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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768106025791/sn5039sup1.cif
Contains datablocks global, (I), (II)

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768106025791/sn5039Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768106025791/sn5039IIsup3.hkl
Contains datablock II

pdf

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
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(I) top
Crystal data top
(C6H14N2)2[Mo8O26]·4H2OV = 2565.0 (6) Å3
Mr = 1483.9Z = 3
Triclinic, P1F(000) = 2112
Hall symbol: -P 1Dx = 2.881 Mg m3
a = 12.3378 (15) ÅMo Kα radiation, λ = 0.71069 Å
b = 14.417 (2) ŵ = 2.95 mm1
c = 16.1439 (16) ÅT = 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
Rint = 0.068
Absorption correction: gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
θmax = 35.0°, θmin = 6.4°
Tmin = 0.595, Tmax = 0.833h = 1919
90290 measured reflectionsk = 2322
21895 independent reflectionsl = 2626
14316 reflections with I > 2σ(I)
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.058Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.001936I2)
wR(F2) = 0.135(Δ/σ)max = 0.001
S = 1.43Δρmax = 1.61 e Å3
21895 reflectionsΔρmin = 1.89 e Å3
730 parameters
Crystal data top
(C6H14N2)2[Mo8O26]·4H2Oγ = 104.11 (1)°
Mr = 1483.9V = 2565.0 (6) Å3
Triclinic, P1Z = 3
a = 12.3378 (15) ÅMo Kα radiation
b = 14.417 (2) ŵ = 2.95 mm1
c = 16.1439 (16) ÅT = 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)
Tmin = 0.595, Tmax = 0.833Rint = 0.068
90290 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.058730 parameters
wR(F2) = 0.135H-atom parameters constrained
S = 1.43Δρmax = 1.61 e Å3
21895 reflectionsΔρmin = 1.89 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo10.25888 (4)0.37951 (3)0.02610 (3)0.01868 (14)
Mo20.47524 (3)0.44973 (3)0.17692 (3)0.01540 (13)
Mo30.78573 (4)0.39209 (3)0.20671 (3)0.01813 (14)
Mo40.57152 (4)0.35669 (3)0.02056 (3)0.01616 (13)
Mo50.19472 (4)0.28345 (3)0.12704 (3)0.01999 (14)
Mo60.40766 (4)0.30695 (3)0.31313 (3)0.01689 (13)
Mo70.73264 (4)0.29683 (3)0.36259 (3)0.01807 (13)
Mo80.50910 (3)0.21841 (3)0.16045 (3)0.01450 (12)
Mo90.25284 (4)0.03970 (3)0.30053 (3)0.01699 (13)
Mo100.47035 (3)0.11159 (3)0.50438 (3)0.01507 (13)
Mo110.79453 (4)0.07729 (3)0.55027 (3)0.01802 (14)
Mo120.58281 (3)0.03153 (3)0.35728 (3)0.01555 (13)
O10.1439 (3)0.4283 (3)0.0297 (3)0.0288 (15)
O20.3126 (3)0.4319 (2)0.1275 (2)0.0197 (12)
O30.2422 (4)0.3269 (3)0.1334 (3)0.0329 (16)
O40.2041 (3)0.2636 (2)0.0066 (2)0.0239 (13)
O50.4323 (3)0.3823 (2)0.0356 (2)0.0190 (12)
O60.6392 (3)0.4761 (3)0.0140 (2)0.0248 (14)
O70.5415 (3)0.5700 (2)0.1852 (2)0.0244 (13)
O80.4883 (3)0.4512 (2)0.2886 (2)0.0216 (12)
O90.3831 (3)0.2770 (2)0.1667 (2)0.0172 (11)
O100.5968 (3)0.3900 (2)0.1659 (2)0.0168 (11)
O110.7750 (3)0.4135 (2)0.3246 (2)0.0207 (12)
O120.6717 (3)0.2411 (2)0.2095 (2)0.0178 (11)
O130.9058 (3)0.3505 (3)0.2219 (3)0.0279 (14)
O140.8396 (3)0.5127 (3)0.2103 (3)0.0300 (15)
O150.7127 (3)0.3312 (2)0.0753 (2)0.0200 (12)
O160.5255 (3)0.2839 (3)0.0866 (2)0.0278 (14)
O170.4933 (3)0.2145 (2)0.0475 (2)0.0204 (12)
O180.0803 (3)0.3319 (3)0.1124 (3)0.0320 (16)
O190.2666 (3)0.3344 (2)0.2581 (2)0.0220 (13)
