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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
CCDC references: 1842658; 1842657
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)]·12H2O | Dx = 3.353 Mg m−3 |
Mr = 4527.40 | Cu Kα radiation, λ = 1.54184 Å |
Trigonal, R3 | Cell parameters from 11603 reflections |
a = 20.3334 (3) Å | θ = 4.3–76.8° |
c = 18.7836 (3) Å | µ = 41.93 mm−1 |
V = 6725.60 (19) Å3 | T = 130 K |
Z = 3 | Block, yellow |
F(000) = 6033 | 0.07 × 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 Source | 5450 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.030 |
Detector resolution: 10.2273 pixels mm-1 | θmax = 77.1°, θmin = 3.4° |
ω scans | h = −25→25 |
Absorption correction: gaussian (CrysAlis PRO; Rigaku OD, 2015) | k = −25→22 |
Tmin = 0.097, Tmax = 0.369 | l = −17→23 |
16672 measured reflections | |
Refinement top
Refinement on F2 | H-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) = 0.098 | Δρmax = 1.53 e Å−3 |
S = 1.02 | Δρmin = −1.89 e Å−3 |
5475 reflections | Extinction correction: SHELXL2014 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
426 parameters | Extinction coefficient: 0.000018 (3) |
1 restraint | Absolute structure: Classical Flack method preferred over Parsons because s.u. lower |
Primary atom site location: dual | Absolute 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
W4 | 0.44911 (3) | 0.69357 (3) | 0.56892 (4) | 0.01497 (17) | |
W1 | 0.41288 (4) | 0.77239 (4) | 0.87226 (4) | 0.01785 (18) | |
W2 | 0.52603 (4) | 0.80714 (4) | 0.70932 (4) | 0.01734 (18) | |
W3 | 0.48229 (4) | 0.62447 (4) | 0.71593 (4) | 0.02049 (19) | |
Dy1 | 0.51195 (5) | 0.65952 (5) | 0.37516 (5) | 0.0164 (2) | |
Si1 | 0.3333 | 0.6667 | 0.7162 (4) | 0.0118 (11) | |
Na1 | 0.3333 | 0.6667 | 0.2727 (9) | 0.043 (3) | |
O3 | 0.4885 (6) | 0.7885 (6) | 0.8053 (6) | 0.017 (2) | |
O8 | 0.5293 (6) | 0.7869 (5) | 0.6112 (6) | 0.0158 (19) | |
O12 | 0.4913 (6) | 0.6406 (6) | 0.6149 (6) | 0.016 (2) | |
O11 | 0.4427 (5) | 0.6170 (6) | 0.8083 (6) | 0.017 (2) | |
O6 | 0.6133 (6) | 0.8872 (6) | 0.7191 (7) | 0.021 (2) | |
O7 | 0.5555 (5) | 0.7296 (6) | 0.7265 (6) | 0.017 (2) | |
O2 | 0.4173 (6) | 0.6883 (6) | 0.9140 (6) | 0.017 (2) | |
O1 | 0.4622 (7) | 0.8404 (7) | 0.9358 (6) | 0.024 (2) | |
O15 | 0.2638 (6) | 0.4988 (7) | 0.3514 (7) | 0.024 (2) | |
O10 | 0.5381 (6) | 0.5854 (6) | 0.7255 (6) | 0.020 (2) | |
C10 | 0.5397 (10) | 0.5640 (10) | 0.5073 (9) | 0.024 (3) | |
O13 | 0.4852 (6) | 0.7001 (6) | 0.4845 (6) | 0.018 (2) | |
O17 | 0.6409 (6) | 0.7464 (6) | 0.3883 (8) | 0.030 (3) | |
O20 | 0.5127 (8) | 0.6757 (8) | 0.2497 (7) | 0.033 (3) | |
C9 | 0.5742 (12) | 0.5423 (11) | 0.5605 (11) | 0.031 (4) | |
O21 | 0.3066 (8) | 0.5641 (8) | 0.1948 (9) | 0.038 (3) | |
O16 | 0.3803 (6) | 0.5977 (7) | 0.3480 (7) | 0.022 (2) | |
N1 | 0.4311 (7) | 0.5416 (7) | 0.4422 (7) | 0.017 (2) | |
O9 | 0.4179 (5) | 0.6902 (5) | 0.6868 (5) | 0.0102 (17) | |
C1 | 0.3314 (8) | 0.5341 (8) | 0.3712 (8) | 0.017 (3) | |
C4 | 0.3389 (10) | 0.4085 (9) | 0.5160 (10) | 0.026 (3) | |
H4 | 0.3069 | 0.3627 | 0.5409 | 0.031* | |
C6 | 0.4613 (9) | 0.5179 (8) | 0.4940 (9) | 0.018 (3) | |
C2 | 0.3576 (8) | 0.5003 (9) | 0.4272 (9) | 0.019 (3) | |
C8 | 0.5273 (12) | 0.4744 (12) | 0.5997 (11) | 0.033 (4) | |
H8 | 0.5501 | 0.4596 | 0.6357 | 0.040* | |
O18 | 0.7546 (9) | 0.7895 (10) | 0.4416 (16) | 0.081 (8) | |
C12 | 0.6903 (10) | 0.6552 (12) | 0.5338 (11) | 0.034 (4) | |
H12 | 0.7430 | 0.6887 | 0.5413 | 0.041* | |
C13 | 0.6505 (9) | 0.6725 (9) | 0.4802 (11) | 0.027 (4) | |
C3 | 0.3093 (10) | 0.4326 (10) | 0.4634 (11) | 0.029 (4) | |
H3 | 0.2570 | 0.4039 | 0.4516 | 0.035* | |
N2 | 0.5771 (7) | 0.6266 (7) | 0.4684 (8) | 0.020 (3) | |
C5 | 0.4156 (11) | 0.4509 (10) | 0.5333 (12) | 0.030 (4) | |
C11 | 0.6533 (12) | 0.5922 (13) | 0.5729 (11) | 0.036 (5) | |
H11 | 0.6792 | 0.5807 | 0.6085 | 0.043* | |
C7 | 0.4529 (13) | 0.4307 (11) | 0.5880 (11) | 0.035 (4) | |
H7 | 0.4241 | 0.3862 | 0.6157 | 0.041* | |
C14 | 0.6855 (10) | 0.7409 (10) | 0.4339 (14) | 0.038 (5) | |
O4 | 0.3333 | 0.6667 | 0.8022 (9) | 0.011 (3) | |
O14 | 0.3542 (5) | 0.6058 (6) | 0.5595 (6) | 0.017 (2) | |
O5 | 0.4639 (6) | 0.8485 (6) | 0.6953 (6) | 0.016 (2) | |
O19 | 0.5444 (8) | 0.5750 (7) | 0.3202 (8) | 0.033 (3) | |
O25 | 0.9043 (12) | 0.8861 (17) | 0.3944 (13) | 0.097 (10) | |
O23 | 0.440 (2) | 0.5157 (19) | 0.207 (2) | 0.135 (15) | |
O26 | 0.7339 (19) | 0.992 (3) | 0.622 (2) | 0.066 (11) | 0.5 |
O28 | 0.525 (2) | 1.000 (2) | 0.950 (2) | 0.058 (9)* | 0.5 |
O27 | 0.578 (2) | 1.010 (2) | 0.775 (2) | 0.061 (9)* | 0.5 |
O22 | 0.3333 | 0.6667 | 0.126 (3) | 0.050 (13)* | 0.5 |
O24 | 0.362 (3) | 0.473 (3) | 0.083 (2) | 0.087 (16) | 0.5 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
