Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807013220/hg2202sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807013220/hg2202Isup2.hkl |
CCDC reference: 647229
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); 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, 2000); software used to prepare material for publication: SHELXTL.
[Ni(C10H8N2)3]2[Mo8O26]·4H2O | F(000) = 2264 |
Mr = 2310.10 | Dx = 2.089 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 7772 reflections |
a = 12.2823 (4) Å | θ = 2.4–28.3° |
b = 13.7818 (4) Å | µ = 1.91 mm−1 |
c = 21.6970 (6) Å | T = 273 K |
β = 90.8703 (7)° | Block, colorless |
V = 3672.28 (19) Å3 | 0.24 × 0.20 × 0.14 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 9119 independent reflections |
Radiation source: fine-focus sealed tube | 7347 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
φ and ω scans | θmax = 28.3°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −16→16 |
Tmin = 0.657, Tmax = 0.776 | k = −18→18 |
36452 measured reflections | l = −28→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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.072 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0361P)2 + 0.5038P] where P = (Fo2 + 2Fc2)/3 |
9119 reflections | (Δ/σ)max = 0.005 |
505 parameters | Δρmax = 0.69 e Å−3 |
24 restraints | Δρmin = −0.48 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 | ||
Mo1 | 0.901617 (18) | 0.534383 (15) | 1.054832 (10) | 0.02709 (6) | |
Mo2 | 0.913304 (18) | 0.617884 (16) | 0.902001 (10) | 0.03113 (6) | |
Mo3 | 0.727849 (19) | 0.459218 (17) | 0.936603 (11) | 0.03420 (6) | |
Mo4 | 1.082596 (19) | 0.693407 (16) | 1.018682 (11) | 0.03262 (6) | |
Ni1 | 0.38567 (3) | 0.96955 (2) | 0.831308 (15) | 0.02978 (8) | |
O1 | 0.92724 (16) | 0.56760 (15) | 0.83120 (9) | 0.0418 (5) | |
O2 | 0.90859 (17) | 0.73960 (14) | 0.88863 (9) | 0.0443 (5) | |
O3 | 1.08672 (18) | 0.79604 (14) | 0.97591 (10) | 0.0506 (5) | |
O4 | 1.23086 (14) | 0.65619 (13) | 1.01866 (9) | 0.0361 (4) | |
O5 | 1.06703 (16) | 0.73233 (15) | 1.09232 (9) | 0.0462 (5) | |
O6 | 1.07475 (13) | 0.52811 (11) | 1.04517 (8) | 0.0273 (4) | |
O7 | 0.89636 (16) | 0.57937 (15) | 1.12731 (8) | 0.0391 (4) | |
O8 | 0.93059 (14) | 0.39781 (12) | 1.07143 (8) | 0.0299 (4) | |
