supplementary materials


su2626 scheme

Acta Cryst. (2013). E69, m605-m606    [ doi:10.1107/S160053681302583X ]

Ethyl­enedi­ammonium sodium tetra­kis­[bis­(ethyl­enedi­amine-[kappa]2N,N')(oxalato-[kappa]2O1,O2)cobalt(III)] [penta­hydrogen di(phosphato­octa­deca­tungstate)] tetra­deca­hydrate

S. Zhang, J. Wang and Y. Xu

Abstract top

The title compound, Na(C2H10N2)[Co(C2O4)(C2H8N2)2]4[H5(P2W18O62)2]·14H2O, prepared under hydro­thermal conditions, consists of two Dawson-type [P2W18O62]6- anions, four isolated [Co(en)2(ox)]+ cations (en = ethyl­enedi­amine and ox = oxalate), one Na+ cation, one [H2en]2+ cation, and a number of ordered (14) and disordered solvent water mol­ecules. The [P2W18O62]6- polyoxidometalate anion has site symmetry 1 and contains two structurally distinct types of W atoms: viz. six W atoms on vertical pseudo-mirror planes grouped in two sets of three, and 12 equatorial W atoms that do not lie in the pseudo-mirror planes grouped in two sets of six. In each [Co(en)2(ox)]+ cation, the CoIII ion is coordinated by four N atoms from two en ligands and two O atoms from the ox ligands, completing a distorted octa­hedral structure. The sodium cation lies on an inversion centre and additionally links the complex cations and anions. In the crystal, the various units are linked by N-H...O and O-H...O hydrogen bonds, which together with C-H...O hydrogen bonds form a three-dimensional structure. The contribution of a region of disordered electron density, possibly highly disordered solvent water mol­ecules, to the scattering was removed with the SQUEEZE option of PLATON [Spek (2009). Acta Cryst. D65, 148-155]. To equilibrate the charges five H+ ions have been added to the polyoxidometalate. These H+ ions and the disordered solvent contribution were not included in the reported mol­ecular weight and density.

Comment top

Polyoxidometalates (POMs), as one kind of significant metal oxide cluster have been attracting extensive interests in fields such as catalysis, medicine, biology, electrochemistry, electrochromism and magnetism for their enormous variety of properties. As their controllable size, shape, oxo-riched surfaces and the high-negative charges, POM's could be used as multi-linking sites or templates in constructing extended POM-based materials. Polyoxidotungstates (POT's) are the largest POM subclass, and to date, the two most studied heteropolyoxidometalates type have been the famous Keggin and Wells–Dawson families, which can be represented by [PW12O40]3- and Wells-Dawson [P2W18O62]6-, respectively. In the past several decades, the synthetic combination of various POMs and transition metal cations or transition metal coordination complexes (TMCs) has been a powerful strategy and an intensive focus in POM chemistry, which leads to a rapidly growing class of functional organic–inorganic hybrid materials with a huge diversity of structures and realised applications in catalysis, photochemistry, and magnetochemistry. In this branch, a variety of organic–inorganic hybrid materials, constructed from components based on saturated Keggin polyoxidoanions and TMCs have been extensively reported. However, in contrast, the role of Wells–Dawson polyoxidoanions as the inorganic building units to construct such extended frameworks are much less common, the reason for which may be that the large size of these POT's decreases the electron density of the surface or the coordination ability of the surface oxygen atoms. In this paper, we report on the synthesis and crystal structure of the title organic–inorganic hybrid compound based on Wells–Dawson POMs and TMCs.

The asymmetric unit of the title compound, Fig. 1, consists of one [P2W18O62]6- polyoxidoanion, two [Co(en)2(ox)]+ coordination cations, 0.5 Na+ cation, a half [H2en]2+ cation and seven lattice water molecules. The [P2W18O62]6- cluster retains a classical α-Dawson-type structure, which may be described as two [α-PW9O34]9- units, generated from the well known [α-PW12O40]3- anion by removal of a set of three corner-sharing WO6 octahedra and fused into a cluster of virtual D3h symmetry. The [P2W18O62]6- polyoxidoanion contains only two structurally distinct types of W atoms: six polar W atoms on vertical mirror planes grouped in two sets of three, and twelve equatorial W atoms that do not lie on mirror planes grouped in two sets of six.

There are two crystallographically independent [Co(en)2(ox)]+ cations. The cobalt centers all exhibit a strongly distorted octahedral geometry, which is defined by four nitrogen atoms from two en ligands with Co–N bond lengths of 1.934 (11) to 1.961 (11) Å and two oxygen atoms from the oxalate ligands with Co–O bond lengths of 1.889 (9) to 1.927 (8) Å. The sodium cation lies on an inversion centre and links the complex cations and anions.

In the crystal, Fig. 2, the various units are linked by N-H···O and O-H···O hydrogen bonds, which together with C-H···O hydrogen bonds form a three-dimensional structure (Table 1).

Related literature top

For general background to polyoxidometalate-based materials, see: Du et al. (2013); Dolbecq et al. (2010); Zheng & Yang (2012). For organic–inorganic hybrid materials constructed from components based on saturated polyoxidoanions and transition metal coordination complexes (TMCs), see: Liu et al. (2011); Wang et al. (2010). For the related organic–inorganic hybrid compounds based on saturated Wells–Dawson-type polyoxidoanions and TMCs, and the synthesis of the POM precursor, Na6[P2W18O62].19H2O, see: Wang et al. (2010); Contant (1990).

Experimental top

The saturated POM precursor, Na6[P2W18O62].19H2O (I), was prepared according to the literature procedure (Wang et al., 2010) and identified by IR spectra. A mixture of 0.406 g of (I), Co(Cl)2.6H2O (0.122 g), ethylenediamine (0.05 ml) and oxalic acid dehydrate (0.268 g) in H2O (10 ml) were stirred at room temperature for 60 min and transferred into a 30 ml Teflon-lined autoclave. It was heated under autogenous pressure at 373 K for two days. It was then allowed to cool to room temperature in air. Pink block-like crystals of the title compound, suitable for X-ray diffraction analysis, were obtained by filtration.

Refinement top

All of the hydrogen atoms were placed in calculated positions and treated as riding atoms: O-H = 0.85 Å, N-H = 0.90 Å, C-H = 0.97 Å with Uiso(H) = 1.2Ueq(O/N/C). The contribution of highly disordered solvent water molecules [ca. 56 electrons for a volume of ca. 620 Å3] to the scattering was removed with the SQUEEZE routine of PLATON [Spek (2009). Acta Cryst. D65 148-155]. To equilibrate the charges five H+ ions have been added to the polyoxidometalate. These H+ ions and the disordered solvent contribution were not included in the reported molecular weight and density.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2009); cell refinement: CrysAlis CCD (Oxford Diffraction, 2009); data reduction: CrysAlis RED (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of the asymmetric unit of the title compound, with partial atom labelling. Displacement ellipsoids are drawn at the 50% probability level. Only half of the diprotonated [H2en]2+ cation, situated about an inversion center, is shown (atoms N5 and C7). The Na+ ion is also situated on an inversion center. The H atoms and water molecules have been omitted for clarity.
[Figure 2] Fig. 2. A view of the crystal packing of the title compound.
Ethylenediammonium sodium tetrakis[bis(ethylenediamine-κ2N,N')(oxalato-κ2O1,O2)cobalt(III)] [pentahydrogen di(phosphatooctadecatungsten)] tetradecahydrate top
Crystal data top
Na(C2H10N2)[Co(C2O4)(C2H8N2)2]4·[H5(P2W18O62)2]·14H2OZ = 1
Mr = 10132.09F(000) = 4464
Triclinic, P1Dx = 3.904 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 14.5999 (4) ÅCell parameters from 12336 reflections
b = 16.5714 (4) Åθ = 2.8–26.5°
c = 18.0165 (4) ŵ = 24.42 mm1
α = 83.693 (2)°T = 293 K
β = 84.586 (2)°Block, pink
γ = 87.992 (2)°0.12 × 0.06 × 0.05 mm
V = 4311.88 (18) Å3
Data collection top
Multiwire proportional
diffractometer
17862 independent reflections
Radiation source: fine-focus sealed tube12523 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.057
phi and ω scansθmax = 26.5°, θmin = 2.8°
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2009)
h = 1816
Tmin = 0.158, Tmax = 0.375k = 2020
49498 measured reflectionsl = 2216
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.075H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.0182P)2]
where P = (Fo2 + 2Fc2)/3
17862 reflections(Δ/σ)max = 0.001
1096 parametersΔρmax = 2.01 e Å3
12 restraintsΔρmin = 1.98 e Å3
Crystal data top
Na(C2H10N2)[Co(C2O4)(C2H8N2)2]4·[H5(P2W18O62)2]·14H2Oγ = 87.992 (2)°
Mr = 10132.09V = 4311.88 (18) Å3
Triclinic, P1Z = 1
a = 14.5999 (4) ÅMo Kα radiation
b = 16.5714 (4) ŵ = 24.42 mm1
c = 18.0165 (4) ÅT = 293 K
α = 83.693 (2)°0.12 × 0.06 × 0.05 mm
β = 84.586 (2)°
Data collection top
Multiwire proportional
diffractometer
12523 reflections with I > 2σ(I)
Absorption correction: multi-scan
(CrysAlis RED; Oxford Diffraction, 2009)
Rint = 0.057
Tmin = 0.158, Tmax = 0.375θmax = 26.5°
49498 measured reflectionsStandard reflections: 0
17862 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.040H-atom parameters constrained
wR(F2) = 0.075Δρmax = 2.01 e Å3
S = 0.96Δρmin = 1.98 e Å3
17862 reflectionsAbsolute structure: ?
1096 parametersAbsolute structure parameter: ?
12 restraintsRogers parameter: ?
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles

