Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805026899/hb6251sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805026899/hb6251Isup2.hkl |
CCDC reference: 285508
Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: XCAD4 (WinGX; Farrugia, 1999); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
(C8H20N)4[Mo8O26] | F(000) = 1688 |
Mr = 1704.52 | Dx = 2.045 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 11.836 (6) Å | θ = 10–15° |
b = 20.032 (7) Å | µ = 1.83 mm−1 |
c = 12.089 (12) Å | T = 293 K |
β = 105.04 (7)° | Needle, colourless |
V = 2768 (3) Å3 | 0.3 × 0.2 × 0.2 mm |
Z = 2 |
Enraf–Nonius CAD-4 diffractometer | 3807 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.020 |
Graphite monochromator | θmax = 25.0°, θmin = 2.0° |
ω–2θ scans | h = 0→14 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→23 |
Tmin = 0.550, Tmax = 0.693 | l = −14→13 |
5097 measured reflections | 2 standard reflections every 60 min |
4851 independent reflections | intensity decay: none |
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)] = 0.068 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.181 | H-atom parameters constrained |
S = 1.18 | w = 1/[σ2(Fo2) + (0.0376P)2 + 76.2716P] where P = (Fo2 + 2Fc2)/3 |
4851 reflections | (Δ/σ)max < 0.001 |
316 parameters | Δρmax = 2.70 e Å−3 |
0 restraints | Δρmin = −1.07 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 | 0.418 (2) | 0.2968 (9) | 0.1174 (17) | 0.081 (7) | |
H1A | 0.4913 | 0.3178 | 0.1555 | 0.098* | |
H1B | 0.3558 | 0.3291 | 0.1148 | 0.098* | |
C2 | 0.419 (3) | 0.2789 (14) | −0.0072 (19) | 0.162 (17) | |
H2A | 0.4316 | 0.3187 | −0.0468 | 0.243* | |
H2B | 0.3460 | 0.2590 | −0.0461 | 0.243* | |
H2C | 0.4816 | 0.2479 | −0.0055 | 0.243* | |
C3 | 0.4939 (17) | 0.1861 (9) | 0.1949 (14) | 0.064 (5) | |
H3A | 0.4909 | 0.1703 | 0.1183 | 0.077* | |
H3B | 0.4751 | 0.1485 | 0.2375 | 0.077* | |
C4 | 0.624 (2) | 0.2083 (12) | 0.254 (3) | 0.124 (11) | |
H4A | 0.6760 | 0.1713 | 0.2549 | 0.187* | |
H4B | 0.6298 | 0.2227 | 0.3307 | 0.187* | |
H4C | 0.6456 | 0.2445 | 0.2111 | 0.187* | |
