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As an extension of our continued inter­est in the preparation of inorganic–organic hybrids, we report the successful hydro­thermal synthesis of sodium tris­[tri­aqua­(μ-1,10-phenanthroline-2,9-di­carboxyl­ato)dysprosium(III)] silico­dodeca­tungstate dodeca­hydrate, {[DyNa(C14H6N2O4)3(H2O)9(SiW12O40)]·12H2O}n or Na[Dy(PDA)(H2O)3]3[SiW12O40]·12H2O (1), and sodium aqua tris­[tetra­aqua­(μ-4-hydroxypyridine-2,6-di­carboxyl­ato)praseodymium(III)] silico­do­deca­tungstate dodeca­hydrate, {[NaPr(C7H3NO5)3(H2O)13(SiW12O40)]·12H2O}n or Na(H2O)[Pr(pydc-OH)(H2O)4]3[SiW12O40]·12H2O (2) (in which H2PDA is 1,10-phenanthroline-2,9-di­carb­oxy­lic acid and H2pydc-OH is 4-hy­droxy­pyri­dine-2,6-di­carb­oxy­lic acid or chelidamic acid). Both compounds have been characterized using elemental analysis, IR spectroscopy and X-ray diffraction methods. Structural characterization by single-crystal X-ray diffraction reveals that these compounds consist of [SiW12O40]4− Keggin-type polyoxometalates (POMs), where a single {W3O13} triad is decorated with a trinuclear Ln complex. Moreover, the decorated polyanions are involved in a series of inter­molecular inter­actions, such as hydrogen bonds and anion–π inter­actions, resulting in three-dimensional supra­molecular architectures. Density functional theory (DFT) studies were conducted to support these inter­molecular inter­actions in both 1 and 2, and have been rationalized using mol­ecular electrostatic potential (MEP) surface calculations.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009580/jr3020sup1.cif
Contains datablocks d23_4, jtm570b_4_a, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229618009580/jr3020jtm570b_4_asup2.hkl
Contains datablock jtm570b_4_a

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618009580/jr3020sup3.pdf
Synthesis details, geometry, IR spectra and additional structural figures

CCDC references: 1842658; 1842657

Computing details top

Data collection: CrysAlis PRO (Rigaku OD, 2015) for d23_4; APEX3 (Bruker, 2016) for jtm570b_4_a. Cell refinement: CrysAlis PRO (Rigaku OD, 2015) for d23_4; SAINT (Bruker, 2016) for jtm570b_4_a. Data reduction: CrysAlis PRO (Rigaku OD, 2015) for d23_4; SAINT (Bruker, 2016) and CELL_NOW (Sheldrick, 2008) for jtm570b_4_a. Program(s) used to solve structure: SHELXT (Sheldrick, 2015a) for d23_4; SHELXT (Sheldrick, 2015a) for jtm570b_4_a. Program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b) for d23_4; SHELXL2018 (Sheldrick, 2015b) for jtm570b_4_a. Molecular graphics: OLEX2 (Dolomanov et al., 2009) for d23_4; DIAMOND (Brandenburg & Putz, 2012) for jtm570b_4_a. Software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009) for d23_4; SHELXTL (Bruker, 2016) for jtm570b_4_a.

Sodium tris[triaqua(µ-1,10-phenanthroline-2,9-dicarboxylato)dysprosium(III)] silicododecatungstate dodecahydrate (d23_4) top
Crystal data top
[DyNa(C14H6N2O4)3(H2O)9(SiW12O40)]·12H2ODx = 3.353 Mg m3
Mr = 4527.40Cu Kα radiation, λ = 1.54184 Å
Trigonal, R3Cell parameters from 11603 reflections
a = 20.3334 (3) Åθ = 4.3–76.8°
c = 18.7836 (3) ŵ = 41.93 mm1
V = 6725.60 (19) Å3T = 130 K
Z = 3Block, yellow
F(000) = 60330.07 × 0.05 × 0.03 mm
Data collection top
SuperNova, Dual, Cu at zero, Atlas
diffractometer
5475 independent reflections
Radiation source: micro-focus sealed X-ray tube, SuperNova (Cu) X-ray Source5450 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.030
Detector resolution: 10.2273 pixels mm-1θmax = 77.1°, θmin = 3.4°
ω scansh = 2525
Absorption correction: gaussian
(CrysAlis PRO; Rigaku OD, 2015)
k = 2522
Tmin = 0.097, Tmax = 0.369l = 1723
16672 measured reflections
Refinement top
Refinement on F2H-atom parameters constrained
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0696P)2 + 182.8632P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.036(Δ/σ)max = 0.001
wR(F2) = 0.098Δρmax = 1.53 e Å3
S = 1.02Δρmin = 1.89 e Å3
5475 reflectionsExtinction correction: SHELXL2014 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
426 parametersExtinction coefficient: 0.000018 (3)
1 restraintAbsolute structure: Classical Flack method preferred over Parsons because s.u. lower