O200.1304 (3)0.1619 (3)0.1169 (3)0.0302 (15)
O210.4502 (3)0.3767 (3)0.4206 (2)0.0269 (14)
O220.3380 (3)0.1833 (2)0.3152 (2)0.0225 (13)
O230.5473 (3)0.2849 (2)0.2999 (2)0.0183 (11)
O240.7375 (4)0.3517 (3)0.4661 (2)0.0318 (15)
O250.6430 (3)0.1530 (3)0.3514 (2)0.0244 (13)
O260.8596 (3)0.2659 (3)0.3768 (3)0.0326 (16)
O270.4466 (3)0.0978 (2)0.1529 (2)0.0236 (13)
O280.2440 (3)0.0133 (3)0.1952 (2)0.0284 (14)
O290.1203 (3)0.0610 (3)0.2882 (3)0.0287 (15)
O300.3059 (3)0.0801 (2)0.4507 (2)0.0181 (11)
O310.4383 (3)0.0457 (2)0.3650 (2)0.0185 (11)
O320.7852 (3)0.0859 (2)0.6684 (2)0.0212 (12)
O330.5254 (3)0.2329 (3)0.5108 (2)0.0255 (13)
O340.4806 (3)0.1136 (2)0.6158 (2)0.0200 (12)
O350.6030 (3)0.0628 (2)0.5022 (2)0.0166 (11)
O360.9235 (3)0.0487 (3)0.5637 (3)0.0313 (16)
O370.8354 (3)0.2015 (3)0.5621 (3)0.0301 (15)
O380.7321 (3)0.0195 (2)0.4192 (2)0.0199 (12)
O390.5488 (3)0.0410 (3)0.2517 (2)0.0273 (14)
O1w0.6356 (5)0.1282 (3)0.0883 (3)0.049 (2)
O2w0.3364 (6)0.2032 (4)0.7346 (4)0.072 (3)
O3w0.9070 (4)0.0220 (4)0.3469 (3)0.058 (3)
O4w0.3259 (5)0.5541 (4)0.3805 (4)0.062 (3)
O5w0.0931 (6)0.4624 (5)0.3786 (5)0.095 (3)
O6w0.0438 (9)0.1717 (8)0.7667 (7)0.155 (6)
N10.8624 (4)0.0250 (4)0.1750 (3)0.040 (2)
N20.7548 (4)0.0513 (3)0.0324 (3)0.0333 (19)
N30.1441 (4)0.3577 (4)0.4954 (3)0.038 (2)
N40.2270 (5)0.2680 (4)0.6006 (4)0.041 (2)
N50.1652 (4)0.7345 (3)0.2214 (3)0.0314 (18)
N60.1766 (4)0.5803 (4)0.1333 (3)0.039 (2)
C10.8958 (6)0.0270 (4)0.1009 (4)0.046 (3)
C20.8160 (6)0.0218 (5)0.0127 (4)0.045 (3)
C30.7329 (7)0.0151 (7)0.1538 (6)0.076 (4)
C40.6688 (6)0.0134 (5)0.0734 (5)0.047 (3)
C50.8963 (5)0.1333 (4)0.1830 (4)0.036 (2)
C60.8431 (6)0.1467 (4)0.0923 (4)0.042 (2)
C70.2757 (6)0.4069 (5)0.5393 (5)0.045 (3)
C80.3254 (6)0.3368 (5)0.5856 (5)0.043 (3)
C90.0873 (6)0.3610 (4)0.5656 (4)0.037 (2)
C100.1576 (7)0.3253 (5)0.6393 (5)0.050 (3)
C110.1189 (6)0.2522 (5)0.4454 (5)0.052 (3)
C120.1450 (6)0.1953 (5)0.5127 (5)0.048 (3)
C130.2889 (6)0.7334 (5)0.2532 (5)0.050 (3)
C140.2968 (6)0.6371 (5)0.2002 (5)0.046 (3)
C150.0833 (6)0.6484 (4)0.2338 (5)0.045 (3)
C160.0915 (6)0.5531 (4)0.1800 (4)0.040 (3)
C170.1283 (6)0.7324 (5)0.1261 (4)0.043 (3)
C180.1367 (6)0.6377 (5)0.0712 (5)0.047 (3)
H10.900680.0149160.2287450.0477*
H20.7132780.0614150.0204270.04*
H30.1133190.3906830.4556320.0458*
H40.2593280.2353690.6400340.0492*
H50.1620460.7925010.2546190.0377*
H60.1798330.5228340.0992840.047*
H70.8837280.0960750.1007050.0546*
H80.9782450.0065660.10960.0546*
H90.8639310.0003350.0226790.0544*
H100.7573950.0867150.0195070.0544*
H110.712480.0120560.2048670.0911*
H120.7093450.0870720.1406140.0911*
H130.6062720.04490.030580.0558*
H140.6363130.0650620.0926380.0558*
H150.9824260.1609330.2032660.0428*
H160.8652150.1658450.2249670.0428*
H170.8040730.1972360.0976740.0501*
H180.9054280.1666390.0676150.0501*
H190.2914470.4688190.5835780.0542*
H200.310640.4178280.4937920.0542*
H210.356910.2990240.5474220.0513*
H220.3869360.3748260.6430610.0513*
H230.0057620.3167520.5395930.0449*
H240.0909030.4289320.5902050.0449*
H250.2123240.3822280.6886310.0599*
H260.1031910.2819130.6592620.0599*
H270.0355180.2244510.4075060.0623*
H280.1700230.249340.4097480.0623*
H290.0713750.1607260.5194160.0582*
