The title compound, [Fe10(C14H11O2)10(CH3O)20], takes the form of a so-called `ferric wheel', consisting of ten Fe cations, linked by carboxylate and methoxo anions. The complex is ring-shaped with the moiety formula [FeIII(carboxylate)(methoxo)2]10 and is located on a crystallographic inversion centre. The unit cell contains two independent regions filled with disordered solvent of unknown composition.
Supporting information
CCDC reference: 182579
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.015 Å
- R factor = 0.078
- wR factor = 0.173
- Data-to-parameter ratio = 16.5
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
RINTA_01 Alert C The value of Rint is greater than 0.10
Rint given 0.119
PLAT_213 Alert C Atom C31A has ADP max/min Ratio ........... 3.20 prolate
PLAT_213 Alert C Atom C107 has ADP max/min Ratio ........... 3.30 prolate
PLAT_213 Alert C Atom C205 has ADP max/min Ratio ........... 3.30 prolate
PLAT_213 Alert C Atom C206 has ADP max/min Ratio ........... 3.80 prolate
PLAT_213 Alert C Atom C207 has ADP max/min Ratio ........... 3.50 prolate
PLAT_213 Alert C Atom C208 has ADP max/min Ratio ........... 3.50 prolate
PLAT_213 Alert C Atom C209 has ADP max/min Ratio ........... 3.40 prolate
PLAT_368 Alert C Short C(sp2)-C(sp2) Bond C(413) - C(414) = 1.19 Ang.
PLAT_602 Alert C VERY LARGE Solvent Accessible VOID(S) in Structure !
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
10 Alert Level C = Please check
The title compound was obtained as a side product in the preparation of
complexes of FeIII cations with
N,N-bis(2-ethyl-5-methylimidazol-4-ylmethyl)aminopropane in the
presence of 2,2-diphenylacetate anions. Crystals were obtained by vapor
diffusion of diethyl ether and toluene into a solution of the complex mixture
in methanol.
The disorder of the Me moieties of the methoxo ions located on the inside of the
ring is described with a two-site model. The occupation factor of the major
component refined to a value of 0.696 (4). Disordered solvent is present in two
voids per unit cell, each located on a crystallographic inversion centre.
Solvents used in synthesis and crystallization (toluene, diethyl ether and
methanol) could not be recognized in the disordered electron density. The
contribution of the disordered solved to the diffraction pattern was therefore
incorporated in the model using PLATON/SQUEEZE (van der Sluis & Spek,
1990; Spek, 2002). A total of 75 e were found in a void of 453 Å3 [located
at (0,0,0)], whereas 92 e were found in a void of 323 Å3 [located at
(0,1/2,0)]. Methyl moieties were described as rigid groups with the C atom as
carrier and were allowed to rotate around the C—C bond. All other H atoms
were included at calculated positions, riding on their carrier atoms.
Isotropic displacement parameters of the H atoms were coupled to the
equivalent isotropic displacement parameter of their carrier atoms by a fixed
factor.
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2002); software used to prepare material for publication: PLATON.
Crystal data top
[Fe10(C14H11O2)10(CH3O)20] | Z = 1 |
Mr = 3291.47 | F(000) = 1710 |
Triclinic, P1 | Quoted _cell_measurement_* data items refer to the initial cell
determination. The cell parameters as reported in _cell_* are based
on the complete data set. |
Hall symbol: -P 1 | Dx = 1.235 Mg m−3 |
a = 12.4268 (12) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 18.8782 (16) Å | Cell parameters from 408 reflections |
c = 19.5576 (16) Å | θ = 2.0–25.0° |
α = 82.98 (1)° | µ = 0.86 mm−1 |
β = 77.686 (10)° | T = 150 K |
γ = 82.656 (10)° | Block, brown |
V = 4424.4 (7) Å3 | 0.20 × 0.15 × 0.10 mm |
Data collection top
Nonius KappaCCD area-detector diffractometer | 8452 reflections with I > 2σ(I) |
Radiation source: Rotating Anode | Rint = 0.119 |
Graphite monochromator | θmax = 25.4°, θmin = 1.1° |
Detector resolution: 18.4 pixels mm-1 | h = −14→14 |
ϕ scans and ω scans with κ offset | k = −22→22 |
91822 measured reflections | l = −23→23 |
16169 independent reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.078 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.173 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.05P)2 + 5.P] where P = (Fo2 + 2Fc2)/3 |
16169 reflections | (Δ/σ)max = 0.008 |
977 parameters | Δρmax = 0.79 e Å−3 |
960 restraints | Δρmin = −0.52 e Å−3 |
Crystal data top
[Fe10(C14H11O2)10(CH3O)20] | γ = 82.656 (10)° |
Mr = 3291.47 | V = 4424.4 (7) Å3 |
Triclinic, P1 | Z = 1 |
a = 12.4268 (12) Å | Mo Kα radiation |
b = 18.8782 (16) Å | µ = 0.86 mm−1 |
c = 19.5576 (16) Å | T = 150 K |
α = 82.98 (1)° | 0.20 × 0.15 × 0.10 mm |
β = 77.686 (10)° | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 8452 reflections with I > 2σ(I) |
91822 measured reflections | Rint = 0.119 |
16169 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.078 | 960 restraints |
wR(F2) = 0.173 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | Δρmax = 0.79 e Å−3 |
16169 reflections | Δρmin = −0.52 e Å−3 |
977 parameters | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Refinement. Refinement on F2 for ALL reflections except those flagged by the user
for potential systematic errors. Weighted R-factors wR and all
goodnesses of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The observed criterion of F2 > σ(F2)
is used only for calculating -R-factor-obs etc. and is not
relevant to the choice of reflections for refinement. R-factors based
on F2 are statistically about twice as large as those based on
F, and R-factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.27243 (7) | 0.22868 (4) | 1.05187 (4) | 0.0440 (3) | |
Fe2 | 0.38596 (7) | 0.23537 (4) | 0.89897 (4) | 0.0532 (3) | |
Fe3 | 0.53431 (8) | 0.15450 (4) | 0.78439 (4) | 0.0620 (3) | |
Fe4 | 0.67531 (8) | 0.01627 (4) | 0.74884 (4) | 0.0584 (3) | |
Fe5 | 0.75093 (7) | −0.13007 (4) | 0.81350 (4) | 0.0442 (3) | |
O11 | 0.2990 (3) | 0.17064 (17) | 0.97046 (16) | 0.0470 (13) | |
O12 | 0.3970 (3) | 0.27267 (18) | 0.98749 (16) | 0.0483 (11) | |
O21 | 0.5269 (3) | 0.17301 (18) | 0.88311 (16) | 0.0498 (13) | |
O22 | 0.3775 (4) | 0.1885 (2) | 0.81577 (18) | 0.0672 (15) | |
O31 | 0.5270 (4) | 0.04968 (18) | 0.80112 (17) | 0.0555 (14) | |
O32 | 0.6932 (3) | 0.11705 (18) | 0.76016 (18) | 0.0638 (14) | |
O41 | 0.7340 (3) | −0.02857 (17) | 0.83229 (16) | 0.0476 (13) | |
O42 | 0.6505 (3) | −0.08477 (18) | 0.75033 (17) | 0.0547 (14) | |
O51 | 0.6352 (3) | −0.16310 (17) | 0.89202 (16) | 0.0408 (11) | |
O52 | 0.8387 (3) | −0.17137 (18) | 0.88552 (17) | 0.0481 (12) | |
O101 | 0.1591 (3) | 0.2966 (2) | 1.00747 (18) | 0.0582 (14) | |
O102 | 0.2465 (3) | 0.3024 (2) | 0.89440 (18) | 0.0672 (16) | |
O201 | 0.4661 (4) | 0.31626 (19) | 0.83888 (19) | 0.0724 (14) | |
O202 | 0.5745 (4) | 0.2568 (2) | 0.75261 (19) | 0.0805 (16) | |
O301 | 0.5180 (4) | 0.1501 (2) | 0.68360 (18) | 0.0829 (16) | |
O302 | 0.6266 (4) | 0.0494 (2) | 0.65520 (18) | 0.0756 (16) | |
O401 | 0.8317 (4) | −0.0017 (2) | 0.68881 (18) | 0.0703 (14) | |
O402 | 0.8872 (3) | −0.11053 (19) | 0.73759 (17) | 0.0572 (14) | |
O501 | 0.7637 (3) | −0.22763 (18) | 0.77654 (16) | 0.0493 (13) | |
O502 | 0.7471 (3) | −0.30137 (17) | 0.87623 (17) | 0.0461 (14) | |
C11A | 0.2131 (8) | 0.1324 (5) | 0.9576 (4) | 0.062 (3) | 0.696 (4) |
C12 | 0.4332 (6) | 0.3404 (3) | 0.9930 (3) | 0.075 (3) | |
C21A | 0.6207 (8) | 0.1884 (5) | 0.9066 (5) | 0.069 (3) | 0.696 (4) |
C22 | 0.2929 (7) | 0.2041 (5) | 0.7743 (3) | 0.105 (3) | |
C31A | 0.4379 (10) | 0.0178 (6) | 0.8070 (10) | 0.158 (7) | 0.696 (4) |
C32 | 0.7784 (6) | 0.1578 (3) | 0.7226 (4) | 0.095 (3) | |
C41A | 0.8120 (9) | 0.0035 (5) | 0.8586 (5) | 0.075 (4) | 0.696 (4) |
C42 | 0.6230 (7) | −0.1182 (4) | 0.6955 (4) | 0.095 (3) | |
C51A | 0.5295 (7) | −0.1819 (5) | 0.8812 (4) | 0.064 (3) | 0.696 (4) |
C52 | 0.9546 (5) | −0.1881 (4) | 0.8747 (4) | 0.084 (3) | |
C103 | 0.1654 (5) | 0.3173 (3) | 0.9433 (3) | 0.063 (2) | |
C104 | 0.0666 (6) | 0.3656 (4) | 0.9217 (3) | 0.082 (3) | |
C105 | 0.0902 (8) | 0.4446 (4) | 0.9044 (4) | 0.096 (3) | |
C106 | −0.0015 (8) | 0.4963 (5) | 0.9144 (4) | 0.131 (4) | |
C107 | 0.0141 (11) | 0.5698 (6) | 0.8968 (6) | 0.144 (4) | |
C108 | 0.1177 (13) | 0.5889 (7) | 0.8751 (7) | 0.180 (6) | |
C109 | 0.2063 (11) | 0.5398 (5) | 0.8667 (7) | 0.190 (6) | |
C110 | 0.1924 (10) | 0.4681 (5) | 0.8832 (6) | 0.146 (4) | |
C111 | 0.0366 (6) | 0.3337 (5) | 0.8609 (4) | 0.087 (3) | |
C112 | −0.0183 (8) | 0.2740 (6) | 0.8765 (5) | 0.121 (4) | |
C113 | −0.0414 (8) | 0.2419 (6) | 0.8220 (5) | 0.143 (5) | |
C114 | −0.0100 (8) | 0.2683 (7) | 0.7531 (5) | 0.130 (5) | |
C115 | 0.0435 (7) | 0.3304 (6) | 0.7373 (4) | 0.117 (4) | |
C116 | 0.0653 (6) | 0.3614 (5) | 0.7919 (4) | 0.097 (3) | |
C203 | 0.5387 (6) | 0.3124 (3) | 0.7835 (3) | 0.078 (3) | |
C204 | 0.5870 (7) | 0.3808 (4) | 0.7503 (4) | 0.104 (3) | |
C205 | 0.5170 (10) | 0.4241 (4) | 0.7023 (4) | 0.128 (3) | |
C206 | 0.4150 (10) | 0.4059 (7) | 0.6992 (8) | 0.234 (6) | |