O9 | 0.92751 (14) | 0.65145 (12) | 1.00711 (8) | 0.0291 (4) | |
O10 | 0.76564 (14) | 0.59177 (13) | 0.91943 (9) | 0.0361 (4) | |
O11 | 0.73853 (17) | 0.41367 (16) | 0.86448 (9) | 0.0478 (5) | |
O12 | 0.59163 (16) | 0.46480 (16) | 0.94854 (11) | 0.0494 (5) | |
O13 | 0.76458 (14) | 0.51910 (13) | 1.03375 (8) | 0.0341 (4) | |
O14 | 0.9120 (4) | 0.0117 (4) | 0.7657 (3) | 0.1648 (19) | |
O15 | 0.0027 (5) | 0.0604 (4) | 0.1165 (3) | 0.200 (2) | |
C1 | 0.4666 (2) | 0.8791 (2) | 0.71198 (13) | 0.0378 (6) | |
H1 | 0.4023 | 0.8434 | 0.7124 | 0.045* | |
C2 | 0.6018 (2) | 1.0525 (2) | 0.81344 (14) | 0.0379 (6) | |
C3 | 0.5834 (2) | 0.9884 (2) | 0.75967 (13) | 0.0353 (6) | |
C4 | 0.1816 (2) | 0.9000 (2) | 0.76256 (14) | 0.0455 (7) | |
H4 | 0.1827 | 0.9604 | 0.7434 | 0.055* | |
C5 | 0.2593 (3) | 0.7912 (2) | 0.83106 (13) | 0.0429 (7) | |
C6 | 0.5355 (3) | 0.8695 (2) | 0.66233 (14) | 0.0448 (7) | |
H6 | 0.5171 | 0.8290 | 0.6295 | 0.054* | |
C7 | 0.2515 (2) | 1.1448 (2) | 0.82641 (13) | 0.0378 (6) | |
C8 | 0.3379 (2) | 1.1269 (2) | 0.73334 (14) | 0.0423 (7) | |
H8 | 0.3850 | 1.0921 | 0.7085 | 0.051* | |
C9 | 0.6562 (3) | 0.9787 (3) | 0.71162 (15) | 0.0512 (8) | |
H9 | 0.7221 | 1.0118 | 0.7128 | 0.061* | |
C10 | 0.5345 (3) | 1.1089 (2) | 0.90569 (14) | 0.0453 (7) | |
H10 | 0.4809 | 1.1072 | 0.9355 | 0.054* | |
C11 | 0.2763 (3) | 0.9827 (2) | 0.95747 (15) | 0.0517 (8) | |
H11 | 0.3105 | 0.9239 | 0.9659 | 0.062* | |
C12 | 0.2900 (3) | 1.2096 (2) | 0.70952 (15) | 0.0484 (8) | |
H12 | 0.3053 | 1.2306 | 0.6699 | 0.058* | |
C13 | 0.3539 (3) | 0.7707 (2) | 0.87177 (14) | 0.0444 (7) | |
C14 | 0.2386 (2) | 1.1071 (2) | 0.88926 (14) | 0.0424 (7) | |
C15 | 0.2193 (3) | 1.2598 (2) | 0.74576 (17) | 0.0572 (9) | |
H15 | 0.1849 | 1.3153 | 0.7307 | 0.069* | |
C16 | 0.1993 (3) | 1.2277 (2) | 0.80490 (16) | 0.0544 (9) | |
H16 | 0.1514 | 1.2612 | 0.8300 | 0.065* | |
C17 | 0.5195 (3) | 0.8273 (3) | 0.90990 (15) | 0.0550 (9) | |
H17 | 0.5703 | 0.8770 | 0.9137 | 0.066* | |
C18 | 0.6305 (3) | 0.9201 (3) | 0.66242 (15) | 0.0529 (8) | |
H18 | 0.6776 | 0.9150 | 0.6294 | 0.064* | |
C19 | 0.6214 (3) | 1.1714 (2) | 0.91405 (16) | 0.0527 (8) | |
H19 | 0.6261 | 1.2110 | 0.9487 | 0.063* | |
C20 | 0.6918 (3) | 1.1137 (2) | 0.81999 (17) | 0.0555 (9) | |
