Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805001856/ac6148sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805001856/ac6148Isup2.hkl |
CCDC reference: 269353
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.005 Å
- R factor = 0.027
- wR factor = 0.075
- Data-to-parameter ratio = 12.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O1W - H2W ... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998) and Diamond (Klaus, 1999); software used to prepare material for publication: SHELXTL.
(C4H14N2)2[Mo5O15(H2PO4)2]·H2O | F(000) = 4320 |
Mr = 1110.02 | Dx = 2.554 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 8918 reflections |
a = 19.4776 (16) Å | θ = 2.4–28.3° |
b = 14.0453 (11) Å | µ = 2.33 mm−1 |
c = 21.1035 (17) Å | T = 273 K |
V = 5773.3 (8) Å3 | Block, colorless |
Z = 8 | 0.35 × 0.20 × 0.12 mm |
Bruker SMART CCD area-detector diffractometer | 5372 independent reflections |
Radiation source: fine-focus sealed tube | 5289 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.067 |
φ and ω scans | θmax = 25.5°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −23→23 |
Tmin = 0.571, Tmax = 0.752 | k = −16→17 |
41302 measured reflections | l = −25→25 |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.075 | H-atom parameters constrained |
S = 1.28 | w = 1/[σ2(Fo2) + (0.0372P)2 + 6.1694P] where P = (Fo2 + 2Fc2)/3 |
5372 reflections | (Δ/σ)max = 0.001 |
420 parameters | Δρmax = 0.67 e Å−3 |
0 restraints | Δρmin = −1.42 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 | 0.742210 (13) | 0.802916 (18) | 0.618878 (12) | 0.01797 (8) | |
Mo2 | 0.574306 (13) | 0.793388 (18) | 0.659101 (13) | 0.01952 (8) | |
Mo3 | 0.728973 (14) | 0.878777 (19) | 0.877404 (12) | 0.01999 (9) | |
Mo4 | 0.838192 (14) | 0.846643 (18) | 0.752507 (12) | 0.01977 (9) | |
Mo5 | 0.566457 (13) | 0.890838 (18) | 0.821084 (13) | 0.01946 (9) | |
P1 | 0.68567 (4) | 0.71073 (5) | 0.76677 (4) | 0.01713 (16) | |
P2 | 0.68748 (4) | 0.97195 (5) | 0.72401 (4) | 0.01557 (15) | |
O1 | 0.78934 (13) | 0.70844 (16) | 0.59310 (12) | 0.0306 (5) | |
O2 | 0.74196 (12) | 0.87963 (17) | 0.55643 (12) | 0.0295 (5) | |
O3 | 0.65248 (11) | 0.74502 (15) | 0.61258 (10) | 0.0219 (4) | |
O4 | 0.81121 (11) | 0.87220 (15) | 0.66736 (10) | 0.0216 (4) | |
O5 | 0.74774 (11) | 0.73412 (15) | 0.72407 (10) | 0.0211 (4) | |
O6 | 0.67238 (11) | 0.88793 (14) | 0.67971 (10) | 0.0193 (4) | |
O7 | 0.51561 (12) | 0.70462 (17) | 0.64624 (12) | 0.0306 (5) | |
O8 | 0.54797 (14) | 0.88055 (18) | 0.60907 (13) | 0.0344 (6) | |
O9 | 0.62482 (11) | 0.68073 (15) | 0.72737 (11) | 0.0219 (4) | |
O10 | 0.54705 (12) | 0.84210 (15) | 0.73893 (11) | 0.0249 (5) | |