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 > 2sigma(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
xyzUiso*/Ueq
W10.33785 (3)0.83307 (3)0.43848 (3)0.0187 (2)
W20.15928 (3)0.84213 (3)0.08087 (3)0.0201 (2)
W30.11692 (3)0.60561 (3)0.43371 (3)0.0202 (2)
W40.36003 (3)0.95497 (3)0.25472 (3)0.0186 (2)
W50.04200 (3)0.70946 (3)0.13226 (3)0.0195 (2)
W60.44450 (3)0.64344 (3)0.10820 (3)0.0194 (2)
W70.59839 (3)0.65478 (3)0.34232 (3)0.0202 (2)
W80.08595 (3)0.80863 (3)0.42223 (3)0.0194 (2)
W90.62006 (3)0.76914 (3)0.17495 (3)0.0193 (2)
W100.19271 (3)0.61973 (3)0.09293 (3)0.0181 (2)
W110.10783 (3)0.93172 (3)0.23866 (3)0.0201 (2)
W120.42288 (3)0.53033 (3)0.27617 (3)0.0204 (2)
W130.09345 (3)0.79987 (3)0.29046 (3)0.0202 (2)
W140.41071 (3)0.86512 (3)0.09684 (3)0.0196 (2)
W150.17009 (3)0.50775 (3)0.26105 (3)0.0193 (2)
W160.36946 (3)0.62933 (3)0.44849 (3)0.0208 (2)
W170.06329 (3)0.59624 (3)0.30233 (3)0.0218 (2)
W180.56863 (3)0.85973 (3)0.33407 (3)0.0197 (2)
P10.13154 (17)0.71896 (17)0.25456 (16)0.0100 (8)
P20.39783 (16)0.74358 (17)0.27104 (16)0.0100 (8)
O10.4970 (4)0.6503 (4)0.4159 (4)0.020 (3)
O20.4671 (4)0.8420 (5)0.4080 (4)0.020 (3)
O30.2108 (5)0.8097 (5)0.4439 (4)0.022 (3)
O40.2399 (5)0.6271 (5)0.4518 (4)0.023 (3)
O50.0265 (4)0.7945 (5)0.3781 (4)0.022 (3)
O60.0050 (4)0.6040 (5)0.3848 (4)0.019 (3)
O70.0735 (5)0.7023 (5)0.4753 (4)0.024 (3)
O80.0403 (5)0.8657 (5)0.4906 (5)0.032 (3)
O90.0915 (5)0.5351 (5)0.5071 (5)0.032 (3)
O100.3349 (5)0.8949 (5)0.5087 (5)0.028 (3)
O110.3605 (5)0.7301 (4)0.4930 (4)0.019 (3)
O120.3868 (5)0.5668 (5)0.5257 (5)0.035 (3)
O130.6269 (5)0.7620 (5)0.3709 (4)0.021 (3)
O140.6653 (5)0.6899 (5)0.2474 (4)0.020 (3)
O150.6385 (5)0.8506 (5)0.2394 (5)0.024 (3)
O160.7121 (5)0.7827 (5)0.1083 (5)0.027 (3)
O170.5303 (4)0.8425 (5)0.1292 (4)0.021 (3)
O180.5555 (5)0.6862 (5)0.1351 (4)0.022 (3)
O190.4420 (5)0.9089 (5)0.0080 (5)0.029 (3)
O200.2809 (5)0.8699 (5)0.0917 (4)0.022 (3)
O210.3207 (4)0.6144 (4)0.1046 (4)0.018 (3)
O220.3997 (5)0.9591 (4)0.1504 (4)0.019 (3)
O230.1998 (4)0.7337 (5)0.0707 (4)0.019 (3)
O240.1123 (5)0.9329 (4)0.1318 (4)0.021 (3)
O250.1761 (5)0.5172 (5)0.1528 (5)0.024 (3)
O260.1821 (4)0.6475 (5)0.2200 (4)0.019 (3)
O270.1445 (4)0.7173 (4)0.3377 (4)0.017 (3)
O280.1592 (4)0.8014 (5)0.2115 (4)0.019 (3)
O290.1151 (5)0.8872 (4)0.3399 (4)0.018 (3)
O300.5362 (5)0.5790 (5)0.2962 (5)0.022 (3)
O310.3025 (5)0.5131 (5)0.2531 (4)0.020 (3)
O320.4577 (5)0.4322 (5)0.2960 (5)0.030 (3)
O330.4645 (5)0.5451 (5)0.1711 (5)0.022 (3)
O340.5031 (4)0.7535 (4)0.2779 (4)0.018 (3)
O350.4819 (4)0.9274 (5)0.2793 (4)0.021 (3)
O360.3651 (4)0.8211 (4)0.2237 (4)0.018 (3)
O370.3218 (5)0.9085 (4)0.3531 (4)0.019 (3)
O380.3600 (5)1.0562 (5)0.2637 (5)0.027 (3)
O390.0248 (4)0.7096 (4)0.2476 (4)0.015 (2)
O400.1179 (4)0.7807 (4)0.1908 (4)0.0154 (17)
O410.1326 (5)0.6900 (5)0.3254 (4)0.022 (3)
O420.1373 (5)0.5204 (5)0.3329 (5)0.030 (3)
O430.1055 (5)0.7037 (5)0.0574 (4)0.026 (3)
O440.0373 (5)0.7964 (5)0.0982 (4)0.021 (3)
O450.0604 (5)0.6396 (4)0.1072 (4)0.021 (3)
O460.2349 (4)0.9498 (5)0.2314 (4)0.021 (3)
O470.4073 (5)0.7537 (5)0.0827 (4)0.023 (3)
O480.3766 (5)0.5602 (5)0.3704 (5)0.025 (3)
O490.1638 (5)0.4045 (5)0.2787 (5)0.025 (3)
O500.3503 (4)0.7355 (5)0.3507 (4)0.019 (3)
O510.4875 (5)0.6154 (5)0.0227 (5)0.030 (3)
O520.1520 (5)0.8824 (5)0.0097 (5)0.032 (3)
O530.6282 (5)0.9312 (5)0.3715 (5)0.028 (3)
O540.1942 (5)0.5880 (5)0.0055 (5)0.029 (3)
O550.0105 (5)0.8801 (5)0.2480 (5)0.025 (3)
O560.1881 (5)0.8578 (5)0.3164 (5)0.032 (3)
O570.0918 (5)0.6206 (5)0.1999 (5)0.027 (3)
O580.0422 (5)0.5345 (5)0.2639 (5)0.023 (3)
O590.1687 (5)0.5397 (4)0.3586 (4)0.021 (3)
O600.0677 (5)1.0281 (5)0.2478 (5)0.032 (3)
O650.3883 (4)0.6677 (4)0.2326 (4)0.018 (3)
O660.6794 (5)0.5958 (5)0.3853 (5)0.033 (3)
Co20.25021 (11)1.19551 (11)0.42865 (10)0.0289 (6)
O610.3623 (5)1.1326 (5)0.4371 (5)0.034 (3)
O620.3081 (5)1.2442 (5)0.3373 (5)0.029 (3)
O630.4377 (5)1.2326 (6)0.2605 (5)0.041 (3)
O640.4987 (6)1.1153 (6)0.3728 (6)0.047 (4)
N10.1978 (7)1.1349 (7)0.5197 (6)0.042 (4)
N20.2013 (7)1.1114 (6)0.3764 (6)0.032 (4)
N30.1426 (7)1.2683 (7)0.4167 (6)0.037 (4)
N40.2958 (8)1.2810 (6)0.4816 (7)0.041 (4)
C10.4227 (8)1.1489 (8)0.3809 (8)0.031 (4)
C20.3885 (9)1.2147 (8)0.3195 (8)0.032 (4)
C30.1439 (9)1.0549 (9)0.4291 (9)0.047 (6)
C40.1781 (11)1.0512 (10)0.5048 (10)0.061 (7)
C50.1431 (10)1.3356 (8)0.4636 (8)0.042 (5)
C60.2422 (10)1.3577 (9)0.4623 (9)0.051 (6)
Co10.75551 (10)0.74539 (10)0.88977 (9)0.0233 (5)
O1000.8081 (5)0.8020 (5)0.7976 (5)0.029 (3)
O1010.8672 (5)0.6799 (5)0.8865 (5)0.028 (3)
O1020.9952 (6)0.6665 (6)0.8108 (5)0.044 (3)
O1030.9297 (6)0.7946 (6)0.7154 (5)0.040 (3)