H300.1836180.1486540.4931420.0582*
H310.3130960.7367540.3166690.0596*
H320.3406310.7899870.2440560.0596*
H330.3527080.6529380.1691470.0553*
H340.3209020.5982680.2407720.0553*
H350.0023650.6503340.2120390.0537*
H360.1070550.6506390.2970520.0537*
H370.1198450.5153950.2203750.0482*
H380.0136990.5140850.1359060.0482*
H390.1803820.7900570.1185230.0522*
H400.0467060.7333040.1058960.0522*
H410.0587560.5986460.0272980.0561*
H420.1943110.6551160.0418990.0561*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01580 (18)0.01817 (18)0.0225 (2)0.00485 (14)0.00681 (16)0.00696 (15)
Mo20.01421 (17)0.01238 (16)0.02019 (19)0.00386 (13)0.00687 (15)0.00489 (13)
Mo30.01457 (18)0.01746 (18)0.0230 (2)0.00302 (14)0.00833 (16)0.00697 (15)
Mo40.01711 (18)0.01583 (17)0.01909 (19)0.00618 (14)0.00918 (15)0.00713 (14)
Mo50.01552 (18)0.01765 (18)0.0279 (2)0.00319 (14)0.00980 (17)0.00805 (15)
Mo60.01832 (19)0.01529 (17)0.02046 (19)0.00559 (14)0.01050 (16)0.00655 (14)
Mo70.01560 (18)0.01834 (18)0.01871 (19)0.00269 (14)0.00569 (15)0.00551 (14)
Mo80.01366 (17)0.01222 (16)0.01815 (18)0.00368 (13)0.00649 (14)0.00443 (13)
Mo90.01405 (17)0.01775 (18)0.01901 (19)0.00330 (13)0.00595 (15)0.00667 (14)
Mo100.01321 (17)0.01381 (17)0.01882 (18)0.00385 (13)0.00652 (14)0.00507 (13)
Mo110.01324 (17)0.01954 (18)0.0219 (2)0.00333 (13)0.00701 (15)0.00811 (15)
Mo120.01403 (17)0.01682 (17)0.01800 (18)0.00478 (13)0.00778 (14)0.00653 (14)
O10.0243 (19)0.030 (2)0.038 (2)0.0123 (15)0.0139 (17)0.0144 (17)
O20.0179 (16)0.0142 (15)0.0280 (18)0.0048 (12)0.0090 (14)0.0066 (13)
O30.036 (2)0.033 (2)0.028 (2)0.0089 (17)0.0106 (18)0.0074 (16)
O40.0244 (18)0.0191 (16)0.0239 (18)0.0027 (13)0.0079 (15)0.0026 (13)
O50.0167 (16)0.0207 (16)0.0222 (17)0.0072 (12)0.0079 (13)0.0080 (13)
O60.0213 (18)0.0234 (18)0.035 (2)0.0073 (14)0.0117 (16)0.0154 (15)
O70.0240 (18)0.0168 (16)0.033 (2)0.0058 (13)0.0105 (16)0.0093 (14)
O80.0248 (18)0.0181 (16)0.0225 (17)0.0048 (13)0.0105 (15)0.0061 (13)
O90.0147 (15)0.0169 (15)0.0225 (16)0.0066 (12)0.0087 (13)0.0057 (12)
O100.0139 (15)0.0181 (15)0.0210 (16)0.0064 (12)0.0078 (13)0.0073 (12)
O110.0217 (17)0.0152 (15)0.0221 (17)0.0011 (12)0.0079 (14)0.0039 (12)
O120.0140 (15)0.0163 (15)0.0251 (17)0.0061 (12)0.0088 (13)0.0060 (12)
O130.0202 (18)0.034 (2)0.032 (2)0.0101 (15)0.0101 (16)0.0090 (16)
O140.028 (2)0.0222 (18)0.040 (2)0.0017 (15)0.0152 (18)0.0124 (16)
O150.0190 (16)0.0210 (16)0.0249 (17)0.0077 (13)0.0120 (14)0.0090 (13)
O160.033 (2)0.0287 (19)0.0232 (18)0.0095 (16)0.0124 (16)0.0080 (15)
O170.0220 (17)0.0180 (16)0.0225 (17)0.0057 (13)0.0102 (14)0.0054 (13)
O180.0228 (19)0.033 (2)0.045 (2)0.0123 (16)0.0143 (18)0.0128 (18)
O190.0218 (17)0.0228 (17)0.0286 (18)0.0104 (14)0.0155 (15)0.0089 (14)
O200.030 (2)0.0213 (18)0.041 (2)0.0022 (15)0.0191 (18)0.0095 (16)
O210.035 (2)0.0249 (18)0.0235 (18)0.0109 (15)0.0135 (16)0.0047 (14)
O220.0206 (17)0.0202 (16)0.0308 (19)0.0060 (13)0.0119 (15)0.0125 (14)
O230.0159 (15)0.0200 (16)0.0191 (16)0.0043 (12)0.0068 (13)0.0062 (12)
O240.037 (2)0.030 (2)0.0228 (19)0.0029 (17)0.0115 (17)0.0024 (15)
O250.0198 (17)0.0237 (17)0.035 (2)0.0066 (14)0.0119 (15)0.0169 (15)
O260.0217 (19)0.039 (2)0.040 (2)0.0125 (17)0.0084 (17)0.0175 (18)
