New girdle-like Mo18 polyanions linked into chains

Liu, G.; Zhang, S.-W.

doi:10.1107/S0108270101017206

New girdle-like Mo₁₈ polyanions linked into chains

From the reduction of heptamolybdate, a polyoxomolybdate was obtained with the formula [Na $_{6}^{+}$ (H₂O)₁₆(NH₂CH₂COO) $_{2}^{-}$ ]⁴⁺·{Na⁺[H₉Mo $_{10}^{\rm VI}$ Mo $_{8}^{\rm V}$ O₅₆(NH₂CH₂COO) $_{2}^{-}$ ]^5-}^4-·20H₂O, i.e. heptasodium nonahydrogen tetracarbamate hexadecaaquahexapentacontaoxaoctadecamolybdate(V,VI) icosahydrate. The 18 Mo atoms are connected by bridging O atoms to form a centrosymmetric girdle-like structure, in which Mo^V-Mo^V units are found. An Na⁺ cation occupies the central hole of the girdle, while four Na⁺ cations are bonded to the O atoms on the girdle edge. The girdles are linked into a one-dimensional chain by the other Na⁺ cations.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101017206/ta1340sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S0108270101017206/ta1340Isup2.hkl Contains datablock I

CCDC reference: 181989

Comment top

Polyoxometalates are molecular metal-oxygen clusters that are of fundamental and practical interest (Pope, 1983; Pope & Müller, 1994). One large branch of these are polyoxomolybdates. Traditional high-nuclearity oxomolybdenum complexes contain Mo^VI centers only (iso- and heteropolymolybdates) or both Mo^V and Mo^VI centers with delocalized d-electrons (heteropoly blues) (Chae et al., 1993). However, a new family of polyoxomolybdates whose Mo^V d-electrons are localized in Mo^V—Mo^V single bonds has emerged in recent years (Chae et al., 1993; Müller et al., 1998; Müller et al., 1999). Chae et al. (1993) concluded that all these compounds have [Mo^V₂O₈]^6- units (Scheme I). Within this unit, the Mo^V—Mo^V bond distance lies in the 2.5–2.7 Å range, while Mo^V—O bond distances are in the 1.6–1.8 Å range for Oa, the 1.9–2.0 Å range for Ob, and the 2.0–2.2 Å range for Oc. Frequently, but not always, a sixth oxygen ligand is weakly bonded to each Mo^V center trans to the Oa ligand. From the reduction of heptamolybdate in aqueous solution of glycine, we have synthesized several oxomolybdenum compounds containing [Mo^V₂O₈]^6- units (Liu, Wei et al., 2000a), among which are two interesting 18-Mo polyanions [Ca²⁺₄(H₂O)₂₂(NH₂CH₂COO^-)₂]⁶⁺. {Ca²⁺[Mo^VI₁₀Mo^V₈O₅₂(OH)₄(NH₃⁺CH₂COO^-)₂]^8-}^6-. 20H₂O (2) and [Ca²⁺₃(H₂O)₁₃(NH₃⁺CH₂COO^-)₃]⁶⁺. {Ca²⁺[Mo^VI₁₀Mo^V₈O₅₂(OH)₄(NH₃⁺CH₂COO^-)₂]^8-}^6-. 19H₂O (3) (Liu, Wei et al., 2000a). Here we report the structure of a new member of this family, [Na⁺₆(H₂O)₁₆(NH₂CH₂COO^-)₂]⁴⁺. {Na⁺[H₉Mo^VI₁₀Mo^V₈O₅₆(NH₂CH₂COO^-)₂]^5-}^4-. 20H₂O (1).

Compound (1) has an 18-Mo centrosymmetric girdle-like structure (Fig. 1). The Mo—O framework of the polyanion is approximately same as those of (2) and (3). Every Mo atom is coordinated by six oxygen atoms and sits in the center of a distorted octahedron. Eight Mo—O octahedra share edges and vertexes with each other to form an octagonal ring. Two octagonal rings, which are related by a symmetry center, overlap together through sixteen µ₃-O atoms to form a slightly ramped girdle. Two Mo centers are situated on the outer edges of the girdle and connect to other Mo centers through four µ-oxygen atoms. A characteristic of this complex is the existence of Mo—Mo single bonds between Mo1 and Mo2, Mo3 and Mo4 as well as their symmetrically equivalent ones. The bond distances are in the range given by Chae et al. (1993). The bond-valence sums of these eight Mo atoms are calculated as 5 according to bond-valence theory (Brown, 1981). The coordination environment of these Mo^V centers are also the same as Chae et al. (1993) described, showing [Mo^V₂O₁₀]^10- units which can be divided into [Mo^V₂O₈]^6- units and weakly coordinated oxygen atoms trans to the terminal oxygen atoms. Two glycine molecules connect Mo1 and Mo4 of the other ring in a µ₂-bridging mode with their carboxyl group. The structural characteristics described above are similar to those of (2) and (3) and can be regarded as common characteristics of this series of compounds.

There are seven Na⁺ cations in (1). One Na⁺ (Na1) is located at the centre of symmetry in the central hole of the girdle and is coordinated by six oxygen atoms of the Mo^V centers. The other six are on the periphery. Na3 is captured by the terminal oxygen atom (O21) of Mo7 and Na4 is captured by the terminal oxygen atom (O23) of Mo9. They stretch out of the girdle but are almost on the ring planes. Na3 and Na4 are connected by two µ₂-O atoms while coordinated by three water molecules each. Na2 sits above the ring plane and is coordinated by six oxygen atoms, two (O18, O20) from one polyanion, two (O19, O25) from another polyanion, and two (O32 and its symmetrically equivalent one) from the glycine molecules that also coordinate to Na1. The four terminal oxygen atoms coordinate to one Na2 cation each, but O32 bridges two adjacent Na2 in a µ₂ mode. Thus, there are two Na2 cations between two polyanions and these Na⁺ cations link the girdles into a one-dimensional chain (Fig 2).