Primary atom site location: dualAbsolute structure parameter: 0.013 (7)
Hydrogen site location: inferred from neighbouring sites
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
W40.44911 (3)0.69357 (3)0.56892 (4)0.01497 (17)
W10.41288 (4)0.77239 (4)0.87226 (4)0.01785 (18)
W20.52603 (4)0.80714 (4)0.70932 (4)0.01734 (18)
W30.48229 (4)0.62447 (4)0.71593 (4)0.02049 (19)
Dy10.51195 (5)0.65952 (5)0.37516 (5)0.0164 (2)
Si10.33330.66670.7162 (4)0.0118 (11)
Na10.33330.66670.2727 (9)0.043 (3)
O30.4885 (6)0.7885 (6)0.8053 (6)0.017 (2)
O80.5293 (6)0.7869 (5)0.6112 (6)0.0158 (19)
O120.4913 (6)0.6406 (6)0.6149 (6)0.016 (2)
O110.4427 (5)0.6170 (6)0.8083 (6)0.017 (2)
O60.6133 (6)0.8872 (6)0.7191 (7)0.021 (2)
O70.5555 (5)0.7296 (6)0.7265 (6)0.017 (2)
O20.4173 (6)0.6883 (6)0.9140 (6)0.017 (2)
O10.4622 (7)0.8404 (7)0.9358 (6)0.024 (2)
O150.2638 (6)0.4988 (7)0.3514 (7)0.024 (2)
O100.5381 (6)0.5854 (6)0.7255 (6)0.020 (2)
C100.5397 (10)0.5640 (10)0.5073 (9)0.024 (3)
O130.4852 (6)0.7001 (6)0.4845 (6)0.018 (2)
O170.6409 (6)0.7464 (6)0.3883 (8)0.030 (3)
O200.5127 (8)0.6757 (8)0.2497 (7)0.033 (3)
C90.5742 (12)0.5423 (11)0.5605 (11)0.031 (4)
O210.3066 (8)0.5641 (8)0.1948 (9)0.038 (3)
O160.3803 (6)0.5977 (7)0.3480 (7)0.022 (2)
N10.4311 (7)0.5416 (7)0.4422 (7)0.017 (2)
O90.4179 (5)0.6902 (5)0.6868 (5)0.0102 (17)
C10.3314 (8)0.5341 (8)0.3712 (8)0.017 (3)
C40.3389 (10)0.4085 (9)0.5160 (10)0.026 (3)
H40.30690.36270.54090.031*
C60.4613 (9)0.5179 (8)0.4940 (9)0.018 (3)
C20.3576 (8)0.5003 (9)0.4272 (9)0.019 (3)
C80.5273 (12)0.4744 (12)0.5997 (11)0.033 (4)
H80.55010.45960.63570.040*
O180.7546 (9)0.7895 (10)0.4416 (16)0.081 (8)
C120.6903 (10)0.6552 (12)0.5338 (11)0.034 (4)
H120.74300.68870.54130.041*
C130.6505 (9)0.6725 (9)0.4802 (11)0.027 (4)
C30.3093 (10)0.4326 (10)0.4634 (11)0.029 (4)
H30.25700.40390.45160.035*
N20.5771 (7)0.6266 (7)0.4684 (8)0.020 (3)
C50.4156 (11)0.4509 (10)0.5333 (12)0.030 (4)
C110.6533 (12)0.5922 (13)0.5729 (11)0.036 (5)
H110.67920.58070.60850.043*
C70.4529 (13)0.4307 (11)0.5880 (11)0.035 (4)
H70.42410.38620.61570.041*
C140.6855 (10)0.7409 (10)0.4339 (14)0.038 (5)
O40.33330.66670.8022 (9)0.011 (3)
O140.3542 (5)0.6058 (6)0.5595 (6)0.017 (2)
O50.4639 (6)0.8485 (6)0.6953 (6)0.016 (2)
O190.5444 (8)0.5750 (7)0.3202 (8)0.033 (3)
O250.9043 (12)0.8861 (17)0.3944 (13)0.097 (10)
O230.440 (2)0.5157 (19)0.207 (2)0.135 (15)
O260.7339 (19)0.992 (3)0.622 (2)0.066 (11)0.5
O280.525 (2)1.000 (2)0.950 (2)0.058 (9)*0.5
O270.578 (2)1.010 (2)0.775 (2)0.061 (9)*0.5
O220.33330.66670.126 (3)0.050 (13)*0.5
O240.362 (3)0.473 (3)0.083 (2)0.087 (16)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W40.0123 (3)0.0143 (3)0.0178 (4)0.0062 (2)0.0011 (2)0.0014 (2)
W10.0173 (3)0.0159 (3)0.0187 (4)0.0071 (2)0.0012 (2)0.0036 (2)
W20.0118 (3)0.0150 (3)0.0229 (4)0.0049 (2)0.0009 (2)0.0024 (2)
W30.0175 (3)0.0197 (3)0.0263 (4)0.0108 (3)0.0022 (3)0.0013 (3)
Dy10.0146 (4)0.0155 (4)0.0208 (5)0.0089 (3)0.0030 (3)0.0004 (3)
Si10.0097 (15)0.0097 (15)0.016 (3)0.0048 (8)0.0000.000
Na10.040 (5)0.040 (5)0.050 (9)0.020 (2)0.0000.000
O30.017 (5)0.019 (5)0.014 (5)0.008 (4)0.002 (4)0.001 (4)
O80.016 (5)0.010 (4)0.019 (5)0.005 (4)0.001 (4)0.002 (4)
O120.016 (5)0.018 (5)0.019 (6)0.012 (4)0.005 (4)0.005 (4)
O110.011 (4)0.018 (5)0.016 (5)0.004 (4)0.001 (4)0.003 (4)
O60.009 (4)0.019 (5)0.032 (6)0.005 (4)0.002 (4)0.001 (4)
O70.011 (4)0.013 (5)0.020 (5)0.001 (4)0.002 (4)0.001 (4)
O20.015 (4)0.017 (5)0.019 (6)0.008 (4)0.002 (4)0.003 (4)
O10.029 (6)0.025 (6)0.017 (6)0.013 (5)0.000 (4)0.003 (4)
O150.014 (5)0.031 (6)0.027 (6)0.011 (4)0.001 (4)0.008 (5)
O100.017 (5)0.025 (5)0.019 (5)0.012 (4)0.001 (4)0.003 (4)
C100.028 (8)0.033 (8)0.018 (8)0.021 (7)0.006 (6)0.013 (6)
O130.015 (5)0.019 (5)0.019 (6)0.008 (4)0.003 (4)0.003 (4)
O170.015 (5)0.020 (6)0.051 (8)0.005 (4)0.005 (5)0.002 (5)
O200.042 (7)0.048 (8)0.021 (7)0.031 (7)0.005 (5)0.004 (5)
C90.044 (11)0.032 (9)0.026 (9)0.026 (8)0.002 (8)0.001 (7)
O210.034 (7)0.035 (7)0.046 (9)0.017 (6)0.010 (6)0.004 (6)
O160.013 (5)0.027 (6)0.026 (6)0.010 (4)0.005 (4)0.002 (5)
N10.020 (6)0.016 (5)0.019 (6)0.013 (5)0.001 (5)0.007 (5)
O90.012 (4)0.007 (4)0.011 (5)0.004 (3)0.003 (3)0.002 (3)
