Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806037433/bi2061sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806037433/bi2061Isup2.hkl |
CCDC reference: 623997
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.
Na[H3Mo8O26][Cu2(C12H7N2O)2]3·0.5H2O | Z = 1 |
Mr = 2770.98 | F(000) = 1340 |
Triclinic, P1 | Dx = 2.259 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.640 (4) Å | Cell parameters from 250 reflections |
b = 13.651 (4) Å | θ = 2.5–25° |
c = 15.952 (5) Å | µ = 2.82 mm−1 |
α = 84.309 (4)° | T = 293 K |
β = 78.972 (4)° | Block, green |
γ = 82.091 (2)° | 0.18 × 0.16 × 0.15 mm |
V = 2035.1 (11) Å3 |
Bruker SMART APEX CCD diffractometer | 6828 independent reflections |
Radiation source: sealed tube | 4626 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.612, Tmax = 0.657 | k = −16→16 |
10029 measured reflections | l = −15→18 |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.159 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0899P)2] where P = (Fo2 + 2Fc2)/3 |
6828 reflections | (Δ/σ)max < 0.001 |
600 parameters | Δρmax = 2.28 e Å−3 |
0 restraints | Δρmin = −0.99 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 | Occ. (<1) | |
Na1 | 0.5000 | 0.0000 | 0.5000 | 0.0492 (15) | |
Mo1 | 0.12760 (8) | −0.06625 (5) | 0.64755 (5) | 0.0264 (2) | |
Mo2 | 0.26405 (8) | −0.21494 (5) | 0.49942 (5) | 0.0278 (2) | |
Mo3 | 0.21953 (8) | −0.03747 (5) | 0.35330 (5) | 0.0267 (2) | |
Mo4 | 0.08165 (7) | 0.10838 (5) | 0.50154 (4) | 0.01874 (19) | |
Cu1 | 0.15672 (12) | −0.47962 (8) | 1.03995 (7) | 0.0337 (3) | |
Cu2 | 0.20685 (13) | −0.63161 (8) | 0.96552 (8) | 0.0364 (3) | |
Cu3 | 0.49671 (12) | −0.57473 (8) | 0.04740 (7) | 0.0336 (3) | |
O1 | 0.2918 (7) | −0.0291 (5) | 0.6346 (4) | 0.0404 (16) | |
O2 | 0.0687 (8) | −0.0817 (5) | 0.7543 (4) | 0.0483 (18) | |
O3 | 0.3047 (7) | −0.3399 (5) | 0.4988 (4) | 0.0456 (17) | |
O4 | 0.4204 (7) | −0.1706 (4) | 0.5000 (4) | 0.0367 (15) | |
O5 | 0.3763 (6) | −0.0037 (4) | 0.3686 (4) | 0.0398 (16) | |
O6 | 0.2279 (8) | −0.0330 (5) | 0.2462 (4) | 0.0502 (19) | |
O7 | 0.2490 (6) | 0.1365 (5) | 0.5025 (4) | 0.0376 (16) | |
O8 | −0.0271 (6) | 0.2221 (4) | 0.5021 (4) | 0.0307 (14) | |
O9 | 0.0206 (6) | 0.0652 (4) | 0.6226 (4) | 0.0267 (13) | |
O10 | 0.1763 (6) | −0.1988 (4) | 0.6176 (4) | 0.0302 (14) | |
O11 | 0.2484 (6) | −0.1758 (4) | 0.3828 (4) | 0.0320 (14) | |
O12 | 0.0970 (6) | 0.0894 (4) | 0.3802 (3) | 0.0230 (13) | |
O13 | 0.1348 (6) | −0.0507 (4) | 0.5008 (3) | 0.0247 (13) | |
O1A | 0.1798 (8) | −0.4021 (5) | 0.9368 (4) | 0.0467 (18) | |
O2A | 0.1838 (7) | −0.7097 (5) | 1.0691 (4) | 0.0439 (17) | |
O3A | 0.4700 (7) | −0.3441 (4) | 0.0441 (4) | 0.0402 (16) | |
