Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270106042508/ln3017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270106042508/ln3017Isup2.hkl |
CCDC reference: 632925
A mixture of Na2WO4·2H2O (4 mmol), 2,2'-bipyridine (2 mmol) and FeCl3·6H2O (1 mmol) was fully disolved in water (20 ml) by stirring at room temperature in a molar ratio of 4:2:1:1111. The mixture was adjsted to pH 3.4 with HCl solution (1:1). The solution was then sealed in a 30 ml Teflon-lined autoclave and heated to 458 K for 4 d. The autoclave was then cooled to room temperature over a period of 2 d at a rate of 10 K h−1, and black block crystals of (I) were obtained. Spectroscopic analysis: IR (KBr disk, ν, cm−1): 1625, 1603, 1466, 1443, 1314, 1292, 1218, 1156, 953, 868, 783, 759, 723, 559, 446.
In the unrestrained refinement, the C8—C9 and C9—C10 bond distances were not normal, the ratios of the maximum and minimum atomic displacement parameters for atoms C2, C12, C23 and C48 were larger than 5, and the Ueq values of atoms O1W and O4W were larger than 0.1. Therefore, the C8—C9 and C9—C10 bond distances were restrained to 1.35 (1) Å, pseudo-isotropic restraints were applied to atoms C2, C12, C23 and C48, and the atomic displacement ellipsoids of atoms W5, Na1, O5, O1W and O4W were restrained to be similar. H atoms bound to C atoms were placed in idealized positions and allowed to ride on their parent atoms, with C—H = 0.93 Å and with Uiso(H) = 1.2Ueq(C). The H atoms associated with the water molecules could not be located reliably and were omitted from the model. One water molecule appears to be disordered across two sites (O5W/O7W); these atoms were assigned fixed site-occupation factors of 0.5.
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.
[Fe(C10H8N2)3]2[NaFeW12O40(H2O)4]·2H2O | Z = 2 |
Mr = 4081.78 | F(000) = 3694 |
Triclinic, P1 | Dx = 3.161 Mg m−3 |
a = 13.7572 (10) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 17.8992 (13) Å | Cell parameters from 250 reflections |
c = 18.8730 (14) Å | θ = 2.5–25° |
α = 88.043 (1)° | µ = 16.62 mm−1 |
β = 72.829 (1)° | T = 293 K |
γ = 75.128 (1)° | Block, black |
V = 4287.1 (5) Å3 | 0.11 × 0.11 × 0.09 mm |
Bruker SMART CCD area-detector diffractometer | 14845 independent reflections |
Radiation source: fine-focus sealed tube | 10640 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
ϕ and ω scans | θmax = 25.0°, θmin = 2.2° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −16→16 |
Tmin = 0.262, Tmax = 0.316 | k = −20→21 |
22240 measured reflections | l = −22→18 |
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0345P)2] where P = (Fo2 + 2Fc2)/3 |
14845 reflections | (Δ/σ)max = 0.001 |
1216 parameters | Δρmax = 1.89 e Å−3 |
50 restraints | Δρmin = −1.87 e Å−3 |
[Fe(C10H8N2)3]2[NaFeW12O40(H2O)4]·2H2O | γ = 75.128 (1)° |
Mr = 4081.78 | V = 4287.1 (5) Å3 |
Triclinic, P1 | Z = 2 |
a = 13.7572 (10) Å | Mo Kα radiation |
b = 17.8992 (13) Å | µ = 16.62 mm−1 |
c = 18.8730 (14) Å | T = 293 K |
α = 88.043 (1)° | 0.11 × 0.11 × 0.09 mm |
β = 72.829 (1)° |
Bruker SMART CCD area-detector diffractometer | 14845 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 10640 reflections with I > 2σ(I) |
Tmin = 0.262, Tmax = 0.316 | Rint = 0.036 |
22240 measured reflections |
R[F2 > 2σ(F2)] = 0.044 | 50 restraints |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 0.98 | Δρmax = 1.89 e Å−3 |
14845 reflections | Δρmin = −1.87 e Å−3 |
1216 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 | 0.63925 (13) | 0.78794 (9) | 0.23428 (10) | 0.0191 (4) | |
Fe2 | 0.71046 (14) | 0.55616 (10) | 0.76161 (11) | 0.0256 (5) | |
Fe3 | 0.88643 (13) | 0.17558 (10) | 0.32532 (11) | 0.0272 (5) | |
W1 | 0.51708 (4) | 0.91392 (3) | 0.12169 (3) | 0.02595 (14) | |
W2 | 0.67390 (4) | 0.74501 (3) | 0.04708 (3) | 0.02271 (13) | |
W3 | 0.44195 (4) | 0.75229 (3) | 0.16640 (3) | 0.02609 (14) | |
W4 | 0.89022 (4) | 0.77743 (3) | 0.11342 (3) | 0.02336 (13) | |
W5 | 0.73781 (4) | 0.95038 (3) | 0.17913 (3) | 0.02715 (15) | |
W6 | 0.84356 (4) | 0.83128 (3) | 0.28918 (3) | 0.02891 (14) | |
W7 | 0.47775 (4) | 0.96709 (3) | 0.31877 (3) | 0.02173 (13) | |
W8 | 0.58052 (4) | 0.83896 (3) | 0.42380 (3) | 0.02433 (13) | |
W9 | 0.38832 (4) | 0.81294 (3) | 0.36346 (3) | 0.02353 (13) | |
W10 | 0.79346 (4) | 0.60124 (3) | 0.16499 (3) | 0.02333 (13) | |
W11 | 0.56218 (4) | 0.61722 (3) | 0.29058 (3) | 0.02719 (14) | |
W12 | 0.76004 (4) | 0.64985 (3) | 0.33924 (3) | 0.02981 (15) | |
O1 | 0.4636 (7) | 0.9934 (5) | 0.0792 (5) | 0.039 (3) | |
O2 | 0.7267 (7) | 0.7115 (4) | −0.0430 (5) | 0.031 (2) | |
O3 | 0.3359 (6) | 0.7282 (5) | 0.1529 (5) | 0.038 (2) | |
O4 | 1.0063 (6) | 0.7537 (4) | 0.0424 (5) | 0.031 (2) | |
O5 | 0.7551 (6) | 1.0398 (4) | 0.1516 (5) | 0.0301 (7) | |
O6 | 0.9312 (7) | 0.8376 (5) | 0.3348 (6) | 0.042 (3) | |
O7 | 0.4124 (6) | 1.0628 (4) | 0.3351 (5) | 0.032 (2) | |
O8 | 0.5885 (7) | 0.8510 (5) | 0.5103 (5) | 0.039 (3) | |
O9 | 0.2665 (6) | 0.8044 (5) | 0.4141 (5) | 0.033 (2) | |
O10 | 0.8802 (7) | 0.5247 (4) | 0.1094 (5) | 0.037 (2) | |
O11 | 0.4959 (7) | 0.5484 (5) | 0.3159 (6) | 0.045 (3) | |
O12 | 0.8175 (7) | 0.6032 (5) | 0.4026 (5) | 0.042 (3) | |
O13 | 0.8201 (6) | 0.9312 (5) | 0.2492 (5) | 0.031 (2) | |
O14 | 0.4447 (6) | 0.8177 (4) | 0.4449 (5) | 0.029 (2) | |
O15 | 0.6793 (6) | 0.5556 (4) | 0.2117 (5) | 0.031 (2) | |
O16 | 0.8354 (6) | 0.7247 (4) | 0.3066 (5) | 0.029 (2) | |
O17 | 0.4696 (6) | 0.7042 (4) | 0.3485 (5) | 0.030 (2) | |
O18 | 0.6060 (6) | 0.8500 (4) | 0.0323 (5) | 0.028 (2) | |
O19 | 0.5158 (6) | 0.9472 (4) | 0.4067 (5) | 0.023 (2) | |
O20 | 0.8730 (6) | 0.6796 (4) | 0.1447 (5) | 0.024 (2) | |
O21 | 0.3575 (6) | 0.9230 (4) | 0.3587 (5) | 0.026 (2) | |
O22 | 0.7230 (6) | 0.6541 (4) | 0.1000 (5) | 0.027 (2) | |
O23 | 0.7903 (6) | 0.7771 (4) | 0.0611 (4) | 0.023 (2) | |
O24 | 0.5398 (6) | 0.7181 (4) | 0.0703 (5) | 0.027 (2) | |
