A novel supramolecular organic–inorganic adduct containing α-Keggin-type [PW12O40]3− anions and benzo-15-crown-5 mol­ecules

Almeida Paz, F.A.; Sousa, F.L.; Soares-Santos, P.C.R.; Cavaleiro, A.M.V.; Nogueira, H.I.S.; Klinowski, J.; Trindade, T.

doi:10.1107/S1600536803024310

A novel supramolecular organic–inorganic adduct containing α-Keggin-type [PW₁₂O₄₀]³⁻ anions and benzo-15-crown-5 molecules

F. A. Almeida Paz, F. L. Sousa, P. C. R. Soares-Santos, A. M. V. Cavaleiro, H. I. S. Nogueira, J. Klinowski and T. Trindade

The structure of the title compound, tris(hydroxonium) μ₁₂-phosphato-tetracosa-μ₂-oxo-dodecaoxododecatungsten hexakis(benzo-15-crown-5)–methanol–water (1/1/1), (H₃O)₃[PW₁₂O₄₀]·6C₁₄H₂₀O₅·CH₃OH·H₂O (where C₁₄H₂₀O₅ is benzo-15-crown-5), has been determined at 180 K. [PW₁₂O₄₀]³⁻ anions are typical of α-Keggin structures, and the [H₃O·(C₁₄H₂₀O₅)₂]⁺ sandwich-type moieties contain a large number of short O

O close contacts, suggesting strong hydrogen bonding within them.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024310/cf6294sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024310/cf6294Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 180 K
Mean (C-C) = 0.018 Å
H-atom completeness 92%
R factor = 0.039
wR factor = 0.083
Data-to-parameter ratio = 14.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ..... =         19

Author Response: When treated anisotropically, several C-atoms showed large tensors in more than one direction suggesting that they are affected by thermal disorder. Consequently, these atoms have been modelled with independent isotropic displacement parameters.

PLAT241_ALERT_2_A Check High   U(eq) as Compared to Neighbors ....        C52

Author Response: This is a direct consequence of the thermal disorder registered for some atoms belonging to the several organic molecules present in the crystal structure.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W

Author Response: H-atoms bound to the oxygen atoms of the crystallisation water molecules could not be located from difference Fourier maps. Since the number of possible hydrogen bonds in which these molecules could be involved is quite large, no attempt was made to place the H-atoms at calculated positions. See also Experimental Section.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O2W

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O4W


Alert level B
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....        O59
PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O69      =       2.78 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O65      =       2.79 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_B Short Inter D...A Contact  O2W    ..  O64      =       2.80 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.


Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ....... =          3
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.32 Ratio
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.19 Ratio
PLAT230_ALERT_2_C Hirshfeld Test Diff for    O47    -   C20      =       5.14 su
PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C13

Author Response: This is a direct consequence of the thermal disorder registered for some atoms belonging to the several organic molecules present in the crystal structure.

PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        O55

Author Response: This is a direct consequence of the thermal disorder registered for some atoms belonging to the several organic molecules present in the crystal structure.

PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C39

Author Response: This is a direct consequence of the thermal disorder registered for some atoms belonging to the several organic molecules present in the crystal structure.

PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        O67

Author Response: This is a direct consequence of the thermal disorder registered for some atoms belonging to the several organic molecules present in the crystal structure.

PLAT241_ALERT_2_C Check High   U(eq) as Compared to Neighbors ....        C78

Author Response: This is a direct consequence of the thermal disorder registered for some atoms belonging to the several organic molecules present in the crystal structure.

PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        C40
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        O68
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        C77
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         18
PLAT410_ALERT_2_C Short Intra H...H Contact  H2     ..  H14A     =       1.98 Ang.
PLAT430_ALERT_2_C Short Inter D...A Contact  O1W    ..  O44      =       2.88 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_C Short Inter D...A Contact  O1W    ..  O49      =       2.88 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_C Short Inter D...A Contact  O2W    ..  O67      =       2.88 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_C Short Inter D...A Contact  O3W    ..  O51      =       2.87 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_C Short Inter D...A Contact  O3W    ..  O58      =       2.88 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.

PLAT430_ALERT_2_C Short Inter D...A Contact  O3W    ..  O59      =       2.89 Ang.

Author Response: H-atoms from the crystallisation water molecules are missing (see Experimental Section). Thus, hydrogen bonds occur between the involved O-atoms referred to in the Alerts.


Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C85 H135 O75 P1 W12
            Atom count from the _atom_site data:  C85 H124 O75 P1 W12
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C85 H135 O75 P W12
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        340.00    340.00    0.00
           H        540.00    496.00   44.00
           O        300.00    300.00    0.00
           P          4.00      4.00    0.00
           W         48.00     48.00    0.00

   7 ALERT level A = In general: serious problem
   4 ALERT level B = Potentially serious problem
  23 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  29 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXTL (Bruker, 2001); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

tris(hydroxonium) µ₁₂-phosphato-tetracosa-µ₂-oxo-dodecaoxododecatungsten hexakis(benzo-15-crown-5)–methanol–water (1/1/1) top

Crystal data top

(H₃O)₃[PW₁₂O₄₀]·6C₁₄H₂₀O₅·CH₄O·H2O	F(000) = 8592
M_r = 4594.10	D_x = 2.519 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 118671 reflections
a = 16.890 (3) Å	θ = 1.0–25.0°
b = 42.101 (8) Å	µ = 11.46 mm⁻¹
c = 17.393 (4) Å	T = 180 K
β = 101.66 (3)°	Block, orange
V = 12112 (4) Å³	0.12 × 0.10 × 0.05 mm
Z = 4

Data collection top

Nonius KappaCCD diffractometer	16507 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.052
Thin–slice ω and φ scans	θ_max = 25.0°, θ_min = 3.5°
Absorption correction: multi-scan (Sortav; Blessing, 1995)	h = −20→20
T_min = 0.269, T_max = 0.559	k = −49→50
71608 measured reflections	l = −20→20
20465 independent reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full with fixed elements per cycle	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.083	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0246P)² + 121.8552P] where P = (F_o² + 2F_c²)/3
20465 reflections	(Δ/σ)_max = 0.001
1449 parameters	Δρ_max = 1.82 e Å⁻³
6 restraints	Δρ_min = −1.25 e Å⁻³

Special details top

Experimental. All atoms directly located from difference Fourier maps.

H-atoms have been placed in calculated positions using HFIX 43 (for aromatic C—H atoms), HFIX 23 for –CH2-, HFIX 147 for –OH and HFIX 33 for –CH3.

Four crystallization water molecules could be directly found from difference Fourier maps, but the attached H-atoms are missing. Since three of these molecules must be protonated (H3O+) in order to compensate the crystal charge, and the number of possible hydrogen bonds to neighbouring crown ethers is large, no attempt was made to place these H-atoms in calculated positions.

Several C-atoms from the organic molecules were found to be affected by thermal disorder. Anisotropic treatment gave large tensors in more than one direction. Thus, these atoms have been modelled with independent isotropic displacement parameters. Atoms: C21 C22 C23 C24 C25 C26 C27 C28 C35 C36 C36 C38 C39 C40 C41 C43 C13 C51 C52

