Abstract
The title arsenatomolybdate, K5[Mo8O24(OH)2(AsO4)]·2H2O, which was obtained hydrothermally, features an [AsMo8O28(OH)2]5− anion, which is formed by two Mo4O14(OH) units that are linked by As in a sandwich-like fashion. The overall symmetry of the anion is m2m. The {Mo4O14(OH)} core is composed of two pairs of confacial bioctahedral {Mo2O9} units with two μ4-O atoms which have been characterized as hydroxyl groups. The anions are further interconnected by potassium cations, forming a three-dimensional network structure with the uncoordinated water molecules occupying the channels. The structure is further stabilized by O—H⋯O hydrogen bonding.
Related literature
For isotypic K5-x(NH4)xP[Mo4O14(OH)]2·2H2O (x = 2.43), see: Chen et al. (2009 ▶). For a general overview of polyoxometalates, see: Pope (1983 ▶). For the Mo/As/O system, see: Sun et al. (2007 ▶); He & Wang (1999 ▶). For bond-valence-sum calculatios, see: Brown (1981 ▶); Hsu & Wang (1997 ▶).
Experimental
Crystal data
K5[Mo8O24(OH)2(AsO4)]·2H2O
M r = 1553.95
Orthorhombic,
a = 8.3024 (12) Å
b = 23.008 (3) Å
c = 15.279 (2) Å
V = 2918.6 (7) Å3
Z = 4
Mo Kα radiation
μ = 5.28 mm−1
T = 293 K
0.20 × 0.18 × 0.16 mm
Data collection
Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.418, T max = 0.486
12346 measured reflections
1606 independent reflections
1216 reflections with I > 2σ(I)
R int = 0.048
Refinement
R[F 2 > 2σ(F 2)] = 0.032
wR(F 2) = 0.098
S = 1.07
1606 reflections
133 parameters
Only H-atom coordinates refined
Δρmax = 1.99 e Å−3
Δρmin = −0.72 e Å−3
Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2007 ▶); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008 ▶).
Supplementary Material
Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810054176/fi2098sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S1600536810054176/fi2098Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Table 1. Hydrogen-bond geometry (Å, °).
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| O1W—H1⋯O12i | 0.82 (9) | 2.06 (9) | 2.831 (11) | 157 (9) |
| O11—H4⋯O1W | 0.87 (11) | 1.81 (11) | 2.684 (13) | 180 (1) |
Symmetry code: (i) 
.
Acknowledgments
This work was supported financially by the National Natural Science Foundation of Heilongjiang Province (Nos. B200901 and B200917).
supplementary crystallographic information
Comment
Polyoxometalates(POMs) are metal-oxygen anionic clusters, which act as multidentate inorganic ligands. They can bind most transition metals, rare earth metals and alkali metals, leading to a family of compounds with a variety of structures (Pope, 1983). Performing as an important part in this field, a number of compounds from the A/Mo/P/O system have been synthesized and structurally characterized, where A is an organic or inorganic cation. In contrast to the rich structural chemistry of molybdenum phosphates, the Mo/As/O system remains relatively undeveloped (Sun et al., 2007; He & Wang, 1999). Here, we have hydrothermally synthesized the title compound, K5Mo8O24(OH)2AsO4.2H2O, which is isostructural with K5-x(NH4)xP[Mo4O14(OH)]2.2 H2O where x=2.43 (Chen et al. (2009).
The structure of the title compound consists of [AsMo8O28(OH)2]5-cluster anions, K+ cations, and water molecules (Fig. 1). The anion is formed by two crystallographically independent {Mo4O14(OH)}cores, linked by an arsenic(V) atom in a sandwich-like fashion. The anion possesses m2m symmetry in that all four molybdenum atoms in the {Mo4O14(OH)}core are coplanar, and one oxygen atom in each core is characterized as hydroxyl (O4 and O11) which is indicated by literature and bond valence sum calculation value (Hsu & Wang 1997, Brown et al., 1981). The [AsMo8O30H2]5-cluster anions are bridged together by K+ cations into one-dimensional strings firstly. The anion-cation interactions are further extended into a three-dimensional architecture by other two K+ cations with each linking four cluster anions and one water molecule.
Experimental
The title compound was synthesized by hydrothermal reaction of Fe(NO3)3.9 H2O(2.5 mmol),As2O3 (2.5 mmol), MoO3.2H2O (3.0 mmol),KOH (5.0 mmol) and H2O(18 ml) were stirred for 120 min. The pH of the mixture was adjusted to 6.5 with 1M nitric acid. The resultant mixture was sealed in a 25 ml Teflon-lined autoclave andheated at 180 oC for 8 d. The autoclave was then cooled to room temperature. The crystalline product was filtered, washed with distilled water and dried at ambient temperature to give black block solids.
