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Acta Crystallogr Sect E Struct Rep Online. 2010 May 1; 66(Pt 5): i34–i35.
Published online 2010 April 10. doi:  10.1107/S1600536810012316
PMCID: PMC2979069

Redetermination of hexa­sodium hepta­molybdate(VI) 14-hydrate

Abstract

The structure of the title compound, Na6(Mo7O24)·14H2O, has been redetermined [Sjöbom & Hedman (1973). Acta Chem. Scand. 27, 3673–3674] and the hydrogen atoms have been located. The Na+ cations adopt distorted octa­hedral geometries and the structure of the [Mo7O24]6− anion is consistent with those of other hepta­molbydates. In the crystal, numerous O—H(...)O hydrogen bonds help to establish the packing.

Related literature

For general background to polyoxometalates, see: Pope & Müller (1991 [triangle]). For polyoxometalates reported by our group, see: Zhang, Dou et al. (2009 [triangle]); Zhang, Wei et al. (2009 [triangle]). For the structures of other [Mo7O24]6− heteropolyanions, see: Evans et al. (1975 [triangle]); Yang et al. (2002 [triangle]). For the previous determination of the title compound, see: Sjöbom & Hedman (1973 [triangle]). For Na—O bond lengths, see: Turpeinen et al. (2001 [triangle]); An et al. (2004 [triangle]).

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Object name is e-66-00i34-scheme1.jpg

Experimental

Crystal data

  • Na6(Mo7O24)·14H2O
  • M r = 1445.74
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-66-00i34-efi1.jpg
  • a = 21.1304 (2) Å
  • b = 10.3733 (1) Å
  • c = 15.6094 (2) Å
  • V = 3421.46 (6) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 2.68 mm−1
  • T = 296 K
  • 0.12 × 0.10 × 0.08 mm

Data collection

  • Bruker APEXII CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2001 [triangle]) T min = 0.739, T max = 0.814
  • 16564 measured reflections
  • 5831 independent reflections
  • 5748 reflections with I > 2σ(I)
  • R int = 0.021

Refinement

  • R[F 2 > 2σ(F 2)] = 0.017
  • wR(F 2) = 0.044
  • S = 1.00
  • 5831 reflections
  • 545 parameters
  • 63 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 1.12 e Å−3
  • Δρmin = −1.00 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 2689 Friedel pairs
  • Flack parameter: −0.02 (2)

Data collection: APEX2 (Bruker, 2004 [triangle]); cell refinement: SAINT-Plus (Bruker, 2001 [triangle]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810012316/hb5372sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810012316/hb5372Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

Financial support from the Inter­national Cooperation Program for Excellent Lecturers of 2008 from Shandong Provincial Education Department, the Research Award Fund for Outstanding Young and Middle-aged Scientists of Shandong Province (2008BS04022), Shandong Provincial Education Department and Shandong Institute of Education are gratefully acknowledged.

supplementary crystallographic information

Comment

The design and synthesis of polyoxometalates has attracted continuous research interest not only because of their appealing structural and topological novelties, but also due to their interesting optical, electronic, magnetic, and catalytic properties, as well as their potential medical applications (Pope & Müller, 1991). In our research group, a series of polyoxomolybdate structures have been reported (Zhang, Dou et al., 2009; Zhang, Wei et al., 2009). Here, we describe the synthesis and structural characterization of the title compound.

As shown in Figure 1, consists of six sodium cations, one Mo7O24 anion, and fourteen water molecules. The Na+ cations are in a distorted octahedral environment, coordinated by six neighboring water molecules. Na—O bond lengths are in the normal range of 2.331 (4)—2.692 (4) Å, compared to the reported ones (Turpeinen et al., 2001; An et al., 2004).

The configuration of the heptamolybdate anion consisting of seven edge-sharing MoO6 octahedra is very similar to that reported for other heptamolybdates (Evans et al., 1975; Yang et al., 2002). The X-ray analysis shows the arrangement in terms of polyhedra, in which three octahedra are approximately in line in the central horizontal level and four are attached forward at a level above. In each heptamolybdate anion, six peripheral Mo atoms (Mo2, Mo3, Mo4 Mo5, Mo6 and Mo7) have two terminal oxygens (t—O), two bridging oxygens (β—O), one capping oxygen (β3—O), and one β4—O atom bonded to four Mo atoms, while the seventh Mo center (Mo1) has four capping oxygens and two β4—O atoms. Although Mo1 has no terminal oxygen atom, Mo=O characters are still obvious in those two very short Mo—O distances [Mo1—O11, 1.746 (3) Å and Mo1—O17, 1.727 (3) Å) opposed to two abnormally long Mo—O distances [Mo1—O10, 2.298 (3) Å and Mo1—O18, 2.238 (3) Å).

O—H···O hydrogen bonding between anionic moieties and water molecules leads to a consolidation of the structure (Fig. 2; Table 2).