O11 | 0.53313 (14) | 0.80416 (17) | 0.86783 (13) | 0.0350 (6) | |
O12 | 0.50904 (12) | 0.98204 (16) | 0.83097 (11) | 0.0264 (5) | |
O13 | 0.62337 (11) | 1.00362 (15) | 0.75775 (10) | 0.0208 (4) | |
O14 | 0.66667 (11) | 0.79504 (14) | 0.80987 (10) | 0.0205 (4) | |
O15 | 0.63951 (11) | 0.93615 (15) | 0.87485 (10) | 0.0221 (5) | |
O16 | 0.72285 (14) | 0.80675 (19) | 0.94152 (12) | 0.0372 (6) | |
O17 | 0.77222 (13) | 0.97581 (17) | 0.90577 (12) | 0.0335 (6) | |
O18 | 0.74474 (11) | 0.94827 (15) | 0.77168 (10) | 0.0204 (4) | |
O19 | 0.80327 (11) | 0.81389 (15) | 0.83490 (10) | 0.0223 (4) | |
O20 | 0.89375 (12) | 0.75377 (18) | 0.74443 (12) | 0.0316 (5) | |
O21 | 0.88894 (13) | 0.94274 (18) | 0.76624 (13) | 0.0332 (5) | |
O22 | 0.71487 (12) | 1.05157 (14) | 0.67790 (11) | 0.0252 (5) | |
O23 | 0.70808 (14) | 0.63025 (16) | 0.81421 (11) | 0.0318 (5) | |
N1 | 0.62567 (15) | −0.0390 (2) | 1.11890 (14) | 0.0277 (6) | |
N2 | 0.62929 (15) | 0.14530 (19) | 0.86939 (13) | 0.0263 (6) | |
N3 | 0.34222 (19) | 0.9621 (3) | 0.47668 (17) | 0.0522 (10) | |
N4 | 0.49966 (15) | 0.8857 (2) | 0.27993 (14) | 0.0292 (6) | |
C1 | 0.61874 (18) | −0.0181 (2) | 1.05008 (17) | 0.0299 (7) | |
C2 | 0.58450 (17) | 0.0774 (2) | 1.04039 (16) | 0.0266 (7) | |
C3 | 0.57524 (17) | 0.1026 (3) | 0.97074 (17) | 0.0292 (7) | |
C4 | 0.64066 (17) | 0.1347 (2) | 0.93902 (15) | 0.0258 (7) | |
C5 | 0.3974 (2) | 0.8968 (3) | 0.49671 (18) | 0.0368 (8) | |
C6 | 0.46018 (19) | 0.9066 (3) | 0.45515 (18) | 0.0356 (8) | |
C7 | 0.44741 (17) | 0.8851 (2) | 0.38598 (17) | 0.0285 (7) | |
C8 | 0.51056 (16) | 0.9084 (2) | 0.34797 (15) | 0.0269 (7) | |
H22B | 0.6272 | 0.0935 | 0.8505 | 0.057 (15)* | |
H3B | 0.5563 | 0.0455 | 0.9487 | 0.043 (12)* | |
H7A | 0.4103 | 0.9246 | 0.3689 | 0.030 (10)* | |
H2A | 0.6088 | 0.1215 | 1.0570 | 0.029 (12)* | |
H3A | 0.5448 | 0.1505 | 0.9651 | 0.041 (12)* | |
H8B | 0.5478 | 0.8744 | 0.3588 | 0.040 (11)* | |
H42C | 0.4822 | 0.8269 | 0.2762 | 0.072 (17)* | |
H6B | 0.4952 | 0.8708 | 0.4705 | 0.065 (15)* | |
H2B | 0.5404 | 0.0737 | 1.0570 | 0.040 (11)* | |
H1A | 0.5951 | −0.0675 | 1.0314 | 0.050 (13)* | |
H7B | 0.4335 | 0.8234 | 0.3840 | 0.028 (10)* | |
H12A | 0.5880 | −0.0464 | 1.1362 | 0.025 (10)* | |
H8A | 0.5135 | 0.9791 | 0.3440 | 0.039 (11)* | |
H1P | 0.7080 | 0.5630 | 0.7988 | 0.039 (11)* | |
H1B | 0.6645 | −0.0239 | 1.0283 | 0.036 (11)* | |
H4A | 0.6570 | 0.1962 | 0.9534 | 0.052 (13)* | |
H12B | 0.6430 | −0.0960 | 1.1155 | 0.063 (16)* | |
H22C | 0.6605 | 0.1828 | 0.8491 | 0.056 (14)* | |
H4B | 0.6776 | 0.0803 | 0.9389 | 0.065 (15)* | |
H12C | 0.6566 | 0.0035 | 1.1379 | 0.040 (11)* | |