C10.020 (7)0.021 (7)0.013 (7)0.014 (6)0.002 (5)0.003 (5)
C40.027 (8)0.015 (7)0.030 (9)0.007 (6)0.008 (7)0.007 (6)
C60.021 (7)0.019 (7)0.019 (8)0.014 (6)0.003 (6)0.005 (5)
C20.018 (7)0.022 (7)0.017 (8)0.010 (6)0.008 (5)0.003 (6)
C80.048 (11)0.046 (11)0.027 (9)0.040 (10)0.006 (8)0.014 (8)
O180.018 (7)0.035 (9)0.17 (3)0.001 (6)0.006 (10)0.017 (12)
C120.023 (8)0.044 (11)0.033 (11)0.015 (8)0.017 (7)0.013 (8)
C130.015 (7)0.018 (7)0.045 (11)0.006 (6)0.007 (7)0.010 (7)
C30.028 (8)0.020 (7)0.039 (11)0.011 (7)0.001 (7)0.000 (7)
N20.019 (6)0.024 (6)0.025 (7)0.016 (5)0.001 (5)0.006 (5)
C50.033 (9)0.019 (7)0.044 (11)0.017 (7)0.004 (8)0.000 (7)
C110.038 (10)0.053 (12)0.032 (10)0.033 (9)0.016 (8)0.017 (9)
C70.054 (12)0.026 (8)0.028 (10)0.024 (9)0.000 (8)0.005 (7)
C140.019 (8)0.018 (8)0.076 (16)0.009 (7)0.011 (8)0.008 (8)
O40.011 (4)0.011 (4)0.011 (8)0.005 (2)0.0000.000
O140.013 (4)0.016 (5)0.021 (6)0.007 (4)0.005 (4)0.003 (4)
O50.017 (5)0.015 (5)0.016 (5)0.009 (4)0.003 (4)0.003 (4)
O190.053 (8)0.025 (6)0.036 (8)0.030 (6)0.018 (6)0.010 (5)
O250.045 (11)0.14 (2)0.048 (14)0.000 (12)0.003 (9)0.015 (13)
O230.18 (4)0.11 (2)0.16 (4)0.11 (3)0.08 (3)0.07 (2)
O260.030 (16)0.09 (3)0.06 (2)0.016 (17)0.015 (15)0.02 (2)
O240.11 (4)0.11 (4)0.04 (2)0.06 (3)0.00 (2)0.04 (2)
Geometric parameters (Å, º) top
W4—O81.949 (10)Na1—O21ii2.378 (18)
W4—O121.888 (10)Na1—O21i2.378 (18)
W4—O131.725 (11)Na1—O212.378 (18)
W4—O92.296 (10)Na1—O16i2.494 (15)
W4—O14i1.940 (10)Na1—O162.494 (15)
W4—O141.870 (10)Na1—O16ii2.494 (15)
W1—O31.884 (11)Na1—O222.76 (7)
W1—O11i1.909 (10)O11—W1ii1.909 (10)
W1—O2i1.952 (10)O2—W1ii1.952 (10)
W1—O21.924 (10)O15—Dy1ii2.306 (10)
W1—O11.719 (11)O15—C11.247 (19)
W1—O42.343 (10)C10—C91.41 (3)
W2—O31.921 (11)C10—C61.41 (2)
W2—O81.896 (11)C10—N21.33 (2)
W2—O61.716 (10)O17—C141.29 (2)
W2—O71.974 (11)C9—C81.43 (3)
W2—O92.332 (9)C9—C111.43 (3)
W2—O51.853 (10)O16—C11.25 (2)
W3—O121.919 (11)N1—C61.36 (2)
W3—O111.886 (11)N1—C21.33 (2)
W3—O71.908 (10)C1—C21.49 (2)
W3—O101.689 (11)C4—C31.37 (3)
W3—O92.356 (9)C4—C51.39 (3)
W3—O5ii1.938 (10)C6—C51.41 (2)
Dy1—O15i2.306 (10)C2—C31.40 (2)
Dy1—O132.375 (11)C8—C71.34 (3)
Dy1—O172.329 (11)O18—C141.26 (2)
Dy1—O202.379 (13)C12—C131.44 (3)
Dy1—O162.374 (11)C12—C111.34 (3)
Dy1—N12.469 (13)C13—N21.32 (2)
Dy1—N22.482 (14)C13—C141.48 (3)
Dy1—O192.364 (12)C5—C71.45 (3)
Si1—O91.633 (10)O4—W1i2.343 (10)
Si1—O9ii1.633 (10)O4—W1ii2.343 (10)
Si1—O9i1.633 (10)O14—W4ii1.940 (10)
Si1—O41.615 (19)O5—W3i1.938 (10)
O8—W4—O973.7 (4)O9i—Si1—O9109.2 (4)
O12—W4—O888.4 (4)O9ii—Si1—O9109.2 (4)
O12—W4—O974.9 (4)O4—Si1—O9ii109.8 (4)
O12—W4—O14i157.7 (5)O4—Si1—O9109.8 (4)
O13—W4—O8100.6 (5)O4—Si1—O9i109.8 (4)
O13—W4—O1299.6 (5)O21ii—Na1—O21i86.1 (7)
O13—W4—O9172.0 (4)O21ii—Na1—O2186.1 (7)
O13—W4—O14i102.6 (5)O21i—Na1—O2186.1 (7)
O13—W4—O14100.6 (5)O21—Na1—O16ii104.8 (4)
O14—W4—O8158.4 (5)O21—Na1—O16i162.2 (4)
O14i—W4—O885.4 (4)O21—Na1—O1680.8 (5)
O14—W4—O1292.6 (5)O21i—Na1—O16ii162.2 (4)
O14i—W4—O982.8 (4)O21i—Na1—O16104.8 (4)
O14—W4—O985.7 (4)O21i—Na1—O16i80.8 (5)
O14—W4—O14i85.6 (6)O21ii—Na1—O16162.2 (4)
O3—W1—O11i86.9 (5)O21ii—Na1—O16i104.8 (4)
O3—W1—O2i158.6 (4)O21ii—Na1—O16ii80.8 (5)
O3—W1—O291.7 (4)O21—Na1—O2252.0 (5)
O3—W1—O485.1 (4)O21i—Na1—O2252.0 (5)
O11i—W1—O2i86.9 (4)O21ii—Na1—O2252.0 (5)
O11i—W1—O2158.5 (5)O16i—Na1—O1691.0 (6)
O11i—W1—O484.1 (4)O16ii—Na1—O1691.0 (6)
O2—W1—O2i86.7 (6)O16ii—Na1—O16i91.0 (6)
O2—W1—O474.4 (4)O16ii—Na1—O22124.5 (4)
O2i—W1—O473.9 (4)O16i—Na1—O22124.5 (4)
O1—W1—O3103.1 (5)O16—Na1—O22124.5 (4)
O1—W1—O11i101.7 (5)W1—O3—W2150.5 (6)
O1—W1—O299.5 (5)W2—O8—W4120.3 (5)
O1—W1—O2i98.2 (5)W4—O12—W3121.2 (5)
O1—W1—O4170.1 (5)W3—O11—W1ii151.5 (6)
O3—W2—O786.4 (5)W3—O7—W2120.0 (5)
O3—W2—O983.7 (4)W1—O2—W1ii120.1 (6)
O8—W2—O3157.4 (4)C1—O15—Dy1ii141.1 (10)
O8—W2—O785.9 (4)C6—C10—C9119.4 (17)
O8—W2—O973.8 (4)N2—C10—C9123.5 (16)
O6—W2—O3101.9 (5)N2—C10—C6117.1 (15)
O6—W2—O8100.3 (5)W4—O13—Dy1158.6 (6)
O6—W2—O799.0 (5)C14—O17—Dy1125.2 (11)
O6—W2—O9170.9 (4)C10—C9—C8118.1 (18)
O6—W2—O5101.6 (5)C10—C9—C11116.9 (18)
O7—W2—O973.9 (4)C11—C9—C8125.0 (19)
O5—W2—O386.0 (5)Dy1—O16—Na1118.1 (5)
O5—W2—O893.8 (4)C1—O16—Dy1125.2 (10)
O5—W2—O7159.1 (4)C1—O16—Na1116.6 (9)