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
W1	0.47452 (2)	0.132366 (9)	0.12882 (2)	0.02531 (9)
W2	0.63057 (2)	0.119988 (9)	0.01037 (2)	0.02496 (9)
W3	0.57495 (2)	0.054338 (9)	0.13060 (2)	0.02393 (9)
W4	0.57888 (2)	0.195853 (9)	0.22356 (2)	0.02622 (9)
W5	0.73161 (2)	0.184586 (9)	0.10106 (2)	0.02532 (9)
W6	0.82947 (2)	0.113440 (9)	0.10174 (2)	0.02641 (9)
W7	0.77480 (2)	0.046436 (9)	0.21859 (2)	0.02652 (9)
W8	0.63156 (2)	0.056312 (9)	0.33100 (2)	0.02550 (9)
W9	0.52729 (2)	0.133505 (9)	0.33047 (2)	0.02446 (9)
W10	0.79481 (2)	0.187333 (9)	0.31713 (2)	0.02589 (9)
W11	0.88796 (2)	0.114996 (9)	0.31807 (2)	0.02710 (9)
W12	0.74225 (2)	0.126188 (9)	0.42732 (2)	0.02613 (9)
P1	0.68156 (13)	0.12204 (5)	0.21982 (13)	0.0206 (5)
O1	0.6013 (3)	0.13878 (14)	0.2240 (3)	0.0243 (13)
O2	0.7071 (3)	0.13120 (14)	0.1425 (3)	0.0250 (14)
O3	0.7466 (3)	0.13295 (14)	0.2888 (3)	0.0244 (14)
O4	0.6706 (3)	0.08636 (14)	0.2233 (3)	0.0264 (14)
O5	0.3794 (3)	0.13184 (16)	0.0733 (4)	0.0337 (16)
O6	0.5899 (4)	0.11536 (15)	−0.0858 (4)	0.0338 (16)
O7	0.5149 (4)	0.02755 (15)	0.0745 (4)	0.0336 (16)
O8	0.5396 (3)	0.13470 (14)	0.0527 (3)	0.0284 (14)
O9	0.6108 (4)	0.08028 (14)	0.0544 (3)	0.0284 (14)
O10	0.5028 (3)	0.08846 (14)	0.1378 (3)	0.0277 (14)
O11	0.6659 (4)	0.16380 (15)	0.0136 (3)	0.0283 (14)
O12	0.7403 (4)	0.10852 (14)	0.0136 (3)	0.0280 (14)
O13	0.6784 (4)	0.03371 (15)	0.1475 (3)	0.0305 (15)
O14	0.5674 (3)	0.04122 (14)	0.2334 (3)	0.0263 (14)
O15	0.4525 (3)	0.12916 (14)	0.2337 (3)	0.0279 (14)
O16	0.4910 (4)	0.17678 (15)	0.1500 (3)	0.0297 (15)
O17	0.6385 (4)	0.19494 (14)	0.1404 (3)	0.0287 (14)
O18	0.7533 (4)	0.21918 (16)	0.0599 (4)	0.0356 (16)
O19	0.8188 (4)	0.15809 (15)	0.0833 (4)	0.0311 (15)
O20	0.9089 (4)	0.10428 (15)	0.0609 (3)	0.0307 (15)
O21	0.7994 (4)	0.07313 (14)	0.1382 (3)	0.0289 (14)
O22	0.8354 (4)	0.01428 (15)	0.2159 (4)	0.0370 (17)
O23	0.7217 (4)	0.03534 (15)	0.3023 (3)	0.0313 (15)
O24	0.6049 (4)	0.03093 (16)	0.3964 (4)	0.0366 (16)
O25	0.5548 (4)	0.08991 (15)	0.3268 (3)	0.0298 (15)
O26	0.4649 (4)	0.13432 (15)	0.3956 (4)	0.0329 (15)
O27	0.5341 (4)	0.17792 (15)	0.3055 (3)	0.0311 (15)
O28	0.5475 (4)	0.23415 (15)	0.2240 (4)	0.0356 (16)
O29	0.7892 (4)	0.18907 (15)	0.2072 (3)	0.0303 (15)
O30	0.8793 (4)	0.12131 (15)	0.2077 (4)	0.0334 (15)
O31	0.8422 (4)	0.07420 (15)	0.2906 (3)	0.0309 (15)
O32	0.7040 (4)	0.08430 (15)	0.3951 (4)	0.0335 (16)
O33	0.6332 (4)	0.13874 (14)	0.3955 (3)	0.0294 (15)
O34	0.6817 (4)	0.19723 (15)	0.2920 (4)	0.0307 (15)
O35	0.8871 (4)	0.16061 (15)	0.3276 (3)	0.0287 (14)
O36	0.8479 (4)	0.11339 (15)	0.4125 (3)	0.0313 (15)
O37	0.7757 (4)	0.16895 (14)	0.4119 (3)	0.0280 (14)
O38	0.8373 (4)	0.22268 (16)	0.3492 (4)	0.0378 (17)
O39	0.9875 (4)	0.10693 (17)	0.3492 (4)	0.0375 (17)
O40	0.7556 (4)	0.12525 (16)	0.5261 (4)	0.0356 (16)
C1	0.8477 (7)	0.1906 (3)	0.7708 (6)	0.043 (3)
C2	0.9286 (7)	0.1817 (3)	0.7932 (7)	0.053 (3)
H2	0.9666	0.1870	0.7618	0.063*
C3	0.9518 (7)	0.1648 (3)	0.8624 (7)	0.052 (3)
H3	1.0066	0.1583	0.8784	0.062*
C4	0.8981 (7)	0.1573 (3)	0.9079 (7)	0.050 (3)
H4	0.9154	0.1458	0.9553	0.060*
C5	0.8187 (6)	0.1664 (2)	0.8853 (6)	0.041 (3)
H5	0.7813	0.1612	0.9174	0.049*
C6	0.7927 (6)	0.1831 (3)	0.8162 (6)	0.039 (2)
C7	0.6520 (6)	0.1695 (3)	0.7822 (7)	0.047 (3)
H7A	0.6010	0.1787	0.7918	0.056*
H7B	0.6682	0.1521	0.8207	0.056*
C8	0.6378 (7)	0.1560 (3)	0.7012 (7)	0.055 (3)
H8A	0.6899	0.1499	0.6875	0.066*
H8B	0.6033	0.1369	0.6978	0.066*
C9	0.5859 (8)	0.1707 (3)	0.5690 (7)	0.061 (3)
H9A	0.5507	0.1517	0.5603	0.073*
H9B	0.6381	0.1653	0.5547	0.073*
C10	0.5470 (8)	0.1972 (3)	0.5192 (7)	0.059 (3)
H10A	0.5311	0.1897	0.4643	0.070*
H10B	0.4971	0.2035	0.5369	0.070*
C11	0.6511 (8)	0.2223 (3)	0.4675 (7)	0.068 (4)
H11A	0.6207	0.2265	0.4136	0.081*
H11B	0.6743	0.2007	0.4686	0.081*
C12	0.7169 (8)	0.2459 (4)	0.4891 (7)	0.068 (4)
H12A	0.7528	0.2441	0.4508	0.082*
H12B	0.6925	0.2673	0.4833	0.082*
C13	0.8198 (10)	0.2210 (4)	0.5704 (9)	0.093 (5)*
H13A	0.8564	0.2260	0.5342	0.112*
H13B	0.7928	0.2006	0.5534	0.112*
C14	0.8707 (7)	0.2172 (4)	0.6546 (7)	0.072 (4)
H14A	0.9137	0.2012	0.6555	0.086*
H14B	0.8962	0.2377	0.6739	0.086*
O41	0.8158 (4)	0.2072 (2)	0.7023 (5)	0.059 (2)
O42	0.7141 (4)	0.19372 (17)	0.7943 (4)	0.0429 (18)
O43	0.5988 (4)	0.17981 (17)	0.6487 (4)	0.0448 (18)
O44	0.5979 (4)	0.22410 (19)	0.5214 (4)	0.050 (2)
O45	0.7649 (5)	0.2434 (2)	0.5651 (5)	0.072 (3)
C15	0.7900 (7)	0.2878 (4)	0.7998 (7)	0.062 (4)
C16	0.8712 (9)	0.2862 (4)	0.8029 (8)	0.085 (5)
H16	0.8953	0.2972	0.7658	0.102*
C17	0.9186 (9)	0.2677 (4)	0.8630 (8)	0.086 (5)
H17	0.9750	0.2658	0.8647	0.104*
C18	0.8856 (9)	0.2526 (4)	0.9188 (9)	0.082 (5)
H18	0.9178	0.2403	0.9593	0.098*
C19	0.8007 (8)	0.2560 (4)	0.9133 (7)	0.070 (4)
H19	0.7748	0.2457	0.9501	0.083*
C20	0.7559 (7)	0.2745 (3)	0.8536 (8)	0.066 (4)
C21	0.6301 (7)	0.2569 (4)	0.8814 (8)	0.074 (4)*
H21A	0.6365	0.2638	0.9367	0.089*
H21B	0.6519	0.2351	0.8810	0.089*
C22	0.5440 (8)	0.2570 (4)	0.8438 (9)	0.091 (5)*
H22A	0.5130	0.2449	0.8766	0.109*
H22B	0.5236	0.2791	0.8395	0.109*
C23	0.4611 (10)	0.2491 (4)	0.7168 (10)	0.093 (5)*
H23A	0.4160	0.2477	0.7452	0.112*
H23B	0.4539	0.2316	0.6779	0.112*
C24	0.4531 (11)	0.2791 (4)	0.6735 (10)	0.106 (6)*
H24A	0.3996	0.2800	0.6376	0.127*
H24B	0.4568	0.2971	0.7107	0.127*
C25	0.5186 (11)	0.3112 (5)	0.5986 (11)	0.120 (7)*
H25A	0.5309	0.3268	0.6419	0.144*
H25B	0.4649	0.3166	0.5667	0.144*
C26	0.5792 (10)	0.3147 (5)	0.5490 (11)	0.115 (6)*
H26A	0.5637	0.3010	0.5022	0.138*
H26B	0.5789	0.3370	0.5307	0.138*
C27	0.7009 (9)	0.3331 (4)	0.6251 (9)	0.081 (4)*
H27A	0.6662	0.3457	0.6534	0.097*
H27B	0.7190	0.3469	0.5860	0.097*
C28	0.7724 (9)	0.3193 (4)	0.6818 (8)	0.074 (4)*
H28A	0.7996	0.3029	0.6556	0.089*
H28B	0.8121	0.3362	0.7021	0.089*
O46	0.7408 (6)	0.3058 (2)	0.7434 (5)	0.077 (3)
O47	0.6723 (6)	0.2768 (2)	0.8426 (5)	0.078 (3)
O48	0.5324 (6)	0.2436 (3)	0.7704 (6)	0.087 (3)
O49	0.5141 (6)	0.2815 (3)	0.6305 (7)	0.100 (4)
O50	0.6593 (6)	0.3066 (2)	0.5889 (6)	0.083 (3)
C29	0.3593 (6)	0.1016 (2)	0.8044 (7)	0.042 (3)
C30	0.4006 (6)	0.1032 (3)	0.8795 (7)	0.049 (3)
H30	0.4213	0.1231	0.9003	0.059*
C31	0.4131 (7)	0.0766 (3)	0.9267 (7)	0.055 (3)
H31	0.4429	0.0781	0.9791	0.065*
C32	0.3825 (6)	0.0484 (3)	0.8973 (6)	0.047 (3)
H32	0.3924	0.0299	0.9290	0.056*
C33	0.3363 (7)	0.0461 (3)	0.8208 (7)	0.046 (3)
H33	0.3138	0.0262	0.8019	0.056*
C34	0.3235 (6)	0.0724 (2)	0.7732 (6)	0.034 (2)
C35	0.2420 (8)	0.0445 (3)	0.6678 (7)	0.056 (3)*
H35A	0.1985	0.0390	0.6961	0.068*
H35B	0.2815	0.0269	0.6744	0.068*
C36	0.2079 (9)	0.0498 (4)	0.5840 (8)	0.078 (4)*
H36A	0.2529	0.0541	0.5568	0.094*
H36B	0.1814	0.0299	0.5617	0.094*
C37	0.1264 (8)	0.0803 (3)	0.4853 (8)	0.067 (4)*
H37A	0.1056	0.0605	0.4576	0.081*
H37B	0.0810	0.0955	0.4798	0.081*
C38	0.1887 (8)	0.0935 (3)	0.4482 (8)	0.069 (4)*
H38A	0.1673	0.0961	0.3912	0.082*
H38B	0.2355	0.0788	0.4552	0.082*
C39	0.2823 (11)	0.1363 (4)	0.4642 (10)	0.113 (6)*
H39A	0.2676	0.1471	0.4128	0.136*
H39B	0.3174	0.1180	0.4580	0.136*
C40	0.3275 (10)	0.1584 (4)	0.5222 (9)	0.090 (5)*
H40A	0.3763	0.1657	0.5039	0.108*
H40B	0.2934	0.1773	0.5261	0.108*
C41	0.3915 (10)	0.1586 (4)	0.6565 (8)	0.088 (5)*
H41A	0.3602	0.1775	0.6666	0.105*
H41B	0.4420	0.1663	0.6423	0.105*
C42	0.4134 (9)	0.1407 (4)	0.7299 (8)	0.079 (4)*
H42A	0.4441	0.1548	0.7710	0.095*
H42B	0.4492	0.1229	0.7223	0.095*
O51	0.3428 (4)	0.12810 (17)	0.7569 (5)	0.055 (2)
O52	0.2805 (4)	0.07320 (17)	0.6980 (4)	0.0457 (19)
O53	0.1551 (6)	0.0732 (2)	0.5686 (5)	0.075 (3)
O54	0.2159 (5)	0.1257 (3)	0.4846 (5)	0.076 (3)
O55	0.3515 (6)	0.1444 (3)	0.5983 (6)	0.107 (4)
C43	0.1504 (6)	0.1248 (2)	0.8360 (6)	0.037 (2)
C44	0.1976 (7)	0.1149 (3)	0.9056 (6)	0.043 (3)
