research communications
κO)manganese(II) decakis(dimethylformamide)-1κ5O,2κ5O-[μ-octadecatungstodiphosphato(V)-κO:κO′]dimanganate(II) dimethylformamide disolvate
of hexakis(dimethylformamide-aLaboratoire de Physico-Chimie des Materiaux, Faculty of Sciences, University of Monastir, Avenue de l'environnement, 5019 Monastir, Tunisia, and bUniversity of Sousse, High School of Sciences and Technology, Rue Lamine Abassi, 4011 Hammam Sousse, Tunisia
*Correspondence e-mail: fatma.dhif@gmail.com
The 3H7NO)6][{Mn(C3H7NO)5}2(μ-P2W18O62)]·2C3H7NO, reveals that the Wells–Dawson-type polyanion [P2W18O62]6−, through terminal O atoms from the belts, bridges two MnII octahedral complexes. In the complex anion [{Mn(dmf)5}2(μ-P2W18O62)]2−, located around a twofold rotation axis, the MnII ions are coordinated by five O atoms from dimethylformamide (dmf) ligands and to a terminal O atom from the [P2W18O62]6− polyanion. Another MnII ion, located on an inversion centre, is coordinated by six O atoms from the dmf ligands and forms the [Mn(dmf)6]2+ cation. The crystal components are connected through numerous weak C—H⋯O hydrogen bonds to construct a three-dimensional network.
of the title compound, [Mn(CCCDC reference: 1058770
1. Chemical context
Over the past few decades, polyoxidometalates (POMs) have been considered to be interesting building blocks for the construction of organic–inorganic hybrid materials because of their nanosize, abundant topologies, controllable shapes and high negative charges (Dolbecq et al., 2010). As a result of their unique redox, catalytic, photochemical and magnetic properties, organic–inorganic hybrid POM–based materials have captured considerable attention and are applied widely in many fields such as material science, catalysis and medicine (Niu et al., 2004; Ben Khelifa et al., 2015). Herein, we report the synthesis, and supramolecular architecture of the title compound, (1).
2. Structural commentary
The 1) consists of one half of the dinuclear complex anion [{Mn(dmf)5}2{μ2-(α-P2W18O62)}]2−, one half of the complex cation [Mn(dmf)6]2+ and one dmf solvent molecule. The [{Mn(dmf)5}2{μ2-(α-P2W18O62)}]2− anion, with the Wells–Dawson-type polyanion [P2W18O62]6− acting as a bridging ligand between the two MnII atoms, is located about a twofold symmetry axis (Fig. 1). The Mn1 ion within this anion is coordinated by five dmf molecules through O atoms and by a terminal O atom from the belt of the Wells–Dawson-type polyanion. The coordination sphere of the Mn1 ion features a trigonal distortion with three shorter [2.137 (6), 2.143 (6) and 2.153 (6) Å] and three longer [2.163 (5), 2.173 (6) and 2.205 (5) Å] Mn1—O bonds. Another MnII atom in this structure, Mn2, is located on an inversion centre and is octahedrally coordinated by six dmf molecules with the formation of the complex cation [Mn(dmf)6]2+ shown in Fig. 2. The Mn2 octahedron is characterized by a rhombic distortion with the following bond length values: 2.214 (9), 2.175 (7) and 2.134 (7) Å. The O—Mn—O bond angles in the complex ions Mn1 and Mn2 vary from 82.9 (2) to 100.0 (2)° and from 84.2 (3) to 90.6 (3)°, respectively, and from 169.7 (2) to 174.5 (3)° for bond angles with O atoms in trans positions in the Mn1 complex. These bond length and angle values show that the octahedral coordination geometry of the MnII ions is distorted and these values are in good agreement with literature data (Niu et al., 2004).
of (The two central P atoms of the POM are tetrahedrally coordinated by four bridging O atoms. The corresponding P1—O bond lengths vary from 1.528 (5) to 1.577 (5) Å (mean value 1.545 Å) and the O—P1—O bond angles are in the range 106.5 (2) to 112.7 (2)°. The W—O distances vary over a wide range: 1.700 (5)–2.384 (4) Å and the bond angles O—W—O are in the range 71.6 (2) to 103.8 (2)°. These bond lengths and angles are consistent with those given in the literature for the α-isomer of the Wells–Dawson-type polyanion (Dhifallah et al., 2016).
3. Supramolecular features
The crystal packing of the title compound is illustrated in Fig. 3. In addition to the electrostatic interactions between the ions, the structure is stabilized by numerous weak C—H⋯O hydrogen bonds (Table 1) that organize all the structure components into a three-dimensional framework.
4. Synthesis and crystallization
The title compound was prepared at room temperature by dissolving successively the potassium salt K6[α-P2W18O62]·11H2O (0.606g, 0.125 mmol), synthesized by a literature method (Mbomekalle et al., 2004) and manganese(II) chloride (MnCl2·4H2O; 0.099 g, 0.5 mmol) in dmf (25 mL) under stirring. The clear solution obtained was allowed to stand for at least one night until it took a stable color indicating that the kinetics of the reaction were complete. Yellow crystals of (1) suitable for X-ray were obtained by diffusion of ethanol into the dmf solution.
5. FT–IR Spectroscopy
The IR spectrum of (1) (Fig. 4) exhibits characteristic bands of metal–oxygen stretching and deformation modes of the POM, in the region 1100–400 cm−1. The vibration bands, attributed to ν(P—Oa), ν(W—Ot), ν(W—Oe) and ν(W—Oc), appear respectively at 1090, 959, 911 and 782 cm−1 (Jin et al., 2007; Dong et al., 2008; Cao et al., 2009). The region 1700–1110 cm−1 corresponds to DMF molecule vibrations and bands observed at 1645, 1498, 1435, 1418, 1378, 1251 and 1109 cm−1 are respectively attributed to ν(CO), δas(CH3), δ(CH), δs(CH3), νas(C′N) and r(CH3) (Durgaprasad et al., 1971).
6. Refinement
Crystal data, data collection and structure . All H atoms were refined using a riding model with C—H = 0.93–0.96 Å and Uiso(H) = 1.5Ueq(C) or 1.2Ueq(C). Restraints (DELU and SIMU) in SHELXL2014 (Sheldrick, 2015) were used in order to maintain a reasonable geometry and atomic displacement parameters for one DMF molecule.
