Commensurate (C6H14N2)2[Mo8O26]·4H2O and incommensurate (C6H14N2)2[Mo8O26]·4.66H2O: a structural versatility linked to solvent content

Evain, M.; Petricek, V.; Coué, V.; Dessapt, R.; Bujoli-Doeuff, M.; Jobic, S.

doi:10.1107/S0108768106025791

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Commensurate (C₆H₁₄N₂)₂[Mo₈O₂₆]·4H₂O and incommensurate (C₆H₁₄N₂)₂[Mo₈O₂₆]·4.66H₂O: a structural versatility linked to solvent content

M. Evain, V. Petricek, V. Coué, R. Dessapt, M. Bujoli-Doeuff and S. Jobic

The syntheses and structure determinations by means of single-crystal X-ray diffraction of commensurate (C₆H₁₄N₂)₂[Mo₈O₂₆]·4H₂O and incommensurate (C₆H₁₄N₂)₂[Mo₈O₂₆]·4.66H₂O, two new organic–inorganic hybrid compounds based on polyoxomolybdates and differing in their solvent content, are reported. Given the important disorder observed in the latter compound, only a combination of non-harmonic waves, crenel functions and TLS tensors offered a good modelling of the structure. (C₆H₁₄N₂)₂[Mo₈O₂₆].nH₂O results from the self-assembly of [Mo₈O₂₆]⁴⁻ anionic chains, C₆H₁₄N₂²⁺ (H₂DABCO²⁺) cations and water molecules. The [Mo₈O₂₆]⁴⁻ chain is built from γ-[Mo₈O₂₈]⁸⁻ octamolybdate clusters, connected to each other through corner sharing. In both compounds, the [Mo₈O₂₆]⁴⁻ chains are separated, in a similar way, by the H₂DABCO²⁺ subunits, acting as charge-compensating cations, and by the water molecules. The orientation of the H₂DABCO²⁺ cations is shown to be different from what has been observed previously in monoclinic (H₂DABCO)₂[Mo₈O₂₆]·4H₂O, and therefore to give a different network of hydrogen bonds.

Keywords: organic–inorganic hybrid materials; polyoxomolybdates; single-crystal X-ray structure determination; aperiodic structures; crenel functions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106025791/sn5039sup1.cif Contains datablocks global, (I), (II)
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768106025791/sn5039Isup2.hkl Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768106025791/sn5039IIsup3.hkl Contains datablock II
	Portable Document Format (PDF) file https://doi.org/10.1107/S0108768106025791/sn5039sup4.pdf Geometric parameters

CCDC reference: 624333

Computing details top

For both compounds, program(s) used to refine structure: (Jana2000; Petricek and Dusek, 2000); software used to prepare material for publication: (Jana2000; Petricek and Dusek, 2000).

Figures top

(I) top

Crystal data top

(C₆H₁₄N₂)₂[Mo₈O₂₆]·4H₂O	V = 2565.0 (6) Å³
M_r = 1483.9	Z = 3
Triclinic, P1	F(000) = 2112
Hall symbol: -P 1	D_x = 2.881 Mg m⁻³
a = 12.3378 (15) Å	Mo Kα radiation, λ = 0.71069 Å
b = 14.417 (2) Å	µ = 2.95 mm⁻¹
c = 16.1439 (16) Å	T = 293 K
α = 100.927 (9)°	Elongated block, colourless
β = 106.487 (8)°	0.18 × 0.10 × 0.08 mm
γ = 104.11 (1)°

Data collection top

Nonius CCD diffractometer	R_int = 0.068
Absorption correction: gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000)	θ_max = 35.0°, θ_min = 6.4°
T_min = 0.595, T_max = 0.833	h = −19→19
90290 measured reflections	k = −23→22
21895 independent reflections	l = −26→26
14316 reflections with I > 2σ(I)

Refinement top

Refinement on F²	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.058	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.001936I²)
wR(F²) = 0.135	(Δ/σ)_max = 0.001
S = 1.43	Δρ_max = 1.61 e Å⁻³
21895 reflections	Δρ_min = −1.89 e Å⁻³
730 parameters

Crystal data top

(C₆H₁₄N₂)₂[Mo₈O₂₆]·4H₂O	γ = 104.11 (1)°
M_r = 1483.9	V = 2565.0 (6) Å³
Triclinic, P1	Z = 3
a = 12.3378 (15) Å	Mo Kα radiation
b = 14.417 (2) Å	µ = 2.95 mm⁻¹
c = 16.1439 (16) Å	T = 293 K
α = 100.927 (9)°	0.18 × 0.10 × 0.08 mm
β = 106.487 (8)°