O5—W2—O985.9 (4)C6—N1—Dy1120.7 (10)
O12—W3—O972.9 (4)C2—N1—Dy1119.8 (11)
O12—W3—O5ii85.8 (5)C2—N1—C6119.5 (13)
O11—W3—O12157.5 (4)W4—O9—W292.2 (3)
O11—W3—O793.3 (5)W4—O9—W391.0 (3)
O11—W3—O985.6 (4)W2—O9—W391.6 (3)
O11—W3—O5ii84.9 (4)Si1—O9—W4124.8 (6)
O7—W3—O1287.5 (5)Si1—O9—W2123.7 (5)
O7—W3—O974.5 (4)Si1—O9—W3123.9 (5)
O7—W3—O5ii157.4 (4)O15—C1—O16124.7 (14)
O10—W3—O1299.0 (5)O15—C1—C2119.4 (14)
O10—W3—O11103.0 (5)O16—C1—C2116.0 (13)
O10—W3—O7100.6 (5)C3—C4—C5120.2 (16)
O10—W3—O9170.5 (5)C10—C6—C5121.8 (16)
O10—W3—O5ii101.7 (5)N1—C6—C10116.8 (15)
O5ii—W3—O982.9 (4)N1—C6—C5121.3 (15)
O15i—Dy1—O1372.5 (4)N1—C2—C1114.1 (14)
O15i—Dy1—O1784.8 (4)N1—C2—C3122.0 (16)
O15i—Dy1—O2071.1 (5)C3—C2—C1123.9 (15)
O15i—Dy1—O1681.1 (4)C7—C8—C9123.0 (17)
O15i—Dy1—N1132.5 (4)C11—C12—C13120.2 (16)
O15i—Dy1—N2134.4 (4)C12—C13—C14124.9 (15)
O15i—Dy1—O19141.5 (4)N2—C13—C12121.1 (17)
O13—Dy1—O20142.7 (4)N2—C13—C14114.0 (16)
O13—Dy1—N174.9 (4)C4—C3—C2119.0 (16)
O13—Dy1—N274.3 (4)C10—N2—Dy1121.3 (10)
O17—Dy1—O1390.6 (4)C13—N2—Dy1119.5 (12)
O17—Dy1—O2094.2 (5)C13—N2—C10119.2 (15)
O17—Dy1—O16165.4 (4)C4—C5—C6117.9 (17)
O17—Dy1—N1129.3 (5)C4—C5—C7124.8 (17)
O17—Dy1—N265.1 (5)C6—C5—C7117.3 (17)
O17—Dy1—O1988.9 (5)C12—C11—C9119.1 (18)
O20—Dy1—N1126.5 (5)C8—C7—C5120.3 (18)
O20—Dy1—N2140.3 (4)O17—C14—C13116.1 (15)
O16—Dy1—O1388.6 (4)O18—C14—O17124 (2)
O16—Dy1—O2077.8 (4)O18—C14—C13120 (2)
O16—Dy1—N164.4 (4)W1i—O4—W1ii91.6 (5)
O16—Dy1—N2128.4 (4)W1—O4—W1ii91.6 (5)
N1—Dy1—N264.1 (4)W1i—O4—W191.6 (5)
O19—Dy1—O13145.6 (4)Si1—O4—W1i124.2 (3)
O19—Dy1—O2071.5 (5)Si1—O4—W1124.2 (3)
O19—Dy1—O1699.9 (5)Si1—O4—W1ii124.2 (3)
O19—Dy1—N179.0 (4)W4—O14—W4ii151.9 (6)
O19—Dy1—N274.4 (5)W2—O5—W3i153.0 (6)
O9i—Si1—O9ii109.2 (4)
Dy1ii—O15—C1—O1687 (2)O9ii—Si1—O9—W2177.8 (4)
Dy1ii—O15—C1—C292.5 (19)O9i—Si1—O9—W258.5 (10)
Dy1—O17—C14—O18178 (2)O9i—Si1—O9—W3177.8 (4)
Dy1—O17—C14—C131 (2)O9ii—Si1—O9—W362.9 (10)
Dy1—O16—C1—O15172.7 (11)O9—Si1—O4—W1i178.1 (3)
Dy1—O16—C1—C28.1 (18)O9i—Si1—O4—W161.9 (3)
Dy1—N1—C6—C100.5 (17)O9ii—Si1—O4—W1178.1 (3)
Dy1—N1—C6—C5179.4 (12)O9—Si1—O4—W158.1 (3)
Dy1—N1—C2—C12.9 (16)O9i—Si1—O4—W1ii178.1 (3)
Dy1—N1—C2—C3179.6 (12)O9ii—Si1—O4—W1ii58.1 (3)
Na1—O16—C1—O1511 (2)O9—Si1—O4—W1ii61.9 (3)
Na1—O16—C1—C2168.5 (10)O9ii—Si1—O4—W1i61.9 (3)
O3—W2—O8—W43.7 (15)O9i—Si1—O4—W1i58.1 (3)
O3—W2—O5—W3i27.3 (13)C1—C2—C3—C4177.1 (15)
O8—W4—O12—W372.3 (6)C4—C5—C7—C8178.6 (19)
O8—W4—O13—Dy1145.2 (15)C6—C10—C9—C81 (2)
O8—W4—O14—W4ii39 (2)C6—C10—C9—C11178.3 (16)
O8—W2—O5—W3i130.1 (13)C6—C10—N2—Dy11.1 (19)
O12—W4—O13—Dy155.1 (16)C6—C10—N2—C13178.4 (14)
O12—W4—O14—W4ii131.1 (14)C6—N1—C2—C1178.0 (12)
O12—W3—O11—W1ii40 (2)C6—N1—C2—C30 (2)
O11i—W1—O3—W224.7 (12)C6—C5—C7—C80 (3)
O6—W2—O8—W4172.6 (6)C2—N1—C6—C10179.7 (13)
O6—W2—O5—W3i128.6 (13)C2—N1—C6—C51 (2)
O7—W2—O8—W474.2 (6)C8—C9—C11—C12178 (2)
O7—W2—O5—W3i42 (2)C12—C13—N2—Dy1179.8 (13)
O7—W3—O11—W1ii130.9 (13)C12—C13—N2—C101 (2)
O2—W1—O3—W2133.9 (13)C12—C13—C14—O17179.3 (18)
O2i—W1—O3—W249 (2)C12—C13—C14—O182 (3)
O1—W1—O3—W2125.9 (13)C13—C12—C11—C90 (3)
O15—C1—C2—N1177.7 (13)C3—C4—C5—C61 (3)
O15—C1—C2—C35 (2)C3—C4—C5—C7180.0 (18)
O10—W3—O11—W1ii127.4 (13)N2—C10—C9—C8178.6 (16)
C10—C9—C8—C70 (3)N2—C10—C9—C111 (3)
C10—C9—C11—C121 (3)N2—C10—C6—N10 (2)
C10—C6—C5—C4179.3 (15)N2—C10—C6—C5178.5 (15)
C10—C6—C5—C70 (2)N2—C13—C14—O171 (3)
O13—W4—O12—W3172.8 (6)N2—C13—C14—O18178 (2)
O13—W4—O14—W4ii128.6 (14)C5—C4—C3—C20 (3)
C9—C10—C6—N1179.9 (14)C11—C9—C8—C7177.5 (19)
C9—C10—C6—C51 (2)C11—C12—C13—N20 (3)
C9—C10—N2—Dy1179.4 (12)C11—C12—C13—C14179.6 (19)
C9—C10—N2—C131 (2)C14—C13—N2—Dy10 (2)
C9—C8—C7—C50 (3)C14—C13—N2—C10179.3 (15)
O16—C1—C2—N13.0 (19)O4—W1—O3—W259.7 (12)
O16—C1—C2—C3174.5 (15)O4—Si1—O9—W4176.8 (4)
N1—C6—C5—C42 (2)O4—Si1—O9—W261.9 (6)
N1—C6—C5—C7179.3 (15)O4—Si1—O9—W357.4 (6)
N1—C2—C3—C40 (3)O14—W4—O12—W386.1 (7)
O9—W4—O12—W31.3 (5)O14i—W4—O12—W31.2 (15)
O9—W4—O14—W4ii56.5 (13)O14i—W4—O13—Dy1127.2 (15)
O9—W2—O8—W40.3 (5)O14—W4—O13—Dy139.4 (16)
O9—W2—O5—W3i56.7 (13)O14i—W4—O14—W4ii26.6 (16)
O9—W3—O11—W1ii56.8 (13)O5—W2—O8—W484.9 (6)
O9i—Si1—O9—W462.8 (6)O5ii—W3—O11—W1ii26.5 (13)
O9ii—Si1—O9—W456.4 (7)
Symmetry codes: (i) y+1, xy+1, z; (ii) x+y, x+1, z.
