metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

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

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[Aguado, R., Pedrosa, M. R. & Arnáiz, F. J. (2005). Z. Anorg. Allg. Chem. 631, 1995-1999.]).

[Scheme 1]

Experimental

Crystal data
  • (C6H11N2)4[Mo8O26]

  • Mr = 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[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.629, Tmax = 0.663

  • 27619 measured reflections

  • 5677 independent reflections

  • 4568 reflections with I > 2σ(I)

  • Rint = 0.027

Refinement
  • R[F2 > 2σ(F2)] = 0.026

  • wR(F2) = 0.070

  • S = 1.04

  • 5677 reflections

  • 298 parameters

  • H-atom parameters constrained

  • Δρmax = 0.66 e Å−3

  • Δρmin = −0.61 e Å−3

Data collection: SMART (Bruker, 1997[Bruker (1997). SMART. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1999[Bruker (1999). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL-Plus (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


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.

Refinement top

All H-atoms were included in the refinement in a riding model approximation with Uiso=1.2Ueq (C) for aromatic (C—H 0.93 Å) and methylene (C—H 0.97 Å) H-atoms, Uiso = 1.5Ueq (C) for methyl H-atoms (C—H 0.96 Å).

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
[Figure 1] 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
Mr = 1628.19Dx = 2.279 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 27619 reflections
a = 15.6338 (6) Åθ = 2.1–28.3°
b = 16.9231 (6) ŵ = 2.13 mm1
c = 17.9380 (7) ÅT = 296 K
V = 4745.9 (3) Å3Block, colourless
Z = 40.24 × 0.22 × 0.21 mm
Data collection top
Bruker APEX CCD area-detector
diffractometer
5677 independent reflections
Radiation source: fine-focus sealed tube4568 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 0.01 pixels mm-1θmax = 28.3°, θmin = 2.1°
ω scansh = 2014
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 2222
Tmin = 0.629, Tmax = 0.663l = 2023
27619 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.070H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0327P)2 + 3.2572P]
where P = (Fo2 + 2Fc2)/3
5677 reflections(Δ/σ)max = 0.002
298 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 0.61 e Å3
Crystal data top
(C6H11N2)4[Mo8O26]V = 4745.9 (3) Å3
Mr = 1628.19Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 15.6338 (6) ŵ = 2.13 mm1
b = 16.9231 (6) ÅT = 296 K
