Tetra­kis(1-ethyl-3-methyl­imidazolium) β-hexa­cosa­oxidoocta­molybdate

Lin, S.; Chen, W.; Zhang, Z.; Liu, W.; Wang, E.

doi:10.1107/S1600536808015936

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 7| July 2008| Page m954

doi:10.1107/S1600536808015936

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Tetrakis(1-ethyl-3-methylimidazolium) β-hexacosaoxidooctamolybdate

Shiwei Lin,^a,^b Weilin Chen,^a Zhiming Zhang,^a Wenli Liu ^a and Enbo Wang ^a ^*

^aKey Laboratory of Polyoxometalate Science of the Ministry of Education, Department of Chemistry, Northeast Normal University, Changchun, Jilin 130024, People's Republic of China, and ^bDepartment of Chemistry, Changchun Normal University, Changchun, Jilin 130024, People's Republic of China
^*Correspondence e-mail: wangenbo@public.cc.jl.cn

(Received 9 March 2008; accepted 27 May 2008; online 21 June 2008)

The title compound, (C₆H₁₁N₂)₄[Mo₈O₂₆] or (emim)₄[β-Mo₈O₂₆] (emim is 1-ethyl-3-methylimidazolium), was obtained from the ionic liquid [emim]BF₄. The asymmetric unit contains two [emim]⁺ cations and one-half of the [β-Mo₈O₂₆]⁴⁻ tetraanion, which occupies a special position on an inversion centre. The β-[Mo₈O₂₆]⁴⁻ tetraanion features eight distorted MoO₆ coordination octahedra linked together through bridging O atoms.

Related literature

For related literature, see: Aguado et al. (2005 ).

Experimental

Crystal data

(C₆H₁₁N₂)₄[Mo₈O₂₆]
M_r = 1628.19
Orthorhombic, P b c a
a = 15.6338 (6) Å
b = 16.9231 (6) Å
c = 17.9380 (7) Å
V = 4745.9 (3) Å³
Z = 4
Mo Kα radiation
μ = 2.13 mm⁻¹
T = 296 (2) K
0.24 × 0.22 × 0.21 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.629, T_max = 0.663
27619 measured reflections
5677 independent reflections
4568 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.026
wR(F²) = 0.070
S = 1.04
5677 reflections
298 parameters
H-atom parameters constrained
Δρ_max = 0.66 e Å⁻³
Δρ_min = −0.61 e Å⁻³

Data collection: SMART (Bruker, 1997 ); cell refinement: SAINT (Bruker, 1999 ); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808015936/ya2072sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808015936/ya2072Isup2.hkl

checkCIF report

Comment top

The asymmetric unit of the title compound, [emim]₄[β-Mo₈O₂₆] (emim = 1-ethyl-3-methylimidazolium), (1), contains two [emim]⁺ cations and one half of the [β-Mo₈O₂₆]^4- anion, which occupies a special position in the inversion centre (Fig. 1). The anion has eight molybdenum atoms with distorted octahedral coordinations and 26 oxygen atoms which fall into four categories, i.e. terminal, µ₂–, µ₃ - and µ₅-bridging atoms. The geometry of tetra-anion is characterized by a wide range of Mo—O distances varying from 1.683 (2) Å for one of the terminal bonds (Mo1—O5) to 2.510 (2) Å for one of the bonds involving 5-coordinated oxygen atom (Mo4—O1). The geometry of the anion is similar to that observed in previous structures, e.g. Aguado et al. (2005).

Related literature top

For related literature, see: Aguado et al. (2005).

Experimental top

A mixture of sodium molydbate, Na₂MoO₄.2H₂O (0.3 mmol), and ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate, [emim]BF₄ (8 ml) was stirred at 170 °C for 24 h in air. The resulting clear solution was filtered and left at room temperature for 3 days. The colourless block crystals were filtered off, washed with cool distilled water and dried in a desiccator at room temperature.

