Heptaguanidinium sodium bis­(penta­aqua­tetra­cosa­oxohepta­molybdo­cobaltate) octa­hydrate

Li, C.-B.

doi:10.1107/S1600536807028772

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Heptaguanidinium sodium bis(pentaaquatetracosaoxoheptamolybdocobaltate) octahydrate

C.-B. Li

The title compound, (CH₆N₃)₇Na[CoMo₇O₂₄(H₂O)₅]₂·8H₂O, features unusual [Co(H₂O)₅Mo₇O₂₄]⁴⁻ polymetallate anions. Two such anions are connected by a bridging octahedral sodium ion (Na site symmetry $\overline{1}$ ) to form an {Na[(Co(H₂O)₅)(Mo₇O₂₄)]₂}⁷⁻ cluster. The Co—O and Mo—O distances are in the ranges 2.081 (11)–2.121 (10) and 1.701 (8)–2.508 (7) Å, respectively. Together with the cluster, the charge-balancing guanidinium cations (one of which is disordered about an inversion centre) and isolated water molecules form a three-dimensional supramolecular network by way of numerous O—H

O and N—H

O hydrogen bonds.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807028772/hb2415sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807028772/hb2415Isup2.hkl Contains datablock I

CCDC reference: 654767

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (N-C) = 0.016 Å
Disorder in solvent or counterion
R factor = 0.041
wR factor = 0.096
Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT221_ALERT_4_B Large Solvent/Anion  N     Ueq(max)/Ueq(min) ...       4.33 Ratio
PLAT223_ALERT_4_B Large Solvent/Anion  H     Ueq(max)/Ueq(min) ...       4.43 Ratio
PLAT416_ALERT_2_B Short Intra D-H..H-D       H1     ..  H2      ..       1.47 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       3.37 Ratio
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................       9.00 Perc.
PLAT395_ALERT_2_C Deviating  X-O-Y  Angle from 120 Deg for     OW6     144.40 Deg.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H8     ..  H15     ..       2.11 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          9

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

In the syntheses of new polyoxometalates (POMs), varying the organic ligand used in the reaction was demonstrated to be an effective strategy (Liu, Li et al., 2006; (Liu, Zhou et al., 2006). As an extension of this work, we have combined sodium molybdate, cobalt(II) acetate, and guanidinium nitrate to yield the title compound, (I), (Fig. 1).

Compound (I) contains a [Co(H₂O)₅Mo₇O₂₄]^4- anion, which is constructed from seven MoO₆ and one CoO₆ octahedra. The Co atom is coordinated by five water molecule O atoms and the remaining position is provided with a terminal oxygen atom from a MoO₆ octahedron. The Co—O and Mo—O distances range from 2.075 (10)–2.121 (9) and 1.696 (7)–2.506 (7) Å, respectively. Bond-valence sum calculations (Brown & Altermatt, 1985) indicate oxidation states of 5.78–6.16 for Mo and 2.01 for Co, in agreement with the expected values of 6 and 2. Adjacent [Co(H₂O)₅Mo₇O₂₄]^4- anions share a Na⁺ ion (site symmetry 1) to form a dimeric [Na(Co(H₂O)₅Mo₇O₂₄)₂]^7- anionic cluster. The sodium cation displays a distorted NaO₆ octahedron coordinated by six terminal oxygen atoms from two neighboring [Co(H₂O)₅Mo₇O₂₄]^4- anions.

The anions, charge balancing guanidinium cations (one of which is is disordered about an inversion centre) and isolated water molecules interact by way of a large number of N—H···O and O—H···O hydrogen-bonding interactions (Table 2), thus forming a three-dimensional supramolecular network as shown in Fig. 2.

Related literature top

For related structures, see: Liu, Li et al. (2006); Liu, Zhou et al., (2006). For related literature, see: Brown & Altermatt (1985).

Experimental top

NaMoO₄^.2H₂O (1.0 g, 4.1 mmol) and Co(CH₃COO)₂^.4H₂O (0.1 g, 0.4 mmol) were dissolved in 20 ml water with stirring. CN₃H_6.NO₃ (0.25 g, 2 mmol) was then added to the solution and the pH was adjusted to about 5.0–5.1 by adding 4 M HCl. The mixture was refluxed at 333 K for about 3 h and cooled to room temperature; the solution was then filtrated into a 50-ml beaker. Slow evaporation of the solvent at room temperature led to pink block-shaped crystals of (I) suitable for X-ray diffraction after one weeks.

Structure description top

For related structures, see: Liu, Li et al. (2006); Liu, Zhou et al., (2006). For related literature, see: Brown & Altermatt (1985).

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Figures top

	Fig. 1. A view of the anionic cluster in (I). Displacement ellipsoids are drawn at the 30% probability level (H atoms, guanidinium cations and uncoordinated water molecules omitted for clarity) [Symmetry code: (i) 1 - x, 1 - y, 1 - z].
	Fig. 2. The packing diagram of (I) (hydrogen bonds indicated by dashed lines).

Heptaguanidinium sodium bis(pentaaquatetracosaoxoheptamolybdocobaltate) octahydrate top

Crystal data top

(CH₆N₃)₇Na[CoMo₇O₂₄(H₂O)₅]₂·8H₂O	F(000) = 2896
M_r = 2996.92	D_x = 2.571 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4954 reflections
a = 18.819 (3) Å	θ = 2.0–27.5°
b = 10.581 (2) Å	µ = 2.73 mm⁻¹
c = 19.926 (3) Å	T = 293 K
β = 102.635 (2)°	Block, pink
V = 3871.7 (11) Å³	0.28 × 0.22 × 0.16 mm
Z = 2

Data collection top

Bruker SMART CCD APEX II diffractometer	7505 independent reflections
Radiation source: fine-focus sealed tube	4569 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.074
Detector resolution: not measured pixels mm^-1	θ_max = 26.0°, θ_min = 2.2°
ω and φ scans	h = −23→16
Absorption correction: multi-scan (SADABS; Bruker, 2002)	k = −13→13
T_min = 0.485, T_max = 0.650	l = −19→24
19853 measured reflections

Refinement top

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.096	H-atom parameters constrained
S = 0.99	w = 1/[σ²(F_o²) + (0.0671P)²] where P = (F_o² + 2F_c²)/3
7505 reflections	(Δ/σ)_max < 0.001
511 parameters	Δρ_max = 0.68 e Å⁻³
0 restraints	Δρ_min = −0.55 e Å⁻³

Crystal data top

(CH₆N₃)₇Na[CoMo₇O₂₄(H₂O)₅]₂·8H₂O	V = 3871.7 (11) Å³
M_r = 2996.92	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 18.819 (3) Å	µ = 2.73 mm⁻¹
b = 10.581 (2) Å	T = 293 K
c = 19.926 (3) Å	0.28 × 0.22 × 0.16 mm
β = 102.635 (2)°

Data collection top

Bruker SMART CCD APEX II diffractometer	7505 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2002)	4569 reflections with I > 2σ(I)
T_min = 0.485, T_max = 0.650	R_int = 0.074
19853 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	0 restraints
wR(F²) = 0.096	H-atom parameters constrained
S = 0.99	Δρ_max = 0.68 e Å⁻³
7505 reflections	Δρ_min = −0.55 e Å⁻³
511 parameters