The position of Na1 in (1) is the same as that of Ca1 in (2) and (3). Generally speaking, Na2 occupies a similar position to Ca2, while Na3 and Na4 occupy the similar positions of Ca3, but the number and coordination details of them are obviously different. However, the oxygen atoms of the polyanion that coordinate to them are similar. O18 and O25, the ones above the ring planes, as well as O21 and O23, the ones stretching out of the girdle but almost on the ring planes, all take part in the coordination to Na⁺ or Ca²⁺ cations. These terminal oxygen atoms can be regarded as the active positions of the polyanions. The similarity of a girdle-like backbone and active positions of these three compounds shows that they can be classified into a structural type with a formula of [Mo^VI₁₀Mo^V₈O₅₆(glycine)₂]^14-. This type of structure, like the famous structural types of Keggin and Dawson anions, can be modified by cations and organic acids while keeping its main structure unchanged.

There are ten water molecules not connected to metal ions per asymmetric unit. One of these waters of hydration is divided between 2 sites (OW14 and OW15, 1.54 Å apart) with occupancies that were fixed at 0.75 and 1/4, respectively, during refinement. No H atoms, except those of the methylene C atom of glycine, were included in this structure determination.

Experimental top

0.70 g (0.57 mmol) (NH₄)₆Mo₇O₂₄·4H₂O, 3.04 g (40.5 mmol) NH₂CH₂COOH, 2.00 g (34.2) mmol NaCl and 0.20 g (1.5 mmol) N₂H₄·H₂SO₄ were added into 60 ml (3.3 mol) water and the solution was stirred for 10 minutes while a color change occurred from yellow to green. The solution was stood without disturbance for one day while the color changed to red. Red crystals were obtained after half a month with the coexistence of a red precipitation. The crystals were carefully selected out and washed quickly with cold water and dried in air at room temperature.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1994); cell refinement: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1994); data reduction: TEXSAN (Molecular Structure Corporation, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Siemens, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top

	Fig. 1. The structure of (I) omitting some water molecules and all H atoms. Mo (large hatched spheres), Na (crossed), O (shaded), C (small hatched) and N (stippled).
	Fig. 2. The linking of girdles into one-dimensional chains.

(I) top

Crystal data top

C₈H₉₇Mo₁₈N₄Na₇O₁₀₀	Z = 1
M_r = 3737.75	F(000) = 1806
Triclinic, P1	D_x = 2.573 Mg m⁻³
a = 11.913 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 15.027 (3) Å	Cell parameters from 25 reflections
c = 15.466 (3) Å	θ = 5.0–11.2°
α = 114.37 (3)°	µ = 2.42 mm⁻¹
β = 99.00 (3)°	T = 293 K
γ = 99.17 (3)°	Planar, red-brown
V = 2412.6 (8) Å³	0.40 × 0.25 × 0.05 mm

Data collection top

AFC6S diffractometer	6755 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.033
Graphite monochromator	θ_max = 25.0°, θ_min = 1.5°
2θ scans	h = −14→13
Absorption correction: psi scan Coppens et al. (1965)	k = 0→17
T_min = 0.494, T_max = 0.886	l = −18→16
8848 measured reflections	3 standard reflections every 400 reflections
8499 independent reflections	intensity decay: 1%

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: hydrogen atoms are generated by HFIX instructions
R[F² > 2σ(F²)] = 0.056	H-atom parameters constrained
wR(F²) = 0.179	w = 1/[σ²(F_o²) + (0.1074P)² + 22.8082P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.004
8499 reflections	Δρ_max = 2.36 e Å⁻³
592 parameters	Δρ_min = −2.03 e Å⁻³
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00063 (17)

Crystal data top

C₈H₉₇Mo₁₈N₄Na₇O₁₀₀	γ = 99.17 (3)°
M_r = 3737.75	V = 2412.6 (8) Å³
Triclinic, P1	Z = 1
a = 11.913 (2) Å	Mo Kα radiation
b = 15.027 (3) Å	µ = 2.42 mm⁻¹
c = 15.466 (3) Å	T = 293 K
α = 114.37 (3)°	0.40 × 0.25 × 0.05 mm
β = 99.00 (3)°

Data collection top

AFC6S diffractometer	6755 reflections with I > 2σ(I)
Absorption correction: psi scan Coppens et al. (1965)	R_int = 0.033
T_min = 0.494, T_max = 0.886	3 standard reflections every 400 reflections
8848 measured reflections	intensity decay: 1%
8499 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.056	0 restraints
wR(F²) = 0.179	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.1074P)² + 22.8082P] where P = (F_o² + 2F_c²)/3
8499 reflections	Δρ_max = 2.36 e Å⁻³
592 parameters	Δρ_min = −2.03 e Å⁻³

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.

