Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102016773/ta1388sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102016773/ta1388Isup2.hkl |
The title compound was synthesized according to the method of Yamase et al. (1994) and recrystallized from an aqueous solution at 277 K.
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).
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).
Na9[Dy(W5O18)2]·35H2O | Z = 2 |
Mr = 3414.54 | F(000) = 3086 |
Triclinic, P1 | Dx = 3.460 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 13.0914 (8) Å | Cell parameters from 27035 reflections |
b = 20.5067 (12) Å | θ = 1.6–27.5° |
c = 12.7721 (6) Å | µ = 18.78 mm−1 |
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 |
Rigaku RAXIS-RAPID diffractometer | 14785 independent reflections |
Radiation source: fine-focus sealed tube | 13098 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
Detector resolution: 10.00 pixels mm-1 | θmax = 27.5°, θmin = 1.0° |
ω scans | h = 0→16 |
Absorption correction: numerical (NUMABS; Higashi, 1999) | k = −26→26 |
Tmin = 0.179, Tmax = 0.315 | l = −16→16 |
33444 measured reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-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 = 1.18 | Δρmax = 4.44 e Å−3 |
14785 reflections | Δρmin = −3.19 e Å−3 |
821 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
426 restraints | Extinction coefficient: 0.00070 (3) |
Primary atom site location: structure-invariant direct methods |
Na9[Dy(W5O18)2]·35H2O | γ = 82.789 (2)° |
Mr = 3414.54 | V = 3277.4 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 13.0914 (8) Å | Mo Kα radiation |
b = 20.5067 (12) Å | µ = 18.78 mm−1 |
c = 12.7721 (6) Å | T = 296 K |
α = 105.519 (1)° | 0.14 × 0.12 × 0.08 mm |
β = 91.231 (2)° |
Rigaku RAXIS-RAPID diffractometer | 14785 independent reflections |
Absorption correction: numerical (NUMABS; Higashi, 1999) | 13098 reflections with I > 2σ(I) |
Tmin = 0.179, Tmax = 0.315 | Rint = 0.052 |
33444 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 426 restraints |
wR(F2) = 0.104 | H-atom parameters not defined |
S = 1.18 | w = 1/[σ2(Fo2) + (0.0579P)2 + 24.6886P] where P = (Fo2 + 2Fc2)/3 |
14785 reflections | Δρmax = 4.44 e Å−3 |
821 parameters | Δρmin = −3.19 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
W1 | 0.19777 (3) | 0.15618 (2) | 0.07585 (3) | 0.00807 (8) | |
W2 | 0.06976 (3) | 0.30697 (2) | 0.16294 (3) | 0.00813 (8) | |
W3 | −0.06830 (3) | 0.24961 (2) | 0.32232 (3) | 0.00833 (8) | |
W4 | 0.06021 (3) | 0.09708 (2) | 0.23668 (3) | 0.00845 (8) | |
W5 | −0.05693 (3) | 0.17255 (2) | 0.05733 (3) | 0.00894 (8) | |
W6 | 0.27757 (3) | 0.23014 (2) | 0.66701 (3) | 0.00821 (8) | |
W7 | 0.46879 (3) | 0.17046 (2) | 0.49337 (3) | 0.00849 (8) | |
W8 | 0.46517 (3) | 0.31991 (2) | 0.45000 (3) | 0.00816 (8) | |
W9 | 0.27257 (3) | 0.38072 (2) | 0.62300 (3) | 0.00812 (8) | |
W10 | 0.49113 (3) | 0.30625 (2) | 0.70245 (3) | 0.00863 (8) | |
Dy | 0.21823 (3) | 0.23691 (2) | 0.37660 (3) | 0.00801 (9) | |
Na1 | 0.5690 (3) | 0.3793 (2) | 1.1999 (4) | 0.0212 (9) | |
Na2 | 0.5479 (3) | 0.2071 (2) | 1.0587 (3) | 0.0162 (8) | |
Na3 | 0.5470 (3) | 0.0621 (2) | 0.8186 (3) | 0.0189 (8) | |
Na4 | 0.2821 (3) | 0.0108 (2) | 0.7962 (4) | 0.0232 (9) | |
Na5 | −0.0093 (3) | 0.0578 (2) | 0.6338 (3) | 0.0155 (8) | |
Na6 | −0.1022 (3) | 0.2327 (2) | 0.6872 (3) | 0.0175 (8) | |
Na7 | −0.1358 (3) | 0.4120 (2) | 0.7473 (4) | 0.0209 (8) | |
Na8 | −0.2059 (3) | 0.5634 (2) | 0.9698 (3) | 0.0183 (8) | |
Na9 | −0.1030 (3) | 0.4907 (2) | 0.5656 (4) | 0.0199 (8) | |
O1 | 0.2862 (5) | 0.1177 (3) | −0.0277 (6) | 0.0156 (13) | |
O2 | 0.0689 (5) | 0.3828 (3) | 0.1283 (6) | 0.0166 (14) | |
