Tetra­kis(1-n-hexyl­pyridinium) octa­molybdate

Guo, M.-L.; Guo, C.-H.; Li, H.-Z.; Chang, H.

doi:10.1107/S1600536807019423

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Tetrakis(1-n-hexylpyridinium) octamolybdate

M.-L. Guo, C.-H. Guo, H.-Z. Li and H. Chang

The asymmetric unit of the title compound, (C₁₁H₁₈N)₄[Mo₈O₂₆], contains two cations and one half-anion; the anion is centrosymmetric. The anion is a β-isomer. Although no classical hydrogen bonds are found, a large number of weak intermolecular C—H

O hydrogen bonds and van der Waals forces stabilize the packing of the ions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807019423/pk2017sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807019423/pk2017Isup2.hkl Contains datablock I

CCDC reference: 646648

checkCIF report

Key indicators

Single-crystal X-ray study
T = 294 K
Mean (C-C) = 0.016 Å
R factor = 0.044
wR factor = 0.114
Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         16

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

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

Comment top

Polymolybdates have attracted considerable interest for application in selective catalysis of oxidation reactions with hydrogen peroxide. The synthesis and crystal structure reported here is part of this study (Guo and Li, 2007).

The title compound, (I), consists of a centrosymmetric β-octamolybdate anion and four n-hexylpyridinium cations. The structure of the anion is constructed from an array of eight edge-shared MoO₆ octahedra. The Mo–O bond lengths can be grouped into four sets: Mo–O(t) 1.672 (6)–1.694 (5) Å, Mo–O(µ2) 1.725 (5)–2.311 (5) Å, Mo–O(µ3) 1.939 (5)–2.311 (5) Å, Mo–O(µ5) 2.128 (5)–2.374 (5) Å. The molecule of the compound is shown in Fig. 1.

In the structure of (I), no classic hydrogen bonds are found, but there exist a number of weak C–H···O interactions (see Table 1). These are further loosely aggregated into a three-dimensional framework via van der Waals forces. A packing diagram for the structure of (I) is shown in Fig. 2.

Related literature top

For related literature, see: Guo & Li (2007); Deng et al. (2005); Wang et al. (1993); Wilson et al. (1984).

Experimental top

A solution of n-hexylpyridinium bromide (1.80 g, 7 mmol) in 10 ml of distilled water was added dropwise to a mixture of 20 ml aqueous solution of dihydrate sodium molybdate (1.2 g, 5 mmol) and 12% dilute hydrogen chloride (1.8 ml, 7 mmol) under stirring at 70°C. A white precipitate was immediately formed. After continuously stirring for 20 min, the resulting product was filtered, washed with water and dried at room temperature to produce the tetra-n-hexylpyridinium octamolybdate in 89% yield. Single crystals were separated from the above filtrate by slowly evaporating over a period of 1 d at 40°C.

Structure description top

For related literature, see: Guo & Li (2007); Deng et al. (2005); Wang et al. (1993); Wilson et al. (1984).

Computing details top

Data collection: SMART (Bruker 1997); cell refinement: SAINT (Bruker 1997); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures top

	Fig. 1. A view of the structure of (I), showing the atom-numbering Scheme; displacement ellipsoids were drawn at the 30% probability level.
	Fig. 2. Packing diagram showing hydrogen bonds interactions, viewed roughly down the diagonal between the a and c axes.

Tetrakis(1-n-hexylpyridinium) octamolybdate top

Crystal data top

(C₁₁H₁₈N)₄[Mo₈O₂₆]	F(000) = 1816
M_r = 1840.58	D_x = 1.983 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2002 reflections
a = 15.474 (4) Å	θ = 2.4–21.6°
b = 12.051 (3) Å	µ = 1.65 mm⁻¹
c = 16.592 (4) Å	T = 294 K
β = 94.964 (5)°	Block, colorless
V = 3082.4 (13) Å³	0.22 × 0.20 × 0.16 mm
Z = 2

Data collection top

Bruker SMART CCD area-detector diffractometer	5450 independent reflections
Radiation source: fine-focus sealed tube	2782 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.082
φ and ω scans	θ_max = 25.0°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −18→11
T_min = 0.698, T_max = 0.765	k = −14→14
15694 measured reflections	l = −19→19

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.114	H-atom parameters constrained
S = 0.95	w = 1/[σ²(F_o²) + (0.0421P)²] where P = (F_o² + 2F_c²)/3
5450 reflections	(Δ/σ)_max < 0.001
370 parameters	Δρ_max = 0.63 e Å⁻³
78 restraints	Δρ_min = −0.62 e Å⁻³

Crystal data top

(C₁₁H₁₈N)₄[Mo₈O₂₆]	V = 3082.4 (13) Å³
M_r = 1840.58	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 15.474 (4) Å	µ = 1.65 mm⁻¹
b = 12.051 (3) Å	T = 294 K
c = 16.592 (4) Å	0.22 × 0.20 × 0.16 mm
β = 94.964 (5)°

