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Acta Cryst. (2000). C56, e441-e442
https://doi.org/10.1107/S0108270100012221
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A new inorganic-organic hybrid: tetra­imid­azolium octa­molyb­date(VI) containing the [beta]-form of the [Mo8O26]4- anion

P. Gili, P. Núñez, P. Martín-Zarza and P. A. Lorenzo-Luis
The title compound, (C3H5N2)4[[beta]-Mo8O26], has been prepared from imidazole octamolybdate, (C3H5N2)4[(C3H4N2)2([gamma]-Mo8O26)], which was described previously. The [gamma][rightwards arrow][beta] conversion is produced in the presence of Cu(NO3)2·3H2O and is reported for the first time in this work. The X-ray structure analysis confirmed the presence of the [Mo8O26]4- anion. The structure consists of [beta]-Mo8O26 polyanions and imidazolium cations. These cations are linked to the terminal and bridging O atoms of the anion by hydrogen bonds.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100012221/qa0386sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012221/qa0386Isup2.hkl
Contains datablock I

CCDC reference: 152656

Comment top

Polyoxometalates of organic cations present considerable interest as a consequence of their photochemical and photochromic properties in solution as well as in the solid state (Yamase, 1998).

In our investigation of octamolybdates, we have tried to prepare a molybdenum oxide cluster in which the octamolybdate ions are linked to the transition metal atoms. Instead of this, we obtained the β-octamolybdate. An imidazole octamolybdate (C3H5N2)4[(C3H4N2)2(γ-Mo8O26)] containing imidazole coordinatively bound to the Mo atom in [γ-Mo8O26]4− has been described previously (Martín-Zarza et al., 1993). When an aqueous solution of this compound is treated with an aqueous solution of Cu(NO3)2·3H2O in a molar ratio Mo:Cu of 1:1, the β-form (C3H5N2)4[β-Mo8O26], (I), is obtained. The β-form does not contain N—Mo bonds and the organic cations are linked to terminal and bridging O atoms of the anion through hydrogen bonds.

Mechanisms of interconversion of polyoxometalates have been described (Masters et al., 1980; Kemplerer & Shum, 1976) but the γ → β conversion in the presence of Cu(NO3)2·3H2O to our knowledge has not been described previously. The structure of the title compound consists of β-Mo8O26 polyanions and organic cations. These anions are constituted by eight MoO6 octahedra sharing edges and corners. The octahedra have different Mo—O bonds, which can be classified as short terminal [1.690 (3)–1.715 (3) Å], intermediate length [1.761 (2)–1.959 (2) Å] and long bonds [1.992 (3)–2.537 (2) Å]. In the idealized octamolybdate anion, there are three different types of MoO6 octahedra: i) octahedra formed by atoms Mo1 and Mo1a, which, being closest to the centroid of the polyanion, are the least distorted; ii) octahedra formed by atoms Mo3 and Mo3a, which are the most distorted since they are furthest from the centroid; and iii) octahedra formed by atoms Mo2, Mo2a, Mo4 and Mo4a, which have an intermediate degree of distortion. Comparing the title compound with (C6H16N)4[β-Mo8O26]·2H2O (Fun et al., 1996), it can be seen that there are only slight differences in the Mo—O bond distances. These differences are due to the cation–polyanion interactions.

Finally, hydrogen bonds are observed between terminal and bridging O atoms of the polyanion and the imidazolium cations: N1—H···O5 2.864 (4) Å, 171.36°; N2—H···O10 2.827 (5) Å, 167.48°; N3—H···O7 2.819 (5) Å, 152.72°; N4—H···O11 2.884 (5) Å, 168.93°.

Experimental top

(C3H5N2)4[(C3H4N2)2(γ-Mo8O26)] containing the γ-form of the [Mo8O26]4− anion was prepared as described previously (Martín-Zarza et al., 1993). An aqueous solution of Cu(NO3)2·3H2O (0.1141 g, 0.47 mmol) was added to an aqueous solution of (C3H5N2)4[(C3H4N2)2(γ-Mo8O26)] (0.750 g, 0.47 mmol) in 600 ml of distilled water. The mixture was heated under reflux with stirring for 1 h. When the volume of this solution was reduced to 100 ml, the solution was allowed to stand at room temperature for few days. Colourless crystals of suitable size for X-ray diffraction analysis were obtained of (I). An uncharacterized pale green precipitate was also obtained.

Refinement top

All H atoms were generated geometrically and allowed to ride on their parent C or N atoms. A global Uiso was refined for H atoms attached to C atoms and another one for those attached to N atoms.

Computing details top

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4/PC (Harms, 1996); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: PLATON (Spek, 1990).