O3 | −0.1758 (5) | 0.2843 (3) | 0.4053 (6) | 0.0134 (13) | |
O4 | 0.0491 (5) | 0.0193 (3) | 0.2584 (6) | 0.0154 (13) | |
O5 | −0.1470 (5) | 0.1543 (4) | −0.0437 (6) | 0.0186 (14) | |
O6 | 0.2162 (5) | 0.1994 (3) | 0.7592 (6) | 0.0150 (13) | |
O7 | 0.5485 (5) | 0.0944 (3) | 0.4555 (6) | 0.0166 (14) | |
O8 | 0.5403 (5) | 0.3576 (3) | 0.3780 (6) | 0.0132 (13) | |
O9 | 0.2048 (5) | 0.4605 (3) | 0.6794 (6) | 0.0149 (13) | |
O10 | 0.5769 (5) | 0.3279 (3) | 0.8074 (6) | 0.0156 (13) | |
O11 | 0.1704 (5) | 0.2486 (3) | 0.0596 (5) | 0.0108 (12) | |
O12 | −0.0471 (5) | 0.3262 (3) | 0.2630 (5) | 0.0099 (12) | |
O13 | −0.0547 (5) | 0.1541 (3) | 0.3231 (5) | 0.0108 (12) | |
O14 | 0.1634 (5) | 0.0777 (3) | 0.1219 (5) | 0.0134 (13) | |
O15 | 0.0703 (5) | 0.1411 (3) | −0.0178 (5) | 0.0118 (12) | |
O16 | −0.0328 (5) | 0.2644 (3) | 0.0549 (5) | 0.0123 (13) | |
O17 | −0.1421 (5) | 0.2184 (3) | 0.1826 (5) | 0.0108 (12) | |
O18 | −0.0396 (5) | 0.0951 (3) | 0.1130 (5) | 0.0091 (12) | |
O19 | 0.2744 (5) | 0.1822 (3) | 0.1950 (6) | 0.0118 (12) | |
O20 | 0.1589 (5) | 0.3145 (3) | 0.2728 (5) | 0.0099 (12) | |
O21 | 0.0374 (5) | 0.2651 (3) | 0.4140 (6) | 0.0123 (13) | |
O22 | 0.1526 (5) | 0.1313 (3) | 0.3351 (5) | 0.0109 (12) | |
O23 | 0.3807 (4) | 0.1543 (3) | 0.6037 (5) | 0.0078 (11) | |
O24 | 0.5355 (4) | 0.2277 (3) | 0.4241 (5) | 0.0081 (12) | |
O25 | 0.3735 (5) | 0.4002 (3) | 0.5291 (5) | 0.0092 (12) | |
O26 | 0.2201 (5) | 0.3269 (3) | 0.7084 (5) | 0.0105 (12) | |
O27 | 0.3929 (5) | 0.2655 (3) | 0.7665 (5) | 0.0096 (12) | |
O28 | 0.5476 (5) | 0.2160 (3) | 0.6270 (6) | 0.0127 (13) | |
O29 | 0.5440 (5) | 0.3368 (3) | 0.5906 (5) | 0.0105 (12) | |
O30 | 0.3896 (5) | 0.3866 (3) | 0.7301 (5) | 0.0124 (13) | |
O31 | 0.1997 (5) | 0.2138 (3) | 0.5496 (5) | 0.0100 (12) | |
O32 | 0.3670 (5) | 0.1606 (3) | 0.3961 (5) | 0.0103 (12) | |
O33 | 0.3649 (5) | 0.2926 (3) | 0.3589 (5) | 0.0108 (12) | |
O34 | 0.1964 (5) | 0.3449 (3) | 0.5094 (5) | 0.0099 (12) | |
O35 | 0.0580 (4) | 0.2021 (3) | 0.1917 (5) | 0.0049 (11) | |
O36 | 0.3770 (4) | 0.2778 (3) | 0.5683 (5) | 0.0090 (12) | |
O37 | 0.7442 (6) | 0.4065 (4) | 1.2359 (7) | 0.0241 (16) | |
O38 | 0.4955 (6) | 0.4977 (4) | 1.2790 (6) | 0.0237 (16) | |
O39 | 0.5502 (6) | 0.4141 (4) | 1.0320 (6) | 0.0253 (16) | |
O40 | 0.6562 (6) | 0.2629 (4) | 1.2012 (6) | 0.0244 (16) | |
O41 | 0.4325 (5) | 0.3100 (4) | 1.1485 (6) | 0.0210 (15) | |
O42 | 0.4878 (6) | 0.1531 (4) | 1.1828 (7) | 0.0221 (15) | |
O43 | 0.6526 (7) | 0.2484 (5) | 0.9507 (9) | 0.042 (2) | |
O44 | 0.6590 (5) | 0.1026 (4) | 0.9715 (6) | 0.0205 (15) | |
O45 | 0.4484 (5) | 0.1703 (3) | 0.8944 (6) | 0.0151 (13) | |
O46 | 0.6520 (6) | 0.0936 (4) | 0.6867 (7) | 0.0297 (18) | |
O47 | 0.6496 (6) | −0.0390 (4) | 0.7728 (6) | 0.0221 (15) | |
O48 | 0.4082 (5) | 0.0376 (4) | 0.6851 (6) | 0.0187 (14) | |
O49 | 0.4402 (6) | −0.0115 (4) | 0.8922 (6) | 0.0229 (16) | |
O50 | 0.2022 (5) | −0.0247 (3) | 0.9295 (6) | 0.0173 (14) | |
O51 | 0.2377 (6) | −0.0913 (4) | 0.6645 (7) | 0.0305 (18) | |
O52 | 0.1267 (5) | 0.0820 (4) | 0.7660 (6) | 0.0179 (14) | |
O53 | −0.1180 (6) | 0.0220 (4) | 0.4802 (6) | 0.0226 (16) | |
O54 | −0.1491 (5) | 0.1367 (3) | 0.7335 (6) | 0.0167 (14) | |
O55 | 0.0146 (5) | 0.1517 (4) | 0.5531 (6) | 0.0194 (15) | |
O56 | 0.0179 (5) | 0.2597 (4) | 0.8422 (6) | 0.0200 (15) | |
O57 | −0.2425 (6) | 0.2165 (4) | 0.5552 (7) | 0.0288 (18) | |
O58 | −0.2096 (5) | 0.3273 (4) | 0.7990 (6) | 0.0199 (15) | |
O59 | −0.0097 (5) | 0.3202 (4) | 0.6376 (6) | 0.0177 (14) | |
O60 | −0.0997 (6) | 0.4577 (4) | 0.9423 (6) | 0.0225 (16) | |
O61 | −0.2799 (6) | 0.5088 (4) | 0.8016 (6) | 0.0213 (15) | |
O62 | −0.3541 (6) | 0.5353 (4) | 1.0544 (6) | 0.0242 (16) | |
O63 | −0.0966 (5) | 0.6111 (4) | 1.1130 (6) | 0.0215 (15) | |