C207 | 0.3496 (11) | 0.4375 (9) | 0.6451 (9) | 0.303 (8) | |
C208 | 0.3971 (13) | 0.4987 (9) | 0.6048 (9) | 0.264 (7) | |
C209 | 0.4950 (13) | 0.5162 (6) | 0.6067 (6) | 0.181 (5) | |
C210 | 0.5557 (10) | 0.4789 (4) | 0.6535 (4) | 0.145 (4) | |
C211 | 0.6163 (9) | 0.4226 (4) | 0.8068 (5) | 0.114 (3) | |
C212 | 0.7147 (11) | 0.4078 (7) | 0.8251 (8) | 0.190 (6) | |
C213 | 0.7404 (11) | 0.4401 (8) | 0.8798 (9) | 0.221 (7) | |
C214 | 0.6609 (12) | 0.4878 (7) | 0.9142 (8) | 0.186 (6) | |
C215 | 0.5623 (10) | 0.5030 (4) | 0.8966 (6) | 0.130 (4) | |
C216 | 0.5394 (8) | 0.4699 (4) | 0.8422 (4) | 0.122 (3) | |
C303 | 0.5678 (6) | 0.1066 (3) | 0.6403 (3) | 0.073 (3) | |
C304 | 0.5549 (7) | 0.1239 (3) | 0.5638 (3) | 0.081 (2) | |
C305 | 0.5971 (6) | 0.1949 (4) | 0.5334 (3) | 0.078 (3) | |
C306 | 0.6725 (9) | 0.1953 (6) | 0.4728 (5) | 0.176 (5) | |
C307 | 0.7116 (11) | 0.2539 (8) | 0.4403 (8) | 0.227 (7) | |
C308 | 0.6879 (9) | 0.3182 (7) | 0.4735 (7) | 0.150 (5) | |
C309 | 0.6058 (9) | 0.3221 (5) | 0.5303 (5) | 0.129 (4) | |
C310 | 0.5602 (8) | 0.2561 (4) | 0.5613 (4) | 0.102 (3) | |
C311 | 0.4395 (8) | 0.1174 (4) | 0.5547 (3) | 0.088 (3) | |
C312 | 0.3435 (8) | 0.1598 (5) | 0.5880 (4) | 0.112 (3) | |
C313 | 0.2367 (9) | 0.1546 (6) | 0.5768 (5) | 0.130 (4) | |
C314 | 0.2237 (11) | 0.1089 (7) | 0.5294 (6) | 0.164 (6) | |
C315 | 0.3162 (12) | 0.0755 (6) | 0.4896 (6) | 0.147 (5) | |
C316 | 0.4175 (11) | 0.0823 (6) | 0.5007 (6) | 0.142 (5) | |
C403 | 0.9013 (6) | −0.0559 (3) | 0.6940 (3) | 0.063 (2) | |
C404 | 1.0114 (6) | −0.0529 (4) | 0.6428 (3) | 0.078 (2) | |
C405 | 1.0205 (6) | −0.0994 (4) | 0.5842 (3) | 0.076 (3) | |
C406 | 0.9820 (7) | −0.1637 (4) | 0.5939 (4) | 0.106 (3) | |
C407 | 0.9998 (9) | −0.2071 (5) | 0.5400 (4) | 0.155 (5) | |
C408 | 1.0575 (10) | −0.1802 (6) | 0.4722 (5) | 0.158 (5) | |
C409 | 1.0974 (8) | −0.1160 (5) | 0.4644 (4) | 0.116 (4) | |
C410 | 1.0804 (6) | −0.0764 (4) | 0.5179 (3) | 0.087 (3) | |
C411 | 1.1088 (9) | −0.0740 (7) | 0.6795 (5) | 0.151 (5) | |
C412 | 1.1442 (8) | −0.1446 (8) | 0.7013 (5) | 0.169 (5) | |
C413 | 1.2340 (11) | −0.1691 (11) | 0.7309 (9) | 0.257 (8) | |
C414 | 1.3002 (17) | −0.1280 (13) | 0.7293 (10) | 0.321 (10) | |
C415 | 1.2887 (15) | −0.0626 (13) | 0.7022 (11) | 0.326 (10) | |
C416 | 1.1887 (13) | −0.0387 (10) | 0.6724 (9) | 0.267 (8) | |
C503 | 0.7563 (5) | −0.2889 (3) | 0.8106 (3) | 0.0472 (19) | |
C504 | 0.7601 (6) | −0.3518 (3) | 0.7690 (3) | 0.0632 (19) | |
C505 | 0.8749 (7) | −0.3770 (3) | 0.7346 (3) | 0.078 (3) | |
C506 | 0.8982 (9) | −0.4436 (4) | 0.7111 (4) | 0.124 (4) | |
C507 | 1.0007 (12) | −0.4698 (7) | 0.6775 (6) | 0.164 (6) | |
C508 | 1.0854 (12) | −0.4299 (7) | 0.6699 (7) | 0.190 (6) | |
C509 | 1.0715 (9) | −0.3613 (6) | 0.6932 (6) | 0.187 (5) | |
C510 | 0.9638 (8) | −0.3377 (4) | 0.7253 (4) | 0.118 (3) | |
C511 | 0.6794 (8) | −0.3330 (3) | 0.7173 (4) | 0.083 (3) | |
C512 | 0.5708 (10) | −0.3480 (5) | 0.7384 (6) | 0.148 (4) | |
C513 | 0.4946 (12) | −0.3267 (6) | 0.6940 (8) | 0.193 (6) | |
C514 | 0.5360 (15) | −0.2923 (6) | 0.6267 (9) | 0.191 (6) | |
C515 | 0.6415 (12) | −0.2784 (6) | 0.6062 (6) | 0.152 (5) | |
C516 | 0.7160 (9) | −0.2974 (4) | 0.6514 (4) | 0.114 (3) | |
C11B | 0.3198 (17) | 0.0941 (11) | 0.9716 (10) | 0.0610* | 0.304 (4) |
C21B | 0.5560 (17) | 0.1179 (11) | 0.9380 (11) | 0.0700* | 0.304 (4) |
C31B | 0.469 (3) | 0.013 (2) | 0.871 (2) | 0.1570* | 0.304 (4) |
C41B | 0.7069 (19) | −0.0030 (12) | 0.8996 (11) | 0.0750* | 0.304 (4) |
C51B | 0.5432 (16) | −0.1179 (11) | 0.9245 (10) | 0.0640* | 0.304 (4) |
H12C | 0.43360 | 0.34500 | 1.04230 | 0.1120* | |
H21A | 0.61560 | 0.16980 | 0.95600 | 0.1040* | 0.696 (4) |
H11A | 0.24680 | 0.09210 | 0.93040 | 0.0920* | 0.696 (4) |
H11B | 0.16520 | 0.16500 | 0.93120 | 0.0920* | 0.696 (4) |
H11C | 0.16910 | 0.11420 | 1.00260 | 0.0920* | 0.696 (4) |
H12A | 0.38270 | 0.37920 | 0.97550 | 0.1120* | |
H12B | 0.50820 | 0.34320 | 0.96480 | 0.1120* | |
H31A | 0.45630 | −0.02560 | 0.78220 | 0.2350* | 0.696 (4) |
H31B | 0.38270 | 0.05040 | 0.78640 | 0.2350* | 0.696 (4) |
H31C | 0.40770 | 0.00480 | 0.85690 | 0.2350* | 0.696 (4) |
H32A | 0.84690 | 0.12590 | 0.71040 | 0.1420* | |
H32B | 0.79040 | 0.19350 | 0.75190 | 0.1420* | |
H32C | 0.75720 | 0.18220 | 0.67960 | 0.1420* | |
H41A | 0.79780 | 0.05590 | 0.85120 | 0.1120* | 0.696 (4) |
H41B | 0.88700 | −0.01180 | 0.83380 | 0.1120* | 0.696 (4) |
H41C | 0.80520 | −0.01130 | 0.90900 | 0.1120* | 0.696 (4) |
H42A | 0.57210 | −0.08490 | 0.67200 | 0.1420* | |
H21B | 0.62340 | 0.24050 | 0.90180 | 0.1040* | 0.696 (4) |
H21C | 0.68800 | 0.16580 | 0.87810 | 0.1040* | 0.696 (4) |
H22A | 0.31630 | 0.23960 | 0.73470 | 0.1580* | |
H22B | 0.22370 | 0.22330 | 0.80350 | 0.1580* | |
H22C | 0.28130 | 0.16000 | 0.75640 | 0.1580* | |
H52A | 0.97620 | −0.20340 | 0.92010 | 0.1250* | |
H52B | 0.99090 | −0.14550 | 0.85260 | 0.1250* | |
H52C | 0.97720 | −0.22690 | 0.84400 | 0.1250* | |
H104 | 0.00240 | 0.36310 | 0.96230 | 0.0980* | |
H106 | −0.07360 | 0.48230 | 0.93290 | 0.1570* | |
H107 | −0.04780 | 0.60520 | 0.90020 | 0.1720* | |
H108 | 0.12820 | 0.63840 | 0.86550 | 0.2150* | |
H109 | 0.27840 | 0.55440 | 0.84960 | 0.2280* | |
H110 | 0.25610 | 0.43400 | 0.87960 | 0.1750* | |
H112 | −0.04040 | 0.25480 | 0.92390 | 0.1450* | |
H113 | −0.08020 | 0.20040 | 0.83280 | 0.1710* | |
H114 | −0.02470 | 0.24450 | 0.71650 | 0.1560* | |
H115 | 0.06430 | 0.35060 | 0.69010 | 0.1410* | |
H116 | 0.10170 | 0.40390 | 0.78170 | 0.1160* | |
H204 | 0.65920 | 0.36550 | 0.71920 | 0.1250* | |
H206 | 0.38380 | 0.37050 | 0.73400 | 0.2800* | |
H207 | 0.28510 | 0.41950 | 0.63830 | 0.3630* | |
H208 | 0.35510 | 0.52840 | 0.57490 | 0.3170* | |
H209 | 0.52450 | 0.55480 | 0.57560 | 0.2170* | |
H210 | 0.62770 | 0.49170 | 0.65200 | 0.1740* | |
H212 | 0.76880 | 0.37470 | 0.80060 | 0.2280* | |
H213 | 0.81060 | 0.42910 | 0.89260 | 0.2650* | |
H214 | 0.67660 | 0.51050 | 0.95120 | 0.2230* | |
H215 | 0.50800 | 0.53610 | 0.92100 | 0.1570* | |
H216 | 0.46880 | 0.48050 | 0.82970 | 0.1460* | |
H304 | 0.60450 | 0.08640 | 0.53680 | 0.0970* | |
H306 | 0.69820 | 0.15120 | 0.45300 | 0.2110* | |
H307 | 0.75610 | 0.25350 | 0.39430 | 0.2730* | |
H308 | 0.72920 | 0.35780 | 0.45590 | 0.1800* | |
H309 | 0.57870 | 0.36640 | 0.54930 | 0.1550* | |
H310 | 0.50300 | 0.25660 | 0.60220 | 0.1220* | |
H312 | 0.35210 | 0.19290 | 0.61900 | 0.1340* | |
H313 | 0.17420 | 0.18200 | 0.60150 | 0.1560* | |
H314 | 0.15180 | 0.10080 | 0.52460 | 0.1960* | |
H315 | 0.30890 | 0.04750 | 0.45390 | 0.1770* | |
H316 | 0.47940 | 0.06150 | 0.46940 | 0.1700* | |
H404 | 1.01590 | −0.00230 | 0.62140 | 0.0930* | |
H406 | 0.94160 | −0.17970 | 0.63890 | 0.1270* | |
H407 | 0.97450 | −0.25340 | 0.54750 | 0.1860* | |
H408 | 1.06760 | −0.20740 | 0.43310 | 0.1900* | |
H409 | 1.13810 | −0.09880 | 0.41990 | 0.1390* | |
H410 | 1.10970 | −0.03140 | 0.51110 | 0.1050* | |
H412 | 1.10060 | −0.18010 | 0.69470 | 0.2030* | |
H413 | 1.24330 | −0.21700 | 0.75200 | 0.3080* | |
H414 | 1.36380 | −0.14420 | 0.74890 | 0.3860* | |
H415 | 1.34250 | −0.03080 | 0.70120 | 0.3910* | |
H416 | 1.18540 | 0.00690 | 0.64600 | 0.3210* | |
H504 | 0.73140 | −0.39220 | 0.80320 | 0.0760* | |
H506 | 0.83970 | −0.47340 | 0.71860 | 0.1490* | |
H507 | 1.01200 | −0.51540 | 0.65970 | 0.1970* | |
H508 | 1.15730 | −0.44880 | 0.64800 | 0.2280* | |
H509 | 1.13130 | −0.33300 | 0.68760 | 0.2250* | |
H510 | 0.95090 | −0.29150 | 0.74180 | 0.1420* | |
H512 | 0.54730 | −0.37290 | 0.78320 | 0.1780* | |
H513 | 0.41890 | −0.33500 | 0.70850 | 0.2310* | |
H514 | 0.48700 | −0.27860 | 0.59500 | 0.2290* | |
H515 | 0.66610 | −0.25550 | 0.56050 | 0.1830* | |
H516 | 0.79040 | −0.28610 | 0.63740 | 0.1370* | |
H42B | 0.58750 | −0.16160 | 0.71560 | 0.1420* | |
H42C | 0.69070 | −0.13110 | 0.66130 | 0.1420* | |
H51A | 0.48470 | −0.19850 | 0.92650 | 0.0950* | 0.696 (4) |
H51B | 0.54360 | −0.22010 | 0.84980 | 0.0950* | 0.696 (4) |
H51C | 0.48950 | −0.13960 | 0.86010 | 0.0950* | 0.696 (4) |
H11D | 0.24920 | 0.07310 | 0.98170 | 0.0920* | 0.304 (4) |
H11E | 0.36180 | 0.07530 | 1.00820 | 0.0920* | 0.304 (4) |
H11F | 0.36260 | 0.08130 | 0.92580 | 0.0920* | 0.304 (4) |
H21D | 0.63520 | 0.10150 | 0.92620 | 0.1040* | 0.304 (4) |
H21E | 0.51300 | 0.07720 | 0.94120 | 0.1040* | 0.304 (4) |
H21F | 0.53930 | 0.13830 | 0.98330 | 0.1040* | 0.304 (4) |
H31D | 0.43090 | 0.04950 | 0.90150 | 0.2350* | 0.304 (4) |
H31E | 0.52400 | −0.01750 | 0.89320 | 0.2350* | 0.304 (4) |
H31F | 0.41500 | −0.01640 | 0.86170 | 0.2350* | 0.304 (4) |
H41D | 0.76260 | 0.02760 | 0.90400 | 0.1120* | 0.304 (4) |
H41E | 0.70540 | −0.04380 | 0.93590 | 0.1120* | 0.304 (4) |
H41F | 0.63390 | 0.02480 | 0.90560 | 0.1120* | 0.304 (4) |
H51D | 0.47470 | −0.13290 | 0.91650 | 0.0950* | 0.304 (4) |
H51E | 0.55030 | −0.06810 | 0.90440 | 0.0950* | 0.304 (4) |
H51F | 0.54120 | −0.12130 | 0.97520 | 0.0950* | 0.304 (4) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0642 (6) | 0.0314 (4) | 0.0294 (4) | 0.0070 (4) | −0.0046 (4) | 0.0030 (3) |