Refinement
The H atoms attached to oxygen molecular were located from difference Fourier maps, and the H atom attached o2w was disordered. The highest peak in the Fourier map is located 1.30Å from O9.
Figures
Fig. 1.
ORTEP drawing of the title compound withthermal ellipsoids at 50% probability.
Fig. 2.
A polyhedral representationof the three-dimensional network structure of the title compound. All of the water molecular is omitted forclarity. [symmetry codes:(i) x, y,z; (ii) -x, -y, 1/2 + z; (iii) x, -y, -z; (iv) -x, y, 1/2 - z; (v) -x, -y, -z; (vi) x, y, 1/2 + z; (vii) -x, y, z; (viii) x, -y, 1/2 + z.]
Crystal data
| K5[Mo8O24(OH)2(AsO4)]·2H2O | F(000) = 2904 |
| Mr = 1553.95 | Dx = 3.541 Mg m−3 |
| Orthorhombic, Cmcm | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -C 2c 2 | Cell parameters from 3063 reflections |
| a = 8.3024 (12) Å | θ = 2.6–26.0° |
| b = 23.008 (3) Å | µ = 5.28 mm−1 |
| c = 15.279 (2) Å | T = 293 K |
| V = 2918.6 (7) Å3 | Block, black |
| Z = 4 | 0.20 × 0.18 × 0.16 mm |
Data collection
| Rigaku R-AXIS RAPID diffractometer | 1606 independent reflections |
| Radiation source: fine-focus sealed tube | 1216 reflections with I > 2σ(I) |
| graphite | Rint = 0.048 |
| Detector resolution: 10 pixels mm-1 | θmax = 26.0°, θmin = 2.2° |
| ω scans | h = −10→10 |
| Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −28→28 |
| Tmin = 0.418, Tmax = 0.486 | l = −18→18 |
| 12346 measured reflections |
Refinement
| Refinement on F2 | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| R[F2 > 2σ(F2)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.098 | Only H-atom coordinates refined |
| S = 1.07 | w = 1/[σ2(Fo2) + (0.055P)2] where P = (Fo2 + 2Fc2)/3 |
| 1606 reflections | (Δ/σ)max < 0.001 |
| 133 parameters | Δρmax = 1.99 e Å−3 |
| 0 restraints | Δρmin = −0.72 e Å−3 |
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)
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| O2W | 0.5000 | 0.3660 (4) | 0.7500 | 0.046 (3) | |
| H2W | 0.4128 | 0.3599 | 0.7224 | 0.069* | 0.50 |
| Mo1 | 0.30043 (6) | 0.49010 (2) | 0.35477 (3) | 0.01904 (18) | |
| Mo2 | 0.30698 (6) | 0.26333 (2) | 0.35911 (3) | 0.02029 (18) | |
| As1 | 0.5000 | 0.37665 (4) | 0.2500 | 0.0140 (3) | |
| K1 | 0.0000 | 0.38267 (14) | 0.2500 | 0.0504 (10) | |
| K2 | 0.5000 | 0.12103 (8) | 0.46558 (14) | 0.0300 (5) | |
| K3 | 0.5000 | 0.36453 (9) | 0.52457 (14) | 0.0341 (5) | |
