Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806016461/hb2046sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806016461/hb2046Isup2.hkl |
CCDC reference: 610783
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.
[Mo(C36H44N4)O]2[Mo6O19] | Z = 1 |
Mr = 2169.02 | F(000) = 1080 |
Triclinic, P1 | Dx = 1.836 Mg m−3 |
Hall symbol: -P 1 | Melting point: not measured K |
a = 11.5979 (11) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.4762 (13) Å | Cell parameters from 2294 reflections |
c = 14.5563 (15) Å | θ = 2.6–24.8° |
α = 62.426 (2)° | µ = 1.31 mm−1 |
β = 77.652 (2)° | T = 223 K |
γ = 79.594 (2)° | Plate, purple |
V = 1961.2 (3) Å3 | 0.18 × 0.14 × 0.08 mm |
Bruker SMART CCD diffractometer | 7157 independent reflections |
Radiation source: fine-focus sealed tube | 4809 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
Detector resolution: 8.366 pixels mm-1 | θmax = 25.4°, θmin = 1.6° |
π and ω scans | h = −13→10 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −16→16 |
Tmin = 0.798, Tmax = 0.902 | l = −17→16 |
11847 measured reflections |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.168 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0945P)2] where P = (Fo2 + 2Fc2)/3 |
7157 reflections | (Δ/σ)max = 0.001 |
501 parameters | Δρmax = 2.93 e Å−3 |
0 restraints | Δρmin = −0.74 e Å−3 |
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 | 0.4050 (7) | 0.3595 (7) | 0.2723 (6) | 0.0245 (19) | |
C2 | 0.3906 (8) | 0.4451 (7) | 0.1692 (6) | 0.028 (2) | |
C3 | 0.3147 (8) | 0.4109 (7) | 0.1303 (6) | 0.029 (2) | |
C4 | 0.2871 (7) | 0.2995 (7) | 0.2079 (6) | 0.0254 (19) | |
C5 | 0.2244 (8) | 0.2143 (7) | 0.2157 (6) | 0.0237 (18) | |
C6 | 0.1747 (8) | 0.1917 (7) | 0.1468 (6) | 0.028 (2) | |
C7 | 0.1330 (8) | 0.0874 (7) | 0.2058 (7) | 0.0259 (19) | |
C8 | 0.1562 (8) | 0.0451 (7) | 0.3102 (7) | 0.0267 (19) | |
C9 | 0.1230 (8) | −0.0572 (7) | 0.3940 (7) | 0.031 (2) | |
H9 | 0.0876 | −0.0987 | 0.3723 | 0.037* | |
C10 | 0.1287 (8) | −0.1115 (7) | 0.4979 (7) | 0.029 (2) | |
H10 | 0.0968 | −0.1812 | 0.5306 | 0.035* | |
C11 | 0.1715 (7) | −0.0877 (7) | 0.5687 (6) | 0.0253 (19) | |
C12 | 0.1597 (8) | −0.1589 (7) | 0.6814 (7) | 0.0266 (19) | |
C13 | 0.2097 (8) | −0.1092 (7) | 0.7255 (7) | 0.033 (2) | |
C14 | 0.2501 (8) | −0.0053 (7) | 0.6400 (6) | 0.0250 (19) | |
C15 | 0.3122 (8) | 0.0812 (7) | 0.6302 (6) | 0.0261 (19) | |
C16 | 0.3506 (8) | 0.1116 (7) | 0.6989 (7) | 0.028 (2) | |