Experimental

A mixture of 2,4'-biphenyldicarboxylic acid (0.2 mmoL 0.05 g), 2-Pyridyl)pyrazole (0.3 mmoL 0.05 g), sodium molybdate (0.4 mmoL, 0.10 g), and copper(II) sulfate pentahydrate (0.2 mmol, 0.05 g) in 14 ml distilled water was sealed in a 25 ml Teflon-lined stainless steel autoclave and was kept at 433 K for three days. Colourless blocks of (I) were obtained.

Refinement

The water H atoms were located in difference maps and refined by using the 'DFIX' command with H···H = 1.38 Å, and O—H = 0.82 (2) Å and Uiso = 1.5Ueq(O).

Figures

Fig. 1.
The molecular structure of (I) with displacement ellipsoids are drawn at the 30% probability level; H atoms are given as spheres of arbitrary radius.
Fig. 2.
The crystal packing of (I), displayed with O—H···O hydrogen bonds as dashed lines.

Crystal data

Na6(Mo7O24)·14H2OF(000) = 2768
Mr = 1445.74Dx = 2.807 Mg m3
Orthorhombic, Pca21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2acCell parameters from 9872 reflections
a = 21.1304 (2) Åθ = 2.2–30.3°
b = 10.3733 (1) ŵ = 2.68 mm1
c = 15.6094 (2) ÅT = 296 K
V = 3421.46 (6) Å3Block, colourless
Z = 40.12 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer5831 independent reflections
Radiation source: fine-focus sealed tube5748 reflections with I > 2σ(I)
graphiteRint = 0.021
ω scansθmax = 25.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −20→25
Tmin = 0.739, Tmax = 0.814k = −12→11
16564 measured reflectionsl = −18→18

Refinement

Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.017w = 1/[σ2(Fo2) + (0.029P)2] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.044(Δ/σ)max = 0.001
S = 1.00Δρmax = 1.12 e Å3
5831 reflectionsΔρmin = −1.00 e Å3
545 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
63 restraintsExtinction coefficient: 0.00258 (7)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), 2689 Friedel pairs
Secondary atom site location: difference Fourier mapFlack parameter: −0.02 (2)