W4 | 0.0123 (3) | 0.0143 (3) | 0.0178 (4) | 0.0062 (2) | 0.0011 (2) | −0.0014 (2) |
W1 | 0.0173 (3) | 0.0159 (3) | 0.0187 (4) | 0.0071 (2) | −0.0012 (2) | −0.0036 (2) |
W2 | 0.0118 (3) | 0.0150 (3) | 0.0229 (4) | 0.0049 (2) | −0.0009 (2) | −0.0024 (2) |
W3 | 0.0175 (3) | 0.0197 (3) | 0.0263 (4) | 0.0108 (3) | −0.0022 (3) | −0.0013 (3) |
Dy1 | 0.0146 (4) | 0.0155 (4) | 0.0208 (5) | 0.0089 (3) | 0.0030 (3) | 0.0004 (3) |
Si1 | 0.0097 (15) | 0.0097 (15) | 0.016 (3) | 0.0048 (8) | 0.000 | 0.000 |
Na1 | 0.040 (5) | 0.040 (5) | 0.050 (9) | 0.020 (2) | 0.000 | 0.000 |
O3 | 0.017 (5) | 0.019 (5) | 0.014 (5) | 0.008 (4) | −0.002 (4) | 0.001 (4) |
O8 | 0.016 (5) | 0.010 (4) | 0.019 (5) | 0.005 (4) | −0.001 (4) | 0.002 (4) |
O12 | 0.016 (5) | 0.018 (5) | 0.019 (6) | 0.012 (4) | −0.005 (4) | −0.005 (4) |
O11 | 0.011 (4) | 0.018 (5) | 0.016 (5) | 0.004 (4) | 0.001 (4) | 0.003 (4) |
O6 | 0.009 (4) | 0.019 (5) | 0.032 (6) | 0.005 (4) | 0.002 (4) | −0.001 (4) |
O7 | 0.011 (4) | 0.013 (5) | 0.020 (5) | 0.001 (4) | −0.002 (4) | −0.001 (4) |
O2 | 0.015 (4) | 0.017 (5) | 0.019 (6) | 0.008 (4) | 0.002 (4) | 0.003 (4) |
O1 | 0.029 (6) | 0.025 (6) | 0.017 (6) | 0.013 (5) | 0.000 (4) | −0.003 (4) |
O15 | 0.014 (5) | 0.031 (6) | 0.027 (6) | 0.011 (4) | −0.001 (4) | −0.008 (5) |
O10 | 0.017 (5) | 0.025 (5) | 0.019 (5) | 0.012 (4) | −0.001 (4) | −0.003 (4) |
C10 | 0.028 (8) | 0.033 (8) | 0.018 (8) | 0.021 (7) | −0.006 (6) | −0.013 (6) |
O13 | 0.015 (5) | 0.019 (5) | 0.019 (6) | 0.008 (4) | −0.003 (4) | −0.003 (4) |
O17 | 0.015 (5) | 0.020 (6) | 0.051 (8) | 0.005 (4) | 0.005 (5) | 0.002 (5) |
O20 | 0.042 (7) | 0.048 (8) | 0.021 (7) | 0.031 (7) | 0.005 (5) | 0.004 (5) |
C9 | 0.044 (11) | 0.032 (9) | 0.026 (9) | 0.026 (8) | 0.002 (8) | 0.001 (7) |
O21 | 0.034 (7) | 0.035 (7) | 0.046 (9) | 0.017 (6) | 0.010 (6) | 0.004 (6) |
O16 | 0.013 (5) | 0.027 (6) | 0.026 (6) | 0.010 (4) | −0.005 (4) | −0.002 (5) |
N1 | 0.020 (6) | 0.016 (5) | 0.019 (6) | 0.013 (5) | 0.001 (5) | −0.007 (5) |
O9 | 0.012 (4) | 0.007 (4) | 0.011 (5) | 0.004 (3) | −0.003 (3) | −0.002 (3) |
C1 | 0.020 (7) | 0.021 (7) | 0.013 (7) | 0.014 (6) | −0.002 (5) | −0.003 (5) |
C4 | 0.027 (8) | 0.015 (7) | 0.030 (9) | 0.007 (6) | 0.008 (7) | 0.007 (6) |
C6 | 0.021 (7) | 0.019 (7) | 0.019 (8) | 0.014 (6) | 0.003 (6) | −0.005 (5) |
C2 | 0.018 (7) | 0.022 (7) | 0.017 (8) | 0.010 (6) | 0.008 (5) | −0.003 (6) |
C8 | 0.048 (11) | 0.046 (11) | 0.027 (9) | 0.040 (10) | 0.006 (8) | 0.014 (8) |
O18 | 0.018 (7) | 0.035 (9) | 0.17 (3) | −0.001 (6) | −0.006 (10) | 0.017 (12) |
C12 | 0.023 (8) | 0.044 (11) | 0.033 (11) | 0.015 (8) | −0.017 (7) | −0.013 (8) |
C13 | 0.015 (7) | 0.018 (7) | 0.045 (11) | 0.006 (6) | −0.007 (7) | −0.010 (7) |
C3 | 0.028 (8) | 0.020 (7) | 0.039 (11) | 0.011 (7) | 0.001 (7) | 0.000 (7) |
N2 | 0.019 (6) | 0.024 (6) | 0.025 (7) | 0.016 (5) | 0.001 (5) | −0.006 (5) |
C5 | 0.033 (9) | 0.019 (7) | 0.044 (11) | 0.017 (7) | 0.004 (8) | 0.000 (7) |
C11 | 0.038 (10) | 0.053 (12) | 0.032 (10) | 0.033 (9) | −0.016 (8) | −0.017 (9) |
C7 | 0.054 (12) | 0.026 (8) | 0.028 (10) | 0.024 (9) | 0.000 (8) | 0.005 (7) |
C14 | 0.019 (8) | 0.018 (8) | 0.076 (16) | 0.009 (7) | −0.011 (8) | −0.008 (8) |
O4 | 0.011 (4) | 0.011 (4) | 0.011 (8) | 0.005 (2) | 0.000 | 0.000 |
O14 | 0.013 (4) | 0.016 (5) | 0.021 (6) | 0.007 (4) | −0.005 (4) | −0.003 (4) |
O5 | 0.017 (5) | 0.015 (5) | 0.016 (5) | 0.009 (4) | 0.003 (4) | −0.003 (4) |
O19 | 0.053 (8) | 0.025 (6) | 0.036 (8) | 0.030 (6) | 0.018 (6) | 0.010 (5) |
O25 | 0.045 (11) | 0.14 (2) | 0.048 (14) | 0.000 (12) | −0.003 (9) | 0.015 (13) |
O23 | 0.18 (4) | 0.11 (2) | 0.16 (4) | 0.11 (3) | −0.08 (3) | −0.07 (2) |
O26 | 0.030 (16) | 0.09 (3) | 0.06 (2) | 0.016 (17) | −0.015 (15) | −0.02 (2) |
O24 | 0.11 (4) | 0.11 (4) | 0.04 (2) | 0.06 (3) | 0.00 (2) | 0.04 (2) |
Geometric parameters (Å, º) top
W4—O8 | 1.949 (10) | Na1—O21ii | 2.378 (18) |
W4—O12 | 1.888 (10) | Na1—O21i | 2.378 (18) |
W4—O13 | 1.725 (11) | Na1—O21 | 2.378 (18) |
W4—O9 | 2.296 (10) | Na1—O16i | 2.494 (15) |
W4—O14i | 1.940 (10) | Na1—O16 | 2.494 (15) |
W4—O14 | 1.870 (10) | Na1—O16ii | 2.494 (15) |
W1—O3 | 1.884 (11) | Na1—O22 | 2.76 (7) |
W1—O11i | 1.909 (10) | O11—W1ii | 1.909 (10) |
W1—O2i | 1.952 (10) | O2—W1ii | 1.952 (10) |
W1—O2 | 1.924 (10) | O15—Dy1ii | 2.306 (10) |
W1—O1 | 1.719 (11) | O15—C1 | 1.247 (19) |
W1—O4 | 2.343 (10) | C10—C9 | 1.41 (3) |
W2—O3 | 1.921 (11) | C10—C6 | 1.41 (2) |
W2—O8 | 1.896 (11) | C10—N2 | 1.33 (2) |
W2—O6 | 1.716 (10) | O17—C14 | 1.29 (2) |
W2—O7 | 1.974 (11) | C9—C8 | 1.43 (3) |
W2—O9 | 2.332 (9) | C9—C11 | 1.43 (3) |
W2—O5 | 1.853 (10) | O16—C1 | 1.25 (2) |
W3—O12 | 1.919 (11) | N1—C6 | 1.36 (2) |
W3—O11 | 1.886 (11) | N1—C2 | 1.33 (2) |
W3—O7 | 1.908 (10) | C1—C2 | 1.49 (2) |
W3—O10 | 1.689 (11) | C4—C3 | 1.37 (3) |