O25 | 0.6514 (6) | 0.7331 (4) | 0.4016 (5) | 0.027 (2) | |
O26 | 0.9463 (6) | 0.7895 (4) | 0.1924 (5) | 0.028 (2) | |
O27 | 0.6468 (6) | 0.9363 (4) | 0.1268 (5) | 0.026 (2) | |
O28 | 0.6477 (7) | 0.5945 (4) | 0.3548 (5) | 0.032 (2) | |
O29 | 0.8572 (6) | 0.8903 (4) | 0.1045 (5) | 0.022 (2) | |
O30 | 0.8398 (6) | 0.5816 (4) | 0.2546 (5) | 0.027 (2) | |
O31 | 0.6163 (6) | 0.9729 (4) | 0.2640 (5) | 0.023 (2) | |
O32 | 0.4627 (6) | 0.9485 (4) | 0.2213 (5) | 0.024 (2) | |
O33 | 0.4139 (6) | 0.8579 (4) | 0.1293 (5) | 0.025 (2) | |
O34 | 0.5052 (6) | 0.6660 (4) | 0.2116 (5) | 0.029 (2) | |
O35 | 0.3856 (6) | 0.8017 (4) | 0.2645 (5) | 0.024 (2) | |
O36 | 0.7129 (6) | 0.8580 (4) | 0.3625 (5) | 0.029 (2) | |
O37 | 0.6792 (5) | 0.6866 (4) | 0.2533 (5) | 0.0197 (19) | |
O38 | 0.7526 (5) | 0.8279 (4) | 0.2097 (5) | 0.020 (2) | |
O39 | 0.5438 (6) | 0.8396 (4) | 0.3170 (4) | 0.0182 (19) | |
O40 | 0.5798 (6) | 0.7975 (4) | 0.1589 (5) | 0.0198 (19) | |
N1 | 0.7551 (8) | 0.4471 (6) | 0.7227 (6) | 0.025 (3) | |
N2 | 0.7883 (8) | 0.5096 (6) | 0.8309 (6) | 0.030 (3) | |
N3 | 0.5814 (8) | 0.5501 (5) | 0.8384 (6) | 0.023 (2) | |
N4 | 0.6686 (8) | 0.6631 (5) | 0.8052 (6) | 0.028 (3) | |
N5 | 0.6413 (7) | 0.5976 (5) | 0.6862 (6) | 0.021 (2) | |
N6 | 0.8336 (8) | 0.5700 (5) | 0.6829 (6) | 0.024 (3) | |
N7 | 0.9408 (8) | 0.2451 (6) | 0.2498 (6) | 0.029 (3) | |
N8 | 0.7949 (8) | 0.2746 (6) | 0.3743 (7) | 0.029 (3) | |
N9 | 0.7705 (7) | 0.1720 (5) | 0.2837 (6) | 0.025 (3) | |
N10 | 0.8201 (8) | 0.1070 (6) | 0.3991 (6) | 0.028 (3) | |
N11 | 0.9891 (8) | 0.0809 (6) | 0.2729 (7) | 0.033 (3) | |
N12 | 0.9980 (8) | 0.1755 (6) | 0.3715 (8) | 0.039 (3) | |
C1 | 0.7368 (11) | 0.4212 (7) | 0.6644 (9) | 0.041 (4) | |
H1A | 0.6929 | 0.4550 | 0.6415 | 0.049* | |
C2 | 0.7802 (11) | 0.3457 (8) | 0.6359 (9) | 0.043 (4) | |
H2A | 0.7655 | 0.3286 | 0.5952 | 0.051* | |
C3 | 0.8458 (13) | 0.2971 (8) | 0.6698 (10) | 0.059 (5) | |
H3A | 0.8770 | 0.2463 | 0.6514 | 0.071* | |
C4 | 0.8662 (11) | 0.3225 (8) | 0.7313 (10) | 0.048 (5) | |
H4A | 0.9107 | 0.2891 | 0.7540 | 0.058* | |
C5 | 0.8194 (10) | 0.3979 (7) | 0.7583 (8) | 0.032 (3) | |
C6 | 0.8308 (9) | 0.4327 (7) | 0.8224 (7) | 0.021 (3) | |
C7 | 0.8812 (10) | 0.3914 (8) | 0.8701 (9) | 0.044 (4) | |
H7A | 0.9085 | 0.3381 | 0.8629 | 0.053* | |
C8 | 0.8907 (11) | 0.4304 (7) | 0.9292 (8) | 0.041 (4) | |
H8A | 0.9258 | 0.4040 | 0.9615 | 0.049* | |
C9 | 0.8473 (9) | 0.5080 (7) | 0.9385 (7) | 0.033 (3) | |
H9A | 0.8509 | 0.5357 | 0.9781 | 0.040* | |
C10 | 0.7985 (11) | 0.5447 (7) | 0.8893 (7) | 0.040 (4) | |
H10A | 0.7700 | 0.5979 | 0.8965 | 0.047* | |
C11 | 0.5410 (11) | 0.4879 (8) | 0.8536 (9) | 0.041 (4) | |
H11A | 0.5758 | 0.4433 | 0.8234 | 0.049* | |
C12 | 0.4517 (12) | 0.4860 (9) | 0.9105 (10) | 0.052 (4) | |
H12A | 0.4240 | 0.4431 | 0.9183 | 0.062* | |
C13 | 0.4065 (14) | 0.5535 (11) | 0.9554 (10) | 0.068 (6) | |
H13A | 0.3465 | 0.5556 | 0.9951 | 0.082* | |
C14 | 0.4455 (13) | 0.6150 (9) | 0.9438 (9) | 0.057 (5) | |
H14A | 0.4148 | 0.6584 | 0.9760 | 0.068* | |
C15 | 0.5315 (10) | 0.6137 (7) | 0.8836 (7) | 0.027 (3) | |
C16 | 0.5796 (11) | 0.6790 (7) | 0.8603 (8) | 0.031 (3) | |
C17 | 0.5327 (12) | 0.7536 (8) | 0.8960 (9) | 0.043 (4) | |
H17A | 0.4713 | 0.7639 | 0.9357 | 0.051* | |
C18 | 0.5852 (11) | 0.8114 (8) | 0.8672 (9) | 0.039 (4) | |
H18A | 0.5575 | 0.8619 | 0.8872 | 0.047* | |
C19 | 0.6778 (13) | 0.7929 (8) | 0.8092 (9) | 0.047 (4) | |
H19A | 0.7140 | 0.8300 | 0.7907 | 0.056* | |
C20 | 0.7138 (11) | 0.7205 (7) | 0.7804 (8) | 0.034 (4) | |
H20A | 0.7747 | 0.7092 | 0.7403 | 0.040* | |
C21 | 0.5361 (10) | 0.6147 (7) | 0.6948 (8) | 0.030 (3) | |
H21A | 0.4922 | 0.6020 | 0.7387 | 0.036* | |
C22 | 0.4916 (12) | 0.6498 (7) | 0.6418 (9) | 0.040 (4) | |
H22A | 0.4194 | 0.6597 | 0.6492 | 0.048* | |
C23 | 0.5569 (12) | 0.6701 (8) | 0.5771 (10) | 0.050 (4) | |
H23A | 0.5291 | 0.6942 | 0.5404 | 0.060* | |
C24 | 0.6632 (10) | 0.6542 (8) | 0.5677 (8) | 0.039 (4) | |
H24A | 0.7077 | 0.6684 | 0.5250 | 0.046* | |
C25 | 0.7040 (10) | 0.6165 (7) | 0.6229 (8) | 0.029 (3) | |
C26 | 0.8154 (10) | 0.5950 (7) | 0.6187 (8) | 0.029 (3) | |
C27 | 0.8959 (11) | 0.5980 (7) | 0.5535 (9) | 0.039 (4) | |
H27A | 0.8799 | 0.6146 | 0.5101 | 0.046* | |
C28 | 0.9984 (12) | 0.5763 (9) | 0.5544 (10) | 0.053 (5) | |
H28A | 1.0535 | 0.5777 | 0.5121 | 0.064* | |
C29 | 1.0164 (12) | 0.5527 (8) | 0.6190 (12) | 0.054 (5) | |
H29A | 1.0855 | 0.5385 | 0.6208 | 0.065* | |
C30 | 0.9355 (11) | 0.5487 (7) | 0.6836 (10) | 0.043 (4) | |
H30A | 0.9515 | 0.5314 | 0.7269 | 0.052* | |
C31 | 1.0141 (11) | 0.2243 (8) | 0.1841 (9) | 0.046 (4) | |
H31A | 1.0466 | 0.1720 | 0.1729 | 0.056* | |
C32 | 1.0432 (11) | 0.2758 (9) | 0.1332 (10) | 0.058 (5) | |
H32A | 1.0961 | 0.2597 | 0.0887 | 0.070* | |
C33 | 0.9916 (13) | 0.3531 (9) | 0.1498 (10) | 0.059 (5) | |
H33A | 1.0109 | 0.3900 | 0.1165 | 0.071* | |
C34 | 0.9140 (12) | 0.3753 (8) | 0.2132 (9) | 0.049 (5) | |
H34A | 0.8764 | 0.4270 | 0.2228 | 0.059* | |
C35 | 0.8909 (10) | 0.3214 (7) | 0.2634 (8) | 0.032 (4) | |
C36 | 0.8079 (10) | 0.3381 (7) | 0.3355 (8) | 0.030 (3) | |
C37 | 0.7494 (11) | 0.4108 (8) | 0.3642 (9) | 0.043 (4) | |
H37A | 0.7602 | 0.4540 | 0.3373 | 0.051* | |
C38 | 0.6753 (12) | 0.4200 (8) | 0.4325 (9) | 0.045 (4) | |
H38A | 0.6341 | 0.4688 | 0.4519 | 0.054* | |
C39 | 0.6637 (10) | 0.3565 (9) | 0.4706 (8) | 0.038 (4) | |
H39A | 0.6146 | 0.3615 | 0.5174 | 0.046* | |
C40 | 0.7229 (10) | 0.2848 (7) | 0.4416 (9) | 0.036 (4) | |
H40A | 0.7133 | 0.2417 | 0.4691 | 0.043* | |
C41 | 0.7463 (11) | 0.2076 (7) | 0.2264 (8) | 0.033 (4) | |
H41A | 0.7951 | 0.2301 | 0.1940 | 0.039* | |
C42 | 0.6516 (12) | 0.2131 (7) | 0.2124 (9) | 0.041 (4) | |
H42A | 0.6370 | 0.2393 | 0.1718 | 0.049* | |
C43 | 0.5791 (12) | 0.1790 (8) | 0.2593 (9) | 0.043 (4) | |
H43A | 0.5156 | 0.1810 | 0.2502 | 0.052* | |