Special details

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Mo10.441554 (16)0.17102 (3)0.95800 (3)0.01241 (9)
Mo20.519892 (17)0.17010 (4)0.76582 (3)0.01523 (10)
Mo30.364901 (18)0.18576 (4)0.76633 (3)0.01518 (10)
Mo40.528881 (18)0.44744 (4)0.95766 (3)0.01502 (9)
Mo50.374213 (18)0.47162 (4)0.95430 (3)0.01652 (10)
Mo60.603656 (18)0.18041 (4)0.93595 (3)0.01647 (10)
Mo70.282633 (18)0.22516 (4)0.93663 (3)0.01714 (10)
Na10.64293 (9)0.6312 (2)0.78932 (12)0.0257 (4)
Na20.27899 (10)−0.0513 (2)0.60777 (14)0.0311 (5)
Na30.38753 (11)−0.0891 (3)1.10058 (16)0.0458 (7)
Na40.48165 (9)0.66440 (19)0.79018 (13)0.0260 (5)
Na50.30429 (10)0.5433 (2)0.71744 (16)0.0364 (6)
Na60.44153 (9)0.0751 (2)0.57623 (13)0.0262 (5)
O10.31809 (17)0.3039 (4)0.7229 (2)0.0243 (8)
O20.36309 (17)0.0599 (3)0.6943 (2)0.0241 (8)
O30.44497 (14)0.2636 (3)0.7335 (2)0.0175 (7)
O40.43894 (15)0.0915 (3)0.8473 (2)0.0155 (7)
O50.51294 (17)0.0389 (3)0.6968 (2)0.0233 (8)
O60.57476 (17)0.2655 (4)0.7163 (2)0.0253 (8)
O70.57567 (17)0.0718 (3)0.8441 (2)0.0206 (7)
O80.66719 (17)0.2509 (4)0.8854 (3)0.0301 (9)
O90.63533 (17)0.0697 (3)1.0055 (2)0.0255 (8)
O100.52100 (14)0.2723 (3)0.8833 (2)0.0150 (7)
O110.50591 (16)0.0893 (3)1.0023 (2)0.0210 (7)
O120.58294 (17)0.3174 (3)1.0138 (2)0.0194 (7)
O130.58341 (16)0.5165 (4)0.8912 (2)0.0266 (8)
O140.52789 (18)0.5444 (3)1.0477 (2)0.0259 (8)
O150.44765 (14)0.3318 (3)1.0129 (2)0.0153 (7)
O160.45439 (14)0.5087 (3)0.9006 (2)0.0184 (7)
O170.37682 (17)0.1012 (3)1.0071 (2)0.0238 (8)
O180.37170 (14)0.2913 (3)0.8856 (2)0.0156 (7)
O190.22488 (17)0.3105 (4)0.8851 (2)0.0299 (9)
O200.24370 (17)0.1265 (4)1.0080 (2)0.0269 (8)
O210.30435 (16)0.1066 (3)0.8458 (2)0.0183 (7)
O220.32638 (17)0.5509 (4)0.8837 (2)0.0290 (9)
O230.31128 (15)0.3577 (3)1.0128 (2)0.0195 (7)
O240.37878 (19)0.5698 (4)1.0429 (3)0.0307 (9)
O1W0.3174 (2)−0.0027 (5)1.1998 (3)0.0462 (11)
O2W0.2972 (3)−0.1913 (5)1.0428 (3)0.0478 (12)
O3W0.4691 (2)−0.1981 (4)1.0305 (2)0.0296 (9)
O4W0.3203 (2)−0.2267 (4)0.6941 (3)0.0352 (9)
O5W0.2912 (3)0.5327 (7)0.5640 (4)0.086 (2)
O6W0.41466 (18)0.5240 (4)0.7083 (2)0.0288 (8)
O7W0.4549 (2)0.7974 (4)0.6737 (3)0.0344 (10)
O8W0.4210 (2)0.8248 (4)0.8668 (3)0.0302 (9)
O9W0.5612 (2)0.5692 (5)0.6945 (3)0.0376 (10)
O10W0.5724 (2)0.7960 (4)0.8444 (3)0.0366 (10)
O11W0.69267 (19)0.7408 (4)0.6777 (2)0.0323 (9)
O12W0.6942 (2)0.4283 (4)0.7449 (3)0.0491 (12)
O13W0.38065 (18)0.2485 (3)0.5149 (3)0.0421 (10)
O14W0.71393 (19)0.1461 (4)0.3624 (3)0.0348 (10)
H1W0.316 (3)0.0761 (6)1.196 (4)0.080*
H2W0.326 (3)−0.029 (5)1.2479 (15)0.080*
H3W0.295 (3)−0.167 (5)0.9929 (12)0.080*
H4W0.299 (4)−0.2700 (9)1.049 (3)0.080*
H5W0.478 (3)−0.170 (4)0.982 (2)0.080*
H6W0.467 (4)−0.2784 (7)1.034 (4)0.080*
H7W0.306 (2)−0.208 (6)0.7412 (14)0.080*
H8W0.3579 (12)−0.209 (8)0.688 (4)0.080*
H9W0.287 (3)0.4546 (11)0.559 (4)0.080*
H10W0.318 (3)0.565 (5)0.532 (4)0.080*
H11W0.428 (2)0.537 (5)0.6599 (12)0.080*
H12W0.427 (2)0.456 (3)0.730 (3)0.080*
H13W0.455 (3)0.768 (5)0.6248 (14)0.080*
H14W0.477 (3)0.862 (5)0.680 (4)0.080*
H15W0.3839 (8)0.803 (5)0.861 (5)0.080*
H16W0.430 (3)0.895 (4)0.845 (6)0.080*
H17W0.562 (4)0.4902 (5)0.693 (4)0.080*
H18W0.559 (3)0.603 (5)0.6473 (17)0.080*
H19W0.584 (3)0.784 (6)0.8939 (13)0.080*
H20W0.564 (3)0.8712 (15)0.832 (4)0.080*
H21W0.7309 (5)0.731 (7)0.683 (4)0.080*
H22W0.679 (3)0.726 (9)0.629 (2)0.080*
H23W0.687 (3)0.376 (4)0.783 (3)0.080*
H24W0.684 (4)0.405 (6)0.6968 (18)0.080*
H25W0.374 (3)0.172 (2)0.526 (5)0.080*
H26W0.413 (2)0.278 (5)0.535 (5)0.080*
H27W0.716 (3)0.0671 (5)0.361 (6)0.080*