Fe2 | 0.0879 (7) | 0.0296 (5) | 0.0305 (4) | 0.0104 (4) | 0.0006 (4) | 0.0031 (3) |
Fe3 | 0.1128 (8) | 0.0301 (5) | 0.0278 (4) | 0.0158 (5) | 0.0025 (4) | 0.0030 (3) |
Fe4 | 0.1044 (7) | 0.0287 (5) | 0.0296 (4) | 0.0134 (5) | −0.0008 (4) | 0.0024 (3) |
Fe5 | 0.0676 (6) | 0.0292 (4) | 0.0298 (4) | 0.0042 (4) | −0.0054 (4) | 0.0034 (3) |
O11 | 0.077 (3) | 0.031 (2) | 0.0300 (18) | −0.0001 (18) | −0.0094 (17) | 0.0001 (15) |
O12 | 0.071 (2) | 0.031 (2) | 0.0353 (19) | 0.0029 (18) | 0.0015 (17) | −0.0035 (15) |
O21 | 0.082 (3) | 0.029 (2) | 0.0292 (18) | 0.0089 (19) | 0.0020 (18) | −0.0057 (15) |
O22 | 0.110 (3) | 0.054 (3) | 0.0290 (19) | 0.025 (2) | −0.013 (2) | −0.0076 (17) |
O31 | 0.100 (3) | 0.026 (2) | 0.0318 (19) | 0.011 (2) | −0.0064 (19) | 0.0012 (15) |
O32 | 0.106 (3) | 0.027 (2) | 0.039 (2) | 0.003 (2) | 0.021 (2) | −0.0003 (16) |
O41 | 0.080 (3) | 0.0288 (19) | 0.0272 (18) | −0.0021 (18) | −0.0002 (17) | 0.0013 (14) |
O42 | 0.095 (3) | 0.029 (2) | 0.036 (2) | 0.0164 (19) | −0.0200 (19) | 0.0011 (15) |
O51 | 0.049 (2) | 0.0274 (19) | 0.0394 (19) | 0.0064 (17) | −0.0046 (16) | 0.0046 (15) |
O52 | 0.057 (2) | 0.046 (2) | 0.038 (2) | −0.0027 (19) | −0.0098 (17) | 0.0059 (16) |
O101 | 0.073 (3) | 0.053 (2) | 0.036 (2) | 0.020 (2) | −0.0053 (18) | 0.0073 (18) |
O102 | 0.093 (3) | 0.056 (3) | 0.034 (2) | 0.030 (2) | −0.003 (2) | 0.0114 (18) |
O201 | 0.114 (3) | 0.027 (2) | 0.049 (2) | 0.012 (2) | 0.028 (2) | 0.0043 (17) |
O202 | 0.142 (4) | 0.029 (2) | 0.041 (2) | 0.016 (2) | 0.026 (2) | 0.0078 (17) |
O301 | 0.163 (4) | 0.040 (2) | 0.026 (2) | 0.036 (3) | −0.006 (2) | 0.0021 (17) |
O302 | 0.143 (4) | 0.040 (2) | 0.031 (2) | 0.027 (2) | −0.014 (2) | 0.0024 (17) |
O401 | 0.115 (3) | 0.033 (2) | 0.040 (2) | 0.012 (2) | 0.017 (2) | 0.0078 (18) |
O402 | 0.080 (3) | 0.041 (2) | 0.038 (2) | 0.002 (2) | 0.0064 (19) | 0.0042 (17) |
O501 | 0.082 (3) | 0.0264 (19) | 0.0339 (19) | 0.0108 (18) | −0.0108 (18) | 0.0003 (15) |
O502 | 0.074 (3) | 0.027 (2) | 0.0298 (19) | 0.0118 (18) | −0.0061 (18) | 0.0013 (15) |
C11A | 0.087 (7) | 0.056 (6) | 0.044 (5) | −0.014 (5) | −0.014 (4) | −0.006 (4) |
C12 | 0.114 (6) | 0.046 (4) | 0.058 (4) | −0.027 (4) | 0.012 (4) | −0.012 (3) |
C21A | 0.077 (6) | 0.068 (7) | 0.056 (5) | 0.004 (5) | 0.006 (4) | −0.024 (5) |
C22 | 0.130 (6) | 0.133 (7) | 0.050 (4) | 0.038 (6) | −0.033 (4) | −0.027 (4) |
C31A | 0.088 (7) | 0.040 (7) | 0.31 (2) | 0.002 (6) | 0.044 (11) | −0.031 (10) |
C32 | 0.131 (6) | 0.033 (4) | 0.092 (5) | −0.005 (4) | 0.041 (5) | −0.008 (4) |
C41A | 0.123 (9) | 0.034 (5) | 0.068 (6) | −0.004 (5) | −0.025 (6) | −0.002 (4) |
C42 | 0.155 (7) | 0.062 (5) | 0.082 (5) | 0.025 (5) | −0.076 (5) | −0.012 (4) |
C51A | 0.070 (6) | 0.047 (6) | 0.065 (6) | −0.004 (5) | −0.006 (5) | 0.014 (4) |
C52 | 0.059 (4) | 0.111 (6) | 0.076 (5) | −0.015 (4) | −0.019 (4) | 0.025 (4) |
C103 | 0.078 (4) | 0.054 (4) | 0.043 (3) | 0.018 (3) | −0.006 (3) | 0.008 (3) |
C104 | 0.087 (5) | 0.091 (4) | 0.053 (4) | 0.039 (4) | −0.017 (3) | 0.006 (3) |
C105 | 0.129 (6) | 0.081 (4) | 0.067 (5) | 0.051 (4) | −0.042 (5) | 0.007 (4) |
C106 | 0.168 (7) | 0.107 (6) | 0.102 (6) | 0.088 (6) | −0.056 (6) | −0.007 (5) |
C107 | 0.202 (9) | 0.102 (6) | 0.122 (8) | 0.099 (7) | −0.084 (8) | −0.019 (6) |
C108 | 0.226 (11) | 0.093 (7) | 0.202 (12) | 0.074 (7) | −0.070 (12) | 0.010 (7) |
C109 | 0.194 (9) | 0.063 (6) | 0.281 (14) | 0.035 (6) | −0.030 (10) | 0.025 (8) |
C110 | 0.152 (7) | 0.067 (5) | 0.202 (10) | 0.033 (5) | −0.045 (8) | 0.020 (6) |
C111 | 0.087 (5) | 0.107 (6) | 0.054 (4) | 0.025 (4) | −0.014 (4) | 0.011 (4) |
C112 | 0.145 (8) | 0.136 (8) | 0.075 (5) | −0.015 (6) | −0.017 (5) | 0.007 (5) |
C113 | 0.145 (8) | 0.189 (10) | 0.098 (6) | −0.042 (7) | −0.019 (6) | −0.010 (6) |
C114 | 0.096 (7) | 0.210 (11) | 0.090 (5) | −0.020 (6) | −0.023 (5) | −0.022 (6) |
C115 | 0.091 (7) | 0.189 (10) | 0.065 (5) | −0.002 (6) | −0.016 (5) | 0.003 (5) |
C116 | 0.094 (6) | 0.132 (7) | 0.057 (4) | 0.005 (5) | −0.025 (4) | 0.020 (4) |
C203 | 0.122 (6) | 0.032 (3) | 0.054 (4) | 0.007 (3) | 0.024 (4) | 0.008 (3) |
C204 | 0.142 (6) | 0.037 (4) | 0.091 (5) | 0.006 (4) | 0.056 (4) | 0.006 (3) |
C205 | 0.184 (8) | 0.044 (4) | 0.098 (5) | 0.025 (5) | 0.060 (5) | 0.031 (4) |
C206 | 0.128 (8) | 0.187 (11) | 0.288 (13) | 0.036 (7) | 0.026 (7) | 0.187 (10) |
C207 | 0.154 (10) | 0.291 (15) | 0.354 (16) | 0.028 (8) | −0.002 (9) | 0.255 (13) |
C208 | 0.200 (12) | 0.191 (12) | 0.281 (14) | 0.073 (9) | 0.051 (10) | 0.172 (11) |
C209 | 0.257 (12) | 0.077 (7) | 0.127 (8) | 0.038 (8) | 0.072 (8) | 0.059 (6) |
C210 | 0.266 (10) | 0.046 (5) | 0.078 (6) | −0.010 (6) | 0.051 (6) | 0.011 (4) |
C211 | 0.143 (7) | 0.034 (4) | 0.125 (6) | −0.008 (5) | 0.059 (5) | −0.005 (4) |
C212 | 0.140 (8) | 0.154 (10) | 0.267 (14) | −0.003 (8) | 0.027 (8) | −0.124 (10) |
C213 | 0.147 (9) | 0.199 (12) | 0.327 (16) | −0.017 (8) | 0.002 (9) | −0.157 (11) |
C214 | 0.193 (11) | 0.129 (10) | 0.223 (12) | −0.036 (9) | 0.043 (9) | −0.095 (9) |
C215 | 0.184 (9) | 0.035 (5) | 0.139 (8) | −0.027 (6) | 0.056 (7) | −0.018 (5) |
C216 | 0.172 (7) | 0.034 (4) | 0.112 (6) | −0.005 (5) | 0.068 (5) | −0.001 (4) |
C303 | 0.136 (6) | 0.042 (4) | 0.029 (3) | 0.020 (4) | −0.008 (3) | 0.000 (3) |
C304 | 0.142 (5) | 0.054 (4) | 0.026 (3) | 0.035 (4) | 0.000 (3) | 0.002 (3) |
C305 | 0.087 (5) | 0.082 (4) | 0.045 (4) | 0.024 (4) | −0.004 (3) | 0.020 (3) |
C306 | 0.168 (9) | 0.124 (7) | 0.143 (8) | 0.072 (6) | 0.073 (7) | 0.079 (6) |
C307 | 0.177 (11) | 0.149 (9) | 0.256 (14) | 0.028 (9) | 0.098 (10) | 0.072 (8) |
C308 | 0.118 (8) | 0.150 (8) | 0.169 (10) | −0.049 (7) | −0.035 (6) | 0.087 (7) |
C309 | 0.196 (10) | 0.110 (6) | 0.099 (6) | −0.053 (7) | −0.073 (6) | 0.039 (5) |
C310 | 0.188 (8) | 0.068 (4) | 0.046 (4) | −0.029 (5) | −0.020 (4) | 0.019 (3) |
C311 | 0.149 (6) | 0.063 (5) | 0.045 (4) | −0.003 (4) | −0.004 (4) | −0.013 (3) |
C312 | 0.142 (6) | 0.115 (7) | 0.077 (5) | −0.004 (6) | −0.021 (5) | −0.016 (5) |
C313 | 0.128 (6) | 0.169 (9) | 0.088 (6) | −0.008 (7) | −0.006 (6) | −0.025 (5) |
C314 | 0.177 (9) | 0.173 (11) | 0.150 (10) | −0.080 (8) | 0.003 (8) | −0.049 (7) |
C315 | 0.212 (11) | 0.115 (8) | 0.130 (9) | −0.002 (9) | −0.061 (8) | −0.041 (6) |
C316 | 0.195 (9) | 0.118 (8) | 0.117 (7) | 0.035 (8) | −0.050 (7) | −0.047 (6) |
C403 | 0.104 (4) | 0.038 (4) | 0.037 (3) | −0.003 (3) | 0.002 (3) | 0.001 (3) |
C404 | 0.095 (4) | 0.063 (4) | 0.056 (4) | −0.001 (4) | 0.010 (3) | 0.020 (3) |
C405 | 0.090 (5) | 0.048 (4) | 0.060 (4) | 0.033 (3) | 0.017 (3) | 0.018 (3) |
C406 | 0.143 (7) | 0.070 (5) | 0.072 (5) | 0.003 (5) | 0.046 (5) | −0.012 (4) |
C407 | 0.247 (11) | 0.098 (7) | 0.087 (6) | −0.033 (7) | 0.063 (7) | −0.031 (5) |
C408 | 0.233 (11) | 0.112 (7) | 0.090 (6) | −0.013 (7) | 0.070 (7) | −0.038 (5) |
C409 | 0.154 (8) | 0.078 (5) | 0.072 (5) | 0.037 (5) | 0.033 (5) | 0.013 (4) |
C410 | 0.096 (5) | 0.071 (5) | 0.061 (4) | 0.032 (4) | 0.020 (4) | 0.015 (3) |
C411 | 0.132 (6) | 0.196 (10) | 0.121 (7) | −0.083 (6) | −0.039 (6) | 0.093 (7) |
C412 | 0.091 (7) | 0.249 (10) | 0.114 (7) | 0.043 (7) | 0.012 (5) | 0.068 (8) |
C413 | 0.101 (9) | 0.372 (17) | 0.238 (13) | −0.031 (9) | −0.014 (9) | 0.179 (13) |
C414 | 0.222 (15) | 0.43 (2) | 0.293 (16) | −0.118 (13) | −0.124 (13) | 0.250 (16) |
C415 | 0.197 (12) | 0.41 (2) | 0.38 (2) | −0.112 (14) | −0.167 (13) | 0.200 (17) |
C416 | 0.196 (12) | 0.345 (15) | 0.280 (15) | −0.119 (11) | −0.142 (11) | 0.158 (13) |
C503 | 0.067 (4) | 0.028 (3) | 0.041 (3) | 0.012 (3) | −0.010 (3) | −0.001 (2) |
C504 | 0.114 (4) | 0.029 (3) | 0.044 (3) | 0.004 (3) | −0.017 (3) | −0.003 (2) |
C505 | 0.130 (5) | 0.038 (4) | 0.045 (4) | 0.030 (4) | 0.002 (4) | 0.007 (3) |
C506 | 0.182 (8) | 0.077 (5) | 0.098 (6) | 0.042 (5) | −0.007 (6) | −0.047 (5) |
C507 | 0.207 (11) | 0.123 (9) | 0.130 (9) | 0.086 (7) | −0.002 (9) | −0.051 (8) |
C508 | 0.196 (10) | 0.131 (10) | 0.164 (10) | 0.067 (8) | 0.082 (10) | 0.003 (8) |
C509 | 0.160 (7) | 0.114 (8) | 0.201 (11) | 0.032 (6) | 0.106 (8) | 0.023 (7) |
C510 | 0.125 (6) | 0.065 (5) | 0.119 (7) | 0.026 (4) | 0.051 (6) | 0.002 (5) |
C511 | 0.160 (6) | 0.032 (4) | 0.072 (4) | 0.002 (4) | −0.061 (5) | −0.004 (3) |
C512 | 0.194 (8) | 0.074 (6) | 0.220 (9) | −0.065 (7) | −0.139 (7) | 0.043 (6) |
C513 | 0.244 (10) | 0.100 (8) | 0.292 (13) | −0.067 (8) | −0.191 (10) | 0.050 (9) |
C514 | 0.323 (13) | 0.075 (7) | 0.244 (12) | −0.048 (10) | −0.215 (12) | 0.018 (7) |
C515 | 0.301 (13) | 0.080 (7) | 0.107 (7) | 0.007 (9) | −0.126 (8) | −0.009 (5) |
C516 | 0.219 (8) | 0.070 (5) | 0.063 (4) | 0.019 (5) | −0.064 (5) | −0.015 (4) |
Geometric parameters (Å, º) top
Fe1—Fe2 | 3.0170 (11) | C52—H52B | 0.9806 |
Fe2—Fe3 | 3.0175 (12) | C52—H52C | 0.9792 |
Fe3—Fe4 | 3.0196 (12) | C203—C204 | 1.509 (10) |
Fe4—Fe5 | 3.0172 (11) | C204—C211 | 1.560 (12) |
Fe5—Fe1i | 3.0161 (11) | C104—H104 | 0.9997 |
Fe1—O11 | 1.989 (3) | C204—C205 | 1.512 (13) |