W3—O9 | 2.356 (9) | C4—C5 | 1.39 (3) |
W3—O5ii | 1.938 (10) | C6—C5 | 1.41 (2) |
Dy1—O15i | 2.306 (10) | C2—C3 | 1.40 (2) |
Dy1—O13 | 2.375 (11) | C8—C7 | 1.34 (3) |
Dy1—O17 | 2.329 (11) | O18—C14 | 1.26 (2) |
Dy1—O20 | 2.379 (13) | C12—C13 | 1.44 (3) |
Dy1—O16 | 2.374 (11) | C12—C11 | 1.34 (3) |
Dy1—N1 | 2.469 (13) | C13—N2 | 1.32 (2) |
Dy1—N2 | 2.482 (14) | C13—C14 | 1.48 (3) |
Dy1—O19 | 2.364 (12) | C5—C7 | 1.45 (3) |
Si1—O9 | 1.633 (10) | O4—W1i | 2.343 (10) |
Si1—O9ii | 1.633 (10) | O4—W1ii | 2.343 (10) |
Si1—O9i | 1.633 (10) | O14—W4ii | 1.940 (10) |
Si1—O4 | 1.615 (19) | O5—W3i | 1.938 (10) |
| | | |
O8—W4—O9 | 73.7 (4) | O9i—Si1—O9 | 109.2 (4) |
O12—W4—O8 | 88.4 (4) | O9ii—Si1—O9 | 109.2 (4) |
O12—W4—O9 | 74.9 (4) | O4—Si1—O9ii | 109.8 (4) |
O12—W4—O14i | 157.7 (5) | O4—Si1—O9 | 109.8 (4) |
O13—W4—O8 | 100.6 (5) | O4—Si1—O9i | 109.8 (4) |
O13—W4—O12 | 99.6 (5) | O21ii—Na1—O21i | 86.1 (7) |
O13—W4—O9 | 172.0 (4) | O21ii—Na1—O21 | 86.1 (7) |
O13—W4—O14i | 102.6 (5) | O21i—Na1—O21 | 86.1 (7) |
O13—W4—O14 | 100.6 (5) | O21—Na1—O16ii | 104.8 (4) |
O14—W4—O8 | 158.4 (5) | O21—Na1—O16i | 162.2 (4) |
O14i—W4—O8 | 85.4 (4) | O21—Na1—O16 | 80.8 (5) |
O14—W4—O12 | 92.6 (5) | O21i—Na1—O16ii | 162.2 (4) |
O14i—W4—O9 | 82.8 (4) | O21i—Na1—O16 | 104.8 (4) |
O14—W4—O9 | 85.7 (4) | O21i—Na1—O16i | 80.8 (5) |
O14—W4—O14i | 85.6 (6) | O21ii—Na1—O16 | 162.2 (4) |
O3—W1—O11i | 86.9 (5) | O21ii—Na1—O16i | 104.8 (4) |
O3—W1—O2i | 158.6 (4) | O21ii—Na1—O16ii | 80.8 (5) |
O3—W1—O2 | 91.7 (4) | O21—Na1—O22 | 52.0 (5) |
O3—W1—O4 | 85.1 (4) | O21i—Na1—O22 | 52.0 (5) |
O11i—W1—O2i | 86.9 (4) | O21ii—Na1—O22 | 52.0 (5) |
O11i—W1—O2 | 158.5 (5) | O16i—Na1—O16 | 91.0 (6) |
O11i—W1—O4 | 84.1 (4) | O16ii—Na1—O16 | 91.0 (6) |
O2—W1—O2i | 86.7 (6) | O16ii—Na1—O16i | 91.0 (6) |
O2—W1—O4 | 74.4 (4) | O16ii—Na1—O22 | 124.5 (4) |
O2i—W1—O4 | 73.9 (4) | O16i—Na1—O22 | 124.5 (4) |
O1—W1—O3 | 103.1 (5) | O16—Na1—O22 | 124.5 (4) |
O1—W1—O11i | 101.7 (5) | W1—O3—W2 | 150.5 (6) |
O1—W1—O2 | 99.5 (5) | W2—O8—W4 | 120.3 (5) |
O1—W1—O2i | 98.2 (5) | W4—O12—W3 | 121.2 (5) |
O1—W1—O4 | 170.1 (5) | W3—O11—W1ii | 151.5 (6) |
O3—W2—O7 | 86.4 (5) | W3—O7—W2 | 120.0 (5) |
O3—W2—O9 | 83.7 (4) | W1—O2—W1ii | 120.1 (6) |
O8—W2—O3 | 157.4 (4) | C1—O15—Dy1ii | 141.1 (10) |
O8—W2—O7 | 85.9 (4) | C6—C10—C9 | 119.4 (17) |
O8—W2—O9 | 73.8 (4) | N2—C10—C9 | 123.5 (16) |
O6—W2—O3 | 101.9 (5) | N2—C10—C6 | 117.1 (15) |
O6—W2—O8 | 100.3 (5) | W4—O13—Dy1 | 158.6 (6) |
O6—W2—O7 | 99.0 (5) | C14—O17—Dy1 | 125.2 (11) |
O6—W2—O9 | 170.9 (4) | C10—C9—C8 | 118.1 (18) |
O6—W2—O5 | 101.6 (5) | C10—C9—C11 | 116.9 (18) |
O7—W2—O9 | 73.9 (4) | C11—C9—C8 | 125.0 (19) |
O5—W2—O3 | 86.0 (5) | Dy1—O16—Na1 | 118.1 (5) |
O5—W2—O8 | 93.8 (4) | C1—O16—Dy1 | 125.2 (10) |
O5—W2—O7 | 159.1 (4) | C1—O16—Na1 | 116.6 (9) |
O5—W2—O9 | 85.9 (4) | C6—N1—Dy1 | 120.7 (10) |
O12—W3—O9 | 72.9 (4) | C2—N1—Dy1 | 119.8 (11) |
O12—W3—O5ii | 85.8 (5) | C2—N1—C6 | 119.5 (13) |
O11—W3—O12 | 157.5 (4) | W4—O9—W2 | 92.2 (3) |
O11—W3—O7 | 93.3 (5) | W4—O9—W3 | 91.0 (3) |
O11—W3—O9 | 85.6 (4) | W2—O9—W3 | 91.6 (3) |
O11—W3—O5ii | 84.9 (4) | Si1—O9—W4 | 124.8 (6) |
O7—W3—O12 | 87.5 (5) | Si1—O9—W2 | 123.7 (5) |
O7—W3—O9 | 74.5 (4) | Si1—O9—W3 | 123.9 (5) |
O7—W3—O5ii | 157.4 (4) | O15—C1—O16 | 124.7 (14) |
O10—W3—O12 | 99.0 (5) | O15—C1—C2 | 119.4 (14) |
O10—W3—O11 | 103.0 (5) | O16—C1—C2 | 116.0 (13) |
O10—W3—O7 | 100.6 (5) | C3—C4—C5 | 120.2 (16) |
O10—W3—O9 | 170.5 (5) | C10—C6—C5 | 121.8 (16) |
O10—W3—O5ii | 101.7 (5) | N1—C6—C10 | 116.8 (15) |
O5ii—W3—O9 | 82.9 (4) | N1—C6—C5 | 121.3 (15) |
O15i—Dy1—O13 | 72.5 (4) | N1—C2—C1 | 114.1 (14) |
O15i—Dy1—O17 | 84.8 (4) | N1—C2—C3 | 122.0 (16) |
O15i—Dy1—O20 | 71.1 (5) | C3—C2—C1 | 123.9 (15) |
O15i—Dy1—O16 | 81.1 (4) | C7—C8—C9 | 123.0 (17) |
O15i—Dy1—N1 | 132.5 (4) | C11—C12—C13 | 120.2 (16) |
O15i—Dy1—N2 | 134.4 (4) | C12—C13—C14 | 124.9 (15) |
O15i—Dy1—O19 | 141.5 (4) | N2—C13—C12 | 121.1 (17) |
O13—Dy1—O20 | 142.7 (4) | N2—C13—C14 | 114.0 (16) |
O13—Dy1—N1 | 74.9 (4) | C4—C3—C2 | 119.0 (16) |
O13—Dy1—N2 | 74.3 (4) | C10—N2—Dy1 | 121.3 (10) |
O17—Dy1—O13 | 90.6 (4) | C13—N2—Dy1 | 119.5 (12) |
O17—Dy1—O20 | 94.2 (5) | C13—N2—C10 | 119.2 (15) |
O17—Dy1—O16 | 165.4 (4) | C4—C5—C6 | 117.9 (17) |
O17—Dy1—N1 | 129.3 (5) | C4—C5—C7 | 124.8 (17) |
O17—Dy1—N2 | 65.1 (5) | C6—C5—C7 | 117.3 (17) |
O17—Dy1—O19 | 88.9 (5) | C12—C11—C9 | 119.1 (18) |
O20—Dy1—N1 | 126.5 (5) | C8—C7—C5 | 120.3 (18) |
O20—Dy1—N2 | 140.3 (4) | O17—C14—C13 | 116.1 (15) |
O16—Dy1—O13 | 88.6 (4) | O18—C14—O17 | 124 (2) |
O16—Dy1—O20 | 77.8 (4) | O18—C14—C13 | 120 (2) |
O16—Dy1—N1 | 64.4 (4) | W1i—O4—W1ii | 91.6 (5) |
O16—Dy1—N2 | 128.4 (4) | W1—O4—W1ii | 91.6 (5) |
N1—Dy1—N2 | 64.1 (4) | W1i—O4—W1 | 91.6 (5) |
O19—Dy1—O13 | 145.6 (4) | Si1—O4—W1i | 124.2 (3) |