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	0.23286 (5)	0.40375 (8)	0.29023 (5)	0.0206 (2)
Mo2	0.41916 (5)	0.38005 (8)	0.32096 (5)	0.0204 (2)
Mo3	0.21258 (5)	0.72412 (8)	0.29143 (5)	0.0230 (2)
Mo4	0.29702 (5)	0.58470 (8)	0.43326 (5)	0.0223 (2)
Mo5	0.33991 (5)	0.29401 (8)	0.43889 (5)	0.0226 (2)
Mo6	0.33209 (5)	0.51210 (8)	0.17789 (5)	0.0219 (2)
Mo7	0.16280 (5)	0.58368 (9)	0.14662 (5)	0.0274 (2)
Co	0.11521 (10)	0.92346 (17)	0.39784 (10)	0.0468 (5)
Na	0.5000	0.5000	0.5000	0.0334 (15)
O1	0.3355 (3)	0.4504 (6)	0.3687 (3)	0.0174 (14)
O2	0.2043 (3)	0.5356 (6)	0.3437 (4)	0.0244 (16)
O3	0.2534 (3)	0.5821 (6)	0.2332 (3)	0.0195 (15)
O4	0.3070 (3)	0.3544 (6)	0.2460 (3)	0.0210 (15)
O5	0.4182 (4)	0.3265 (7)	0.5009 (4)	0.0291 (17)
O6	0.1292 (3)	0.6644 (7)	0.2197 (4)	0.0276 (17)
O7	0.2766 (4)	0.4170 (6)	0.4667 (4)	0.0266 (17)
O8	0.2994 (3)	0.7066 (6)	0.3606 (4)	0.0230 (16)
O9	0.3850 (3)	0.2345 (6)	0.3678 (3)	0.0223 (15)
O10	0.4597 (4)	0.2828 (6)	0.2713 (4)	0.0279 (17)
O11	0.2337 (4)	0.4758 (7)	0.1215 (4)	0.0323 (18)
O12	0.3756 (4)	0.4051 (7)	0.1354 (4)	0.0318 (18)
O13	0.4039 (3)	0.5263 (6)	0.2629 (3)	0.0221 (15)
O14	0.2396 (4)	0.6598 (7)	0.4755 (4)	0.0333 (18)
O15	0.1561 (4)	0.7910 (7)	0.3388 (4)	0.0358 (19)
O16	0.1561 (4)	0.3929 (7)	0.2242 (4)	0.0325 (18)
O17	0.2389 (4)	0.8481 (7)	0.2483 (4)	0.038 (2)
O18	0.4892 (4)	0.4353 (7)	0.3844 (4)	0.0286 (17)
O19	0.3473 (4)	0.6553 (6)	0.1447 (4)	0.0328 (18)
O20	0.0851 (4)	0.5101 (8)	0.1010 (4)	0.045 (2)
O21	0.1733 (4)	0.7153 (7)	0.0994 (4)	0.040 (2)
O22	0.2293 (4)	0.2733 (6)	0.3430 (4)	0.0306 (17)
O23	0.3049 (4)	0.1576 (7)	0.4644 (4)	0.0365 (19)
O24	0.3843 (4)	0.6113 (7)	0.4815 (4)	0.0337 (18)
OW1	0.0144 (4)	0.8959 (9)	0.3291 (5)	0.059 (3)
H1	0.0002	0.9427	0.3611	0.071*
H2	0.0022	0.8188	0.3280	0.071*
OW2	0.0921 (5)	0.7733 (9)	0.4603 (5)	0.043 (3)
H3	0.0926	0.7055	0.4391	0.052*
H4	0.1233	0.7761	0.4962	0.052*
OW3	0.2183 (5)	0.9444 (9)	0.4619 (6)	0.048 (3)
H5	0.2468	0.9682	0.4381	0.058*
H6	0.2252	0.9938	0.4934	0.058*
OW4	0.1321 (5)	1.0711 (8)	0.3324 (5)	0.044 (3)
H7	0.1225	1.1381	0.3452	0.053*
H8	0.0918	1.0234	0.3012	0.053*
OW5	0.0675 (6)	1.0433 (11)	0.4582 (6)	0.057 (3)
H10	0.0770	1.1195	0.4321	0.068*
H9	0.0893	1.0200	0.5008	0.068*
OW6	0.0746 (7)	0.9225 (12)	0.1733 (9)	0.138 (6)
H11	0.1078	0.8720	0.1779	0.166*
H12	0.0286	0.9327	0.1757	0.166*
OW7	0.0768 (6)	0.5417 (13)	0.3912 (7)	0.104 (4)
H13	0.1182	0.5098	0.3877	0.124*
H14	0.0616	0.4852	0.4204	0.124*
OW8	−0.0030 (6)	0.6593 (11)	0.2614 (7)	0.094 (4)
H15	−0.0015	0.6459	0.2154	0.113*
H16	0.0315	0.6172	0.2830	0.113*
OW9	0.0197 (8)	0.3218 (14)	0.4569 (8)	0.132 (5)
H17	−0.0119	0.3036	0.4109	0.158*
H18	−0.0256	0.3354	0.4743	0.158*
N1	0.4305 (5)	0.7968 (8)	0.3149 (5)	0.038 (2)
H1A	0.4026	0.7406	0.3268	0.046*
H1B	0.4638	0.7745	0.2938	0.046*
N2	0.3716 (4)	0.9528 (8)	0.3612 (5)	0.031 (2)
H2A	0.3648	1.0315	0.3685	0.037*
H2B	0.3450	0.8964	0.3749	0.037*
N3	0.4635 (5)	1.0043 (8)	0.3075 (5)	0.034 (2)
H3A	0.4572	1.0833	0.3146	0.041*
H3B	0.4967	0.9809	0.2865	0.041*
N4	0.3851 (5)	0.1298 (9)	0.1373 (5)	0.042 (3)
H4A	0.3842	0.2087	0.1475	0.051*
H4B	0.4112	0.1044	0.1095	0.051*
N5	0.3072 (5)	0.0844 (9)	0.2063 (5)	0.040 (3)
H5A	0.3054	0.1627	0.2172	0.048*
H5B	0.2825	0.0292	0.2233	0.048*
N6	0.3486 (6)	−0.0740 (9)	0.1460 (6)	0.056 (3)
H6A	0.3232	−0.1286	0.1625	0.067*
H6B	0.3750	−0.0977	0.1180	0.067*
N7	0.1706 (6)	0.4791 (11)	0.5664 (6)	0.060 (3)
H7A	0.1474	0.5386	0.5818	0.072*
H7B	0.1951	0.4954	0.5357	0.072*
N8	0.1343 (6)	0.3325 (12)	0.6347 (6)	0.062 (3)
H8A	0.1342	0.2550	0.6476	0.075*
H8B	0.1108	0.3885	0.6524	0.075*
N9	0.2033 (6)	0.2764 (11)	0.5629 (6)	0.059 (3)
H9A	0.2022	0.1996	0.5768	0.071*
H9B	0.2273	0.2951	0.5322	0.071*
N10	0.4687 (5)	0.0622 (10)	0.5260 (5)	0.051 (3)
H10A	0.4377	0.0766	0.5511	0.062*
H10B	0.4801	0.1389	0.5186	0.062*
N11	0.4383 (7)	−0.1460 (12)	0.5436 (7)	0.012 (3)	0.50
H11A	0.4099	−0.1289	0.5710	0.014*	0.50
H11B	0.4449	−0.2232	0.5329	0.014*	0.50
C1	0.4223 (6)	0.9190 (10)	0.3290 (5)	0.029 (3)