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL-Plus (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. The cations and anion in the structure of the title compound. Thermal displacement ellipsoids are drawn at 30% probability level; H atoms are shown as small circles of arbitrary radius. The unlabeled atoms are related to their symmetry related counterparts by the (2 - x, -y, 1 - z) transformation.

Tetrakis(1-ethyl-3-methylimidazolium) β-hexacosaoxidooctamolybdate top

Crystal data top

(C₆H₁₁N₂)₄[Mo₈O₂₆]	F(000) = 3152
M_r = 1628.19	D_x = 2.279 Mg m⁻³
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 27619 reflections
a = 15.6338 (6) Å	θ = 2.1–28.3°
b = 16.9231 (6) Å	µ = 2.13 mm⁻¹
c = 17.9380 (7) Å	T = 296 K
V = 4745.9 (3) Å³	Block, colourless
Z = 4	0.24 × 0.22 × 0.21 mm

Data collection top

Bruker APEX CCD area-detector diffractometer	5677 independent reflections
Radiation source: fine-focus sealed tube	4568 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
Detector resolution: 0.01 pixels mm^-1	θ_max = 28.3°, θ_min = 2.1°
ω scans	h = −20→14
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −22→22
T_min = 0.629, T_max = 0.663	l = −20→23
27619 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)] = 0.026	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.070	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0327P)² + 3.2572P] where P = (F_o² + 2F_c²)/3
5677 reflections	(Δ/σ)_max = 0.002
298 parameters	Δρ_max = 0.66 e Å⁻³
0 restraints	Δρ_min = −0.61 e Å⁻³

Crystal data top

(C₆H₁₁N₂)₄[Mo₈O₂₆]	V = 4745.9 (3) Å³
M_r = 1628.19	Z = 4
Orthorhombic, Pbca	Mo Kα radiation
a = 15.6338 (6) Å	µ = 2.13 mm⁻¹
b = 16.9231 (6) Å	T = 296 K
c = 17.9380 (7) Å	0.24 × 0.22 × 0.21 mm