| O12 | 0.1808 (7) | 0.5103 (3) | 0.2500 | 0.0332 (16) | |
| O11 | 0.5000 | 0.2312 (3) | 0.2500 | 0.0198 (18) | |
| O10 | 0.1715 (6) | 0.4466 (2) | 0.4095 (3) | 0.0379 (12) | |
| O9 | 0.5000 | 0.4605 (3) | 0.3962 (4) | 0.0328 (15) | |
| O8 | 0.2890 (6) | 0.55608 (19) | 0.4041 (3) | 0.0404 (13) | |
| O7 | 0.2196 (7) | 0.1971 (2) | 0.3681 (3) | 0.0516 (15) | |
| O6 | 0.5000 | 0.2443 (3) | 0.4234 (4) | 0.0341 (16) | |
| O5 | 0.2029 (6) | 0.30763 (19) | 0.4280 (3) | 0.0382 (12) | |
| O4 | 0.5000 | 0.5206 (3) | 0.2500 | 0.0189 (17) | |
| O3 | 0.3350 (7) | 0.4194 (2) | 0.2500 | 0.0268 (14) | |
| O2 | 0.5000 | 0.3333 (2) | 0.3397 (4) | 0.0288 (15) | |
| O1 | 0.2301 (8) | 0.2928 (3) | 0.2500 | 0.0338 (15) | |
| O1W | 0.5000 | 0.1146 (4) | 0.2500 | 0.067 (5) | |
| H1 | 0.426 (11) | 0.091 (4) | 0.2500 | 0.04 (3)* | |
| H4 | 0.5000 | 0.193 (5) | 0.2500 | 0.02 (3)* | |
| H3 | 0.5000 | 0.562 (5) | 0.2500 | 0.02 (3)* |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| O2W | 0.046 (7) | 0.017 (5) | 0.076 (8) | 0.000 | 0.000 | 0.000 |
| Mo1 | 0.0219 (3) | 0.0168 (3) | 0.0184 (3) | 0.0015 (2) | 0.0028 (2) | −0.00153 (19) |
| Mo2 | 0.0246 (4) | 0.0173 (3) | 0.0190 (3) | −0.0017 (2) | 0.0040 (2) | 0.00186 (19) |
| As1 | 0.0179 (6) | 0.0104 (5) | 0.0138 (6) | 0.000 | 0.000 | 0.000 |
| K1 | 0.0242 (18) | 0.047 (2) | 0.080 (3) | 0.000 | 0.000 | 0.000 |
| K2 | 0.0328 (12) | 0.0281 (11) | 0.0291 (11) | 0.000 | 0.000 | −0.0002 (8) |
| K3 | 0.0390 (13) | 0.0324 (11) | 0.0310 (11) | 0.000 | 0.000 | −0.0039 (9) |
| O12 | 0.027 (4) | 0.039 (4) | 0.034 (4) | 0.006 (3) | 0.000 | 0.000 |
| O11 | 0.032 (5) | 0.012 (4) | 0.016 (4) | 0.000 | 0.000 | 0.000 |
| O10 | 0.036 (3) | 0.035 (3) | 0.042 (3) | −0.004 (2) | 0.016 (2) | 0.000 (2) |
| O9 | 0.029 (4) | 0.038 (4) | 0.031 (4) | 0.000 | 0.000 | 0.005 (3) |
| O8 | 0.051 (4) | 0.028 (2) | 0.042 (3) | 0.005 (2) | 0.006 (3) | −0.006 (2) |
| O7 | 0.058 (4) | 0.031 (3) | 0.066 (4) | −0.013 (3) | 0.021 (3) | 0.006 (2) |
| O6 | 0.042 (4) | 0.035 (4) | 0.025 (3) | 0.000 | 0.000 | 0.005 (3) |
| O5 | 0.046 (3) | 0.034 (3) | 0.034 (3) | 0.002 (2) | 0.021 (2) | 0.000 (2) |
| O4 | 0.021 (5) | 0.009 (4) | 0.027 (4) | 0.000 | 0.000 | 0.000 |
| O3 | 0.030 (4) | 0.025 (3) | 0.025 (3) | −0.006 (3) | 0.000 | 0.000 |
| O2 | 0.032 (4) | 0.027 (3) | 0.027 (3) | 0.000 | 0.000 | −0.005 (3) |
| O1 | 0.029 (4) | 0.047 (4) | 0.026 (3) | 0.003 (3) | 0.000 | 0.000 |