C17 | 0.4217 (8) | 0.2014 (7) | 0.6352 (7) | 0.028 (2) | |
C18 | 0.4214 (7) | 0.2244 (7) | 0.5283 (6) | 0.0263 (19) | |
C19 | 0.4779 (8) | 0.3137 (7) | 0.4433 (7) | 0.0276 (19) | |
H19 | 0.5326 | 0.3417 | 0.4625 | 0.033* | |
C20 | 0.4706 (8) | 0.3697 (7) | 0.3367 (7) | 0.031 (2) | |
H20 | 0.5214 | 0.4273 | 0.2998 | 0.037* | |
C21 | 0.4440 (8) | 0.5554 (7) | 0.1158 (6) | 0.032 (2) | |
H21A | 0.5226 | 0.5437 | 0.1357 | 0.038* | |
H21B | 0.4544 | 0.5815 | 0.0397 | 0.038* | |
C22 | 0.3710 (10) | 0.6447 (8) | 0.1419 (8) | 0.052 (3) | |
H22A | 0.2966 | 0.6635 | 0.1148 | 0.079* | |
H22B | 0.4138 | 0.7111 | 0.1107 | 0.079* | |
H22C | 0.3553 | 0.6176 | 0.2174 | 0.079* | |
C23 | 0.2581 (9) | 0.4849 (7) | 0.0331 (6) | 0.033 (2) | |
H23A | 0.2647 | 0.4440 | −0.0089 | 0.040* | |
H23B | 0.3013 | 0.5519 | −0.0092 | 0.040* | |
C24 | 0.1289 (9) | 0.5211 (9) | 0.0587 (8) | 0.048 (3) | |
H24A | 0.0869 | 0.4552 | 0.1048 | 0.071* | |
H24B | 0.0944 | 0.5623 | −0.0055 | 0.071* | |
H24C | 0.1226 | 0.5690 | 0.0932 | 0.071* | |
C25 | 0.1746 (9) | 0.2603 (9) | 0.0308 (7) | 0.043 (3) | |
H25A | 0.1488 | 0.3390 | 0.0155 | 0.052* | |
H25B | 0.1183 | 0.2330 | 0.0082 | 0.052* | |
C26 | 0.2981 (11) | 0.2521 (10) | −0.0295 (8) | 0.058 (3) | |
H26A | 0.3544 | 0.2760 | −0.0049 | 0.087* | |
H26B | 0.2972 | 0.3003 | −0.1037 | 0.087* | |
H26C | 0.3211 | 0.1750 | −0.0184 | 0.087* | |
C27 | 0.0759 (9) | 0.0245 (8) | 0.1668 (8) | 0.040 (2) | |
H27A | 0.0115 | −0.0147 | 0.2208 | 0.049* | |
H27B | 0.0410 | 0.0787 | 0.1043 | 0.049* | |
C28 | 0.1617 (11) | −0.0597 (9) | 0.1404 (9) | 0.054 (3) | |
H28A | 0.2300 | −0.0231 | 0.0928 | 0.080* | |
H28B | 0.1233 | −0.0902 | 0.1073 | 0.080* | |
H28C | 0.1872 | −0.1201 | 0.2041 | 0.080* | |
C29 | 0.1053 (9) | −0.2697 (7) | 0.7357 (7) | 0.036 (2) | |
H29A | 0.0432 | −0.2661 | 0.6977 | 0.043* | |
H29B | 0.0682 | −0.2822 | 0.8068 | 0.043* | |
C30 | 0.1967 (10) | −0.3681 (8) | 0.7415 (8) | 0.047 (3) | |
H30A | 0.2358 | −0.3548 | 0.6714 | 0.071* | |
H30B | 0.1575 | −0.4367 | 0.7731 | 0.071* | |
H30C | 0.2550 | −0.3756 | 0.7837 | 0.071* | |
C31 | 0.2300 (9) | −0.1600 (8) | 0.8364 (7) | 0.035 (2) | |
H31A | 0.1803 | −0.2222 | 0.8791 | 0.042* | |
H31B | 0.2070 | −0.1035 | 0.8633 | 0.042* | |
C32 | 0.3606 (10) | −0.2036 (8) | 0.8457 (8) | 0.049 (3) | |
H32A | 0.3817 | −0.2635 | 0.8241 | 0.073* | |
H32B | 0.3727 | −0.2322 | 0.9179 | 0.073* | |
H32C | 0.4100 | −0.1427 | 0.8011 | 0.073* | |
C33 | 0.3146 (9) | 0.0755 (8) | 0.8142 (7) | 0.035 (2) | |