Data collection top

Bruker SMART CCD area-detector diffractometer	5450 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2782 reflections with I > 2σ(I)
T_min = 0.698, T_max = 0.765	R_int = 0.082
15694 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	78 restraints
wR(F²) = 0.114	H-atom parameters constrained
S = 0.95	Δρ_max = 0.63 e Å⁻³
5450 reflections	Δρ_min = −0.62 e Å⁻³
370 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 > 2σ(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
Mo1	0.41536 (5)	0.20179 (6)	0.04058 (5)	0.0450 (2)
Mo2	0.48353 (5)	0.07732 (7)	0.20537 (5)	0.0499 (3)
Mo3	0.53068 (5)	0.16326 (7)	−0.12012 (5)	0.0476 (2)
Mo4	0.39661 (5)	−0.03796 (6)	−0.04320 (5)	0.0408 (2)
O1	0.4177 (4)	0.3339 (5)	0.0102 (4)	0.0603 (18)
O2	0.3120 (4)	0.1786 (5)	0.0627 (4)	0.0545 (17)
O3	0.5349 (4)	0.1230 (6)	0.2923 (4)	0.0670 (19)
O4	0.3787 (4)	0.0657 (5)	0.2242 (4)	0.0588 (18)
O5	0.4897 (4)	0.2894 (5)	−0.1449 (4)	0.0638 (19)
O6	0.6361 (4)	0.1711 (5)	−0.1393 (4)	0.0618 (19)
O7	0.2955 (3)	−0.0510 (5)	−0.0137 (3)	0.0504 (16)
O8	0.4487 (3)	−0.1747 (4)	0.0012 (3)	0.0404 (14)
O9	0.4740 (3)	0.2126 (5)	0.1435 (3)	0.0497 (16)
O10	0.4588 (3)	0.0179 (4)	0.0689 (3)	0.0412 (14)
O11	0.4034 (3)	0.1201 (4)	−0.0639 (3)	0.0424 (15)
O12	0.4840 (3)	0.0770 (5)	−0.2070 (3)	0.0494 (16)
O13	0.3885 (3)	−0.0793 (5)	−0.1431 (3)	0.0484 (15)
N1	0.2719 (6)	0.4703 (7)	0.8434 (5)	0.063 (2)
N2	0.1678 (5)	0.0741 (6)	0.2113 (5)	0.0553 (18)
C1	0.2063 (8)	0.5384 (10)	0.8243 (7)	0.078 (3)
H1	0.1574	0.5123	0.7935	0.094*
C2	0.2091 (9)	0.6445 (10)	0.8486 (9)	0.095 (4)
H2	0.1626	0.6918	0.8354	0.114*
C3	0.2804 (12)	0.6813 (11)	0.8924 (9)	0.113 (5)
H3	0.2836	0.7549	0.9092	0.136*
C4	0.3472 (10)	0.6120 (14)	0.9121 (9)	0.109 (5)
H4	0.3958	0.6377	0.9435	0.131*
C5	0.3441 (8)	0.5047 (11)	0.8863 (7)	0.081 (3)
H5	0.3906	0.4569	0.8981	0.097*
C6	0.2610 (6)	0.3530 (8)	0.8199 (6)	0.072 (2)
H6A	0.3178	0.3195	0.8179	0.086*
H6B	0.2312	0.3490	0.7661	0.086*
C7	0.2105 (6)	0.2877 (8)	0.8775 (6)	0.070 (2)
H7A	0.2436	0.2828	0.9297	0.084*
H7B	0.1564	0.3254	0.8848	0.084*
C8	0.1920 (6)	0.1735 (8)	0.8450 (7)	0.073 (2)
H8A	0.2466	0.1354	0.8405	0.088*
H8B	0.1628	0.1796	0.7911	0.088*
C9	0.1370 (7)	0.1045 (9)	0.8962 (7)	0.078 (2)
H9A	0.0820	0.1418	0.9006	0.094*
H9B	0.1659	0.0978	0.9502	0.094*
C10	0.1201 (7)	−0.0099 (9)	0.8613 (7)	0.084 (2)
H10A	0.0911	−0.0031	0.8073	0.101*
H10B	0.1751	−0.0471	0.8568	0.101*
C11	0.0653 (8)	−0.0788 (10)	0.9123 (7)	0.103 (4)
H11A	0.0974	−0.0949	0.9632	0.155*
H11B	0.0500	−0.1470	0.8848	0.155*
H11C	0.0136	−0.0387	0.9218	0.155*
C12	0.1944 (6)	0.0055 (8)	0.1554 (6)	0.053 (3)
H12	0.2310	0.0314	0.1180	0.064*
C13	0.1683 (6)	−0.1019 (9)	0.1532 (7)	0.067 (3)
H13	0.1884	−0.1507	0.1155	0.080*
C14	0.1128 (7)	−0.1372 (9)	0.2062 (8)	0.078 (3)
H14	0.0915	−0.2094	0.2032	0.094*
C15	0.0881 (7)	−0.0664 (11)	0.2643 (7)	0.091 (4)
H15	0.0536	−0.0917	0.3036	0.109*
C16	0.1140 (7)	0.0401 (10)	0.2642 (6)	0.076 (3)
H16	0.0942	0.0900	0.3012	0.092*
C17	0.1953 (6)	0.1912 (7)	0.2100 (6)	0.0611 (19)
H17A	0.2547	0.1946	0.1958	0.073*
H17B	0.1939	0.2221	0.2639	0.073*
C18	0.1401 (6)	0.2599 (8)	0.1522 (6)	0.068 (2)
H18A	0.0831	0.2671	0.1718	0.082*
H18B	0.1332	0.2220	0.1005	0.082*