C2	0.3473 (6)	0.0494 (10)	0.1641 (6)	0.031 (3)
C3	0.1687 (7)	0.3640 (14)	0.5888 (7)	0.048 (3)
C4	0.4765 (12)	−0.057 (2)	0.5158 (12)	0.029 (5)	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0210 (5)	0.0199 (5)	0.0215 (5)	−0.0035 (4)	0.0058 (4)	−0.0004 (4)
Mo2	0.0212 (5)	0.0191 (5)	0.0213 (5)	0.0009 (4)	0.0056 (4)	−0.0018 (4)
Mo3	0.0230 (5)	0.0217 (5)	0.0254 (5)	0.0036 (4)	0.0073 (4)	0.0016 (4)
Mo4	0.0248 (5)	0.0217 (5)	0.0208 (5)	0.0043 (4)	0.0060 (4)	−0.0017 (4)
Mo5	0.0265 (5)	0.0187 (5)	0.0227 (5)	0.0000 (4)	0.0059 (4)	0.0033 (4)
Mo6	0.0239 (5)	0.0214 (5)	0.0216 (5)	0.0000 (4)	0.0075 (4)	0.0003 (4)
Mo7	0.0224 (5)	0.0368 (6)	0.0216 (5)	−0.0013 (4)	0.0019 (4)	0.0034 (4)
Co	0.0481 (11)	0.0433 (11)	0.0491 (12)	0.0022 (8)	0.0112 (8)	−0.0018 (9)
Na	0.028 (3)	0.035 (4)	0.038 (4)	0.000 (3)	0.008 (3)	−0.010 (3)
O1	0.018 (3)	0.017 (3)	0.017 (4)	0.000 (3)	0.003 (3)	0.004 (3)
O2	0.022 (4)	0.022 (4)	0.031 (4)	−0.005 (3)	0.010 (3)	−0.003 (3)
O3	0.023 (4)	0.019 (3)	0.016 (4)	0.002 (3)	0.004 (3)	0.004 (3)
O4	0.025 (4)	0.018 (4)	0.019 (4)	−0.001 (3)	0.003 (3)	0.001 (3)
O5	0.033 (4)	0.032 (4)	0.020 (4)	−0.001 (3)	0.000 (3)	0.001 (3)
O6	0.021 (4)	0.029 (4)	0.033 (5)	0.003 (3)	0.007 (3)	0.001 (3)
O7	0.026 (4)	0.034 (4)	0.023 (4)	0.007 (3)	0.012 (3)	0.006 (3)
O8	0.020 (4)	0.019 (4)	0.030 (4)	0.001 (3)	0.008 (3)	0.000 (3)
O9	0.028 (3)	0.013 (3)	0.026 (3)	−0.001 (3)	0.006 (3)	0.000 (3)
O10	0.035 (4)	0.022 (4)	0.032 (4)	0.004 (3)	0.018 (3)	−0.002 (3)
O11	0.020 (4)	0.045 (5)	0.030 (5)	0.006 (3)	0.000 (3)	−0.003 (4)
O12	0.038 (4)	0.038 (4)	0.021 (4)	0.004 (3)	0.008 (3)	0.002 (3)
O13	0.021 (4)	0.024 (4)	0.022 (4)	−0.003 (3)	0.010 (3)	0.000 (3)
O14	0.037 (4)	0.033 (4)	0.035 (5)	0.015 (4)	0.018 (4)	0.007 (4)
O15	0.035 (5)	0.039 (5)	0.035 (5)	0.016 (4)	0.011 (4)	−0.003 (4)
O16	0.032 (4)	0.037 (4)	0.028 (5)	−0.003 (3)	0.005 (3)	−0.005 (4)
O17	0.045 (5)	0.027 (4)	0.042 (5)	−0.003 (4)	0.010 (4)	0.001 (4)
O18	0.025 (4)	0.041 (4)	0.020 (4)	0.003 (3)	0.004 (3)	−0.002 (3)
O19	0.038 (5)	0.019 (4)	0.043 (5)	0.003 (3)	0.012 (4)	0.005 (3)
O20	0.032 (5)	0.069 (6)	0.031 (5)	−0.004 (4)	0.002 (4)	−0.002 (4)
O21	0.046 (5)	0.038 (5)	0.037 (5)	0.001 (4)	0.009 (4)	0.010 (4)
O22	0.038 (4)	0.027 (4)	0.027 (4)	−0.004 (3)	0.008 (3)	0.002 (3)
O23	0.040 (5)	0.028 (4)	0.040 (5)	−0.010 (4)	0.004 (4)	0.005 (4)
O24	0.030 (4)	0.034 (4)	0.032 (5)	0.007 (3)	−0.004 (3)	0.001 (4)
OW1	0.035 (5)	0.062 (6)	0.080 (8)	0.012 (4)	0.010 (5)	−0.001 (6)
OW2	0.066 (7)	0.039 (6)	0.020 (6)	0.000 (5)	0.001 (5)	0.003 (5)
OW3	0.048 (7)	0.039 (6)	0.049 (7)	−0.017 (5)	−0.009 (5)	0.009 (5)
OW4	0.055 (7)	0.023 (5)	0.048 (7)	−0.016 (5)	−0.005 (5)	0.005 (5)
OW5	0.065 (5)	0.056 (5)	0.050 (5)	0.002 (4)	0.011 (4)	0.005 (4)
OW6	0.082 (10)	0.115 (11)	0.209 (18)	0.021 (8)	0.011 (10)	0.068 (12)
OW7	0.067 (8)	0.142 (11)	0.113 (11)	−0.014 (8)	0.044 (7)	−0.013 (9)
OW8	0.089 (5)	0.098 (5)	0.095 (6)	−0.004 (4)	0.021 (4)	−0.011 (4)
OW9	0.128 (7)	0.134 (7)	0.132 (7)	−0.005 (5)	0.024 (5)	0.002 (5)
N1	0.044 (6)	0.023 (5)	0.056 (7)	0.002 (4)	0.028 (5)	−0.002 (5)
N2	0.024 (5)	0.029 (5)	0.044 (6)	0.000 (4)	0.017 (4)	−0.006 (4)
N3	0.032 (5)	0.017 (5)	0.056 (7)	−0.002 (4)	0.016 (5)	0.001 (5)
N4	0.065 (7)	0.026 (5)	0.043 (7)	−0.004 (5)	0.026 (5)	−0.008 (5)
N5	0.049 (6)	0.026 (5)	0.047 (7)	0.004 (5)	0.013 (5)	0.010 (5)
N6	0.080 (9)	0.037 (6)	0.057 (8)	0.004 (6)	0.030 (6)	−0.014 (6)
N7	0.053 (7)	0.065 (8)	0.070 (9)	0.014 (6)	0.030 (6)	0.043 (7)
N8	0.073 (8)	0.067 (8)	0.058 (8)	0.002 (7)	0.040 (7)	0.027 (7)
N9	0.056 (8)	0.059 (8)	0.067 (9)	−0.003 (6)	0.024 (6)	0.007 (7)
N10	0.048 (7)	0.067 (8)	0.037 (7)	0.020 (6)	0.004 (5)	0.002 (6)
N11	0.012 (3)	0.012 (3)	0.012 (3)	−0.0001 (10)	0.0028 (12)	−0.0008 (10)
C1	0.032 (6)	0.035 (6)	0.016 (6)	0.004 (5)	−0.002 (5)	−0.005 (5)
C2	0.053 (8)	0.019 (6)	0.022 (6)	0.010 (5)	0.011 (5)	−0.003 (5)
C3	0.037 (8)	0.060 (9)	0.048 (9)	0.016 (7)	0.010 (6)	0.022 (7)
C4	0.030 (6)	0.026 (6)	0.030 (7)	0.004 (5)	0.002 (5)	−0.004 (5)