H33A | 0.3676 | 0.1036 | 0.8392 | 0.042* | |
H33B | 0.3224 | −0.0068 | 0.8514 | 0.042* | |
C34 | 0.1877 (10) | 0.1196 (10) | 0.8382 (8) | 0.050 (3) | |
H34A | 0.1825 | 0.2008 | 0.8106 | 0.076* | |
H34B | 0.1630 | 0.0866 | 0.9135 | 0.076* | |
H34C | 0.1364 | 0.0998 | 0.8059 | 0.076* | |
C35 | 0.4866 (9) | 0.2611 (9) | 0.6709 (7) | 0.040 (2) | |
H35A | 0.4905 | 0.3397 | 0.6186 | 0.049* | |
H35B | 0.4438 | 0.2600 | 0.7371 | 0.049* | |
C36 | 0.6053 (12) | 0.2070 (12) | 0.6852 (11) | 0.078 (4) | |
H36A | 0.6015 | 0.1278 | 0.7325 | 0.118* | |
H36B | 0.6437 | 0.2416 | 0.7146 | 0.118* | |
H36C | 0.6503 | 0.2155 | 0.6181 | 0.118* | |
Mo1 | 0.32309 (6) | 0.11342 (6) | 0.41409 (5) | 0.0216 (2) | |
Mo2 | 0.07639 (7) | 0.34445 (6) | 0.47186 (6) | 0.0254 (2) | |
Mo3 | −0.18862 (7) | 0.47653 (6) | 0.48692 (6) | 0.0287 (2) | |
Mo4 | −0.03248 (7) | 0.38596 (6) | 0.67966 (6) | 0.0298 (2) | |
N1 | 0.3404 (6) | 0.2729 (5) | 0.2940 (5) | 0.0260 (16) | |
N2 | 0.2144 (6) | 0.1219 (5) | 0.3148 (5) | 0.0214 (15) | |
N3 | 0.2283 (6) | 0.0028 (5) | 0.5479 (5) | 0.0244 (16) | |
N4 | 0.3548 (6) | 0.1533 (5) | 0.5263 (5) | 0.0225 (15) | |
O1 | 0.4427 (6) | 0.0366 (5) | 0.3927 (5) | 0.0404 (16) | |
O2 | 0.1314 (5) | 0.2315 (5) | 0.4491 (5) | 0.0297 (14) | |
O3 | 0.2125 (5) | 0.3930 (5) | 0.4871 (5) | 0.0307 (14) | |
O4 | 0.0330 (6) | 0.2802 (4) | 0.6208 (4) | 0.0304 (14) | |
O5 | −0.0905 (5) | 0.3571 (5) | 0.4635 (5) | 0.0280 (14) | |
O6 | 0.0882 (5) | 0.4679 (5) | 0.3308 (4) | 0.0298 (14) | |
O7 | −0.1265 (5) | 0.5771 (5) | 0.3437 (4) | 0.0302 (14) | |
O8 | −0.1783 (6) | 0.3891 (5) | 0.6325 (5) | 0.0364 (16) | |
O9 | −0.0557 (6) | 0.3021 (5) | 0.8094 (5) | 0.0428 (17) | |
O10 | −0.3252 (6) | 0.4622 (6) | 0.4757 (6) | 0.0451 (17) | |
O11 | 0.0000 | 0.5000 | 0.5000 | 0.0208 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.022 (5) | 0.026 (4) | 0.027 (5) | −0.014 (4) | 0.007 (4) | −0.013 (4) |
C2 | 0.031 (5) | 0.027 (5) | 0.026 (5) | −0.013 (4) | 0.008 (4) | −0.013 (4) |
C3 | 0.029 (5) | 0.030 (5) | 0.024 (4) | −0.004 (4) | 0.002 (4) | −0.010 (4) |
C4 | 0.025 (5) | 0.030 (5) | 0.025 (4) | −0.003 (4) | −0.005 (4) | −0.015 (4) |
C5 | 0.028 (5) | 0.023 (4) | 0.024 (4) | −0.013 (4) | 0.000 (3) | −0.012 (4) |
C6 | 0.029 (5) | 0.039 (5) | 0.020 (4) | −0.014 (4) | −0.001 (4) | −0.014 (4) |
C7 | 0.027 (5) | 0.026 (4) | 0.030 (5) | −0.010 (4) | −0.002 (4) | −0.015 (4) |
C8 | 0.023 (5) | 0.025 (4) | 0.033 (5) | −0.006 (4) | 0.000 (4) | −0.014 (4) |