N70.8064 (6)0.8239 (6)0.9455 (6)0.031 (4)
N80.6479 (7)0.8172 (6)0.8883 (6)0.031 (4)
N90.6956 (6)0.6703 (6)0.8350 (6)0.032 (4)
N100.7108 (7)0.6771 (6)0.9801 (6)0.032 (4)
C90.7515 (9)0.8998 (8)0.9410 (8)0.043 (5)
C100.6537 (8)0.8759 (7)0.9428 (7)0.028 (4)
C110.6425 (9)0.6106 (9)0.8874 (8)0.040 (5)
C120.6927 (8)0.5962 (8)0.9557 (8)0.030 (4)
C130.8866 (8)0.7714 (7)0.7746 (8)0.027 (4)
C140.9204 (9)0.7003 (8)0.8286 (7)0.028 (4)
N51.0313 (7)0.5240 (7)0.8966 (6)0.039 (4)
C70.9898 (9)0.5365 (8)0.9698 (8)0.039 (5)
O1W0.4838 (9)1.3078 (9)0.4114 (8)0.108 (7)
O2W1.2170 (9)0.4589 (10)0.8845 (9)0.120 (8)
O3W0.0429 (11)1.3503 (10)0.3525 (9)0.135 (8)
O4W0.3016 (9)0.4337 (9)0.3171 (9)0.121 (8)
O5W1.0002 (9)0.8663 (11)0.8857 (9)0.154 (9)
O6W1.3741 (14)0.5597 (15)0.8622 (19)0.34 (2)
O7W0.4460 (13)0.7681 (13)0.9018 (11)0.172 (11)
Na10.500001.000000.500000.0182 (19)
H1A0.237501.132900.555200.0500*
H1B0.145401.159800.536600.0500*
H2A0.167201.134900.340400.0390*
H2B0.248201.083500.354100.0390*
H3A0.147401.001300.412000.0560*
H3B0.080101.073800.431300.0560*
H3C0.142401.288600.368300.0450*
H3D0.091001.240000.429500.0450*
H4A0.131901.027800.542600.0730*
H4B0.233501.017300.506700.0730*
H4C0.288901.266700.531400.0490*
H4D0.356001.288400.467700.0490*
H5A0.117901.318600.514500.0500*
H5B0.106801.381600.443500.0500*
H6A0.264301.382800.412900.0610*
H6B0.249001.395800.498500.0610*
H7C0.807300.803400.993800.0370*
H7D0.864800.834000.926800.0370*
H8D0.645100.843500.842100.0380*
H8E0.596700.788100.900000.0380*
H9A0.769600.933600.894900.0510*
H9B0.759900.929800.983000.0510*
H9C0.657600.698200.804300.0370*
H9D0.738400.644100.806600.0370*
H10A0.632300.851800.992600.0340*
H10B0.615100.923300.930200.0340*
H10C0.753300.672101.013500.0380*
H10D0.658800.698801.001400.0380*
H11A0.638200.560300.865000.0480*
H11B0.580800.631700.899700.0480*
H12A0.750300.567000.944900.0360*
H12B0.656000.564000.995200.0360*
H7A0.923800.543500.968100.0470*
H7B1.012800.586000.984700.0470*
H8A1.018800.566700.864300.0580*
H8B1.009000.479600.882100.0580*
H8C1.092000.518000.897800.0580*
H1WA0.511801.280400.445400.1300*
H1WB0.515701.346200.388100.1300*
H2WA1.223400.443200.841000.1430*
H2WB1.258600.493000.886700.1430*
H3WA0.027201.340900.307600.1620*
H3WB0.069901.396600.351500.1620*
H4WA0.329800.431400.360700.1450*
H4WB0.251900.458800.317600.1450*
H5WA1.032600.874900.920600.1850*
H5WB1.001000.907800.853300.1850*
H6WC1.409700.566200.821900.4130*
H6WD1.397500.522500.891500.4130*
H7WA0.444000.808500.927100.2070*
H7WB0.456700.725500.930800.2070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.0157 (2)0.0251 (3)0.0166 (3)0.0004 (2)0.0040 (2)0.0054 (2)
W20.0187 (2)0.0238 (3)0.0179 (3)0.0017 (2)0.0061 (2)0.0003 (2)
W30.0195 (2)0.0257 (3)0.0152 (3)0.0048 (2)0.0014 (2)0.0007 (2)
W40.0179 (2)0.0180 (3)0.0206 (3)0.0005 (2)0.0041 (2)0.0030 (2)
W50.0133 (2)0.0288 (3)0.0182 (3)0.0017 (2)0.0066 (2)0.0074 (2)
W60.0148 (2)0.0254 (3)0.0188 (3)0.0014 (2)0.0010 (2)0.0072 (2)
W70.0135 (2)0.0253 (3)0.0223 (3)0.0003 (2)0.0071 (2)0.0000 (2)
W80.0151 (2)0.0274 (3)0.0172 (3)0.0002 (2)0.0018 (2)0.0087 (2)
W90.0120 (2)0.0280 (3)0.0180 (3)0.0008 (2)0.0015 (2)0.0032 (2)
W100.0153 (2)0.0233 (3)0.0171 (3)0.0016 (2)0.0034 (2)0.0074 (2)
W110.0176 (2)0.0198 (3)0.0237 (3)0.0031 (2)0.0043 (2)0.0046 (2)
W120.0178 (2)0.0188 (3)0.0256 (3)0.0016 (2)0.0063 (2)0.0040 (2)
W130.0108 (2)0.0297 (3)0.0216 (3)0.0021 (2)0.0026 (2)0.0094 (2)
W140.0179 (2)0.0241 (3)0.0162 (3)0.0009 (2)0.0023 (2)0.0007 (2)
W150.0185 (2)0.0189 (3)0.0214 (3)0.0008 (2)0.0041 (2)0.0042 (2)
W160.0200 (2)0.0256 (3)0.0167 (3)0.0019 (2)0.0043 (2)0.0009 (2)
W170.0141 (2)0.0283 (3)0.0237 (3)0.0042 (2)0.0032 (2)0.0032 (2)
W180.0132 (2)0.0249 (3)0.0224 (3)0.0013 (2)0.0053 (2)0.0059 (2)
P10.0077 (13)0.0150 (15)0.0080 (15)0.0001 (11)0.0015 (11)0.0034 (12)
P20.0055 (12)0.0163 (16)0.0083 (15)0.0005 (11)0.0023 (10)0.0008 (12)
O10.013 (4)0.020 (5)0.027 (5)0.002 (3)0.004 (3)0.001 (4)
O20.012 (4)0.033 (5)0.018 (5)0.004 (3)0.006 (3)0.006 (4)
O30.014 (4)0.034 (5)0.021 (5)0.001 (3)0.005 (3)0.009 (4)
O40.021 (4)0.024 (5)0.025 (5)0.006 (3)0.003 (3)0.011 (4)
O50.009 (4)0.039 (5)0.019 (5)0.001 (3)0.000 (3)0.006 (4)
O60.015 (4)0.025 (5)0.017 (5)0.009 (3)0.003 (3)0.003 (4)
O70.024 (4)0.030 (5)0.020 (5)0.007 (4)0.001 (4)0.005 (4)
O80.027 (5)0.048 (6)0.022 (5)0.001 (4)0.002 (4)0.016 (4)
O90.035 (5)0.037 (6)0.026 (5)0.010 (4)0.012 (4)0.001 (4)
O100.026 (4)0.039 (5)0.021 (5)0.001 (4)0.005 (4)0.017 (4)
O110.019 (4)0.021 (5)0.019 (5)0.002 (3)0.001 (3)0.011 (4)
O120.031 (5)0.042 (6)0.031 (6)0.008 (4)0.004 (4)0.004 (4)
O130.019 (4)0.022 (5)0.021 (5)0.001 (3)0.007 (3)0.000 (4)