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) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mo1	0.45544 (7)	0.20523 (6)	0.41646 (6)	0.0200 (2)
Mo2	0.34451 (7)	0.23688 (6)	0.27704 (6)	0.0194 (2)
Mo3	0.39151 (7)	0.48204 (6)	0.24202 (6)	0.0192 (2)
Mo4	0.54359 (7)	0.65407 (6)	0.34949 (6)	0.0202 (2)
Mo5	0.18376 (7)	0.20589 (6)	0.44240 (6)	0.0229 (2)
Mo6	0.04084 (7)	0.23893 (6)	0.26445 (6)	0.0227 (2)
Mo7	0.08759 (7)	0.47684 (6)	0.23182 (6)	0.0223 (2)
Mo8	0.27859 (8)	0.69214 (6)	0.37146 (6)	0.0230 (2)
Mo9	0.19091 (8)	0.27778 (6)	0.11418 (6)	0.0227 (2)
Na1	0.5000	0.5000	0.5000	0.0234 (11)
Na2	0.0193 (4)	0.6066 (4)	0.4837 (3)	0.0364 (10)
Na3	−0.1946 (6)	0.3886 (5)	0.0111 (4)	0.0639 (16)
Na4	−0.0920 (7)	0.1558 (5)	−0.1174 (5)	0.081 (2)
O1	0.2953 (6)	0.1412 (5)	0.3319 (5)	0.0214 (14)
O2	0.3409 (6)	0.3537 (5)	0.2465 (5)	0.0199 (14)
O3	0.5696 (6)	0.2914 (5)	0.5514 (5)	0.0201 (14)
O4	0.2157 (5)	0.3017 (5)	0.3682 (5)	0.0193 (14)
O5	0.3897 (6)	0.6234 (5)	0.2605 (5)	0.0246 (15)
O6	0.3450 (5)	0.2730 (5)	0.5125 (5)	0.0205 (14)
O7	0.2234 (6)	0.4220 (5)	0.1462 (5)	0.0218 (14)
O8	0.0921 (6)	0.3446 (5)	0.2281 (5)	0.0243 (15)
O9	0.2608 (6)	0.5299 (5)	0.3369 (5)	0.0198 (14)
O10	0.5069 (6)	0.5307 (5)	0.3633 (5)	0.0201 (14)
O11	0.4717 (6)	0.3238 (5)	0.3922 (5)	0.0211 (14)
O12	0.1759 (6)	0.1899 (5)	0.1787 (5)	0.0203 (14)
O13	0.0662 (7)	0.1454 (5)	0.3186 (5)	0.0295 (16)
O14	0.1575 (6)	0.6113 (5)	0.2512 (5)	0.0246 (15)
O15	−0.0668 (7)	0.1576 (6)	0.1627 (6)	0.039 (2)
O16	0.5455 (6)	0.1385 (5)	0.3588 (5)	0.0282 (16)
O17	0.4089 (7)	0.1694 (6)	0.1909 (5)	0.0343 (18)
O18	0.0072 (7)	0.5069 (6)	0.3169 (6)	0.0348 (18)
O19	0.1131 (7)	0.2829 (6)	0.5172 (6)	0.0336 (17)
O20	0.1972 (7)	0.7089 (6)	0.4563 (6)	0.0356 (18)
O21	−0.0093 (7)	0.4395 (6)	0.1229 (5)	0.0349 (18)
O22	0.4623 (7)	0.4430 (6)	0.1519 (5)	0.0342 (18)
O23	0.0584 (7)	0.2315 (6)	0.0302 (5)	0.0371 (19)
O24	0.1623 (8)	0.0999 (6)	0.4621 (6)	0.042 (2)
O25	−0.0326 (7)	0.3065 (6)	0.3456 (6)	0.0335 (17)
O26	0.3000 (8)	0.8011 (6)	0.3580 (6)	0.041 (2)
O27	0.6462 (7)	0.6394 (6)	0.2828 (6)	0.0339 (17)
O28	0.2882 (7)	0.2366 (6)	0.0439 (6)	0.0365 (18)
O29	0.5689 (6)	0.8066 (5)	0.3650 (5)	0.0247 (15)
O30	0.4198 (6)	0.0970 (5)	0.4743 (5)	0.0260 (15)
C1	0.4089 (9)	0.1115 (8)	0.5588 (8)	0.025 (2)
C2	0.3630 (11)	0.0183 (8)	0.5699 (8)	0.033 (3)
H2A	0.2896	−0.0204	0.5212	0.080*
H2B	0.4187	−0.0233	0.5580	0.080*
N1	0.3437 (10)	0.0431 (7)	0.6682 (8)	0.044 (3)
O31	0.6987 (6)	0.5019 (5)	0.5047 (5)	0.0257 (15)
O32	0.1356 (7)	0.5209 (6)	0.5371 (6)	0.0354 (18)
C3	0.7563 (9)	0.4678 (8)	0.4436 (7)	0.025 (2)
C4	0.6899 (11)	0.4069 (13)	0.3367 (8)	0.057 (4)
H3	0.6299	0.3511	0.3303	0.080*
H4	0.6508	0.4493	0.3161	0.080*
N2	0.7656 (8)	0.3674 (8)	0.2725 (7)	0.039 (2)
OW1	−0.0816 (10)	0.3236 (9)	−0.1116 (8)	0.067 (3)
OW2	−0.1966 (11)	0.2371 (10)	0.0303 (11)	0.082 (4)
OW3	−0.1612 (10)	0.5559 (8)	0.0221 (8)	0.063 (3)
OW4	−0.3741 (11)	0.3253 (10)	−0.1074 (9)	0.076 (3)
OW5	−0.2671 (13)	0.4722 (11)	0.1542 (11)	0.098 (4)*
OW6	−0.1303 (18)	0.0181 (10)	−0.0618 (12)	0.128 (7)
OW7	−0.2476 (13)	0.0742 (11)	−0.2612 (11)	0.097 (4)*
OW8	0.0365 (15)	0.0607 (13)	−0.1996 (13)	0.118 (5)*
OW9	0.8268 (11)	1.1280 (9)	0.3740 (10)	0.091 (4)
OW10	−0.3233 (13)	0.1564 (11)	0.2121 (12)	0.098 (4)
OW11	0.5499 (15)	0.2530 (15)	0.0782 (15)	0.126 (6)
OW12	0.4416 (16)	0.8863 (12)	0.1906 (12)	0.121 (6)
OW13	0.085 (2)	0.3152 (18)	0.7134 (15)	0.154 (8)
OW14	0.624 (3)	0.663 (2)	0.074 (2)	0.161 (11)*	0.75
OW15	0.533 (5)	0.561 (4)	0.035 (4)	0.089 (15)*	0.25
OW16	0.204 (2)	0.181 (2)	0.744 (2)	0.204 (11)*
OW17	0.400 (3)	0.950 (3)	0.035 (3)	0.270 (16)*
OW18	0.272 (3)	0.049 (3)	−0.121 (3)	0.269 (16)*
OW19	−0.039 (5)	0.106 (4)	0.579 (4)	0.42 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0232 (5)	0.0173 (4)	0.0168 (4)	0.0034 (3)	0.0015 (3)	0.0068 (3)
Mo2	0.0218 (4)	0.0172 (4)	0.0160 (4)	0.0032 (3)	0.0016 (3)	0.0062 (3)