C9 | 0.042 (6) | 0.030 (5) | 0.030 (5) | −0.016 (4) | −0.001 (4) | −0.017 (4) |
C10 | 0.037 (6) | 0.027 (5) | 0.031 (5) | −0.016 (4) | −0.005 (4) | −0.013 (4) |
C11 | 0.021 (5) | 0.027 (4) | 0.025 (4) | −0.011 (4) | 0.006 (3) | −0.009 (4) |
C12 | 0.024 (5) | 0.026 (4) | 0.032 (5) | −0.009 (4) | 0.001 (4) | −0.015 (4) |
C13 | 0.039 (6) | 0.033 (5) | 0.030 (5) | −0.011 (4) | 0.005 (4) | −0.018 (4) |
C14 | 0.025 (5) | 0.022 (4) | 0.029 (5) | −0.005 (4) | 0.002 (4) | −0.013 (4) |
C15 | 0.029 (5) | 0.028 (5) | 0.022 (4) | −0.010 (4) | −0.001 (4) | −0.010 (4) |
C16 | 0.027 (5) | 0.036 (5) | 0.027 (5) | −0.016 (4) | −0.007 (4) | −0.014 (4) |
C17 | 0.031 (5) | 0.033 (5) | 0.030 (5) | −0.012 (4) | −0.001 (4) | −0.020 (4) |
C18 | 0.023 (5) | 0.023 (4) | 0.030 (5) | −0.012 (4) | 0.001 (4) | −0.007 (4) |
C19 | 0.024 (5) | 0.038 (5) | 0.032 (5) | −0.014 (4) | −0.006 (4) | −0.020 (4) |
C20 | 0.027 (5) | 0.033 (5) | 0.033 (5) | −0.013 (4) | 0.002 (4) | −0.014 (4) |
C21 | 0.037 (6) | 0.034 (5) | 0.021 (4) | −0.025 (4) | 0.013 (4) | −0.009 (4) |
C22 | 0.063 (8) | 0.039 (6) | 0.047 (6) | −0.021 (5) | 0.019 (5) | −0.018 (5) |
C23 | 0.049 (6) | 0.029 (5) | 0.019 (4) | −0.023 (4) | 0.005 (4) | −0.005 (4) |
C24 | 0.052 (7) | 0.049 (6) | 0.038 (6) | −0.010 (5) | −0.012 (5) | −0.012 (5) |
C25 | 0.060 (7) | 0.049 (6) | 0.026 (5) | −0.025 (5) | −0.009 (5) | −0.013 (5) |
C26 | 0.082 (9) | 0.059 (7) | 0.033 (6) | −0.027 (6) | 0.018 (6) | −0.023 (5) |
C27 | 0.055 (7) | 0.042 (6) | 0.035 (5) | −0.026 (5) | −0.005 (5) | −0.019 (5) |
C28 | 0.077 (9) | 0.045 (6) | 0.055 (7) | −0.013 (6) | −0.018 (6) | −0.029 (6) |
C29 | 0.050 (6) | 0.026 (5) | 0.030 (5) | −0.023 (4) | −0.001 (4) | −0.007 (4) |
C30 | 0.065 (8) | 0.036 (6) | 0.043 (6) | −0.017 (5) | −0.003 (5) | −0.017 (5) |
C31 | 0.046 (6) | 0.033 (5) | 0.028 (5) | −0.022 (4) | 0.003 (4) | −0.011 (4) |
C32 | 0.076 (9) | 0.034 (5) | 0.037 (6) | −0.006 (5) | −0.025 (5) | −0.009 (5) |
C33 | 0.046 (6) | 0.037 (5) | 0.030 (5) | −0.016 (4) | −0.008 (4) | −0.014 (4) |
C34 | 0.049 (7) | 0.071 (8) | 0.038 (6) | −0.017 (6) | 0.010 (5) | −0.033 (6) |
C35 | 0.047 (7) | 0.054 (6) | 0.027 (5) | −0.021 (5) | −0.007 (4) | −0.017 (5) |
C36 | 0.078 (10) | 0.085 (10) | 0.100 (11) | −0.034 (8) | −0.028 (8) | −0.049 (9) |
Mo1 | 0.0234 (4) | 0.0215 (4) | 0.0213 (4) | −0.0085 (3) | −0.0008 (3) | −0.0095 (3) |
Mo2 | 0.0254 (4) | 0.0217 (4) | 0.0339 (4) | −0.0074 (3) | 0.0006 (3) | −0.0166 (3) |