O64 | −0.2978 (5) | 0.6763 (3) | 1.0194 (6) | 0.0159 (14) | |
O65 | −0.0168 (5) | 0.4898 (3) | 0.7282 (6) | 0.0184 (14) | |
O66 | −0.2051 (5) | 0.4070 (4) | 0.5728 (6) | 0.0214 (15) | |
O67 | −0.2417 (5) | 0.5702 (3) | 0.6463 (6) | 0.0141 (13) | |
O68 | −0.0207 (5) | 0.5816 (3) | 0.5463 (6) | 0.0166 (14) | |
O69 | −0.1830 (6) | 0.3581 (4) | 0.0205 (7) | 0.0332 (19) | |
O70 | 0.6127 (5) | 0.4733 (3) | 0.5183 (6) | 0.0178 (14) | |
O71 | 0.7361 (6) | −0.0449 (4) | 0.5443 (7) | 0.0277 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
W1 | 0.00810 (16) | 0.00650 (15) | 0.00981 (17) | −0.00300 (11) | −0.00007 (12) | 0.00157 (13) |
W2 | 0.00956 (16) | 0.00580 (15) | 0.00974 (17) | −0.00274 (11) | −0.00141 (12) | 0.00258 (13) |
W3 | 0.00729 (15) | 0.00847 (15) | 0.00948 (17) | −0.00262 (11) | −0.00068 (12) | 0.00212 (13) |
W4 | 0.00948 (16) | 0.00647 (15) | 0.01054 (17) | −0.00432 (12) | −0.00126 (12) | 0.00281 (13) |
W5 | 0.00838 (16) | 0.00967 (16) | 0.00932 (17) | −0.00446 (12) | −0.00223 (12) | 0.00215 (13) |
W6 | 0.00836 (16) | 0.00755 (15) | 0.00983 (17) | −0.00391 (12) | −0.00108 (12) | 0.00300 (13) |
W7 | 0.00807 (16) | 0.00639 (15) | 0.01087 (17) | −0.00170 (11) | −0.00097 (12) | 0.00177 (13) |
W8 | 0.00836 (16) | 0.00736 (15) | 0.00970 (17) | −0.00428 (12) | −0.00069 (12) | 0.00245 (13) |
W9 | 0.00828 (15) | 0.00585 (15) | 0.00985 (17) | −0.00257 (11) | −0.00095 (12) | 0.00076 (13) |
W10 | 0.00797 (16) | 0.00900 (16) | 0.00911 (17) | −0.00369 (12) | −0.00229 (12) | 0.00169 (13) |
Dy | 0.00815 (18) | 0.00600 (17) | 0.01030 (19) | −0.00304 (13) | −0.00126 (14) | 0.00201 (15) |
Na1 | 0.023 (2) | 0.0189 (19) | 0.022 (2) | −0.0071 (16) | −0.0028 (17) | 0.0045 (17) |
Na2 | 0.0160 (18) | 0.0154 (18) | 0.017 (2) | −0.0033 (14) | −0.0003 (15) | 0.0034 (16) |
Na3 | 0.0184 (19) | 0.0172 (19) | 0.018 (2) | 0.0007 (15) | −0.0026 (16) | 0.0007 (17) |
Na4 | 0.022 (2) | 0.023 (2) | 0.029 (2) | −0.0063 (16) | 0.0019 (18) | 0.0122 (19) |
Na5 | 0.0160 (18) | 0.0111 (16) | 0.018 (2) | −0.0052 (14) | 0.0000 (15) | 0.0008 (15) |
Na6 | 0.0186 (19) | 0.0137 (17) | 0.021 (2) | −0.0031 (14) | 0.0010 (16) | 0.0059 (16) |
Na7 | 0.028 (2) | 0.0151 (18) | 0.022 (2) | −0.0064 (16) | −0.0001 (17) | 0.0066 (17) |
Na8 | 0.023 (2) | 0.0140 (18) | 0.0145 (19) | −0.0004 (15) | −0.0027 (16) | −0.0010 (16) |
Na9 | 0.0185 (19) | 0.0156 (18) | 0.026 (2) | −0.0037 (15) | 0.0042 (16) | 0.0045 (17) |
O1 | 0.015 (3) | 0.017 (3) | 0.017 (3) | −0.004 (2) | 0.000 (2) | 0.008 (2) |
O2 | 0.017 (3) | 0.017 (3) | 0.018 (3) | −0.004 (2) | 0.000 (2) | 0.008 (2) |
O3 | 0.012 (3) | 0.012 (3) | 0.015 (3) | −0.001 (2) | 0.000 (2) | 0.001 (2) |
O4 | 0.016 (3) | 0.014 (3) | 0.019 (3) | −0.004 (2) | −0.002 (2) | 0.007 (2) |
O5 | 0.016 (3) | 0.020 (3) | 0.022 (3) | −0.007 (2) | −0.001 (2) | 0.006 (3) |
O6 | 0.015 (3) | 0.014 (3) | 0.020 (3) | −0.007 (2) | 0.004 (2) | 0.010 (2) |
O7 | 0.018 (3) | 0.011 (3) | 0.020 (3) | 0.002 (2) | 0.002 (2) | 0.003 (2) |
O8 | 0.015 (3) | 0.010 (2) | 0.015 (3) | −0.005 (2) | 0.002 (2) | 0.003 (2) |
O9 | 0.0152 (19) | 0.0115 (19) | 0.017 (2) | −0.0021 (15) | 0.0010 (16) | 0.0027 (16) |
O10 | 0.012 (3) | 0.017 (3) | 0.018 (3) | −0.007 (2) | −0.004 (2) | 0.004 (2) |
O11 | 0.013 (3) | 0.008 (2) | 0.011 (3) | −0.002 (2) | 0.002 (2) | 0.003 (2) |
O12 | 0.010 (2) | 0.010 (2) | 0.008 (3) | 0.000 (2) | −0.001 (2) | 0.000 (2) |
O13 | 0.015 (3) | 0.010 (2) | 0.011 (3) | −0.007 (2) | −0.004 (2) | 0.006 (2) |
O14 | 0.014 (3) | 0.015 (3) | 0.013 (3) | −0.004 (2) | −0.002 (2) | 0.005 (2) |
O15 | 0.014 (3) | 0.011 (3) | 0.011 (3) | −0.006 (2) | −0.001 (2) | 0.002 (2) |
O16 | 0.011 (3) | 0.012 (3) | 0.016 (3) | −0.001 (2) | 0.001 (2) | 0.006 (2) |