details are summarized in Table 2
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Supporting information
CCDC reference: 1058770
https://doi.org/10.1107/S2056989016007842/gk2660sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989016007842/gk2660Isup3.hkl
Data collection: CrysAlis PRO (Agilent, 2014); cell
CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRO (Agilent, 2014); program(s) used to solve structure: SIR2004 (Burla et al., 2005); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 1997); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).[Mn(C3H7NO)6][Mn2(P2W18O62)(C3H7NO)10]·2C3H7NO | F(000) = 10612 |
Mr = 5843.78 | Dx = 3.155 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 26.9702 (5) Å | Cell parameters from 36494 reflections |
b = 14.3845 (2) Å | θ = 3.6–29.1° |
c = 34.1762 (7) Å | µ = 17.18 mm−1 |
β = 111.896 (2)° | T = 203 K |
V = 12302.3 (4) Å3 | Cuboid, yellow |
Z = 4 | 0.24 × 0.18 × 0.07 mm |
Agilent SuperNova Dual Source diffractometer with an Atlas detector | 14565 independent reflections |
Radiation source: SuperNova (Mo) X-ray Source | 12616 reflections with I > 2σ(I) |
Detector resolution: 5.3048 pixels mm-1 | Rint = 0.076 |
CCD plate, AtlasS2 scans | θmax = 27.9°, θmin = 3.3° |
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014) | h = −35→35 |
Tmin = 0.133, Tmax = 1.000 | k = −18→18 |
110388 measured reflections | l = −44→44 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0162P)2 + 165.2372P] where P = (Fo2 + 2Fc2)/3 |
14565 reflections | (Δ/σ)max = 0.002 |
804 parameters | Δρmax = 2.07 e Å−3 |
7 restraints | Δρmin = −2.08 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
W1 | 0.37578 (2) | 0.25005 (2) | 0.09160 (2) | 0.01620 (6) | |
W2 | 0.50414 (2) | 0.24682 (2) | 0.09871 (2) | 0.01727 (7) | |
W3 | 0.43807 (2) | 0.04441 (2) | 0.09488 (2) | 0.01678 (7) | |
W4 | 0.40732 (2) | −0.02952 (2) | 0.18763 (2) | 0.01452 (6) | |
W5 | 0.34442 (2) | 0.17355 (2) | 0.18329 (2) | 0.01371 (6) | |
W6 | 0.41338 (2) | 0.39654 (2) | 0.18805 (2) | 0.01413 (6) | |
W7 | 0.54022 (2) | 0.39688 (2) | 0.19367 (2) | 0.01493 (6) | |
W8 | 0.61092 (2) | 0.17568 (2) | 0.19893 (2) | 0.01534 (6) | |
W9 | 0.54669 (2) | −0.02755 (2) | 0.19409 (2) | 0.01516 (6) | |
P1 | 0.47540 (6) | 0.18140 (11) | 0.18750 (5) | 0.0083 (3) | |
Mn2 | 0.2500 | −0.2500 | 0.0000 | 0.0409 (5) | |
Mn1 | 0.19102 (4) | 0.22616 (8) | 0.14462 (3) | 0.0211 (2) | |
O1 | 0.43086 (19) | 0.2875 (3) | 0.07249 (14) | 0.0173 (10) | |
O2 | 0.48124 (18) | 0.1261 (3) | 0.07564 (14) | 0.0163 (10) | |
O3 | 0.38000 (18) | 0.1277 (3) | 0.06966 (14) | 0.0185 (11) | |
O4 | 0.39411 (18) | 0.3486 (3) | 0.13100 (14) | 0.0146 (10) | |
O5 | 0.51474 (18) | 0.3470 (3) | 0.13758 (14) | 0.0169 (10) | |
O6 | 0.56452 (19) | 0.1928 (3) | 0.14063 (15) | 0.0182 (10) | |
O7 | 0.50353 (19) | 0.0014 (3) | 0.13637 (15) | 0.0189 (11) | |
O8 | 0.40523 (18) | 0.0009 (3) | 0.13129 (14) | 0.0164 (10) | |
O9 | 0.34566 (18) | 0.1923 (3) | 0.12803 (14) | 0.0163 (10) | |
O10 | 0.4228 (2) | −0.0405 (3) | 0.05695 (15) | 0.0238 (11) | |
O11 | 0.3207 (2) | 0.2898 (3) | 0.05154 (15) | 0.0235 (11) | |
O12 | 0.5302 (2) | 0.2890 (4) | 0.06374 (16) | 0.0247 (12) | |
O13 | 0.45612 (18) | 0.1809 (3) | 0.13790 (14) | 0.0147 (10) | |
O14 | 0.43198 (18) | 0.1303 (3) | 0.19850 (13) | 0.0130 (9) | |
O15 | 0.52899 (17) | 0.1298 (3) | 0.20425 (14) | 0.0135 (10) | |
O16 | 0.48044 (17) | 0.2830 (3) | 0.20144 (13) | 0.0132 (9) | |
O17 | 0.47296 (19) | 0.4582 (3) | 0.18215 (14) | 0.0189 (11) | |
O18 | 0.59021 (19) | 0.2974 (3) | 0.20752 (15) | 0.0184 (10) | |
O19 | 0.60400 (18) | 0.0442 (3) | 0.18997 (15) | 0.0163 (10) | |
O20 | 0.48063 (18) | −0.0510 (3) | 0.20113 (14) | 0.0154 (10) | |
O21 | 0.34336 (17) | 0.0432 (3) | 0.17492 (14) | 0.0155 (10) | |
O22 | 0.37225 (18) | 0.2954 (3) | 0.19530 (14) | 0.0149 (10) | |
O23 | 0.36766 (19) | 0.4849 (3) | 0.17599 (15) | 0.0195 (11) | |
O24 | 0.44329 (19) | 0.4122 (3) | 0.24722 (14) | 0.0180 (10) | |
O25 | 0.5769 (2) | 0.4870 (3) | 0.18580 (15) | 0.0227 (11) | |
O26 | 0.6705 (2) | 0.1949 (3) | 0.19370 (15) | 0.0233 (11) | |
O27 | 0.5661 (2) | −0.1362 (3) | 0.18549 (16) | 0.0248 (12) | |
O28 | 0.58041 (19) | −0.0248 (3) | 0.25425 (15) | 0.0194 (11) | |
O29 | 0.3805 (2) | −0.1384 (3) | 0.17621 (16) | 0.0237 (11) | |
O30 | 0.36338 (18) | 0.1547 (3) | 0.24209 (15) | 0.0171 (10) | |
O31 | 0.27687 (18) | 0.1915 (3) | 0.17009 (15) | 0.0196 (11) | |
O32 | 0.1799 (2) | 0.1920 (4) | 0.20183 (17) | 0.0331 (13) | |
