A new β-octa­molybdate(VI) salt based on 1,4-bis­(2-methyl-1H-imidazol-1-yl)butane

Li, S.-L.; Tan, K.

doi:10.1107/S1600536808035022

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 12| December 2008| Page m1487

doi:10.1107/S1600536808035022

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A new β-octamolybdate(VI) salt based on 1,4-bis(2-methyl-1H-imidazol-1-yl)butane

Shun-Li Li ^a ^* and Ke Tan ^b

^aDepartment of Chemistry, Northeast Normal University, Changchun 130024, People's Republic of China, and ^bBiological Scientific and Technical College, Changchun University, Changchun 130022, People's Republic of China
^*Correspondence e-mail: lishunli@yahoo.cn

(Received 12 September 2008; accepted 28 October 2008; online 8 November 2008)

The title compound, bis[2,2′-dimethyl-3,3′-(butane-1,4-diyl)diimidazol-1-ium] β-octamolybdate(VI), (C₁₂H₂₀N₄)₂[Mo₈O₂₆], was produced by hydrothermal reaction of an acidified aqueous solution of Na₂MoO₄ and 1,4-bis(2-methyl-1H-imidazol-1-yl)butane (hereafter L). The structure of the title compound consists of the β-octamolybdate anions having a center of symmetry, and protonated [H₂L]²⁺ cations, which link the β-octamolybdate anions, generating a supramolecular chain via hydrogen bonds.

Related literature

For the applications of polyoxometalates (POMs) chemistry, see: Kozhevnikov (1998 ); Rhule et al. (1998 ); Li et al. (2007 ). For the coordination ability of polyoxometalates with different transition-metal organic units, see: Hagrman et al. (1997 ); Li et al. (2008 ). For the introduction of POMs into coordination polymers for the construction of polymers with desired properties, see: Bu et al. (2001 ); Wu et al. (2002 ).

Experimental

Crystal data

(C₁₂H₂₀N₄)₂[Mo₈O₂₆]
M_r = 1624.16
Triclinic, $[P \overline 1]$
a = 10.5680 (3) Å
b = 11.4890 (5) Å
c = 11.5600 (8) Å
α = 60.7770 (10)°
β = 68.1550 (10)°
γ = 70.4000 (10)°
V = 1116.29 (10) Å³
Z = 1
Mo Kα radiation
μ = 2.27 mm⁻¹
T = 293 (2) K
0.27 × 0.26 × 0.20 mm

Data collection

Bruker APEX CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.49, T_max = 0.63
6962 measured reflections
5123 independent reflections
3776 reflections with I > 2σ(I)
R_int = 0.016

Refinement

R[F² > 2σ(F²)] = 0.032
wR(F²) = 0.079
S = 1.04
5123 reflections
306 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.53 e Å⁻³
Δρ_min = −0.71 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H2N⋯O9ⁱ	0.87 (3)	2.37 (4)	3.031 (5)	134 (4)
N2—H2N⋯O10ⁱ	0.87 (3)	2.20 (2)	3.001 (5)	153 (5)
N4—H4N⋯O12ⁱⁱ	0.86 (3)	2.39 (4)	3.052 (5)	134 (4)
N4—H4N⋯O4ⁱⁱⁱ	0.86 (3)	2.12 (3)	2.873 (4)	146 (5)
Symmetry codes: (i) -x+1, -y+1, -z; (ii) x-1, y-1, z+1; (iii) -x, -y, -z+2.

Data collection: SMART (Bruker, 1999 ); 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 global, I. DOI: 10.1107/S1600536808035022/bg2208sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808035022/bg2208Isup2.hkl

checkCIF report

Comment top

Polyoxometalates (POMs), a unique class of metal-oxide clusters, have many properties that make them attractive for applications in catalysis, biology, magnetism, optics, medicine, etc (Kozhevnikov, 1998; Rhule et al., 1998; Li et al., 2007). In recent times a remarkable approach to the construction of multifunctional materials is being realized exploting the ability of polyoxometalates to coordinate to different transition-metal organic units (Hagrman et al., 1997; Li et al., 2008). The POMs, acting as unusual inorganic ligands are introduced into a variety of POM-based coordination polymers with desired properties (Bu et al., 2001; Wu et al., 2002). During our ongoing studies of related materials, we obtained the title compound, (I), and present its crystal structure here.

The asymmetric unit of compound (I) contains a complete (C₁₂H₂₀N₄²⁺) cation (hereafter [H₂L]²⁺) and half a [Mo₈O₂₆]^4- anion. The complete [Mo₈O₂₆]^4- moiety is generated from the asymmetric unit atoms by a crystallographic inversion center (Fig. 1). It consists of eight edge-sharing MoO₆ octahedra and displays the characteristic β-octamolybdate arrangement. Each protonated [H₂L]²⁺ cation donates two N—H···O hydrogen bonds to two terminal oxygen atoms from one [Mo₈O₂₆]^4- anion and two ones to two bridging oxygen atoms from the other [Mo₈O₂₆]^4- anion. So each [Mo₈O₂₆]^4- anion joins four protonated [H₂L]²⁺ cations (see the hydrogen bonding table for numerical values) to generate a one-dimensional supramolecular double-chain structure (Fig. 2).

Related literature top

For the applications of polyoxometalates (POMs) chemistry, see: Kozhevnikov (1998); Rhule et al. (1998); Li et al. (2007). For the coordination ability of polyoxometalates with different transition-metal organic units, see: Hagrman et al. (1997); Li et al. (2008). For the introduction of POMs into coordination polymers for the construction of polymers with desired properties, see: Bu et al. (2001); Wu et al. (2002).