H28W0.7484 (13)0.182 (5)0.361 (6)0.080*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Mo10.0120 (2)0.01206 (19)0.0131 (2)−0.00056 (13)−0.00043 (16)0.00097 (16)
Mo20.0147 (2)0.0172 (2)0.01380 (19)−0.00019 (14)0.00116 (17)−0.00129 (16)
Mo30.0143 (2)0.0164 (2)0.01480 (19)−0.00104 (15)−0.00192 (17)−0.00082 (16)
Mo40.01592 (19)0.01323 (19)0.01592 (19)−0.00242 (14)−0.00039 (17)0.00063 (16)
Mo50.01692 (19)0.01323 (19)0.0194 (2)0.00094 (14)0.00030 (17)−0.00124 (16)
Mo60.01212 (19)0.0185 (2)0.0187 (2)0.00150 (14)−0.00171 (16)0.00215 (16)
Mo70.01230 (19)0.0199 (2)0.0192 (2)−0.00179 (15)0.00169 (16)0.00027 (17)
Na10.0219 (10)0.0308 (11)0.0244 (11)−0.0043 (8)0.0011 (8)0.0013 (9)
Na20.0243 (11)0.0370 (13)0.0321 (11)0.0014 (9)0.0002 (9)0.0022 (10)
Na30.0321 (13)0.0686 (19)0.0366 (13)0.0158 (12)0.0011 (10)0.0072 (13)
Na40.0311 (12)0.0249 (11)0.0219 (10)−0.0007 (8)0.0007 (8)0.0024 (8)
Na50.0246 (12)0.0302 (13)0.0543 (15)0.0009 (9)0.0001 (10)0.0007 (11)
Na60.0241 (11)0.0284 (12)0.0260 (11)0.0030 (8)−0.0005 (8)−0.0041 (9)
O10.0218 (19)0.025 (2)0.027 (2)0.0010 (15)−0.0034 (15)0.0026 (15)
O20.0251 (19)0.0249 (19)0.0223 (19)−0.0018 (15)−0.0007 (15)−0.0037 (15)
O30.0144 (17)0.0182 (18)0.0198 (18)−0.0009 (13)0.0017 (12)0.0042 (14)
O40.0175 (18)0.0149 (17)0.0140 (17)−0.0016 (13)0.0002 (12)−0.0010 (13)
O50.026 (2)0.022 (2)0.0210 (18)0.0011 (14)−0.0012 (15)−0.0060 (15)
O60.0202 (18)0.029 (2)0.026 (2)−0.0086 (15)0.0028 (15)0.0000 (15)
O70.0232 (19)0.0191 (18)0.0196 (18)0.0089 (15)−0.0032 (14)−0.0017 (14)
O80.0200 (19)0.032 (2)0.038 (2)−0.0013 (16)0.0051 (17)0.0019 (17)
O90.0207 (19)0.027 (2)0.0284 (19)0.0035 (15)−0.0036 (15)0.0043 (16)
O100.0129 (17)0.0169 (18)0.0152 (16)−0.0006 (12)−0.0004 (13)−0.0015 (13)
O110.0217 (18)0.0199 (18)0.0215 (17)0.0038 (14)−0.0044 (15)0.0019 (14)
O120.0197 (17)0.0209 (18)0.0178 (18)0.0015 (13)−0.0056 (15)0.0011 (14)
O130.025 (2)0.028 (2)0.027 (2)−0.0051 (15)0.0063 (15)0.0025 (16)
O140.034 (2)0.022 (2)0.0216 (19)0.0002 (15)−0.0038 (16)−0.0059 (15)
O150.0169 (17)0.0159 (17)0.0131 (17)−0.0004 (12)0.0025 (13)−0.0002 (13)
O160.0196 (17)0.0150 (17)0.0205 (17)−0.0006 (13)−0.0024 (13)0.0029 (14)
O170.0273 (19)0.0213 (18)0.0229 (18)−0.0062 (14)0.0036 (15)0.0020 (14)
O180.0124 (16)0.0198 (17)0.0146 (17)−0.0009 (13)0.0017 (13)0.0010 (14)
O190.0235 (19)0.034 (2)0.032 (2)0.0050 (16)−0.0054 (17)−0.0014 (17)
O200.0202 (19)0.031 (2)0.0292 (19)−0.0080 (16)0.0041 (15)0.0039 (17)
O210.0182 (18)0.0191 (18)0.0176 (17)−0.0076 (14)−0.0002 (14)−0.0005 (13)
O220.025 (2)0.027 (2)0.035 (2)0.0029 (16)−0.0056 (17)0.0051 (17)
O230.0197 (17)0.0194 (17)0.0192 (17)−0.0010 (14)0.0058 (14)−0.0020 (14)
O240.039 (2)0.0199 (19)0.033 (2)−0.0003 (16)0.0012 (18)−0.0086 (16)
O1W0.051 (3)0.042 (3)0.046 (3)−0.001 (2)0.006 (2)−0.003 (2)
O2W0.066 (3)0.040 (3)0.038 (3)0.014 (2)−0.004 (2)−0.006 (2)
O3W0.032 (2)0.027 (2)0.030 (2)−0.0028 (17)−0.0004 (18)0.0008 (16)
O4W0.036 (2)0.030 (2)0.039 (2)0.0001 (18)−0.0006 (19)−0.0010 (19)
O5W0.096 (5)0.107 (5)0.054 (3)−0.064 (4)−0.009 (3)0.002 (3)
O6W0.029 (2)0.025 (2)0.032 (2)−0.0035 (16)0.0051 (17)0.0035 (16)
O7W0.053 (3)0.025 (2)0.025 (2)−0.0062 (19)0.0011 (18)0.0016 (17)
O8W0.034 (2)0.026 (2)0.031 (2)−0.0006 (17)0.0015 (19)−0.0023 (16)
O9W0.030 (2)0.047 (3)0.036 (2)0.002 (2)−0.0058 (18)−0.015 (2)
O10W0.046 (3)0.023 (2)0.041 (3)0.0031 (19)−0.004 (2)−0.0026 (18)
O11W0.024 (2)0.046 (3)0.026 (2)−0.0014 (18)−0.0036 (16)0.0077 (18)
O12W0.034 (2)0.041 (3)0.073 (3)0.0010 (19)0.013 (2)0.006 (2)
O13W0.035 (2)0.041 (3)0.051 (3)−0.0027 (19)−0.008 (2)0.010 (2)
O14W0.026 (2)0.031 (2)0.047 (2)−0.0036 (18)−0.0036 (19)−0.005 (2)