c = 17.9380 (7) Å0.24 × 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)
Tmin = 0.629, Tmax = 0.663Rint = 0.027
27619 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.070H-atom parameters constrained
S = 1.04Δρmax = 0.66 e Å3
5677 reflectionsΔρmin = 0.61 e Å3
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
xyzUiso*/Ueq
Mo10.919942 (16)0.001136 (16)0.429035 (13)0.03331 (7)
Mo21.078576 (18)0.118127 (18)0.408995 (16)0.04219 (8)
Mo31.048047 (18)0.149211 (16)0.436802 (15)0.03908 (8)
Mo41.212312 (18)0.030332 (19)0.417154 (16)0.04370 (8)
O11.05538 (13)0.01203 (12)0.44123 (11)0.0345 (4)
O20.95510 (13)0.10911 (12)0.43767 (11)0.0385 (5)
O30.93026 (12)0.11030 (12)0.46027 (12)0.0372 (5)
O40.81442 (14)0.01285 (13)0.45821 (12)0.0436 (5)
O50.91133 (15)0.01019 (14)0.33592 (12)0.0490 (6)
O61.19117 (14)0.08062 (14)0.42354 (12)0.0456 (5)
O71.16753 (14)0.13133 (13)0.44644 (13)0.0470 (5)
O81.03691 (16)0.15263 (15)0.34304 (13)0.0546 (6)
O91.04161 (16)0.24423 (14)0.46552 (15)0.0579 (6)
O101.20274 (17)0.04091 (16)0.32313 (14)0.0617 (7)
O111.31854 (16)0.03784 (17)0.43493 (15)0.0641 (7)
O121.06442 (16)0.10397 (17)0.31615 (14)0.0631 (7)
O131.09196 (18)0.21648 (16)0.41944 (16)0.0644 (7)
N11.5874 (2)0.0109 (2)0.35763 (17)0.0562 (8)
N21.2156 (2)0.28339 (19)0.6125 (2)0.0619 (8)
N31.48859 (19)0.09691 (18)0.33891 (15)0.0513 (7)
N41.1552 (2)0.23736 (18)0.71109 (19)0.0599 (8)
C11.5344 (2)0.0403 (2)0.3079 (2)0.0551 (9)
H1A1.52990.02370.25870.066*
C21.5147 (3)0.1051 (3)0.4115 (2)0.0647 (11)
H2A1.49410.14130.44610.078*
C31.4202 (3)0.1411 (3)0.3036 (2)0.0635 (11)
H3A1.41510.12510.25250.095*
H3B1.43300.19660.30580.095*
H3C1.36740.13100.32920.095*
C41.5752 (3)0.0513 (3)0.4230 (2)0.0702 (12)
H4A1.60420.04270.46750.084*
C51.6476 (3)0.0559 (3)0.3444 (2)0.0754 (13)
H5A1.65750.06140.29130.091*
H5B1.70200.04430.36800.091*
C61.1661 (2)0.2273 (2)0.6388 (2)0.0596 (10)
H6A1.14230.18660.61070.072*
C71.1062 (3)0.1867 (2)0.7611 (2)0.0708 (11)
H7A1.07020.21940.79250.085*
H7B1.06930.15280.73180.085*
C81.2360 (3)0.3315 (3)0.6708 (3)0.0759 (13)
H8A1.26980.37660.66810.091*
C91.2417 (3)0.2920 (3)0.5351 (3)0.0872 (15)
H9A1.21830.24940.50620.131*
H9B1.30300.29090.53200.131*
H9C1.22100.34140.51600.131*
C101.1999 (3)0.3033 (3)0.7313 (3)0.0806 (14)
H10A1.20410.32430.77900.097*
C111.6139 (4)0.1312 (3)0.3742 (4)0.115 (2)
H11A1.65390.17290.36400.172*
H11B1.56020.14300.35080.172*
H11C1.60590.12650.42700.172*
C121.1603 (4)0.1381 (4)0.8080 (3)0.118 (2)
H12A1.12520.10540.83920.177*