Experimental top

A mixture of Na₂MoO₄.2H₂O (0.242 g, 1.0 mmol) and L (0.218 g, 1.0 mmol) in water (10 ml) was adjusted with HCl (2M) to pH = 3. Then the mixture was placed in a 23 ml Teflon-lined autoclave and kept under autogenous pressure at 150 °C for 2 days. After the mixture was cooled to room temperature at 10°C.h^-1, colorless crystals of the title compound were obtained.

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SMART (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. A view of the molecule of (I). Displacement ellipsoids are drawn at the 30% probability level. All crystallographic related oxygen atoms are unlabled for clarity. Symmetry code: (i) 1 - x, 1 - y, -z.
	Fig. 2. Ball-stick representation of the one-dimensional supramolecular structure of (I).

bis[2,2'-dimethyl-3,3'-(butane-1,4-diyl)diimidazol-1-ium] β-octamolybdate top

Crystal data top

(C₁₂H₂₀N₄)₂[Mo₈O₂₆]	Z = 1
M_r = 1624.16	F(000) = 784
Triclinic, P1	D_x = 2.416 Mg m⁻³
Hall symbol: -p1	Mo Kα radiation, λ = 0.71069 Å
a = 10.5680 (3) Å	Cell parameters from 879 reflections
b = 11.4890 (5) Å	θ = 2.1–28.3°
c = 11.5600 (8) Å	µ = 2.27 mm⁻¹
α = 60.777 (1)°	T = 293 K
β = 68.155 (1)°	Block, colorless
γ = 70.400 (1)°	0.27 × 0.26 × 0.20 mm
V = 1116.29 (10) Å³

Data collection top

Bruker APEX CCD area-detector diffractometer	5123 independent reflections
Radiation source: fine-focus sealed tube	3776 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.016
ω scans	θ_max = 28.3°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→13
T_min = 0.49, T_max = 0.63	k = −8→15
6962 measured reflections	l = −12→15

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ²(F_o²) + (0.0329P)²] where P = (F_o² + 2F_c²)/3
5123 reflections	(Δ/σ)_max = 0.001
306 parameters	Δρ_max = 0.53 e Å⁻³
2 restraints	Δρ_min = −0.71 e Å⁻³

Crystal data top

(C₁₂H₂₀N₄)₂[Mo₈O₂₆]	γ = 70.400 (1)°
M_r = 1624.16	V = 1116.29 (10) Å³
Triclinic, P1	Z = 1
a = 10.5680 (3) Å	Mo Kα radiation
b = 11.4890 (5) Å	µ = 2.27 mm⁻¹
c = 11.5600 (8) Å	T = 293 K
α = 60.777 (1)°	0.27 × 0.26 × 0.20 mm
β = 68.155 (1)°