H22A | 0.5840 | 0.1675 | 0.8568 | 0.064 (16)* | |
H42B | 0.5398 | 0.8815 | 0.2556 | 0.064 (16)* | |
H5B | 0.3805 | 0.8292 | 0.4949 | 0.054 (13)* | |
H5A | 0.4111 | 0.9154 | 0.5410 | 0.036 (11)* | |
H42A | 0.4696 | 0.9329 | 0.2599 | 0.042 (12)* | |
H6A | 0.4734 | 0.9753 | 0.4564 | 0.055 (14)* | |
H2P | 0.7135 | 1.1122 | 0.6884 | 0.048 (13)* | |
H32A | 0.3569 | 1.0219 | 0.4794 | 0.079* | |
H32B | 0.3059 | 0.9544 | 0.5018 | 0.079* | |
H32C | 0.3304 | 0.9492 | 0.4369 | 0.079* | |
H1W | 0.8489 | 0.1343 | 0.9234 | 0.048 (13)* | |
H2W | 0.8901 | 0.1846 | 0.9831 | 0.048 (13)* | |
O1W | 0.8674 (2) | 0.1355 (4) | 0.9583 (3) | 0.0995 (17) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.01703 (14) | 0.01652 (14) | 0.02034 (15) | 0.00051 (9) | 0.00165 (9) | 0.00050 (9) |
Mo2 | 0.01616 (14) | 0.01764 (14) | 0.02475 (16) | −0.00061 (9) | −0.00176 (10) | −0.00303 (10) |
Mo3 | 0.02128 (15) | 0.01856 (14) | 0.02011 (15) | 0.00348 (10) | −0.00234 (10) | −0.00084 (9) |
Mo4 | 0.01518 (15) | 0.02002 (15) | 0.02411 (15) | 0.00135 (9) | −0.00094 (9) | 0.00187 (10) |
Mo5 | 0.01691 (14) | 0.01637 (14) | 0.02511 (16) | −0.00009 (9) | 0.00342 (10) | −0.00257 (10) |
P1 | 0.0176 (4) | 0.0124 (3) | 0.0214 (4) | 0.0009 (3) | 0.0023 (3) | 0.0003 (3) |
P2 | 0.0147 (3) | 0.0121 (3) | 0.0199 (4) | −0.0004 (3) | −0.0012 (3) | 0.0005 (3) |
O1 | 0.0301 (13) | 0.0268 (12) | 0.0350 (13) | 0.0070 (10) | 0.0062 (10) | −0.0036 (10) |
O2 | 0.0295 (12) | 0.0307 (12) | 0.0282 (13) | −0.0011 (10) | −0.0003 (10) | 0.0082 (10) |
O3 | 0.0221 (11) | 0.0190 (10) | 0.0246 (11) | −0.0010 (9) | 0.0000 (9) | −0.0040 (8) |
O4 | 0.0181 (11) | 0.0233 (11) | 0.0235 (11) | −0.0016 (8) | 0.0010 (9) | 0.0039 (8) |
O5 | 0.0172 (10) | 0.0205 (10) | 0.0256 (11) | 0.0016 (8) | 0.0027 (8) | 0.0039 (9) |
O6 | 0.0161 (10) | 0.0175 (10) | 0.0244 (11) | −0.0011 (8) | −0.0001 (8) | −0.0030 (8) |
O7 | 0.0228 (12) | 0.0311 (13) | 0.0379 (13) | −0.0075 (10) | −0.0018 (10) | −0.0067 (10) |
O8 | 0.0348 (14) | 0.0303 (13) | 0.0379 (14) | 0.0073 (11) | −0.0066 (11) | 0.0012 (10) |
O9 | 0.0195 (11) | 0.0183 (10) | 0.0278 (11) | −0.0041 (8) | 0.0018 (9) | −0.0022 (9) |
O10 | 0.0175 (11) | 0.0254 (12) | 0.0320 (12) | −0.0018 (8) | −0.0003 (9) | −0.0075 (9) |
O11 | 0.0351 (14) | 0.0260 (12) | 0.0437 (15) | −0.0049 (10) | 0.0142 (12) | 0.0030 (10) |
O12 | 0.0212 (11) | 0.0254 (12) | 0.0326 (12) | 0.0039 (9) | 0.0041 (9) | −0.0039 (9) |
O13 | 0.0183 (10) | 0.0172 (10) | 0.0269 (11) | 0.0038 (8) | 0.0008 (9) | −0.0014 (8) |
O14 | 0.0187 (10) | 0.0175 (10) | 0.0253 (11) | 0.0012 (8) | 0.0005 (8) | −0.0028 (8) |