Geometric parameters (Å, °)

Mo1—O171.727 (3)Na4—O7W2.352 (5)
Mo1—O111.746 (3)Na4—O6W2.399 (4)
Mo1—O151.880 (3)Na4—O8W2.417 (5)
Mo1—O41.915 (3)Na4—O162.430 (4)
Mo1—O182.238 (3)Na4—O9W2.455 (5)
Mo1—O102.298 (3)Na4—O10W2.501 (5)
Mo2—O61.709 (3)Na5—O6W2.345 (4)
Mo2—O51.741 (3)Na5—O12Wv2.384 (5)
Mo2—O31.924 (3)Na5—O5W2.413 (7)
Mo2—O71.981 (3)Na5—O4Wvi2.437 (5)
Mo2—O102.119 (3)Na5—O12.503 (4)
Mo2—O42.283 (3)Na5—O222.638 (5)
Mo3—O11.715 (4)Na6—O13W2.410 (4)
Mo3—O21.723 (3)Na6—O11iii2.339 (4)
Mo3—O31.943 (3)Na6—O3Wiii2.388 (5)
Mo3—O211.962 (3)Na6—O52.442 (4)
Mo3—O182.164 (3)Na6—O9iii2.472 (4)
Mo3—O42.237 (3)Na6—O22.484 (4)
Mo4—O131.707 (3)O5—Na3iii2.637 (4)
Mo4—O141.729 (3)O6—Na3iii2.692 (4)
Mo4—O161.917 (3)O9—Na2iv2.421 (4)
Mo4—O121.973 (3)O9—Na6iv2.472 (4)
Mo4—O102.162 (3)O11—Na6iv2.339 (4)
Mo4—O152.264 (3)O19—Na1v2.366 (4)
Mo5—O221.706 (4)O20—Na2vii2.461 (4)
Mo5—O241.720 (4)O1W—Na2vii2.543 (5)
Mo5—O161.929 (3)O12W—Na5i2.384 (5)
Mo5—O232.000 (3)O1W—H1W0.821 (4)
Mo5—O182.157 (3)O1W—H2W0.82 (3)
Mo5—O152.312 (3)O2W—Na2vii2.395 (5)
Mo6—O91.717 (3)O2W—H3W0.82 (3)
Mo6—O81.720 (4)O2W—H4W0.823 (15)
Mo6—O71.917 (3)O3W—Na6iv2.388 (5)
Mo6—O121.920 (3)O3W—H5W0.83 (4)
Mo6—O102.153 (3)O3W—H6W0.835 (9)
Mo6—O112.497 (4)O4W—Na5viii2.437 (5)
Mo7—O191.709 (4)O4W—H7W0.82 (3)
Mo7—O201.722 (4)O4W—H8W0.82 (3)
Mo7—O231.915 (3)O5W—H9W0.819 (15)
Mo7—O211.932 (3)O5W—H10W0.83 (6)
Mo7—O182.156 (3)O6W—H11W0.82 (3)
Na1—O11W2.331 (4)O6W—H12W0.83 (4)
Na1—O132.352 (4)O7W—H13W0.82 (3)
Na1—O9W2.364 (5)O7W—H14W0.82 (6)
Na1—O19i2.366 (4)O8W—H15W0.82 (2)
Na1—O10W2.426 (5)O8W—H16W0.83 (5)
Na1—O12W2.467 (5)O9W—H17W0.820 (10)
Na2—O2Wii2.395 (5)O9W—H18W0.82 (3)
Na2—O9iii2.421 (4)O10W—H19W0.82 (3)
Na2—O4W2.427 (5)O10W—H20W0.82 (2)
Na2—O20ii2.461 (4)O11W—H21W0.818 (15)
Na2—O22.513 (4)O11W—H22W0.83 (4)
Na2—O1Wii2.543 (5)O12W—H23W0.82 (5)
Na3—O1W2.324 (5)O12W—H24W0.82 (4)
Na3—O3W2.334 (5)O13W—H25W0.82 (3)
Na3—O2W2.362 (6)O13W—H26W0.81 (5)
Na3—O172.466 (4)O14W—H27W0.821 (9)
Na3—O5iv2.637 (4)O14W—H28W0.82 (4)
Na3—O6iv2.692 (4)
O17—Mo1—O11103.74 (18)O2Wii—Na2—O1Wii79.69 (18)
O17—Mo1—O15102.93 (16)O9iii—Na2—O1Wii170.76 (17)
O11—Mo1—O15101.36 (15)O4W—Na2—O1Wii97.07 (17)
O17—Mo1—O4101.36 (15)O20ii—Na2—O1Wii93.04 (16)
O11—Mo1—O499.83 (15)O2—Na2—O1Wii99.87 (15)
O15—Mo1—O4142.70 (15)O1W—Na3—O3W166.03 (19)
O17—Mo1—O1886.29 (15)O1W—Na3—O2W84.99 (18)
O11—Mo1—O18169.87 (14)O3W—Na3—O2W101.55 (18)
O15—Mo1—O1877.34 (13)O1W—Na3—O1791.55 (17)
O4—Mo1—O1876.45 (13)O3W—Na3—O17100.28 (16)
O17—Mo1—O10174.48 (15)O2W—Na3—O1793.40 (17)