C5 | 0.2852 (19) | 0.2017 (9) | 0.1337 (15) | 0.072 (6) | |
H5A | 0.2888 | 0.1822 | 0.0612 | 0.086* | |
H5B | 0.2771 | 0.1655 | 0.1845 | 0.086* | |
C6 | 0.1807 (18) | 0.2455 (11) | 0.1144 (18) | 0.081 (6) | |
H6A | 0.1116 | 0.2199 | 0.0815 | 0.122* | |
H6B | 0.1874 | 0.2810 | 0.0630 | 0.122* | |
H6C | 0.1754 | 0.2641 | 0.1861 | 0.122* | |
C7 | 0.4039 (16) | 0.2641 (8) | 0.3045 (15) | 0.060 (5) | |
H7A | 0.4795 | 0.2850 | 0.3343 | 0.072* | |
H7B | 0.3452 | 0.2988 | 0.2972 | 0.072* | |
C8 | 0.3865 (19) | 0.2160 (10) | 0.3912 (15) | 0.071 (5) | |
H8A | 0.3916 | 0.2390 | 0.4621 | 0.107* | |
H8B | 0.4459 | 0.1822 | 0.4029 | 0.107* | |
H8C | 0.3108 | 0.1957 | 0.3651 | 0.107* | |
C9 | 0.2754 (15) | 0.5519 (8) | 0.8105 (14) | 0.054 (4) | |
H9A | 0.2997 | 0.5770 | 0.7520 | 0.065* | |
H9B | 0.2727 | 0.5051 | 0.7896 | 0.065* | |
C10 | 0.3649 (19) | 0.5617 (11) | 0.9255 (17) | 0.090 (7) | |
H10A | 0.4404 | 0.5472 | 0.9196 | 0.134* | |
H10B | 0.3421 | 0.5361 | 0.9832 | 0.134* | |
H10C | 0.3685 | 0.6081 | 0.9459 | 0.134* | |
C11 | 0.160 (2) | 0.6494 (11) | 0.821 (2) | 0.110 (9) | |
H11A | 0.2053 | 0.6612 | 0.8971 | 0.131* | |
H11B | 0.2042 | 0.6648 | 0.7683 | 0.131* | |
C12 | 0.053 (3) | 0.6884 (13) | 0.797 (2) | 0.125 (11) | |
H12A | 0.0725 | 0.7351 | 0.8049 | 0.188* | |
H12B | 0.0093 | 0.6766 | 0.8508 | 0.188* | |
H12C | 0.0074 | 0.6796 | 0.7208 | 0.188* | |
C13 | 0.1188 (17) | 0.5421 (13) | 0.9111 (14) | 0.082 (7) | |
H13A | 0.1665 | 0.5596 | 0.9829 | 0.099* | |
H13B | 0.0386 | 0.5554 | 0.9049 | 0.099* | |
C14 | 0.126 (2) | 0.4670 (13) | 0.915 (2) | 0.121 (11) | |
H14A | 0.0984 | 0.4510 | 0.9786 | 0.182* | |
H14B | 0.2051 | 0.4532 | 0.9244 | 0.182* | |
H14C | 0.0774 | 0.4489 | 0.8452 | 0.182* | |
C15 | 0.0635 (17) | 0.5548 (10) | 0.6978 (15) | 0.069 (5) | |
H15A | 0.0576 | 0.5065 | 0.6932 | 0.082* | |
H15B | −0.0120 | 0.5717 | 0.7022 | 0.082* | |
C16 | 0.0851 (16) | 0.5781 (8) | 0.5973 (14) | 0.058 (4) | |
H16A | 0.0236 | 0.5636 | 0.5332 | 0.088* | |
H16B | 0.1585 | 0.5608 | 0.5902 | 0.088* | |
H16C | 0.0880 | 0.6260 | 0.5988 | 0.088* | |