Fe1—O12 | 1.978 (4) | C205—C206 | 1.370 (18) |
Fe1—O101 | 2.042 (4) | C205—C210 | 1.379 (12) |
Fe1—O51i | 1.974 (4) | C206—C207 | 1.49 (2) |
Fe1—O52i | 1.978 (4) | C106—H106 | 0.9500 |
Fe1—O502i | 2.040 (3) | C107—H107 | 0.9489 |
Fe2—O11 | 1.973 (3) | C207—C208 | 1.43 (2) |
Fe2—O12 | 1.984 (3) | C108—H108 | 0.9504 |
Fe2—O21 | 1.970 (4) | C208—C209 | 1.31 (2) |
Fe2—O22 | 1.972 (4) | C109—H109 | 0.9505 |
Fe2—O102 | 2.022 (4) | C209—C210 | 1.380 (17) |
Fe2—O201 | 2.039 (4) | C110—H110 | 0.9503 |
Fe3—O21 | 1.985 (3) | C211—C212 | 1.333 (18) |
Fe3—O22 | 1.963 (5) | C211—C216 | 1.357 (12) |
Fe3—O31 | 1.976 (4) | C112—H112 | 0.9492 |
Fe3—O32 | 1.987 (4) | C212—C213 | 1.40 (2) |
Fe3—O202 | 2.046 (4) | C113—H113 | 0.9506 |
Fe3—O301 | 2.037 (4) | C213—C214 | 1.37 (2) |
Fe4—O31 | 1.974 (5) | C214—C215 | 1.33 (2) |
Fe4—O32 | 1.988 (4) | C114—H114 | 0.9503 |
Fe4—O41 | 1.981 (3) | C215—C216 | 1.393 (14) |
Fe4—O42 | 1.967 (4) | C115—H115 | 0.9496 |
Fe4—O302 | 2.051 (4) | C116—H116 | 0.9504 |
Fe4—O401 | 2.056 (5) | C303—C304 | 1.530 (8) |
Fe5—O41 | 1.972 (3) | C304—C305 | 1.509 (10) |
Fe5—O42 | 1.985 (4) | C304—C311 | 1.504 (13) |
Fe5—O51 | 1.967 (3) | C204—H204 | 1.0011 |
Fe5—O52 | 1.988 (4) | C305—C310 | 1.325 (11) |
Fe5—O402 | 2.040 (4) | C305—C306 | 1.345 (12) |
Fe5—O501 | 2.035 (3) | C306—C307 | 1.303 (19) |
O11—C11A | 1.442 (11) | C206—H206 | 0.9501 |
O11—C11B | 1.43 (2) | C307—C308 | 1.41 (2) |
O12—C12 | 1.432 (7) | C207—H207 | 0.9496 |
O21—C21A | 1.415 (11) | C308—C309 | 1.341 (16) |
O21—C21B | 1.47 (2) | C208—H208 | 0.9508 |
O22—C22 | 1.441 (9) | C209—H209 | 0.9488 |
O31—C31A | 1.304 (14) | C309—C310 | 1.446 (13) |
O31—C31B | 1.53 (4) | C210—H210 | 0.9498 |
O32—C32 | 1.411 (8) | C311—C312 | 1.428 (13) |
O41—C41A | 1.418 (11) | C311—C316 | 1.403 (14) |
O41—C41B | 1.42 (2) | C312—C313 | 1.408 (15) |
O42—C42 | 1.429 (9) | C212—H212 | 0.9489 |
O51—C51A | 1.467 (10) | C213—H213 | 0.9492 |
O51—C51B | 1.42 (2) | C313—C314 | 1.387 (16) |
O52—C52 | 1.410 (8) | C314—C315 | 1.370 (19) |
O101—C103 | 1.257 (7) | C214—H214 | 0.9501 |
O102—C103 | 1.262 (7) | C215—H215 | 0.9493 |
O201—C203 | 1.256 (7) | C315—C316 | 1.35 (2) |
O202—C203 | 1.259 (7) | C216—H216 | 0.9509 |
O301—C303 | 1.261 (7) | C403—C404 | 1.516 (10) |
O302—C303 | 1.264 (7) | C404—C405 | 1.504 (9) |
O401—C403 | 1.261 (8) | C404—C411 | 1.522 (13) |
O402—C403 | 1.260 (7) | C304—H304 | 1.0005 |
O501—C503 | 1.266 (7) | C405—C406 | 1.339 (11) |
O502—C503 | 1.260 (7) | C405—C410 | 1.399 (9) |
C103—C104 | 1.536 (10) | C406—C407 | 1.377 (11) |
C104—C105 | 1.540 (11) | C306—H306 | 0.9503 |
C104—C111 | 1.529 (10) | C307—H307 | 0.9506 |
C105—C106 | 1.399 (13) | C407—C408 | 1.433 (13) |
C105—C110 | 1.362 (16) | C408—C409 | 1.347 (15) |
C106—C107 | 1.416 (15) | C308—H308 | 0.9490 |
C107—C108 | 1.35 (2) | C309—H309 | 0.9495 |
C108—C109 | 1.341 (19) | C409—C410 | 1.325 (11) |
C109—C110 | 1.377 (14) | C310—H310 | 0.9502 |
C111—C112 | 1.361 (14) | C411—C416 | 1.24 (2) |
C111—C116 | 1.375 (11) | C411—C412 | 1.394 (19) |
C11A—H11C | 0.9800 | C412—C413 | 1.368 (19) |
C11A—H11A | 0.9796 | C312—H312 | 0.9522 |
C11A—H11B | 0.9795 | C413—C414 | 1.19 (3) |
C11B—H11D | 0.9807 | C313—H313 | 0.9500 |
C11B—H11E | 0.9801 | C414—C415 | 1.29 (3) |
C11B—H11F | 0.9800 | C314—H314 | 0.9512 |
C12—H12A | 0.9800 | C315—H315 | 0.9511 |
C112—C113 | 1.385 (14) | C415—C416 | 1.48 (3) |
C12—H12B | 0.9807 | C316—H316 | 0.9494 |
C12—H12C | 0.9797 | C503—C504 | 1.510 (8) |
C113—C114 | 1.370 (14) | C504—C505 | 1.486 (11) |
C114—C115 | 1.391 (16) | C504—C511 | 1.552 (11) |
C115—C116 | 1.369 (12) | C404—H404 | 0.9984 |
C21A—H21C | 0.9799 | C505—C510 | 1.377 (12) |
C21A—H21A | 0.9785 | C505—C506 | 1.366 (9) |
C21A—H21B | 0.9807 | C506—C507 | 1.364 (17) |
C21B—H21D | 0.9800 | C406—H406 | 0.9504 |
C21B—H21E | 0.9792 | C407—H407 | 0.9506 |
C21B—H21F | 0.9802 | C507—C508 | 1.34 (2) |
C22—H22C | 0.9797 | C408—H408 | 0.9501 |
C22—H22B | 0.9790 | C508—C509 | 1.403 (17) |
C22—H22A | 0.9800 | C409—H409 | 0.9507 |
C31A—H31A | 0.9802 | C509—C510 | 1.393 (15) |
C31A—H31B | 0.9803 | C410—H410 | 0.9501 |
C31A—H31C | 0.9810 | C511—C512 | 1.380 (16) |
C31B—H31D | 0.9754 | C511—C516 | 1.391 (11) |
C31B—H31F | 0.9815 | C412—H412 | 0.9503 |
C31B—H31E | 0.9757 | C512—C513 | 1.407 (19) |
C32—H32B | 0.9805 | C413—H413 | 0.9507 |
C32—H32A | 0.9806 | C513—C514 | 1.42 (2) |
C32—H32C | 0.9786 | C514—C515 | 1.34 (2) |
C41A—H41C | 0.9798 | C414—H414 | 0.9507 |
C41A—H41A | 0.9808 | C515—C516 | 1.398 (17) |
C41A—H41B | 0.9798 | C415—H415 | 0.9497 |
C41B—H41D | 0.9798 | C416—H416 | 0.9490 |
C41B—H41E | 0.9808 | C504—H504 | 0.9997 |
C41B—H41F | 0.9798 | C506—H506 | 0.9515 |
C42—H42B | 0.9799 | C507—H507 | 0.9505 |
C42—H42C | 0.9808 | C508—H508 | 0.9496 |
C42—H42A | 0.9789 | C509—H509 | 0.9498 |
C51A—H51C | 0.9801 | C510—H510 | 0.9495 |
C51A—H51B | 0.9787 | C512—H512 | 0.9483 |
C51A—H51A | 0.9795 | C513—H513 | 0.9502 |
C51B—H51E | 0.9809 | C514—H514 | 0.9506 |
C51B—H51D | 0.9790 | C515—H515 | 0.9497 |
C51B—H51F | 0.9810 | C516—H516 | 0.9505 |
C52—H52A | 0.9813 | | |
| | | |
Fe1···H41Ei | 3.4486 | H11F···C21B | 2.6495 |
Fe2···H31D | 3.4778 | H11F···Fe3 | 3.3785 |
Fe2···H51Fi | 3.2664 | H11F···O22 | 2.7608 |
Fe3···H11F | 3.3785 | H12B···H21B | 2.5394 |
Fe3···H41F | 3.4935 | H12B···O201 | 2.7424 |
Fe4···H51E | 3.4115 | H12C···O502i | 2.6240 |
Fe5···H31E | 3.5073 | H21A···H51Ai | 2.4572 |
O102···C116 | 3.327 (9) | H21B···C203 | 2.8652 |
O102···C110 | 3.105 (10) | H21B···O201 | 2.6948 |
O11···H51Fi | 2.4750 | H21B···H12B | 2.5394 |
O11···H41Ei | 2.8301 | H21C···H41A | 2.3832 |
O12···H51Fi | 2.9080 | H21C···O32 | 2.5713 |
O12···H21F | 2.9001 | H21C···C32 | 3.0241 |
O12···H51Ai | 2.6276 | H21C···H32B | 2.5494 |
O21···H11F | 2.7724 | H21D···C41B | 2.1354 |
O21···H31D | 2.7041 | H21D···H41F | 1.5526 |
O21···H51Fi | 2.8103 | H21D···H41D | 1.9828 |
O22···H31B | 2.7273 | H21E···H11E | 2.0504 |
O22···H11F | 2.7608 | H21E···C41B | 2.7005 |
O31···H21E | 2.8155 | H21E···O31 | 2.8155 |
O31···H41F | 2.6314 | H21E···C11B | 2.3369 |
O32···H41A | 2.5087 | H21E···C31B | 2.1329 |
O32···H21C | 2.5713 | H21E···H51Fi | 1.8814 |
O41···H31E | 2.6208 | H21E···H31E | 2.0950 |
O41···H51E | 2.5617 | H21E···H11F | 1.9461 |
O42···H31A | 2.5099 | H21E···H31D | 1.5782 |
O42···H51C | 2.7995 | H21E···H41F | 1.7501 |
O51···H11Ei | 2.7193 | H21E···C51Bi | 2.7479 |
O51···H41E | 2.8042 | H21F···H11E | 2.5667 |
O52···H41E | 2.8946 | H21F···C11B | 3.0139 |
O52···H11Ci | 2.5342 | H21F···O12 | 2.9001 |
O101···H107ii | 2.7763 | H21F···H51Ei | 2.5382 |
O101···H52Ai | 2.6571 | H21F···C51Bi | 1.8957 |
O201···C206 | 3.173 (15) | H21F···H51Di | 1.9213 |
O201···C216 | 3.161 (9) | H21F···H51Fi | 1.1977 |
O102···H110 | 2.4810 | H22A···O301 | 2.8979 |
O102···H11B | 2.8584 | H22A···H312 | 2.4604 |
O102···H22B | 2.5382 | H22B···H11B | 2.5953 |
O202···C206 | 3.418 (14) | H22B···O102 | 2.5382 |
O201···H21B | 2.6948 | H22B···C111 | 3.0380 |
O201···H206 | 2.5329 | H22B···C116 | 3.0752 |
O201···H12B | 2.7424 | H22C···H31B | 2.3590 |
O301···C312 | 3.127 (10) | H31A···C42 | 2.9194 |
O301···C310 | 2.926 (8) | H31A···C415v | 3.0500 |
O202···H32C | 2.7328 | H31A···O42 | 2.5099 |
O202···H32B | 2.7919 | H31A···H415v | 2.3555 |
O301···H22A | 2.8979 | H31A···H51C | 2.5224 |
O301···H310 | 2.4207 | H31B···O22 | 2.7273 |
O301···H312 | 2.6334 | H31B···H415v | 2.5595 |
O302···H42A | 2.6711 | H31B···C22 | 2.9728 |
O302···H315iii | 2.8968 | H31B···H22C | 2.3590 |
O402···C412 | 3.120 (11) | H31D···O21 | 2.7041 |
O402···C406 | 3.044 (8) | H31D···Fe2 | 3.4778 |
O401···H409iv | 2.6677 | H31D···H41F | 2.5227 |
O401···H32A | 2.5329 | H31D···C21B | 2.4095 |
O501···C510 | 3.103 (9) | H31D···H21E | 1.5782 |
O501···C516 | 3.112 (9) | H31E···H41E | 2.5379 |
O402···H41B | 2.8051 | H31E···Fe5 | 3.5073 |
O402···H412 | 2.8091 | H31E···O41 | 2.6208 |
O402···H52B | 2.7950 | H31E···C21B | 2.9009 |
O402···H406 | 2.3919 | H31E···C41B | 2.3548 |
O501···H42B | 2.7966 | H31E···H21E | 2.0950 |
O501···H51B | 2.7987 | H31E···H41F | 1.7404 |
O501···H510 | 2.4771 | H31F···H51D | 2.4253 |
O502···H51B | 2.8962 | H31F···C51B | 2.6827 |
O502···H12Ci | 2.6240 | H32A···O401 | 2.5329 |
C11A···C103 | 3.452 (11) | H32B···C113vi | 3.0166 |
C11B···C41Bi | 2.85 (3) | H32B···C114vi | 3.0125 |
C11B···C51Bi | 3.02 (3) | H32B···H21C | 2.5494 |
C11B···C21B | 2.95 (3) | H32B···H113vi | 2.5090 |
C21A···C203 | 3.372 (11) | H32B···H114vi | 2.5318 |
C21B···C41B | 2.83 (3) | H32B···O202 | 2.7919 |
C21B···C11B | 2.95 (3) | H32C···O202 | 2.7328 |
C21B···C31B | 2.93 (4) | H41A···O32 | 2.5087 |
C21B···C51Bi | 2.71 (3) | H41A···C32 | 3.0070 |
C31B···C41B | 3.10 (5) | H41A···H21C | 2.3832 |
C31B···C21B | 2.93 (4) | H41B···C403 | 2.9175 |
C41A···C403 | 3.449 (11) | H41B···O402 | 2.8051 |
C41B···C31B | 3.10 (5) | H41C···H11Ci | 2.4740 |
C41B···C21B | 2.83 (3) | H41D···C21B | 2.8930 |
C41B···C51B | 3.09 (3) | H41D···H21D | 1.9828 |
C41B···C11Bi | 2.85 (3) | H41E···H11Ei | 1.3509 |
C42···C516 | 3.579 (11) | H41E···C51B | 2.6567 |
