Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807052294/zl2074sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807052294/zl2074Isup2.hkl |
CCDC reference: 667220
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.023
- wR factor = 0.054
- Data-to-parameter ratio = 16.2
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.481 0.684 Tmin(prime) and Tmax expected: 0.562 0.684 RR(prime) = 0.856 Please check that your absorption correction is appropriate. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.83 PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo2 - O5 .. 5.88 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo3 - O6 .. 5.58 su PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo1 (6) 5.81 PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo2 (6) 5.93 PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo3 (6) 5.91 PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo4 (6) 5.91
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 6 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 4 ALERT type 5 Informative message, check
A mixture of Na2MoO4.2H2O (0.242 g, 1.0 mmol) and L (0.316 g, 1.0 mmol) in water (10 ml) was adjusted with HCl (6M) to pH = 2. Then the mixture was placed in a 23 ml Teflon-lined autoclave and kept under autogenous pressure at 150 °C for 3 days. After the mixture was cooled to room temperature at 10°C h-1, colorless crystals of the title compound were obtained.
All H atoms on C atoms were poisitioned geometrically and refined as riding atoms, with C—H = 0.93 - 0.97 Å, and Uiso=1.2Ueq (C). The H atoms of N5 and N6 were located in a difference Fourier map and then refined isotropically.
Important advances in polyoxometalate (POM) chemistry (Pope, 1983) have recently been made in the coordination chemistry of polyoxoanions with classical transition metal coordination complexes or fragments. The introduction of metal complexes does not only enrich the frameworks of polyoxometalates but also ameliorates their electronic and magnetic properties (Chen et al., 2002; Lu et al., 2002; Reinoso et al., 2005). During our ongoing studies of such materials, we obtained the title compound, and present its crystal structure here.
The asymmetric part of the unit cell contains each one [H2L]2+ cation 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. Through N—H···O hydrogen bonds each protonated [H2L]2+ cation is linked two [Mo8O26]4- anions, and each [Mo8O26]4- anion joins four protonated [H2L]2+ cations (see the hydrogen bonding table for numerical values). The hydrogen bonds in the title compound thus create a two-dimensional supramolecular layerlike structure (Fig. 2).
For related literature on polyoxometalate (POM) chemistry, see: Pope (1983). Chen et al. (2002), Lu et al. (2002) and Reinoso et al. (2005) describe how forming metal complexes of polyoxometalates influences the POM frameworks and ameliorates their electronic and magnetic properties.
Data collection: SMART (Bruker, 1997); cell refinement: SMART (Bruker, 1997); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
(C18H18N6)2[Mo8O26] | Z = 4 |
Mr = 1820.28 | F(000) = 3520 |
Monoclinic, C2/c | Dx = 2.368 Mg m−3 |
Hall symbol: -C2yc | Mo Kα radiation, λ = 0.71069 Å |
a = 23.1640 (4) Å | θ = 1.9–28.3° |
b = 10.4740 (5) Å | µ = 2.00 mm−1 |
c = 22.7770 (8) Å | T = 293 K |
β = 112.494 (1)° | Block, colorless |