Mo3 | 0.0211 (4) | 0.0312 (4) | 0.0414 (5) | −0.0109 (3) | −0.0003 (3) | −0.0214 (4) |
Mo4 | 0.0346 (5) | 0.0267 (4) | 0.0255 (4) | −0.0102 (3) | 0.0027 (3) | −0.0099 (3) |
N1 | 0.030 (4) | 0.022 (4) | 0.026 (4) | −0.011 (3) | 0.001 (3) | −0.009 (3) |
N2 | 0.026 (4) | 0.025 (4) | 0.019 (3) | −0.014 (3) | −0.003 (3) | −0.010 (3) |
N3 | 0.032 (4) | 0.020 (4) | 0.024 (4) | −0.014 (3) | −0.001 (3) | −0.009 (3) |
N4 | 0.031 (4) | 0.026 (4) | 0.014 (3) | −0.009 (3) | −0.002 (3) | −0.010 (3) |
O1 | 0.047 (4) | 0.036 (4) | 0.043 (4) | −0.007 (3) | −0.011 (3) | −0.018 (3) |
O2 | 0.027 (4) | 0.026 (3) | 0.034 (3) | −0.008 (3) | −0.003 (3) | −0.011 (3) |
O3 | 0.020 (3) | 0.028 (3) | 0.051 (4) | −0.004 (3) | −0.001 (3) | −0.025 (3) |
O4 | 0.043 (4) | 0.021 (3) | 0.028 (3) | −0.009 (3) | 0.003 (3) | −0.013 (3) |
O5 | 0.021 (3) | 0.025 (3) | 0.042 (4) | −0.012 (2) | 0.002 (3) | −0.017 (3) |
O6 | 0.038 (4) | 0.028 (3) | 0.021 (3) | −0.010 (3) | 0.004 (3) | −0.010 (3) |
O7 | 0.036 (4) | 0.033 (3) | 0.029 (3) | −0.010 (3) | −0.009 (3) | −0.017 (3) |
O8 | 0.037 (4) | 0.036 (4) | 0.034 (4) | −0.020 (3) | 0.008 (3) | −0.013 (3) |
O9 | 0.060 (5) | 0.030 (3) | 0.031 (4) | −0.010 (3) | −0.004 (3) | −0.006 (3) |
O10 | 0.028 (4) | 0.053 (4) | 0.063 (5) | −0.013 (3) | −0.001 (3) | −0.033 (4) |
O11 | 0.015 (4) | 0.023 (4) | 0.026 (4) | −0.008 (3) | −0.006 (3) | −0.009 (3) |
C1—N1 | 1.377 (10) | C27—H27A | 0.9800 |
C1—C20 | 1.391 (12) | C27—H27B | 0.9800 |
C1—C2 | 1.431 (12) | C28—H28A | 0.9700 |
C2—C3 | 1.381 (13) | C28—H28B | 0.9700 |
C2—C21 | 1.501 (11) | C28—H28C | 0.9700 |
C3—C4 | 1.442 (11) | C29—C30 | 1.522 (13) |
C3—C23 | 1.511 (12) | C29—H29A | 0.9800 |
C4—N1 | 1.384 (11) | C29—H29B | 0.9800 |
C4—C5 | 1.418 (11) | C30—H30A | 0.9700 |
C5—N2 | 1.400 (10) | C30—H30B | 0.9700 |
C5—C6 | 1.423 (12) | C30—H30C | 0.9700 |
C6—C7 | 1.378 (11) | C31—C32 | 1.533 (14) |
C6—C25 | 1.503 (12) | C31—H31A | 0.9800 |
C7—C8 | 1.423 (12) | C31—H31B | 0.9800 |
C7—C27 | 1.513 (12) | C32—H32A | 0.9700 |
C8—N2 | 1.367 (10) | C32—H32B | 0.9700 |
C8—C9 | 1.404 (11) | C32—H32C | 0.9700 |
C9—C10 | 1.351 (12) | C33—C34 | 1.516 (14) |
C9—H9 | 0.9400 | C33—H33A | 0.9800 |
C10—C11 | 1.412 (12) | C33—H33B | 0.9800 |
C10—H10 | 0.9400 | C34—H34A | 0.9700 |
C11—N3 | 1.371 (10) | C34—H34B | 0.9700 |
C11—C12 | 1.458 (11) | C34—H34C | 0.9700 |
C12—C13 | 1.377 (12) | C35—C36 | 1.445 (16) |
C12—C29 | 1.512 (11) | C35—H35A | 0.9800 |
C13—C14 | 1.451 (11) | C35—H35B | 0.9800 |