C19	0.1760 (7)	0.3735 (9)	0.1398 (6)	0.074 (2)
H19A	0.1864	0.4092	0.1922	0.088*
H19B	0.2316	0.3658	0.1175	0.088*
C20	0.1206 (7)	0.4467 (9)	0.0863 (7)	0.084 (2)
H20A	0.0653	0.4567	0.1087	0.101*
H20B	0.1096	0.4118	0.0337	0.101*
C21	0.1629 (8)	0.5616 (9)	0.0757 (7)	0.092 (3)
H21A	0.1800	0.5928	0.1285	0.111*
H21B	0.2147	0.5526	0.0473	0.111*
C22	0.1029 (8)	0.6387 (11)	0.0300 (8)	0.119 (4)
H22A	0.0886	0.6101	−0.0235	0.179*
H22B	0.1302	0.7099	0.0265	0.179*
H22C	0.0510	0.6464	0.0572	0.179*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0468 (5)	0.0387 (5)	0.0525 (6)	0.0037 (4)	0.0212 (4)	−0.0021 (4)
Mo2	0.0500 (5)	0.0571 (6)	0.0447 (6)	0.0045 (4)	0.0156 (4)	−0.0054 (4)
Mo3	0.0508 (5)	0.0426 (5)	0.0529 (6)	−0.0015 (4)	0.0245 (4)	0.0059 (4)
Mo4	0.0381 (4)	0.0379 (5)	0.0484 (5)	−0.0023 (4)	0.0154 (4)	−0.0029 (4)
O1	0.071 (4)	0.036 (4)	0.078 (5)	0.005 (3)	0.029 (4)	0.001 (3)
O2	0.048 (4)	0.059 (4)	0.061 (4)	0.003 (3)	0.027 (3)	0.004 (3)
O3	0.070 (5)	0.079 (5)	0.054 (4)	0.010 (4)	0.013 (3)	−0.016 (4)
O4	0.045 (4)	0.073 (5)	0.061 (4)	0.007 (3)	0.023 (3)	0.003 (4)
O5	0.073 (5)	0.053 (4)	0.069 (5)	0.004 (4)	0.027 (4)	0.017 (4)
O6	0.051 (4)	0.069 (5)	0.070 (5)	−0.008 (3)	0.031 (3)	0.013 (4)
O7	0.040 (4)	0.045 (4)	0.069 (4)	−0.004 (3)	0.021 (3)	−0.001 (3)
O8	0.043 (3)	0.038 (3)	0.043 (4)	0.001 (3)	0.020 (3)	−0.001 (3)
O9	0.050 (4)	0.045 (4)	0.056 (4)	−0.001 (3)	0.015 (3)	−0.013 (3)
O10	0.043 (3)	0.033 (3)	0.050 (4)	−0.002 (3)	0.018 (3)	−0.002 (3)
O11	0.040 (3)	0.042 (4)	0.046 (4)	0.003 (3)	0.015 (3)	0.007 (3)
O12	0.050 (4)	0.063 (4)	0.038 (4)	0.013 (3)	0.017 (3)	0.006 (3)
O13	0.047 (4)	0.049 (4)	0.050 (4)	−0.001 (3)	0.011 (3)	−0.007 (3)
N1	0.065 (6)	0.053 (6)	0.072 (6)	−0.011 (5)	0.011 (5)	0.000 (5)
N2	0.054 (4)	0.049 (4)	0.066 (4)	0.010 (3)	0.027 (4)	−0.001 (4)
C1	0.082 (9)	0.058 (8)	0.095 (10)	−0.017 (7)	0.019 (7)	0.000 (7)
C2	0.100 (11)	0.055 (9)	0.133 (13)	−0.013 (7)	0.020 (9)	−0.009 (8)
C3	0.169 (17)	0.053 (9)	0.121 (14)	−0.023 (10)	0.027 (12)	−0.004 (9)
C4	0.109 (12)	0.092 (12)	0.123 (13)	−0.048 (10)	−0.002 (9)	0.008 (10)
C5	0.082 (9)	0.081 (10)	0.080 (9)	−0.010 (7)	0.007 (7)	0.018 (7)
C6	0.066 (5)	0.055 (5)	0.093 (6)	−0.008 (4)	0.008 (4)	−0.003 (5)
C7	0.066 (4)	0.054 (4)	0.090 (5)	−0.005 (4)	0.004 (4)	0.001 (4)
C8	0.070 (4)	0.057 (4)	0.093 (5)	−0.002 (4)	0.004 (4)	0.003 (4)
C9	0.072 (4)	0.062 (4)	0.099 (5)	−0.003 (4)	0.002 (4)	0.005 (4)
C10	0.079 (5)	0.068 (5)	0.105 (5)	−0.005 (4)	0.001 (4)	0.007 (5)
C11	0.101 (5)	0.096 (5)	0.111 (5)	−0.003 (4)	0.001 (4)	0.006 (4)
C12	0.048 (6)	0.054 (7)	0.059 (7)	−0.002 (5)	0.020 (5)	−0.004 (5)
C13	0.052 (7)	0.058 (8)	0.094 (9)	0.011 (5)	0.022 (6)	0.007 (6)
C14	0.070 (8)	0.048 (7)	0.117 (11)	0.008 (6)	0.013 (7)	0.013 (7)
C15	0.077 (9)	0.104 (11)	0.099 (10)	0.013 (8)	0.047 (7)	0.051 (9)
C16	0.073 (8)	0.078 (9)	0.085 (9)	0.030 (7)	0.049 (7)	0.022 (7)
C17	0.064 (4)	0.053 (4)	0.070 (4)	0.007 (4)	0.024 (4)	−0.005 (4)
C18	0.071 (4)	0.060 (4)	0.078 (5)	0.005 (4)	0.024 (4)	−0.003 (4)
C19	0.081 (5)	0.065 (5)	0.079 (5)	0.002 (4)	0.026 (4)	−0.003 (4)
C20	0.091 (5)	0.077 (5)	0.086 (5)	0.003 (4)	0.025 (4)	−0.001 (4)
C21	0.102 (5)	0.086 (5)	0.091 (5)	0.005 (5)	0.026 (5)	0.004 (5)
C22	0.126 (5)	0.115 (5)	0.117 (5)	−0.002 (4)	0.014 (4)	0.003 (4)