Data collection top

Nonius CCD diffractometer	21895 independent reflections
Absorption correction: gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000)	14316 reflections with I > 2σ(I)
T_min = 0.595, T_max = 0.833	R_int = 0.068
90290 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.058	730 parameters
wR(F²) = 0.135	H-atom parameters constrained
S = 1.43	Δρ_max = 1.61 e Å⁻³
21895 reflections	Δρ_min = −1.89 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Mo1	0.25888 (4)	0.37951 (3)	−0.02610 (3)	0.01868 (14)
Mo2	0.47524 (3)	0.44973 (3)	0.17692 (3)	0.01540 (13)
Mo3	0.78573 (4)	0.39209 (3)	0.20671 (3)	0.01813 (14)
Mo4	0.57152 (4)	0.35669 (3)	0.02056 (3)	0.01616 (13)
Mo5	0.19472 (4)	0.28345 (3)	0.12704 (3)	0.01999 (14)
Mo6	0.40766 (4)	0.30695 (3)	0.31313 (3)	0.01689 (13)
Mo7	0.73264 (4)	0.29683 (3)	0.36259 (3)	0.01807 (13)
Mo8	0.50910 (3)	0.21841 (3)	0.16045 (3)	0.01450 (12)
Mo9	0.25284 (4)	0.03970 (3)	0.30053 (3)	0.01699 (13)
Mo10	0.47035 (3)	0.11159 (3)	0.50438 (3)	0.01507 (13)
Mo11	0.79453 (4)	0.07729 (3)	0.55027 (3)	0.01802 (14)
Mo12	0.58281 (3)	0.03153 (3)	0.35728 (3)	0.01555 (13)
O1	0.1439 (3)	0.4283 (3)	−0.0297 (3)	0.0288 (15)
O2	0.3126 (3)	0.4319 (2)	0.1275 (2)	0.0197 (12)
O3	0.2422 (4)	0.3269 (3)	−0.1334 (3)	0.0329 (16)
O4	0.2041 (3)	0.2636 (2)	0.0066 (2)	0.0239 (13)
O5	0.4323 (3)	0.3823 (2)	0.0356 (2)	0.0190 (12)
O6	0.6392 (3)	0.4761 (3)	0.0140 (2)	0.0248 (14)
O7	0.5415 (3)	0.5700 (2)	0.1852 (2)	0.0244 (13)
O8	0.4883 (3)	0.4512 (2)	0.2886 (2)	0.0216 (12)
O9	0.3831 (3)	0.2770 (2)	0.1667 (2)	0.0172 (11)
O10	0.5968 (3)	0.3900 (2)	0.1659 (2)	0.0168 (11)
O11	0.7750 (3)	0.4135 (2)	0.3246 (2)	0.0207 (12)
O12	0.6717 (3)	0.2411 (2)	0.2095 (2)	0.0178 (11)
O13	0.9058 (3)	0.3505 (3)	0.2219 (3)	0.0279 (14)
O14	0.8396 (3)	0.5127 (3)	0.2103 (3)	0.0300 (15)
O15	0.7127 (3)	0.3312 (2)	0.0753 (2)	0.0200 (12)
O16	0.5255 (3)	0.2839 (3)	−0.0866 (2)	0.0278 (14)
O17	0.4933 (3)	0.2145 (2)	0.0475 (2)	0.0204 (12)
O18	0.0803 (3)	0.3319 (3)	0.1124 (3)	0.0320 (16)
O19	0.2666 (3)	0.3344 (2)	0.2581 (2)	0.0220 (13)
O20	0.1304 (3)	0.1619 (3)	0.1169 (3)	0.0302 (15)
O21	0.4502 (3)	0.3767 (3)	0.4206 (2)	0.0269 (14)
O22	0.3380 (3)	0.1833 (2)	0.3152 (2)	0.0225 (13)
O23	0.5473 (3)	0.2849 (2)	0.2999 (2)	0.0183 (11)
O24	0.7375 (4)	0.3517 (3)	0.4661 (2)	0.0318 (15)
O25	0.6430 (3)	0.1530 (3)	0.3514 (2)	0.0244 (13)
O26	0.8596 (3)	0.2659 (3)	0.3768 (3)	0.0326 (16)
O27	0.4466 (3)	0.0978 (2)	0.1529 (2)	0.0236 (13)
O28	0.2440 (3)	−0.0133 (3)	0.1952 (2)	0.0284 (14)
O29	0.1203 (3)	0.0610 (3)	0.2882 (3)	0.0287 (15)
O30	0.3059 (3)	0.0801 (2)	0.4507 (2)	0.0181 (11)
O31	0.4383 (3)	0.0457 (2)	0.3650 (2)	0.0185 (11)
O32	0.7852 (3)	0.0859 (2)	0.6684 (2)	0.0212 (12)
O33	0.5254 (3)	0.2329 (3)	0.5108 (2)	0.0255 (13)
O34	0.4806 (3)	0.1136 (2)	0.6158 (2)	0.0200 (12)
O35	0.6030 (3)	0.0628 (2)	0.5022 (2)	0.0166 (11)
O36	0.9235 (3)	0.0487 (3)	0.5637 (3)	0.0313 (16)
O37	0.8354 (3)	0.2015 (3)	0.5621 (3)	0.0301 (15)
O38	0.7321 (3)	0.0195 (2)	0.4192 (2)	0.0199 (12)
O39	0.5488 (3)	−0.0410 (3)	0.2517 (2)	0.0273 (14)
O1w	0.6356 (5)	0.1282 (3)	−0.0883 (3)	0.049 (2)
O2w	0.3364 (6)	0.2032 (4)	0.7346 (4)	0.072 (3)
O3w	0.9070 (4)	0.0220 (4)	0.3469 (3)	0.058 (3)
O4w	0.3259 (5)	0.5541 (4)	0.3805 (4)	0.062 (3)
O5w	0.0931 (6)	0.4624 (5)	0.3786 (5)	0.095 (3)
O6w	0.0438 (9)	0.1717 (8)	0.7667 (7)	0.155 (6)
N1	0.8624 (4)	0.0250 (4)	0.1750 (3)	0.040 (2)
N2	0.7548 (4)	0.0513 (3)	0.0324 (3)	0.0333 (19)
N3	0.1441 (4)	0.3577 (4)	0.4954 (3)	0.038 (2)
N4	0.2270 (5)	0.2680 (4)	0.6006 (4)	0.041 (2)
N5	0.1652 (4)	0.7345 (3)	0.2214 (3)	0.0314 (18)
N6	0.1766 (4)	0.5803 (4)	0.1333 (3)	0.039 (2)
C1	0.8958 (6)	−0.0270 (4)	0.1009 (4)	0.046 (3)
C2	0.8160 (6)	−0.0218 (5)	0.0127 (4)	0.045 (3)
C3	0.7329 (7)	−0.0151 (7)	0.1538 (6)	0.076 (4)
C4	0.6688 (6)	0.0134 (5)	0.0734 (5)	0.047 (3)
C5	0.8963 (5)	0.1333 (4)	0.1830 (4)	0.036 (2)
C6	0.8431 (6)	0.1467 (4)	0.0923 (4)	0.042 (2)
C7	0.2757 (6)	0.4069 (5)	0.5393 (5)	0.045 (3)
C8	0.3254 (6)	0.3368 (5)	0.5856 (5)	0.043 (3)