C13—C31 | 1.486 (12) | C36—H36A | 0.9700 |
C14—N3 | 1.368 (11) | C36—H36B | 0.9700 |
C14—C15 | 1.415 (11) | C36—H36C | 0.9700 |
C15—N4 | 1.404 (10) | Mo1—O1 | 1.640 (7) |
C15—C16 | 1.415 (12) | Mo1—N3 | 2.052 (6) |
C16—C17 | 1.414 (11) | Mo1—N4 | 2.058 (6) |
C16—C33 | 1.498 (12) | Mo1—N1 | 2.060 (6) |
C17—C18 | 1.441 (12) | Mo1—N2 | 2.065 (7) |
C17—C35 | 1.502 (12) | Mo2—O2 | 1.691 (6) |
C18—N4 | 1.347 (10) | Mo2—O3 | 1.904 (6) |
C18—C19 | 1.403 (11) | Mo2—O4 | 1.912 (6) |
C19—C20 | 1.391 (12) | Mo2—O5 | 1.937 (6) |
C19—H19 | 0.9400 | Mo2—O6 | 1.950 (5) |
C20—H20 | 0.9400 | Mo2—O11 | 2.3055 (7) |
C21—C22 | 1.493 (13) | Mo3—O10 | 1.680 (7) |
C21—H21A | 0.9800 | Mo3—O8 | 1.908 (6) |
C21—H21B | 0.9800 | Mo3—O5 | 1.919 (6) |
C22—H22A | 0.9700 | Mo3—O3i | 1.925 (6) |
C22—H22B | 0.9700 | Mo3—O7 | 1.949 (6) |
C22—H22C | 0.9700 | Mo3—O11 | 2.3251 (8) |
C23—C24 | 1.512 (14) | Mo4—O9 | 1.683 (6) |
C23—H23A | 0.9800 | Mo4—O6i | 1.903 (6) |
C23—H23B | 0.9800 | Mo4—O7i | 1.916 (6) |
C24—H24A | 0.9700 | Mo4—O8 | 1.943 (7) |
C24—H24B | 0.9700 | Mo4—O4 | 1.950 (5) |
C24—H24C | 0.9700 | Mo4—O11 | 2.3260 (8) |
C25—C26 | 1.526 (14) | O3—Mo3i | 1.925 (6) |
C25—H25A | 0.9800 | O6—Mo4i | 1.903 (6) |
C25—H25B | 0.9800 | O7—Mo4i | 1.916 (6) |
C26—H26A | 0.9700 | O11—Mo2i | 2.3056 (7) |
C26—H26B | 0.9700 | O11—Mo3i | 2.3251 (8) |
C26—H26C | 0.9700 | O11—Mo4i | 2.3260 (8) |
C27—C28 | 1.502 (14) | ||
N1—C1—C20 | 128.7 (8) | C32—C31—H31A | 109.5 |
N1—C1—C2 | 107.9 (8) | C13—C31—H31B | 109.5 |
C20—C1—C2 | 123.4 (7) | C32—C31—H31B | 109.5 |
C3—C2—C1 | 108.2 (7) | H31A—C31—H31B | 108.0 |
C3—C2—C21 | 126.4 (8) | C31—C32—H32A | 109.5 |
C1—C2—C21 | 125.4 (8) | C31—C32—H32B | 109.5 |
C2—C3—C4 | 106.8 (8) | H32A—C32—H32B | 109.5 |
C2—C3—C23 | 125.1 (8) | C31—C32—H32C | 109.5 |
C4—C3—C23 | 127.4 (8) | H32A—C32—H32C | 109.5 |
N1—C4—C5 | 115.4 (7) | H32B—C32—H32C | 109.5 |
N1—C4—C3 | 108.0 (7) | C16—C33—C34 | 111.2 (8) |
C5—C4—C3 | 136.6 (8) | C16—C33—H33A | 109.4 |
N2—C5—C4 | 114.0 (7) | C34—C33—H33A | 109.4 |
N2—C5—C6 | 108.9 (7) | C16—C33—H33B | 109.4 |
C4—C5—C6 | 137.0 (8) | C34—C33—H33B | 109.4 |
C7—C6—C5 | 106.2 (7) | H33A—C33—H33B | 108.0 |
C7—C6—C25 | 125.0 (8) | C33—C34—H34A | 109.5 |
C5—C6—C25 | 128.6 (8) | C33—C34—H34B | 109.5 |
C6—C7—C8 | 108.9 (7) | H34A—C34—H34B | 109.5 |
C6—C7—C27 | 126.4 (8) | C33—C34—H34C | 109.5 |
C8—C7—C27 | 124.7 (7) | H34A—C34—H34C | 109.5 |
N2—C8—C9 | 126.2 (8) | H34B—C34—H34C | 109.5 |