O19—Dy1—O20 | 71.5 (5) | Si1—O4—W1 | 124.2 (3) |
O19—Dy1—O16 | 99.9 (5) | Si1—O4—W1ii | 124.2 (3) |
O19—Dy1—N1 | 79.0 (4) | W4—O14—W4ii | 151.9 (6) |
O19—Dy1—N2 | 74.4 (5) | W2—O5—W3i | 153.0 (6) |
O9i—Si1—O9ii | 109.2 (4) | | |
| | | |
Dy1ii—O15—C1—O16 | −87 (2) | O9ii—Si1—O9—W2 | 177.8 (4) |
Dy1ii—O15—C1—C2 | 92.5 (19) | O9i—Si1—O9—W2 | 58.5 (10) |
Dy1—O17—C14—O18 | −178 (2) | O9i—Si1—O9—W3 | 177.8 (4) |
Dy1—O17—C14—C13 | 1 (2) | O9ii—Si1—O9—W3 | −62.9 (10) |
Dy1—O16—C1—O15 | −172.7 (11) | O9—Si1—O4—W1i | 178.1 (3) |
Dy1—O16—C1—C2 | 8.1 (18) | O9i—Si1—O4—W1 | −61.9 (3) |
Dy1—N1—C6—C10 | 0.5 (17) | O9ii—Si1—O4—W1 | 178.1 (3) |
Dy1—N1—C6—C5 | 179.4 (12) | O9—Si1—O4—W1 | 58.1 (3) |
Dy1—N1—C2—C1 | −2.9 (16) | O9i—Si1—O4—W1ii | 178.1 (3) |
Dy1—N1—C2—C3 | 179.6 (12) | O9ii—Si1—O4—W1ii | 58.1 (3) |
Na1—O16—C1—O15 | 11 (2) | O9—Si1—O4—W1ii | −61.9 (3) |
Na1—O16—C1—C2 | −168.5 (10) | O9ii—Si1—O4—W1i | −61.9 (3) |
O3—W2—O8—W4 | 3.7 (15) | O9i—Si1—O4—W1i | 58.1 (3) |
O3—W2—O5—W3i | −27.3 (13) | C1—C2—C3—C4 | −177.1 (15) |
O8—W4—O12—W3 | 72.3 (6) | C4—C5—C7—C8 | 178.6 (19) |
O8—W4—O13—Dy1 | 145.2 (15) | C6—C10—C9—C8 | −1 (2) |
O8—W4—O14—W4ii | 39 (2) | C6—C10—C9—C11 | −178.3 (16) |
O8—W2—O5—W3i | 130.1 (13) | C6—C10—N2—Dy1 | −1.1 (19) |
O12—W4—O13—Dy1 | 55.1 (16) | C6—C10—N2—C13 | 178.4 (14) |
O12—W4—O14—W4ii | 131.1 (14) | C6—N1—C2—C1 | 178.0 (12) |
O12—W3—O11—W1ii | 40 (2) | C6—N1—C2—C3 | 0 (2) |
O11i—W1—O3—W2 | −24.7 (12) | C6—C5—C7—C8 | 0 (3) |
O6—W2—O8—W4 | 172.6 (6) | C2—N1—C6—C10 | 179.7 (13) |
O6—W2—O5—W3i | −128.6 (13) | C2—N1—C6—C5 | −1 (2) |
O7—W2—O8—W4 | 74.2 (6) | C8—C9—C11—C12 | −178 (2) |
O7—W2—O5—W3i | 42 (2) | C12—C13—N2—Dy1 | −179.8 (13) |
O7—W3—O11—W1ii | 130.9 (13) | C12—C13—N2—C10 | 1 (2) |
O2—W1—O3—W2 | 133.9 (13) | C12—C13—C14—O17 | 179.3 (18) |
O2i—W1—O3—W2 | 49 (2) | C12—C13—C14—O18 | −2 (3) |
O1—W1—O3—W2 | −125.9 (13) | C13—C12—C11—C9 | 0 (3) |
O15—C1—C2—N1 | 177.7 (13) | C3—C4—C5—C6 | −1 (3) |
O15—C1—C2—C3 | −5 (2) | C3—C4—C5—C7 | −180.0 (18) |
O10—W3—O11—W1ii | −127.4 (13) | N2—C10—C9—C8 | 178.6 (16) |
C10—C9—C8—C7 | 0 (3) | N2—C10—C9—C11 | 1 (3) |
C10—C9—C11—C12 | −1 (3) | N2—C10—C6—N1 | 0 (2) |
C10—C6—C5—C4 | −179.3 (15) | N2—C10—C6—C5 | −178.5 (15) |
C10—C6—C5—C7 | 0 (2) | N2—C13—C14—O17 | −1 (3) |
O13—W4—O12—W3 | 172.8 (6) | N2—C13—C14—O18 | 178 (2) |
O13—W4—O14—W4ii | −128.6 (14) | C5—C4—C3—C2 | 0 (3) |
C9—C10—C6—N1 | 179.9 (14) | C11—C9—C8—C7 | 177.5 (19) |
C9—C10—C6—C5 | 1 (2) | C11—C12—C13—N2 | 0 (3) |
C9—C10—N2—Dy1 | 179.4 (12) | C11—C12—C13—C14 | 179.6 (19) |
C9—C10—N2—C13 | −1 (2) | C14—C13—N2—Dy1 | 0 (2) |
C9—C8—C7—C5 | 0 (3) | C14—C13—N2—C10 | −179.3 (15) |
O16—C1—C2—N1 | −3.0 (19) | O4—W1—O3—W2 | 59.7 (12) |
O16—C1—C2—C3 | 174.5 (15) | O4—Si1—O9—W4 | 176.8 (4) |
N1—C6—C5—C4 | 2 (2) | O4—Si1—O9—W2 | −61.9 (6) |
N1—C6—C5—C7 | −179.3 (15) | O4—Si1—O9—W3 | 57.4 (6) |
N1—C2—C3—C4 | 0 (3) | O14—W4—O12—W3 | −86.1 (7) |
O9—W4—O12—W3 | −1.3 (5) | O14i—W4—O12—W3 | −1.2 (15) |
O9—W4—O14—W4ii | 56.5 (13) | O14i—W4—O13—Dy1 | −127.2 (15) |
O9—W2—O8—W4 | −0.3 (5) | O14—W4—O13—Dy1 | −39.4 (16) |
O9—W2—O5—W3i | 56.7 (13) | O14i—W4—O14—W4ii | −26.6 (16) |
O9—W3—O11—W1ii | 56.8 (13) | O5—W2—O8—W4 | −84.9 (6) |
O9i—Si1—O9—W4 | −62.8 (6) | O5ii—W3—O11—W1ii | −26.5 (13) |
O9ii—Si1—O9—W4 | 56.4 (7) | | |
Symmetry codes: (i) −y+1, x−y+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)]·12H2O | Dx = 3.601 Mg m−3 |
Mr = 4307.67 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 9882 reflections |
a = 18.119 (3) Å | θ = 2.3–29.1° |
c = 21.078 (3) Å | µ = 19.14 mm−1 |
V = 5993 (2) Å3 | T = 100 K |
Z = 3 | Column, light yellow |
F(000) = 5790 | 0.24 × 0.13 × 0.12 mm |
Data collection top
Bruker SMART APEX CCD diffractometer | 7142 independent reflections |
Radiation source: fine-focus sealed tube | 6106 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.085 |
Detector resolution: 8.3333 pixels mm-1 | θmax = 29.2°, θmin = 1.6° |
φ and ω scans | h = −24→24 |
Absorption correction: multi-scan (TWINABS; Sheldrick, 2009) | k = −24→24 |
Tmin = 0.09, Tmax = 0.22 | l = −28→28 |
74256 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.030 | H-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 reflections | Δρmax = 1.97 e Å−3 |
385 parameters | Δρmin = −2.07 e Å−3 |
241 restraints | Absolute structure: Flack x determined using 2688 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013) |
Primary atom site location: structure-invariant direct methods | Absolute 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Na1 | 0.333333 | 0.666667 | 0.2314 (5) | 0.038 (3) | |
W1 | 0.25977 (4) | 0.53062 (4) | 0.48154 (2) | 0.00999 (12) | |
W2 | 0.13249 (4) | 0.48260 (4) | 0.60810 (2) | 0.01449 (13) | |
W3 | 0.15307 (4) | 0.69539 (4) | 0.61336 (2) | 0.01467 (14) | |
