (2) | 0.004 (2) | −0.002 (2) |
O17 | 0.031 (2) | 0.042 (2) | 0.055 (3) | 0.0078 (18) | −0.0014 (18) | 0.016 (2) |
C17 | 0.035 (3) | 0.020 (3) | 0.028 (3) | 0.000 (2) | 0.003 (2) | 0.002 (2) |
O18 | 0.062 (3) | 0.053 (3) | 0.045 (3) | −0.025 (2) | 0.017 (2) | 0.001 (2) |
C18 | 0.039 (3) | 0.028 (3) | 0.026 (3) | 0.006 (2) | 0.002 (2) | 0.005 (2) |
O19 | 0.070 (3) | 0.099 (4) | 0.048 (3) | −0.003 (3) | 0.005 (3) | 0.000 (3) |
C19 | 0.029 (3) | 0.032 (3) | 0.036 (3) | 0.003 (2) | −0.006 (2) | 0.004 (2) |
C20 | 0.025 (3) | 0.029 (3) | 0.029 (3) | −0.002 (2) | −0.003 (2) | 0.003 (2) |
C21 | 0.023 (3) | 0.027 (3) | 0.023 (3) | 0.001 (2) | 0.001 (2) | −0.010 (2) |
C22A | 0.036 (4) | 0.053 (7) | 0.022 (4) | −0.013 (4) | 0.001 (3) | −0.001 (4) |
F22A | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
F22B | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
F22C | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
C22B | 0.036 (4) | 0.053 (7) | 0.022 (4) | −0.013 (4) | 0.001 (3) | −0.001 (4) |
F22D | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
F22E | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
F22F | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
C22C | 0.036 (4) | 0.053 (7) | 0.022 (4) | −0.013 (4) | 0.001 (3) | −0.001 (4) |
F22G | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
F22H | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
F22I | 0.032 (2) | 0.0412 (19) | 0.0376 (16) | −0.0150 (16) | −0.0043 (14) | −0.0077 (14) |
C23 | 0.022 (2) | 0.030 (3) | 0.022 (3) | −0.001 (2) | 0.0013 (19) | 0.006 (2) |
C24A | 0.041 (4) | 0.022 (3) | 0.033 (3) | −0.007 (3) | −0.004 (3) | 0.005 (2) |
F24A | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
F24B | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
F24C | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
C24B | 0.041 (4) | 0.022 (3) | 0.033 (3) | −0.007 (3) | −0.004 (3) | 0.005 (2) |
F24D | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
F24E | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
F24F | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
C24C | 0.041 (4) | 0.022 (3) | 0.033 (3) | −0.007 (3) | −0.004 (3) | 0.005 (2) |
F24G | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
F24H | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
F24I | 0.070 (3) | 0.041 (3) | 0.0316 (17) | −0.006 (2) | −0.017 (2) | 0.0068 (16) |
C25 | 0.025 (3) | 0.032 (3) | 0.017 (3) | −0.002 (2) | −0.0014 (19) | −0.001 (2) |
C26A | 0.031 (3) | 0.038 (3) | 0.038 (4) | −0.007 (3) | 0.012 (3) | −0.006 (3) |
F26A | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
F26B | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
F26C | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
C26B | 0.031 (3) | 0.038 (3) | 0.038 (4) | −0.007 (3) | 0.012 (3) | −0.006 (3) |
F26D | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
F26E | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
F26F | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
C26C | 0.031 (3) | 0.038 (3) | 0.038 (4) | −0.007 (3) | 0.012 (3) | −0.006 (3) |
F26G | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
F26H | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
F26I | 0.0302 (18) | 0.053 (2) | 0.051 (3) | −0.0066 (14) | 0.018 (2) | −0.0130 (17) |
C27 | 0.020 (2) | 0.028 (3) | 0.013 (2) | −0.004 (2) | 0.0012 (18) | 0.0010 (19) |
C28A | 0.020 (2) | 0.024 (3) | 0.038 (3) | −0.001 (2) | 0.002 (2) | −0.003 (2) |
F28A | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
F28B | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
F28C | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
C28B | 0.020 (2) | 0.024 (3) | 0.038 (3) | −0.001 (2) | 0.002 (2) | −0.003 (2) |
F28D | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
F28E | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
F28F | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
C28C | 0.020 (2) | 0.024 (3) | 0.038 (3) | −0.001 (2) | 0.002 (2) | −0.003 (2) |
F28G | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
F28H | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
F28I | 0.0224 (11) | 0.034 (2) | 0.061 (3) | −0.0077 (13) | 0.0078 (16) | −0.0110 (19) |
C29 | 0.021 (2) | 0.023 (3) | 0.024 (3) | −0.005 (2) | 0.001 (2) | −0.001 (2) |
C30A | 0.023 (3) | 0.039 (4) | 0.038 (4) | −0.002 (3) | −0.004 (2) | −0.007 (3) |
F30A | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
F30B | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
F30C | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
C30B | 0.023 (3) | 0.039 (4) | 0.038 (4) | −0.002 (3) | −0.004 (2) | −0.007 (3) |
F30D | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
F30E | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
F30F | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
C30C | 0.023 (3) | 0.039 (4) | 0.038 (4) | −0.002 (3) | −0.004 (2) | −0.007 (3) |
F30G | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
F30H | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
F30I | 0.038 (2) | 0.060 (3) | 0.042 (2) | 0.004 (2) | 0.0073 (17) | −0.020 (2) |
C31 | 0.019 (2) | 0.029 (3) | 0.021 (3) | 0.000 (2) | 0.0000 (19) | 0.002 (2) |
C32A | 0.053 (4) | 0.018 (3) | 0.026 (3) | −0.001 (2) | −0.004 (2) | −0.002 (2) |
F32A | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
F32B | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
F32C | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
C32B | 0.053 (4) | 0.018 (3) | 0.026 (3) | −0.001 (2) | −0.004 (2) | −0.002 (2) |
F32D | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
F32E | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
F32F | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
C32C | 0.053 (4) | 0.018 (3) | 0.026 (3) | −0.001 (2) | −0.004 (2) | −0.002 (2) |
F32I | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
F32H | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
F32G | 0.060 (3) | 0.0399 (19) | 0.0280 (14) | 0.005 (2) | 0.0100 (18) | −0.0003 (14) |
C33 | 0.023 (3) | 0.028 (3) | 0.026 (3) | −0.003 (2) | 0.000 (2) | −0.007 (2) |
C34A | 0.023 (3) | 0.045 (3) | 0.032 (3) | −0.007 (2) | 0.009 (2) | −0.009 (3) |
F34A | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
F34B | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
F34C | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