C42···C315iii | 3.550 (14) | H41E···H31E | 2.5379 |
C51A···C503 | 3.391 (11) | H41E···O51 | 2.8042 |
C51B···C21Bi | 2.71 (3) | H41E···O52 | 2.8946 |
C51B···C11Bi | 3.02 (3) | H41E···H11Di | 1.8197 |
C51B···C41B | 3.09 (3) | H41E···Fe1i | 3.4486 |
C103···C11A | 3.452 (11) | H41E···H51E | 2.2597 |
C106···C106ii | 3.376 (11) | H41E···H51F | 2.5912 |
C110···C116 | 3.555 (14) | H41E···O11i | 2.8301 |
C110···O102 | 3.105 (10) | H41E···C11Bi | 1.9202 |
C11B···H21F | 3.0139 | H41F···O31 | 2.6314 |
C11B···H51Fi | 2.3353 | H41F···Fe3 | 3.4935 |
C11B···H41Ei | 1.9202 | H41F···H31D | 2.5227 |
C11B···H21E | 2.3369 | H41F···H31E | 1.7404 |
C116···C110 | 3.555 (14) | H41F···C21B | 2.0008 |
C116···O102 | 3.327 (9) | H41F···C31B | 2.3349 |
C21B···H11E | 2.6774 | H41F···C51B | 3.0032 |
C21B···H51Di | 2.8337 | H41F···H21D | 1.5526 |
C21B···H41F | 2.0008 | H41F···H21E | 1.7501 |
C21B···H41D | 2.8930 | H41F···H11Ei | 2.3769 |
C21B···H31E | 2.9009 | H41F···H51E | 2.1545 |
C21B···H51Fi | 1.8647 | H42A···O302 | 2.6711 |
C21B···H31D | 2.4095 | H42B···O501 | 2.7966 |
C21B···H11F | 2.6495 | H42B···C516 | 3.0958 |
C22···H312 | 2.9959 | H42C···H315iii | 2.5875 |
C22···H31B | 2.9728 | H42C···C315iii | 3.0243 |
C31A···H51C | 3.0597 | H51A···O12i | 2.6276 |
C31A···H415v | 2.8840 | H51A···H21Ai | 2.4572 |
C31B···H21E | 2.1329 | H51B···O501 | 2.7987 |
C31B···H41F | 2.3349 | H51B···O502 | 2.8962 |
C31B···H51D | 2.7859 | H51B···C503 | 2.7861 |
C31B···H11E | 3.0338 | H51C···C31A | 3.0597 |
C32···H41A | 3.0070 | H51C···H31A | 2.5224 |
C32···H21C | 3.0241 | H51C···O42 | 2.7995 |
C32···H409iv | 3.0519 | H51D···C21Bi | 2.8337 |
C32···H114vi | 3.0874 | H51D···H31F | 2.4253 |
C41B···H31E | 2.3548 | H51D···H21Fi | 1.9213 |
C41B···H11Di | 2.6538 | H51D···C31B | 2.7859 |
C41B···H21D | 2.1354 | H51E···Fe4 | 3.4115 |
C41B···H21E | 2.7005 | H51E···O41 | 2.5617 |
C41B···H11Ei | 2.2098 | H51E···C41B | 2.4107 |
C41B···H51E | 2.4107 | H51E···H41E | 2.2597 |
C42···H31A | 2.9194 | H51E···H41F | 2.1545 |
C42···H315iii | 3.0522 | H51E···H11Ei | 2.1989 |
C51B···H11Ei | 2.2220 | H51E···H21Fi | 2.5382 |
C51B···H41F | 3.0032 | H51F···H21Ei | 1.8814 |
C51B···H21Ei | 2.7479 | H51F···H21Fi | 1.1977 |
C51B···H21Fi | 1.8957 | H51F···O12i | 2.9080 |
C51B···H31F | 2.6827 | H51F···O21i | 2.8103 |
C51B···H41E | 2.6567 | H51F···C11Bi | 2.3353 |
C52···H11Ci | 2.9605 | H51F···C21Bi | 1.8647 |
C103···H110 | 2.6535 | H51F···H11Ei | 1.6781 |
C103···H11B | 2.9139 | H51F···H41E | 2.5912 |
C203···C21A | 3.372 (11) | H51F···Fe2i | 3.2664 |
C103···H112 | 3.0613 | H51F···O11i | 2.4750 |
C105···H116 | 2.5779 | H52A···O101i | 2.6571 |
C206···O202 | 3.418 (14) | H52B···O402 | 2.7950 |
C106···H213v | 2.9253 | H52C···H510 | 2.5623 |
C206···O201 | 3.173 (15) | H104···H106 | 2.3787 |
C209···C513vii | 3.597 (17) | H104···H112 | 2.4188 |
C110···H116 | 2.9277 | H106···C213v | 2.9585 |
C111···H22B | 3.0380 | H106···H104 | 2.3787 |
C113···H32Bv | 3.0166 | H106···H213v | 2.1789 |
C114···H32Bv | 3.0125 | H107···O101ii | 2.7763 |
C116···H22B | 3.0752 | H109···H216 | 2.5675 |
C216···O201 | 3.161 (9) | H110···O102 | 2.4810 |
C203···H21B | 2.8652 | H110···C103 | 2.6535 |
C203···H206 | 2.4168 | H112···H104 | 2.4188 |
C205···H216 | 2.7476 | H112···C103 | 3.0613 |
C306···C410iv | 3.588 (14) | H113···H32Bv | 2.5090 |
C306···C409iv | 3.447 (15) | H114···H32Bv | 2.5318 |
C307···C514iii | 3.55 (2) | H114···C32v | 3.0874 |
C207···H508viii | 2.9969 | H115···H507viii | 2.5597 |
C208···H508viii | 2.9920 | H116···C110 | 2.9277 |
C210···H309 | 3.0659 | H116···C105 | 2.5779 |
C310···C312 | 3.354 (14) | H204···H212 | 2.3393 |
C310···O301 | 2.926 (8) | H206···C203 | 2.4168 |
C312···C310 | 3.354 (14) | H206···O201 | 2.5329 |
C312···O301 | 3.127 (10) | H208···H508viii | 2.5792 |
C213···H106vi | 2.9585 | H208···C308ix | 2.9526 |
C214···H504vii | 3.0177 | H208···H308ix | 2.3352 |
C314···C408iii | 3.586 (19) | H212···H204 | 2.3393 |
C314···C407iii | 3.559 (17) | H213···C106vi | 2.9253 |
C215···H512vii | 3.0392 | H213···H106vi | 2.1789 |
C315···C42iii | 3.550 (14) | H216···C205 | 2.7476 |
C216···H512vii | 3.0557 | H216···H109 | 2.5675 |
C316···C316iii | 3.497 (17) | H304···H306 | 2.1444 |
C303···H310 | 2.8948 | H304···H316 | 2.3638 |
C303···H312 | 3.0342 | H306···H304 | 2.1444 |
C403···C41A | 3.449 (11) | H306···C410iv | 3.0603 |
C306···H514iii | 2.8239 | H307···C412iv | 2.9253 |
C406···C412 | 3.284 (13) | H307···C413iv | 3.0536 |
C406···O402 | 3.044 (8) | H307···H412iv | 2.5995 |
C407···C314iii | 3.559 (17) | H307···H509iv | 2.4019 |
C307···H514iii | 2.6718 | H308···H208ix | 2.3352 |
C308···H514iii | 2.9966 | H309···C210 | 3.0659 |
C408···C314iii | 3.586 (19) | H310···C312 | 2.9377 |
C308···H208ix | 2.9526 | H310···H312 | 2.2995 |
C409···C306iv | 3.447 (15) | H310···O301 | 2.4207 |
C310···H312 | 2.9325 | H310···C303 | 2.8948 |
C410···C306iv | 3.588 (14) | H312···H310 | 2.2995 |
C410···C410iv | 3.381 (11) | H312···C303 | 3.0342 |
C412···C406 | 3.284 (13) | H312···O301 | 2.6334 |
C412···O402 | 3.120 (11) | H312···C22 | 2.9959 |
C312···H310 | 2.9377 | H312···C310 | 2.9325 |
C313···H416v | 3.0293 | H312···H22A | 2.4604 |
C314···H416v | 2.7987 | H314···C408iii | 2.8235 |
C315···H42Ciii | 3.0243 | H314···C409iii | 3.0368 |
C316···H316iii | 2.8975 | H314···C407iii | 2.9328 |
C403···H406 | 2.6383 | H315···O302iii | 2.8968 |
C503···C51A | 3.391 (11) | H315···C42iii | 3.0522 |
C403···H41B | 2.9175 | H315···H42Ciii | 2.5875 |
C405···H412 | 2.7762 | H316···H304 | 2.3638 |
C406···H412 | 2.6698 | H316···C316iii | 2.8975 |
C506···C516 | 3.585 (13) | H316···H316iii | 2.5228 |
C407···H314iii | 2.9328 | H404···H410 | 2.3168 |
C408···H314iii | 2.8235 | H404···H416 | 2.2901 |
C409···H404iv | 3.0122 | H404···C409iv | 3.0122 |
C409···H314iii | 3.0368 | H406···O402 | 2.3919 |
C510···O501 | 3.103 (9) | H406···C403 | 2.6383 |
C410···H410iv | 3.0173 | H406···H412 | 2.4513 |
C410···H306iv | 3.0603 | H409···O401iv | 2.6677 |
C412···H307iv | 2.9253 | H409···C32iv | 3.0519 |
C513···C209x | 3.597 (17) | H410···H404 | 2.3168 |
C413···H307iv | 3.0536 | H410···C410iv | 3.0173 |
C514···C307iii | 3.55 (2) | H412···C406 | 2.6698 |
C415···H31Avi | 3.0500 | H412···O402 | 2.8091 |
C516···O501 | 3.112 (9) | H412···C405 | 2.7762 |
C516···C42 | 3.579 (11) | H412···H406 | 2.4513 |
C516···C506 | 3.585 (13) | H412···H307iv | 2.5995 |
C503···H51B | 2.7861 | H415···H31Avi | 2.3555 |
C503···H510 | 2.5018 | H415···C31Avi | 2.8840 |
C505···H516 | 2.6934 | H415···H31Bvi | 2.5595 |
C510···H516 | 3.0301 | H416···C314vi | 2.7987 |
C516···H42B | 3.0958 | H416···C313vi | 3.0293 |
H11B···C103 | 2.9139 | H416···H404 | 2.2901 |
H11B···O102 | 2.8584 | H504···H512 | 2.3777 |
H11B···H22B | 2.5953 | H504···C214x | 3.0177 |
H11C···H41Ci | 2.4740 | H504···H506 | 2.4579 |
H11C···O52i | 2.5342 | H506···H504 | 2.4579 |
H11C···C52i | 2.9605 | H507···H115xi | 2.5597 |
H11D···H41Ei | 1.8197 | H508···C207xi | 2.9969 |
H11D···C41Bi | 2.6538 | H508···C208xi | 2.9920 |
H11E···C21B | 2.6774 | H508···H208xi | 2.5792 |
H11E···C31B | 3.0338 | H509···H307iv | 2.4019 |
H11E···C51Bi | 2.2220 | H510···O501 | 2.4771 |
H11E···H41Ei | 1.3509 | H510···C503 | 2.5018 |
H11E···H41Fi | 2.3769 | H510···H52C | 2.5623 |
H11E···H51Ei | 2.1989 | H512···C215x | 3.0392 |
H11E···H51Fi | 1.6781 | H512···C216x | 3.0557 |
H11E···H21F | 2.5667 | H512···H504 | 2.3777 |
H11E···O51i | 2.7193 | H514···C306iii | 2.8239 |
H11E···C41Bi | 2.2098 | H514···C307iii | 2.6718 |
H11E···H21E | 2.0504 | H514···C308iii | 2.9966 |
H11F···H21E | 1.9461 | H516···C505 | 2.6934 |
H11F···O21 | 2.7724 | H516···C510 | 3.0301 |
| | | |
Fe5i—Fe1—Fe2 | 141.90 (4) | O42—C42—H42A | 109.51 |
Fe1—Fe2—Fe3 | 145.88 (4) | H51B—C51A—H51C | 109.47 |
Fe2—Fe3—Fe4 | 145.94 (4) | O51—C51A—H51C | 109.53 |
Fe3—Fe4—Fe5 | 142.30 (4) | O51—C51A—H51A | 109.49 |
Fe4—Fe5—Fe1i | 143.88 (4) | O51—C51A—H51B | 109.46 |
O11—Fe1—O12 | 78.01 (14) | H51A—C51A—H51B | 109.49 |
O11—Fe1—O101 | 89.32 (15) | H51A—C51A—H51C | 109.39 |
O11—Fe1—O51i | 96.48 (14) | O51—C51B—H51F | 109.46 |
O11—Fe1—O52i | 96.87 (14) | O51—C51B—H51E | 109.46 |
O11—Fe1—O502i | 170.87 (14) | H51E—C51B—H51F | 109.32 |
O12—Fe1—O101 | 91.58 (15) | H51D—C51B—H51E | 109.54 |
O12—Fe1—O51i | 95.88 (15) | H51D—C51B—H51F | 109.48 |
O12—Fe1—O52i | 171.74 (15) | O51—C51B—H51D | 109.57 |
O12—Fe1—O502i | 94.26 (14) | H52B—C52—H52C | 109.48 |
O51i—Fe1—O101 | 171.35 (15) | O52—C52—H52C | 109.53 |
O52i—Fe1—O101 | 94.86 (15) | O52—C52—H52B | 109.42 |
O101—Fe1—O502i | 86.00 (14) | O52—C52—H52A | 109.40 |
O51i—Fe1—O52i | 78.12 (15) | H52A—C52—H52B | 109.47 |
O51i—Fe1—O502i | 89.09 (14) | H52A—C52—H52C | 109.52 |
O52i—Fe1—O502i | 91.34 (14) | O202—C203—C204 | 116.7 (6) |
O11—Fe2—O12 | 78.25 (14) | O201—C203—O202 | 126.1 (6) |
O11—Fe2—O21 | 98.28 (14) | O201—C203—C204 | 117.2 (5) |
O11—Fe2—O22 | 97.47 (15) | C105—C104—H104 | 107.89 |
O11—Fe2—O102 | 89.56 (15) | C103—C104—H104 | 107.84 |
O11—Fe2—O201 | 169.01 (14) | C205—C204—C211 | 115.5 (6) |