N1 | 0.3988 (14) | 0.2387 (7) | 0.1854 (12) | 0.061 (4) | |
N2 | 0.1580 (12) | 0.5739 (6) | 0.8142 (12) | 0.052 (3) | |
O1 | 0.2159 (8) | 0.4766 (5) | 0.4075 (7) | 0.038 (2) | |
O2 | 0.1718 (9) | 0.5507 (6) | 0.2091 (9) | 0.054 (3) | |
O3 | 0.4022 (8) | 0.5113 (4) | 0.2170 (7) | 0.036 (2) | |
O4 | 0.2166 (9) | 0.4219 (5) | 0.1929 (8) | 0.048 (3) | |
O5 | 0.2127 (9) | 0.3376 (6) | 0.4317 (9) | 0.055 (3) | |
O6 | 0.3837 (8) | 0.5698 (4) | 0.4033 (8) | 0.035 (2) | |
O7 | 0.3915 (7) | 0.4944 (4) | 0.6101 (7) | 0.0289 (18) | |
O8 | 0.1864 (9) | 0.4152 (5) | 0.6055 (9) | 0.047 (2) | |
O9 | 0.4073 (8) | 0.3641 (4) | 0.6114 (8) | 0.038 (2) | |
O10 | 0.6004 (10) | 0.3500 (5) | 0.8016 (9) | 0.052 (3) | |
O11 | 0.4098 (9) | 0.4191 (5) | 0.8271 (8) | 0.046 (2) | |
O12 | 0.5876 (7) | 0.5801 (5) | 0.5999 (8) | 0.035 (2) | |
O13 | 0.3700 (8) | 0.6360 (4) | 0.6106 (8) | 0.036 (2) | |
Mo1 | 0.26755 (10) | 0.49031 (6) | 0.27169 (10) | 0.0360 (3) | |
Mo2 | 0.27131 (10) | 0.40425 (6) | 0.51351 (10) | 0.0337 (3) | |
Mo3 | 0.50468 (11) | 0.41132 (6) | 0.73966 (10) | 0.0330 (3) | |
Mo4 | 0.43351 (9) | 0.57040 (5) | 0.55576 (9) | 0.0238 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.116 (17) | 0.038 (10) | 0.088 (14) | −0.039 (11) | 0.020 (13) | 0.008 (9) |
C2 | 0.32 (5) | 0.12 (2) | 0.062 (15) | −0.11 (3) | 0.07 (2) | 0.004 (15) |
C3 | 0.102 (15) | 0.049 (10) | 0.049 (10) | −0.011 (10) | 0.034 (10) | −0.010 (8) |
C4 | 0.097 (18) | 0.077 (16) | 0.21 (3) | −0.025 (14) | 0.05 (2) | −0.077 (19) |
C5 | 0.111 (17) | 0.052 (11) | 0.045 (10) | −0.031 (11) | 0.006 (10) | −0.007 (8) |
C6 | 0.080 (14) | 0.072 (13) | 0.080 (14) | −0.019 (12) | −0.001 (11) | −0.006 (11) |
C7 | 0.066 (11) | 0.036 (9) | 0.077 (12) | −0.004 (8) | 0.020 (9) | −0.038 (8) |
C8 | 0.095 (15) | 0.064 (12) | 0.054 (11) | 0.008 (11) | 0.018 (10) | 0.000 (9) |
C9 | 0.073 (11) | 0.037 (9) | 0.063 (10) | −0.011 (8) | 0.036 (9) | −0.002 (7) |
C10 | 0.091 (16) | 0.080 (15) | 0.072 (14) | 0.009 (12) | −0.024 (12) | −0.004 (11) |
C11 | 0.11 (2) | 0.058 (13) | 0.14 (2) | 0.022 (13) | −0.003 (17) | −0.034 (14) |