C9	0.0873 (6)	0.3610 (4)	0.5656 (4)	0.037 (2)
C10	0.1576 (7)	0.3253 (5)	0.6393 (5)	0.050 (3)
C11	0.1189 (6)	0.2522 (5)	0.4454 (5)	0.052 (3)
C12	0.1450 (6)	0.1953 (5)	0.5127 (5)	0.048 (3)
C13	0.2889 (6)	0.7334 (5)	0.2532 (5)	0.050 (3)
C14	0.2968 (6)	0.6371 (5)	0.2002 (5)	0.046 (3)
C15	0.0833 (6)	0.6484 (4)	0.2338 (5)	0.045 (3)
C16	0.0915 (6)	0.5531 (4)	0.1800 (4)	0.040 (3)
C17	0.1283 (6)	0.7324 (5)	0.1261 (4)	0.043 (3)
C18	0.1367 (6)	0.6377 (5)	0.0712 (5)	0.047 (3)
H1	0.90068	0.014916	0.228745	0.0477*
H2	0.713278	0.061415	−0.020427	0.04*
H3	0.113319	0.390683	0.455632	0.0458*
H4	0.259328	0.235369	0.640034	0.0492*
H5	0.162046	0.792501	0.254619	0.0377*
H6	0.179833	0.522834	0.099284	0.047*
H7	0.883728	−0.096075	0.100705	0.0546*
H8	0.978245	0.006566	0.1096	0.0546*
H9	0.863931	−0.000335	−0.022679	0.0544*
H10	0.757395	−0.086715	−0.019507	0.0544*
H11	0.71248	0.012056	0.204867	0.0911*
H12	0.709345	−0.087072	0.140614	0.0911*
H13	0.606272	−0.0449	0.03058	0.0558*
H14	0.636313	0.065062	0.092638	0.0558*
H15	0.982426	0.160933	0.203266	0.0428*
H16	0.865215	0.165845	0.224967	0.0428*
H17	0.804073	0.197236	0.097674	0.0501*
H18	0.905428	0.166639	0.067615	0.0501*
H19	0.291447	0.468819	0.583578	0.0542*
H20	0.31064	0.417828	0.493792	0.0542*
H21	0.35691	0.299024	0.547422	0.0513*
H22	0.386936	0.374826	0.643061	0.0513*
H23	0.005762	0.316752	0.539593	0.0449*
H24	0.090903	0.428932	0.590205	0.0449*
H25	0.212324	0.382228	0.688631	0.0599*
H26	0.103191	0.281913	0.659262	0.0599*
H27	0.035518	0.224451	0.407506	0.0623*
H28	0.170023	0.24934	0.409748	0.0623*
H29	0.071375	0.160726	0.519416	0.0582*
H30	0.183618	0.148654	0.493142	0.0582*
H31	0.313096	0.736754	0.316669	0.0596*
H32	0.340631	0.789987	0.244056	0.0596*
H33	0.352708	0.652938	0.169147	0.0553*
H34	0.320902	0.598268	0.240772	0.0553*
H35	0.002365	0.650334	0.212039	0.0537*
H36	0.107055	0.650639	0.297052	0.0537*
H37	0.119845	0.515395	0.220375	0.0482*
H38	0.013699	0.514085	0.135906	0.0482*
H39	0.180382	0.790057	0.118523	0.0522*
H40	0.046706	0.733304	0.105896	0.0522*
H41	0.058756	0.598646	0.027298	0.0561*
H42	0.194311	0.655116	0.041899	0.0561*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.01580 (18)	0.01817 (18)	0.0225 (2)	0.00485 (14)	0.00681 (16)	0.00696 (15)
Mo2	0.01421 (17)	0.01238 (16)	0.02019 (19)	0.00386 (13)	0.00687 (15)	0.00489 (13)
Mo3	0.01457 (18)	0.01746 (18)	0.0230 (2)	0.00302 (14)	0.00833 (16)	0.00697 (15)
Mo4	0.01711 (18)	0.01583 (17)	0.01909 (19)	0.00618 (14)	0.00918 (15)	0.00713 (14)
Mo5	0.01552 (18)	0.01765 (18)	0.0279 (2)	0.00319 (14)	0.00980 (17)	0.00805 (15)
Mo6	0.01832 (19)	0.01529 (17)	0.02046 (19)	0.00559 (14)	0.01050 (16)	0.00655 (14)
Mo7	0.01560 (18)	0.01834 (18)	0.01871 (19)	0.00269 (14)	0.00569 (15)	0.00551 (14)
Mo8	0.01366 (17)	0.01222 (16)	0.01815 (18)	0.00368 (13)	0.00649 (14)	0.00443 (13)
Mo9	0.01405 (17)	0.01775 (18)	0.01901 (19)	0.00330 (13)	0.00595 (15)	0.00667 (14)
Mo10	0.01321 (17)	0.01381 (17)	0.01882 (18)	0.00385 (13)	0.00652 (14)	0.00507 (13)
Mo11	0.01324 (17)	0.01954 (18)	0.0219 (2)	0.00333 (13)	0.00701 (15)	0.00811 (15)
Mo12	0.01403 (17)	0.01682 (17)	0.01800 (18)	0.00478 (13)	0.00778 (14)	0.00653 (14)
O1	0.0243 (19)	0.030 (2)	0.038 (2)	0.0123 (15)	0.0139 (17)	0.0144 (17)
O2	0.0179 (16)	0.0142 (15)	0.0280 (18)	0.0048 (12)	0.0090 (14)	0.0066 (13)
O3	0.036 (2)	0.033 (2)	0.028 (2)	0.0089 (17)	0.0106 (18)	0.0074 (16)
O4	0.0244 (18)	0.0191 (16)	0.0239 (18)	0.0027 (13)	0.0079 (15)	0.0026 (13)
O5	0.0167 (16)	0.0207 (16)	0.0222 (17)	0.0072 (12)	0.0079 (13)	0.0080 (13)
O6	0.0213 (18)	0.0234 (18)	0.035 (2)	0.0073 (14)	0.0117 (16)	0.0154 (15)
O7	0.0240 (18)	0.0168 (16)	0.033 (2)	0.0058 (13)	0.0105 (16)	0.0093 (14)
O8	0.0248 (18)	0.0181 (16)	0.0225 (17)	0.0048 (13)	0.0105 (15)	0.0061 (13)
O9	0.0147 (15)	0.0169 (15)	0.0225 (16)	0.0066 (12)	0.0087 (13)	0.0057 (12)
O10	0.0139 (15)	0.0181 (15)	0.0210 (16)	0.0064 (12)	0.0078 (13)	0.0073 (12)
O11	0.0217 (17)	0.0152 (15)	0.0221 (17)	0.0011 (12)	0.0079 (14)	0.0039 (12)
O12	0.0140 (15)	0.0163 (15)	0.0251 (17)	0.0061 (12)	0.0088 (13)	0.0060 (12)