N2—C8—C7 | 108.2 (7) | C36—C35—C17 | 110.2 (9) |
C9—C8—C7 | 125.6 (8) | C36—C35—H35A | 109.6 |
C10—C9—C8 | 136.5 (9) | C17—C35—H35A | 109.6 |
C10—C9—H9 | 111.7 | C36—C35—H35B | 109.6 |
C8—C9—H9 | 111.7 | C17—C35—H35B | 109.6 |
C9—C10—C11 | 134.8 (8) | H35A—C35—H35B | 108.1 |
C9—C10—H10 | 112.6 | C35—C36—H36A | 109.5 |
C11—C10—H10 | 112.6 | C35—C36—H36B | 109.5 |
N3—C11—C10 | 128.5 (7) | H36A—C36—H36B | 109.5 |
N3—C11—C12 | 107.5 (7) | C35—C36—H36C | 109.5 |
C10—C11—C12 | 124.0 (7) | H36A—C36—H36C | 109.5 |
C13—C12—C11 | 108.1 (7) | H36B—C36—H36C | 109.5 |
C13—C12—C29 | 127.9 (8) | O1—Mo1—N3 | 104.2 (3) |
C11—C12—C29 | 124.0 (8) | O1—Mo1—N4 | 105.3 (3) |
C12—C13—C14 | 106.1 (8) | N3—Mo1—N4 | 77.7 (3) |
C12—C13—C31 | 125.9 (8) | O1—Mo1—N1 | 105.6 (3) |
C14—C13—C31 | 127.6 (8) | N3—Mo1—N1 | 150.3 (3) |
N3—C14—C15 | 115.5 (7) | N4—Mo1—N1 | 94.6 (3) |
N3—C14—C13 | 109.1 (7) | O1—Mo1—N2 | 104.0 (3) |
C15—C14—C13 | 135.2 (8) | N3—Mo1—N2 | 95.0 (3) |
N4—C15—C16 | 109.2 (7) | N4—Mo1—N2 | 150.7 (3) |
N4—C15—C14 | 114.0 (7) | N1—Mo1—N2 | 77.6 (3) |
C16—C15—C14 | 136.7 (8) | O2—Mo2—O3 | 103.6 (3) |
C17—C16—C15 | 106.5 (7) | O2—Mo2—O4 | 103.4 (3) |
C17—C16—C33 | 122.1 (8) | O3—Mo2—O4 | 88.6 (3) |
C15—C16—C33 | 130.8 (8) | O2—Mo2—O5 | 102.7 (3) |
C16—C17—C18 | 106.6 (7) | O3—Mo2—O5 | 153.6 (2) |
C16—C17—C35 | 127.3 (8) | O4—Mo2—O5 | 87.2 (3) |
C18—C17—C35 | 126.2 (8) | O2—Mo2—O6 | 102.4 (3) |
N4—C18—C19 | 128.3 (8) | O3—Mo2—O6 | 86.9 (3) |
N4—C18—C17 | 109.6 (7) | O4—Mo2—O6 | 154.2 (2) |
C19—C18—C17 | 122.0 (8) | O5—Mo2—O6 | 85.7 (3) |
C20—C19—C18 | 133.8 (8) | O2—Mo2—O11 | 178.9 (2) |
C20—C19—H19 | 113.1 | O3—Mo2—O11 | 76.95 (16) |
C18—C19—H19 | 113.1 | O4—Mo2—O11 | 77.53 (16) |
C19—C20—C1 | 134.4 (8) | O5—Mo2—O11 | 76.67 (16) |
C19—C20—H20 | 112.8 | O6—Mo2—O11 | 76.67 (16) |
C1—C20—H20 | 112.8 | O10—Mo3—O8 | 104.4 (3) |
C22—C21—C2 | 113.6 (7) | O10—Mo3—O5 | 104.1 (3) |
C22—C21—H21A | 108.8 | O8—Mo3—O5 | 87.7 (3) |
C2—C21—H21A | 108.8 | O10—Mo3—O3i | 103.3 (3) |
C22—C21—H21B | 108.8 | O8—Mo3—O3i | 86.9 (3) |
C2—C21—H21B | 108.8 | O5—Mo3—O3i | 152.6 (3) |
H21A—C21—H21B | 107.7 | O10—Mo3—O7 | 102.5 (3) |
C21—C22—H22A | 109.5 | O8—Mo3—O7 | 153.1 (3) |
C21—C22—H22B | 109.5 | O5—Mo3—O7 | 86.9 (2) |
H22A—C22—H22B | 109.5 | O3i—Mo3—O7 | 85.8 (2) |
C21—C22—H22C | 109.5 | O10—Mo3—O11 | 178.9 (3) |
H22A—C22—H22C | 109.5 | O8—Mo3—O11 | 76.48 (19) |
H22B—C22—H22C | 109.5 | O5—Mo3—O11 | 76.51 (17) |
C3—C23—C24 | 112.4 (7) | O3i—Mo3—O11 | 76.08 (18) |