C12 | 0.18 (3) | 0.084 (18) | 0.084 (17) | 0.024 (19) | −0.007 (18) | −0.007 (14) |
C13 | 0.063 (12) | 0.16 (2) | 0.033 (9) | −0.012 (13) | 0.033 (9) | 0.013 (11) |
C14 | 0.11 (2) | 0.13 (2) | 0.100 (19) | −0.054 (17) | −0.015 (15) | 0.068 (17) |
C15 | 0.077 (13) | 0.070 (12) | 0.055 (11) | −0.032 (10) | 0.010 (9) | −0.005 (9) |
C16 | 0.072 (11) | 0.042 (9) | 0.052 (10) | −0.014 (8) | 0.000 (8) | −0.001 (8) |
N1 | 0.086 (11) | 0.043 (8) | 0.053 (8) | −0.030 (8) | 0.015 (8) | −0.016 (6) |
N2 | 0.069 (9) | 0.039 (7) | 0.062 (8) | 0.001 (6) | 0.042 (7) | 0.000 (6) |
O1 | 0.031 (5) | 0.051 (6) | 0.032 (5) | −0.001 (4) | 0.007 (4) | 0.003 (4) |
O2 | 0.042 (6) | 0.066 (7) | 0.048 (6) | 0.012 (5) | 0.003 (5) | 0.017 (5) |
O3 | 0.047 (5) | 0.040 (5) | 0.027 (4) | 0.000 (4) | 0.022 (4) | 0.002 (4) |
O4 | 0.055 (6) | 0.047 (6) | 0.042 (6) | −0.004 (5) | 0.013 (5) | −0.011 (5) |
O5 | 0.053 (6) | 0.060 (7) | 0.048 (6) | −0.006 (5) | 0.007 (5) | −0.019 (5) |
O6 | 0.037 (5) | 0.029 (5) | 0.045 (5) | −0.001 (4) | 0.022 (4) | 0.007 (4) |
O7 | 0.026 (4) | 0.026 (4) | 0.037 (5) | −0.010 (4) | 0.014 (4) | 0.004 (4) |
O8 | 0.047 (6) | 0.038 (6) | 0.061 (7) | 0.002 (5) | 0.025 (5) | 0.007 (5) |
O9 | 0.045 (6) | 0.028 (5) | 0.050 (6) | −0.004 (4) | 0.026 (5) | 0.007 (4) |
O10 | 0.065 (7) | 0.036 (6) | 0.056 (6) | 0.026 (5) | 0.019 (5) | 0.014 (5) |
O11 | 0.064 (7) | 0.042 (6) | 0.041 (5) | −0.009 (5) | 0.028 (5) | 0.007 (4) |
O12 | 0.027 (5) | 0.044 (5) | 0.038 (5) | 0.001 (4) | 0.013 (4) | −0.008 (4) |
O13 | 0.043 (5) | 0.022 (4) | 0.050 (6) | 0.003 (4) | 0.025 (4) | −0.005 (4) |
Mo1 | 0.0337 (6) | 0.0448 (7) | 0.0294 (6) | 0.0020 (5) | 0.0081 (5) | −0.0017 (5) |
Mo2 | 0.0344 (6) | 0.0283 (6) | 0.0419 (7) | −0.0042 (5) | 0.0164 (5) | −0.0009 (5) |
Mo3 | 0.0419 (7) | 0.0278 (6) | 0.0334 (6) | 0.0034 (5) | 0.0171 (5) | 0.0071 (5) |
Mo4 | 0.0301 (6) | 0.0167 (5) | 0.0291 (5) | 0.0004 (4) | 0.0160 (4) | −0.0005 (4) |
C1—N1 | 1.48 (2) | C12—H12C | 0.9600 |
C1—C2 | 1.55 (3) | C13—C14 | 1.51 (3) |
C1—H1A | 0.9700 | C13—N2 | 1.508 (19) |