Data collection top

Bruker APEX CCD area-detector diffractometer	5677 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	4568 reflections with I > 2σ(I)
T_min = 0.629, T_max = 0.663	R_int = 0.027
27619 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.026	0 restraints
wR(F²) = 0.070	H-atom parameters constrained
S = 1.04	Δρ_max = 0.66 e Å⁻³
5677 reflections	Δρ_min = −0.61 e Å⁻³
298 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
Mo1	0.919942 (16)	0.001136 (16)	0.429035 (13)	0.03331 (7)
Mo2	1.078576 (18)	−0.118127 (18)	0.408995 (16)	0.04219 (8)
Mo3	1.048047 (18)	0.149211 (16)	0.436802 (15)	0.03908 (8)
Mo4	1.212312 (18)	0.030332 (19)	0.417154 (16)	0.04370 (8)
O1	1.05538 (13)	0.01203 (12)	0.44123 (11)	0.0345 (4)
O2	0.95510 (13)	−0.10911 (12)	0.43767 (11)	0.0385 (5)
O3	0.93026 (12)	0.11030 (12)	0.46027 (12)	0.0372 (5)
O4	0.81442 (14)	−0.01285 (13)	0.45821 (12)	0.0436 (5)
O5	0.91133 (15)	0.01019 (14)	0.33592 (12)	0.0490 (6)
O6	1.19117 (14)	−0.08062 (14)	0.42354 (12)	0.0456 (5)
O7	1.16753 (14)	0.13133 (13)	0.44644 (13)	0.0470 (5)
O8	1.03691 (16)	0.15263 (15)	0.34304 (13)	0.0546 (6)
O9	1.04161 (16)	0.24423 (14)	0.46552 (15)	0.0579 (6)
O10	1.20274 (17)	0.04091 (16)	0.32313 (14)	0.0617 (7)
O11	1.31854 (16)	0.03784 (17)	0.43493 (15)	0.0641 (7)
O12	1.06442 (16)	−0.10397 (17)	0.31615 (14)	0.0631 (7)
O13	1.09196 (18)	−0.21648 (16)	0.41944 (16)	0.0644 (7)
N1	1.5874 (2)	0.0109 (2)	0.35763 (17)	0.0562 (8)
N2	1.2156 (2)	0.28339 (19)	0.6125 (2)	0.0619 (8)
N3	1.48859 (19)	0.09691 (18)	0.33891 (15)	0.0513 (7)
N4	1.1552 (2)	0.23736 (18)	0.71109 (19)	0.0599 (8)
C1	1.5344 (2)	0.0403 (2)	0.3079 (2)	0.0551 (9)
H1A	1.5299	0.0237	0.2587	0.066*
C2	1.5147 (3)	0.1051 (3)	0.4115 (2)	0.0647 (11)
H2A	1.4941	0.1413	0.4461	0.078*
C3	1.4202 (3)	0.1411 (3)	0.3036 (2)	0.0635 (11)
H3A	1.4151	0.1251	0.2525	0.095*
H3B	1.4330	0.1966	0.3058	0.095*
H3C	1.3674	0.1310	0.3292	0.095*
C4	1.5752 (3)	0.0513 (3)	0.4230 (2)	0.0702 (12)
H4A	1.6042	0.0427	0.4675	0.084*
C5	1.6476 (3)	−0.0559 (3)	0.3444 (2)	0.0754 (13)
H5A	1.6575	−0.0614	0.2913	0.091*
H5B	1.7020	−0.0443	0.3680	0.091*
C6	1.1661 (2)	0.2273 (2)	0.6388 (2)	0.0596 (10)
H6A	1.1423	0.1866	0.6107	0.072*
C7	1.1062 (3)	0.1867 (2)	0.7611 (2)	0.0708 (11)
H7A	1.0702	0.2194	0.7925	0.085*
H7B	1.0693	0.1528	0.7318	0.085*
C8	1.2360 (3)	0.3315 (3)	0.6708 (3)	0.0759 (13)
H8A	1.2698	0.3766	0.6681	0.091*
C9	1.2417 (3)	0.2920 (3)	0.5351 (3)	0.0872 (15)
H9A	1.2183	0.2494	0.5062	0.131*
H9B	1.3030	0.2909	0.5320	0.131*
H9C	1.2210	0.3414	0.5160	0.131*
C10	1.1999 (3)	0.3033 (3)	0.7313 (3)	0.0806 (14)
H10A	1.2041	0.3243	0.7790	0.097*
C11	1.6139 (4)	−0.1312 (3)	0.3742 (4)	0.115 (2)
H11A	1.6539	−0.1729	0.3640	0.172*