Mo3	0.0216 (4)	0.0196 (4)	0.0147 (4)	0.0036 (3)	0.0018 (3)	0.0075 (3)
Mo4	0.0221 (4)	0.0196 (4)	0.0167 (4)	0.0024 (3)	0.0021 (3)	0.0080 (3)
Mo5	0.0217 (5)	0.0241 (4)	0.0213 (4)	0.0014 (3)	0.0021 (3)	0.0114 (4)
Mo6	0.0195 (4)	0.0252 (5)	0.0188 (4)	0.0011 (3)	0.0004 (3)	0.0086 (4)
Mo7	0.0207 (4)	0.0242 (5)	0.0181 (4)	0.0044 (3)	−0.0001 (3)	0.0078 (3)
Mo8	0.0235 (5)	0.0206 (4)	0.0207 (4)	0.0059 (3)	−0.0002 (3)	0.0072 (3)
Mo9	0.0266 (5)	0.0222 (4)	0.0132 (4)	0.0031 (3)	0.0002 (3)	0.0050 (3)
Na1	0.024 (3)	0.027 (3)	0.020 (3)	0.006 (2)	0.006 (2)	0.011 (2)
Na2	0.031 (2)	0.043 (3)	0.029 (2)	0.010 (2)	0.0078 (19)	0.010 (2)
Na3	0.065 (4)	0.068 (4)	0.052 (3)	0.010 (3)	−0.004 (3)	0.029 (3)
Na4	0.081 (5)	0.064 (4)	0.062 (4)	0.004 (3)	−0.016 (4)	0.011 (3)
O1	0.017 (3)	0.018 (3)	0.024 (4)	−0.001 (3)	−0.002 (3)	0.009 (3)
O2	0.018 (3)	0.018 (3)	0.026 (4)	−0.004 (3)	0.005 (3)	0.015 (3)
O3	0.019 (3)	0.022 (3)	0.021 (3)	0.009 (3)	0.006 (3)	0.010 (3)
O4	0.013 (3)	0.020 (3)	0.023 (3)	−0.001 (3)	0.005 (3)	0.010 (3)
O5	0.031 (4)	0.023 (4)	0.017 (3)	0.011 (3)	−0.003 (3)	0.007 (3)
O6	0.015 (3)	0.024 (3)	0.020 (3)	0.003 (3)	0.003 (3)	0.009 (3)
O7	0.019 (3)	0.020 (3)	0.018 (3)	−0.002 (3)	−0.004 (3)	0.005 (3)
O8	0.032 (4)	0.021 (3)	0.019 (3)	0.008 (3)	0.004 (3)	0.009 (3)
O9	0.021 (3)	0.015 (3)	0.019 (3)	−0.001 (3)	−0.001 (3)	0.007 (3)
O10	0.021 (3)	0.017 (3)	0.021 (3)	−0.008 (3)	0.006 (3)	0.012 (3)
O11	0.027 (4)	0.018 (3)	0.017 (3)	−0.002 (3)	0.004 (3)	0.010 (3)
O12	0.019 (3)	0.022 (3)	0.019 (3)	0.001 (3)	0.004 (3)	0.010 (3)
O13	0.039 (4)	0.022 (4)	0.018 (4)	0.000 (3)	−0.004 (3)	0.007 (3)
O14	0.026 (4)	0.023 (4)	0.025 (4)	0.004 (3)	0.002 (3)	0.013 (3)
O15	0.027 (4)	0.042 (5)	0.031 (4)	−0.006 (3)	−0.008 (3)	0.009 (4)
O16	0.029 (4)	0.028 (4)	0.032 (4)	0.012 (3)	0.009 (3)	0.016 (3)
O17	0.039 (4)	0.032 (4)	0.024 (4)	0.010 (3)	0.006 (3)	0.005 (3)
O18	0.038 (4)	0.035 (4)	0.029 (4)	0.008 (3)	0.012 (3)	0.012 (3)
O19	0.027 (4)	0.044 (5)	0.036 (4)	0.011 (3)	0.014 (3)	0.020 (4)
O20	0.033 (4)	0.036 (4)	0.029 (4)	0.010 (3)	0.003 (3)	0.007 (3)
O21	0.036 (4)	0.038 (4)	0.023 (4)	0.001 (3)	−0.006 (3)	0.013 (3)
O22	0.047 (5)	0.027 (4)	0.022 (4)	0.006 (3)	0.008 (3)	0.006 (3)
O23	0.038 (5)	0.039 (4)	0.021 (4)	0.004 (4)	−0.007 (3)	0.007 (3)
O24	0.044 (5)	0.042 (5)	0.043 (5)	0.006 (4)	0.004 (4)	0.026 (4)
O25	0.034 (4)	0.042 (4)	0.028 (4)	0.012 (3)	0.011 (3)	0.017 (4)
O26	0.046 (5)	0.031 (4)	0.039 (5)	0.013 (4)	−0.006 (4)	0.011 (4)
O27	0.038 (4)	0.035 (4)	0.028 (4)	0.005 (3)	0.010 (3)	0.014 (3)
O28	0.045 (5)	0.037 (4)	0.025 (4)	0.013 (4)	0.010 (4)	0.010 (3)
O29	0.028 (4)	0.014 (3)	0.033 (4)	−0.007 (3)	0.004 (3)	0.016 (3)
O30	0.023 (4)	0.023 (4)	0.032 (4)	0.004 (3)	0.008 (3)	0.013 (3)
C1	0.024 (5)	0.025 (5)	0.028 (6)	0.008 (4)	0.000 (4)	0.014 (5)
C2	0.047 (7)	0.027 (6)	0.038 (6)	0.015 (5)	0.014 (5)	0.023 (5)
N1	0.069 (8)	0.033 (5)	0.037 (6)	0.001 (5)	0.019 (5)	0.023 (5)
O31	0.023 (4)	0.034 (4)	0.017 (3)	0.008 (3)	0.004 (3)	0.009 (3)
O32	0.029 (4)	0.042 (5)	0.031 (4)	0.013 (3)	0.009 (3)	0.010 (4)
C3	0.022 (5)	0.030 (5)	0.020 (5)	0.004 (4)	0.004 (4)	0.011 (4)
C4	0.024 (6)	0.102 (12)	0.019 (6)	0.018 (7)	0.010 (5)	0.001 (7)
N2	0.025 (5)	0.061 (7)	0.023 (5)	0.017 (5)	0.009 (4)	0.008 (5)
OW1	0.077 (8)	0.075 (7)	0.050 (6)	0.012 (6)	0.004 (5)	0.035 (6)
OW2	0.063 (8)	0.079 (8)	0.112 (11)	0.009 (6)	0.004 (7)	0.059 (8)
OW3	0.082 (8)	0.068 (7)	0.049 (6)	0.019 (6)	0.009 (5)	0.037 (5)
OW4	0.081 (8)	0.086 (8)	0.060 (7)	0.006 (7)	0.002 (6)	0.044 (7)
OW6	0.194 (19)	0.055 (8)	0.089 (11)	−0.003 (10)	0.022 (12)	0.004 (7)
OW9	0.074 (8)	0.064 (8)	0.092 (9)	−0.018 (6)	0.038 (7)	0.001 (7)
OW10	0.096 (10)	0.096 (10)	0.122 (12)	0.030 (8)	0.043 (9)	0.058 (9)
OW11	0.097 (12)	0.141 (15)	0.164 (17)	0.046 (11)	0.041 (12)	0.082 (14)
OW12	0.131 (14)	0.094 (11)	0.109 (12)	0.017 (10)	−0.026 (10)	0.042 (10)
OW13	0.18 (2)	0.21 (2)	0.140 (17)	0.092 (18)	0.082 (16)	0.116 (17)

