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In the crystal structure of the title compound, Na9[Dy(W5O18)2]·35H2O, the complex anion has approximate D4d symmetry, with Dy-O and W-O distances in the ranges 2.355 (6)-2.405 (6) and 1.715 (7)-2.369 (5) Å, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102016773/ta1388sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102016773/ta1388Isup2.hkl
Contains datablock I

Comment top

To date, the emission spectra of various polyoxometallolanthanoates have been studied. In particular, trivalent Eu3+ ions in polyoxometallates exhibit strong red emissions under excitation of the oxygen-to-metal (M = Mo, W or Nb) polyoxometallate charge-transfer bands (O M ligand-to-metal charge transfer, LMCT), and their emission properties have been examined in order to gain a molecular insight into the intramolecular energy transfer to the 5D0 and 5D1 states of Eu3+ (Yamase, 1998).

In recent years, we have studied dysprosium oxide solids, which emit in the yellow and blue regions with a resultant white light (Su et al., 1995). Powdered solids of decatungstodysprosate containing trivalent Dy3+ show a white or yellow luminescence on irradiation with 320 nm light, corresponding to the O W LMCT band excitation. In the present study, the crystal structure of nonasodium decatungstodysprosate, Na9[Dy(W5O18)2], as the pentatriacontahydrate, (I), has been determined and it is compared with that of another decatungstodysprosate complex, K3Na4H2[DyW10O36].21H2O, (II), previously reported by Ozeki & Yamase (1994a?). \sch

The structure of the complex anion in the title compound, (I), with the atomic numbering, is shown in Fig. 1, the arrangement of the Na polyhedra is shown in Fig. 2 and the crystal structure is shown in Fig. 3. There is one decatungstodysprosate anion, together with nine Na+ cations and 35 water molecules, in the asymmetric unit.

The metal-oxygen framework of (I) is almost the same as that found in (II). The Dy—O distances in the two [W5O18]6- groups of (I) are in the range 2.355 (6)–2.392 (6) Å [average 2.38 (1) Å] for O atoms attached to W1—W4 and 2.391 (6)–2.405 (6) Å [average 2.40 (1) Å] for O atoms attached to W6—W9; almost the same values were observed for (II) [average 2.39 (2) and 2.40 (2) Å, respectively]. The Dy—W distances in (I), which range from 3.7725 (6) to 3.8242 (5) Å [average 3.801 (2) Å], are slightly shorter than those in (II) [average 3.83 (2) Å]. A similar trend has been reported in other decatungstolanthanoate complexes, with Ln = Sm3+ (Ozeki & Yamase, 1994b?) and Gd3+ (Yamase et al., 1994). The slight differences originate from the crystal packing of the compounds. The O atoms bonded by the lanthanide atoms in (II) also coordinate the K+ cations in their vicinity. Such a bipolar interaction of these O atoms reduces their electron densities, with a resultant elongation of the Ln—W distances in these salts.

Other lanthanide-incorporating compounds show similar structures with a variety of Ln—W distances due to the lanthanoid contraction; the Ce—W distances in Na6H2[Ce(W5O18)2].30H2O (Iball et al., 1974) are in the range 3.784–3.797 Å [average 3.79 Å], slightly shorter than the Dy—W distances in (I) [average 3.801 (2) Å]. Similarly, an actinide-incorporating compound, Na8[Th(W5O18)2].28H2O (Griffith et al., 2000), has long Th—W distances [average 3.822 Å] compared with (I).

The Na+ cations in (I), except for atom Na9, are octahedrally coordinated by O atoms, with Na—O distances in the range 2.658 (8)–2.708 (8) Å [average 2.44 (6) Å], while atom Na9 is square-pyramidally coordinated by O atoms, with Na—O distances in the range 2.286 (8)–2.346 (9) Å [average 2.33 (2) Å]. These NaOn (n = 5–6) polyhedra are connected by an edge-sharing linkage for Na1—Na4 and Na5—Na9, and by a corner-sharing linkage between Na4 and Na5 sites (Fig. 4). Such hydrated Na+ cations interact with the highly-charged [LnW10O36]9- anions to balance the charge, leading to a large number of water molecules in the lattice, as exemplified by other sodium salts of decatungstolanthanoate, namely Na6H2[Ce(W5O18)2].30H2O (Iball et al., 1974), Na6H3[Sm(W5O18)2].28H2O (Ozeki & Yamase, 1994b?) and Na8H[Gd(W5O18)2].30H2O (Yamase et al., 1994).

Experimental top

The title compound was synthesized according to the method of Yamase et al. (1994) and recrystallized from an aqueous solution at 277 K.

Refinement top

The positions of the H atoms of the water molecules were not determined. In the difference Fourier map, the highest peak is 4.44 e Å-3 (0.77 Å from W5) and the deepest hole is -3.19 e Å-3 (1.15 Å from O19).

Computing details top

Data collection: PROCESS-AUTO (Rigaku Corporation, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Molecular Structure Corporation & Rigaku Corporation, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997).