W4 | 0.21000 (4) | 0.61161 (4) | 0.75405 (3) | 0.01871 (15) | |
Pr1 | 0.16948 (6) | 0.42412 (6) | 0.29909 (4) | 0.0231 (2) | |
Si1 | 0.333333 | 0.666667 | 0.6130 (3) | 0.0060 (10) | |
O1 | 0.3227 (7) | 0.4982 (7) | 0.2939 (5) | 0.025 (2) | |
O2 | 0.4232 (7) | 0.6357 (7) | 0.2907 (5) | 0.031 (3) | |
O3 | 0.6776 (7) | 0.7460 (7) | 0.3773 (5) | 0.024 (2) | |
O4 | 0.7212 (8) | 0.6804 (8) | 0.4459 (5) | 0.039 (3) | |
O5 | 0.4381 (9) | 0.4029 (8) | 0.4840 (6) | 0.042 (3) | |
H5 | 0.389837 | 0.364795 | 0.471572 | 0.063* | |
O6 | 0.2088 (10) | 0.4350 (9) | 0.1846 (6) | 0.056 (4) | |
H6A | 0.263966 | 0.464596 | 0.181036 | 0.085* | |
H6B | 0.186077 | 0.460446 | 0.164136 | 0.085* | |
O7 | 0.0718 (9) | 0.4521 (9) | 0.2250 (6) | 0.053 (4) | |
H7A | 0.019239 | 0.421080 | 0.237491 | 0.079* | |
H7B | 0.076639 | 0.438468 | 0.186281 | 0.079* | |
O8 | 0.0681 (7) | 0.2813 (7) | 0.2456 (5) | 0.032 (3) | |
H8A | 0.097665 | 0.261656 | 0.226972 | 0.047* | |
H8B | 0.037425 | 0.289026 | 0.217472 | 0.047* | |
O9 | 0.2233 (7) | 0.3224 (7) | 0.3174 (5) | 0.037 (3) | |
H9A | 0.183122 | 0.275868 | 0.334543 | 0.056* | |
H9B | 0.267011 | 0.345728 | 0.342743 | 0.056* | |
O10 | 0.2354 (6) | 0.4843 (6) | 0.4074 (4) | 0.015 (2) | |
O11 | 0.0276 (7) | 0.4063 (7) | 0.6181 (5) | 0.022 (2) | |
O12 | 0.1309 (7) | 0.5762 (7) | 0.8086 (5) | 0.025 (2) | |
O13 | 0.0551 (7) | 0.6863 (7) | 0.6217 (5) | 0.024 (2) | |
O14 | 0.3762 (5) | 0.6132 (5) | 0.4720 (4) | 0.0095 (18) | |
O15 | 0.2857 (6) | 0.4523 (6) | 0.5222 (4) | 0.015 (2) | |
O16 | 0.1485 (6) | 0.4700 (6) | 0.5200 (4) | 0.016 (2) | |
O17 | 0.1244 (6) | 0.5798 (6) | 0.5935 (4) | 0.016 (2) | |
O18 | 0.1632 (6) | 0.5225 (6) | 0.6932 (4) | 0.019 (2) | |
O19 | 0.1760 (6) | 0.6706 (6) | 0.6954 (4) | 0.018 (2) | |
O20 | 0.2894 (6) | 0.7213 (6) | 0.7886 (5) | 0.022 (2) | |
O21 | 0.2267 (6) | 0.8131 (6) | 0.6237 (4) | 0.015 (2) | |
O22 | 0.2918 (5) | 0.7230 (5) | 0.5879 (4) | 0.0076 (17) | |
O23 | 0.333333 | 0.666667 | 0.6905 (7) | 0.011 (3) | |
N1 | 0.5262 (8) | 0.6094 (7) | 0.3649 (6) | 0.020 (3) | |
C1 | 0.3930 (11) | 0.5599 (11) | 0.3123 (8) | 0.029 (4) | |
C2 | 0.4468 (10) | 0.5463 (10) | 0.3609 (7) | 0.021 (3) | |
C3 | 0.4127 (11) | 0.4739 (10) | 0.3990 (7) | 0.028 (4) | |
H3 | 0.355016 | 0.429804 | 0.395111 | 0.033* | |
C4 | 0.4670 (11) | 0.4694 (11) | 0.4427 (8) | 0.027 (4) | |
C5 | 0.5495 (10) | 0.5347 (10) | 0.4472 (7) | 0.021 (3) | |
H5A | 0.586555 | 0.531993 | 0.477771 | 0.026* | |
C6 | 0.5795 (10) | 0.6054 (10) | 0.4071 (7) | 0.017 (3) | |
C7 | 0.6672 (9) | 0.6826 (9) | 0.4105 (7) | 0.018 (3) | |
O24 | 0.8781 (10) | 0.7242 (11) | 0.3652 (7) | 0.076 (5) | |
H24A | 0.832420 | 0.675348 | 0.358365 | 0.114* | |
H24B | 0.908181 | 0.718589 | 0.394985 | 0.114* | |
O25 | 0.9855 (12) | 0.7199 (12) | 0.4581 (8) | 0.078 (5) | |
O26 | 0.419 (3) | 0.796 (3) | 0.162 (3) | 0.089 (17) | 0.333 |
H26A | 0.407985 | 0.833191 | 0.180072 | 0.133* | 0.3333 |
H26B | 0.398461 | 0.801453 | 0.126332 | 0.133* | 0.3333 |
O27 | 0.8519 (17) | 0.8712 (16) | 0.3783 (11) | 0.047 (7) | 0.5 |
H27A | 0.894064 | 0.862536 | 0.386301 | 0.071* | 0.5 |
H27B | 0.845674 | 0.872527 | 0.337500 | 0.071* | 0.5 |
O28 | 0.1006 (19) | 0.5532 (18) | 0.1200 (14) | 0.062 (8) | 0.5 |
H28A | 0.106582 | 0.552073 | 0.160863 | 0.093* | 0.5 |
H28B | 0.057832 | 0.560834 | 0.111714 | 0.093* | 0.5 |
O29 | 0.539 (2) | 0.4313 (19) | 0.5778 (13) | 0.030 (5) | 0.3822 |
H29A | 0.575381 | 0.471452 | 0.602593 | 0.045* | 0.3822 |
H29B | 0.489431 | 0.427642 | 0.581411 | 0.045* | 0.3822 |
O29A | 0.843 (2) | 1.032 (2) | 0.2569 (17) | 0.030 (5) | 0.3047 |
H29C | 0.820662 | 1.043854 | 0.224200 | 0.045* | 0.3047 |
H29D | 0.842092 | 1.061804 | 0.289391 | 0.045* | 0.3047 |
O29B | 0.860 (2) | 0.949 (2) | 0.2776 (17) | 0.030 (5) | 0.3134 |
H29E | 0.865937 | 0.999268 | 0.275746 | 0.045* | 0.3134 |
H29F | 0.858118 | 0.929738 | 0.239316 | 0.045* | 0.3134 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.051 (5) | 0.051 (5) | 0.013 (6) | 0.025 (2) | 0.000 | 0.000 |
W1 | 0.0121 (3) | 0.0115 (3) | 0.0055 (2) | 0.0051 (2) | −0.0007 (2) | −0.0016 (2) |
W2 | 0.0142 (3) | 0.0158 (3) | 0.0107 (3) | 0.0054 (3) | 0.0044 (2) | 0.0018 (2) |
W3 | 0.0154 (3) | 0.0195 (3) | 0.0107 (3) | 0.0099 (3) | 0.0037 (2) | 0.0002 (2) |
W4 | 0.0241 (3) | 0.0247 (3) | 0.0068 (3) | 0.0118 (3) | 0.0057 (2) | 0.0023 (2) |
Pr1 | 0.0280 (5) | 0.0301 (5) | 0.0095 (4) | 0.0132 (4) | −0.0055 (3) | −0.0069 (3) |
Si1 | 0.0078 (15) | 0.0078 (15) | 0.002 (2) | 0.0039 (7) | 0.000 | 0.000 |
O1 | 0.024 (5) | 0.026 (5) | 0.024 (5) | 0.011 (4) | 0.004 (4) | −0.005 (4) |
O2 | 0.033 (5) | 0.029 (5) | 0.026 (5) | 0.012 (4) | 0.001 (4) | 0.001 (4) |
O3 | 0.025 (5) | 0.025 (5) | 0.025 (5) | 0.015 (4) | −0.001 (4) | −0.003 (4) |