H44	0.2325	0.1293	0.9380	0.051*
C45	0.1935 (7)	0.0830 (3)	0.9283 (7)	0.051 (3)
H45	0.2273	0.0757	0.9754	0.061*
C46	0.1406 (8)	0.0623 (3)	0.8824 (8)	0.065 (4)
H46	0.1368	0.0409	0.8984	0.078*
C47	0.0929 (8)	0.0731 (3)	0.8125 (7)	0.061 (3)
H47	0.0576	0.0588	0.7799	0.073*
C48	0.0966 (6)	0.1040 (3)	0.7904 (6)	0.047 (3)
C49	0.0038 (7)	0.0987 (3)	0.6671 (7)	0.061 (4)
H49A	−0.0378	0.0874	0.6895	0.073*
H49B	0.0380	0.0827	0.6474	0.073*
C50	−0.0347 (7)	0.1204 (3)	0.6027 (7)	0.062 (4)
H50A	−0.0710	0.1081	0.5614	0.074*
H50B	−0.0677	0.1365	0.6235	0.074*
C51	−0.0067 (9)	0.1629 (4)	0.5306 (9)	0.081 (4)*
H51A	−0.0371	0.1749	0.5641	0.097*
H51B	−0.0456	0.1565	0.4825	0.097*
C52	0.0531 (10)	0.1839 (4)	0.5083 (11)	0.118 (6)*
H52A	0.0706	0.1743	0.4624	0.141*
H52B	0.0258	0.2041	0.4904	0.141*
C53	0.1232 (8)	0.2178 (3)	0.6115 (7)	0.065 (4)
H53A	0.0830	0.2152	0.6454	0.078*
H53B	0.1082	0.2367	0.5780	0.078*
C54	0.2058 (8)	0.2220 (3)	0.6610 (7)	0.060 (3)
H54A	0.2461	0.2214	0.6268	0.071*
H54B	0.2092	0.2430	0.6866	0.071*
C55	0.2024 (8)	0.2058 (3)	0.7923 (6)	0.056 (3)
H55A	0.1456	0.2132	0.7825	0.067*
H55B	0.2375	0.2230	0.8192	0.067*
C56	0.2117 (7)	0.1767 (3)	0.8417 (7)	0.052 (3)
H56A	0.2655	0.1670	0.8437	0.063*
H56B	0.2063	0.1819	0.8959	0.063*
O56	0.1493 (5)	0.15534 (17)	0.8062 (4)	0.0493 (19)
O57	0.0509 (5)	0.1181 (2)	0.7237 (5)	0.058 (2)
O58	0.0246 (5)	0.1356 (2)	0.5704 (5)	0.065 (2)
O59	0.1237 (5)	0.19114 (19)	0.5652 (4)	0.052 (2)
O60	0.2251 (4)	0.19795 (17)	0.7199 (4)	0.0455 (18)
C57	0.1941 (6)	−0.0003 (2)	0.4147 (5)	0.032 (2)
C58	0.2135 (7)	−0.0213 (3)	0.4764 (6)	0.044 (3)
H58	0.2684	−0.0246	0.5012	0.052*
C59	0.1521 (7)	−0.0380 (3)	0.5024 (7)	0.051 (3)
H59	0.1658	−0.0523	0.5453	0.061*
C60	0.0735 (7)	−0.0339 (3)	0.4675 (7)	0.049 (3)
H60	0.0324	−0.0454	0.4857	0.059*
C61	0.0533 (6)	−0.0127 (2)	0.4043 (6)	0.040 (3)
H61	−0.0017	−0.0097	0.3794	0.048*
C62	0.1137 (6)	0.0039 (2)	0.3781 (5)	0.030 (2)
C63	0.0208 (6)	0.0289 (3)	0.2731 (6)	0.040 (3)
H63A	−0.0157	0.0363	0.3072	0.048*
H63B	0.0000	0.0085	0.2488	0.048*
C64	0.0258 (7)	0.0529 (3)	0.2113 (6)	0.049 (3)
H64A	−0.0291	0.0584	0.1823	0.059*
H64B	0.0521	0.0725	0.2356	0.059*
C65	0.0974 (6)	0.0624 (3)	0.1085 (6)	0.041 (3)
H65A	0.0518	0.0769	0.0882	0.050*
H65B	0.1116	0.0512	0.0630	0.050*
C66	0.1686 (7)	0.0817 (3)	0.1482 (7)	0.049 (3)
H66A	0.1822	0.0977	0.1114	0.059*
H66B	0.1554	0.0929	0.1940	0.059*
C67	0.3036 (6)	0.0773 (3)	0.2185 (8)	0.055 (3)
H67A	0.2894	0.0863	0.2665	0.066*
H67B	0.3200	0.0950	0.1875	0.066*
C69	0.3737 (6)	0.0387 (3)	0.3737 (6)	0.045 (3)
H69A	0.3532	0.0603	0.3800	0.054*
H69B	0.4328	0.0385	0.3943	0.054*
C70	0.3336 (6)	0.0156 (3)	0.4181 (6)	0.045 (3)
H70A	0.3522	−0.0063	0.4108	0.054*
H70B	0.3458	0.0207	0.4749	0.054*
O61	0.2480 (4)	0.01855 (18)	0.3866 (4)	0.0429 (18)
O62	0.1011 (4)	0.02498 (17)	0.3178 (4)	0.0381 (17)
O63	0.0719 (4)	0.03963 (17)	0.1590 (4)	0.0386 (17)
O64	0.2356 (4)	0.06106 (17)	0.1732 (4)	0.0460 (19)
O65	0.3572 (4)	0.03010 (18)	0.2938 (4)	0.049 (2)
C68	0.3717 (6)	0.0540 (3)	0.2400 (7)	0.054 (3)
H68A	0.3811	0.0436	0.1916	0.064*
H68B	0.4216	0.0657	0.2637	0.064*
C71	0.4066 (6)	0.9458 (3)	0.2910 (6)	0.042 (3)
C72	0.4894 (8)	0.9438 (3)	0.3204 (8)	0.064 (4)
H72	0.5264	0.9505	0.2892	0.077*
C73	0.5181 (9)	0.9321 (4)	0.3961 (9)	0.083 (5)
H73	0.5747	0.9303	0.4150	0.100*
C74	0.4670 (9)	0.9232 (3)	0.4431 (8)	0.076 (4)
H74	0.4876	0.9151	0.4942	0.091*
C75	0.3852 (9)	0.9260 (3)	0.4156 (7)	0.064 (4)
H75	0.3488	0.9206	0.4487	0.077*
C76	0.3549 (7)	0.9368 (3)	0.3389 (7)	0.047 (3)
C77	0.2147 (7)	0.9186 (3)	0.3144 (7)	0.048 (3)
H77A	0.1720	0.9265	0.3410	0.058*
H77B	0.2406	0.9000	0.3441	0.058*
C78	0.1781 (10)	0.9089 (3)	0.2327 (7)	0.071 (4)
H78A	0.2208	0.9015	0.2054	0.085*
H78B	0.1395	0.8913	0.2333	0.085*
C79	0.1063 (9)	0.9291 (3)	0.1093 (7)	0.067 (4)
H79A	0.0615	0.9135	0.1031	0.081*
H79B	0.1498	0.9201	0.0853	0.081*
C80	0.0770 (8)	0.9598 (3)	0.0705 (7)	0.061 (3)
H80A	0.0467	0.9552	0.0167	0.074*
H80B	0.0388	0.9696	0.0998	0.074*
C81	0.1874 (8)	0.9755 (3)	0.0081 (7)	0.058 (3)
H81A	0.1536	0.9775	−0.0452	0.070*
H81B	0.2089	0.9536	0.0148	0.070*
C82	0.2547 (8)	0.9987 (3)	0.0187 (7)	0.055 (3)
H82A	0.2835	0.9963	−0.0252	0.066*
H82B	0.2321	1.0204	0.0163	0.066*
C83	0.3691 (8)	0.9709 (3)	0.0877 (7)	0.056 (3)
H83A	0.4025	0.9771	0.0494	0.067*
H83B	0.3413	0.9508	0.0696	0.067*
C84	0.4216 (7)	0.9661 (3)	0.1648 (7)	0.055 (3)
H84A	0.4628	0.9497	0.1614	0.066*
H84B	0.4497	0.9861	0.1837	0.066*
O66	0.3710 (4)	0.95598 (18)	0.2173 (4)	0.0439 (18)
O67	0.2743 (5)	0.9431 (2)	0.3135 (6)	0.072 (3)
O68	0.1370 (5)	0.93576 (18)	0.1925 (4)	0.050 (2)
O69	0.1400 (5)	0.98217 (18)	0.0659 (4)	0.050 (2)
O70	0.3106 (5)	0.99490 (17)	0.0904 (4)	0.0491 (19)
O71	0.4926 (14)	0.2158 (5)	0.9946 (14)	0.226 (9)*
H71	0.5001	0.2080	1.0400	0.338*
C85	0.429 (2)	0.2000 (9)	0.946 (2)	0.251 (16)*
H85A	0.3869	0.2153	0.9243	0.376*
H85B	0.4071	0.1840	0.9769	0.376*
H85C	0.4492	0.1896	0.9035	0.376*
O1W	0.6608 (5)	0.24538 (19)	0.6796 (4)	0.052 (2)
O2W	0.2199 (5)	0.99772 (18)	0.2171 (4)	0.052 (2)
O3W	0.1932 (5)	0.13447 (19)	0.6450 (5)	0.056 (2)
O4W	0.1121 (14)	0.1487 (6)	0.2817 (14)	0.248*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
W1	0.01851 (19)	0.0284 (2)	0.0273 (2)	0.00087 (16)	0.00063 (15)	0.00311 (16)
W2	0.0235 (2)	0.0287 (2)	0.02187 (19)	−0.00152 (16)	0.00257 (14)	0.00042 (16)
W3	0.0226 (2)	0.02211 (19)	0.02577 (19)	−0.00213 (15)	0.00170 (15)	−0.00028 (15)
W4	0.0263 (2)	0.0214 (2)	0.0313 (2)	0.00210 (16)	0.00666 (16)	0.00114 (16)
W5	0.0262 (2)	0.0227 (2)	0.0277 (2)	−0.00144 (16)	0.00708 (15)	0.00332 (16)
W6	0.0226 (2)	0.0283 (2)	0.0295 (2)	−0.00010 (16)	0.00820 (15)	−0.00064 (16)
W7	0.0232 (2)	0.0227 (2)	0.0336 (2)	0.00327 (16)	0.00570 (16)	0.00283 (16)
W8	0.0236 (2)	0.0241 (2)	0.0276 (2)	−0.00179 (16)	0.00252 (15)	0.00603 (16)
W9	0.02059 (19)	0.0276 (2)	0.02573 (19)	0.00017 (16)	0.00606 (15)	0.00099 (16)
W10	0.0256 (2)	0.0255 (2)	0.0259 (2)	−0.00601 (16)	0.00346 (15)	−0.00150 (16)
W11	0.01786 (19)	0.0348 (2)	0.0269 (2)	0.00014 (16)	0.00026 (15)	−0.00041 (17)
W12	0.0254 (2)	0.0298 (2)	0.02139 (19)	−0.00202 (16)	0.00055 (15)	0.00149 (16)
P1	0.0200 (12)	0.0206 (12)	0.0205 (11)	0.0011 (9)	0.0028 (9)	0.0010 (9)
O1	0.020 (3)	0.021 (3)	0.030 (3)	0.001 (3)	0.001 (3)	0.002 (3)
O2	0.020 (3)	0.032 (4)	0.024 (3)	0.001 (3)	0.007 (2)	0.008 (3)
O3	0.022 (3)	0.025 (3)	0.026 (3)	−0.004 (3)	0.003 (3)	0.006 (3)
O4	0.024 (3)	0.027 (4)	0.027 (3)	−0.002 (3)	0.003 (3)	0.001 (3)
O5	0.016 (3)	0.044 (4)	0.038 (4)	0.006 (3)	−0.002 (3)	0.004 (3)
O6	0.039 (4)	0.036 (4)	0.026 (3)	−0.001 (3)	0.006 (3)	0.001 (3)
O7	0.031 (4)	0.030 (4)	0.036 (4)	−0.008 (3)	−0.002 (3)	−0.003 (3)
O8	0.026 (3)	0.028 (4)	0.032 (4)	0.000 (3)	0.006 (3)	0.006 (3)
O9	0.030 (4)	0.027 (4)	0.028 (3)	0.004 (3)	0.006 (3)	0.001 (3)
O10	0.021 (3)	0.030 (4)	0.032 (4)	0.003 (3)	0.007 (3)	0.004 (3)
O11	0.028 (4)	0.029 (4)	0.027 (3)	0.000 (3)	0.004 (3)	−0.001 (3)
O12	0.029 (4)	0.026 (4)	0.029 (3)	−0.001 (3)	0.007 (3)	−0.002 (3)
O13	0.031 (4)	0.030 (4)	0.029 (3)	0.005 (3)	0.002 (3)	0.004 (3)
O14	0.024 (3)	0.026 (4)	0.029 (3)	−0.004 (3)	0.008 (3)	0.001 (3)
O15	0.020 (3)	0.029 (4)	0.033 (4)	−0.002 (3)	0.002 (3)	0.001 (3)
O16	0.028 (4)	0.027 (4)	0.032 (4)	0.002 (3)	0.002 (3)	0.005 (3)
O17	0.032 (4)	0.021 (3)	0.033 (4)	0.003 (3)	0.008 (3)	0.002 (3)
O18	0.040 (4)	0.035 (4)	0.034 (4)	0.000 (3)	0.011 (3)	0.009 (3)
O19	0.024 (3)	0.038 (4)	0.033 (4)	−0.005 (3)	0.009 (3)	0.000 (3)
O20	0.031 (4)	0.033 (4)	0.030 (4)	−0.001 (3)	0.009 (3)	0.003 (3)
O21	0.032 (4)	0.027 (4)	0.030 (3)	−0.002 (3)	0.011 (3)	−0.002 (3)
O22	0.028 (4)	0.030 (4)	0.049 (4)	0.013 (3)	0.000 (3)	0.003 (3)
O23	0.025 (3)	0.038 (4)	0.028 (3)	0.000 (3)	0.000 (3)	0.000 (3)