C1 | 0.1360 (3) | 0.1824 (5) | 0.2056 (3) | 0.0267 (17) | |
H1 | 0.1054 | 0.1777 | 0.1813 | 0.032* | |
N1 | 0.1307 (3) | 0.1788 (4) | 0.2425 (2) | 0.0292 (15) | |
C2 | 0.1757 (4) | 0.1879 (8) | 0.2817 (3) | 0.051 (3) | |
H2A | 0.2080 | 0.1913 | 0.2761 | 0.077* | |
H2B | 0.1773 | 0.1349 | 0.2992 | 0.077* | |
H2C | 0.1719 | 0.2434 | 0.2959 | 0.077* | |
C3 | 0.0781 (4) | 0.1705 (6) | 0.2448 (3) | 0.039 (2) | |
H3A | 0.0516 | 0.1654 | 0.2168 | 0.059* | |
H3B | 0.0710 | 0.2245 | 0.2584 | 0.059* | |
H3C | 0.0770 | 0.1161 | 0.2607 | 0.059* | |
O33 | 0.1758 (3) | 0.0825 (4) | 0.12398 (19) | 0.0391 (15) | |
C4 | 0.2072 (4) | 0.0196 (6) | 0.1289 (3) | 0.042 (2) | |
H4 | 0.2430 | 0.0358 | 0.1368 | 0.051* | |
N2 | 0.1956 (3) | −0.0703 (5) | 0.1241 (2) | 0.043 (2) | |
C5 | 0.2378 (4) | −0.1366 (7) | 0.1287 (4) | 0.061 (3) | |
H5A | 0.2712 | −0.1043 | 0.1358 | 0.091* | |
H5B | 0.2300 | −0.1697 | 0.1027 | 0.091* | |
H5C | 0.2403 | −0.1798 | 0.1508 | 0.091* | |
C6 | 0.1425 (5) | −0.1066 (9) | 0.1137 (5) | 0.083 (4) | |
H6A | 0.1202 | −0.0598 | 0.1187 | 0.124* | |
H6B | 0.1438 | −0.1599 | 0.1309 | 0.124* | |
H6C | 0.1282 | −0.1244 | 0.0845 | 0.124* | |
O34 | 0.1075 (2) | 0.2531 (5) | 0.1134 (2) | 0.0490 (18) | |
C7 | 0.0757 (4) | 0.3129 (8) | 0.0919 (3) | 0.047 (3) | |
H7 | 0.0626 | 0.3560 | 0.1060 | 0.057* | |
N3 | 0.0595 (3) | 0.3190 (6) | 0.0512 (2) | 0.046 (2) | |
C8 | 0.0175 (6) | 0.3811 (11) | 0.0260 (4) | 0.102 (6) | |
H8A | 0.0122 | 0.3740 | −0.0032 | 0.153* | |
H8B | −0.0150 | 0.3665 | 0.0300 | 0.153* | |
H8C | 0.0276 | 0.4442 | 0.0345 | 0.153* | |
C9 | 0.0798 (5) | 0.2567 (9) | 0.0271 (3) | 0.070 (4) | |
H9A | 0.0634 | 0.2715 | −0.0024 | 0.105* | |
H9B | 0.1179 | 0.2640 | 0.0361 | 0.105* | |
H9C | 0.0717 | 0.1936 | 0.0316 | 0.105* | |
O35 | 0.2046 (2) | 0.2857 (4) | 0.09136 (17) | 0.0309 (13) | |
C10 | 0.2390 (3) | 0.3475 (5) | 0.0961 (2) | 0.0229 (16) | |
H10 | 0.2683 | 0.3492 | 0.1214 | 0.027* | |
N4 | 0.2362 (3) | 0.4106 (4) | 0.0672 (2) | 0.0265 (15) | |
C11 | 0.1928 (4) | 0.4060 (7) | 0.0266 (3) | 0.047 (3) | |
H11A | 0.1972 | 0.3522 | 0.0116 | 0.071* | |
H11B | 0.1930 | 0.4609 | 0.0107 | 0.071* | |
H11C | 0.1595 | 0.4018 | 0.0305 | 0.071* | |
C12 | 0.2799 (3) | 0.4762 (5) | 0.0728 (3) | 0.0312 (19) | |
H12A | 0.3031 | 0.4782 | 0.1020 | 0.047* | |
H12B | 0.2655 | 0.5370 | 0.0639 | 0.047* | |
H12C | 0.2999 | 0.4564 | 0.0562 | 0.047* | |
O36 | 0.2124 (3) | 0.3636 (4) | 0.1703 (2) | 0.0421 (16) | |
C13 | 0.2043 (3) | 0.4050 (6) | 0.1989 (3) | 0.036 (2) | |
H13 | 0.1689 | 0.4132 | 0.1960 | 0.043* | |
N5 | 0.2409 (3) | 0.4385 (5) | 0.2327 (2) | 0.0294 (15) | |
C14 | 0.2278 (4) | 0.4882 (8) | 0.2646 (3) | 0.056 (3) | |
H14A | 0.2602 | 0.5071 | 0.2870 | 0.084* | |
H14B | 0.2069 | 0.5421 | 0.2522 | 0.084* | |
H14C | 0.2078 | 0.4483 | 0.2758 | 0.084* | |
C15 | 0.2964 (4) | 0.4234 (11) | 0.2408 (4) | 0.092 (5) | |
H15A | 0.3123 | 0.3885 | 0.2663 | 0.138* | |
H15B | 0.3142 | 0.4823 | 0.2436 | 0.138* | |
H15C | 0.2999 | 0.3895 | 0.2177 | 0.138* | |
O37 | 0.3191 (3) | −0.2804 (5) | 0.0546 (2) | 0.058 (2) | |
C16 | 0.3642 (4) | −0.2458 (7) | 0.0716 (3) | 0.045 (2) | |
H16 | 0.3728 | −0.1956 | 0.0581 | 0.054* | |
N6 | 0.4007 (3) | −0.2743 (5) | 0.1069 (2) | 0.0357 (17) | |
C17 | 0.4532 (4) | −0.2344 (7) | 0.1243 (3) | 0.053 (3) | |
H17A | 0.4794 | −0.2818 | 0.1272 | 0.080* | |
H17B | 0.4589 | −0.2082 | 0.1515 | 0.080* | |
H17C | 0.4565 | −0.1865 | 0.1058 | 0.080* | |
C18 | 0.3876 (5) | −0.3450 (8) | 0.1311 (4) | 0.070 (4) | |
H18A | 0.3500 | −0.3577 | 0.1190 | 0.106* | |
H18B | 0.3970 | −0.3240 | 0.1596 | 0.106* | |
H18C | 0.4071 | −0.4007 | 0.1309 | 0.106* | |
O38 | 0.2501 (3) | −0.1093 (5) | 0.0233 (2) | 0.058 (2) | |
C19 | 0.2095 (5) | −0.0671 (8) | 0.0183 (3) | 0.054 (3) | |
H19 | 0.1771 | −0.0971 | 0.0045 | 0.065* | |
N7 | 0.2083 (4) | 0.0211 (5) | 0.0315 (2) | 0.044 (2) | |
C20 | 0.2519 (6) | 0.0778 (11) | 0.0525 (5) | 0.104 (6) | |
H20A | 0.2840 | 0.0413 | 0.0617 | 0.156* | |
H20B | 0.2474 | 0.1056 | 0.0765 | 0.156* | |
H20C | 0.2543 | 0.1257 | 0.0337 | 0.156* | |
C21 | 0.1563 (6) | 0.0636 (9) | 0.0208 (4) | 0.079 (4) | |
H21A | 0.1290 | 0.0182 | 0.0079 | 0.119* | |
H21B | 0.1526 | 0.1140 | 0.0016 | 0.119* | |
H21C | 0.1527 | 0.0868 | 0.0460 | 0.119* | |
O39 | 0.2057 (3) | −0.2996 (5) | 0.0390 (3) | 0.067 (2) | |
C22 | 0.1679 (6) | −0.3436 (8) | 0.0404 (4) | 0.069 (3) | |
H22 | 0.1387 | −0.3512 | 0.0153 | 0.083* | |
N8 | 0.1648 (5) | −0.3803 (7) | 0.0733 (3) | 0.067 (3) | |