C34B | 0.023 (3) | 0.045 (3) | 0.032 (3) | −0.007 (2) | 0.009 (2) | −0.009 (3) |
F34D | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
F34E | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
F34F | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
C34C | 0.023 (3) | 0.045 (3) | 0.032 (3) | −0.007 (2) | 0.009 (2) | −0.009 (3) |
F34G | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
F34H | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
F34I | 0.0219 (12) | 0.033 (2) | 0.056 (2) | 0.0026 (13) | 0.0044 (13) | −0.0126 (15) |
C35 | 0.023 (3) | 0.044 (3) | 0.027 (3) | −0.002 (2) | 0.000 (2) | 0.002 (2) |
C36A | 0.018 (3) | 0.040 (5) | 0.051 (5) | 0.009 (3) | −0.011 (3) | −0.005 (4) |
F36A | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
F36B | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
F36C | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
C36B | 0.018 (3) | 0.040 (5) | 0.051 (5) | 0.009 (3) | −0.011 (3) | −0.005 (4) |
F36D | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
F36E | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
F36F | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
C36C | 0.018 (3) | 0.040 (5) | 0.051 (5) | 0.009 (3) | −0.011 (3) | −0.005 (4) |
F36G | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
F36H | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
F36I | 0.021 (2) | 0.083 (3) | 0.051 (3) | −0.0043 (17) | 0.0053 (18) | 0.006 (2) |
C37 | 0.028 (3) | 0.065 (4) | 0.044 (4) | −0.001 (3) | 0.008 (3) | 0.009 (3) |
C38A | 0.025 (4) | 0.113 (7) | 0.054 (5) | −0.006 (4) | 0.005 (3) | 0.041 (5) |
F38A | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
F38B | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
F38C | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
C38B | 0.025 (4) | 0.113 (7) | 0.054 (5) | −0.006 (4) | 0.005 (3) | 0.041 (5) |
F38D | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
F38E | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
F38F | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
C38C | 0.025 (4) | 0.113 (7) | 0.054 (5) | −0.006 (4) | 0.005 (3) | 0.041 (5) |
F38G | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
F38H | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
F38I | 0.057 (2) | 0.079 (3) | 0.064 (3) | −0.0312 (19) | −0.0045 (18) | 0.024 (2) |
O1A | 0.0178 (16) | 0.0170 (16) | 0.0178 (17) | −0.0010 (12) | 0.0000 (12) | 0.0023 (12) |
O1B | 0.0148 (15) | 0.0147 (16) | 0.0215 (18) | −0.0007 (12) | −0.0013 (12) | −0.0017 (12) |
Fe1—O1A | 1.837 (3) | C22C—F22G | 1.325 (10) |
Fe1—O6 | 2.031 (3) | C22C—F22I | 1.328 (10) |
Fe1—O4 | 2.062 (3) | C22C—F22H | 1.332 (10) |
Fe1—O2 | 2.068 (3) | C23—C24B | 1.535 (7) |
Fe1—N1 | 2.107 (4) | C23—C24C | 1.535 (7) |
Fe1—N2 | 2.148 (4) | C23—C24A | 1.535 (7) |
Fe1—Fe4 | 3.3059 (11) | C24A—F24B | 1.327 (9) |
Fe1—Fe3 | 3.4738 (11) | C24A—F24A | 1.332 (9) |
N1—C1 | 1.351 (6) | C24A—F24C | 1.332 (9) |
N1—C5 | 1.353 (6) | C24B—F24E | 1.326 (8) |
C1—C2 | 1.379 (7) | C24B—F24D | 1.329 (9) |
C1—H1 | 0.9500 | C24B—F24F | 1.333 (9) |
Fe2—O1B | 1.840 (3) | C24C—F24G | 1.327 (9) |
Fe2—O8 | 2.030 (3) | C24C—F24H | 1.328 (8) |
Fe2—O10 | 2.042 (3) | C24C—F24I | 1.333 (9) |
Fe2—O12 | 2.052 (3) | C25—C26C | 1.523 (7) |
Fe2—N3 | 2.097 (4) | C25—C26B | 1.523 (7) |
Fe2—N4 | 2.117 (4) | C25—C26A | 1.523 (7) |
Fe2—Fe3 | 3.3128 (11) | C26A—F26A | 1.332 (9) |
Fe2—Fe4 | 3.4502 (11) | C26A—F26C | 1.335 (9) |
O2—C21 | 1.252 (6) | C26A—F26B | 1.342 (9) |
N2—C10 | 1.335 (7) | C26B—F26F | 1.325 (8) |
N2—C6 | 1.356 (7) | C26B—F26D | 1.327 (8) |
C2—C3 | 1.367 (8) | C26B—F26E | 1.342 (8) |
C2—H2 | 0.9500 | C26C—F26I | 1.320 (9) |
Fe3—O1B | 1.916 (3) | C26C—F26G | 1.323 (9) |
Fe3—O1A | 1.960 (3) | C26C—F26H | 1.330 (9) |
Fe3—O14 | 2.002 (3) | C27—C28B | 1.537 (6) |
Fe3—O3 | 2.029 (3) | C27—C28A | 1.537 (6) |
Fe3—O13 | 2.049 (3) | C27—C28C | 1.537 (6) |
Fe3—O9 | 2.102 (3) | C28A—F28C | 1.323 (9) |
Fe3—Fe4 | 2.8934 (11) | C28A—F28B | 1.326 (9) |
O3—C21 | 1.247 (6) | C28A—F28A | 1.332 (9) |
N3—C15 | 1.340 (6) | C28B—F28E | 1.321 (7) |
N3—C11 | 1.342 (6) | C28B—F28F | 1.325 (8) |
C3—C4 | 1.375 (9) | C28B—F28D | 1.339 (8) |
C3—H3 | 0.9500 | C28C—F28H | 1.327 (9) |
Fe4—O1A | 1.922 (3) | C28C—F28I | 1.333 (9) |
Fe4—O1B | 1.953 (3) | C28C—F28G | 1.335 (9) |
Fe4—O16 | 1.974 (3) | C29—C30A | 1.540 (7) |
Fe4—O11 | 2.032 (3) | C29—C30B | 1.540 (7) |
Fe4—O5 | 2.046 (3) | C29—C30C | 1.540 (7) |
Fe4—O7 | 2.121 (3) | C30A—F30A | 1.315 (9) |
O4—C23 | 1.245 (6) | C30A—F30B | 1.318 (9) |
N4—C20 | 1.335 (6) | C30A—F30C | 1.325 (9) |
N4—C16 | 1.342 (6) | C30B—F30E | 1.328 (9) |
C4—C5 | 1.388 (8) | C30B—F30D | 1.330 (9) |
C4—H4 | 0.9500 | C30B—F30F | 1.335 (9) |
O5—C23 | 1.237 (6) | C30C—F30H | 1.324 (8) |
C5—C6 | 1.478 (8) | C30C—F30I | 1.336 (8) |
O6—C25 | 1.253 (6) | C30C—F30G | 1.336 (8) |
C6—C7 | 1.378 (7) | C31—C32B | 1.537 (12) |
O7—C25 | 1.243 (6) | C31—C32A | 1.537 (12) |
C7—C8 | 1.379 (9) | C31—C32C | 1.560 (14) |
C7—H7 | 0.9500 | C32A—F32A | 1.327 (9) |
O8—C27 | 1.240 (6) | C32A—F32C | 1.328 (10) |
C8—C9 | 1.358 (10) | C32A—F32B | 1.330 (9) |
C8—H8 | 0.9500 | C32B—F32D | 1.324 (9) |
O9—C27 | 1.243 (5) | C32B—F32E | 1.327 (9) |
C9—C10 | 1.394 (8) | C32B—F32F | 1.329 (9) |
C9—H9 | 0.9500 | C32C—F32I | 1.324 (9) |
O10—C29 | 1.243 (6) | C32C—F32G | 1.330 (9) |
C10—H10 | 0.9500 | C32C—F32H | 1.331 (9) |
O11—C29 | 1.254 (6) | C33—C34A | 1.540 (7) |
C11—C12 | 1.371 (7) | C33—C34B | 1.540 (7) |
C11—H11 | 0.9500 | C33—C34C | 1.541 (7) |
O12—C31 | 1.244 (6) | C34A—F34A | 1.324 (9) |
C12—C13 | 1.372 (7) | C34A—F34B | 1.324 (9) |
C12—H12 | 0.9500 | C34A—F34C | 1.327 (9) |
O13—C31 | 1.239 (6) | C34B—F34E | 1.328 (8) |
C13—C14 | 1.377 (7) | C34B—F34D | 1.329 (8) |
C13—H13 | 0.9500 | C34B—F34F | 1.332 (8) |
O14—C33 | 1.275 (6) | C34C—F34I | 1.342 (10) |
C14—C15 | 1.383 (7) | C34C—F34G | 1.344 (9) |
C14—H14 | 0.9500 | C34C—F34H | 1.344 (9) |
O15—C33 | 1.212 (6) | C35—C36C | 1.548 (7) |
C15—C16 | 1.485 (7) | C35—C36B | 1.549 (7) |
O16—C35 | 1.282 (6) | C35—C36A | 1.549 (7) |
C16—C17 | 1.381 (7) | C36A—F36C | 1.343 (9) |
O17—C35 | 1.196 (6) | C36A—F36B | 1.347 (9) |
C17—C18 | 1.377 (7) | C36A—F36A | 1.356 (9) |
C17—H17 | 0.9500 | C36B—F36F | 1.322 (8) |
O18—C37 | 1.273 (7) | C36B—F36D | 1.340 (9) |
O18—H18A | 0.8400 | C36B—F36E | 1.352 (9) |
C18—C19 | 1.365 (7) | C36C—F36I | 1.301 (9) |