(I) top
Crystal data top
(C3H5N2)4[Mo8O26]Z = 1
Mr = 1459.88F(000) = 692
Triclinic, P1Dx = 2.925 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 9.3491 (15) ÅCell parameters from 25 reflections
b = 9.7506 (12) Åθ = 2.8–30.4°
c = 10.3634 (16) ŵ = 3.04 mm−1
α = 83.938 (11)°T = 293 K
β = 75.667 (12)°Prism, colourless
γ = 64.891 (10)°0.3 × 0.25 × 0.2 mm
V = 828.8 (2) Å3
Data collection top
Enraf-nonius CAD-4
diffractometer		4355 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.018
Graphite monochromatorθmax = 30.4°, θmin = 2.8°
ω scansh = 0→13
Absorption correction: ψ scan
(North et al., 1968)		k = −12→13
Tmin = 0.402, Tmax = 0.569l = −14→14
5293 measured reflections3 standard reflections every 120 min
5012 independent reflections intensity decay: none
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.024 w = 1/[σ2(Fo2) + (0.1P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.076(Δ/σ)max = 0.001
S = 0.93Δρmax = 0.54 e Å−3
5012 reflectionsΔρmin = −0.98 e Å−3
246 parameters
Crystal data top
(C3H5N2)4[Mo8O26]γ = 64.891 (10)°
Mr = 1459.88V = 828.8 (2) Å3
Triclinic, P1Z = 1
a = 9.3491 (15) ÅMo Kα radiation
b = 9.7506 (12) ŵ = 3.04 mm−1
c = 10.3634 (16) ÅT = 293 K
α = 83.938 (11)°0.3 × 0.25 × 0.2 mm
β = 75.667 (12)°
Data collection top
Enraf-nonius CAD-4
diffractometer		4355 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)		Rint = 0.018
Tmin = 0.402, Tmax = 0.5693 standard reflections every 120 min
5293 measured reflections intensity decay: none
5012 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.076H-atom parameters constrained
S = 0.93Δρmax = 0.54 e Å−3
5012 reflectionsΔρmin = −0.98 e Å−3
246 parameters
Special details top

Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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
Mo10.29766 (3)0.05761 (2)0.98010 (2)0.0138 (1)
Mo20.58171 (3)−0.02538 (3)0.71681 (2)0.0160 (1)
Mo30.30904 (3)−0.23220 (3)1.21359 (2)0.0189 (1)
Mo40.60385 (3)−0.31449 (3)0.94700 (2)0.0165 (1)
O10.5002 (2)−0.1145 (2)1.0909 (2)0.0163 (5)
O20.4325 (2)−0.0972 (2)0.84764 (19)0.0163 (5)
O30.7410 (3)0.0537 (2)0.6907 (2)0.0214 (6)
O40.4066 (3)−0.3233 (2)1.0410 (2)0.0205 (6)
O50.7238 (2)−0.1814 (2)0.87328 (19)0.0163 (5)
O60.6453 (3)−0.4055 (3)0.8026 (2)0.0259 (6)
O70.1883 (2)−0.0416 (2)1.0758 (2)0.0194 (5)
O80.6820 (3)−0.1734 (3)0.6095 (2)0.0260 (6)
O90.1335 (3)−0.2547 (3)1.2645 (3)0.0316 (7)
O100.4402 (3)0.1089 (3)0.6415 (2)0.0266 (6)
O110.4421 (3)−0.3624 (3)1.3004 (2)0.0293 (7)
O120.1648 (3)0.1870 (3)0.8966 (2)0.0257 (6)
O130.7409 (3)−0.4356 (3)1.0332 (3)0.0288 (7)
N1−0.0036 (3)−0.3883 (3)0.6901 (3)0.0293 (8)
N20.1909 (4)−0.6004 (4)0.6252 (4)0.0379 (9)
C10.0727 (5)−0.5286 (4)0.7269 (4)0.0352 (10)
C20.1888 (5)−0.5036 (5)0.5199 (4)0.0382 (11)
C30.0653 (4)−0.3698 (4)0.5602 (4)0.0316 (10)
N30.1300 (4)−0.1150 (4)0.7754 (3)0.0361 (9)
N40.3262 (4)−0.3257 (4)0.7230 (4)0.0416 (10)
C40.2036 (5)−0.2516 (5)0.8185 (4)0.0382 (11)
C50.3316 (5)−0.2356 (6)0.6162 (4)0.0451 (14)
C60.2077 (5)−0.1000 (5)0.6489 (5)0.0421 (12)
H10.04790−0.570100.810000.056 (7)*
H20.25920−0.525800.436500.056 (7)*
H30.03290−0.281800.509700.056 (7)*
H7−0.08420−0.318800.739700.052 (8)*
H80.25860−0.693600.625300.052 (8)*
H40.17400−0.289600.902100.056 (7)*
H50.40670−0.262100.535100.056 (7)*
H60.18080−0.013700.595900.056 (7)*
H90.04500−0.044700.820300.052 (8)*
H100.39370−0.418400.727700.052 (8)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0118 (1)0.0153 (1)0.0147 (1)−0.0053 (1)−0.0040 (1)−0.0001 (1)
Mo20.0176 (1)0.0166 (1)0.0126 (1)−0.0058 (1)−0.0039 (1)0.0001 (1)
Mo30.0195 (1)0.0186 (1)0.0185 (1)−0.0091 (1)−0.0028 (1)0.0013 (1)
Mo40.0171 (1)0.0137 (1)0.0183 (1)−0.0065 (1)−0.0027 (1)−0.0006 (1)
O10.0164 (9)0.0165 (8)0.0161 (8)−0.0065 (7)−0.0042 (7)0.0001 (7)
O20.0170 (9)0.0165 (8)0.0166 (9)−0.0075 (7)−0.0046 (7)−0.0010 (7)
O30.0216 (10)0.0226 (10)0.0186 (9)−0.0100 (8)−0.0006 (8)−0.0004 (8)
O40.0230 (10)0.0214 (9)0.0212 (10)−0.0144 (8)−0.0017 (8)−0.0013 (8)
O50.0159 (8)0.0176 (9)0.0145 (8)−0.0067 (7)−0.0015 (7)−0.0021 (7)
O60.0320 (12)0.0212 (10)0.0242 (11)−0.0118 (9)−0.0025 (9)−0.0050 (8)
O70.0167 (9)0.0216 (9)0.0208 (9)−0.0091 (8)−0.0033 (7)−0.0002 (8)
O80.0289 (11)0.0256 (10)0.0193 (10)−0.0066 (9)−0.0045 (8)−0.0051 (8)
O90.0282 (12)0.0368 (13)0.0321 (12)−0.0187 (11)−0.0022 (10)0.0028 (10)
O100.0258 (11)0.0263 (11)0.0228 (10)−0.0045 (9)−0.0102 (9)0.0036 (9)
O110.0336 (13)0.0229 (11)0.0271 (11)−0.0068 (9)−0.0093 (10)0.0019 (9)
O120.0231 (10)0.0237 (10)0.0295 (11)−0.0060 (9)−0.0134 (9)0.0048 (9)