O140.015 (4)0.027 (5)0.018 (5)0.005 (3)0.000 (3)0.002 (4)
O150.032 (4)0.021 (5)0.022 (5)0.008 (4)0.013 (4)0.001 (4)
O160.015 (4)0.040 (5)0.026 (5)0.003 (4)0.000 (4)0.007 (4)
O170.015 (4)0.026 (5)0.019 (5)0.000 (3)0.005 (3)0.009 (4)
O180.016 (4)0.027 (5)0.024 (5)0.003 (3)0.005 (3)0.003 (4)
O190.029 (5)0.030 (5)0.025 (5)0.001 (4)0.001 (4)0.004 (4)
O200.013 (4)0.033 (5)0.019 (5)0.004 (3)0.000 (3)0.001 (4)
O210.015 (4)0.024 (5)0.017 (5)0.003 (3)0.003 (3)0.007 (3)
O220.019 (4)0.018 (4)0.019 (5)0.006 (3)0.001 (3)0.002 (3)
O230.013 (4)0.029 (5)0.017 (5)0.002 (3)0.001 (3)0.006 (4)
O240.016 (4)0.020 (5)0.027 (5)0.000 (3)0.004 (3)0.004 (4)
O250.016 (4)0.032 (5)0.025 (5)0.002 (3)0.008 (3)0.004 (4)
O260.009 (4)0.024 (5)0.025 (5)0.001 (3)0.007 (3)0.000 (4)
O270.013 (4)0.028 (5)0.012 (4)0.003 (3)0.008 (3)0.007 (3)
O280.009 (4)0.023 (5)0.023 (5)0.001 (3)0.000 (3)0.002 (4)
O290.018 (4)0.024 (5)0.014 (4)0.001 (3)0.002 (3)0.009 (3)
O300.012 (4)0.021 (5)0.034 (5)0.007 (3)0.003 (3)0.013 (4)
O310.016 (4)0.024 (5)0.021 (5)0.003 (3)0.000 (3)0.011 (4)
O320.032 (5)0.027 (5)0.032 (6)0.007 (4)0.003 (4)0.006 (4)
O330.016 (4)0.021 (5)0.031 (5)0.005 (3)0.008 (3)0.008 (4)
O340.007 (4)0.023 (5)0.024 (5)0.001 (3)0.004 (3)0.005 (4)
O350.015 (4)0.028 (5)0.020 (5)0.006 (3)0.004 (3)0.003 (4)
O360.013 (4)0.024 (5)0.015 (4)0.000 (3)0.003 (3)0.003 (4)
O370.021 (4)0.021 (5)0.014 (4)0.002 (3)0.006 (3)0.002 (3)
O380.022 (4)0.014 (4)0.044 (6)0.004 (3)0.004 (4)0.004 (4)
O390.010 (4)0.023 (4)0.013 (4)0.004 (3)0.007 (3)0.007 (3)
O400.011 (3)0.025 (3)0.011 (3)0.003 (3)0.008 (3)0.001 (3)
O410.016 (4)0.029 (5)0.023 (5)0.001 (3)0.007 (3)0.009 (4)
O420.023 (4)0.035 (5)0.032 (6)0.014 (4)0.007 (4)0.001 (4)
O430.014 (4)0.044 (6)0.020 (5)0.004 (4)0.002 (3)0.003 (4)
O440.015 (4)0.023 (5)0.025 (5)0.004 (3)0.008 (3)0.003 (4)
O450.020 (4)0.020 (5)0.026 (5)0.000 (3)0.008 (3)0.011 (4)
O460.010 (4)0.035 (5)0.020 (5)0.001 (3)0.006 (3)0.006 (4)
O470.028 (4)0.020 (5)0.021 (5)0.004 (3)0.003 (4)0.001 (4)
O480.022 (4)0.028 (5)0.024 (5)0.001 (4)0.010 (4)0.004 (4)
O490.021 (4)0.029 (5)0.027 (5)0.005 (4)0.002 (4)0.006 (4)
O500.014 (4)0.033 (5)0.011 (4)0.003 (3)0.002 (3)0.004 (4)
O510.024 (4)0.041 (6)0.024 (5)0.000 (4)0.003 (4)0.007 (4)
O520.034 (5)0.029 (5)0.033 (6)0.003 (4)0.009 (4)0.003 (4)
O530.023 (4)0.033 (5)0.029 (5)0.003 (4)0.004 (4)0.009 (4)
O540.024 (4)0.036 (5)0.029 (5)0.001 (4)0.002 (4)0.010 (4)
O550.012 (4)0.028 (5)0.036 (6)0.000 (3)0.010 (4)0.002 (4)
O560.021 (4)0.045 (6)0.031 (6)0.011 (4)0.009 (4)0.014 (4)
O570.026 (4)0.028 (5)0.029 (5)0.003 (4)0.015 (4)0.002 (4)
O580.013 (4)0.025 (5)0.031 (5)0.002 (3)0.004 (3)0.003 (4)
O590.018 (4)0.021 (5)0.026 (5)0.002 (3)0.002 (3)0.013 (4)
O600.030 (5)0.018 (5)0.048 (6)0.001 (4)0.007 (4)0.003 (4)
O650.016 (4)0.017 (4)0.021 (5)0.002 (3)0.005 (3)0.004 (4)
O660.018 (4)0.034 (5)0.047 (6)0.003 (4)0.013 (4)0.003 (5)
Co20.0374 (10)0.0298 (10)0.0202 (10)0.0058 (8)0.0065 (8)0.0052 (8)
O610.036 (5)0.051 (6)0.014 (5)0.018 (4)0.010 (4)0.001 (4)
O620.038 (5)0.029 (5)0.021 (5)0.001 (4)0.015 (4)0.001 (4)
O630.027 (5)0.052 (7)0.039 (6)0.001 (4)0.005 (4)0.009 (5)
O640.034 (5)0.055 (7)0.049 (7)0.008 (5)0.016 (5)0.011 (5)
N10.047 (7)0.045 (8)0.031 (8)0.018 (6)0.007 (6)0.008 (6)
N20.033 (6)0.026 (6)0.041 (8)0.004 (5)0.013 (5)0.011 (5)
N30.039 (6)0.046 (8)0.029 (7)0.007 (5)0.012 (5)0.010 (6)
N40.057 (7)0.031 (7)0.040 (8)0.011 (6)0.023 (6)0.017 (6)
C10.028 (7)0.039 (8)0.028 (8)0.003 (6)0.018 (6)0.002 (6)
C20.039 (6)0.032 (6)0.032 (7)0.003 (5)0.021 (6)0.015 (5)
C30.046 (9)0.052 (10)0.039 (10)0.003 (7)0.018 (8)0.003 (8)
C40.067 (11)0.047 (11)0.057 (13)0.010 (8)0.029 (9)0.018 (9)
C50.072 (11)0.031 (8)0.025 (8)0.017 (7)0.001 (7)0.018 (6)
C60.073 (11)0.049 (10)0.037 (10)0.005 (8)0.019 (8)0.022 (8)
Co10.0241 (8)0.0266 (10)0.0196 (10)0.0023 (7)0.0039 (7)0.0031 (7)
O1000.038 (5)0.035 (5)0.015 (5)0.002 (4)0.015 (4)0.001 (4)
O1010.027 (4)0.036 (5)0.020 (5)0.006 (4)0.003 (4)0.001 (4)
O1020.041 (5)0.046 (6)0.038 (6)0.020 (5)0.007 (5)0.004 (5)
O1030.041 (5)0.047 (6)0.029 (6)0.003 (5)0.002 (4)0.000 (5)
N70.030 (6)0.039 (7)0.025 (7)0.002 (5)0.013 (5)0.001 (5)
N80.031 (6)0.036 (7)0.027 (7)0.002 (5)0.005 (5)0.004 (5)
N90.029 (6)0.037 (7)0.028 (7)0.001 (5)0.002 (5)0.002 (5)
N100.036 (6)0.036 (7)0.025 (7)0.005 (5)0.010 (5)0.008 (5)
C90.057 (9)0.034 (9)0.035 (9)0.001 (7)0.002 (7)0.002 (7)
C100.042 (8)0.012 (7)0.028 (8)0.009 (5)0.010 (6)0.006 (6)
C110.034 (8)0.055 (10)0.033 (9)0.013 (7)0.000 (6)0.015 (7)
C120.023 (6)0.027 (8)0.036 (9)0.006 (5)0.004 (6)0.011 (6)
C130.032 (7)0.021 (7)0.030 (8)0.004 (6)0.000 (6)0.012 (6)
C140.038 (8)0.034 (8)0.013 (7)0.009 (6)0.000 (6)0.006 (6)