C18—H18 | 0.9500 | C36C—F36H | 1.317 (9) |
O19—C37 | 1.180 (8) | C36C—F36G | 1.328 (9) |
C19—C20 | 1.381 (7) | C37—C38B | 1.542 (9) |
C19—H19 | 0.9500 | C37—C38C | 1.542 (9) |
C20—H20 | 0.9500 | C37—C38A | 1.543 (9) |
C21—C22C | 1.537 (7) | C38A—F38C | 1.354 (9) |
C21—C22B | 1.537 (7) | C38A—F38A | 1.354 (9) |
C21—C22A | 1.537 (7) | C38A—F38B | 1.354 (9) |
C22A—F22A | 1.333 (9) | C38B—F38E | 1.317 (9) |
C22A—F22C | 1.334 (9) | C38B—F38D | 1.320 (8) |
C22A—F22B | 1.336 (9) | C38B—F38F | 1.323 (8) |
C22B—F22F | 1.327 (8) | C38C—F38I | 1.319 (9) |
C22B—F22D | 1.332 (8) | C38C—F38G | 1.319 (10) |
C22B—F22E | 1.333 (8) | C38C—F38H | 1.320 (10) |
O1A—Fe1—O6 | 96.68 (13) | F24D—C24B—C23 | 112.3 (8) |
O1A—Fe1—O4 | 97.74 (13) | F24F—C24B—C23 | 110.2 (8) |
O6—Fe1—O4 | 87.05 (14) | F24G—C24C—F24H | 106.1 (7) |
O1A—Fe1—O2 | 94.88 (13) | F24G—C24C—F24I | 106.5 (8) |
O6—Fe1—O2 | 88.43 (14) | F24H—C24C—F24I | 106.2 (7) |
O4—Fe1—O2 | 167.01 (13) | F24G—C24C—C23 | 111.8 (7) |
O1A—Fe1—N1 | 95.15 (15) | F24H—C24C—C23 | 115.9 (9) |
O6—Fe1—N1 | 168.13 (15) | F24I—C24C—C23 | 109.7 (7) |
O4—Fe1—N1 | 92.43 (15) | O7—C25—O6 | 129.1 (4) |
O2—Fe1—N1 | 89.50 (15) | O7—C25—C26C | 115.9 (8) |
O1A—Fe1—N2 | 170.59 (16) | O6—C25—C26C | 114.9 (8) |
O6—Fe1—N2 | 92.27 (16) | O7—C25—C26B | 115.5 (6) |
O4—Fe1—N2 | 85.59 (15) | O6—C25—C26B | 115.1 (6) |
O2—Fe1—N2 | 82.43 (14) | O7—C25—C26A | 116.8 (7) |
N1—Fe1—N2 | 75.86 (17) | O6—C25—C26A | 113.8 (7) |
C1—N1—C5 | 118.4 (5) | F26A—C26A—F26C | 107.1 (8) |
C1—N1—Fe1 | 123.2 (3) | F26A—C26A—F26B | 106.5 (8) |
C5—N1—Fe1 | 118.3 (4) | F26C—C26A—F26B | 105.4 (8) |
N1—C1—C2 | 122.6 (5) | F26A—C26A—C25 | 112.7 (13) |
N1—C1—H1 | 118.7 | F26C—C26A—C25 | 113.4 (12) |
C2—C1—H1 | 118.7 | F26B—C26A—C25 | 111.2 (11) |
O1B—Fe2—O8 | 95.55 (13) | F26F—C26B—F26D | 107.5 (7) |
O1B—Fe2—O10 | 96.06 (13) | F26F—C26B—F26E | 107.6 (7) |
O8—Fe2—O10 | 87.99 (13) | F26D—C26B—F26E | 105.7 (7) |
O1B—Fe2—O12 | 96.35 (13) | F26F—C26B—C25 | 114.6 (9) |
O8—Fe2—O12 | 88.11 (13) | F26D—C26B—C25 | 115.5 (9) |
O10—Fe2—O12 | 167.30 (13) | F26E—C26B—C25 | 105.2 (8) |
O1B—Fe2—N3 | 95.95 (14) | F26I—C26C—F26G | 108.1 (9) |
O8—Fe2—N3 | 168.50 (14) | F26I—C26C—F26H | 107.8 (9) |
O10—Fe2—N3 | 90.54 (14) | F26G—C26C—F26H | 108.1 (9) |
O12—Fe2—N3 | 90.89 (14) | F26I—C26C—C25 | 109.4 (12) |
O1B—Fe2—N4 | 173.06 (14) | F26G—C26C—C25 | 110.1 (14) |
O8—Fe2—N4 | 91.38 (14) | F26H—C26C—C25 | 113.2 (13) |
O10—Fe2—N4 | 84.58 (14) | O8—C27—O9 | 129.4 (4) |
O12—Fe2—N4 | 83.44 (14) | O8—C27—C28B | 115.5 (5) |
N3—Fe2—N4 | 77.12 (15) | O9—C27—C28B | 115.1 (5) |
C21—O2—Fe1 | 126.3 (3) | O8—C27—C28A | 116.8 (6) |
C10—N2—C6 | 119.9 (5) | O9—C27—C28A | 113.7 (6) |
C10—N2—Fe1 | 124.1 (4) | O8—C27—C28C | 115.0 (6) |
C6—N2—Fe1 | 115.8 (3) | O9—C27—C28C | 115.6 (6) |
C3—C2—C1 | 118.7 (5) | F28C—C28A—F28B | 108.3 (8) |
C3—C2—H2 | 120.6 | F28C—C28A—F28A | 107.4 (8) |
C1—C2—H2 | 120.6 | F28B—C28A—F28A | 106.7 (8) |
O1B—Fe3—O1A | 83.39 (13) | F28C—C28A—C27 | 106.6 (9) |
O1B—Fe3—O14 | 100.94 (13) | F28B—C28A—C27 | 114.3 (10) |
O1A—Fe3—O14 | 92.99 (13) | F28A—C28A—C27 | 113.3 (9) |
O1B—Fe3—O3 | 166.56 (12) | F28E—C28B—F28F | 109.3 (6) |
O1A—Fe3—O3 | 90.39 (13) | F28E—C28B—F28D | 107.3 (6) |
O14—Fe3—O3 | 91.25 (13) | F28F—C28B—F28D | 107.3 (6) |
O1B—Fe3—O13 | 98.07 (13) | F28E—C28B—C27 | 112.6 (7) |
O1A—Fe3—O13 | 178.46 (13) | F28F—C28B—C27 | 111.6 (6) |
O14—Fe3—O13 | 86.24 (13) | F28D—C28B—C27 | 108.6 (6) |
O3—Fe3—O13 | 88.29 (13) | F28H—C28C—F28I | 107.9 (8) |
O1B—Fe3—O9 | 88.14 (12) | F28H—C28C—F28G | 107.0 (8) |
O1A—Fe3—O9 | 94.69 (13) | F28I—C28C—F28G | 106.3 (8) |
O14—Fe3—O9 | 168.73 (13) | F28H—C28C—C27 | 110.4 (11) |
O3—Fe3—O9 | 80.48 (12) | F28I—C28C—C27 | 114.8 (10) |
O13—Fe3—O9 | 85.88 (13) | F28G—C28C—C27 | 110.2 (10) |
C21—O3—Fe3 | 123.1 (3) | O10—C29—O11 | 129.0 (4) |
C15—N3—C11 | 119.6 (4) | O10—C29—C30A | 117.0 (6) |
C15—N3—Fe2 | 116.9 (3) | O11—C29—C30A | 114.0 (6) |
C11—N3—Fe2 | 123.5 (3) | O10—C29—C30B | 118.6 (7) |
C2—C3—C4 | 119.6 (6) | O11—C29—C30B | 112.3 (7) |
C2—C3—H3 | 120.2 | O10—C29—C30C | 111.7 (5) |
C4—C3—H3 | 120.2 | O11—C29—C30C | 119.2 (5) |
O1A—Fe4—O1B | 83.44 (13) | F30A—C30A—F30B | 109.8 (8) |
O1A—Fe4—O16 | 99.41 (13) | F30A—C30A—F30C | 108.9 (8) |
O1B—Fe4—O16 | 93.24 (13) | F30B—C30A—F30C | 107.9 (8) |
O1A—Fe4—O11 | 166.84 (13) | F30A—C30A—C29 | 111.1 (9) |
O1B—Fe4—O11 | 92.20 (13) | F30B—C30A—C29 | 113.6 (8) |
O16—Fe4—O11 | 93.21 (13) | F30C—C30A—C29 | 105.2 (8) |
O1A—Fe4—O5 | 97.02 (13) | F30E—C30B—F30D | 107.0 (8) |
O1B—Fe4—O5 | 178.53 (13) | F30E—C30B—F30F | 107.3 (9) |
O16—Fe4—O5 | 88.06 (13) | F30D—C30B—F30F | 106.4 (8) |
O11—Fe4—O5 | 87.04 (13) | F30E—C30B—C29 | 110.9 (10) |
O1A—Fe4—O7 | 88.10 (12) | F30D—C30B—C29 | 113.4 (10) |
O1B—Fe4—O7 | 95.51 (13) | F30F—C30B—C29 | 111.5 (11) |
O16—Fe4—O7 | 169.07 (13) | F30H—C30C—F30I | 107.7 (7) |
O11—Fe4—O7 | 79.94 (13) | F30H—C30C—F30G | 106.1 (7) |
O5—Fe4—O7 | 83.12 (13) | F30I—C30C—F30G | 105.4 (7) |
C23—O4—Fe1 | 126.0 (3) | F30H—C30C—C29 | 109.6 (7) |
C20—N4—C16 | 119.2 (4) | F30I—C30C—C29 | 112.8 (7) |
C20—N4—Fe2 | 125.2 (3) | F30G—C30C—C29 | 114.8 (7) |
C16—N4—Fe2 | 115.6 (3) | O13—C31—O12 | 129.7 (4) |
C3—C4—C5 | 119.6 (5) | O13—C31—C32B | 117.3 (6) |
C3—C4—H4 | 120.2 | O12—C31—C32B | 112.9 (6) |
C5—C4—H4 | 120.2 | O13—C31—C32A | 112.5 (7) |
C23—O5—Fe4 | 131.3 (3) | O12—C31—C32A | 117.8 (7) |
N1—C5—C4 | 121.1 (5) | O13—C31—C32C | 114.7 (5) |
N1—C5—C6 | 114.0 (5) | O12—C31—C32C | 115.6 (5) |
C4—C5—C6 | 124.9 (5) | F32A—C32A—F32C | 108.1 (9) |
C25—O6—Fe1 | 128.8 (3) | F32A—C32A—F32B | 107.0 (9) |
N2—C6—C7 | 121.1 (6) | F32C—C32A—F32B | 107.2 (9) |
N2—C6—C5 | 115.6 (4) | F32A—C32A—C31 | 114.8 (13) |
C7—C6—C5 | 123.2 (6) | F32C—C32A—C31 | 107.3 (12) |
C25—O7—Fe4 | 128.1 (3) | F32B—C32A—C31 | 112.1 (12) |
C6—C7—C8 | 118.7 (7) | F32D—C32B—F32E | 107.9 (9) |
C6—C7—H7 | 120.7 | F32D—C32B—F32F | 107.7 (9) |
C8—C7—H7 | 120.7 | F32E—C32B—F32F | 106.4 (8) |
C27—O8—Fe2 | 128.4 (3) | F32D—C32B—C31 | 109.5 (9) |
C9—C8—C7 | 120.3 (6) | F32E—C32B—C31 | 111.6 (9) |
C9—C8—H8 | 119.9 | F32F—C32B—C31 | 113.6 (9) |
C7—C8—H8 | 119.9 | F32I—C32C—F32G | 107.3 (8) |
C27—O9—Fe3 | 130.4 (3) | F32I—C32C—F32H | 108.0 (8) |
C8—C9—C10 | 119.2 (6) | F32G—C32C—F32H | 107.3 (8) |
C8—C9—H9 | 120.4 | F32I—C32C—C31 | 114.1 (8) |
C10—C9—H9 | 120.4 | F32G—C32C—C31 | 110.5 (8) |