N1 | 0.2523 (9) | −0.7366 (6) | 0.8788 (5) | 0.039 (2) | |
N2 | 0.2166 (8) | −0.5415 (6) | 0.8673 (5) | 0.0302 (17) | |
N3 | 0.1066 (8) | −0.3712 (6) | 1.1254 (5) | 0.0354 (19) | |
N4 | 0.1379 (8) | −0.5696 (6) | 1.1384 (5) | 0.0321 (18) | |
N5 | 0.4860 (8) | −0.6790 (5) | 0.1481 (5) | 0.0368 (19) | |
N6 | 0.4535 (7) | −0.4817 (5) | 0.1339 (5) | 0.0301 (17) | |
C1 | 0.2751 (13) | −0.8348 (8) | 0.8871 (9) | 0.062 (3) | |
H1A | 0.2665 | −0.8660 | 0.9421 | 0.075* | |
C2 | 0.3111 (15) | −0.8930 (10) | 0.8185 (11) | 0.077 (4) | |
H2A | 0.3215 | −0.9618 | 0.8279 | 0.093* | |
C3 | 0.3312 (13) | −0.8508 (9) | 0.7378 (11) | 0.069 (4) | |
H3A | 0.3595 | −0.8897 | 0.6915 | 0.083* | |
C4 | 0.3085 (11) | −0.7456 (8) | 0.7246 (8) | 0.051 (3) | |
C5 | 0.2710 (9) | −0.6932 (7) | 0.7982 (6) | 0.035 (2) | |
C6 | 0.3266 (11) | −0.6882 (11) | 0.6415 (8) | 0.058 (3) | |
H6A | 0.3544 | −0.7212 | 0.5916 | 0.070* | |
C7 | 0.3040 (11) | −0.5898 (9) | 0.6362 (6) | 0.046 (3) | |
H7A | 0.3142 | −0.5553 | 0.5825 | 0.055* | |
C8 | 0.2640 (9) | −0.5349 (8) | 0.7120 (6) | 0.041 (3) | |
C9 | 0.2493 (10) | −0.5865 (7) | 0.7914 (6) | 0.033 (2) | |
C10 | 0.2425 (10) | −0.4308 (8) | 0.7103 (6) | 0.041 (3) | |
H10A | 0.2485 | −0.3932 | 0.6581 | 0.049* | |
C11 | 0.2127 (10) | −0.3848 (8) | 0.7848 (7) | 0.041 (3) | |
H11A | 0.1989 | −0.3159 | 0.7838 | 0.049* | |
C12 | 0.2031 (9) | −0.4437 (6) | 0.8648 (6) | 0.030 (2) | |
C13 | 0.0947 (10) | −0.2732 (7) | 1.1154 (7) | 0.038 (2) | |
H13A | 0.1096 | −0.2423 | 1.0603 | 0.046* | |
C14 | 0.0603 (11) | −0.2144 (7) | 1.1857 (8) | 0.049 (3) | |
H14A | 0.0513 | −0.1456 | 1.1774 | 0.059* | |
C15 | 0.0399 (11) | −0.2605 (8) | 1.2675 (8) | 0.051 (3) | |
H15A | 0.0159 | −0.2217 | 1.3140 | 0.061* | |
C16 | 0.0542 (9) | −0.3629 (8) | 1.2823 (6) | 0.039 (2) | |
C17 | 0.0907 (9) | −0.4184 (7) | 1.2052 (6) | 0.031 (2) | |
C18 | 0.0391 (10) | −0.4182 (9) | 1.3615 (7) | 0.045 (3) | |
H18A | 0.0189 | −0.3848 | 1.4113 | 0.054* | |
C19 | 0.0529 (10) | −0.5184 (8) | 1.3682 (6) | 0.039 (2) | |
H19A | 0.0406 | −0.5523 | 1.4221 | 0.047* | |
C20 | 0.0866 (10) | −0.5738 (7) | 1.2923 (6) | 0.038 (2) | |
C21 | 0.1043 (9) | −0.5210 (6) | 1.2136 (6) | 0.028 (2) | |
C22 | 0.1044 (10) | −0.6793 (7) | 1.2941 (6) | 0.039 (2) | |
H22A | 0.0958 | −0.7167 | 1.3464 | 0.047* | |
C23 | 0.1332 (10) | −0.7252 (7) | 1.2213 (7) | 0.044 (3) | |
H23A | 0.1425 | −0.7940 | 1.2226 | 0.052* | |
C24 | 0.1495 (10) | −0.6657 (7) | 1.1406 (6) | 0.034 (2) | |
C25 | 0.5067 (12) | −0.7772 (7) | 0.1523 (7) | 0.052 (3) | |
H25A | 0.5296 | −0.8091 | 0.1017 | 0.062* | |
C26 | 0.4950 (13) | −0.8344 (7) | 0.2307 (8) | 0.055 (3) | |
H26A | 0.5037 | −0.9032 | 0.2317 | 0.066* | |
C27 | 0.4705 (11) | −0.7881 (7) | 0.3072 (8) | 0.050 (3) | |