O4 | 0.037 (6) | 0.039 (7) | 0.029 (6) | 0.010 (5) | −0.014 (5) | 0.004 (5) |
O5 | 0.056 (8) | 0.037 (7) | 0.032 (6) | 0.023 (6) | 0.016 (6) | 0.009 (5) |
O6 | 0.061 (8) | 0.073 (9) | 0.030 (7) | 0.030 (7) | 0.003 (6) | −0.003 (6) |
O7 | 0.052 (8) | 0.060 (8) | 0.019 (6) | 0.007 (6) | −0.020 (5) | 0.007 (5) |
O8 | 0.024 (5) | 0.035 (6) | 0.035 (6) | 0.015 (5) | −0.007 (5) | −0.020 (5) |
O9 | 0.024 (6) | 0.031 (6) | 0.049 (7) | 0.008 (5) | 0.002 (5) | −0.008 (5) |
O10 | 0.012 (4) | 0.016 (4) | 0.010 (4) | 0.003 (3) | 0.001 (3) | −0.004 (3) |
O11 | 0.022 (5) | 0.024 (5) | 0.019 (5) | 0.011 (5) | 0.003 (4) | 0.001 (4) |
O12 | 0.032 (6) | 0.031 (6) | 0.014 (5) | 0.017 (5) | 0.005 (4) | 0.007 (4) |
O13 | 0.023 (5) | 0.029 (6) | 0.019 (5) | 0.012 (5) | 0.003 (4) | 0.002 (4) |
O14 | 0.014 (4) | 0.011 (4) | 0.002 (4) | 0.006 (3) | −0.001 (3) | −0.001 (3) |
O15 | 0.016 (4) | 0.014 (4) | 0.012 (4) | 0.006 (3) | 0.002 (3) | −0.001 (3) |
O16 | 0.021 (4) | 0.016 (4) | 0.011 (4) | 0.010 (4) | −0.001 (3) | −0.001 (3) |
O17 | 0.012 (4) | 0.022 (4) | 0.012 (4) | 0.008 (4) | 0.001 (3) | −0.002 (3) |
O18 | 0.020 (4) | 0.023 (5) | 0.012 (4) | 0.009 (4) | 0.003 (4) | 0.001 (4) |
O19 | 0.022 (4) | 0.019 (4) | 0.013 (4) | 0.009 (4) | 0.005 (4) | −0.003 (3) |
O20 | 0.025 (5) | 0.026 (5) | 0.015 (4) | 0.014 (4) | −0.001 (4) | −0.003 (4) |
O21 | 0.021 (4) | 0.018 (4) | 0.010 (4) | 0.013 (4) | 0.000 (3) | −0.001 (3) |
O22 | 0.008 (2) | 0.008 (2) | 0.007 (2) | 0.0039 (15) | −0.0016 (13) | 0.0004 (13) |
O23 | 0.013 (4) | 0.013 (4) | 0.005 (5) | 0.0067 (18) | 0.000 | 0.000 |
N1 | 0.028 (5) | 0.016 (5) | 0.018 (5) | 0.013 (4) | −0.003 (4) | −0.006 (4) |
C1 | 0.030 (6) | 0.030 (6) | 0.028 (6) | 0.016 (5) | 0.005 (5) | −0.008 (5) |
C2 | 0.025 (6) | 0.022 (6) | 0.018 (6) | 0.013 (5) | −0.001 (5) | −0.004 (5) |
C3 | 0.027 (6) | 0.029 (6) | 0.026 (6) | 0.013 (5) | 0.011 (5) | −0.001 (5) |
C4 | 0.030 (6) | 0.028 (6) | 0.023 (6) | 0.015 (5) | 0.014 (5) | −0.007 (5) |
C5 | 0.022 (6) | 0.026 (6) | 0.017 (6) | 0.012 (5) | −0.003 (5) | −0.004 (5) |
C6 | 0.021 (6) | 0.021 (6) | 0.010 (5) | 0.012 (5) | 0.001 (4) | −0.006 (4) |
C7 | 0.021 (6) | 0.021 (6) | 0.015 (5) | 0.012 (5) | 0.002 (4) | −0.004 (4) |
O24 | 0.054 (9) | 0.103 (11) | 0.058 (9) | 0.030 (8) | −0.006 (7) | −0.004 (8) |
O25 | 0.098 (10) | 0.076 (10) | 0.069 (9) | 0.050 (8) | −0.012 (8) | −0.011 (8) |
O26 | 0.09 (2) | 0.10 (2) | 0.08 (2) | 0.047 (15) | −0.009 (13) | 0.017 (13) |
O27 | 0.062 (12) | 0.048 (12) | 0.028 (11) | 0.025 (10) | 0.001 (9) | 0.002 (9) |
O28 | 0.073 (14) | 0.051 (12) | 0.058 (13) | 0.028 (10) | −0.019 (11) | 0.013 (10) |
O29 | 0.036 (8) | 0.026 (7) | 0.028 (7) | 0.016 (6) | −0.003 (6) | 0.000 (6) |
O29A | 0.036 (8) | 0.026 (7) | 0.028 (7) | 0.016 (6) | −0.003 (6) | 0.000 (6) |
O29B | 0.036 (8) | 0.026 (7) | 0.028 (7) | 0.016 (6) | −0.003 (6) | 0.000 (6) |
Geometric parameters (Å, º) top
Na1—O2i | 2.333 (13) | Si1—O22 | 1.629 (9) |
Na1—O2ii | 2.333 (13) | Si1—O22i | 1.629 (9) |
Na1—O2 | 2.333 (13) | Si1—O22ii | 1.629 (9) |
Na1—O26 | 2.53 (5) | Si1—O23 | 1.633 (16) |
Na1—O26ii | 2.53 (5) | O1—C1 | 1.264 (19) |
Na1—O26i | 2.53 (5) | O2—C1 | 1.282 (19) |
Na1—Pr1i | 4.137 (4) | O3—C7 | 1.276 (17) |
Na1—Pr1 | 4.137 (4) | O4—C7 | 1.247 (18) |
Na1—Pr1ii | 4.137 (4) | O5—C4 | 1.36 (2) |
W1—O10 | 1.724 (9) | O5—H5 | 0.8399 |
W1—O14 | 1.890 (9) | O6—H6A | 0.8699 |
W1—O15 | 1.906 (9) | O6—H6B | 0.8701 |
W1—O16 | 1.927 (10) | O7—H7A | 0.8699 |
W1—O14ii | 1.938 (8) | O7—H7B | 0.8701 |
W1—O22i | 2.320 (8) | O8—H8A | 0.8701 |
W2—O11 | 1.714 (10) | O8—H8B | 0.8701 |
W2—O17 | 1.864 (10) | O9—H9A | 0.8700 |
W2—O18 | 1.911 (9) | O9—H9B | 0.8701 |
W2—O16 | 1.911 (9) | N1—C2 | 1.318 (18) |
W2—O21i | 1.969 (9) | N1—C6 | 1.340 (19) |
W2—O22i | 2.321 (8) | C1—C2 | 1.52 (2) |
W3—O13 | 1.708 (11) | C2—C3 | 1.39 (2) |
W3—O21 | 1.879 (9) | C3—C4 | 1.38 (2) |
W3—O19 | 1.884 (10) | C3—H3 | 0.9500 |
W3—O17 | 1.936 (10) | C4—C5 | 1.37 (2) |
W3—O15ii | 1.945 (9) | C5—C6 | 1.40 (2) |
W3—O22 | 2.367 (9) | C5—H5A | 0.9500 |
W4—O12 | 1.693 (10) | C6—C7 | 1.51 (2) |
W4—O18 | 1.897 (10) | O24—H24A | 0.8700 |
W4—O20i | 1.919 (10) | O24—H24B | 0.8700 |
W4—O20 | 1.922 (10) | O26—H26A | 0.8692 |
W4—O19 | 1.926 (10) | O26—H26B | 0.8697 |
W4—O23 | 2.357 (8) | O27—H27A | 0.8700 |
Pr1—O1 | 2.407 (11) | O27—H27B | 0.8700 |
Pr1—O3ii | 2.468 (10) | O28—H28A | 0.8699 |
Pr1—O2ii | 2.477 (11) | O28—H28B | 0.8702 |
Pr1—O6 | 2.496 (13) | O29—H29A | 0.8701 |
Pr1—O9 | 2.509 (12) | O29—H29B | 0.8698 |
Pr1—O10 | 2.554 (9) | O29A—H29C | 0.8702 |
Pr1—N1ii | 2.567 (12) | O29A—H29D | 0.8699 |
Pr1—O8 | 2.567 (11) | O29B—H29E | 0.8698 |
Pr1—O7 | 2.593 (12) | O29B—H29F | 0.8701 |
| | | |
O2i—Na1—O2ii | 94.0 (5) | O9—Pr1—O10 | 84.6 (3) |
O2i—Na1—O2 | 94.0 (5) | O1—Pr1—N1ii | 124.3 (4) |