| O1W | 0.039 (8) | 0.012 (5) | 0.150 (14) | 0.000 | 0.000 | 0.000 |
Geometric parameters (Å, °)
| Mo1—O10 | 1.687 (4) | K2—O8viii | 2.979 (5) |
| Mo1—O8 | 1.697 (4) | K2—O8ix | 2.979 (5) |
| Mo1—O9 | 1.900 (3) | K2—O7ii | 3.272 (6) |
| Mo1—O12 | 1.940 (3) | K2—O7 | 3.272 (6) |
| Mo1—O3 | 2.300 (4) | K2—O1W | 3.297 (2) |
| Mo1—O4 | 2.409 (2) | K2—O1W | 3.297 (2) |
| Mo1—Mo1i | 3.2015 (10) | K2—Mo2ii | 3.9915 (18) |
| Mo1—K1 | 3.859 (2) | K3—O8x | 2.756 (5) |
| Mo2—O7 | 1.692 (5) | K3—O8xi | 2.756 (5) |
| Mo2—O5 | 1.701 (4) | K3—O7vi | 2.833 (5) |
| Mo2—O1 | 1.910 (3) | K3—O7vii | 2.833 (5) |
| Mo2—O6 | 1.930 (3) | K3—O2 | 2.914 (6) |
| Mo2—O2 | 2.291 (4) | K3—O9 | 2.953 (6) |
| Mo2—O11 | 2.427 (2) | K3—O5 | 3.158 (5) |
| Mo2—Mo2ii | 3.2050 (12) | K3—O5ii | 3.158 (5) |
| Mo2—K3 | 3.792 (2) | K3—O6 | 3.168 (6) |
| Mo2—K2 | 3.9915 (18) | K3—Mo2ii | 3.7922 (19) |
| Mo2—K1 | 4.100 (2) | K3—K2xii | 4.1672 (6) |
| As1—O3iii | 1.687 (6) | O12—Mo1i | 1.940 (3) |
| As1—O3 | 1.687 (6) | O11—Mo2ii | 2.427 (2) |
| As1—O2 | 1.695 (6) | O11—Mo2i | 2.427 (2) |
| As1—O2i | 1.695 (6) | O11—Mo2iii | 2.427 (2) |
| K1—O1iv | 2.815 (7) | O10—K2vii | 2.844 (5) |
| K1—O1 | 2.815 (7) | O9—Mo1ii | 1.900 (3) |
| K1—O3 | 2.907 (6) | O8—K3x | 2.756 (5) |
| K1—O3iv | 2.907 (6) | O8—K2xiii | 2.979 (5) |
| K1—O10 | 3.183 (5) | O7—K3vii | 2.833 (5) |
| K1—O10v | 3.183 (5) | O6—Mo2ii | 1.930 (3) |
| K1—O10iv | 3.183 (5) | O5—K2vii | 2.859 (4) |
| K1—O10i | 3.183 (5) | O4—Mo1i | 2.409 (2) |
| K1—O12iv | 3.298 (7) | O4—Mo1ii | 2.409 (2) |
| K1—O12 | 3.298 (7) | O4—Mo1iii | 2.409 (2) |
| K1—Mo1i | 3.859 (2) | O3—Mo1i | 2.300 (4) |
| K2—O10vi | 2.844 (5) | O2—Mo2ii | 2.291 (4) |
| K2—O10vii | 2.844 (5) | O1—Mo2i | 1.910 (3) |
| K2—O5vi | 2.859 (4) | O1W—O1W | 0.00 (2) |
| K2—O5vii | 2.859 (4) | O1W—K2i | 3.297 (2) |
| K2—O6 | 2.909 (6) | ||
| O10—Mo1—O8 | 106.0 (2) | O10vi—K2—O7ii | 104.00 (13) |
| O10—Mo1—O9 | 100.1 (2) | O10vii—K2—O7ii | 162.64 (14) |
| O8—Mo1—O9 | 102.8 (3) | O5vi—K2—O7ii | 62.12 (14) |
| O10—Mo1—O12 | 103.1 (2) | O5vii—K2—O7ii | 111.77 (14) |
| O8—Mo1—O12 | 97.1 (2) | O6—K2—O7ii | 51.49 (10) |
| O9—Mo1—O12 | 143.8 (2) | O8viii—K2—O7ii | 134.27 (14) |
| O10—Mo1—O3 | 90.3 (2) | O8ix—K2—O7ii | 63.37 (14) |
| O8—Mo1—O3 | 161.5 (2) | O10vi—K2—O7 | 162.64 (14) |
| O9—Mo1—O3 | 82.5 (2) | O10vii—K2—O7 | 104.00 (13) |
| O12—Mo1—O3 | 70.04 (19) | O5vi—K2—O7 | 111.77 (14) |