H12B1.19550.17140.83850.177*
H12C1.19590.10540.77720.177*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.03345 (14)0.03938 (14)0.02710 (13)0.00539 (11)0.00506 (9)0.00023 (10)
Mo20.04347 (17)0.04620 (16)0.03690 (15)0.00116 (13)0.00226 (11)0.00868 (12)
Mo30.04015 (16)0.03777 (14)0.03932 (15)0.00623 (12)0.00155 (11)0.00535 (11)
Mo40.03562 (15)0.05413 (18)0.04136 (16)0.00311 (13)0.00151 (11)0.00798 (13)
O10.0351 (11)0.0394 (11)0.0289 (10)0.0030 (9)0.0017 (8)0.0008 (8)
O20.0416 (12)0.0382 (11)0.0357 (11)0.0072 (9)0.0048 (9)0.0064 (9)
O30.0364 (11)0.0367 (11)0.0385 (12)0.0003 (9)0.0014 (9)0.0001 (9)
O40.0362 (12)0.0553 (13)0.0392 (12)0.0066 (10)0.0057 (9)0.0017 (10)
O50.0548 (14)0.0600 (15)0.0322 (12)0.0031 (11)0.0100 (10)0.0004 (10)
O60.0393 (12)0.0519 (13)0.0456 (13)0.0050 (11)0.0061 (9)0.0019 (10)
O70.0383 (12)0.0488 (13)0.0540 (14)0.0123 (10)0.0017 (10)0.0065 (11)
O80.0538 (15)0.0651 (16)0.0450 (14)0.0102 (12)0.0027 (11)0.0139 (12)
O90.0633 (16)0.0413 (13)0.0689 (17)0.0040 (12)0.0009 (13)0.0003 (12)
O100.0706 (18)0.0699 (17)0.0446 (14)0.0031 (14)0.0051 (12)0.0117 (12)
O110.0398 (14)0.083 (2)0.0689 (17)0.0065 (13)0.0012 (12)0.0155 (14)
O120.0624 (17)0.089 (2)0.0376 (13)0.0027 (14)0.0031 (11)0.0157 (13)
O130.0703 (18)0.0481 (15)0.0748 (19)0.0002 (13)0.0033 (14)0.0174 (13)
N10.0514 (18)0.072 (2)0.0457 (17)0.0034 (15)0.0109 (14)0.0023 (15)
N20.0543 (19)0.0583 (19)0.073 (2)0.0168 (16)0.0121 (16)0.0017 (17)
N30.0540 (18)0.0637 (18)0.0363 (15)0.0049 (15)0.0002 (13)0.0049 (14)
N40.0528 (18)0.0563 (18)0.070 (2)0.0094 (15)0.0104 (16)0.0100 (16)
C10.055 (2)0.072 (2)0.0383 (18)0.0020 (19)0.0073 (16)0.0061 (17)
C20.069 (3)0.085 (3)0.041 (2)0.002 (2)0.0005 (18)0.013 (2)
C30.063 (3)0.078 (3)0.049 (2)0.016 (2)0.0034 (18)0.004 (2)
C40.077 (3)0.098 (4)0.036 (2)0.010 (3)0.0116 (18)0.004 (2)
C50.064 (3)0.097 (3)0.065 (3)0.016 (3)0.024 (2)0.011 (2)
C60.061 (2)0.055 (2)0.064 (2)0.0145 (19)0.0155 (19)0.0003 (19)
C70.063 (3)0.073 (3)0.076 (3)0.004 (2)0.004 (2)0.004 (2)
C80.069 (3)0.058 (2)0.100 (4)0.023 (2)0.006 (3)0.017 (2)
C90.088 (3)0.097 (4)0.077 (3)0.038 (3)0.011 (3)0.015 (3)
C100.076 (3)0.079 (3)0.087 (3)0.017 (2)0.003 (3)0.033 (3)
C110.124 (5)0.087 (4)0.134 (5)0.016 (4)0.007 (4)0.019 (4)
C120.099 (4)0.143 (5)0.112 (5)0.022 (4)0.008 (4)0.047 (4)
Geometric parameters (Å, º) top
Mo1—O51.683 (2)N2—C81.363 (5)
Mo1—O41.747 (2)N2—C91.454 (6)
Mo1—O31.937 (2)N3—C11.319 (5)
Mo1—O21.951 (2)N3—C21.372 (4)
Mo1—O12.137 (2)N3—C31.451 (5)