Figures top
[Figure 1] Fig. 1. A view of the decatungstodysprosate anion in (I). Displacement ellipsoids are drawn at the 50% probability level.
[Figure 2] Fig. 2. A view of (I) except for the anion. Displacement ellipsoids are drawn at the 50% probability level [symmetry codes: (i) x, y, 1 + z, (ii) -x, -y, 1 - z, (iii) -x, 1 - y, 1 - z]. The Na+ cations are octahedrally coordinated, except for Na9 which is coordinated square-pyramidally.
[Figure 3] Fig. 3. The crystal structure of (I) viewed down the c axis. Dark spheres show Na+ cations and white spheres show water O atoms.
[Figure 4] Fig. 4. A schematic diagram of the NaOn (n = 5–6) polyhedra linkage system. Single lines indicate Na—O bonds. All labels of aqueous atoms have been omitted for clarity. There are two groups of edge-shared NaOn polyhedra, Na1—Na4 (Group A) and Na5—Na9 (Group B). Group B is connected to another B at each end by edge-sharing. Four O atoms of the decatungstodysprosate anion are connected to atoms Na1, Na4, Na5 and Na8.
Nonasodium decatungstodysprosate pentatriacontahydrate top
Crystal data top
Na9[Dy(W5O18)2]·35H2OZ = 2
Mr = 3414.54F(000) = 3086
Triclinic, P1Dx = 3.460 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 13.0914 (8) ÅCell parameters from 27035 reflections
b = 20.5067 (12) Åθ = 1.6–27.5°
c = 12.7721 (6) ŵ = 18.78 mm1
α = 105.519 (1)°T = 296 K
β = 91.231 (2)°Prism, colourless
γ = 82.789 (2)°0.14 × 0.12 × 0.08 mm
V = 3277.4 (3) Å3
Data collection top
Rigaku RAXIS-RAPID
diffractometer
14785 independent reflections
Radiation source: fine-focus sealed tube13098 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 10.00 pixels mm-1θmax = 27.5°, θmin = 1.0°
ω scansh = 016
Absorption correction: numerical
(NUMABS; Higashi, 1999)
k = 2626
Tmin = 0.179, Tmax = 0.315l = 1616
33444 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH-atom parameters not defined
R[F2 > 2σ(F2)] = 0.036 w = 1/[σ2(Fo2) + (0.0579P)2 + 24.6886P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.104(Δ/σ)max = 0.031
S = 1.18Δρmax = 4.44 e Å3
14785 reflectionsΔρmin = 3.19 e Å3
821 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
426 restraintsExtinction coefficient: 0.00070 (3)
Primary atom site location: structure-invariant direct methods
Crystal data top
Na9[Dy(W5O18)2]·35H2Oγ = 82.789 (2)°
Mr = 3414.54V = 3277.4 (3) Å3
Triclinic, P1Z = 2
a = 13.0914 (8) ÅMo Kα radiation
b = 20.5067 (12) ŵ = 18.78 mm1
c = 12.7721 (6) ÅT = 296 K
α = 105.519 (1)°0.14 × 0.12 × 0.08 mm
β = 91.231 (2)°
Data collection top
Rigaku RAXIS-RAPID
diffractometer
14785 independent reflections
Absorption correction: numerical
(NUMABS; Higashi, 1999)
13098 reflections with I > 2σ(I)
Tmin = 0.179, Tmax = 0.315Rint = 0.052
33444 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036426 restraints
wR(F2) = 0.104H-atom parameters not defined
S = 1.18 w = 1/[σ2(Fo2) + (0.0579P)2 + 24.6886P]
where P = (Fo2 + 2Fc2)/3
14785 reflectionsΔρmax = 4.44 e Å3
821 parametersΔρmin = 3.19 e Å3
Special details top