H20 | 0.7458 | 1.1138 | 0.7904 | 0.067* | |
C21 | 0.7000 (3) | 1.1736 (2) | 0.87039 (18) | 0.0597 (9) | |
H21 | 0.7590 | 1.2155 | 0.8747 | 0.072* | |
C22 | 0.5404 (3) | 0.7383 (3) | 0.93838 (17) | 0.0700 (12) | |
H22 | 0.6055 | 0.7279 | 0.9598 | 0.084* | |
C23 | 0.4646 (4) | 0.6675 (3) | 0.93440 (19) | 0.0767 (13) | |
H23 | 0.4766 | 0.6085 | 0.9541 | 0.092* | |
C24 | 0.3702 (4) | 0.6824 (3) | 0.90140 (17) | 0.0664 (11) | |
H24 | 0.3176 | 0.6339 | 0.8988 | 0.080* | |
C25 | 0.1747 (3) | 0.7257 (2) | 0.82001 (18) | 0.0610 (10) | |
H25 | 0.1724 | 0.6669 | 0.8409 | 0.073* | |
C26 | 0.0940 (3) | 0.7499 (3) | 0.77720 (19) | 0.0699 (11) | |
H26 | 0.0375 | 0.7067 | 0.7688 | 0.084* | |
C27 | 0.0977 (3) | 0.8367 (3) | 0.74765 (17) | 0.0602 (9) | |
H27 | 0.0453 | 0.8533 | 0.7181 | 0.072* | |
C28 | 0.2146 (3) | 1.0244 (3) | 1.00283 (16) | 0.0668 (11) | |
H28 | 0.2061 | 0.9941 | 1.0407 | 0.080* | |
C29 | 0.1661 (4) | 1.1116 (3) | 0.99045 (19) | 0.0837 (14) | |
H29 | 0.1256 | 1.1427 | 1.0205 | 0.100* | |
C30 | 0.1775 (4) | 1.1529 (3) | 0.93363 (18) | 0.0756 (13) | |
H30 | 0.1440 | 1.2119 | 0.9248 | 0.091* | |
N1 | 0.48971 (17) | 0.93841 (16) | 0.75929 (10) | 0.0314 (5) | |
N2 | 0.32034 (19) | 1.09430 (16) | 0.79022 (10) | 0.0348 (5) | |
N3 | 0.26045 (19) | 0.87866 (16) | 0.80288 (10) | 0.0362 (5) | |
N4 | 0.52400 (19) | 1.05084 (16) | 0.85664 (11) | 0.0356 (5) | |
N5 | 0.4278 (2) | 0.84235 (17) | 0.87725 (11) | 0.0405 (6) | |
N6 | 0.28958 (19) | 1.02235 (16) | 0.90219 (11) | 0.0373 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.02702 (11) | 0.02610 (11) | 0.02826 (11) | 0.00128 (8) | 0.00449 (9) | −0.00450 (8) |
Mo2 | 0.03251 (12) | 0.03002 (12) | 0.03080 (12) | 0.00028 (9) | −0.00145 (9) | 0.00129 (9) |
Mo3 | 0.02794 (12) | 0.03619 (13) | 0.03841 (13) | −0.00186 (9) | −0.00167 (10) | −0.00352 (10) |
Mo4 | 0.03134 (12) | 0.02527 (11) | 0.04119 (13) | −0.00216 (9) | −0.00156 (10) | −0.00635 (10) |
Ni1 | 0.03229 (18) | 0.02604 (16) | 0.03110 (17) | 0.00256 (13) | 0.00320 (14) | −0.00033 (13) |
O1 | 0.0470 (12) | 0.0453 (11) | 0.0329 (10) | −0.0009 (10) | −0.0026 (9) | −0.0019 (9) |
O2 | 0.0520 (13) | 0.0340 (11) | 0.0467 (11) | 0.0003 (9) | −0.0060 (10) | 0.0047 (9) |
O3 | 0.0544 (13) | 0.0312 (10) | 0.0661 (14) | −0.0059 (10) | −0.0039 (11) | 0.0035 (10) |