O130.0281 (12)0.0239 (11)0.0343 (13)−0.0087 (9)−0.0131 (10)0.0062 (9)
N10.0220 (12)0.0253 (13)0.0307 (14)−0.0033 (10)−0.0008 (10)0.0002 (11)
N20.0263 (14)0.0227 (13)0.058 (2)−0.0015 (11)−0.0113 (14)−0.0053 (13)
C10.0346 (18)0.0328 (18)0.0343 (18)−0.0111 (15)−0.0095 (15)0.0079 (14)
C20.0316 (18)0.051 (2)0.0340 (18)−0.0229 (17)0.0040 (14)−0.0106 (16)
C30.0310 (17)0.0354 (18)0.0306 (16)−0.0168 (14)−0.0086 (13)0.0081 (13)
N30.0236 (14)0.0376 (16)0.0407 (17)−0.0042 (12)−0.0073 (12)−0.0101 (13)
N40.0276 (15)0.0294 (15)0.067 (2)−0.0032 (12)−0.0211 (16)−0.0092 (15)
C40.040 (2)0.048 (2)0.0374 (19)−0.0269 (18)−0.0148 (16)0.0082 (16)
C50.0328 (19)0.061 (3)0.038 (2)−0.0175 (19)0.0013 (16)−0.0163 (19)
C60.045 (2)0.039 (2)0.045 (2)−0.0203 (18)−0.0142 (18)0.0117 (17)
Geometric parameters (Å, º) top
Mo1—O12.386 (2)Mo4—O61.697 (2)
Mo1—O21.9282 (19)Mo4—O131.701 (3)
Mo1—O71.761 (2)N1—C11.312 (5)
Mo1—O121.690 (3)N1—C31.370 (5)
Mo1—O1i2.130 (2)N2—C11.321 (6)
Mo1—O5i1.9588 (19)N2—C21.364 (6)
Mo2—O21.992 (2)N1—H70.8601
Mo2—O31.902 (3)N2—H80.8593
Mo2—O52.353 (2)N3—C61.359 (6)
Mo2—O81.695 (2)N3—C41.302 (6)
Mo2—O101.703 (3)N4—C41.305 (6)
Mo2—O1i2.313 (2)N4—C51.343 (6)
Mo3—O12.537 (2)N3—H90.8602
Mo3—O41.913 (2)N4—H100.8599
Mo3—O72.2857 (19)C2—C31.344 (6)
Mo3—O91.695 (3)C1—H10.9308
Mo3—O111.715 (3)C2—H20.9295
Mo3—O3i1.917 (2)C3—H30.9300
Mo4—O12.2936 (19)C5—C61.344 (7)
Mo4—O22.3645 (19)C4—H40.9301
Mo4—O41.893 (3)C5—H50.9305
Mo4—O52.031 (2)C6—H60.9296
Mo1···N33.799 (4)O9···H9ii2.8512
Mo1···C44.088 (5)O10···H5iii2.7513
Mo1···N3ii4.013 (4)O10···H8vii1.9792
Mo2···O10iii3.956 (2)O11···H5vi2.6098
Mo2···C6iii4.136 (5)O11···H2vi2.8452
Mo2···N1iv3.958 (3)O11···H10v2.0335
Mo2···C54.060 (5)O12···H1vii2.3344
Mo2···C64.091 (5)O13···H1v2.8711
Mo3···O6v3.391 (3)O13···H4v2.5174
Mo3···Mo4v4.5604 (8)N1···Mo2x3.958 (3)
Mo3···C2vi4.163 (4)N1···Mo4x3.795 (3)
Mo4···C1iv4.131 (5)N1···O5x2.867 (3)
Mo4···Mo3v4.5604 (8)N1···O8x3.057 (4)
Mo4···Mo4v4.7044 (9)N1···C43.338 (6)
Mo4···N43.926 (4)N2···O10xi2.825 (5)
Mo4···N1iv3.795 (3)N2···O8viii3.110 (4)
Mo4···O4v3.563 (2)N3···O23.175 (5)
Mo4···C44.062 (5)N3···Mo1ii4.013 (4)
Mo1···H9ii3.4006N3···O7ii2.817 (4)
Mo1···H7ii3.6442N3···Mo13.799 (4)
Mo2···H8vii3.6009N4···Mo43.926 (4)
Mo2···H5iii3.6410N4···O63.049 (5)
Mo2···H6iii3.5316N4···O11v2.882 (5)
Mo2···H7iv3.2615C1···Mo4x4.131 (5)
Mo3···H3vi3.6249C1···O12xi3.036 (4)
Mo3···H5vi3.6188C1···O13v3.284 (5)
Mo3···H2vi3.5988C1···O9ix3.394 (6)
Mo3···H9ii3.3406C2···O8viii3.168 (5)
Mo3···H10v3.4734C2···O6viii3.355 (5)
Mo4···H7iv3.1521C2···Mo3xii4.163 (4)
O2···N33.175 (5)C2···O9xii3.379 (5)
O2···C43.176 (5)C2···C3xiii3.397 (7)
O2···C53.369 (5)C3···O8x3.201 (5)
O2···C63.296 (6)C3···O9xii3.158 (5)
O4···Mo4v3.563 (2)C3···C53.448 (7)
O4···C43.179 (5)C3···C2xiii3.397 (7)
O4···O6v3.106 (3)C4···O13v3.162 (5)