O17 | 0.006 (2) | 0.013 (3) | 0.014 (3) | −0.004 (2) | −0.003 (2) | 0.003 (2) |
O18 | 0.011 (3) | 0.010 (2) | 0.007 (3) | −0.007 (2) | 0.000 (2) | 0.001 (2) |
O19 | 0.010 (2) | 0.009 (2) | 0.016 (3) | 0.000 (2) | −0.001 (2) | 0.004 (2) |
O20 | 0.010 (2) | 0.006 (2) | 0.012 (3) | −0.002 (2) | 0.001 (2) | −0.001 (2) |
O21 | 0.014 (3) | 0.008 (2) | 0.016 (3) | −0.006 (2) | −0.001 (2) | 0.004 (2) |
O22 | 0.011 (3) | 0.005 (2) | 0.016 (3) | −0.001 (2) | 0.002 (2) | 0.002 (2) |
O23 | 0.009 (2) | 0.004 (2) | 0.011 (3) | −0.0017 (19) | 0.000 (2) | 0.002 (2) |
O24 | 0.010 (2) | 0.005 (2) | 0.006 (3) | −0.0008 (19) | −0.001 (2) | −0.003 (2) |
O25 | 0.011 (2) | 0.005 (2) | 0.012 (3) | −0.005 (2) | −0.002 (2) | 0.001 (2) |
O26 | 0.010 (3) | 0.011 (3) | 0.008 (3) | −0.004 (2) | −0.004 (2) | −0.002 (2) |
O27 | 0.011 (3) | 0.010 (2) | 0.007 (3) | −0.002 (2) | −0.002 (2) | 0.000 (2) |
O28 | 0.011 (3) | 0.011 (3) | 0.017 (3) | −0.001 (2) | −0.001 (2) | 0.006 (2) |
O29 | 0.011 (3) | 0.012 (3) | 0.009 (3) | −0.006 (2) | −0.003 (2) | 0.001 (2) |
O30 | 0.013 (3) | 0.011 (3) | 0.012 (3) | −0.001 (2) | −0.003 (2) | 0.001 (2) |
O31 | 0.010 (2) | 0.009 (2) | 0.012 (3) | −0.002 (2) | 0.002 (2) | 0.004 (2) |
O32 | 0.011 (2) | 0.006 (2) | 0.014 (3) | −0.002 (2) | 0.000 (2) | 0.002 (2) |
O33 | 0.009 (2) | 0.008 (2) | 0.015 (3) | −0.004 (2) | −0.001 (2) | 0.002 (2) |
O34 | 0.008 (2) | 0.011 (2) | 0.010 (3) | −0.003 (2) | −0.007 (2) | 0.001 (2) |
O35 | 0.008 (2) | 0.002 (2) | 0.005 (2) | −0.0015 (19) | −0.002 (2) | 0.000 (2) |
O36 | 0.008 (2) | 0.010 (2) | 0.009 (3) | −0.003 (2) | 0.000 (2) | 0.002 (2) |
O37 | 0.025 (3) | 0.022 (3) | 0.025 (3) | −0.007 (3) | −0.007 (3) | 0.005 (3) |
O38 | 0.026 (3) | 0.020 (3) | 0.025 (3) | −0.007 (3) | 0.000 (3) | 0.004 (3) |
O39 | 0.033 (3) | 0.024 (3) | 0.019 (3) | −0.009 (3) | −0.004 (3) | 0.006 (3) |
O40 | 0.018 (3) | 0.029 (3) | 0.022 (3) | −0.004 (3) | −0.007 (3) | −0.001 (3) |
O41 | 0.020 (3) | 0.021 (3) | 0.022 (3) | −0.004 (2) | −0.003 (3) | 0.006 (3) |
O42 | 0.019 (3) | 0.021 (3) | 0.027 (3) | −0.006 (2) | 0.002 (3) | 0.008 (3) |
O43 | 0.037 (4) | 0.047 (4) | 0.050 (4) | −0.006 (3) | −0.001 (3) | 0.028 (3) |
O44 | 0.021 (3) | 0.021 (3) | 0.021 (3) | −0.006 (2) | −0.002 (3) | 0.006 (3) |
O45 | 0.013 (3) | 0.013 (3) | 0.020 (3) | −0.003 (2) | 0.003 (2) | 0.005 (2) |
O46 | 0.027 (3) | 0.036 (3) | 0.031 (4) | −0.010 (3) | −0.008 (3) | 0.015 (3) |
O47 | 0.023 (3) | 0.018 (3) | 0.024 (3) | −0.002 (2) | −0.003 (3) | 0.004 (3) |
O48 | 0.022 (3) | 0.017 (3) | 0.018 (3) | −0.005 (2) | 0.000 (2) | 0.007 (3) |
O49 | 0.019 (3) | 0.025 (3) | 0.025 (3) | −0.003 (2) | 0.002 (3) | 0.007 (3) |
O50 | 0.015 (3) | 0.016 (3) | 0.021 (3) | −0.008 (2) | 0.000 (2) | 0.003 (2) |
O51 | 0.029 (3) | 0.030 (3) | 0.033 (4) | −0.005 (3) | 0.006 (3) | 0.007 (3) |
O52 | 0.017 (3) | 0.019 (3) | 0.019 (3) | −0.010 (2) | −0.003 (2) | 0.004 (3) |
O53 | 0.021 (3) | 0.021 (3) | 0.023 (3) | −0.005 (2) | 0.000 (3) | 0.000 (3) |
O54 | 0.021 (3) | 0.016 (3) | 0.014 (3) | −0.003 (2) | 0.000 (2) | 0.004 (2) |
O55 | 0.018 (3) | 0.017 (3) | 0.023 (3) | −0.004 (2) | 0.007 (2) | 0.005 (3) |
O56 | 0.019 (3) | 0.022 (3) | 0.020 (3) | −0.001 (2) | 0.000 (2) | 0.007 (3) |
O57 | 0.025 (3) | 0.035 (3) | 0.030 (4) | −0.005 (3) | 0.002 (3) | 0.015 (3) |
O58 | 0.016 (3) | 0.020 (3) | 0.023 (3) | −0.003 (2) | 0.003 (2) | 0.006 (3) |
O59 | 0.017 (3) | 0.019 (3) | 0.019 (3) | −0.004 (2) | −0.001 (2) | 0.008 (3) |
O60 | 0.025 (3) | 0.018 (3) | 0.025 (3) | −0.002 (2) | −0.001 (3) | 0.007 (3) |
O61 | 0.025 (3) | 0.021 (3) | 0.019 (3) | −0.005 (2) | −0.001 (3) | 0.006 (3) |
O62 | 0.030 (3) | 0.023 (3) | 0.019 (3) | −0.008 (3) | 0.001 (3) | 0.002 (3) |