C29—O10—Fe2 | 127.9 (3) | F32H—C32C—C31 | 109.4 (8) |
N2—C10—C9 | 120.8 (6) | O15—C33—O14 | 127.9 (5) |
N2—C10—H10 | 119.6 | O15—C33—C34A | 117.8 (6) |
C9—C10—H10 | 119.6 | O14—C33—C34A | 114.1 (6) |
C29—O11—Fe4 | 124.8 (3) | O15—C33—C34B | 117.2 (6) |
N3—C11—C12 | 122.2 (5) | O14—C33—C34B | 114.9 (6) |
N3—C11—H11 | 118.9 | O15—C33—C34C | 122.2 (8) |
C12—C11—H11 | 118.9 | O14—C33—C34C | 109.9 (8) |
C31—O12—Fe2 | 129.1 (3) | F34A—C34A—F34B | 108.3 (8) |
C11—C12—C13 | 118.6 (5) | F34A—C34A—F34C | 108.4 (8) |
C11—C12—H12 | 120.7 | F34B—C34A—F34C | 108.0 (8) |
C13—C12—H12 | 120.7 | F34A—C34A—C33 | 104.2 (9) |
C31—O13—Fe3 | 129.1 (3) | F34B—C34A—C33 | 113.8 (13) |
C12—C13—C14 | 119.5 (5) | F34C—C34A—C33 | 113.9 (9) |
C12—C13—H13 | 120.2 | F34E—C34B—F34D | 108.2 (7) |
C14—C13—H13 | 120.2 | F34E—C34B—F34F | 108.8 (7) |
C33—O14—Fe3 | 128.0 (3) | F34D—C34B—F34F | 106.2 (7) |
C13—C14—C15 | 119.5 (5) | F34E—C34B—C33 | 109.2 (8) |
C13—C14—H14 | 120.2 | F34D—C34B—C33 | 112.1 (7) |
C15—C14—H14 | 120.2 | F34F—C34B—C33 | 112.2 (7) |
N3—C15—C14 | 120.6 (4) | F34I—C34C—F34G | 104.8 (9) |
N3—C15—C16 | 114.6 (4) | F34I—C34C—F34H | 105.6 (9) |
C14—C15—C16 | 124.8 (4) | F34G—C34C—F34H | 104.7 (9) |
C35—O16—Fe4 | 129.5 (3) | F34I—C34C—C33 | 108.3 (15) |
N4—C16—C17 | 121.2 (5) | F34G—C34C—C33 | 115.1 (14) |
N4—C16—C15 | 115.7 (4) | F34H—C34C—C33 | 117.3 (18) |
C17—C16—C15 | 123.0 (4) | O17—C35—O16 | 129.7 (5) |
C18—C17—C16 | 119.2 (5) | O17—C35—C36C | 112.4 (6) |
C18—C17—H17 | 120.4 | O16—C35—C36C | 117.8 (6) |
C16—C17—H17 | 120.4 | O17—C35—C36B | 118.0 (6) |
C37—O18—H18A | 109.5 | O16—C35—C36B | 112.0 (6) |
C19—C18—C17 | 119.4 (5) | O17—C35—C36A | 125.7 (7) |
C19—C18—H18 | 120.3 | O16—C35—C36A | 104.5 (7) |
C17—C18—H18 | 120.3 | F36C—C36A—F36B | 105.9 (8) |
C18—C19—C20 | 118.9 (5) | F36C—C36A—F36A | 103.2 (8) |
C18—C19—H19 | 120.6 | F36B—C36A—F36A | 102.8 (8) |
C20—C19—H19 | 120.6 | F36C—C36A—C35 | 113.4 (11) |
N4—C20—C19 | 122.0 (5) | F36B—C36A—C35 | 111.2 (10) |
N4—C20—H20 | 119.0 | F36A—C36A—C35 | 119.0 (11) |
C19—C20—H20 | 119.0 | F36F—C36B—F36D | 109.1 (7) |
O3—C21—O2 | 129.0 (4) | F36F—C36B—F36E | 105.2 (7) |
O3—C21—C22C | 120.6 (7) | F36D—C36B—F36E | 103.7 (7) |
O2—C21—C22C | 109.4 (7) | F36F—C36B—C35 | 115.4 (7) |
O3—C21—C22B | 114.0 (5) | F36D—C36B—C35 | 113.1 (7) |
O2—C21—C22B | 116.9 (5) | F36E—C36B—C35 | 109.3 (7) |
O3—C21—C22A | 110.9 (6) | F36I—C36C—F36H | 111.4 (8) |
O2—C21—C22A | 119.6 (6) | F36I—C36C—F36G | 111.3 (8) |
F22A—C22A—F22C | 107.5 (8) | F36H—C36C—F36G | 106.7 (7) |
F22A—C22A—F22B | 105.6 (8) | F36I—C36C—C35 | 107.9 (8) |
F22C—C22A—F22B | 106.6 (8) | F36H—C36C—C35 | 109.9 (8) |
F22A—C22A—C21 | 113.0 (8) | F36G—C36C—C35 | 109.6 (8) |
F22C—C22A—C21 | 111.6 (9) | O19—C37—O18 | 130.1 (6) |
F22B—C22A—C21 | 112.1 (9) | O19—C37—C38B | 120.9 (7) |
F22F—C22B—F22D | 107.7 (7) | O18—C37—C38B | 109.0 (7) |
F22F—C22B—F22E | 106.4 (7) | O19—C37—C38C | 110.7 (9) |
F22D—C22B—F22E | 108.1 (7) | O18—C37—C38C | 118.9 (9) |
F22F—C22B—C21 | 111.8 (9) | O19—C37—C38A | 122.7 (8) |
F22D—C22B—C21 | 112.1 (7) | O18—C37—C38A | 107.1 (8) |
F22E—C22B—C21 | 110.5 (8) | F38C—C38A—F38A | 104.9 (8) |
F22G—C22C—F22I | 105.6 (14) | F38C—C38A—F38B | 103.5 (8) |
F22G—C22C—F22H | 108.9 (13) | F38A—C38A—F38B | 103.5 (8) |
F22I—C22C—F22H | 112.2 (15) | F38C—C38A—C37 | 107.7 (13) |
F22G—C22C—C21 | 116.9 (11) | F38A—C38A—C37 | 117.3 (11) |
F22I—C22C—C21 | 105.8 (14) | F38B—C38A—C37 | 118.4 (12) |
F22H—C22C—C21 | 107.4 (11) | F38E—C38B—F38D | 108.8 (8) |
O5—C23—O4 | 129.3 (5) | F38E—C38B—F38F | 110.8 (8) |
O5—C23—C24B | 114.9 (6) | F38D—C38B—F38F | 110.6 (7) |
O4—C23—C24B | 115.8 (6) | F38E—C38B—C37 | 112.0 (8) |
O5—C23—C24C | 113.7 (6) | F38D—C38B—C37 | 109.3 (9) |
O4—C23—C24C | 116.9 (6) | F38F—C38B—C37 | 105.3 (9) |
O5—C23—C24A | 115.3 (6) | F38I—C38C—F38G | 108.8 (10) |
O4—C23—C24A | 115.4 (6) | F38I—C38C—F38H | 108.2 (10) |
F24B—C24A—F24A | 107.4 (8) | F38G—C38C—F38H | 109.1 (10) |
F24B—C24A—F24C | 106.8 (8) | F38I—C38C—C37 | 125.3 (18) |
F24A—C24A—F24C | 106.7 (8) | F38G—C38C—C37 | 105.1 (14) |
F24B—C24A—C23 | 107.3 (9) | F38H—C38C—C37 | 99.3 (14) |
F24A—C24A—C23 | 113.8 (10) | Fe1—O1A—Fe4 | 123.17 (16) |
F24C—C24A—C23 | 114.4 (9) | Fe1—O1A—Fe3 | 132.35 (17) |
F24E—C24B—F24D | 108.2 (7) | Fe4—O1A—Fe3 | 96.36 (13) |
F24E—C24B—F24F | 108.1 (8) | Fe2—O1B—Fe3 | 123.74 (16) |
F24D—C24B—F24F | 107.0 (8) | Fe2—O1B—Fe4 | 130.90 (16) |
F24E—C24B—C23 | 110.9 (9) | Fe3—O1B—Fe4 | 96.80 (13) |
O1A—Fe1—N1—C1 | −4.5 (4) | Fe1—O6—C25—O7 | −1.8 (8) |
O4—Fe1—N1—C1 | 93.5 (4) | Fe1—O6—C25—C26C | −179.9 (8) |
O2—Fe1—N1—C1 | −99.4 (4) | Fe1—O6—C25—C26B | 171.7 (6) |
N2—Fe1—N1—C1 | 178.3 (4) | Fe1—O6—C25—C26A | 171.8 (6) |
O1A—Fe1—N1—C5 | 172.2 (4) | O7—C25—C26A—F26A | −134.5 (9) |
O6—Fe1—N1—C5 | −2.6 (10) | O6—C25—C26A—F26A | 51.1 (11) |
O4—Fe1—N1—C5 | −89.8 (4) | O7—C25—C26A—F26C | −12.6 (13) |
O2—Fe1—N1—C5 | 77.4 (4) | O6—C25—C26A—F26C | 173.0 (9) |
N2—Fe1—N1—C5 | −5.0 (4) | O7—C25—C26A—F26B | 106.0 (10) |
C5—N1—C1—C2 | −0.4 (8) | O6—C25—C26A—F26B | −68.4 (11) |
Fe1—N1—C1—C2 | 176.4 (4) | O7—C25—C26B—F26F | −30.1 (11) |
O1A—Fe1—O2—C21 | −27.5 (4) | O6—C25—C26B—F26F | 155.5 (7) |
O6—Fe1—O2—C21 | −124.1 (4) | O7—C25—C26B—F26D | −155.9 (7) |
O4—Fe1—O2—C21 | 166.3 (5) | O6—C25—C26B—F26D | 29.7 (10) |
N1—Fe1—O2—C21 | 67.6 (4) | O7—C25—C26B—F26E | 87.9 (8) |
N2—Fe1—O2—C21 | 143.4 (4) | O6—C25—C26B—F26E | −86.5 (8) |
O6—Fe1—N2—C10 | 0.6 (4) | O7—C25—C26C—F26I | −37.9 (14) |
O4—Fe1—N2—C10 | −86.3 (4) | O6—C25—C26C—F26I | 140.5 (9) |
O2—Fe1—N2—C10 | 88.7 (4) | O7—C25—C26C—F26G | −156.6 (10) |
N1—Fe1—N2—C10 | −179.9 (5) | O6—C25—C26C—F26G | 21.8 (12) |
O6—Fe1—N2—C6 | −174.7 (4) | O7—C25—C26C—F26H | 82.3 (12) |
O4—Fe1—N2—C6 | 98.5 (4) | O6—C25—C26C—F26H | −99.3 (11) |
O2—Fe1—N2—C6 | −86.6 (4) | Fe2—O8—C27—O9 | 15.0 (7) |
N1—Fe1—N2—C6 | 4.9 (4) | Fe2—O8—C27—C28B | −166.2 (4) |
N1—C1—C2—C3 | 0.8 (9) | Fe2—O8—C27—C28A | −168.3 (6) |
O1B—Fe3—O3—C21 | 9.1 (8) | Fe2—O8—C27—C28C | −164.4 (6) |
O1A—Fe3—O3—C21 | −53.1 (4) | Fe3—O9—C27—O8 | 2.6 (7) |
O14—Fe3—O3—C21 | −146.0 (4) | Fe3—O9—C27—C28B | −176.1 (4) |
O13—Fe3—O3—C21 | 127.8 (4) | Fe3—O9—C27—C28A | −174.2 (6) |
O9—Fe3—O3—C21 | 41.6 (4) | Fe3—O9—C27—C28C | −177.9 (6) |
O1B—Fe2—N3—C15 | −178.8 (3) | O8—C27—C28A—F28C | −91.8 (9) |
O8—Fe2—N3—C15 | 2.5 (9) | O9—C27—C28A—F28C | 85.4 (9) |