| O10—Mo1—O4 | 159.8 (2) | O5vii—K2—O7 | 62.12 (13) |
| O8—Mo1—O4 | 94.2 (2) | O6—K2—O7 | 51.49 (10) |
| O9—Mo1—O4 | 74.11 (18) | O8viii—K2—O7 | 63.37 (13) |
| O12—Mo1—O4 | 74.57 (16) | O8ix—K2—O7 | 134.27 (14) |
| O3—Mo1—O4 | 70.0 (2) | O7ii—K2—O7 | 90.72 (18) |
| O10—Mo1—Mo1i | 119.71 (17) | O10vi—K2—O1W | 130.22 (18) |
| O8—Mo1—Mo1i | 116.36 (16) | O10vii—K2—O1W | 130.22 (18) |
| O9—Mo1—Mo1i | 109.46 (18) | O5vi—K2—O1W | 126.43 (16) |
| O12—Mo1—Mo1i | 34.40 (15) | O5vii—K2—O1W | 126.43 (16) |
| O3—Mo1—Mo1i | 45.89 (10) | O6—K2—O1W | 79.8 (2) |
| O4—Mo1—Mo1i | 48.35 (5) | O8viii—K2—O1W | 70.27 (14) |
| O10—Mo1—K1 | 54.24 (16) | O8ix—K2—O1W | 70.27 (14) |
| O8—Mo1—K1 | 136.12 (19) | O7ii—K2—O1W | 64.48 (14) |
| O9—Mo1—K1 | 118.16 (19) | O7—K2—O1W | 64.48 (14) |
| O12—Mo1—K1 | 58.68 (19) | O10vi—K2—O1W | 130.22 (18) |
| O3—Mo1—K1 | 48.63 (15) | O10vii—K2—O1W | 130.22 (18) |
| O4—Mo1—K1 | 110.84 (10) | O5vi—K2—O1W | 126.43 (16) |
| Mo1i—Mo1—K1 | 65.495 (16) | O5vii—K2—O1W | 126.43 (16) |
| O7—Mo2—O5 | 105.7 (2) | O6—K2—O1W | 79.8 (2) |
| O7—Mo2—O1 | 104.3 (3) | O8viii—K2—O1W | 70.27 (14) |
| O5—Mo2—O1 | 99.1 (2) | O8ix—K2—O1W | 70.27 (14) |
| O7—Mo2—O6 | 96.4 (3) | O7ii—K2—O1W | 64.48 (14) |
| O5—Mo2—O6 | 104.0 (2) | O7—K2—O1W | 64.48 (14) |
| O1—Mo2—O6 | 143.4 (2) | O1W—K2—O1W | 0.0 (4) |
| O7—Mo2—O2 | 160.5 (2) | O10vi—K2—Mo2ii | 121.40 (10) |
| O5—Mo2—O2 | 90.80 (19) | O10vii—K2—Mo2ii | 157.37 (11) |
| O1—Mo2—O2 | 82.6 (2) | O5vi—K2—Mo2ii | 61.60 (9) |
| O6—Mo2—O2 | 69.15 (19) | O5vii—K2—Mo2ii | 89.85 (10) |
| O7—Mo2—O11 | 93.7 (2) | O6—K2—Mo2ii | 27.12 (6) |
| O5—Mo2—O11 | 160.5 (2) | O8viii—K2—Mo2ii | 127.33 (10) |
| O1—Mo2—O11 | 74.28 (19) | O8ix—K2—Mo2ii | 87.68 (9) |
| O6—Mo2—O11 | 74.49 (16) | O7ii—K2—Mo2ii | 24.47 (9) |
| O2—Mo2—O11 | 70.33 (19) | O7—K2—Mo2ii | 70.20 (9) |
| O7—Mo2—Mo2ii | 115.4 (2) | O1W—K2—Mo2ii | 68.26 (16) |
| O5—Mo2—Mo2ii | 120.53 (17) | O1W—K2—Mo2ii | 68.26 (16) |
| O1—Mo2—Mo2ii | 109.53 (19) | O8x—K3—O8xi | 78.9 (2) |
| O6—Mo2—Mo2ii | 33.86 (14) | O8x—K3—O7vi | 72.18 (16) |
| O2—Mo2—Mo2ii | 45.62 (10) | O8xi—K3—O7vi | 120.80 (17) |
| O11—Mo2—Mo2ii | 48.69 (5) | O8x—K3—O7vii | 120.80 (17) |
| O7—Mo2—K3 | 132.82 (18) | O8xi—K3—O7vii | 72.18 (16) |
| O5—Mo2—K3 | 55.55 (17) | O7vi—K3—O7vii | 80.1 (2) |
| O1—Mo2—K3 | 120.34 (19) | O8x—K3—O2 | 123.14 (14) |
| O6—Mo2—K3 | 56.54 (18) | O8xi—K3—O2 | 123.14 (14) |