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 > 2σ(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
W10.19777 (3)0.15618 (2)0.07585 (3)0.00807 (8)
W20.06976 (3)0.30697 (2)0.16294 (3)0.00813 (8)
W30.06830 (3)0.24961 (2)0.32232 (3)0.00833 (8)
W40.06021 (3)0.09708 (2)0.23668 (3)0.00845 (8)
W50.05693 (3)0.17255 (2)0.05733 (3)0.00894 (8)
W60.27757 (3)0.23014 (2)0.66701 (3)0.00821 (8)
W70.46879 (3)0.17046 (2)0.49337 (3)0.00849 (8)
W80.46517 (3)0.31991 (2)0.45000 (3)0.00816 (8)
W90.27257 (3)0.38072 (2)0.62300 (3)0.00812 (8)
W100.49113 (3)0.30625 (2)0.70245 (3)0.00863 (8)
Dy0.21823 (3)0.23691 (2)0.37660 (3)0.00801 (9)
Na10.5690 (3)0.3793 (2)1.1999 (4)0.0212 (9)
Na20.5479 (3)0.2071 (2)1.0587 (3)0.0162 (8)
Na30.5470 (3)0.0621 (2)0.8186 (3)0.0189 (8)
Na40.2821 (3)0.0108 (2)0.7962 (4)0.0232 (9)
Na50.0093 (3)0.0578 (2)0.6338 (3)0.0155 (8)
Na60.1022 (3)0.2327 (2)0.6872 (3)0.0175 (8)
Na70.1358 (3)0.4120 (2)0.7473 (4)0.0209 (8)
Na80.2059 (3)0.5634 (2)0.9698 (3)0.0183 (8)
Na90.1030 (3)0.4907 (2)0.5656 (4)0.0199 (8)
O10.2862 (5)0.1177 (3)0.0277 (6)0.0156 (13)
O20.0689 (5)0.3828 (3)0.1283 (6)0.0166 (14)
O30.1758 (5)0.2843 (3)0.4053 (6)0.0134 (13)
O40.0491 (5)0.0193 (3)0.2584 (6)0.0154 (13)
O50.1470 (5)0.1543 (4)0.0437 (6)0.0186 (14)
O60.2162 (5)0.1994 (3)0.7592 (6)0.0150 (13)
O70.5485 (5)0.0944 (3)0.4555 (6)0.0166 (14)
O80.5403 (5)0.3576 (3)0.3780 (6)0.0132 (13)
O90.2048 (5)0.4605 (3)0.6794 (6)0.0149 (13)
O100.5769 (5)0.3279 (3)0.8074 (6)0.0156 (13)
O110.1704 (5)0.2486 (3)0.0596 (5)0.0108 (12)
O120.0471 (5)0.3262 (3)0.2630 (5)0.0099 (12)
O130.0547 (5)0.1541 (3)0.3231 (5)0.0108 (12)
O140.1634 (5)0.0777 (3)0.1219 (5)0.0134 (13)
O150.0703 (5)0.1411 (3)0.0178 (5)0.0118 (12)
O160.0328 (5)0.2644 (3)0.0549 (5)0.0123 (13)
O170.1421 (5)0.2184 (3)0.1826 (5)0.0108 (12)
O180.0396 (5)0.0951 (3)0.1130 (5)0.0091 (12)
O190.2744 (5)0.1822 (3)0.1950 (6)0.0118 (12)
O200.1589 (5)0.3145 (3)0.2728 (5)0.0099 (12)
O210.0374 (5)0.2651 (3)0.4140 (6)0.0123 (13)
O220.1526 (5)0.1313 (3)0.3351 (5)0.0109 (12)
O230.3807 (4)0.1543 (3)0.6037 (5)0.0078 (11)
O240.5355 (4)0.2277 (3)0.4241 (5)0.0081 (12)
O250.3735 (5)0.4002 (3)0.5291 (5)0.0092 (12)
O260.2201 (5)0.3269 (3)0.7084 (5)0.0105 (12)
O270.3929 (5)0.2655 (3)0.7665 (5)0.0096 (12)
O280.5476 (5)0.2160 (3)0.6270 (6)0.0127 (13)
O290.5440 (5)0.3368 (3)0.5906 (5)0.0105 (12)
O300.3896 (5)0.3866 (3)0.7301 (5)0.0124 (13)
O310.1997 (5)0.2138 (3)0.5496 (5)0.0100 (12)
O320.3670 (5)0.1606 (3)0.3961 (5)0.0103 (12)
O330.3649 (5)0.2926 (3)0.3589 (5)0.0108 (12)
O340.1964 (5)0.3449 (3)0.5094 (5)0.0099 (12)
O350.0580 (4)0.2021 (3)0.1917 (5)0.0049 (11)
O360.3770 (4)0.2778 (3)0.5683 (5)0.0090 (12)
O370.7442 (6)0.4065 (4)1.2359 (7)0.0241 (16)
O380.4955 (6)0.4977 (4)1.2790 (6)0.0237 (16)
O390.5502 (6)0.4141 (4)1.0320 (6)0.0253 (16)
O400.6562 (6)0.2629 (4)1.2012 (6)0.0244 (16)
O410.4325 (5)0.3100 (4)1.1485 (6)0.0210 (15)
O420.4878 (6)0.1531 (4)1.1828 (7)0.0221 (15)
O430.6526 (7)0.2484 (5)0.9507 (9)0.042 (2)
O440.6590 (5)0.1026 (4)0.9715 (6)0.0205 (15)
O450.4484 (5)0.1703 (3)0.8944 (6)0.0151 (13)
O460.6520 (6)0.0936 (4)0.6867 (7)0.0297 (18)
O470.6496 (6)0.0390 (4)0.7728 (6)0.0221 (15)
O480.4082 (5)0.0376 (4)0.6851 (6)0.0187 (14)
O490.4402 (6)0.0115 (4)0.8922 (6)0.0229 (16)
O500.2022 (5)0.0247 (3)0.9295 (6)0.0173 (14)
O510.2377 (6)0.0913 (4)0.6645 (7)0.0305 (18)
O520.1267 (5)0.0820 (4)0.7660 (6)0.0179 (14)
O530.1180 (6)0.0220 (4)0.4802 (6)0.0226 (16)
O540.1491 (5)0.1367 (3)0.7335 (6)0.0167 (14)
O550.0146 (5)0.1517 (4)0.5531 (6)0.0194 (15)
O560.0179 (5)0.2597 (4)0.8422 (6)0.0200 (15)
O570.2425 (6)0.2165 (4)0.5552 (7)0.0288 (18)
O580.2096 (5)0.3273 (4)0.7990 (6)0.0199 (15)
O590.0097 (5)0.3202 (4)0.6376 (6)0.0177 (14)
O600.0997 (6)0.4577 (4)0.9423 (6)0.0225 (16)
O610.2799 (6)0.5088 (4)0.8016 (6)0.0213 (15)