Sodium aqua tris[tetraaqua(µ-4-hydroxypyridine-2,6-dicarboxylato)praseodymium(III)] silicododecatungstate dodecahydrate (jtm570b_4_a) top
Crystal data top
[NaPr(C7H3NO5)3(H2O)13(SiW12O40)]·12H2ODx = 3.601 Mg m3
Mr = 4307.67Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3Cell parameters from 9882 reflections
a = 18.119 (3) Åθ = 2.3–29.1°
c = 21.078 (3) ŵ = 19.14 mm1
V = 5993 (2) Å3T = 100 K
Z = 3Column, light yellow
F(000) = 57900.24 × 0.13 × 0.12 mm
Data collection top
Bruker SMART APEX CCD
diffractometer
7142 independent reflections
Radiation source: fine-focus sealed tube6106 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.085
Detector resolution: 8.3333 pixels mm-1θmax = 29.2°, θmin = 1.6°
φ and ω scansh = 2424
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2009)
k = 2424
Tmin = 0.09, Tmax = 0.22l = 2828
74256 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0314P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
7142 reflectionsΔρmax = 1.97 e Å3
385 parametersΔρmin = 2.07 e Å3
241 restraintsAbsolute structure: Flack x determined using 2688 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.006 (7)
Special details top

Experimental. The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5° in ω, colllected at φ = 0.00, 90.00 and 180.00° and 2 sets of 800 frames, each of width 0.45° in φ, collected at ω = -30.00 and 210.00°. The scan time was 10 sec/frame. Analysis of 1347 reflections having I/σ(I) > 12 and chosen from the full data set with CELL_NOW (Sheldrick, 2008) showed the crystal to belong to the trigonal system and to have a very minor twin component. The raw data were processed using the multi-component version of SAINT under control of the two-component orientation file generated by CELL_NOW.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hatoms attached to carbon were placed in calculated positions (C—H = 0.95 Å) while those attached to oxygen were placed in positions that would generate the most favorable hydrogen bonding interactions with O—H = 0.87 Å. All were included as riding contributions with displacement parameters 1.2 - 1.5 times those of the attached atoms. An attempt to refine the model with the full twinned data led to some atoms becoming NPD and since the twin component was minor, it was not included in the final refinement.

the crystal used was mounted on a nylon loop with a drop of heavy oil and mounted in a cold nitrogen stream on a Bruker Smart APEX CCD diffractometer. A full sphere of data was collected from which it was determined that the crystal consisted of two components (CELL-NOW). The raw data were converted to F2 values using the multi-component version of SAINT under the control of the 2-component orientation file generated by CELL-NOW. Correction for absorption and merging of equivalent reflections for the 2-component reflection file was carried out with TWINABS which also extracted a single-component reflection file from the full data set for structure solution. The structure was solved by direct methods and refined by full-matrix, least squares.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Na10.3333330.6666670.2314 (5)0.038 (3)
W10.25977 (4)0.53062 (4)0.48154 (2)0.00999 (12)
W20.13249 (4)0.48260 (4)0.60810 (2)0.01449 (13)
W30.15307 (4)0.69539 (4)0.61336 (2)0.01467 (14)
W40.21000 (4)0.61161 (4)0.75405 (3)0.01871 (15)
Pr10.16948 (6)0.42412 (6)0.29909 (4)0.0231 (2)
Si10.3333330.6666670.6130 (3)0.0060 (10)
O10.3227 (7)0.4982 (7)0.2939 (5)0.025 (2)
O20.4232 (7)0.6357 (7)0.2907 (5)0.031 (3)
O30.6776 (7)0.7460 (7)0.3773 (5)0.024 (2)
O40.7212 (8)0.6804 (8)0.4459 (5)0.039 (3)
O50.4381 (9)0.4029 (8)0.4840 (6)0.042 (3)
H50.3898370.3647950.4715720.063*
O60.2088 (10)0.4350 (9)0.1846 (6)0.056 (4)
H6A0.2639660.4645960.1810360.085*
H6B0.1860770.4604460.1641360.085*
O70.0718 (9)0.4521 (9)0.2250 (6)0.053 (4)
H7A0.0192390.4210800.2374910.079*
H7B0.0766390.4384680.1862810.079*
O80.0681 (7)0.2813 (7)0.2456 (5)0.032 (3)
H8A0.0976650.2616560.2269720.047*
H8B0.0374250.2890260.2174720.047*
O90.2233 (7)0.3224 (7)0.3174 (5)0.037 (3)
H9A0.1831220.2758680.3345430.056*
H9B0.2670110.3457280.3427430.056*
O100.2354 (6)0.4843 (6)0.4074 (4)0.015 (2)
O110.0276 (7)0.4063 (7)0.6181 (5)0.022 (2)
O120.1309 (7)0.5762 (7)0.8086 (5)0.025 (2)
O130.0551 (7)0.6863 (7)0.6217 (5)0.024 (2)
O140.3762 (5)0.6132 (5)0.4720 (4)0.0095 (18)
O150.2857 (6)0.4523 (6)0.5222 (4)0.015 (2)
O160.1485 (6)0.4700 (6)0.5200 (4)0.016 (2)