C44 | 0.6016 (10) | 0.1432 (8) | 0.3180 (9) | 0.036 (4) | |
H44A | 0.5513 | 0.1231 | 0.3517 | 0.044* | |
C45 | 0.7010 (10) | 0.1355 (7) | 0.3296 (7) | 0.025 (3) | |
C46 | 0.7338 (10) | 0.0946 (7) | 0.3881 (8) | 0.031 (3) | |
C47 | 0.6845 (10) | 0.0389 (7) | 0.4288 (8) | 0.033 (4) | |
H47A | 0.6240 | 0.0304 | 0.4218 | 0.039* | |
C48 | 0.7316 (10) | −0.0028 (7) | 0.4803 (8) | 0.033 (3) | |
H48A | 0.7037 | −0.0409 | 0.5072 | 0.039* | |
C49 | 0.8166 (11) | 0.0130 (7) | 0.4900 (8) | 0.041 (4) | |
H49A | 0.8469 | −0.0135 | 0.5247 | 0.050* | |
C50 | 0.8597 (10) | 0.0673 (8) | 0.4501 (10) | 0.045 (4) | |
H50A | 0.9186 | 0.0772 | 0.4585 | 0.054* | |
C51 | 0.9763 (11) | 0.0310 (8) | 0.2265 (9) | 0.043 (4) | |
H51A | 0.9136 | 0.0429 | 0.2142 | 0.051* | |
C52 | 1.0490 (13) | −0.0351 (9) | 0.1968 (11) | 0.071 (7) | |
H52A | 1.0351 | −0.0690 | 0.1670 | 0.085* | |
C53 | 1.1451 (15) | −0.0513 (10) | 0.2119 (11) | 0.072 (7) | |
H53A | 1.1971 | −0.0963 | 0.1926 | 0.087* | |
C54 | 1.1608 (12) | 0.0001 (11) | 0.2553 (10) | 0.061 (5) | |
H54A | 1.2259 | −0.0089 | 0.2640 | 0.074* | |
C55 | 1.0835 (12) | 0.0651 (10) | 0.2871 (9) | 0.049 (5) | |
C56 | 1.0877 (11) | 0.1199 (9) | 0.3407 (9) | 0.040 (4) | |
C57 | 1.1800 (13) | 0.1160 (11) | 0.3615 (12) | 0.072 (6) | |
H57A | 1.2425 | 0.0798 | 0.3381 | 0.086* | |
C58 | 1.1764 (14) | 0.1666 (11) | 0.4169 (12) | 0.068 (6) | |
H58A | 1.2357 | 0.1653 | 0.4315 | 0.081* | |
C59 | 1.0808 (17) | 0.2191 (10) | 0.4495 (13) | 0.084 (7) | |
H59A | 1.0742 | 0.2533 | 0.4877 | 0.101* | |
C60 | 0.9958 (12) | 0.2203 (8) | 0.4251 (11) | 0.060 (6) | |
H60A | 0.9323 | 0.2556 | 0.4484 | 0.072* | |
Na1 | 0.7947 (5) | 1.0995 (4) | 0.0270 (4) | 0.0751 (15) | |
O1W | 0.7839 (9) | 1.2094 (7) | −0.0504 (7) | 0.0794 (19) | |
O2W | 0.8830 (9) | 0.9698 (6) | −0.0244 (7) | 0.074 (4) | |
O3W | 0.6430 (9) | 1.0906 (6) | 0.0079 (7) | 0.073 (4) | |
O4W | 0.9220 (9) | 1.1344 (7) | 0.0645 (7) | 0.0767 (19) | |
O5W | 0.3093 (14) | 0.6046 (9) | 0.8143 (12) | 0.044 (6) | 0.50 |
O6W | 0.7497 (9) | 0.9148 (6) | −0.0845 (7) | 0.073 (4) | |
O7W | 0.0495 (14) | 0.9066 (12) | 0.4157 (13) | 0.064 (7) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0208 (9) | 0.0183 (9) | 0.0178 (11) | −0.0033 (7) | −0.0068 (8) | 0.0007 (8) |
Fe2 | 0.0319 (10) | 0.0225 (10) | 0.0247 (12) | −0.0059 (8) | −0.0127 (9) | −0.0004 (8) |
Fe3 | 0.0238 (10) | 0.0234 (10) | 0.0356 (14) | −0.0064 (8) | −0.0110 (9) | 0.0105 (9) |
W1 | 0.0358 (3) | 0.0204 (3) | 0.0200 (3) | 0.0003 (2) | −0.0124 (3) | 0.0030 (2) |
W2 | 0.0294 (3) | 0.0229 (3) | 0.0141 (3) | −0.0025 (2) | −0.0072 (2) | −0.0004 (2) |
W3 | 0.0274 (3) | 0.0313 (3) | 0.0233 (4) | −0.0099 (2) | −0.0109 (3) | −0.0008 (3) |
W4 | 0.0220 (3) | 0.0217 (3) | 0.0219 (3) | −0.0019 (2) | −0.0029 (2) | 0.0002 (2) |
W5 | 0.0270 (3) | 0.0184 (3) | 0.0321 (4) | −0.0062 (2) | −0.0024 (3) | −0.0006 (2) |
W6 | 0.0251 (3) | 0.0378 (3) | 0.0259 (4) | −0.0072 (2) | −0.0107 (3) | −0.0051 (3) |
W7 | 0.0233 (3) | 0.0188 (3) | 0.0208 (3) | −0.0018 (2) | −0.0058 (2) | −0.0021 (2) |
W8 | 0.0298 (3) | 0.0264 (3) | 0.0155 (3) | −0.0028 (2) | −0.0084 (2) | −0.0017 (2) |
W9 | 0.0246 (3) | 0.0247 (3) | 0.0194 (3) | −0.0069 (2) | −0.0029 (2) | −0.0008 (2) |
W10 | 0.0306 (3) | 0.0168 (3) | 0.0183 (3) | −0.0001 (2) | −0.0059 (2) | 0.0007 (2) |
W11 | 0.0335 (3) | 0.0193 (3) | 0.0256 (4) | −0.0075 (2) | −0.0036 (3) | 0.0033 (2) |
W12 | 0.0421 (3) | 0.0236 (3) | 0.0215 (4) | 0.0034 (2) | −0.0166 (3) | 0.0027 (2) |
O1 | 0.056 (6) | 0.032 (5) | 0.015 (6) | 0.012 (5) | −0.009 (5) | 0.002 (4) |
O2 | 0.043 (5) | 0.027 (5) | 0.017 (6) | 0.003 (4) | −0.009 (4) | −0.003 (4) |
O3 | 0.029 (5) | 0.057 (6) | 0.033 (7) | −0.012 (5) | −0.014 (5) | −0.008 (5) |
O4 | 0.033 (5) | 0.027 (5) | 0.025 (6) | −0.003 (4) | −0.002 (4) | 0.001 (4) |
O5 | 0.0299 (10) | 0.0209 (10) | 0.0350 (11) | −0.0063 (10) | −0.0030 (10) | −0.0005 (10) |
O6 | 0.034 (5) | 0.049 (6) | 0.051 (8) | 0.000 (5) | −0.032 (5) | −0.005 (5) |
O7 | 0.027 (5) | 0.018 (4) | 0.039 (7) | 0.002 (4) | 0.000 (4) | −0.003 (4) |
O8 | 0.050 (6) | 0.044 (6) | 0.030 (7) | −0.013 (5) | −0.019 (5) | −0.001 (5) |
O9 | 0.028 (5) | 0.046 (6) | 0.027 (6) | −0.012 (4) | −0.009 (4) | −0.001 (5) |
O10 | 0.047 (6) | 0.020 (5) | 0.030 (6) | 0.006 (4) | −0.007 (5) | 0.002 (4) |
O11 | 0.050 (6) | 0.033 (5) | 0.043 (7) | −0.015 (5) | 0.004 (5) | 0.002 (5) |
O12 | 0.065 (7) | 0.039 (6) | 0.019 (6) | 0.007 (5) | −0.028 (5) | 0.002 (5) |
O13 | 0.031 (5) | 0.029 (5) | 0.033 (6) | −0.006 (4) | −0.008 (4) | −0.006 (4) |
O14 | 0.038 (5) | 0.018 (4) | 0.019 (6) | 0.000 (4) | 0.002 (4) | 0.002 (4) |
O15 | 0.038 (5) | 0.023 (5) | 0.029 (6) | −0.004 (4) | −0.006 (5) | 0.002 (4) |
O16 | 0.020 (4) | 0.031 (5) | 0.032 (6) | 0.002 (4) | −0.006 (4) | −0.005 (4) |
O17 | 0.036 (5) | 0.023 (5) | 0.029 (6) | −0.008 (4) | −0.006 (4) | −0.003 (4) |
O18 | 0.035 (5) | 0.028 (5) | 0.020 (6) | −0.001 (4) | −0.014 (4) | 0.000 (4) |
O19 | 0.025 (5) | 0.026 (5) | 0.016 (5) | −0.004 (4) | −0.004 (4) | −0.003 (4) |
O20 | 0.026 (5) | 0.026 (5) | 0.021 (6) | −0.008 (4) | −0.005 (4) | −0.001 (4) |
O21 | 0.025 (5) | 0.031 (5) | 0.024 (6) | −0.013 (4) | −0.004 (4) | 0.000 (4) |
O22 | 0.031 (5) | 0.023 (5) | 0.024 (6) | −0.004 (4) | −0.006 (4) | 0.003 (4) |
O23 | 0.029 (5) | 0.024 (4) | 0.011 (5) | −0.007 (4) | 0.001 (4) | 0.002 (4) |
O24 | 0.031 (5) | 0.029 (5) | 0.025 (6) | −0.006 (4) | −0.015 (4) | −0.013 (4) |
O25 | 0.032 (5) | 0.028 (5) | 0.019 (6) | 0.003 (4) | −0.015 (4) | 0.005 (4) |
O26 | 0.026 (5) | 0.030 (5) | 0.028 (6) | −0.003 (4) | −0.010 (4) | −0.012 (4) |
O27 | 0.043 (5) | 0.019 (4) | 0.014 (5) | −0.009 (4) | −0.006 (4) | 0.002 (4) |
O28 | 0.047 (6) | 0.023 (5) | 0.018 (6) | −0.002 (4) | −0.003 (5) | 0.000 (4) |
O29 | 0.028 (5) | 0.017 (4) | 0.025 (6) | −0.010 (4) | −0.010 (4) | 0.000 (4) |
O30 | 0.035 (5) | 0.026 (5) | 0.021 (6) | −0.006 (4) | −0.012 (4) | 0.007 (4) |