C1—H1B | 0.9700 | C13—H13A | 0.9700 |
C2—H2A | 0.9600 | C13—H13B | 0.9700 |
C2—H2B | 0.9600 | C14—H14A | 0.9600 |
C2—H2C | 0.9600 | C14—H14B | 0.9600 |
C3—N1 | 1.52 (2) | C14—H14C | 0.9600 |
C3—C4 | 1.59 (3) | C15—C16 | 1.39 (2) |
C3—H3A | 0.9700 | C15—N2 | 1.60 (2) |
C3—H3B | 0.9700 | C15—H15A | 0.9700 |
C4—H4A | 0.9600 | C15—H15B | 0.9700 |
C4—H4B | 0.9600 | C16—H16A | 0.9600 |
C4—H4C | 0.9600 | C16—H16B | 0.9600 |
C5—C6 | 1.49 (3) | C16—H16C | 0.9600 |
C5—N1 | 1.52 (2) | O1—Mo1 | 1.915 (9) |
C5—H5A | 0.9700 | O1—Mo2 | 1.933 (9) |
C5—H5B | 0.9700 | O2—Mo1 | 1.696 (10) |
C6—H6A | 0.9600 | O3—Mo3i | 1.895 (9) |
C6—H6B | 0.9600 | O3—Mo1 | 1.924 (9) |
C6—H6C | 0.9600 | O4—Mo1 | 1.688 (10) |
C7—C8 | 1.48 (2) | O5—Mo2 | 1.700 (10) |
C7—N1 | 1.51 (2) | O6—Mo4 | 1.783 (9) |
C7—H7A | 0.9700 | O6—Mo1 | 2.413 (9) |
C7—H7B | 0.9700 | O6—Mo3i | 2.462 (8) |
C8—H8A | 0.9600 | O7—Mo4 | 1.780 (8) |
C8—H8B | 0.9600 | O7—Mo2 | 2.405 (8) |
C8—H8C | 0.9600 | O7—Mo3 | 2.434 (8) |
C9—N2 | 1.47 (2) | O8—Mo2 | 1.696 (10) |
C9—C10 | 1.53 (2) | O9—Mo2 | 1.910 (10) |
C9—H9A | 0.9700 | O9—Mo3 | 1.923 (10) |
C9—H9B | 0.9700 | O10—Mo3 | 1.706 (9) |
C10—H10A | 0.9600 | O11—Mo3 | 1.737 (10) |
C10—H10B | 0.9600 | O12—Mo4 | 1.773 (9) |
C10—H10C | 0.9600 | O12—Mo2i | 2.440 (9) |
C11—C12 | 1.45 (3) | O12—Mo1i | 2.441 (9) |
C11—N2 | 1.51 (2) | O13—Mo4 | 1.729 (8) |
C11—H11A | 0.9700 | Mo1—O12i | 2.441 (9) |
C11—H11B | 0.9700 | Mo2—O12i | 2.440 (9) |
C12—H12A | 0.9600 | Mo3—O3i | 1.895 (9) |
C12—H12B | 0.9600 | Mo3—O6i | 2.462 (8) |
N1—C1—C2 | 113.5 (16) | N2—C15—H15A | 108.2 |
N1—C1—H1A | 108.9 | C16—C15—H15B | 108.2 |
C2—C1—H1A | 108.9 | N2—C15—H15B | 108.2 |
N1—C1—H1B | 108.9 | H15A—C15—H15B | 107.3 |
C2—C1—H1B | 108.9 | C15—C16—H16A | 109.5 |
H1A—C1—H1B | 107.7 | C15—C16—H16B | 109.5 |
C1—C2—H2A | 109.5 | H16A—C16—H16B | 109.5 |
C1—C2—H2B | 109.5 | C15—C16—H16C | 109.5 |
H2A—C2—H2B | 109.5 | H16A—C16—H16C | 109.5 |
C1—C2—H2C | 109.5 | H16B—C16—H16C | 109.5 |
H2A—C2—H2C | 109.5 | C1—N1—C7 | 106.8 (13) |
H2B—C2—H2C | 109.5 | C1—N1—C5 | 113.6 (15) |