O4···O4v3.228 (3)C4···O23.176 (5)
O5···N1iv2.867 (3)C4···Mo14.088 (5)
O6···N43.049 (5)C4···Mo44.062 (5)
O6···O11v3.072 (4)C4···O43.179 (5)
O6···O9v3.114 (4)C4···N13.338 (6)
O6···O82.934 (3)C5···O11xii3.377 (5)
O6···C2viii3.355 (5)C5···O23.369 (5)
O6···O4v3.106 (3)C5···Mo24.060 (5)
O6···Mo3v3.391 (3)C5···C33.448 (7)
O7···N3ii2.817 (4)C6···O23.296 (6)
O8···N2viii3.110 (4)C6···Mo24.091 (5)
O8···C3iv3.201 (5)C6···Mo2iii4.136 (5)
O8···C2viii3.168 (5)H1···O12xi2.3344
O8···O10iii2.997 (3)H1···O13v2.8711
O8···N1iv3.057 (4)H2···O8viii2.8159
O8···O62.934 (3)H2···Mo3xii3.5988
O9···C1ix3.394 (6)H2···O11xii2.8452
O9···C2vi3.379 (5)H2···O6viii2.4766
O9···C3vi3.158 (5)H3···Mo3xii3.6248
O9···O6v3.114 (4)H3···O9xii2.5095
O10···O8iii2.997 (3)H4···O42.7843
O10···Mo2iii3.956 (2)H4···O13v2.5174
O10···O123.097 (3)H5···O11xii2.6098
O10···N2vii2.825 (5)H5···Mo3xii3.6188
O11···N4v2.882 (5)H5···Mo2iii3.6410
O11···C5vi3.377 (5)H5···O10iii2.7513
O11···O6v3.072 (4)H6···Mo2iii3.5316
O12···O13i3.112 (4)H6···O3iii2.9045
O12···O103.097 (3)H7···Mo1ii3.6442
O12···C1vii3.036 (4)H7···Mo4x3.1521
O13···C4v3.162 (5)H7···O5x2.0134
O13···C1v3.284 (6)H7···Mo2x3.2615
O13···O12i3.112 (4)H7···O8x2.6523
O3···H6iii2.9045H7···O6x2.9012
O4···H42.7843H8···O8viii2.7014
O5···H7iv2.0134H8···O10xi1.9792
O6···H2viii2.4766H8···Mo2xi3.6009
O6···H102.7069H9···Mo1ii3.4006
O6···H7iv2.9012H9···Mo3ii3.3406
O7···H9ii2.0238H9···O7ii2.0238
O8···H8viii2.7014H9···O9ii2.8512
O8···H2viii2.8159H10···O62.7069
O8···H7iv2.6523H10···Mo3v3.4734
O9···H3vi2.5095H10···O11v2.0335
O1—Mo1—O277.34 (8)O4—Mo4—O6102.90 (12)
O1—Mo1—O780.99 (8)O4—Mo4—O13103.32 (12)
O1—Mo1—O12175.13 (11)O5—Mo4—O696.75 (11)
O1—Mo1—O1i75.26 (7)O5—Mo4—O1396.83 (12)
O1—Mo1—O5i77.84 (7)O6—Mo4—O13105.17 (14)
O2—Mo1—O797.00 (9)Mo1—O1—Mo390.72 (7)
O2—Mo1—O12102.49 (10)Mo1—O1—Mo497.80 (8)
O1i—Mo1—O278.68 (8)Mo1—O1—Mo1i104.74 (8)
O2—Mo1—O5i149.71 (9)Mo1—O1—Mo2i97.49 (7)
O7—Mo1—O12103.84 (12)Mo3—O1—Mo485.06 (6)
O1i—Mo1—O7156.24 (9)Mo1i—O1—Mo3164.52 (10)
O5i—Mo1—O795.98 (9)Mo2i—O1—Mo385.16 (7)
O1i—Mo1—O1299.90 (11)Mo1i—O1—Mo493.51 (8)
O5i—Mo1—O12100.77 (10)Mo2i—O1—Mo4161.93 (9)
O1i—Mo1—O5i78.44 (8)Mo1i—O1—Mo2i91.87 (8)
O2—Mo2—O3146.53 (9)Mo1—O2—Mo2109.17 (9)
O2—Mo2—O571.79 (8)Mo1—O2—Mo4110.07 (9)
O2—Mo2—O8101.19 (11)Mo2—O2—Mo4105.09 (9)
O2—Mo2—O1097.47 (11)Mo2—O3—Mo3i118.72 (13)
O1i—Mo2—O273.12 (7)Mo3—O4—Mo4118.44 (14)
O3—Mo2—O583.27 (8)Mo2—O5—Mo4104.19 (9)
O3—Mo2—O899.70 (12)Mo1i—O5—Mo2109.68 (8)
O3—Mo2—O10101.67 (12)Mo1i—O5—Mo4107.78 (9)
O1i—Mo2—O378.29 (8)Mo1—O7—Mo3119.44 (11)
O5—Mo2—O887.68 (10)C1—N1—C3109.3 (3)
O5—Mo2—O10164.47 (9)C1—N2—C2109.4 (4)
O1i—Mo2—O572.20 (7)C1—N1—H7125.37
O8—Mo2—O10105.74 (12)C3—N1—H7125.30
O1i—Mo2—O8159.89 (10)C1—N2—H8125.34
O1i—Mo2—O1094.21 (9)C2—N2—H8125.26
O1—Mo3—O472.25 (9)C4—N3—C6109.8 (4)
O1—Mo3—O768.85 (7)C4—N4—C5109.9 (4)