Geometric parameters (Å, º) top

Mo1—O1	1.672 (6)	C6—H6A	0.9700
Mo1—O2	1.694 (5)	C6—H6B	0.9700
Mo2—O3	1.678 (6)	C7—C8	1.496 (12)
Mo2—O4	1.684 (5)	C7—H7A	0.9700
Mo3—O5	1.684 (6)	C7—H7B	0.9700
Mo3—O6	1.692 (5)	C8—C9	1.504 (13)
Mo4—O7	1.686 (5)	C8—H8A	0.9700
Mo1—O9	1.867 (6)	C8—H8B	0.9700
Mo2—O12ⁱ	1.925 (6)	C9—C10	1.510 (13)
Mo2—O9	1.926 (6)	C9—H9A	0.9700
Mo2—O13ⁱ	2.311 (5)	C9—H9B	0.9700
Mo3—O12	1.870 (6)	C10—C11	1.501 (14)
Mo4—O13	1.725 (5)	C10—H10A	0.9700
Mo1—O11	1.989 (5)	C10—H10B	0.9700
Mo1—O8ⁱ	2.295 (5)	C11—H11A	0.9600
Mo3—O8ⁱ	1.976 (5)	C11—H11B	0.9600
Mo3—O11	2.311 (5)	C11—H11C	0.9600
Mo4—O11	1.939 (5)	C12—C13	1.355 (12)
Mo4—O8	1.951 (5)	C12—H12	0.9300
Mo2—O10	2.374 (5)	C13—C14	1.351 (13)
Mo1—O10	2.351 (5)	C13—H13	0.9300
Mo3—O10ⁱ	2.344 (5)	C14—C15	1.367 (15)
Mo4—O10	2.128 (5)	C14—H14	0.9300
Mo4—O10ⁱ	2.327 (5)	C15—C16	1.345 (15)
Mo1—Mo4	3.2085 (13)	C15—H15	0.9300
Mo1—Mo2	3.2154 (14)	C16—H16	0.9300
Mo3—Mo4ⁱ	3.2188 (13)	C17—C18	1.481 (12)
Mo4—Mo3ⁱ	3.2188 (13)	C17—H17A	0.9700
N1—C1	1.322 (12)	C17—H17B	0.9700
N1—C5	1.338 (13)	C18—C19	1.499 (13)
N1—C6	1.472 (12)	C18—H18A	0.9700
N2—C16	1.325 (10)	C18—H18B	0.9700
N2—C12	1.333 (10)	C19—C20	1.474 (13)
N2—C17	1.475 (11)	C19—H19A	0.9700
C1—C2	1.340 (14)	C19—H19B	0.9700
C1—H1	0.9300	C20—C21	1.547 (14)
C2—C3	1.342 (17)	C20—H20A	0.9700
C2—H2	0.9300	C20—H20B	0.9700
C3—C4	1.347 (17)	C21—C22	1.476 (15)
C3—H3	0.9300	C21—H21A	0.9700
C4—C5	1.362 (17)	C21—H21B	0.9700
C4—H4	0.9300	C22—H22A	0.9600
C5—H5	0.9300	C22—H22B	0.9600
C6—C7	1.507 (12)	C22—H22C	0.9600