O13	0.0202 (18)	0.034 (2)	0.032 (2)	0.0101 (15)	0.0101 (16)	0.0090 (16)
O14	0.028 (2)	0.0222 (18)	0.040 (2)	0.0017 (15)	0.0152 (18)	0.0124 (16)
O15	0.0190 (16)	0.0210 (16)	0.0249 (17)	0.0077 (13)	0.0120 (14)	0.0090 (13)
O16	0.033 (2)	0.0287 (19)	0.0232 (18)	0.0095 (16)	0.0124 (16)	0.0080 (15)
O17	0.0220 (17)	0.0180 (16)	0.0225 (17)	0.0057 (13)	0.0102 (14)	0.0054 (13)
O18	0.0228 (19)	0.033 (2)	0.045 (2)	0.0123 (16)	0.0143 (18)	0.0128 (18)
O19	0.0218 (17)	0.0228 (17)	0.0286 (18)	0.0104 (14)	0.0155 (15)	0.0089 (14)
O20	0.030 (2)	0.0213 (18)	0.041 (2)	0.0022 (15)	0.0191 (18)	0.0095 (16)
O21	0.035 (2)	0.0249 (18)	0.0235 (18)	0.0109 (15)	0.0135 (16)	0.0047 (14)
O22	0.0206 (17)	0.0202 (16)	0.0308 (19)	0.0060 (13)	0.0119 (15)	0.0125 (14)
O23	0.0159 (15)	0.0200 (16)	0.0191 (16)	0.0043 (12)	0.0068 (13)	0.0062 (12)
O24	0.037 (2)	0.030 (2)	0.0228 (19)	0.0029 (17)	0.0115 (17)	0.0024 (15)
O25	0.0198 (17)	0.0237 (17)	0.035 (2)	0.0066 (14)	0.0119 (15)	0.0169 (15)
O26	0.0217 (19)	0.039 (2)	0.040 (2)	0.0125 (17)	0.0084 (17)	0.0175 (18)
O27	0.0228 (18)	0.0166 (15)	0.0284 (19)	0.0018 (13)	0.0087 (15)	0.0056 (13)
O28	0.033 (2)	0.0264 (18)	0.0224 (18)	0.0041 (15)	0.0107 (16)	0.0048 (14)
O29	0.0204 (18)	0.034 (2)	0.041 (2)	0.0139 (16)	0.0131 (17)	0.0200 (17)
O30	0.0163 (15)	0.0228 (16)	0.0178 (16)	0.0084 (13)	0.0073 (13)	0.0068 (12)
O31	0.0154 (15)	0.0203 (16)	0.0203 (16)	0.0052 (12)	0.0068 (13)	0.0061 (12)
O32	0.0226 (17)	0.0164 (15)	0.0239 (17)	0.0029 (13)	0.0097 (14)	0.0062 (13)
O33	0.0245 (18)	0.0197 (16)	0.032 (2)	0.0037 (14)	0.0108 (16)	0.0102 (14)
O34	0.0170 (16)	0.0217 (16)	0.0181 (16)	0.0021 (12)	0.0071 (13)	0.0024 (12)
O35	0.0151 (15)	0.0177 (15)	0.0163 (15)	0.0040 (11)	0.0056 (12)	0.0043 (12)
O36	0.0201 (18)	0.047 (2)	0.036 (2)	0.0154 (17)	0.0142 (17)	0.0196 (18)
O37	0.031 (2)	0.0240 (18)	0.032 (2)	0.0004 (15)	0.0105 (17)	0.0108 (15)
O38	0.0172 (16)	0.0245 (17)	0.0220 (17)	0.0085 (13)	0.0107 (14)	0.0072 (13)
O39	0.029 (2)	0.0315 (19)	0.0225 (18)	0.0103 (16)	0.0096 (16)	0.0070 (15)
O1w	0.059 (3)	0.035 (2)	0.042 (3)	0.024 (2)	−0.003 (2)	0.001 (2)
O2w	0.084 (4)	0.047 (3)	0.062 (4)	0.032 (3)	−0.006 (3)	−0.001 (3)
O3w	0.045 (3)	0.110 (4)	0.041 (3)	0.044 (3)	0.022 (2)	0.032 (3)
O4w	0.071 (4)	0.048 (3)	0.063 (4)	0.018 (3)	0.027 (3)	0.003 (3)
O5w	0.070 (4)	0.085 (5)	0.088 (5)	−0.011 (3)	−0.018 (4)	0.045 (4)
O6w	0.127 (8)	0.147 (9)	0.149 (9)	0.028 (7)	0.018 (7)	0.010 (7)
N1	0.036 (3)	0.051 (3)	0.029 (3)	0.007 (2)	0.006 (2)	0.021 (2)
N2	0.028 (2)	0.035 (3)	0.033 (3)	0.014 (2)	0.003 (2)	0.008 (2)
N3	0.031 (3)	0.045 (3)	0.038 (3)	0.013 (2)	0.011 (2)	0.009 (2)
N4	0.040 (3)	0.037 (3)	0.051 (3)	0.015 (2)	0.017 (3)	0.015 (2)
N5	0.033 (3)	0.018 (2)	0.037 (3)	0.0040 (17)	0.012 (2)	−0.0021 (18)
N6	0.039 (3)	0.028 (2)	0.047 (3)	0.006 (2)	0.024 (3)	−0.005 (2)
C1	0.043 (4)	0.030 (3)	0.049 (4)	0.019 (3)	−0.003 (3)	−0.003 (3)
C2	0.047 (4)	0.051 (4)	0.036 (3)	0.026 (3)	0.015 (3)	−0.004 (3)
C3	0.041 (5)	0.111 (8)	0.061 (5)	−0.011 (5)	0.021 (4)	0.030 (5)
C4	0.021 (3)	0.053 (4)	0.058 (4)	0.005 (3)	0.015 (3)	0.005 (3)
C5	0.031 (3)	0.029 (3)	0.036 (3)	0.008 (2)	0.006 (3)	−0.003 (2)
C6	0.035 (3)	0.028 (3)	0.049 (4)	0.005 (2)	0.000 (3)	0.008 (3)
C7	0.033 (3)	0.039 (4)	0.067 (5)	0.009 (3)	0.025 (3)	0.013 (3)
C8	0.027 (3)	0.038 (3)	0.051 (4)	0.007 (3)	0.004 (3)	0.004 (3)
C9	0.033 (3)	0.034 (3)	0.042 (3)	0.011 (2)	0.017 (3)	−0.003 (3)
C10	0.062 (5)	0.058 (5)	0.048 (4)	0.034 (4)	0.032 (4)	0.017 (3)
C11	0.040 (4)	0.047 (4)	0.049 (4)	0.013 (3)	0.005 (3)	−0.015 (3)
C12	0.033 (3)	0.026 (3)	0.076 (5)	0.003 (2)	0.019 (3)	−0.003 (3)
C13	0.029 (3)	0.042 (4)	0.054 (4)	0.002 (3)	−0.004 (3)	−0.002 (3)
C14	0.037 (4)	0.051 (4)	0.060 (5)	0.020 (3)	0.024 (3)	0.017 (3)
C15	0.051 (4)	0.035 (3)	0.051 (4)	0.005 (3)	0.035 (4)	0.002 (3)
C16	0.046 (4)	0.024 (3)	0.048 (4)	0.000 (2)	0.028 (3)	0.001 (2)
C17	0.041 (4)	0.042 (4)	0.042 (4)	0.005 (3)	0.012 (3)	0.014 (3)
C18	0.039 (4)	0.049 (4)	0.040 (4)	0.003 (3)	0.018 (3)	−0.006 (3)