N1—C3—C4 | 116.9 (14) | C7—N1—C5 | 111.6 (14) |
N1—C3—H3A | 108.1 | C1—N1—C3 | 111.9 (15) |
C4—C3—H3A | 108.1 | C7—N1—C3 | 108.3 (13) |
N1—C3—H3B | 108.1 | C5—N1—C3 | 104.6 (13) |
C4—C3—H3B | 108.1 | C9—N2—C13 | 112.4 (14) |
H3A—C3—H3B | 107.3 | C9—N2—C11 | 107.3 (15) |
C3—C4—H4A | 109.5 | C13—N2—C11 | 112.7 (17) |
C3—C4—H4B | 109.5 | C9—N2—C15 | 110.6 (13) |
H4A—C4—H4B | 109.5 | C13—N2—C15 | 107.3 (13) |
C3—C4—H4C | 109.5 | C11—N2—C15 | 106.4 (15) |
H4A—C4—H4C | 109.5 | Mo1—O1—Mo2 | 123.2 (5) |
H4B—C4—H4C | 109.5 | Mo3i—O3—Mo1 | 123.9 (4) |
C6—C5—N1 | 112.9 (15) | Mo4—O6—Mo1 | 131.7 (4) |
C6—C5—H5A | 109.0 | Mo4—O6—Mo3i | 129.1 (4) |
N1—C5—H5A | 109.0 | Mo1—O6—Mo3i | 87.5 (3) |
C6—C5—H5B | 109.0 | Mo4—O7—Mo2 | 130.5 (4) |
N1—C5—H5B | 109.0 | Mo4—O7—Mo3 | 131.5 (4) |
H5A—C5—H5B | 107.8 | Mo2—O7—Mo3 | 87.5 (3) |
C5—C6—H6A | 109.5 | Mo2—O9—Mo3 | 121.7 (5) |
C5—C6—H6B | 109.5 | Mo4—O12—Mo2i | 130.2 (5) |
H6A—C6—H6B | 109.5 | Mo4—O12—Mo1i | 128.8 (5) |
C5—C6—H6C | 109.5 | Mo2i—O12—Mo1i | 87.8 (3) |
H6A—C6—H6C | 109.5 | O4—Mo1—O2 | 103.2 (5) |
H6B—C6—H6C | 109.5 | O4—Mo1—O1 | 102.7 (5) |
C8—C7—N1 | 118.5 (13) | O2—Mo1—O1 | 99.2 (5) |
C8—C7—H7A | 107.7 | O4—Mo1—O3 | 100.9 (4) |
N1—C7—H7A | 107.7 | O2—Mo1—O3 | 102.0 (5) |
C8—C7—H7B | 107.7 | O1—Mo1—O3 | 143.5 (4) |
N1—C7—H7B | 107.7 | O4—Mo1—O6 | 165.1 (4) |
H7A—C7—H7B | 107.1 | O2—Mo1—O6 | 91.4 (4) |
C7—C8—H8A | 109.5 | O1—Mo1—O6 | 77.5 (3) |
C7—C8—H8B | 109.5 | O3—Mo1—O6 | 72.6 (3) |
H8A—C8—H8B | 109.5 | O4—Mo1—O12i | 88.8 (4) |
C7—C8—H8C | 109.5 | O2—Mo1—O12i | 166.9 (4) |
H8A—C8—H8C | 109.5 | O1—Mo1—O12i | 72.5 (3) |
H8B—C8—H8C | 109.5 | O3—Mo1—O12i | 80.6 (3) |
N2—C9—C10 | 111.9 (15) | O6—Mo1—O12i | 77.0 (3) |
N2—C9—H9A | 109.2 | O8—Mo2—O5 | 105.2 (5) |
C10—C9—H9A | 109.2 | O8—Mo2—O9 | 101.3 (4) |
N2—C9—H9B | 109.2 | O5—Mo2—O9 | 100.4 (5) |
C10—C9—H9B | 109.2 | O8—Mo2—O1 | 100.4 (4) |
H9A—C9—H9B | 107.9 | O5—Mo2—O1 | 100.7 (5) |
C9—C10—H10A | 109.5 | O9—Mo2—O1 | 144.3 (4) |
C9—C10—H10B | 109.5 | O8—Mo2—O7 | 87.8 (4) |
H10A—C10—H10B | 109.5 | O5—Mo2—O7 | 166.7 (4) |