O24	0.038 (4)	0.039 (4)	0.030 (4)	−0.009 (3)	0.001 (3)	0.011 (3)
O25	0.025 (3)	0.031 (4)	0.032 (4)	−0.001 (3)	0.001 (3)	0.000 (3)
O26	0.028 (4)	0.036 (4)	0.038 (4)	−0.002 (3)	0.012 (3)	−0.007 (3)
O27	0.030 (4)	0.032 (4)	0.031 (4)	−0.004 (3)	0.003 (3)	0.000 (3)
O28	0.039 (4)	0.022 (4)	0.047 (4)	0.003 (3)	0.011 (3)	0.000 (3)
O29	0.024 (3)	0.035 (4)	0.032 (4)	0.002 (3)	0.007 (3)	0.002 (3)
O30	0.034 (4)	0.034 (4)	0.032 (4)	−0.005 (3)	0.005 (3)	0.002 (3)
O31	0.026 (3)	0.036 (4)	0.030 (4)	−0.002 (3)	0.003 (3)	0.004 (3)
O32	0.028 (4)	0.033 (4)	0.037 (4)	0.007 (3)	−0.002 (3)	0.005 (3)
O33	0.030 (4)	0.023 (3)	0.031 (4)	0.000 (3)	−0.003 (3)	−0.004 (3)
O34	0.023 (3)	0.035 (4)	0.034 (4)	−0.002 (3)	0.004 (3)	−0.004 (3)
O35	0.031 (4)	0.031 (4)	0.025 (3)	0.000 (3)	0.009 (3)	0.001 (3)
O36	0.030 (4)	0.033 (4)	0.029 (4)	−0.005 (3)	0.001 (3)	−0.001 (3)
O37	0.031 (4)	0.024 (3)	0.029 (3)	0.000 (3)	0.006 (3)	0.005 (3)
O38	0.037 (4)	0.033 (4)	0.045 (4)	−0.009 (3)	0.011 (3)	−0.012 (3)
O39	0.020 (3)	0.050 (5)	0.037 (4)	−0.001 (3)	−0.005 (3)	0.002 (3)
O40	0.031 (4)	0.042 (4)	0.032 (4)	−0.005 (3)	0.001 (3)	0.003 (3)
C1	0.047 (7)	0.054 (7)	0.031 (6)	0.005 (6)	0.015 (5)	0.008 (5)
C2	0.037 (7)	0.076 (9)	0.048 (7)	0.005 (6)	0.015 (5)	0.002 (6)
C3	0.040 (7)	0.056 (8)	0.054 (7)	0.015 (6)	−0.003 (5)	−0.008 (6)
C4	0.057 (8)	0.048 (7)	0.043 (7)	0.012 (6)	0.005 (6)	0.004 (5)
C5	0.048 (7)	0.033 (6)	0.042 (6)	−0.003 (5)	0.012 (5)	−0.001 (5)
C6	0.036 (6)	0.041 (6)	0.040 (6)	−0.002 (5)	0.011 (5)	−0.002 (5)
C7	0.034 (6)	0.045 (7)	0.063 (8)	−0.004 (5)	0.012 (5)	0.016 (6)
C8	0.046 (7)	0.045 (7)	0.072 (9)	0.003 (6)	0.008 (6)	0.003 (6)
C9	0.054 (8)	0.058 (9)	0.071 (9)	−0.005 (6)	0.013 (6)	−0.023 (7)
C10	0.061 (8)	0.056 (8)	0.055 (8)	0.003 (7)	0.003 (6)	−0.014 (6)
C11	0.071 (9)	0.080 (10)	0.050 (8)	−0.006 (8)	0.008 (7)	−0.023 (7)
C12	0.056 (8)	0.104 (12)	0.044 (7)	−0.003 (8)	0.011 (6)	0.013 (7)
C14	0.036 (7)	0.128 (13)	0.056 (8)	0.015 (8)	0.024 (6)	0.031 (8)
O41	0.038 (4)	0.088 (7)	0.056 (5)	0.013 (4)	0.023 (4)	0.026 (5)
O42	0.031 (4)	0.048 (5)	0.051 (5)	0.000 (3)	0.012 (3)	0.003 (4)
O43	0.041 (4)	0.036 (4)	0.056 (5)	0.000 (3)	0.007 (4)	−0.007 (4)
O44	0.045 (5)	0.057 (5)	0.049 (5)	−0.005 (4)	0.012 (4)	−0.016 (4)
O45	0.057 (6)	0.114 (8)	0.052 (5)	0.023 (5)	0.023 (4)	0.019 (5)
C15	0.044 (7)	0.103 (12)	0.035 (7)	−0.006 (7)	−0.006 (5)	0.004 (7)
C16	0.082 (11)	0.124 (14)	0.044 (8)	−0.028 (10)	0.002 (7)	0.005 (8)
C17	0.069 (10)	0.120 (14)	0.068 (10)	−0.044 (10)	0.011 (8)	−0.014 (9)
C18	0.066 (10)	0.094 (12)	0.073 (10)	−0.009 (9)	−0.016 (8)	−0.005 (9)
C19	0.069 (9)	0.092 (11)	0.051 (8)	−0.021 (8)	0.021 (7)	−0.002 (7)
C20	0.027 (7)	0.087 (11)	0.076 (9)	−0.014 (7)	−0.006 (6)	0.012 (8)
O46	0.070 (6)	0.098 (8)	0.062 (6)	−0.023 (6)	0.014 (5)	0.015 (5)
O47	0.092 (7)	0.088 (7)	0.060 (6)	0.009 (6)	0.032 (5)	0.011 (5)
O48	0.071 (7)	0.108 (9)	0.083 (7)	−0.007 (6)	0.020 (5)	−0.033 (6)
O49	0.070 (7)	0.123 (10)	0.115 (9)	0.029 (6)	0.035 (6)	0.027 (7)
O50	0.084 (7)	0.076 (7)	0.079 (7)	0.005 (6)	−0.007 (5)	−0.004 (5)
C29	0.040 (6)	0.027 (6)	0.058 (7)	0.003 (5)	0.003 (5)	0.006 (5)
C30	0.031 (6)	0.039 (7)	0.068 (8)	−0.005 (5)	−0.012 (5)	−0.009 (6)
C31	0.038 (7)	0.068 (9)	0.052 (7)	0.002 (6)	−0.005 (5)	−0.002 (6)
C32	0.027 (6)	0.058 (8)	0.050 (7)	0.005 (5)	−0.005 (5)	0.012 (6)
C33	0.047 (7)	0.034 (6)	0.058 (7)	−0.007 (5)	0.009 (6)	0.002 (5)
C34	0.030 (6)	0.026 (6)	0.046 (6)	0.005 (4)	0.009 (5)	−0.001 (5)
O51	0.041 (5)	0.036 (4)	0.079 (6)	−0.003 (4)	−0.006 (4)	0.017 (4)
O52	0.057 (5)	0.035 (4)	0.038 (4)	−0.009 (4)	−0.007 (3)	0.000 (3)
O53	0.096 (7)	0.069 (6)	0.049 (5)	0.007 (5)	−0.007 (5)	−0.006 (5)
O54	0.051 (5)	0.113 (8)	0.066 (6)	0.000 (5)	0.017 (4)	−0.007 (6)
O55	0.076 (7)	0.178 (12)	0.065 (6)	−0.051 (7)	0.008 (5)	0.031 (7)
C43	0.040 (6)	0.037 (6)	0.039 (6)	0.008 (5)	0.018 (5)	0.001 (5)
C44	0.053 (7)	0.045 (7)	0.030 (6)	−0.003 (5)	0.008 (5)	−0.001 (5)
C45	0.065 (8)	0.042 (7)	0.048 (7)	0.006 (6)	0.018 (6)	0.014 (6)
C46	0.074 (9)	0.054 (8)	0.065 (9)	−0.002 (7)	0.011 (7)	0.020 (7)
C47	0.063 (8)	0.058 (9)	0.061 (8)	−0.027 (7)	0.010 (6)	0.005 (7)
C48	0.038 (6)	0.058 (8)	0.042 (6)	−0.007 (6)	0.005 (5)	0.008 (6)
C49	0.049 (8)	0.079 (10)	0.049 (7)	−0.023 (7)	−0.003 (6)	0.006 (7)
C50	0.041 (7)	0.076 (10)	0.066 (8)	0.000 (7)	0.002 (6)	−0.002 (7)
C53	0.089 (10)	0.064 (9)	0.047 (7)	0.039 (8)	0.027 (7)	0.015 (7)
C54	0.096 (10)	0.031 (7)	0.053 (8)	−0.008 (6)	0.016 (7)	−0.010 (6)
C55	0.089 (10)	0.034 (7)	0.044 (7)	−0.006 (6)	0.013 (6)	−0.001 (5)
C56	0.065 (8)	0.044 (7)	0.044 (7)	−0.009 (6)	0.004 (6)	−0.008 (6)
O56	0.055 (5)	0.034 (4)	0.054 (5)	−0.002 (4)	0.002 (4)	0.005 (4)
O57	0.056 (5)	0.059 (6)	0.051 (5)	−0.010 (4)	−0.006 (4)	−0.002 (4)
O58	0.047 (5)	0.070 (6)	0.066 (6)	−0.009 (4)	−0.017 (4)	0.025 (5)
O59	0.049 (5)	0.050 (5)	0.053 (5)	−0.011 (4)	0.000 (4)	0.012 (4)
O60	0.058 (5)	0.032 (4)	0.044 (4)	−0.002 (4)	0.007 (4)	0.006 (3)
C57	0.037 (6)	0.029 (5)	0.029 (5)	0.007 (5)	0.003 (4)	0.000 (4)
C58	0.036 (6)	0.042 (7)	0.050 (7)	0.007 (5)	0.005 (5)	−0.001 (5)
C59	0.057 (8)	0.040 (7)	0.051 (7)	0.014 (6)	0.002 (6)	0.009 (6)
C60	0.046 (7)	0.047 (7)	0.053 (7)	−0.004 (6)	0.006 (6)	0.005 (6)
C61	0.040 (6)	0.026 (6)	0.057 (7)	0.003 (5)	0.015 (5)	0.000 (5)
C62	0.037 (6)	0.026 (5)	0.027 (5)	0.007 (4)	0.006 (4)	0.001 (4)
C63	0.031 (6)	0.046 (7)	0.041 (6)	0.006 (5)	0.004 (5)	0.005 (5)
C64	0.042 (7)	0.065 (8)	0.043 (7)	0.016 (6)	0.013 (5)	0.010 (6)
C65	0.024 (5)	0.057 (7)	0.041 (6)	0.003 (5)	0.001 (4)	0.006 (5)
C66	0.052 (7)	0.036 (7)	0.064 (8)	0.000 (6)	0.023 (6)	0.008 (6)
C67	0.034 (7)	0.051 (8)	0.080 (9)	−0.011 (6)	0.011 (6)	0.001 (6)
C69	0.024 (6)	0.054 (7)	0.055 (7)	−0.010 (5)	0.005 (5)	−0.015 (6)
C70	0.018 (5)	0.053 (7)	0.052 (7)	−0.002 (5)	−0.016 (5)	−0.001 (6)
O61	0.021 (4)	0.063 (5)	0.041 (4)	0.000 (3)	−0.002 (3)	−0.001 (4)
O62	0.020 (4)	0.053 (5)	0.041 (4)	0.002 (3)	0.003 (3)	0.010 (3)
O63	0.036 (4)	0.045 (4)	0.035 (4)	0.004 (3)	0.007 (3)	0.005 (3)
O64	0.033 (4)	0.036 (4)	0.067 (5)	−0.004 (3)	0.004 (4)	0.004 (4)
O65	0.040 (4)	0.052 (5)	0.056 (5)	−0.013 (4)	0.007 (4)	−0.009 (4)
C68	0.030 (6)	0.054 (8)	0.079 (9)	−0.015 (6)	0.016 (6)	0.009 (7)
C71	0.039 (6)	0.035 (6)	0.054 (7)	0.007 (5)	0.015 (5)	−0.001 (5)
C72	0.050 (8)	0.072 (10)	0.075 (9)	0.001 (7)	0.023 (7)	0.004 (7)
C73	0.057 (9)	0.089 (12)	0.088 (11)	−0.024 (8)	−0.023 (8)	0.022 (9)
C74	0.079 (11)	0.072 (10)	0.066 (9)	−0.009 (8)	−0.012 (8)	0.013 (8)
C75	0.101 (11)	0.038 (7)	0.059 (8)	0.010 (7)	0.030 (8)	0.009 (6)
C76	0.040 (7)	0.038 (7)	0.070 (8)	0.011 (5)	0.024 (6)	0.003 (6)
C77	0.053 (7)	0.045 (7)	0.054 (7)	−0.005 (6)	0.026 (6)	0.004 (6)
C78	0.132 (13)	0.035 (7)	0.050 (8)	0.000 (8)	0.028 (8)	0.010 (6)
C79	0.106 (11)	0.052 (8)	0.041 (7)	−0.020 (8)	0.006 (7)	−0.008 (6)
C80	0.068 (9)	0.060 (9)	0.052 (8)	−0.011 (7)	−0.001 (6)	−0.005 (6)
C81	0.082 (9)	0.058 (8)	0.037 (7)	0.013 (7)	0.018 (6)	−0.002 (6)
C82	0.086 (10)	0.038 (7)	0.048 (7)	0.004 (6)	0.032 (7)	0.015 (6)
C83	0.074 (9)	0.056 (8)	0.048 (7)	0.011 (7)	0.035 (7)	−0.001 (6)
C84	0.055 (8)	0.059 (8)	0.060 (8)	0.003 (6)	0.031 (6)	−0.001 (6)
O66	0.032 (4)	0.055 (5)	0.050 (5)	0.006 (3)	0.019 (3)	0.016 (4)
O67	0.044 (5)	0.069 (6)	0.103 (7)	0.008 (4)	0.011 (5)	0.045 (5)
O68	0.073 (6)	0.041 (5)	0.036 (4)	−0.003 (4)	0.009 (4)	−0.002 (3)
O69	0.069 (5)	0.044 (5)	0.041 (4)	0.004 (4)	0.019 (4)	−0.002 (4)
O70	0.067 (5)	0.042 (5)	0.043 (4)	0.005 (4)	0.020 (4)	0.003 (4)
O1W	0.051 (5)	0.051 (5)	0.054 (5)	0.001 (4)	0.016 (4)	0.001 (4)
O2W	0.066 (5)	0.041 (5)	0.047 (5)	−0.012 (4)	0.006 (4)	0.000 (4)
O3W	0.058 (5)	0.048 (5)	0.062 (5)	0.000 (4)	0.012 (4)	−0.006 (4)