O1—Mo3—O9157.70 (11)C4—N3—H9125.12
O1—Mo3—O1195.92 (11)C6—N3—H9125.05
O1—Mo3—O3i72.47 (9)C5—N4—H10124.99
O4—Mo3—O777.07 (8)C4—N4—H10125.10
O4—Mo3—O9105.64 (13)N1—C1—N2107.9 (3)
O4—Mo3—O1198.75 (10)N2—C2—C3106.7 (4)
O3i—Mo3—O4141.93 (9)N1—C3—C2106.7 (3)
O7—Mo3—O988.94 (11)N1—C1—H1126.02
O7—Mo3—O11164.77 (11)N2—C1—H1126.08
O3i—Mo3—O777.29 (8)C3—C2—H2126.68
O9—Mo3—O11106.28 (14)N2—C2—H2126.65
O3i—Mo3—O9101.53 (13)C2—C3—H3126.66
O3i—Mo3—O1198.65 (11)N1—C3—H3126.67
O1—Mo4—O271.41 (7)N3—C4—N4107.6 (4)
O1—Mo4—O478.66 (8)N4—C5—C6106.8 (4)
O1—Mo4—O573.25 (7)N3—C6—C5105.8 (4)
O1—Mo4—O6157.61 (10)N3—C4—H4126.24
O1—Mo4—O1396.03 (11)N4—C4—H4126.17
O2—Mo4—O483.84 (8)N4—C5—H5126.55
O2—Mo4—O570.91 (8)C6—C5—H5126.60
O2—Mo4—O686.46 (10)N3—C6—H6127.11
O2—Mo4—O13164.30 (11)C5—C6—H6127.07
O4—Mo4—O5146.86 (8)
O2—Mo1—O1—Mo3−99.42 (8)O8—Mo2—O1i—Mo1−94.5 (3)
O2—Mo1—O1—Mo4−14.30 (8)O8—Mo2—O1i—Mo1i10.6 (4)
O2—Mo1—O1—Mo1i81.43 (9)O8—Mo2—O1i—Mo3i100.7 (3)
O2—Mo1—O1—Mo2i175.37 (9)O10—Mo2—O1i—Mo178.16 (11)
O7—Mo1—O1—Mo3−0.09 (7)O10—Mo2—O1i—Mo1i−176.71 (11)
O7—Mo1—O1—Mo485.03 (9)O10—Mo2—O1i—Mo3i−86.62 (11)
O7—Mo1—O1—Mo1i−179.24 (10)O4—Mo3—O1—Mo182.71 (9)
O7—Mo1—O1—Mo2i−85.31 (9)O4—Mo3—O1—Mo4−15.05 (8)
O1i—Mo1—O1—Mo3179.15 (8)O4—Mo3—O1—Mo2i−179.84 (9)
O1i—Mo1—O1—Mo4−95.73 (8)O7—Mo3—O1—Mo10.07 (6)
O1i—Mo1—O1—Mo1i0.00 (8)O7—Mo3—O1—Mo4−97.69 (7)
O1i—Mo1—O1—Mo2i93.94 (8)O7—Mo3—O1—Mo2i97.53 (7)
O5i—Mo1—O1—Mo398.08 (8)O9—Mo3—O1—Mo1−5.3 (3)
O5i—Mo1—O1—Mo4−176.80 (9)O9—Mo3—O1—Mo4−103.1 (3)
O5i—Mo1—O1—Mo1i−81.07 (9)O9—Mo3—O1—Mo2i92.1 (3)
O5i—Mo1—O1—Mo2i12.87 (8)O11—Mo3—O1—Mo1−179.97 (9)
O1—Mo1—O2—Mo2−100.22 (10)O11—Mo3—O1—Mo482.27 (9)
O1—Mo1—O2—Mo414.64 (8)O11—Mo3—O1—Mo2i−82.51 (9)
O7—Mo1—O2—Mo2−179.31 (10)O3i—Mo3—O1—Mo1−82.73 (9)
O7—Mo1—O2—Mo4−64.44 (11)O3i—Mo3—O1—Mo4179.50 (10)
O12—Mo1—O2—Mo274.79 (14)O3i—Mo3—O1—Mo2i14.72 (8)
O12—Mo1—O2—Mo4−170.35 (12)O1—Mo3—O4—Mo420.89 (9)
O1i—Mo1—O2—Mo2−22.98 (9)O7—Mo3—O4—Mo492.52 (11)
O1i—Mo1—O2—Mo491.88 (10)O9—Mo3—O4—Mo4177.70 (13)
O5i—Mo1—O2—Mo2−64.57 (18)O11—Mo3—O4—Mo4−72.57 (14)
O5i—Mo1—O2—Mo450.29 (19)O3i—Mo3—O4—Mo443.8 (2)
O1—Mo1—O7—Mo30.11 (11)O1—Mo3—O7—Mo1−0.11 (9)
O2—Mo1—O7—Mo376.05 (11)O4—Mo3—O7—Mo1−75.84 (13)
O12—Mo1—O7—Mo3−179.20 (11)O9—Mo3—O7—Mo1177.84 (14)
O1i—Mo1—O7—Mo3−1.7 (3)O3i—Mo3—O7—Mo175.77 (13)
O5i—Mo1—O7—Mo3−76.53 (11)O1—Mo3—O3i—Mo2i−20.56 (10)
O1—Mo1—O1i—Mo298.25 (7)O4—Mo3—O3i—Mo2i−43.4 (2)
O1—Mo1—O1i—Mo1i0.00 (7)O7—Mo3—O3i—Mo2i−92.10 (12)
O1—Mo1—O1i—Mo4i−99.01 (8)O9—Mo3—O3i—Mo2i−178.35 (14)
O2—Mo1—O1i—Mo218.53 (7)O11—Mo3—O3i—Mo2i72.96 (14)
O2—Mo1—O1i—Mo1i−79.72 (8)O2—Mo4—O1—Mo111.97 (7)
O2—Mo1—O1i—Mo4i−178.73 (9)O2—Mo4—O1—Mo3102.02 (7)
O7—Mo1—O1i—Mo2100.1 (2)O2—Mo4—O1—Mo1i−93.44 (8)
O7—Mo1—O1i—Mo1i1.9 (2)O4—Mo4—O1—Mo1−75.28 (9)
O7—Mo1—O1i—Mo4i−97.15 (19)O4—Mo4—O1—Mo314.77 (7)
O12—Mo1—O1i—Mo2−82.37 (9)O4—Mo4—O1—Mo1i179.32 (9)