Data collection top

Bruker APEX CCD area-detector diffractometer	5123 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3776 reflections with I > 2σ(I)
T_min = 0.49, T_max = 0.63	R_int = 0.016
6962 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.032	2 restraints
wR(F²) = 0.079	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	Δρ_max = 0.53 e Å⁻³
5123 reflections	Δρ_min = −0.71 e Å⁻³
306 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
C1	0.4508 (5)	0.2008 (5)	0.1689 (5)	0.0480 (13)
H1	0.5040	0.1222	0.2199	0.058*
C2	0.4674 (5)	0.2537 (5)	0.0338 (5)	0.0516 (14)
H2	0.5345	0.2198	−0.0273	0.062*
C3	0.2898 (5)	0.3852 (5)	0.1169 (5)	0.0398 (12)
C4	0.1745 (7)	0.4991 (6)	0.1210 (6)	0.078 (2)
H4A	0.0929	0.4647	0.1863	0.117*
H4B	0.1566	0.5524	0.0320	0.117*
H4C	0.1983	0.5547	0.1475	0.117*
C5	0.2836 (5)	0.2607 (5)	0.3649 (4)	0.0455 (13)
H5A	0.2434	0.3477	0.3706	0.055*
H5B	0.3589	0.2175	0.4099	0.055*
C6	0.1756 (5)	0.1742 (5)	0.4387 (4)	0.0357 (11)
H6A	0.2156	0.0864	0.4349	0.043*
H6B	0.1002	0.2167	0.3940	0.043*
C7	0.1188 (5)	0.1543 (5)	0.5889 (5)	0.0454 (13)
H7A	0.1859	0.0893	0.6405	0.055*
H7B	0.1035	0.2398	0.5943	0.055*
C8	−0.0135 (5)	0.1044 (5)	0.6487 (4)	0.0380 (11)
H8A	−0.0808	0.1724	0.5989	0.046*
H8B	0.0018	0.0228	0.6362	0.046*
C9	−0.0909 (5)	0.1582 (4)	0.8570 (5)	0.0333 (10)
H9	−0.0603	0.2401	0.8147	0.040*
C10	−0.1608 (5)	0.1011 (5)	0.9878 (5)	0.0375 (11)
H10	−0.1887	0.1351	1.0536	0.045*
C11	−0.1292 (4)	−0.0326 (4)	0.8885 (4)	0.0305 (10)
C12	−0.1334 (6)	−0.1486 (5)	0.8684 (5)	0.0504 (14)
H12A	−0.2059	−0.1234	0.8248	0.076*
H12B	−0.1511	−0.2244	0.9557	0.076*
H12C	−0.0458	−0.1735	0.8117	0.076*
O1	0.8514 (3)	0.1866 (3)	0.4043 (3)	0.0368 (8)
O2	0.7405 (3)	0.2236 (3)	0.2112 (3)	0.0440 (8)
O3	0.6495 (3)	0.1219 (3)	0.7129 (3)	0.0382 (8)
O4	0.3883 (3)	0.1137 (3)	0.7404 (3)	0.0358 (7)
O5	0.5723 (3)	0.1829 (3)	0.4809 (3)	0.0296 (7)
O6	0.3415 (3)	0.3836 (3)	0.5375 (3)	0.0242 (6)
O7	0.6125 (3)	0.3992 (3)	0.4802 (3)	0.0224 (6)
O8	0.2891 (3)	0.6211 (3)	0.3047 (3)	0.0350 (7)
O9	0.5161 (3)	0.4268 (3)	0.2790 (3)	0.0280 (6)
O10	0.7738 (3)	0.4496 (3)	0.2258 (3)	0.0289 (7)
O11	0.9029 (3)	0.4409 (3)	0.4018 (3)	0.0368 (8)
O12	0.8404 (3)	0.6795 (3)	0.1956 (3)	0.0368 (7)
O13	0.5532 (3)	0.6534 (3)	0.2769 (3)	0.0228 (6)
Mo1	0.71426 (4)	0.27605 (4)	0.33399 (4)	0.02625 (10)
Mo2	0.42574 (3)	0.52592 (3)	0.37192 (3)	0.02135 (9)
Mo3	0.51296 (4)	0.21069 (3)	0.64292 (4)	0.02435 (10)
Mo4	0.77331 (3)	0.54199 (3)	0.32507 (3)	0.02360 (10)
N1	0.3404 (4)	0.2840 (4)	0.2189 (4)	0.0347 (9)
N2	0.3664 (4)	0.3676 (4)	0.0030 (4)	0.0434 (10)
H2N	0.355 (5)	0.420 (4)	−0.079 (2)	0.064*
N3	−0.0723 (3)	0.0740 (3)	0.7959 (3)	0.0266 (8)
N4	−0.1830 (4)	−0.0186 (4)	1.0052 (4)	0.0362 (9)
H4N	−0.220 (5)	−0.079 (4)	1.082 (3)	0.054*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.042 (3)	0.046 (3)	0.040 (3)	−0.004 (2)	−0.010 (2)	−0.009 (2)
C2	0.042 (3)	0.059 (4)	0.039 (3)	−0.003 (3)	0.007 (2)	−0.025 (3)
C3	0.044 (3)	0.037 (3)	0.028 (2)	−0.013 (2)	0.003 (2)	−0.012 (2)
C4	0.091 (5)	0.053 (4)	0.048 (4)	0.012 (3)	−0.003 (3)	−0.018 (3)
C5	0.056 (3)	0.065 (4)	0.022 (2)	−0.035 (3)	−0.003 (2)	−0.013 (2)
C6	0.039 (3)	0.045 (3)	0.024 (2)	−0.016 (2)	0.002 (2)	−0.016 (2)
C7	0.047 (3)	0.063 (4)	0.028 (3)	−0.028 (3)	0.004 (2)	−0.018 (2)
C8	0.043 (3)	0.050 (3)	0.023 (2)	−0.020 (2)	0.000 (2)	−0.017 (2)
C9	0.036 (3)	0.028 (2)	0.034 (3)	−0.0015 (19)	−0.010 (2)	−0.013 (2)
C10	0.038 (3)	0.048 (3)	0.030 (3)	−0.001 (2)	−0.008 (2)	−0.024 (2)
C11	0.029 (2)	0.035 (3)	0.027 (2)	−0.0091 (19)	−0.0080 (19)	−0.011 (2)
C12	0.064 (4)	0.051 (3)	0.043 (3)	−0.025 (3)	−0.012 (3)	−0.017 (3)
O1	0.0320 (17)	0.0321 (18)	0.0421 (19)	0.0006 (14)	−0.0092 (15)	−0.0167 (15)
O2	0.054 (2)	0.050 (2)	0.0372 (19)	−0.0100 (17)	−0.0053 (16)	−0.0287 (17)
O3	0.0367 (18)	0.0301 (17)	0.0383 (18)	0.0010 (14)	−0.0130 (15)	−0.0093 (14)
O4	0.0330 (17)	0.0286 (17)	0.0356 (18)	−0.0082 (13)	−0.0006 (14)	−0.0100 (14)
O5	0.0331 (16)	0.0244 (15)	0.0319 (16)	−0.0076 (13)	−0.0042 (13)	−0.0139 (13)
O6	0.0260 (15)	0.0217 (14)	0.0251 (15)	−0.0066 (12)	−0.0046 (12)	−0.0100 (12)
O7	0.0222 (14)	0.0224 (14)	0.0195 (14)	−0.0035 (11)	−0.0025 (11)	−0.0087 (12)
O8	0.0335 (17)	0.0356 (18)	0.0318 (17)	−0.0043 (14)	−0.0144 (14)	−0.0081 (14)
O9	0.0282 (16)	0.0340 (17)	0.0226 (15)	−0.0049 (13)	−0.0037 (12)	−0.0149 (13)
O10	0.0288 (16)	0.0342 (17)	0.0223 (15)	−0.0055 (13)	0.0011 (12)	−0.0164 (13)
O11	0.0273 (16)	0.0384 (19)	0.0373 (18)	−0.0035 (14)	−0.0056 (14)	−0.0139 (15)
O12	0.0338 (17)	0.0374 (18)	0.0343 (18)	−0.0156 (14)	−0.0015 (14)	−0.0109 (14)
O13	0.0231 (14)	0.0254 (15)	0.0178 (14)	−0.0056 (12)	−0.0043 (11)	−0.0074 (12)
Mo1	0.0270 (2)	0.0275 (2)	0.02393 (19)	−0.00334 (15)	−0.00188 (15)	−0.01489 (16)
Mo2	0.02117 (18)	0.02459 (19)	0.01723 (18)	−0.00511 (14)	−0.00434 (13)	−0.00779 (14)
Mo3	0.02464 (19)	0.02039 (19)	0.02227 (19)	−0.00412 (14)	−0.00317 (15)	−0.00671 (15)
Mo4	0.01997 (18)	0.0257 (2)	0.02189 (19)	−0.00583 (14)	−0.00081 (14)	−0.00971 (15)
N1	0.041 (2)	0.040 (2)	0.025 (2)	−0.0187 (18)	−0.0054 (17)	−0.0099 (17)
N2	0.047 (2)	0.041 (3)	0.022 (2)	−0.008 (2)	0.0007 (19)	−0.0061 (18)
N3	0.0265 (18)	0.033 (2)	0.0194 (17)	−0.0074 (15)	−0.0018 (14)	−0.0118 (15)
N4	0.035 (2)	0.046 (3)	0.0212 (19)	−0.0169 (19)	0.0011 (17)	−0.0095 (18)