C23 | 0.1136 (8) | −0.4306 (18) | 0.0683 (8) | 0.184 (11) | |
H23A | 0.1160 | −0.4551 | 0.0951 | 0.276* | |
H23B | 0.0842 | −0.3879 | 0.0581 | 0.276* | |
H23C | 0.1081 | −0.4806 | 0.0485 | 0.276* | |
C24 | 0.2036 (7) | −0.3869 (10) | 0.1143 (4) | 0.096 (5) | |
H24A | 0.2367 | −0.3613 | 0.1148 | 0.144* | |
H24B | 0.2087 | −0.4510 | 0.1227 | 0.144* | |
H24C | 0.1918 | −0.3529 | 0.1334 | 0.144* | |
O40 | 0.4111 (6) | −0.3352 (9) | 0.0133 (4) | 0.136 (5) | |
C25 | 0.4542 (6) | −0.3711 (11) | 0.0229 (6) | 0.109 (6) | |
H25 | 0.4747 | −0.3531 | 0.0076 | 0.131* | |
N9 | 0.4758 (5) | −0.4331 (10) | 0.0530 (5) | 0.111 (5) | |
C26 | 0.4464 (9) | −0.4739 (11) | 0.0759 (5) | 0.125 (7) | |
H26A | 0.4150 | −0.4376 | 0.0717 | 0.188* | |
H26B | 0.4684 | −0.4754 | 0.1054 | 0.188* | |
H26C | 0.4362 | −0.5361 | 0.0660 | 0.188* | |
C27 | 0.5270 (9) | −0.4643 (16) | 0.0653 (11) | 0.27 (2) | |
H27A | 0.5304 | −0.5217 | 0.0804 | 0.410* | |
H27B | 0.5508 | −0.4189 | 0.0833 | 0.410* | |
H27C | 0.5359 | −0.4743 | 0.0409 | 0.410* |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.01490 (14) | 0.02190 (14) | 0.01007 (13) | 0.00222 (11) | 0.00265 (11) | 0.00061 (10) |
W2 | 0.01742 (15) | 0.02454 (15) | 0.01067 (13) | −0.00453 (12) | 0.00617 (11) | −0.00034 (11) |
W3 | 0.02004 (15) | 0.01751 (13) | 0.01187 (14) | −0.00120 (11) | 0.00488 (11) | −0.00361 (10) |
W4 | 0.01286 (14) | 0.01258 (13) | 0.01811 (14) | −0.00222 (10) | 0.00579 (11) | −0.00138 (10) |
W5 | 0.00908 (13) | 0.01626 (13) | 0.01540 (14) | 0.00011 (10) | 0.00411 (11) | 0.00085 (10) |
W6 | 0.01424 (14) | 0.01239 (13) | 0.01491 (14) | 0.00162 (10) | 0.00446 (11) | 0.00112 (10) |
W7 | 0.01552 (14) | 0.01431 (13) | 0.01575 (14) | −0.00319 (11) | 0.00675 (11) | 0.00008 (10) |
W8 | 0.01178 (14) | 0.02008 (14) | 0.01606 (14) | −0.00088 (11) | 0.00738 (11) | −0.00110 (10) |
W9 | 0.01322 (14) | 0.01455 (13) | 0.01807 (15) | 0.00186 (10) | 0.00625 (11) | −0.00268 (10) |
P1 | 0.0058 (8) | 0.0100 (7) | 0.0089 (8) | 0.0000 (6) | 0.0025 (6) | 0.0000 (6) |
Mn2 | 0.0532 (13) | 0.0319 (10) | 0.0293 (10) | 0.0081 (9) | 0.0059 (9) | 0.0001 (8) |
Mn1 | 0.0162 (6) | 0.0282 (6) | 0.0178 (6) | 0.0026 (5) | 0.0052 (4) | 0.0002 (4) |
O1 | 0.018 (3) | 0.024 (2) | 0.008 (2) | −0.002 (2) | 0.0035 (19) | 0.0029 (19) |
O2 | 0.018 (3) | 0.018 (2) | 0.016 (2) | 0.002 (2) | 0.009 (2) | −0.0013 (19) |
O3 | 0.012 (2) | 0.025 (3) | 0.012 (2) | −0.002 (2) | −0.0043 (19) | −0.0049 (19) |
O4 | 0.015 (2) | 0.016 (2) | 0.012 (2) | 0.0017 (19) | 0.0049 (19) | 0.0009 (18) |
O5 | 0.016 (2) | 0.022 (2) | 0.013 (2) | −0.002 (2) | 0.006 (2) | 0.0003 (19) |
O6 | 0.018 (3) | 0.022 (2) | 0.015 (2) | −0.001 (2) | 0.007 (2) | −0.0022 (19) |
O7 | 0.019 (3) | 0.020 (2) | 0.017 (3) | 0.003 (2) | 0.007 (2) | −0.0027 (19) |
O8 | 0.014 (2) | 0.020 (2) | 0.014 (2) | −0.0013 (19) | 0.0036 (19) | −0.0015 (19) |
O9 | 0.015 (2) | 0.020 (2) | 0.013 (2) | −0.0005 (19) | 0.0044 (19) | 0.0004 (19) |
O10 | 0.029 (3) | 0.023 (3) | 0.019 (3) | −0.003 (2) | 0.010 (2) | −0.009 (2) |
O11 | 0.019 (3) | 0.029 (3) | 0.018 (3) | 0.003 (2) | 0.002 (2) | 0.001 (2) |
O12 | 0.019 (3) | 0.036 (3) | 0.022 (3) | −0.006 (2) | 0.011 (2) | 0.002 (2) |
O13 | 0.015 (2) | 0.018 (2) | 0.012 (2) | −0.0001 (19) | 0.0053 (19) | −0.0004 (18) |
O14 | 0.017 (2) | 0.012 (2) | 0.010 (2) | 0.0009 (18) | 0.0064 (19) | −0.0024 (17) |
O15 | 0.013 (2) | 0.013 (2) | 0.013 (2) | −0.0034 (18) | 0.0029 (19) | −0.0026 (18) |
O16 | 0.014 (2) | 0.018 (2) | 0.008 (2) | 0.0017 (19) | 0.0044 (18) | 0.0029 (18) |
O17 | 0.024 (3) | 0.016 (2) | 0.015 (2) | −0.001 (2) | 0.005 (2) | 0.0035 (19) |
O18 | 0.020 (3) | 0.021 (2) | 0.016 (2) | −0.002 (2) | 0.009 (2) | 0.0021 (19) |
O19 | 0.009 (2) | 0.020 (2) | 0.022 (3) | 0.0038 (19) | 0.008 (2) | 0.0028 (19) |
O20 | 0.013 (2) | 0.016 (2) | 0.018 (2) | −0.0002 (19) | 0.0061 (19) | 0.0010 (19) |
O21 | 0.009 (2) | 0.015 (2) | 0.021 (3) | −0.0022 (18) | 0.0035 (19) | 0.0048 (19) |
O22 | 0.013 (2) | 0.017 (2) | 0.012 (2) | 0.0032 (19) | 0.0019 (19) | 0.0007 (18) |
O23 | 0.021 (3) | 0.019 (2) | 0.016 (3) | 0.004 (2) | 0.005 (2) | 0.0037 (19) |
O24 | 0.019 (3) | 0.016 (2) | 0.018 (3) | −0.001 (2) | 0.007 (2) | −0.0009 (19) |
O25 | 0.026 (3) | 0.022 (3) | 0.023 (3) | −0.008 (2) | 0.012 (2) | 0.001 (2) |
O26 | 0.021 (3) | 0.032 (3) | 0.019 (3) | −0.002 (2) | 0.009 (2) | −0.002 (2) |
O27 | 0.028 (3) | 0.022 (3) | 0.022 (3) | 0.007 (2) | 0.006 (2) | −0.006 (2) |
O28 | 0.017 (3) | 0.022 (3) | 0.019 (3) | −0.001 (2) | 0.006 (2) | −0.002 (2) |