V = 5105.7 (3) Å3 | 0.28 × 0.26 × 0.19 mm |
Bruker APEX CCD area-detector diffractometer | 6141 independent reflections |
Radiation source: fine-focus sealed tube | 5242 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ω scans | θmax = 28.3°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −29→30 |
Tmin = 0.481, Tmax = 0.684 | k = −13→8 |
15475 measured reflections | l = −29→28 |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0237P)2 + 2.9429P] where P = (Fo2 + 2Fc2)/3 |
6141 reflections | (Δ/σ)max = 0.003 |
378 parameters | Δρmax = 0.32 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
(C18H18N6)2[Mo8O26] | V = 5105.7 (3) Å3 |
Mr = 1820.28 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 23.1640 (4) Å | µ = 2.00 mm−1 |
b = 10.4740 (5) Å | T = 293 K |
c = 22.7770 (8) Å | 0.28 × 0.26 × 0.19 mm |
β = 112.494 (1)° |
Bruker APEX CCD area-detector diffractometer | 6141 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5242 reflections with I > 2σ(I) |
Tmin = 0.481, Tmax = 0.684 | Rint = 0.020 |
15475 measured reflections |
R[F2 > 2σ(F2)] = 0.023 | 0 restraints |
wR(F2) = 0.054 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 0.32 e Å−3 |
6141 reflections | Δρmin = −0.48 e Å−3 |
378 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.89870 (14) | −0.0869 (3) | 0.27475 (14) | 0.0441 (7) | |
H1 | 0.9358 | −0.1323 | 0.2928 | 0.053* | |
C2 | 0.84466 (13) | −0.1193 (3) | 0.28019 (13) | 0.0405 (7) | |
H2 | 0.8379 | −0.1887 | 0.3022 | 0.049* | |
C12 | 0.87836 (16) | 0.0072 (3) | 0.03172 (16) | 0.0545 (8) | |
H12 | 0.8468 | −0.0268 | −0.0039 | 0.065* | |
C3 | 0.83246 (12) | 0.0547 (2) | 0.22249 (12) | 0.0315 (6) | |
C4 | 0.80217 (12) | 0.1615 (2) | 0.18149 (12) | 0.0322 (6) | |
C5 | 0.78785 (14) | 0.3224 (3) | 0.11565 (13) | 0.0402 (7) | |
H5 | 0.7941 | 0.3871 | 0.0907 | 0.048* | |
C6 | 0.73332 (14) | 0.2882 (3) | 0.11943 (13) | 0.0411 (7) | |
H6 | 0.6950 | 0.3267 | 0.0968 | 0.049* | |
C7 | 0.89781 (12) | 0.2422 (3) | 0.16363 (14) | 0.0378 (6) | |
H7A | 0.9237 | 0.2246 | 0.2077 | 0.045* | |
H7B | 0.9089 | 0.3262 | 0.1533 | 0.045* | |
C8 | 0.91118 (12) | 0.1443 (2) | 0.12192 (12) | 0.0325 (6) | |
C9 | 0.97181 (14) | 0.1054 (3) | 0.13511 (14) | 0.0427 (7) | |
H9 | 1.0045 | 0.1378 | 0.1702 | 0.051* | |
C10 | 0.98359 (15) | 0.0179 (3) | 0.09575 (16) | 0.0483 (8) | |
H10 | 1.0243 | −0.0082 | 0.1041 | 0.058* | |
C11 | 0.86399 (14) | 0.0944 (3) | 0.06898 (15) | 0.0466 (7) | |
H11 | 0.8228 | 0.1197 | 0.0587 | 0.056* | |
C13 | 0.73548 (12) | −0.0334 (3) | 0.23536 (12) | 0.0336 (6) | |
H13A | 0.7248 | −0.1209 | 0.2410 | 0.040* | |
H13B | 0.7117 | −0.0102 | 0.1915 | 0.040* | |
C14 | 0.71528 (12) | 0.0512 (2) | 0.27743 (12) | 0.0316 (6) | |
C15 | 0.65174 (13) | 0.0563 (3) | 0.26529 (13) | 0.0385 (6) | |
H15 | 0.6234 | 0.0126 | 0.2307 | 0.046* | |
C16 | 0.63082 (16) | 0.1256 (3) | 0.30408 (15) | 0.0503 (8) | |
H16 | 0.5883 | 0.1298 | 0.2959 | 0.060* | |
C17 | 0.7328 (2) | 0.1859 (3) | 0.36671 (16) | 0.0633 (10) | |
H17 | 0.7600 | 0.2301 | 0.4018 | 0.076* | |
C18 | 0.75615 (15) | 0.1192 (3) | 0.32810 (14) | 0.0486 (8) | |
H18 | 0.7987 | 0.1203 | 0.3362 | 0.058* | |
N1 | 0.74194 (10) | 0.1887 (2) | 0.16133 (11) | 0.0384 (5) | |
N2 | 0.83244 (10) | 0.2425 (2) | 0.15601 (11) | 0.0345 (5) | |
N3 | 0.80131 (10) | −0.0286 (2) | 0.24644 (10) | 0.0329 (5) | |
N4 | 0.89177 (11) | 0.0223 (2) | 0.23895 (11) | 0.0409 (6) | |