O31 | 0.028 (5) | 0.019 (4) | 0.024 (6) | −0.003 (4) | −0.012 (4) | −0.002 (4) |
O32 | 0.026 (5) | 0.021 (4) | 0.025 (6) | −0.007 (4) | −0.007 (4) | 0.009 (4) |
O33 | 0.028 (5) | 0.027 (5) | 0.022 (6) | −0.004 (4) | −0.015 (4) | −0.002 (4) |
O34 | 0.030 (5) | 0.024 (5) | 0.038 (7) | −0.012 (4) | −0.011 (5) | −0.002 (4) |
O35 | 0.028 (5) | 0.028 (5) | 0.020 (6) | −0.015 (4) | −0.007 (4) | 0.003 (4) |
O36 | 0.032 (5) | 0.028 (5) | 0.021 (6) | −0.002 (4) | −0.005 (4) | −0.007 (4) |
O37 | 0.014 (4) | 0.025 (4) | 0.019 (5) | 0.002 (3) | −0.010 (4) | 0.003 (4) |
O38 | 0.014 (4) | 0.018 (4) | 0.030 (6) | 0.002 (3) | −0.013 (4) | −0.004 (4) |
O39 | 0.022 (4) | 0.017 (4) | 0.015 (5) | −0.004 (3) | −0.006 (4) | −0.002 (4) |
O40 | 0.032 (5) | 0.012 (4) | 0.017 (5) | −0.002 (3) | −0.013 (4) | 0.001 (4) |
N1 | 0.031 (6) | 0.027 (6) | 0.021 (7) | −0.006 (5) | −0.013 (5) | −0.014 (5) |
N2 | 0.036 (6) | 0.022 (6) | 0.033 (8) | 0.002 (5) | −0.016 (6) | −0.002 (5) |
N3 | 0.041 (6) | 0.019 (5) | 0.016 (7) | −0.007 (5) | −0.017 (5) | 0.000 (5) |
N4 | 0.033 (6) | 0.024 (6) | 0.029 (8) | −0.004 (5) | −0.016 (6) | 0.008 (5) |
N5 | 0.026 (6) | 0.023 (6) | 0.020 (7) | −0.006 (5) | −0.015 (5) | −0.001 (5) |
N6 | 0.024 (6) | 0.025 (6) | 0.026 (7) | −0.006 (5) | −0.010 (5) | −0.005 (5) |
N7 | 0.028 (6) | 0.033 (6) | 0.030 (8) | −0.014 (5) | −0.011 (6) | 0.012 (5) |
N8 | 0.024 (6) | 0.030 (6) | 0.037 (8) | −0.009 (5) | −0.016 (6) | 0.014 (6) |
N9 | 0.025 (6) | 0.020 (5) | 0.029 (8) | −0.009 (5) | −0.005 (5) | 0.004 (5) |
N10 | 0.034 (6) | 0.026 (6) | 0.030 (8) | −0.008 (5) | −0.019 (6) | 0.005 (5) |
N11 | 0.022 (6) | 0.032 (6) | 0.035 (8) | −0.004 (5) | 0.000 (5) | 0.023 (6) |
N12 | 0.032 (7) | 0.021 (6) | 0.072 (11) | −0.008 (5) | −0.026 (7) | 0.021 (6) |
C1 | 0.044 (9) | 0.031 (8) | 0.038 (11) | 0.004 (7) | −0.010 (8) | −0.016 (7) |
C2 | 0.043 (4) | 0.043 (4) | 0.043 (4) | −0.0111 (14) | −0.0128 (15) | 0.0012 (11) |
C3 | 0.086 (13) | 0.022 (8) | 0.068 (14) | 0.000 (8) | −0.033 (11) | −0.009 (8) |
C4 | 0.041 (9) | 0.027 (8) | 0.067 (13) | 0.009 (7) | −0.016 (9) | −0.014 (8) |
C5 | 0.039 (8) | 0.034 (8) | 0.028 (9) | −0.007 (6) | −0.018 (7) | 0.000 (7) |
C6 | 0.018 (6) | 0.027 (7) | 0.021 (8) | −0.002 (5) | −0.011 (6) | −0.011 (6) |
C7 | 0.033 (8) | 0.039 (9) | 0.053 (12) | 0.002 (7) | −0.012 (8) | −0.007 (8) |
C8 | 0.060 (10) | 0.031 (8) | 0.032 (10) | 0.004 (7) | −0.028 (8) | 0.005 (7) |
C9 | 0.036 (8) | 0.053 (9) | 0.024 (9) | −0.021 (7) | −0.019 (7) | 0.007 (7) |
C10 | 0.055 (10) | 0.021 (7) | 0.036 (11) | 0.000 (7) | −0.010 (8) | −0.004 (7) |
C11 | 0.058 (10) | 0.030 (8) | 0.039 (11) | −0.013 (7) | −0.020 (8) | 0.003 (7) |
C12 | 0.052 (4) | 0.052 (4) | 0.052 (4) | −0.0134 (15) | −0.0154 (16) | 0.0024 (11) |
C13 | 0.074 (13) | 0.094 (15) | 0.040 (13) | −0.044 (12) | −0.003 (10) | 0.013 (11) |
C14 | 0.074 (12) | 0.045 (10) | 0.038 (12) | −0.017 (9) | 0.006 (9) | −0.010 (8) |
C15 | 0.038 (8) | 0.028 (7) | 0.013 (8) | −0.004 (6) | −0.011 (6) | 0.007 (6) |
C16 | 0.049 (9) | 0.015 (7) | 0.035 (10) | −0.002 (6) | −0.026 (8) | 0.001 (6) |
C17 | 0.064 (10) | 0.040 (9) | 0.029 (10) | −0.008 (8) | −0.027 (8) | 0.001 (7) |
C18 | 0.045 (9) | 0.026 (8) | 0.047 (11) | 0.001 (7) | −0.025 (8) | −0.001 (7) |
C19 | 0.074 (12) | 0.030 (8) | 0.041 (11) | −0.015 (8) | −0.024 (9) | 0.002 (7) |
C20 | 0.039 (8) | 0.040 (8) | 0.026 (9) | −0.016 (7) | −0.010 (7) | 0.002 (7) |
C21 | 0.027 (7) | 0.029 (7) | 0.030 (10) | −0.007 (6) | −0.003 (7) | −0.010 (6) |
C22 | 0.052 (9) | 0.035 (8) | 0.044 (11) | 0.001 (7) | −0.040 (8) | 0.002 (7) |
C23 | 0.050 (4) | 0.050 (4) | 0.050 (4) | −0.0128 (15) | −0.0150 (16) | 0.0023 (11) |
C24 | 0.031 (8) | 0.063 (10) | 0.022 (9) | −0.011 (7) | −0.010 (7) | 0.008 (8) |
C25 | 0.034 (8) | 0.034 (8) | 0.021 (9) | −0.009 (6) | −0.010 (7) | 0.006 (6) |
C26 | 0.035 (8) | 0.027 (7) | 0.024 (9) | −0.010 (6) | −0.003 (7) | −0.008 (6) |
C27 | 0.046 (9) | 0.032 (8) | 0.034 (10) | −0.005 (7) | −0.009 (8) | −0.007 (7) |
C28 | 0.040 (10) | 0.060 (11) | 0.045 (13) | −0.006 (8) | 0.004 (9) | −0.011 (10) |
C29 | 0.027 (8) | 0.034 (9) | 0.091 (17) | −0.002 (7) | −0.004 (10) | −0.016 (10) |
C30 | 0.046 (9) | 0.024 (8) | 0.063 (13) | −0.005 (7) | −0.024 (9) | 0.003 (8) |
C31 | 0.041 (9) | 0.038 (9) | 0.049 (12) | −0.001 (7) | −0.006 (8) | 0.006 (8) |
C32 | 0.038 (9) | 0.056 (11) | 0.064 (14) | −0.012 (8) | 0.011 (9) | 0.005 (10) |
C33 | 0.063 (11) | 0.048 (10) | 0.060 (14) | −0.023 (9) | −0.005 (10) | 0.027 (9) |
C34 | 0.060 (10) | 0.028 (8) | 0.052 (12) | −0.009 (7) | −0.008 (9) | 0.015 (8) |
C35 | 0.021 (7) | 0.032 (8) | 0.044 (11) | −0.002 (6) | −0.016 (7) | 0.002 (7) |
C36 | 0.040 (8) | 0.023 (7) | 0.038 (10) | −0.013 (6) | −0.025 (7) | 0.014 (7) |
C37 | 0.042 (9) | 0.035 (8) | 0.057 (13) | −0.007 (7) | −0.025 (9) | 0.004 (8) |
C38 | 0.047 (10) | 0.037 (9) | 0.048 (12) | −0.001 (7) | −0.017 (9) | −0.007 (8) |
C39 | 0.028 (8) | 0.064 (10) | 0.029 (10) | −0.014 (7) | −0.015 (7) | 0.005 (8) |
C40 | 0.043 (9) | 0.027 (7) | 0.037 (10) | 0.004 (6) | −0.021 (8) | −0.014 (7) |
C41 | 0.038 (8) | 0.028 (8) | 0.029 (10) | −0.003 (6) | −0.010 (7) | 0.014 (7) |
C42 | 0.072 (11) | 0.028 (8) | 0.034 (10) | −0.009 (8) | −0.037 (9) | −0.001 (7) |
C43 | 0.055 (10) | 0.037 (9) | 0.045 (12) | −0.013 (8) | −0.026 (9) | −0.015 (8) |
C44 | 0.032 (8) | 0.044 (9) | 0.036 (11) | −0.018 (7) | −0.007 (7) | −0.011 (8) |
C45 | 0.031 (7) | 0.026 (7) | 0.018 (8) | −0.002 (6) | −0.011 (6) | −0.006 (6) |
C46 | 0.025 (7) | 0.027 (7) | 0.046 (11) | −0.007 (6) | −0.019 (7) | 0.009 (7) |
C47 | 0.033 (8) | 0.025 (7) | 0.035 (10) | −0.011 (6) | 0.000 (7) | −0.002 (7) |
C48 | 0.033 (3) | 0.032 (3) | 0.032 (3) | −0.0087 (13) | −0.0090 (14) | 0.0021 (11) |
C49 | 0.057 (10) | 0.031 (8) | 0.026 (10) | 0.001 (7) | −0.008 (8) | 0.000 (7) |