O15 | 0.0218 (11) | 0.0204 (10) | 0.0243 (11) | 0.0032 (9) | 0.0004 (8) | −0.0039 (8) |
O16 | 0.0434 (15) | 0.0379 (14) | 0.0303 (13) | 0.0115 (12) | 0.0034 (11) | 0.0097 (11) |
O17 | 0.0325 (13) | 0.0286 (13) | 0.0393 (14) | 0.0017 (10) | −0.0102 (11) | −0.0098 (11) |
O18 | 0.0182 (10) | 0.0190 (10) | 0.0239 (11) | 0.0030 (8) | −0.0031 (8) | −0.0009 (8) |
O19 | 0.0206 (11) | 0.0225 (10) | 0.0239 (11) | 0.0041 (9) | −0.0016 (9) | 0.0018 (8) |
O20 | 0.0237 (12) | 0.0336 (13) | 0.0376 (13) | 0.0098 (10) | 0.0011 (10) | 0.0015 (10) |
O21 | 0.0243 (12) | 0.0338 (13) | 0.0414 (14) | −0.0071 (10) | −0.0041 (11) | 0.0013 (11) |
O22 | 0.0301 (12) | 0.0157 (10) | 0.0299 (12) | −0.0030 (9) | 0.0021 (10) | 0.0043 (9) |
O23 | 0.0469 (15) | 0.0181 (11) | 0.0304 (13) | 0.0067 (10) | 0.0004 (11) | 0.0042 (9) |
N1 | 0.0266 (15) | 0.0233 (14) | 0.0333 (15) | −0.0033 (12) | −0.0005 (12) | 0.0050 (11) |
N2 | 0.0310 (15) | 0.0222 (14) | 0.0257 (14) | −0.0055 (11) | 0.0025 (12) | 0.0016 (11) |
N3 | 0.048 (2) | 0.066 (2) | 0.0421 (19) | 0.0276 (19) | 0.0087 (17) | −0.0002 (18) |
N4 | 0.0245 (15) | 0.0348 (15) | 0.0284 (15) | 0.0021 (12) | 0.0020 (12) | −0.0006 (12) |
C1 | 0.0330 (18) | 0.0251 (16) | 0.0314 (17) | −0.0001 (14) | 0.0017 (14) | −0.0001 (13) |
C2 | 0.0247 (16) | 0.0304 (17) | 0.0247 (16) | 0.0010 (14) | 0.0019 (13) | 0.0003 (13) |
C3 | 0.0233 (16) | 0.0376 (19) | 0.0266 (18) | 0.0015 (14) | 0.0001 (13) | 0.0044 (14) |
C4 | 0.0254 (16) | 0.0256 (16) | 0.0265 (17) | −0.0026 (13) | −0.0017 (13) | −0.0007 (13) |
C5 | 0.039 (2) | 0.043 (2) | 0.0287 (18) | 0.0049 (16) | 0.0019 (16) | 0.0051 (15) |
C6 | 0.0301 (18) | 0.048 (2) | 0.0287 (18) | 0.0008 (16) | −0.0015 (15) | 0.0014 (16) |
C7 | 0.0223 (16) | 0.0327 (18) | 0.0303 (18) | 0.0019 (14) | −0.0007 (13) | −0.0024 (13) |
C8 | 0.0240 (16) | 0.0267 (17) | 0.0301 (17) | 0.0005 (13) | 0.0002 (13) | −0.0018 (13) |
O1W | 0.072 (3) | 0.097 (3) | 0.130 (4) | 0.019 (3) | 0.045 (3) | 0.033 (3) |
Mo1—O2 | 1.702 (2) | N1—C1 | 1.488 (4) |
Mo1—O1 | 1.703 (2) | N1—H12A | 0.8259 |
Mo1—O3 | 1.932 (2) | N1—H12B | 0.8717 |
Mo1—O4 | 1.949 (2) | N1—H12C | 0.9389 |
Mo1—O6 | 2.219 (2) | N2—C4 | 1.493 (4) |
Mo1—O5 | 2.424 (2) | N2—H22B | 0.8311 |
Mo2—O8 | 1.696 (2) | N2—H22C | 0.9114 |
Mo2—O7 | 1.713 (2) | N2—H22A | 0.9721 |
Mo2—O10 | 1.894 (2) | N3—C5 | 1.475 (5) |
Mo2—O3 | 1.935 (2) | N3—H32A | 0.8900 |
Mo2—O9 | 2.355 (2) | N3—H32B | 0.8900 |
Mo2—O6 | 2.367 (2) | N3—H32C | 0.8900 |
Mo3—O16 | 1.694 (2) | N4—C8 | 1.486 (4) |
Mo3—O17 | 1.710 (2) | N4—H42C | 0.8965 |
Mo3—O15 | 1.921 (2) | N4—H42B | 0.9361 |
Mo3—O19 | 1.931 (2) | N4—H42A | 0.9797 |
Mo3—O14 | 2.211 (2) | C1—C2 | 1.512 (5) |