O12—Fe2—O21 | 99.23 (15) | C203—C204—C211 | 111.0 (6) |
O12—Fe2—O22 | 174.23 (15) | C111—C104—H104 | 107.79 |
O12—Fe2—O102 | 90.25 (15) | C203—C204—C205 | 111.9 (7) |
O12—Fe2—O201 | 92.14 (15) | C204—C205—C210 | 122.7 (11) |
O21—Fe2—O22 | 77.41 (17) | C204—C205—C206 | 121.5 (9) |
O21—Fe2—O102 | 168.73 (14) | C206—C205—C210 | 115.4 (10) |
O21—Fe2—O201 | 88.44 (16) | C205—C206—C207 | 124.8 (12) |
O22—Fe2—O102 | 93.62 (17) | C105—C106—H106 | 120.38 |
O22—Fe2—O201 | 92.46 (16) | C107—C106—H106 | 120.23 |
O102—Fe2—O201 | 85.11 (17) | C206—C207—C208 | 110.9 (13) |
O21—Fe3—O22 | 77.29 (16) | C108—C107—H107 | 120.39 |
O21—Fe3—O31 | 97.75 (14) | C106—C107—H107 | 120.30 |
O21—Fe3—O32 | 98.93 (15) | C109—C108—H108 | 119.20 |
O21—Fe3—O202 | 88.94 (15) | C107—C108—H108 | 119.17 |
O21—Fe3—O301 | 169.35 (17) | C207—C208—C209 | 123.9 (15) |
O22—Fe3—O31 | 100.06 (18) | C108—C109—H109 | 120.20 |
O22—Fe3—O32 | 175.62 (15) | C110—C109—H109 | 120.12 |
O22—Fe3—O202 | 91.93 (18) | C208—C209—C210 | 120.6 (12) |
O22—Fe3—O301 | 93.33 (18) | C105—C110—H110 | 119.07 |
O31—Fe3—O32 | 78.15 (18) | C109—C110—H110 | 118.91 |
O31—Fe3—O202 | 167.29 (18) | C205—C210—C209 | 123.3 (12) |
O31—Fe3—O301 | 88.75 (15) | C204—C211—C212 | 120.1 (9) |
O32—Fe3—O202 | 90.18 (17) | C212—C211—C216 | 118.9 (10) |
O32—Fe3—O301 | 90.63 (17) | C204—C211—C216 | 120.8 (9) |
O202—Fe3—O301 | 86.34 (16) | C211—C212—C213 | 121.6 (12) |
O31—Fe4—O32 | 78.20 (16) | C111—C112—H112 | 120.51 |
O31—Fe4—O41 | 96.07 (15) | C113—C112—H112 | 120.68 |
O31—Fe4—O42 | 97.33 (16) | C114—C113—H113 | 119.18 |
O31—Fe4—O302 | 90.48 (17) | C212—C213—C214 | 117.9 (13) |
O31—Fe4—O401 | 170.93 (15) | C112—C113—H113 | 118.94 |
O32—Fe4—O41 | 96.79 (14) | C213—C214—C215 | 121.2 (13) |
O32—Fe4—O42 | 172.88 (14) | C113—C114—H114 | 120.39 |
O32—Fe4—O302 | 90.05 (15) | C115—C114—H114 | 120.33 |
O32—Fe4—O401 | 93.60 (16) | C214—C215—C216 | 119.5 (10) |
O41—Fe4—O42 | 78.05 (14) | C116—C115—H115 | 121.07 |
O41—Fe4—O302 | 171.36 (15) | C114—C115—H115 | 121.02 |
O41—Fe4—O401 | 88.68 (15) | C111—C116—H116 | 118.64 |
O42—Fe4—O302 | 95.56 (15) | C211—C216—C215 | 121.0 (10) |
O42—Fe4—O401 | 91.21 (15) | C115—C116—H116 | 118.60 |
O302—Fe4—O401 | 85.62 (17) | O301—C303—C304 | 117.5 (5) |
O41—Fe5—O42 | 77.83 (14) | O302—C303—C304 | 117.3 (5) |
O41—Fe5—O51 | 97.61 (14) | O301—C303—O302 | 125.2 (5) |
O41—Fe5—O52 | 98.82 (14) | C303—C304—C311 | 112.4 (6) |
O41—Fe5—O402 | 88.89 (15) | C305—C304—C311 | 114.0 (6) |
O41—Fe5—O501 | 169.64 (13) | C211—C204—H204 | 105.97 |
O42—Fe5—O51 | 96.89 (15) | C303—C304—C305 | 110.9 (5) |
O42—Fe5—O52 | 173.62 (15) | C203—C204—H204 | 105.80 |
O42—Fe5—O402 | 91.41 (15) | C205—C204—H204 | 105.88 |
O42—Fe5—O501 | 93.06 (14) | C304—C305—C306 | 117.0 (7) |
O51—Fe5—O52 | 78.06 (15) | C306—C305—C310 | 119.3 (8) |
O51—Fe5—O402 | 170.37 (15) | C304—C305—C310 | 123.6 (6) |
O51—Fe5—O501 | 88.29 (14) | C205—C206—H206 | 117.57 |
O52—Fe5—O402 | 93.97 (15) | C207—C206—H206 | 117.68 |
O52—Fe5—O501 | 90.71 (14) | C305—C306—C307 | 122.4 (11) |
O402—Fe5—O501 | 86.39 (14) | C206—C207—H207 | 124.48 |
Fe1—O11—Fe2 | 99.22 (15) | C306—C307—C308 | 120.0 (13) |
Fe1—O11—C11A | 121.0 (4) | C208—C207—H207 | 124.57 |
Fe1—O11—C11B | 127.3 (8) | C209—C208—H208 | 117.93 |
Fe2—O11—C11A | 124.3 (4) | C307—C308—C309 | 118.7 (12) |
Fe2—O11—C11B | 122.0 (8) | C207—C208—H208 | 118.15 |
Fe1—O12—Fe2 | 99.19 (16) | C210—C209—H209 | 119.69 |
Fe1—O12—C12 | 125.7 (3) | C208—C209—H209 | 119.76 |
Fe2—O12—C12 | 125.8 (3) | C308—C309—C310 | 117.2 (9) |
Fe2—O21—Fe3 | 99.47 (16) | C205—C210—H210 | 118.47 |
Fe2—O21—C21A | 121.7 (4) | C305—C310—C309 | 120.9 (8) |
Fe2—O21—C21B | 121.2 (9) | C209—C210—H210 | 118.24 |
Fe3—O21—C21A | 122.0 (4) | C312—C311—C316 | 111.8 (9) |
Fe3—O21—C21B | 124.0 (8) | C304—C311—C312 | 123.6 (7) |
Fe2—O22—Fe3 | 100.1 (2) | C304—C311—C316 | 123.0 (8) |
Fe2—O22—C22 | 126.7 (4) | C311—C312—C313 | 122.6 (8) |
Fe3—O22—C22 | 127.9 (4) | C211—C212—H212 | 119.30 |
Fe3—O31—Fe4 | 99.71 (19) | C213—C212—H212 | 119.12 |
Fe3—O31—C31A | 125.2 (6) | C312—C313—C314 | 119.3 (10) |
Fe3—O31—C31B | 122.8 (14) | C212—C213—H213 | 121.01 |
Fe4—O31—C31A | 125.0 (7) | C214—C213—H213 | 121.06 |
Fe4—O31—C31B | 124.7 (15) | C213—C214—H214 | 119.39 |
Fe3—O32—Fe4 | 98.88 (17) | C215—C214—H214 | 119.45 |
Fe3—O32—C32 | 124.7 (3) | C313—C314—C315 | 118.9 (12) |
Fe4—O32—C32 | 126.8 (3) | C216—C215—H215 | 120.37 |
Fe4—O41—Fe5 | 99.52 (15) | C214—C215—H215 | 120.18 |
Fe4—O41—C41A | 121.6 (4) | C314—C315—C316 | 120.3 (11) |
Fe4—O41—C41B | 125.4 (9) | C211—C216—H216 | 119.42 |
Fe5—O41—C41A | 124.1 (5) | C311—C316—C315 | 125.6 (11) |
Fe5—O41—C41B | 125.7 (9) | C215—C216—H216 | 119.59 |
Fe4—O42—Fe5 | 99.54 (16) | O401—C403—O402 | 125.9 (6) |
Fe4—O42—C42 | 127.3 (4) | O402—C403—C404 | 118.6 (6) |
Fe5—O42—C42 | 125.2 (4) | O401—C403—C404 | 115.4 (5) |
Fe5—O51—C51A | 122.2 (4) | C403—C404—C405 | 111.6 (6) |
Fe5—O51—C51B | 124.1 (8) | C303—C304—H304 | 106.32 |
Fe1i—O51—Fe5 | 99.88 (17) | C305—C304—H304 | 106.38 |
Fe1i—O51—C51A | 121.7 (4) | C311—C304—H304 | 106.27 |
Fe1i—O51—C51B | 121.4 (8) | C403—C404—C411 | 111.8 (6) |
Fe5—O52—C52 | 126.8 (4) | C405—C404—C411 | 109.9 (7) |
Fe1i—O52—Fe5 | 99.01 (17) | C404—C405—C406 | 123.2 (6) |
Fe1i—O52—C52 | 125.8 (4) | C406—C405—C410 | 118.9 (6) |
Fe1—O101—C103 | 127.1 (4) | C404—C405—C410 | 117.7 (6) |
Fe2—O102—C103 | 128.9 (4) | C307—C306—H306 | 118.84 |
Fe2—O201—C203 | 128.1 (4) | C305—C306—H306 | 118.74 |
Fe3—O202—C203 | 127.6 (4) | C405—C406—C407 | 121.3 (7) |
Fe3—O301—C303 | 128.8 (4) | C306—C307—H307 | 120.07 |
Fe4—O302—C303 | 127.2 (4) | C406—C407—C408 | 117.9 (9) |
Fe4—O401—C403 | 127.7 (4) | C308—C307—H307 | 119.93 |
Fe5—O402—C403 | 128.1 (4) | C407—C408—C409 | 119.4 (9) |
Fe5—O501—C503 | 129.0 (3) | C307—C308—H308 | 120.69 |
Fe1i—O502—C503 | 127.7 (3) | C309—C308—H308 | 120.65 |
O101—C103—O102 | 125.8 (6) | C408—C409—C410 | 120.8 (8) |
O101—C103—C104 | 117.8 (5) | C308—C309—H309 | 121.33 |
O102—C103—C104 | 116.4 (5) | C310—C309—H309 | 121.43 |
C103—C104—C105 | 112.1 (6) | C305—C310—H310 | 119.53 |
C103—C104—C111 | 107.5 (6) | C309—C310—H310 | 119.61 |
C105—C104—C111 | 113.5 (6) | C405—C410—C409 | 121.5 (7) |
C104—C105—C106 | 116.6 (8) | C404—C411—C412 | 123.8 (10) |
C104—C105—C110 | 125.6 (8) | C404—C411—C416 | 124.6 (12) |
C106—C105—C110 | 117.7 (8) | C412—C411—C416 | 107.1 (13) |
C105—C106—C107 | 119.4 (10) | C311—C312—H312 | 118.68 |
C106—C107—C108 | 119.3 (11) | C313—C312—H312 | 118.71 |
C107—C108—C109 | 121.6 (12) | C411—C412—C413 | 128.0 (14) |
C108—C109—C110 | 119.7 (13) | C412—C413—C414 | 117 (2) |
C105—C110—C109 | 122.0 (11) | C312—C313—H313 | 120.37 |
C104—C111—C112 | 117.7 (7) | C314—C313—H313 | 120.37 |
C104—C111—C116 | 123.0 (8) | C413—C414—C415 | 123 (2) |
C112—C111—C116 | 119.3 (8) | C313—C314—H314 | 120.62 |
O11—C11A—H11B | 109.35 | C315—C314—H314 | 120.47 |
O11—C11A—H11C | 109.40 | C314—C315—H315 | 119.92 |
H11A—C11A—H11B | 109.64 | C316—C315—H315 | 119.82 |
H11A—C11A—H11C | 109.46 | C414—C415—C416 | 117.6 (19) |
H11B—C11A—H11C | 109.53 | C411—C416—C415 | 124.6 (17) |
O11—C11A—H11A | 109.44 | C311—C316—H316 | 117.13 |
O11—C11B—H11D | 109.54 | C315—C316—H316 | 117.27 |
O11—C11B—H11E | 109.55 | O501—C503—O502 | 125.0 (5) |
H11E—C11B—H11F | 109.39 | O502—C503—C504 | 117.7 (5) |
H11D—C11B—H11E | 109.30 | O501—C503—C504 | 117.2 (5) |
H11D—C11B—H11F | 109.45 | C505—C504—C511 | 113.7 (5) |
O11—C11B—H11F | 109.60 | C503—C504—C511 | 109.5 (5) |
O12—C12—H12A | 109.39 | C503—C504—C505 | 112.3 (6) |
H12A—C12—H12B | 109.46 | C403—C404—H404 | 107.82 |
O12—C12—H12C | 109.46 | C411—C404—H404 | 107.76 |
C111—C112—C113 | 118.8 (9) | C405—C404—H404 | 107.75 |
O12—C12—H12B | 109.37 | C504—C505—C506 | 120.2 (8) |
H12B—C12—H12C | 109.50 | C504—C505—C510 | 124.2 (6) |
H12A—C12—H12C | 109.64 | C506—C505—C510 | 115.6 (8) |
C112—C113—C114 | 121.9 (10) | C405—C406—H406 | 119.30 |
C113—C114—C115 | 119.3 (10) | C407—C406—H406 | 119.38 |
C114—C115—C116 | 117.9 (8) | C505—C506—C507 | 123.7 (10) |
C111—C116—C115 | 122.8 (8) | C506—C507—C508 | 118.8 (12) |
O21—C21A—H21C | 109.46 | C408—C407—H407 | 121.03 |
H21B—C21A—H21C | 109.37 | C406—C407—H407 | 121.07 |
O21—C21A—H21A | 109.49 | C507—C508—C509 | 122.4 (13) |
O21—C21A—H21B | 109.42 | C407—C408—H408 | 120.34 |
H21A—C21A—H21B | 109.44 | C409—C408—H408 | 120.28 |
H21A—C21A—H21C | 109.65 | C508—C509—C510 | 115.3 (11) |
O21—C21B—H21F | 109.43 | C410—C409—H409 | 119.55 |
O21—C21B—H21D | 109.51 | C408—C409—H409 | 119.60 |
O21—C21B—H21E | 109.58 | C405—C410—H410 | 119.27 |
H21D—C21B—H21E | 109.43 | C505—C510—C509 | 124.2 (8) |
H21D—C21B—H21F | 109.43 | C409—C410—H410 | 119.23 |
H21E—C21B—H21F | 109.44 | C504—C511—C516 | 119.4 (8) |
O22—C22—H22A | 109.43 | C512—C511—C516 | 120.7 (9) |
H22A—C22—H22B | 109.47 | C504—C511—C512 | 119.9 (7) |
H22A—C22—H22C | 109.46 | C413—C412—H412 | 116.03 |
O22—C22—H22B | 109.54 | C411—C412—H412 | 115.93 |
H22B—C22—H22C | 109.48 | C511—C512—C513 | 120.6 (11) |