Bond lengths (Å) top

Mo1—O1	1.722 (5)	Mo7—O12	2.284 (3)
Mo1—O2	2.295 (4)	Mo7—O23	2.170 (3)
Mo1—O3	1.685 (4)	Mo7—O24	1.685 (4)
Mo1—O4	1.874 (4)	Mo7—O25	2.045 (4)
Mo1—O5	2.075 (3)	Mo7—O26	1.697 (5)
Mo1—O6ⁱ	2.094 (4)	Mo8—O9	1.959 (4)
Mo2—O2	1.869 (3)	Mo8—O10	2.419 (3)
Mo2—O5	2.156 (3)	Mo8—O12	1.854 (3)
Mo2—O7	1.689 (3)	Mo8—O17	1.767 (4)
Mo2—O8	1.760 (4)	Mo8—O23	2.138 (3)
Mo2—O9	2.425 (3)	Mo8—O27	1.687 (3)
Mo2—O10	1.936 (4)	Mo9—O22	2.014 (3)
Mo3—O10	2.226 (3)	Mo9—O28	1.687 (4)
Mo3—O11	1.916 (4)	Mo9—O29	1.701 (4)
Mo3—O12	2.303 (3)	Mo9—O30	2.241 (3)
Mo3—O13	1.702 (4)	Mo9—O31	2.200 (3)
Mo3—O14	1.686 (4)	Mo9—O32ⁱⁱ	1.953 (4)
Mo3—O15	1.976 (3)	Mo10—O30	1.865 (3)
Mo4—O5	1.913 (4)	Mo10—O31	2.150 (3)
Mo4—O6	1.758 (4)	Mo10—O33	1.686 (4)
Mo4—O10	2.218 (4)	Mo10—O34	1.760 (4)
Mo4—O15	1.874 (4)	Mo10—O35	1.939 (4)
Mo4—O16	1.697 (3)	Mo10—O35ⁱⁱ	2.427 (3)
Mo4—O17	2.221 (4)	Mo11—O30ⁱⁱ	2.300 (3)
Mo5—O2	2.273 (3)	Mo11—O32	1.926 (4)
Mo5—O4	1.952 (4)	Mo11—O35	2.210 (3)
Mo5—O9	2.259 (4)	Mo11—O36	1.706 (5)
Mo5—O18	1.700 (5)	Mo11—O37	1.695 (4)
Mo5—O19	1.957 (3)	Mo11—O38	1.964 (3)
Mo5—O20	1.694 (4)	Mo12—O25	1.760 (4)
Mo6—O8	2.236 (4)	Mo12—O31	1.880 (4)
Mo6—O9	2.238 (4)	Mo12—O34ⁱⁱ	2.218 (4)
Mo6—O19	1.888 (4)	Mo12—O35	2.225 (3)
Mo6—O21	1.691 (4)	Mo12—O38	1.896 (4)
Mo6—O22	1.792 (4)	Mo12—O39	1.697 (4)
Mo6—O23	1.888 (4)	C2—O20ⁱⁱⁱ	2.953 (9)
Mo7—O11	1.904 (4)

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

(II) top

Crystal data top

C₁₂H_37.32Mo₈N₄O_30.66	V = 878.20 (9) Å³
M_r = 1495.8	Z = 1
Triclinic, P1(αβγ)0†	F(000) = 709
q = 0.06330a* + -0.42840b* + -0.41590c*	D_x = 2.828 Mg m⁻³
a = 7.8907 (5) Å	Mo Kα radiation, λ = 0.71069 Å
b = 10.0855 (3) Å	µ = 2.87 mm⁻¹
c = 12.4131 (8) Å	T = 293 K
α = 113.685 (4)°	Elongated block, colorless
β = 92.857 (7)°	0.24 × 0.10 × 0.08 mm
γ = 101.244 (5)°

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) −x₁, −x₂, −x₃, −x₄.

Data collection top

Nonius CCD diffractometer	R_int = 0.064
Absorption correction: gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000)	θ_max = 35.9°, θ_min = 5.0°
T_min = 0.649, T_max = 0.826	h = −13→12
153057 measured reflections	k = −16→16
39145 independent reflections	l = −20→20
21512 reflections with I > 2σ(I)

Refinement top

Refinement on F²	Const
R[F² > 2σ(F²)] = 0.052	Weighting scheme based on measured s.u.'s w = 1/(σ²(I) + 0.001936I²)
wR(F²) = 0.133	(Δ/σ)_max = 0.002
S = 1.34	Δρ_max = 2.11 e Å⁻³
39145 reflections	Δρ_min = −1.88 e Å⁻³
566 parameters

Crystal data top

C₁₂H_37.32Mo₈N₄O_30.66	β = 92.857 (7)°
M_r = 1495.8	γ = 101.244 (5)°
Triclinic, P1(αβγ)0†	V = 878.20 (9) Å³
q = 0.06330a* + -0.42840b* + -0.41590c*	Z = 1
a = 7.8907 (5) Å	Mo Kα radiation
b = 10.0855 (3) Å	µ = 2.87 mm⁻¹
c = 12.4131 (8) Å	T = 293 K
α = 113.685 (4)°	0.24 × 0.10 × 0.08 mm

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) −x₁, −x₂, −x₃, −x₄.