Geometric parameters (Å, º) top

Mo1—O16	1.732 (7)	OW1—H2	0.8455
Mo1—O22	1.745 (7)	OW2—H3	0.8334
Mo1—O4	1.880 (7)	OW2—H4	0.8210
Mo1—O2	1.903 (7)	OW3—H5	0.8290
Mo1—O1	2.258 (6)	OW3—H6	0.8066
Mo1—O3	2.279 (6)	OW4—H7	0.7875
Mo2—O10	1.717 (7)	OW4—H8	1.0051
Mo2—O18	1.717 (7)	OW5—H10	0.9960
Mo2—O13	1.916 (7)	OW5—H9	0.8934
Mo2—O9	1.980 (6)	OW6—H11	0.8123
Mo2—O1	2.142 (6)	OW6—H12	0.8843
Mo2—O4	2.320 (6)	OW7—H13	0.8657
Mo3—O17	1.701 (8)	OW7—H14	0.9208
Mo3—O15	1.720 (7)	OW8—H15	0.9342
Mo3—O8	1.901 (7)	OW8—H16	0.8261
Mo3—O6	1.980 (7)	OW9—H17	0.9962
Mo3—O3	2.141 (6)	OW9—H18	0.9975
Mo3—O2	2.271 (7)	N1—C1	1.340 (13)
Mo4—O14	1.704 (7)	N1—H1A	0.8600
Mo4—O24	1.735 (7)	N1—H1B	0.8600
Mo4—O8	1.947 (7)	N2—C1	1.310 (13)
Mo4—O7	1.963 (7)	N2—H2A	0.8600
Mo4—O1	2.147 (6)	N2—H2B	0.8600
Mo4—O2	2.266 (7)	N3—C1	1.321 (13)
Mo5—O23	1.709 (7)	N3—H3A	0.8600
Mo5—O5	1.737 (7)	N3—H3B	0.8600
Mo5—O9	1.910 (7)	N4—C2	1.297 (14)
Mo5—O7	1.926 (7)	N4—H4A	0.8600
Mo5—O1	2.156 (6)	N4—H4B	0.8600
Mo5—O22	2.508 (7)	N5—C2	1.301 (14)
Mo6—O19	1.702 (7)	N5—H5A	0.8600
Mo6—O12	1.724 (7)	N5—H5B	0.8600
Mo6—O13	1.928 (7)	N6—C2	1.357 (13)
Mo6—O11	1.983 (7)	N6—H6A	0.8600
Mo6—O3	2.161 (6)	N6—H6B	0.8600
Mo6—O4	2.265 (6)	N7—C3	1.301 (16)
Mo7—O21	1.716 (8)	N7—H7A	0.8600
Mo7—O20	1.729 (8)	N7—H7B	0.8600
Mo7—O11	1.905 (7)	N8—C3	1.275 (16)
Mo7—O6	1.912 (7)	N8—H8A	0.8600
Mo7—O3	2.144 (6)	N8—H8B	0.8600
Co—OW5	2.081 (11)	N9—C3	1.302 (16)
Co—O15	2.082 (7)	N9—H9A	0.8600
Co—OW3	2.087 (9)	N9—H9B	0.8600
Co—OW4	2.103 (9)	N10—C4	1.29 (2)
Co—OW1	2.103 (9)	N10—C4ⁱⁱ	1.46 (2)
Co—OW2	2.121 (10)	N10—H10A	0.8600
Na—O18	2.369 (7)	N10—H10B	0.8605
Na—O18ⁱ	2.369 (7)	N11—C4	1.37 (2)
Na—O5	2.399 (7)	N11—H11A	0.8600
Na—O5ⁱ	2.399 (7)	N11—H11B	0.8600
Na—O24ⁱ	2.431 (7)	C4—N10ⁱⁱ	1.46 (2)
Na—O24	2.431 (7)	C4—C4ⁱⁱ	1.70 (4)
OW1—H1	0.8926