Geometric parameters (Å, º) top

W1—O5	1.699 (6)	C31—C32	1.354 (16)
W1—O8	1.886 (6)	C31—H31	0.950
W1—O10	1.908 (6)	C32—C33	1.403 (15)
W1—O16	1.915 (6)	C32—H32	0.950
W1—O15	1.939 (6)	C33—C34	1.373 (14)
W1—O1	2.443 (6)	C33—H33	0.950
W2—O6	1.686 (6)	C34—O52	1.363 (11)
W2—O9	1.896 (6)	C35—O52	1.420 (13)
W2—O12	1.905 (6)	C35—C36	1.472 (17)
W2—O8	1.935 (6)	C35—H35A	0.990
W2—O11	1.936 (6)	C35—H35B	0.990
W2—O2	2.444 (6)	C36—O53	1.320 (15)
W3—O7	1.688 (6)	C36—H36A	0.990
W3—O14	1.900 (6)	C36—H36B	0.990
W3—O10	1.904 (6)	C37—C38	1.453 (17)
W3—O9	1.908 (6)	C37—O53	1.461 (15)
W3—O13	1.920 (6)	C37—H37A	0.990
W3—O4	2.444 (6)	C37—H37B	0.990
W4—O28	1.698 (6)	C38—O54	1.526 (15)
W4—O34	1.899 (6)	C38—H38A	0.990
W4—O27	1.900 (6)	C38—H38B	0.990
W4—O17	1.922 (6)	C39—O54	1.321 (18)
W4—O16	1.928 (6)	C39—C40	1.470 (19)
W4—O1	2.432 (6)	C39—H39A	0.990
W5—O18	1.695 (6)	C39—H39B	0.990
W5—O17	1.889 (6)	C40—O55	1.432 (17)
W5—O11	1.904 (6)	C40—H40A	0.990
W5—O29	1.915 (6)	C40—H40B	0.990
W5—O19	1.922 (6)	C41—O55	1.249 (17)
W5—O2	2.421 (6)	C41—C42	1.463 (19)
W6—O20	1.686 (6)	C41—H41A	0.990
W6—O30	1.893 (6)	C41—H41B	0.990
W6—O19	1.909 (6)	C42—O51	1.467 (15)
W6—O21	1.916 (6)	C42—H42A	0.990
W6—O12	1.931 (6)	C42—H42B	0.990
W6—O2	2.435 (6)	C43—C44	1.374 (14)
W7—O22	1.704 (6)	C43—O56	1.383 (12)
W7—O21	1.904 (6)	C43—C48	1.390 (15)
W7—O13	1.911 (6)	C44—C45	1.403 (15)
W7—O31	1.912 (6)	C44—H44	0.950
W7—O23	1.915 (6)	C45—C46	1.383 (17)
W7—O4	2.447 (6)	C45—H45	0.950
W8—O24	1.687 (6)	C46—C47	1.392 (17)
W8—O32	1.892 (6)	C46—H46	0.950
W8—O25	1.910 (6)	C47—C48	1.364 (16)
W8—O23	1.911 (6)	C47—H47	0.950
W8—O14	1.928 (6)	C48—O57	1.390 (13)
W8—O4	2.458 (6)	C49—O57	1.399 (13)
W9—O26	1.696 (6)	C49—C50	1.491 (16)
W9—O15	1.898 (6)	C49—H49A	0.990
W9—O25	1.898 (6)	C49—H49B	0.990
W9—O33	1.926 (6)	C50—O58	1.397 (14)
W9—O27	1.929 (6)	C50—H50A	0.990
W9—O1	2.444 (6)	C50—H50B	0.990
W10—O38	1.697 (6)	C51—O58	1.391 (16)
W10—O29	1.896 (6)	C51—C52	1.452 (19)
W10—O35	1.901 (6)	C51—H51A	0.990
W10—O37	1.906 (6)	C51—H51B	0.990
W10—O34	1.917 (6)	C52—O59	1.421 (18)
W10—O3	2.447 (6)	C52—H52A	0.990
W11—O39	1.693 (6)	C52—H52B	0.990
W11—O36	1.900 (6)	C53—O59	1.382 (14)
W11—O31	1.904 (6)	C53—C54	1.494 (17)
W11—O30	1.915 (6)	C53—H53A	0.990
W11—O35	1.928 (6)	C53—H53B	0.990
W11—O3	2.458 (6)	C54—O60	1.429 (13)
W12—O40	1.687 (6)	C54—H54A	0.990
W12—O33	1.889 (6)	C54—H54B	0.990
W12—O37	1.922 (6)	C55—O60	1.428 (13)
W12—O32	1.922 (7)	C55—C56	1.487 (15)
W12—O36	1.930 (6)	C55—H55A	0.990
W12—O3	2.441 (6)	C55—H55B	0.990
P1—O4	1.517 (6)	C56—O56	1.427 (13)
P1—O3	1.525 (6)	C56—H56A	0.990
P1—O2	1.542 (6)	C56—H56B	0.990
P1—O1	1.543 (6)	C57—O61	1.370 (11)
C1—C6	1.373 (14)	C57—C58	1.379 (14)
C1—O41	1.392 (12)	C57—C62	1.389 (13)
C1—C2	1.394 (15)	C58—C59	1.400 (15)
C2—C3	1.385 (16)	C58—H58	0.950
C2—H2	0.950	C59—C60	1.355 (15)
C3—C4	1.356 (15)	C59—H59	0.950
C3—H3	0.950	C60—C61	1.405 (15)
C4—C5	1.374 (15)	C60—H60	0.950
C4—H4	0.950	C61—C62	1.386 (13)
C5—C6	1.386 (14)	C61—H61	0.950
C5—H5	0.950	C62—O62	1.359 (11)
C6—O42	1.378 (12)	C63—O62	1.429 (11)
C7—O42	1.449 (12)	C63—C64	1.491 (14)
C7—C8	1.493 (16)	C63—H63A	0.990
C7—H7A	0.990	C63—H63B	0.990
C7—H7B	0.990	C64—O63	1.426 (12)
C8—O43	1.424 (13)	C64—H64A	0.990
C8—H8A	0.990	C64—H64B	0.990
C8—H8B	0.990	C65—O63	1.425 (12)
C9—O43	1.414 (13)	C65—C66	1.499 (15)
C9—C10	1.481 (17)	C65—H65A	0.990
C9—H9A	0.990	C65—H65B	0.990
C9—H9B	0.990	C66—O64	1.422 (13)
C10—O44	1.419 (14)	C66—H66A	0.990
C10—H10A	0.990	C66—H66B	0.990
C10—H10B	0.990	C67—O64	1.430 (13)
C11—O44	1.425 (14)	C67—C68	1.501 (16)
C11—C12	1.481 (17)	C67—H67A	0.990
C11—H11A	0.990	C67—H67B	0.990
C11—H11B	0.990	C69—O65	1.408 (12)
C12—O45	1.408 (14)	C69—C70	1.487 (15)
C12—H12A	0.990	C69—H69A	0.990
C12—H12B	0.990	C69—H69B	0.990
C13—O45	1.313 (17)	C70—O61	1.444 (11)
C13—C14	1.550 (19)	C70—H70A	0.990
C13—H13A	0.990	C70—H70B	0.990
C13—H13B	0.990	O65—C68	1.429 (13)
C14—O41	1.427 (12)	C68—H68A	0.990
C14—H14A	0.990	C68—H68B	0.990
C14—H14B	0.990	C71—O66	1.369 (12)
C15—C20	1.318 (17)	C71—C76	1.377 (14)
C15—C16	1.363 (18)	C71—C72	1.391 (16)
C15—O46	1.378 (15)	C72—C73	1.398 (18)
C16—C17	1.41 (2)	C72—H72	0.950
C16—H16	0.950	C73—C74	1.355 (19)
C17—C18	1.371 (19)	C73—H73	0.950
C17—H17	0.950	C74—C75	1.374 (18)
C18—C19	1.425 (18)	C74—H74	0.950
C18—H18	0.950	C75—C76	1.405 (16)
C19—C20	1.393 (18)	C75—H75	0.950
C19—H19	0.950	C76—O67	1.369 (13)
C20—O47	1.389 (14)	C77—O67	1.446 (13)
C21—O47	1.365 (15)	C77—C78	1.488 (16)
C21—C22	1.469 (19)	C77—H77A	0.990
C21—H21A	0.990	C77—H77B	0.990
C21—H21B	0.990	C78—O68	1.434 (14)
C22—O48	1.373 (16)	C78—H78A	0.990
C22—H22A	0.990	C78—H78B	0.990
C22—H22B	0.990	C79—O68	1.462 (13)
C23—O48	1.385 (17)	C79—C80	1.496 (17)
C23—C24	1.461 (19)	C79—H79A	0.990
C23—H23A	0.990	C79—H79B	0.990
C23—H23B	0.990	C80—O69	1.436 (14)
C24—O49	1.395 (18)	C80—H80A	0.990
C24—H24A	0.990	C80—H80B	0.990
C24—H24B	0.990	C81—O69	1.434 (13)
C25—O49	1.38 (2)	C81—C82	1.480 (17)
C25—C26	1.472 (19)	C81—H81A	0.990
C25—H25A	0.990	C81—H81B	0.990
C25—H25B	0.990	C82—O70	1.412 (13)
C26—O50	1.433 (19)	C82—H82A	0.990
C26—H26A	0.990	C82—H82B	0.990
C26—H26B	0.990	C83—O70	1.419 (13)
C27—O50	1.400 (16)	C83—C84	1.465 (16)
C27—C28	1.513 (19)	C83—H83A	0.990
C27—H27A	0.990	C83—H83B	0.990
C27—H27B	0.990	C84—O66	1.436 (12)
C28—O46	1.410 (15)	C84—H84A	0.990
C28—H28A	0.990	C84—H84B	0.990
C28—H28B	0.990	O71—C85	1.39 (3)
C29—C30	1.353 (15)	O71—H71	0.840
C29—O51	1.382 (12)	C85—H85A	0.980
C29—C34	1.430 (14)	C85—H85B	0.980
C30—C31	1.379 (16)	C85—H85C	0.980
C30—H30	0.950