O29 | 0.029 (3) | 0.017 (2) | 0.025 (3) | −0.007 (2) | 0.011 (2) | −0.005 (2) |
O30 | 0.013 (2) | 0.022 (2) | 0.019 (3) | −0.0005 (19) | 0.009 (2) | 0.0016 (19) |
O31 | 0.011 (2) | 0.025 (3) | 0.022 (3) | −0.001 (2) | 0.004 (2) | −0.001 (2) |
O32 | 0.028 (3) | 0.052 (4) | 0.021 (3) | 0.006 (3) | 0.012 (2) | 0.007 (3) |
C1 | 0.032 (5) | 0.023 (4) | 0.025 (4) | −0.001 (3) | 0.011 (4) | 0.001 (3) |
N1 | 0.037 (4) | 0.029 (4) | 0.022 (4) | 0.002 (3) | 0.012 (3) | 0.002 (3) |
C2 | 0.043 (6) | 0.090 (8) | 0.023 (5) | −0.001 (5) | 0.014 (4) | −0.008 (5) |
C3 | 0.044 (6) | 0.043 (5) | 0.042 (6) | −0.004 (4) | 0.028 (5) | 0.001 (4) |
O33 | 0.045 (4) | 0.032 (3) | 0.036 (4) | −0.003 (3) | 0.010 (3) | −0.004 (3) |
C4 | 0.043 (6) | 0.042 (5) | 0.033 (5) | −0.008 (5) | 0.004 (4) | 0.000 (4) |
N2 | 0.055 (5) | 0.029 (4) | 0.031 (4) | −0.010 (4) | −0.001 (4) | 0.000 (3) |
C5 | 0.057 (7) | 0.048 (6) | 0.068 (8) | −0.006 (5) | 0.013 (6) | −0.008 (6) |
C6 | 0.062 (8) | 0.079 (9) | 0.103 (11) | −0.028 (7) | 0.025 (8) | −0.020 (8) |
O34 | 0.021 (3) | 0.084 (5) | 0.040 (4) | 0.005 (3) | 0.010 (3) | 0.027 (4) |
C7 | 0.037 (6) | 0.074 (7) | 0.040 (6) | 0.013 (5) | 0.023 (5) | 0.005 (5) |
N3 | 0.028 (4) | 0.075 (6) | 0.032 (4) | 0.019 (4) | 0.008 (3) | 0.008 (4) |
C8 | 0.100 (11) | 0.145 (14) | 0.060 (9) | 0.082 (11) | 0.029 (8) | 0.041 (9) |
C9 | 0.053 (7) | 0.101 (10) | 0.047 (7) | −0.004 (7) | 0.008 (6) | −0.040 (7) |
O35 | 0.031 (3) | 0.038 (3) | 0.023 (3) | −0.006 (3) | 0.010 (2) | 0.004 (2) |
C10 | 0.024 (4) | 0.031 (4) | 0.011 (4) | 0.002 (3) | 0.004 (3) | 0.002 (3) |
N4 | 0.030 (4) | 0.029 (3) | 0.020 (3) | 0.006 (3) | 0.008 (3) | 0.003 (3) |
C11 | 0.043 (6) | 0.065 (7) | 0.025 (5) | −0.010 (5) | 0.002 (4) | 0.013 (4) |
C12 | 0.026 (4) | 0.028 (4) | 0.036 (5) | 0.000 (3) | 0.008 (4) | 0.005 (4) |
O36 | 0.056 (4) | 0.037 (3) | 0.044 (4) | −0.001 (3) | 0.030 (3) | −0.015 (3) |
C13 | 0.027 (5) | 0.039 (5) | 0.038 (5) | 0.007 (4) | 0.008 (4) | −0.011 (4) |
N5 | 0.022 (4) | 0.033 (4) | 0.033 (4) | 0.009 (3) | 0.010 (3) | −0.004 (3) |
C14 | 0.051 (7) | 0.079 (8) | 0.036 (6) | 0.020 (6) | 0.012 (5) | −0.015 (5) |
C15 | 0.028 (6) | 0.140 (13) | 0.097 (11) | 0.004 (7) | 0.012 (6) | −0.046 (10) |
O37 | 0.056 (5) | 0.059 (5) | 0.040 (4) | −0.004 (4) | −0.002 (4) | 0.003 (3) |
C16 | 0.053 (7) | 0.039 (5) | 0.044 (6) | 0.003 (5) | 0.020 (5) | 0.003 (4) |
N6 | 0.043 (5) | 0.029 (4) | 0.030 (4) | −0.008 (3) | 0.009 (3) | 0.004 (3) |
C17 | 0.038 (6) | 0.049 (6) | 0.065 (7) | −0.008 (5) | 0.012 (5) | −0.003 (5) |
C18 | 0.073 (8) | 0.065 (7) | 0.060 (8) | −0.021 (6) | 0.010 (6) | 0.031 (6) |
O38 | 0.076 (6) | 0.047 (4) | 0.051 (5) | 0.008 (4) | 0.024 (4) | −0.003 (3) |
C19 | 0.077 (8) | 0.053 (7) | 0.038 (6) | −0.006 (6) | 0.029 (6) | 0.002 (5) |
N7 | 0.072 (6) | 0.032 (4) | 0.036 (5) | 0.000 (4) | 0.030 (4) | −0.004 (3) |
C20 | 0.112 (12) | 0.141 (13) | 0.099 (11) | −0.079 (11) | 0.086 (10) | −0.065 (10) |
C21 | 0.099 (11) | 0.088 (10) | 0.052 (8) | 0.020 (8) | 0.031 (7) | 0.012 (7) |
O39 | 0.077 (6) | 0.051 (5) | 0.086 (6) | −0.010 (4) | 0.045 (5) | −0.021 (4) |
C22 | 0.081 (9) | 0.061 (7) | 0.071 (8) | 0.021 (6) | 0.035 (7) | 0.017 (6) |
N8 | 0.092 (8) | 0.076 (7) | 0.053 (6) | 0.032 (6) | 0.049 (6) | 0.018 (5) |
C23 | 0.098 (15) | 0.28 (3) | 0.22 (3) | 0.007 (18) | 0.110 (17) | −0.01 (2) |
C24 | 0.162 (16) | 0.078 (9) | 0.054 (9) | 0.028 (10) | 0.048 (10) | −0.009 (7) |
O40 | 0.129 (11) | 0.134 (10) | 0.145 (11) | 0.037 (9) | 0.051 (9) | 0.054 (9) |
C25 | 0.046 (8) | 0.098 (11) | 0.190 (19) | 0.031 (8) | 0.051 (10) | 0.063 (12) |
N9 | 0.083 (10) | 0.097 (10) | 0.136 (13) | 0.024 (8) | 0.021 (9) | 0.022 (9) |
C26 | 0.22 (2) | 0.088 (11) | 0.069 (10) | 0.044 (13) | 0.060 (12) | 0.050 (9) |
C27 | 0.096 (17) | 0.14 (2) | 0.55 (6) | 0.046 (15) | 0.08 (3) | 0.14 (3) |
W1—O11 | 1.700 (5) | C4—H4 | 0.9300 |
W1—O4 | 1.890 (4) | N2—C6 | 1.439 (13) |
W1—O1 | 1.910 (5) | N2—C5 | 1.448 (13) |
W1—O9 | 1.912 (5) | C5—H5A | 0.9600 |
W1—O3 | 1.933 (5) | C5—H5B | 0.9600 |
W1—O13 | 2.373 (4) | C5—H5C | 0.9600 |
W2—O12 | 1.708 (5) | C6—H6A | 0.9600 |
W2—O6 | 1.889 (5) | C6—H6B | 0.9600 |
W2—O5 | 1.908 (5) | C6—H6C | 0.9600 |
W2—O2 | 1.912 (4) | O34—C7 | 1.243 (11) |
W2—O1 | 1.932 (5) | C7—N3 | 1.296 (12) |
W2—O13 | 2.380 (5) | C7—H7 | 0.9300 |
W3—O10 | 1.715 (5) | N3—C8 | 1.447 (13) |
W3—O8 | 1.883 (5) | N3—C9 | 1.458 (13) |
W3—O3 | 1.904 (5) | C8—H8A | 0.9600 |
W3—O7 | 1.909 (5) | C8—H8B | 0.9600 |
W3—O2 | 1.934 (5) | C8—H8C | 0.9600 |