O270.0228 (18)0.0166 (15)0.0284 (19)0.0018 (13)0.0087 (15)0.0056 (13)
O280.033 (2)0.0264 (18)0.0224 (18)0.0041 (15)0.0107 (16)0.0048 (14)
O290.0204 (18)0.034 (2)0.041 (2)0.0139 (16)0.0131 (17)0.0200 (17)
O300.0163 (15)0.0228 (16)0.0178 (16)0.0084 (13)0.0073 (13)0.0068 (12)
O310.0154 (15)0.0203 (16)0.0203 (16)0.0052 (12)0.0068 (13)0.0061 (12)
O320.0226 (17)0.0164 (15)0.0239 (17)0.0029 (13)0.0097 (14)0.0062 (13)
O330.0245 (18)0.0197 (16)0.032 (2)0.0037 (14)0.0108 (16)0.0102 (14)
O340.0170 (16)0.0217 (16)0.0181 (16)0.0021 (12)0.0071 (13)0.0024 (12)
O350.0151 (15)0.0177 (15)0.0163 (15)0.0040 (11)0.0056 (12)0.0043 (12)
O360.0201 (18)0.047 (2)0.036 (2)0.0154 (17)0.0142 (17)0.0196 (18)
O370.031 (2)0.0240 (18)0.032 (2)0.0004 (15)0.0105 (17)0.0108 (15)
O380.0172 (16)0.0245 (17)0.0220 (17)0.0085 (13)0.0107 (14)0.0072 (13)
O390.029 (2)0.0315 (19)0.0225 (18)0.0103 (16)0.0096 (16)0.0070 (15)
O1w0.059 (3)0.035 (2)0.042 (3)0.024 (2)0.003 (2)0.001 (2)
O2w0.084 (4)0.047 (3)0.062 (4)0.032 (3)0.006 (3)0.001 (3)
O3w0.045 (3)0.110 (4)0.041 (3)0.044 (3)0.022 (2)0.032 (3)
O4w0.071 (4)0.048 (3)0.063 (4)0.018 (3)0.027 (3)0.003 (3)
O5w0.070 (4)0.085 (5)0.088 (5)0.011 (3)0.018 (4)0.045 (4)
O6w0.127 (8)0.147 (9)0.149 (9)0.028 (7)0.018 (7)0.010 (7)
N10.036 (3)0.051 (3)0.029 (3)0.007 (2)0.006 (2)0.021 (2)
N20.028 (2)0.035 (3)0.033 (3)0.014 (2)0.003 (2)0.008 (2)
N30.031 (3)0.045 (3)0.038 (3)0.013 (2)0.011 (2)0.009 (2)
N40.040 (3)0.037 (3)0.051 (3)0.015 (2)0.017 (3)0.015 (2)
N50.033 (3)0.018 (2)0.037 (3)0.0040 (17)0.012 (2)0.0021 (18)
N60.039 (3)0.028 (2)0.047 (3)0.006 (2)0.024 (3)0.005 (2)
C10.043 (4)0.030 (3)0.049 (4)0.019 (3)0.003 (3)0.003 (3)
C20.047 (4)0.051 (4)0.036 (3)0.026 (3)0.015 (3)0.004 (3)
C30.041 (5)0.111 (8)0.061 (5)0.011 (5)0.021 (4)0.030 (5)
C40.021 (3)0.053 (4)0.058 (4)0.005 (3)0.015 (3)0.005 (3)
C50.031 (3)0.029 (3)0.036 (3)0.008 (2)0.006 (3)0.003 (2)
C60.035 (3)0.028 (3)0.049 (4)0.005 (2)0.000 (3)0.008 (3)
C70.033 (3)0.039 (4)0.067 (5)0.009 (3)0.025 (3)0.013 (3)
C80.027 (3)0.038 (3)0.051 (4)0.007 (3)0.004 (3)0.004 (3)
C90.033 (3)0.034 (3)0.042 (3)0.011 (2)0.017 (3)0.003 (3)
C100.062 (5)0.058 (5)0.048 (4)0.034 (4)0.032 (4)0.017 (3)
C110.040 (4)0.047 (4)0.049 (4)0.013 (3)0.005 (3)0.015 (3)
C120.033 (3)0.026 (3)0.076 (5)0.003 (2)0.019 (3)0.003 (3)
C130.029 (3)0.042 (4)0.054 (4)0.002 (3)0.004 (3)0.002 (3)
C140.037 (4)0.051 (4)0.060 (5)0.020 (3)0.024 (3)0.017 (3)
C150.051 (4)0.035 (3)0.051 (4)0.005 (3)0.035 (4)0.002 (3)
C160.046 (4)0.024 (3)0.048 (4)0.000 (2)0.028 (3)0.001 (2)
C170.041 (4)0.042 (4)0.042 (4)0.005 (3)0.012 (3)0.014 (3)
C180.039 (4)0.049 (4)0.040 (4)0.003 (3)0.018 (3)0.006 (3)
Bond lengths (Å) top
Mo1—O11.722 (5)Mo7—O122.284 (3)
Mo1—O22.295 (4)Mo7—O232.170 (3)
Mo1—O31.685 (4)Mo7—O241.685 (4)
Mo1—O41.874 (4)Mo7—O252.045 (4)
Mo1—O52.075 (3)Mo7—O261.697 (5)
Mo1—O6i2.094 (4)Mo8—O91.959 (4)
Mo2—O21.869 (3)Mo8—O102.419 (3)
Mo2—O52.156 (3)Mo8—O121.854 (3)
Mo2—O71.689 (3)Mo8—O171.767 (4)
Mo2—O81.760 (4)Mo8—O232.138 (3)
Mo2—O92.425 (3)Mo8—O271.687 (3)
Mo2—O101.936 (4)Mo9—O222.014 (3)
Mo3—O102.226 (3)Mo9—O281.687 (4)
Mo3—O111.916 (4)Mo9—O291.701 (4)
Mo3—O122.303 (3)Mo9—O302.241 (3)
Mo3—O131.702 (4)Mo9—O312.200 (3)
Mo3—O141.686 (4)Mo9—O32ii1.953 (4)
Mo3—O151.976 (3)Mo10—O301.865 (3)