Geometric parameters (Å, º) top

C1—C2	1.334 (7)	C11—C12	1.477 (6)
C1—N1	1.378 (6)	C12—H12A	0.9600
C1—H1	0.9300	C12—H12B	0.9600
C2—N2	1.367 (6)	C12—H12C	0.9600
C2—H2	0.9300	O1—Mo1	1.697 (3)
C3—N1	1.319 (6)	O2—Mo1	1.699 (3)
C3—N2	1.337 (6)	O3—Mo3	1.688 (3)
C3—C4	1.465 (7)	O4—Mo3	1.703 (3)
C4—H4A	0.9600	O5—Mo3	1.892 (3)
C4—H4B	0.9600	O5—Mo1	1.920 (3)
C4—H4C	0.9600	O6—Mo2	1.945 (3)
C5—N1	1.481 (5)	O6—Mo3	2.362 (3)
C5—C6	1.492 (6)	O7—Mo3	2.327 (2)
C5—H5A	0.9700	O7—Mo4	2.350 (3)
C5—H5B	0.9700	O7—Mo2	2.390 (3)
C6—C7	1.535 (6)	O7—Mo1	2.444 (3)
C6—H6A	0.9700	O8—Mo2	1.682 (3)
C6—H6B	0.9700	O9—Mo2	1.750 (3)
C7—C8	1.480 (6)	O9—Mo1	2.296 (3)
C7—H7A	0.9700	O10—Mo4	1.904 (3)
C7—H7B	0.9700	O10—Mo1	1.938 (3)
C8—N3	1.478 (5)	O11—Mo4	1.686 (3)
C8—H8A	0.9700	O12—Mo4	1.700 (3)
C8—H8B	0.9700	O13—Mo2	1.954 (3)
C9—C10	1.337 (6)	O13—Mo4	2.373 (3)
C9—N3	1.382 (5)	Mo2—Mo4ⁱ	3.2019 (5)
C9—H9	0.9300	Mo2—Mo3ⁱ	3.2144 (5)
C10—N4	1.377 (6)	Mo4—O6ⁱ	1.981 (3)
C10—H10	0.9300	N2—H2N	0.87 (3)
C11—N3	1.320 (5)	N4—H4N	0.86 (3)
C11—N4	1.322 (5)