H27A | 0.4707 | −0.8251 | 0.3594 | 0.060* | |
C28 | 0.4455 (9) | −0.6843 (7) | 0.3033 (6) | 0.034 (2) | |
C29 | 0.4571 (9) | −0.6326 (6) | 0.2231 (5) | 0.027 (2) | |
C30 | 0.4143 (10) | −0.6281 (8) | 0.3773 (6) | 0.042 (3) | |
H30A | 0.4078 | −0.6613 | 0.4314 | 0.051* | |
C31 | 0.3944 (10) | −0.5295 (8) | 0.3701 (6) | 0.040 (2) | |
H31A | 0.3734 | −0.4957 | 0.4197 | 0.049* | |
C32 | 0.4043 (9) | −0.4730 (7) | 0.2882 (6) | 0.029 (2) | |
C33 | 0.4387 (9) | −0.5280 (7) | 0.2157 (6) | 0.029 (2) | |
C34 | 0.3880 (9) | −0.3721 (7) | 0.2745 (6) | 0.038 (2) | |
H34A | 0.3620 | −0.3338 | 0.3213 | 0.045* | |
C35 | 0.4087 (9) | −0.3259 (7) | 0.1936 (6) | 0.032 (2) | |
H35A | 0.3991 | −0.2570 | 0.1857 | 0.038* | |
C36 | 0.4458 (9) | −0.3853 (7) | 0.1206 (6) | 0.028 (2) | |
O1W | 0.371 (8) | −0.038 (5) | 0.040 (5) | 0.08 (2)* | 0.125 |
O2W | 0.028 (6) | −0.138 (4) | 0.925 (3) | 0.046 (14)* | 0.125 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1 | 0.053 (4) | 0.049 (4) | 0.049 (4) | −0.014 (3) | −0.015 (3) | −0.002 (3) |
Mo1 | 0.0278 (4) | 0.0238 (4) | 0.0285 (5) | −0.0002 (3) | −0.0089 (3) | −0.0034 (3) |
Mo2 | 0.0269 (4) | 0.0227 (4) | 0.0326 (5) | 0.0028 (3) | −0.0056 (3) | −0.0042 (3) |
Mo3 | 0.0247 (4) | 0.0257 (4) | 0.0274 (5) | −0.0009 (3) | 0.0001 (3) | −0.0026 (3) |
Mo4 | 0.0180 (4) | 0.0164 (4) | 0.0223 (4) | −0.0038 (3) | −0.0027 (3) | −0.0031 (3) |
Cu1 | 0.0398 (7) | 0.0324 (7) | 0.0297 (7) | −0.0082 (5) | −0.0038 (5) | −0.0056 (5) |
Cu2 | 0.0421 (7) | 0.0276 (6) | 0.0389 (7) | −0.0044 (5) | −0.0044 (6) | −0.0047 (5) |
Cu3 | 0.0392 (7) | 0.0313 (7) | 0.0298 (7) | −0.0058 (5) | −0.0034 (5) | −0.0029 (5) |
O1 | 0.032 (4) | 0.040 (4) | 0.051 (4) | 0.000 (3) | −0.012 (3) | −0.007 (3) |
O2 | 0.059 (5) | 0.047 (4) | 0.039 (4) | −0.006 (4) | −0.010 (4) | −0.005 (3) |
O3 | 0.046 (4) | 0.041 (4) | 0.045 (4) | 0.010 (3) | −0.007 (3) | −0.005 (3) |
O4 | 0.037 (4) | 0.037 (4) | 0.036 (4) | −0.002 (3) | −0.008 (3) | −0.005 (3) |
O5 | 0.028 (4) | 0.035 (4) | 0.055 (4) | −0.007 (3) | 0.002 (3) | −0.010 (3) |
O6 | 0.065 (5) | 0.044 (4) | 0.038 (4) | 0.002 (4) | −0.004 (4) | −0.008 (3) |
O7 | 0.030 (4) | 0.039 (4) | 0.046 (4) | −0.007 (3) | −0.009 (3) | −0.008 (3) |
O8 | 0.035 (4) | 0.021 (3) | 0.035 (4) | −0.003 (3) | −0.004 (3) | −0.005 (2) |
O9 | 0.027 (3) | 0.026 (3) | 0.026 (3) | −0.002 (3) | −0.002 (3) | −0.008 (2) |
O10 | 0.035 (4) | 0.022 (3) | 0.031 (4) | 0.004 (3) | −0.005 (3) | −0.003 (2) |
O11 | 0.034 (4) | 0.030 (3) | 0.030 (4) | −0.005 (3) | 0.002 (3) | −0.005 (3) |
O12 | 0.031 (3) | 0.015 (3) | 0.021 (3) | 0.001 (2) | −0.005 (3) | 0.000 (2) |
O13 | 0.018 (3) | 0.024 (3) | 0.034 (4) | −0.007 (2) | −0.006 (3) | −0.002 (3) |