N5 | 0.93715 (14) | −0.0286 (3) | 0.04640 (14) | 0.0485 (7) | |
N6 | 0.67189 (17) | 0.1870 (3) | 0.35373 (15) | 0.0588 (8) | |
O1 | 0.54584 (8) | 0.29320 (16) | 0.04539 (8) | 0.0358 (4) | |
O2 | 0.48100 (9) | 0.19921 (19) | 0.13672 (10) | 0.0456 (5) | |
O3 | 0.50867 (8) | −0.0374 (2) | 0.18620 (8) | 0.0414 (5) | |
O4 | 0.49368 (7) | −0.15179 (15) | 0.06816 (7) | 0.0262 (4) | |
O5 | 0.56402 (7) | 0.04669 (16) | 0.10224 (7) | 0.0265 (4) | |
O6 | 0.54342 (7) | −0.07885 (15) | −0.01015 (7) | 0.0253 (4) | |
O7 | 0.62419 (7) | 0.12170 (16) | 0.02375 (8) | 0.0296 (4) | |
O8 | 0.60282 (8) | −0.00043 (17) | −0.08372 (8) | 0.0297 (4) | |
O9 | 0.65482 (9) | −0.22313 (19) | −0.02666 (9) | 0.0443 (5) | |
O10 | 0.72562 (8) | −0.0123 (2) | 0.00907 (9) | 0.0466 (5) | |
O11 | 0.58417 (9) | −0.32189 (17) | 0.06189 (9) | 0.0377 (4) | |
O12 | 0.61036 (8) | −0.18874 (17) | 0.17013 (8) | 0.0359 (4) | |
O13 | 0.65713 (8) | −0.10327 (17) | 0.08166 (8) | 0.0313 (4) | |
Mo1 | 0.653779 (10) | −0.06854 (2) | −0.002152 (10) | 0.03034 (6) | |
Mo2 | 0.584432 (10) | −0.17049 (2) | 0.090220 (10) | 0.02619 (6) | |
Mo3 | 0.549524 (9) | 0.139409 (19) | 0.023708 (9) | 0.02377 (6) | |
Mo4 | 0.484198 (10) | 0.04345 (2) | 0.116550 (10) | 0.02825 (6) | |
H5N | 0.9441 (15) | −0.079 (3) | 0.0245 (15) | 0.052 (10)* | |
H6N | 0.6554 (17) | 0.225 (4) | 0.3730 (17) | 0.070 (12)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0370 (16) | 0.0398 (16) | 0.0520 (18) | 0.0077 (13) | 0.0130 (14) | 0.0042 (14) |
C2 | 0.0447 (17) | 0.0339 (14) | 0.0431 (16) | 0.0005 (13) | 0.0172 (14) | 0.0047 (12) |
C12 | 0.052 (2) | 0.0518 (19) | 0.054 (2) | −0.0037 (16) | 0.0147 (16) | −0.0143 (16) |
C3 | 0.0297 (13) | 0.0293 (13) | 0.0369 (14) | −0.0029 (11) | 0.0144 (11) | −0.0021 (11) |
C4 | 0.0350 (14) | 0.0302 (13) | 0.0347 (14) | −0.0015 (11) | 0.0170 (12) | −0.0036 (11) |
C5 | 0.0508 (18) | 0.0310 (14) | 0.0418 (16) | 0.0035 (13) | 0.0209 (14) | 0.0030 (12) |
C6 | 0.0415 (16) | 0.0368 (15) | 0.0417 (16) | 0.0049 (13) | 0.0124 (13) | 0.0026 (12) |
C7 | 0.0340 (15) | 0.0334 (14) | 0.0504 (17) | −0.0053 (12) | 0.0210 (13) | −0.0030 (12) |
C8 | 0.0348 (14) | 0.0276 (13) | 0.0395 (15) | −0.0044 (11) | 0.0193 (12) | 0.0027 (11) |
C9 | 0.0388 (16) | 0.0433 (17) | 0.0463 (17) | 0.0006 (13) | 0.0167 (14) | 0.0015 (14) |
C10 | 0.0465 (18) | 0.0465 (18) | 0.060 (2) | 0.0088 (15) | 0.0302 (17) | 0.0102 (16) |
C11 | 0.0364 (16) | 0.0445 (17) | 0.0553 (19) | −0.0026 (13) | 0.0135 (14) | −0.0104 (15) |
C13 | 0.0322 (14) | 0.0353 (14) | 0.0350 (14) | −0.0065 (11) | 0.0148 (12) | −0.0032 (11) |
C14 | 0.0351 (14) | 0.0337 (13) | 0.0269 (13) | −0.0065 (11) | 0.0129 (11) | 0.0015 (10) |
C15 | 0.0368 (15) | 0.0476 (17) | 0.0326 (15) | −0.0007 (13) | 0.0151 (12) | 0.0020 (12) |
C16 | 0.057 (2) | 0.0530 (19) | 0.0518 (19) | 0.0047 (16) | 0.0328 (17) | 0.0121 (16) |
C17 | 0.090 (3) | 0.054 (2) | 0.050 (2) | −0.029 (2) | 0.032 (2) | −0.0212 (16) |
C18 | 0.0483 (18) | 0.0533 (19) | 0.0460 (18) | −0.0195 (15) | 0.0201 (15) | −0.0128 (15) |
N1 | 0.0347 (13) | 0.0393 (13) | 0.0417 (13) | 0.0039 (10) | 0.0152 (11) | 0.0017 (10) |
N2 | 0.0354 (12) | 0.0281 (11) | 0.0466 (13) | −0.0002 (10) | 0.0228 (11) | 0.0003 (10) |
N3 | 0.0330 (12) | 0.0308 (11) | 0.0361 (12) | −0.0041 (9) | 0.0146 (10) | −0.0018 (9) |
N4 | 0.0344 (13) | 0.0374 (13) | 0.0524 (15) | 0.0018 (10) | 0.0184 (11) | 0.0038 (11) |
N5 | 0.0660 (19) | 0.0373 (14) | 0.0538 (17) | 0.0026 (13) | 0.0357 (16) | −0.0050 (13) |