O4 | 0.0295 (9) | 0.0334 (10) | 0.0455 (11) | −0.0067 (8) | 0.0009 (8) | −0.0038 (9) |
O5 | 0.0417 (11) | 0.0459 (12) | 0.0508 (12) | −0.0019 (10) | −0.0036 (10) | −0.0208 (10) |
O6 | 0.0279 (9) | 0.0249 (9) | 0.0292 (9) | 0.0009 (7) | 0.0017 (7) | −0.0026 (7) |
O7 | 0.0414 (11) | 0.0418 (11) | 0.0342 (10) | 0.0044 (9) | 0.0053 (8) | −0.0094 (9) |
O8 | 0.0320 (9) | 0.0265 (9) | 0.0313 (9) | −0.0020 (7) | 0.0032 (7) | 0.0000 (7) |
O9 | 0.0289 (9) | 0.0236 (8) | 0.0349 (9) | 0.0024 (7) | 0.0003 (7) | −0.0034 (7) |
O10 | 0.0310 (9) | 0.0356 (10) | 0.0416 (11) | 0.0041 (8) | −0.0037 (8) | 0.0009 (8) |
O11 | 0.0496 (12) | 0.0530 (13) | 0.0408 (11) | −0.0053 (10) | −0.0032 (10) | −0.0100 (10) |
O12 | 0.0298 (11) | 0.0560 (14) | 0.0621 (14) | 0.0000 (9) | −0.0013 (10) | −0.0007 (11) |
O13 | 0.0286 (9) | 0.0369 (10) | 0.0369 (10) | 0.0010 (8) | 0.0042 (8) | −0.0046 (8) |
O14 | 0.139 (4) | 0.192 (4) | 0.164 (4) | 0.031 (3) | 0.028 (3) | 0.023 (4) |
O15 | 0.271 (6) | 0.179 (4) | 0.149 (4) | −0.005 (4) | 0.037 (4) | 0.028 (4) |
C1 | 0.0339 (14) | 0.0402 (15) | 0.0392 (15) | −0.0002 (12) | 0.0010 (12) | −0.0077 (12) |
C2 | 0.0353 (15) | 0.0342 (14) | 0.0442 (16) | −0.0052 (12) | −0.0050 (12) | 0.0016 (12) |
C3 | 0.0287 (13) | 0.0361 (14) | 0.0411 (15) | −0.0005 (11) | −0.0012 (12) | 0.0027 (12) |
C4 | 0.0423 (17) | 0.0511 (18) | 0.0431 (16) | −0.0081 (14) | 0.0045 (14) | −0.0013 (14) |
C5 | 0.0544 (18) | 0.0353 (15) | 0.0397 (15) | −0.0037 (13) | 0.0202 (14) | −0.0005 (13) |
C6 | 0.0467 (17) | 0.0525 (18) | 0.0353 (15) | 0.0070 (14) | 0.0038 (13) | −0.0075 (14) |
C7 | 0.0408 (15) | 0.0295 (13) | 0.0430 (15) | 0.0042 (12) | −0.0038 (13) | −0.0036 (12) |
C8 | 0.0462 (17) | 0.0388 (16) | 0.0419 (16) | −0.0004 (13) | 0.0015 (13) | 0.0030 (13) |
C9 | 0.0380 (17) | 0.063 (2) | 0.0532 (19) | −0.0124 (15) | 0.0118 (15) | −0.0026 (16) |
C10 | 0.0511 (18) | 0.0430 (17) | 0.0416 (16) | 0.0004 (14) | −0.0065 (14) | −0.0070 (14) |
C11 | 0.064 (2) | 0.0499 (19) | 0.0415 (17) | 0.0159 (16) | 0.0115 (16) | 0.0041 (15) |
C12 | 0.057 (2) | 0.0402 (17) | 0.0472 (17) | −0.0095 (15) | −0.0121 (15) | 0.0105 (14) |
C13 | 0.065 (2) | 0.0278 (13) | 0.0416 (16) | 0.0078 (14) | 0.0257 (15) | 0.0044 (12) |