O63 | 0.018 (3) | 0.021 (3) | 0.024 (3) | 0.000 (2) | 0.004 (3) | 0.004 (3) |
O64 | 0.017 (3) | 0.015 (3) | 0.015 (3) | −0.005 (2) | −0.004 (2) | 0.003 (2) |
O65 | 0.020 (3) | 0.012 (3) | 0.024 (3) | −0.002 (2) | 0.001 (2) | 0.005 (2) |
O66 | 0.018 (3) | 0.020 (3) | 0.024 (3) | −0.002 (2) | −0.004 (3) | 0.002 (3) |
O67 | 0.015 (3) | 0.006 (2) | 0.022 (3) | −0.001 (2) | 0.000 (2) | 0.003 (2) |
O68 | 0.021 (3) | 0.011 (3) | 0.017 (3) | 0.000 (2) | 0.003 (2) | 0.004 (2) |
O69 | 0.029 (3) | 0.037 (4) | 0.030 (4) | 0.011 (3) | −0.004 (3) | 0.008 (3) |
O70 | 0.017 (3) | 0.017 (3) | 0.021 (3) | −0.009 (2) | −0.007 (2) | 0.005 (3) |
O71 | 0.033 (3) | 0.030 (3) | 0.024 (3) | −0.014 (3) | −0.003 (3) | 0.010 (3) |
W1—O1 | 1.729 (7) | Dy—O21 | 2.392 (6) |
W1—O19 | 1.800 (7) | Dy—O32 | 2.393 (6) |
W1—O11 | 1.950 (6) | Dy—O33 | 2.398 (6) |
W1—O14 | 1.958 (7) | Dy—O31 | 2.405 (6) |
W1—O15 | 2.039 (6) | Na1—O41 | 2.394 (9) |
W1—O35 | 2.315 (6) | Na1—O39 | 2.434 (9) |
W2—O2 | 1.725 (7) | Na1—O37 | 2.433 (9) |
W2—O20 | 1.792 (6) | Na1—O38 | 2.447 (9) |
W2—O11 | 1.935 (6) | Na1—O8i | 2.476 (8) |
W2—O12 | 1.947 (6) | Na1—O40 | 2.517 (9) |
W2—O16 | 2.009 (7) | Na2—O43 | 2.345 (11) |
W2—O35 | 2.301 (5) | Na2—O42 | 2.361 (9) |
W3—O3 | 1.738 (6) | Na2—O40 | 2.410 (8) |
W3—O21 | 1.797 (6) | Na2—O45 | 2.440 (8) |
W3—O13 | 1.947 (6) | Na2—O44 | 2.441 (8) |
W3—O12 | 1.969 (6) | Na2—O41 | 2.455 (8) |
W3—O17 | 1.999 (6) | Na3—O47 | 2.265 (8) |
W3—O35 | 2.305 (6) | Na3—O45 | 2.389 (7) |
W4—O4 | 1.715 (7) | Na3—O44 | 2.443 (8) |
W4—O22 | 1.792 (6) | Na3—O46 | 2.459 (10) |
W4—O14 | 1.943 (7) | Na3—O48 | 2.469 (8) |
W4—O13 | 1.946 (6) | Na3—O49 | 2.542 (9) |
W4—O18 | 2.023 (6) | Na4—O50 | 2.335 (8) |
W4—O35 | 2.369 (5) | Na4—O48 | 2.406 (8) |
W5—O5 | 1.726 (7) | Na4—O51 | 2.435 (10) |
W5—O15 | 1.892 (6) | Na4—O52 | 2.438 (8) |
W5—O18 | 1.893 (6) | Na4—O49 | 2.439 (9) |
W5—O17 | 1.922 (6) | Na4—O1i | 2.694 (8) |
W5—O16 | 1.957 (6) | Na5—O53ii | 2.392 (8) |
W5—O35 | 2.266 (6) | Na5—O53 | 2.405 (8) |
W6—O6 | 1.730 (7) | Na5—O54 | 2.417 (8) |
W6—O31 | 1.775 (6) | Na5—O52 | 2.432 (8) |
W6—O23 | 1.935 (6) | Na5—O4ii | 2.462 (8) |
W6—O26 | 1.966 (6) | Na5—O55 | 2.470 (8) |
W6—O27 | 2.029 (6) | Na6—O54 | 2.355 (8) |
W6—O36 | 2.300 (6) | Na6—O58 | 2.386 (8) |
W7—O7 | 1.722 (6) | Na6—O55 | 2.447 (8) |
W7—O32 | 1.795 (6) | Na6—O57 | 2.459 (9) |
W7—O24 | 1.943 (6) | Na6—O56 | 2.490 (8) |
W7—O23 | 1.960 (6) | Na6—O59 | 2.503 (8) |
W7—O28 | 2.041 (7) | Na7—O58 | 2.336 (8) |
W7—O36 | 2.338 (6) | Na7—O66 | 2.370 (9) |
W8—O8 | 1.738 (7) | Na7—O65 | 2.424 (8) |
W8—O33 | 1.778 (6) | Na7—O60 | 2.473 (9) |
W8—O24 | 1.942 (6) | Na7—O59 | 2.478 (8) |
W8—O25 | 1.960 (6) | Na7—O61 | 2.522 (8) |
W8—O29 | 2.021 (6) | Na8—O60 | 2.369 (8) |
W8—O36 | 2.320 (6) | Na8—O63 | 2.374 (9) |
W9—O9 | 1.736 (6) | Na8—O61 | 2.388 (8) |
W9—O34 | 1.786 (6) | Na8—O64 | 2.399 (8) |
W9—O26 | 1.935 (7) | Na8—O62 | 2.444 (9) |
W9—O25 | 1.949 (6) | Na8—O2iii | 2.708 (8) |
W9—O30 | 2.025 (6) | Na9—O68iii | 2.286 (8) |
W9—O36 | 2.310 (6) | Na9—O66 | 2.324 (9) |
W10—O10 | 1.731 (7) | Na9—O68 | 2.336 (8) |
W10—O29 | 1.882 (6) | Na9—O67 | 2.337 (7) |
W10—O28 | 1.906 (6) | Na9—O65 | 2.346 (9) |
W10—O27 | 1.925 (6) | O1—Na4iv | 2.694 (8) |
W10—O30 | 1.940 (6) | O2—Na8iii | 2.708 (8) |
W10—O36 | 2.254 (6) | O4—Na5ii | 2.462 (8) |
Dy—O22 | 2.355 (6) | O8—Na1iv | 2.476 (8) |
Dy—O19 | 2.378 (7) | O53—Na5ii | 2.392 (8) |
Dy—O20 | 2.380 (6) | O68—Na9iii | 2.286 (8) |
Dy—O34 | 2.391 (6) | ||
O1—W1—O19 | 104.8 (3) | O41—Na1—O39 | 90.5 (3) |
O1—W1—O11 | 102.0 (3) | O41—Na1—O37 | 158.1 (3) |
O19—W1—O11 | 92.9 (3) | O39—Na1—O37 | 96.0 (3) |
O1—W1—O14 | 101.8 (3) | O41—Na1—O38 | 109.3 (3) |