Geometric parameters (Å, º) top

Mo1—O16	1.691 (7)	Mo9—O12	1.960 (6)
Mo1—O11	1.954 (6)	Mo9—O7	1.969 (7)
Mo1—O1	1.967 (6)	Mo9—O2	2.228 (7)
Mo1—O3	2.050 (7)	Mo9—O8	2.250 (7)
Mo1—O30	2.173 (7)	Na1—O31ⁱ	2.352 (7)
Mo1—O6	2.182 (7)	Na1—O31	2.352 (7)
Mo1—Mo2	2.6033 (13)	Na1—O10ⁱ	2.352 (6)
Mo2—O17	1.687 (8)	Na1—O10	2.352 (6)
Mo2—O11	1.943 (7)	Na1—O11ⁱ	2.409 (7)
Mo2—O2	2.001 (6)	Na1—O11	2.409 (7)
Mo2—O1	2.006 (7)	Na2—O32	2.313 (9)
Mo2—O12	2.134 (7)	Na2—O32ⁱⁱ	2.315 (9)
Mo2—O4	2.305 (6)	Na2—O18	2.354 (9)
Mo2—Mo9	3.2038 (15)	Na2—O25ⁱⁱ	2.379 (9)
Mo3—O22	1.687 (8)	Na2—O19ⁱⁱ	2.469 (9)
Mo3—O10	1.920 (7)	Na2—O20	2.611 (9)
Mo3—O2	1.960 (6)	Na2—Na2ⁱⁱ	3.416 (10)
Mo3—O5	2.028 (7)	Na3—OW4	2.350 (13)
Mo3—O7	2.101 (6)	Na3—O21	2.371 (9)
Mo3—O9	2.301 (7)	Na3—OW2	2.411 (13)
Mo3—Mo4	2.5974 (18)	Na3—OW3	2.412 (12)
Mo3—Mo9	3.196 (2)	Na3—OW5	2.424 (17)
Mo4—O27	1.703 (8)	Na3—OW1	2.461 (14)
Mo4—O10	1.943 (6)	Na3—Na4	3.750 (10)
Mo4—O5	1.971 (7)	Na4—OW7	2.371 (17)
Mo4—O6ⁱ	2.059 (7)	Na4—O23	2.376 (10)
Mo4—O29	2.169 (6)	Na4—OW8	2.409 (19)
Mo4—O3ⁱ	2.191 (6)	Na4—OW1	2.469 (14)
Mo5—O19	1.701 (8)	Na4—OW6	2.554 (19)
Mo5—O24	1.728 (8)	Na4—OW2	2.709 (17)
Mo5—O6	1.927 (6)	O3—Mo8ⁱ	1.922 (6)
Mo5—O13	1.942 (7)	O3—Mo4ⁱ	2.191 (6)
Mo5—O4	2.205 (6)	O6—Mo4ⁱ	2.059 (7)
Mo5—O1	2.320 (7)	O19—Na2ⁱⁱ	2.469 (9)
Mo6—O15	1.702 (7)	O25—Na2ⁱⁱ	2.379 (9)
Mo6—O25	1.717 (8)	O29—C1ⁱ	1.255 (12)
Mo6—O8	1.936 (7)	O30—C1	1.266 (12)
Mo6—O13	1.949 (7)	C1—O29ⁱ	1.255 (12)
Mo6—O4	2.209 (6)	C1—C2	1.507 (14)
Mo6—O12	2.264 (7)	C2—N1	1.474 (15)
Mo7—O21	1.700 (7)	C2—H2A	0.9700
Mo7—O18	1.701 (8)	C2—H2B	0.9700
Mo7—O14	1.937 (7)	O31—C3	1.242 (12)
Mo7—O8	1.973 (7)	O32—C3ⁱ	1.243 (12)
Mo7—O9	2.211 (6)	O32—Na2ⁱⁱ	2.315 (9)
Mo7—O7	2.291 (7)	C3—O32ⁱ	1.243 (12)
Mo8—O20	1.711 (8)	C3—C4	1.519 (15)
Mo8—O26	1.719 (8)	C4—N2	1.456 (14)
Mo8—O3ⁱ	1.922 (7)	C4—N2	1.456 (14)
Mo8—O14	1.938 (7)	C4—H3	0.9700
Mo8—O9	2.236 (6)	C4—H4	0.9700
Mo8—O5	2.333 (7)	OW14—OW15	1.54 (6)
Mo9—O23	1.710 (8)	OW15—OW15ⁱⁱⁱ	1.67 (11)
Mo9—O28	1.725 (8)