C2—C1—N1	107.4 (4)	O5—Mo1—O7	73.80 (10)
C2—C1—H1	126.3	O10—Mo1—O7	74.23 (10)
N1—C1—H1	126.3	O9—Mo1—O7	69.81 (9)
C1—C2—N2	106.5 (4)	O8—Mo2—O9	104.33 (14)
C1—C2—H2	126.8	O8—Mo2—O6	101.53 (13)
N2—C2—H2	126.8	O9—Mo2—O6	96.72 (12)
N1—C3—N2	106.9 (4)	O8—Mo2—O13	101.33 (13)
N1—C3—C4	128.6 (5)	O9—Mo2—O13	95.61 (12)
N2—C3—C4	124.6 (5)	O6—Mo2—O13	150.39 (11)
C3—C4—H4A	109.5	O8—Mo2—O7ⁱ	99.39 (13)
C3—C4—H4B	109.5	O9—Mo2—O7ⁱ	156.26 (12)
H4A—C4—H4B	109.5	O6—Mo2—O7ⁱ	79.18 (10)
C3—C4—H4C	109.5	O13—Mo2—O7ⁱ	78.73 (10)
H4A—C4—H4C	109.5	O8—Mo2—O7	175.33 (12)
H4B—C4—H4C	109.5	O9—Mo2—O7	80.34 (11)
N1—C5—C6	112.8 (4)	O6—Mo2—O7	77.54 (10)
N1—C5—H5A	109.0	O13—Mo2—O7	78.15 (10)
C6—C5—H5A	109.0	O7ⁱ—Mo2—O7	75.94 (10)
N1—C5—H5B	109.0	O8—Mo2—Mo4ⁱ	90.41 (10)
C6—C5—H5B	109.0	O9—Mo2—Mo4ⁱ	132.43 (9)
H5A—C5—H5B	107.8	O6—Mo2—Mo4ⁱ	35.72 (8)
C5—C6—C7	110.9 (4)	O13—Mo2—Mo4ⁱ	125.92 (8)
C5—C6—H6A	109.5	O7ⁱ—Mo2—Mo4ⁱ	47.21 (7)
C7—C6—H6A	109.5	O7—Mo2—Mo4ⁱ	86.22 (6)
C5—C6—H6B	109.5	O8—Mo2—Mo3ⁱ	90.58 (10)
C7—C6—H6B	109.5	O9—Mo2—Mo3ⁱ	131.56 (9)
H6A—C6—H6B	108.1	O6—Mo2—Mo3ⁱ	125.49 (8)
C8—C7—C6	109.9 (4)	O13—Mo2—Mo3ⁱ	35.96 (8)
C8—C7—H7A	109.7	O7ⁱ—Mo2—Mo3ⁱ	46.33 (7)
C6—C7—H7A	109.7	O7—Mo2—Mo3ⁱ	86.33 (6)
C8—C7—H7B	109.7	Mo4ⁱ—Mo2—Mo3ⁱ	92.286 (13)
C6—C7—H7B	109.7	O3—Mo3—O4	104.79 (15)
H7A—C7—H7B	108.2	O3—Mo3—O5	101.97 (14)
N3—C8—C7	114.0 (4)	O4—Mo3—O5	101.64 (14)
N3—C8—H8A	108.8	O3—Mo3—O13ⁱ	97.07 (13)
C7—C8—H8A	108.8	O4—Mo3—O13ⁱ	100.09 (13)
N3—C8—H8B	108.8	O5—Mo3—O13ⁱ	146.22 (11)
C7—C8—H8B	108.8	O3—Mo3—O7	96.22 (12)
H8A—C8—H8B	107.6	O4—Mo3—O7	158.65 (12)
C10—C9—N3	107.8 (4)	O5—Mo3—O7	77.19 (10)
C10—C9—H9	126.1	O13ⁱ—Mo3—O7	73.19 (10)
N3—C9—H9	126.1	O3—Mo3—O6	165.01 (12)
C9—C10—N4	106.0 (4)	O4—Mo3—O6	87.24 (12)
C9—C10—H10	127.0	O5—Mo3—O6	83.90 (11)
N4—C10—H10	127.0	O13ⁱ—Mo3—O6	71.63 (10)
N3—C11—N4	108.0 (4)	O7—Mo3—O6	71.41 (9)
N3—C11—C12	127.0 (4)	O3—Mo3—Mo2ⁱ	86.46 (11)
N4—C11—C12	125.0 (4)	O4—Mo3—Mo2ⁱ	135.19 (10)
C11—C12—H12A	109.5	O5—Mo3—Mo2ⁱ	118.52 (8)
C11—C12—H12B	109.5	O13ⁱ—Mo3—Mo2ⁱ	35.10 (7)
H12A—C12—H12B	109.5	O7—Mo3—Mo2ⁱ	41.34 (6)
C11—C12—H12C	109.5	O6—Mo3—Mo2ⁱ	78.65 (6)
H12A—C12—H12C	109.5	O11—Mo4—O12	104.90 (15)
H12B—C12—H12C	109.5	O11—Mo4—O10	101.89 (14)
Mo3—O5—Mo1	117.70 (14)	O12—Mo4—O10	101.07 (14)
Mo2—O6—Mo4ⁱ	109.31 (12)	O11—Mo4—O6ⁱ	98.62 (13)
Mo2—O6—Mo3	110.72 (12)	O12—Mo4—O6ⁱ	100.79 (13)
Mo4ⁱ—O6—Mo3	104.16 (11)	O10—Mo4—O6ⁱ	144.88 (11)
Mo2ⁱ—O7—Mo3	92.33 (9)	O11—Mo4—O7	94.31 (12)
Mo2ⁱ—O7—Mo4	91.22 (10)	O12—Mo4—O7	160.60 (12)
Mo3—O7—Mo4	163.12 (12)	O10—Mo4—O7	77.14 (10)
Mo2ⁱ—O7—Mo2	104.06 (10)	O6ⁱ—Mo4—O7	73.14 (10)
Mo3—O7—Mo2	97.67 (9)	O11—Mo4—O13	164.42 (12)
Mo4—O7—Mo2	97.46 (9)	O12—Mo4—O13	89.13 (12)
Mo2ⁱ—O7—Mo1	163.93 (13)	O10—Mo4—O13	81.58 (11)
Mo3—O7—Mo1	86.24 (8)	O6ⁱ—Mo4—O13	71.62 (10)
Mo4—O7—Mo1	85.80 (8)	O7—Mo4—O13	71.48 (9)
Mo2—O7—Mo1	91.98 (9)	O11—Mo4—Mo2ⁱ	86.16 (10)
Mo2—O9—Mo1	117.87 (14)	O12—Mo4—Mo2ⁱ	135.73 (11)
Mo4—O10—Mo1	116.36 (13)	O10—Mo4—Mo2ⁱ	118.71 (8)
Mo2—O13—Mo3ⁱ	108.94 (12)	O6ⁱ—Mo4—Mo2ⁱ	34.97 (7)
Mo2—O13—Mo4	110.49 (11)	O7—Mo4—Mo2ⁱ	41.57 (6)
Mo3ⁱ—O13—Mo4	103.28 (11)	O13—Mo4—Mo2ⁱ	78.96 (6)
O1—Mo1—O2	104.71 (15)	C3—N1—C1	109.3 (4)
O1—Mo1—O5	99.04 (13)	C3—N1—C5	125.2 (4)
O2—Mo1—O5	103.61 (14)	C1—N1—C5	125.4 (4)
O1—Mo1—O10	98.14 (13)	C3—N2—C2	109.9 (4)
O2—Mo1—O10	101.72 (14)	C3—N2—H2N	126 (3)
O5—Mo1—O10	144.48 (11)	C2—N2—H2N	125 (3)
O1—Mo1—O9	163.59 (12)	C11—N3—C9	108.5 (4)
O2—Mo1—O9	91.61 (13)	C11—N3—C8	125.1 (4)
O5—Mo1—O9	78.38 (11)	C9—N3—C8	126.1 (4)
O10—Mo1—O9	76.43 (11)	C11—N4—C10	109.8 (4)
O1—Mo1—O7	93.85 (12)	C11—N4—H4N	125 (4)
O2—Mo1—O7	161.41 (13)	C10—N4—H4N	125 (4)