Mo4—O51.913 (4)Mo10—O312.150 (3)
Mo4—O61.758 (4)Mo10—O331.686 (4)
Mo4—O102.218 (4)Mo10—O341.760 (4)
Mo4—O151.874 (4)Mo10—O351.939 (4)
Mo4—O161.697 (3)Mo10—O35ii2.427 (3)
Mo4—O172.221 (4)Mo11—O30ii2.300 (3)
Mo5—O22.273 (3)Mo11—O321.926 (4)
Mo5—O41.952 (4)Mo11—O352.210 (3)
Mo5—O92.259 (4)Mo11—O361.706 (5)
Mo5—O181.700 (5)Mo11—O371.695 (4)
Mo5—O191.957 (3)Mo11—O381.964 (3)
Mo5—O201.694 (4)Mo12—O251.760 (4)
Mo6—O82.236 (4)Mo12—O311.880 (4)
Mo6—O92.238 (4)Mo12—O34ii2.218 (4)
Mo6—O191.888 (4)Mo12—O352.225 (3)
Mo6—O211.691 (4)Mo12—O381.896 (4)
Mo6—O221.792 (4)Mo12—O391.697 (4)
Mo6—O231.888 (4)C2—O20iii2.953 (9)
Mo7—O111.904 (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
C12H37.32Mo8N4O30.66V = 878.20 (9) Å3
Mr = 1495.8Z = 1
Triclinic, P1(αβγ)0†F(000) = 709
q = 0.06330a* + -0.42840b* + -0.41590c*Dx = 2.828 Mg m3
a = 7.8907 (5) ÅMo Kα radiation, λ = 0.71069 Å
b = 10.0855 (3) ŵ = 2.87 mm1
c = 12.4131 (8) ÅT = 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
Rint = 0.064
Absorption correction: gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
θmax = 35.9°, θmin = 5.0°
Tmin = 0.649, Tmax = 0.826h = 1312
153057 measured reflectionsk = 1616
39145 independent reflectionsl = 2020
21512 reflections with I > 2σ(I)
Refinement top
Refinement on F2Const
R[F2 > 2σ(F2)] = 0.052Weighting scheme based on measured s.u.'s w = 1/(σ2(I) + 0.001936I2)
wR(F2) = 0.133(Δ/σ)max = 0.002
S = 1.34Δρmax = 2.11 e Å3
39145 reflectionsΔρmin = 1.88 e Å3
566 parameters
Crystal data top
C12H37.32Mo8N4O30.66β = 92.857 (7)°
Mr = 1495.8γ = 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) ÅMo Kα radiation
b = 10.0855 (3) ŵ = 2.87 mm1
c = 12.4131 (8) ÅT = 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)
Tmin = 0.649, Tmax = 0.826Rint = 0.064
153057 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.052566 parameters
wR(F2) = 0.133Const
S = 1.34Δρmax = 2.11 e Å3
39145 reflectionsΔρmin = 1.88 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mo10.01475 (2)0.10641 (2)0.793165 (14)0.01834 (6)
Mo20.41800 (2)0.149828 (18)0.739826 (14)0.01804 (5)
Mo30.304037 (18)0.117739 (17)0.419560 (14)0.01527 (5)
Mo40.114145 (19)0.118717 (16)0.480196 (13)0.01409 (5)
O10.06329 (17)0.05779 (15)0.60558 (12)0.0165 (4)
O20.1051 (2)0.2348 (2)0.84722 (16)0.0333 (6)
O30.17194 (18)0.08043 (17)0.72417 (13)0.0206 (5)
O40.0839 (2)0.0760 (2)0.91185 (15)0.0317 (6)
O50.18520 (18)0.04563 (16)0.68331 (12)0.0185 (4)
O60.22161 (19)0.23677 (16)0.78452 (13)0.0218 (5)
O70.4736 (2)0.1296 (2)0.86514 (15)0.0343 (7)
O80.55103 (18)0.00333 (17)0.64663 (13)0.0233 (5)
O90.5569 (2)0.30712 (19)0.75102 (17)0.0328 (6)
O100.30421 (17)0.08414 (15)0.55868 (12)0.0179 (4)
O110.4254 (2)0.29384 (18)0.46168 (15)0.0260 (5)
O120.09476 (18)0.23147 (16)0.49390 (13)0.0205 (5)
O130.2353 (2)0.24376 (18)0.54182 (15)0.0258 (5)
O1w0.2991 (6)0.4617 (3)0.3448 (4)0.0890 (17)0.932 (3)
O2w0.3184 (6)0.1670 (7)0.1090 (4)0.0745 (18)0.855 (4)
O3w0.2867 (14)0.4379 (9)0.0478 (7)0.129 (5)0.554 (16)
N1a0.0186 (3)0.6031 (3)0.7674 (3)0.0327 (8)0.487
N2a0.3348 (6)0.7035 (6)0.8312 (5)0.049 (5)0.487
C1a0.0534 (7)0.7570 (6)0.8508 (5)0.0447 (17)0.487
C2a0.1028 (7)0.5898 (6)0.6645 (5)0.049 (2)0.487
C3a0.0843 (7)0.5154 (7)0.8242 (6)0.0554 (19)0.487