C50 | 0.025 (8) | 0.035 (9) | 0.068 (13) | −0.001 (7) | −0.008 (8) | −0.004 (8) |
C51 | 0.028 (8) | 0.038 (9) | 0.057 (12) | −0.011 (7) | −0.003 (8) | 0.001 (8) |
C52 | 0.054 (11) | 0.044 (10) | 0.077 (16) | −0.004 (9) | 0.033 (11) | −0.009 (10) |
C53 | 0.063 (13) | 0.039 (10) | 0.073 (17) | 0.025 (9) | 0.008 (11) | 0.016 (10) |
C54 | 0.033 (9) | 0.088 (14) | 0.051 (14) | −0.012 (10) | 0.002 (9) | 0.022 (11) |
C55 | 0.035 (9) | 0.067 (11) | 0.028 (11) | −0.002 (8) | 0.003 (8) | 0.022 (9) |
C56 | 0.030 (8) | 0.055 (10) | 0.031 (10) | −0.014 (7) | −0.005 (7) | 0.024 (8) |
C57 | 0.034 (10) | 0.087 (14) | 0.087 (18) | −0.020 (10) | −0.011 (10) | 0.062 (13) |
C58 | 0.051 (12) | 0.061 (12) | 0.103 (19) | −0.006 (10) | −0.050 (12) | 0.036 (12) |
C59 | 0.133 (19) | 0.044 (11) | 0.13 (2) | −0.041 (12) | −0.111 (17) | 0.029 (12) |
C60 | 0.054 (10) | 0.014 (7) | 0.116 (18) | 0.002 (7) | −0.037 (11) | −0.011 (9) |
Na1 | 0.068 (3) | 0.072 (3) | 0.077 (3) | −0.007 (2) | −0.019 (3) | 0.007 (3) |
O1W | 0.073 (3) | 0.076 (3) | 0.081 (4) | −0.008 (3) | −0.020 (3) | 0.009 (3) |
O2W | 0.076 (8) | 0.077 (8) | 0.058 (10) | −0.009 (7) | −0.012 (7) | 0.020 (7) |
O3W | 0.083 (9) | 0.072 (8) | 0.065 (10) | −0.010 (7) | −0.036 (7) | 0.013 (7) |
O4W | 0.070 (3) | 0.073 (3) | 0.078 (4) | −0.008 (3) | −0.019 (3) | 0.007 (3) |
O5W | 0.048 (12) | 0.012 (9) | 0.087 (18) | −0.003 (8) | −0.045 (12) | 0.013 (10) |
O6W | 0.079 (8) | 0.059 (7) | 0.068 (10) | −0.024 (6) | 0.004 (7) | 0.011 (7) |
O7W | 0.034 (12) | 0.084 (16) | 0.054 (17) | 0.027 (11) | −0.015 (11) | −0.054 (13) |
Fe1—O37 | 1.811 (7) | N11—C55 | 1.360 (18) |
Fe1—O39 | 1.811 (7) | N12—C60 | 1.299 (19) |
Fe1—O38 | 1.812 (7) | N12—C56 | 1.355 (16) |
Fe1—O40 | 1.822 (8) | C1—C2 | 1.384 (17) |
Fe2—N3 | 1.959 (10) | C1—H1A | 0.9300 |
Fe2—N6 | 1.959 (10) | C2—C3 | 1.37 (2) |
Fe2—N5 | 1.961 (10) | C2—H2A | 0.9300 |
Fe2—N2 | 1.962 (12) | C3—C4 | 1.39 (2) |
Fe2—N4 | 1.983 (10) | C3—H3A | 0.9300 |
Fe2—N1 | 1.986 (9) | C4—C5 | 1.381 (17) |
Fe3—N8 | 1.965 (11) | C4—H4A | 0.9300 |
Fe3—N7 | 1.966 (11) | C5—C6 | 1.445 (18) |
Fe3—N11 | 1.976 (11) | C6—C7 | 1.38 (2) |
Fe3—N12 | 1.977 (12) | C7—C8 | 1.390 (19) |
Fe3—N9 | 1.990 (11) | C7—H7A | 0.9300 |
Fe3—N10 | 1.996 (11) | C8—C9 | 1.359 (9) |
W1—O1 | 1.715 (9) | C8—H8A | 0.9300 |
W1—O32 | 1.867 (8) | C9—C10 | 1.357 (9) |
W1—O33 | 1.909 (8) | C9—H9A | 0.9300 |
W1—O27 | 1.956 (8) | C10—H10A | 0.9300 |
W1—O18 | 1.961 (8) | C11—C12 | 1.380 (19) |
W1—O40 | 2.217 (7) | C11—H11A | 0.9300 |
W2—O2 | 1.702 (8) | C12—C13 | 1.39 (2) |
W2—O18 | 1.923 (8) | C12—H12A | 0.9300 |
W2—O23 | 1.923 (8) | C13—C14 | 1.328 (19) |
W2—O24 | 1.947 (8) | C13—H13A | 0.9300 |
W2—O22 | 1.957 (8) | C14—C15 | 1.373 (18) |
W2—O40 | 2.216 (8) | C14—H14A | 0.9300 |
W3—O3 | 1.712 (8) | C15—C16 | 1.478 (17) |
W3—O34 | 1.878 (9) | C16—C17 | 1.421 (17) |
W3—O24 | 1.920 (8) | C17—C18 | 1.415 (18) |
W3—O35 | 1.930 (8) | C17—H17A | 0.9300 |
W3—O33 | 1.976 (8) | C18—C19 | 1.383 (19) |
W3—O40 | 2.213 (7) | C18—H18A | 0.9300 |
W4—O4 | 1.718 (8) | C19—C20 | 1.333 (17) |
W4—O20 | 1.880 (8) | C19—H19A | 0.9300 |
W4—O26 | 1.910 (9) | C20—H20A | 0.9300 |
W4—O23 | 1.916 (9) | C21—C22 | 1.375 (19) |
W4—O29 | 1.967 (7) | C21—H21A | 0.9300 |
W4—O38 | 2.214 (7) | C22—C23 | 1.39 (2) |
W5—O5 | 1.718 (8) | C22—H22A | 0.9300 |
W5—O27 | 1.875 (9) | C23—C24 | 1.373 (18) |
W5—O31 | 1.908 (8) | C23—H23A | 0.9300 |
W5—O29 | 1.915 (8) | C24—C25 | 1.400 (19) |
W5—O13 | 1.950 (10) | C24—H24A | 0.9300 |
W5—O38 | 2.222 (7) | C25—C26 | 1.459 (18) |
W6—O6 | 1.702 (9) | C26—C27 | 1.402 (18) |
W6—O36 | 1.874 (8) | C27—C28 | 1.37 (2) |
W6—O13 | 1.904 (9) | C27—H27A | 0.9300 |
W6—O16 | 1.951 (8) | C28—C29 | 1.35 (2) |
W6—O26 | 1.980 (8) | C28—H28A | 0.9300 |
W6—O38 | 2.229 (8) | C29—C30 | 1.40 (2) |
W7—O7 | 1.709 (7) | C29—H29A | 0.9300 |
W7—O19 | 1.878 (9) | C30—H30A | 0.9300 |
W7—O31 | 1.908 (8) | C31—C32 | 1.35 (2) |
W7—O21 | 1.954 (7) | C31—H31A | 0.9300 |
W7—O32 | 1.960 (9) | C32—C33 | 1.38 (2) |
W7—O39 | 2.226 (7) | C32—H32A | 0.9300 |
W8—O8 | 1.692 (10) | C33—C34 | 1.34 (2) |
W8—O25 | 1.893 (7) | C33—H33A | 0.9300 |
W8—O14 | 1.926 (8) | C34—C35 | 1.360 (19) |
W8—O36 | 1.954 (8) | C34—H34A | 0.9300 |
W8—O19 | 1.973 (8) | C35—C36 | 1.477 (18) |
W8—O39 | 2.216 (8) | C36—C37 | 1.374 (17) |
W9—O9 | 1.708 (8) | C37—C38 | 1.37 (2) |
W9—O35 | 1.898 (9) | C37—H37A | 0.9300 |
W9—O21 | 1.911 (8) | C38—C39 | 1.343 (19) |
W9—O14 | 1.928 (9) | C38—H38A | 0.9300 |
W9—O17 | 1.962 (8) | C39—C40 | 1.363 (17) |
W9—O39 | 2.228 (7) | C39—H39A | 0.9300 |
W10—O10 | 1.709 (8) | C40—H40A | 0.9300 |
W10—O22 | 1.868 (9) | C41—C42 | 1.383 (19) |
W10—O15 | 1.924 (8) | C41—H41A | 0.9300 |
W10—O20 | 1.952 (7) | C42—C43 | 1.380 (19) |
W10—O30 | 1.967 (9) | C42—H42A | 0.9300 |
W10—O37 | 2.231 (7) | C43—C44 | 1.34 (2) |
W11—O11 | 1.690 (8) | C43—H43A | 0.9300 |
W11—O17 | 1.876 (8) | C44—C45 | 1.421 (18) |
W11—O28 | 1.892 (10) | C44—H44A | 0.9300 |
W11—O15 | 1.953 (8) | C45—C46 | 1.424 (18) |
W11—O34 | 1.962 (9) | C46—C47 | 1.426 (16) |
W11—O37 | 2.220 (7) | C47—C48 | 1.413 (19) |
W12—O12 | 1.704 (9) | C47—H47A | 0.9300 |
W12—O16 | 1.879 (8) | C48—C49 | 1.335 (18) |
W12—O30 | 1.912 (8) | C48—H48A | 0.9300 |
W12—O25 | 1.943 (8) | C49—C50 | 1.358 (18) |
W12—O28 | 1.988 (8) | C49—H49A | 0.9300 |
W12—O37 | 2.218 (8) | C50—H50A | 0.9300 |
O5—Na1 | 2.518 (12) | C51—C52 | 1.349 (18) |
N1—C1 | 1.324 (17) | C51—H51A | 0.9300 |
N1—C5 | 1.384 (16) | C52—C53 | 1.39 (3) |
N2—C6 | 1.343 (14) | C52—H52A | 0.9300 |
N2—C10 | 1.347 (16) | C53—C54 | 1.35 (2) |
N3—C15 | 1.347 (15) | C53—H53A | 0.9300 |
N3—C11 | 1.353 (15) | C54—C55 | 1.37 (2) |
N4—C16 | 1.324 (16) | C54—H54A | 0.9300 |
N4—C20 | 1.336 (15) | C55—C56 | 1.46 (2) |
N5—C25 | 1.342 (15) | C56—C57 | 1.42 (2) |
N5—C21 | 1.361 (15) | C57—C58 | 1.39 (3) |
N6—C26 | 1.348 (17) | C57—H57A | 0.9300 |
N6—C30 | 1.359 (16) | C58—C59 | 1.39 (2) |