N1—C1—C2—N2	−0.6 (6)	Mo1—O5—Mo3—O6	93.10 (15)
N1—C5—C6—C7	−179.3 (4)	Mo1—O5—Mo3—Mo2ⁱ	19.56 (18)
C5—C6—C7—C8	163.4 (4)	Mo2ⁱ—O7—Mo3—O3	−77.41 (13)
C6—C7—C8—N3	176.4 (4)	Mo4—O7—Mo3—O3	24.5 (5)
N3—C9—C10—N4	0.5 (5)	Mo2—O7—Mo3—O3	178.06 (13)
Mo3—O5—Mo1—O1	71.31 (18)	Mo1—O7—Mo3—O3	86.56 (12)
Mo3—O5—Mo1—O2	178.95 (16)	Mo2ⁱ—O7—Mo3—O4	92.4 (3)
Mo3—O5—Mo1—O10	−46.7 (3)	Mo4—O7—Mo3—O4	−165.6 (4)
Mo3—O5—Mo1—O9	−92.21 (16)	Mo2—O7—Mo3—O4	−12.1 (4)
Mo3—O5—Mo1—O7	−20.10 (14)	Mo1—O7—Mo3—O4	−103.6 (3)
Mo4—O10—Mo1—O1	−69.16 (17)	Mo2ⁱ—O7—Mo3—O5	−178.32 (12)
Mo4—O10—Mo1—O2	−176.11 (16)	Mo4—O7—Mo3—O5	−76.4 (4)
Mo4—O10—Mo1—O5	49.1 (3)	Mo2—O7—Mo3—O5	77.15 (11)
Mo4—O10—Mo1—O9	95.07 (15)	Mo1—O7—Mo3—O5	−14.35 (10)
Mo4—O10—Mo1—O7	22.57 (13)	Mo2ⁱ—O7—Mo3—O13ⁱ	18.11 (10)
Mo2—O9—Mo1—O1	−5.8 (5)	Mo4—O7—Mo3—O13ⁱ	120.1 (4)
Mo2—O9—Mo1—O2	−179.75 (17)	Mo2—O7—Mo3—O13ⁱ	−86.41 (10)
Mo2—O9—Mo1—O5	76.68 (16)	Mo1—O7—Mo3—O13ⁱ	−177.91 (10)
Mo2—O9—Mo1—O10	−78.08 (16)	Mo2ⁱ—O7—Mo3—O6	93.89 (10)
Mo2—O9—Mo1—O7	−0.15 (13)	Mo4—O7—Mo3—O6	−164.2 (5)
Mo2ⁱ—O7—Mo1—O1	1.4 (5)	Mo2—O7—Mo3—O6	−10.64 (8)
Mo3—O7—Mo1—O1	−83.95 (12)	Mo1—O7—Mo3—O6	−102.14 (10)
Mo4—O7—Mo1—O1	81.15 (12)	Mo4—O7—Mo3—Mo2ⁱ	102.0 (5)
Mo2—O7—Mo1—O1	178.50 (11)	Mo2—O7—Mo3—Mo2ⁱ	−104.53 (11)
Mo2ⁱ—O7—Mo1—O2	−175.8 (4)	Mo1—O7—Mo3—Mo2ⁱ	163.97 (13)
Mo3—O7—Mo1—O2	98.9 (4)	Mo2—O6—Mo3—O3	49.4 (5)
Mo4—O7—Mo1—O2	−96.0 (4)	Mo4ⁱ—O6—Mo3—O3	−68.0 (5)
Mo2—O7—Mo1—O2	1.3 (4)	Mo2—O6—Mo3—O4	−166.62 (16)
Mo2ⁱ—O7—Mo1—O5	99.7 (5)	Mo4ⁱ—O6—Mo3—O4	75.99 (14)
Mo3—O7—Mo1—O5	14.36 (10)	Mo2—O6—Mo3—O5	−64.60 (14)
Mo4—O7—Mo1—O5	179.46 (11)	Mo4ⁱ—O6—Mo3—O5	178.01 (13)
Mo2—O7—Mo1—O5	−83.20 (11)	Mo2—O6—Mo3—O13ⁱ	91.79 (13)
Mo2ⁱ—O7—Mo1—O10	−96.0 (5)	Mo4ⁱ—O6—Mo3—O13ⁱ	−25.60 (11)
Mo3—O7—Mo1—O10	178.68 (11)	Mo2—O6—Mo3—O7	13.91 (11)
Mo4—O7—Mo1—O10	−16.22 (10)	Mo4ⁱ—O6—Mo3—O7	−103.48 (12)
Mo2—O7—Mo1—O10	81.12 (11)	Mo2—O6—Mo3—Mo2ⁱ	56.15 (10)
Mo2ⁱ—O7—Mo1—O9	−177.0 (5)	Mo4ⁱ—O6—Mo3—Mo2ⁱ	−61.24 (9)
Mo3—O7—Mo1—O9	97.65 (10)	Mo1—O10—Mo4—O11	68.55 (18)
Mo4—O7—Mo1—O9	−97.25 (10)	Mo1—O10—Mo4—O12	176.55 (15)
Mo2—O7—Mo1—O9	0.09 (8)	Mo1—O10—Mo4—O6ⁱ	−55.9 (3)
Mo1—O9—Mo2—O8	−179.70 (14)	Mo1—O10—Mo4—O7	−23.21 (14)
Mo1—O9—Mo2—O6	−75.94 (15)	Mo1—O10—Mo4—O13	−96.01 (15)
Mo1—O9—Mo2—O13	77.08 (15)	Mo1—O10—Mo4—Mo2ⁱ	−23.58 (18)
Mo1—O9—Mo2—O7ⁱ	2.4 (4)	Mo2ⁱ—O7—Mo4—O11	79.27 (13)
Mo1—O9—Mo2—O7	0.14 (12)	Mo3—O7—Mo4—O11	−22.9 (4)
Mo1—O9—Mo2—Mo4ⁱ	−75.60 (17)	Mo2—O7—Mo4—O11	−176.38 (13)
Mo1—O9—Mo2—Mo3ⁱ	76.39 (16)	Mo1—O7—Mo4—O11	−84.92 (12)
Mo4ⁱ—O6—Mo2—O8	−74.26 (16)	Mo2ⁱ—O7—Mo4—O12	−92.7 (4)
Mo3—O6—Mo2—O8	171.55 (14)	Mo3—O7—Mo4—O12	165.2 (4)
Mo4ⁱ—O6—Mo2—O9	179.57 (13)	Mo2—O7—Mo4—O12	11.7 (4)
Mo3—O6—Mo2—O9	65.39 (14)	Mo1—O7—Mo4—O12	103.1 (4)
Mo4ⁱ—O6—Mo2—O13	65.6 (3)	Mo2ⁱ—O7—Mo4—O10	−179.50 (12)
Mo3—O6—Mo2—O13	−48.6 (3)	Mo3—O7—Mo4—O10	78.4 (4)