O1—Mo1—O2	105.6 (3)	Mo4—O11—Mo3	110.7 (2)
O1—Mo1—O9	100.8 (3)	Mo1—O11—Mo3	102.8 (2)
O2—Mo1—O9	101.9 (3)	Mo3—O12—Mo2ⁱ	116.3 (3)
O1—Mo1—O11	102.2 (3)	Mo4—O13—Mo2ⁱ	115.7 (3)
O2—Mo1—O11	95.1 (2)	C1—N1—C5	121.6 (10)
O9—Mo1—O11	146.4 (2)	C1—N1—C6	117.7 (9)
O1—Mo1—O8ⁱ	90.0 (2)	C5—N1—C6	120.6 (10)
O2—Mo1—O8ⁱ	161.6 (2)	C16—N2—C12	121.2 (9)
O9—Mo1—O8ⁱ	84.3 (2)	C16—N2—C17	120.2 (8)
O11—Mo1—O8ⁱ	71.63 (19)	C12—N2—C17	118.5 (8)
O1—Mo1—O10	160.9 (2)	N1—C1—C2	121.0 (12)
O2—Mo1—O10	93.4 (2)	N1—C1—H1	119.5
O9—Mo1—O10	77.0 (2)	C2—C1—H1	119.5
O11—Mo1—O10	73.2 (2)	C1—C2—C3	118.8 (14)
O8ⁱ—Mo1—O10	70.90 (17)	C1—C2—H2	120.6
O1—Mo1—Mo4	136.9 (2)	C3—C2—H2	120.6
O2—Mo1—Mo4	83.9 (2)	C2—C3—C4	120.3 (14)
O9—Mo1—Mo4	118.54 (17)	C2—C3—H3	119.9
O11—Mo1—Mo4	34.73 (15)	C4—C3—H3	119.9
O8ⁱ—Mo1—Mo4	77.98 (13)	C3—C4—C5	120.4 (14)
O10—Mo1—Mo4	41.53 (13)	C3—C4—H4	119.8
O1—Mo1—Mo2	133.4 (2)	C5—C4—H4	119.8
O2—Mo1—Mo2	89.1 (2)	N1—C5—C4	117.8 (12)
O9—Mo1—Mo2	32.60 (17)	N1—C5—H5	121.1
O11—Mo1—Mo2	120.61 (16)	C4—C5—H5	121.1
O8ⁱ—Mo1—Mo2	87.06 (14)	N1—C6—C7	112.8 (8)
O10—Mo1—Mo2	47.42 (13)	N1—C6—H6A	109.0
Mo4—Mo1—Mo2	87.65 (3)	C7—C6—H6A	109.0
O3—Mo2—O4	105.1 (3)	N1—C6—H6B	109.0
O3—Mo2—O12ⁱ	101.6 (3)	C7—C6—H6B	109.0
O4—Mo2—O12ⁱ	99.9 (3)	H6A—C6—H6B	107.8
O3—Mo2—O9	100.9 (3)	C8—C7—C6	110.3 (9)
O4—Mo2—O9	98.0 (3)	C8—C7—H7A	109.6
O12ⁱ—Mo2—O9	146.4 (2)	C6—C7—H7A	109.6
O3—Mo2—O13ⁱ	91.2 (2)	C8—C7—H7B	109.6
O4—Mo2—O13ⁱ	163.7 (3)	C6—C7—H7B	109.6
O12ⁱ—Mo2—O13ⁱ	77.5 (2)	H7A—C7—H7B	108.1
O9—Mo2—O13ⁱ	77.4 (2)	C7—C8—C9	113.9 (9)
O3—Mo2—O10	160.7 (2)	C7—C8—H8A	108.8
O4—Mo2—O10	94.2 (2)	C9—C8—H8A	108.8
O12ⁱ—Mo2—O10	75.1 (2)	C7—C8—H8B	108.8
O9—Mo2—O10	75.4 (2)	C9—C8—H8B	108.8
O13ⁱ—Mo2—O10	69.54 (18)	H8A—C8—H8B	107.7
O3—Mo2—Mo1	132.4 (2)	C8—C9—C10	112.0 (9)
O4—Mo2—Mo1	86.9 (2)	C8—C9—H9A	109.2
O12ⁱ—Mo2—Mo1	121.87 (17)	C10—C9—H9A	109.2
O9—Mo2—Mo1	31.49 (17)	C8—C9—H9B	109.2
O13ⁱ—Mo2—Mo1	81.13 (15)	C10—C9—H9B	109.2
O10—Mo2—Mo1	46.81 (13)	H9A—C9—H9B	107.9
O5—Mo3—O6	104.6 (3)	C11—C10—C9	112.1 (10)
O5—Mo3—O12	101.6 (3)	C11—C10—H10A	109.2
O6—Mo3—O12	101.6 (3)	C9—C10—H10A	109.2
O5—Mo3—O8ⁱ	101.9 (3)	C11—C10—H10B	109.2
O6—Mo3—O8ⁱ	96.3 (3)	C9—C10—H10B	109.2
O12—Mo3—O8ⁱ	145.7 (2)	H10A—C10—H10B	107.9
O5—Mo3—O11	89.2 (2)	C10—C11—H11A	109.5
O6—Mo3—O11	163.4 (2)	C10—C11—H11B	109.5
O12—Mo3—O11	84.3 (2)	H11A—C11—H11B	109.5
O8ⁱ—Mo3—O11	71.48 (19)	C10—C11—H11C	109.5
O5—Mo3—O10ⁱ	160.5 (2)	H11A—C11—H11C	109.5
O6—Mo3—O10ⁱ	94.7 (2)	H11B—C11—H11C	109.5
O12—Mo3—O10ⁱ	76.8 (2)	N2—C12—C13	120.1 (9)
O8ⁱ—Mo3—O10ⁱ	72.70 (19)	N2—C12—H12	119.9
O11—Mo3—O10ⁱ	71.27 (18)	C13—C12—H12	119.9
O5—Mo3—Mo4ⁱ	136.5 (2)	C14—C13—C12	119.2 (10)
O6—Mo3—Mo4ⁱ	85.0 (2)	C14—C13—H13	120.4
O12—Mo3—Mo4ⁱ	118.11 (17)	C12—C13—H13	120.4
O8ⁱ—Mo3—Mo4ⁱ	34.68 (15)	C13—C14—C15	119.7 (11)
O11—Mo3—Mo4ⁱ	78.62 (13)	C13—C14—H14	120.2
O10ⁱ—Mo3—Mo4ⁱ	41.35 (13)	C15—C14—H14	120.2
O7—Mo4—O13	105.1 (3)	C16—C15—C14	119.6 (10)
O7—Mo4—O11	102.0 (2)	C16—C15—H15	120.2
O13—Mo4—O11	96.5 (2)	C14—C15—H15	120.2
O7—Mo4—O8	100.1 (2)	N2—C16—C15	120.0 (10)
O13—Mo4—O8	96.5 (2)	N2—C16—H16	120.0
O11—Mo4—O8	150.4 (2)	C15—C16—H16	120.0
O7—Mo4—O10	97.8 (2)	N2—C17—C18	113.2 (8)
O13—Mo4—O10	157.1 (2)	N2—C17—H17A	108.9
O11—Mo4—O10	79.4 (2)	C18—C17—H17A	108.9
O8—Mo4—O10	78.3 (2)	N2—C17—H17B	108.9
O7—Mo4—O10ⁱ	173.7 (2)	C18—C17—H17B	108.9
O13—Mo4—O10ⁱ	81.1 (2)	H17A—C17—H17B	107.8
O11—Mo4—O10ⁱ	78.36 (19)	C17—C18—C19	113.5 (9)
O8—Mo4—O10ⁱ	77.54 (19)	C17—C18—H18A	108.9
O10—Mo4—O10ⁱ	76.0 (2)	C19—C18—H18A	108.9
O7—Mo4—Mo1	90.55 (19)	C17—C18—H18B	108.9
O13—Mo4—Mo1	132.26 (19)	C19—C18—H18B	108.9
O11—Mo4—Mo1	35.74 (16)	H18A—C18—H18B	107.7
O8—Mo4—Mo1	125.31 (16)	C20—C19—C18	115.2 (9)
O10—Mo4—Mo1	47.10 (14)	C20—C19—H19A	108.5
O10ⁱ—Mo4—Mo1	86.19 (13)	C18—C19—H19A	108.5
O7—Mo4—Mo3ⁱ	88.7 (2)	C20—C19—H19B	108.5
O13—Mo4—Mo3ⁱ	131.65 (19)	C18—C19—H19B	108.5
O11—Mo4—Mo3ⁱ	126.12 (16)	H19A—C19—H19B	107.5
O8—Mo4—Mo3ⁱ	35.19 (15)	C19—C20—C21	111.9 (10)
O10—Mo4—Mo3ⁱ	46.69 (14)	C19—C20—H20A	109.2
O10ⁱ—Mo4—Mo3ⁱ	86.06 (13)	C21—C20—H20A	109.2
Mo1—Mo4—Mo3ⁱ	92.62 (3)	C19—C20—H20B	109.2
Mo4—O8—Mo3ⁱ	110.1 (2)	C21—C20—H20B	109.2
Mo4—O8—Mo1ⁱ	111.4 (2)	H20A—C20—H20B	107.9
Mo3ⁱ—O8—Mo1ⁱ	103.8 (2)	C22—C21—C20	111.6 (11)
Mo1—O9—Mo2	115.9 (3)	C22—C21—H21A	109.3
Mo4—O10—Mo4ⁱ	104.0 (2)	C20—C21—H21A	109.3
Mo4—O10—Mo3ⁱ	91.96 (19)	C22—C21—H21B	109.3
Mo4ⁱ—O10—Mo3ⁱ	97.19 (19)	C20—C21—H21B	109.3
Mo4—O10—Mo1	91.4 (2)	H21A—C21—H21B	108.0
Mo4ⁱ—O10—Mo1	97.37 (18)	C21—C22—H22A	109.5
Mo3ⁱ—O10—Mo1	163.8 (2)	C21—C22—H22B	109.5
Mo4—O10—Mo2	162.3 (2)	H22A—C22—H22B	109.5
Mo4ⁱ—O10—Mo2	93.72 (19)	C21—C22—H22C	109.5
Mo3ⁱ—O10—Mo2	86.24 (18)	H22A—C22—H22C	109.5
Mo1—O10—Mo2	85.76 (17)	H22B—C22—H22C	109.5
Mo4—O11—Mo1	109.5 (2)