Data collection top

Nonius CCD diffractometer	39145 independent reflections
Absorption correction: gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000)	21512 reflections with I > 2σ(I)
T_min = 0.649, T_max = 0.826	R_int = 0.064
153057 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.052	566 parameters
wR(F²) = 0.133	Const
S = 1.34	Δρ_max = 2.11 e Å⁻³
39145 reflections	Δρ_min = −1.88 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mo1	0.01475 (2)	0.10641 (2)	0.793165 (14)	0.01834 (6)
Mo2	0.41800 (2)	0.149828 (18)	0.739826 (14)	0.01804 (5)
Mo3	0.304037 (18)	0.117739 (17)	0.419560 (14)	0.01527 (5)
Mo4	−0.114145 (19)	0.118717 (16)	0.480196 (13)	0.01409 (5)
O1	−0.06329 (17)	0.05779 (15)	0.60558 (12)	0.0165 (4)
O2	−0.1051 (2)	0.2348 (2)	0.84722 (16)	0.0333 (6)
O3	−0.17194 (18)	−0.08043 (17)	0.72417 (13)	0.0206 (5)
O4	0.0839 (2)	0.0760 (2)	0.91185 (15)	0.0317 (6)
O5	0.18520 (18)	−0.04563 (16)	0.68331 (12)	0.0185 (4)
O6	0.22161 (19)	0.23677 (16)	0.78452 (13)	0.0218 (5)
O7	0.4736 (2)	0.1296 (2)	0.86514 (15)	0.0343 (7)
O8	0.55103 (18)	−0.00333 (17)	0.64663 (13)	0.0233 (5)
O9	0.5569 (2)	0.30712 (19)	0.75102 (17)	0.0328 (6)
O10	0.30421 (17)	0.08414 (15)	0.55868 (12)	0.0179 (4)
O11	0.4254 (2)	0.29384 (18)	0.46168 (15)	0.0260 (5)
O12	0.09476 (18)	0.23147 (16)	0.49390 (13)	0.0205 (5)
O13	−0.2353 (2)	0.24376 (18)	0.54182 (15)	0.0258 (5)
O1w	0.2991 (6)	0.4617 (3)	0.3448 (4)	0.0890 (17)	0.932 (3)
O2w	0.3184 (6)	0.1670 (7)	0.1090 (4)	0.0745 (18)	0.855 (4)
O3w	0.2867 (14)	0.4379 (9)	0.0478 (7)	0.129 (5)	0.554 (16)
N1a	0.0186 (3)	0.6031 (3)	0.7674 (3)	0.0327 (8)	0.487
N2a	0.3348 (6)	0.7035 (6)	0.8312 (5)	0.049 (5)	0.487
C1a	0.0534 (7)	0.7570 (6)	0.8508 (5)	0.0447 (17)	0.487
C2a	0.1028 (7)	0.5898 (6)	0.6645 (5)	0.049 (2)	0.487
C3a	0.0843 (7)	0.5154 (7)	0.8242 (6)	0.0554 (19)	0.487
C4a	0.2446 (7)	0.8174 (6)	0.8873 (5)	0.049 (4)	0.487
C5a	0.2949 (8)	0.6500 (8)	0.7027 (6)	0.067 (5)	0.487
C6a	0.2787 (7)	0.5790 (7)	0.8664 (6)	0.062 (5)	0.487
H1a	−0.1000 (3)	0.5690 (3)	0.7435 (3)	0.0481 (15)	0.487
H2a	0.4527 (3)	0.7440 (3)	0.8547 (3)	0.076 (9)	0.487
H3a	−0.0027 (3)	0.7650 (3)	0.9203 (3)	0.074 (3)	0.487
H4a	0.0075 (3)	0.8137 (3)	0.8140 (3)	0.065 (3)	0.487
H5a	0.0585 (3)	0.6464 (3)	0.6269 (3)	0.066 (3)	0.487
H6a	0.0798 (3)	0.4857 (3)	0.6091 (3)	0.075 (3)	0.487
H7a	0.0642 (3)	0.4124 (3)	0.7669 (3)	0.082 (3)	0.487
H8a	0.0241 (3)	0.5213 (3)	0.8916 (3)	0.083 (3)	0.487
H9a	0.2824 (3)	0.8988 (3)	0.8646 (3)	0.073 (5)	0.487
H10a	0.2714 (3)	0.8547 (3)	0.9729 (3)	0.072 (5)	0.487
H11a	0.3551 (3)	0.5721 (3)	0.6636 (3)	0.106 (8)	0.487
H12a	0.3342 (3)	0.7315 (3)	0.6804 (3)	0.095 (7)	0.487
H13a	0.3006 (3)	0.6165 (3)	0.9522 (3)	0.084 (6)	0.487
H14a	0.3412 (3)	0.5023 (3)	0.8286 (3)	0.098 (7)	0.487
N1b	0.2228 (8)	0.5251 (4)	0.8063 (4)	0.087 (3)	0.513
N2b	0.2257 (11)	0.7672 (6)	0.8018 (6)	0.068 (18)	0.513
C1b	0.2981 (11)	0.5322 (7)	0.7048 (6)	0.149 (8)	0.513
C2b	0.3241 (11)	0.6415 (7)	0.9140 (6)	0.256 (10)	0.513
C3b	0.0412 (12)	0.5424 (7)	0.7988 (7)	0.306 (11)	0.513
C4b	0.3020 (11)	0.6795 (7)	0.7040 (6)	0.158 (17)	0.513
C5b	0.3256 (13)	0.7887 (7)	0.9120 (7)	0.29 (2)	0.513
C6b	0.0414 (13)	0.6900 (7)	0.7931 (7)	0.22 (2)	0.513
H1b	0.2259 (8)	0.4347 (4)	0.8070 (4)	0.128 (5)	0.513
H2b	0.2307 (8)	0.8579 (4)	0.7995 (4)	0.10 (3)	0.513
H3b	0.2284 (8)	0.4541 (4)	0.6326 (4)	0.341 (13)	0.513
H4b	0.4160 (8)	0.5183 (4)	0.7090 (4)	0.272 (16)	0.513
H5b	0.4428 (8)	0.6293 (4)	0.9192 (4)	0.375 (18)	0.513
H6b	0.2720 (8)	0.6368 (4)	0.9819 (4)	0.505 (13)	0.513
H7b	−0.0077 (8)	0.5410 (4)	0.8686 (4)	0.567 (17)	0.513
H8b	−0.0280 (8)	0.4616 (4)	0.7277 (4)	0.51 (2)	0.513
H9b	0.4219 (8)	0.7308 (4)	0.7097 (4)	0.35 (3)	0.513
H10b	0.2373 (8)	0.6655 (4)	0.6302 (4)	0.31 (2)	0.513
H11b	0.2745 (8)	0.8479 (4)	0.9791 (4)	0.54 (3)	0.513
H12b	0.4450 (8)	0.8411 (4)	0.9177 (4)	0.50 (4)	0.513
H13b	−0.0227 (8)	0.6719 (4)	0.7179 (4)	0.34 (3)	0.513
H14b	−0.0101 (8)	0.7505 (4)	0.8594 (4)	0.42 (3)	0.513