Mo4ⁱ—O6—Mo2—O7ⁱ	23.24 (12)	Mo2—O7—Mo4—O10	−75.15 (11)
Mo3—O6—Mo2—O7ⁱ	−90.94 (12)	Mo1—O7—Mo4—O10	16.30 (10)
Mo4ⁱ—O6—Mo2—O7	101.06 (13)	Mo2ⁱ—O7—Mo4—O6ⁱ	−18.44 (10)
Mo3—O6—Mo2—O7	−13.13 (10)	Mo3—O7—Mo4—O6ⁱ	−120.6 (4)
Mo3—O6—Mo2—Mo4ⁱ	−114.19 (18)	Mo2—O7—Mo4—O6ⁱ	85.91 (11)
Mo4ⁱ—O6—Mo2—Mo3ⁱ	24.83 (16)	Mo1—O7—Mo4—O6ⁱ	177.37 (11)
Mo3—O6—Mo2—Mo3ⁱ	−89.36 (11)	Mo2ⁱ—O7—Mo4—O13	−94.20 (10)
Mo3ⁱ—O13—Mo2—O8	75.02 (15)	Mo3—O7—Mo4—O13	163.7 (5)
Mo4—O13—Mo2—O8	−172.19 (13)	Mo2—O7—Mo4—O13	10.15 (8)
Mo3ⁱ—O13—Mo2—O9	−179.12 (13)	Mo1—O7—Mo4—O13	101.60 (9)
Mo4—O13—Mo2—O9	−66.32 (14)	Mo3—O7—Mo4—Mo2ⁱ	−102.1 (5)
Mo3ⁱ—O13—Mo2—O6	−64.9 (3)	Mo2—O7—Mo4—Mo2ⁱ	104.35 (11)
Mo4—O13—Mo2—O6	47.9 (3)	Mo1—O7—Mo4—Mo2ⁱ	−164.19 (12)
Mo3ⁱ—O13—Mo2—O7ⁱ	−22.44 (12)	Mo2—O13—Mo4—O11	−38.2 (5)
Mo4—O13—Mo2—O7ⁱ	90.36 (12)	Mo3ⁱ—O13—Mo4—O11	78.2 (5)
Mo3ⁱ—O13—Mo2—O7	−100.24 (12)	Mo2—O13—Mo4—O12	167.31 (15)
Mo4—O13—Mo2—O7	12.55 (10)	Mo3ⁱ—O13—Mo4—O12	−76.32 (14)
Mo3ⁱ—O13—Mo2—Mo4ⁱ	−23.85 (15)	Mo2—O13—Mo4—O10	65.99 (13)
Mo4—O13—Mo2—Mo4ⁱ	88.95 (11)	Mo3ⁱ—O13—Mo4—O10	−177.64 (12)
Mo4—O13—Mo2—Mo3ⁱ	112.80 (16)	Mo2—O13—Mo4—O6ⁱ	−91.00 (13)
Mo2ⁱ—O7—Mo2—O9	179.05 (13)	Mo3ⁱ—O13—Mo4—O6ⁱ	25.37 (11)
Mo3—O7—Mo2—O9	−86.59 (12)	Mo2—O13—Mo4—O7	−13.19 (11)
Mo4—O7—Mo2—O9	85.91 (12)	Mo3ⁱ—O13—Mo4—O7	103.18 (11)
Mo1—O7—Mo2—O9	−0.12 (10)	Mo2—O13—Mo4—Mo2ⁱ	−55.58 (10)
Mo2ⁱ—O7—Mo2—O6	−81.79 (12)	Mo3ⁱ—O13—Mo4—Mo2ⁱ	60.79 (8)
Mo3—O7—Mo2—O6	12.57 (10)	N2—C3—N1—C1	0.0 (6)
Mo4—O7—Mo2—O6	−174.94 (12)	C4—C3—N1—C1	−178.8 (6)
Mo1—O7—Mo2—O6	99.04 (10)	N2—C3—N1—C5	−177.8 (4)
Mo2ⁱ—O7—Mo2—O13	81.18 (12)	C4—C3—N1—C5	3.4 (8)
Mo3—O7—Mo2—O13	175.54 (12)	C2—C1—N1—C3	0.4 (6)
Mo4—O7—Mo2—O13	−11.97 (10)	C2—C1—N1—C5	178.2 (4)
Mo1—O7—Mo2—O13	−97.99 (10)	C6—C5—N1—C3	89.7 (6)
Mo2ⁱ—O7—Mo2—O7ⁱ	0.0	C6—C5—N1—C1	−87.7 (6)
Mo3—O7—Mo2—O7ⁱ	94.36 (11)	N1—C3—N2—C2	−0.4 (6)
Mo4—O7—Mo2—O7ⁱ	−93.14 (11)	C4—C3—N2—C2	178.5 (6)
Mo1—O7—Mo2—O7ⁱ	−179.17 (14)	C1—C2—N2—C3	0.6 (6)
Mo2ⁱ—O7—Mo2—Mo4ⁱ	−46.75 (8)	N4—C11—N3—C9	0.1 (5)
Mo3—O7—Mo2—Mo4ⁱ	47.61 (7)	C12—C11—N3—C9	−179.8 (5)
Mo4—O7—Mo2—Mo4ⁱ	−139.89 (7)	N4—C11—N3—C8	−173.5 (4)
Mo1—O7—Mo2—Mo4ⁱ	134.08 (6)	C12—C11—N3—C8	6.6 (7)
Mo2ⁱ—O7—Mo2—Mo3ⁱ	45.79 (8)	C10—C9—N3—C11	−0.4 (5)
Mo3—O7—Mo2—Mo3ⁱ	140.15 (7)	C10—C9—N3—C8	173.1 (4)
Mo4—O7—Mo2—Mo3ⁱ	−47.35 (7)	C7—C8—N3—C11	−138.3 (5)
Mo1—O7—Mo2—Mo3ⁱ	−133.38 (6)	C7—C8—N3—C9	49.2 (6)
Mo1—O5—Mo3—O3	−72.93 (18)	N3—C11—N4—C10	0.2 (5)
Mo1—O5—Mo3—O4	179.01 (15)	C12—C11—N4—C10	−179.9 (4)
Mo1—O5—Mo3—O13ⁱ	50.0 (3)	C9—C10—N4—C11	−0.4 (5)
Mo1—O5—Mo3—O7	20.83 (14)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O9ⁱⁱ	0.87 (3)	2.37 (4)	3.031 (5)	134 (4)
N2—H2N···O10ⁱⁱ	0.87 (3)	2.20 (2)	3.001 (5)	153 (5)
N4—H4N···O12ⁱⁱⁱ	0.86 (3)	2.39 (4)	3.052 (5)	134 (4)
N4—H4N···O4^iv	0.86 (3)	2.12 (3)	2.873 (4)	146 (5)