O620.3541 (6)0.5353 (4)1.0544 (6)0.0242 (16)
O630.0966 (5)0.6111 (4)1.1130 (6)0.0215 (15)
O640.2978 (5)0.6763 (3)1.0194 (6)0.0159 (14)
O650.0168 (5)0.4898 (3)0.7282 (6)0.0184 (14)
O660.2051 (5)0.4070 (4)0.5728 (6)0.0214 (15)
O670.2417 (5)0.5702 (3)0.6463 (6)0.0141 (13)
O680.0207 (5)0.5816 (3)0.5463 (6)0.0166 (14)
O690.1830 (6)0.3581 (4)0.0205 (7)0.0332 (19)
O700.6127 (5)0.4733 (3)0.5183 (6)0.0178 (14)
O710.7361 (6)0.0449 (4)0.5443 (7)0.0277 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.00810 (16)0.00650 (15)0.00981 (17)0.00300 (11)0.00007 (12)0.00157 (13)
W20.00956 (16)0.00580 (15)0.00974 (17)0.00274 (11)0.00141 (12)0.00258 (13)
W30.00729 (15)0.00847 (15)0.00948 (17)0.00262 (11)0.00068 (12)0.00212 (13)
W40.00948 (16)0.00647 (15)0.01054 (17)0.00432 (12)0.00126 (12)0.00281 (13)
W50.00838 (16)0.00967 (16)0.00932 (17)0.00446 (12)0.00223 (12)0.00215 (13)
W60.00836 (16)0.00755 (15)0.00983 (17)0.00391 (12)0.00108 (12)0.00300 (13)
W70.00807 (16)0.00639 (15)0.01087 (17)0.00170 (11)0.00097 (12)0.00177 (13)
W80.00836 (16)0.00736 (15)0.00970 (17)0.00428 (12)0.00069 (12)0.00245 (13)
W90.00828 (15)0.00585 (15)0.00985 (17)0.00257 (11)0.00095 (12)0.00076 (13)
W100.00797 (16)0.00900 (16)0.00911 (17)0.00369 (12)0.00229 (12)0.00169 (13)
Dy0.00815 (18)0.00600 (17)0.01030 (19)0.00304 (13)0.00126 (14)0.00201 (15)
Na10.023 (2)0.0189 (19)0.022 (2)0.0071 (16)0.0028 (17)0.0045 (17)
Na20.0160 (18)0.0154 (18)0.017 (2)0.0033 (14)0.0003 (15)0.0034 (16)
Na30.0184 (19)0.0172 (19)0.018 (2)0.0007 (15)0.0026 (16)0.0007 (17)
Na40.022 (2)0.023 (2)0.029 (2)0.0063 (16)0.0019 (18)0.0122 (19)
Na50.0160 (18)0.0111 (16)0.018 (2)0.0052 (14)0.0000 (15)0.0008 (15)
Na60.0186 (19)0.0137 (17)0.021 (2)0.0031 (14)0.0010 (16)0.0059 (16)
Na70.028 (2)0.0151 (18)0.022 (2)0.0064 (16)0.0001 (17)0.0066 (17)
Na80.023 (2)0.0140 (18)0.0145 (19)0.0004 (15)0.0027 (16)0.0010 (16)
Na90.0185 (19)0.0156 (18)0.026 (2)0.0037 (15)0.0042 (16)0.0045 (17)
O10.015 (3)0.017 (3)0.017 (3)0.004 (2)0.000 (2)0.008 (2)
O20.017 (3)0.017 (3)0.018 (3)0.004 (2)0.000 (2)0.008 (2)
O30.012 (3)0.012 (3)0.015 (3)0.001 (2)0.000 (2)0.001 (2)
O40.016 (3)0.014 (3)0.019 (3)0.004 (2)0.002 (2)0.007 (2)
O50.016 (3)0.020 (3)0.022 (3)0.007 (2)0.001 (2)0.006 (3)
O60.015 (3)0.014 (3)0.020 (3)0.007 (2)0.004 (2)0.010 (2)
O70.018 (3)0.011 (3)0.020 (3)0.002 (2)0.002 (2)0.003 (2)
O80.015 (3)0.010 (2)0.015 (3)0.005 (2)0.002 (2)0.003 (2)
O90.0152 (19)0.0115 (19)0.017 (2)0.0021 (15)0.0010 (16)0.0027 (16)
O100.012 (3)0.017 (3)0.018 (3)0.007 (2)0.004 (2)0.004 (2)
O110.013 (3)0.008 (2)0.011 (3)0.002 (2)0.002 (2)0.003 (2)
O120.010 (2)0.010 (2)0.008 (3)0.000 (2)0.001 (2)0.000 (2)
O130.015 (3)0.010 (2)0.011 (3)0.007 (2)0.004 (2)0.006 (2)
O140.014 (3)0.015 (3)0.013 (3)0.004 (2)0.002 (2)0.005 (2)
O150.014 (3)0.011 (3)0.011 (3)0.006 (2)0.001 (2)0.002 (2)
O160.011 (3)0.012 (3)0.016 (3)0.001 (2)0.001 (2)0.006 (2)
O170.006 (2)0.013 (3)0.014 (3)0.004 (2)0.003 (2)0.003 (2)
O180.011 (3)0.010 (2)0.007 (3)0.007 (2)0.000 (2)0.001 (2)
O190.010 (2)0.009 (2)0.016 (3)0.000 (2)0.001 (2)0.004 (2)
O200.010 (2)0.006 (2)0.012 (3)0.002 (2)0.001 (2)0.001 (2)
O210.014 (3)0.008 (2)0.016 (3)0.006 (2)0.001 (2)0.004 (2)
O220.011 (3)0.005 (2)0.016 (3)0.001 (2)0.002 (2)0.002 (2)
O230.009 (2)0.004 (2)0.011 (3)0.0017 (19)0.000 (2)0.002 (2)
O240.010 (2)0.005 (2)0.006 (3)0.0008 (19)0.001 (2)0.003 (2)
O250.011 (2)0.005 (2)0.012 (3)0.005 (2)0.002 (2)0.001 (2)
O260.010 (3)0.011 (3)0.008 (3)0.004 (2)0.004 (2)0.002 (2)
O270.011 (3)0.010 (2)0.007 (3)0.002 (2)0.002 (2)0.000 (2)
O280.011 (3)0.011 (3)0.017 (3)0.001 (2)0.001 (2)0.006 (2)
O290.011 (3)0.012 (3)0.009 (3)0.006 (2)0.003 (2)0.001 (2)
O300.013 (3)0.011 (3)0.012 (3)0.001 (2)0.003 (2)0.001 (2)
O310.010 (2)0.009 (2)0.012 (3)0.002 (2)0.002 (2)0.004 (2)
O320.011 (2)0.006 (2)0.014 (3)0.002 (2)0.000 (2)0.002 (2)