O12—Mo1—O1i—Mo1i179.39 (9)O5—Mo4—O1—Mo186.95 (8)
O12—Mo1—O1i—Mo4i80.38 (10)O5—Mo4—O1—Mo3177.00 (8)
O5i—Mo1—O1i—Mo2178.55 (8)O5—Mo4—O1—Mo1i−18.45 (7)
O1—Mo1—O5i—Mo2i−13.32 (8)O6—Mo4—O1—Mo121.1 (3)
O1—Mo1—O5i—Mo4i99.51 (10)O6—Mo4—O1—Mo3111.1 (3)
O2—Mo1—O5i—Mo2i−48.89 (19)O6—Mo4—O1—Mo1i−84.3 (3)
O2—Mo1—O5i—Mo4i63.94 (18)O13—Mo4—O1—Mo1−177.70 (12)
O7—Mo1—O5i—Mo2i66.09 (10)O13—Mo4—O1—Mo3−87.65 (11)
O7—Mo1—O5i—Mo4i178.92 (10)O13—Mo4—O1—Mo1i76.89 (12)
O12—Mo1—O5i—Mo2i171.44 (12)O1—Mo4—O2—Mo1−15.70 (9)
O12—Mo1—O5i—Mo4i−75.72 (13)O1—Mo4—O2—Mo2101.72 (9)
O3—Mo2—O2—Mo154.09 (18)O4—Mo4—O2—Mo164.37 (11)
O3—Mo2—O2—Mo4−63.94 (16)O4—Mo4—O2—Mo2−178.20 (10)
O5—Mo2—O2—Mo197.94 (10)O5—Mo4—O2—Mo1−93.85 (10)
O5—Mo2—O2—Mo4−20.09 (7)O5—Mo4—O2—Mo223.58 (8)
O8—Mo2—O2—Mo1−178.28 (12)O6—Mo4—O2—Mo1167.76 (13)
O8—Mo2—O2—Mo463.68 (12)O6—Mo4—O2—Mo2−74.81 (12)
O10—Mo2—O2—Mo1−70.54 (12)O1—Mo4—O4—Mo3−22.52 (10)
O10—Mo2—O2—Mo4171.43 (10)O2—Mo4—O4—Mo3−94.74 (11)
O1i—Mo2—O2—Mo121.62 (9)O5—Mo4—O4—Mo3−54.8 (2)
O1i—Mo2—O2—Mo4−96.42 (9)O6—Mo4—O4—Mo3−179.66 (12)
O2—Mo2—O3—Mo3i−53.7 (2)O13—Mo4—O4—Mo371.06 (14)
O5—Mo2—O3—Mo3i−95.18 (12)O1—Mo4—O5—Mo2−95.34 (8)
O8—Mo2—O3—Mo3i178.35 (13)O1—Mo4—O5—Mo1i21.14 (8)
O10—Mo2—O3—Mo3i69.91 (13)O2—Mo4—O5—Mo2−19.70 (7)
O1i—Mo2—O3—Mo3i−22.03 (11)O2—Mo4—O5—Mo1i96.78 (9)
O2—Mo2—O5—Mo423.47 (8)O4—Mo4—O5—Mo2−62.16 (18)
O2—Mo2—O5—Mo1i−91.68 (10)O4—Mo4—O5—Mo1i54.3 (2)
O3—Mo2—O5—Mo4−179.16 (9)O6—Mo4—O5—Mo264.17 (12)
O3—Mo2—O5—Mo1i65.69 (10)O6—Mo4—O5—Mo1i−179.35 (12)
O8—Mo2—O5—Mo4−79.11 (12)O13—Mo4—O5—Mo2170.40 (11)
O8—Mo2—O5—Mo1i165.74 (13)O13—Mo4—O5—Mo1i−73.12 (13)
O1i—Mo2—O5—Mo4101.02 (9)C3—N1—C1—N21.2 (5)
O1i—Mo2—O5—Mo1i−14.13 (9)C1—N1—C3—C2−1.2 (5)
O2—Mo2—O1i—Mo1−18.37 (7)C2—N2—C1—N1−0.7 (5)
O2—Mo2—O1i—Mo1i86.75 (8)C1—N2—C2—C30.0 (6)
O2—Mo2—O1i—Mo3i176.84 (8)C6—N3—C4—N4−0.4 (6)
O3—Mo2—O1i—Mo1179.23 (8)C4—N3—C6—C50.9 (6)
O3—Mo2—O1i—Mo1i−75.64 (8)C4—N4—C5—C60.7 (6)
O3—Mo2—O1i—Mo3i14.45 (7)C5—N4—C4—N3−0.2 (6)
O5—Mo2—O1i—Mo1−94.16 (8)N2—C2—C3—N10.7 (5)
O5—Mo2—O1i—Mo1i10.97 (7)N4—C5—C6—N3−1.0 (6)
O5—Mo2—O1i—Mo3i101.06 (7)
Symmetry codes: (i) −x+1, −y, −z+2; (ii) −x, −y, −z+2; (iii) −x+1, −y, −z+1; (iv) x+1, y, z; (v) −x+1, −y−1, −z+2; (vi) x, y, z+1; (vii) x, y+1, z; (viii) −x+1, −y−1, −z+1; (ix) −x, −y−1, −z+2; (x) x−1, y, z; (xi) x, y−1, z; (xii) x, y, z−1; (xiii) −x, −y−1, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H7···O5x0.86012.01342.867 (3)171.51
N2—H8···O10xi0.85931.97922.825 (5)167.95
N3—H9···O7ii0.86022.02382.817 (4)152.86
N4—H10···O11v0.85992.03352.882 (5)168.77
C1—H1···O12xi0.93082.33443.036 (4)131.90
C2—H2···O6viii0.92952.47663.355 (5)157.59
C3—H3···O9xii0.93002.50953.158 (5)126.98
C4—H4···O13v0.93012.51743.162 (5)126.61
Symmetry codes: (ii) −x, −y, −z+2; (v) −x+1, −y−1, −z+2; (viii) −x+1, −y−1, −z+1; (x) x−1, y, z; (xi) x, y−1, z; (xii) x, y, z−1.