O10—Fe2—N3—C15 | 85.0 (3) | O8—C27—C28A—F28B | 27.7 (12) |
O12—Fe2—N3—C15 | −82.4 (3) | O9—C27—C28A—F28B | −155.0 (8) |
N4—Fe2—N3—C15 | 0.7 (3) | O8—C27—C28A—F28A | 150.2 (8) |
O1B—Fe2—N3—C11 | 0.1 (4) | O9—C27—C28A—F28A | −32.5 (11) |
O8—Fe2—N3—C11 | −178.6 (6) | C28B—C27—C28A—F28A | 97 (18) |
O10—Fe2—N3—C11 | −96.1 (4) | C28C—C27—C28A—F28A | 88 (11) |
O12—Fe2—N3—C11 | 96.5 (4) | O8—C27—C28B—F28E | 0.1 (9) |
N4—Fe2—N3—C11 | 179.6 (4) | O9—C27—C28B—F28E | 179.1 (6) |
C1—C2—C3—C4 | −0.7 (9) | O8—C27—C28B—F28F | −123.2 (7) |
O1A—Fe1—O4—C23 | −35.6 (4) | O9—C27—C28B—F28F | 55.7 (8) |
O6—Fe1—O4—C23 | 60.8 (4) | O8—C27—C28B—F28D | 118.8 (7) |
O2—Fe1—O4—C23 | 130.5 (6) | O9—C27—C28B—F28D | −62.3 (8) |
N1—Fe1—O4—C23 | −131.1 (4) | C28A—C27—C28B—F28D | −114 (18) |
N2—Fe1—O4—C23 | 153.3 (4) | C28C—C27—C28B—F28D | 45 (25) |
O8—Fe2—N4—C20 | 1.4 (4) | O9—C27—C28C—F28H | 150.1 (8) |
O10—Fe2—N4—C20 | 89.3 (4) | O8—C27—C28C—F28I | −152.5 (9) |
O12—Fe2—N4—C20 | −86.5 (4) | O8—C27—C28C—F28G | 87.6 (10) |
N3—Fe2—N4—C20 | −178.9 (4) | Fe2—O10—C29—O11 | 8.0 (7) |
O8—Fe2—N4—C16 | −179.4 (3) | Fe2—O10—C29—C30A | −174.7 (5) |
O10—Fe2—N4—C16 | −91.6 (3) | Fe2—O10—C29—C30B | −173.7 (6) |
O12—Fe2—N4—C16 | 92.7 (3) | Fe2—O10—C29—C30C | −170.1 (4) |
N3—Fe2—N4—C16 | 0.2 (3) | Fe4—O11—C29—O10 | 39.1 (7) |
C2—C3—C4—C5 | 0.2 (9) | Fe4—O11—C29—C30A | −138.3 (6) |
O1A—Fe4—O5—C23 | −8.6 (4) | Fe4—O11—C29—C30B | −139.3 (6) |
O16—Fe4—O5—C23 | 90.6 (4) | Fe4—O11—C29—C30C | −142.9 (5) |
O11—Fe4—O5—C23 | −176.0 (4) | O10—C29—C30A—F30A | −44.0 (11) |
O7—Fe4—O5—C23 | −95.8 (4) | O11—C29—C30A—F30A | 133.7 (8) |
C1—N1—C5—C4 | −0.2 (8) | O10—C29—C30A—F30B | −168.4 (8) |
Fe1—N1—C5—C4 | −177.1 (4) | O11—C29—C30A—F30B | 9.3 (11) |
C1—N1—C5—C6 | −178.8 (4) | O10—C29—C30A—F30C | 73.7 (9) |
Fe1—N1—C5—C6 | 4.3 (6) | O10—C29—C30B—F30E | −127.2 (10) |
C3—C4—C5—N1 | 0.3 (8) | O10—C29—C30B—F30D | −6.8 (13) |
C3—C4—C5—C6 | 178.8 (5) | O11—C29—C30B—F30D | 171.7 (9) |
O1A—Fe1—O6—C25 | 10.9 (4) | O10—C29—C30B—F30F | 113.2 (10) |
O4—Fe1—O6—C25 | −86.6 (4) | O11—C29—C30B—F30F | −68.2 (12) |
O2—Fe1—O6—C25 | 105.6 (4) | O10—C29—C30C—F30H | −83.0 (8) |
N1—Fe1—O6—C25 | −174.4 (7) | O11—C29—C30C—F30H | 98.7 (7) |
N2—Fe1—O6—C25 | −172.0 (4) | O10—C29—C30C—F30I | 157.0 (7) |
C10—N2—C6—C7 | 0.9 (8) | O11—C29—C30C—F30I | −21.4 (10) |
Fe1—N2—C6—C7 | 176.3 (4) | O10—C29—C30C—F30G | 36.2 (9) |
C10—N2—C6—C5 | −179.7 (5) | Fe3—O13—C31—O12 | 15.7 (7) |
Fe1—N2—C6—C5 | −4.2 (6) | Fe3—O13—C31—C32B | −162.5 (5) |
N1—C5—C6—N2 | 0.1 (7) | Fe3—O13—C31—C32A | −164.5 (7) |
C4—C5—C6—N2 | −178.5 (5) | Fe3—O13—C31—C32C | −164.1 (5) |
N1—C5—C6—C7 | 179.5 (5) | Fe2—O12—C31—O13 | 4.5 (8) |
C4—C5—C6—C7 | 0.9 (9) | Fe2—O12—C31—C32B | −177.2 (5) |
O1A—Fe4—O7—C25 | −44.8 (4) | Fe2—O12—C31—C32A | −175.3 (7) |
O1B—Fe4—O7—C25 | −128.0 (4) | Fe2—O12—C31—C32C | −175.7 (5) |
O16—Fe4—O7—C25 | 89.0 (8) | O13—C31—C32A—F32A | 167.9 (9) |
O11—Fe4—O7—C25 | 140.7 (4) | O12—C31—C32A—F32A | −12.2 (14) |
O5—Fe4—O7—C25 | 52.5 (4) | O13—C31—C32A—F32C | −71.9 (11) |
N2—C6—C7—C8 | −0.2 (9) | O12—C31—C32A—F32C | 108.0 (10) |
C5—C6—C7—C8 | −179.6 (5) | O13—C31—C32A—F32B | 45.5 (12) |
O1B—Fe2—O8—C27 | 6.1 (4) | O12—C31—C32A—F32B | −134.7 (10) |
O10—Fe2—O8—C27 | 102.0 (4) | O13—C31—C32B—F32D | −137.7 (7) |
O12—Fe2—O8—C27 | −90.1 (4) | O12—C31—C32B—F32D | 43.8 (10) |
N3—Fe2—O8—C27 | −175.2 (6) | O13—C31—C32B—F32E | 102.9 (8) |
N4—Fe2—O8—C27 | −173.4 (4) | O12—C31—C32B—F32E | −75.6 (9) |
C6—C7—C8—C9 | −1.1 (10) | O13—C31—C32B—F32F | −17.3 (11) |
O1B—Fe3—O9—C27 | −33.3 (4) | O12—C31—C32B—F32F | 164.2 (7) |
O1A—Fe3—O9—C27 | −116.5 (4) | O13—C31—C32C—F32I | −165.7 (6) |
O14—Fe3—O9—C27 | 110.7 (7) | O12—C31—C32C—F32I | 14.5 (9) |
O3—Fe3—O9—C27 | 153.9 (4) | O13—C31—C32C—F32G | −44.7 (9) |
O13—Fe3—O9—C27 | 65.0 (4) | O12—C31—C32C—F32G | 135.5 (6) |
C7—C8—C9—C10 | 1.7 (10) | O13—C31—C32C—F32H | 73.2 (8) |
O1B—Fe2—O10—C29 | −27.4 (4) | O12—C31—C32C—F32H | −106.6 (7) |
O8—Fe2—O10—C29 | −122.8 (4) | Fe3—O14—C33—O15 | −2.1 (8) |
O12—Fe2—O10—C29 | 165.1 (5) | Fe3—O14—C33—C34A | 172.4 (5) |
N3—Fe2—O10—C29 | 68.7 (4) | Fe3—O14—C33—C34B | 175.0 (5) |
N4—Fe2—O10—C29 | 145.7 (4) | Fe3—O14—C33—C34C | 179.0 (8) |
C6—N2—C10—C9 | −0.2 (8) | O15—C33—C34A—F34A | 76.2 (9) |
Fe1—N2—C10—C9 | −175.3 (4) | O14—C33—C34A—F34A | −98.9 (9) |
C8—C9—C10—N2 | −1.0 (9) | O15—C33—C34A—F34B | −41.5 (12) |
O1A—Fe4—O11—C29 | 22.8 (8) | O14—C33—C34A—F34B | 143.4 (8) |
O1B—Fe4—O11—C29 | −47.5 (4) | O15—C33—C34A—F34C | −165.9 (7) |
O16—Fe4—O11—C29 | −140.8 (4) | O14—C33—C34A—F34C | 19.0 (11) |
O5—Fe4—O11—C29 | 131.3 (4) | O15—C33—C34B—F34E | −25.2 (9) |
O7—Fe4—O11—C29 | 47.7 (4) | O14—C33—C34B—F34E | 157.3 (7) |
C15—N3—C11—C12 | 0.8 (7) | O15—C33—C34B—F34D | 94.7 (8) |
Fe2—N3—C11—C12 | −178.0 (4) | O14—C33—C34B—F34D | −82.7 (9) |
O1B—Fe2—O12—C31 | −30.9 (4) | O15—C33—C34B—F34F | −145.9 (6) |
O8—Fe2—O12—C31 | 64.5 (4) | O14—C33—C34B—F34F | 36.7 (9) |
O10—Fe2—O12—C31 | 136.6 (6) | O15—C33—C34C—F34I | −128.8 (11) |
N3—Fe2—O12—C31 | −127.0 (4) | O14—C33—C34C—F34I | 50.2 (14) |
N4—Fe2—O12—C31 | 156.1 (4) | O15—C33—C34C—F34G | 114.3 (12) |
N3—C11—C12—C13 | 0.6 (8) | O14—C33—C34C—F34G | −66.7 (14) |
O1B—Fe3—O13—C31 | −2.8 (4) | O15—C33—C34C—F34H | −9.6 (16) |
O14—Fe3—O13—C31 | 97.8 (4) | O14—C33—C34C—F34H | 169.4 (11) |
O3—Fe3—O13—C31 | −170.9 (4) | Fe4—O16—C35—O17 | 4.3 (9) |
O9—Fe3—O13—C31 | −90.3 (4) | Fe4—O16—C35—C36C | −179.0 (5) |
C11—C12—C13—C14 | −1.7 (8) | Fe4—O16—C35—C36B | −168.8 (5) |
O1B—Fe3—O14—C33 | 45.7 (4) | Fe4—O16—C35—C36A | −179.4 (6) |
O1A—Fe3—O14—C33 | 129.5 (4) | O17—C35—C36A—F36C | −100.8 (11) |
O3—Fe3—O14—C33 | −140.0 (4) | O16—C35—C36A—F36C | 82.8 (10) |
O13—Fe3—O14—C33 | −51.8 (4) | O17—C35—C36A—F36A | 137.6 (10) |
O9—Fe3—O14—C33 | −97.5 (7) | O16—C35—C36A—F36A | −38.9 (12) |
C12—C13—C14—C15 | 1.4 (8) | O17—C35—C36B—F36F | −11.6 (11) |
C11—N3—C15—C14 | −1.1 (7) | O16—C35—C36B—F36F | 162.5 (7) |
Fe2—N3—C15—C14 | 177.8 (4) | O17—C35—C36B—F36D | −138.3 (8) |
C11—N3—C15—C16 | 179.6 (4) | O16—C35—C36B—F36D | 35.8 (10) |
Fe2—N3—C15—C16 | −1.4 (5) | O17—C35—C36B—F36E | 106.7 (8) |
C13—C14—C15—N3 | 0.0 (7) | O16—C35—C36B—F36E | −79.2 (8) |
C13—C14—C15—C16 | 179.2 (5) | O17—C35—C36C—F36I | −69.5 (9) |
O1A—Fe4—O16—C35 | 46.1 (4) | O16—C35—C36C—F36I | 113.3 (8) |
O1B—Fe4—O16—C35 | 130.0 (4) | O17—C35—C36C—F36H | 52.2 (10) |