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.01765 (7)	0.02411 (8)	0.01514 (7)	0.00836 (6)	0.00484 (5)	0.00828 (6)
Mo2	0.01580 (7)	0.02150 (7)	0.01672 (7)	0.00599 (5)	0.00213 (5)	0.00724 (6)
Mo3	0.01236 (6)	0.01932 (7)	0.01823 (7)	0.00569 (5)	0.00447 (5)	0.01086 (6)
Mo4	0.01378 (6)	0.01632 (6)	0.01532 (7)	0.00663 (5)	0.00372 (5)	0.00822 (5)
O1	0.0160 (5)	0.0198 (5)	0.0162 (5)	0.0059 (4)	0.0029 (4)	0.0093 (4)
O2	0.0317 (8)	0.0347 (8)	0.0328 (9)	0.0180 (7)	0.0112 (7)	0.0079 (7)
O3	0.0180 (6)	0.0297 (7)	0.0203 (6)	0.0068 (5)	0.0041 (5)	0.0159 (5)
O4	0.0331 (8)	0.0440 (9)	0.0226 (7)	0.0111 (7)	0.0048 (6)	0.0176 (7)
O5	0.0185 (6)	0.0244 (6)	0.0176 (6)	0.0089 (5)	0.0042 (5)	0.0118 (5)
O6	0.0194 (6)	0.0212 (6)	0.0235 (7)	0.0084 (5)	0.0053 (5)	0.0063 (5)
O7	0.0341 (9)	0.0518 (10)	0.0235 (8)	0.0176 (8)	0.0022 (6)	0.0191 (7)
O8	0.0188 (6)	0.0308 (7)	0.0251 (7)	0.0140 (5)	0.0075 (5)	0.0124 (6)
O9	0.0246 (7)	0.0270 (7)	0.0414 (9)	0.0020 (6)	0.0044 (7)	0.0108 (7)
O10	0.0156 (5)	0.0216 (6)	0.0181 (6)	0.0044 (4)	0.0023 (4)	0.0100 (5)
O11	0.0210 (6)	0.0239 (6)	0.0352 (8)	0.0028 (5)	0.0051 (6)	0.0155 (6)
O12	0.0172 (6)	0.0201 (6)	0.0266 (7)	0.0062 (5)	0.0058 (5)	0.0110 (5)
O13	0.0269 (7)	0.0267 (7)	0.0282 (7)	0.0167 (6)	0.0080 (6)	0.0108 (6)
O1w	0.096 (3)	0.0367 (13)	0.114 (3)	0.0113 (15)	−0.036 (2)	0.0194 (16)
O2w	0.0485 (17)	0.120 (3)	0.0554 (18)	−0.0029 (19)	−0.0035 (14)	0.048 (2)
O3w	0.169 (10)	0.092 (6)	0.077 (5)	−0.019 (5)	−0.014 (5)	0.013 (4)
N1a	0.0295 (9)	0.0334 (10)	0.0397 (12)	0.0061 (8)	0.0042 (8)	0.0205 (9)
N2a	0.0284 (11)	0.060 (8)	0.065 (9)	0.006 (2)	0.005 (2)	0.037 (7)
C1a	0.043 (4)	0.0424 (12)	0.044 (2)	0.019 (2)	0.002 (2)	0.0094 (13)
C2a	0.057 (3)	0.053 (4)	0.032 (2)	0.009 (3)	0.009 (2)	0.016 (2)
C3a	0.051 (2)	0.052 (3)	0.081 (3)	0.001 (2)	−0.0018 (18)	0.052 (2)
C4a	0.050 (5)	0.039 (4)	0.050 (6)	0.001 (4)	−0.012 (4)	0.017 (4)
C5a	0.0504 (19)	0.094 (8)	0.060 (8)	0.013 (3)	0.030 (3)	0.036 (7)
C6a	0.049 (2)	0.064 (8)	0.093 (6)	0.015 (3)	−0.008 (3)	0.054 (6)
H1a	0.0309 (9)	0.050 (2)	0.063 (2)	0.0024 (10)	−0.0015 (10)	0.0273 (18)
H2a	0.0292 (13)	0.096 (13)	0.107 (15)	0.000 (3)	0.000 (4)	0.056 (12)
H3a	0.060 (7)	0.095 (3)	0.051 (2)	0.034 (4)	0.020 (3)	0.0075 (19)
H4a	0.065 (5)	0.0394 (16)	0.081 (4)	0.026 (2)	−0.016 (3)	0.0125 (19)
H5a	0.083 (4)	0.078 (5)	0.040 (3)	0.000 (4)	−0.007 (3)	0.036 (3)
H6a	0.088 (6)	0.066 (4)	0.046 (2)	0.021 (5)	0.009 (3)	−0.003 (2)
H7a	0.080 (4)	0.042 (2)	0.132 (5)	0.002 (3)	−0.017 (3)	0.053 (3)
H8a	0.070 (4)	0.111 (4)	0.098 (3)	−0.012 (4)	0.004 (3)	0.089 (3)
H9a	0.075 (6)	0.040 (4)	0.093 (10)	−0.014 (4)	−0.030 (6)	0.033 (5)
H10a	0.076 (9)	0.065 (5)	0.049 (6)	0.005 (6)	−0.021 (6)	0.007 (4)
H11a	0.071 (4)	0.143 (12)	0.095 (11)	0.043 (7)	0.053 (6)	0.029 (10)
H12a	0.074 (3)	0.142 (11)	0.082 (12)	−0.009 (5)	0.031 (5)	0.074 (10)
H13a	0.074 (4)	0.103 (11)	0.099 (7)	0.006 (6)	−0.025 (4)	0.079 (7)
H14a	0.070 (3)	0.078 (11)	0.161 (11)	0.038 (5)	−0.013 (4)	0.060 (9)
N1b	0.141 (6)	0.0365 (17)	0.112 (3)	0.043 (3)	0.061 (3)	0.044 (2)
N2b	0.11 (4)	0.038 (6)	0.067 (19)	0.027 (14)	0.01 (2)	0.034 (9)
C1b	0.303 (14)	0.140 (10)	0.099 (10)	0.175 (9)	0.117 (10)	0.080 (9)
C2b	0.61 (2)	0.081 (7)	0.074 (8)	0.128 (11)	−0.082 (10)	0.024 (6)
C3b	0.15 (3)	0.180 (8)	0.762 (12)	0.093 (12)	0.207 (13)	0.331 (8)
C4b	0.25 (3)	0.204 (16)	0.19 (2)	0.194 (18)	0.17 (2)	0.177 (16)
C5b	0.62 (5)	0.041 (9)	0.14 (2)	0.070 (18)	−0.20 (2)	−0.008 (12)
C6b	0.13 (5)	0.154 (8)	0.523 (18)	0.097 (17)	0.17 (2)	0.241 (10)
H1b	0.177 (12)	0.052 (2)	0.207 (5)	0.060 (4)	0.094 (6)	0.083 (3)
H2b	0.13 (7)	0.059 (10)	0.14 (3)	0.03 (2)	0.01 (4)	0.072 (16)
H3b	0.79 (2)	0.180 (17)	0.066 (10)	0.310 (16)	0.005 (11)	−0.016 (11)
H4b	0.36 (3)	0.314 (17)	0.46 (2)	0.306 (16)	0.34 (2)	0.346 (17)
H5b	0.56 (4)	0.108 (13)	0.381 (16)	0.01 (2)	−0.349 (18)	0.104 (12)
H6b	1.35 (3)	0.260 (16)	0.083 (9)	0.481 (18)	0.181 (12)	0.115 (10)
H7b	0.51 (3)	0.462 (16)	1.30 (2)	0.415 (18)	0.73 (2)	0.741 (17)
H8b	0.14 (5)	0.178 (13)	1.241 (19)	−0.06 (2)	−0.13 (2)	0.378 (13)
H9b	0.28 (5)	0.42 (3)	0.79 (4)	0.31 (3)	0.40 (4)	0.56 (3)
H10b	0.70 (5)	0.32 (3)	0.10 (2)	0.40 (3)	0.19 (2)	0.15 (2)
H11b	1.40 (7)	0.143 (16)	0.07 (3)	0.37 (3)	−0.08 (3)	−0.027 (18)
H12b	0.58 (8)	0.073 (16)	0.67 (4)	−0.09 (3)	−0.54 (4)	0.13 (2)
H13b	0.10 (7)	0.174 (15)	0.77 (2)	0.00 (3)	−0.11 (3)	0.253 (14)
H14b	0.48 (7)	0.363 (15)	0.88 (3)	0.38 (3)	0.59 (3)	0.522 (18)

Bond lengths (Å) top

	Average	Minimum	Maximum
O1w—O9ⁱ	3.073 (16)	2.924 (16)	3.232 (17)
O1w—O11	2.918 (17)	2.885 (16)	2.960 (17)
O1w—O11ⁱ	3.031 (12)	2.888 (12)	3.191 (12)
O1w—O13ⁱⁱ	2.905 (12)	2.823 (12)	2.951 (13)
O1w—O2w	3.341 (19)	3.068 (19)	3.502 (18)
O1w—O3w	3.56 (2)	3.11 (2)	4.15 (2)
O2w—O3ⁱⁱⁱ	2.770 (19)	2.662 (18)	3.00 (2)
O2w—O4^iv	2.753 (16)	2.595 (14)	2.867 (15)
O2w—O7^iv	3.222 (17)	3.046 (19)	3.459 (17)
O2w—O3w	3.26 (3)	2.75 (3)	3.49 (3)
O3w—O6^iv	3.028 (12)	2.970 (12)	3.075 (12)
O3w—O9ⁱ	2.787 (12)	2.755 (11)	2.840 (12)

Symmetry codes: (i) −x₁+1, −x₂+1, −x₃+1, −x₄; (ii) −x₁, −x₂+1, −x₃+1, −x₄; (iii) −x₁, −x₂, −x₃+1, −x₄; (iv) x₁, x₂, x₃−1, x₄.