O330.009 (2)0.008 (2)0.015 (3)0.004 (2)0.001 (2)0.002 (2)
O340.008 (2)0.011 (2)0.010 (3)0.003 (2)0.007 (2)0.001 (2)
O350.008 (2)0.002 (2)0.005 (2)0.0015 (19)0.002 (2)0.000 (2)
O360.008 (2)0.010 (2)0.009 (3)0.003 (2)0.000 (2)0.002 (2)
O370.025 (3)0.022 (3)0.025 (3)0.007 (3)0.007 (3)0.005 (3)
O380.026 (3)0.020 (3)0.025 (3)0.007 (3)0.000 (3)0.004 (3)
O390.033 (3)0.024 (3)0.019 (3)0.009 (3)0.004 (3)0.006 (3)
O400.018 (3)0.029 (3)0.022 (3)0.004 (3)0.007 (3)0.001 (3)
O410.020 (3)0.021 (3)0.022 (3)0.004 (2)0.003 (3)0.006 (3)
O420.019 (3)0.021 (3)0.027 (3)0.006 (2)0.002 (3)0.008 (3)
O430.037 (4)0.047 (4)0.050 (4)0.006 (3)0.001 (3)0.028 (3)
O440.021 (3)0.021 (3)0.021 (3)0.006 (2)0.002 (3)0.006 (3)
O450.013 (3)0.013 (3)0.020 (3)0.003 (2)0.003 (2)0.005 (2)
O460.027 (3)0.036 (3)0.031 (4)0.010 (3)0.008 (3)0.015 (3)
O470.023 (3)0.018 (3)0.024 (3)0.002 (2)0.003 (3)0.004 (3)
O480.022 (3)0.017 (3)0.018 (3)0.005 (2)0.000 (2)0.007 (3)
O490.019 (3)0.025 (3)0.025 (3)0.003 (2)0.002 (3)0.007 (3)
O500.015 (3)0.016 (3)0.021 (3)0.008 (2)0.000 (2)0.003 (2)
O510.029 (3)0.030 (3)0.033 (4)0.005 (3)0.006 (3)0.007 (3)
O520.017 (3)0.019 (3)0.019 (3)0.010 (2)0.003 (2)0.004 (3)
O530.021 (3)0.021 (3)0.023 (3)0.005 (2)0.000 (3)0.000 (3)
O540.021 (3)0.016 (3)0.014 (3)0.003 (2)0.000 (2)0.004 (2)
O550.018 (3)0.017 (3)0.023 (3)0.004 (2)0.007 (2)0.005 (3)
O560.019 (3)0.022 (3)0.020 (3)0.001 (2)0.000 (2)0.007 (3)
O570.025 (3)0.035 (3)0.030 (4)0.005 (3)0.002 (3)0.015 (3)
O580.016 (3)0.020 (3)0.023 (3)0.003 (2)0.003 (2)0.006 (3)
O590.017 (3)0.019 (3)0.019 (3)0.004 (2)0.001 (2)0.008 (3)
O600.025 (3)0.018 (3)0.025 (3)0.002 (2)0.001 (3)0.007 (3)
O610.025 (3)0.021 (3)0.019 (3)0.005 (2)0.001 (3)0.006 (3)
O620.030 (3)0.023 (3)0.019 (3)0.008 (3)0.001 (3)0.002 (3)
O630.018 (3)0.021 (3)0.024 (3)0.000 (2)0.004 (3)0.004 (3)
O640.017 (3)0.015 (3)0.015 (3)0.005 (2)0.004 (2)0.003 (2)
O650.020 (3)0.012 (3)0.024 (3)0.002 (2)0.001 (2)0.005 (2)
O660.018 (3)0.020 (3)0.024 (3)0.002 (2)0.004 (3)0.002 (3)
O670.015 (3)0.006 (2)0.022 (3)0.001 (2)0.000 (2)0.003 (2)
O680.021 (3)0.011 (3)0.017 (3)0.000 (2)0.003 (2)0.004 (2)
O690.029 (3)0.037 (4)0.030 (4)0.011 (3)0.004 (3)0.008 (3)
O700.017 (3)0.017 (3)0.021 (3)0.009 (2)0.007 (2)0.005 (3)
O710.033 (3)0.030 (3)0.024 (3)0.014 (3)0.003 (3)0.010 (3)
Geometric parameters (Å, º) top
W1—O11.729 (7)Dy—O212.392 (6)
W1—O191.800 (7)Dy—O322.393 (6)
W1—O111.950 (6)Dy—O332.398 (6)
W1—O141.958 (7)Dy—O312.405 (6)
W1—O152.039 (6)Na1—O412.394 (9)
W1—O352.315 (6)Na1—O392.434 (9)
W2—O21.725 (7)Na1—O372.433 (9)
W2—O201.792 (6)Na1—O382.447 (9)
W2—O111.935 (6)Na1—O8i2.476 (8)
W2—O121.947 (6)Na1—O402.517 (9)
W2—O162.009 (7)Na2—O432.345 (11)
W2—O352.301 (5)Na2—O422.361 (9)
W3—O31.738 (6)Na2—O402.410 (8)
W3—O211.797 (6)Na2—O452.440 (8)
W3—O131.947 (6)Na2—O442.441 (8)
W3—O121.969 (6)Na2—O412.455 (8)
W3—O171.999 (6)Na3—O472.265 (8)
W3—O352.305 (6)Na3—O452.389 (7)
W4—O41.715 (7)Na3—O442.443 (8)
W4—O221.792 (6)Na3—O462.459 (10)
W4—O141.943 (7)Na3—O482.469 (8)
W4—O131.946 (6)Na3—O492.542 (9)
W4—O182.023 (6)Na4—O502.335 (8)
W4—O352.369 (5)Na4—O482.406 (8)
W5—O51.726 (7)Na4—O512.435 (10)
W5—O151.892 (6)Na4—O522.438 (8)
W5—O181.893 (6)Na4—O492.439 (9)
W5—O171.922 (6)Na4—O1i2.694 (8)
W5—O161.957 (6)Na5—O53ii2.392 (8)
W5—O352.266 (6)Na5—O532.405 (8)
W6—O61.730 (7)Na5—O542.417 (8)
W6—O311.775 (6)Na5—O522.432 (8)
W6—O231.935 (6)Na5—O4ii2.462 (8)
W6—O261.966 (6)Na5—O552.470 (8)
W6—O272.029 (6)Na6—O542.355 (8)
W6—O362.300 (6)Na6—O582.386 (8)
W7—O71.722 (6)Na6—O552.447 (8)
W7—O321.795 (6)Na6—O572.459 (9)
W7—O241.943 (6)Na6—O562.490 (8)
W7—O231.960 (6)Na6—O592.503 (8)
W7—O282.041 (7)Na7—O582.336 (8)
W7—O362.338 (6)Na7—O662.370 (9)
W8—O81.738 (7)Na7—O652.424 (8)
W8—O331.778 (6)Na7—O602.473 (9)
W8—O241.942 (6)Na7—O592.478 (8)