Mo3—O18 | 2.455 (2) | C1—H1A | 0.9216 |
Mo4—O21 | 1.698 (2) | C1—H1B | 1.0065 |
Mo4—O20 | 1.703 (2) | C2—C3 | 1.523 (5) |
Mo4—O4 | 1.906 (2) | C2—H2A | 0.8544 |
Mo4—O19 | 1.923 (2) | C2—H2B | 0.9297 |
Mo4—O18 | 2.348 (2) | C3—C4 | 1.508 (5) |
Mo4—O5 | 2.442 (2) | C3—H3B | 0.9970 |
Mo5—O11 | 1.696 (2) | C3—H3A | 0.9044 |
Mo5—O12 | 1.713 (2) | C4—H4A | 0.9689 |
Mo5—O10 | 1.902 (2) | C4—H4B | 1.0498 |
Mo5—O15 | 1.928 (2) | C5—C6 | 1.510 (5) |
Mo5—O13 | 2.350 (2) | C5—H5B | 1.0061 |
Mo5—O14 | 2.383 (2) | C5—H5A | 1.0066 |
P1—O9 | 1.508 (2) | C6—C7 | 1.511 (5) |
P1—O14 | 1.538 (2) | C6—H6B | 0.9080 |
P1—O5 | 1.543 (2) | C6—H6A | 0.9986 |
P1—O23 | 1.572 (2) | C7—C8 | 1.504 (5) |
P2—O13 | 1.505 (2) | C7—H7A | 0.9804 |
P2—O6 | 1.534 (2) | C7—H7B | 0.9088 |
P2—O18 | 1.538 (2) | C8—H8B | 0.8981 |
P2—O22 | 1.576 (2) | C8—H8A | 0.9985 |
O22—H2P | 0.8802 | O1W—H1W | 0.8193 |
O23—H1P | 0.9995 | O1W—H2W | 0.9690 |
O2—Mo1—O1 | 104.33 (12) | Mo1—O5—Mo4 | 89.95 (7) |
O2—Mo1—O3 | 102.15 (11) | P2—O6—Mo1 | 130.48 (12) |
O1—Mo1—O3 | 97.92 (11) | P2—O6—Mo2 | 134.29 (12) |
O2—Mo1—O4 | 95.30 (10) | Mo1—O6—Mo2 | 94.96 (7) |
O1—Mo1—O4 | 100.66 (11) | P1—O9—Mo2 | 118.55 (12) |
O3—Mo1—O4 | 150.44 (9) | Mo2—O10—Mo5 | 152.26 (13) |
O2—Mo1—O6 | 96.05 (10) | P2—O13—Mo5 | 117.47 (12) |
O1—Mo1—O6 | 159.17 (10) | P1—O14—Mo3 | 131.20 (12) |
O3—Mo1—O6 | 73.25 (8) | P1—O14—Mo5 | 133.67 (12) |
O4—Mo1—O6 | 81.39 (9) | Mo3—O14—Mo5 | 94.89 (7) |
O2—Mo1—O5 | 164.08 (10) | Mo3—O15—Mo5 | 123.20 (11) |
O1—Mo1—O5 | 87.59 (10) | P2—O18—Mo4 | 125.50 (12) |
O3—Mo1—O5 | 86.30 (8) | P2—O18—Mo3 | 126.13 (12) |
O4—Mo1—O5 | 71.80 (8) | Mo4—O18—Mo3 | 90.68 (7) |
O6—Mo1—O5 | 73.25 (7) | Mo4—O19—Mo3 | 124.90 (11) |
O8—Mo2—O7 | 102.99 (12) | P2—O22—H2P | 121.3 |
O8—Mo2—O10 | 102.02 (11) | P1—O23—H1P | 118.2 |
O7—Mo2—O10 | 102.52 (11) | C1—N1—H12A | 112.0 |
O8—Mo2—O3 | 100.10 (11) | C1—N1—H12B | 97.7 |
O7—Mo2—O3 | 100.91 (10) | H12A—N1—H12B | 105.3 |
O10—Mo2—O3 | 143.00 (10) | C1—N1—H12C | 110.5 |
O8—Mo2—O9 | 172.77 (11) | H12A—N1—H12C | 117.5 |
O7—Mo2—O9 | 83.50 (10) | H12B—N1—H12C | 111.8 |
O10—Mo2—O9 | 79.38 (9) | C4—N2—H22B | 113.1 |
O3—Mo2—O9 | 75.28 (8) | C4—N2—H22C | 114.8 |
O8—Mo2—O6 | 87.33 (11) | H22B—N2—H22C | 108.3 |
O7—Mo2—O6 | 167.43 (10) | C4—N2—H22A | 115.7 |
O10—Mo2—O6 | 81.96 (9) | H22B—N2—H22A | 96.1 |
O3—Mo2—O6 | 69.82 (8) | H22C—N2—H22A | 107.0 |
O9—Mo2—O6 | 85.83 (7) | C5—N3—H32A | 109.5 |
O16—Mo3—O17 | 103.36 (13) | C5—N3—H32B | 109.5 |
O16—Mo3—O15 | 102.07 (11) | H32A—N3—H32B | 109.5 |
O17—Mo3—O15 | 97.03 (11) | C5—N3—H32C | 109.5 |
O16—Mo3—O19 | 98.16 (11) | H32A—N3—H32C | 109.5 |
O17—Mo3—O19 | 99.76 (11) | H32B—N3—H32C | 109.5 |