C14 | 0.0460 (17) | 0.0371 (15) | 0.0441 (16) | 0.0088 (13) | 0.0048 (13) | −0.0070 (13) |
C15 | 0.074 (2) | 0.0327 (16) | 0.064 (2) | 0.0084 (16) | −0.0207 (19) | 0.0050 (15) |
C16 | 0.065 (2) | 0.0381 (16) | 0.059 (2) | 0.0198 (16) | −0.0085 (17) | −0.0083 (15) |
C17 | 0.059 (2) | 0.058 (2) | 0.0485 (18) | 0.0208 (17) | 0.0095 (16) | 0.0120 (16) |
C18 | 0.0453 (18) | 0.069 (2) | 0.0449 (18) | −0.0012 (17) | 0.0171 (15) | −0.0071 (17) |
C19 | 0.062 (2) | 0.0420 (17) | 0.0540 (19) | −0.0026 (16) | −0.0171 (17) | −0.0085 (15) |
C20 | 0.0422 (18) | 0.058 (2) | 0.066 (2) | −0.0155 (16) | −0.0003 (16) | −0.0042 (17) |
C21 | 0.057 (2) | 0.049 (2) | 0.073 (2) | −0.0197 (17) | −0.0166 (19) | −0.0081 (18) |
C22 | 0.074 (3) | 0.082 (3) | 0.054 (2) | 0.044 (2) | 0.0123 (19) | 0.022 (2) |
C23 | 0.111 (4) | 0.053 (2) | 0.068 (3) | 0.033 (2) | 0.031 (3) | 0.026 (2) |
C24 | 0.096 (3) | 0.0428 (19) | 0.061 (2) | 0.011 (2) | 0.028 (2) | 0.0166 (17) |
C25 | 0.072 (2) | 0.0429 (18) | 0.069 (2) | −0.0181 (18) | 0.030 (2) | 0.0003 (17) |
C26 | 0.060 (2) | 0.075 (3) | 0.075 (3) | −0.030 (2) | 0.018 (2) | −0.014 (2) |
C27 | 0.0456 (19) | 0.078 (3) | 0.057 (2) | −0.0203 (18) | 0.0035 (16) | −0.0054 (19) |
C28 | 0.083 (3) | 0.076 (3) | 0.0426 (19) | 0.022 (2) | 0.0214 (18) | 0.0013 (18) |
C29 | 0.107 (4) | 0.087 (3) | 0.058 (2) | 0.048 (3) | 0.032 (2) | −0.007 (2) |
C30 | 0.098 (3) | 0.066 (2) | 0.064 (2) | 0.046 (2) | 0.025 (2) | −0.002 (2) |
N1 | 0.0290 (11) | 0.0333 (11) | 0.0321 (11) | 0.0003 (9) | 0.0021 (9) | −0.0021 (9) |
N2 | 0.0381 (12) | 0.0305 (11) | 0.0357 (12) | 0.0024 (10) | −0.0002 (10) | 0.0016 (10) |
N3 | 0.0393 (13) | 0.0340 (12) | 0.0357 (12) | −0.0037 (10) | 0.0115 (10) | −0.0032 (10) |
N4 | 0.0375 (12) | 0.0326 (12) | 0.0367 (12) | 0.0000 (10) | −0.0035 (10) | −0.0024 (10) |
N5 | 0.0488 (14) | 0.0351 (12) | 0.0380 (13) | 0.0131 (11) | 0.0107 (11) | 0.0059 (11) |
N6 | 0.0425 (13) | 0.0339 (12) | 0.0357 (12) | 0.0064 (10) | 0.0056 (10) | −0.0018 (10) |
Mo1—O7 | 1.6925 (18) | C6—C18 | 1.359 (4) |
Mo1—O13 | 1.7502 (18) | C6—H6 | 0.9300 |
Mo1—O9 | 1.9458 (17) | C7—N2 | 1.355 (3) |
Mo1—O8 | 1.9481 (17) | C7—C16 | 1.387 (4) |
Mo1—O6 | 2.1417 (17) | C7—C14 | 1.470 (4) |
Mo1—O6i | 2.3565 (17) | C8—N2 | 1.334 (4) |