O1A | 0.070 (5) | 0.031 (4) | 0.041 (4) | −0.016 (4) | −0.009 (4) | −0.001 (3) |
O2A | 0.056 (5) | 0.029 (4) | 0.046 (5) | −0.004 (3) | −0.009 (4) | −0.002 (3) |
O3A | 0.063 (5) | 0.030 (4) | 0.030 (4) | −0.008 (3) | −0.009 (3) | −0.007 (3) |
N1 | 0.042 (5) | 0.027 (4) | 0.049 (6) | 0.000 (4) | −0.013 (4) | −0.005 (4) |
N2 | 0.028 (4) | 0.040 (5) | 0.022 (4) | −0.006 (3) | −0.001 (3) | −0.004 (3) |
N3 | 0.034 (5) | 0.035 (5) | 0.040 (5) | −0.006 (4) | −0.007 (4) | −0.010 (4) |
N4 | 0.034 (4) | 0.034 (5) | 0.029 (4) | −0.008 (4) | −0.006 (3) | −0.002 (3) |
N5 | 0.036 (5) | 0.028 (4) | 0.042 (5) | 0.001 (4) | 0.000 (4) | −0.004 (4) |
N6 | 0.023 (4) | 0.030 (4) | 0.034 (5) | 0.002 (3) | 0.003 (3) | −0.011 (3) |
C1 | 0.069 (8) | 0.033 (6) | 0.084 (10) | 0.009 (6) | −0.023 (7) | −0.002 (6) |
C2 | 0.080 (10) | 0.038 (7) | 0.115 (13) | −0.004 (7) | −0.006 (9) | −0.039 (8) |
C3 | 0.046 (7) | 0.042 (7) | 0.120 (13) | 0.012 (6) | −0.008 (8) | −0.046 (8) |
C4 | 0.026 (6) | 0.058 (7) | 0.073 (9) | 0.003 (5) | −0.009 (5) | −0.032 (6) |
C5 | 0.022 (5) | 0.042 (6) | 0.043 (6) | −0.010 (4) | 0.004 (4) | −0.018 (5) |
C6 | 0.033 (6) | 0.102 (11) | 0.045 (7) | −0.001 (6) | −0.008 (5) | −0.033 (7) |
C7 | 0.041 (6) | 0.062 (8) | 0.030 (6) | −0.002 (5) | 0.000 (5) | −0.001 (5) |
C8 | 0.017 (5) | 0.070 (8) | 0.035 (6) | −0.008 (5) | 0.002 (4) | −0.007 (5) |
C9 | 0.031 (5) | 0.027 (5) | 0.040 (6) | 0.008 (4) | −0.010 (4) | −0.006 (4) |
C10 | 0.031 (6) | 0.057 (7) | 0.034 (6) | −0.013 (5) | −0.006 (4) | 0.010 (5) |
C11 | 0.034 (6) | 0.048 (6) | 0.041 (6) | −0.010 (5) | −0.012 (5) | 0.013 (5) |
C12 | 0.024 (5) | 0.027 (5) | 0.040 (6) | 0.003 (4) | −0.006 (4) | −0.013 (4) |
C13 | 0.037 (6) | 0.034 (6) | 0.047 (6) | −0.007 (4) | −0.012 (5) | −0.008 (5) |
C14 | 0.043 (6) | 0.025 (6) | 0.083 (9) | 0.006 (5) | −0.017 (6) | −0.021 (6) |
C15 | 0.038 (6) | 0.041 (6) | 0.080 (9) | −0.001 (5) | −0.013 (6) | −0.033 (6) |
C16 | 0.013 (5) | 0.062 (7) | 0.040 (6) | −0.004 (4) | 0.006 (4) | −0.022 (5) |
C17 | 0.019 (5) | 0.042 (6) | 0.036 (6) | −0.001 (4) | −0.006 (4) | −0.016 (4) |
C18 | 0.032 (6) | 0.067 (8) | 0.038 (6) | −0.005 (5) | 0.001 (5) | −0.020 (5) |
C19 | 0.031 (6) | 0.058 (7) | 0.024 (5) | −0.005 (5) | 0.005 (4) | −0.004 (5) |
C20 | 0.022 (5) | 0.047 (6) | 0.040 (6) | −0.004 (4) | 0.000 (4) | 0.000 (5) |
C21 | 0.024 (5) | 0.023 (5) | 0.034 (5) | 0.001 (4) | −0.002 (4) | −0.002 (4) |
C22 | 0.037 (6) | 0.047 (6) | 0.029 (6) | −0.016 (5) | 0.005 (4) | 0.012 (5) |
C23 | 0.038 (6) | 0.030 (6) | 0.062 (8) | 0.002 (4) | −0.011 (5) | −0.003 (5) |
C24 | 0.038 (6) | 0.028 (5) | 0.034 (6) | −0.005 (4) | 0.000 (4) | −0.006 (4) |