O170.1244 (6)0.5798 (6)0.5935 (4)0.016 (2)
O180.1632 (6)0.5225 (6)0.6932 (4)0.019 (2)
O190.1760 (6)0.6706 (6)0.6954 (4)0.018 (2)
O200.2894 (6)0.7213 (6)0.7886 (5)0.022 (2)
O210.2267 (6)0.8131 (6)0.6237 (4)0.015 (2)
O220.2918 (5)0.7230 (5)0.5879 (4)0.0076 (17)
O230.3333330.6666670.6905 (7)0.011 (3)
N10.5262 (8)0.6094 (7)0.3649 (6)0.020 (3)
C10.3930 (11)0.5599 (11)0.3123 (8)0.029 (4)
C20.4468 (10)0.5463 (10)0.3609 (7)0.021 (3)
C30.4127 (11)0.4739 (10)0.3990 (7)0.028 (4)
H30.3550160.4298040.3951110.033*
C40.4670 (11)0.4694 (11)0.4427 (8)0.027 (4)
C50.5495 (10)0.5347 (10)0.4472 (7)0.021 (3)
H5A0.5865550.5319930.4777710.026*
C60.5795 (10)0.6054 (10)0.4071 (7)0.017 (3)
C70.6672 (9)0.6826 (9)0.4105 (7)0.018 (3)
O240.8781 (10)0.7242 (11)0.3652 (7)0.076 (5)
H24A0.8324200.6753480.3583650.114*
H24B0.9081810.7185890.3949850.114*
O250.9855 (12)0.7199 (12)0.4581 (8)0.078 (5)
O260.419 (3)0.796 (3)0.162 (3)0.089 (17)0.333
H26A0.4079850.8331910.1800720.133*0.3333
H26B0.3984610.8014530.1263320.133*0.3333
O270.8519 (17)0.8712 (16)0.3783 (11)0.047 (7)0.5
H27A0.8940640.8625360.3863010.071*0.5
H27B0.8456740.8725270.3375000.071*0.5
O280.1006 (19)0.5532 (18)0.1200 (14)0.062 (8)0.5
H28A0.1065820.5520730.1608630.093*0.5
H28B0.0578320.5608340.1117140.093*0.5
O290.539 (2)0.4313 (19)0.5778 (13)0.030 (5)0.3822
H29A0.5753810.4714520.6025930.045*0.3822
H29B0.4894310.4276420.5814110.045*0.3822
O29A0.843 (2)1.032 (2)0.2569 (17)0.030 (5)0.3047
H29C0.8206621.0438540.2242000.045*0.3047
H29D0.8420921.0618040.2893910.045*0.3047
O29B0.860 (2)0.949 (2)0.2776 (17)0.030 (5)0.3134
H29E0.8659370.9992680.2757460.045*0.3134
H29F0.8581180.9297380.2393160.045*0.3134
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.051 (5)0.051 (5)0.013 (6)0.025 (2)0.0000.000
W10.0121 (3)0.0115 (3)0.0055 (2)0.0051 (2)0.0007 (2)0.0016 (2)
W20.0142 (3)0.0158 (3)0.0107 (3)0.0054 (3)0.0044 (2)0.0018 (2)
W30.0154 (3)0.0195 (3)0.0107 (3)0.0099 (3)0.0037 (2)0.0002 (2)
W40.0241 (3)0.0247 (3)0.0068 (3)0.0118 (3)0.0057 (2)0.0023 (2)
Pr10.0280 (5)0.0301 (5)0.0095 (4)0.0132 (4)0.0055 (3)0.0069 (3)
Si10.0078 (15)0.0078 (15)0.002 (2)0.0039 (7)0.0000.000
O10.024 (5)0.026 (5)0.024 (5)0.011 (4)0.004 (4)0.005 (4)
O20.033 (5)0.029 (5)0.026 (5)0.012 (4)0.001 (4)0.001 (4)
O30.025 (5)0.025 (5)0.025 (5)0.015 (4)0.001 (4)0.003 (4)
O40.037 (6)0.039 (7)0.029 (6)0.010 (5)0.014 (5)0.004 (5)
O50.056 (8)0.037 (7)0.032 (6)0.023 (6)0.016 (6)0.009 (5)
O60.061 (8)0.073 (9)0.030 (7)0.030 (7)0.003 (6)0.003 (6)
O70.052 (8)0.060 (8)0.019 (6)0.007 (6)0.020 (5)0.007 (5)
O80.024 (5)0.035 (6)0.035 (6)0.015 (5)0.007 (5)0.020 (5)
O90.024 (6)0.031 (6)0.049 (7)0.008 (5)0.002 (5)0.008 (5)
O100.012 (4)0.016 (4)0.010 (4)0.003 (3)0.001 (3)0.004 (3)
O110.022 (5)0.024 (5)0.019 (5)0.011 (5)0.003 (4)0.001 (4)
O120.032 (6)0.031 (6)0.014 (5)0.017 (5)0.005 (4)0.007 (4)
O130.023 (5)0.029 (6)0.019 (5)0.012 (5)0.003 (4)0.002 (4)
O140.014 (4)0.011 (4)0.002 (4)0.006 (3)0.001 (3)0.001 (3)
O150.016 (4)0.014 (4)0.012 (4)0.006 (3)0.002 (3)0.001 (3)
O160.021 (4)0.016 (4)0.011 (4)0.010 (4)0.001 (3)0.001 (3)
O170.012 (4)0.022 (4)0.012 (4)0.008 (4)0.001 (3)0.002 (3)
O180.020 (4)0.023 (5)0.012 (4)0.009 (4)0.003 (4)0.001 (4)
O190.022 (4)0.019 (4)0.013 (4)0.009 (4)0.005 (4)0.003 (3)
O200.025 (5)0.026 (5)0.015 (4)0.014 (4)0.001 (4)0.003 (4)
O210.021 (4)0.018 (4)0.010 (4)0.013 (4)0.000 (3)0.001 (3)
O220.008 (2)0.008 (2)0.007 (2)0.0039 (15)0.0016 (13)0.0004 (13)
O230.013 (4)0.013 (4)0.005 (5)0.0067 (18)0.0000.000
N10.028 (5)0.016 (5)0.018 (5)0.013 (4)0.003 (4)0.006 (4)
C10.030 (6)0.030 (6)0.028 (6)0.016 (5)0.005 (5)0.008 (5)
C20.025 (6)0.022 (6)0.018 (6)0.013 (5)0.001 (5)0.004 (5)
C30.027 (6)0.029 (6)0.026 (6)0.013 (5)0.011 (5)0.001 (5)
C40.030 (6)0.028 (6)0.023 (6)0.015 (5)0.014 (5)0.007 (5)
C50.022 (6)0.026 (6)0.017 (6)0.012 (5)0.003 (5)0.004 (5)
C60.021 (6)0.021 (6)0.010 (5)0.012 (5)0.001 (4)0.006 (4)
C70.021 (6)0.021 (6)0.015 (5)0.012 (5)0.002 (4)0.004 (4)
O240.054 (9)0.103 (11)0.058 (9)0.030 (8)0.006 (7)0.004 (8)
O250.098 (10)0.076 (10)0.069 (9)0.050 (8)0.012 (8)0.011 (8)
O260.09 (2)0.10 (2)0.08 (2)0.047 (15)0.009 (13)0.017 (13)
O270.062 (12)0.048 (12)0.028 (11)0.025 (10)0.001 (9)0.002 (9)
O280.073 (14)0.051 (12)0.058 (13)0.028 (10)0.019 (11)0.013 (10)
O290.036 (8)0.026 (7)0.028 (7)0.016 (6)0.003 (6)0.000 (6)
O29A0.036 (8)0.026 (7)0.028 (7)0.016 (6)0.003 (6)0.000 (6)
O29B0.036 (8)0.026 (7)0.028 (7)0.016 (6)0.003 (6)0.000 (6)
Geometric parameters (Å, º) top