O11—Mo1—O1081.61 (14)O1W—Na3—O5iv93.01 (16)
O15—Mo1—O1077.03 (13)O3W—Na3—O5iv76.91 (14)
O4—Mo1—O1076.14 (13)O2W—Na3—O5iv161.95 (19)
O18—Mo1—O1088.33 (12)O17—Na3—O5iv104.60 (15)
O6—Mo2—O5103.31 (17)O1W—Na3—O6iv90.19 (17)
O6—Mo2—O398.51 (16)O3W—Na3—O6iv76.51 (14)
O5—Mo2—O399.36 (16)O2W—Na3—O6iv100.99 (18)
O6—Mo2—O799.99 (17)O17—Na3—O6iv165.60 (16)
O5—Mo2—O791.69 (16)O5iv—Na3—O6iv61.03 (12)
O3—Mo2—O7155.63 (14)O7W—Na4—O6W78.62 (15)
O6—Mo2—O1095.41 (15)O7W—Na4—O8W81.45 (16)
O5—Mo2—O10158.01 (15)O6W—Na4—O8W111.64 (16)
O3—Mo2—O1089.05 (13)O7W—Na4—O16151.77 (16)
O7—Mo2—O1073.56 (13)O6W—Na4—O1680.47 (13)
O6—Mo2—O4165.32 (15)O8W—Na4—O1688.92 (14)
O5—Mo2—O490.13 (14)O7W—Na4—O9W85.99 (17)
O3—Mo2—O473.11 (13)O6W—Na4—O9W80.55 (14)
O7—Mo2—O485.29 (13)O8W—Na4—O9W160.16 (18)
O10—Mo2—O472.81 (12)O16—Na4—O9W109.03 (16)
O1—Mo3—O2105.69 (17)O7W—Na4—O10W97.22 (17)
O1—Mo3—O395.81 (16)O6W—Na4—O10W164.52 (16)
O2—Mo3—O399.35 (16)O8W—Na4—O10W82.12 (15)
O1—Mo3—O2199.95 (16)O16—Na4—O10W107.71 (15)
O2—Mo3—O2194.63 (16)O9W—Na4—O10W84.31 (16)
O3—Mo3—O21155.25 (14)O6W—Na5—O12Wv172.8 (2)
O1—Mo3—O1891.01 (15)O6W—Na5—O5W92.9 (2)
O2—Mo3—O18161.01 (15)O12Wv—Na5—O5W94.1 (2)
O3—Mo3—O1887.63 (13)O6W—Na5—O4Wvi86.34 (15)
O21—Mo3—O1873.21 (12)O12Wv—Na5—O4Wvi92.41 (17)
O1—Mo3—O4160.00 (15)O5W—Na5—O4Wvi85.0 (2)
O2—Mo3—O493.03 (15)O6W—Na5—O178.54 (14)
O3—Mo3—O473.83 (13)O12Wv—Na5—O1103.31 (16)
O21—Mo3—O485.18 (13)O5W—Na5—O190.1 (2)
O18—Mo3—O471.84 (12)O4Wvi—Na5—O1163.84 (16)
O13—Mo4—O14104.96 (18)O6W—Na5—O2283.46 (14)
O13—Mo4—O1697.62 (16)O12Wv—Na5—O2289.57 (18)
O14—Mo4—O16100.09 (16)O5W—Na5—O22176.3 (2)
O13—Mo4—O1299.54 (16)O4Wvi—Na5—O2295.37 (15)
O14—Mo4—O1292.49 (16)O1—Na5—O2288.60 (13)
O16—Mo4—O12155.31 (14)O13W—Na6—O11iii126.98 (17)
O13—Mo4—O1094.50 (15)O13W—Na6—O3Wiii84.49 (15)
O14—Mo4—O10157.58 (15)O11iii—Na6—O3Wiii82.35 (14)
O16—Mo4—O1088.05 (13)O13W—Na6—O5138.66 (17)
O12—Mo4—O1073.06 (13)O11iii—Na6—O588.57 (13)
O13—Mo4—O15164.76 (15)O3Wiii—Na6—O579.87 (14)
O14—Mo4—O1589.38 (15)O13W—Na6—O9iii85.71 (15)
O16—Mo4—O1574.36 (13)O11iii—Na6—O9iii69.45 (13)
O12—Mo4—O1584.70 (13)O3Wiii—Na6—O9iii135.27 (15)
O10—Mo4—O1572.60 (12)O5—Na6—O9iii131.09 (15)
O22—Mo5—O24105.50 (19)O13W—Na6—O289.20 (15)
O22—Mo5—O1698.23 (16)O11iii—Na6—O2129.55 (15)
O24—Mo5—O16100.49 (17)O3Wiii—Na6—O2141.55 (15)
O22—Mo5—O23100.70 (16)O5—Na6—O280.23 (14)
O24—Mo5—O2391.18 (16)O9iii—Na6—O281.64 (13)
O16—Mo5—O23154.21 (14)Mo3—O1—Na5142.2 (2)
O22—Mo5—O1894.71 (15)Mo3—O2—Na6114.91 (18)
O24—Mo5—O18156.14 (16)Mo3—O2—Na2135.58 (19)