O1W···O42	2.965 (10)	O2W···O69	2.780 (10)
O1W···O43	2.962 (11)	O2W···O70	2.929 (11)
O1W···O44	2.885 (10)	O3W···O51	2.873 (11)
O1W···O45	2.913 (11)	O3W···O53	2.915 (12)
O1W···O46	2.989 (13)	O3W···O54	2.914 (12)
O1W···O48	2.928 (12)	O3W···O55	2.976 (12)
O1W···O49	2.884 (13)	O3W···O58	2.881 (11)
O2W···O64ⁱ	2.801 (10)	O3W···O59	2.887 (11)
O2W···O65ⁱ	2.786 (10)	O3W···O60	2.974 (11)
O2W···O67	2.884 (11)	O4W···O46ⁱⁱ	3.07 (3)
O2W···O68	2.951 (10)

O5—W1—O8	102.7 (3)	H22A—C22—H22B	108.1
O5—W1—O10	103.1 (3)	O48—C23—C24	117.9 (15)
O8—W1—O10	86.3 (3)	O48—C23—H23A	107.8
O5—W1—O16	101.9 (3)	C24—C23—H23A	107.8
O8—W1—O16	90.1 (3)	O48—C23—H23B	107.8
O10—W1—O16	155.0 (2)	C24—C23—H23B	107.8
O5—W1—O15	101.2 (3)	H23A—C23—H23B	107.2
O8—W1—O15	156.0 (2)	O49—C24—C23	109.7 (14)
O10—W1—O15	87.0 (3)	O49—C24—H24A	109.7
O16—W1—O15	86.3 (3)	C23—C24—H24A	109.7
O5—W1—O1	170.2 (3)	O49—C24—H24B	109.7
O8—W1—O1	85.1 (2)	C23—C24—H24B	109.7
O10—W1—O1	83.2 (2)	H24A—C24—H24B	108.2
O16—W1—O1	71.8 (2)	O49—C25—C26	115.4 (16)
O15—W1—O1	71.2 (2)	O49—C25—H25A	108.4
O6—W2—O9	103.3 (3)	C26—C25—H25A	108.4
O6—W2—O12	101.5 (3)	O49—C25—H25B	108.4
O9—W2—O12	90.8 (3)	C26—C25—H25B	108.4
O6—W2—O8	102.7 (3)	H25A—C25—H25B	107.5
O9—W2—O8	84.9 (3)	O50—C26—C25	113.1 (16)
O12—W2—O8	155.9 (2)	O50—C26—H26A	109.0
O6—W2—O11	101.6 (3)	C25—C26—H26A	109.0
O9—W2—O11	155.0 (2)	O50—C26—H26B	109.0
O12—W2—O11	87.0 (3)	C25—C26—H26B	109.0
O8—W2—O11	87.0 (3)	H26A—C26—H26B	107.8
O6—W2—O2	170.7 (3)	O50—C27—C28	104.3 (12)
O9—W2—O2	83.9 (2)	O50—C27—H27A	110.9
O12—W2—O2	72.2 (2)	C28—C27—H27A	110.9
O8—W2—O2	83.7 (2)	O50—C27—H27B	110.9
O11—W2—O2	71.8 (2)	C28—C27—H27B	110.9
O7—W3—O14	101.7 (3)	H27A—C27—H27B	108.9
O7—W3—O10	103.0 (3)	O46—C28—C27	105.9 (12)
O14—W3—O10	89.5 (3)	O46—C28—H28A	110.5
O7—W3—O9	102.7 (3)	C27—C28—H28A	110.5
O14—W3—O9	155.6 (3)	O46—C28—H28B	110.5
O10—W3—O9	84.9 (3)	C27—C28—H28B	110.5
O7—W3—O13	102.0 (3)	H28A—C28—H28B	108.7
O14—W3—O13	87.5 (3)	C15—O46—C28	119.7 (11)
O10—W3—O13	154.9 (3)	C21—O47—C20	120.4 (11)
O9—W3—O13	87.6 (3)	C22—O48—C23	119.9 (12)
O7—W3—O4	171.5 (3)	C25—O49—C24	112.9 (12)
O14—W3—O4	72.6 (2)	C27—O50—C26	111.5 (12)
O10—W3—O4	83.5 (2)	C30—C29—O51	122.7 (10)
O9—W3—O4	83.2 (2)	C30—C29—C34	120.4 (10)
O13—W3—O4	71.8 (2)	O51—C29—C34	116.7 (9)
O28—W4—O34	102.4 (3)	C29—C30—C31	121.4 (10)
O28—W4—O27	101.6 (3)	C29—C30—H30	119.3
O34—W4—O27	89.7 (3)	C31—C30—H30	119.3
O28—W4—O17	103.6 (3)	C32—C31—C30	119.1 (11)
O34—W4—O17	85.4 (3)	C32—C31—H31	120.5
O27—W4—O17	154.8 (3)	C30—C31—H31	120.5
O28—W4—O16	101.5 (3)	C31—C32—C33	121.2 (11)
O34—W4—O16	156.0 (3)	C31—C32—H32	119.4
O27—W4—O16	87.8 (3)	C33—C32—H32	119.4
O17—W4—O16	86.7 (3)	C34—C33—C32	120.3 (10)
O28—W4—O1	170.6 (3)	C34—C33—H33	119.9
O34—W4—O1	84.6 (2)	C32—C33—H33	119.9
O27—W4—O1	72.0 (2)	O52—C34—C33	126.0 (9)
O17—W4—O1	83.0 (2)	O52—C34—C29	116.4 (8)
O16—W4—O1	71.9 (2)	C33—C34—C29	117.6 (9)
O18—W5—O17	102.8 (3)	O52—C35—C36	107.3 (10)
O18—W5—O11	101.4 (3)	O52—C35—H35A	110.3
O17—W5—O11	90.1 (3)	C36—C35—H35A	110.3
O18—W5—O29	102.2 (3)	O52—C35—H35B	110.3
O17—W5—O29	85.7 (3)	C36—C35—H35B	110.3
O11—W5—O29	156.3 (3)	H35A—C35—H35B	108.5
O18—W5—O19	101.1 (3)	O53—C36—C35	115.1 (12)
O17—W5—O19	156.0 (3)	O53—C36—H36A	108.5
O11—W5—O19	86.9 (3)	C35—C36—H36A	108.5
O29—W5—O19	87.5 (3)	O53—C36—H36B	108.5
O18—W5—O2	171.0 (3)	C35—C36—H36B	108.5
O17—W5—O2	84.3 (2)	H36A—C36—H36B	107.5
O11—W5—O2	72.8 (2)	C38—C37—O53	113.3 (11)
O29—W5—O2	83.6 (2)	C38—C37—H37A	108.9
O19—W5—O2	72.1 (2)	O53—C37—H37A	108.9
O20—W6—O30	102.4 (3)	C38—C37—H37B	108.9
O20—W6—O19	102.1 (3)	O53—C37—H37B	108.9
O30—W6—O19	90.0 (3)	H37A—C37—H37B	107.7
O20—W6—O21	102.9 (3)	C37—C38—O54	109.8 (11)
O30—W6—O21	85.9 (3)	C37—C38—H38A	109.7
O19—W6—O21	154.9 (2)	O54—C38—H38A	109.7
O20—W6—O12	101.6 (3)	C37—C38—H38B	109.7
O30—W6—O12	156.0 (3)	O54—C38—H38B	109.7
O19—W6—O12	86.6 (3)	H38A—C38—H38B	108.2
O21—W6—O12	87.2 (3)	O54—C39—C40	112.4 (15)
O20—W6—O2	171.3 (2)	O54—C39—H39A	109.1
O30—W6—O2	84.2 (2)	C40—C39—H39A	109.1
O19—W6—O2	71.9 (2)	O54—C39—H39B	109.1
O21—W6—O2	83.0 (2)	C40—C39—H39B	109.1
O12—W6—O2	72.1 (2)	H39A—C39—H39B	107.8
O22—W7—O21	103.1 (3)	O55—C40—C39	112.6 (14)
O22—W7—O13	101.4 (3)	O55—C40—H40A	109.1
O21—W7—O13	88.5 (3)	C39—C40—H40A	109.1
O22—W7—O31	102.8 (3)	O55—C40—H40B	109.1
O21—W7—O31	86.1 (3)	C39—C40—H40B	109.1
O13—W7—O31	155.8 (3)	H40A—C40—H40B	107.8
O22—W7—O23	101.8 (3)	O55—C41—C42	117.5 (14)
O21—W7—O23	155.1 (3)	O55—C41—H41A	107.9
O13—W7—O23	87.4 (3)	C42—C41—H41A	107.9
O31—W7—O23	87.7 (3)	O55—C41—H41B	107.9
O22—W7—O4	170.8 (3)	C42—C41—H41B	107.9
O21—W7—O4	83.4 (2)	H41A—C41—H41B	107.2
O13—W7—O4	71.9 (2)	C41—C42—O51	112.7 (12)
O31—W7—O4	84.0 (2)	C41—C42—H42A	109.0
O23—W7—O4	72.0 (2)	O51—C42—H42A	109.0
O24—W8—O32	103.1 (3)	C41—C42—H42B	109.0
O24—W8—O25	102.9 (3)	O51—C42—H42B	109.0
O32—W8—O25	85.1 (3)	H42A—C42—H42B	107.8
O24—W8—O23	102.6 (3)	C29—O51—C42	113.8 (8)
O32—W8—O23	89.3 (3)	C34—O52—C35	116.6 (8)
O25—W8—O23	154.4 (3)	C36—O53—C37	115.3 (11)
O24—W8—O14	101.9 (3)	C39—O54—C38	112.9 (11)
O32—W8—O14	154.9 (3)	C41—O55—C40	123.9 (13)
O25—W8—O14	87.4 (3)	C44—C43—O56	125.1 (10)
O23—W8—O14	87.3 (2)	C44—C43—C48	120.5 (10)
O24—W8—O4	171.5 (3)	O56—C43—C48	114.4 (9)
O32—W8—O4	83.5 (2)	C43—C44—C45	119.2 (11)
O25—W8—O4	82.8 (2)	C43—C44—H44	120.4
O23—W8—O4	71.8 (2)	C45—C44—H44	120.4
O14—W8—O4	71.8 (2)	C46—C45—C44	120.3 (11)
O26—W9—O15	101.7 (3)	C46—C45—H45	119.9
O26—W9—O25	103.4 (3)	C44—C45—H45	119.9
O15—W9—O25	90.0 (3)	C45—C46—C47	119.4 (12)
O26—W9—O33	103.6 (3)	C45—C46—H46	120.3
O15—W9—O33	154.7 (3)	C47—C46—H46	120.3
O25—W9—O33	85.7 (3)	C48—C47—C46	120.5 (12)
O26—W9—O27	101.8 (3)	C48—C47—H47	119.8
O15—W9—O27	87.3 (3)	C46—C47—H47	119.8
O25—W9—O27	154.7 (3)	C47—C48—C43	120.2 (11)
O33—W9—O27	86.0 (3)	C47—C48—O57	126.5 (11)
O26—W9—O1	170.3 (3)	C43—C48—O57	113.4 (10)
O15—W9—O1	71.8 (2)	O57—C49—C50	105.6 (11)
O25—W9—O1	84.0 (2)	O57—C49—H49A	110.6
O33—W9—O1	83.0 (2)	C50—C49—H49A	110.6
O27—W9—O1	71.2 (2)	O57—C49—H49B	110.6
O38—W10—O29	103.2 (3)	C50—C49—H49B	110.6
O38—W10—O35	101.7 (3)	H49A—C49—H49B	108.8
O29—W10—O35	89.5 (3)	O58—C50—C49	110.0 (10)
O38—W10—O37	101.9 (3)	O58—C50—H50A	109.7
O29—W10—O37	154.8 (3)	C49—C50—H50A	109.7
O35—W10—O37	87.5 (3)	O58—C50—H50B	109.7
O38—W10—O34	102.7 (3)	C49—C50—H50B	109.7
O29—W10—O34	85.3 (3)	H50A—C50—H50B	108.2
O35—W10—O34	155.6 (3)	O58—C51—C52	114.9 (14)
O37—W10—O34	87.2 (3)	O58—C51—H51A	108.5
O38—W10—O3	171.3 (3)	C52—C51—H51A	108.5
O29—W10—O3	83.5 (2)	O58—C51—H51B	108.5
O35—W10—O3	72.5 (2)	C52—C51—H51B	108.5
O37—W10—O3	71.7 (2)	H51A—C51—H51B	107.5
O34—W10—O3	83.2 (2)	O59—C52—C51	118.4 (15)
O39—W11—O36	102.7 (3)	O59—C52—H52A	107.7
O39—W11—O31	103.0 (3)	C51—C52—H52A	107.7
O36—W11—O31	89.3 (3)	O59—C52—H52B	107.7
O39—W11—O30	102.6 (3)	C51—C52—H52B	107.7
O36—W11—O30	154.6 (3)	H52A—C52—H52B	107.1
O31—W11—O30	85.9 (3)	O59—C53—C54	108.4 (9)
O39—W11—O35	101.3 (3)	O59—C53—H53A	110.0
O36—W11—O35	87.2 (3)	C54—C53—H53A	110.0
O31—W11—O35	155.6 (3)	O59—C53—H53B	110.0
O30—W11—O35	87.0 (3)	C54—C53—H53B	110.0
O39—W11—O3	171.2 (3)	H53A—C53—H53B	108.4
O36—W11—O3	71.9 (2)	O60—C54—C53	112.4 (10)
O31—W11—O3	84.1 (2)	O60—C54—H54A	109.1
O30—W11—O3	82.9 (2)	C53—C54—H54A	109.1
O35—W11—O3	71.8 (2)	O60—C54—H54B	109.1
O40—W12—O33	103.1 (3)	C53—C54—H54B	109.1
O40—W12—O37	100.5 (3)	H54A—C54—H54B	107.8
O33—W12—O37	89.7 (3)	O60—C55—C56	107.6 (9)
O40—W12—O32	104.1 (3)	O60—C55—H55A	110.2
O33—W12—O32	85.5 (3)	C56—C55—H55A	110.2
O37—W12—O32	155.5 (3)	O60—C55—H55B	110.2
O40—W12—O36	101.1 (3)	C56—C55—H55B	110.2
O33—W12—O36	155.8 (3)	H55A—C55—H55B	108.5
O37—W12—O36	86.4 (3)	O56—C56—C55	106.7 (9)
O32—W12—O36	88.3 (3)	O56—C56—H56A	110.4
O40—W12—O3	169.3 (3)	C55—C56—H56A	110.4
O33—W12—O3	84.3 (2)	O56—C56—H56B	110.4
O37—W12—O3	71.6 (2)	C55—C56—H56B	110.4
O32—W12—O3	83.9 (2)	H56A—C56—H56B	108.6
O36—W12—O3	71.8 (2)	C43—O56—C56	118.0 (8)
O4—P1—O3	109.9 (3)	C48—O57—C49	118.5 (10)
O4—P1—O2	109.9 (3)	C51—O58—C50	110.3 (10)
O3—P1—O2	109.1 (3)	C53—O59—C52	118.6 (12)
O4—P1—O1	109.6 (3)	C55—O60—C54	113.9 (9)
O3—P1—O1	109.0 (3)	O61—C57—C58	125.4 (9)
O2—P1—O1	109.3 (3)	O61—C57—C62	115.0 (8)
P1—O1—W4	126.1 (3)	C58—C57—C62	119.5 (9)
P1—O1—W1	125.2 (3)	C57—C58—C59	119.9 (10)
W4—O1—W1	89.56 (18)	C57—C58—H58	120.1
P1—O1—W9	125.7 (3)	C59—C58—H58	120.1
W4—O1—W9	89.38 (19)	C60—C59—C58	121.1 (11)
W1—O1—W9	89.49 (19)	C60—C59—H59	119.5
P1—O2—W5	125.9 (3)	C58—C59—H59	119.5
P1—O2—W6	125.5 (3)	C59—C60—C61	119.4 (11)
W5—O2—W6	89.54 (18)	C59—C60—H60	120.3
P1—O2—W2	125.7 (3)	C61—C60—H60	120.3
W5—O2—W2	89.39 (18)	C62—C61—C60	119.9 (10)
W6—O2—W2	89.17 (19)	C62—C61—H61	120.0
P1—O3—W12	125.6 (3)	C60—C61—H61	120.0
P1—O3—W10	126.7 (3)	O62—C62—C61	124.8 (9)
W12—O3—W10	89.19 (19)	O62—C62—C57	115.0 (8)
P1—O3—W11	125.8 (3)	C61—C62—C57	120.2 (9)
W12—O3—W11	88.95 (18)	O62—C63—C64	106.5 (8)
W10—O3—W11	88.63 (18)	O62—C63—H63A	110.4
P1—O4—W3	126.1 (3)	C64—C63—H63A	110.4
P1—O4—W7	125.8 (3)	O62—C63—H63B	110.4
W3—O4—W7	89.0 (2)	C64—C63—H63B	110.4
P1—O4—W8	126.5 (3)	H63A—C63—H63B	108.6
W3—O4—W8	88.61 (19)	O63—C64—C63	108.1 (9)
W7—O4—W8	88.72 (19)	O63—C64—H64A	110.1
W1—O8—W2	150.5 (3)	C63—C64—H64A	110.1
W2—O9—W3	153.1 (3)	O63—C64—H64B	110.1
W3—O10—W1	151.5 (3)	C63—C64—H64B	110.1
W5—O11—W2	126.0 (3)	H64A—C64—H64B	108.4
W2—O12—W6	126.5 (3)	O63—C65—C66	113.2 (8)
W7—O13—W3	127.0 (3)	O63—C65—H65A	108.9
W3—O14—W8	126.9 (3)	C66—C65—H65A	108.9
W9—O15—W1	127.4 (3)	O63—C65—H65B	108.9
W1—O16—W4	126.6 (3)	C66—C65—H65B	108.9
W5—O17—W4	151.5 (3)	H65A—C65—H65B	107.8
W6—O19—W5	126.4 (3)	O64—C66—C65	109.0 (9)
W7—O21—W6	151.4 (3)	O64—C66—H66A	109.9
W8—O23—W7	127.3 (3)	C65—C66—H66A	109.9
W9—O25—W8	152.1 (3)	O64—C66—H66B	109.9
W4—O27—W9	127.2 (3)	C65—C66—H66B	109.9
W10—O29—W5	151.7 (3)	H66A—C66—H66B	108.3
W6—O30—W11	151.7 (4)	O64—C67—C68	108.3 (10)
W11—O31—W7	150.8 (3)	O64—C67—H67A	110.0
W8—O32—W12	152.0 (3)	C68—C67—H67A	110.0
W12—O33—W9	151.1 (3)	O64—C67—H67B	110.0
W4—O34—W10	151.6 (4)	C68—C67—H67B	110.0
W10—O35—W11	127.0 (3)	H67A—C67—H67B	108.4
W11—O36—W12	127.3 (3)	O65—C69—C70	109.0 (8)
W10—O37—W12	127.4 (3)	O65—C69—H69A	109.9
C6—C1—O41	114.7 (9)	C70—C69—H69A	109.9
C6—C1—C2	121.1 (10)	O65—C69—H69B	109.9
O41—C1—C2	124.2 (9)	C70—C69—H69B	109.9
C3—C2—C1	118.1 (10)	H69A—C69—H69B	108.3
C3—C2—H2	120.9	O61—C70—C69	105.8 (8)
C1—C2—H2	120.9	O61—C70—H70A	110.6
C4—C3—C2	121.4 (11)	C69—C70—H70A	110.6
C4—C3—H3	119.3	O61—C70—H70B	110.6
C2—C3—H3	119.3	C69—C70—H70B	110.6
C3—C4—C5	119.8 (11)	H70A—C70—H70B	108.7
C3—C4—H4	120.1	C57—O61—C70	120.0 (8)
C5—C4—H4	120.1	C62—O62—C63	118.6 (7)
C4—C5—C6	120.7 (10)	C65—O63—C64	113.7 (8)
C4—C5—H5	119.7	C66—O64—C67	112.2 (9)
C6—C5—H5	119.7	C69—O65—C68	116.1 (9)
C1—C6—O42	119.5 (9)	O65—C68—C67	113.6 (9)
C1—C6—C5	118.9 (10)	O65—C68—H68A	108.8
O42—C6—C5	121.6 (9)	C67—C68—H68A	108.8
O42—C7—C8	112.2 (9)	O65—C68—H68B	108.8
O42—C7—H7A	109.2	C67—C68—H68B	108.8
C8—C7—H7A	109.2	H68A—C68—H68B	107.7
O42—C7—H7B	109.2	O66—C71—C76	116.1 (9)
C8—C7—H7B	109.2	O66—C71—C72	125.6 (10)
H7A—C7—H7B	107.9	C76—C71—C72	118.3 (11)
O43—C8—C7	107.7 (9)	C71—C72—C73	120.0 (12)
O43—C8—H8A	110.2	C71—C72—H72	120.0
C7—C8—H8A	110.2	C73—C72—H72	120.0
O43—C8—H8B	110.2	C74—C73—C72	121.6 (13)
C7—C8—H8B	110.2	C74—C73—H73	119.2
H8A—C8—H8B	108.5	C72—C73—H73	119.2
O43—C9—C10	109.4 (10)	C73—C74—C75	119.0 (13)
O43—C9—H9A	109.8	C73—C74—H74	120.5
C10—C9—H9A	109.8	C75—C74—H74	120.5
O43—C9—H9B	109.8	C74—C75—C76	120.4 (13)
C10—C9—H9B	109.8	C74—C75—H75	119.8
H9A—C9—H9B	108.2	C76—C75—H75	119.8
O44—C10—C9	113.0 (10)	O67—C76—C71	117.5 (10)
O44—C10—H10A	109.0	O67—C76—C75	121.1 (11)
C9—C10—H10A	109.0	C71—C76—C75	120.7 (11)
O44—C10—H10B	109.0	O67—C77—C78	109.9 (9)
C9—C10—H10B	109.0	O67—C77—H77A	109.7
H10A—C10—H10B	107.8	C78—C77—H77A	109.7
O44—C11—C12	109.8 (10)	O67—C77—H77B	109.7
O44—C11—H11A	109.7	C78—C77—H77B	109.7
C12—C11—H11A	109.7	H77A—C77—H77B	108.2
O44—C11—H11B	109.7	O68—C78—C77	108.5 (10)
C12—C11—H11B	109.7	O68—C78—H78A	110.0
H11A—C11—H11B	108.2	C77—C78—H78A	110.0
O45—C12—C11	116.7 (11)	O68—C78—H78B	110.0
O45—C12—H12A	108.1	C77—C78—H78B	110.0
C11—C12—H12A	108.1	H78A—C78—H78B	108.4
O45—C12—H12B	108.1	O68—C79—C80	107.4 (10)
C11—C12—H12B	108.1	O68—C79—H79A	110.2
H12A—C12—H12B	107.3	C80—C79—H79A	110.2
O45—C13—C14	112.9 (13)	O68—C79—H79B	110.2
O45—C13—H13A	109.0	C80—C79—H79B	110.2
C14—C13—H13A	109.0	H79A—C79—H79B	108.5
O45—C13—H13B	109.0	O69—C80—C79	114.3 (11)
C14—C13—H13B	109.0	O69—C80—H80A	108.7
H13A—C13—H13B	107.8	C79—C80—H80A	108.7
O41—C14—C13	106.2 (11)	O69—C80—H80B	108.7
O41—C14—H14A	110.5	C79—C80—H80B	108.7
C13—C14—H14A	110.5	H80A—C80—H80B	107.6
O41—C14—H14B	110.5	O69—C81—C82	108.0 (10)
C13—C14—H14B	110.5	O69—C81—H81A	110.1
H14A—C14—H14B	108.7	C82—C81—H81A	110.1
C1—O41—C14	117.5 (8)	O69—C81—H81B	110.1
C6—O42—C7	116.1 (8)	C82—C81—H81B	110.1
C9—O43—C8	113.4 (9)	H81A—C81—H81B	108.4
C10—O44—C11	113.5 (9)	O70—C82—C81	113.3 (9)
C13—O45—C12	112.5 (12)	O70—C82—H82A	108.9
C20—C15—C16	122.1 (12)	C81—C82—H82A	108.9
C20—C15—O46	116.8 (11)	O70—C82—H82B	108.9
C16—C15—O46	120.8 (12)	C81—C82—H82B	108.9
C15—C16—C17	118.0 (13)	H82A—C82—H82B	107.7
C15—C16—H16	121.0	O70—C83—C84	111.5 (9)
C17—C16—H16	121.0	O70—C83—H83A	109.3
C18—C17—C16	122.0 (15)	C84—C83—H83A	109.3
C18—C17—H17	119.0	O70—C83—H83B	109.3
C16—C17—H17	119.0	C84—C83—H83B	109.3
C17—C18—C19	116.9 (14)	H83A—C83—H83B	108.0
C17—C18—H18	121.5	O66—C84—C83	107.2 (10)
C19—C18—H18	121.5	O66—C84—H84A	110.3
C20—C19—C18	119.6 (13)	C83—C84—H84A	110.3
C20—C19—H19	120.2	O66—C84—H84B	110.3
C18—C19—H19	120.2	C83—C84—H84B	110.3
C15—C20—O47	116.7 (12)	H84A—C84—H84B	108.5
C15—C20—C19	121.2 (12)	C71—O66—C84	118.8 (8)
O47—C20—C19	121.7 (12)	C76—O67—C77	120.4 (9)
O47—C21—C22	110.3 (12)	C78—O68—C79	111.7 (9)
O47—C21—H21A	109.6	C81—O69—C80	115.8 (9)
C22—C21—H21A	109.6	C82—O70—C83	113.4 (8)
O47—C21—H21B	109.6	C85—O71—H71	109.5
C22—C21—H21B	109.6	O71—C85—H85A	109.5
H21A—C21—H21B	108.1	O71—C85—H85B	109.5
O48—C22—C21	110.8 (13)	H85A—C85—H85B	109.5
O48—C22—H22A	109.5	O71—C85—H85C	109.5
C21—C22—H22A	109.5	H85A—C85—H85C	109.5
O48—C22—H22B	109.5	H85B—C85—H85C	109.5
C21—C22—H22B	109.5