N50.051 (7)0.032 (7)0.032 (8)0.006 (5)0.002 (6)0.001 (5)
C70.039 (8)0.029 (8)0.050 (10)0.006 (6)0.015 (7)0.002 (7)
O1W0.109 (10)0.134 (13)0.083 (11)0.069 (9)0.058 (8)0.042 (10)
O2W0.093 (10)0.176 (17)0.105 (14)0.003 (10)0.040 (9)0.057 (11)
O3W0.189 (16)0.124 (14)0.080 (12)0.038 (12)0.033 (12)0.008 (10)
O4W0.088 (10)0.148 (15)0.131 (15)0.044 (10)0.053 (10)0.074 (11)
O5W0.085 (10)0.24 (2)0.130 (16)0.062 (12)0.071 (10)0.080 (15)
O6W0.167 (19)0.21 (3)0.55 (6)0.080 (18)0.22 (3)0.16 (3)
O7W0.195 (19)0.19 (2)0.139 (19)0.055 (16)0.043 (15)0.055 (15)
Na10.020 (3)0.019 (3)0.017 (4)0.003 (3)0.011 (3)0.000 (3)
Geometric parameters (Å, º) top
W1—O21.921 (6)W18—O21.905 (7)
W1—O31.900 (7)W18—O131.887 (8)
W1—O101.710 (9)W18—O151.921 (9)
W1—O111.908 (7)W18—O342.394 (7)
W1—O371.900 (7)W18—O351.931 (7)
W1—O502.374 (8)W18—O531.724 (8)
W2—O201.883 (7)Co2—N11.934 (11)
W2—O231.895 (8)Co2—O611.919 (8)
W2—O241.920 (7)Co2—O621.889 (9)
W2—O282.376 (7)Co2—N41.960 (11)
W2—O441.945 (7)Co2—N21.955 (10)
W2—O521.705 (9)Co2—N31.961 (11)
W3—O41.907 (7)Co1—N101.950 (11)
W3—O61.931 (6)Co1—N91.948 (10)
W3—O71.906 (8)Co1—N81.938 (10)
W3—O91.688 (9)Co1—O1001.922 (9)
W3—O272.408 (7)Co1—O1011.927 (8)
W3—O591.916 (7)Co1—N71.936 (10)
W4—O221.908 (7)P1—O281.542 (8)
W4—O351.902 (6)P1—O391.590 (6)
W4—O362.344 (7)P1—O271.525 (8)
W4—O371.895 (7)P1—O261.533 (8)
W4—O381.703 (8)P2—O341.569 (6)
W4—O461.920 (6)P2—O501.528 (8)
W5—O392.378 (7)P2—O651.517 (7)
W5—O401.922 (7)P2—O361.549 (7)
W5—O431.720 (7)O61—C11.290 (16)
W5—O441.892 (8)O62—C21.282 (15)
W5—O451.909 (7)O63—C21.239 (16)
W5—O571.922 (8)O64—C11.227 (15)
W6—O181.915 (8)O100—C131.288 (14)
W6—O211.895 (6)O101—C141.262 (15)
W6—O331.910 (9)O102—C141.241 (16)
W6—O471.907 (8)O103—C131.217 (16)
W6—O511.714 (9)O1W—H1WA0.8500
W6—O652.385 (7)O1W—H1WB0.8500
W7—O11.889 (7)O2W—H2WA0.8500
W7—O131.972 (8)O2W—H2WB0.8500
W7—O141.930 (7)N1—C41.48 (2)
W7—O301.882 (8)N2—C31.480 (18)
W7—O342.385 (7)N3—C51.472 (18)
W7—O661.697 (8)N4—C61.494 (18)
W8—O31.901 (7)N1—H1A0.9000
W8—O51.923 (6)N1—H1B0.9000
W8—O71.916 (8)N2—H2B0.9000
W8—O81.707 (9)N2—H2A0.9000
W8—O272.348 (7)N3—H3D0.9000
W8—O291.890 (7)N3—H3C0.9000
W9—O141.895 (8)O3W—H3WB0.8500
W9—O151.916 (9)O3W—H3WA0.8500
W9—O161.719 (8)N4—H4D0.9000
W9—O171.936 (7)N4—H4C0.9000
W9—O181.931 (8)N7—C91.466 (16)
W9—O342.398 (7)N8—C101.466 (16)
W10—O211.898 (6)N9—C111.477 (17)
W10—O231.892 (8)N10—C121.496 (17)
W10—O251.920 (9)O4W—H4WA0.8500
W10—O262.374 (7)O4W—H4WB0.8500
W10—O451.946 (7)N7—H7C0.9000
W10—O541.713 (9)N7—H7D0.9000
W11—O241.918 (7)N8—H8E0.9000
W11—O282.348 (8)N8—H8D0.9000
W11—O291.902 (7)N9—H9C0.9000
W11—O461.880 (6)N9—H9D0.9000
W11—O551.940 (8)N10—H10D0.9000
W11—O601.702 (8)N10—H10C0.9000
W12—O301.946 (8)N5—C71.432 (18)
W12—O311.882 (7)N5—H8C0.8900
W12—O321.697 (8)N5—H8A0.8900
W12—O331.925 (9)N5—H8B0.8900
W12—O481.878 (9)O5W—H5WB0.8500
W12—O652.378 (7)O5W—H5WA0.8500
W13—O51.926 (7)O6W—H6WD0.8500
W13—O392.374 (6)O6W—H6WC0.8500
W13—O401.925 (7)O7W—H7WA0.8500
W13—O411.947 (8)O7W—H7WB0.8500
W13—O551.880 (8)C1—C21.569 (19)
W13—O561.713 (8)C3—C41.49 (2)
W14—O171.905 (6)C5—C61.50 (2)
W14—O191.711 (9)C3—H3A0.9700
W14—O201.905 (7)C3—H3B0.9700
W14—O221.915 (7)C4—H4A0.9700
W14—O362.362 (7)C4—H4B0.9700
W14—O471.894 (8)C5—H5B0.9700
W15—O251.933 (9)C5—H5A0.9700
W15—O262.360 (8)C6—H6A0.9700
W15—O311.929 (7)C6—H6B0.9700
W15—O491.710 (8)C9—C101.492 (18)
W15—O581.901 (7)C11—C121.484 (19)
W15—O591.889 (7)C13—C141.542 (18)
W16—O11.931 (6)C9—H9B0.9700
W16—O41.888 (7)C9—H9A0.9700
W16—O111.926 (7)C10—H10A0.9700
W16—O121.675 (9)C10—H10B0.9700
W16—O481.903 (9)C11—H11B0.9700
W16—O502.378 (8)C11—H11A0.9700
W17—O61.884 (7)C12—H12B0.9700
W17—O392.383 (7)C12—H12A0.9700
W17—O411.888 (8)C7—C7i1.576 (19)
W17—O421.697 (8)C7—H7B0.9700
W17—O571.927 (9)C7—H7A0.9700
W17—O581.935 (8)
O2—W1—O3164.0 (3)O2—W18—O1391.1 (3)
O2—W1—O1096.5 (3)O2—W18—O15156.0 (3)
O2—W1—O1190.0 (3)O2—W18—O3483.9 (3)
O2—W1—O3785.2 (3)O2—W18—O3584.3 (3)
O2—W1—O5081.8 (3)O2—W18—O53101.3 (4)
O3—W1—O1099.3 (3)O13—W18—O1587.8 (3)
O3—W1—O1189.7 (3)O13—W18—O3473.6 (3)
O3—W1—O3788.9 (3)O13—W18—O35156.6 (3)
O3—W1—O5082.8 (3)O13—W18—O53101.9 (4)
O10—W1—O11100.5 (4)O15—W18—O3472.8 (3)
O10—W1—O37102.2 (4)O15—W18—O3587.2 (3)
O10—W1—O50173.3 (3)O15—W18—O53102.4 (4)
O11—W1—O37157.1 (3)O34—W18—O3583.1 (3)
O11—W1—O5073.0 (3)O34—W18—O53173.3 (3)
O37—W1—O5084.2 (3)O35—W18—O53101.5 (4)
O20—W2—O2389.7 (3)O61—Co2—O6285.8 (4)
O20—W2—O2490.7 (3)O61—Co2—N189.2 (4)
O20—W2—O2882.3 (3)O61—Co2—N289.8 (4)
O20—W2—O44163.3 (3)O61—Co2—N3174.8 (4)
O20—W2—O5299.0 (3)O61—Co2—N491.7 (4)
O23—W2—O24157.1 (3)O62—Co2—N1173.8 (4)
O23—W2—O2884.3 (3)O62—Co2—N290.6 (4)