Mo2—O1 | 1.6963 (19) | C8—C12 | 1.380 (4) |
Mo2—O2 | 1.7032 (19) | C8—H8 | 0.9300 |
Mo2—O10 | 1.8928 (18) | C9—C18 | 1.371 (5) |
Mo2—O8i | 2.0054 (18) | C9—H9 | 0.9300 |
Mo2—O6i | 2.3191 (16) | C10—N4 | 1.336 (4) |
Mo2—O9 | 2.3310 (17) | C10—C19 | 1.381 (4) |
Mo3—O11 | 1.693 (2) | C10—H10 | 0.9300 |
Mo3—O12 | 1.699 (2) | C11—N6 | 1.330 (4) |
Mo3—O10 | 1.9227 (19) | C11—C28 | 1.377 (4) |
Mo3—O4i | 1.9273 (19) | C11—H11 | 0.9300 |
Mo3—O13 | 2.3018 (18) | C12—C15 | 1.368 (5) |
Mo3—O6i | 2.4568 (17) | C12—H12 | 0.9300 |
Mo4—O3 | 1.693 (2) | C13—N5 | 1.345 (4) |
Mo4—O5 | 1.699 (2) | C13—C24 | 1.390 (4) |
Mo4—O4 | 1.8919 (18) | C14—N6 | 1.353 (3) |
Mo4—O9 | 2.0028 (17) | C14—C30 | 1.382 (4) |
Mo4—O8i | 2.3280 (17) | C15—C16 | 1.383 (5) |
Mo4—O6 | 2.3518 (16) | C15—H15 | 0.9300 |
Ni1—N3 | 2.070 (2) | C16—H16 | 0.9300 |
Ni1—N1 | 2.078 (2) | C17—N5 | 1.338 (4) |
Ni1—N5 | 2.078 (2) | C17—C22 | 1.395 (5) |
Ni1—N6 | 2.084 (2) | C17—H17 | 0.9300 |
Ni1—N2 | 2.091 (2) | C18—H18 | 0.9300 |
Ni1—N4 | 2.101 (2) | C19—C21 | 1.364 (5) |
O4—Mo3i | 1.9273 (19) | C19—H19 | 0.9300 |
O6—Mo2i | 2.3191 (16) | C20—C21 | 1.373 (5) |
O6—Mo1i | 2.3565 (17) | C20—H20 | 0.9300 |
O6—Mo3i | 2.4568 (17) | C21—H21 | 0.9300 |
O8—Mo2i | 2.0054 (17) | C22—C23 | 1.350 (6) |
O8—Mo4i | 2.3280 (17) | C22—H22 | 0.9300 |
C1—N1 | 1.339 (3) | C23—C24 | 1.369 (6) |
C1—C6 | 1.387 (4) | C23—H23 | 0.9300 |
C1—H1 | 0.9300 | C24—H24 | 0.9300 |
C2—N4 | 1.349 (4) | C25—C26 | 1.389 (6) |
C2—C20 | 1.396 (4) | C25—H25 | 0.9300 |
C2—C3 | 1.478 (4) | C26—C27 | 1.359 (5) |
C3—N1 | 1.341 (3) | C26—H26 | 0.9300 |
C3—C9 | 1.390 (4) | C27—H27 | 0.9300 |
C4—N3 | 1.329 (4) | C28—C29 | 1.367 (5) |
C4—C27 | 1.384 (4) | C28—H28 | 0.9300 |
C4—H4 | 0.9300 | C29—C30 | 1.367 (5) |
C5—N3 | 1.352 (3) | C29—H29 | 0.9300 |
C5—C25 | 1.395 (4) | C30—H30 | 0.9300 |
C5—C13 | 1.476 (5) | ||
O7—Mo1—O13 | 103.70 (9) | N1—C3—C2 | 115.6 (2) |
O7—Mo1—O9 | 101.51 (9) | C9—C3—C2 | 123.9 (3) |
O13—Mo1—O9 | 97.18 (8) | N3—C4—C27 | 123.2 (3) |
O7—Mo1—O8 | 101.04 (9) | N3—C4—H4 | 118.4 |
O13—Mo1—O8 | 95.98 (8) | C27—C4—H4 | 118.4 |
O9—Mo1—O8 | 150.30 (7) | N3—C5—C25 | 120.8 (3) |
O7—Mo1—O6 | 99.07 (8) | N3—C5—C13 | 115.3 (3) |
O13—Mo1—O6 | 157.21 (8) | C25—C5—C13 | 123.8 (3) |
O9—Mo1—O6 | 79.10 (7) | C18—C6—C1 | 118.9 (3) |