O11—Fe4—O16—C35 | −137.6 (4) | O16—C35—C36C—F36H | −125.1 (8) |
O5—Fe4—O16—C35 | −50.7 (4) | O17—C35—C36C—F36G | 169.2 (7) |
O7—Fe4—O16—C35 | −86.9 (8) | O16—C35—C36C—F36G | −8.1 (10) |
C20—N4—C16—C17 | 1.3 (7) | O19—C37—C38A—F38C | 84.1 (11) |
Fe2—N4—C16—C17 | −177.9 (4) | O18—C37—C38A—F38C | −98.7 (10) |
C20—N4—C16—C15 | 178.2 (4) | O19—C37—C38A—F38A | −33.7 (15) |
Fe2—N4—C16—C15 | −1.1 (5) | O18—C37—C38A—F38A | 143.4 (10) |
N3—C15—C16—N4 | 1.6 (6) | O19—C37—C38A—F38B | −159.1 (10) |
C14—C15—C16—N4 | −177.6 (4) | O18—C37—C38A—F38B | 18.1 (13) |
N3—C15—C16—C17 | 178.5 (4) | O19—C37—C38B—F38E | −137.3 (9) |
C14—C15—C16—C17 | −0.8 (8) | O18—C37—C38B—F38E | 43.2 (10) |
N4—C16—C17—C18 | −1.5 (7) | O19—C37—C38B—F38D | −16.7 (11) |
C15—C16—C17—C18 | −178.1 (5) | O18—C37—C38B—F38D | 163.9 (7) |
C16—C17—C18—C19 | 1.3 (8) | O19—C37—C38B—F38F | 102.2 (9) |
C17—C18—C19—C20 | −1.0 (8) | O18—C37—C38B—F38F | −77.3 (9) |
C16—N4—C20—C19 | −1.0 (7) | O19—C37—C38C—F38I | 124.9 (15) |
Fe2—N4—C20—C19 | 178.2 (4) | O18—C37—C38C—F38I | −49.6 (18) |
C18—C19—C20—N4 | 0.8 (8) | O19—C37—C38C—F38G | −2.0 (15) |
Fe3—O3—C21—O2 | 48.3 (7) | O18—C37—C38C—F38G | −176.5 (11) |
Fe3—O3—C21—C22C | −143.8 (8) | O19—C37—C38C—F38H | −114.8 (12) |
Fe3—O3—C21—C22B | −135.1 (5) | O18—C37—C38C—F38H | 70.7 (13) |
Fe3—O3—C21—C22A | −123.3 (6) | O6—Fe1—O1A—Fe4 | −46.2 (2) |
C22C—C21—C22A—F22A | −85 (2) | O4—Fe1—O1A—Fe4 | 41.7 (2) |
C22B—C21—C22A—F22A | −99 (3) | O2—Fe1—O1A—Fe4 | −135.23 (18) |
O3—C21—C22B—F22D | 175.2 (7) | N1—Fe1—O1A—Fe4 | 134.8 (2) |
O2—C21—C22B—F22D | −7.8 (11) | O6—Fe1—O1A—Fe3 | 94.6 (2) |
C22C—C21—C22B—F22D | −53 (5) | O4—Fe1—O1A—Fe3 | −177.5 (2) |
C22A—C21—C22B—F22D | 99 (3) | O2—Fe1—O1A—Fe3 | 5.6 (2) |
O3—C21—C22B—F22E | 54.6 (9) | N1—Fe1—O1A—Fe3 | −84.4 (2) |
O2—C21—C22B—F22E | −128.4 (7) | O1B—Fe4—O1A—Fe1 | 151.4 (2) |
O3—C21—C22C—F22G | −163.7 (11) | O16—Fe4—O1A—Fe1 | −116.43 (19) |
O2—C21—C22C—F22G | 6.2 (17) | O11—Fe4—O1A—Fe1 | 80.1 (6) |
C22B—C21—C22C—F22G | 144 (6) | O5—Fe4—O1A—Fe1 | −27.2 (2) |
C22A—C21—C22C—F22G | 129 (3) | O7—Fe4—O1A—Fe1 | 55.59 (19) |
O3—C21—C22C—F22I | −46.5 (16) | O1B—Fe4—O1A—Fe3 | −0.61 (12) |
O2—C21—C22C—F22I | 123.4 (13) | O16—Fe4—O1A—Fe3 | 91.60 (14) |
C22B—C21—C22C—F22I | −98 (6) | O11—Fe4—O1A—Fe3 | −71.9 (6) |
C22A—C21—C22C—F22I | −114 (3) | O5—Fe4—O1A—Fe3 | −179.21 (12) |
O3—C21—C22C—F22H | 73.5 (15) | O7—Fe4—O1A—Fe3 | −96.38 (13) |
O2—C21—C22C—F22H | −116.5 (12) | O1B—Fe3—O1A—Fe1 | −147.2 (2) |
Fe4—O5—C23—O4 | 18.5 (8) | O14—Fe3—O1A—Fe1 | 112.1 (2) |
Fe4—O5—C23—C24B | −158.9 (5) | O3—Fe3—O1A—Fe1 | 20.8 (2) |
Fe4—O5—C23—C24C | −165.8 (5) | O9—Fe3—O1A—Fe1 | −59.6 (2) |
Fe4—O5—C23—C24A | −157.4 (6) | O1B—Fe3—O1A—Fe4 | 0.62 (12) |
Fe1—O4—C23—O5 | 8.0 (7) | O14—Fe3—O1A—Fe4 | −100.05 (14) |
Fe1—O4—C23—C24B | −174.7 (5) | O3—Fe3—O1A—Fe4 | 168.68 (13) |
Fe1—O4—C23—C24C | −167.6 (5) | O9—Fe3—O1A—Fe4 | 88.20 (13) |
Fe1—O4—C23—C24A | −176.1 (6) | O8—Fe2—O1B—Fe3 | −47.9 (2) |
O5—C23—C24A—F24B | −114.9 (9) | O10—Fe2—O1B—Fe3 | −136.49 (18) |
O4—C23—C24A—F24B | 68.5 (10) | O12—Fe2—O1B—Fe3 | 40.77 (19) |
O5—C23—C24A—F24A | 3.7 (12) | N3—Fe2—O1B—Fe3 | 132.33 (19) |
O4—C23—C24A—F24A | −172.8 (8) | O8—Fe2—O1B—Fe4 | 92.1 (2) |
O5—C23—C24A—F24C | 126.8 (9) | O10—Fe2—O1B—Fe4 | 3.6 (2) |
O4—C23—C24A—F24C | −49.8 (11) | O12—Fe2—O1B—Fe4 | −179.1 (2) |
C24B—C23—C24A—F24C | −160 (33) | N3—Fe2—O1B—Fe4 | −87.6 (2) |
C24C—C23—C24A—F24C | −153 (6) | O1A—Fe3—O1B—Fe2 | 150.15 (19) |
O5—C23—C24B—F24E | −145.7 (7) | O14—Fe3—O1B—Fe2 | −118.08 (19) |
O4—C23—C24B—F24E | 36.5 (10) | O3—Fe3—O1B—Fe2 | 87.2 (6) |
O5—C23—C24B—F24D | −24.5 (10) | O13—Fe3—O1B—Fe2 | −30.4 (2) |
O4—C23—C24B—F24D | 157.7 (7) | O9—Fe3—O1B—Fe2 | 55.20 (19) |
O5—C23—C24B—F24F | 94.6 (9) | O1A—Fe3—O1B—Fe4 | −0.61 (12) |
O4—C23—C24B—F24F | −83.1 (9) | O14—Fe3—O1B—Fe4 | 91.16 (14) |
O5—C23—C24C—F24G | −56.5 (9) | O3—Fe3—O1B—Fe4 | −63.5 (6) |
O4—C23—C24C—F24G | 119.8 (8) | O13—Fe3—O1B—Fe4 | 178.87 (12) |
O5—C23—C24C—F24H | −178.3 (7) | O9—Fe3—O1B—Fe4 | −95.56 (13) |
O4—C23—C24C—F24H | −2.0 (11) | O1A—Fe4—O1B—Fe2 | −146.9 (2) |
O5—C23—C24C—F24I | 61.5 (9) | O16—Fe4—O1B—Fe2 | 114.0 (2) |
O4—C23—C24C—F24I | −122.3 (8) | O11—Fe4—O1B—Fe2 | 20.7 (2) |
C24B—C23—C24C—F24I | −41 (6) | O7—Fe4—O1B—Fe2 | −59.4 (2) |
C24A—C23—C24C—F24I | −42 (5) | O1A—Fe4—O1B—Fe3 | 0.63 (12) |
Fe4—O7—C25—O6 | 23.6 (7) | O16—Fe4—O1B—Fe3 | −98.49 (14) |
Fe4—O7—C25—C26C | −158.3 (8) | O11—Fe4—O1B—Fe3 | 168.17 (13) |
Fe4—O7—C25—C26B | −149.9 (6) | O7—Fe4—O1B—Fe3 | 88.07 (13) |
Fe4—O7—C25—C26A | −149.8 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
O18—H18A···O15 | 0.84 | 1.82 | 2.637 (5) | 164 |
C1—H1···O1A | 0.95 | 2.58 | 3.094 (6) | 114 |
C1—H1···O14 | 0.95 | 2.38 | 3.217 (6) | 146 |
C10—H10···O6 | 0.95 | 2.56 | 3.118 (7) | 118 |
C20—H20···O8 | 0.95 | 2.52 | 3.083 (6) | 118 |
C11—H11···O1B | 0.95 | 2.59 | 3.109 (6) | 115 |
Experimental details
(I) | (II) | |
Crystal data | ||
Chemical formula | [Fe2O(C2F3O2)4(C10H8N2)2] | [Fe4O2(C2F3O2)8(C10H8N2)2]·C2HF3O2 |
Mr | 892.15 | 1585.96 |
Crystal system, space group | Monoclinic, P21/n | Monoclinic, P21/n |
Temperature (K) | 110 | 173 |
a, b, c (Å) | 10.3902 (16), 16.751 (3), 18.960 (3) | 12.733 (3), 19.015 (4), 22.222 (4) |
α, β, γ (°) | 90, 98.046 (4), 90 | 90, 91.63 (3), 90 |
V (Å3) | 3267.4 (9) | 5378 (2) |
Z | 4 | 4 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 1.02 | 1.23 |
Crystal size (mm) | 0.40 × 0.28 × 0.06 | 0.35 × 0.27 × 0.19 |
Data collection | ||
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer | Bruker SMART 1000 CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.627, 0.942 | 0.670, 0.803 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 23339, 6984, 5087 | 24224, 10470, 7787 |
Rint | 0.037 | 0.040 |
(sin θ/λ)max (Å−1) | 0.649 | 0.637 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.118, 1.04 | 0.060, 0.136, 1.07 |
No. of reflections | 6984 | 10470 |
No. of parameters | 529 | 972 |
No. of restraints | 53 | 190 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.0535P)2 + 2.838P] where P = (Fo2 + 2Fc2)/3 | w = 1/[σ2(Fo2) + (0.0406P)2 + 19.8269P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.65, −0.58 | 0.85, −0.60 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2001), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2000).