O22—C22—H22C | 109.45 | C512—C513—C514 | 116.9 (14) |
H31A—C31A—H31C | 109.61 | C412—C413—H413 | 121.28 |
O31—C31A—H31C | 109.37 | C414—C413—H413 | 121.25 |
H31A—C31A—H31B | 109.50 | C513—C514—C515 | 122.3 (15) |
O31—C31A—H31B | 109.42 | C413—C414—H414 | 118.78 |
H31B—C31A—H31C | 109.43 | C415—C414—H414 | 118.69 |
O31—C31A—H31A | 109.51 | C416—C415—H415 | 121.16 |
H31D—C31B—H31F | 109.62 | C514—C515—C516 | 120.6 (12) |
O31—C31B—H31D | 109.27 | C414—C415—H415 | 121.27 |
O31—C31B—H31E | 109.22 | C411—C416—H416 | 117.63 |
O31—C31B—H31F | 108.83 | C511—C516—C515 | 118.9 (10) |
H31D—C31B—H31E | 110.20 | C415—C416—H416 | 117.73 |
H31E—C31B—H31F | 109.68 | C505—C504—H504 | 107.02 |
H32B—C32—H32C | 109.52 | C503—C504—H504 | 107.01 |
O32—C32—H32A | 109.41 | C511—C504—H504 | 106.89 |
O32—C32—H32B | 109.45 | C507—C506—H506 | 118.12 |
H32A—C32—H32B | 109.39 | C505—C506—H506 | 118.22 |
H32A—C32—H32C | 109.57 | C508—C507—H507 | 120.60 |
O32—C32—H32C | 109.49 | C506—C507—H507 | 120.62 |
H41A—C41A—H41C | 109.38 | C507—C508—H508 | 118.86 |
H41B—C41A—H41C | 109.46 | C509—C508—H508 | 118.75 |
H41A—C41A—H41B | 109.43 | C508—C509—H509 | 122.38 |
O41—C41A—H41A | 109.52 | C510—C509—H509 | 122.37 |
O41—C41A—H41C | 109.55 | C509—C510—H510 | 117.86 |
O41—C41A—H41B | 109.48 | C505—C510—H510 | 117.89 |
H41D—C41B—H41F | 109.52 | C511—C512—H512 | 119.72 |
O41—C41B—H41D | 109.50 | C513—C512—H512 | 119.71 |
H41D—C41B—H41E | 109.44 | C514—C513—H513 | 121.56 |
H41E—C41B—H41F | 109.40 | C512—C513—H513 | 121.55 |
O41—C41B—H41E | 109.47 | C513—C514—H514 | 118.83 |
O41—C41B—H41F | 109.50 | C515—C514—H514 | 118.84 |
O42—C42—H42C | 109.42 | C516—C515—H515 | 119.71 |
O42—C42—H42B | 109.48 | C514—C515—H515 | 119.72 |
H42B—C42—H42C | 109.46 | C515—C516—H516 | 120.56 |
H42A—C42—H42B | 109.45 | C511—C516—H516 | 120.53 |
H42A—C42—H42C | 109.50 | | |
| | | |
O12—Fe1—O11—Fe2 | −17.52 (15) | O52—Fe5—O402—C403 | −138.2 (5) |
O12—Fe1—O11—C11A | −157.3 (5) | O501—Fe5—O402—C403 | 131.3 (5) |
O101—Fe1—O11—Fe2 | 74.24 (17) | O42—Fe5—O501—C503 | −133.7 (5) |
O101—Fe1—O11—C11A | −65.6 (5) | O51—Fe5—O501—C503 | −36.9 (5) |
O51i—Fe1—O11—Fe2 | −112.18 (16) | O52—Fe5—O501—C503 | 41.2 (5) |
O51i—Fe1—O11—C11A | 108.0 (5) | O402—Fe5—O501—C503 | 135.1 (5) |
O52i—Fe1—O11—Fe2 | 169.06 (16) | Fe2—O201—C203—C204 | −178.4 (5) |
O52i—Fe1—O11—C11A | 29.2 (5) | Fe2—O201—C203—O202 | 2.2 (10) |
O11—Fe1—O12—Fe2 | 17.42 (15) | Fe3—O202—C203—O201 | −3.9 (10) |
O11—Fe1—O12—C12 | 165.1 (4) | Fe3—O202—C203—C204 | 176.8 (5) |
O101—Fe1—O12—Fe2 | −71.56 (16) | Fe4—O401—C403—O402 | 0.6 (9) |
O101—Fe1—O12—C12 | 76.1 (4) | Fe4—O401—C403—C404 | −178.8 (4) |
O51i—Fe1—O12—Fe2 | 112.82 (15) | Fe5—O402—C403—C404 | 179.0 (4) |
O51i—Fe1—O12—C12 | −99.5 (4) | Fe5—O402—C403—O401 | −0.3 (9) |
O502i—Fe1—O12—Fe2 | −157.66 (15) | O101—C103—C104—H104 | −14.36 |
O502i—Fe1—O12—C12 | −10.0 (4) | O102—C103—C104—H104 | 166.13 |
O11—Fe1—O101—C103 | −38.5 (5) | O201—C203—C204—C211 | 45.3 (10) |
O12—Fe1—O101—C103 | 39.5 (5) | O202—C203—C204—C205 | 94.1 (8) |
O52i—Fe1—O101—C103 | −135.3 (5) | O201—C203—C204—C205 | −85.3 (8) |
O502i—Fe1—O101—C103 | 133.7 (5) | O202—C203—C204—C211 | −135.2 (7) |
O11—Fe1—O51i—Fe5i | −112.64 (15) | H104—C104—C105—C106 | −34.09 |
O11—Fe1—O51i—C51Ai | 109.3 (4) | H104—C104—C105—C110 | 143.00 |
O12—Fe1—O51i—Fe5i | 168.81 (14) | C203—C204—C205—C206 | 8.5 (12) |
O12—Fe1—O51i—C51Ai | 30.8 (4) | C203—C204—C205—C210 | −164.0 (7) |
O11—Fe1—O52i—Fe5i | 111.94 (15) | C211—C204—C205—C206 | −119.8 (11) |
O11—Fe1—O52i—C52i | −98.5 (5) | C211—C204—C205—C210 | 67.7 (11) |
O101—Fe1—O52i—Fe5i | −158.16 (15) | C203—C204—C211—C212 | 87.0 (12) |
O101—Fe1—O52i—C52i | −8.6 (5) | C203—C204—C211—C216 | −87.4 (9) |
O12—Fe1—O502i—C503i | −131.9 (5) | C205—C204—C211—C212 | −144.3 (10) |
O101—Fe1—O502i—C503i | 136.8 (5) | C205—C204—C211—C216 | 41.3 (12) |
O12—Fe2—O11—Fe1 | 17.45 (15) | H104—C104—C111—C116 | 141.45 |
O12—Fe2—O11—C11A | 155.4 (5) | H104—C104—C111—C112 | −40.43 |
O21—Fe2—O11—Fe1 | 115.23 (16) | C210—C205—C206—C207 | 4.1 (18) |
O21—Fe2—O11—C11A | −106.8 (5) | C204—C205—C206—C207 | −168.9 (12) |
O22—Fe2—O11—Fe1 | −166.49 (18) | C104—C105—C106—H106 | 2.61 |
O22—Fe2—O11—C11A | −28.5 (5) | C204—C205—C210—C209 | 176.3 (8) |
O102—Fe2—O11—Fe1 | −72.90 (16) | C206—C205—C210—C209 | 3.3 (14) |
O102—Fe2—O11—C11A | 65.1 (5) | C106—C105—C110—H110 | 175.19 |
O11—Fe2—O12—Fe1 | −17.55 (15) | C110—C105—C106—H106 | −174.72 |
O11—Fe2—O12—C12 | −165.2 (5) | C104—C105—C110—H110 | −1.88 |
O21—Fe2—O12—Fe1 | −114.17 (16) | C205—C206—C207—C208 | −11 (2) |
O21—Fe2—O12—C12 | 98.2 (5) | C105—C106—C107—H107 | 175.59 |
O102—Fe2—O12—Fe1 | 71.95 (16) | H106—C106—C107—C108 | 175.58 |
O102—Fe2—O12—C12 | −75.7 (5) | H106—C106—C107—H107 | −4.51 |
O201—Fe2—O12—Fe1 | 157.07 (18) | C106—C107—C108—H108 | −176.97 |
O201—Fe2—O12—C12 | 9.4 (5) | H107—C107—C108—C109 | −176.86 |
O11—Fe2—O21—Fe3 | 113.83 (15) | H107—C107—C108—H108 | 3.12 |
O11—Fe2—O21—C21A | −108.9 (5) | C206—C207—C208—C209 | 12 (2) |
O12—Fe2—O21—Fe3 | −166.82 (15) | C107—C108—C109—H109 | 177.56 |
O12—Fe2—O21—C21A | −29.5 (5) | H108—C108—C109—H109 | −2.42 |
O22—Fe2—O21—Fe3 | 17.97 (16) | H108—C108—C109—C110 | 177.35 |
O22—Fe2—O21—C21A | 155.3 (5) | C207—C208—C209—C210 | −6 (2) |
O201—Fe2—O21—Fe3 | −74.90 (17) | C108—C109—C110—H110 | −176.43 |
O201—Fe2—O21—C21A | 62.4 (5) | C208—C209—C210—C205 | −2.8 (17) |
O11—Fe2—O22—Fe3 | −115.08 (17) | H109—C109—C110—H110 | 3.34 |
O11—Fe2—O22—C22 | 89.2 (5) | H109—C109—C110—C105 | −176.55 |
O21—Fe2—O22—Fe3 | −18.22 (15) | C104—C111—C116—H116 | −3.72 |
O21—Fe2—O22—C22 | −173.9 (5) | C116—C111—C112—H112 | −178.44 |
O102—Fe2—O22—Fe3 | 154.89 (16) | C104—C111—C112—H112 | 3.37 |
O102—Fe2—O22—C22 | −0.8 (5) | C112—C111—C116—H116 | 178.19 |
O201—Fe2—O22—Fe3 | 69.63 (19) | C212—C211—C216—C215 | 0.3 (14) |
O201—Fe2—O22—C22 | −86.1 (5) | C204—C211—C216—C215 | 174.8 (8) |
O11—Fe2—O102—C103 | 35.7 (5) | C204—C211—C212—C213 | −174.7 (11) |
O12—Fe2—O102—C103 | −42.6 (5) | C216—C211—C212—C213 | −0.2 (19) |
O22—Fe2—O102—C103 | 133.1 (5) | H112—C112—C113—C114 | −179.69 |
O201—Fe2—O102—C103 | −134.7 (5) | C111—C112—C113—H113 | −179.56 |
O12—Fe2—O201—C203 | 138.7 (6) | H112—C112—C113—H113 | 0.36 |
O21—Fe2—O201—C203 | 39.5 (6) | C211—C212—C213—C214 | 0 (2) |
O22—Fe2—O201—C203 | −37.8 (6) | H113—C113—C114—C115 | 177.86 |
O102—Fe2—O201—C203 | −131.2 (6) | H113—C113—C114—H114 | −2.04 |
O22—Fe3—O21—Fe2 | −18.07 (16) | C112—C113—C114—H114 | 178.01 |
O22—Fe3—O21—C21A | −155.2 (5) | C212—C213—C214—C215 | 0 (2) |
O31—Fe3—O21—Fe2 | −116.70 (19) | H114—C114—C115—H115 | 1.68 |
O31—Fe3—O21—C21A | 106.2 (5) | C113—C114—C115—H115 | −178.22 |
O32—Fe3—O21—Fe2 | 164.17 (15) | H114—C114—C115—C116 | −178.25 |
O32—Fe3—O21—C21A | 27.1 (5) | C213—C214—C215—C216 | 0.0 (19) |
O202—Fe3—O21—Fe2 | 74.15 (19) | C214—C215—C216—C211 | −0.2 (15) |
O202—Fe3—O21—C21A | −62.9 (5) | H115—C115—C116—H116 | 0.18 |
O21—Fe3—O22—Fe2 | 18.08 (15) | C114—C115—C116—H116 | −179.89 |
O21—Fe3—O22—C22 | 173.4 (6) | H115—C115—C116—C111 | −179.92 |
O31—Fe3—O22—Fe2 | 113.84 (17) | O402—C403—C404—C405 | 76.4 (7) |
O31—Fe3—O22—C22 | −90.9 (6) | O402—C403—C404—C411 | −47.2 (9) |
O202—Fe3—O22—Fe2 | −70.39 (17) | O302—C303—C304—H304 | −5.42 |
O202—Fe3—O22—C22 | 84.9 (6) | O301—C303—C304—H304 | 175.32 |
O301—Fe3—O22—Fe2 | −156.83 (17) | O401—C403—C404—C405 | −104.2 (7) |
O301—Fe3—O22—C22 | −1.6 (6) | O401—C403—C404—C411 | 132.3 (8) |
O21—Fe3—O31—Fe4 | −114.70 (17) | C411—C404—C405—C406 | 85.9 (10) |
O21—Fe3—O31—C31A | 98.9 (10) | C403—C404—C411—C416 | −130.2 (13) |
O22—Fe3—O31—Fe4 | 166.92 (16) | C411—C404—C405—C410 | −88.6 (9) |
O22—Fe3—O31—C31A | 20.5 (11) | C403—C404—C411—C412 | 76.8 (11) |
O32—Fe3—O31—Fe4 | −17.15 (16) | C403—C404—C405—C410 | 146.7 (7) |
O32—Fe3—O31—C31A | −163.6 (11) | C403—C404—C405—C406 | −38.8 (10) |
O301—Fe3—O31—Fe4 | 73.8 (2) | H304—C304—C305—C306 | 11.57 |
O301—Fe3—O31—C31A | −72.7 (11) | H304—C304—C305—C310 | −171.70 |
O21—Fe3—O32—Fe4 | 113.10 (15) | H304—C304—C311—C312 | 177.12 |
O21—Fe3—O32—C32 | −99.1 (4) | H304—C304—C311—C316 | −18.55 |
O31—Fe3—O32—Fe4 | 16.98 (14) | C405—C404—C411—C412 | −47.7 (11) |
O31—Fe3—O32—C32 | 164.8 (5) | C405—C404—C411—C416 | 105.3 (14) |
O202—Fe3—O32—Fe4 | −157.95 (16) | C404—C405—C406—C407 | −174.7 (8) |
O202—Fe3—O32—C32 | −10.2 (5) | C410—C405—C406—C407 | −0.3 (13) |
O301—Fe3—O32—Fe4 | −71.61 (16) | C404—C405—C410—C409 | 176.4 (8) |
O301—Fe3—O32—C32 | 76.2 (5) | C406—C405—C410—C409 | 1.6 (12) |
O21—Fe3—O202—C203 | −36.4 (6) | C310—C305—C306—H306 | −179.63 |
O22—Fe3—O202—C203 | 40.8 (6) | C304—C305—C310—H310 | −1.28 |
O32—Fe3—O202—C203 | −135.4 (6) | C304—C305—C306—H306 | −2.74 |
O301—Fe3—O202—C203 | 134.0 (6) | C306—C305—C310—H310 | 175.38 |
O22—Fe3—O301—C303 | −146.3 (5) | C405—C406—C407—C408 | −2.3 (15) |
O31—Fe3—O301—C303 | −46.3 (6) | H306—C306—C307—H307 | 9.48 |
O32—Fe3—O301—C303 | 31.8 (5) | C305—C306—C307—H307 | −170.56 |
O202—Fe3—O301—C303 | 122.0 (6) | H306—C306—C307—C308 | −170.47 |