W3—O13 | 2.392 (4) | C9—H9A | 0.9600 |
W4—O29 | 1.707 (5) | C9—H9B | 0.9600 |
W4—O20 | 1.881 (4) | C9—H9C | 0.9600 |
W4—O28i | 1.889 (5) | O35—C10 | 1.252 (9) |
W4—O21 | 1.924 (4) | C10—N4 | 1.321 (9) |
W4—O8 | 1.955 (5) | C10—H10 | 0.9300 |
W4—O14 | 2.384 (4) | N4—C11 | 1.445 (10) |
W5—O31 | 1.725 (5) | N4—C12 | 1.467 (10) |
W5—O22 | 1.890 (4) | C11—H11A | 0.9600 |
W5—O21 | 1.895 (4) | C11—H11B | 0.9600 |
W5—O30 | 1.899 (5) | C11—H11C | 0.9600 |
W5—O9 | 1.920 (5) | C12—H12A | 0.9600 |
W5—O14 | 2.306 (4) | C12—H12B | 0.9600 |
W6—O23 | 1.711 (5) | C12—H12C | 0.9600 |
W6—O24 | 1.891 (5) | O36—C13 | 1.230 (10) |
W6—O22 | 1.901 (5) | C13—N5 | 1.301 (10) |
W6—O17 | 1.911 (5) | C13—H13 | 0.9300 |
W6—O4 | 1.947 (4) | N5—C15 | 1.434 (12) |
W6—O16 | 2.352 (4) | N5—C14 | 1.453 (11) |
W7—O25 | 1.711 (5) | C14—H14A | 0.9600 |
W7—O18 | 1.901 (5) | C14—H14B | 0.9600 |
W7—O24i | 1.912 (5) | C14—H14C | 0.9600 |
W7—O5 | 1.918 (5) | C15—H15A | 0.9600 |
W7—O17 | 1.921 (5) | C15—H15B | 0.9600 |
W7—O16 | 2.381 (4) | C15—H15C | 0.9600 |
W8—O26 | 1.704 (5) | O37—C16 | 1.241 (11) |
W8—O18 | 1.894 (5) | C16—N6 | 1.306 (11) |
W8—O30i | 1.895 (5) | C16—H16 | 0.9300 |
W8—O19 | 1.913 (5) | N6—C18 | 1.435 (11) |
W8—O6 | 1.933 (5) | N6—C17 | 1.436 (11) |
W8—O15 | 2.377 (4) | C17—H17A | 0.9600 |
W9—O27 | 1.709 (5) | C17—H17B | 0.9600 |
W9—O19 | 1.907 (5) | C17—H17C | 0.9600 |
W9—O28 | 1.913 (5) | C18—H18A | 0.9600 |
W9—O20 | 1.915 (4) | C18—H18B | 0.9600 |
W9—O7 | 1.925 (5) | C18—H18C | 0.9600 |
W9—O15 | 2.365 (4) | O38—C19 | 1.208 (13) |
P1—O16 | 1.528 (5) | C19—N7 | 1.350 (12) |
P1—O15 | 1.533 (5) | C19—H19 | 0.9300 |
P1—O14 | 1.543 (5) | N7—C20 | 1.389 (14) |
P1—O13 | 1.577 (5) | N7—C21 | 1.448 (15) |
Mn2—O37ii | 2.133 (7) | C20—H20A | 0.9600 |
Mn2—O37 | 2.134 (7) | C20—H20B | 0.9600 |
Mn2—O38ii | 2.175 (7) | C20—H20C | 0.9600 |
Mn2—O38 | 2.175 (7) | C21—H21A | 0.9600 |
Mn2—O39ii | 2.214 (9) | C21—H21B | 0.9600 |
Mn2—O39 | 2.214 (9) | C21—H21C | 0.9600 |
Mn1—O34 | 2.137 (6) | O39—C22 | 1.216 (14) |
Mn1—O32 | 2.143 (6) | C22—N8 | 1.272 (14) |
Mn1—O36 | 2.153 (6) | C22—H22 | 0.9300 |
Mn1—O35 | 2.163 (5) | N8—C24 | 1.404 (16) |
Mn1—O33 | 2.173 (6) | N8—C23 | 1.51 (2) |
Mn1—O31 | 2.205 (5) | C23—H23A | 0.9600 |
O24—W7i | 1.912 (5) | C23—H23B | 0.9600 |
O28—W4i | 1.889 (5) | C23—H23C | 0.9600 |
O30—W8i | 1.895 (5) | C24—H24A | 0.9600 |
O32—C1 | 1.245 (9) | C24—H24B | 0.9600 |
C1—N1 | 1.322 (10) | C24—H24C | 0.9600 |
C1—H1 | 0.9300 | O40—C25 | 1.201 (16) |
N1—C2 | 1.439 (11) | C25—N9 | 1.320 (19) |
N1—C3 | 1.454 (11) | C25—H25 | 0.9300 |
C2—H2A | 0.9600 | N9—C27 | 1.36 (2) |
C2—H2B | 0.9600 | N9—C26 | 1.43 (2) |
C2—H2C | 0.9600 | C26—H26A | 0.9600 |
C3—H3A | 0.9600 | C26—H26B | 0.9600 |
C3—H3B | 0.9600 | C26—H26C | 0.9600 |
C3—H3C | 0.9600 | C27—H27A | 0.9600 |
O33—C4 | 1.207 (11) | C27—H27B | 0.9600 |
C4—N2 | 1.325 (11) | C27—H27C | 0.9600 |
O11—W1—O4 | 103.8 (2) | W5—O14—W4 | 91.28 (16) |
O11—W1—O1 | 100.8 (2) | P1—O15—W9 | 128.5 (2) |
O4—W1—O1 | 90.1 (2) | P1—O15—W8 | 127.6 (2) |
O11—W1—O9 | 102.4 (2) | W9—O15—W8 | 90.60 (16) |
O4—W1—O9 | 85.64 (19) | P1—O16—W6 | 129.1 (3) |
O1—W1—O9 | 156.78 (19) | P1—O16—W7 | 127.5 (3) |
O11—W1—O3 | 98.9 (2) | W6—O16—W7 | 90.25 (15) |
O4—W1—O3 | 157.21 (18) | W6—O17—W7 | 122.1 (2) |
O1—W1—O3 | 87.6 (2) | W8—O18—W7 | 151.7 (3) |
O9—W1—O3 | 87.6 (2) | W9—O19—W8 | 123.8 (2) |
O11—W1—O13 | 169.8 (2) | W4—O20—W9 | 151.9 (3) |
O4—W1—O13 | 84.73 (17) | W5—O21—W4 | 122.8 (2) |
O1—W1—O13 | 73.32 (17) | W5—O22—W6 | 152.2 (3) |
O9—W1—O13 | 83.55 (18) | W6—O24—W7i | 162.7 (3) |
O3—W1—O13 | 72.89 (16) | W4i—O28—W9 | 162.9 (3) |
O12—W2—O6 | 102.3 (2) | W8i—O30—W5 | 161.8 (3) |
O12—W2—O5 | 103.0 (2) | W5—O31—Mn1 | 171.1 (3) |
O6—W2—O5 | 85.4 (2) | C1—O32—Mn1 | 125.6 (5) |
O12—W2—O2 | 100.9 (2) | O32—C1—N1 | 123.3 (8) |
O6—W2—O2 | 89.63 (19) | O32—C1—H1 | 118.4 |
O5—W2—O2 | 156.2 (2) | N1—C1—H1 | 118.4 |
O12—W2—O1 | 100.6 (2) | C1—N1—C2 | 122.0 (8) |
O6—W2—O1 | 157.0 (2) | C1—N1—C3 | 120.6 (7) |
O5—W2—O1 | 87.5 (2) | C2—N1—C3 | 117.3 (7) |
O2—W2—O1 | 88.1 (2) | N1—C2—H2A | 109.5 |
O12—W2—O13 | 171.0 (2) | N1—C2—H2B | 109.5 |
O6—W2—O13 | 84.57 (18) | H2A—C2—H2B | 109.5 |
O5—W2—O13 | 83.16 (18) | N1—C2—H2C | 109.5 |
O2—W2—O13 | 73.16 (17) | H2A—C2—H2C | 109.5 |
O1—W2—O13 | 72.82 (17) | H2B—C2—H2C | 109.5 |
O10—W3—O8 | 102.9 (2) | N1—C3—H3A | 109.5 |
O10—W3—O3 | 100.4 (2) | N1—C3—H3B | 109.5 |
O8—W3—O3 | 89.9 (2) | H3A—C3—H3B | 109.5 |
O10—W3—O7 | 103.0 (2) | N1—C3—H3C | 109.5 |