O15—Mo3—O19 | 149.87 (9) | C8—N4—H42C | 109.6 |
O16—Mo3—O14 | 99.12 (11) | C8—N4—H42B | 115.1 |
O17—Mo3—O14 | 156.92 (10) | H42C—N4—H42B | 102.1 |
O15—Mo3—O14 | 72.97 (8) | C8—N4—H42A | 110.9 |
O19—Mo3—O14 | 82.00 (9) | H42C—N4—H42A | 111.1 |
O16—Mo3—O18 | 166.54 (10) | H42B—N4—H42A | 107.7 |
O17—Mo3—O18 | 86.54 (10) | N1—C1—C2 | 110.3 (3) |
O15—Mo3—O18 | 85.48 (8) | N1—C1—H1A | 108.3 |
O19—Mo3—O18 | 70.84 (8) | C2—C1—H1A | 112.9 |
O14—Mo3—O18 | 72.20 (7) | N1—C1—H1B | 110.5 |
O21—Mo4—O20 | 104.83 (13) | C2—C1—H1B | 113.6 |
O21—Mo4—O4 | 99.89 (11) | H1A—C1—H1B | 100.8 |
O20—Mo4—O4 | 103.00 (11) | C1—C2—C3 | 112.9 (3) |
O21—Mo4—O19 | 103.99 (11) | C1—C2—H2A | 110.1 |
O20—Mo4—O19 | 97.59 (11) | C3—C2—H2A | 107.1 |
O4—Mo4—O19 | 143.12 (10) | C1—C2—H2B | 107.9 |
O21—Mo4—O18 | 86.48 (10) | C3—C2—H2B | 105.5 |
O20—Mo4—O18 | 167.20 (10) | H2A—C2—H2B | 113.4 |
O4—Mo4—O18 | 80.46 (9) | C4—C3—C2 | 113.4 (3) |
O19—Mo4—O18 | 73.47 (8) | C4—C3—H3B | 110.2 |
O21—Mo4—O5 | 167.57 (10) | C2—C3—H3B | 107.9 |
O20—Mo4—O5 | 86.45 (10) | C4—C3—H3A | 105.9 |
O4—Mo4—O5 | 72.02 (8) | C2—C3—H3A | 112.1 |
O19—Mo4—O5 | 79.17 (9) | H3B—C3—H3A | 107.2 |
O18—Mo4—O5 | 82.91 (8) | N2—C4—C3 | 109.9 (3) |
O11—Mo5—O12 | 102.48 (12) | N2—C4—H4A | 105.6 |
O11—Mo5—O10 | 101.29 (12) | C3—C4—H4A | 113.9 |
O12—Mo5—O10 | 104.50 (11) | N2—C4—H4B | 99.9 |
O11—Mo5—O15 | 100.20 (12) | C3—C4—H4B | 111.3 |
O12—Mo5—O15 | 99.40 (10) | H4A—C4—H4B | 115.0 |
O10—Mo5—O15 | 143.32 (9) | N3—C5—C6 | 111.5 (3) |
O11—Mo5—O13 | 174.27 (11) | N3—C5—H5B | 109.6 |
O12—Mo5—O13 | 82.72 (9) | C6—C5—H5B | 109.3 |
O10—Mo5—O13 | 79.51 (9) | N3—C5—H5A | 107.3 |
O15—Mo5—O13 | 76.36 (8) | C6—C5—H5A | 107.6 |
O11—Mo5—O14 | 88.05 (10) | H5B—C5—H5A | 111.5 |
O12—Mo5—O14 | 165.73 (9) | C5—C6—C7 | 114.2 (3) |
O10—Mo5—O14 | 82.47 (9) | C5—C6—H6B | 110.5 |
O15—Mo5—O14 | 68.91 (8) | C7—C6—H6B | 111.0 |
O13—Mo5—O14 | 86.43 (7) | C5—C6—H6A | 106.3 |
O9—P1—O14 | 110.62 (12) | C7—C6—H6A | 105.2 |
O9—P1—O5 | 110.69 (12) | H6B—C6—H6A | 109.3 |
O14—P1—O5 | 111.71 (12) | C8—C7—C6 | 109.7 (3) |
O9—P1—O23 | 111.62 (14) | C8—C7—H7A | 106.5 |
O14—P1—O23 | 104.10 (12) | C6—C7—H7A | 111.2 |
O5—P1—O23 | 107.91 (13) | C8—C7—H7B | 115.2 |
O13—P2—O6 | 110.90 (12) | C6—C7—H7B | 106.5 |
O13—P2—O18 | 110.87 (12) | H7A—C7—H7B | 107.7 |
O6—P2—O18 | 111.79 (12) | N4—C8—C7 | 110.6 (3) |
O13—P2—O22 | 111.32 (12) | N4—C8—H8B | 104.3 |
O6—P2—O22 | 103.56 (12) | C7—C8—H8B | 114.2 |
O18—P2—O22 | 108.17 (13) | N4—C8—H8A | 98.1 |
Mo1—O3—Mo2 | 121.95 (11) | C7—C8—H8A | 107.9 |
Mo4—O4—Mo1 | 126.22 (11) | H8B—C8—H8A | 120.2 |
P1—O5—Mo1 | 125.79 (12) | H1W—O1W—H2W | 134.3 |