Experimental details

Crystal data
Chemical formula(C3H5N2)4[Mo8O26]
Mr1459.88
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.3491 (15), 9.7506 (12), 10.3634 (16)
α, β, γ (°)83.938 (11), 75.667 (12), 64.891 (10)
V (Å3)828.8 (2)
Z1
Radiation typeMo Kα
µ (mm−1)3.04
Crystal size (mm)0.3 × 0.25 × 0.2
Data collection
DiffractometerEnraf-nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.402, 0.569
No. of measured, independent and
observed [I > 2σ(I)] reflections		5293, 5012, 4355
Rint0.018
(sin θ/λ)max (Å−1)0.712
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.076, 0.93
No. of reflections5012
No. of parameters246
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.54, −0.98

Computer programs: CAD-4 EXPRESS (Enraf-Nonius, 1994), CAD-4 EXPRESS, XCAD4/PC (Harms, 1996), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1990).

Selected geometric parameters (Å, º) top
Mo1—O12.386 (2)Mo3—O111.715 (3)
Mo1—O21.9282 (19)Mo3—O3i1.917 (2)
Mo1—O71.761 (2)Mo4—O12.2936 (19)
Mo1—O121.690 (3)Mo4—O22.3645 (19)
Mo1—O1i2.130 (2)Mo4—O41.893 (3)
Mo1—O5i1.9588 (19)Mo4—O52.031 (2)
Mo2—O21.992 (2)Mo4—O61.697 (2)
Mo2—O31.902 (3)Mo4—O131.701 (3)
Mo2—O52.353 (2)N1—C11.312 (5)
Mo2—O81.695 (2)N1—C31.370 (5)
Mo2—O101.703 (3)N2—C11.321 (6)
Mo2—O1i2.313 (2)N2—C21.364 (6)
Mo3—O12.537 (2)N3—C61.359 (6)
Mo3—O41.913 (2)N3—C41.302 (6)
Mo3—O72.2857 (19)N4—C41.305 (6)
Mo3—O91.695 (3)N4—C51.343 (6)
O1—Mo1—O277.34 (8)O1—Mo4—O271.41 (7)
O1—Mo1—O780.99 (8)O1—Mo4—O478.66 (8)
O1—Mo1—O12175.13 (11)O1—Mo4—O573.25 (7)
O1—Mo1—O1i75.26 (7)O1—Mo4—O6157.61 (10)
O1—Mo1—O5i77.84 (7)O1—Mo4—O1396.03 (11)
O2—Mo1—O797.00 (9)O2—Mo4—O483.84 (8)
O2—Mo1—O12102.49 (10)O2—Mo4—O570.91 (8)
O1i—Mo1—O278.68 (8)O2—Mo4—O686.46 (10)
O2—Mo1—O5i149.71 (9)O2—Mo4—O13164.30 (11)
O7—Mo1—O12103.84 (12)O4—Mo4—O5146.86 (8)
O1i—Mo1—O7156.24 (9)O4—Mo4—O6102.90 (12)
O5i—Mo1—O795.98 (9)O4—Mo4—O13103.32 (12)
O1i—Mo1—O1299.90 (11)O5—Mo4—O696.75 (11)
O5i—Mo1—O12100.77 (10)O5—Mo4—O1396.83 (12)
O1i—Mo1—O5i78.44 (8)O6—Mo4—O13105.17 (14)
O2—Mo2—O3146.53 (9)Mo1—O1—Mo390.72 (7)
O2—Mo2—O571.79 (8)Mo1—O1—Mo497.80 (8)
O2—Mo2—O8101.19 (11)Mo1—O1—Mo1i104.74 (8)
O2—Mo2—O1097.47 (11)Mo1—O1—Mo2i97.49 (7)
O1i—Mo2—O273.12 (7)Mo3—O1—Mo485.06 (6)
O3—Mo2—O583.27 (8)Mo1i—O1—Mo3164.52 (10)
O3—Mo2—O899.70 (12)Mo2i—O1—Mo385.16 (7)
O3—Mo2—O10101.67 (12)Mo1i—O1—Mo493.51 (8)
O1i—Mo2—O378.29 (8)Mo2i—O1—Mo4161.93 (9)
O5—Mo2—O887.68 (10)Mo1i—O1—Mo2i91.87 (8)
O5—Mo2—O10164.47 (9)Mo1—O2—Mo2109.17 (9)
O1i—Mo2—O572.20 (7)Mo1—O2—Mo4110.07 (9)
O8—Mo2—O10105.74 (12)Mo2—O2—Mo4105.09 (9)
O1i—Mo2—O8159.89 (10)Mo2—O3—Mo3i118.72 (13)
O1i—Mo2—O1094.21 (9)Mo3—O4—Mo4118.44 (14)
O1—Mo3—O472.25 (9)Mo2—O5—Mo4104.19 (9)
O1—Mo3—O768.85 (7)Mo1i—O5—Mo2109.68 (8)
O1—Mo3—O9157.70 (11)Mo1i—O5—Mo4107.78 (9)
O1—Mo3—O1195.92 (11)Mo1—O7—Mo3119.44 (11)
O1—Mo3—O3i72.47 (9)C1—N1—C3109.3 (3)
O4—Mo3—O777.07 (8)C1—N2—C2109.4 (4)
O4—Mo3—O9105.64 (13)C4—N3—C6109.8 (4)
O4—Mo3—O1198.75 (10)C4—N4—C5109.9 (4)
O3i—Mo3—O4141.93 (9)N1—C1—N2107.9 (3)
O7—Mo3—O988.94 (11)N2—C2—C3106.7 (4)
O7—Mo3—O11164.77 (11)N1—C3—C2106.7 (3)
O3i—Mo3—O777.29 (8)N3—C4—N4107.6 (4)
O9—Mo3—O11106.28 (14)N4—C5—C6106.8 (4)
O3i—Mo3—O9101.53 (13)N3—C6—C5105.8 (4)
O3i—Mo3—O1198.65 (11)
Symmetry code: (i) −x+1, −y, −z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H7···O5ii0.86012.01342.867 (3)171.51
N2—H8···O10iii0.85931.97922.825 (5)167.95
N3—H9···O7iv0.86022.02382.817 (4)152.86
N4—H10···O11v0.85992.03352.882 (5)168.77
C1—H1···O12iii0.93082.33443.036 (4)131.90
C2—H2···O6vi0.92952.47663.355 (5)157.59
C3—H3···O9vii0.93002.50953.158 (5)126.98
C4—H4···O13v0.93012.51743.162 (5)126.61
Symmetry codes: (ii) x−1, y, z; (iii) x, y−1, z; (iv) −x, −y, −z+2; (v) −x+1, −y−1, −z+2; (vi) −x+1, −y−1, −z+1; (vii) x, y, z−1.
 

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