C3—C23—H23A | 109.1 | O7—Mo3—O11 | 76.59 (18) |
C24—C23—H23A | 109.1 | O9—Mo4—O6i | 103.6 (3) |
C3—C23—H23B | 109.1 | O9—Mo4—O7i | 103.0 (3) |
C24—C23—H23B | 109.1 | O6i—Mo4—O7i | 88.7 (3) |
H23A—C23—H23B | 107.9 | O9—Mo4—O8 | 104.0 (3) |
C23—C24—H24A | 109.5 | O6i—Mo4—O8 | 87.0 (3) |
C23—C24—H24B | 109.5 | O7i—Mo4—O8 | 152.9 (2) |
H24A—C24—H24B | 109.5 | O9—Mo4—O4 | 103.0 (3) |
C23—C24—H24C | 109.5 | O6i—Mo4—O4 | 153.3 (2) |
H24A—C24—H24C | 109.5 | O7i—Mo4—O4 | 86.8 (3) |
H24B—C24—H24C | 109.5 | O8—Mo4—O4 | 85.2 (3) |
C6—C25—C26 | 110.7 (9) | O9—Mo4—O11 | 179.3 (2) |
C6—C25—H25A | 109.5 | O6i—Mo4—O11 | 77.03 (16) |
C26—C25—H25A | 109.5 | O7i—Mo4—O11 | 77.15 (17) |
C6—C25—H25B | 109.5 | O8—Mo4—O11 | 75.82 (17) |
C26—C25—H25B | 109.5 | O4—Mo4—O11 | 76.31 (16) |
H25A—C25—H25B | 108.1 | C1—N1—C4 | 109.0 (7) |
C25—C26—H26A | 109.5 | C1—N1—Mo1 | 134.6 (6) |
C25—C26—H26B | 109.5 | C4—N1—Mo1 | 116.0 (5) |
H26A—C26—H26B | 109.5 | C8—N2—C5 | 107.8 (6) |
C25—C26—H26C | 109.5 | C8—N2—Mo1 | 134.2 (6) |
H26A—C26—H26C | 109.5 | C5—N2—Mo1 | 115.5 (5) |
H26B—C26—H26C | 109.5 | C14—N3—C11 | 109.2 (7) |
C28—C27—C7 | 112.9 (9) | C14—N3—Mo1 | 115.7 (5) |
C28—C27—H27A | 109.0 | C11—N3—Mo1 | 132.4 (5) |
C7—C27—H27A | 109.0 | C18—N4—C15 | 108.0 (7) |
C28—C27—H27B | 109.0 | C18—N4—Mo1 | 135.8 (5) |
C7—C27—H27B | 109.0 | C15—N4—Mo1 | 115.4 (5) |
H27A—C27—H27B | 107.8 | Mo2—O3—Mo3i | 117.2 (3) |
C27—C28—H28A | 109.5 | Mo2—O4—Mo4 | 116.1 (3) |
C27—C28—H28B | 109.5 | Mo3—O5—Mo2 | 116.6 (3) |
H28A—C28—H28B | 109.5 | Mo4i—O6—Mo2 | 116.3 (3) |
C27—C28—H28C | 109.5 | Mo4i—O7—Mo3 | 116.4 (3) |
H28A—C28—H28C | 109.5 | Mo3—O8—Mo4 | 117.5 (3) |
H28B—C28—H28C | 109.5 | Mo2—O11—Mo2i | 180.000 (1) |
C12—C29—C30 | 112.2 (8) | Mo2—O11—Mo3 | 90.21 (3) |
C12—C29—H29A | 109.2 | Mo2i—O11—Mo3 | 89.79 (3) |
C30—C29—H29A | 109.2 | Mo2—O11—Mo3i | 89.79 (3) |
C12—C29—H29B | 109.2 | Mo2i—O11—Mo3i | 90.21 (3) |
C30—C29—H29B | 109.2 | Mo3—O11—Mo3i | 180.0 |
H29A—C29—H29B | 107.9 | Mo2—O11—Mo4 | 90.05 (3) |
C29—C30—H30A | 109.5 | Mo2i—O11—Mo4 | 89.95 (3) |
C29—C30—H30B | 109.5 | Mo3—O11—Mo4 | 90.15 (3) |
H30A—C30—H30B | 109.5 | Mo3i—O11—Mo4 | 89.85 (3) |
C29—C30—H30C | 109.5 | Mo2—O11—Mo4i | 89.95 (3) |
H30A—C30—H30C | 109.5 | Mo2i—O11—Mo4i | 90.05 (3) |
H30B—C30—H30C | 109.5 | Mo3—O11—Mo4i | 89.85 (3) |
C13—C31—C32 | 110.9 (7) | Mo3i—O11—Mo4i | 90.16 (3) |
C13—C31—H31A | 109.5 | Mo4—O11—Mo4i | 180.00 (4) |
Symmetry code: (i) −x, −y+1, −z+1. |