O8—W3—O7 | 86.2 (2) | H3A—C3—H3C | 109.5 |
O3—W3—O7 | 156.52 (19) | H3B—C3—H3C | 109.5 |
O10—W3—O2 | 100.4 (2) | C4—O33—Mn1 | 129.1 (6) |
O8—W3—O2 | 156.61 (19) | O33—C4—N2 | 126.4 (9) |
O3—W3—O2 | 87.8 (2) | O33—C4—H4 | 116.8 |
O7—W3—O2 | 86.7 (2) | N2—C4—H4 | 116.8 |
O10—W3—O13 | 170.2 (2) | C4—N2—C6 | 123.5 (10) |
O8—W3—O13 | 84.54 (18) | C4—N2—C5 | 119.3 (9) |
O3—W3—O13 | 72.92 (17) | C6—N2—C5 | 117.2 (9) |
O7—W3—O13 | 83.66 (17) | N2—C5—H5A | 109.5 |
O2—W3—O13 | 72.54 (17) | N2—C5—H5B | 109.5 |
O29—W4—O20 | 102.8 (2) | H5A—C5—H5B | 109.5 |
O29—W4—O28i | 99.6 (2) | N2—C5—H5C | 109.5 |
O20—W4—O28i | 89.5 (2) | H5A—C5—H5C | 109.5 |
O29—W4—O21 | 100.4 (2) | H5B—C5—H5C | 109.5 |
O20—W4—O21 | 156.48 (19) | N2—C6—H6A | 109.5 |
O28i—W4—O21 | 90.5 (2) | N2—C6—H6B | 109.5 |
O29—W4—O8 | 97.2 (2) | H6A—C6—H6B | 109.5 |
O20—W4—O8 | 85.41 (19) | N2—C6—H6C | 109.5 |
O28i—W4—O8 | 163.13 (19) | H6A—C6—H6C | 109.5 |
O21—W4—O8 | 87.81 (19) | H6B—C6—H6C | 109.5 |
O29—W4—O14 | 171.8 (2) | C7—O34—Mn1 | 142.0 (7) |
O20—W4—O14 | 85.05 (17) | O34—C7—N3 | 124.3 (10) |
O28i—W4—O14 | 82.65 (18) | O34—C7—H7 | 117.9 |
O21—W4—O14 | 71.64 (17) | N3—C7—H7 | 117.9 |
O8—W4—O14 | 80.89 (17) | C7—N3—C8 | 123.8 (9) |
O31—W5—O22 | 102.3 (2) | C7—N3—C9 | 121.3 (9) |
O31—W5—O21 | 98.8 (2) | C8—N3—C9 | 114.7 (9) |
O22—W5—O21 | 158.81 (19) | N3—C8—H8A | 109.5 |
O31—W5—O30 | 98.0 (2) | N3—C8—H8B | 109.5 |
O22—W5—O30 | 88.52 (19) | H8A—C8—H8B | 109.5 |
O21—W5—O30 | 90.1 (2) | N3—C8—H8C | 109.5 |
O31—W5—O9 | 97.2 (2) | H8A—C8—H8C | 109.5 |
O22—W5—O9 | 86.14 (19) | H8B—C8—H8C | 109.5 |
O21—W5—O9 | 89.71 (19) | N3—C9—H9A | 109.5 |
O30—W5—O9 | 164.60 (19) | N3—C9—H9B | 109.5 |
O31—W5—O14 | 172.79 (19) | H9A—C9—H9B | 109.5 |
O22—W5—O14 | 84.89 (17) | N3—C9—H9C | 109.5 |
O21—W5—O14 | 73.96 (17) | H9A—C9—H9C | 109.5 |
O30—W5—O14 | 82.76 (17) | H9B—C9—H9C | 109.5 |
O9—W5—O14 | 82.39 (17) | C10—O35—Mn1 | 121.5 (5) |
O23—W6—O24 | 98.7 (2) | O35—C10—N4 | 123.9 (7) |
O23—W6—O22 | 101.4 (2) | O35—C10—H10 | 118.1 |
O24—W6—O22 | 89.35 (19) | N4—C10—H10 | 118.1 |
O23—W6—O17 | 100.9 (2) | C10—N4—C11 | 119.2 (7) |
O24—W6—O17 | 91.0 (2) | C10—N4—C12 | 121.6 (6) |
O22—W6—O17 | 157.46 (19) | C11—N4—C12 | 118.5 (7) |
O23—W6—O4 | 97.0 (2) | N4—C11—H11A | 109.5 |
O24—W6—O4 | 164.03 (19) | N4—C11—H11B | 109.5 |
O22—W6—O4 | 84.77 (19) | H11A—C11—H11B | 109.5 |
O17—W6—O4 | 88.8 (2) | N4—C11—H11C | 109.5 |
O23—W6—O16 | 174.7 (2) | H11A—C11—H11C | 109.5 |
O24—W6—O16 | 83.35 (18) | H11B—C11—H11C | 109.5 |
O22—W6—O16 | 83.51 (17) | N4—C12—H12A | 109.5 |
O17—W6—O16 | 74.15 (17) | N4—C12—H12B | 109.5 |
O4—W6—O16 | 81.25 (17) | H12A—C12—H12B | 109.5 |
O25—W7—O18 | 102.2 (2) | N4—C12—H12C | 109.5 |
O25—W7—O24i | 99.1 (2) | H12A—C12—H12C | 109.5 |
O18—W7—O24i | 87.7 (2) | H12B—C12—H12C | 109.5 |
O25—W7—O5 | 98.0 (2) | C13—O36—Mn1 | 132.0 (6) |
O18—W7—O5 | 85.6 (2) | O36—C13—N5 | 125.7 (8) |
O24i—W7—O5 | 162.62 (19) | O36—C13—H13 | 117.1 |
O25—W7—O17 | 100.2 (2) | N5—C13—H13 | 117.1 |
O18—W7—O17 | 157.6 (2) | C13—N5—C15 | 120.4 (8) |
O24i—W7—O17 | 89.6 (2) | C13—N5—C14 | 122.2 (8) |
O5—W7—O17 | 90.5 (2) | C15—N5—C14 | 117.3 (8) |
O25—W7—O16 | 173.4 (2) | N5—C14—H14A | 109.5 |
O18—W7—O16 | 84.35 (18) | N5—C14—H14B | 109.5 |
O24i—W7—O16 | 82.06 (18) | H14A—C14—H14B | 109.5 |
O5—W7—O16 | 81.33 (17) | N5—C14—H14C | 109.5 |
O17—W7—O16 | 73.26 (17) | H14A—C14—H14C | 109.5 |
O26—W8—O18 | 102.1 (2) | H14B—C14—H14C | 109.5 |
O26—W8—O30i | 98.8 (2) | N5—C15—H15A | 109.5 |
O18—W8—O30i | 89.7 (2) | N5—C15—H15B | 109.5 |
O26—W8—O19 | 100.6 (2) | H15A—C15—H15B | 109.5 |
O18—W8—O19 | 157.2 (2) | N5—C15—H15C | 109.5 |
O30i—W8—O19 | 89.3 (2) | H15A—C15—H15C | 109.5 |
O26—W8—O6 | 98.3 (2) | H15B—C15—H15C | 109.5 |
O18—W8—O6 | 85.8 (2) | C16—O37—Mn2 | 135.4 (7) |
O30i—W8—O6 | 162.9 (2) | O37—C16—N6 | 125.2 (9) |
O19—W8—O6 | 88.49 (19) | O37—C16—H16 | 117.4 |
O26—W8—O15 | 173.1 (2) | N6—C16—H16 | 117.4 |
O18—W8—O15 | 84.77 (18) | C16—N6—C18 | 119.5 (8) |
O30i—W8—O15 | 81.74 (17) | C16—N6—C17 | 122.9 (8) |
O19—W8—O15 | 72.53 (17) | C18—N6—C17 | 117.5 (8) |
O6—W8—O15 | 81.44 (18) | N6—C17—H17A | 109.5 |
O27—W9—O19 | 100.0 (2) | N6—C17—H17B | 109.5 |
O27—W9—O28 | 98.7 (2) | H17A—C17—H17B | 109.5 |
O19—W9—O28 | 89.7 (2) | N6—C17—H17C | 109.5 |
O27—W9—O20 | 102.7 (2) | H17A—C17—H17C | 109.5 |
O19—W9—O20 | 157.30 (19) | H17B—C17—H17C | 109.5 |
O28—W9—O20 | 87.7 (2) | N6—C18—H18A | 109.5 |
O27—W9—O7 | 97.4 (2) | N6—C18—H18B | 109.5 |
O19—W9—O7 | 90.2 (2) | H18A—C18—H18B | 109.5 |