H11B	1.5602	−0.1430	0.3508	0.172*
H11C	1.6059	−0.1265	0.4270	0.172*
C12	1.1603 (4)	0.1381 (4)	0.8080 (3)	0.118 (2)
H12A	1.1252	0.1054	0.8392	0.177*
H12B	1.1955	0.1714	0.8385	0.177*
H12C	1.1959	0.1054	0.7772	0.177*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.03345 (14)	0.03938 (14)	0.02710 (13)	−0.00539 (11)	−0.00506 (9)	−0.00023 (10)
Mo2	0.04347 (17)	0.04620 (16)	0.03690 (15)	−0.00116 (13)	0.00226 (11)	−0.00868 (12)
Mo3	0.04015 (16)	0.03777 (14)	0.03932 (15)	−0.00623 (12)	−0.00155 (11)	0.00535 (11)
Mo4	0.03562 (15)	0.05413 (18)	0.04136 (16)	−0.00311 (13)	0.00151 (11)	0.00798 (13)
O1	0.0351 (11)	0.0394 (11)	0.0289 (10)	−0.0030 (9)	−0.0017 (8)	0.0008 (8)
O2	0.0416 (12)	0.0382 (11)	0.0357 (11)	−0.0072 (9)	−0.0048 (9)	−0.0064 (9)
O3	0.0364 (11)	0.0367 (11)	0.0385 (12)	0.0003 (9)	−0.0014 (9)	0.0001 (9)
O4	0.0362 (12)	0.0553 (13)	0.0392 (12)	−0.0066 (10)	−0.0057 (9)	0.0017 (10)
O5	0.0548 (14)	0.0600 (15)	0.0322 (12)	−0.0031 (11)	−0.0100 (10)	0.0004 (10)
O6	0.0393 (12)	0.0519 (13)	0.0456 (13)	0.0050 (11)	0.0061 (9)	0.0019 (10)
O7	0.0383 (12)	0.0488 (13)	0.0540 (14)	−0.0123 (10)	−0.0017 (10)	0.0065 (11)
O8	0.0538 (15)	0.0651 (16)	0.0450 (14)	−0.0102 (12)	−0.0027 (11)	0.0139 (12)
O9	0.0633 (16)	0.0413 (13)	0.0689 (17)	−0.0040 (12)	−0.0009 (13)	−0.0003 (12)
O10	0.0706 (18)	0.0699 (17)	0.0446 (14)	0.0031 (14)	0.0051 (12)	0.0117 (12)
O11	0.0398 (14)	0.083 (2)	0.0689 (17)	−0.0065 (13)	0.0012 (12)	0.0155 (14)
O12	0.0624 (17)	0.089 (2)	0.0376 (13)	−0.0027 (14)	0.0031 (11)	−0.0157 (13)
O13	0.0703 (18)	0.0481 (15)	0.0748 (19)	0.0002 (13)	0.0033 (14)	−0.0174 (13)
N1	0.0514 (18)	0.072 (2)	0.0457 (17)	−0.0034 (15)	−0.0109 (14)	−0.0023 (15)
N2	0.0543 (19)	0.0583 (19)	0.073 (2)	−0.0168 (16)	−0.0121 (16)	0.0017 (17)
N3	0.0540 (18)	0.0637 (18)	0.0363 (15)	−0.0049 (15)	0.0002 (13)	−0.0049 (14)
N4	0.0528 (18)	0.0563 (18)	0.070 (2)	−0.0094 (15)	−0.0104 (16)	−0.0100 (16)
C1	0.055 (2)	0.072 (2)	0.0383 (18)	0.0020 (19)	−0.0073 (16)	−0.0061 (17)
C2	0.069 (3)	0.085 (3)	0.041 (2)	−0.002 (2)	0.0005 (18)	−0.013 (2)
C3	0.063 (3)	0.078 (3)	0.049 (2)	0.016 (2)	0.0034 (18)	−0.004 (2)
C4	0.077 (3)	0.098 (4)	0.036 (2)	−0.010 (3)	−0.0116 (18)	−0.004 (2)
C5	0.064 (3)	0.097 (3)	0.065 (3)	0.016 (3)	−0.024 (2)	−0.011 (2)
C6	0.061 (2)	0.055 (2)	0.064 (2)	−0.0145 (19)	−0.0155 (19)	−0.0003 (19)
C7	0.063 (3)	0.073 (3)	0.076 (3)	−0.004 (2)	−0.004 (2)	−0.004 (2)
C8	0.069 (3)	0.058 (2)	0.100 (4)	−0.023 (2)	−0.006 (3)	−0.017 (2)
C9	0.088 (3)	0.097 (4)	0.077 (3)	−0.038 (3)	−0.011 (3)	0.015 (3)
C10	0.076 (3)	0.079 (3)	0.087 (3)	−0.017 (2)	−0.003 (3)	−0.033 (3)
C11	0.124 (5)	0.087 (4)	0.134 (5)	0.016 (4)	−0.007 (4)	0.019 (4)
C12	0.099 (4)	0.143 (5)	0.112 (5)	0.022 (4)	−0.008 (4)	0.047 (4)