O16—Mo1—O11	106.3 (3)	O23—Mo9—O8	86.5 (3)
O16—Mo1—O1	107.5 (3)	O28—Mo9—O8	169.9 (3)
O11—Mo1—O1	94.2 (3)	O12—Mo9—O8	74.2 (3)
O16—Mo1—O3	98.7 (3)	O7—Mo9—O8	75.1 (3)
O11—Mo1—O3	89.4 (3)	O2—Mo9—O8	81.0 (2)
O1—Mo1—O3	151.3 (3)	O23—Mo9—Mo3	141.0 (3)
O16—Mo1—O30	87.7 (3)	O28—Mo9—Mo3	86.7 (3)
O11—Mo1—O30	165.2 (3)	O12—Mo9—Mo3	112.75 (19)
O1—Mo1—O30	85.9 (3)	O7—Mo9—Mo3	39.72 (19)
O3—Mo1—O30	83.6 (3)	O2—Mo9—Mo3	37.25 (16)
O16—Mo1—O6	166.4 (3)	O8—Mo9—Mo3	85.20 (18)
O11—Mo1—O6	86.1 (3)	O23—Mo9—Mo2	141.6 (3)
O1—Mo1—O6	76.4 (3)	O28—Mo9—Mo2	87.1 (3)
O3—Mo1—O6	75.5 (2)	O12—Mo9—Mo2	40.48 (19)
O30—Mo1—O6	79.5 (3)	O7—Mo9—Mo2	112.27 (19)
O16—Mo1—Mo2	100.5 (2)	O2—Mo9—Mo2	38.18 (16)
O11—Mo1—Mo2	47.9 (2)	O8—Mo9—Mo2	85.06 (17)
O1—Mo1—Mo2	49.70 (19)	Mo3—Mo9—Mo2	75.24 (4)
O3—Mo1—Mo2	136.64 (18)	O31ⁱ—Na1—O31	180.0
O30—Mo1—Mo2	135.43 (19)	O31ⁱ—Na1—O10ⁱ	83.0 (2)
O6—Mo1—Mo2	91.91 (17)	O31—Na1—O10ⁱ	97.0 (2)
O17—Mo2—O11	105.7 (3)	O31ⁱ—Na1—O10	97.0 (2)
O17—Mo2—O2	100.1 (3)	O31—Na1—O10	83.0 (2)
O11—Mo2—O2	89.1 (3)	O10ⁱ—Na1—O10	180.0
O17—Mo2—O1	102.0 (3)	O31ⁱ—Na1—O11ⁱ	82.7 (2)
O11—Mo2—O1	93.3 (3)	O31—Na1—O11ⁱ	97.3 (2)
O2—Mo2—O1	156.3 (3)	O10ⁱ—Na1—O11ⁱ	87.4 (2)
O17—Mo2—O12	94.8 (3)	O10—Na1—O11ⁱ	92.6 (2)
O11—Mo2—O12	157.3 (3)	O31ⁱ—Na1—O11	97.3 (2)
O2—Mo2—O12	77.5 (3)	O31—Na1—O11	82.7 (2)
O1—Mo2—O12	92.0 (3)	O10ⁱ—Na1—O11	92.6 (2)
O17—Mo2—O4	166.2 (3)	O10—Na1—O11	87.4 (2)
O11—Mo2—O4	88.0 (3)	O11ⁱ—Na1—O11	180.0
O2—Mo2—O4	82.4 (2)	O32—Na2—O32ⁱⁱ	84.8 (3)
O1—Mo2—O4	74.2 (3)	O32—Na2—O18	94.0 (3)
O12—Mo2—O4	72.4 (2)	O32ⁱⁱ—Na2—O18	84.9 (3)
O17—Mo2—Mo1	95.9 (3)	O32—Na2—O25ⁱⁱ	81.3 (3)
O11—Mo2—Mo1	48.26 (18)	O32ⁱⁱ—Na2—O25ⁱⁱ	91.8 (3)
O2—Mo2—Mo1	137.21 (19)	O18—Na2—O25ⁱⁱ	174.5 (4)
O1—Mo2—Mo1	48.42 (18)	O32—Na2—O19ⁱⁱ	160.8 (3)
O12—Mo2—Mo1	140.39 (17)	O32ⁱⁱ—Na2—O19ⁱⁱ	91.4 (3)
O4—Mo2—Mo1	91.31 (16)	O18—Na2—O19ⁱⁱ	104.4 (3)
O17—Mo2—Mo9	88.3 (3)	O25ⁱⁱ—Na2—O19ⁱⁱ	80.0 (3)
O11—Mo2—Mo9	132.54 (19)	O32—Na2—O20	92.2 (3)
O2—Mo2—Mo9	43.47 (19)	O32ⁱⁱ—Na2—O20	162.7 (3)
O1—Mo2—Mo9	128.59 (19)	O18—Na2—O20	78.3 (3)
O12—Mo2—Mo9	36.61 (17)	O25ⁱⁱ—Na2—O20	104.6 (3)
O4—Mo2—Mo9	84.21 (16)	O19ⁱⁱ—Na2—O20	96.8 (3)
Mo1—Mo2—Mo9	175.35 (4)	O32—Na2—Na2ⁱⁱ	42.5 (2)
O22—Mo3—O10	106.6 (3)	O32ⁱⁱ—Na2—Na2ⁱⁱ	42.4 (2)
O22—Mo3—O2	98.7 (3)	O18—Na2—Na2ⁱⁱ	89.2 (3)
O10—Mo3—O2	89.7 (3)	O25ⁱⁱ—Na2—Na2ⁱⁱ	85.4 (3)
O22—Mo3—O5	101.9 (3)	O19ⁱⁱ—Na2—Na2ⁱⁱ	130.9 (3)
O10—Mo3—O5	92.8 (3)	O20—Na2—Na2ⁱⁱ	132.3 (3)
O2—Mo3—O5	157.6 (3)	OW4—Na3—O21	175.2 (5)
O22—Mo3—O7	94.5 (3)	OW4—Na3—OW2	96.3 (5)
O10—Mo3—O7	156.9 (3)	O21—Na3—OW2	80.4 (4)
O2—Mo3—O7	77.8 (3)	OW4—Na3—OW3	95.0 (4)
O5—Mo3—O7	91.8 (3)	O21—Na3—OW3	88.5 (4)
O22—Mo3—O9	167.2 (3)	OW2—Na3—OW3	168.4 (5)
O10—Mo3—O9	86.1 (3)	OW4—Na3—OW5	98.0 (5)
O2—Mo3—O9	83.0 (3)	O21—Na3—OW5	85.8 (5)
O5—Mo3—O9	74.9 (3)	OW2—Na3—OW5	95.1 (5)
O7—Mo3—O9	73.3 (2)	OW3—Na3—OW5	80.6 (5)
O22—Mo3—Mo4	95.5 (3)	OW4—Na3—OW1	93.3 (5)
O10—Mo3—Mo4	48.12 (18)	O21—Na3—OW1	83.0 (4)
O2—Mo3—Mo4	137.8 (2)	OW2—Na3—OW1	86.4 (5)
O5—Mo3—Mo4	48.55 (19)	OW3—Na3—OW1	95.8 (4)
O7—Mo3—Mo4	140.31 (18)	OW5—Na3—OW1	168.4 (5)
O9—Mo3—Mo4	91.53 (16)	OW4—Na3—Na4	92.6 (4)
O22—Mo3—Mo9	87.6 (3)	O21—Na3—Na4	82.6 (3)
O10—Mo3—Mo9	133.04 (18)	OW2—Na3—Na4	46.1 (4)
O2—Mo3—Mo9	43.46 (19)	OW3—Na3—Na4	136.1 (4)
O5—Mo3—Mo9	128.6 (2)	OW5—Na3—Na4	140.8 (4)
O7—Mo3—Mo9	36.80 (18)	OW1—Na3—Na4	40.5 (3)
O9—Mo3—Mo9	85.03 (16)	OW7—Na4—O23	176.6 (6)
Mo4—Mo3—Mo9	176.17 (4)	OW7—Na4—OW8	91.7 (6)
O27—Mo4—O10	105.4 (3)	O23—Na4—OW8	89.1 (5)
O27—Mo4—O5	108.2 (3)	OW7—Na4—OW1	93.2 (5)
O10—Mo4—O5	93.9 (3)	O23—Na4—OW1	89.4 (4)
O27—Mo4—O6ⁱ	98.6 (3)	OW8—Na4—OW1	117.4 (6)
O10—Mo4—O6ⁱ	90.7 (3)	OW7—Na4—OW6	95.7 (6)
O5—Mo4—O6ⁱ	150.5 (3)	O23—Na4—OW6	81.1 (5)