O19—W1—O14 | 91.2 (3) | O39—Na1—O38 | 82.2 (3) |
O11—W1—O14 | 154.0 (3) | O37—Na1—O38 | 92.4 (3) |
O1—W1—O15 | 96.0 (3) | O41—Na1—O8i | 81.8 (3) |
O19—W1—O15 | 159.3 (3) | O39—Na1—O8i | 164.9 (3) |
O11—W1—O15 | 83.5 (3) | O37—Na1—O8i | 95.9 (3) |
O14—W1—O15 | 83.6 (3) | O38—Na1—O8i | 88.0 (3) |
O1—W1—O35 | 170.0 (3) | O41—Na1—O40 | 77.8 (3) |
O19—W1—O35 | 85.2 (2) | O39—Na1—O40 | 121.1 (3) |
O11—W1—O35 | 77.7 (2) | O37—Na1—O40 | 80.9 (3) |
O14—W1—O35 | 77.0 (2) | O38—Na1—O40 | 156.2 (3) |
O15—W1—O35 | 74.1 (2) | O8i—Na1—O40 | 70.2 (3) |
O2—W2—O20 | 103.5 (3) | O43—Na2—O42 | 163.9 (3) |
O2—W2—O11 | 100.6 (3) | O43—Na2—O40 | 82.4 (3) |
O20—W2—O11 | 92.5 (3) | O42—Na2—O40 | 87.7 (3) |
O2—W2—O12 | 102.6 (3) | O43—Na2—O45 | 85.8 (3) |
O20—W2—O12 | 91.5 (3) | O42—Na2—O45 | 105.1 (3) |
O11—W2—O12 | 154.9 (3) | O40—Na2—O45 | 166.8 (3) |
O2—W2—O16 | 98.9 (3) | O43—Na2—O44 | 79.5 (3) |
O20—W2—O16 | 157.6 (3) | O42—Na2—O44 | 90.2 (3) |
O11—W2—O16 | 84.0 (3) | O40—Na2—O44 | 102.0 (3) |
O12—W2—O16 | 82.9 (3) | O45—Na2—O44 | 81.5 (3) |
O2—W2—O35 | 173.1 (3) | O43—Na2—O41 | 102.3 (3) |
O20—W2—O35 | 83.4 (2) | O42—Na2—O41 | 88.2 (3) |
O11—W2—O35 | 78.4 (2) | O40—Na2—O41 | 78.7 (3) |
O12—W2—O35 | 77.5 (2) | O45—Na2—O41 | 98.2 (3) |
O16—W2—O35 | 74.2 (2) | O44—Na2—O41 | 178.2 (3) |
O3—W3—O21 | 103.4 (3) | O47—Na3—O45 | 171.2 (3) |
O3—W3—O13 | 102.3 (3) | O47—Na3—O44 | 89.6 (3) |
O21—W3—O13 | 91.5 (3) | O45—Na3—O44 | 82.5 (3) |
O3—W3—O12 | 101.1 (3) | O47—Na3—O46 | 85.1 (3) |
O21—W3—O12 | 92.1 (3) | O45—Na3—O46 | 99.2 (3) |
O13—W3—O12 | 154.7 (3) | O44—Na3—O46 | 94.2 (3) |
O3—W3—O17 | 97.8 (3) | O47—Na3—O48 | 100.4 (3) |
O21—W3—O17 | 158.8 (3) | O45—Na3—O48 | 87.2 (3) |
O13—W3—O17 | 84.7 (3) | O44—Na3—O48 | 169.0 (3) |
O12—W3—O17 | 83.0 (3) | O46—Na3—O48 | 91.3 (3) |
O3—W3—O35 | 171.7 (3) | O47—Na3—O49 | 79.5 (3) |
O21—W3—O35 | 84.8 (3) | O45—Na3—O49 | 98.4 (3) |
O13—W3—O35 | 78.5 (2) | O44—Na3—O49 | 101.9 (3) |
O12—W3—O35 | 76.9 (2) | O46—Na3—O49 | 157.5 (3) |
O17—W3—O35 | 74.0 (2) | O48—Na3—O49 | 75.7 (3) |
O4—W4—O22 | 103.6 (3) | O50—Na4—O48 | 163.5 (3) |
O4—W4—O14 | 104.7 (3) | O50—Na4—O51 | 87.9 (3) |
O22—W4—O14 | 90.3 (3) | O48—Na4—O51 | 96.9 (3) |
O4—W4—O13 | 101.5 (3) | O50—Na4—O52 | 92.7 (3) |
O22—W4—O13 | 92.6 (3) | O48—Na4—O52 | 102.7 (3) |
O14—W4—O13 | 152.2 (3) | O51—Na4—O52 | 94.2 (3) |
O4—W4—O18 | 99.8 (3) | O50—Na4—O49 | 84.7 (3) |
O22—W4—O18 | 156.6 (3) | O48—Na4—O49 | 78.8 (3) |
O14—W4—O18 | 83.5 (3) | O51—Na4—O49 | 112.3 (3) |
O13—W4—O18 | 83.0 (3) | O52—Na4—O49 | 153.3 (3) |
O4—W4—O35 | 172.8 (3) | O50—Na4—O1i | 77.4 (3) |
O22—W4—O35 | 83.6 (2) | O48—Na4—O1i | 99.0 (3) |
O14—W4—O35 | 76.0 (2) | O51—Na4—O1i | 163.9 (3) |
O13—W4—O35 | 76.9 (2) | O52—Na4—O1i | 80.2 (2) |
O18—W4—O35 | 73.1 (2) | O49—Na4—O1i | 73.3 (3) |
O5—W5—O15 | 103.5 (3) | O53ii—Na5—O53 | 83.0 (3) |
O5—W5—O18 | 104.5 (3) | O53ii—Na5—O54 | 174.3 (3) |
O15—W5—O18 | 89.0 (3) | O53—Na5—O54 | 91.4 (3) |
O5—W5—O17 | 102.1 (3) | O53ii—Na5—O52 | 86.4 (3) |
O15—W5—O17 | 154.2 (3) | O53—Na5—O52 | 169.2 (3) |
O18—W5—O17 | 87.6 (3) | O54—Na5—O52 | 99.2 (3) |
O5—W5—O16 | 101.6 (3) | O53ii—Na5—O4ii | 95.8 (3) |
O15—W5—O16 | 87.0 (3) | O53—Na5—O4ii | 99.8 (3) |
O18—W5—O16 | 153.9 (3) | O54—Na5—O4ii | 86.0 (3) |
O17—W5—O16 | 84.9 (3) | O52—Na5—O4ii | 83.1 (3) |
O5—W5—O35 | 177.1 (3) | O53ii—Na5—O55 | 94.3 (3) |
O15—W5—O35 | 77.9 (2) | O53—Na5—O55 | 84.3 (3) |
O18—W5—O35 | 77.9 (2) | O54—Na5—O55 | 84.3 (3) |
O17—W5—O35 | 76.3 (2) | O52—Na5—O55 | 94.6 (3) |
O16—W5—O35 | 76.0 (2) | O4ii—Na5—O55 | 169.5 (3) |
O6—W6—O31 | 104.4 (3) | O54—Na6—O58 | 104.7 (3) |
O6—W6—O23 | 102.1 (3) | O54—Na6—O55 | 86.1 (3) |
O31—W6—O23 | 92.9 (3) | O58—Na6—O55 | 168.8 (3) |
O6—W6—O26 | 101.4 (3) | O54—Na6—O57 | 85.8 (3) |