P1—O5—Mo4 | 124.03 (12) | ||
O2—Mo1—O3—Mo2 | −93.94 (15) | O13—Mo5—O10—Mo2 | 59.3 (3) |
O1—Mo1—O3—Mo2 | 159.47 (14) | O14—Mo5—O10—Mo2 | −28.4 (3) |
O4—Mo1—O3—Mo2 | 30.9 (3) | O6—P2—O13—Mo5 | 59.01 (15) |
O6—Mo1—O3—Mo2 | −1.20 (11) | O18—P2—O13—Mo5 | −65.79 (15) |
O5—Mo1—O3—Mo2 | 72.42 (13) | O22—P2—O13—Mo5 | 173.75 (12) |
O8—Mo2—O3—Mo1 | 84.49 (15) | O12—Mo5—O13—P2 | −176.95 (15) |
O7—Mo2—O3—Mo1 | −170.03 (14) | O10—Mo5—O13—P2 | −70.67 (14) |
O10—Mo2—O3—Mo1 | −41.5 (2) | O15—Mo5—O13—P2 | 81.49 (14) |
O9—Mo2—O3—Mo1 | −89.81 (13) | O14—Mo5—O13—P2 | 12.33 (13) |
O6—Mo2—O3—Mo1 | 1.14 (11) | O9—P1—O14—Mo3 | −177.82 (15) |
O21—Mo4—O4—Mo1 | −171.63 (15) | O5—P1—O14—Mo3 | −54.04 (19) |
O20—Mo4—O4—Mo1 | 80.50 (16) | O23—P1—O14—Mo3 | 62.15 (19) |
O19—Mo4—O4—Mo1 | −41.7 (2) | O9—P1—O14—Mo5 | −4.9 (2) |
O18—Mo4—O4—Mo1 | −86.93 (14) | O5—P1—O14—Mo5 | 118.84 (16) |
O5—Mo4—O4—Mo1 | −1.35 (12) | O23—P1—O14—Mo5 | −124.97 (17) |
O2—Mo1—O4—Mo4 | 171.82 (15) | O16—Mo3—O14—P1 | −84.22 (18) |
O1—Mo1—O4—Mo4 | −82.50 (16) | O17—Mo3—O14—P1 | 109.0 (3) |
O3—Mo1—O4—Mo4 | 45.5 (3) | O15—Mo3—O14—P1 | 175.86 (19) |
O6—Mo1—O4—Mo4 | 76.47 (14) | O19—Mo3—O14—P1 | 12.83 (16) |
O5—Mo1—O4—Mo4 | 1.37 (12) | O18—Mo3—O14—P1 | 85.18 (16) |
O9—P1—O5—Mo1 | 33.15 (18) | O16—Mo3—O14—Mo5 | 100.94 (11) |
O14—P1—O5—Mo1 | −90.59 (16) | O17—Mo3—O14—Mo5 | −65.9 (3) |
O23—P1—O5—Mo1 | 155.57 (14) | O15—Mo3—O14—Mo5 | 1.02 (8) |
O9—P1—O5—Mo4 | 152.20 (13) | O19—Mo3—O14—Mo5 | −162.01 (9) |
O14—P1—O5—Mo4 | 28.46 (18) | O18—Mo3—O14—Mo5 | −89.65 (8) |
O23—P1—O5—Mo4 | −85.39 (16) | O11—Mo5—O14—P1 | 82.61 (19) |
O2—Mo1—O5—P1 | 95.7 (4) | O12—Mo5—O14—P1 | −139.4 (4) |
O1—Mo1—O5—P1 | −125.24 (16) | O10—Mo5—O14—P1 | −19.05 (17) |
O3—Mo1—O5—P1 | −27.14 (15) | O15—Mo5—O14—P1 | −175.67 (19) |
O4—Mo1—O5—P1 | 132.71 (16) | O13—Mo5—O14—P1 | −98.92 (17) |
O6—Mo1—O5—P1 | 46.47 (14) | O11—Mo5—O14—Mo3 | −102.76 (11) |
O2—Mo1—O5—Mo4 | −37.9 (4) | O12—Mo5—O14—Mo3 | 35.2 (4) |
O1—Mo1—O5—Mo4 | 101.19 (10) | O10—Mo5—O14—Mo3 | 155.58 (9) |
O3—Mo1—O5—Mo4 | −160.71 (8) | O15—Mo5—O14—Mo3 | −1.04 (8) |
O4—Mo1—O5—Mo4 | −0.86 (8) | O13—Mo5—O14—Mo3 | 75.71 (8) |
O6—Mo1—O5—Mo4 | −87.10 (8) | O16—Mo3—O15—Mo5 | −97.48 (15) |
O21—Mo4—O5—P1 | −83.3 (5) | O17—Mo3—O15—Mo5 | 157.19 (15) |
O20—Mo4—O5—P1 | 121.14 (16) | O19—Mo3—O15—Mo5 | 33.6 (3) |
O4—Mo4—O5—P1 | −133.96 (16) | O14—Mo3—O15—Mo5 | −1.50 (12) |
O19—Mo4—O5—P1 | 22.71 (14) | O18—Mo3—O15—Mo5 | 71.25 (13) |
O18—Mo4—O5—P1 | −51.73 (14) | O11—Mo5—O15—Mo3 | 85.32 (15) |
O21—Mo4—O5—Mo1 | 51.5 (5) | O12—Mo5—O15—Mo3 | −170.07 (14) |
O20—Mo4—O5—Mo1 | −104.02 (10) | O10—Mo5—O15—Mo3 | −39.8 (2) |