Experimental details

	(I)	(II)
Crystal data
Chemical formula	(C₆H₁₄N₂)₂[Mo₈O₂₆]·4H₂O	C₁₂H_37.32Mo₈N₄O_30.66
M_r	1483.9	1495.8
Crystal system, space group	Triclinic, P1	Triclinic, P1(αβγ)0†
Temperature (K)	293	293
a, b, c (Å)	12.3378 (15), 14.417 (2), 16.1439 (16)	?
α, β, γ (°)	100.927 (9), 106.487 (8), 104.11 (1)	7.8907 (5), 10.0855 (3), 12.4131 (8)
V (Å³)	2565.0 (6)	113.685 (4), 92.857 (7), 101.244 (5)
Z	3	878.20 (9)
Radiation type	Mo Kα	?
µ (mm⁻¹)	2.95	?
Crystal size (mm)	0.18 × 0.10 × 0.08	Colorless

Data collection
Diffractometer	Nonius CCD diffractometer	Nonius CCD diffractometer
Absorption correction	Gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000)	Gaussian (Jana2000; Petricek, Dusek & Palatinus, 2000)
T_min, T_max	0.595, 0.833	0.649, 0.826
No. of measured, independent and observed [I > 2σ(I)] reflections	90290, 21895, 14316	153057, 39145, 21512
R_int	0.068	0.064
(sin θ/λ)_max (Å⁻¹)	0.807	0.826

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.058, 0.135, 1.43	0.052, 0.133, 1.34
No. of reflections	21895	39145
No. of parameters	730	566
No. of restraints	?	?
H-atom treatment	H-atom parameters constrained	Const
Δρ_max, Δρ_min (e Å⁻³)	1.61, −1.89	2.11, −1.88

† Symmetry operations: (1) x₁, x₂, x₃, x₄; (2) −x₁, −x₂, −x₃, −x₄.

Computer programs: (Jana2000; Petricek and Dusek, 2000).

Selected bond lengths (Å) for (I) top

Mo1—O1	1.722 (5)	Mo7—O12	2.284 (3)
Mo1—O2	2.295 (4)	Mo7—O23	2.170 (3)
Mo1—O3	1.685 (4)	Mo7—O24	1.685 (4)
Mo1—O4	1.874 (4)	Mo7—O25	2.045 (4)
Mo1—O5	2.075 (3)	Mo7—O26	1.697 (5)
Mo1—O6ⁱ	2.094 (4)	Mo8—O9	1.959 (4)
Mo2—O2	1.869 (3)	Mo8—O10	2.419 (3)
Mo2—O5	2.156 (3)	Mo8—O12	1.854 (3)
Mo2—O7	1.689 (3)	Mo8—O17	1.767 (4)
Mo2—O8	1.760 (4)	Mo8—O23	2.138 (3)
Mo2—O9	2.425 (3)	Mo8—O27	1.687 (3)
Mo2—O10	1.936 (4)	Mo9—O22	2.014 (3)
Mo3—O10	2.226 (3)	Mo9—O28	1.687 (4)
Mo3—O11	1.916 (4)	Mo9—O29	1.701 (4)
Mo3—O12	2.303 (3)	Mo9—O30	2.241 (3)
Mo3—O13	1.702 (4)	Mo9—O31	2.200 (3)
Mo3—O14	1.686 (4)	Mo9—O32ⁱⁱ	1.953 (4)
Mo3—O15	1.976 (3)	Mo10—O30	1.865 (3)
Mo4—O5	1.913 (4)	Mo10—O31	2.150 (3)
Mo4—O6	1.758 (4)	Mo10—O33	1.686 (4)
Mo4—O10	2.218 (4)	Mo10—O34	1.760 (4)
Mo4—O15	1.874 (4)	Mo10—O35	1.939 (4)
Mo4—O16	1.697 (3)	Mo10—O35ⁱⁱ	2.427 (3)
Mo4—O17	2.221 (4)	Mo11—O30ⁱⁱ	2.300 (3)
Mo5—O2	2.273 (3)	Mo11—O32	1.926 (4)
Mo5—O4	1.952 (4)	Mo11—O35	2.210 (3)
Mo5—O9	2.259 (4)	Mo11—O36	1.706 (5)
Mo5—O18	1.700 (5)	Mo11—O37	1.695 (4)
Mo5—O19	1.957 (3)	Mo11—O38	1.964 (3)
Mo5—O20	1.694 (4)	Mo12—O25	1.760 (4)
Mo6—O8	2.236 (4)	Mo12—O31	1.880 (4)
Mo6—O9	2.238 (4)	Mo12—O34ⁱⁱ	2.218 (4)
Mo6—O19	1.888 (4)	Mo12—O35	2.225 (3)
Mo6—O21	1.691 (4)	Mo12—O38	1.896 (4)
Mo6—O22	1.792 (4)	Mo12—O39	1.697 (4)
Mo6—O23	1.888 (4)	C2—O20ⁱⁱⁱ	2.953 (9)
Mo7—O11	1.904 (4)

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

Selected bond lengths (Å) for (II) top

	Average	Minimum	Maximum
O1w—O9ⁱ	3.073 (16)	2.924 (16)	3.232 (17)
O1w—O11	2.918 (17)	2.885 (16)	2.960 (17)
O1w—O11ⁱ	3.031 (12)	2.888 (12)	3.191 (12)
O1w—O13ⁱⁱ	2.905 (12)	2.823 (12)	2.951 (13)
O1w—O2w	3.341 (19)	3.068 (19)	3.502 (18)
O1w—O3w	3.56 (2)	3.11 (2)	4.15 (2)
O2w—O3ⁱⁱⁱ	2.770 (19)	2.662 (18)	3.00 (2)
O2w—O4^iv	2.753 (16)	2.595 (14)	2.867 (15)
O2w—O7^iv	3.222 (17)	3.046 (19)	3.459 (17)
O2w—O3w	3.26 (3)	2.75 (3)	3.49 (3)
O3w—O6^iv	3.028 (12)	2.970 (12)	3.075 (12)
O3w—O9ⁱ	2.787 (12)	2.755 (11)	2.840 (12)

Symmetry codes: (i) −x₁+1, −x₂+1, −x₃+1, −x₄; (ii) −x₁, −x₂+1, −x₃+1, −x₄; (iii) −x₁, −x₂, −x₃+1, −x₄; (iv) x₁, x₂, x₃−1, x₄.

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