N6 | 0.093 (3) | 0.0454 (16) | 0.063 (2) | −0.0071 (16) | 0.058 (2) | −0.0098 (14) |
O1 | 0.0408 (11) | 0.0279 (9) | 0.0389 (10) | −0.0042 (8) | 0.0155 (9) | −0.0040 (8) |
O2 | 0.0472 (12) | 0.0439 (12) | 0.0516 (12) | −0.0061 (9) | 0.0253 (10) | −0.0137 (10) |
O3 | 0.0334 (10) | 0.0642 (13) | 0.0275 (10) | −0.0030 (9) | 0.0127 (8) | 0.0045 (9) |
O4 | 0.0249 (9) | 0.0288 (9) | 0.0237 (8) | −0.0023 (7) | 0.0080 (7) | 0.0039 (7) |
O5 | 0.0238 (8) | 0.0334 (9) | 0.0209 (8) | −0.0026 (7) | 0.0069 (7) | 0.0006 (7) |
O6 | 0.0222 (8) | 0.0283 (8) | 0.0248 (9) | −0.0011 (7) | 0.0082 (7) | 0.0016 (7) |
O7 | 0.0231 (9) | 0.0346 (9) | 0.0295 (9) | −0.0044 (7) | 0.0082 (7) | 0.0002 (7) |
O8 | 0.0257 (9) | 0.0386 (10) | 0.0266 (9) | −0.0013 (8) | 0.0120 (7) | 0.0029 (8) |
O9 | 0.0540 (13) | 0.0415 (11) | 0.0438 (11) | 0.0116 (10) | 0.0259 (10) | 0.0066 (9) |
O10 | 0.0281 (10) | 0.0668 (14) | 0.0460 (12) | 0.0000 (10) | 0.0153 (9) | 0.0103 (11) |
O11 | 0.0397 (11) | 0.0322 (10) | 0.0408 (11) | 0.0028 (8) | 0.0149 (9) | −0.0013 (8) |
O12 | 0.0336 (10) | 0.0447 (11) | 0.0261 (9) | −0.0011 (8) | 0.0079 (8) | 0.0070 (8) |
O13 | 0.0242 (9) | 0.0398 (10) | 0.0277 (9) | 0.0014 (8) | 0.0074 (7) | 0.0063 (8) |
Mo1 | 0.02537 (12) | 0.03820 (13) | 0.02936 (12) | 0.00348 (9) | 0.01259 (9) | 0.00555 (9) |
Mo2 | 0.02420 (11) | 0.02897 (11) | 0.02414 (11) | 0.00120 (9) | 0.00783 (9) | 0.00379 (8) |
Mo3 | 0.02227 (11) | 0.02433 (10) | 0.02358 (11) | −0.00386 (8) | 0.00752 (8) | −0.00023 (8) |
Mo4 | 0.02511 (11) | 0.03664 (12) | 0.02427 (11) | −0.00324 (9) | 0.01086 (9) | −0.00291 (9) |
C1—C2 | 1.348 (4) | C16—H16 | 0.9300 |
C1—N4 | 1.378 (4) | C17—N6 | 1.327 (5) |
C1—H1 | 0.9300 | C17—C18 | 1.384 (4) |
C2—N3 | 1.382 (3) | C17—H17 | 0.9300 |
C2—H2 | 0.9300 | C18—H18 | 0.9300 |
C12—N5 | 1.326 (4) | N5—H5N | 0.79 (3) |
C12—C11 | 1.371 (4) | N6—H6N | 0.79 (3) |
C12—H12 | 0.9300 | O1—Mo3 | 1.6964 (17) |
C3—N4 | 1.323 (3) | O2—Mo4 | 1.7042 (19) |
C3—N3 | 1.372 (3) | O3—Mo4 | 1.6934 (18) |
C3—C4 | 1.454 (4) | O4—Mo3i | 1.9479 (16) |
C4—N1 | 1.322 (3) | O4—Mo2 | 1.9753 (16) |
C4—N2 | 1.364 (3) | O4—Mo4 | 2.3728 (16) |
C5—C6 | 1.347 (4) | O5—Mo3 | 1.9483 (16) |
C5—N2 | 1.373 (3) | O5—Mo4 | 1.9967 (16) |
C5—H5 | 0.9300 | O5—Mo2 | 2.3605 (17) |
C6—N1 | 1.376 (3) | O6—Mo3i | 2.1503 (15) |
C6—H6 | 0.9300 | O6—Mo4i | 2.2878 (15) |
C7—N2 | 1.457 (3) | O6—Mo2 | 2.3212 (15) |
C7—C8 | 1.508 (4) | O6—Mo3 | 2.3995 (16) |
C7—H7A | 0.9700 | O6—Mo1 | 2.4948 (16) |
C7—H7B | 0.9700 | O7—Mo3 | 1.7390 (16) |
C8—C9 | 1.381 (4) | O7—Mo1 | 2.2578 (17) |
C8—C11 | 1.383 (4) | O8—Mo4i | 1.9163 (16) |
C9—C10 | 1.380 (4) | O8—Mo1 | 1.9172 (16) |
C9—H9 | 0.9300 | O9—Mo1 | 1.716 (2) |
C10—N5 | 1.316 (4) | O10—Mo1 | 1.6902 (19) |
C10—H10 | 0.9300 | O11—Mo2 | 1.7111 (18) |
C11—H11 | 0.9300 | O12—Mo2 | 1.6952 (17) |
C13—N3 | 1.448 (3) | O13—Mo2 | 1.9028 (17) |
C13—C14 | 1.506 (4) | O13—Mo1 | 1.9155 (17) |
C13—H13A | 0.9700 | Mo2—Mo3i | 3.2104 (3) |
C13—H13B | 0.9700 | Mo3—O4i | 1.9479 (16) |
C14—C18 | 1.378 (4) | Mo3—O6i | 2.1503 (15) |
C14—C15 | 1.391 (4) | Mo3—Mo4 | 3.1969 (3) |
C15—C16 | 1.367 (4) | Mo3—Mo2i | 3.2104 (3) |
C15—H15 | 0.9300 | Mo4—O8i | 1.9163 (16) |
C16—N6 | 1.332 (4) | Mo4—O6i | 2.2878 (15) |
C2—C1—N4 | 111.2 (3) | Mo3—O6—Mo1 | 90.14 (5) |
C2—C1—H1 | 124.4 | Mo3—O7—Mo1 | 119.69 (8) |
N4—C1—H1 | 124.4 | Mo4i—O8—Mo1 | 117.16 (8) |