O16—Mo1—O22	105.7 (3)	O3—Mo7—Mo3	41.69 (17)
O16—Mo1—O4	101.9 (3)	O21—Mo7—Mo6	94.0 (3)
O22—Mo1—O4	101.1 (3)	O20—Mo7—Mo6	133.4 (3)
O16—Mo1—O2	100.6 (3)	O11—Mo7—Mo6	35.4 (2)
O22—Mo1—O2	100.9 (3)	O6—Mo7—Mo6	116.0 (2)
O4—Mo1—O2	142.7 (3)	O3—Mo7—Mo6	42.17 (17)
O16—Mo1—O1	170.3 (3)	Mo3—Mo7—Mo6	81.47 (3)
O22—Mo1—O1	84.0 (3)	OW5—Co—O15	174.8 (4)
O4—Mo1—O1	77.0 (3)	OW5—Co—OW3	92.4 (5)
O2—Mo1—O1	75.8 (3)	O15—Co—OW3	90.4 (4)
O16—Mo1—O3	83.1 (3)	OW5—Co—OW4	92.8 (4)
O22—Mo1—O3	171.2 (3)	O15—Co—OW4	91.4 (4)
O4—Mo1—O3	76.8 (2)	OW3—Co—OW4	93.1 (4)
O2—Mo1—O3	76.8 (3)	OW5—Co—OW1	91.1 (4)
O1—Mo1—O3	87.2 (2)	O15—Co—OW1	86.1 (3)
O10—Mo2—O18	105.2 (3)	OW3—Co—OW1	176.4 (4)
O10—Mo2—O13	99.4 (3)	OW4—Co—OW1	86.4 (4)
O18—Mo2—O13	99.2 (3)	OW5—Co—OW2	87.0 (4)
O10—Mo2—O9	92.1 (3)	O15—Co—OW2	88.6 (4)
O18—Mo2—O9	101.2 (3)	OW3—Co—OW2	90.2 (4)
O13—Mo2—O9	153.1 (3)	OW4—Co—OW2	176.8 (4)
O10—Mo2—O1	157.8 (3)	OW1—Co—OW2	90.4 (4)
O18—Mo2—O1	94.3 (3)	O18—Na—O18ⁱ	180.000 (1)
O13—Mo2—O1	87.7 (3)	O18—Na—O5	82.4 (2)
O9—Mo2—O1	73.4 (2)	O18ⁱ—Na—O5	97.6 (2)
O10—Mo2—O4	90.9 (3)	O18—Na—O5ⁱ	97.6 (2)
O18—Mo2—O4	163.3 (3)	O18ⁱ—Na—O5ⁱ	82.4 (2)
O13—Mo2—O4	73.2 (2)	O5—Na—O5ⁱ	180.0 (2)
O9—Mo2—O4	82.5 (2)	O18—Na—O24ⁱ	83.8 (2)
O1—Mo2—O4	70.9 (2)	O18ⁱ—Na—O24ⁱ	96.2 (2)
O10—Mo2—Mo5	126.4 (2)	O5—Na—O24ⁱ	100.6 (2)
O18—Mo2—Mo5	87.8 (2)	O5ⁱ—Na—O24ⁱ	79.4 (2)
O13—Mo2—Mo5	130.14 (19)	O18—Na—O24	96.2 (2)
O9—Mo2—Mo5	34.45 (19)	O18ⁱ—Na—O24	83.8 (2)
O1—Mo2—Mo5	42.47 (16)	O5—Na—O24	79.4 (2)
O4—Mo2—Mo5	86.25 (16)	O5ⁱ—Na—O24	100.6 (2)
O17—Mo3—O15	104.1 (4)	O24ⁱ—Na—O24	180.000 (1)
O17—Mo3—O8	98.2 (3)	O18—Na—Mo5	67.64 (17)
O15—Mo3—O8	100.2 (3)	O18ⁱ—Na—Mo5	112.36 (17)
O17—Mo3—O6	98.9 (3)	O5—Na—Mo5	22.23 (16)
O15—Mo3—O6	92.3 (3)	O5ⁱ—Na—Mo5	157.77 (16)
O8—Mo3—O6	155.7 (3)	O24ⁱ—Na—Mo5	113.72 (17)
O17—Mo3—O3	95.1 (3)	O24—Na—Mo5	66.28 (17)
O15—Mo3—O3	157.5 (3)	O18—Na—Mo5ⁱ	112.36 (17)
O8—Mo3—O3	88.3 (3)	O18ⁱ—Na—Mo5ⁱ	67.64 (17)
O6—Mo3—O3	72.9 (3)	O5—Na—Mo5ⁱ	157.77 (16)
O17—Mo3—O2	165.0 (3)	O5ⁱ—Na—Mo5ⁱ	22.23 (16)
O15—Mo3—O2	89.8 (3)	O24ⁱ—Na—Mo5ⁱ	66.28 (17)
O8—Mo3—O2	73.5 (3)	O24—Na—Mo5ⁱ	113.72 (17)
O6—Mo3—O2	85.9 (3)	Mo5—Na—Mo5ⁱ	180.00 (4)
O3—Mo3—O2	72.6 (2)	Mo2—O1—Mo4	150.8 (3)
O17—Mo3—Mo7	87.9 (3)	Mo2—O1—Mo5	95.4 (2)
O15—Mo3—Mo7	126.3 (3)	Mo4—O1—Mo5	95.1 (2)
O8—Mo3—Mo7	130.1 (2)	Mo2—O1—Mo1	102.5 (3)
O6—Mo3—Mo7	34.0 (2)	Mo4—O1—Mo1	102.1 (2)
O3—Mo3—Mo7	41.76 (17)	Mo5—O1—Mo1	100.8 (2)
O2—Mo3—Mo7	88.28 (18)	Mo1—O2—Mo4	110.3 (3)
O14—Mo4—O24	106.1 (4)	Mo1—O2—Mo3	109.3 (3)
O14—Mo4—O8	100.3 (3)	Mo4—O2—Mo3	92.4 (2)
O24—Mo4—O8	97.6 (3)	Mo3—O3—Mo7	96.5 (2)
O14—Mo4—O7	93.5 (3)	Mo3—O3—Mo6	152.2 (3)
O24—Mo4—O7	101.0 (3)	Mo7—O3—Mo6	96.0 (3)
O8—Mo4—O7	152.8 (3)	Mo3—O3—Mo1	101.0 (3)
O14—Mo4—O1	159.8 (3)	Mo7—O3—Mo1	102.4 (3)
O24—Mo4—O1	92.1 (3)	Mo6—O3—Mo1	100.4 (2)
O8—Mo4—O1	85.8 (3)	Mo1—O4—Mo6	110.5 (3)
O7—Mo4—O1	73.9 (3)	Mo1—O4—Mo2	109.2 (3)
O14—Mo4—O2	92.0 (3)	Mo6—O4—Mo2	91.1 (2)
O24—Mo4—O2	161.0 (3)	Mo5—O5—Na	126.3 (4)
O8—Mo4—O2	72.8 (3)	Mo7—O6—Mo3	110.5 (3)
O7—Mo4—O2	83.5 (3)	Mo5—O7—Mo4	109.5 (3)
O1—Mo4—O2	71.3 (2)	Mo3—O8—Mo4	116.6 (3)
O14—Mo4—Mo5	128.2 (3)	Mo5—O9—Mo2	109.6 (3)
O24—Mo4—Mo5	86.3 (2)	Mo7—O11—Mo6	110.8 (4)
O8—Mo4—Mo5	128.40 (19)	Mo2—O13—Mo6	116.8 (3)
O7—Mo4—Mo5	34.88 (19)	Mo3—O15—Co	159.4 (5)
O1—Mo4—Mo5	42.56 (16)	Mo2—O18—Na	134.7 (4)
O2—Mo4—Mo5	87.23 (17)	Mo1—O22—Mo5	104.8 (3)
O23—Mo5—O5	106.1 (3)	Mo4—O24—Na	135.5 (4)
O23—Mo5—O9	101.8 (3)	Co—OW1—H1	79.9
O5—Mo5—O9	98.5 (3)	Co—OW1—H2	110.6
O23—Mo5—O7	100.5 (3)	H1—OW1—H2	115.6
O5—Mo5—O7	98.2 (3)	Co—OW2—H3	108.7
O9—Mo5—O7	147.1 (3)	Co—OW2—H4	106.6
O23—Mo5—O1	151.4 (3)	H3—OW2—H4	112.9
O5—Mo5—O1	102.5 (3)	Co—OW3—H5	108.4
O9—Mo5—O1	74.5 (2)	Co—OW3—H6	121.1
O7—Mo5—O1	74.4 (3)	H5—OW3—H6	103.4
O23—Mo5—O22	81.0 (3)	Co—OW4—H7	113.1
O5—Mo5—O22	172.9 (3)	Co—OW4—H8	79.3
O9—Mo5—O22	80.5 (3)	H7—OW4—H8	117.1
O7—Mo5—O22	79.4 (3)	Co—OW5—H10	92.5
O1—Mo5—O22	70.4 (2)	Co—OW5—H9	102.4
O23—Mo5—Mo4	135.8 (3)	H10—OW5—H9	128.5
O5—Mo5—Mo4	90.2 (2)	H11—OW6—H12	144.4
O9—Mo5—Mo4	116.34 (19)	H13—OW7—H14	101.9
O7—Mo5—Mo4	35.7 (2)	H15—OW8—H16	103.9
O1—Mo5—Mo4	42.32 (17)	H17—OW9—H18	88.0
O22—Mo5—Mo4	84.00 (16)	C1—N1—H1A	120.2
O23—Mo5—Mo2	137.3 (3)	C1—N1—H1B	119.8
O5—Mo5—Mo2	90.4 (2)	H1A—N1—H1B	120.0
O9—Mo5—Mo2	35.90 (18)	C1—N2—H2A	119.8
O7—Mo5—Mo2	116.1 (2)	C1—N2—H2B	120.2
O1—Mo5—Mo2	42.14 (16)	H2A—N2—H2B	120.0
O22—Mo5—Mo2	84.67 (17)	C1—N3—H3A	119.9
Mo4—Mo5—Mo2	81.56 (3)	C1—N3—H3B	120.1
O23—Mo5—Na	137.6 (3)	H3A—N3—H3B	120.0
O5—Mo5—Na	31.5 (2)	C2—N4—H4A	119.9
O9—Mo5—Na	88.66 (19)	C2—N4—H4B	120.1
O7—Mo5—Na	91.0 (2)	H4A—N4—H4B	120.0
O1—Mo5—Na	71.01 (16)	C2—N5—H5A	119.9
O22—Mo5—Na	141.44 (16)	C2—N5—H5B	120.1
Mo4—Mo5—Na	67.89 (2)	H5A—N5—H5B	120.0
Mo2—Mo5—Na	66.11 (2)	C2—N6—H6A	120.0
O19—Mo6—O12	104.8 (4)	C2—N6—H6B	120.0
O19—Mo6—O13	97.3 (3)	H6A—N6—H6B	120.0
O12—Mo6—O13	99.6 (3)	C3—N7—H7A	120.5
O19—Mo6—O11	99.7 (3)	C3—N7—H7B	119.5
O12—Mo6—O11	94.5 (3)	H7A—N7—H7B	120.0
O13—Mo6—O11	154.4 (3)	C3—N8—H8A	119.9
O19—Mo6—O3	94.9 (3)	C3—N8—H8B	120.1
O12—Mo6—O3	158.0 (3)	H8A—N8—H8B	120.0
O13—Mo6—O3	87.2 (3)	C3—N9—H9A	119.8
O11—Mo6—O3	72.3 (3)	C3—N9—H9B	120.2
O19—Mo6—O4	164.4 (3)	H9A—N9—H9B	120.0
O12—Mo6—O4	89.7 (3)	C4—N10—C4ⁱⁱ	75.9 (17)
O13—Mo6—O4	74.3 (2)	C4—N10—H10A	112.3
O11—Mo6—O4	84.6 (3)	C4ⁱⁱ—N10—H10A	171.8
O3—Mo6—O4	72.0 (2)	C4—N10—H10B	148.4
O19—Mo6—Mo7	87.6 (2)	C4ⁱⁱ—N10—H10B	72.6
O12—Mo6—Mo7	128.2 (2)	H10A—N10—H10B	99.3
O13—Mo6—Mo7	128.96 (19)	C4—N11—H11A	124.4
O11—Mo6—Mo7	33.8 (2)	C4—N11—H11B	115.6
O3—Mo6—Mo7	41.78 (17)	H11A—N11—H11B	120.0
O4—Mo6—Mo7	87.79 (16)	N2—C1—N3	121.0 (10)
O21—Mo7—O20	105.2 (4)	N2—C1—N1	119.7 (10)
O21—Mo7—O11	99.8 (4)	N3—C1—N1	119.2 (10)
O20—Mo7—O11	98.8 (4)	N4—C2—N5	121.8 (10)
O21—Mo7—O6	98.8 (3)	N4—C2—N6	118.6 (11)
O20—Mo7—O6	102.7 (3)	N5—C2—N6	119.5 (11)
O11—Mo7—O6	146.7 (3)	N8—C3—N7	123.2 (14)
O21—Mo7—O3	106.3 (3)	N8—C3—N9	118.3 (13)
O20—Mo7—O3	148.4 (3)	N7—C3—N9	118.5 (13)
O11—Mo7—O3	74.2 (3)	N10—C4—N11	121.1 (19)
O6—Mo7—O3	74.2 (3)	N10—C4—N10ⁱⁱ	104.1 (16)
O21—Mo7—Mo3	94.1 (3)	N11—C4—N10ⁱⁱ	134.8 (18)
O20—Mo7—Mo3	136.9 (3)	N10—C4—C4ⁱⁱ	56.5 (13)
O11—Mo7—Mo3	115.6 (2)	N11—C4—C4ⁱⁱ	177 (3)
O6—Mo7—Mo3	35.4 (2)	N10ⁱⁱ—C4—C4ⁱⁱ	47.6 (12)