Fe1—O1 | 1.7793 (17) | Fe2—O5 | 2.1440 (18) |
Fe1—O6 | 1.9987 (18) | Fe2—N3 | 2.177 (2) |
Fe1—O4 | 2.0403 (19) | O3—C21 | 1.252 (3) |
Fe1—N2 | 2.122 (2) | O2—C21 | 1.246 (3) |
Fe1—O2 | 2.1384 (19) | O5—C23 | 1.249 (3) |
Fe1—N1 | 2.177 (2) | O4—C23 | 1.250 (3) |
Fe1—Fe2 | 3.1492 (6) | O6—C25 | 1.270 (3) |
O1—Fe2 | 1.7780 (17) | O7—C25 | 1.213 (3) |
Fe2—O8 | 1.9894 (19) | O8—C27 | 1.272 (3) |
Fe2—O3 | 2.0664 (19) | O9—C27 | 1.215 (4) |
Fe2—N4 | 2.134 (2) | ||
O1—Fe1—O6 | 96.32 (8) | O1—Fe2—O8 | 97.35 (8) |
O1—Fe1—O4 | 100.27 (8) | O1—Fe2—O3 | 99.84 (8) |
O6—Fe1—O4 | 91.34 (8) | O8—Fe2—O3 | 91.84 (8) |
O1—Fe1—N2 | 95.02 (8) | O1—Fe2—N4 | 93.70 (8) |
O6—Fe1—N2 | 93.65 (8) | O8—Fe2—N4 | 94.18 (8) |
O4—Fe1—N2 | 163.30 (8) | O3—Fe2—N4 | 164.35 (8) |
O1—Fe1—O2 | 94.00 (8) | O1—Fe2—O5 | 94.88 (8) |
O6—Fe1—O2 | 168.96 (8) | O8—Fe2—O5 | 167.04 (8) |
O4—Fe1—O2 | 82.94 (8) | O3—Fe2—O5 | 81.83 (7) |
N2—Fe1—O2 | 89.35 (8) | N4—Fe2—O5 | 89.28 (8) |
O1—Fe1—N1 | 170.16 (9) | O1—Fe2—N3 | 168.34 (9) |
O6—Fe1—N1 | 85.73 (8) | O8—Fe2—N3 | 84.72 (8) |
O4—Fe1—N1 | 89.29 (8) | O3—Fe2—N3 | 91.53 (8) |
N2—Fe1—N1 | 75.22 (9) | N4—Fe2—N3 | 74.68 (8) |
O2—Fe1—N1 | 84.77 (7) | O5—Fe2—N3 | 84.15 (7) |
Fe2—O1—Fe1 | 124.57 (11) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···O4 | 0.95 | 2.49 | 3.059 (3) | 119 |
C7—H7···O1 | 0.95 | 2.54 | 3.062 (3) | 115 |
C20—H20···O1 | 0.95 | 2.50 | 3.028 (3) | 115 |
C11—H11···O3 | 0.95 | 2.57 | 3.145 (3) | 119 |
C20—H20···F22Ai | 0.95 | 2.79 | 3.251 (3) | 111 |
C17—H17···F22Bii | 0.95 | 2.64 | 3.428 (3) | 141 |
C2—H2···F22Ciii | 0.95 | 2.58 | 3.257 (3) | 128 |
C12—H12···F24Aiv | 0.95 | 2.61 | 3.095 (3) | 112 |
C12—H12···F24Bv | 0.95 | 2.45 | 3.284 (3) | 146 |
C10—H10···F24Cvi | 0.95 | 2.45 | 3.271 (3) | 144 |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) x−1/2, −y+3/2, z−1/2; (iii) x+1, y, z; (iv) −x, −y+1, −z; (v) x−1, y, z; (vi) x+1/2, −y+3/2, z+1/2. |
Fe1—O1A | 1.837 (3) | Fe2—Fe4 | 3.4502 (11) |
Fe1—O6 | 2.031 (3) | Fe3—O1B | 1.916 (3) |
Fe1—O4 | 2.062 (3) | Fe3—O1A | 1.960 (3) |
Fe1—O2 | 2.068 (3) | Fe3—O14 | 2.002 (3) |
Fe1—N1 | 2.107 (4) | Fe3—O3 | 2.029 (3) |
Fe1—N2 | 2.148 (4) | Fe3—O13 | 2.049 (3) |
Fe1—Fe4 | 3.3059 (11) | Fe3—O9 | 2.102 (3) |
Fe1—Fe3 | 3.4738 (11) | Fe3—Fe4 | 2.8934 (11) |
Fe2—O1B | 1.840 (3) | Fe4—O1A | 1.922 (3) |
Fe2—O8 | 2.030 (3) | Fe4—O1B | 1.953 (3) |
Fe2—O10 | 2.042 (3) | Fe4—O16 | 1.974 (3) |
Fe2—O12 | 2.052 (3) | Fe4—O11 | 2.032 (3) |
Fe2—N3 | 2.097 (4) | Fe4—O5 | 2.046 (3) |
Fe2—N4 | 2.117 (4) | Fe4—O7 | 2.121 (3) |
Fe2—Fe3 | 3.3128 (11) | ||
O1A—Fe1—O6 | 96.68 (13) | O1B—Fe3—O3 | 166.56 (12) |
O1A—Fe1—O4 | 97.74 (13) | O1A—Fe3—O3 | 90.39 (13) |
O6—Fe1—O4 | 87.05 (14) | O14—Fe3—O3 | 91.25 (13) |
O1A—Fe1—O2 | 94.88 (13) | O1B—Fe3—O13 | 98.07 (13) |
O6—Fe1—O2 | 88.43 (14) | O1A—Fe3—O13 | 178.46 (13) |
O4—Fe1—O2 | 167.01 (13) | O14—Fe3—O13 | 86.24 (13) |
O1A—Fe1—N1 | 95.15 (15) | O3—Fe3—O13 | 88.29 (13) |
O6—Fe1—N1 | 168.13 (15) | O1B—Fe3—O9 | 88.14 (12) |
O4—Fe1—N1 | 92.43 (15) | O1A—Fe3—O9 | 94.69 (13) |
O2—Fe1—N1 | 89.50 (15) | O14—Fe3—O9 | 168.73 (13) |
O1A—Fe1—N2 | 170.59 (16) | O3—Fe3—O9 | 80.48 (12) |
O6—Fe1—N2 | 92.27 (16) | O13—Fe3—O9 | 85.88 (13) |
O4—Fe1—N2 | 85.59 (15) | O1A—Fe4—O1B | 83.44 (13) |
O2—Fe1—N2 | 82.43 (14) | O1A—Fe4—O16 | 99.41 (13) |
N1—Fe1—N2 | 75.86 (17) | O1B—Fe4—O16 | 93.24 (13) |
O1B—Fe2—O8 | 95.55 (13) | O1A—Fe4—O11 | 166.84 (13) |
O1B—Fe2—O10 | 96.06 (13) | O1B—Fe4—O11 | 92.20 (13) |
O8—Fe2—O10 | 87.99 (13) | O16—Fe4—O11 | 93.21 (13) |
O1B—Fe2—O12 | 96.35 (13) | O1A—Fe4—O5 | 97.02 (13) |
O8—Fe2—O12 | 88.11 (13) | O1B—Fe4—O5 | 178.53 (13) |
O10—Fe2—O12 | 167.30 (13) | O16—Fe4—O5 | 88.06 (13) |
O1B—Fe2—N3 | 95.95 (14) | O11—Fe4—O5 | 87.04 (13) |
O8—Fe2—N3 | 168.50 (14) | O1A—Fe4—O7 | 88.10 (12) |
O10—Fe2—N3 | 90.54 (14) | O1B—Fe4—O7 | 95.51 (13) |
O12—Fe2—N3 | 90.89 (14) | O16—Fe4—O7 | 169.07 (13) |
O1B—Fe2—N4 | 173.06 (14) | O11—Fe4—O7 | 79.94 (13) |
O8—Fe2—N4 | 91.38 (14) | O5—Fe4—O7 | 83.12 (13) |
O10—Fe2—N4 | 84.58 (14) | Fe1—O1A—Fe4 | 123.17 (16) |
O12—Fe2—N4 | 83.44 (14) | Fe1—O1A—Fe3 | 132.35 (17) |
N3—Fe2—N4 | 77.12 (15) | Fe4—O1A—Fe3 | 96.36 (13) |
O1B—Fe3—O1A | 83.39 (13) | Fe2—O1B—Fe3 | 123.74 (16) |
O1B—Fe3—O14 | 100.94 (13) | Fe2—O1B—Fe4 | 130.90 (16) |
O1A—Fe3—O14 | 92.99 (13) | Fe3—O1B—Fe4 | 96.80 (13) |
D—H···A | D—H | H···A | D···A | D—H···A |
O18—H18A···O15 | 0.84 | 1.82 | 2.637 (5) | 164 |
C1—H1···O1A | 0.95 | 2.58 | 3.094 (6) | 114 |
C1—H1···O14 | 0.95 | 2.38 | 3.217 (6) | 146 |
C10—H10···O6 | 0.95 | 2.56 | 3.118 (7) | 118 |
C20—H20···O8 | 0.95 | 2.52 | 3.083 (6) | 118 |
C11—H11···O1B | 0.95 | 2.59 | 3.109 (6) | 115 |
Molecules containing two or more oxo-bridged Fe atoms have generated substantial interest and have been the subject of extensive investigation in a variety of contexts. These clusters exhibit interesting magnetic properties and have been found to behave as single-molecule magnets (Wernsdorfer & Sessoli, 1999). Moreover, polynuclear oxo-bridged iron units are located in the active sites of different proteins, and ferritin, the iron-storage protein found in most living organisms, contains a polynuclear oxo–iron(III) core (Gilles et al., 2002). The active sites in hemerythrin and myohemerythrin, the oxygen transport proteins, have been shown to contain dinuclear FeIII cores bridged by oxide and carboxylate ions (Stenkamp et al., 1984). An iron-based model compound for hemerythrin contains two FeIII ions bridged by oxide and carboxylate ions (Lippard et al., 1984). The typical hexacoordination of the iron centers in this cluster is completed by N atoms from imidazole groups. In Fe clusters, oxo, hydroxo and alkoxo bridges are a prominent feature because of the high affinity of Fe ions for oxygen-based ligands (Wilkinson et al., 1988). We report here the structures of a new dinuclear iron–oxo complex, [Fe2(µ-O)(µ-O2CCF3)2(O2CCF3)2(C10H8N2)2], (I), and a tetranuclear complex, [Fe4(µ3-O)2(µ-O2CCF3)6(O2CCF3)2(C10H8N2)2]. (HO2CCF3), (II). The synthesis of (II) is unusual in that it was obtained using (I) as a building block. The fluorinated peripheries of (I) and (II) enhance the solubility of the compounds as evidenced by the fact that both are soluble in acetone, tetrahydrofuran, acetonitrile, methanol, ethanol, nitromethane, dimethylformaldehyde and dimethyl sulfoxide. It is of interest to note that the trifluoroacetate ions are easily replaced by other ligands. Therefore, these compounds, together with suitable bridging ligands, can be used as precursors for new high-nuclearity clusters under mild reaction conditions. The iron centers are assigned a formal charge of +3 by summing the Fe—O bond valences (which are typical of FeIII ions; Brown & Altermatt, 1985).
