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
Key indicators
- Single-crystal X-ray study
- T = 223 K
- Mean (C-C) = 0.014 Å
- R factor = 0.064
- wR factor = 0.168
- Data-to-parameter ratio = 14.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. N3 .. 2.86 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. N4 .. 2.87 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.97 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.25 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.58 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mo1 - O1 .. 5.08 su PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14 PLAT410_ALERT_2_C Short Intra H...H Contact H23A .. H25A .. 1.99 Ang. PLAT410_ALERT_2_C Short Intra H...H Contact H31B .. H33B .. 1.96 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact O2 .. N1 .. 2.88 Ang. PLAT430_ALERT_2_C Short Inter D...A Contact O2 .. N2 .. 2.88 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O3 .. C18 .. 2.96 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 68.00 A 3
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 11 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
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. |
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