C25 | 0.069 (8) | 0.036 (6) | 0.045 (7) | −0.004 (5) | 0.006 (6) | −0.006 (5) |
C26 | 0.069 (8) | 0.022 (5) | 0.068 (8) | 0.007 (5) | −0.013 (6) | 0.006 (5) |
C27 | 0.041 (6) | 0.033 (6) | 0.067 (8) | 0.006 (5) | −0.007 (6) | 0.015 (5) |
C28 | 0.024 (5) | 0.031 (5) | 0.044 (6) | 0.005 (4) | −0.011 (4) | 0.004 (4) |
C29 | 0.024 (5) | 0.032 (5) | 0.021 (5) | 0.002 (4) | 0.002 (4) | 0.000 (4) |
C30 | 0.039 (6) | 0.056 (7) | 0.028 (6) | 0.002 (5) | −0.004 (4) | 0.003 (5) |
C31 | 0.040 (6) | 0.049 (7) | 0.031 (6) | 0.009 (5) | −0.010 (5) | −0.011 (5) |
C32 | 0.020 (5) | 0.039 (6) | 0.027 (5) | −0.006 (4) | −0.002 (4) | −0.001 (4) |
C33 | 0.020 (5) | 0.036 (5) | 0.027 (5) | 0.008 (4) | −0.003 (4) | −0.001 (4) |
C34 | 0.023 (5) | 0.046 (6) | 0.042 (6) | 0.000 (4) | −0.002 (4) | −0.005 (5) |
C35 | 0.029 (5) | 0.021 (5) | 0.047 (6) | 0.005 (4) | −0.008 (4) | −0.019 (4) |
C36 | 0.024 (5) | 0.034 (5) | 0.027 (5) | −0.002 (4) | −0.001 (4) | −0.010 (4) |
Na1—O4 | 2.550 (6) | N5—C25 | 1.324 (12) |
Na1—O4i | 2.550 (6) | N5—C29 | 1.372 (11) |
Na1—O5i | 2.610 (6) | N6—C36 | 1.306 (11) |
Na1—O5 | 2.610 (6) | N6—C33 | 1.384 (11) |
Na1—O1 | 2.682 (6) | C1—C2 | 1.380 (17) |
Na1—O1i | 2.682 (6) | C1—H1A | 0.930 |
Na1—O7i | 2.840 (6) | C2—C3 | 1.346 (19) |
Na1—O7 | 2.840 (6) | C2—H2A | 0.930 |
Mo1—O2 | 1.690 (7) | C3—C4 | 1.423 (16) |
Mo1—O1 | 1.698 (6) | C3—H3A | 0.930 |
Mo1—O10 | 1.891 (6) | C4—C5 | 1.398 (14) |
Mo1—O9 | 1.987 (6) | C4—C6 | 1.465 (17) |
Mo1—O13 | 2.319 (5) | C5—C9 | 1.439 (13) |
Mo1—O12ii | 2.359 (6) | C6—C7 | 1.328 (15) |
Mo1—Mo4 | 3.2104 (12) | C6—H6A | 0.930 |
Mo2—O3 | 1.698 (6) | C7—C8 | 1.447 (14) |
Mo2—O4 | 1.702 (6) | C7—H7A | 0.930 |
Mo2—O11 | 1.912 (6) | C8—C9 | 1.379 (13) |
Mo2—O10 | 1.934 (6) | C8—C10 | 1.406 (14) |
Mo2—O8ii | 2.304 (6) | C10—C11 | 1.363 (14) |
Mo2—O13 | 2.410 (5) | C10—H10A | 0.930 |
Mo3—O6 | 1.691 (7) | C11—C12 | 1.433 (13) |
Mo3—O5 | 1.706 (6) | C11—H11A | 0.930 |
Mo3—O11 | 1.895 (6) | C13—C14 | 1.406 (14) |
Mo3—O12 | 1.992 (5) | C13—H13A | 0.930 |
Mo3—O13 | 2.335 (6) | C14—C15 | 1.382 (16) |
Mo3—O9ii | 2.350 (6) | C14—H14A | 0.930 |
Mo3—Mo4 | 3.2134 (12) | C15—C16 | 1.386 (14) |
Mo4—O7 | 1.712 (6) | C15—H15A | 0.930 |
Mo4—O8 | 1.749 (6) | C16—C18 | 1.399 (14) |
Mo4—O12 | 1.953 (5) | C16—C17 | 1.469 (13) |
Mo4—O9 | 1.965 (6) | C17—C21 | 1.384 (12) |
Mo4—O13 | 2.162 (5) | C18—C19 | 1.352 (14) |
Mo4—O13ii | 2.337 (5) | C18—H18A | 0.930 |
Cu1—O1A | 1.860 (7) | C19—C20 | 1.450 (14) |
Cu1—N4 | 1.892 (7) | C19—H19A | 0.930 |
Cu1—N3 | 2.058 (8) | C20—C21 | 1.378 (13) |
Cu1—Cu2 | 2.4374 (17) | C20—C22 | 1.425 (14) |
Cu2—O2A | 1.868 (6) | C22—C23 | 1.338 (14) |
Cu2—N2 | 1.890 (7) | C22—H22A | 0.930 |
Cu2—N1 | 2.037 (8) | C23—C24 | 1.446 (14) |