C1—C2—N3 | 106.2 (2) | Mo2—O13—Mo1 | 118.19 (8) |
C1—C2—H2 | 126.9 | O10—Mo1—O9 | 104.05 (10) |
N3—C2—H2 | 126.9 | O10—Mo1—O13 | 104.68 (8) |
N5—C12—C11 | 120.1 (3) | O9—Mo1—O13 | 98.32 (8) |
N5—C12—H12 | 120.0 | O10—Mo1—O8 | 102.85 (8) |
C11—C12—H12 | 120.0 | O9—Mo1—O8 | 96.66 (8) |
N4—C3—N3 | 111.8 (2) | O13—Mo1—O8 | 144.25 (7) |
N4—C3—C4 | 125.0 (2) | O10—Mo1—O7 | 91.86 (8) |
N3—C3—C4 | 123.2 (2) | O9—Mo1—O7 | 164.00 (8) |
N1—C4—N2 | 111.4 (2) | O13—Mo1—O7 | 78.92 (7) |
N1—C4—C3 | 125.0 (2) | O8—Mo1—O7 | 77.81 (7) |
N2—C4—C3 | 123.5 (2) | O10—Mo1—O6 | 161.50 (8) |
C6—C5—N2 | 106.2 (2) | O9—Mo1—O6 | 94.41 (8) |
C6—C5—H5 | 126.9 | O13—Mo1—O6 | 73.39 (6) |
N2—C5—H5 | 126.9 | O8—Mo1—O6 | 73.24 (6) |
C5—C6—N1 | 110.8 (3) | O7—Mo1—O6 | 69.65 (5) |
C5—C6—H6 | 124.6 | O12—Mo2—O11 | 104.42 (9) |
N1—C6—H6 | 124.6 | O12—Mo2—O13 | 100.83 (8) |
N2—C7—C8 | 112.4 (2) | O11—Mo2—O13 | 100.36 (8) |
N2—C7—H7A | 109.1 | O12—Mo2—O4 | 100.93 (8) |
C8—C7—H7A | 109.1 | O11—Mo2—O4 | 98.40 (8) |
N2—C7—H7B | 109.1 | O13—Mo2—O4 | 146.58 (7) |
C8—C7—H7B | 109.1 | O12—Mo2—O6 | 161.34 (8) |
H7A—C7—H7B | 107.9 | O11—Mo2—O6 | 94.06 (7) |
C9—C8—C11 | 118.5 (3) | O13—Mo2—O6 | 77.93 (6) |
C9—C8—C7 | 120.0 (2) | O4—Mo2—O6 | 73.36 (6) |
C11—C8—C7 | 121.5 (2) | O12—Mo2—O5 | 89.34 (7) |
C10—C9—C8 | 119.5 (3) | O11—Mo2—O5 | 164.76 (7) |
C10—C9—H9 | 120.3 | O13—Mo2—O5 | 83.09 (7) |
C8—C9—H9 | 120.3 | O4—Mo2—O5 | 72.12 (6) |
N5—C10—C9 | 120.0 (3) | O6—Mo2—O5 | 72.01 (5) |
N5—C10—H10 | 120.0 | O12—Mo2—Mo3i | 135.65 (6) |
C9—C10—H10 | 120.0 | O11—Mo2—Mo3i | 85.77 (6) |
C12—C11—C8 | 119.6 (3) | O13—Mo2—Mo3i | 119.95 (5) |
C12—C11—H11 | 120.2 | O4—Mo2—Mo3i | 34.80 (5) |
C8—C11—H11 | 120.2 | O6—Mo2—Mo3i | 42.03 (4) |
N3—C13—C14 | 115.6 (2) | O5—Mo2—Mo3i | 79.71 (4) |
N3—C13—H13A | 108.4 | O1—Mo3—O7 | 105.18 (8) |
C14—C13—H13A | 108.4 | O1—Mo3—O4i | 100.78 (8) |
N3—C13—H13B | 108.4 | O7—Mo3—O4i | 96.30 (7) |
C14—C13—H13B | 108.4 | O1—Mo3—O5 | 102.49 (8) |
H13A—C13—H13B | 107.5 | O7—Mo3—O5 | 97.14 (7) |
C18—C14—C15 | 118.8 (3) | O4i—Mo3—O5 | 148.94 (7) |
C18—C14—C13 | 123.8 (3) | O1—Mo3—O6i | 99.37 (8) |
C15—C14—C13 | 117.3 (2) | O7—Mo3—O6i | 155.43 (7) |
C16—C15—C14 | 120.1 (3) | O4i—Mo3—O6i | 77.92 (6) |
C16—C15—H15 | 119.9 | O5—Mo3—O6i | 78.24 (6) |
C14—C15—H15 | 119.9 | O1—Mo3—O6 | 174.18 (7) |
N6—C16—C15 | 119.4 (3) | O7—Mo3—O6 | 80.50 (7) |
N6—C16—H16 | 120.3 | O4i—Mo3—O6 | 77.02 (6) |
C15—C16—H16 | 120.3 | O5—Mo3—O6 | 77.78 (6) |
N6—C17—C18 | 120.2 (3) | O6i—Mo3—O6 | 74.94 (6) |
N6—C17—H17 | 119.9 | O1—Mo3—Mo4 | 90.96 (6) |
C18—C17—H17 | 119.9 | O7—Mo3—Mo4 | 133.50 (6) |
C14—C18—C17 | 118.9 (3) | O4i—Mo3—Mo4 | 123.56 (5) |
C14—C18—H18 | 120.6 | O5—Mo3—Mo4 | 36.38 (5) |
C17—C18—H18 | 120.6 | O6i—Mo3—Mo4 | 45.65 (4) |
C4—N1—C6 | 104.9 (2) | O6—Mo3—Mo4 | 85.89 (4) |
C4—N2—C5 | 106.7 (2) | O1—Mo3—Mo2i | 89.91 (6) |
C4—N2—C7 | 128.9 (2) | O7—Mo3—Mo2i | 131.66 (5) |
C5—N2—C7 | 124.2 (2) | O4i—Mo3—Mo2i | 35.37 (5) |
C3—N3—C2 | 106.1 (2) | O5—Mo3—Mo2i | 124.50 (5) |
C3—N3—C13 | 129.2 (2) | O6i—Mo3—Mo2i | 46.28 (4) |
C2—N3—C13 | 124.4 (2) | O6—Mo3—Mo2i | 85.24 (4) |
C3—N4—C1 | 104.7 (2) | Mo4—Mo3—Mo2i | 90.620 (8) |
C10—N5—C12 | 122.4 (3) | O3—Mo4—O2 | 105.07 (10) |
C10—N5—H5N | 120 (2) | O3—Mo4—O8i | 99.97 (8) |
C12—N5—H5N | 118 (2) | O2—Mo4—O8i | 100.52 (9) |
C17—N6—C16 | 122.5 (3) | O3—Mo4—O5 | 99.35 (8) |
C17—N6—H6N | 125 (3) | O2—Mo4—O5 | 99.57 (8) |
C16—N6—H6N | 112 (3) | O8i—Mo4—O5 | 147.33 (7) |