C9—C10—H10C | 109.5 | O9—Mo2—O7 | 73.6 (3) |
H10A—C10—H10C | 109.5 | O1—Mo2—O7 | 79.4 (3) |
H10B—C10—H10C | 109.5 | O8—Mo2—O12i | 163.8 (4) |
C12—C11—N2 | 122 (2) | O5—Mo2—O12i | 90.6 (4) |
C12—C11—H11A | 106.9 | O9—Mo2—O12i | 79.2 (3) |
N2—C11—H11A | 106.9 | O1—Mo2—O12i | 72.2 (3) |
C12—C11—H11B | 106.9 | O7—Mo2—O12i | 76.8 (3) |
N2—C11—H11B | 106.9 | O10—Mo3—O11 | 104.9 (5) |
H11A—C11—H11B | 106.7 | O10—Mo3—O3i | 101.3 (5) |
C11—C12—H12A | 109.5 | O11—Mo3—O3i | 100.3 (4) |
C11—C12—H12B | 109.5 | O10—Mo3—O9 | 101.0 (5) |
H12A—C12—H12B | 109.5 | O11—Mo3—O9 | 100.8 (4) |
C11—C12—H12C | 109.5 | O3i—Mo3—O9 | 144.0 (4) |
H12A—C12—H12C | 109.5 | O10—Mo3—O7 | 165.0 (4) |
H12B—C12—H12C | 109.5 | O11—Mo3—O7 | 89.7 (4) |
C14—C13—N2 | 115.0 (18) | O3i—Mo3—O7 | 78.6 (3) |
C14—C13—H13A | 108.5 | O9—Mo3—O7 | 72.7 (3) |
N2—C13—H13A | 108.5 | O10—Mo3—O6i | 90.2 (4) |
C14—C13—H13B | 108.5 | O11—Mo3—O6i | 164.3 (4) |
N2—C13—H13B | 108.5 | O3i—Mo3—O6i | 71.9 (3) |
H13A—C13—H13B | 107.5 | O9—Mo3—O6i | 80.1 (3) |
C13—C14—H14A | 109.5 | O7—Mo3—O6i | 75.5 (3) |
C13—C14—H14B | 109.5 | O13—Mo4—O12 | 108.5 (4) |
H14A—C14—H14B | 109.5 | O13—Mo4—O7 | 108.5 (4) |
C13—C14—H14C | 109.5 | O12—Mo4—O7 | 110.3 (4) |
H14A—C14—H14C | 109.5 | O13—Mo4—O6 | 110.0 (4) |
H14B—C14—H14C | 109.5 | O12—Mo4—O6 | 110.5 (4) |
C16—C15—N2 | 116.4 (14) | O7—Mo4—O6 | 109.0 (4) |
C16—C15—H15A | 108.2 | ||
C2—C1—N1—C7 | 178 (2) | Mo1—O1—Mo2—O8 | −175.3 (6) |
C2—C1—N1—C5 | −59 (3) | Mo1—O1—Mo2—O5 | −67.5 (6) |
C2—C1—N1—C3 | 60 (3) | Mo1—O1—Mo2—O9 | 58.0 (9) |
C8—C7—N1—C1 | 179.4 (18) | Mo1—O1—Mo2—O7 | 99.0 (5) |
C8—C7—N1—C5 | 55 (2) | Mo1—O1—Mo2—O12i | 19.7 (5) |
C8—C7—N1—C3 | −60 (2) | Mo4—O7—Mo2—O8 | −124.1 (6) |
C6—C5—N1—C1 | −56 (2) | Mo3—O7—Mo2—O8 | 89.2 (4) |
C6—C5—N1—C7 | 65 (2) | Mo4—O7—Mo2—O5 | 69 (2) |
C6—C5—N1—C3 | −178.4 (16) | Mo3—O7—Mo2—O5 | −78.1 (19) |
C4—C3—N1—C1 | 60 (2) | Mo4—O7—Mo2—O9 | 133.4 (6) |
C4—C3—N1—C7 | −57 (2) | Mo3—O7—Mo2—O9 | −13.3 (3) |
C4—C3—N1—C5 | −176.4 (18) | Mo4—O7—Mo2—O1 | −23.1 (6) |
C10—C9—N2—C13 | −53.2 (19) | Mo3—O7—Mo2—O1 | −169.8 (3) |