N7—C31 | 1.339 (17) | C58—H58A | 0.9300 |
N7—C35 | 1.357 (15) | C59—C60 | 1.37 (2) |
N8—C40 | 1.345 (16) | C59—H59A | 0.9300 |
N8—C36 | 1.353 (15) | C60—H60A | 0.9300 |
N9—C41 | 1.320 (17) | Na1—O3W | 2.265 (14) |
N9—C45 | 1.373 (15) | Na1—O4W | 2.298 (15) |
N10—C46 | 1.335 (15) | Na1—O1W | 2.410 (14) |
N10—C50 | 1.340 (19) | Na1—O2W | 2.413 (13) |
N11—C51 | 1.350 (18) | ||
O37—Fe1—O39 | 109.0 (4) | W11—O37—W10 | 96.0 (3) |
O37—Fe1—O38 | 109.7 (3) | Fe1—O38—W4 | 120.0 (4) |
O39—Fe1—O38 | 108.8 (3) | Fe1—O38—W5 | 121.0 (4) |
O37—Fe1—O40 | 109.3 (3) | W4—O38—W5 | 96.3 (3) |
O39—Fe1—O40 | 109.5 (4) | Fe1—O38—W6 | 121.5 (4) |
O38—Fe1—O40 | 110.5 (4) | W4—O38—W6 | 96.5 (3) |
N3—Fe2—N6 | 175.6 (4) | W5—O38—W6 | 95.6 (3) |
N3—Fe2—N5 | 95.8 (4) | Fe1—O39—W8 | 121.7 (4) |
N6—Fe2—N5 | 81.0 (4) | Fe1—O39—W7 | 120.7 (4) |
N3—Fe2—N2 | 87.6 (4) | W8—O39—W7 | 95.8 (3) |
N6—Fe2—N2 | 95.8 (5) | Fe1—O39—W9 | 120.8 (4) |
N5—Fe2—N2 | 175.6 (4) | W8—O39—W9 | 96.3 (3) |
N3—Fe2—N4 | 81.6 (4) | W7—O39—W9 | 95.1 (3) |
N6—Fe2—N4 | 95.2 (4) | Fe1—O40—W3 | 121.4 (4) |
N5—Fe2—N4 | 87.7 (4) | Fe1—O40—W2 | 120.3 (4) |
N2—Fe2—N4 | 95.7 (4) | W3—O40—W2 | 96.0 (3) |
N3—Fe2—N1 | 97.6 (4) | Fe1—O40—W1 | 119.9 (3) |
N6—Fe2—N1 | 85.7 (4) | W3—O40—W1 | 97.0 (3) |
N5—Fe2—N1 | 95.5 (4) | W2—O40—W1 | 96.4 (3) |
N2—Fe2—N1 | 81.2 (4) | C1—N1—C5 | 120.1 (11) |
N4—Fe2—N1 | 176.8 (5) | C1—N1—Fe2 | 126.2 (9) |
N8—Fe3—N7 | 81.5 (4) | C5—N1—Fe2 | 113.5 (9) |
N8—Fe3—N11 | 174.7 (4) | C6—N2—C10 | 115.8 (11) |
N7—Fe3—N11 | 94.3 (4) | C6—N2—Fe2 | 116.5 (9) |
N8—Fe3—N12 | 94.2 (5) | C10—N2—Fe2 | 127.5 (8) |
N7—Fe3—N12 | 90.3 (5) | C15—N3—C11 | 117.0 (11) |
N11—Fe3—N12 | 82.6 (5) | C15—N3—Fe2 | 115.7 (8) |
N8—Fe3—N9 | 86.0 (4) | C11—N3—Fe2 | 127.2 (9) |
N7—Fe3—N9 | 93.0 (4) | C16—N4—C20 | 118.4 (11) |
N11—Fe3—N9 | 97.5 (5) | C16—N4—Fe2 | 113.9 (8) |
N12—Fe3—N9 | 176.6 (5) | C20—N4—Fe2 | 127.3 (9) |
N8—Fe3—N10 | 97.0 (4) | C25—N5—C21 | 117.9 (12) |
N7—Fe3—N10 | 175.1 (5) | C25—N5—Fe2 | 115.6 (8) |
N11—Fe3—N10 | 87.5 (4) | C21—N5—Fe2 | 126.2 (9) |
N12—Fe3—N10 | 94.5 (5) | C26—N6—C30 | 117.2 (12) |
N9—Fe3—N10 | 82.1 (4) | C26—N6—Fe2 | 115.5 (9) |
O1—W1—O32 | 101.2 (4) | C30—N6—Fe2 | 126.8 (11) |
O1—W1—O33 | 98.6 (4) | C31—N7—C35 | 117.3 (12) |
O32—W1—O33 | 93.2 (3) | C31—N7—Fe3 | 126.8 (9) |
O1—W1—O27 | 102.0 (4) | C35—N7—Fe3 | 115.6 (9) |
O32—W1—O27 | 85.3 (3) | C40—N8—C36 | 118.0 (11) |
O33—W1—O27 | 159.3 (3) | C40—N8—Fe3 | 126.6 (9) |
O1—W1—O18 | 98.3 (4) | C36—N8—Fe3 | 115.4 (9) |
O32—W1—O18 | 159.8 (3) | C41—N9—C45 | 118.8 (12) |
O33—W1—O18 | 88.8 (3) | C41—N9—Fe3 | 129.1 (9) |
O27—W1—O18 | 85.8 (3) | C45—N9—Fe3 | 111.4 (9) |
O1—W1—O40 | 168.0 (4) | C46—N10—C50 | 119.3 (12) |
O32—W1—O40 | 88.2 (3) | C46—N10—Fe3 | 113.4 (10) |
O33—W1—O40 | 73.4 (3) | C50—N10—Fe3 | 126.7 (9) |
O27—W1—O40 | 85.9 (3) | C51—N11—C55 | 117.4 (13) |
O18—W1—O40 | 73.1 (3) | C51—N11—Fe3 | 128.2 (10) |
O2—W2—O18 | 99.4 (4) | C55—N11—Fe3 | 114.4 (11) |
O2—W2—O23 | 99.8 (4) | C60—N12—C56 | 118.5 (13) |
O18—W2—O23 | 90.8 (3) | C60—N12—Fe3 | 129.2 (10) |
O2—W2—O24 | 99.8 (4) | C56—N12—Fe3 | 112.3 (11) |
O18—W2—O24 | 90.2 (3) | N1—C1—C2 | 122.7 (15) |
O23—W2—O24 | 160.0 (3) | N1—C1—H1A | 118.7 |
O2—W2—O22 | 102.0 (4) | C2—C1—H1A | 118.7 |
O18—W2—O22 | 158.6 (4) | C3—C2—C1 | 117.6 (16) |
O23—W2—O22 | 84.3 (3) | C3—C2—H2A | 121.2 |
O24—W2—O22 | 87.5 (3) | C1—C2—H2A | 121.2 |
O2—W2—O40 | 170.0 (4) | C2—C3—C4 | 121.0 (14) |
O18—W2—O40 | 73.8 (3) | C2—C3—H3A | 119.5 |
O23—W2—O40 | 87.8 (3) | C4—C3—H3A | 119.5 |
O24—W2—O40 | 73.3 (3) | C5—C4—C3 | 119.1 (15) |
O22—W2—O40 | 85.2 (3) | C5—C4—H4A | 120.5 |
O3—W3—O34 | 103.9 (4) | C3—C4—H4A | 120.5 |
O3—W3—O24 | 97.8 (4) | C4—C5—N1 | 119.5 (14) |
O34—W3—O24 | 92.4 (4) | C4—C5—C6 | 125.9 (14) |
O3—W3—O35 | 103.0 (4) | N1—C5—C6 | 114.6 (11) |
O34—W3—O35 | 86.0 (4) | N2—C6—C7 | 122.9 (13) |
O24—W3—O35 | 159.0 (3) | N2—C6—C5 | 113.7 (12) |
O3—W3—O33 | 97.0 (4) | C7—C6—C5 | 123.4 (12) |
O34—W3—O33 | 158.8 (3) | C6—C7—C8 | 119.2 (13) |
O24—W3—O33 | 88.0 (3) | C6—C7—H7A | 120.4 |
O35—W3—O33 | 86.1 (3) | C8—C7—H7A | 120.4 |
O3—W3—O40 | 166.4 (4) | C9—C8—C7 | 118.2 (13) |
O34—W3—O40 | 87.5 (3) | C9—C8—H8A | 120.9 |
O24—W3—O40 | 73.9 (3) | C7—C8—H8A | 120.9 |
O35—W3—O40 | 85.1 (3) | C10—C9—C8 | 119.2 (13) |
O33—W3—O40 | 72.3 (3) | C10—C9—H9A | 120.4 |
O4—W4—O20 | 102.0 (3) | C8—C9—H9A | 120.4 |
O4—W4—O26 | 98.5 (4) | N2—C10—C9 | 124.7 (12) |
O20—W4—O26 | 91.6 (4) | N2—C10—H10A | 117.7 |
O4—W4—O23 | 101.0 (4) | C9—C10—H10A | 117.7 |
O20—W4—O23 | 85.9 (3) | N3—C11—C12 | 124.7 (13) |
O26—W4—O23 | 160.4 (3) | N3—C11—H11A | 117.7 |
O4—W4—O29 | 98.0 (3) | C12—C11—H11A | 117.7 |
O20—W4—O29 | 159.7 (3) | C11—C12—C13 | 114.5 (15) |
O26—W4—O29 | 88.9 (3) | C11—C12—H12A | 122.8 |
O23—W4—O29 | 87.0 (3) | C13—C12—H12A | 122.8 |
O4—W4—O38 | 168.3 (3) | C14—C13—C12 | 122.7 (16) |
O20—W4—O38 | 87.4 (3) | C14—C13—H13A | 118.6 |
O26—W4—O38 | 74.1 (3) | C12—C13—H13A | 118.6 |
O23—W4—O38 | 86.4 (3) | C13—C14—C15 | 119.3 (14) |
O29—W4—O38 | 73.2 (3) | C13—C14—H14A | 120.4 |
O5—W5—O27 | 101.5 (4) | C15—C14—H14A | 120.4 |
O5—W5—O31 | 104.1 (3) | N3—C15—C14 | 121.7 (12) |
O27—W5—O31 | 85.9 (3) | N3—C15—C16 | 112.5 (11) |
O5—W5—O29 | 96.9 (3) | C14—C15—C16 | 125.8 (12) |
O27—W5—O29 | 91.0 (3) | N4—C16—C17 | 122.7 (13) |
O31—W5—O29 | 158.9 (3) | N4—C16—C15 | 115.9 (11) |
O5—W5—O13 | 99.1 (4) | C17—C16—C15 | 121.4 (13) |
O27—W5—O13 | 159.2 (3) | C18—C17—C16 | 115.8 (14) |
O31—W5—O13 | 86.4 (4) | C18—C17—H17A | 122.1 |
O29—W5—O13 | 89.3 (4) | C16—C17—H17A | 122.1 |
O5—W5—O38 | 167.7 (3) | C19—C18—C17 | 120.0 (13) |
O27—W5—O38 | 87.0 (3) | C19—C18—H18A | 120.0 |
O31—W5—O38 | 85.1 (3) | C17—C18—H18A | 120.0 |
O29—W5—O38 | 73.9 (3) | C20—C19—C18 | 118.5 (14) |
O13—W5—O38 | 73.1 (3) | C20—C19—H19A | 120.7 |
O6—W6—O36 | 104.0 (4) | C18—C19—H19A | 120.7 |
O6—W6—O13 | 100.5 (4) | C19—C20—N4 | 124.6 (14) |