O31—W6—O26 | 91.4 (3) | O58—Na6—O57 | 88.5 (3) |
O23—W6—O26 | 154.3 (3) | O55—Na6—O57 | 89.7 (3) |
O6—W6—O27 | 96.5 (3) | O54—Na6—O56 | 93.4 (3) |
O31—W6—O27 | 159.0 (3) | O58—Na6—O56 | 82.8 (3) |
O23—W6—O27 | 84.3 (2) | O55—Na6—O56 | 99.5 (3) |
O26—W6—O27 | 82.7 (2) | O57—Na6—O56 | 170.8 (3) |
O6—W6—O36 | 170.4 (3) | O54—Na6—O59 | 166.2 (3) |
O31—W6—O36 | 85.1 (3) | O58—Na6—O59 | 85.8 (3) |
O23—W6—O36 | 78.2 (2) | O55—Na6—O59 | 83.9 (3) |
O26—W6—O36 | 76.9 (2) | O57—Na6—O59 | 103.6 (3) |
O27—W6—O36 | 73.9 (2) | O56—Na6—O59 | 78.9 (3) |
O7—W7—O32 | 104.5 (3) | O58—Na7—O66 | 103.1 (3) |
O7—W7—O24 | 102.0 (3) | O58—Na7—O65 | 162.3 (3) |
O32—W7—O24 | 92.9 (3) | O66—Na7—O65 | 92.2 (3) |
O7—W7—O23 | 101.7 (3) | O58—Na7—O60 | 86.2 (3) |
O32—W7—O23 | 91.4 (3) | O66—Na7—O60 | 159.5 (3) |
O24—W7—O23 | 153.9 (2) | O65—Na7—O60 | 82.2 (3) |
O7—W7—O28 | 97.8 (3) | O58—Na7—O59 | 87.5 (3) |
O32—W7—O28 | 157.6 (3) | O66—Na7—O59 | 81.2 (3) |
O24—W7—O28 | 84.0 (3) | O65—Na7—O59 | 86.2 (3) |
O23—W7—O28 | 82.3 (3) | O60—Na7—O59 | 117.8 (3) |
O7—W7—O36 | 171.1 (3) | O58—Na7—O61 | 99.6 (3) |
O32—W7—O36 | 84.4 (2) | O66—Na7—O61 | 81.5 (3) |
O24—W7—O36 | 78.1 (2) | O65—Na7—O61 | 91.2 (3) |
O23—W7—O36 | 76.7 (2) | O60—Na7—O61 | 79.0 (3) |
O28—W7—O36 | 73.3 (2) | O59—Na7—O61 | 162.3 (3) |
O8—W8—O33 | 104.0 (3) | O60—Na8—O63 | 88.8 (3) |
O8—W8—O24 | 103.1 (3) | O60—Na8—O61 | 83.8 (3) |
O33—W8—O24 | 92.4 (3) | O63—Na8—O61 | 166.8 (3) |
O8—W8—O25 | 100.2 (3) | O60—Na8—O64 | 171.7 (3) |
O33—W8—O25 | 90.7 (3) | O63—Na8—O64 | 82.9 (3) |
O24—W8—O25 | 155.0 (3) | O61—Na8—O64 | 104.4 (3) |
O8—W8—O29 | 98.7 (3) | O60—Na8—O62 | 98.7 (3) |
O33—W8—O29 | 157.2 (3) | O63—Na8—O62 | 106.7 (3) |
O24—W8—O29 | 84.1 (2) | O61—Na8—O62 | 85.3 (3) |
O25—W8—O29 | 83.5 (3) | O64—Na8—O62 | 83.2 (3) |
O8—W8—O36 | 171.7 (3) | O60—Na8—O2iii | 92.9 (3) |
O33—W8—O36 | 84.0 (3) | O63—Na8—O2iii | 76.3 (3) |
O24—W8—O36 | 78.6 (2) | O61—Na8—O2iii | 93.1 (3) |
O25—W8—O36 | 77.1 (2) | O64—Na8—O2iii | 85.7 (3) |
O29—W8—O36 | 73.3 (2) | O62—Na8—O2iii | 168.0 (3) |
O9—W9—O34 | 103.4 (3) | O68iii—Na9—O66 | 95.6 (3) |
O9—W9—O26 | 101.3 (3) | O68iii—Na9—O68 | 88.2 (3) |
O34—W9—O26 | 91.6 (3) | O66—Na9—O68 | 171.7 (3) |
O9—W9—O25 | 102.8 (3) | O68iii—Na9—O67 | 167.9 (3) |
O34—W9—O25 | 91.8 (3) | O66—Na9—O67 | 86.8 (3) |
O26—W9—O25 | 154.1 (3) | O68—Na9—O67 | 88.0 (3) |
O9—W9—O30 | 98.1 (3) | O68iii—Na9—O65 | 95.9 (3) |
O34—W9—O30 | 158.5 (3) | O66—Na9—O65 | 95.4 (3) |
O26—W9—O30 | 83.6 (3) | O68—Na9—O65 | 91.5 (3) |
O25—W9—O30 | 83.9 (3) | O67—Na9—O65 | 95.7 (3) |
O9—W9—O36 | 172.2 (3) | W1—O1—Na4iv | 132.3 (3) |
O34—W9—O36 | 84.3 (2) | W2—O2—Na8iii | 134.4 (3) |
O26—W9—O36 | 77.2 (2) | W4—O4—Na5ii | 154.9 (4) |
O25—W9—O36 | 77.5 (2) | W8—O8—Na1iv | 145.2 (4) |
O30—W9—O36 | 74.1 (2) | W2—O11—W1 | 113.4 (3) |
O10—W10—O29 | 103.7 (3) | W2—O12—W3 | 113.9 (3) |
O10—W10—O28 | 102.7 (3) | W4—O13—W3 | 114.6 (3) |
O29—W10—O28 | 88.1 (3) | W4—O14—W1 | 116.2 (3) |
O10—W10—O27 | 101.9 (3) | W5—O15—W1 | 115.2 (3) |
O29—W10—O27 | 154.3 (3) | W5—O16—W2 | 115.3 (3) |
O28—W10—O27 | 87.2 (3) | W5—O17—W3 | 116.1 (3) |
O10—W10—O30 | 102.6 (3) | W5—O18—W4 | 116.9 (3) |
O29—W10—O30 | 87.3 (3) | W1—O19—Dy | 128.6 (3) |
O28—W10—O30 | 154.7 (3) | W2—O20—Dy | 130.8 (3) |
O27—W10—O30 | 86.2 (3) | W3—O21—Dy | 129.0 (3) |
O10—W10—O36 | 178.8 (3) | W4—O22—Dy | 130.9 (3) |
O29—W10—O36 | 77.4 (2) | W6—O23—W7 | 114.3 (3) |
O28—W10—O36 | 77.7 (2) | W8—O24—W7 | 113.7 (3) |
O27—W10—O36 | 76.9 (2) | W9—O25—W8 | 114.2 (3) |
O30—W10—O36 | 77.0 (2) | W9—O26—W6 | 114.2 (3) |
O22—Dy—O19 | 75.4 (2) | W10—O27—W6 | 115.0 (3) |
O22—Dy—O20 | 117.8 (2) | W10—O28—W7 | 115.7 (3) |
O19—Dy—O20 | 74.1 (2) | W10—O29—W8 | 116.3 (3) |