O4—P1—O1—W4	178.8 (3)	O22—W7—O21—W6	−129.0 (7)
O3—P1—O1—W4	58.5 (5)	O13—W7—O21—W6	129.6 (7)
O2—P1—O1—W4	−60.7 (5)	O31—W7—O21—W6	−26.8 (7)
O4—P1—O1—W1	−61.1 (5)	O23—W7—O21—W6	49.1 (11)
O3—P1—O1—W1	178.6 (3)	O4—W7—O21—W6	57.6 (7)
O2—P1—O1—W1	59.4 (5)	O20—W6—O21—W7	128.1 (7)
O4—P1—O1—W9	58.4 (5)	O30—W6—O21—W7	26.3 (7)
O3—P1—O1—W9	−61.9 (5)	O19—W6—O21—W7	−54.9 (11)
O2—P1—O1—W9	178.9 (3)	O12—W6—O21—W7	−130.7 (7)
O34—W4—O1—P1	−41.5 (4)	O2—W6—O21—W7	−58.4 (7)
O27—W4—O1—P1	−132.9 (4)	O24—W8—O23—W7	169.9 (4)
O17—W4—O1—P1	44.5 (4)	O32—W8—O23—W7	−86.9 (4)
O16—W4—O1—P1	133.4 (4)	O25—W8—O23—W7	−9.9 (8)
O34—W4—O1—W1	−176.5 (2)	O14—W8—O23—W7	68.3 (4)
O27—W4—O1—W1	92.1 (2)	O4—W8—O23—W7	−3.5 (3)
O17—W4—O1—W1	−90.4 (2)	O22—W7—O23—W8	−169.5 (4)
O16—W4—O1—W1	−1.6 (2)	O21—W7—O23—W8	12.4 (9)
O34—W4—O1—W9	94.0 (2)	O13—W7—O23—W8	−68.4 (4)
O27—W4—O1—W9	2.6 (2)	O31—W7—O23—W8	87.9 (4)
O17—W4—O1—W9	−179.9 (2)	O4—W7—O23—W8	3.5 (3)
O16—W4—O1—W9	−91.1 (2)	O26—W9—O25—W8	−130.2 (7)
O8—W1—O1—P1	−42.3 (4)	O15—W9—O25—W8	127.8 (7)
O10—W1—O1—P1	44.6 (4)	O33—W9—O25—W8	−27.2 (7)
O16—W1—O1—P1	−134.0 (4)	O27—W9—O25—W8	44.0 (11)
O15—W1—O1—P1	133.8 (4)	O1—W9—O25—W8	56.2 (7)
O8—W1—O1—W4	93.3 (2)	O24—W8—O25—W9	129.8 (7)
O10—W1—O1—W4	−179.8 (2)	O32—W8—O25—W9	27.5 (7)
O16—W1—O1—W4	1.6 (2)	O23—W8—O25—W9	−50.4 (11)
O15—W1—O1—W4	−90.6 (2)	O14—W8—O25—W9	−128.5 (7)
O8—W1—O1—W9	−177.3 (2)	O4—W8—O25—W9	−56.5 (7)
O10—W1—O1—W9	−90.4 (2)	O28—W4—O27—W9	168.8 (4)
O16—W1—O1—W9	91.0 (2)	O34—W4—O27—W9	−88.6 (4)
O15—W1—O1—W9	−1.2 (2)	O17—W4—O27—W9	−10.2 (8)
O15—W9—O1—P1	−133.4 (4)	O16—W4—O27—W9	67.5 (4)
O25—W9—O1—P1	−41.3 (4)	O1—W4—O27—W9	−4.2 (3)
O33—W9—O1—P1	45.1 (4)	O26—W9—O27—W4	−168.9 (4)
O27—W9—O1—P1	133.2 (4)	O15—W9—O27—W4	−67.5 (4)
O15—W9—O1—W4	90.8 (2)	O25—W9—O27—W4	16.9 (8)
O25—W9—O1—W4	−177.2 (2)	O33—W9—O27—W4	88.1 (4)
O33—W9—O1—W4	−90.8 (2)	O1—W9—O27—W4	4.2 (3)
O27—W9—O1—W4	−2.6 (2)	O38—W10—O29—W5	−130.6 (8)
O15—W9—O1—W1	1.3 (2)	O35—W10—O29—W5	127.4 (8)
O25—W9—O1—W1	93.3 (2)	O37—W10—O29—W5	44.4 (11)
O33—W9—O1—W1	179.7 (2)	O34—W10—O29—W5	−28.7 (8)
O27—W9—O1—W1	−92.2 (2)	O3—W10—O29—W5	55.0 (8)
O4—P1—O2—W5	178.8 (3)	O18—W5—O29—W10	130.6 (8)
O3—P1—O2—W5	−60.5 (5)	O17—W5—O29—W10	28.4 (8)
O1—P1—O2—W5	58.6 (5)	O11—W5—O29—W10	−52.2 (11)
O4—P1—O2—W6	−60.9 (5)	O19—W5—O29—W10	−128.6 (8)
O3—P1—O2—W6	59.8 (5)	O2—W5—O29—W10	−56.3 (8)
O1—P1—O2—W6	178.8 (3)	O20—W6—O30—W11	−129.7 (8)
O4—P1—O2—W2	58.5 (5)	O19—W6—O30—W11	127.9 (8)
O3—P1—O2—W2	179.2 (3)	O21—W6—O30—W11	−27.3 (8)
O1—P1—O2—W2	−61.7 (5)	O12—W6—O30—W11	46.4 (12)
O17—W5—O2—P1	−41.8 (4)	O2—W6—O30—W11	56.1 (8)
O11—W5—O2—P1	−133.7 (4)	O39—W11—O30—W6	130.6 (8)
O29—W5—O2—P1	44.5 (4)	O36—W11—O30—W6	−51.5 (12)
O19—W5—O2—P1	133.9 (4)	O31—W11—O30—W6	28.1 (8)
O17—W5—O2—W6	−177.1 (2)	O35—W11—O30—W6	−128.5 (8)
O11—W5—O2—W6	90.9 (2)	O3—W11—O30—W6	−56.5 (8)
O29—W5—O2—W6	−90.8 (2)	O39—W11—O31—W7	−131.0 (7)
O19—W5—O2—W6	−1.4 (2)	O36—W11—O31—W7	126.1 (7)
O17—W5—O2—W2	93.7 (2)	O30—W11—O31—W7	−29.0 (7)
O11—W5—O2—W2	1.8 (2)	O35—W11—O31—W7	44.5 (11)
O29—W5—O2—W2	−180.0 (2)	O3—W11—O31—W7	54.2 (7)
O19—W5—O2—W2	−90.6 (2)	O22—W7—O31—W11	131.4 (7)
O30—W6—O2—P1	−42.3 (4)	O21—W7—O31—W11	28.8 (7)
O19—W6—O2—P1	−134.2 (5)	O13—W7—O31—W11	−48.7 (11)
O21—W6—O2—P1	44.2 (4)	O23—W7—O31—W11	−127.1 (7)
O12—W6—O2—P1	133.5 (5)	O4—W7—O31—W11	−54.9 (7)
O30—W6—O2—W5	93.3 (2)	O24—W8—O32—W12	−131.7 (8)
O19—W6—O2—W5	1.4 (2)	O25—W8—O32—W12	−29.6 (8)
O21—W6—O2—W5	179.9 (2)	O23—W8—O32—W12	125.5 (8)
O12—W6—O2—W5	−90.8 (2)	O14—W8—O32—W12	43.4 (12)
O30—W6—O2—W2	−177.3 (2)	O4—W8—O32—W12	53.7 (8)
O19—W6—O2—W2	90.8 (2)	O40—W12—O32—W8	132.6 (8)
O21—W6—O2—W2	−90.8 (2)	O33—W12—O32—W8	30.1 (8)
O12—W6—O2—W2	−1.4 (2)	O37—W12—O32—W8	−49.0 (12)
O9—W2—O2—P1	−40.5 (4)	O36—W12—O32—W8	−126.5 (8)
O12—W2—O2—P1	−133.4 (5)	O3—W12—O32—W8	−54.6 (8)
O8—W2—O2—P1	45.0 (4)	O40—W12—O33—W9	−131.8 (7)
O11—W2—O2—P1	133.9 (5)	O37—W12—O33—W9	127.6 (8)
O9—W2—O2—W5	−176.2 (2)	O32—W12—O33—W9	−28.3 (7)
O12—W2—O2—W5	91.0 (2)	O36—W12—O33—W9	47.2 (11)
O8—W2—O2—W5	−90.7 (2)	O3—W12—O33—W9	56.0 (7)
O11—W2—O2—W5	−1.7 (2)	O26—W9—O33—W12	130.5 (7)
O9—W2—O2—W6	94.3 (2)	O15—W9—O33—W12	−53.2 (11)
O12—W2—O2—W6	1.5 (2)	O25—W9—O33—W12	27.8 (7)
O8—W2—O2—W6	179.8 (2)	O27—W9—O33—W12	−128.3 (8)
O11—W2—O2—W6	−91.3 (2)	O1—W9—O33—W12	−56.7 (7)
O4—P1—O3—W12	−60.1 (5)	O28—W4—O34—W10	−132.5 (8)
O2—P1—O3—W12	179.3 (3)	O27—W4—O34—W10	125.7 (8)
O1—P1—O3—W12	60.0 (5)	O17—W4—O34—W10	−29.6 (8)
O4—P1—O3—W10	179.2 (3)	O16—W4—O34—W10	41.7 (12)
O2—P1—O3—W10	58.6 (5)	O1—W4—O34—W10	53.7 (8)
O1—P1—O3—W10	−60.7 (5)	O38—W10—O34—W4	132.3 (8)
O4—P1—O3—W11	59.1 (5)	O29—W10—O34—W4	29.7 (8)
O2—P1—O3—W11	−61.5 (5)	O35—W10—O34—W4	−48.7 (12)
O1—P1—O3—W11	179.2 (3)	O37—W10—O34—W4	−126.2 (8)
O40—W12—O3—P1	−177.3 (13)	O3—W10—O34—W4	−54.2 (8)
O33—W12—O3—P1	−42.9 (4)	O38—W10—O35—W11	169.7 (4)
O37—W12—O3—P1	−134.5 (5)	O29—W10—O35—W11	−86.9 (4)
O32—W12—O3—P1	43.1 (4)	O37—W10—O35—W11	68.1 (4)
O36—W12—O3—P1	133.3 (5)	O34—W10—O35—W11	−9.4 (8)
O40—W12—O3—W10	−41.0 (15)	O3—W10—O35—W11	−3.6 (3)
O33—W12—O3—W10	93.5 (2)	O39—W11—O35—W10	−170.7 (4)
O37—W12—O3—W10	2.0 (2)	O36—W11—O35—W10	−68.3 (4)
O32—W12—O3—W10	179.6 (2)	O31—W11—O35—W10	13.7 (8)
O36—W12—O3—W10	−90.3 (2)	O30—W11—O35—W10	87.0 (4)
O40—W12—O3—W11	47.7 (15)	O3—W11—O35—W10	3.6 (3)
O33—W12—O3—W11	−177.8 (2)	O39—W11—O36—W12	170.1 (4)
O37—W12—O3—W11	90.6 (2)	O31—W11—O36—W12	−86.7 (4)
O32—W12—O3—W11	−91.8 (2)	O30—W11—O36—W12	−7.8 (9)
O36—W12—O3—W11	−1.6 (2)	O35—W11—O36—W12	69.1 (4)
O29—W10—O3—P1	−41.6 (4)	O3—W11—O36—W12	−2.6 (3)
O35—W10—O3—P1	−133.2 (4)	O40—W12—O36—W11	−169.1 (4)
O37—W10—O3—P1	133.6 (5)	O33—W12—O36—W11	11.9 (9)
O34—W10—O3—P1	44.4 (4)	O37—W12—O36—W11	−69.2 (4)
O29—W10—O3—W12	−177.2 (2)	O32—W12—O36—W11	86.8 (4)
O35—W10—O3—W12	91.2 (2)	O3—W12—O36—W11	2.7 (3)
O37—W10—O3—W12	−2.0 (2)	O38—W10—O37—W12	−170.7 (4)
O34—W10—O3—W12	−91.2 (2)	O29—W10—O37—W12	14.3 (8)
O29—W10—O3—W11	93.8 (2)	O35—W10—O37—W12	−69.2 (4)
O35—W10—O3—W11	2.2 (2)	O34—W10—O37—W12	86.9 (4)
O37—W10—O3—W11	−90.9 (2)	O3—W10—O37—W12	3.2 (3)
O34—W10—O3—W11	179.8 (2)	O40—W12—O37—W10	169.5 (4)
O36—W11—O3—P1	−133.1 (4)	O33—W12—O37—W10	−87.2 (4)
O31—W11—O3—P1	−41.9 (4)	O32—W12—O37—W10	−8.9 (9)
O30—W11—O3—P1	44.7 (4)	O36—W12—O37—W10	68.9 (4)
O35—W11—O3—P1	133.8 (4)	O3—W12—O37—W10	−3.2 (3)
O36—W11—O3—W12	1.7 (2)	C6—C1—C2—C3	0.2 (18)
O31—W11—O3—W12	92.8 (2)	O41—C1—C2—C3	−178.9 (11)
O30—W11—O3—W12	179.4 (2)	C1—C2—C3—C4	−0.5 (19)
O35—W11—O3—W12	−91.4 (2)	C2—C3—C4—C5	0.3 (18)
O36—W11—O3—W10	90.9 (2)	C3—C4—C5—C6	0.2 (17)
O31—W11—O3—W10	−178.0 (2)	O41—C1—C6—O42	−4.0 (15)
O30—W11—O3—W10	−91.4 (2)	C2—C1—C6—O42	176.7 (10)
O35—W11—O3—W10	−2.2 (2)	O41—C1—C6—C5	179.5 (10)
O3—P1—O4—W3	179.4 (3)	C2—C1—C6—C5	0.3 (17)
O2—P1—O4—W3	−60.4 (5)	C4—C5—C6—C1	−0.5 (16)
O1—P1—O4—W3	59.7 (5)	C4—C5—C6—O42	−176.9 (10)
O3—P1—O4—W7	−60.6 (5)	O42—C7—C8—O43	−70.8 (11)
O2—P1—O4—W7	59.6 (5)	O43—C9—C10—O44	66.5 (13)
O1—P1—O4—W7	179.7 (3)	O44—C11—C12—O45	58.0 (16)
O3—P1—O4—W8	59.3 (5)	O45—C13—C14—O41	64.0 (17)
O2—P1—O4—W8	179.4 (3)	C6—C1—O41—C14	176.7 (11)
O1—P1—O4—W8	−60.5 (5)	C2—C1—O41—C14	−4.0 (18)
O14—W3—O4—P1	−133.9 (5)	C13—C14—O41—C1	155.9 (11)
O10—W3—O4—P1	−42.3 (4)	C1—C6—O42—C7	122.4 (11)
O9—W3—O4—P1	43.3 (4)	C5—C6—O42—C7	−61.2 (13)
O13—W3—O4—P1	132.9 (5)	C8—C7—O42—C6	−85.4 (11)
O14—W3—O4—W7	90.7 (2)	C10—C9—O43—C8	−178.7 (10)
O10—W3—O4—W7	−177.7 (2)	C7—C8—O43—C9	176.7 (9)
O9—W3—O4—W7	−92.1 (2)	C9—C10—O44—C11	84.8 (13)
O13—W3—O4—W7	−2.4 (2)	C12—C11—O44—C10	−163.5 (11)