Mo1—O1i2.370 (2)N4—C61.319 (5)
Mo1—Mo33.2109 (4)N4—C101.366 (5)
Mo1—Mo23.2177 (4)N4—C71.458 (5)
Mo2—O131.688 (3)C1—H1A0.9300
Mo2—O121.697 (3)C2—C41.328 (6)
Mo2—O61.889 (2)C2—H2A0.9300
Mo2—O22.004 (2)C3—H3A0.9600
Mo2—O12.306 (2)C3—H3B0.9600
Mo2—O3i2.353 (2)C3—H3C0.9600
Mo3—O91.692 (2)C4—H4A0.9300
Mo3—O81.692 (2)C5—C111.478 (7)
Mo3—O71.900 (2)C5—H5A0.9700
Mo3—O32.000 (2)C5—H5B0.9700
Mo3—O12.326 (2)C6—H6A0.9300
Mo3—O2i2.352 (2)C7—C121.448 (6)
Mo4—O111.696 (3)C7—H7A0.9700
Mo4—O101.703 (2)C7—H7B0.9700
Mo4—O61.910 (2)C8—C101.313 (6)
Mo4—O71.920 (2)C8—H8A0.9300
Mo4—O4i2.294 (2)C9—H9A0.9600
Mo4—O12.510 (2)C9—H9B0.9600
O1—Mo1i2.370 (2)C9—H9C0.9600
O2—Mo3i2.352 (2)C10—H10A0.9300
O3—Mo2i2.353 (2)C11—H11A0.9600
O4—Mo4i2.294 (2)C11—H11B0.9600
N1—C11.315 (4)C11—H11C0.9600
N1—C41.371 (5)C12—H12A0.9600
N1—C51.490 (5)C12—H12B0.9600
N2—C61.313 (5)C12—H12C0.9600
O5—Mo1—O4103.54 (11)Mo1—O1—Mo292.74 (7)
O5—Mo1—O3101.94 (10)Mo1—O1—Mo391.94 (8)
O4—Mo1—O396.96 (9)Mo2—O1—Mo3162.30 (10)
O5—Mo1—O2100.86 (10)Mo1—O1—Mo1i104.70 (8)
O4—Mo1—O296.47 (10)Mo2—O1—Mo1i97.52 (7)
O3—Mo1—O2149.93 (8)Mo3—O1—Mo1i97.78 (7)
O5—Mo1—O199.96 (10)Mo1—O1—Mo4164.07 (10)
O4—Mo1—O1156.48 (9)Mo2—O1—Mo485.47 (7)
O3—Mo1—O178.79 (8)Mo3—O1—Mo485.36 (6)
O2—Mo1—O178.18 (8)Mo1i—O1—Mo491.23 (7)
O5—Mo1—O1i175.21 (10)Mo1—O2—Mo2108.90 (10)
O4—Mo1—O1i81.19 (8)Mo1—O2—Mo3i110.24 (9)
O3—Mo1—O1i78.00 (8)Mo2—O2—Mo3i104.12 (9)
O2—Mo1—O1i77.66 (8)Mo1—O3—Mo3109.25 (10)
O1—Mo1—O1i75.30 (8)Mo1—O3—Mo2i109.70 (9)
O5—Mo1—Mo391.25 (8)Mo3—O3—Mo2i104.20 (9)
O4—Mo1—Mo3132.98 (7)Mo1—O4—Mo4i118.79 (10)
O3—Mo1—Mo336.03 (6)Mo2—O6—Mo4118.90 (12)
O2—Mo1—Mo3124.55 (6)Mo3—O7—Mo4118.38 (11)
O1—Mo1—Mo346.38 (5)C1—N1—C4107.6 (4)
O1i—Mo1—Mo385.94 (5)C1—N1—C5125.2 (3)
O5—Mo1—Mo290.45 (8)C4—N1—C5127.1 (3)
O4—Mo1—Mo2132.56 (7)C6—N2—C8107.1 (4)
O3—Mo1—Mo2124.49 (6)C6—N2—C9125.5 (3)
O2—Mo1—Mo236.09 (6)C8—N2—C9127.4 (4)
O1—Mo1—Mo245.71 (5)C1—N3—C2108.1 (3)
O1i—Mo1—Mo285.71 (5)C1—N3—C3126.2 (3)
Mo3—Mo1—Mo290.780 (10)C2—N3—C3125.6 (3)
O13—Mo2—O12105.32 (14)C6—N4—C10107.5 (4)
O13—Mo2—O6101.56 (12)C6—N4—C7126.6 (3)
O12—Mo2—O6102.10 (11)C10—N4—C7125.9 (4)
O13—Mo2—O299.56 (11)N1—C1—N3109.4 (3)
O12—Mo2—O296.63 (10)N1—C1—H1A125.3
O6—Mo2—O2146.78 (9)N3—C1—H1A125.3
O13—Mo2—O1159.00 (11)C4—C2—N3106.9 (4)
O12—Mo2—O195.20 (11)C4—C2—H2A126.6
O6—Mo2—O177.94 (9)N3—C2—H2A126.6
O2—Mo2—O173.22 (8)N3—C3—H3A109.5
O13—Mo2—O3i87.26 (11)N3—C3—H3B109.5
O12—Mo2—O3i164.26 (11)H3A—C3—H3B109.5
O6—Mo2—O3i84.15 (8)N3—C3—H3C109.5