O16—Mo5—O1888.77 (13)Na6—O2—Na295.85 (14)
O23—Mo5—O1872.41 (13)Mo2—O3—Mo3115.98 (17)
O22—Mo5—O15162.75 (16)Mo1—O4—Mo3109.98 (15)
O24—Mo5—O1590.90 (16)Mo1—O4—Mo2109.10 (14)
O16—Mo5—O1573.01 (12)Mo3—O4—Mo293.03 (12)
O23—Mo5—O1583.97 (13)Mo2—O5—Na6114.14 (18)
O18—Mo5—O1570.68 (12)Mo2—O5—Na3iii97.50 (16)
O9—Mo6—O8105.68 (18)Na6—O5—Na3iii91.33 (14)
O9—Mo6—O7101.52 (16)Mo2—O6—Na3iii96.37 (17)
O8—Mo6—O798.49 (17)Mo6—O7—Mo2110.01 (17)
O9—Mo6—O12100.59 (16)Mo6—O9—Na2iv139.6 (2)
O8—Mo6—O1298.84 (17)Mo6—O9—Na6iv115.65 (18)
O7—Mo6—O12146.93 (15)Na2iv—O9—Na6iv98.57 (14)
O9—Mo6—O10148.66 (15)Mo2—O10—Mo696.77 (13)
O8—Mo6—O10105.66 (16)Mo2—O10—Mo4152.37 (17)
O7—Mo6—O1074.02 (13)Mo6—O10—Mo496.01 (12)
O12—Mo6—O1074.28 (13)Mo2—O10—Mo1101.67 (13)
O9—Mo6—O1178.85 (14)Mo6—O10—Mo1101.34 (13)
O8—Mo6—O11175.47 (15)Mo4—O10—Mo199.68 (12)
O7—Mo6—O1180.35 (13)Mo1—O11—Na6iv156.9 (2)
O12—Mo6—O1180.15 (13)Mo1—O11—Mo6107.22 (16)
O10—Mo6—O1169.81 (11)Na6iv—O11—Mo695.04 (13)
O19—Mo7—O20105.74 (19)Mo6—O12—Mo4110.89 (16)
O19—Mo7—O2398.41 (17)Mo4—O13—Na1169.7 (2)
O20—Mo7—O23100.14 (17)Mo1—O15—Mo4110.38 (15)
O19—Mo7—O2198.83 (17)Mo1—O15—Mo5109.28 (15)
O20—Mo7—O21102.13 (16)Mo4—O15—Mo591.48 (12)
O23—Mo7—O21146.83 (14)Mo4—O16—Mo5116.91 (17)
O19—Mo7—O18106.55 (16)Mo4—O16—Na4110.82 (15)
O20—Mo7—O18147.69 (15)Mo5—O16—Na4130.46 (16)
O23—Mo7—O1874.04 (13)Mo1—O17—Na3121.71 (19)
O21—Mo7—O1873.97 (13)Mo7—O18—Mo596.53 (12)
O11W—Na1—O13173.62 (16)Mo7—O18—Mo395.68 (12)
O11W—Na1—O9W89.69 (16)Mo5—O18—Mo3150.20 (16)
O13—Na1—O9W83.96 (16)Mo7—O18—Mo1102.24 (13)
O11W—Na1—O19i91.00 (15)Mo5—O18—Mo1102.48 (13)
O13—Na1—O19i95.36 (15)Mo3—O18—Mo1101.32 (13)
O9W—Na1—O19i178.99 (19)Mo7—O19—Na1v162.3 (2)
O11W—Na1—O10W101.45 (18)Mo7—O20—Na2vii161.4 (2)
O13—Na1—O10W77.76 (15)Mo7—O21—Mo3110.65 (16)
O9W—Na1—O10W87.96 (16)Mo5—O22—Na5136.5 (2)
O19i—Na1—O10W92.63 (16)Mo7—O23—Mo5110.56 (15)
O11W—Na1—O12W90.47 (17)H1W—O1W—H2W114 (6)
O13—Na1—O12W89.60 (16)H3W—O2W—H4W115 (5)
O9W—Na1—O12W84.97 (18)H5W—O3W—H6W115 (5)
O19i—Na1—O12W94.28 (17)H7W—O4W—H8W114 (6)
O10W—Na1—O12W166.11 (18)H9W—O5W—H10W115 (6)
O2Wii—Na2—O9iii100.14 (17)H11W—O6W—H12W114 (5)
O2Wii—Na2—O4W91.30 (17)H13W—O7W—H14W114 (6)
O9iii—Na2—O4W92.17 (15)H15W—O8W—H16W115 (6)
O2Wii—Na2—O20ii93.17 (17)H17W—O9W—H18W114 (5)
O9iii—Na2—O20ii77.72 (14)H19W—O10W—H20W116 (6)
O4W—Na2—O20ii169.53 (16)H21W—O11W—H22W115 (6)
O2Wii—Na2—O2169.12 (18)H23W—O12W—H24W115 (5)
O9iii—Na2—O282.06 (13)H25W—O13W—H26W115 (6)
O4W—Na2—O277.93 (14)H27W—O14W—H28W114 (5)
O20ii—Na2—O297.71 (14)