O23—W2—O4484.6 (3)O62—Co2—N390.3 (4)
O23—W2—O52102.9 (4)O62—Co2—N490.0 (4)
O24—W2—O2873.1 (3)N1—Co2—N285.8 (5)
O24—W2—O4488.6 (3)N1—Co2—N394.9 (5)
O24—W2—O5299.6 (4)N1—Co2—N493.7 (5)
O28—W2—O4481.6 (3)N2—Co2—N393.7 (4)
O28—W2—O52172.6 (3)N2—Co2—N4178.4 (5)
O44—W2—O5297.5 (3)N3—Co2—N484.8 (5)
O4—W3—O6161.3 (3)N7—Co1—N885.6 (4)
O4—W3—O790.6 (3)N7—Co1—N9175.8 (4)
O4—W3—O999.1 (3)N7—Co1—N1093.4 (4)
O4—W3—O2781.8 (3)N8—Co1—N990.4 (4)
O4—W3—O5987.3 (3)N8—Co1—N1095.4 (4)
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O59—W3—O7—W86.6 (11)O22—W14—O36—P2140.7 (5)
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O27—W3—O6—W1758.3 (11)O20—W14—O47—W6136.2 (9)
O7—W3—O27—W82.3 (3)O22—W14—O47—W654.5 (14)
O27—W3—O7—W83.4 (4)O36—W14—O47—W654.5 (8)
O59—W3—O6—W1727.2 (11)O22—W14—O36—W41.6 (3)
O7—W3—O27—P1139.6 (5)O19—W14—O47—W6126.3 (8)
O6—W3—O27—P146.9 (5)O17—W14—O36—W494.0 (3)
O9—W3—O59—W15126.4 (8)O20—W14—O36—W490.2 (3)
O27—W3—O59—W1553.0 (8)O19—W14—O17—W9130.7 (9)
O6—W3—O59—W1527.9 (8)O31—W15—O26—P1129.6 (5)
O6—W3—O7—W883.5 (5)O59—W15—O25—W101.8 (12)
O7—W3—O6—W17130.7 (11)O25—W15—O26—P1139.6 (5)
O9—W3—O6—W17128.3 (11)O58—W15—O25—W1085.2 (5)
O4—W3—O27—W890.9 (3)O59—W15—O58—W1725.6 (10)
O4—W3—O27—P1127.2 (5)O31—W15—O25—W1079.0 (5)
O59—W3—O27—P139.2 (5)O58—W15—O26—W1093.8 (3)
O6—W3—O27—W895.0 (3)O49—W15—O25—W10175.8 (4)
O59—W3—O27—W8179.0 (3)O26—W15—O59—W353.5 (8)
O4—W3—O7—W877.8 (5)O49—W15—O58—W17127.6 (10)
O7—W3—O59—W1549.8 (13)O25—W15—O26—W102.2 (3)
O4—W3—O59—W15134.9 (8)O25—W15—O59—W354.8 (14)
O35—W4—O36—P248.0 (5)O58—W15—O26—P148.0 (5)
O46—W4—O36—P2127.3 (5)O26—W15—O25—W103.2 (4)
O22—W4—O36—P2140.8 (5)O26—W15—O58—W1759.9 (10)
O36—W4—O22—W142.3 (4)O59—W15—O26—P140.9 (5)
O46—W4—O22—W1479.4 (5)O31—W15—O26—W1088.6 (3)
O46—W4—O37—W1135.0 (9)O49—W15—O59—W3127.5 (8)
O38—W4—O35—W18131.5 (9)O25—W15—O58—W17133.6 (10)
O38—W4—O37—W1127.8 (8)O59—W15—O26—W10177.3 (3)
O37—W4—O36—P238.6 (5)O31—W15—O59—W3135.7 (8)
O37—W4—O22—W143.8 (11)O58—W15—O59—W328.7 (8)
O35—W4—O37—W129.8 (9)O48—W16—O50—W1179.5 (3)
O46—W4—O36—W1490.3 (3)O4—W16—O50—W190.2 (3)
O35—W4—O36—W1494.4 (3)O11—W16—O50—W12.4 (2)
O37—W4—O35—W1828.8 (9)O12—W16—O1—W7127.9 (8)
O37—W4—O36—W14179.0 (3)O50—W16—O1—W761.4 (8)
O38—W4—O22—W14176.9 (4)O11—W16—O1—W7133.9 (8)
O22—W4—O37—W151.5 (14)O50—W16—O11—W13.5 (4)
O22—W4—O36—W141.6 (3)O48—W16—O1—W724.0 (8)
O36—W4—O35—W1856.8 (9)O50—W16—O48—W1249.9 (10)
O36—W4—O37—W152.9 (8)O11—W16—O48—W1245.4 (15)
O35—W4—O22—W1484.3 (5)O4—W16—O48—W12132.6 (10)
O22—W4—O35—W18129.6 (9)O1—W16—O48—W1231.0 (10)
O45—W5—O39—W13178.5 (3)O1—W16—O50—P247.8 (5)
O45—W5—O40—W136.9 (10)O1—W16—O50—W194.7 (3)
O39—W5—O40—W131.1 (3)O12—W16—O11—W1178.8 (5)
O43—W5—O40—W13170.9 (4)O12—W16—O48—W12127.4 (10)
O57—W5—O40—W1371.0 (4)O48—W16—O50—P238.1 (5)
O44—W5—O40—W1385.8 (4)O11—W16—O50—P2140.1 (5)
O39—W5—O45—W1058.3 (8)O48—W16—O11—W18.2 (11)
O57—W5—O44—W246.8 (14)O4—W16—O50—P2127.4 (5)
O40—W5—O45—W1052.7 (13)O1—W16—O11—W183.7 (5)
O57—W5—O45—W10130.5 (8)O4—W16—O11—W178.7 (5)
O40—W5—O39—W130.8 (2)O57—W17—O39—W51.5 (3)
O44—W5—O39—W1391.8 (3)O41—W17—O39—W131.6 (3)
O45—W5—O57—W1786.9 (5)O41—W17—O6—W3131.3 (11)
O57—W5—O39—W1391.9 (3)O6—W17—O39—W5176.2 (3)
O43—W5—O44—W2128.8 (9)O6—W17—O39—W1393.3 (3)
O45—W5—O44—W228.7 (9)O57—W17—O58—W15132.3 (10)
O43—W5—O45—W10129.5 (8)O58—W17—O39—W590.6 (3)
O44—W5—O45—W1026.9 (8)O39—W17—O6—W357.8 (11)
O44—W5—O57—W1711.7 (12)O41—W17—O39—W592.1 (3)
O40—W5—O57—W1771.1 (5)O42—W17—O6—W3125.7 (11)
O44—W5—O39—P142.7 (5)O6—W17—O58—W1523.9 (10)
O45—W5—O39—P144.0 (5)O58—W17—O39—P144.4 (5)
O40—W5—O44—W2129.2 (9)O6—W17—O57—W514.9 (11)
O39—W5—O44—W255.8 (9)O41—W17—O58—W1553.6 (15)
O45—W5—O39—W1791.1 (3)O6—W17—O41—W1385.6 (5)
O43—W5—O57—W17172.7 (5)O39—W17—O41—W132.3 (4)
O57—W5—O39—P1133.6 (5)O58—W17—O6—W326.0 (11)
O44—W5—O39—W17177.8 (3)O42—W17—O57—W5173.5 (5)
O40—W5—O39—P1133.8 (5)O57—W17—O39—P1133.4 (5)
O40—W5—O39—W1791.1 (3)O41—W17—O39—P1133.0 (5)
O39—W5—O57—W172.3 (4)O39—W17—O58—W1560.1 (10)
O57—W5—O39—W171.6 (3)O42—W17—O58—W15127.1 (10)
O18—W6—O33—W1287.4 (5)O39—W17—O57—W52.3 (4)
O18—W6—O47—W1429.2 (9)O41—W17—O57—W570.9 (5)
O33—W6—O47—W1452.6 (14)O57—W17—O6—W345.8 (16)
O33—W6—O65—W123.2 (3)O6—W17—O39—P141.3 (5)
O18—W6—O65—W1295.7 (3)O58—W17—O39—W13178.9 (3)
O47—W6—O65—P239.6 (5)O57—W17—O39—W1392.1 (3)
O21—W6—O65—P2128.5 (5)O58—W17—O41—W139.0 (11)
O18—W6—O65—P247.2 (5)O57—W17—O41—W1369.3 (5)
O21—W6—O65—W1288.7 (3)O58—W17—O57—W586.3 (5)
O65—W6—O47—W1454.3 (8)O42—W17—O41—W13170.2 (5)
O33—W6—O18—W9124.0 (9)O15—W18—O13—W772.7 (5)
O65—W6—O18—W951.0 (8)O53—W18—O35—W4128.9 (9)
O47—W6—O33—W126.5 (11)O2—W18—O15—W919.1 (11)
O21—W6—O33—W1277.1 (5)O53—W18—O2—W1130.2 (10)