O27—Mo4—O29	87.2 (3)	OW8—Na4—OW6	83.6 (6)
O10—Mo4—O29	166.3 (3)	OW1—Na4—OW6	157.0 (6)
O5—Mo4—O29	86.9 (3)	OW7—Na4—OW2	104.8 (5)
O6ⁱ—Mo4—O29	82.1 (3)	O23—Na4—OW2	73.4 (4)
O27—Mo4—O3ⁱ	167.3 (3)	OW8—Na4—OW2	155.6 (6)
O10—Mo4—O3ⁱ	85.9 (3)	OW1—Na4—OW2	80.0 (4)
O5—Mo4—O3ⁱ	76.2 (3)	OW6—Na4—OW2	77.2 (5)
O6ⁱ—Mo4—O3ⁱ	75.1 (2)	OW7—Na4—Na3	98.3 (4)
O29—Mo4—O3ⁱ	81.0 (3)	O23—Na4—Na3	82.2 (3)
O27—Mo4—Mo3	99.3 (3)	OW8—Na4—Na3	155.8 (5)
O10—Mo4—Mo3	47.4 (2)	OW1—Na4—Na3	40.4 (3)
O5—Mo4—Mo3	50.4 (2)	OW6—Na4—Na3	117.0 (5)
O6ⁱ—Mo4—Mo3	137.53 (19)	OW2—Na4—Na3	39.9 (3)
O29—Mo4—Mo3	136.85 (19)	Mo1—O1—Mo2	81.9 (2)
O3ⁱ—Mo4—Mo3	92.64 (18)	Mo1—O1—Mo5	101.4 (3)
O19—Mo5—O24	104.6 (4)	Mo2—O1—Mo5	110.4 (3)
O19—Mo5—O6	100.9 (3)	Mo3—O2—Mo2	160.9 (4)
O24—Mo5—O6	102.1 (3)	Mo3—O2—Mo9	99.3 (3)
O19—Mo5—O13	100.5 (4)	Mo2—O2—Mo9	98.3 (3)
O24—Mo5—O13	95.5 (4)	Mo8ⁱ—O3—Mo1	143.0 (3)
O6—Mo5—O13	147.7 (3)	Mo8ⁱ—O3—Mo4ⁱ	108.5 (3)
O19—Mo5—O4	93.3 (3)	Mo1—O3—Mo4ⁱ	104.4 (3)
O24—Mo5—O4	160.1 (3)	Mo5—O4—Mo6	95.3 (2)
O6—Mo5—O4	82.6 (3)	Mo5—O4—Mo2	104.1 (3)
O13—Mo5—O4	72.3 (3)	Mo6—O4—Mo2	105.7 (3)
O19—Mo5—O1	163.3 (3)	Mo4—O5—Mo3	81.0 (2)
O24—Mo5—O1	92.1 (3)	Mo4—O5—Mo8	101.5 (3)
O6—Mo5—O1	73.9 (3)	Mo3—O5—Mo8	109.8 (3)
O13—Mo5—O1	78.7 (3)	Mo5—O6—Mo4ⁱ	143.2 (4)
O4—Mo5—O1	70.4 (2)	Mo5—O6—Mo1	107.8 (3)
O15—Mo6—O25	104.4 (4)	Mo4ⁱ—O6—Mo1	104.4 (3)
O15—Mo6—O8	100.7 (3)	Mo9—O7—Mo3	103.5 (3)
O25—Mo6—O8	95.0 (3)	Mo9—O7—Mo7	103.0 (3)
O15—Mo6—O13	98.0 (4)	Mo3—O7—Mo7	109.4 (3)
O25—Mo6—O13	97.8 (3)	Mo6—O8—Mo7	150.4 (4)
O8—Mo6—O13	153.9 (3)	Mo6—O8—Mo9	104.7 (3)
O15—Mo6—O4	158.3 (3)	Mo7—O8—Mo9	104.4 (3)
O25—Mo6—O4	96.1 (3)	Mo7—O9—Mo8	94.5 (2)
O8—Mo6—O4	84.0 (3)	Mo7—O9—Mo3	105.2 (3)
O13—Mo6—O4	72.1 (3)	Mo8—O9—Mo3	103.9 (3)
O15—Mo6—O12	89.0 (3)	Mo3—O10—Mo4	84.5 (3)
O25—Mo6—O12	164.3 (3)	Mo3—O10—Na1	130.2 (3)
O8—Mo6—O12	74.3 (3)	Mo4—O10—Na1	132.6 (3)
O13—Mo6—O12	88.1 (3)	Mo2—O11—Mo1	83.8 (3)
O4—Mo6—O12	71.8 (2)	Mo2—O11—Na1	128.2 (3)
O21—Mo7—O18	105.3 (4)	Mo1—O11—Na1	131.7 (3)
O21—Mo7—O14	97.1 (3)	Mo9—O12—Mo2	102.9 (3)
O18—Mo7—O14	99.1 (3)	Mo9—O12—Mo6	103.4 (3)
O21—Mo7—O8	100.3 (3)	Mo2—O12—Mo6	109.8 (3)
O18—Mo7—O8	94.5 (3)	Mo5—O13—Mo6	114.0 (3)
O14—Mo7—O8	154.2 (3)	Mo7—O14—Mo8	114.8 (3)
O21—Mo7—O9	157.3 (3)	Mo7—O18—Na2	143.3 (5)
O18—Mo7—O9	96.5 (3)	Mo5—O19—Na2ⁱⁱ	140.6 (4)
O14—Mo7—O9	72.6 (3)	Mo8—O20—Na2	138.8 (4)
O8—Mo7—O9	84.3 (3)	Mo7—O21—Na3	157.5 (5)
O21—Mo7—O7	88.1 (3)	Mo9—O23—Na4	164.0 (5)
O18—Mo7—O7	163.9 (3)	Mo6—O25—Na2ⁱⁱ	141.7 (4)
O14—Mo7—O7	87.7 (3)	C1ⁱ—O29—Mo4	129.4 (6)
O8—Mo7—O7	74.0 (3)	C1—O30—Mo1	129.6 (6)
O9—Mo7—O7	71.6 (2)	O29ⁱ—C1—O30	128.5 (9)
O20—Mo8—O26	106.0 (4)	O29ⁱ—C1—C2	115.5 (9)
O20—Mo8—O3ⁱ	100.7 (3)	O30—C1—C2	116.0 (9)
O26—Mo8—O3ⁱ	101.1 (3)	N1—C2—C1	112.1 (9)
O20—Mo8—O14	100.6 (3)	N1—C2—H2A	109.2
O26—Mo8—O14	96.3 (3)	C1—C2—H2A	109.2
O3ⁱ—Mo8—O14	147.4 (3)	N1—C2—H2B	109.2
O20—Mo8—O9	92.1 (3)	C1—C2—H2B	109.2
O26—Mo8—O9	160.1 (3)	H2A—C2—H2B	107.9
O3ⁱ—Mo8—O9	82.9 (3)	C3—O31—Na1	136.0 (6)
O14—Mo8—O9	72.0 (3)	C3ⁱ—O32—Na2	131.6 (7)
O20—Mo8—O5	162.2 (3)	C3ⁱ—O32—Na2ⁱⁱ	132.5 (7)
O26—Mo8—O5	91.7 (4)	Na2—O32—Na2ⁱⁱ	95.2 (3)
O3ⁱ—Mo8—O5	73.7 (3)	O31—C3—O32ⁱ	125.2 (9)
O14—Mo8—O5	78.5 (3)	O31—C3—C4	117.7 (9)
O9—Mo8—O5	70.6 (2)	O32ⁱ—C3—C4	117.1 (9)
O23—Mo9—O28	103.6 (4)	N2—C4—C3	112.9 (9)
O23—Mo9—O12	101.3 (3)	N2—C4—H3	109.0
O28—Mo9—O12	103.6 (3)	C3—C4—H3	109.0
O23—Mo9—O7	101.4 (3)	N2—C4—H4	109.0
O28—Mo9—O7	102.2 (3)	C3—C4—H4	109.0
O12—Mo9—O7	140.1 (3)	H3—C4—H4	107.8
O23—Mo9—O2	167.5 (3)	Na3—OW1—Na4	99.1 (5)
O28—Mo9—O2	88.9 (3)	Na3—OW2—Na4	94.0 (5)
O12—Mo9—O2	76.1 (2)	OW14—OW15—OW15ⁱⁱⁱ	159 (6)
O7—Mo9—O2	74.6 (2)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1; (iii) −x+1, −y+1, −z.