Symmetry codes: (i) x+1/2, −y+1, z; (ii) −x+1/2, y, z−1/2; (iii) −x+1, −y, z−1/2; (iv) −x+1, −y, z+1/2; (v) x−1/2, −y+1, z; (vi) x, y+1, z; (vii) −x+1/2, y, z+1/2; (viii) x, y−1, z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O6W—H12W···O30.83 (4)2.04 (2)2.804 (5)156 (5)
O9W—H17W···O60.82 (1)2.37 (1)3.182 (6)168 (6)
O12W—H23W···O80.82 (5)2.10 (5)2.920 (6)176 (5)
O12W—H24W···O60.82 (4)2.73 (7)3.069 (6)106 (6)
O1W—H1W···O11Wix0.82 (1)1.93 (1)2.747 (7)175 (7)
O2W—H3W···O14Wiv0.82 (3)2.06 (1)2.865 (7)168 (5)
O2W—H4W···O24viii0.82 (2)2.37 (7)3.018 (6)136 (8)
O3W—H5W···O8Wviii0.83 (4)2.16 (6)2.760 (6)129 (6)
O4W—H7W···O14Wiv0.82 (3)2.04 (3)2.850 (6)169 (5)
O4W—H8W···O7Wviii0.82 (3)2.06 (2)2.872 (6)168 (9)
O5W—H9W···O23ii0.82 (2)2.41 (6)2.937 (6)123 (6)
O5W—H10W···O12x0.83 (6)2.45 (4)3.179 (6)149 (8)
O6W—H11W···O14x0.82 (3)2.15 (3)2.874 (5)147 (4)
O7W—H13W···O12x0.82 (3)2.11 (3)2.878 (5)157 (6)
O7W—H13W···O11x0.82 (3)2.55 (5)3.036 (5)119 (5)
O7W—H14W···O5vi0.82 (6)2.00 (5)2.812 (6)168 (9)
O8W—H15W···O14Wix0.82 (2)2.13 (3)2.868 (6)149 (5)
O8W—H16W···O4vi0.83 (5)2.05 (4)2.808 (5)154 (10)
O9W—H18W···O15x0.82 (3)2.21 (3)3.021 (6)172 (6)
O10W—H19W···O13Wix0.82 (3)2.06 (3)2.877 (7)176 (6)
O10W—H20W···O7vi0.82 (2)2.10 (2)2.862 (5)154 (5)
O11W—H21W···O1i0.82 (2)1.98 (3)2.781 (5)167 (5)
O11W—H22W···O23x0.83 (4)2.03 (3)2.771 (5)150 (6)
O13W—H25W···O20ii0.82 (3)2.55 (5)2.918 (6)109 (4)
O13W—H26W···O14x0.81 (5)2.23 (3)2.935 (6)144 (5)
O14W—H27W···O21iii0.82 (1)1.87 (2)2.662 (5)163 (6)
O14W—H28W···O8xi0.82 (4)1.96 (2)2.761 (5)167 (9)

Symmetry codes: (ix) −x+1, −y+1, z+1/2; (iv) −x+1, −y, z+1/2; (viii) x, y−1, z; (ii) −x+1/2, y, z−1/2; (x) −x+1, −y+1, z−1/2; (vi) x, y+1, z; (i) x+1/2, −y+1, z; (iii) −x+1, −y, z−1/2; (xi) −x+3/2, y, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5372).

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