| O2—Mo2—K3 | 50.13 (14) | O7vi—K3—O2 | 115.96 (14) |
| O11—Mo2—K3 | 111.44 (10) | O7vii—K3—O2 | 115.96 (14) |
| Mo2ii—Mo2—K3 | 65.002 (16) | O8x—K3—O9 | 76.54 (14) |
| O7—Mo2—K2 | 53.2 (2) | O8xi—K3—O9 | 76.54 (14) |
| O5—Mo2—K2 | 116.31 (15) | O7vi—K3—O9 | 139.37 (12) |
| O1—Mo2—K2 | 141.38 (18) | O7vii—K3—O9 | 139.37 (12) |
| O6—Mo2—K2 | 43.40 (17) | O2—K3—O9 | 62.64 (17) |
| O2—Mo2—K2 | 110.39 (11) | O8x—K3—O5 | 162.95 (14) |
| O11—Mo2—K2 | 76.43 (14) | O8xi—K3—O5 | 87.88 (13) |
| Mo2ii—Mo2—K2 | 66.329 (14) | O7vi—K3—O5 | 124.43 (15) |
| K3—Mo2—K2 | 93.57 (4) | O7vii—K3—O5 | 63.91 (14) |
| O7—Mo2—K1 | 111.7 (2) | O2—K3—O5 | 56.30 (9) |
| O5—Mo2—K1 | 62.27 (16) | O9—K3—O5 | 89.98 (12) |
| O1—Mo2—K1 | 36.82 (17) | O8x—K3—O5ii | 87.88 (13) |
| O6—Mo2—K1 | 151.01 (18) | O8xi—K3—O5ii | 162.95 (14) |
| O2—Mo2—K1 | 84.92 (11) | O7vi—K3—O5ii | 63.91 (14) |
| O11—Mo2—K1 | 109.56 (11) | O7vii—K3—O5ii | 124.43 (15) |
| Mo2ii—Mo2—K1 | 128.43 (3) | O2—K3—O5ii | 56.30 (9) |
| K3—Mo2—K1 | 97.04 (4) | O9—K3—O5ii | 89.98 (12) |
| K2—Mo2—K1 | 164.67 (4) | O5—K3—O5ii | 102.71 (16) |
| O3iii—As1—O3 | 108.6 (4) | O8x—K3—O6 | 140.50 (10) |
| O3iii—As1—O2 | 110.06 (13) | O8xi—K3—O6 | 140.50 (10) |
| O3—As1—O2 | 110.06 (13) | O7vi—K3—O6 | 81.10 (14) |
| O3iii—As1—O2i | 110.06 (13) | O7vii—K3—O6 | 81.10 (14) |
| O3—As1—O2i | 110.06 (13) | O2—K3—O6 | 46.54 (15) |
| O2—As1—O2i | 108.0 (4) | O9—K3—O6 | 109.18 (17) |
| O1iv—K1—O1 | 85.5 (3) | O5—K3—O6 | 53.87 (9) |
| O1iv—K1—O3 | 149.7 (2) | O5ii—K3—O6 | 53.87 (9) |
| O1—K1—O3 | 64.18 (17) | O8x—K3—Mo2 | 159.94 (12) |
| O1iv—K1—O3iv | 64.18 (17) | O8xi—K3—Mo2 | 113.71 (10) |
| O1—K1—O3iv | 149.7 (2) | O7vi—K3—Mo2 | 110.51 (12) |
| O3—K1—O3iv | 146.2 (3) | O7vii—K3—Mo2 | 78.84 (11) |
| O1iv—K1—O10 | 130.02 (9) | O2—K3—Mo2 | 37.12 (8) |
| O1—K1—O10 | 92.05 (13) | O9—K3—Mo2 | 90.93 (12) |
| O3—K1—O10 | 55.77 (9) | O5—K3—Mo2 | 26.37 (8) |
| O3iv—K1—O10 | 107.08 (13) | O5ii—K3—Mo2 | 76.36 (9) |
| O1iv—K1—O10v | 92.05 (13) | O6—K3—Mo2 | 30.55 (6) |
| O1—K1—O10v | 130.02 (9) | O8x—K3—Mo2ii | 113.71 (10) |
| O3—K1—O10v | 107.08 (13) | O8xi—K3—Mo2ii | 159.94 (12) |
| O3iv—K1—O10v | 55.77 (9) | O7vi—K3—Mo2ii | 78.84 (11) |
| O10—K1—O10v | 53.16 (17) | O7vii—K3—Mo2ii | 110.51 (12) |
| O1iv—K1—O10iv | 92.05 (13) | O2—K3—Mo2ii | 37.12 (8) |
| O1—K1—O10iv | 130.02 (9) | O9—K3—Mo2ii | 90.93 (12) |