O36—W6—O13 | 92.2 (3) | C19—C20—H20A | 117.7 |
O6—W6—O16 | 100.9 (4) | N4—C20—H20A | 117.7 |
O36—W6—O16 | 85.2 (3) | N5—C21—C22 | 123.3 (14) |
O13—W6—O16 | 158.4 (4) | N5—C21—H21A | 118.3 |
O6—W6—O26 | 97.9 (4) | C22—C21—H21A | 118.3 |
O36—W6—O26 | 157.5 (4) | C21—C22—C23 | 118.3 (14) |
O13—W6—O26 | 89.0 (4) | C21—C22—H22A | 120.9 |
O16—W6—O26 | 85.5 (3) | C23—C22—H22A | 120.9 |
O6—W6—O38 | 168.7 (4) | C24—C23—C22 | 119.4 (16) |
O36—W6—O38 | 86.2 (3) | C24—C23—H23A | 120.3 |
O13—W6—O38 | 73.8 (3) | C22—C23—H23A | 120.3 |
O16—W6—O38 | 84.7 (3) | C23—C24—C25 | 119.6 (14) |
O26—W6—O38 | 72.5 (3) | C23—C24—H24A | 120.2 |
O7—W7—O19 | 100.0 (4) | C25—C24—H24A | 120.2 |
O7—W7—O31 | 101.6 (3) | N5—C25—C24 | 121.5 (12) |
O19—W7—O31 | 92.0 (3) | N5—C25—C26 | 113.8 (12) |
O7—W7—O21 | 98.4 (3) | C24—C25—C26 | 124.7 (13) |
O19—W7—O21 | 90.6 (4) | N6—C26—C27 | 123.2 (13) |
O31—W7—O21 | 159.1 (3) | N6—C26—C25 | 113.5 (12) |
O7—W7—O32 | 100.4 (4) | C27—C26—C25 | 123.2 (14) |
O19—W7—O32 | 159.6 (3) | C28—C27—C26 | 119.3 (16) |
O31—W7—O32 | 84.8 (3) | C28—C27—H27A | 120.3 |
O21—W7—O32 | 85.5 (3) | C26—C27—H27A | 120.3 |
O7—W7—O39 | 169.8 (3) | C29—C28—C27 | 117.4 (16) |
O19—W7—O39 | 74.0 (3) | C29—C28—H28A | 121.3 |
O31—W7—O39 | 87.0 (3) | C27—C28—H28A | 121.3 |
O21—W7—O39 | 73.8 (3) | C28—C29—C30 | 122.9 (16) |
O32—W7—O39 | 85.7 (3) | C28—C29—H29A | 118.6 |
O8—W8—O25 | 101.5 (4) | C30—C29—H29A | 118.6 |
O8—W8—O14 | 101.6 (4) | N6—C30—C29 | 119.9 (16) |
O25—W8—O14 | 92.0 (3) | N6—C30—H30A | 120.0 |
O8—W8—O36 | 101.4 (4) | C29—C30—H30A | 120.0 |
O25—W8—O36 | 84.9 (3) | N7—C31—C32 | 123.2 (14) |
O14—W8—O36 | 156.9 (4) | N7—C31—H31A | 118.4 |
O8—W8—O19 | 99.3 (4) | C32—C31—H31A | 118.4 |
O25—W8—O19 | 158.5 (4) | C31—C32—C33 | 117.6 (15) |
O14—W8—O19 | 89.1 (3) | C31—C32—H32A | 121.2 |
O36—W8—O19 | 85.7 (3) | C33—C32—H32A | 121.2 |
O8—W8—O39 | 169.9 (3) | C34—C33—C32 | 120.6 (15) |
O25—W8—O39 | 87.4 (3) | C34—C33—H33A | 119.7 |
O14—W8—O39 | 72.8 (3) | C32—C33—H33A | 119.7 |
O36—W8—O39 | 84.2 (3) | C33—C34—C35 | 119.1 (14) |
O19—W8—O39 | 72.5 (3) | C33—C34—H34A | 120.5 |
O9—W9—O35 | 102.2 (4) | C35—C34—H34A | 120.5 |
O9—W9—O21 | 99.1 (4) | N7—C35—C34 | 122.0 (13) |
O35—W9—O21 | 91.6 (3) | N7—C35—C36 | 113.3 (12) |
O9—W9—O14 | 98.0 (4) | C34—C35—C36 | 124.6 (12) |
O35—W9—O14 | 159.1 (3) | N8—C36—C37 | 120.9 (14) |
O21—W9—O14 | 90.4 (3) | N8—C36—C35 | 114.1 (11) |
O9—W9—O17 | 101.3 (4) | C37—C36—C35 | 125.0 (13) |
O35—W9—O17 | 84.6 (4) | C38—C37—C36 | 120.2 (14) |
O21—W9—O17 | 159.5 (3) | C38—C37—H37A | 119.9 |
O14—W9—O17 | 86.3 (3) | C36—C37—H37A | 119.9 |
O9—W9—O39 | 168.3 (4) | C39—C38—C37 | 118.2 (14) |
O35—W9—O39 | 88.0 (3) | C39—C38—H38A | 120.9 |
O21—W9—O39 | 74.6 (3) | C37—C38—H38A | 120.9 |
O14—W9—O39 | 72.6 (3) | C38—C39—C40 | 120.8 (15) |
O17—W9—O39 | 85.2 (3) | C38—C39—H39A | 119.6 |
O10—W10—O22 | 101.6 (4) | C40—C39—H39A | 119.6 |
O10—W10—O15 | 100.4 (4) | N8—C40—C39 | 121.8 (14) |
O22—W10—O15 | 92.1 (4) | N8—C40—H40A | 119.1 |
O10—W10—O20 | 101.7 (4) | C39—C40—H40A | 119.1 |
O22—W10—O20 | 85.4 (3) | N9—C41—C42 | 122.9 (13) |
O15—W10—O20 | 157.9 (3) | N9—C41—H41A | 118.5 |
O10—W10—O30 | 99.1 (4) | C42—C41—H41A | 118.5 |
O22—W10—O30 | 158.8 (3) | C43—C42—C41 | 119.2 (14) |
O15—W10—O30 | 88.3 (4) | C43—C42—H42A | 120.4 |
O20—W10—O30 | 86.3 (3) | C41—C42—H42A | 120.4 |
O10—W10—O37 | 170.0 (4) | C44—C43—C42 | 118.9 (15) |
O22—W10—O37 | 86.6 (3) | C44—C43—H43A | 120.6 |
O15—W10—O37 | 73.5 (3) | C42—C43—H43A | 120.6 |
O20—W10—O37 | 84.4 (3) | C43—C44—C45 | 121.0 (14) |
O30—W10—O37 | 73.2 (3) | C43—C44—H44A | 119.5 |
O11—W11—O17 | 102.6 (4) | C45—C44—H44A | 119.5 |
O11—W11—O28 | 98.8 (5) | N9—C45—C44 | 118.9 (13) |
O17—W11—O28 | 93.7 (4) | N9—C45—C46 | 116.3 (11) |
O11—W11—O15 | 97.0 (4) | C44—C45—C46 | 124.8 (13) |
O17—W11—O15 | 159.6 (3) | N10—C46—C45 | 115.6 (12) |
O28—W11—O15 | 88.9 (4) | N10—C46—C47 | 121.1 (13) |
O11—W11—O34 | 101.5 (4) | C45—C46—C47 | 123.1 (12) |
O17—W11—O34 | 83.9 (4) | C48—C47—C46 | 117.0 (13) |
O28—W11—O34 | 159.6 (3) | C48—C47—H47A | 121.5 |
O15—W11—O34 | 86.7 (4) | C46—C47—H47A | 121.5 |
O11—W11—O37 | 167.8 (4) | C49—C48—C47 | 119.3 (13) |
O17—W11—O37 | 88.0 (3) | C49—C48—H48A | 120.3 |
O28—W11—O37 | 74.3 (3) | C47—C48—H48A | 120.3 |
O15—W11—O37 | 73.2 (3) | C48—C49—C50 | 121.1 (16) |
O34—W11—O37 | 85.3 (3) | C48—C49—H49A | 119.5 |
O12—W12—O16 | 102.4 (4) | C50—C49—H49A | 119.5 |
O12—W12—O30 | 98.8 (4) | N10—C50—C49 | 122.1 (14) |
O16—W12—O30 | 93.2 (3) | N10—C50—H50A | 118.9 |
O12—W12—O25 | 100.8 (4) | C49—C50—H50A | 118.9 |
O16—W12—O25 | 85.9 (3) | C52—C51—N11 | 124.1 (16) |
O30—W12—O25 | 160.1 (4) | C52—C51—H51A | 118.0 |
O12—W12—O28 | 97.5 (4) | N11—C51—H51A | 118.0 |
O16—W12—O28 | 159.6 (4) | C51—C52—C53 | 118.2 (18) |
O30—W12—O28 | 88.3 (3) | C51—C52—H52A | 120.9 |
O25—W12—O28 | 85.9 (3) | C53—C52—H52A | 120.9 |
O12—W12—O37 | 167.9 (4) | C54—C53—C52 | 118.3 (16) |
O16—W12—O37 | 88.1 (3) | C54—C53—H53A | 120.9 |
O30—W12—O37 | 74.5 (3) | C52—C53—H53A | 120.9 |
O25—W12—O37 | 85.6 (3) | C53—C54—C55 | 121.9 (18) |
O28—W12—O37 | 72.6 (3) | C53—C54—H54A | 119.1 |
W5—O5—Na1 | 133.1 (5) | C55—C54—H54A | 119.1 |
W6—O13—W5 | 117.6 (4) | N11—C55—C54 | 120.0 (17) |
W8—O14—W9 | 118.3 (4) | N11—C55—C56 | 113.3 (13) |
W10—O15—W11 | 117.2 (4) | C54—C55—C56 | 126.6 (16) |
W12—O16—W6 | 152.3 (4) | N12—C56—C57 | 120.4 (16) |
W11—O17—W9 | 153.7 (5) | N12—C56—C55 | 116.9 (14) |
W2—O18—W1 | 116.7 (4) | C57—C56—C55 | 122.7 (16) |
W7—O19—W8 | 117.7 (4) | C58—C57—C56 | 119.7 (17) |
W4—O20—W10 | 152.3 (5) | C58—C57—H57A | 120.2 |
W9—O21—W7 | 116.5 (4) | C56—C57—H57A | 120.2 |
W10—O22—W2 | 153.8 (5) | C59—C58—C57 | 117.2 (17) |
W4—O23—W2 | 152.4 (4) | C59—C58—H58A | 121.4 |
W3—O24—W2 | 116.7 (4) | C57—C58—H58A | 121.4 |
W8—O25—W12 | 152.0 (5) | C60—C59—C58 | 119.5 (18) |
W4—O26—W6 | 116.9 (4) | C60—C59—H59A | 120.2 |