C4a0.2446 (7)0.8174 (6)0.8873 (5)0.049 (4)0.487
C5a0.2949 (8)0.6500 (8)0.7027 (6)0.067 (5)0.487
C6a0.2787 (7)0.5790 (7)0.8664 (6)0.062 (5)0.487
H1a0.1000 (3)0.5690 (3)0.7435 (3)0.0481 (15)0.487
H2a0.4527 (3)0.7440 (3)0.8547 (3)0.076 (9)0.487
H3a0.0027 (3)0.7650 (3)0.9203 (3)0.074 (3)0.487
H4a0.0075 (3)0.8137 (3)0.8140 (3)0.065 (3)0.487
H5a0.0585 (3)0.6464 (3)0.6269 (3)0.066 (3)0.487
H6a0.0798 (3)0.4857 (3)0.6091 (3)0.075 (3)0.487
H7a0.0642 (3)0.4124 (3)0.7669 (3)0.082 (3)0.487
H8a0.0241 (3)0.5213 (3)0.8916 (3)0.083 (3)0.487
H9a0.2824 (3)0.8988 (3)0.8646 (3)0.073 (5)0.487
H10a0.2714 (3)0.8547 (3)0.9729 (3)0.072 (5)0.487
H11a0.3551 (3)0.5721 (3)0.6636 (3)0.106 (8)0.487
H12a0.3342 (3)0.7315 (3)0.6804 (3)0.095 (7)0.487
H13a0.3006 (3)0.6165 (3)0.9522 (3)0.084 (6)0.487
H14a0.3412 (3)0.5023 (3)0.8286 (3)0.098 (7)0.487
N1b0.2228 (8)0.5251 (4)0.8063 (4)0.087 (3)0.513
N2b0.2257 (11)0.7672 (6)0.8018 (6)0.068 (18)0.513
C1b0.2981 (11)0.5322 (7)0.7048 (6)0.149 (8)0.513
C2b0.3241 (11)0.6415 (7)0.9140 (6)0.256 (10)0.513
C3b0.0412 (12)0.5424 (7)0.7988 (7)0.306 (11)0.513
C4b0.3020 (11)0.6795 (7)0.7040 (6)0.158 (17)0.513
C5b0.3256 (13)0.7887 (7)0.9120 (7)0.29 (2)0.513
C6b0.0414 (13)0.6900 (7)0.7931 (7)0.22 (2)0.513
H1b0.2259 (8)0.4347 (4)0.8070 (4)0.128 (5)0.513
H2b0.2307 (8)0.8579 (4)0.7995 (4)0.10 (3)0.513
H3b0.2284 (8)0.4541 (4)0.6326 (4)0.341 (13)0.513
H4b0.4160 (8)0.5183 (4)0.7090 (4)0.272 (16)0.513
H5b0.4428 (8)0.6293 (4)0.9192 (4)0.375 (18)0.513
H6b0.2720 (8)0.6368 (4)0.9819 (4)0.505 (13)0.513
H7b0.0077 (8)0.5410 (4)0.8686 (4)0.567 (17)0.513
H8b0.0280 (8)0.4616 (4)0.7277 (4)0.51 (2)0.513
H9b0.4219 (8)0.7308 (4)0.7097 (4)0.35 (3)0.513
H10b0.2373 (8)0.6655 (4)0.6302 (4)0.31 (2)0.513
H11b0.2745 (8)0.8479 (4)0.9791 (4)0.54 (3)0.513
H12b0.4450 (8)0.8411 (4)0.9177 (4)0.50 (4)0.513
H13b0.0227 (8)0.6719 (4)0.7179 (4)0.34 (3)0.513
H14b0.0101 (8)0.7505 (4)0.8594 (4)0.42 (3)0.513
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.01765 (7)0.02411 (8)0.01514 (7)0.00836 (6)0.00484 (5)0.00828 (6)
Mo20.01580 (7)0.02150 (7)0.01672 (7)0.00599 (5)0.00213 (5)0.00724 (6)
Mo30.01236 (6)0.01932 (7)0.01823 (7)0.00569 (5)0.00447 (5)0.01086 (6)
Mo40.01378 (6)0.01632 (6)0.01532 (7)0.00663 (5)0.00372 (5)0.00822 (5)
O10.0160 (5)0.0198 (5)0.0162 (5)0.0059 (4)0.0029 (4)0.0093 (4)
O20.0317 (8)0.0347 (8)0.0328 (9)0.0180 (7)0.0112 (7)0.0079 (7)
O30.0180 (6)0.0297 (7)0.0203 (6)0.0068 (5)0.0041 (5)0.0159 (5)
O40.0331 (8)0.0440 (9)0.0226 (7)0.0111 (7)0.0048 (6)0.0176 (7)
O50.0185 (6)0.0244 (6)0.0176 (6)0.0089 (5)0.0042 (5)0.0118 (5)
O60.0194 (6)0.0212 (6)0.0235 (7)0.0084 (5)0.0053 (5)0.0063 (5)
O70.0341 (9)0.0518 (10)0.0235 (8)0.0176 (8)0.0022 (6)0.0191 (7)
O80.0188 (6)0.0308 (7)0.0251 (7)0.0140 (5)0.0075 (5)0.0124 (6)
O90.0246 (7)0.0270 (7)0.0414 (9)0.0020 (6)0.0044 (7)0.0108 (7)
O100.0156 (5)0.0216 (6)0.0181 (6)0.0044 (4)0.0023 (4)0.0100 (5)
O110.0210 (6)0.0239 (6)0.0352 (8)0.0028 (5)0.0051 (6)0.0155 (6)
O120.0172 (6)0.0201 (6)0.0266 (7)0.0062 (5)0.0058 (5)0.0110 (5)
O130.0269 (7)0.0267 (7)0.0282 (7)0.0167 (6)0.0080 (6)0.0108 (6)
O1w0.096 (3)0.0367 (13)0.114 (3)0.0113 (15)0.036 (2)0.0194 (16)
O2w0.0485 (17)0.120 (3)0.0554 (18)0.0029 (19)0.0035 (14)0.048 (2)