O4—Mo4—O5—Mo1 | 0.88 (8) | O13—Mo5—O15—Mo3 | −90.00 (13) |
O19—Mo4—O5—Mo1 | 157.55 (9) | O14—Mo5—O15—Mo3 | 1.43 (11) |
O18—Mo4—O5—Mo1 | 83.11 (7) | O13—P2—O18—Mo4 | 156.50 (13) |
O13—P2—O6—Mo1 | −177.45 (14) | O6—P2—O18—Mo4 | 32.20 (18) |
O18—P2—O6—Mo1 | −53.17 (19) | O22—P2—O18—Mo4 | −81.19 (16) |
O22—P2—O6—Mo1 | 63.05 (18) | O13—P2—O18—Mo3 | 33.90 (17) |
O13—P2—O6—Mo2 | −5.0 (2) | O6—P2—O18—Mo3 | −90.40 (16) |
O18—P2—O6—Mo2 | 119.26 (16) | O22—P2—O18—Mo3 | 156.21 (13) |
O22—P2—O6—Mo2 | −124.52 (17) | O21—Mo4—O18—P2 | 119.29 (17) |
O2—Mo1—O6—P2 | −83.70 (17) | O20—Mo4—O18—P2 | −88.2 (5) |
O1—Mo1—O6—P2 | 108.1 (3) | O4—Mo4—O18—P2 | 18.64 (15) |
O3—Mo1—O6—P2 | 175.40 (18) | O19—Mo4—O18—P2 | −134.99 (16) |
O4—Mo1—O6—P2 | 10.76 (16) | O5—Mo4—O18—P2 | −54.23 (14) |
O5—Mo1—O6—P2 | 84.24 (16) | O21—Mo4—O18—Mo3 | −103.59 (10) |
O2—Mo1—O6—Mo2 | 101.73 (10) | O20—Mo4—O18—Mo3 | 48.9 (5) |
O1—Mo1—O6—Mo2 | −66.4 (3) | O4—Mo4—O18—Mo3 | 155.76 (9) |
O3—Mo1—O6—Mo2 | 0.83 (8) | O19—Mo4—O18—Mo3 | 2.13 (8) |
O4—Mo1—O6—Mo2 | −163.80 (9) | O5—Mo4—O18—Mo3 | 82.89 (7) |
O5—Mo1—O6—Mo2 | −90.32 (8) | O16—Mo3—O18—P2 | 98.3 (5) |
O8—Mo2—O6—P2 | 83.14 (19) | O17—Mo3—O18—P2 | −123.87 (16) |
O7—Mo2—O6—P2 | −131.3 (4) | O15—Mo3—O18—P2 | −26.53 (15) |
O10—Mo2—O6—P2 | −19.40 (17) | O19—Mo3—O18—P2 | 134.55 (16) |
O3—Mo2—O6—P2 | −175.07 (19) | O14—Mo3—O18—P2 | 47.02 (14) |
O9—Mo2—O6—P2 | −99.24 (17) | O16—Mo3—O18—Mo4 | −38.4 (5) |
O8—Mo2—O6—Mo1 | −102.63 (11) | O17—Mo3—O18—Mo4 | 99.43 (10) |
O7—Mo2—O6—Mo1 | 43.0 (5) | O15—Mo3—O18—Mo4 | −163.23 (8) |
O10—Mo2—O6—Mo1 | 154.83 (10) | O19—Mo3—O18—Mo4 | −2.15 (8) |
O3—Mo2—O6—Mo1 | −0.85 (8) | O14—Mo3—O18—Mo4 | −89.68 (8) |
O9—Mo2—O6—Mo1 | 74.99 (8) | O21—Mo4—O19—Mo3 | 78.66 (16) |
O14—P1—O9—Mo2 | 58.95 (16) | O20—Mo4—O19—Mo3 | −173.92 (15) |
O5—P1—O9—Mo2 | −65.43 (15) | O4—Mo4—O19—Mo3 | −50.2 (2) |
O23—P1—O9—Mo2 | 174.36 (12) | O18—Mo4—O19—Mo3 | −3.30 (12) |
O7—Mo2—O9—P1 | −174.95 (16) | O5—Mo4—O19—Mo3 | −89.03 (14) |
O10—Mo2—O9—P1 | −70.87 (14) | O16—Mo3—O19—Mo4 | 175.20 (15) |
O3—Mo2—O9—P1 | 81.94 (14) | O17—Mo3—O19—Mo4 | −79.64 (16) |
O6—Mo2—O9—P1 | 11.72 (13) | O15—Mo3—O19—Mo4 | 43.3 (3) |
O8—Mo2—O10—Mo5 | −113.8 (3) | O14—Mo3—O19—Mo4 | 77.06 (14) |
O7—Mo2—O10—Mo5 | 139.8 (3) | O18—Mo3—O19—Mo4 | 3.20 (12) |
O3—Mo2—O10—Mo5 | 11.7 (4) | N1—C1—C2—C3 | −179.4 (3) |
O9—Mo2—O10—Mo5 | 59.0 (3) | C1—C2—C3—C4 | −76.2 (4) |
O6—Mo2—O10—Mo5 | −28.2 (3) | C2—C3—C4—N2 | 172.4 (3) |
O11—Mo5—O10—Mo2 | −114.9 (3) | N3—C5—C6—C7 | −60.1 (5) |
O12—Mo5—O10—Mo2 | 138.9 (3) | C5—C6—C7—C8 | 173.2 (3) |
O15—Mo5—O10—Mo2 | 9.9 (4) | C6—C7—C8—N4 | 178.8 (3) |
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