Na1—O2i2.333 (13)Si1—O221.629 (9)
Na1—O2ii2.333 (13)Si1—O22i1.629 (9)
Na1—O22.333 (13)Si1—O22ii1.629 (9)
Na1—O262.53 (5)Si1—O231.633 (16)
Na1—O26ii2.53 (5)O1—C11.264 (19)
Na1—O26i2.53 (5)O2—C11.282 (19)
Na1—Pr1i4.137 (4)O3—C71.276 (17)
Na1—Pr14.137 (4)O4—C71.247 (18)
Na1—Pr1ii4.137 (4)O5—C41.36 (2)
W1—O101.724 (9)O5—H50.8399
W1—O141.890 (9)O6—H6A0.8699
W1—O151.906 (9)O6—H6B0.8701
W1—O161.927 (10)O7—H7A0.8699
W1—O14ii1.938 (8)O7—H7B0.8701
W1—O22i2.320 (8)O8—H8A0.8701
W2—O111.714 (10)O8—H8B0.8701
W2—O171.864 (10)O9—H9A0.8700
W2—O181.911 (9)O9—H9B0.8701
W2—O161.911 (9)N1—C21.318 (18)
W2—O21i1.969 (9)N1—C61.340 (19)
W2—O22i2.321 (8)C1—C21.52 (2)
W3—O131.708 (11)C2—C31.39 (2)
W3—O211.879 (9)C3—C41.38 (2)
W3—O191.884 (10)C3—H30.9500
W3—O171.936 (10)C4—C51.37 (2)
W3—O15ii1.945 (9)C5—C61.40 (2)
W3—O222.367 (9)C5—H5A0.9500
W4—O121.693 (10)C6—C71.51 (2)
W4—O181.897 (10)O24—H24A0.8700
W4—O20i1.919 (10)O24—H24B0.8700
W4—O201.922 (10)O26—H26A0.8692
W4—O191.926 (10)O26—H26B0.8697
W4—O232.357 (8)O27—H27A0.8700
Pr1—O12.407 (11)O27—H27B0.8700
Pr1—O3ii2.468 (10)O28—H28A0.8699
Pr1—O2ii2.477 (11)O28—H28B0.8702
Pr1—O62.496 (13)O29—H29A0.8701
Pr1—O92.509 (12)O29—H29B0.8698
Pr1—O102.554 (9)O29A—H29C0.8702
Pr1—N1ii2.567 (12)O29A—H29D0.8699
Pr1—O82.567 (11)O29B—H29E0.8698
Pr1—O72.593 (12)O29B—H29F0.8701
O2i—Na1—O2ii94.0 (5)O9—Pr1—O1084.6 (3)
O2i—Na1—O294.0 (5)O1—Pr1—N1ii124.3 (4)
O2ii—Na1—O294.0 (5)O3ii—Pr1—N1ii63.0 (4)
O2i—Na1—O2671.8 (14)O2ii—Pr1—N1ii63.5 (4)
O2ii—Na1—O26151.8 (13)O6—Pr1—N1ii134.0 (4)
O2—Na1—O26110.8 (12)O9—Pr1—N1ii134.7 (4)
O2i—Na1—O26ii151.8 (13)O10—Pr1—N1ii66.7 (3)
O2ii—Na1—O26ii110.8 (12)O1—Pr1—O8125.9 (3)
O2—Na1—O26ii71.8 (14)O3ii—Pr1—O869.6 (4)
O26—Na1—O26ii90.2 (18)O2ii—Pr1—O8139.6 (4)
O2i—Na1—O26i110.8 (12)O6—Pr1—O871.8 (4)
O2ii—Na1—O26i71.8 (14)O9—Pr1—O870.8 (4)
O2—Na1—O26i151.8 (13)O10—Pr1—O8140.3 (3)
O26—Na1—O26i90.2 (18)N1ii—Pr1—O8109.7 (4)
O26ii—Na1—O26i90.2 (18)O1—Pr1—O7125.0 (4)
O2i—Na1—Pr1i77.1 (3)O3ii—Pr1—O7102.9 (4)
O2ii—Na1—Pr1i121.4 (4)O2ii—Pr1—O766.6 (4)
O2—Na1—Pr1i31.7 (3)O6—Pr1—O766.3 (5)
O26—Na1—Pr1i80.0 (12)O9—Pr1—O7142.2 (4)
O26ii—Na1—Pr1i78.6 (14)O10—Pr1—O7132.4 (4)
O26i—Na1—Pr1i165.0 (13)N1ii—Pr1—O770.2 (4)
O2i—Na1—Pr1121.4 (4)O8—Pr1—O773.6 (4)
O2ii—Na1—Pr131.7 (3)O1—Pr1—Na151.4 (3)
O2—Na1—Pr177.1 (3)O3ii—Pr1—Na1153.4 (3)
O26—Na1—Pr1165.0 (13)O2ii—Pr1—Na129.7 (3)
O26ii—Na1—Pr180.0 (12)O6—Pr1—Na163.7 (4)
O26i—Na1—Pr178.6 (14)O9—Pr1—Na1119.8 (3)
Pr1i—Na1—Pr1108.75 (14)O10—Pr1—Na185.4 (3)
O2i—Na1—Pr1ii31.7 (3)N1ii—Pr1—Na193.1 (3)
O2ii—Na1—Pr1ii77.1 (3)O8—Pr1—Na1133.7 (3)
O2—Na1—Pr1ii121.4 (4)O7—Pr1—Na177.4 (3)
O26—Na1—Pr1ii78.6 (14)O22—Si1—O22i110.0 (4)
O26ii—Na1—Pr1ii165.0 (13)O22—Si1—O22ii110.0 (4)
O26i—Na1—Pr1ii80.0 (12)O22i—Si1—O22ii110.0 (4)
Pr1i—Na1—Pr1ii108.75 (14)O22—Si1—O23108.9 (4)
Pr1—Na1—Pr1ii108.75 (14)O22i—Si1—O23108.9 (4)
O10—W1—O14101.6 (4)O22ii—Si1—O23108.9 (4)
O10—W1—O1598.3 (4)C1—O1—Pr1148.2 (10)
O14—W1—O1592.6 (4)C1—O2—Na1118.2 (10)
O10—W1—O1699.4 (4)C1—O2—Pr1i122.8 (10)
O14—W1—O16158.7 (4)Na1—O2—Pr1i118.7 (5)
O15—W1—O1687.9 (4)C7—O3—Pr1i126.1 (9)
O10—W1—O14ii102.5 (4)C4—O5—H5108.1
O14—W1—O14ii86.4 (5)Pr1—O6—H6A109.1
O15—W1—O14ii159.0 (4)Pr1—O6—H6B109.3
O16—W1—O14ii85.6 (4)H6A—O6—H6B109.5
O10—W1—O22i169.9 (4)Pr1—O7—H7A109.0
O14—W1—O22i86.3 (3)Pr1—O7—H7B109.5
O15—W1—O22i75.0 (3)H7A—O7—H7B109.5
O16—W1—O22i73.2 (3)Pr1—O8—H8A109.5
O14ii—W1—O22i84.0 (3)Pr1—O8—H8B109.2
O11—W2—O17101.7 (4)H8A—O8—H8B109.5
O11—W2—O18100.7 (5)Pr1—O9—H9A109.4
O17—W2—O1886.8 (4)Pr1—O9—H9B109.3
O11—W2—O16101.3 (5)H9A—O9—H9B109.5
O17—W2—O1692.3 (4)W1—O10—Pr1165.8 (5)
O18—W2—O16157.7 (4)W1—O14—W1i150.4 (5)
O11—W2—O21i99.9 (4)W1—O15—W3i120.7 (5)
O17—W2—O21i158.2 (4)W2—O16—W1121.2 (5)
O18—W2—O21i86.6 (4)W2—O17—W3151.8 (5)
O16—W2—O21i86.1 (4)W4—O18—W2151.4 (6)
O11—W2—O22i171.1 (4)W3—O19—W4153.0 (5)
O17—W2—O22i85.9 (4)W4ii—O20—W4121.9 (5)
O18—W2—O22i84.3 (4)W3—O21—W2ii122.2 (5)
O16—W2—O22i73.4 (4)Si1—O22—W1ii123.8 (5)
O21i—W2—O22i72.8 (3)Si1—O22—W2ii123.7 (4)
O13—W3—O21102.2 (5)W1ii—O22—W2ii92.2 (3)
O13—W3—O19103.0 (4)Si1—O22—W3124.6 (5)
O21—W3—O1992.8 (4)W1ii—O22—W391.1 (3)
O13—W3—O17102.4 (4)W2ii—O22—W391.9 (3)
O21—W3—O17155.2 (4)Si1—O23—W4124.7 (3)
O19—W3—O1785.0 (4)Si1—O23—W4ii124.7 (3)
O13—W3—O15ii98.8 (4)W4—O23—W4ii90.9 (4)
O21—W3—O15ii87.6 (4)Si1—O23—W4i124.7 (3)
O19—W3—O15ii157.6 (4)W4—O23—W4i90.9 (4)
O17—W3—O15ii85.3 (4)W4ii—O23—W4i90.9 (4)
O13—W3—O22170.7 (4)C2—N1—C6119.9 (13)
O21—W3—O2273.2 (3)C2—N1—Pr1i120.3 (10)
O19—W3—O2285.5 (4)C6—N1—Pr1i119.6 (10)