O8—Mo1—O6 | 78.48 (7) | C18—C6—H6 | 120.5 |
O7—Mo1—O6i | 175.11 (8) | C1—C6—H6 | 120.5 |
O13—Mo1—O6i | 81.18 (7) | N2—C7—C16 | 121.1 (3) |
O9—Mo1—O6i | 77.86 (6) | N2—C7—C14 | 115.7 (2) |
O8—Mo1—O6i | 78.02 (6) | C16—C7—C14 | 123.2 (3) |
O6—Mo1—O6i | 76.05 (7) | N2—C8—C12 | 123.4 (3) |
O1—Mo2—O2 | 104.58 (10) | N2—C8—H8 | 118.3 |
O1—Mo2—O10 | 102.32 (9) | C12—C8—H8 | 118.3 |
O2—Mo2—O10 | 101.02 (9) | C18—C9—C3 | 119.8 (3) |
O1—Mo2—O8i | 96.15 (8) | C18—C9—H9 | 120.1 |
O2—Mo2—O8i | 100.67 (9) | C3—C9—H9 | 120.1 |
O10—Mo2—O8i | 146.81 (8) | N4—C10—C19 | 122.9 (3) |
O1—Mo2—O6i | 94.97 (8) | N4—C10—H10 | 118.6 |
O2—Mo2—O6i | 160.12 (8) | C19—C10—H10 | 118.6 |
O10—Mo2—O6i | 77.87 (7) | N6—C11—C28 | 123.3 (3) |
O8i—Mo2—O6i | 73.22 (6) | N6—C11—H11 | 118.3 |
O1—Mo2—O9 | 163.75 (8) | C28—C11—H11 | 118.3 |
O2—Mo2—O9 | 88.45 (8) | C15—C12—C8 | 118.3 (3) |
O10—Mo2—O9 | 84.26 (7) | C15—C12—H12 | 120.9 |
O8i—Mo2—O9 | 71.52 (6) | C8—C12—H12 | 120.9 |
O6i—Mo2—O9 | 71.66 (6) | N5—C13—C24 | 120.6 (3) |
O11—Mo3—O12 | 104.36 (11) | N5—C13—C5 | 115.9 (2) |
O11—Mo3—O10 | 98.68 (10) | C24—C13—C5 | 123.4 (3) |
O12—Mo3—O10 | 103.17 (9) | N6—C14—C30 | 120.3 (3) |
O11—Mo3—O4i | 97.82 (10) | N6—C14—C7 | 116.2 (2) |
O12—Mo3—O4i | 102.29 (9) | C30—C14—C7 | 123.5 (3) |
O10—Mo3—O4i | 145.01 (8) | C12—C15—C16 | 119.6 (3) |
O11—Mo3—O13 | 164.25 (9) | C12—C15—H15 | 120.2 |
O12—Mo3—O13 | 91.37 (9) | C16—C15—H15 | 120.2 |
O10—Mo3—O13 | 78.01 (7) | C15—C16—C7 | 119.2 (3) |
O4i—Mo3—O13 | 77.77 (7) | C15—C16—H16 | 120.4 |
O11—Mo3—O6i | 94.88 (8) | C7—C16—H16 | 120.4 |
O12—Mo3—O6i | 160.75 (9) | N5—C17—C22 | 121.2 (4) |
O10—Mo3—O6i | 73.92 (7) | N5—C17—H17 | 119.4 |
O4i—Mo3—O6i | 74.11 (7) | C22—C17—H17 | 119.4 |
O13—Mo3—O6i | 69.38 (6) | C6—C18—C9 | 119.4 (3) |
O3—Mo4—O5 | 104.86 (11) | C6—C18—H18 | 120.3 |
O3—Mo4—O4 | 100.93 (10) | C9—C18—H18 | 120.3 |
O5—Mo4—O4 | 102.00 (9) | C21—C19—C10 | 118.5 (3) |
O3—Mo4—O9 | 102.05 (9) | C21—C19—H19 | 120.8 |
O5—Mo4—O9 | 95.09 (8) | C10—C19—H19 | 120.8 |
O4—Mo4—O9 | 146.65 (8) | C21—C20—C2 | 119.5 (3) |
O3—Mo4—O8i | 89.60 (9) | C21—C20—H20 | 120.2 |
O5—Mo4—O8i | 162.35 (8) | C2—C20—H20 | 120.2 |
O4—Mo4—O8i | 84.73 (7) | C19—C21—C20 | 119.7 (3) |
O9—Mo4—O8i | 71.63 (6) | C19—C21—H21 | 120.2 |
O3—Mo4—O6 | 160.91 (9) | C20—C21—H21 | 120.2 |