Cu3—O3Aiii | 1.873 (6) | C23—H23A | 0.930 |
Cu3—N6 | 1.916 (7) | C25—C26 | 1.401 (14) |
Cu3—N5 | 2.036 (7) | C25—H25A | 0.930 |
Cu3—Cu3iii | 2.417 (2) | C26—C27 | 1.396 (15) |
O8—Mo2ii | 2.304 (6) | C26—H26A | 0.930 |
O9—Mo3ii | 2.350 (6) | C27—C28 | 1.402 (13) |
O12—Mo1ii | 2.359 (6) | C27—H27A | 0.930 |
O13—Mo4ii | 2.337 (5) | C28—C29 | 1.391 (12) |
O1A—C12 | 1.299 (11) | C28—C30 | 1.433 (14) |
O2A—C24 | 1.307 (11) | C29—C33 | 1.410 (12) |
O3A—C36 | 1.284 (10) | C30—C31 | 1.330 (13) |
O3A—Cu3iii | 1.873 (6) | C30—H30A | 0.930 |
N1—C1 | 1.325 (13) | C31—C32 | 1.443 (13) |
N1—C5 | 1.351 (12) | C31—H31A | 0.930 |
N2—C12 | 1.321 (11) | C32—C34 | 1.365 (13) |
N2—C9 | 1.375 (12) | C32—C33 | 1.403 (12) |
N3—C13 | 1.324 (11) | C34—C35 | 1.372 (13) |
N3—C17 | 1.359 (12) | C34—H34A | 0.930 |
N4—C24 | 1.300 (11) | C35—C36 | 1.446 (12) |
N4—C21 | 1.391 (11) | C35—H35A | 0.930 |
O4—Na1—O4i | 180.00 (8) | Mo4—O12—Mo1ii | 109.7 (2) |
O4—Na1—O5i | 109.41 (19) | Mo3—O12—Mo1ii | 104.6 (2) |
O4i—Na1—O5i | 70.59 (19) | Mo4—O13—Mo1 | 91.5 (2) |
O4—Na1—O5 | 70.59 (19) | Mo4—O13—Mo3 | 91.12 (19) |
O4i—Na1—O5 | 109.41 (19) | Mo1—O13—Mo3 | 161.7 (3) |
O5i—Na1—O5 | 180.0 | Mo4—O13—Mo4ii | 104.0 (2) |
O4—Na1—O1 | 70.02 (19) | Mo1—O13—Mo4ii | 98.7 (2) |
O4i—Na1—O1 | 109.98 (19) | Mo3—O13—Mo4ii | 98.26 (19) |
O5i—Na1—O1 | 76.61 (19) | Mo4—O13—Mo2 | 162.8 (3) |
O5—Na1—O1 | 103.39 (19) | Mo1—O13—Mo2 | 86.28 (18) |
O4—Na1—O1i | 109.98 (19) | Mo3—O13—Mo2 | 85.92 (19) |
O4i—Na1—O1i | 70.02 (19) | Mo4ii—O13—Mo2 | 93.20 (17) |
O5i—Na1—O1i | 103.39 (19) | C12—O1A—Cu1 | 120.0 (6) |
O5—Na1—O1i | 76.61 (19) | C24—O2A—Cu2 | 118.7 (6) |
O1—Na1—O1i | 180.0 | C36—O3A—Cu3iii | 118.1 (6) |
O4—Na1—O7i | 74.64 (18) | C1—N1—C5 | 117.0 (9) |
O4i—Na1—O7i | 105.36 (18) | C1—N1—Cu2 | 132.6 (8) |
O5i—Na1—O7i | 66.19 (19) | C5—N1—Cu2 | 110.3 (6) |
O5—Na1—O7i | 113.81 (19) | C12—N2—C9 | 118.8 (8) |
O1—Na1—O7i | 114.88 (18) | C12—N2—Cu2 | 127.3 (6) |
O1i—Na1—O7i | 65.12 (18) | C9—N2—Cu2 | 113.8 (6) |
O4—Na1—O7 | 105.36 (18) | C13—N3—C17 | 120.4 (8) |
O4i—Na1—O7 | 74.64 (18) | C13—N3—Cu1 | 132.7 (7) |
O5i—Na1—O7 | 113.81 (19) | C17—N3—Cu1 | 106.8 (6) |
O5—Na1—O7 | 66.19 (19) | C24—N4—C21 | 120.9 (8) |
O1—Na1—O7 | 65.12 (18) | C24—N4—Cu1 | 127.1 (6) |
O1i—Na1—O7 | 114.88 (18) | C21—N4—Cu1 | 112.0 (6) |
O7i—Na1—O7 | 180.0 (3) | C25—N5—C29 | 118.6 (8) |
O2—Mo1—O1 | 106.5 (3) | C25—N5—Cu3 | 132.2 (7) |
O2—Mo1—O10 | 101.9 (3) | C29—N5—Cu3 | 109.1 (6) |
O1—Mo1—O10 | 100.6 (3) | C36—N6—C33 | 121.6 (8) |
O2—Mo1—O9 | 99.6 (3) | C36—N6—Cu3 | 126.0 (6) |
O1—Mo1—O9 | 97.8 (3) | C33—N6—Cu3 | 112.3 (6) |
O10—Mo1—O9 | 146.3 (2) | N1—C1—C2 | 123.4 (13) |
O2—Mo1—O13 | 162.0 (3) | N1—C1—H1A | 118.3 |
O1—Mo1—O13 | 91.2 (3) | C2—C1—H1A | 118.3 |