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

Experimental details

Crystal data
Chemical formula	(C₁₂H₂₀N₄)₂[Mo₈O₂₆]
M_r	1624.16
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	10.5680 (3), 11.4890 (5), 11.5600 (8)
α, β, γ (°)	60.777 (1), 68.155 (1), 70.400 (1)
V (Å³)	1116.29 (10)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	2.27
Crystal size (mm)	0.27 × 0.26 × 0.20

Data collection
Diffractometer	Bruker APEX CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.49, 0.63
No. of measured, independent and observed [I > 2σ(I)] reflections	6962, 5123, 3776
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.667

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.032, 0.079, 1.04
No. of reflections	5123
No. of parameters	306
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.53, −0.71

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2N···O9ⁱ	0.87 (3)	2.37 (4)	3.031 (5)	134 (4)
N2—H2N···O10ⁱ	0.87 (3)	2.20 (2)	3.001 (5)	153 (5)
N4—H4N···O12ⁱⁱ	0.86 (3)	2.39 (4)	3.052 (5)	134 (4)
N4—H4N···O4ⁱⁱⁱ	0.86 (3)	2.12 (3)	2.873 (4)	146 (5)

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

References

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Volume 64| Part 12| December 2008| Page m1487

doi:10.1107/S1600536808035022

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

A new β-octa­molybdate(VI) salt based on 1,4-bis­­(2-methyl-1H-imidazol-1-yl)butane

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

References

metal-organic compounds

A new β-octamolybdate(VI) salt based on 1,4-bis(2-methyl-1H-imidazol-1-yl)butane