O32—Fe4—O31—Fe3 | 17.14 (16) | C406—C407—C408—C409 | 3.7 (16) |
O32—Fe4—O31—C31A | 163.6 (10) | H307—C307—C308—H308 | −15.12 |
O41—Fe4—O31—Fe3 | 112.83 (16) | H307—C307—C308—C309 | 164.80 |
O41—Fe4—O31—C31A | −100.7 (10) | C306—C307—C308—H308 | 164.83 |
O42—Fe4—O31—Fe3 | −168.49 (16) | H308—C308—C309—H309 | 10.89 |
O42—Fe4—O31—C31A | −22.0 (10) | C307—C308—C309—H309 | −169.03 |
O302—Fe4—O31—Fe3 | −72.82 (18) | H308—C308—C309—C310 | −169.21 |
O302—Fe4—O31—C31A | 73.7 (10) | C407—C408—C409—C410 | −2.5 (17) |
O31—Fe4—O32—Fe3 | −17.00 (15) | H309—C309—C310—C305 | 178.53 |
O31—Fe4—O32—C32 | −163.8 (5) | H309—C309—C310—H310 | −1.44 |
O41—Fe4—O32—Fe3 | −111.82 (16) | C308—C309—C310—H310 | 178.66 |
O41—Fe4—O32—C32 | 101.4 (5) | C408—C409—C410—C405 | −0.2 (14) |
O302—Fe4—O32—Fe3 | 73.47 (18) | C304—C311—C312—H312 | −2.28 |
O302—Fe4—O32—C32 | −73.3 (5) | C404—C411—C412—C413 | 176.0 (12) |
O401—Fe4—O32—Fe3 | 159.09 (16) | C416—C411—C412—C413 | 19.0 (18) |
O401—Fe4—O32—C32 | 12.3 (5) | C404—C411—C416—C415 | −173.5 (15) |
O31—Fe4—O41—Fe5 | 113.35 (17) | C412—C411—C416—C415 | −17 (2) |
O31—Fe4—O41—C41A | −106.3 (5) | C316—C311—C312—H312 | −168.16 |
O32—Fe4—O41—Fe5 | −167.86 (16) | C304—C311—C316—H316 | 0.87 |
O32—Fe4—O41—C41A | −27.5 (5) | C312—C311—C316—H316 | 166.83 |
O42—Fe4—O41—Fe5 | 17.12 (15) | C311—C312—C313—H313 | 177.05 |
O42—Fe4—O41—C41A | 157.5 (5) | H312—C312—C313—C314 | 177.18 |
O401—Fe4—O41—Fe5 | −74.40 (17) | H312—C312—C313—H313 | −2.96 |
O401—Fe4—O41—C41A | 66.0 (5) | C411—C412—C413—C414 | −12 (2) |
O31—Fe4—O42—Fe5 | −111.68 (16) | H313—C313—C314—C315 | 173.69 |
O31—Fe4—O42—C42 | 98.8 (5) | H313—C313—C314—H314 | −6.39 |
O41—Fe4—O42—Fe5 | −16.99 (15) | C312—C313—C314—H314 | 173.48 |
O41—Fe4—O42—C42 | −166.5 (5) | C412—C413—C414—C415 | 1 (3) |
O302—Fe4—O42—Fe5 | 157.11 (17) | H314—C314—C315—H315 | 5.79 |
O302—Fe4—O42—C42 | 7.6 (5) | C413—C414—C415—C416 | 0 (3) |
O401—Fe4—O42—Fe5 | 71.40 (17) | C313—C314—C315—H315 | −174.28 |
O401—Fe4—O42—C42 | −78.1 (5) | H314—C314—C315—C316 | −174.38 |
O31—Fe4—O302—C303 | 41.1 (6) | C314—C315—C316—H316 | −174.99 |
O32—Fe4—O302—C303 | −37.1 (6) | H315—C315—C316—C311 | −175.02 |
O42—Fe4—O302—C303 | 138.5 (5) | H315—C315—C316—H316 | 4.85 |
O401—Fe4—O302—C303 | −130.7 (6) | C414—C415—C416—C411 | 10 (3) |
O32—Fe4—O401—C403 | 135.5 (5) | O501—C503—C504—H504 | −163.62 |
O41—Fe4—O401—C403 | 38.8 (5) | O502—C503—C504—H504 | 17.04 |
O42—Fe4—O401—C403 | −39.2 (5) | H504—C504—C505—C506 | 45.24 |
O302—Fe4—O401—C403 | −134.7 (5) | H504—C504—C505—C510 | −133.39 |
O42—Fe5—O41—Fe4 | −16.96 (15) | H504—C504—C511—C512 | 25.62 |
O42—Fe5—O41—C41A | −156.0 (5) | H504—C504—C511—C516 | −158.02 |
O51—Fe5—O41—Fe4 | −112.42 (16) | C504—C505—C506—H506 | −1.73 |
O51—Fe5—O41—C41A | 108.6 (5) | C510—C505—C506—H506 | 177.00 |
O52—Fe5—O41—Fe4 | 168.56 (16) | C504—C505—C510—H510 | −0.18 |
O52—Fe5—O41—C41A | 29.5 (5) | C506—C505—C510—H510 | −178.86 |
O402—Fe5—O41—Fe4 | 74.72 (16) | C505—C506—C507—H507 | −176.37 |
O402—Fe5—O41—C41A | −64.3 (5) | H506—C506—C507—C508 | −176.46 |
O41—Fe5—O42—Fe4 | 17.09 (15) | H506—C506—C507—H507 | 3.67 |
O41—Fe5—O42—C42 | 167.5 (5) | C506—C507—C508—H508 | 177.80 |
O51—Fe5—O42—Fe4 | 113.43 (15) | H507—C507—C508—C509 | 177.72 |
O51—Fe5—O42—C42 | −96.1 (5) | H507—C507—C508—H508 | −2.33 |
O402—Fe5—O42—Fe4 | −71.47 (16) | C507—C508—C509—H509 | −179.66 |
O402—Fe5—O42—C42 | 79.0 (5) | H508—C508—C509—C510 | −179.45 |
O501—Fe5—O42—Fe4 | −157.92 (15) | H508—C508—C509—H509 | 0.39 |
O501—Fe5—O42—C42 | −7.5 (5) | C508—C509—C510—H510 | −179.97 |
O41—Fe5—O51—C51A | 108.0 (5) | H509—C509—C510—C505 | −179.86 |
O41—Fe5—O51—Fe1i | −114.33 (15) | H509—C509—C510—H510 | 0.18 |
O42—Fe5—O51—C51A | 29.4 (5) | C504—C511—C512—H512 | −4.58 |
O42—Fe5—O51—Fe1i | 167.10 (14) | C516—C511—C512—H512 | 179.11 |
O52—Fe5—O51—C51A | −154.6 (5) | C504—C511—C516—H516 | 2.16 |
O52—Fe5—O51—Fe1i | −16.87 (14) | C512—C511—C516—H516 | 178.49 |
O501—Fe5—O51—C51A | −63.5 (5) | C511—C512—C513—H513 | −177.54 |
O501—Fe5—O51—Fe1i | 74.22 (15) | H512—C512—C513—C514 | −177.52 |
O41—Fe5—O52—C52 | −98.1 (5) | H512—C512—C513—H513 | 2.49 |
O41—Fe5—O52—Fe1i | 112.77 (15) | C512—C513—C514—H514 | 178.11 |
O51—Fe5—O52—C52 | 165.9 (5) | H513—C513—C514—C515 | 178.08 |
O51—Fe5—O52—Fe1i | 16.79 (14) | H513—C513—C514—H514 | −1.90 |
O402—Fe5—O52—C52 | −8.6 (5) | C513—C514—C515—H515 | 179.60 |
O402—Fe5—O52—Fe1i | −157.75 (15) | H514—C514—C515—C516 | 179.70 |
O501—Fe5—O52—C52 | 77.8 (5) | H514—C514—C515—H515 | −0.42 |
O501—Fe5—O52—Fe1i | −71.32 (15) | C514—C515—C516—H516 | −177.92 |
O41—Fe5—O402—C403 | −39.5 (5) | H515—C515—C516—C511 | −177.93 |
O42—Fe5—O402—C403 | 38.3 (5) | H515—C515—C516—H516 | 2.20 |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x, −y+1, −z+2; (iii) −x+1, −y, −z+1; (iv) −x+2, −y, −z+1; (v) x−1, y, z; (vi) x+1, y, z; (vii) x, y+1, z; (viii) x−1, y+1, z; (ix) −x+1, −y+1, −z+1; (x) x, y−1, z; (xi) x+1, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C11A—H11C···O52i | 0.98 | 2.53 | 3.156 (8) | 121 |
C21A—H21C···O32 | 0.98 | 2.57 | 3.219 (10) | 124 |
C22—H22B···O102 | 0.98 | 2.54 | 3.083 (8) | 115 |
C31A—H31A···O42 | 0.98 | 2.51 | 3.150 (14) | 123 |
C32—H32A···O401 | 0.98 | 2.53 | 3.120 (7) | 118 |
C41A—H41A···O32 | 0.98 | 2.51 | 3.143 (11) | 122 |
C110—H110···O102 | 0.95 | 2.48 | 3.105 (10) | 123 |
C206—H206···O201 | 0.95 | 2.53 | 3.173 (15) | 125 |
C310—H310···O301 | 0.95 | 2.42 | 2.926 (8) | 113 |
C406—H406···O402 | 0.95 | 2.39 | 3.044 (8) | 126 |
C510—H510···O501 | 0.95 | 2.48 | 3.103 (9) | 124 |
Symmetry code: (i) −x+1, −y, −z+2. |
Experimental details
Crystal data |
Chemical formula | [Fe10(C14H11O2)10(CH3O)20] |
Mr | 3291.47 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 150 |
a, b, c (Å) | 12.4268 (12), 18.8782 (16), 19.5576 (16) |
α, β, γ (°) | 82.98 (1), 77.686 (10), 82.656 (10) |
V (Å3) | 4424.4 (7) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.86 |
Crystal size (mm) | 0.20 × 0.15 × 0.10 |
|
Data collection |
Diffractometer | Nonius KappaCCD area-detector diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 91822, 16169, 8452 |
Rint | 0.119 |
(sin θ/λ)max (Å−1) | 0.604 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.078, 0.173, 1.11 |
No. of reflections | 16169 |
No. of parameters | 977 |
No. of restraints | 960 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.79, −0.52 |
Selected geometric parameters (Å, º) topFe1—Fe2 | 3.0170 (11) | Fe4—Fe5 | 3.0172 (11) |
Fe2—Fe3 | 3.0175 (12) | Fe5—Fe1i | 3.0161 (11) |
Fe3—Fe4 | 3.0196 (12) | | |
| | | |
Fe5i—Fe1—Fe2 | 141.90 (4) | Fe3—Fe4—Fe5 | 142.30 (4) |
Fe1—Fe2—Fe3 | 145.88 (4) | Fe4—Fe5—Fe1i | 143.88 (4) |
Fe2—Fe3—Fe4 | 145.94 (4) | | |
Symmetry code: (i) −x+1, −y, −z+2. |
The title compound, (I), was obtained as a side product in the study of the coordination behaviour of a tridentate nitrogen-containing organic ligand in the presence of various carboxylates (Mimmi et al., 2002)
The decairon complex presented here is a so-called `ferric wheel', a circular array containing ten segments (see Fig. 1). Each segment consists of an iron cation, connected to the next Fe cation by a triple link formed by two methoxo anions and one carboxylate anion. The moiety formula of the wheel is therefore [FeIII(carboxylate)(methoxo)2]10. The wheel is located on the crystallographic inversion centre with coordinates (1/2,0,0). The FeO6 chromophores display a distorted octahedral coordination sphere, with deviations from ideal angles up to 12°. All Fe cations lie in one plane [maximum deviation of the least-squares plane through the ten Fe ions is 0.030 (1) Å]. Similar structures have been reported with other carboxylate anions: chloroacetate (Taft et al., 1994), acetate (Benelli, 1996) and 3-(4-methylbenzoyl)proprionate (Frey et al., 2000). In all these structures, the triple link between pairs of adjacent iron cations is formed by one carboxylate anion and two methoxo anions. The Fe···Fe distances and Fe···Fe···Fe angles in (I) lie in the same ranges as found for the previously reported ferric-wheel structures.
The methoxo ions pointing inward (i.e. to the `axle' of the wheel) are disordered over two positions, which can be characterized as axial or equatorial with respect to the Fe10 plane. In both orientations, the angle between the vector O—Me and the plane Fe—O—F–e is equal, however. An all-equatorial conformation is not possible due to the occurrence of collisions between the methyl moieties. The phenyl moieties display high anistropicity in their atomic displacement parameters, indicative of slight disorder (see Fig. 1). Attempts to refine two-site disorder models to describe this disorder gave unsatisfactory results. The crystal structure contains two separate areas filled with disordered solvent molecules, each located on a crystallographic inversion centre. The nature of the solvent could not be established unambiguously (see Experimental).