O51—W6—O33—W12175.1 (5)O13—W18—O15—W968.8 (5)
O33—W6—O65—P2139.7 (5)O34—W18—O2—W154.1 (10)
O47—W6—O18—W933.8 (9)O15—W18—O34—W93.1 (3)
O47—W6—O65—W12177.6 (3)O34—W18—O35—W456.0 (9)
O51—W6—O47—W14125.9 (8)O35—W18—O2—W129.6 (10)
O21—W6—O47—W14136.4 (9)O34—W18—O15—W94.7 (4)
O65—W6—O33—W124.7 (4)O35—W18—O15—W988.4 (5)
O51—W6—O18—W9135.2 (9)O35—W18—O34—W992.3 (3)
O34—W7—O13—W180.0 (4)O13—W18—O35—W451.2 (14)
O14—W7—O13—W1873.7 (5)O15—W18—O35—W4129.0 (9)
O13—W7—O34—W990.1 (3)O15—W18—O34—P2132.5 (6)
O30—W7—O13—W185.4 (11)O35—W18—O34—P243.3 (5)
O1—W7—O34—W1891.0 (3)O13—W18—O2—W1127.5 (10)
O34—W7—O30—W1256.4 (10)O15—W18—O2—W140.3 (16)
O13—W7—O34—P2135.5 (5)O2—W18—O34—W9177.3 (3)
O13—W7—O14—W972.5 (5)O2—W18—O34—P241.7 (5)
O30—W7—O34—W992.0 (3)O13—W18—O34—P2134.7 (5)
O1—W7—O14—W94.1 (11)O53—W18—O13—W7174.9 (5)
O66—W7—O30—W12129.2 (10)O2—W18—O35—W428.5 (9)
O66—W7—O13—W18174.2 (5)O2—W18—O34—W793.0 (3)
O30—W7—O34—W18177.9 (3)O13—W18—O34—W70.0 (3)
O34—W7—O14—W90.6 (4)O15—W18—O34—W792.9 (3)
O1—W7—O13—W1883.0 (4)O34—W18—O13—W70.0 (4)
O1—W7—O34—P244.5 (5)O35—W18—O13—W75.0 (10)
O30—W7—O14—W985.2 (5)O2—W18—O13—W783.3 (4)
O1—W7—O34—W9178.9 (3)O53—W18—O15—W9170.5 (5)
O30—W7—O34—P242.4 (5)O35—W18—O34—W7178.0 (3)
O14—W7—O1—W1658.2 (12)O13—W18—O34—W989.8 (3)
O13—W7—O1—W16134.0 (8)O61—Co2—O62—C22.9 (9)
O14—W7—O34—W1890.4 (3)O62—Co2—O61—C10.8 (8)
O66—W7—O1—W16125.6 (8)N1—Co2—O61—C1175.6 (9)
O66—W7—O14—W9172.1 (5)N2—Co2—O61—C189.8 (9)
O14—W7—O34—W90.4 (3)O62—Co2—N2—C3178.4 (8)
O14—W7—O34—P2134.1 (5)N1—Co2—N2—C36.6 (8)
O30—W7—O1—W1623.7 (8)N3—Co2—N2—C388.1 (9)
O14—W7—O30—W12129.4 (10)O62—Co2—N3—C5101.3 (9)
O13—W7—O34—W180.0 (2)N1—Co2—N3—C582.0 (9)
O1—W7—O30—W1226.9 (10)O61—Co2—N4—C6158.7 (9)
O13—W7—O30—W1251.2 (16)N3—Co2—N4—C617.4 (9)
O34—W7—O1—W1661.6 (8)N1—Co2—N4—C6112.0 (9)
O5—W8—O27—P147.2 (5)N4—Co2—N3—C511.3 (9)
O7—W8—O27—W32.3 (2)N2—Co2—N3—C5168.1 (9)
O5—W8—O27—W393.7 (3)N2—Co2—O62—C286.8 (9)
O29—W8—O27—P140.1 (5)N3—Co2—O62—C2179.5 (9)
O29—W8—O27—W3179.0 (3)N4—Co2—O62—C294.6 (9)
O27—W8—O5—W1356.8 (9)N2—Co2—N1—C417.5 (9)
O7—W8—O27—P1138.6 (5)O61—Co2—N2—C395.8 (8)
O29—W8—O5—W1326.9 (9)N4—Co2—N1—C4164.0 (9)
O8—W8—O29—W11124.8 (9)O62—Co2—N4—C672.9 (9)
O8—W8—O5—W13129.7 (9)N3—Co2—N1—C4110.9 (9)
O7—W8—O5—W13130.6 (9)O61—Co2—N1—C472.3 (9)
O8—W8—O7—W3176.9 (5)N4—Co2—O61—C190.7 (9)
O3—W8—O27—W390.1 (3)N10—Co1—O101—C14175.4 (9)
O3—W8—O29—W11137.9 (9)O100—Co1—N7—C977.1 (8)
O27—W8—O29—W1154.7 (9)O101—Co1—N7—C9162.7 (8)
O5—W8—O29—W1128.2 (9)N8—Co1—N7—C913.5 (8)
O5—W8—O7—W385.9 (5)N10—Co1—N8—C1079.1 (8)
O29—W8—O7—W36.7 (11)N7—Co1—N10—C12162.6 (7)
O27—W8—O7—W33.4 (4)O101—Co1—N10—C1269.7 (7)
O3—W8—O7—W379.2 (5)N7—Co1—N8—C1013.9 (8)
O3—W8—O27—P1129.1 (5)N10—Co1—N7—C9108.6 (8)
O7—W8—O29—W1151.6 (14)N9—Co1—N8—C10165.2 (8)
O15—W9—O18—W636.7 (15)N8—Co1—N10—C12111.6 (7)
O16—W9—O17—W14129.6 (9)N9—Co1—O101—C1489.4 (9)
O34—W9—O17—W1455.5 (8)O100—Co1—N9—C11179.9 (8)
O18—W9—O34—P241.8 (5)O101—Co1—N9—C1194.5 (8)
O15—W9—O34—P2132.5 (5)N9—Co1—N10—C1221.5 (7)
O16—W9—O14—W7174.0 (5)O100—Co1—N8—C10103.7 (8)
O18—W9—O17—W1429.9 (9)O101—Co1—O100—C132.6 (8)
O14—W9—O34—P2133.4 (5)N8—Co1—N9—C1189.3 (8)
O15—W9—O17—W14128.4 (9)N10—Co1—N9—C116.1 (8)
O17—W9—O34—P243.0 (5)N7—Co1—O101—C1491.3 (9)
O15—W9—O14—W771.8 (5)N7—Co1—O100—C1395.6 (8)
O15—W9—O34—W183.1 (3)N9—Co1—O100—C1388.5 (8)
O17—W9—O34—W1892.6 (3)O100—Co1—O101—C141.6 (8)
O16—W9—O18—W6133.0 (9)N8—Co1—O100—C13178.9 (8)
O18—W9—O34—W18177.5 (3)O39—P1—O27—W862.9 (5)
O14—W9—O17—W1446.6 (14)O39—P1—O26—W1065.1 (6)
O17—W9—O18—W633.7 (9)O28—P1—O27—W853.8 (5)
O18—W9—O14—W785.2 (5)O28—P1—O26—W1052.0 (6)
O14—W9—O34—W70.4 (3)O39—P1—O27—W364.8 (5)
O18—W9—O34—W791.9 (3)O27—P1—O26—W1553.9 (5)
O17—W9—O15—W1888.8 (5)O27—P1—O26—W10177.5 (4)
O34—W9—O18—W650.5 (8)O27—P1—O28—W1152.8 (5)
O34—W9—O14—W70.6 (4)O26—P1—O27—W8179.9 (4)
O14—W9—O18—W6123.7 (9)O26—P1—O28—W11178.7 (4)
O15—W9—O34—W793.7 (3)O27—P1—O39—W5179.1 (4)
O14—W9—O34—W1891.0 (3)O27—P1—O28—W2178.2 (4)
O17—W9—O34—W7176.7 (3)O39—P1—O28—W264.8 (5)
O17—W9—O14—W79.8 (12)O26—P1—O39—W13179.8 (4)
O34—W9—O15—W184.7 (4)O27—P1—O39—W1359.5 (5)
O18—W9—O15—W1819.1 (12)O39—P1—O28—W1164.1 (5)
O16—W9—O15—W18171.3 (5)O26—P1—O28—W252.3 (5)
O14—W9—O15—W1868.2 (5)O26—P1—O39—W560.6 (5)
O45—W10—O23—W231.9 (9)O39—P1—O26—W1563.5 (5)
O54—W10—O45—W5128.7 (8)O26—P1—O27—W352.5 (5)
O21—W10—O23—W2132.8 (9)O28—P1—O27—W3178.5 (4)
O26—W10—O45—W558.4 (8)O28—P1—O26—W15179.4 (4)
O26—W10—O23—W250.0 (9)O28—P1—O39—W1359.8 (6)
O21—W10—O25—W1579.0 (4)O26—P1—O39—W1760.2 (6)
O21—W10—O26—P1127.3 (5)O28—P1—O39—W17179.4 (4)
O25—W10—O23—W242.4 (13)O27—P1—O39—W1760.1 (5)
O23—W10—O45—W527.0 (8)O28—P1—O39—W559.8 (5)