Mo3i—O4—Mo2 | 109.83 (8) | O3—Mo4—O6i | 158.62 (8) |
Mo3i—O4—Mo4 | 109.92 (7) | O2—Mo4—O6i | 96.14 (8) |
Mo2—O4—Mo4 | 104.24 (7) | O8i—Mo4—O6i | 78.38 (6) |
Mo3—O5—Mo4 | 108.26 (7) | O5—Mo4—O6i | 74.06 (6) |
Mo3—O5—Mo2 | 110.22 (7) | O3—Mo4—O4 | 86.94 (8) |
Mo4—O5—Mo2 | 103.99 (7) | O2—Mo4—O4 | 166.31 (8) |
Mo3i—O6—Mo4i | 92.11 (6) | O8i—Mo4—O4 | 83.49 (7) |
Mo3i—O6—Mo2 | 91.69 (6) | O5—Mo4—O4 | 71.51 (6) |
Mo4i—O6—Mo2 | 162.46 (8) | O6i—Mo4—O4 | 71.68 (6) |
Mo3i—O6—Mo3 | 105.06 (6) | O3—Mo4—Mo3 | 134.70 (6) |
Mo4i—O6—Mo3 | 98.29 (6) | O2—Mo4—Mo3 | 87.58 (7) |
Mo2—O6—Mo3 | 97.23 (6) | O8i—Mo4—Mo3 | 120.61 (5) |
Mo3i—O6—Mo1 | 164.78 (8) | O5—Mo4—Mo3 | 35.36 (5) |
Mo4i—O6—Mo1 | 86.20 (5) | O6i—Mo4—Mo3 | 42.23 (4) |
Mo2—O6—Mo1 | 85.65 (5) | O4—Mo4—Mo3 | 79.18 (4) |
N4—C1—C2—N3 | 0.4 (3) | Mo3—O6—Mo2—Mo3i | 105.42 (7) |
N4—C3—C4—N1 | 174.9 (3) | Mo1—O6—Mo2—Mo3i | −164.99 (8) |
N3—C3—C4—N1 | −1.9 (4) | Mo3—O5—Mo2—O12 | 166.34 (9) |
N4—C3—C4—N2 | −1.2 (4) | Mo4—O5—Mo2—O12 | −77.83 (8) |
N3—C3—C4—N2 | −178.0 (2) | Mo3—O5—Mo2—O11 | −38.8 (3) |
N2—C5—C6—N1 | 0.2 (3) | Mo4—O5—Mo2—O11 | 77.0 (3) |
N2—C7—C8—C9 | −161.8 (2) | Mo3—O5—Mo2—O13 | 65.35 (8) |
N2—C7—C8—C11 | 20.1 (4) | Mo4—O5—Mo2—O13 | −178.82 (8) |
C11—C8—C9—C10 | −0.4 (4) | Mo3—O5—Mo2—O4 | −91.95 (8) |
C7—C8—C9—C10 | −178.5 (3) | Mo4—O5—Mo2—O4 | 23.89 (6) |
C8—C9—C10—N5 | −0.6 (4) | Mo3—O5—Mo2—O6 | −14.16 (7) |
N5—C12—C11—C8 | −0.1 (5) | Mo4—O5—Mo2—O6 | 101.68 (7) |
C9—C8—C11—C12 | 0.7 (4) | Mo3—O5—Mo2—Mo3i | −56.87 (6) |
C7—C8—C11—C12 | 178.8 (3) | Mo4—O5—Mo2—Mo3i | 58.97 (5) |
N3—C13—C14—C18 | −7.0 (4) | Mo1—O7—Mo3—O1 | 179.96 (9) |
N3—C13—C14—C15 | 175.5 (2) | Mo1—O7—Mo3—O4i | −77.03 (10) |
C18—C14—C15—C16 | −1.4 (4) | Mo1—O7—Mo3—O5 | 74.91 (9) |
C13—C14—C15—C16 | 176.2 (2) | Mo1—O7—Mo3—O6i | −2.4 (2) |
C14—C15—C16—N6 | −0.5 (4) | Mo1—O7—Mo3—O6 | −1.37 (8) |
C15—C14—C18—C17 | 2.7 (4) | Mo1—O7—Mo3—Mo4 | 73.62 (11) |
C13—C14—C18—C17 | −174.8 (3) | Mo1—O7—Mo3—Mo2i | −76.20 (10) |
N6—C17—C18—C14 | −2.0 (5) | Mo4—O5—Mo3—O1 | 74.24 (9) |
N2—C4—N1—C6 | 2.3 (3) | Mo2—O5—Mo3—O1 | −172.64 (8) |
C3—C4—N1—C6 | −174.3 (3) | Mo4—O5—Mo3—O7 | −178.43 (8) |
C5—C6—N1—C4 | −1.5 (3) | Mo2—O5—Mo3—O7 | −65.30 (8) |
N1—C4—N2—C5 | −2.2 (3) | Mo4—O5—Mo3—O4i | −63.43 (16) |
C3—C4—N2—C5 | 174.4 (2) | Mo2—O5—Mo3—O4i | 49.69 (16) |
N1—C4—N2—C7 | −177.1 (2) | Mo4—O5—Mo3—O6i | −22.90 (7) |
C3—C4—N2—C7 | −0.5 (4) | Mo2—O5—Mo3—O6i | 90.22 (7) |
C6—C5—N2—C4 | 1.2 (3) | Mo4—O5—Mo3—O6 | −99.81 (8) |
C6—C5—N2—C7 | 176.4 (2) | Mo2—O5—Mo3—O6 | 13.31 (6) |
C8—C7—N2—C4 | 79.5 (3) | Mo2—O5—Mo3—Mo4 | 113.12 (10) |
C8—C7—N2—C5 | −94.6 (3) | Mo4—O5—Mo3—Mo2i | −24.40 (10) |
N4—C3—N3—C2 | 0.0 (3) | Mo2—O5—Mo3—Mo2i | 88.72 (7) |
C4—C3—N3—C2 | 177.2 (2) | Mo3i—O6—Mo3—O7 | −179.56 (8) |
N4—C3—N3—C13 | −174.4 (2) | Mo4i—O6—Mo3—O7 | −85.10 (7) |
C4—C3—N3—C13 | 2.8 (4) | Mo2—O6—Mo3—O7 | 86.71 (7) |
C1—C2—N3—C3 | −0.2 (3) | Mo1—O6—Mo3—O7 | 1.08 (6) |
C1—C2—N3—C13 | 174.5 (2) | Mo3i—O6—Mo3—O4i | −80.77 (7) |
C14—C13—N3—C3 | −85.4 (3) | Mo4i—O6—Mo3—O4i | 13.69 (6) |
C14—C13—N3—C2 | 101.1 (3) | Mo2—O6—Mo3—O4i | −174.50 (7) |
N3—C3—N4—C1 | 0.3 (3) | Mo1—O6—Mo3—O4i | 99.87 (6) |
C4—C3—N4—C1 | −176.9 (3) | Mo3i—O6—Mo3—O5 | 80.93 (7) |
C2—C1—N4—C3 | −0.4 (3) | Mo4i—O6—Mo3—O5 | 175.39 (7) |
C9—C10—N5—C12 | 1.3 (5) | Mo2—O6—Mo3—O5 | −12.80 (6) |
C11—C12—N5—C10 | −1.0 (5) | Mo1—O6—Mo3—O5 | −98.43 (6) |
C18—C17—N6—C16 | 0.0 (5) | Mo3i—O6—Mo3—O6i | 0.0 |