O2—Mo2—O3i71.54 (7)H3A—C3—H3C109.5
O1—Mo2—O3i71.77 (7)H3B—C3—H3C109.5
O13—Mo2—Mo1134.56 (10)C2—C4—N1108.0 (3)
O12—Mo2—Mo185.45 (9)C2—C4—H4A126.0
O6—Mo2—Mo1119.47 (7)N1—C4—H4A126.0
O2—Mo2—Mo135.01 (6)C11—C5—N1111.8 (4)
O1—Mo2—Mo141.55 (5)C11—C5—H5A109.3
O3i—Mo2—Mo178.94 (5)N1—C5—H5A109.3
O9—Mo3—O8105.31 (13)C11—C5—H5B109.3
O9—Mo3—O7100.50 (11)N1—C5—H5B109.3
O8—Mo3—O7101.36 (11)H5A—C5—H5B107.9
O9—Mo3—O3101.19 (11)N2—C6—N4109.6 (3)
O8—Mo3—O397.23 (10)N2—C6—H6A125.2
O7—Mo3—O3146.45 (9)N4—C6—H6A125.2
O9—Mo3—O1160.30 (10)C12—C7—N4112.6 (4)
O8—Mo3—O194.20 (10)C12—C7—H7A109.1
O7—Mo3—O177.85 (8)N4—C7—H7A109.1
O3—Mo3—O173.12 (8)C12—C7—H7B109.1
O9—Mo3—O2i88.94 (10)N4—C7—H7B109.1
O8—Mo3—O2i163.60 (10)H7A—C7—H7B107.8
O7—Mo3—O2i83.54 (9)C10—C8—N2108.5 (4)
O3—Mo3—O2i71.60 (8)C10—C8—H8A125.8
O1—Mo3—O2i71.36 (7)N2—C8—H8A125.8
O9—Mo3—Mo1135.89 (9)N2—C9—H9A109.5
O8—Mo3—Mo185.38 (8)N2—C9—H9B109.5
O7—Mo3—Mo1119.53 (7)H9A—C9—H9B109.5
O3—Mo3—Mo134.72 (6)N2—C9—H9C109.5
O1—Mo3—Mo141.69 (5)H9A—C9—H9C109.5
O2i—Mo3—Mo178.66 (5)H9B—C9—H9C109.5
O11—Mo4—O10105.33 (13)C8—C10—N4107.3 (4)
O11—Mo4—O6103.41 (12)C8—C10—H10A126.3
O10—Mo4—O698.49 (11)N4—C10—H10A126.3
O11—Mo4—O7103.82 (12)C5—C11—H11A109.5
O10—Mo4—O798.36 (11)C5—C11—H11B109.5
O6—Mo4—O7142.70 (9)H11A—C11—H11B109.5
O11—Mo4—O4i90.28 (10)C5—C11—H11C109.5
O10—Mo4—O4i164.39 (11)H11A—C11—H11C109.5
O6—Mo4—O4i77.48 (8)H11B—C11—H11C109.5
O7—Mo4—O4i77.39 (9)C7—C12—H12A109.5
O11—Mo4—O1159.07 (10)C7—C12—H12B109.5
O10—Mo4—O195.59 (10)H12A—C12—H12B109.5
O6—Mo4—O172.50 (8)C7—C12—H12C109.5
O7—Mo4—O172.93 (8)H12A—C12—H12C109.5
O4i—Mo4—O168.80 (7)H12B—C12—H12C109.5
Symmetry code: (i) x+2, y, z+1.

Experimental details

Crystal data
Chemical formula(C6H11N2)4[Mo8O26]
Mr1628.19
Crystal system, space groupOrthorhombic, Pbca
Temperature (K)296
a, b, c (Å)15.6338 (6), 16.9231 (6), 17.9380 (7)
V3)4745.9 (3)
Z4
Radiation typeMo Kα
µ (mm1)2.13
Crystal size (mm)0.24 × 0.22 × 0.21
Data collection
DiffractometerBruker APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.629, 0.663
No. of measured, independent and
observed [I > 2σ(I)] reflections
27619, 5677, 4568
Rint0.027
(sin θ/λ)max1)0.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.070, 1.04
No. of reflections5677
No. of parameters298
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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

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

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