The molecular structure of (I) contains an [Fe2O]4+ core bridged by an oxide ion and two trifluoroacetate groups (Fig. 1). Each FeIII ion is in a distorted octahedral environment and is coordinated to a µ-oxide ion, 2,2'-bipyridine and three trifluoroacetate ions. The ortho H atoms of the bipyridine unit donate hydrogen bonds to the bridging oxide ion and to the O atoms of the coordinated trifluoroacetate ions (C1—H1···O4, C7—H7···O1, C11—H11···O3 and C20—H20···O1). These H atoms enhance the chelating nature of bipyridine and may even result in monodentate coordination of some of the trifluoroacetate ions. The 2,2'-bipyridine is a capping ligand and is less labile than the trifluoroacetate ligands. Two of the four trifluoroacetate ions are bridging (and bidentate) while the other ions coordinate to the FeIII atom through one O atom. The trifluoro groups of the non-bridging trifluoroacetate ions are considerably disordered. The ordered trifluoro groups accept weak (but important) hydrogen bonds from the bipyridyl units (C20—H20···F22Ai, C2—H2···F22Ciii, C12—H12···F24Aiv, C12—H12···F24Bv, C10—H10···F24Cvi; symmetry codes are given in Table 2). This behavior contrasts with that of the methyl groups of acetate ions, which normally donate hydrogen bonds. Thus, these trifluoro groups are anionic rather than cationic. The bridging trifluoro groups are disordered in a complicated manner; there is rotational disorder as well as displacement of the C—C axes. This disorder was modeled using three separate –CF3 components for each disordered –CF3 group (including C atoms) with C—F and F···F distances restrained to be equal, in order to maintain tetrahedral geometry, and refined. Only one component of the disorder is shown in Fig. 1. The C—O bond distances [1.246 (3)–1.252 (3) Å] of the bridging trifluoroacetate ions correspond to intermediate single and double bonds, while the C—O bond distances [1.213 (3) and 1.272 (3) Å] belonging to monodentate trifluoroacetate ions correspond to C—O single and double bonds. The complex is neutral and contains two FeIII centers and an oxide ion. All four trifluoroacetate groups are deprotonated. The Fe···Fe separation is 3.1492 (6) Å, which is typical for dinuclear FeIII complexes with bridging oxo and carboxylate groups (Christou et al., 2000). The bridging groups across the Fe···Fe internuclear axis are nearly eclipsing, with O—Fe—Fe—O torsion angles of 17.45 (8) and 16.31 (8)°. This conformation is, in part, a consequence of the rigidity of the O—C—O bond angles, which cannot accommodate a staggered arrangement across these two FeIII ions. The bridging carboxylate ligands also have an effect on the orientation of the two FeO4N2 coordination polyhedra. These two corner-sharing octahedra are tilted towards one another, with the dihedral angle between the N1/N2/Fe1/O1/O4 and N3/O8/Fe2/O1/O5 square planes being 35.73 (7)°.
The molecular structure of (II) contains an [Fe4O2]4+ core bridged by two µ3-oxide and six trifluoroacetate ions (Fig. 2). All FeIII ions are in distorted octahedral environments. The two outer FeIII ions, Fe1 and Fe2, are coordinated to 2,2'-bipyridine, a µ3-oxide and three bridging trifluoroacetate ions. As in (I), the H atoms ortho to the N atoms of the bipyridine group form hydrogen bonds with the bridging oxide ions and the O atoms of the coordinated trifluoroacetate ions (C1—H1···O1A, C10—H10···O6, C11—H11···O1B and C20—H20···O8). The trifluoroacetic acid solvent molecule of crystallization donates a hydrogen bond to an O atom of a coordinated trifluoroacetate ion (O18—H18A···O15). All the trifluoro groups are disordered and only one component of this disorder is shown in Fig. 2. Each of the two inner FeIII ions, Fe3 and Fe4, is coordinated to two µ3-oxide ions, three bridging trifluoroacetate ions and one monodentate trifluoroacetate ion. Several clusters containing [Fe4O2]4+ cores have been reported in the literature, but the two inner FeIII ions are usually bridged by carboxylate groups. In this new compound, the two FeIII ions are bridged by two oxide ions. The core is non-planar, with the Fe1/Fe3/Fe4 and Fe2/Fe3/Fe4 planes forming a dihedral angle of 28.76 (3)°. The two inner FeIII ions and two µ3-oxide ions, however, are nearly coplanar. Atoms O1A and O1B are displaced 0.053 (11) Å from the Fe3/Fe4/O1A/O1B plane. The [Fe4O2]4+ core has no imposed crystallographic symmetry, even though we might expect a core of this type to have D2 h or C2 symmetry. This absence of symmetry is a consequence of the two pairs of iron(III) atoms Fe1 and Fe4, and Fe2 and Fe3, being bridged by two carboxylate groups each, while the two pairs Fe1 and Fe3, and Fe2 and Fe4, are bridged by a single carboxylate ligand each. The distances between atoms Fe1 and Fe4 [3.3063 (9) Å], and Fe2 and Fe3 [3.3131 (11) Å], are therefore shorter than the distances between atoms Fe1 and Fe3 [3.4735 (11) Å], and Fe2 and Fe4 [3.4505 (12) Å]. The shortest Fe···Fe separation [Fe3···Fe4 = 2.8934 (11) Å] occurs between the two inner FeIII atoms and is typical for [Fe4O2]4+ clusters.
It is worth noting some of the differences between acetate and trifluoroacetate ions. Replacing electropositive H with F atoms results in a reduction of the negative charge on the carboxylate O atoms, weaker coordination bonds to metal cations and slightly longer C—C bond distances. The carboxylate groups reduce the negative charge on the F atoms substantially. These F atoms have slight anionic character and form weak intermolecular bonds, and therefore CF3 groups are typically disordered.
Magnetic data clearly indicate that both complexes exhibit an S = 0 ground state, which arises from antiferromagnetic coupling of the FeIII ions. An increase in the effective moment of the complex is observed as the temperature is increased as aresult of thermal population of spin states with S greater than 0.