C15—C16—N6—C17 | 1.3 (5) | Mo4i—O6—Mo3—O6i | 94.46 (7) |
Mo2—O13—Mo1—O10 | −179.55 (10) | Mo2—O6—Mo3—O6i | −93.73 (7) |
Mo2—O13—Mo1—O9 | −72.58 (11) | Mo1—O6—Mo3—O6i | −179.36 (9) |
Mo2—O13—Mo1—O8 | 41.23 (18) | Mo3i—O6—Mo3—Mo4 | 45.06 (5) |
Mo2—O13—Mo1—O7 | 91.42 (10) | Mo4i—O6—Mo3—Mo4 | 139.52 (5) |
Mo2—O13—Mo1—O6 | 19.57 (8) | Mo2—O6—Mo3—Mo4 | −48.67 (4) |
Mo4i—O8—Mo1—O10 | 179.11 (10) | Mo1—O6—Mo3—Mo4 | −134.30 (4) |
Mo4i—O8—Mo1—O9 | 73.01 (11) | Mo3i—O6—Mo3—Mo2i | −45.91 (5) |
Mo4i—O8—Mo1—O13 | −41.29 (18) | Mo4i—O6—Mo3—Mo2i | 48.55 (4) |
Mo4i—O8—Mo1—O7 | −91.75 (10) | Mo2—O6—Mo3—Mo2i | −139.64 (5) |
Mo4i—O8—Mo1—O6 | −19.61 (8) | Mo1—O6—Mo3—Mo2i | 134.73 (4) |
Mo3—O7—Mo1—O10 | −179.44 (10) | Mo3—O5—Mo4—O3 | −179.00 (9) |
Mo3—O7—Mo1—O9 | 6.6 (3) | Mo2—O5—Mo4—O3 | 63.79 (9) |
Mo3—O7—Mo1—O13 | −74.85 (10) | Mo3—O5—Mo4—O2 | −71.85 (10) |
Mo3—O7—Mo1—O8 | 77.82 (10) | Mo2—O5—Mo4—O2 | 170.94 (8) |
Mo3—O7—Mo1—O6 | 1.39 (8) | Mo3—O5—Mo4—O8i | 55.44 (16) |
Mo3i—O6—Mo1—O10 | 178.9 (3) | Mo2—O5—Mo4—O8i | −61.77 (14) |
Mo4i—O6—Mo1—O10 | 94.8 (2) | Mo3—O5—Mo4—O6i | 21.86 (7) |
Mo2—O6—Mo1—O10 | −100.7 (2) | Mo2—O5—Mo4—O6i | −95.35 (7) |
Mo3—O6—Mo1—O10 | −3.5 (3) | Mo3—O5—Mo4—O4 | 97.44 (8) |
Mo3i—O6—Mo1—O9 | 2.9 (3) | Mo2—O5—Mo4—O4 | −19.77 (5) |
Mo4i—O6—Mo1—O9 | −81.12 (8) | Mo2—O5—Mo4—Mo3 | −117.21 (10) |
Mo2—O6—Mo1—O9 | 83.34 (7) | Mo3i—O4—Mo4—O3 | 165.30 (9) |
Mo3—O6—Mo1—O9 | −179.42 (7) | Mo2—O4—Mo4—O3 | −77.04 (8) |
Mo3i—O6—Mo1—O13 | −94.4 (3) | Mo3i—O4—Mo4—O2 | −43.0 (4) |
Mo4i—O6—Mo1—O13 | −178.50 (7) | Mo2—O4—Mo4—O2 | 74.6 (3) |
Mo2—O6—Mo1—O13 | −14.04 (6) | Mo3i—O4—Mo4—O8i | 64.90 (8) |
Mo3—O6—Mo1—O13 | 83.20 (7) | Mo2—O4—Mo4—O8i | −177.44 (8) |
Mo3i—O6—Mo1—O8 | 98.6 (3) | Mo3i—O4—Mo4—O5 | −93.79 (8) |
Mo4i—O6—Mo1—O8 | 14.51 (6) | Mo2—O4—Mo4—O5 | 23.87 (7) |
Mo2—O6—Mo1—O8 | 178.97 (7) | Mo3i—O4—Mo4—O6i | −14.99 (7) |
Mo3—O6—Mo1—O8 | −83.79 (7) | Mo2—O4—Mo4—O6i | 102.67 (7) |
Mo3i—O6—Mo1—O7 | −178.5 (3) | Mo3i—O4—Mo4—Mo3 | −58.03 (6) |
Mo4i—O6—Mo1—O7 | 97.43 (6) | Mo2—O4—Mo4—Mo3 | 59.63 (5) |
Mo2—O6—Mo1—O7 | −98.11 (6) | O1—Mo3—Mo4—O3 | −108.60 (12) |
Mo3—O6—Mo1—O7 | −0.87 (5) | O7—Mo3—Mo4—O3 | 3.54 (13) |
Mo1—O13—Mo2—O12 | 178.35 (10) | O4i—Mo3—Mo4—O3 | 147.77 (11) |
Mo1—O13—Mo2—O11 | 71.32 (11) | O5—Mo3—Mo4—O3 | 1.39 (12) |
Mo1—O13—Mo2—O4 | −51.82 (18) | O6i—Mo3—Mo4—O3 | 149.20 (12) |
Mo1—O13—Mo2—O6 | −20.65 (9) | O6—Mo3—Mo4—O3 | 76.30 (11) |
Mo1—O13—Mo2—O5 | −93.66 (10) | Mo2i—Mo3—Mo4—O3 | 161.48 (10) |
Mo1—O13—Mo2—Mo3i | −19.76 (12) | O1—Mo3—Mo4—O2 | 0.31 (9) |
Mo3i—O4—Mo2—O12 | −176.50 (8) | O7—Mo3—Mo4—O2 | 112.46 (10) |
Mo4—O4—Mo2—O12 | 65.77 (8) | O4i—Mo3—Mo4—O2 | −103.32 (9) |
Mo3i—O4—Mo2—O11 | −69.94 (9) | O5—Mo3—Mo4—O2 | 110.30 (11) |
Mo4—O4—Mo2—O11 | 172.33 (8) | O6i—Mo3—Mo4—O2 | −101.89 (9) |
Mo3i—O4—Mo2—O13 | 53.69 (16) | O6—Mo3—Mo4—O2 | −174.78 (8) |
Mo4—O4—Mo2—O13 | −64.03 (14) | Mo2i—Mo3—Mo4—O2 | −89.60 (7) |
Mo3i—O4—Mo2—O6 | 21.81 (7) | O1—Mo3—Mo4—O8i | 101.11 (9) |
Mo4—O4—Mo2—O6 | −95.92 (7) | O7—Mo3—Mo4—O8i | −146.74 (10) |
Mo3i—O4—Mo2—O5 | 97.78 (8) | O4i—Mo3—Mo4—O8i | −2.52 (9) |
Mo4—O4—Mo2—O5 | −19.95 (5) | O5—Mo3—Mo4—O8i | −148.90 (10) |
Mo4—O4—Mo2—Mo3i | −117.73 (10) | O6i—Mo3—Mo4—O8i | −1.09 (8) |
Mo3i—O6—Mo2—O12 | −93.0 (2) | O6—Mo3—Mo4—O8i | −73.98 (7) |
Mo4i—O6—Mo2—O12 | 164.5 (2) | Mo2i—Mo3—Mo4—O8i | 11.20 (6) |
Mo3—O6—Mo2—O12 | 12.4 (2) | O1—Mo3—Mo4—O5 | −109.99 (10) |