C10—C9—N2—C11 | 71.3 (19) | Mo4—O7—Mo2—O12i | 51.0 (5) |
C10—C9—N2—C15 | −173.1 (14) | Mo3—O7—Mo2—O12i | −95.7 (3) |
C14—C13—N2—C9 | −53 (2) | Mo2—O9—Mo3—O10 | 174.2 (5) |
C14—C13—N2—C11 | −174.7 (18) | Mo2—O9—Mo3—O11 | 66.5 (6) |
C14—C13—N2—C15 | 69 (2) | Mo2—O9—Mo3—O3i | −58.5 (9) |
C12—C11—N2—C9 | 165 (2) | Mo2—O9—Mo3—O7 | −19.8 (4) |
C12—C11—N2—C13 | −71 (3) | Mo2—O9—Mo3—O6i | −97.6 (5) |
C12—C11—N2—C15 | 46 (3) | Mo4—O7—Mo3—O10 | −65.9 (19) |
C16—C15—N2—C9 | −56 (2) | Mo2—O7—Mo3—O10 | 80.2 (17) |
C16—C15—N2—C13 | −178.5 (18) | Mo4—O7—Mo3—O11 | 125.7 (6) |
C16—C15—N2—C11 | 61 (2) | Mo2—O7—Mo3—O11 | −88.2 (4) |
Mo2—O1—Mo1—O4 | 65.0 (6) | Mo4—O7—Mo3—O3i | 25.1 (6) |
Mo2—O1—Mo1—O2 | 170.9 (6) | Mo2—O7—Mo3—O3i | 171.2 (3) |
Mo2—O1—Mo1—O3 | −64.2 (9) | Mo4—O7—Mo3—O9 | −132.9 (6) |
Mo2—O1—Mo1—O6 | −99.8 (5) | Mo2—O7—Mo3—O9 | 13.3 (3) |
Mo2—O1—Mo1—O12i | −19.6 (5) | Mo4—O7—Mo3—O6i | −48.9 (5) |
Mo3i—O3—Mo1—O4 | 174.3 (6) | Mo2—O7—Mo3—O6i | 97.2 (3) |
Mo3i—O3—Mo1—O2 | 68.1 (7) | Mo2i—O12—Mo4—O13 | −118.2 (6) |
Mo3i—O3—Mo1—O1 | −56.1 (9) | Mo1i—O12—Mo4—O13 | 114.0 (6) |
Mo3i—O3—Mo1—O6 | −19.6 (5) | Mo2i—O12—Mo4—O7 | 123.1 (6) |
Mo3i—O3—Mo1—O12i | −98.8 (5) | Mo1i—O12—Mo4—O7 | −4.8 (6) |
Mo4—O6—Mo1—O4 | −65.2 (17) | Mo2i—O12—Mo4—O6 | 2.4 (7) |
Mo3i—O6—Mo1—O4 | 78.5 (16) | Mo1i—O12—Mo4—O6 | −125.4 (5) |
Mo4—O6—Mo1—O2 | 126.4 (7) | Mo2—O7—Mo4—O13 | 113.6 (6) |
Mo3i—O6—Mo1—O2 | −89.8 (4) | Mo3—O7—Mo4—O13 | −113.5 (6) |
Mo4—O6—Mo1—O1 | 27.3 (6) | Mo2—O7—Mo4—O12 | −127.7 (5) |
Mo3i—O6—Mo1—O1 | 171.1 (4) | Mo3—O7—Mo4—O12 | 5.2 (7) |
Mo4—O6—Mo1—O3 | −131.4 (7) | Mo2—O7—Mo4—O6 | −6.2 (6) |
Mo3i—O6—Mo1—O3 | 12.4 (3) | Mo3—O7—Mo4—O6 | 126.7 (5) |
Mo4—O6—Mo1—O12i | −47.3 (6) | Mo1—O6—Mo4—O13 | −115.0 (6) |
Mo3i—O6—Mo1—O12i | 96.5 (3) | Mo3i—O6—Mo4—O13 | 114.5 (6) |
Mo3—O9—Mo2—O8 | −64.3 (6) | Mo1—O6—Mo4—O12 | 125.2 (6) |
Mo3—O9—Mo2—O5 | −172.2 (6) | Mo3i—O6—Mo4—O12 | −5.2 (7) |
Mo3—O9—Mo2—O1 | 62.2 (9) | Mo1—O6—Mo4—O7 | 3.9 (7) |
Mo3—O9—Mo2—O7 | 20.0 (4) | Mo3i—O6—Mo4—O7 | −126.6 (5) |
Mo3—O9—Mo2—O12i | 99.2 (5) |
Symmetry code: (i) −x+1, −y+1, −z+1. |