O1—Mo1—Mo2—O3	−0.1 (4)	O8—Mo4—O10—Mo2	−101.8 (9)
O2—Mo1—Mo2—O3	−110.9 (3)	O10ⁱ—Mo4—O10—Mo2	178.3 (10)
O9—Mo1—Mo2—O3	3.0 (4)	Mo1—Mo4—O10—Mo2	80.4 (8)
O11—Mo1—Mo2—O3	153.7 (3)	Mo3ⁱ—Mo4—O10—Mo2	−83.8 (8)
O8ⁱ—Mo1—Mo2—O3	87.1 (3)	O1—Mo1—O10—Mo4	−96.1 (8)
O10—Mo1—Mo2—O3	153.6 (3)	O2—Mo1—O10—Mo4	76.8 (2)
Mo4—Mo1—Mo2—O3	165.2 (3)	O9—Mo1—O10—Mo4	178.2 (2)
O1—Mo1—Mo2—O4	107.6 (3)	O11—Mo1—O10—Mo4	−17.47 (18)
O2—Mo1—Mo2—O4	−3.2 (3)	O8ⁱ—Mo1—O10—Mo4	−93.4 (2)
O9—Mo1—Mo2—O4	110.7 (4)	Mo2—Mo1—O10—Mo4	162.5 (2)
O11—Mo1—Mo2—O4	−98.6 (3)	O1—Mo1—O10—Mo4ⁱ	8.2 (9)
O8ⁱ—Mo1—Mo2—O4	−165.2 (2)	O2—Mo1—O10—Mo4ⁱ	−178.9 (2)
O10—Mo1—Mo2—O4	−98.7 (3)	O9—Mo1—O10—Mo4ⁱ	−77.5 (2)
Mo4—Mo1—Mo2—O4	−87.1 (2)	O11—Mo1—O10—Mo4ⁱ	86.8 (2)
O1—Mo1—Mo2—O12ⁱ	−152.7 (3)	O8ⁱ—Mo1—O10—Mo4ⁱ	10.94 (18)
O2—Mo1—Mo2—O12ⁱ	96.5 (3)	Mo4—Mo1—O10—Mo4ⁱ	104.3 (2)
O9—Mo1—Mo2—O12ⁱ	−149.6 (4)	Mo2—Mo1—O10—Mo4ⁱ	−93.2 (2)
O11—Mo1—Mo2—O12ⁱ	1.1 (3)	O1—Mo1—O10—Mo3ⁱ	162.0 (9)
O8ⁱ—Mo1—Mo2—O12ⁱ	−65.6 (2)	O2—Mo1—O10—Mo3ⁱ	−25.0 (10)
O10—Mo1—Mo2—O12ⁱ	1.0 (2)	O9—Mo1—O10—Mo3ⁱ	76.4 (10)
Mo4—Mo1—Mo2—O12ⁱ	12.53 (19)	O11—Mo1—O10—Mo3ⁱ	−119.3 (10)
O1—Mo1—Mo2—O9	−3.2 (4)	O8ⁱ—Mo1—O10—Mo3ⁱ	164.8 (10)
O2—Mo1—Mo2—O9	−114.0 (4)	Mo4—Mo1—O10—Mo3ⁱ	−101.9 (10)
O11—Mo1—Mo2—O9	150.7 (3)	Mo2—Mo1—O10—Mo3ⁱ	60.6 (9)
O8ⁱ—Mo1—Mo2—O9	84.0 (3)	O1—Mo1—O10—Mo2	101.4 (8)
O10—Mo1—Mo2—O9	150.6 (3)	O2—Mo1—O10—Mo2	−85.7 (2)
Mo4—Mo1—Mo2—O9	162.1 (3)	O9—Mo1—O10—Mo2	15.75 (18)
O1—Mo1—Mo2—O13ⁱ	−83.5 (3)	O11—Mo1—O10—Mo2	−180.0 (2)
O2—Mo1—Mo2—O13ⁱ	165.7 (2)	O8ⁱ—Mo1—O10—Mo2	104.2 (2)
O9—Mo1—Mo2—O13ⁱ	−80.4 (3)	Mo4—Mo1—O10—Mo2	−162.5 (2)
O11—Mo1—Mo2—O13ⁱ	70.3 (2)	O3—Mo2—O10—Mo4	−177.9 (8)
O8ⁱ—Mo1—Mo2—O13ⁱ	3.65 (19)	O4—Mo2—O10—Mo4	0.6 (9)
O10—Mo1—Mo2—O13ⁱ	70.2 (2)	O12ⁱ—Mo2—O10—Mo4	99.7 (9)
Mo4—Mo1—Mo2—O13ⁱ	81.73 (14)	O9—Mo2—O10—Mo4	−96.6 (9)
O1—Mo1—Mo2—O10	−153.8 (3)	O13ⁱ—Mo2—O10—Mo4	−178.4 (9)
O2—Mo1—Mo2—O10	95.4 (3)	Mo1—Mo2—O10—Mo4	−81.2 (8)
O9—Mo1—Mo2—O10	−150.6 (3)	O3—Mo2—O10—Mo4ⁱ	0.5 (9)
O11—Mo1—Mo2—O10	0.1 (2)	O4—Mo2—O10—Mo4ⁱ	178.9 (2)
O8ⁱ—Mo1—Mo2—O10	−66.6 (2)	O12ⁱ—Mo2—O10—Mo4ⁱ	−82.0 (2)
Mo4—Mo1—Mo2—O10	11.52 (16)	O9—Mo2—O10—Mo4ⁱ	81.8 (2)
O1—Mo1—Mo4—O7	−108.3 (4)	O13ⁱ—Mo2—O10—Mo4ⁱ	−0.02 (17)
O2—Mo1—Mo4—O7	−2.0 (3)	Mo1—Mo2—O10—Mo4ⁱ	97.12 (18)
O9—Mo1—Mo4—O7	98.2 (3)	O3—Mo2—O10—Mo3ⁱ	97.4 (8)
O11—Mo1—Mo4—O7	−110.1 (3)	O4—Mo2—O10—Mo3ⁱ	−84.1 (2)
O8ⁱ—Mo1—Mo4—O7	174.9 (2)	O12ⁱ—Mo2—O10—Mo3ⁱ	14.98 (19)
O10—Mo1—Mo4—O7	100.2 (3)	O9—Mo2—O10—Mo3ⁱ	178.7 (2)
Mo2—Mo1—Mo4—O7	87.4 (2)	O13ⁱ—Mo2—O10—Mo3ⁱ	97.0 (2)
O1—Mo1—Mo4—O13	2.8 (4)	Mo1—Mo2—O10—Mo3ⁱ	−165.9 (2)
O2—Mo1—Mo4—O13	109.1 (3)	O3—Mo2—O10—Mo1	−96.7 (8)
O9—Mo1—Mo4—O13	−150.6 (3)	O4—Mo2—O10—Mo1	81.8 (2)
O11—Mo1—Mo4—O13	1.0 (3)	O12ⁱ—Mo2—O10—Mo1	−179.1 (2)
O8ⁱ—Mo1—Mo4—O13	−74.0 (3)	O9—Mo2—O10—Mo1	−15.36 (18)
O10—Mo1—Mo4—O13	−148.7 (3)	O13ⁱ—Mo2—O10—Mo1	−97.14 (19)
Mo2—Mo1—Mo4—O13	−161.5 (2)	O7—Mo4—O11—Mo1	73.8 (3)
O1—Mo1—Mo4—O11	1.8 (4)	O13—Mo4—O11—Mo1	−179.2 (3)
O2—Mo1—Mo4—O11	108.1 (3)	O8—Mo4—O11—Mo1	−63.7 (5)
O9—Mo1—Mo4—O11	−151.7 (3)	O10—Mo4—O11—Mo1	−22.1 (2)
O8ⁱ—Mo1—Mo4—O11	−75.0 (3)	O10ⁱ—Mo4—O11—Mo1	−99.8 (3)
O10—Mo1—Mo4—O11	−149.7 (3)	Mo3ⁱ—Mo4—O11—Mo1	−23.5 (3)
Mo2—Mo1—Mo4—O11	−162.5 (2)	O7—Mo4—O11—Mo3	−173.5 (3)
O1—Mo1—Mo4—O8	148.9 (3)	O13—Mo4—O11—Mo3	−66.6 (3)
O2—Mo1—Mo4—O8	−104.8 (3)	O8—Mo4—O11—Mo3	48.9 (5)
O9—Mo1—Mo4—O8	−4.5 (3)	O10—Mo4—O11—Mo3	90.6 (2)
O11—Mo1—Mo4—O8	147.1 (3)	O10ⁱ—Mo4—O11—Mo3	12.9 (2)
O8ⁱ—Mo1—Mo4—O8	72.1 (2)	Mo1—Mo4—O11—Mo3	112.7 (3)
O10—Mo1—Mo4—O8	−2.6 (2)	Mo3ⁱ—Mo4—O11—Mo3	89.2 (2)