| O3—K1—O10iv | 107.08 (13) | O5—K3—Mo2ii | 76.36 (9) |
| O3iv—K1—O10iv | 55.77 (9) | O5ii—K3—Mo2ii | 26.37 (8) |
| O10—K1—O10iv | 125.0 (2) | O6—K3—Mo2ii | 30.55 (6) |
| O10v—K1—O10iv | 99.94 (17) | Mo2—K3—Mo2ii | 50.00 (3) |
| O1iv—K1—O10i | 130.02 (9) | O8x—K3—K2xii | 45.54 (10) |
| O1—K1—O10i | 92.05 (13) | O8xi—K3—K2xii | 124.48 (12) |
| O3—K1—O10i | 55.77 (9) | O7vi—K3—K2xii | 51.54 (12) |
| O3iv—K1—O10i | 107.08 (13) | O7vii—K3—K2xii | 131.30 (14) |
| O10—K1—O10i | 99.94 (17) | O2—K3—K2xii | 93.13 (4) |
| O10v—K1—O10i | 125.0 (2) | O9—K3—K2xii | 87.96 (4) |
| O10iv—K1—O10i | 53.16 (17) | O5—K3—K2xii | 145.89 (10) |
| O1iv—K1—O12iv | 110.18 (16) | O5ii—K3—K2xii | 43.27 (8) |
| O1—K1—O12iv | 164.35 (19) | O6—K3—K2xii | 95.00 (4) |
| O3—K1—O12iv | 100.17 (18) | Mo2—K3—K2xii | 119.60 (5) |
| O3iv—K1—O12iv | 46.00 (15) | Mo2ii—K3—K2xii | 69.64 (3) |
| O10—K1—O12iv | 78.02 (13) | Mo1—O12—Mo1i | 111.2 (3) |
| O10v—K1—O12iv | 52.04 (9) | Mo1—O12—K1 | 91.2 (2) |
| O10iv—K1—O12iv | 52.04 (9) | Mo1i—O12—K1 | 91.2 (2) |
| O10i—K1—O12iv | 78.02 (13) | Mo2ii—O11—Mo2i | 144.6 (3) |
| O1iv—K1—O12 | 164.35 (19) | Mo2ii—O11—Mo2iii | 86.75 (11) |
| O1—K1—O12 | 110.18 (16) | Mo2i—O11—Mo2iii | 82.63 (10) |
| O3—K1—O12 | 46.00 (15) | Mo2ii—O11—Mo2 | 82.63 (10) |
| O3iv—K1—O12 | 100.17 (18) | Mo2i—O11—Mo2 | 86.75 (11) |
| O10—K1—O12 | 52.04 (9) | Mo2iii—O11—Mo2 | 144.6 (3) |
| O10v—K1—O12 | 78.02 (13) | Mo1—O10—K2vii | 167.1 (3) |
| O10iv—K1—O12 | 78.02 (13) | Mo1—O10—K1 | 100.3 (2) |
| O10i—K1—O12 | 52.04 (9) | K2vii—O10—K1 | 92.12 (14) |
| O12iv—K1—O12 | 54.2 (2) | Mo1ii—O9—Mo1 | 121.4 (3) |
| O1iv—K1—Mo1 | 155.37 (3) | Mo1ii—O9—K3 | 119.31 (16) |
| O1—K1—Mo1 | 91.82 (12) | Mo1—O9—K3 | 119.31 (16) |
| O3—K1—Mo1 | 36.42 (8) | Mo1—O8—K3x | 137.1 (3) |
| O3iv—K1—Mo1 | 115.59 (13) | Mo1—O8—K2xiii | 129.3 (3) |
| O10—K1—Mo1 | 25.48 (8) | K3x—O8—K2xiii | 93.14 (13) |
| O10v—K1—Mo1 | 71.07 (10) | Mo2—O7—K3vii | 140.7 (3) |
| O10iv—K1—Mo1 | 108.11 (12) | Mo2—O7—K2 | 102.3 (3) |
| O10i—K1—Mo1 | 74.48 (9) | K3vii—O7—K2 | 85.77 (13) |
| O12iv—K1—Mo1 | 73.98 (11) | Mo2ii—O6—Mo2 | 112.3 (3) |
| O12—K1—Mo1 | 30.17 (6) | Mo2ii—O6—K2 | 109.48 (19) |
| O1iv—K1—Mo1i | 155.37 (3) | Mo2—O6—K2 | 109.48 (19) |
| O1—K1—Mo1i | 91.82 (12) | Mo2ii—O6—K3 | 92.91 (19) |
| O3—K1—Mo1i | 36.42 (8) | Mo2—O6—K3 | 92.91 (19) |
| O3iv—K1—Mo1i | 115.59 (13) | K2—O6—K3 | 138.0 (2) |
| O10—K1—Mo1i | 74.48 (9) | Mo2—O5—K2vii | 174.3 (3) |