O10—Mo1—O13 | 77.4 (2) | C3—C2—C1 | 120.3 (13) |
O9—Mo1—O13 | 74.2 (2) | C3—C2—H2A | 119.9 |
O2—Mo1—O12ii | 91.0 (3) | C1—C2—H2A | 119.9 |
O1—Mo1—O12ii | 160.7 (2) | C2—C3—C4 | 119.0 (12) |
O10—Mo1—O12ii | 83.1 (2) | C2—C3—H3A | 120.5 |
O9—Mo1—O12ii | 70.8 (2) | C4—C3—H3A | 120.5 |
O13—Mo1—O12ii | 71.00 (18) | C5—C4—C3 | 116.4 (12) |
O2—Mo1—Mo4 | 134.9 (2) | C5—C4—C6 | 117.7 (10) |
O1—Mo1—Mo4 | 83.4 (2) | C3—C4—C6 | 125.9 (12) |
O10—Mo1—Mo4 | 119.73 (17) | N1—C5—C4 | 123.9 (10) |
O9—Mo1—Mo4 | 35.44 (16) | N1—C5—C9 | 115.6 (8) |
O13—Mo1—Mo4 | 42.32 (13) | C4—C5—C9 | 120.5 (10) |
O12ii—Mo1—Mo4 | 78.45 (12) | C7—C6—C4 | 121.1 (10) |
O3—Mo2—O4 | 105.4 (3) | C7—C6—H6A | 119.4 |
O3—Mo2—O11 | 102.7 (3) | C4—C6—H6A | 119.4 |
O4—Mo2—O11 | 98.3 (3) | C6—C7—C8 | 121.5 (10) |
O3—Mo2—O10 | 102.2 (3) | C6—C7—H7A | 119.2 |
O4—Mo2—O10 | 98.6 (3) | C8—C7—H7A | 119.2 |
O11—Mo2—O10 | 144.8 (3) | C9—C8—C10 | 117.0 (9) |
O3—Mo2—O8ii | 92.8 (3) | C9—C8—C7 | 118.9 (10) |
O4—Mo2—O8ii | 161.8 (2) | C10—C8—C7 | 124.0 (9) |
O11—Mo2—O8ii | 76.9 (2) | N2—C9—C8 | 123.6 (9) |
O10—Mo2—O8ii | 77.4 (2) | N2—C9—C5 | 116.2 (8) |
O3—Mo2—O13 | 162.5 (3) | C8—C9—C5 | 120.2 (9) |
O4—Mo2—O13 | 92.1 (2) | C11—C10—C8 | 120.3 (9) |
O11—Mo2—O13 | 74.4 (2) | C11—C10—H10A | 119.8 |
O10—Mo2—O13 | 74.4 (2) | C8—C10—H10A | 119.8 |
O8ii—Mo2—O13 | 69.67 (18) | C10—C11—C12 | 119.3 (10) |
O6—Mo3—O5 | 106.4 (3) | C10—C11—H11A | 120.4 |
O6—Mo3—O11 | 102.2 (3) | C12—C11—H11A | 120.4 |
O5—Mo3—O11 | 100.4 (3) | O1A—C12—N2 | 118.3 (8) |
O6—Mo3—O12 | 100.5 (3) | O1A—C12—C11 | 120.8 (9) |
O5—Mo3—O12 | 97.9 (3) | N2—C12—C11 | 120.9 (9) |
O11—Mo3—O12 | 145.3 (2) | N3—C13—C14 | 121.8 (10) |
O6—Mo3—O13 | 162.1 (3) | N3—C13—H13A | 119.1 |
O5—Mo3—O13 | 91.3 (3) | C14—C13—H13A | 119.1 |
O11—Mo3—O13 | 76.6 (2) | C15—C14—C13 | 118.9 (10) |
O12—Mo3—O13 | 73.9 (2) | C15—C14—H14A | 120.5 |
O6—Mo3—O9ii | 90.9 (3) | C13—C14—H14A | 120.5 |
O5—Mo3—O9ii | 161.1 (3) | C14—C15—C16 | 122.1 (10) |
O11—Mo3—O9ii | 82.8 (2) | C14—C15—H15A | 118.9 |
O12—Mo3—O9ii | 71.0 (2) | C16—C15—H15A | 118.9 |
O13—Mo3—O9ii | 71.24 (19) | C15—C16—C18 | 127.6 (10) |
O6—Mo3—Mo4 | 135.4 (2) | C15—C16—C17 | 115.3 (10) |
O5—Mo3—Mo4 | 83.8 (2) | C18—C16—C17 | 117.2 (10) |
O11—Mo3—Mo4 | 118.83 (18) | N3—C17—C21 | 119.1 (8) |
O12—Mo3—Mo4 | 35.06 (15) | N3—C17—C16 | 121.5 (9) |
O13—Mo3—Mo4 | 42.28 (13) | C21—C17—C16 | 119.4 (9) |
O9ii—Mo3—Mo4 | 78.49 (14) | C19—C18—C16 | 122.4 (10) |
O7—Mo4—O8 | 105.6 (3) | C19—C18—H18A | 118.8 |
O7—Mo4—O12 | 100.5 (3) | C16—C18—H18A | 118.8 |
O8—Mo4—O12 | 97.0 (2) | C18—C19—C20 | 120.8 (9) |
O7—Mo4—O9 | 101.0 (3) | C18—C19—H19A | 119.6 |
O8—Mo4—O9 | 96.9 (3) | C20—C19—H19A | 119.6 |