O5—Mo4—O6 | 94.04 (9) | C23—C22—C17 | 119.0 (4) |
O4—Mo4—O6 | 77.32 (7) | C23—C22—H22 | 120.5 |
O9—Mo4—O6 | 73.06 (6) | C17—C22—H22 | 120.5 |
O8i—Mo4—O6 | 71.31 (6) | C22—C23—C24 | 120.2 (4) |
N3—Ni1—N1 | 96.52 (9) | C22—C23—H23 | 119.9 |
N3—Ni1—N5 | 79.11 (10) | C24—C23—H23 | 119.9 |
N1—Ni1—N5 | 92.00 (9) | C23—C24—C13 | 119.2 (4) |
N3—Ni1—N6 | 90.27 (9) | C23—C24—H24 | 120.4 |
N1—Ni1—N6 | 171.31 (9) | C13—C24—H24 | 120.4 |
N5—Ni1—N6 | 94.61 (9) | C26—C25—C5 | 118.8 (3) |
N3—Ni1—N2 | 95.27 (9) | C26—C25—H25 | 120.6 |
N1—Ni1—N2 | 94.91 (9) | C5—C25—H25 | 120.6 |
N5—Ni1—N2 | 171.56 (9) | C27—C26—C25 | 119.8 (3) |
N6—Ni1—N2 | 79.02 (9) | C27—C26—H26 | 120.1 |
N3—Ni1—N4 | 174.02 (9) | C25—C26—H26 | 120.1 |
N1—Ni1—N4 | 78.63 (9) | C26—C27—C4 | 118.4 (4) |
N5—Ni1—N4 | 97.45 (10) | C26—C27—H27 | 120.8 |
N6—Ni1—N4 | 94.90 (9) | C4—C27—H27 | 120.8 |
N2—Ni1—N4 | 88.66 (9) | C29—C28—C11 | 118.0 (3) |
Mo4—O4—Mo3i | 118.00 (9) | C29—C28—H28 | 121.0 |
Mo1—O6—Mo2i | 92.41 (6) | C11—C28—H28 | 121.0 |
Mo1—O6—Mo4 | 91.67 (6) | C30—C29—C28 | 119.5 (3) |
Mo2i—O6—Mo4 | 163.47 (8) | C30—C29—H29 | 120.2 |
Mo1—O6—Mo1i | 103.95 (7) | C28—C29—H29 | 120.2 |
Mo2i—O6—Mo1i | 97.48 (6) | C29—C30—C14 | 120.2 (3) |
Mo4—O6—Mo1i | 97.06 (6) | C29—C30—H30 | 119.9 |
Mo1—O6—Mo3i | 163.79 (8) | C14—C30—H30 | 119.9 |
Mo2i—O6—Mo3i | 85.83 (6) | C1—N1—C3 | 119.3 (2) |
Mo4—O6—Mo3i | 85.79 (5) | C1—N1—Ni1 | 125.21 (18) |
Mo1i—O6—Mo3i | 92.24 (6) | C3—N1—Ni1 | 115.27 (18) |
Mo1—O8—Mo2i | 109.18 (8) | C8—N2—C7 | 118.3 (2) |
Mo1—O8—Mo4i | 110.87 (8) | C8—N2—Ni1 | 127.19 (19) |
Mo2i—O8—Mo4i | 103.72 (7) | C7—N2—Ni1 | 114.46 (18) |
Mo1—O9—Mo4 | 109.60 (8) | C4—N3—C5 | 118.9 (3) |
Mo1—O9—Mo2 | 110.22 (7) | C4—N3—Ni1 | 126.4 (2) |
Mo4—O9—Mo2 | 103.70 (7) | C5—N3—Ni1 | 114.7 (2) |
Mo2—O10—Mo3 | 117.01 (9) | C10—N4—C2 | 118.9 (3) |
Mo1—O13—Mo3 | 117.18 (9) | C10—N4—Ni1 | 126.5 (2) |
N1—C1—C6 | 121.9 (3) | C2—N4—Ni1 | 113.94 (18) |
N1—C1—H1 | 119.0 | C17—N5—C13 | 119.6 (3) |
C6—C1—H1 | 119.0 | C17—N5—Ni1 | 125.9 (2) |
N4—C2—C20 | 120.5 (3) | C13—N5—Ni1 | 114.4 (2) |
N4—C2—C3 | 115.9 (2) | C11—N6—C14 | 118.6 (3) |
C20—C2—C3 | 123.5 (3) | C11—N6—Ni1 | 126.9 (2) |
N1—C3—C9 | 120.5 (3) | C14—N6—Ni1 | 114.45 (18) |
Symmetry code: (i) −x+2, −y+1, −z+2. |