Geometric parameters (Å, º) top

Mo1—O5	1.683 (2)	N2—C8	1.363 (5)
Mo1—O4	1.747 (2)	N2—C9	1.454 (6)
Mo1—O3	1.937 (2)	N3—C1	1.319 (5)
Mo1—O2	1.951 (2)	N3—C2	1.372 (4)
Mo1—O1	2.137 (2)	N3—C3	1.451 (5)
Mo1—O1ⁱ	2.370 (2)	N4—C6	1.319 (5)
Mo1—Mo3	3.2109 (4)	N4—C10	1.366 (5)
Mo1—Mo2	3.2177 (4)	N4—C7	1.458 (5)
Mo2—O13	1.688 (3)	C1—H1A	0.9300
Mo2—O12	1.697 (3)	C2—C4	1.328 (6)
Mo2—O6	1.889 (2)	C2—H2A	0.9300
Mo2—O2	2.004 (2)	C3—H3A	0.9600
Mo2—O1	2.306 (2)	C3—H3B	0.9600
Mo2—O3ⁱ	2.353 (2)	C3—H3C	0.9600
Mo3—O9	1.692 (2)	C4—H4A	0.9300
Mo3—O8	1.692 (2)	C5—C11	1.478 (7)
Mo3—O7	1.900 (2)	C5—H5A	0.9700
Mo3—O3	2.000 (2)	C5—H5B	0.9700
Mo3—O1	2.326 (2)	C6—H6A	0.9300
Mo3—O2ⁱ	2.352 (2)	C7—C12	1.448 (6)
Mo4—O11	1.696 (3)	C7—H7A	0.9700
Mo4—O10	1.703 (2)	C7—H7B	0.9700
Mo4—O6	1.910 (2)	C8—C10	1.313 (6)
Mo4—O7	1.920 (2)	C8—H8A	0.9300
Mo4—O4ⁱ	2.294 (2)	C9—H9A	0.9600
Mo4—O1	2.510 (2)	C9—H9B	0.9600
O1—Mo1ⁱ	2.370 (2)	C9—H9C	0.9600
O2—Mo3ⁱ	2.352 (2)	C10—H10A	0.9300
O3—Mo2ⁱ	2.353 (2)	C11—H11A	0.9600
O4—Mo4ⁱ	2.294 (2)	C11—H11B	0.9600
N1—C1	1.315 (4)	C11—H11C	0.9600
N1—C4	1.371 (5)	C12—H12A	0.9600
N1—C5	1.490 (5)	C12—H12B	0.9600
N2—C6	1.313 (5)	C12—H12C	0.9600