Mo1—O6—Mo2—O12 | 102.0 (2) | O7—Mo3—Mo4—O5 | 2.15 (11) |
Mo3i—O6—Mo2—O11 | 79.11 (8) | O4i—Mo3—Mo4—O5 | 146.38 (10) |
Mo4i—O6—Mo2—O11 | −23.4 (3) | O6i—Mo3—Mo4—O5 | 147.81 (10) |
Mo3—O6—Mo2—O11 | −175.48 (7) | O6—Mo3—Mo4—O5 | 74.92 (9) |
Mo1—O6—Mo2—O11 | −85.89 (7) | Mo2i—Mo3—Mo4—O5 | 160.09 (8) |
Mo3i—O6—Mo2—O13 | 178.84 (7) | O1—Mo3—Mo4—O6i | 102.20 (9) |
Mo4i—O6—Mo2—O13 | 76.4 (3) | O7—Mo3—Mo4—O6i | −145.65 (10) |
Mo3—O6—Mo2—O13 | −75.74 (7) | O4i—Mo3—Mo4—O6i | −1.43 (8) |
Mo1—O6—Mo2—O13 | 13.85 (6) | O5—Mo3—Mo4—O6i | −147.81 (10) |
Mo3i—O6—Mo2—O4 | −18.46 (6) | O6—Mo3—Mo4—O6i | −72.89 (8) |
Mo4i—O6—Mo2—O4 | −120.9 (3) | Mo2i—Mo3—Mo4—O6i | 12.29 (6) |
Mo3—O6—Mo2—O4 | 86.95 (7) | O1—Mo3—Mo4—O4 | 176.80 (7) |
Mo1—O6—Mo2—O4 | 176.54 (7) | O7—Mo3—Mo4—O4 | −71.06 (8) |
Mo3i—O6—Mo2—O5 | −94.59 (6) | O4i—Mo3—Mo4—O4 | 73.17 (8) |
Mo4i—O6—Mo2—O5 | 162.9 (3) | O5—Mo3—Mo4—O4 | −73.21 (9) |
Mo3—O6—Mo2—O5 | 10.83 (5) | O6i—Mo3—Mo4—O4 | 74.60 (7) |
Mo1—O6—Mo2—O5 | 100.42 (5) | O6—Mo3—Mo4—O4 | 1.70 (5) |
Mo4i—O6—Mo2—Mo3i | −102.5 (3) | Mo2i—Mo3—Mo4—O4 | 86.88 (4) |
Symmetry code: (i) −x+1, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N5—H5N···O11ii | 0.79 (3) | 2.09 (3) | 2.801 (3) | 150 (3) |
N6—H6N···O9iii | 0.79 (3) | 2.29 (4) | 2.923 (3) | 138 (3) |
Symmetry codes: (ii) −x+3/2, −y−1/2, −z; (iii) x, −y, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | (C18H18N6)2[Mo8O26] |
Mr | 1820.28 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 23.1640 (4), 10.4740 (5), 22.7770 (8) |
β (°) | 112.494 (1) |
V (Å3) | 5105.7 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.00 |
Crystal size (mm) | 0.28 × 0.26 × 0.19 |
Data collection | |
Diffractometer | Bruker APEX CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.481, 0.684 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15475, 6141, 5242 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.668 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.023, 0.054, 1.02 |
No. of reflections | 6141 |
No. of parameters | 378 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.32, −0.48 |
Computer programs: SMART (Bruker, 1997), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL-Plus (Sheldrick, 1990).
D—H···A | D—H | H···A | D···A | D—H···A |
N5—H5N···O11i | 0.79 (3) | 2.09 (3) | 2.801 (3) | 150 (3) |
N6—H6N···O9ii | 0.79 (3) | 2.29 (4) | 2.923 (3) | 138 (3) |
Symmetry codes: (i) −x+3/2, −y−1/2, −z; (ii) x, −y, z+1/2. |
Important advances in polyoxometalate (POM) chemistry (Pope, 1983) have recently been made in the coordination chemistry of polyoxoanions with classical transition metal coordination complexes or fragments. The introduction of metal complexes does not only enrich the frameworks of polyoxometalates but also ameliorates their electronic and magnetic properties (Chen et al., 2002; Lu et al., 2002; Reinoso et al., 2005). During our ongoing studies of such materials, we obtained the title compound, and present its crystal structure here.
The asymmetric part of the unit cell contains each one [H2L]2+ cation 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. Through N—H···O hydrogen bonds each protonated [H2L]2+ cation is linked two [Mo8O26]4- anions, and each [Mo8O26]4- anion joins four protonated [H2L]2+ cations (see the hydrogen bonding table for numerical values). The hydrogen bonds in the title compound thus create a two-dimensional supramolecular layerlike structure (Fig. 2).