O2ii—Na1—O2 | 94.0 (5) | O3ii—Pr1—N1ii | 63.0 (4) |
O2i—Na1—O26 | 71.8 (14) | O2ii—Pr1—N1ii | 63.5 (4) |
O2ii—Na1—O26 | 151.8 (13) | O6—Pr1—N1ii | 134.0 (4) |
O2—Na1—O26 | 110.8 (12) | O9—Pr1—N1ii | 134.7 (4) |
O2i—Na1—O26ii | 151.8 (13) | O10—Pr1—N1ii | 66.7 (3) |
O2ii—Na1—O26ii | 110.8 (12) | O1—Pr1—O8 | 125.9 (3) |
O2—Na1—O26ii | 71.8 (14) | O3ii—Pr1—O8 | 69.6 (4) |
O26—Na1—O26ii | 90.2 (18) | O2ii—Pr1—O8 | 139.6 (4) |
O2i—Na1—O26i | 110.8 (12) | O6—Pr1—O8 | 71.8 (4) |
O2ii—Na1—O26i | 71.8 (14) | O9—Pr1—O8 | 70.8 (4) |
O2—Na1—O26i | 151.8 (13) | O10—Pr1—O8 | 140.3 (3) |
O26—Na1—O26i | 90.2 (18) | N1ii—Pr1—O8 | 109.7 (4) |
O26ii—Na1—O26i | 90.2 (18) | O1—Pr1—O7 | 125.0 (4) |
O2i—Na1—Pr1i | 77.1 (3) | O3ii—Pr1—O7 | 102.9 (4) |
O2ii—Na1—Pr1i | 121.4 (4) | O2ii—Pr1—O7 | 66.6 (4) |
O2—Na1—Pr1i | 31.7 (3) | O6—Pr1—O7 | 66.3 (5) |
O26—Na1—Pr1i | 80.0 (12) | O9—Pr1—O7 | 142.2 (4) |
O26ii—Na1—Pr1i | 78.6 (14) | O10—Pr1—O7 | 132.4 (4) |
O26i—Na1—Pr1i | 165.0 (13) | N1ii—Pr1—O7 | 70.2 (4) |
O2i—Na1—Pr1 | 121.4 (4) | O8—Pr1—O7 | 73.6 (4) |
O2ii—Na1—Pr1 | 31.7 (3) | O1—Pr1—Na1 | 51.4 (3) |
O2—Na1—Pr1 | 77.1 (3) | O3ii—Pr1—Na1 | 153.4 (3) |
O26—Na1—Pr1 | 165.0 (13) | O2ii—Pr1—Na1 | 29.7 (3) |
O26ii—Na1—Pr1 | 80.0 (12) | O6—Pr1—Na1 | 63.7 (4) |
O26i—Na1—Pr1 | 78.6 (14) | O9—Pr1—Na1 | 119.8 (3) |
Pr1i—Na1—Pr1 | 108.75 (14) | O10—Pr1—Na1 | 85.4 (3) |
O2i—Na1—Pr1ii | 31.7 (3) | N1ii—Pr1—Na1 | 93.1 (3) |
O2ii—Na1—Pr1ii | 77.1 (3) | O8—Pr1—Na1 | 133.7 (3) |
O2—Na1—Pr1ii | 121.4 (4) | O7—Pr1—Na1 | 77.4 (3) |
O26—Na1—Pr1ii | 78.6 (14) | O22—Si1—O22i | 110.0 (4) |
O26ii—Na1—Pr1ii | 165.0 (13) | O22—Si1—O22ii | 110.0 (4) |
O26i—Na1—Pr1ii | 80.0 (12) | O22i—Si1—O22ii | 110.0 (4) |
Pr1i—Na1—Pr1ii | 108.75 (14) | O22—Si1—O23 | 108.9 (4) |
Pr1—Na1—Pr1ii | 108.75 (14) | O22i—Si1—O23 | 108.9 (4) |
O10—W1—O14 | 101.6 (4) | O22ii—Si1—O23 | 108.9 (4) |
O10—W1—O15 | 98.3 (4) | C1—O1—Pr1 | 148.2 (10) |
O14—W1—O15 | 92.6 (4) | C1—O2—Na1 | 118.2 (10) |
O10—W1—O16 | 99.4 (4) | C1—O2—Pr1i | 122.8 (10) |
O14—W1—O16 | 158.7 (4) | Na1—O2—Pr1i | 118.7 (5) |
O15—W1—O16 | 87.9 (4) | C7—O3—Pr1i | 126.1 (9) |
O10—W1—O14ii | 102.5 (4) | C4—O5—H5 | 108.1 |
O14—W1—O14ii | 86.4 (5) | Pr1—O6—H6A | 109.1 |
O15—W1—O14ii | 159.0 (4) | Pr1—O6—H6B | 109.3 |
O16—W1—O14ii | 85.6 (4) | H6A—O6—H6B | 109.5 |
O10—W1—O22i | 169.9 (4) | Pr1—O7—H7A | 109.0 |
O14—W1—O22i | 86.3 (3) | Pr1—O7—H7B | 109.5 |
O15—W1—O22i | 75.0 (3) | H7A—O7—H7B | 109.5 |
O16—W1—O22i | 73.2 (3) | Pr1—O8—H8A | 109.5 |
O14ii—W1—O22i | 84.0 (3) | Pr1—O8—H8B | 109.2 |
O11—W2—O17 | 101.7 (4) | H8A—O8—H8B | 109.5 |
O11—W2—O18 | 100.7 (5) | Pr1—O9—H9A | 109.4 |
O17—W2—O18 | 86.8 (4) | Pr1—O9—H9B | 109.3 |
O11—W2—O16 | 101.3 (5) | H9A—O9—H9B | 109.5 |
O17—W2—O16 | 92.3 (4) | W1—O10—Pr1 | 165.8 (5) |
O18—W2—O16 | 157.7 (4) | W1—O14—W1i | 150.4 (5) |
O11—W2—O21i | 99.9 (4) | W1—O15—W3i | 120.7 (5) |
O17—W2—O21i | 158.2 (4) | W2—O16—W1 | 121.2 (5) |
O18—W2—O21i | 86.6 (4) | W2—O17—W3 | 151.8 (5) |
O16—W2—O21i | 86.1 (4) | W4—O18—W2 | 151.4 (6) |
O11—W2—O22i | 171.1 (4) | W3—O19—W4 | 153.0 (5) |
O17—W2—O22i | 85.9 (4) | W4ii—O20—W4 | 121.9 (5) |
O18—W2—O22i | 84.3 (4) | W3—O21—W2ii | 122.2 (5) |
O16—W2—O22i | 73.4 (4) | Si1—O22—W1ii | 123.8 (5) |
O21i—W2—O22i | 72.8 (3) | Si1—O22—W2ii | 123.7 (4) |
O13—W3—O21 | 102.2 (5) | W1ii—O22—W2ii | 92.2 (3) |
O13—W3—O19 | 103.0 (4) | Si1—O22—W3 | 124.6 (5) |
O21—W3—O19 | 92.8 (4) | W1ii—O22—W3 | 91.1 (3) |
O13—W3—O17 | 102.4 (4) | W2ii—O22—W3 | 91.9 (3) |
O21—W3—O17 | 155.2 (4) | Si1—O23—W4 | 124.7 (3) |
O19—W3—O17 | 85.0 (4) | Si1—O23—W4ii | 124.7 (3) |
O13—W3—O15ii | 98.8 (4) | W4—O23—W4ii | 90.9 (4) |
O21—W3—O15ii | 87.6 (4) | Si1—O23—W4i | 124.7 (3) |
O19—W3—O15ii | 157.6 (4) | W4—O23—W4i | 90.9 (4) |
O17—W3—O15ii | 85.3 (4) | W4ii—O23—W4i | 90.9 (4) |
O13—W3—O22 | 170.7 (4) | C2—N1—C6 | 119.9 (13) |
O21—W3—O22 | 73.2 (3) | C2—N1—Pr1i | 120.3 (10) |
O19—W3—O22 | 85.5 (4) | C6—N1—Pr1i | 119.6 (10) |
O17—W3—O22 | 82.0 (3) | O1—C1—O2 | 122.7 (15) |
O15ii—W3—O22 | 73.2 (3) | O1—C1—C2 | 120.6 (15) |
O12—W4—O18 | 101.7 (5) | O2—C1—C2 | 116.7 (15) |
O12—W4—O20i | 100.7 (5) | N1—C2—C3 | 123.9 (14) |
O18—W4—O20i | 90.7 (4) | N1—C2—C1 | 114.5 (14) |
O12—W4—O20 | 100.9 (5) | C3—C2—C1 | 121.6 (14) |
O18—W4—O20 | 157.2 (4) | C4—C3—C2 | 116.6 (15) |
O20i—W4—O20 | 88.7 (6) | C4—C3—H3 | 121.7 |
O12—W4—O19 | 101.6 (4) | C2—C3—H3 | 121.7 |
O18—W4—O19 | 84.7 (4) | O5—C4—C5 | 119.5 (15) |
O20i—W4—O19 | 157.7 (4) | O5—C4—C3 | 120.5 (16) |
O20—W4—O19 | 87.2 (4) | C5—C4—C3 | 119.8 (15) |
O12—W4—O23 | 171.9 (5) | C4—C5—C6 | 120.5 (14) |
O18—W4—O23 | 84.4 (4) | C4—C5—H5A | 119.8 |
O20i—W4—O23 | 73.6 (4) | C6—C5—H5A | 119.8 |
O20—W4—O23 | 73.6 (4) | N1—C6—C5 | 119.3 (14) |
O19—W4—O23 | 84.2 (4) | N1—C6—C7 | 115.9 (13) |
O1—Pr1—O3ii | 131.7 (4) | C5—C6—C7 | 124.7 (13) |