O28—W9—O7 | 163.7 (2) | N6—C18—H18C | 109.5 |
O20—W9—O7 | 86.1 (2) | H18A—C18—H18C | 109.5 |
O27—W9—O15 | 172.9 (2) | H18B—C18—H18C | 109.5 |
O19—W9—O15 | 72.92 (17) | C19—O38—Mn2 | 122.6 (8) |
O28—W9—O15 | 82.15 (18) | O38—C19—N7 | 123.8 (11) |
O20—W9—O15 | 84.38 (17) | O38—C19—H19 | 118.1 |
O7—W9—O15 | 82.27 (17) | N7—C19—H19 | 118.1 |
O16—P1—O15 | 112.7 (2) | C19—N7—C20 | 127.1 (11) |
O16—P1—O14 | 111.5 (2) | C19—N7—C21 | 116.9 (10) |
O15—P1—O14 | 111.9 (3) | C20—N7—C21 | 115.8 (11) |
O16—P1—O13 | 107.1 (2) | N7—C20—H20A | 109.5 |
O15—P1—O13 | 106.6 (3) | N7—C20—H20B | 109.5 |
O14—P1—O13 | 106.5 (2) | H20A—C20—H20B | 109.5 |
O37ii—Mn2—O37 | 180.0 | N7—C20—H20C | 109.5 |
O37ii—Mn2—O38ii | 89.4 (3) | H20A—C20—H20C | 109.5 |
O37—Mn2—O38ii | 90.6 (3) | H20B—C20—H20C | 109.5 |
O37ii—Mn2—O38 | 90.6 (3) | N7—C21—H21A | 109.5 |
O37—Mn2—O38 | 89.4 (3) | N7—C21—H21B | 109.5 |
O38ii—Mn2—O38 | 180.0 | H21A—C21—H21B | 109.5 |
O37ii—Mn2—O39ii | 84.2 (3) | N7—C21—H21C | 109.5 |
O37—Mn2—O39ii | 95.8 (3) | H21A—C21—H21C | 109.5 |
O38ii—Mn2—O39ii | 90.4 (3) | H21B—C21—H21C | 109.5 |
O38—Mn2—O39ii | 89.6 (3) | C22—O39—Mn2 | 147.2 (9) |
O37ii—Mn2—O39 | 95.8 (3) | O39—C22—N8 | 125.7 (14) |
O37—Mn2—O39 | 84.2 (3) | O39—C22—H22 | 117.2 |
O38ii—Mn2—O39 | 89.6 (3) | N8—C22—H22 | 117.2 |
O38—Mn2—O39 | 90.4 (3) | C22—N8—C24 | 129.8 (14) |
O39ii—Mn2—O39 | 180.0 | C22—N8—C23 | 117.1 (14) |
O34—Mn1—O32 | 91.0 (2) | C24—N8—C23 | 112.9 (13) |
O34—Mn1—O36 | 96.2 (3) | N8—C23—H23A | 109.5 |
O32—Mn1—O36 | 86.9 (2) | N8—C23—H23B | 109.5 |
O34—Mn1—O35 | 89.2 (2) | H23A—C23—H23B | 109.5 |
O32—Mn1—O35 | 169.7 (2) | N8—C23—H23C | 109.5 |
O36—Mn1—O35 | 82.9 (2) | H23A—C23—H23C | 109.5 |
O34—Mn1—O33 | 88.5 (3) | H23B—C23—H23C | 109.5 |
O32—Mn1—O33 | 90.2 (2) | N8—C24—H24A | 109.5 |
O36—Mn1—O33 | 174.5 (3) | N8—C24—H24B | 109.5 |
O35—Mn1—O33 | 100.0 (2) | H24A—C24—H24B | 109.5 |
O34—Mn1—O31 | 173.6 (2) | N8—C24—H24C | 109.5 |
O32—Mn1—O31 | 94.1 (2) | H24A—C24—H24C | 109.5 |
O36—Mn1—O31 | 88.0 (2) | H24B—C24—H24C | 109.5 |
O35—Mn1—O31 | 86.5 (2) | O40—C25—N9 | 127.3 (17) |
O33—Mn1—O31 | 87.5 (2) | O40—C25—H25 | 116.4 |
W1—O1—W2 | 123.2 (2) | N9—C25—H25 | 116.4 |
W2—O2—W3 | 123.7 (2) | C25—N9—C27 | 124.5 (19) |
W3—O3—W1 | 123.7 (2) | C25—N9—C26 | 121.9 (14) |
W1—O4—W6 | 151.7 (3) | C27—N9—C26 | 113.6 (18) |
W2—O5—W7 | 152.0 (3) | N9—C26—H26A | 109.5 |
W2—O6—W8 | 151.4 (3) | N9—C26—H26B | 109.5 |
W3—O7—W9 | 150.4 (3) | H26A—C26—H26B | 109.5 |
W3—O8—W4 | 151.3 (3) | N9—C26—H26C | 109.5 |
W1—O9—W5 | 150.3 (3) | H26A—C26—H26C | 109.5 |
P1—O13—W1 | 124.6 (3) | H26B—C26—H26C | 109.5 |
P1—O13—W2 | 124.9 (2) | N9—C27—H27A | 109.5 |
W1—O13—W2 | 90.64 (15) | N9—C27—H27B | 109.5 |
P1—O13—W3 | 125.1 (2) | H27A—C27—H27B | 109.5 |
W1—O13—W3 | 90.47 (15) | N9—C27—H27C | 109.5 |
W2—O13—W3 | 90.57 (16) | H27A—C27—H27C | 109.5 |
P1—O14—W5 | 128.5 (2) | H27B—C27—H27C | 109.5 |
P1—O14—W4 | 127.9 (2) |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1/2, −y−1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···O34 | 0.93 | 2.58 | 3.122 (10) | 118 |
C2—H2C···O29iii | 0.96 | 2.61 | 3.500 (12) | 154 |
C4—H4···O21 | 0.93 | 2.53 | 3.431 (11) | 163 |
C4—H4···O31 | 0.93 | 2.52 | 3.108 (10) | 121 |
C8—H8A···O2iv | 0.96 | 2.55 | 3.488 (14) | 167 |
C8—H8B···O10v | 0.96 | 2.57 | 3.307 (14) | 134 |
C9—H9A···O1iv | 0.96 | 2.60 | 3.366 (12) | 137 |
C9—H9B···O35 | 0.96 | 2.42 | 3.289 (12) | 151 |
C12—H12A···O23 | 0.96 | 2.48 | 3.439 (9) | 176 |
C12—H12C···O11 | 0.96 | 2.48 | 3.086 (10) | 121 |
C13—H13···O19v | 0.93 | 2.53 | 3.287 (9) | 139 |
C14—H14B···O30iii | 0.96 | 2.56 | 3.379 (11) | 144 |
C16—H16···O10 | 0.93 | 2.62 | 3.473 (11) | 153 |
C17—H17C···O10 | 0.96 | 2.63 | 3.513 (12) | 154 |
C19—H19···O40ii | 0.93 | 2.43 | 3.331 (19) | 164 |
C21—H21B···O11iv | 0.96 | 2.59 | 3.478 (14) | 154 |
C21—H21C···O33 | 0.96 | 2.50 | 3.375 (14) | 151 |
C24—H24C···O26vi | 0.96 | 2.43 | 3.369 (14) | 164 |
C25—H25···O12vii | 0.93 | 2.56 | 3.358 (19) | 144 |
C26—H26C···O1viii | 0.96 | 2.55 | 3.453 (17) | 156 |
Symmetry codes: (ii) −x+1/2, −y−1/2, −z; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x+1/2, −y+1/2, −z; (v) x−1/2, y+1/2, z; (vi) x−1/2, y−1/2, z; (vii) −x+1, −y, −z; (viii) x, y−1, z. |
Acknowledgements
The authors gratefully acknowledge financial support from the Ministry of Higher Education and Scientific Research of Tunisia and acknowledge Dr Michel Giorgi, from the University of Aix-Marseille, for the data collection.
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