Experimental details

Crystal data
Chemical formula	C₈H₉₇Mo₁₈N₄Na₇O₁₀₀
M_r	3737.75
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	11.913 (2), 15.027 (3), 15.466 (3)
α, β, γ (°)	114.37 (3), 99.00 (3), 99.17 (3)
V (Å³)	2412.6 (8)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.42
Crystal size (mm)	0.40 × 0.25 × 0.05

Data collection
Diffractometer	AFC6S diffractometer
Absorption correction	Psi scan Coppens et al. (1965)
T_min, T_max	0.494, 0.886
No. of measured, independent and observed [I > 2σ(I)] reflections	8848, 8499, 6755
R_int	0.033
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.056, 0.179, 1.08
No. of reflections	8499
No. of parameters	592
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.1074P)² + 22.8082P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	2.36, −2.03

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1994), TEXSAN (Molecular Structure Corporation, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP in SHELXTL (Siemens, 1990).

Selected bond lengths (Å) top

Mo1—O16	1.691 (7)	Mo5—O6	1.927 (6)
Mo1—O11	1.954 (6)	Mo5—O13	1.942 (7)
Mo1—O1	1.967 (6)	Mo5—O4	2.205 (6)
Mo1—O3	2.050 (7)	Mo5—O1	2.320 (7)
Mo1—O30	2.173 (7)	Mo6—O15	1.702 (7)
Mo1—O6	2.182 (7)	Mo6—O25	1.717 (8)
Mo1—Mo2	2.6033 (13)	Mo6—O8	1.936 (7)
Mo2—O17	1.687 (8)	Mo6—O13	1.949 (7)
Mo2—O11	1.943 (7)	Mo6—O4	2.209 (6)
Mo2—O2	2.001 (6)	Mo6—O12	2.264 (7)
Mo2—O1	2.006 (7)	Mo7—O21	1.700 (7)
Mo2—O12	2.134 (7)	Mo7—O18	1.701 (8)
Mo2—O4	2.305 (6)	Mo7—O14	1.937 (7)
Mo2—Mo9	3.2038 (15)	Mo7—O8	1.973 (7)
Mo3—O22	1.687 (8)	Mo7—O9	2.211 (6)
Mo3—O10	1.920 (7)	Mo7—O7	2.291 (7)
Mo3—O2	1.960 (6)	Mo8—O20	1.711 (8)
Mo3—O5	2.028 (7)	Mo8—O26	1.719 (8)
Mo3—O7	2.101 (6)	Mo8—O3ⁱ	1.922 (7)
Mo3—O9	2.301 (7)	Mo8—O14	1.938 (7)
Mo3—Mo4	2.5974 (18)	Mo8—O9	2.236 (6)
Mo4—O27	1.703 (8)	Mo8—O5	2.333 (7)
Mo4—O10	1.943 (6)	Mo9—O23	1.710 (8)
Mo4—O5	1.971 (7)	Mo9—O28	1.725 (8)
Mo4—O6ⁱ	2.059 (7)	Mo9—O12	1.960 (6)
Mo4—O29	2.169 (6)	Mo9—O7	1.969 (7)
Mo4—O3ⁱ	2.191 (6)	Mo9—O2	2.228 (7)
Mo5—O19	1.701 (8)	Mo9—O8	2.250 (7)
Mo5—O24	1.728 (8)

Symmetry code: (i) −x+1, −y+1, −z+1.

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