O14—W3—O4—W8	2.0 (2)	C14—C13—O45—C12	−177.6 (11)
O10—W3—O4—W8	93.6 (2)	C11—C12—O45—C13	79.4 (16)
O9—W3—O4—W8	179.2 (2)	C20—C15—C16—C17	5 (2)
O13—W3—O4—W8	−91.1 (2)	O46—C15—C16—C17	178.9 (13)
O21—W7—O4—P1	−42.6 (4)	C15—C16—C17—C18	−2 (2)
O13—W7—O4—P1	−133.2 (4)	C16—C17—C18—C19	1 (2)
O31—W7—O4—P1	44.1 (4)	C17—C18—C19—C20	−1 (2)
O23—W7—O4—P1	133.6 (4)	C16—C15—C20—O47	−178.0 (13)
O21—W7—O4—W3	93.0 (2)	O46—C15—C20—O47	7 (2)
O13—W7—O4—W3	2.4 (2)	C16—C15—C20—C19	−5 (2)
O31—W7—O4—W3	179.7 (2)	O46—C15—C20—C19	−179.6 (13)
O23—W7—O4—W3	−90.8 (2)	C18—C19—C20—C15	3 (2)
O21—W7—O4—W8	−178.4 (2)	C18—C19—C20—O47	175.6 (13)
O13—W7—O4—W8	91.0 (2)	O47—C21—C22—O48	67.1 (17)
O31—W7—O4—W8	−91.7 (2)	O48—C23—C24—O49	60 (2)
O23—W7—O4—W8	−2.1 (2)	O49—C25—C26—O50	−57 (2)
O32—W8—O4—P1	−41.7 (4)	O50—C27—C28—O46	−72.5 (14)
O25—W8—O4—P1	44.1 (4)	C20—C15—O46—C28	−176.6 (13)
O23—W8—O4—P1	−133.1 (5)	C16—C15—O46—C28	9 (2)
O14—W8—O4—P1	133.7 (5)	C27—C28—O46—C15	171.9 (12)
O32—W8—O4—W3	−177.4 (2)	C22—C21—O47—C20	−162.8 (13)
O25—W8—O4—W3	−91.6 (2)	C15—C20—O47—C21	161.7 (13)
O23—W8—O4—W3	91.2 (2)	C19—C20—O47—C21	−11 (2)
O14—W8—O4—W3	−2.0 (2)	C21—C22—O48—C23	−162.0 (13)
O32—W8—O4—W7	93.5 (2)	C24—C23—O48—C22	80 (2)
O25—W8—O4—W7	179.4 (2)	C26—C25—O49—C24	−176.9 (16)
O23—W8—O4—W7	2.2 (2)	C23—C24—O49—C25	−170.0 (16)
O14—W8—O4—W7	−91.0 (2)	C28—C27—O50—C26	164.6 (12)
O5—W1—O8—W2	−131.9 (7)	C25—C26—O50—C27	−91.2 (18)
O10—W1—O8—W2	−29.3 (7)	O51—C29—C30—C31	177.1 (10)
O16—W1—O8—W2	125.9 (7)	C34—C29—C30—C31	3.6 (17)
O15—W1—O8—W2	44.9 (11)	C29—C30—C31—C32	−0.9 (18)
O1—W1—O8—W2	54.1 (7)	C30—C31—C32—C33	−2.0 (18)
O6—W2—O8—W1	132.0 (7)	C31—C32—C33—C34	2.1 (17)
O9—W2—O8—W1	29.5 (7)	C32—C33—C34—O52	179.6 (10)
O12—W2—O8—W1	−50.9 (11)	C32—C33—C34—C29	0.5 (15)
O11—W2—O8—W1	−126.8 (7)	C30—C29—C34—O52	177.6 (10)
O2—W2—O8—W1	−54.8 (7)	O51—C29—C34—O52	3.7 (14)
O6—W2—O9—W3	−132.1 (8)	C30—C29—C34—C33	−3.3 (16)
O12—W2—O9—W3	126.0 (8)	O51—C29—C34—C33	−177.2 (9)
O8—W2—O9—W3	−30.3 (8)	O52—C35—C36—O53	−59.0 (16)
O11—W2—O9—W3	41.3 (11)	O53—C37—C38—O54	−64.2 (14)
O2—W2—O9—W3	53.9 (8)	O54—C39—C40—O55	59 (2)
O7—W3—O9—W2	131.7 (8)	O55—C41—C42—O51	−58 (2)
O14—W3—O9—W2	−47.9 (11)	C30—C29—O51—C42	73.4 (14)
O10—W3—O9—W2	29.5 (8)	C34—C29—O51—C42	−112.9 (11)
O13—W3—O9—W2	−126.5 (8)	C41—C42—O51—C29	155.0 (12)
O4—W3—O9—W2	−54.5 (8)	C33—C34—O52—C35	3.5 (15)
O7—W3—O10—W1	−128.8 (7)	C29—C34—O52—C35	−177.4 (9)
O14—W3—O10—W1	129.3 (7)	C36—C35—O52—C34	−173.3 (10)
O9—W3—O10—W1	−27.0 (7)	C35—C36—O53—C37	174.8 (11)
O13—W3—O10—W1	46.2 (11)	C38—C37—O53—C36	−67.8 (16)
O4—W3—O10—W1	56.8 (7)	C40—C39—O54—C38	−154.9 (14)
O5—W1—O10—W3	129.9 (7)	C37—C38—O54—C39	168.1 (13)
O8—W1—O10—W3	27.7 (7)	C42—C41—O55—C40	−178.3 (14)
O16—W1—O10—W3	−54.7 (11)	C39—C40—O55—C41	179.0 (16)
O15—W1—O10—W3	−129.3 (7)	O56—C43—C44—C45	−179.1 (9)
O1—W1—O10—W3	−57.8 (7)	C48—C43—C44—C45	3.0 (16)
O18—W5—O11—W2	170.1 (4)	C43—C44—C45—C46	−2.3 (17)
O17—W5—O11—W2	−86.8 (4)	C44—C45—C46—C47	1.7 (19)
O29—W5—O11—W2	−7.1 (9)	C45—C46—C47—C48	−2 (2)
O19—W5—O11—W2	69.4 (4)	C46—C47—C48—C43	2.6 (19)
O2—W5—O11—W2	−2.8 (3)	C46—C47—C48—O57	−178.0 (11)
O6—W2—O11—W5	−170.6 (4)	C44—C43—C48—C47	−3.2 (17)
O9—W2—O11—W5	16.0 (8)	O56—C43—C48—C47	178.7 (10)
O12—W2—O11—W5	−69.5 (4)	C44—C43—C48—O57	177.3 (9)
O8—W2—O11—W5	87.1 (4)	O56—C43—C48—O57	−0.8 (13)
O2—W2—O11—W5	2.7 (3)	O57—C49—C50—O58	61.7 (14)
O6—W2—O12—W6	170.7 (4)	O58—C51—C52—O59	−46 (2)
O9—W2—O12—W6	−85.6 (4)	O59—C53—C54—O60	−69.7 (13)
O8—W2—O12—W6	−6.4 (9)	O60—C55—C56—O56	−70.3 (12)
O11—W2—O12—W6	69.5 (4)	C44—C43—O56—C56	12.6 (15)
O2—W2—O12—W6	−2.3 (3)	C48—C43—O56—C56	−169.5 (10)
O20—W6—O12—W2	−171.5 (4)	C55—C56—O56—C43	172.6 (9)
O30—W6—O12—W2	12.4 (9)	C47—C48—O57—C49	−9.2 (18)
O19—W6—O12—W2	−69.8 (4)	C43—C48—O57—C49	170.3 (10)
O21—W6—O12—W2	85.8 (4)	C50—C49—O57—C48	−178.0 (10)
O2—W6—O12—W2	2.3 (3)	C52—C51—O58—C50	168.2 (14)
O22—W7—O13—W3	169.6 (4)	C49—C50—O58—C51	−160.0 (12)
O21—W7—O13—W3	−87.3 (4)	C54—C53—O59—C52	−174.9 (11)
O31—W7—O13—W3	−10.4 (9)	C51—C52—O59—C53	−91.8 (18)
O23—W7—O13—W3	68.1 (4)	C56—C55—O60—C54	169.5 (10)
O4—W7—O13—W3	−3.8 (3)	C53—C54—O60—C55	−89.6 (11)
O7—W3—O13—W7	−170.1 (4)	O61—C57—C58—C59	176.4 (10)
O14—W3—O13—W7	−68.6 (4)	C62—C57—C58—C59	−1.1 (15)
O10—W3—O13—W7	14.9 (8)	C57—C58—C59—C60	0.6 (17)
O9—W3—O13—W7	87.5 (4)	C58—C59—C60—C61	−0.1 (17)
O4—W3—O13—W7	3.8 (3)	C59—C60—C61—C62	0.1 (16)
O7—W3—O14—W8	170.3 (4)	C60—C61—C62—O62	−179.8 (10)
O10—W3—O14—W8	−86.5 (4)	C60—C61—C62—C57	−0.5 (15)
O9—W3—O14—W8	−10.0 (9)	O61—C57—C62—O62	2.6 (12)
O13—W3—O14—W8	68.6 (4)	C58—C57—C62—O62	−179.7 (9)
O4—W3—O14—W8	−3.2 (3)	O61—C57—C62—C61	−176.7 (9)
O24—W8—O14—W3	−170.9 (4)	C58—C57—C62—C61	1.0 (14)
O32—W8—O14—W3	13.9 (9)	O62—C63—C64—O63	66.3 (11)
O25—W8—O14—W3	86.4 (4)	O63—C65—C66—O64	62.1 (12)
O23—W8—O14—W3	−68.6 (4)	O65—C69—C70—O61	−62.1 (11)
O4—W8—O14—W3	3.2 (3)	C58—C57—O61—C70	4.6 (15)
O26—W9—O15—W1	170.6 (4)	C62—C57—O61—C70	−177.8 (9)
O25—W9—O15—W1	−85.7 (4)	C69—C70—O61—C57	178.8 (8)
O33—W9—O15—W1	−5.7 (9)	C61—C62—O62—C63	−5.4 (14)
O27—W9—O15—W1	69.1 (4)	C57—C62—O62—C63	175.3 (8)
O1—W9—O15—W1	−2.0 (3)	C64—C63—O62—C62	−179.3 (9)
O5—W1—O15—W9	−171.5 (4)	C66—C65—O63—C64	78.1 (11)
O8—W1—O15—W9	11.7 (9)	C63—C64—O63—C65	−166.0 (8)
O10—W1—O15—W9	85.8 (4)	C65—C66—O64—C67	−174.3 (9)
O16—W1—O15—W9	−70.1 (4)	C68—C67—O64—C66	−178.4 (9)
O1—W1—O15—W9	2.0 (3)	C70—C69—O65—C68	163.4 (9)
O5—W1—O16—W4	169.6 (4)	C69—O65—C68—C67	−82.5 (12)
O8—W1—O16—W4	−87.4 (4)	O64—C67—C68—O65	−67.8 (13)
O10—W1—O16—W4	−5.8 (9)	O66—C71—C72—C73	−177.9 (12)
O15—W1—O16—W4	68.9 (4)	C76—C71—C72—C73	1.8 (19)
O1—W1—O16—W4	−2.5 (3)	C71—C72—C73—C74	−2 (2)
O28—W4—O16—W1	−170.6 (4)	C72—C73—C74—C75	0 (2)
O34—W4—O16—W1	15.1 (9)	C73—C74—C75—C76	2 (2)
O27—W4—O16—W1	−69.2 (4)	O66—C71—C76—O67	−9.4 (15)
O17—W4—O16—W1	86.2 (4)	C72—C71—C76—O67	170.9 (11)
O1—W4—O16—W1	2.5 (3)	O66—C71—C76—C75	179.9 (10)
O18—W5—O17—W4	−129.6 (7)	C72—C71—C76—C75	0.2 (17)
O11—W5—O17—W4	128.7 (7)	C74—C75—C76—O67	−172.6 (12)
O29—W5—O17—W4	−28.0 (7)	C74—C75—C76—C71	−2.3 (19)
O19—W5—O17—W4	46.0 (11)	O67—C77—C78—O68	−62.7 (13)
O2—W5—O17—W4	56.0 (7)	O68—C79—C80—O69	68.9 (14)
O28—W4—O17—W5	130.1 (7)	O69—C81—C82—O70	66.4 (13)
O34—W4—O17—W5	28.4 (7)	O70—C83—C84—O66	61.3 (13)
O27—W4—O17—W5	−51.0 (11)	C76—C71—O66—C84	179.3 (10)
O16—W4—O17—W5	−128.9 (7)	C72—C71—O66—C84	−1.0 (16)
O1—W4—O17—W5	−56.8 (7)	C83—C84—O66—C71	171.6 (9)
O20—W6—O19—W5	171.1 (4)	C71—C76—O67—C77	130.7 (11)
O30—W6—O19—W5	−86.2 (4)	C75—C76—O67—C77	−58.7 (16)
O21—W6—O19—W5	−5.9 (9)	C78—C77—O67—C76	−110.0 (13)
O12—W6—O19—W5	70.0 (4)	C77—C78—O68—C79	174.2 (10)
O2—W6—O19—W5	−2.2 (3)	C80—C79—O68—C78	−170.9 (11)
O18—W5—O19—W6	−171.7 (4)	C82—C81—O69—C80	−173.2 (9)
O17—W5—O19—W6	12.8 (9)	C79—C80—O69—C81	75.0 (13)
O11—W5—O19—W6	−70.6 (4)	C81—C82—O70—C83	82.8 (12)
O29—W5—O19—W6	86.4 (4)	C84—C83—O70—C82	−175.3 (10)
O2—W5—O19—W6	2.3 (3)

Symmetry codes: (i) x, y+1, z; (ii) x−1/2, −y+1/2, z−1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O71—H71···O16ⁱⁱⁱ	0.84	2.35	3.17 (2)	164

Symmetry code: (iii) x, y, z+1.

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A novel supramolecular organic–inorganic adduct containing α-Keggin-type [PW12O40]3− anions and benzo-15-crown-5 mol­ecules

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checkCIF/PLATON results

A novel supramolecular organic–inorganic adduct containing α-Keggin-type [PW₁₂O₄₀]³⁻ anions and benzo-15-crown-5 molecules