W8—O251.960 (6)Na7—O612.522 (8)
W8—O292.021 (6)Na8—O602.369 (8)
W8—O362.320 (6)Na8—O632.374 (9)
W9—O91.736 (6)Na8—O612.388 (8)
W9—O341.786 (6)Na8—O642.399 (8)
W9—O261.935 (7)Na8—O622.444 (9)
W9—O251.949 (6)Na8—O2iii2.708 (8)
W9—O302.025 (6)Na9—O68iii2.286 (8)
W9—O362.310 (6)Na9—O662.324 (9)
W10—O101.731 (7)Na9—O682.336 (8)
W10—O291.882 (6)Na9—O672.337 (7)
W10—O281.906 (6)Na9—O652.346 (9)
W10—O271.925 (6)O1—Na4iv2.694 (8)
W10—O301.940 (6)O2—Na8iii2.708 (8)
W10—O362.254 (6)O4—Na5ii2.462 (8)
Dy—O222.355 (6)O8—Na1iv2.476 (8)
Dy—O192.378 (7)O53—Na5ii2.392 (8)
Dy—O202.380 (6)O68—Na9iii2.286 (8)
Dy—O342.391 (6)
O1—W1—O19104.8 (3)O41—Na1—O3990.5 (3)
O1—W1—O11102.0 (3)O41—Na1—O37158.1 (3)
O19—W1—O1192.9 (3)O39—Na1—O3796.0 (3)
O1—W1—O14101.8 (3)O41—Na1—O38109.3 (3)
O19—W1—O1491.2 (3)O39—Na1—O3882.2 (3)
O11—W1—O14154.0 (3)O37—Na1—O3892.4 (3)
O1—W1—O1596.0 (3)O41—Na1—O8i81.8 (3)
O19—W1—O15159.3 (3)O39—Na1—O8i164.9 (3)
O11—W1—O1583.5 (3)O37—Na1—O8i95.9 (3)
O14—W1—O1583.6 (3)O38—Na1—O8i88.0 (3)
O1—W1—O35170.0 (3)O41—Na1—O4077.8 (3)
O19—W1—O3585.2 (2)O39—Na1—O40121.1 (3)
O11—W1—O3577.7 (2)O37—Na1—O4080.9 (3)
O14—W1—O3577.0 (2)O38—Na1—O40156.2 (3)
O15—W1—O3574.1 (2)O8i—Na1—O4070.2 (3)
O2—W2—O20103.5 (3)O43—Na2—O42163.9 (3)
O2—W2—O11100.6 (3)O43—Na2—O4082.4 (3)
O20—W2—O1192.5 (3)O42—Na2—O4087.7 (3)
O2—W2—O12102.6 (3)O43—Na2—O4585.8 (3)
O20—W2—O1291.5 (3)O42—Na2—O45105.1 (3)
O11—W2—O12154.9 (3)O40—Na2—O45166.8 (3)
O2—W2—O1698.9 (3)O43—Na2—O4479.5 (3)
O20—W2—O16157.6 (3)O42—Na2—O4490.2 (3)
O11—W2—O1684.0 (3)O40—Na2—O44102.0 (3)
O12—W2—O1682.9 (3)O45—Na2—O4481.5 (3)
O2—W2—O35173.1 (3)O43—Na2—O41102.3 (3)
O20—W2—O3583.4 (2)O42—Na2—O4188.2 (3)
O11—W2—O3578.4 (2)O40—Na2—O4178.7 (3)
O12—W2—O3577.5 (2)O45—Na2—O4198.2 (3)
O16—W2—O3574.2 (2)O44—Na2—O41178.2 (3)
O3—W3—O21103.4 (3)O47—Na3—O45171.2 (3)
O3—W3—O13102.3 (3)O47—Na3—O4489.6 (3)
O21—W3—O1391.5 (3)O45—Na3—O4482.5 (3)
O3—W3—O12101.1 (3)O47—Na3—O4685.1 (3)
O21—W3—O1292.1 (3)O45—Na3—O4699.2 (3)
O13—W3—O12154.7 (3)O44—Na3—O4694.2 (3)
O3—W3—O1797.8 (3)O47—Na3—O48100.4 (3)
O21—W3—O17158.8 (3)O45—Na3—O4887.2 (3)
O13—W3—O1784.7 (3)O44—Na3—O48169.0 (3)
O12—W3—O1783.0 (3)O46—Na3—O4891.3 (3)
O3—W3—O35171.7 (3)O47—Na3—O4979.5 (3)
O21—W3—O3584.8 (3)O45—Na3—O4998.4 (3)
O13—W3—O3578.5 (2)O44—Na3—O49101.9 (3)
O12—W3—O3576.9 (2)O46—Na3—O49157.5 (3)
O17—W3—O3574.0 (2)O48—Na3—O4975.7 (3)
O4—W4—O22103.6 (3)O50—Na4—O48163.5 (3)
O4—W4—O14104.7 (3)O50—Na4—O5187.9 (3)
O22—W4—O1490.3 (3)O48—Na4—O5196.9 (3)
O4—W4—O13101.5 (3)O50—Na4—O5292.7 (3)
O22—W4—O1392.6 (3)O48—Na4—O52102.7 (3)
O14—W4—O13152.2 (3)O51—Na4—O5294.2 (3)
O4—W4—O1899.8 (3)O50—Na4—O4984.7 (3)
O22—W4—O18156.6 (3)O48—Na4—O4978.8 (3)
O14—W4—O1883.5 (3)O51—Na4—O49112.3 (3)
O13—W4—O1883.0 (3)O52—Na4—O49153.3 (3)
O4—W4—O35172.8 (3)O50—Na4—O1i77.4 (3)
O22—W4—O3583.6 (2)O48—Na4—O1i99.0 (3)
O14—W4—O3576.0 (2)O51—Na4—O1i163.9 (3)
O13—W4—O3576.9 (2)O52—Na4—O1i80.2 (2)
O18—W4—O3573.1 (2)O49—Na4—O1i73.3 (3)
O5—W5—O15103.5 (3)O53ii—Na5—O5383.0 (3)
O5—W5—O18104.5 (3)O53ii—Na5—O54174.3 (3)
O15—W5—O1889.0 (3)O53—Na5—O5491.4 (3)
O5—W5—O17102.1 (3)O53ii—Na5—O5286.4 (3)
O15—W5—O17154.2 (3)O53—Na5—O52169.2 (3)
O18—W5—O1787.6 (3)O54—Na5—O5299.2 (3)
O5—W5—O16101.6 (3)O53ii—Na5—O4ii95.8 (3)
O15—W5—O1687.0 (3)O53—Na5—O4ii99.8 (3)
O18—W5—O16153.9 (3)O54—Na5—O4ii86.0 (3)
O17—W5—O1684.9 (3)O52—Na5—O4ii83.1 (3)
O5—W5—O35177.1 (3)O53ii—Na5—O5594.3 (3)
O15—W5—O3577.9 (2)O53—Na5—O5584.3 (3)
O18—W5—O3577.9 (2)O54—Na5—O5584.3 (3)
O17—W5—O3576.3 (2)O52—Na5—O5594.6 (3)
O16—W5—O3576.0 (2)O4ii—Na5—O55169.5 (3)
O6—W6—O31104.4 (3)O54—Na6—O58104.7 (3)
O6—W6—O23102.1 (3)O54—Na6—O5586.1 (3)
O31—W6—O2392.9 (3)O58—Na6—O55168.8 (3)
O6—W6—O26101.4 (3)O54—Na6—O5785.8 (3)
O31—W6—O2691.4 (3)O58—Na6—O5788.5 (3)
O23—W6—O26154.3 (3)O55—Na6—O5789.7 (3)
O6—W6—O2796.5 (3)O54—Na6—O5693.4 (3)