O17—W3—O2282.0 (3)O1—C1—O2122.7 (15)
O15ii—W3—O2273.2 (3)O1—C1—C2120.6 (15)
O12—W4—O18101.7 (5)O2—C1—C2116.7 (15)
O12—W4—O20i100.7 (5)N1—C2—C3123.9 (14)
O18—W4—O20i90.7 (4)N1—C2—C1114.5 (14)
O12—W4—O20100.9 (5)C3—C2—C1121.6 (14)
O18—W4—O20157.2 (4)C4—C3—C2116.6 (15)
O20i—W4—O2088.7 (6)C4—C3—H3121.7
O12—W4—O19101.6 (4)C2—C3—H3121.7
O18—W4—O1984.7 (4)O5—C4—C5119.5 (15)
O20i—W4—O19157.7 (4)O5—C4—C3120.5 (16)
O20—W4—O1987.2 (4)C5—C4—C3119.8 (15)
O12—W4—O23171.9 (5)C4—C5—C6120.5 (14)
O18—W4—O2384.4 (4)C4—C5—H5A119.8
O20i—W4—O2373.6 (4)C6—C5—H5A119.8
O20—W4—O2373.6 (4)N1—C6—C5119.3 (14)
O19—W4—O2384.2 (4)N1—C6—C7115.9 (13)
O1—Pr1—O3ii131.7 (4)C5—C6—C7124.7 (13)
O1—Pr1—O2ii75.1 (4)O4—C7—O3126.4 (14)
O3ii—Pr1—O2ii125.7 (4)O4—C7—C6118.6 (13)
O1—Pr1—O673.0 (4)O3—C7—C6115.0 (13)
O3ii—Pr1—O6141.3 (4)H24A—O24—H24B109.5
O2ii—Pr1—O685.6 (4)Na1—O26—H26A101.6
O1—Pr1—O969.7 (4)Na1—O26—H26B120.6
O3ii—Pr1—O976.4 (4)H26A—O26—H26B91.2
O2ii—Pr1—O9144.2 (4)H27A—O27—H27B109.5
O6—Pr1—O990.4 (4)H28A—O28—H28B109.5
O1—Pr1—O1068.9 (3)H29A—O29—H29B109.5
O3ii—Pr1—O1074.7 (3)H29C—O29A—H29D109.5
O2ii—Pr1—O1076.6 (3)H29E—O29B—H29F109.5
O6—Pr1—O10140.9 (4)
O14—W1—O10—Pr1127 (2)O22i—Si1—O23—W458.5 (3)
O15—W1—O10—Pr1138 (2)O22ii—Si1—O23—W4178.5 (3)
O16—W1—O10—Pr149 (2)O22—Si1—O23—W4ii58.5 (3)
O14ii—W1—O10—Pr139 (2)O22i—Si1—O23—W4ii178.5 (3)
O22i—W1—O10—Pr191 (3)O22ii—Si1—O23—W4ii61.5 (3)
O10—W1—O14—W1i131.2 (10)O22—Si1—O23—W4i178.5 (3)
O15—W1—O14—W1i129.8 (10)O22i—Si1—O23—W4i61.5 (3)
O16—W1—O14—W1i39.1 (17)O22ii—Si1—O23—W4i58.5 (3)
O14ii—W1—O14—W1i29.2 (11)Pr1—O1—C1—O278 (3)
O22i—W1—O14—W1i55.0 (10)Pr1—O1—C1—C2103 (2)
O11—W2—O17—W3123.6 (11)Na1—O2—C1—O113 (2)
O18—W2—O17—W323.4 (11)Pr1i—O2—C1—O1160.3 (11)
O16—W2—O17—W3134.3 (11)Na1—O2—C1—C2168.4 (10)
O21i—W2—O17—W349.0 (18)Pr1i—O2—C1—C218.4 (18)
O22i—W2—O17—W361.1 (11)C6—N1—C2—C31 (2)
O12—W4—O18—W2127.5 (12)Pr1i—N1—C2—C3174.0 (11)
O20i—W4—O18—W2131.4 (12)C6—N1—C2—C1178.7 (12)
O20—W4—O18—W242.9 (19)Pr1i—N1—C2—C13.9 (16)
O19—W4—O18—W226.7 (12)O1—C1—C2—N1164.6 (13)
O23—W4—O18—W257.9 (11)O2—C1—C2—N114.1 (19)
O13—W3—O19—W4130.1 (13)O1—C1—C2—C317 (2)
O21—W3—O19—W4126.7 (13)O2—C1—C2—C3163.8 (14)
O17—W3—O19—W428.6 (12)N1—C2—C3—C41 (2)
O15ii—W3—O19—W436 (2)C1—C2—C3—C4178.3 (13)
O22—W3—O19—W453.8 (12)C2—C3—C4—O5176.9 (13)
O13—W3—O21—W2ii171.8 (5)C2—C3—C4—C51 (2)
O19—W3—O21—W2ii84.3 (6)O5—C4—C5—C6177.3 (14)
O17—W3—O21—W2ii0.2 (13)C3—C4—C5—C61 (2)
O15ii—W3—O21—W2ii73.3 (5)C2—N1—C6—C51 (2)
O22—W3—O21—W2ii0.1 (4)Pr1i—N1—C6—C5173.7 (10)
O22i—Si1—O22—W1ii58.1 (6)C2—N1—C6—C7176.7 (12)
O22ii—Si1—O22—W1ii63.2 (6)Pr1i—N1—C6—C71.9 (15)
O23—Si1—O22—W1ii177.4 (3)C4—C5—C6—N11 (2)
O22i—Si1—O22—W2ii178.2 (3)C4—C5—C6—C7176.4 (13)
O22ii—Si1—O22—W2ii56.9 (9)Pr1i—O3—C7—O4173.4 (11)
O23—Si1—O22—W2ii62.4 (5)Pr1i—O3—C7—C69.0 (16)
O22i—Si1—O22—W361.3 (9)N1—C6—C7—O4175.5 (13)
O22ii—Si1—O22—W3177.5 (4)C5—C6—C7—O49 (2)
O23—Si1—O22—W358.1 (5)N1—C6—C7—O36.6 (17)
O22—Si1—O23—W461.5 (3)C5—C6—C7—O3168.6 (13)
Symmetry codes: (i) y+1, xy+1, z; (ii) x+y, x+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H6A···O26ii0.872.122.91 (6)151
O7—H7A···O11iii0.872.363.084 (17)141
O7—H7A···O21iv0.872.292.988 (18)138
O7—H7B···O4v0.872.162.956 (19)152
O8—H8A···O12vi0.872.172.929 (15)146
O8—H8B···O4v0.872.403.103 (17)138
O9—H9A···O29Bii0.872.503.09 (4)123
C5—H5A···O290.952.643.28 (3)126
O24—H24A···O11vii0.872.483.109 (19)130
O26—H26A···O7ii0.872.233.10 (6)180
O26—H26B···O27viii0.871.972.84 (6)179
O27—H27A···O240.872.422.94 (3)120
O27—H27B···O29B0.871.792.51 (4)138
O28—H28A···O70.872.092.75 (3)132
O29—H29A···O11i0.872.593.18 (3)127
O29A—H29C···O5ix0.871.962.83 (4)180
O29A—H29D···O24x0.871.912.78 (4)175
O29B—H29F···O12xi0.872.273.03 (4)146
Symmetry codes: (i) y+1, xy+1, z; (ii) x+y, x+1, z; (iii) y+1/3, xy+2/3, z1/3; (iv) x+y2/3, x+2/3, z1/3; (v) x2/3, y1/3, z1/3; (vi) x+y1/3, x+1/3, z2/3; (vii) x+y+1/3, x+2/3, z1/3; (viii) x+y+1/3, x+5/3, z1/3; (ix) x+1/3, y+2/3, z1/3; (x) x+y+1, x+2, z; (xi) x+2/3, y+1/3, z2/3.
Selected bond lengths (Å) for 1 and 2 top
Compound 1Compound 2
Dy1—O15i2.306 (10)Pr1—O12.407 (11)
Dy1—O132.375 (11)Pr1—O3ii2.468 (10)
Dy1—O172.329 (11)Pr1—O2ii2.477 (11)
Dy1—O202.379 (13)Pr1—O62.496 (13)
Dy1—O162.374 (11)Pr1—O92.509 (12)
Dy1—N12.469 (13)Pr1—O102.554 (9)
Dy1—N22.482 (14)Pr1—N1ii2.567 (12)
Dy1—O192.364 (12)Pr1—O82.567 (11)
Pr1—O72.593 (12)
Symmetry codes: (i) -y+1, x-y+1, z; (ii) -x+y, -x+1, z.
 

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