O3w0.169 (10)0.092 (6)0.077 (5)0.019 (5)0.014 (5)0.013 (4)
N1a0.0295 (9)0.0334 (10)0.0397 (12)0.0061 (8)0.0042 (8)0.0205 (9)
N2a0.0284 (11)0.060 (8)0.065 (9)0.006 (2)0.005 (2)0.037 (7)
C1a0.043 (4)0.0424 (12)0.044 (2)0.019 (2)0.002 (2)0.0094 (13)
C2a0.057 (3)0.053 (4)0.032 (2)0.009 (3)0.009 (2)0.016 (2)
C3a0.051 (2)0.052 (3)0.081 (3)0.001 (2)0.0018 (18)0.052 (2)
C4a0.050 (5)0.039 (4)0.050 (6)0.001 (4)0.012 (4)0.017 (4)
C5a0.0504 (19)0.094 (8)0.060 (8)0.013 (3)0.030 (3)0.036 (7)
C6a0.049 (2)0.064 (8)0.093 (6)0.015 (3)0.008 (3)0.054 (6)
H1a0.0309 (9)0.050 (2)0.063 (2)0.0024 (10)0.0015 (10)0.0273 (18)
H2a0.0292 (13)0.096 (13)0.107 (15)0.000 (3)0.000 (4)0.056 (12)
H3a0.060 (7)0.095 (3)0.051 (2)0.034 (4)0.020 (3)0.0075 (19)
H4a0.065 (5)0.0394 (16)0.081 (4)0.026 (2)0.016 (3)0.0125 (19)
H5a0.083 (4)0.078 (5)0.040 (3)0.000 (4)0.007 (3)0.036 (3)
H6a0.088 (6)0.066 (4)0.046 (2)0.021 (5)0.009 (3)0.003 (2)
H7a0.080 (4)0.042 (2)0.132 (5)0.002 (3)0.017 (3)0.053 (3)
H8a0.070 (4)0.111 (4)0.098 (3)0.012 (4)0.004 (3)0.089 (3)
H9a0.075 (6)0.040 (4)0.093 (10)0.014 (4)0.030 (6)0.033 (5)
H10a0.076 (9)0.065 (5)0.049 (6)0.005 (6)0.021 (6)0.007 (4)
H11a0.071 (4)0.143 (12)0.095 (11)0.043 (7)0.053 (6)0.029 (10)
H12a0.074 (3)0.142 (11)0.082 (12)0.009 (5)0.031 (5)0.074 (10)
H13a0.074 (4)0.103 (11)0.099 (7)0.006 (6)0.025 (4)0.079 (7)
H14a0.070 (3)0.078 (11)0.161 (11)0.038 (5)0.013 (4)0.060 (9)
N1b0.141 (6)0.0365 (17)0.112 (3)0.043 (3)0.061 (3)0.044 (2)
N2b0.11 (4)0.038 (6)0.067 (19)0.027 (14)0.01 (2)0.034 (9)
C1b0.303 (14)0.140 (10)0.099 (10)0.175 (9)0.117 (10)0.080 (9)
C2b0.61 (2)0.081 (7)0.074 (8)0.128 (11)0.082 (10)0.024 (6)
C3b0.15 (3)0.180 (8)0.762 (12)0.093 (12)0.207 (13)0.331 (8)
C4b0.25 (3)0.204 (16)0.19 (2)0.194 (18)0.17 (2)0.177 (16)
C5b0.62 (5)0.041 (9)0.14 (2)0.070 (18)0.20 (2)0.008 (12)
C6b0.13 (5)0.154 (8)0.523 (18)0.097 (17)0.17 (2)0.241 (10)
H1b0.177 (12)0.052 (2)0.207 (5)0.060 (4)0.094 (6)0.083 (3)
H2b0.13 (7)0.059 (10)0.14 (3)0.03 (2)0.01 (4)0.072 (16)
H3b0.79 (2)0.180 (17)0.066 (10)0.310 (16)0.005 (11)0.016 (11)
H4b0.36 (3)0.314 (17)0.46 (2)0.306 (16)0.34 (2)0.346 (17)
H5b0.56 (4)0.108 (13)0.381 (16)0.01 (2)0.349 (18)0.104 (12)
H6b1.35 (3)0.260 (16)0.083 (9)0.481 (18)0.181 (12)0.115 (10)
H7b0.51 (3)0.462 (16)1.30 (2)0.415 (18)0.73 (2)0.741 (17)
H8b0.14 (5)0.178 (13)1.241 (19)0.06 (2)0.13 (2)0.378 (13)
H9b0.28 (5)0.42 (3)0.79 (4)0.31 (3)0.40 (4)0.56 (3)
H10b0.70 (5)0.32 (3)0.10 (2)0.40 (3)0.19 (2)0.15 (2)
H11b1.40 (7)0.143 (16)0.07 (3)0.37 (3)0.08 (3)0.027 (18)
H12b0.58 (8)0.073 (16)0.67 (4)0.09 (3)0.54 (4)0.13 (2)
H13b0.10 (7)0.174 (15)0.77 (2)0.00 (3)0.11 (3)0.253 (14)
H14b0.48 (7)0.363 (15)0.88 (3)0.38 (3)0.59 (3)0.522 (18)
Bond lengths (Å) top
AverageMinimumMaximum
O1w—O9i3.073 (16)2.924 (16)3.232 (17)
O1w—O112.918 (17)2.885 (16)2.960 (17)
O1w—O11i3.031 (12)2.888 (12)3.191 (12)
O1w—O13ii2.905 (12)2.823 (12)2.951 (13)
O1w—O2w3.341 (19)3.068 (19)3.502 (18)
O1w—O3w3.56 (2)3.11 (2)4.15 (2)
O2w—O3iii2.770 (19)2.662 (18)3.00 (2)
O2w—O4iv2.753 (16)2.595 (14)2.867 (15)
O2w—O7iv3.222 (17)3.046 (19)3.459 (17)
O2w—O3w3.26 (3)2.75 (3)3.49 (3)
O3w—O6iv3.028 (12)2.970 (12)3.075 (12)
O3w—O9i2.787 (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, x31, x4.