Mo2—Mo1—Mo4—O8	−15.39 (17)	O1—Mo1—O11—Mo4	−178.8 (3)
O1—Mo1—Mo4—O10	151.5 (4)	O2—Mo1—O11—Mo4	−71.6 (3)
O2—Mo1—Mo4—O10	−102.2 (3)	O9—Mo1—O11—Mo4	48.9 (5)
O9—Mo1—Mo4—O10	−2.0 (3)	O8ⁱ—Mo1—O11—Mo4	95.4 (3)
O11—Mo1—Mo4—O10	149.7 (3)	O10—Mo1—O11—Mo4	20.4 (2)
O8ⁱ—Mo1—Mo4—O10	74.7 (2)	Mo2—Mo1—O11—Mo4	20.4 (3)
Mo2—Mo1—Mo4—O10	−12.82 (18)	O1—Mo1—O11—Mo3	63.5 (3)
O1—Mo1—Mo4—O10ⁱ	77.1 (3)	O2—Mo1—O11—Mo3	170.7 (2)
O2—Mo1—Mo4—O10ⁱ	−176.6 (2)	O9—Mo1—O11—Mo3	−68.8 (5)
O9—Mo1—Mo4—O10ⁱ	−76.4 (2)	O8ⁱ—Mo1—O11—Mo3	−22.35 (18)
O11—Mo1—Mo4—O10ⁱ	75.3 (3)	O10—Mo1—O11—Mo3	−97.3 (2)
O8ⁱ—Mo1—Mo4—O10ⁱ	0.28 (19)	Mo4—Mo1—O11—Mo3	−117.7 (3)
O10—Mo1—Mo4—O10ⁱ	−74.4 (2)	Mo2—Mo1—O11—Mo3	−97.32 (18)
Mo2—Mo1—Mo4—O10ⁱ	−87.21 (14)	O5—Mo3—O11—Mo4	166.5 (3)
O1—Mo1—Mo4—Mo3ⁱ	163.0 (3)	O6—Mo3—O11—Mo4	−46.8 (10)
O2—Mo1—Mo4—Mo3ⁱ	−90.7 (2)	O12—Mo3—O11—Mo4	64.7 (3)
O9—Mo1—Mo4—Mo3ⁱ	9.51 (18)	O8ⁱ—Mo3—O11—Mo4	−90.7 (3)
O11—Mo1—Mo4—Mo3ⁱ	161.2 (2)	O10ⁱ—Mo3—O11—Mo4	−13.2 (2)
O8ⁱ—Mo1—Mo4—Mo3ⁱ	86.15 (14)	Mo4ⁱ—Mo3—O11—Mo4	−55.5 (2)
O10—Mo1—Mo4—Mo3ⁱ	11.47 (18)	O5—Mo3—O11—Mo1	−76.6 (3)
Mo2—Mo1—Mo4—Mo3ⁱ	−1.34 (3)	O6—Mo3—O11—Mo1	70.1 (9)
O7—Mo4—O8—Mo3ⁱ	−73.0 (3)	O12—Mo3—O11—Mo1	−178.4 (3)
O13—Mo4—O8—Mo3ⁱ	−179.7 (3)	O8ⁱ—Mo3—O11—Mo1	26.2 (2)
O11—Mo4—O8—Mo3ⁱ	64.8 (5)	O10ⁱ—Mo3—O11—Mo1	103.7 (2)
O10—Mo4—O8—Mo3ⁱ	23.0 (2)	Mo4ⁱ—Mo3—O11—Mo1	61.42 (18)
O10ⁱ—Mo4—O8—Mo3ⁱ	101.0 (3)	O5—Mo3—O12—Mo2ⁱ	178.7 (3)
Mo1—Mo4—O8—Mo3ⁱ	24.9 (3)	O6—Mo3—O12—Mo2ⁱ	70.9 (3)
O7—Mo4—O8—Mo1ⁱ	172.3 (3)	O8ⁱ—Mo3—O12—Mo2ⁱ	−48.9 (5)
O13—Mo4—O8—Mo1ⁱ	65.7 (3)	O11—Mo3—O12—Mo2ⁱ	−93.3 (3)
O11—Mo4—O8—Mo1ⁱ	−49.8 (5)	O10ⁱ—Mo3—O12—Mo2ⁱ	−21.3 (2)
O10—Mo4—O8—Mo1ⁱ	−91.7 (2)	Mo4ⁱ—Mo3—O12—Mo2ⁱ	−19.5 (3)
O10ⁱ—Mo4—O8—Mo1ⁱ	−13.6 (2)	O7—Mo4—O13—Mo2ⁱ	−178.5 (3)
Mo1—Mo4—O8—Mo1ⁱ	−89.8 (2)	O11—Mo4—O13—Mo2ⁱ	77.1 (3)
Mo3ⁱ—Mo4—O8—Mo1ⁱ	−114.7 (4)	O8—Mo4—O13—Mo2ⁱ	−76.2 (3)
O1—Mo1—O9—Mo2	177.7 (3)	O10—Mo4—O13—Mo2ⁱ	−1.2 (8)
O2—Mo1—O9—Mo2	69.0 (3)	O10ⁱ—Mo4—O13—Mo2ⁱ	0.0 (3)
O11—Mo1—O9—Mo2	−49.7 (5)	Mo1—Mo4—O13—Mo2ⁱ	76.5 (3)
O8ⁱ—Mo1—O9—Mo2	−93.4 (3)	Mo3ⁱ—Mo4—O13—Mo2ⁱ	−76.5 (3)
O10—Mo1—O9—Mo2	−21.8 (2)	C5—N1—C1—C2	−1.2 (17)
Mo4—Mo1—O9—Mo2	−20.4 (3)	C6—N1—C1—C2	175.2 (10)
O3—Mo2—O9—Mo1	−177.7 (3)	N1—C1—C2—C3	1 (2)
O4—Mo2—O9—Mo1	−70.6 (3)	C1—C2—C3—C4	−1 (2)
O12ⁱ—Mo2—O9—Mo1	50.9 (6)	C2—C3—C4—C5	1 (2)
O13ⁱ—Mo2—O9—Mo1	93.5 (3)	C1—N1—C5—C4	1.9 (17)
O10—Mo2—O9—Mo1	21.7 (2)	C6—N1—C5—C4	−174.4 (10)
O7—Mo4—O10—Mo4ⁱ	178.6 (2)	C3—C4—C5—N1	−2 (2)
O13—Mo4—O10—Mo4ⁱ	1.3 (7)	C1—N1—C6—C7	−80.5 (12)
O11—Mo4—O10—Mo4ⁱ	−80.5 (2)	C5—N1—C6—C7	95.9 (11)
O8—Mo4—O10—Mo4ⁱ	79.9 (2)	N1—C6—C7—C8	172.8 (9)
O10ⁱ—Mo4—O10—Mo4ⁱ	0.0	C6—C7—C8—C9	−176.4 (9)
Mo1—Mo4—O10—Mo4ⁱ	−97.9 (2)	C7—C8—C9—C10	−179.9 (9)
Mo3ⁱ—Mo4—O10—Mo4ⁱ	97.9 (2)	C8—C9—C10—C11	179.9 (10)
O7—Mo4—O10—Mo3ⁱ	80.7 (2)	C16—N2—C12—C13	−1.7 (15)
O13—Mo4—O10—Mo3ⁱ	−96.7 (6)	C17—N2—C12—C13	−178.0 (9)
O11—Mo4—O10—Mo3ⁱ	−178.4 (2)	N2—C12—C13—C14	2.3 (16)
O8—Mo4—O10—Mo3ⁱ	−18.00 (17)	C12—C13—C14—C15	−4.0 (17)
O10ⁱ—Mo4—O10—Mo3ⁱ	−97.9 (2)	C13—C14—C15—C16	5.1 (19)
Mo1—Mo4—O10—Mo3ⁱ	164.2 (2)	C12—N2—C16—C15	2.7 (17)
O7—Mo4—O10—Mo1	−83.4 (2)	C17—N2—C16—C15	179.0 (10)
O13—Mo4—O10—Mo1	99.2 (6)	C14—C15—C16—N2	−4.4 (19)
O11—Mo4—O10—Mo1	17.44 (17)	C16—N2—C17—C18	−93.2 (11)
O8—Mo4—O10—Mo1	177.9 (2)	C12—N2—C17—C18	83.2 (10)
O10ⁱ—Mo4—O10—Mo1	97.9 (2)	N2—C17—C18—C19	−170.0 (8)
Mo3ⁱ—Mo4—O10—Mo1	−164.2 (2)	C17—C18—C19—C20	−176.7 (9)
O7—Mo4—O10—Mo2	−3.1 (9)	C18—C19—C20—C21	−179.2 (9)
O13—Mo4—O10—Mo2	179.6 (7)	C19—C20—C21—C22	−173.3 (10)
O11—Mo4—O10—Mo2	97.8 (9)