O31—W6—O27159.0 (3)O58—Na6—O5682.8 (3)
O23—W6—O2784.3 (2)O55—Na6—O5699.5 (3)
O26—W6—O2782.7 (2)O57—Na6—O56170.8 (3)
O6—W6—O36170.4 (3)O54—Na6—O59166.2 (3)
O31—W6—O3685.1 (3)O58—Na6—O5985.8 (3)
O23—W6—O3678.2 (2)O55—Na6—O5983.9 (3)
O26—W6—O3676.9 (2)O57—Na6—O59103.6 (3)
O27—W6—O3673.9 (2)O56—Na6—O5978.9 (3)
O7—W7—O32104.5 (3)O58—Na7—O66103.1 (3)
O7—W7—O24102.0 (3)O58—Na7—O65162.3 (3)
O32—W7—O2492.9 (3)O66—Na7—O6592.2 (3)
O7—W7—O23101.7 (3)O58—Na7—O6086.2 (3)
O32—W7—O2391.4 (3)O66—Na7—O60159.5 (3)
O24—W7—O23153.9 (2)O65—Na7—O6082.2 (3)
O7—W7—O2897.8 (3)O58—Na7—O5987.5 (3)
O32—W7—O28157.6 (3)O66—Na7—O5981.2 (3)
O24—W7—O2884.0 (3)O65—Na7—O5986.2 (3)
O23—W7—O2882.3 (3)O60—Na7—O59117.8 (3)
O7—W7—O36171.1 (3)O58—Na7—O6199.6 (3)
O32—W7—O3684.4 (2)O66—Na7—O6181.5 (3)
O24—W7—O3678.1 (2)O65—Na7—O6191.2 (3)
O23—W7—O3676.7 (2)O60—Na7—O6179.0 (3)
O28—W7—O3673.3 (2)O59—Na7—O61162.3 (3)
O8—W8—O33104.0 (3)O60—Na8—O6388.8 (3)
O8—W8—O24103.1 (3)O60—Na8—O6183.8 (3)
O33—W8—O2492.4 (3)O63—Na8—O61166.8 (3)
O8—W8—O25100.2 (3)O60—Na8—O64171.7 (3)
O33—W8—O2590.7 (3)O63—Na8—O6482.9 (3)
O24—W8—O25155.0 (3)O61—Na8—O64104.4 (3)
O8—W8—O2998.7 (3)O60—Na8—O6298.7 (3)
O33—W8—O29157.2 (3)O63—Na8—O62106.7 (3)
O24—W8—O2984.1 (2)O61—Na8—O6285.3 (3)
O25—W8—O2983.5 (3)O64—Na8—O6283.2 (3)
O8—W8—O36171.7 (3)O60—Na8—O2iii92.9 (3)
O33—W8—O3684.0 (3)O63—Na8—O2iii76.3 (3)
O24—W8—O3678.6 (2)O61—Na8—O2iii93.1 (3)
O25—W8—O3677.1 (2)O64—Na8—O2iii85.7 (3)
O29—W8—O3673.3 (2)O62—Na8—O2iii168.0 (3)
O9—W9—O34103.4 (3)O68iii—Na9—O6695.6 (3)
O9—W9—O26101.3 (3)O68iii—Na9—O6888.2 (3)
O34—W9—O2691.6 (3)O66—Na9—O68171.7 (3)
O9—W9—O25102.8 (3)O68iii—Na9—O67167.9 (3)
O34—W9—O2591.8 (3)O66—Na9—O6786.8 (3)
O26—W9—O25154.1 (3)O68—Na9—O6788.0 (3)
O9—W9—O3098.1 (3)O68iii—Na9—O6595.9 (3)
O34—W9—O30158.5 (3)O66—Na9—O6595.4 (3)
O26—W9—O3083.6 (3)O68—Na9—O6591.5 (3)
O25—W9—O3083.9 (3)O67—Na9—O6595.7 (3)
O9—W9—O36172.2 (3)W1—O1—Na4iv132.3 (3)
O34—W9—O3684.3 (2)W2—O2—Na8iii134.4 (3)
O26—W9—O3677.2 (2)W4—O4—Na5ii154.9 (4)
O25—W9—O3677.5 (2)W8—O8—Na1iv145.2 (4)
O30—W9—O3674.1 (2)W2—O11—W1113.4 (3)
O10—W10—O29103.7 (3)W2—O12—W3113.9 (3)
O10—W10—O28102.7 (3)W4—O13—W3114.6 (3)
O29—W10—O2888.1 (3)W4—O14—W1116.2 (3)
O10—W10—O27101.9 (3)W5—O15—W1115.2 (3)
O29—W10—O27154.3 (3)W5—O16—W2115.3 (3)
O28—W10—O2787.2 (3)W5—O17—W3116.1 (3)
O10—W10—O30102.6 (3)W5—O18—W4116.9 (3)
O29—W10—O3087.3 (3)W1—O19—Dy128.6 (3)
O28—W10—O30154.7 (3)W2—O20—Dy130.8 (3)
O27—W10—O3086.2 (3)W3—O21—Dy129.0 (3)
O10—W10—O36178.8 (3)W4—O22—Dy130.9 (3)
O29—W10—O3677.4 (2)W6—O23—W7114.3 (3)
O28—W10—O3677.7 (2)W8—O24—W7113.7 (3)
O27—W10—O3676.9 (2)W9—O25—W8114.2 (3)
O30—W10—O3677.0 (2)W9—O26—W6114.2 (3)
O22—Dy—O1975.4 (2)W10—O27—W6115.0 (3)
O22—Dy—O20117.8 (2)W10—O28—W7115.7 (3)
O19—Dy—O2074.1 (2)W10—O29—W8116.3 (3)
O22—Dy—O34139.6 (2)W10—O30—W9114.8 (3)
O19—Dy—O34143.0 (2)W6—O31—Dy130.8 (3)
O20—Dy—O3476.7 (2)W7—O32—Dy131.1 (3)
O22—Dy—O2175.1 (2)W8—O33—Dy132.1 (3)
O19—Dy—O21118.7 (2)W9—O34—Dy131.6 (3)
O20—Dy—O2174.3 (2)W5—O35—W294.4 (2)
O34—Dy—O2173.4 (2)W5—O35—W393.4 (2)
O22—Dy—O3278.0 (2)W2—O35—W390.87 (19)
O19—Dy—O3275.9 (2)W5—O35—W192.8 (2)
O20—Dy—O32140.4 (2)W2—O35—W189.4 (2)
O34—Dy—O32116.0 (2)W3—O35—W1173.7 (3)
O21—Dy—O32144.1 (2)W5—O35—W492.1 (2)
O22—Dy—O33144.6 (2)W2—O35—W4173.5 (3)
O19—Dy—O3377.6 (2)W3—O35—W489.0 (2)
O20—Dy—O3375.3 (2)W1—O35—W489.98 (18)
O34—Dy—O3373.4 (2)W10—O36—W694.1 (2)
O21—Dy—O33139.1 (2)W10—O36—W994.1 (2)
O32—Dy—O3373.5 (2)W6—O36—W990.6 (2)
O22—Dy—O3175.3 (2)W10—O36—W892.9 (2)
O19—Dy—O31141.3 (2)W6—O36—W8172.8 (3)
O20—Dy—O31143.1 (2)W9—O36—W890.3 (2)
O34—Dy—O3173.4 (2)W10—O36—W793.3 (2)
O21—Dy—O3176.8 (2)W6—O36—W789.7 (2)
O32—Dy—O3173.7 (2)W9—O36—W7172.5 (3)
O33—Dy—O31115.2 (2)W8—O36—W788.5 (2)
Symmetry codes: (i) x, y, z+1; (ii) x, y, z+1; (iii) x, y+1, z+1; (iv) x, y, z1.