O1—Pr1—O2ii | 75.1 (4) | O4—C7—O3 | 126.4 (14) |
O3ii—Pr1—O2ii | 125.7 (4) | O4—C7—C6 | 118.6 (13) |
O1—Pr1—O6 | 73.0 (4) | O3—C7—C6 | 115.0 (13) |
O3ii—Pr1—O6 | 141.3 (4) | H24A—O24—H24B | 109.5 |
O2ii—Pr1—O6 | 85.6 (4) | Na1—O26—H26A | 101.6 |
O1—Pr1—O9 | 69.7 (4) | Na1—O26—H26B | 120.6 |
O3ii—Pr1—O9 | 76.4 (4) | H26A—O26—H26B | 91.2 |
O2ii—Pr1—O9 | 144.2 (4) | H27A—O27—H27B | 109.5 |
O6—Pr1—O9 | 90.4 (4) | H28A—O28—H28B | 109.5 |
O1—Pr1—O10 | 68.9 (3) | H29A—O29—H29B | 109.5 |
O3ii—Pr1—O10 | 74.7 (3) | H29C—O29A—H29D | 109.5 |
O2ii—Pr1—O10 | 76.6 (3) | H29E—O29B—H29F | 109.5 |
O6—Pr1—O10 | 140.9 (4) | | |
| | | |
O14—W1—O10—Pr1 | −127 (2) | O22i—Si1—O23—W4 | −58.5 (3) |
O15—W1—O10—Pr1 | 138 (2) | O22ii—Si1—O23—W4 | −178.5 (3) |
O16—W1—O10—Pr1 | 49 (2) | O22—Si1—O23—W4ii | −58.5 (3) |
O14ii—W1—O10—Pr1 | −39 (2) | O22i—Si1—O23—W4ii | −178.5 (3) |
O22i—W1—O10—Pr1 | 91 (3) | O22ii—Si1—O23—W4ii | 61.5 (3) |
O10—W1—O14—W1i | 131.2 (10) | O22—Si1—O23—W4i | −178.5 (3) |
O15—W1—O14—W1i | −129.8 (10) | O22i—Si1—O23—W4i | 61.5 (3) |
O16—W1—O14—W1i | −39.1 (17) | O22ii—Si1—O23—W4i | −58.5 (3) |
O14ii—W1—O14—W1i | 29.2 (11) | Pr1—O1—C1—O2 | −78 (3) |
O22i—W1—O14—W1i | −55.0 (10) | Pr1—O1—C1—C2 | 103 (2) |
O11—W2—O17—W3 | 123.6 (11) | Na1—O2—C1—O1 | 13 (2) |
O18—W2—O17—W3 | 23.4 (11) | Pr1i—O2—C1—O1 | −160.3 (11) |
O16—W2—O17—W3 | −134.3 (11) | Na1—O2—C1—C2 | −168.4 (10) |
O21i—W2—O17—W3 | −49.0 (18) | Pr1i—O2—C1—C2 | 18.4 (18) |
O22i—W2—O17—W3 | −61.1 (11) | C6—N1—C2—C3 | 1 (2) |
O12—W4—O18—W2 | 127.5 (12) | Pr1i—N1—C2—C3 | −174.0 (11) |
O20i—W4—O18—W2 | −131.4 (12) | C6—N1—C2—C1 | 178.7 (12) |
O20—W4—O18—W2 | −42.9 (19) | Pr1i—N1—C2—C1 | 3.9 (16) |
O19—W4—O18—W2 | 26.7 (12) | O1—C1—C2—N1 | 164.6 (13) |
O23—W4—O18—W2 | −57.9 (11) | O2—C1—C2—N1 | −14.1 (19) |
O13—W3—O19—W4 | 130.1 (13) | O1—C1—C2—C3 | −17 (2) |
O21—W3—O19—W4 | −126.7 (13) | O2—C1—C2—C3 | 163.8 (14) |
O17—W3—O19—W4 | 28.6 (12) | N1—C2—C3—C4 | −1 (2) |
O15ii—W3—O19—W4 | −36 (2) | C1—C2—C3—C4 | −178.3 (13) |
O22—W3—O19—W4 | −53.8 (12) | C2—C3—C4—O5 | 176.9 (13) |
O13—W3—O21—W2ii | −171.8 (5) | C2—C3—C4—C5 | 1 (2) |
O19—W3—O21—W2ii | 84.3 (6) | O5—C4—C5—C6 | −177.3 (14) |
O17—W3—O21—W2ii | 0.2 (13) | C3—C4—C5—C6 | −1 (2) |
O15ii—W3—O21—W2ii | −73.3 (5) | C2—N1—C6—C5 | −1 (2) |
O22—W3—O21—W2ii | −0.1 (4) | Pr1i—N1—C6—C5 | 173.7 (10) |
O22i—Si1—O22—W1ii | −58.1 (6) | C2—N1—C6—C7 | −176.7 (12) |
O22ii—Si1—O22—W1ii | 63.2 (6) | Pr1i—N1—C6—C7 | −1.9 (15) |
O23—Si1—O22—W1ii | −177.4 (3) | C4—C5—C6—N1 | 1 (2) |
O22i—Si1—O22—W2ii | −178.2 (3) | C4—C5—C6—C7 | 176.4 (13) |
O22ii—Si1—O22—W2ii | −56.9 (9) | Pr1i—O3—C7—O4 | 173.4 (11) |
O23—Si1—O22—W2ii | 62.4 (5) | Pr1i—O3—C7—C6 | −9.0 (16) |
O22i—Si1—O22—W3 | 61.3 (9) | N1—C6—C7—O4 | −175.5 (13) |
O22ii—Si1—O22—W3 | −177.5 (4) | C5—C6—C7—O4 | 9 (2) |
O23—Si1—O22—W3 | −58.1 (5) | N1—C6—C7—O3 | 6.6 (17) |
O22—Si1—O23—W4 | 61.5 (3) | C5—C6—C7—O3 | −168.6 (13) |
Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6A···O26ii | 0.87 | 2.12 | 2.91 (6) | 151 |
O7—H7A···O11iii | 0.87 | 2.36 | 3.084 (17) | 141 |
O7—H7A···O21iv | 0.87 | 2.29 | 2.988 (18) | 138 |
O7—H7B···O4v | 0.87 | 2.16 | 2.956 (19) | 152 |
O8—H8A···O12vi | 0.87 | 2.17 | 2.929 (15) | 146 |
O8—H8B···O4v | 0.87 | 2.40 | 3.103 (17) | 138 |
O9—H9A···O29Bii | 0.87 | 2.50 | 3.09 (4) | 123 |
C5—H5A···O29 | 0.95 | 2.64 | 3.28 (3) | 126 |
O24—H24A···O11vii | 0.87 | 2.48 | 3.109 (19) | 130 |
O26—H26A···O7ii | 0.87 | 2.23 | 3.10 (6) | 180 |
O26—H26B···O27viii | 0.87 | 1.97 | 2.84 (6) | 179 |
O27—H27A···O24 | 0.87 | 2.42 | 2.94 (3) | 120 |
O27—H27B···O29B | 0.87 | 1.79 | 2.51 (4) | 138 |
O28—H28A···O7 | 0.87 | 2.09 | 2.75 (3) | 132 |
O29—H29A···O11i | 0.87 | 2.59 | 3.18 (3) | 127 |
O29A—H29C···O5ix | 0.87 | 1.96 | 2.83 (4) | 180 |
O29A—H29D···O24x | 0.87 | 1.91 | 2.78 (4) | 175 |
O29B—H29F···O12xi | 0.87 | 2.27 | 3.03 (4) | 146 |
Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, z; (iii) −y+1/3, x−y+2/3, z−1/3; (iv) −x+y−2/3, −x+2/3, z−1/3; (v) x−2/3, y−1/3, z−1/3; (vi) −x+y−1/3, −x+1/3, z−2/3; (vii) −x+y+1/3, −x+2/3, z−1/3; (viii) −x+y+1/3, −x+5/3, z−1/3; (ix) x+1/3, y+2/3, z−1/3; (x) −x+y+1, −x+2, z; (xi) x+2/3, y+1/3, z−2/3. |
Selected bond lengths (Å) for 1 and 2 topCompound 1 | Compound 2 | | |
Dy1—O15i | 2.306 (10) | Pr1—O1 | 2.407 (11) |
Dy1—O13 | 2.375 (11) | Pr1—O3ii | 2.468 (10) |
Dy1—O17 | 2.329 (11) | Pr1—O2ii | 2.477 (11) |
Dy1—O20 | 2.379 (13) | Pr1—O6 | 2.496 (13) |
Dy1—O16 | 2.374 (11) | Pr1—O9 | 2.509 (12) |
Dy1—N1 | 2.469 (13) | Pr1—O10 | 2.554 (9) |
Dy1—N2 | 2.482 (14) | Pr1—N1ii | 2.567 (12) |
Dy1—O19 | 2.364 (12) | Pr1—O8 | 2.567 (11) |
| | Pr1—O7 | 2.593 (12) |
Symmetry codes:
(i) -y+1, x-y+1, z;
(ii) -x+y, -x+1, z. |
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