W5—O27—W1 | 152.3 (5) | C58—C59—H59A | 120.2 |
W11—O28—W12 | 116.8 (4) | N12—C60—C59 | 124.5 (16) |
W5—O29—W4 | 116.6 (4) | N12—C60—H60A | 117.8 |
W12—O30—W10 | 116.5 (4) | C59—C60—H60A | 117.8 |
W5—O31—W7 | 153.1 (5) | O3W—Na1—O4W | 166.0 (5) |
W1—O32—W7 | 152.5 (4) | O3W—Na1—O1W | 86.1 (5) |
W1—O33—W3 | 117.3 (4) | O4W—Na1—O1W | 89.8 (5) |
W3—O34—W11 | 152.6 (5) | O3W—Na1—O2W | 91.2 (5) |
W9—O35—W3 | 152.2 (5) | O4W—Na1—O2W | 102.3 (5) |
W6—O36—W8 | 154.0 (4) | O1W—Na1—O2W | 121.8 (5) |
Fe1—O37—W12 | 120.7 (4) | O3W—Na1—O5 | 93.3 (4) |
Fe1—O37—W11 | 121.2 (3) | O4W—Na1—O5 | 84.0 (5) |
W12—O37—W11 | 96.3 (3) | O1W—Na1—O5 | 151.8 (5) |
Fe1—O37—W10 | 120.9 (4) | O2W—Na1—O5 | 86.4 (4) |
W12—O37—W10 | 95.7 (3) |
D—H···A | D···A |
O2W···O6W | 2.80 (2) |
O2W···O4Wii | 2.753 (15) |
O3W···O33iiii | 2.972 (17) |
O6W···O18 | 2.923 (14) |
O7W···O9 | 3.07 (2) |
Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+1, −y+2, −z. |
Experimental details
Crystal data | |
Chemical formula | [Fe(C10H8N2)3]2[NaFeW12O40(H2O)4]·2H2O |
Mr | 4081.78 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 13.7572 (10), 17.8992 (13), 18.8730 (14) |
α, β, γ (°) | 88.043 (1), 72.829 (1), 75.128 (1) |
V (Å3) | 4287.1 (5) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 16.62 |
Crystal size (mm) | 0.11 × 0.11 × 0.09 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.262, 0.316 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22240, 14845, 10640 |
Rint | 0.036 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.044, 0.095, 0.98 |
No. of reflections | 14845 |
No. of parameters | 1216 |
No. of restraints | 50 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.89, −1.87 |
Computer programs: SMART (Bruker, 2001), SMART, SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001), SHELXTL.
Fe1—O37 | 1.811 (7) | Fe1—O38 | 1.812 (7) |
Fe1—O39 | 1.811 (7) | Fe1—O40 | 1.822 (8) |
O37—Fe1—O39 | 109.0 (4) | O37—Fe1—O40 | 109.3 (3) |
O37—Fe1—O38 | 109.7 (3) | O39—Fe1—O40 | 109.5 (4) |
O39—Fe1—O38 | 108.8 (3) | O38—Fe1—O40 | 110.5 (4) |
D—H···A | D···A |
O2W···O6W | 2.80 (2) |
O2W···O4Wii | 2.753 (15) |
O3W···O33iiii | 2.972 (17) |
O6W···O18 | 2.923 (14) |
O7W···O9 | 3.07 (2) |
Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+1, −y+2, −z. |
Polyoxometallates (POMs) have been studied extensively in the field of solid-state materials due to their varied potential applications in magnetism, medicine and catalysis (Xu et al., 2002; Judd et al., 2001; Hill, 2004), as well as the variety of their structures (Hagrman et al., 1999). Of the various POM structures, the most interesting is the Keggin family, which act as versatile inorganic building blocks for constructing more abundant organic–inorganic hybrid materials. However, most of the work reported to date has been on Keggin-type polyoxotungstates with main group 3 A atoms (B, Si, Ge, P, As) located in the central tetrahedral cavity of the Keggin cage (Zonnevijlle et al., 1982), while studies of the analogues with transition metal ions acting as heteratoms remain in their infancy. In particular, reports of Keggin-type polyanions with the transition metal FeIII ion as the central atom are rather scarce (Gómez-García et al., 1995; Weiner et al., 2005). We report here the synthesis and structure of the title compound, (I), which contains the Keggin polyanion.
The structure of (I) comprises a polyanionic [Na(H2O)4FeW12O40]4− framework, a pair of [Fe(2,2'-bipy)3]2+ complex cations and two uncoordinated water molecules, one of which is disordered (O5W/O7W) (Fig. 1). As shown in Fig. 2, the [Na(H2O)4FeW12O40]4− polyanion comprises the Keggin [FeIIIW12O40]5− skeleton, onto which a trigonal–bipyramidal [Na(H2O)4]+ cation is grafted via a bridging O atom. The Keggin [FeIIIW12O40]5− moiety is constructed from an FeO4 tetrahedron surrounded by 12 WO6 octahedra, present in four corner-sharing W3O13 groups, as found in other Keggin anions (Pope, 1983). In each [WO6] octahedron, the W—O bond lengths and O—W—O angles are in the ranges 1.690 (8)–2.231 (7) Å and 72.3 (3)–104.1 (3)°, respectively, which indicates substantial distortion from a regular octahedron.
According to the different coordination modes in the Keggin framework, the O atoms can be classified into three groups, namely terminal Ot atoms [W—O = 1.690 (8)–1.718 (8) Å], µ2-O atoms [W—O = 1.867 (8)–1.988 (8) Å] and µ4-O atoms [W—O = 2.213 (7)–2.231 (7) Å]. For the FeO4 tetrahedron, the Fe—O distances range from 1.811 (7) to 1.822 (8) Å with an average bond length of 1.814 (7) Å, while the O—Fe—O angles vary from 108.8 (3) to 110.5 (4)° (Table 1).
It is noteworthy that the asymmetric unit of (I) contains two complex [Fe(2,2'-bipy)3]2+ cations, which is confirmed by bond-valence sum calculations (Brese & O'Keeffe, 1991). These calculations show that the values for the calculated oxidation states of atoms Fe1, Fe2 and Fe3 are 3.222, 2.240 and 2.180, respectively, which is consistent with the formula of the title compound. In the course of the reaction, the 2,2'-bipyridine acts as an effective agent to reduce FeIII to FeII, and then the reduced FeII is coordinated by additional 2,2'-bipyridine residues to form the complex [Fe(2,2'-bipy)3]2+ cations, which self-assemble with [FeIIIW12O40]5− during crystal formation and separate out from the hydrothermal solution. A similar experimental phenomenon has been observed previously (Yang et al., 2002).
There are multiple O···O contacts suitable for O—H···O hydrogen bonding, with O···O distances in the range 2.80 (2)–3.07 (2) Å (Table 2). These interactions link the water molecules and the anionic cages into infinite one-dimensional chains that run parallel to the a axis (Fig. 3). In addition, the complex [Fe(2,2'-bipy)3]2+ cations fill the space between the polyanions and thereby contribute to the robustness of the crystal structure.