Experimental details

Crystal data
Chemical formulaNa9[Dy(W5O18)2]·35H2O
Mr3414.54
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)13.0914 (8), 20.5067 (12), 12.7721 (6)
α, β, γ (°)105.519 (1), 91.231 (2), 82.789 (2)
V3)3277.4 (3)
Z2
Radiation typeMo Kα
µ (mm1)18.78
Crystal size (mm)0.14 × 0.12 × 0.08
Data collection
DiffractometerRigaku RAXIS-RAPID
diffractometer
Absorption correctionNumerical
(NUMABS; Higashi, 1999)
Tmin, Tmax0.179, 0.315
No. of measured, independent and
observed [I > 2σ(I)] reflections
33444, 14785, 13098
Rint0.052
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.036, 0.104, 1.18
No. of reflections14785
No. of parameters821
No. of restraints426
H-atom treatmentH-atom parameters not defined
w = 1/[σ2(Fo2) + (0.0579P)2 + 24.6886P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)4.44, 3.19

Computer programs: PROCESS-AUTO (Rigaku Corporation, 1998), PROCESS-AUTO, CrystalStructure (Molecular Structure Corporation & Rigaku Corporation, 2001), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997).

Selected bond lengths (Å) top
W1—O11.729 (7)W6—O272.029 (6)
W1—O191.800 (7)W6—O362.300 (6)
W1—O111.950 (6)W7—O71.722 (6)
W1—O141.958 (7)W7—O321.795 (6)
W1—O152.039 (6)W7—O241.943 (6)
W1—O352.315 (6)W7—O231.960 (6)
W2—O21.725 (7)W7—O282.041 (7)
W2—O201.792 (6)W7—O362.338 (6)
W2—O111.935 (6)W8—O81.738 (7)
W2—O121.947 (6)W8—O331.778 (6)
W2—O162.009 (7)W8—O241.942 (6)
W2—O352.301 (5)W8—O251.960 (6)
W3—O31.738 (6)W8—O292.021 (6)
W3—O211.797 (6)W8—O362.320 (6)
W3—O131.947 (6)W9—O91.736 (6)
W3—O121.969 (6)W9—O341.786 (6)
W3—O171.999 (6)W9—O261.935 (7)
W3—O352.305 (6)W9—O251.949 (6)
W4—O41.715 (7)W9—O302.025 (6)
W4—O221.792 (6)W9—O362.310 (6)
W4—O141.943 (7)W10—O101.731 (7)
W4—O131.946 (6)W10—O291.882 (6)
W4—O182.023 (6)W10—O281.906 (6)
W4—O352.369 (5)W10—O271.925 (6)
W5—O51.726 (7)W10—O301.940 (6)
W5—O151.892 (6)W10—O362.254 (6)
W5—O181.893 (6)Dy—O222.355 (6)
W5—O171.922 (6)Dy—O192.378 (7)
W5—O161.957 (6)Dy—O202.380 (6)
W5—O352.266 (6)Dy—O342.391 (6)
W6—O61.730 (7)Dy—O212.392 (6)
W6—O311.775 (6)Dy—O322.393 (6)
W6—O231.935 (6)Dy—O332.398 (6)
W6—O261.966 (6)Dy—O312.405 (6)
 

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