O25—W10—O45—W5132.0 (8)O65—P2—O34—W18179.4 (4)
O45—W10—O26—P148.6 (5)O65—P2—O34—W959.9 (5)
O54—W10—O23—W2127.4 (9)O50—P2—O34—W1859.4 (6)
O25—W10—O26—P1139.7 (5)O36—P2—O34—W1860.6 (5)
O23—W10—O26—P137.3 (5)O36—P2—O65—W652.2 (5)
O23—W10—O26—W15179.3 (2)O65—P2—O50—W1178.7 (4)
O25—W10—O26—W152.2 (3)O34—P2—O65—W664.3 (5)
O45—W10—O26—W1593.4 (2)O50—P2—O34—W9179.9 (4)
O45—W10—O25—W1584.8 (4)O50—P2—O65—W1251.9 (5)
O23—W10—O25—W1511.1 (11)O34—P2—O50—W1664.8 (6)
O54—W10—O25—W15179.0 (4)O36—P2—O50—W16178.9 (4)
O21—W10—O26—W1590.8 (3)O65—P2—O50—W1652.3 (5)
O26—W10—O25—W153.2 (4)O50—P2—O65—W6178.8 (4)
O55—W11—O29—W827.3 (9)O36—P2—O50—W152.0 (5)
O46—W11—O29—W8137.0 (9)O36—P2—O65—W12178.5 (4)
O24—W11—O29—W849.1 (14)O36—P2—O34—W7179.0 (4)
O60—W11—O29—W8123.9 (9)O50—P2—O34—W761.1 (6)
O60—W11—O55—W13128.5 (11)O36—P2—O34—W960.2 (5)
O28—W11—O29—W854.6 (9)O50—P2—O36—W452.0 (5)
O29—W11—O28—P138.8 (5)O65—P2—O36—W4178.5 (4)
O29—W11—O24—W210.5 (11)O34—P2—O36—W1464.8 (5)
O55—W11—O24—W286.1 (5)O50—P2—O36—W14178.6 (4)
O28—W11—O24—W24.8 (4)O65—P2—O36—W1452.1 (5)
O24—W11—O28—W23.3 (3)O34—P2—O65—W1265.0 (5)
O24—W11—O55—W13131.8 (11)O34—P2—O50—W164.3 (5)
O29—W11—O28—W2178.9 (3)O65—P2—O34—W758.9 (5)
O46—W11—O28—W289.4 (3)O34—P2—O36—W464.6 (5)
O46—W11—O28—P1128.4 (5)Co2—O61—C1—O64178.3 (11)
O29—W11—O55—W1326.3 (11)Co2—O61—C1—C21.0 (13)
O55—W11—O28—P147.1 (5)Co2—O62—C2—C14.0 (13)
O60—W11—O24—W2176.5 (4)Co2—O62—C2—O63175.1 (11)
O46—W11—O24—W277.0 (5)Co1—O100—C13—O103175.6 (10)
O24—W11—O28—P1139.0 (5)Co1—O100—C13—C142.9 (12)
O28—W11—O55—W1358.1 (11)Co1—O101—C14—O102177.1 (11)
O55—W11—O28—W295.1 (3)Co1—O101—C14—C130.5 (13)
O48—W12—O65—P237.4 (5)Co2—N1—C4—C337.8 (13)
O30—W12—O33—W685.9 (5)Co2—N2—C3—C429.1 (13)
O48—W12—O33—W613.4 (11)Co2—N3—C5—C636.7 (12)
O33—W12—O65—W63.1 (3)Co2—N4—C6—C542.1 (13)
O32—W12—O33—W6177.7 (5)Co1—N7—C9—C1037.0 (12)
O65—W12—O33—W64.7 (4)Co1—N8—C10—C938.1 (11)
O32—W12—O48—W16127.9 (10)Co1—N9—C11—C1232.5 (12)
O30—W12—O65—P248.4 (5)Co1—N10—C12—C1145.3 (11)
O31—W12—O65—W689.4 (3)O61—C1—C2—O623.4 (16)
O33—W12—O65—P2139.3 (5)O64—C1—C2—O62179.3 (12)
O30—W12—O65—W693.9 (3)O64—C1—C2—O632 (2)
O65—W12—O30—W756.7 (10)O61—C1—C2—O63175.8 (12)
O31—W12—O33—W678.5 (5)N2—C3—C4—N143.2 (15)
O65—W12—O48—W1649.3 (10)N3—C5—C6—N450.8 (14)
O33—W12—O30—W7129.8 (10)N7—C9—C10—N848.6 (13)
O48—W12—O65—W6179.8 (3)N9—C11—C12—N1050.9 (13)
O31—W12—O48—W16132.9 (10)O100—C13—C14—O1011.7 (16)
O30—W12—O48—W1632.2 (10)O103—C13—C14—O1020.9 (19)
O33—W12—O48—W1640.9 (16)O100—C13—C14—O102179.4 (11)
O32—W12—O30—W7131.2 (10)O103—C13—C14—O101176.9 (12)
O48—W12—O30—W728.6 (10)N5—C7—C7i—N5i180.0 (10)
O31—W12—O65—P2128.2 (5)
Symmetry code: (i) x+2, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···O100ii0.902.593.314 (14)138
N2—H2A···O103ii0.902.072.940 (14)163
N2—H2B···O380.902.263.115 (13)157
O2W—H2WA···O57iii0.852.442.919 (17)117
N3—H3C···O103ii0.902.482.994 (14)117
O2W—H2WB···O6W0.852.042.86 (3)162
N4—H4D···O1W0.902.062.939 (18)167
O3W—H3WA···O102ii0.852.163.000 (18)172
O4W—H4WA···O12iv0.852.142.983 (18)173
N7—H7D···O5W0.902.113.010 (17)176
O4W—H4WB···O420.852.052.891 (16)173
N5—H8A···O1020.891.862.740 (15)170
N5—H8B···O45iii0.892.233.076 (13)158
N5—H8B···O57iii0.892.543.166 (14)128
N5—H8C···O2W0.892.052.881 (17)155
N8—H8E···O7W0.902.233.07 (2)154
N9—H9C···O63ii0.902.123.023 (13)175
N9—H9D···O49iii0.902.203.088 (13)170
C3—H3A···O290.972.493.417 (17)160
C4—H4B···O100.972.473.396 (18)160
C11—H11A···O33iii0.972.523.376 (17)147
C12—H12A···O25iii0.972.513.297 (16)139
Symmetry codes: (ii) x+1, y+2, z+1; (iii) x+1, y+1, z+1; (iv) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···O100i0.902.593.314 (14)138
N2—H2A···O103i0.902.072.940 (14)163
N2—H2B···O380.902.263.115 (13)157
O2W—H2WA···O57ii0.852.442.919 (17)117
N3—H3C···O103i0.902.482.994 (14)117
O2W—H2WB···O6W0.852.042.86 (3)162
N4—H4D···O1W0.902.062.939 (18)167
O3W—H3WA···O102i0.852.163.000 (18)172
O4W—H4WA···O12iii0.852.142.983 (18)173
N7—H7D···O5W0.902.113.010 (17)176
O4W—H4WB···O420.852.052.891 (16)173
N5—H8A···O1020.891.862.740 (15)170
N5—H8B···O45ii0.892.233.076 (13)158
N5—H8B···O57ii0.892.543.166 (14)128
N5—H8C···O2W0.892.052.881 (17)155
N8—H8E···O7W0.902.233.07 (2)154
N9—H9C···O63i0.902.123.023 (13)175
N9—H9D···O49ii0.902.203.088 (13)170
C3—H3A···O290.972.493.417 (17)160
C4—H4B···O100.972.473.396 (18)160
C11—H11A···O33ii0.972.523.376 (17)147
C12—H12A···O25ii0.972.513.297 (16)139
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y+1, z+1; (iii) x, y+1, z+1.
Acknowledgements top

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references
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