O12—Mo4—O9 | 150.2 (2) | C21—C20—C22 | 117.9 (9) |
O7—Mo4—O13 | 97.3 (3) | C21—C20—C19 | 117.9 (9) |
O8—Mo4—O13 | 157.1 (2) | C22—C20—C19 | 124.2 (9) |
O12—Mo4—O13 | 78.7 (2) | C20—C21—C17 | 122.3 (9) |
O9—Mo4—O13 | 78.3 (2) | C20—C21—N4 | 120.7 (8) |
O7—Mo4—O13ii | 173.3 (2) | C17—C21—N4 | 116.9 (8) |
O8—Mo4—O13ii | 81.1 (2) | C23—C22—C20 | 120.8 (9) |
O12—Mo4—O13ii | 78.0 (2) | C23—C22—H22A | 119.6 |
O9—Mo4—O13ii | 78.2 (2) | C20—C22—H22A | 119.6 |
O13—Mo4—O13ii | 76.0 (2) | C22—C23—C24 | 118.7 (9) |
O7—Mo4—Mo1 | 88.6 (2) | C22—C23—H23A | 120.6 |
O8—Mo4—Mo1 | 132.81 (19) | C24—C23—H23A | 120.6 |
O12—Mo4—Mo1 | 124.92 (15) | N4—C24—O2A | 119.6 (8) |
O9—Mo4—Mo1 | 35.91 (17) | N4—C24—C23 | 120.9 (9) |
O13—Mo4—Mo1 | 46.22 (14) | O2A—C24—C23 | 119.4 (8) |
O13ii—Mo4—Mo1 | 86.96 (13) | N5—C25—C26 | 121.9 (10) |
O7—Mo4—Mo3 | 88.4 (2) | N5—C25—H25A | 119.0 |
O8—Mo4—Mo3 | 132.84 (19) | C26—C25—H25A | 119.0 |
O12—Mo4—Mo3 | 35.87 (15) | C27—C26—C25 | 120.0 (10) |
O9—Mo4—Mo3 | 124.88 (16) | C27—C26—H26A | 120.0 |
O13—Mo4—Mo3 | 46.60 (14) | C25—C26—H26A | 120.0 |
O13ii—Mo4—Mo3 | 86.68 (14) | C26—C27—C28 | 118.1 (9) |
Mo1—Mo4—Mo3 | 91.33 (3) | C26—C27—H27A | 120.9 |
O1A—Cu1—N4 | 174.3 (3) | C28—C27—H27A | 120.9 |
O1A—Cu1—N3 | 100.5 (3) | C29—C28—C27 | 118.3 (9) |
N4—Cu1—N3 | 85.1 (3) | C29—C28—C30 | 118.1 (9) |
O1A—Cu1—Cu2 | 91.5 (2) | C27—C28—C30 | 123.6 (9) |
N4—Cu1—Cu2 | 82.9 (2) | N5—C29—C28 | 122.8 (8) |
N3—Cu1—Cu2 | 168.0 (2) | N5—C29—C33 | 116.8 (7) |
O2A—Cu2—N2 | 173.7 (3) | C28—C29—C33 | 120.4 (8) |
O2A—Cu2—N1 | 101.6 (3) | C31—C30—C28 | 121.3 (9) |
N2—Cu2—N1 | 84.0 (3) | C31—C30—H30A | 119.3 |
O2A—Cu2—Cu1 | 91.6 (2) | C28—C30—H30A | 119.3 |
N2—Cu2—Cu1 | 82.8 (2) | C30—C31—C32 | 122.4 (9) |
N1—Cu2—Cu1 | 166.8 (2) | C30—C31—H31A | 118.8 |
O3Aiii—Cu3—N6 | 174.3 (3) | C32—C31—H31A | 118.8 |
O3Aiii—Cu3—N5 | 100.5 (3) | C34—C32—C33 | 117.2 (8) |
N6—Cu3—N5 | 84.6 (3) | C34—C32—C31 | 126.6 (9) |
O3Aiii—Cu3—Cu3iii | 92.4 (2) | C33—C32—C31 | 116.2 (8) |
N6—Cu3—Cu3iii | 82.6 (2) | N6—C33—C32 | 121.2 (8) |
N5—Cu3—Cu3iii | 167.1 (2) | N6—C33—C29 | 117.2 (8) |
Mo1—O1—Na1 | 134.7 (3) | C32—C33—C29 | 121.6 (8) |
Mo2—O4—Na1 | 135.9 (3) | C32—C34—C35 | 121.8 (9) |
Mo3—O5—Na1 | 135.6 (3) | C32—C34—H34A | 119.1 |
Mo4—O7—Na1 | 126.5 (3) | C35—C34—H34A | 119.1 |
Mo4—O8—Mo2ii | 116.0 (3) | C34—C35—C36 | 119.2 (9) |
Mo4—O9—Mo1 | 108.6 (3) | C34—C35—H35A | 120.4 |
Mo4—O9—Mo3ii | 109.6 (2) | C36—C35—H35A | 120.4 |
Mo1—O9—Mo3ii | 105.2 (2) | O3A—C36—N6 | 120.7 (8) |
Mo1—O10—Mo2 | 115.5 (3) | O3A—C36—C35 | 120.6 (8) |
Mo3—O11—Mo2 | 116.3 (3) | N6—C36—C35 | 118.7 (8) |
Mo4—O12—Mo3 | 109.1 (2) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x, −y, −z+1; (iii) −x+1, −y−1, −z. |