Experimental details

(I)(II)
Crystal data
Chemical formula(C6H14N2)2[Mo8O26]·4H2OC12H37.32Mo8N4O30.66
Mr1483.91495.8
Crystal system, space groupTriclinic, P1Triclinic, P1(αβγ)0†
Temperature (K)293293
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)
V3)2565.0 (6)113.685 (4), 92.857 (7), 101.244 (5)
Z3878.20 (9)
Radiation typeMo Kα?
µ (mm1)2.95?
Crystal size (mm)0.18 × 0.10 × 0.08Colorless
Data collection
DiffractometerNonius CCD
diffractometer
Nonius CCD
diffractometer
Absorption correctionGaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
Gaussian
(Jana2000; Petricek, Dusek & Palatinus, 2000)
Tmin, Tmax0.595, 0.8330.649, 0.826
No. of measured, independent and
observed [I > 2σ(I)] reflections
90290, 21895, 14316 153057, 39145, 21512
Rint0.0680.064
(sin θ/λ)max1)0.8070.826
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.058, 0.135, 1.43 0.052, 0.133, 1.34
No. of reflections2189539145
No. of parameters730566
No. of restraints??
H-atom treatmentH-atom parameters constrainedConst
Δρmax, Δρmin (e Å3)1.61, 1.892.11, 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—O11.722 (5)Mo7—O122.284 (3)
Mo1—O22.295 (4)Mo7—O232.170 (3)
Mo1—O31.685 (4)Mo7—O241.685 (4)
Mo1—O41.874 (4)Mo7—O252.045 (4)
Mo1—O52.075 (3)Mo7—O261.697 (5)
Mo1—O6i2.094 (4)Mo8—O91.959 (4)
Mo2—O21.869 (3)Mo8—O102.419 (3)
Mo2—O52.156 (3)Mo8—O121.854 (3)
Mo2—O71.689 (3)Mo8—O171.767 (4)
Mo2—O81.760 (4)Mo8—O232.138 (3)
Mo2—O92.425 (3)Mo8—O271.687 (3)
Mo2—O101.936 (4)Mo9—O222.014 (3)
Mo3—O102.226 (3)Mo9—O281.687 (4)
Mo3—O111.916 (4)Mo9—O291.701 (4)
Mo3—O122.303 (3)Mo9—O302.241 (3)
Mo3—O131.702 (4)Mo9—O312.200 (3)
Mo3—O141.686 (4)Mo9—O32ii1.953 (4)
Mo3—O151.976 (3)Mo10—O301.865 (3)
Mo4—O51.913 (4)Mo10—O312.150 (3)
Mo4—O61.758 (4)Mo10—O331.686 (4)
Mo4—O102.218 (4)Mo10—O341.760 (4)
Mo4—O151.874 (4)Mo10—O351.939 (4)
Mo4—O161.697 (3)Mo10—O35ii2.427 (3)
Mo4—O172.221 (4)Mo11—O30ii2.300 (3)
Mo5—O22.273 (3)Mo11—O321.926 (4)
Mo5—O41.952 (4)Mo11—O352.210 (3)
Mo5—O92.259 (4)Mo11—O361.706 (5)
Mo5—O181.700 (5)Mo11—O371.695 (4)
Mo5—O191.957 (3)Mo11—O381.964 (3)
Mo5—O201.694 (4)Mo12—O251.760 (4)
Mo6—O82.236 (4)Mo12—O311.880 (4)
Mo6—O92.238 (4)Mo12—O34ii2.218 (4)
Mo6—O191.888 (4)Mo12—O352.225 (3)
Mo6—O211.691 (4)Mo12—O381.896 (4)
Mo6—O221.792 (4)Mo12—O391.697 (4)
Mo6—O231.888 (4)C2—O20iii2.953 (9)
Mo7—O111.904 (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
AverageMinimumMaximum
O1w—O9i3.073 (16)2.924 (16)3.232 (17)
O1w—O112.918 (17)2.885 (16)2.960 (17)
O1w—O11i3.031 (12)2.888 (12)3.191 (12)
O1w—O13ii2.905 (12)2.823 (12)2.951 (13)
O1w—O2w3.341 (19)3.068 (19)3.502 (18)
O1w—O3w3.56 (2)3.11 (2)4.15 (2)
O2w—O3iii2.770 (19)2.662 (18)3.00 (2)
O2w—O4iv2.753 (16)2.595 (14)2.867 (15)
O2w—O7iv3.222 (17)3.046 (19)3.459 (17)
O2w—O3w3.26 (3)2.75 (3)3.49 (3)
O3w—O6iv3.028 (12)2.970 (12)3.075 (12)
O3w—O9i2.787 (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, x31, x4.
 

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