O22—Dy—O34 | 139.6 (2) | W10—O30—W9 | 114.8 (3) |
O19—Dy—O34 | 143.0 (2) | W6—O31—Dy | 130.8 (3) |
O20—Dy—O34 | 76.7 (2) | W7—O32—Dy | 131.1 (3) |
O22—Dy—O21 | 75.1 (2) | W8—O33—Dy | 132.1 (3) |
O19—Dy—O21 | 118.7 (2) | W9—O34—Dy | 131.6 (3) |
O20—Dy—O21 | 74.3 (2) | W5—O35—W2 | 94.4 (2) |
O34—Dy—O21 | 73.4 (2) | W5—O35—W3 | 93.4 (2) |
O22—Dy—O32 | 78.0 (2) | W2—O35—W3 | 90.87 (19) |
O19—Dy—O32 | 75.9 (2) | W5—O35—W1 | 92.8 (2) |
O20—Dy—O32 | 140.4 (2) | W2—O35—W1 | 89.4 (2) |
O34—Dy—O32 | 116.0 (2) | W3—O35—W1 | 173.7 (3) |
O21—Dy—O32 | 144.1 (2) | W5—O35—W4 | 92.1 (2) |
O22—Dy—O33 | 144.6 (2) | W2—O35—W4 | 173.5 (3) |
O19—Dy—O33 | 77.6 (2) | W3—O35—W4 | 89.0 (2) |
O20—Dy—O33 | 75.3 (2) | W1—O35—W4 | 89.98 (18) |
O34—Dy—O33 | 73.4 (2) | W10—O36—W6 | 94.1 (2) |
O21—Dy—O33 | 139.1 (2) | W10—O36—W9 | 94.1 (2) |
O32—Dy—O33 | 73.5 (2) | W6—O36—W9 | 90.6 (2) |
O22—Dy—O31 | 75.3 (2) | W10—O36—W8 | 92.9 (2) |
O19—Dy—O31 | 141.3 (2) | W6—O36—W8 | 172.8 (3) |
O20—Dy—O31 | 143.1 (2) | W9—O36—W8 | 90.3 (2) |
O34—Dy—O31 | 73.4 (2) | W10—O36—W7 | 93.3 (2) |
O21—Dy—O31 | 76.8 (2) | W6—O36—W7 | 89.7 (2) |
O32—Dy—O31 | 73.7 (2) | W9—O36—W7 | 172.5 (3) |
O33—Dy—O31 | 115.2 (2) | W8—O36—W7 | 88.5 (2) |
Symmetry codes: (i) x, y, z+1; (ii) −x, −y, −z+1; (iii) −x, −y+1, −z+1; (iv) x, y, z−1. |
Experimental details
Crystal data | |
Chemical formula | Na9[Dy(W5O18)2]·35H2O |
Mr | 3414.54 |
Crystal system, space group | Triclinic, 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) |
V (Å3) | 3277.4 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 18.78 |
Crystal size (mm) | 0.14 × 0.12 × 0.08 |
Data collection | |
Diffractometer | Rigaku RAXIS-RAPID diffractometer |
Absorption correction | Numerical (NUMABS; Higashi, 1999) |
Tmin, Tmax | 0.179, 0.315 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 33444, 14785, 13098 |
Rint | 0.052 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.104, 1.18 |
No. of reflections | 14785 |
No. of parameters | 821 |
No. of restraints | 426 |
H-atom treatment | H-atom parameters not defined |
w = 1/[σ2(Fo2) + (0.0579P)2 + 24.6886P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 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).
W1—O1 | 1.729 (7) | W6—O27 | 2.029 (6) |
W1—O19 | 1.800 (7) | W6—O36 | 2.300 (6) |
W1—O11 | 1.950 (6) | W7—O7 | 1.722 (6) |
W1—O14 | 1.958 (7) | W7—O32 | 1.795 (6) |
W1—O15 | 2.039 (6) | W7—O24 | 1.943 (6) |
W1—O35 | 2.315 (6) | W7—O23 | 1.960 (6) |
W2—O2 | 1.725 (7) | W7—O28 | 2.041 (7) |
W2—O20 | 1.792 (6) | W7—O36 | 2.338 (6) |
W2—O11 | 1.935 (6) | W8—O8 | 1.738 (7) |
W2—O12 | 1.947 (6) | W8—O33 | 1.778 (6) |
W2—O16 | 2.009 (7) | W8—O24 | 1.942 (6) |
W2—O35 | 2.301 (5) | W8—O25 | 1.960 (6) |
W3—O3 | 1.738 (6) | W8—O29 | 2.021 (6) |
W3—O21 | 1.797 (6) | W8—O36 | 2.320 (6) |
W3—O13 | 1.947 (6) | W9—O9 | 1.736 (6) |
W3—O12 | 1.969 (6) | W9—O34 | 1.786 (6) |
W3—O17 | 1.999 (6) | W9—O26 | 1.935 (7) |
W3—O35 | 2.305 (6) | W9—O25 | 1.949 (6) |
W4—O4 | 1.715 (7) | W9—O30 | 2.025 (6) |
W4—O22 | 1.792 (6) | W9—O36 | 2.310 (6) |
W4—O14 | 1.943 (7) | W10—O10 | 1.731 (7) |
W4—O13 | 1.946 (6) | W10—O29 | 1.882 (6) |
W4—O18 | 2.023 (6) | W10—O28 | 1.906 (6) |
W4—O35 | 2.369 (5) | W10—O27 | 1.925 (6) |
W5—O5 | 1.726 (7) | W10—O30 | 1.940 (6) |
W5—O15 | 1.892 (6) | W10—O36 | 2.254 (6) |
W5—O18 | 1.893 (6) | Dy—O22 | 2.355 (6) |
W5—O17 | 1.922 (6) | Dy—O19 | 2.378 (7) |
W5—O16 | 1.957 (6) | Dy—O20 | 2.380 (6) |
W5—O35 | 2.266 (6) | Dy—O34 | 2.391 (6) |
W6—O6 | 1.730 (7) | Dy—O21 | 2.392 (6) |
W6—O31 | 1.775 (6) | Dy—O32 | 2.393 (6) |
W6—O23 | 1.935 (6) | Dy—O33 | 2.398 (6) |
W6—O26 | 1.966 (6) | Dy—O31 | 2.405 (6) |
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).