| O10v—K1—Mo1i | 108.11 (12) | Mo2—O5—K3 | 98.1 (2) |
| O10iv—K1—Mo1i | 71.07 (10) | K2vii—O5—K3 | 87.51 (12) |
| O10i—K1—Mo1i | 25.48 (8) | Mo1i—O4—Mo1ii | 146.1 (3) |
| O12iv—K1—Mo1i | 73.98 (11) | Mo1i—O4—Mo1 | 83.31 (9) |
| O12—K1—Mo1i | 30.17 (6) | Mo1ii—O4—Mo1 | 86.93 (10) |
| Mo1—K1—Mo1i | 49.01 (3) | Mo1i—O4—Mo1iii | 86.93 (10) |
| O10vi—K2—O10vii | 60.1 (2) | Mo1ii—O4—Mo1iii | 83.31 (9) |
| O10vi—K2—O5vi | 68.74 (15) | Mo1—O4—Mo1iii | 146.1 (3) |
| O10vii—K2—O5vi | 103.14 (16) | As1—O3—Mo1i | 120.9 (2) |
| O10vi—K2—O5vii | 103.14 (16) | As1—O3—Mo1 | 120.9 (2) |
| O10vii—K2—O5vii | 68.74 (15) | Mo1i—O3—Mo1 | 88.2 (2) |
| O5vi—K2—O5vii | 72.2 (2) | As1—O3—K1 | 127.4 (3) |
| O10vi—K2—O6 | 132.99 (14) | Mo1i—O3—K1 | 94.95 (18) |
| O10vii—K2—O6 | 132.99 (14) | Mo1—O3—K1 | 94.95 (18) |
| O5vi—K2—O6 | 64.28 (13) | As1—O2—Mo2 | 121.18 (19) |
| O5vii—K2—O6 | 64.28 (13) | As1—O2—Mo2ii | 121.18 (19) |
| O10vi—K2—O8viii | 109.91 (14) | Mo2—O2—Mo2ii | 88.8 (2) |
| O10vii—K2—O8viii | 62.22 (14) | As1—O2—K3 | 129.7 (3) |
| O5vi—K2—O8viii | 160.37 (15) | Mo2—O2—K3 | 92.75 (17) |
| O5vii—K2—O8viii | 89.59 (13) | Mo2ii—O2—K3 | 92.75 (17) |
| O6—K2—O8viii | 114.80 (11) | Mo2—O1—Mo2i | 121.6 (3) |
| O10vi—K2—O8ix | 62.22 (14) | Mo2—O1—K1 | 119.19 (17) |
| O10vii—K2—O8ix | 109.91 (14) | Mo2i—O1—K1 | 119.19 (17) |
| O5vi—K2—O8ix | 89.59 (13) | O1W—O1W—K2i | 0(10) |
| O5vii—K2—O8ix | 160.37 (15) | O1W—O1W—K2 | 0(10) |
| O6—K2—O8ix | 114.80 (11) | K2i—O1W—K2 | 174.9 (4) |
| O8viii—K2—O8ix | 107.32 (19) |
Symmetry codes: (i) x, y, −z+1/2; (ii) −x+1, y, z; (iii) −x+1, y, −z+1/2; (iv) −x, y, −z+1/2; (v) −x, y, z; (vi) x+1/2, −y+1/2, −z+1; (vii) −x+1/2, −y+1/2, −z+1; (viii) −x+1/2, y−1/2, z; (ix) x+1/2, y−1/2, z; (x) −x+1, −y+1, −z+1; (xi) x, −y+1, −z+1; (xii) −x+3/2, −y+1/2, −z+1; (xiii) x−1/2, y+1/2, z.
Hydrogen-bond geometry (Å, °)
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1W—H1···O12xiv | 0.82 (9) | 2.06 (9) | 2.831 (11) | 157 (9) |
| O11—H4···O1W | 0.87 (11) | 1.81 (11) | 2.684 (13) | 180.(1) |
Symmetry codes: (xiv) −x+1/2, y−1/2, −z+1/2.
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FI2098).
References
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810054176/fi2098sup1.cif
Structure factors: contains datablocks I. DOI: 10.1107/S1600536810054176/fi2098Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report