O10—Mo2—O1—Mo4	−179.9 (7)	O4—Mo1—O3—Mo3	−157.6 (3)
O18—Mo2—O1—Mo4	28.6 (7)	O2—Mo1—O3—Mo3	−4.2 (3)
O13—Mo2—O1—Mo4	−70.4 (6)	O1—Mo1—O3—Mo3	−80.3 (3)
O9—Mo2—O1—Mo4	129.0 (7)	O16—Mo1—O3—Mo7	−0.9 (3)
O4—Mo2—O1—Mo4	−143.4 (7)	O4—Mo1—O3—Mo7	103.1 (3)
Mo5—Mo2—O1—Mo4	110.7 (7)	O2—Mo1—O3—Mo7	−103.5 (3)
O10—Mo2—O1—Mo5	69.5 (8)	O1—Mo1—O3—Mo7	−179.6 (3)
O18—Mo2—O1—Mo5	−82.0 (3)	O16—Mo1—O3—Mo6	−99.5 (3)
O13—Mo2—O1—Mo5	178.9 (3)	O4—Mo1—O3—Mo6	4.4 (3)
O9—Mo2—O1—Mo5	18.4 (2)	O2—Mo1—O3—Mo6	157.8 (3)
O4—Mo2—O1—Mo5	106.0 (3)	O1—Mo1—O3—Mo6	81.7 (3)
O10—Mo2—O1—Mo1	−32.8 (9)	O16—Mo1—O4—Mo6	75.5 (4)
O18—Mo2—O1—Mo1	175.7 (3)	O22—Mo1—O4—Mo6	−175.7 (3)
O13—Mo2—O1—Mo1	76.6 (3)	O2—Mo1—O4—Mo6	−50.4 (6)
O9—Mo2—O1—Mo1	−83.9 (3)	O1—Mo1—O4—Mo6	−94.6 (3)
O4—Mo2—O1—Mo1	3.7 (2)	O3—Mo1—O4—Mo6	−4.4 (3)
Mo5—Mo2—O1—Mo1	−102.3 (3)	O16—Mo1—O4—Mo2	174.3 (3)
O14—Mo4—O1—Mo2	177.5 (7)	O22—Mo1—O4—Mo2	−76.9 (3)
O24—Mo4—O1—Mo2	−28.5 (7)	O2—Mo1—O4—Mo2	48.4 (6)
O8—Mo4—O1—Mo2	68.9 (6)	O1—Mo1—O4—Mo2	4.2 (3)
O7—Mo4—O1—Mo2	−129.4 (7)	O3—Mo1—O4—Mo2	94.3 (3)
O2—Mo4—O1—Mo2	142.2 (7)	O19—Mo6—O4—Mo1	38.3 (12)
Mo5—Mo4—O1—Mo2	−110.7 (7)	O12—Mo6—O4—Mo1	−162.9 (4)
O14—Mo4—O1—Mo5	−71.8 (9)	O13—Mo6—O4—Mo1	97.0 (3)
O24—Mo4—O1—Mo5	82.2 (3)	O11—Mo6—O4—Mo1	−68.4 (3)
O8—Mo4—O1—Mo5	179.6 (3)	O3—Mo6—O4—Mo1	4.8 (3)
O7—Mo4—O1—Mo5	−18.6 (2)	O19—Mo6—O4—Mo2	−72.7 (11)
O2—Mo4—O1—Mo5	−107.1 (3)	O12—Mo6—O4—Mo2	86.0 (3)
O14—Mo4—O1—Mo1	30.4 (9)	O13—Mo6—O4—Mo2	−14.0 (2)
O24—Mo4—O1—Mo1	−175.6 (3)	O11—Mo6—O4—Mo2	−179.4 (3)
O8—Mo4—O1—Mo1	−78.2 (3)	O3—Mo6—O4—Mo2	−106.2 (3)
O7—Mo4—O1—Mo1	83.5 (3)	O10—Mo2—O4—Mo1	162.5 (3)
O2—Mo4—O1—Mo1	−4.9 (2)	O18—Mo2—O4—Mo1	−33.4 (11)
Mo5—Mo4—O1—Mo1	102.2 (3)	O13—Mo2—O4—Mo1	−98.0 (3)
O23—Mo5—O1—Mo2	−105.2 (7)	O9—Mo2—O4—Mo1	70.5 (3)
O5—Mo5—O1—Mo2	76.5 (3)	O1—Mo2—O4—Mo1	−4.5 (3)
O9—Mo5—O1—Mo2	−19.0 (2)	O10—Mo2—O4—Mo6	−85.4 (3)
O7—Mo5—O1—Mo2	171.7 (3)	O18—Mo2—O4—Mo6	78.8 (10)
O22—Mo5—O1—Mo2	−104.2 (3)	O13—Mo2—O4—Mo6	14.2 (2)
Mo4—Mo5—O1—Mo2	152.7 (3)	O9—Mo2—O4—Mo6	−177.3 (3)
Na—Mo5—O1—Mo2	75.05 (17)	O1—Mo2—O4—Mo6	107.6 (3)
O23—Mo5—O1—Mo4	102.1 (7)	O23—Mo5—O5—Na	178.2 (4)
O5—Mo5—O1—Mo4	−76.2 (3)	O9—Mo5—O5—Na	73.2 (4)
O9—Mo5—O1—Mo4	−171.7 (3)	O7—Mo5—O5—Na	−78.4 (4)
O7—Mo5—O1—Mo4	19.0 (3)	O1—Mo5—O5—Na	−2.7 (5)
O22—Mo5—O1—Mo4	103.0 (3)	O18—Na—O5—Mo5	−46.6 (4)
Mo2—Mo5—O1—Mo4	−152.7 (3)	O18ⁱ—Na—O5—Mo5	133.4 (4)
Na—Mo5—O1—Mo4	−77.69 (17)	O24ⁱ—Na—O5—Mo5	−128.7 (4)
O23—Mo5—O1—Mo1	−1.3 (8)	O24—Na—O5—Mo5	51.3 (4)
O5—Mo5—O1—Mo1	−179.6 (3)	O21—Mo7—O6—Mo3	−84.8 (4)
O9—Mo5—O1—Mo1	84.9 (3)	O20—Mo7—O6—Mo3	167.4 (4)
O7—Mo5—O1—Mo1	−84.4 (3)	O11—Mo7—O6—Mo3	38.6 (7)
O22—Mo5—O1—Mo1	−0.3 (2)	O3—Mo7—O6—Mo3	19.8 (3)
Mo4—Mo5—O1—Mo1	−103.4 (3)	O17—Mo3—O6—Mo7	72.6 (4)
Mo2—Mo5—O1—Mo1	103.9 (3)	O15—Mo3—O6—Mo7	177.3 (4)
Na—Mo5—O1—Mo1	178.9 (2)	O8—Mo3—O6—Mo7	−61.3 (8)
O22—Mo1—O1—Mo2	98.5 (3)	O3—Mo3—O6—Mo7	−20.0 (3)
O4—Mo1—O1—Mo2	−4.4 (3)	O2—Mo3—O6—Mo7	−93.0 (3)
O2—Mo1—O1—Mo2	−158.6 (3)	O23—Mo5—O7—Mo4	−173.2 (4)
O3—Mo1—O1—Mo2	−81.5 (3)	O5—Mo5—O7—Mo4	78.6 (4)
O22—Mo1—O1—Mo4	−97.2 (3)	O9—Mo5—O7—Mo4	−41.2 (7)
O4—Mo1—O1—Mo4	159.9 (3)	O1—Mo5—O7—Mo4	−22.1 (3)
O2—Mo1—O1—Mo4	5.7 (3)	O22—Mo5—O7—Mo4	−94.5 (3)
O3—Mo1—O1—Mo4	82.8 (3)	O14—Mo4—O7—Mo5	−173.9 (4)
O4—Mo1—O1—Mo5	−102.4 (3)	O24—Mo4—O7—Mo5	−66.8 (4)
O2—Mo1—O1—Mo5	103.4 (3)	O8—Mo4—O7—Mo5	65.4 (7)
O3—Mo1—O1—Mo5	−179.5 (3)	O1—Mo4—O7—Mo5	22.2 (3)
O16—Mo1—O2—Mo4	−176.3 (3)	O2—Mo4—O7—Mo5	94.6 (3)
O22—Mo1—O2—Mo4	75.2 (4)	O17—Mo3—O8—Mo4	173.8 (4)
O4—Mo1—O2—Mo4	−50.1 (6)	O15—Mo3—O8—Mo4	67.8 (4)
O1—Mo1—O2—Mo4	−5.6 (3)	O6—Mo3—O8—Mo4	−52.1 (8)
O3—Mo1—O2—Mo4	−96.1 (3)	O3—Mo3—O8—Mo4	−91.3 (4)
O16—Mo1—O2—Mo3	−76.2 (4)	O2—Mo3—O8—Mo4	−19.0 (3)
O22—Mo1—O2—Mo3	175.4 (3)	O14—Mo4—O8—Mo3	−69.8 (4)
O4—Mo1—O2—Mo3	50.1 (6)	O24—Mo4—O8—Mo3	−177.7 (4)
O1—Mo1—O2—Mo3	94.6 (3)	O7—Mo4—O8—Mo3	49.5 (7)
O3—Mo1—O2—Mo3	4.1 (3)	O1—Mo4—O8—Mo3	90.7 (4)
O14—Mo4—O2—Mo1	−162.4 (4)	O2—Mo4—O8—Mo3	19.1 (3)
O24—Mo4—O2—Mo1	35.8 (10)	O23—Mo5—O9—Mo2	172.7 (3)
O8—Mo4—O2—Mo1	97.5 (3)	O5—Mo5—O9—Mo2	−78.8 (4)
O7—Mo4—O2—Mo1	−69.1 (3)	O7—Mo5—O9—Mo2	41.0 (7)
O1—Mo4—O2—Mo1	6.1 (3)	O1—Mo5—O9—Mo2	21.8 (3)
O14—Mo4—O2—Mo3	86.0 (3)	O22—Mo5—O9—Mo2	94.0 (3)
O24—Mo4—O2—Mo3	−75.9 (9)	O10—Mo2—O9—Mo5	175.0 (4)
O8—Mo4—O2—Mo3	−14.2 (2)	O18—Mo2—O9—Mo5	69.1 (4)
O7—Mo4—O2—Mo3	179.3 (3)	O13—Mo2—O9—Mo5	−69.3 (7)
O1—Mo4—O2—Mo3	−105.6 (3)	O1—Mo2—O9—Mo5	−22.1 (3)
O17—Mo3—O2—Mo1	−40.2 (13)	O4—Mo2—O9—Mo5	−94.4 (3)
O15—Mo3—O2—Mo1	161.3 (4)	O21—Mo7—O11—Mo6	83.0 (4)
O8—Mo3—O2—Mo1	−98.0 (3)	O20—Mo7—O11—Mo6	−169.8 (4)