Symmetry code: (i) −x+1, −y, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C19—H19A···O4ⁱⁱ	0.97	2.60	3.391 (12)	139
C17—H17B···O6ⁱⁱⁱ	0.97	2.30	3.200 (11)	154
C17—H17A···O4	0.97	2.48	3.207 (11)	131
C17—H17A···O2	0.97	2.46	3.166 (10)	130
C16—H16···O5ⁱⁱⁱ	0.93	2.40	3.271 (11)	155
C15—H15···O9^iv	0.93	2.56	3.257 (13)	132
C12—H12···O2	0.93	2.40	3.243 (11)	151
C7—H7B···O3ⁱⁱⁱ	0.97	2.40	3.143 (12)	133
C5—H5···O1^v	0.93	2.39	3.059 (13)	129
C4—H4···O8^vi	0.93	2.56	3.295 (15)	136
C1—H1···O3ⁱⁱⁱ	0.93	2.50	3.295 (13)	144

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

Experimental details

Crystal data
Chemical formula	(C₁₁H₁₈N)₄[Mo₈O₂₆]
M_r	1840.58
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	294
a, b, c (Å)	15.474 (4), 12.051 (3), 16.592 (4)
β (°)	94.964 (5)
V (Å³)	3082.4 (13)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.65
Crystal size (mm)	0.22 × 0.20 × 0.16

Data collection
Diffractometer	Bruker SMART CCD area-detector
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.698, 0.765
No. of measured, independent and observed [I > 2σ(I)] reflections	15694, 5450, 2782
R_int	0.082
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.114, 0.95
No. of reflections	5450
No. of parameters	370
No. of restraints	78
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.63, −0.62

Computer programs: SMART (Bruker 1997), SAINT (Bruker 1997), SAINT, SHELXTL (Bruker, 2001), SHELXTL.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C19—H19A···O4ⁱ	0.97	2.60	3.391 (12)	139.4
C17—H17B···O6ⁱⁱ	0.97	2.30	3.200 (11)	154.1
C17—H17A···O4	0.97	2.48	3.207 (11)	131.4
C17—H17A···O2	0.97	2.46	3.166 (10)	129.7
C16—H16···O5ⁱⁱ	0.93	2.40	3.271 (11)	155.1
C15—H15···O9ⁱⁱⁱ	0.93	2.56	3.257 (13)	131.6
C12—H12···O2	0.93	2.40	3.243 (11)	150.7
C7—H7B···O3ⁱⁱ	0.97	2.40	3.143 (12)	132.6
C5—H5···O1^iv	0.93	2.39	3.059 (13)	129.1
C4—H4···O8^v	0.93	2.56	3.295 (15)	136.0
C1—H1···O3ⁱⁱ	0.93	2.50	3.295 (13)	143.7

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

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