O5—Mo1—O4	103.54 (11)	Mo1—O1—Mo2	92.74 (7)
O5—Mo1—O3	101.94 (10)	Mo1—O1—Mo3	91.94 (8)
O4—Mo1—O3	96.96 (9)	Mo2—O1—Mo3	162.30 (10)
O5—Mo1—O2	100.86 (10)	Mo1—O1—Mo1ⁱ	104.70 (8)
O4—Mo1—O2	96.47 (10)	Mo2—O1—Mo1ⁱ	97.52 (7)
O3—Mo1—O2	149.93 (8)	Mo3—O1—Mo1ⁱ	97.78 (7)
O5—Mo1—O1	99.96 (10)	Mo1—O1—Mo4	164.07 (10)
O4—Mo1—O1	156.48 (9)	Mo2—O1—Mo4	85.47 (7)
O3—Mo1—O1	78.79 (8)	Mo3—O1—Mo4	85.36 (6)
O2—Mo1—O1	78.18 (8)	Mo1ⁱ—O1—Mo4	91.23 (7)
O5—Mo1—O1ⁱ	175.21 (10)	Mo1—O2—Mo2	108.90 (10)
O4—Mo1—O1ⁱ	81.19 (8)	Mo1—O2—Mo3ⁱ	110.24 (9)
O3—Mo1—O1ⁱ	78.00 (8)	Mo2—O2—Mo3ⁱ	104.12 (9)
O2—Mo1—O1ⁱ	77.66 (8)	Mo1—O3—Mo3	109.25 (10)
O1—Mo1—O1ⁱ	75.30 (8)	Mo1—O3—Mo2ⁱ	109.70 (9)
O5—Mo1—Mo3	91.25 (8)	Mo3—O3—Mo2ⁱ	104.20 (9)
O4—Mo1—Mo3	132.98 (7)	Mo1—O4—Mo4ⁱ	118.79 (10)
O3—Mo1—Mo3	36.03 (6)	Mo2—O6—Mo4	118.90 (12)
O2—Mo1—Mo3	124.55 (6)	Mo3—O7—Mo4	118.38 (11)
O1—Mo1—Mo3	46.38 (5)	C1—N1—C4	107.6 (4)
O1ⁱ—Mo1—Mo3	85.94 (5)	C1—N1—C5	125.2 (3)
O5—Mo1—Mo2	90.45 (8)	C4—N1—C5	127.1 (3)
O4—Mo1—Mo2	132.56 (7)	C6—N2—C8	107.1 (4)
O3—Mo1—Mo2	124.49 (6)	C6—N2—C9	125.5 (3)
O2—Mo1—Mo2	36.09 (6)	C8—N2—C9	127.4 (4)
O1—Mo1—Mo2	45.71 (5)	C1—N3—C2	108.1 (3)
O1ⁱ—Mo1—Mo2	85.71 (5)	C1—N3—C3	126.2 (3)
Mo3—Mo1—Mo2	90.780 (10)	C2—N3—C3	125.6 (3)
O13—Mo2—O12	105.32 (14)	C6—N4—C10	107.5 (4)
O13—Mo2—O6	101.56 (12)	C6—N4—C7	126.6 (3)
O12—Mo2—O6	102.10 (11)	C10—N4—C7	125.9 (4)
O13—Mo2—O2	99.56 (11)	N1—C1—N3	109.4 (3)
O12—Mo2—O2	96.63 (10)	N1—C1—H1A	125.3
O6—Mo2—O2	146.78 (9)	N3—C1—H1A	125.3
O13—Mo2—O1	159.00 (11)	C4—C2—N3	106.9 (4)
O12—Mo2—O1	95.20 (11)	C4—C2—H2A	126.6
O6—Mo2—O1	77.94 (9)	N3—C2—H2A	126.6
O2—Mo2—O1	73.22 (8)	N3—C3—H3A	109.5
O13—Mo2—O3ⁱ	87.26 (11)	N3—C3—H3B	109.5
O12—Mo2—O3ⁱ	164.26 (11)	H3A—C3—H3B	109.5
O6—Mo2—O3ⁱ	84.15 (8)	N3—C3—H3C	109.5
O2—Mo2—O3ⁱ	71.54 (7)	H3A—C3—H3C	109.5
O1—Mo2—O3ⁱ	71.77 (7)	H3B—C3—H3C	109.5
O13—Mo2—Mo1	134.56 (10)	C2—C4—N1	108.0 (3)
O12—Mo2—Mo1	85.45 (9)	C2—C4—H4A	126.0
O6—Mo2—Mo1	119.47 (7)	N1—C4—H4A	126.0
O2—Mo2—Mo1	35.01 (6)	C11—C5—N1	111.8 (4)
O1—Mo2—Mo1	41.55 (5)	C11—C5—H5A	109.3
O3ⁱ—Mo2—Mo1	78.94 (5)	N1—C5—H5A	109.3
O9—Mo3—O8	105.31 (13)	C11—C5—H5B	109.3
O9—Mo3—O7	100.50 (11)	N1—C5—H5B	109.3
O8—Mo3—O7	101.36 (11)	H5A—C5—H5B	107.9
O9—Mo3—O3	101.19 (11)	N2—C6—N4	109.6 (3)
O8—Mo3—O3	97.23 (10)	N2—C6—H6A	125.2
O7—Mo3—O3	146.45 (9)	N4—C6—H6A	125.2
O9—Mo3—O1	160.30 (10)	C12—C7—N4	112.6 (4)
O8—Mo3—O1	94.20 (10)	C12—C7—H7A	109.1
O7—Mo3—O1	77.85 (8)	N4—C7—H7A	109.1