O6—Mo3—O2—Mo1	68.9 (3)	O6—Mo7—O11—Mo6	−40.1 (7)
O3—Mo3—O2—Mo1	−4.5 (3)	O3—Mo7—O11—Mo6	−21.3 (3)
O17—Mo3—O2—Mo4	72.3 (13)	O19—Mo6—O11—Mo7	−70.7 (4)
O15—Mo3—O2—Mo4	−86.3 (3)	O12—Mo6—O11—Mo7	−176.6 (4)
O8—Mo3—O2—Mo4	14.5 (2)	O13—Mo6—O11—Mo7	60.0 (8)
O6—Mo3—O2—Mo4	−178.6 (3)	O3—Mo6—O11—Mo7	21.4 (3)
O3—Mo3—O2—Mo4	108.0 (3)	O4—Mo6—O11—Mo7	94.2 (4)
O17—Mo3—O3—Mo7	−81.0 (3)	O10—Mo2—O13—Mo6	69.2 (4)
O15—Mo3—O3—Mo7	67.6 (8)	O18—Mo2—O13—Mo6	176.4 (4)
O8—Mo3—O3—Mo7	−179.1 (3)	O9—Mo2—O13—Mo6	−44.9 (8)
O6—Mo3—O3—Mo7	16.7 (3)	O1—Mo2—O13—Mo6	−89.6 (4)
O2—Mo3—O3—Mo7	107.7 (3)	O4—Mo2—O13—Mo6	−18.9 (3)
O17—Mo3—O3—Mo6	35.3 (7)	O19—Mo6—O13—Mo2	−174.1 (4)
O15—Mo3—O3—Mo6	−176.0 (7)	O12—Mo6—O13—Mo2	−67.7 (4)
O8—Mo3—O3—Mo6	−62.7 (7)	O11—Mo6—O13—Mo2	54.7 (8)
O6—Mo3—O3—Mo6	133.1 (7)	O3—Mo6—O13—Mo2	91.3 (3)
O2—Mo3—O3—Mo6	−135.9 (7)	O4—Mo6—O13—Mo2	19.2 (3)
O17—Mo3—O3—Mo1	174.9 (3)	O17—Mo3—O15—Co	−35.9 (13)
O15—Mo3—O3—Mo1	−36.5 (9)	O8—Mo3—O15—Co	65.3 (13)
O8—Mo3—O3—Mo1	76.8 (3)	O6—Mo3—O15—Co	−135.6 (13)
O6—Mo3—O3—Mo1	−87.4 (3)	O3—Mo3—O15—Co	176.4 (8)
O2—Mo3—O3—Mo1	3.6 (2)	O2—Mo3—O15—Co	138.5 (13)
O21—Mo7—O3—Mo3	77.5 (4)	OW3—Co—O15—Mo3	−49.1 (13)
O20—Mo7—O3—Mo3	−105.7 (6)	OW4—Co—O15—Mo3	43.9 (13)
O11—Mo7—O3—Mo3	173.4 (3)	OW1—Co—O15—Mo3	130.2 (13)
O6—Mo7—O3—Mo3	−17.2 (3)	OW2—Co—O15—Mo3	−139.3 (13)
O21—Mo7—O3—Mo6	−77.6 (3)	O10—Mo2—O18—Na	−150.1 (5)
O20—Mo7—O3—Mo6	99.1 (6)	O13—Mo2—O18—Na	107.5 (5)
O11—Mo7—O3—Mo6	18.3 (3)	O9—Mo2—O18—Na	−54.8 (5)
O6—Mo7—O3—Mo6	−172.3 (3)	O1—Mo2—O18—Na	19.2 (5)
O21—Mo7—O3—Mo1	−179.7 (3)	O4—Mo2—O18—Na	46.4 (13)
O20—Mo7—O3—Mo1	−2.9 (7)	O5—Na—O18—Mo2	38.4 (5)
O11—Mo7—O3—Mo1	−83.8 (3)	O5ⁱ—Na—O18—Mo2	−141.6 (5)
O6—Mo7—O3—Mo1	85.6 (3)	O24ⁱ—Na—O18—Mo2	140.0 (6)
O19—Mo6—O3—Mo3	−35.6 (7)	O24—Na—O18—Mo2	−40.0 (6)
O12—Mo6—O3—Mo3	170.5 (7)	O16—Mo1—O22—Mo5	−179.1 (3)
O13—Mo6—O3—Mo3	61.5 (7)	O4—Mo1—O22—Mo5	75.1 (3)
O11—Mo6—O3—Mo3	−134.2 (7)	O2—Mo1—O22—Mo5	−74.7 (3)
O4—Mo6—O3—Mo3	135.9 (7)	O1—Mo1—O22—Mo5	−0.4 (3)
Mo7—Mo6—O3—Mo3	−116.5 (8)	O23—Mo5—O22—Mo1	−180.0 (4)
O19—Mo6—O3—Mo7	80.9 (3)	O9—Mo5—O22—Mo1	−76.3 (3)
O12—Mo6—O3—Mo7	−73.0 (8)	O7—Mo5—O22—Mo1	77.5 (3)
O13—Mo6—O3—Mo7	178.0 (3)	O1—Mo5—O22—Mo1	0.5 (3)
O11—Mo6—O3—Mo7	−17.7 (3)	O14—Mo4—O24—Na	152.4 (5)
O4—Mo6—O3—Mo7	−107.6 (3)	O8—Mo4—O24—Na	−104.6 (5)
O19—Mo6—O3—Mo1	−175.2 (3)	O7—Mo4—O24—Na	55.5 (6)
O12—Mo6—O3—Mo1	30.9 (9)	O1—Mo4—O24—Na	−18.5 (6)
O13—Mo6—O3—Mo1	−78.1 (3)	O2—Mo4—O24—Na	−46.5 (12)
O11—Mo6—O3—Mo1	86.2 (3)	O18—Na—O24—Mo4	40.2 (6)
O4—Mo6—O3—Mo1	−3.8 (2)	O18ⁱ—Na—O24—Mo4	−139.8 (6)
Mo7—Mo6—O3—Mo1	103.9 (3)	O5—Na—O24—Mo4	−40.9 (5)
O16—Mo1—O3—Mo3	98.4 (3)	O5ⁱ—Na—O24—Mo4	139.1 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
OW1—H1···OW5	0.89	2.33	2.988 (15)	131
OW1—H2···OW8	0.85	2.14	2.827 (15)	139
OW1—H1···O20ⁱⁱⁱ	0.89	2.05	2.837 (12)	147
OW2—H3···OW7	0.83	1.97	2.795 (17)	170
OW2—H4···O21^iv	0.82	2.07	2.859 (12)	162
OW3—H5···O23^v	0.83	2.29	2.778 (12)	118
OW3—H5···O23^v	0.83	2.29	2.778 (12)	118
OW4—H8···OW1	1.01	2.15	2.879 (13)	128
OW4—H8···OW8ⁱⁱⁱ	1.01	2.35	2.879 (16)	112
OW4—H7···O22^v	0.79	2.48	2.793 (11)	106
OW5—H10···OW4	1.00	2.49	3.029 (16)	114
OW5—H9···O20^iv	0.89	2.04	2.849 (15)	150
OW6—H11···O6	0.81	2.35	2.993 (14)	136
OW6—H12···OW7ⁱⁱⁱ	0.88	2.42	3.123 (17)	136
OW7—H13···O2	0.87	2.02	2.767 (13)	144
OW7—H14···OW9	0.92	2.10	2.98 (2)	161
OW8—H16···O6	0.83	2.50	2.791 (13)	102
OW8—H16···O6	0.83	2.50	2.791 (13)	102
OW8—H16···OW7	0.83	2.28	2.965 (19)	140
OW9—H17···OW6^vi	1.00	2.22	3.00 (2)	134
OW9—H18···OW2^vii	1.00	2.30	3.111 (18)	137
N1—H1A···O8	0.86	2.22	2.968 (11)	145
N1—H1B···O10^viii	0.86	2.14	2.967 (11)	161
N2—H2A···O9^v	0.86	2.18	2.992 (11)	157
N2—H2B···O8	0.86	2.18	2.936 (11)	147
N3—H3A···O9^v	0.86	2.48	3.216 (11)	144
N3—H3A···O10^v	0.86	2.28	3.031 (11)	145
N3—H3B···O13^viii	0.86	2.35	3.128 (11)	151
N4—H4B···O5^ix	0.86	2.31	2.954 (12)	131
N4—H4A···O12	0.86	2.09	2.918 (12)	160
N5—H5A···O4	0.86	2.11	2.965 (11)	177
N5—H5B···O17^x	0.86	2.18	3.011 (12)	161
N6—H6A···O19^x	0.86	2.37	2.864 (12)	117
N7—H7B···O7	0.86	2.42	3.175 (13)	147
N7—H7B···O14	0.86	2.37	3.107 (13)	144
N8—H8A···O16^xi	0.86	2.16	2.952 (13)	153
N8—H8B···OW6^iv	0.86	2.18	2.992 (18)	157
N9—H9A···O11^xi	0.86	2.09	2.918 (14)	162
N9—H9B···O7	0.86	2.18	2.992 (13)	157
N10—H10A···O12^xi	0.86	2.26	3.100 (13)	167
N10—H10B···O5	0.86	2.29	2.960 (12)	135
N11—H11B···O24^x	0.86	2.22	2.935 (15)	141
N11—H11A···O19^xi	0.86	2.09	2.916 (16)	160

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

Experimental details

Crystal data
Chemical formula	(CH₆N₃)₇Na[CoMo₇O₂₄(H₂O)₅]₂·8H₂O
M_r	2996.92
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	18.819 (3), 10.581 (2), 19.926 (3)
β (°)	102.635 (2)
V (Å³)	3871.7 (11)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.73
Crystal size (mm)	0.28 × 0.22 × 0.16

Data collection
Diffractometer	Bruker SMART CCD APEX II
Absorption correction	Multi-scan (SADABS; Bruker, 2002)
T_min, T_max	0.485, 0.650
No. of measured, independent and observed [I > 2σ(I)] reflections	19853, 7505, 4569
R_int	0.074
(sin θ/λ)_max (Å⁻¹)	0.618

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.096, 0.99
No. of reflections	7505
No. of parameters	511
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.68, −0.55

Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXTL (Bruker, 1997), SHELXTL, DIAMOND (Brandenburg, 1999).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
OW1—H1···OW5	0.89	2.33	2.988 (15)	131
OW1—H2···OW8	0.85	2.14	2.827 (15)	139
OW1—H1···O20ⁱ	0.89	2.05	2.837 (12)	147
OW2—H3···OW7	0.83	1.97	2.795 (17)	170
OW2—H4···O21ⁱⁱ	0.82	2.07	2.859 (12)	162
OW3—H5···O23ⁱⁱⁱ	0.83	2.29	2.778 (12)	118
OW3—H5···O23ⁱⁱⁱ	0.83	2.29	2.778 (12)	118
OW4—H8···OW1	1.01	2.15	2.879 (13)	128
OW4—H8···OW8ⁱ	1.01	2.35	2.879 (16)	112
OW4—H7···O22ⁱⁱⁱ	0.79	2.48	2.793 (11)	106
OW5—H10···OW4	1.00	2.49	3.029 (16)	114
OW5—H9···O20ⁱⁱ	0.89	2.04	2.849 (15)	150
OW6—H11···O6	0.81	2.35	2.993 (14)	136
OW6—H12···OW7ⁱ	0.88	2.42	3.123 (17)	136
OW7—H13···O2	0.87	2.02	2.767 (13)	144
OW7—H14···OW9	0.92	2.10	2.98 (2)	161
OW8—H16···O6	0.83	2.50	2.791 (13)	102
OW8—H16···O6	0.83	2.50	2.791 (13)	102
OW8—H16···OW7	0.83	2.28	2.965 (19)	140
OW9—H17···OW6^iv	1.00	2.22	3.00 (2)	134
OW9—H18···OW2^v	1.00	2.30	3.111 (18)	137
N1—H1A···O8	0.86	2.22	2.968 (11)	145
N1—H1B···O10^vi	0.86	2.14	2.967 (11)	161
N2—H2A···O9ⁱⁱⁱ	0.86	2.18	2.992 (11)	157
N2—H2B···O8	0.86	2.18	2.936 (11)	147
N3—H3A···O9ⁱⁱⁱ	0.86	2.48	3.216 (11)	144
N3—H3A···O10ⁱⁱⁱ	0.86	2.28	3.031 (11)	145
N3—H3B···O13^vi	0.86	2.35	3.128 (11)	151
N4—H4B···O5^vii	0.86	2.31	2.954 (12)	131
N4—H4A···O12	0.86	2.09	2.918 (12)	160
N5—H5A···O4	0.86	2.11	2.965 (11)	177
N5—H5B···O17^viii	0.86	2.18	3.011 (12)	161
N6—H6A···O19^viii	0.86	2.37	2.864 (12)	117
N7—H7B···O7	0.86	2.42	3.175 (13)	147
N7—H7B···O14	0.86	2.37	3.107 (13)	144
N8—H8A···O16^ix	0.86	2.16	2.952 (13)	153
N8—H8B···OW6ⁱⁱ	0.86	2.18	2.992 (18)	157
N9—H9A···O11^ix	0.86	2.09	2.918 (14)	162
N9—H9B···O7	0.86	2.18	2.992 (13)	157
N10—H10A···O12^ix	0.86	2.26	3.100 (13)	167
N10—H10B···O5	0.86	2.29	2.960 (12)	135
N11—H11B···O24^viii	0.86	2.22	2.935 (15)	141
N11—H11A···O19^ix	0.86	2.09	2.916 (16)	160

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

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