O3—Mo3—O1	73.12 (8)	C12—C7—H7B	109.1
O9—Mo3—O2ⁱ	88.94 (10)	N4—C7—H7B	109.1
O8—Mo3—O2ⁱ	163.60 (10)	H7A—C7—H7B	107.8
O7—Mo3—O2ⁱ	83.54 (9)	C10—C8—N2	108.5 (4)
O3—Mo3—O2ⁱ	71.60 (8)	C10—C8—H8A	125.8
O1—Mo3—O2ⁱ	71.36 (7)	N2—C8—H8A	125.8
O9—Mo3—Mo1	135.89 (9)	N2—C9—H9A	109.5
O8—Mo3—Mo1	85.38 (8)	N2—C9—H9B	109.5
O7—Mo3—Mo1	119.53 (7)	H9A—C9—H9B	109.5
O3—Mo3—Mo1	34.72 (6)	N2—C9—H9C	109.5
O1—Mo3—Mo1	41.69 (5)	H9A—C9—H9C	109.5
O2ⁱ—Mo3—Mo1	78.66 (5)	H9B—C9—H9C	109.5
O11—Mo4—O10	105.33 (13)	C8—C10—N4	107.3 (4)
O11—Mo4—O6	103.41 (12)	C8—C10—H10A	126.3
O10—Mo4—O6	98.49 (11)	N4—C10—H10A	126.3
O11—Mo4—O7	103.82 (12)	C5—C11—H11A	109.5
O10—Mo4—O7	98.36 (11)	C5—C11—H11B	109.5
O6—Mo4—O7	142.70 (9)	H11A—C11—H11B	109.5
O11—Mo4—O4ⁱ	90.28 (10)	C5—C11—H11C	109.5
O10—Mo4—O4ⁱ	164.39 (11)	H11A—C11—H11C	109.5
O6—Mo4—O4ⁱ	77.48 (8)	H11B—C11—H11C	109.5
O7—Mo4—O4ⁱ	77.39 (9)	C7—C12—H12A	109.5
O11—Mo4—O1	159.07 (10)	C7—C12—H12B	109.5
O10—Mo4—O1	95.59 (10)	H12A—C12—H12B	109.5
O6—Mo4—O1	72.50 (8)	C7—C12—H12C	109.5
O7—Mo4—O1	72.93 (8)	H12A—C12—H12C	109.5
O4ⁱ—Mo4—O1	68.80 (7)	H12B—C12—H12C	109.5

Symmetry code: (i) −x+2, −y, −z+1.

Experimental details

Crystal data
Chemical formula	(C₆H₁₁N₂)₄[Mo₈O₂₆]
M_r	1628.19
Crystal system, space group	Orthorhombic, Pbca
Temperature (K)	296
a, b, c (Å)	15.6338 (6), 16.9231 (6), 17.9380 (7)
V (Å³)	4745.9 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	2.13
Crystal size (mm)	0.24 × 0.22 × 0.21

Data collection
Diffractometer	Bruker APEX CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.629, 0.663
No. of measured, independent and observed [I > 2σ(I)] reflections	27619, 5677, 4568
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.070, 1.04
No. of reflections	5677
No. of parameters	298
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.66, −0.61

Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL-Plus (Sheldrick, 2008).

Acknowledgements

This work was supported by the Postdoctoral Station Foundation of the Ministry of Education of China (No. 20060200002) and the Testing Foundation of Northeast Normal University.

References

Aguado, R., Pedrosa, M. R. & Arnáiz, F. J. (2005). Z. Anorg. Allg. Chem. 631, 1995–1999. Web of Science CSD CrossRef CAS Google Scholar
Bruker (1997). SMART. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (1999). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar