Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806018976/hb2054sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806018976/hb2054Isup2.hkl |
CCDC reference: 610789
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- Disorder in solvent or counterion
- R factor = 0.025
- wR factor = 0.069
- Data-to-parameter ratio = 11.4
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact O14 .. C5A .. 3.00 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O15 .. C6 .. 2.95 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O22 .. C3B .. 2.99 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 7
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 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 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 2000); molecular graphics: SHELXTL/PC (Sheldrick, 1999); software used to prepare material for publication: SHELXTL/PC.
(C2H10N2)3[Mo5O15(PO4)2]·3H2O | Z = 2 |
Mr = 1150.05 | F(000) = 1124 |
Triclinic, P1 | Dx = 2.511 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.014 (4) Å | Cell parameters from 6589 reflections |
b = 10.699 (4) Å | θ = 2.3–27.1° |
c = 17.543 (7) Å | µ = 2.22 mm−1 |
α = 78.611 (7)° | T = 298 K |
β = 80.228 (6)° | Block, colorless |
γ = 67.198 (6)° | 0.50 × 0.40 × 0.20 mm |
V = 1520.8 (11) Å3 |
Bruker SMART 1K CCD area-detector diffractometer | 5211 independent reflections |
Radiation source: fine-focus sealed tube | 5075 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 25.1°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −10→10 |
Tmin = 0.403, Tmax = 0.665 | k = −12→12 |
6233 measured reflections | l = −11→20 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.026 | H-atom parameters constrained |
wR(F2) = 0.070 | w = 1/[σ2(Fo2) + (0.0123P)2 + 3.1377P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max = 0.003 |
5211 reflections | Δρmax = 0.64 e Å−3 |
459 parameters | Δρmin = −0.71 e Å−3 |
16 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0064 (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) | |
Mo1 | 0.43372 (4) | 0.01744 (3) | 0.352231 (19) | 0.02318 (10) | |
Mo2 | 0.26841 (4) | 0.32386 (3) | 0.419032 (18) | 0.02269 (10) | |
Mo3 | 0.14921 (4) | 0.57502 (3) | 0.267433 (19) | 0.02313 (10) | |
Mo4 | 0.19319 (4) | 0.43324 (3) | 0.104986 (19) | 0.02577 (10) | |
Mo5 | 0.31573 (4) | 0.08698 (3) | 0.153145 (19) | 0.02467 (10) | |
P1 | 0.05920 (11) | 0.28154 (9) | 0.28675 (5) | 0.01974 (19) | |
P2 | 0.48838 (11) | 0.28853 (9) | 0.23037 (5) | 0.0211 (2) | |
O1 | −0.1060 (3) | 0.3198 (3) | 0.33351 (16) | 0.0291 (6) | |
O2 | 0.1982 (3) | 0.2215 (2) | 0.34105 (15) | 0.0238 (5) | |
O3 | 0.0715 (3) | 0.4128 (2) | 0.23236 (14) | 0.0228 (5) | |
O4 | 0.0857 (3) | 0.1730 (2) | 0.23423 (15) | 0.0240 (5) | |
O5 | 0.6113 (3) | 0.3473 (3) | 0.18472 (17) | 0.0337 (6) | |
O6 | 0.5692 (3) | 0.1446 (3) | 0.27457 (16) | 0.0264 (6) | |
O7 | 0.3762 (3) | 0.3847 (2) | 0.29042 (15) | 0.0238 (5) | |
O8 | 0.3809 (3) | 0.2731 (2) | 0.17293 (15) | 0.0245 (5) | |
O9 | 0.3927 (3) | 0.0021 (3) | 0.25101 (16) | 0.0278 (6) | |
O10 | 0.4324 (3) | 0.1405 (3) | 0.42004 (15) | 0.0278 (6) | |
O11 | 0.1065 (3) | 0.4872 (3) | 0.36984 (15) | 0.0262 (6) | |
O12 | 0.2357 (3) | 0.5563 (3) | 0.16010 (15) | 0.0276 (6) | |
O13 | 0.1913 (3) | 0.2571 (3) | 0.09086 (15) | 0.0297 (6) | |
O14 | 0.3046 (3) | −0.0577 (3) | 0.40806 (17) | 0.0332 (6) | |
O15 | 0.6177 (3) | −0.1124 (3) | 0.36160 (17) | 0.0339 (6) | |
O16 | 0.1423 (3) | 0.2984 (3) | 0.50050 (17) | 0.0354 (7) | |
O17 | 0.3851 (3) | 0.3958 (3) | 0.45157 (17) | 0.0339 (6) | |
O18 | −0.0471 (3) | 0.6893 (3) | 0.25558 (17) | 0.0342 (6) | |
O19 | 0.2439 (3) | 0.6770 (3) | 0.28528 (19) | 0.0370 (7) | |
O20 | 0.0012 (4) | 0.5327 (3) | 0.08187 (17) | 0.0368 (7) | |
O21 | 0.3164 (4) | 0.4611 (3) | 0.02154 (17) | 0.0360 (7) | |
O22 | 0.2256 (4) | −0.0190 (3) | 0.13580 (18) | 0.0376 (7) | |
O23 | 0.4962 (4) | 0.0390 (3) | 0.09310 (18) | 0.0403 (7) | |
O24 | 0.6354 (4) | 0.7624 (3) | 0.06923 (18) | 0.0477 (8) | |
H11 | 0.6000 | 0.8456 | 0.0758 | 0.071* | |
H12 | 0.7012 | 0.7513 | 0.0279 | 0.071* | |
O25 | 0.1874 (4) | 0.6914 (4) | 0.4752 (2) | 0.0560 (9) | |
H13 | 0.2454 | 0.6352 | 0.4441 | 0.084* | |
H14 | 0.0885 | 0.6985 | 0.4779 | 0.084* | |
O26 | 0.8284 (6) | 0.9329 (5) | 0.1514 (4) | 0.1027 (19) | |
H15 | 0.8458 | 0.9208 | 0.1990 | 0.154* | |
H16 | 0.8880 | 0.8611 | 0.1315 | 0.154* | |
C1 | 0.6030 (5) | 0.6628 (4) | 0.2566 (2) | 0.0298 (8) | |
H1A | 0.4982 | 0.7049 | 0.2365 | 0.036* | |
H1B | 0.6473 | 0.7338 | 0.2517 | 0.036* | |
C2 | 0.5793 (5) | 0.6086 (4) | 0.3424 (2) | 0.0319 (9) | |
H2A | 0.4891 | 0.6773 | 0.3677 | 0.038* | |
H2B | 0.5521 | 0.5278 | 0.3474 | 0.038* | |
C3A | 0.7320 (14) | 0.1923 (14) | 0.0160 (6) | 0.061 (3) | 0.565 (7) |
H3A1 | 0.7518 | 0.0962 | 0.0170 | 0.073* | |
H3A2 | 0.6569 | 0.2212 | 0.0614 | 0.073* | |
C3B | 0.7855 (14) | 0.1668 (13) | −0.0100 (9) | 0.062 (4) | 0.435 (7) |
C4 | 0.8919 (6) | 0.2009 (5) | 0.0279 (3) | 0.0554 (14) | |
H4A | 0.9834 | 0.1277 | 0.0068 | 0.066* | |
H4B | 0.8986 | 0.2882 | 0.0029 | 0.066* | |
C5A | 0.8362 (12) | 0.0011 (10) | 0.4291 (5) | 0.033 (2) | 0.565 (7) |
H5A1 | 0.7617 | −0.0435 | 0.4546 | 0.039* | |
H5A2 | 0.9175 | −0.0200 | 0.4643 | 0.039* | |
C5B | 0.9007 (18) | 0.0274 (14) | 0.4219 (8) | 0.043 (3) | 0.435 (7) |
C6 | 0.9190 (6) | −0.0622 (5) | 0.3569 (3) | 0.0495 (12) | |
H6A | 0.9234 | −0.1560 | 0.3672 | 0.059* | |
H6B | 0.8481 | −0.0150 | 0.3159 | 0.059* | |
N1 | 0.7122 (4) | 0.5570 (3) | 0.2068 (2) | 0.0319 (7) | |
H1C | 0.8111 | 0.5222 | 0.2223 | 0.048* | |
H1D | 0.7164 | 0.5956 | 0.1571 | 0.048* | |
H1E | 0.6739 | 0.4903 | 0.2115 | 0.048* | |
N2 | 0.7265 (4) | 0.5725 (4) | 0.3831 (2) | 0.0346 (8) | |
H2C | 0.8023 | 0.4962 | 0.3683 | 0.052* | |
H2D | 0.7010 | 0.5594 | 0.4346 | 0.052* | |
H2E | 0.7637 | 0.6406 | 0.3706 | 0.052* | |
N3A | 0.6473 (8) | 0.2679 (8) | −0.0534 (5) | 0.050 (2) | 0.565 (7) |
H3A3 | 0.6537 | 0.3506 | −0.0647 | 0.076* | |
H3A4 | 0.5439 | 0.2765 | −0.0438 | 0.076* | |
H3A5 | 0.6932 | 0.2222 | −0.0938 | 0.076* | |
N4A | 0.8884 (7) | 0.1866 (6) | 0.1146 (4) | 0.0355 (18) | 0.565 (7) |
H4C | 0.8899 | 0.1035 | 0.1361 | 0.053* | |
H4D | 0.7987 | 0.2497 | 0.1333 | 0.053* | |
H4E | 0.9744 | 0.1979 | 0.1260 | 0.053* | |
N3B | 0.6335 (11) | 0.2828 (11) | 0.0048 (8) | 0.050 (3) | 0.435 (7) |
N4B | 0.8700 (10) | 0.2962 (10) | 0.0727 (5) | 0.042 (2) | 0.435 (7) |
N5 | 0.7454 (4) | 0.1507 (4) | 0.4198 (2) | 0.0370 (8) | |
H5A | 0.7980 | 0.1921 | 0.3825 | 0.056* | |
H5B | 0.7363 | 0.1812 | 0.4647 | 0.056* | |
H5C | 0.6473 | 0.1688 | 0.4066 | 0.056* | |
N6A | 1.0735 (6) | −0.0667 (5) | 0.3253 (3) | 0.0249 (14) | 0.565 (7) |
H6C | 1.0671 | 0.0145 | 0.2981 | 0.037* | |
H6D | 1.1166 | −0.1307 | 0.2940 | 0.037* | |
H6E | 1.1355 | −0.0866 | 0.3638 | 0.037* | |
N6B | 0.9059 (11) | 0.0067 (10) | 0.2795 (6) | 0.046 (3) | 0.435 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.02474 (18) | 0.01730 (16) | 0.02539 (18) | −0.00646 (13) | −0.00169 (13) | −0.00166 (13) |
Mo2 | 0.02594 (18) | 0.02121 (17) | 0.02050 (17) | −0.00789 (13) | −0.00127 (12) | −0.00461 (13) |
Mo3 | 0.02293 (17) | 0.01704 (16) | 0.02858 (19) | −0.00727 (13) | −0.00164 (13) | −0.00239 (13) |
Mo4 | 0.03152 (19) | 0.02402 (18) | 0.02117 (18) | −0.01213 (14) | −0.00117 (13) | 0.00080 (13) |
Mo5 | 0.03010 (18) | 0.02226 (17) | 0.02276 (18) | −0.01056 (14) | 0.00141 (13) | −0.00728 (13) |
P1 | 0.0206 (4) | 0.0176 (4) | 0.0208 (5) | −0.0077 (4) | −0.0001 (3) | −0.0022 (4) |
P2 | 0.0208 (4) | 0.0190 (4) | 0.0237 (5) | −0.0084 (4) | 0.0017 (4) | −0.0048 (4) |
O1 | 0.0252 (13) | 0.0259 (13) | 0.0351 (15) | −0.0107 (11) | 0.0051 (11) | −0.0059 (12) |
O2 | 0.0275 (13) | 0.0196 (12) | 0.0241 (13) | −0.0079 (10) | −0.0047 (10) | −0.0024 (10) |
O3 | 0.0261 (13) | 0.0206 (12) | 0.0229 (13) | −0.0111 (10) | −0.0029 (10) | −0.0003 (10) |
O4 | 0.0261 (13) | 0.0205 (12) | 0.0269 (13) | −0.0104 (10) | −0.0023 (10) | −0.0036 (10) |
O5 | 0.0323 (15) | 0.0295 (14) | 0.0413 (17) | −0.0165 (12) | 0.0082 (12) | −0.0090 (13) |
O6 | 0.0229 (13) | 0.0223 (13) | 0.0316 (14) | −0.0067 (10) | −0.0012 (11) | −0.0034 (11) |
O7 | 0.0246 (13) | 0.0218 (12) | 0.0242 (13) | −0.0075 (10) | 0.0001 (10) | −0.0060 (10) |
O8 | 0.0276 (13) | 0.0215 (12) | 0.0247 (13) | −0.0083 (10) | −0.0032 (11) | −0.0044 (10) |
O9 | 0.0292 (14) | 0.0231 (13) | 0.0300 (14) | −0.0070 (11) | −0.0015 (11) | −0.0078 (11) |
O10 | 0.0310 (14) | 0.0231 (13) | 0.0274 (14) | −0.0066 (11) | −0.0077 (11) | −0.0026 (11) |
O11 | 0.0277 (13) | 0.0219 (13) | 0.0250 (13) | −0.0051 (11) | −0.0008 (10) | −0.0043 (11) |
O12 | 0.0344 (14) | 0.0219 (13) | 0.0271 (14) | −0.0146 (11) | 0.0006 (11) | 0.0009 (11) |
O13 | 0.0377 (15) | 0.0314 (14) | 0.0236 (14) | −0.0161 (12) | −0.0044 (11) | −0.0040 (11) |
O14 | 0.0371 (16) | 0.0299 (14) | 0.0332 (15) | −0.0154 (12) | 0.0003 (12) | −0.0026 (12) |
O15 | 0.0326 (15) | 0.0228 (13) | 0.0421 (17) | −0.0052 (12) | −0.0080 (13) | −0.0019 (12) |
O16 | 0.0369 (16) | 0.0335 (15) | 0.0298 (15) | −0.0104 (13) | 0.0037 (12) | −0.0021 (12) |
O17 | 0.0396 (16) | 0.0366 (15) | 0.0306 (15) | −0.0165 (13) | −0.0065 (12) | −0.0085 (12) |
O18 | 0.0309 (15) | 0.0254 (14) | 0.0405 (17) | −0.0062 (12) | −0.0045 (12) | 0.0007 (12) |
O19 | 0.0339 (15) | 0.0283 (15) | 0.0537 (19) | −0.0151 (12) | −0.0015 (13) | −0.0115 (14) |
O20 | 0.0370 (16) | 0.0381 (16) | 0.0320 (16) | −0.0109 (13) | −0.0058 (13) | −0.0016 (13) |
O21 | 0.0427 (17) | 0.0322 (15) | 0.0309 (15) | −0.0168 (13) | 0.0040 (13) | 0.0002 (12) |
O22 | 0.0484 (18) | 0.0351 (16) | 0.0378 (17) | −0.0218 (14) | −0.0023 (14) | −0.0128 (13) |
O23 | 0.0431 (17) | 0.0426 (17) | 0.0364 (17) | −0.0179 (14) | 0.0127 (13) | −0.0178 (14) |
O24 | 0.064 (2) | 0.0345 (17) | 0.0323 (17) | −0.0092 (15) | 0.0065 (15) | −0.0063 (14) |
O25 | 0.049 (2) | 0.060 (2) | 0.068 (2) | −0.0258 (17) | 0.0066 (17) | −0.0278 (19) |
O26 | 0.087 (3) | 0.085 (3) | 0.131 (5) | −0.042 (3) | −0.049 (3) | 0.052 (3) |
C1 | 0.029 (2) | 0.0227 (18) | 0.036 (2) | −0.0080 (16) | −0.0026 (16) | −0.0034 (16) |
C2 | 0.0258 (19) | 0.029 (2) | 0.039 (2) | −0.0094 (16) | 0.0024 (17) | −0.0067 (18) |
C3A | 0.082 (5) | 0.066 (5) | 0.046 (5) | −0.030 (4) | −0.019 (4) | −0.018 (4) |
C3B | 0.068 (6) | 0.056 (6) | 0.056 (6) | −0.010 (4) | −0.006 (4) | −0.017 (4) |
C4 | 0.065 (3) | 0.035 (3) | 0.052 (3) | −0.012 (2) | 0.010 (3) | 0.000 (2) |
C5A | 0.038 (5) | 0.035 (5) | 0.027 (4) | −0.017 (4) | −0.003 (4) | −0.002 (3) |
C5B | 0.050 (9) | 0.039 (7) | 0.030 (6) | −0.010 (6) | −0.007 (6) | 0.007 (5) |
C6 | 0.056 (3) | 0.040 (3) | 0.044 (3) | −0.012 (2) | 0.002 (2) | −0.007 (2) |
N1 | 0.0350 (18) | 0.0275 (17) | 0.0332 (19) | −0.0115 (14) | −0.0049 (15) | −0.0036 (14) |
N2 | 0.0381 (19) | 0.0344 (18) | 0.0317 (19) | −0.0130 (16) | −0.0018 (15) | −0.0081 (15) |
N3A | 0.029 (4) | 0.043 (4) | 0.068 (6) | −0.018 (3) | −0.008 (4) | 0.028 (4) |
N4A | 0.020 (3) | 0.029 (3) | 0.055 (4) | −0.001 (2) | −0.007 (3) | −0.016 (3) |
N3B | 0.042 (6) | 0.057 (7) | 0.064 (8) | −0.036 (5) | 0.019 (5) | −0.021 (6) |
N4B | 0.040 (5) | 0.053 (6) | 0.031 (5) | −0.013 (4) | −0.002 (4) | −0.013 (4) |
N5 | 0.0319 (18) | 0.0357 (19) | 0.045 (2) | −0.0167 (15) | 0.0034 (16) | −0.0063 (17) |
N6A | 0.027 (3) | 0.016 (3) | 0.033 (3) | −0.009 (2) | −0.004 (2) | −0.003 (2) |
N6B | 0.036 (5) | 0.061 (6) | 0.046 (5) | −0.026 (4) | 0.007 (4) | −0.011 (5) |
Mo1—O15 | 1.710 (3) | C1—N1 | 1.500 (5) |
Mo1—O14 | 1.728 (3) | C1—C2 | 1.514 (6) |
Mo1—O9 | 1.924 (3) | C1—H1A | 0.9700 |
Mo1—O10 | 1.936 (3) | C1—H1B | 0.9700 |
Mo1—O6 | 2.278 (3) | C2—N2 | 1.495 (5) |
Mo1—O2 | 2.385 (3) | C2—H2A | 0.9700 |
Mo2—O16 | 1.716 (3) | C2—H2B | 0.9700 |
Mo2—O17 | 1.740 (3) | C3A—N3A | 1.473 (8) |
Mo2—O10 | 1.945 (3) | C3A—C4 | 1.530 (8) |
Mo2—O11 | 1.945 (3) | C3A—H3A1 | 0.9700 |
Mo2—O2 | 2.212 (2) | C3A—H3A2 | 0.9700 |
Mo2—O7 | 2.372 (3) | C3B—C4 | 1.442 (9) |
Mo3—O19 | 1.722 (3) | C3B—N3B | 1.474 (9) |
Mo3—O18 | 1.737 (3) | C4—N4B | 1.343 (10) |
Mo3—O11 | 1.907 (3) | C4—N4A | 1.494 (8) |
Mo3—O12 | 1.930 (3) | C4—H4A | 0.9700 |
Mo3—O7 | 2.285 (3) | C4—H4B | 0.9700 |
Mo3—O3 | 2.323 (2) | C5A—N5 | 1.478 (10) |
Mo4—O20 | 1.712 (3) | C5A—C6 | 1.499 (10) |
Mo4—O21 | 1.732 (3) | C5A—H5A1 | 0.9700 |
Mo4—O13 | 1.956 (3) | C5A—H5A2 | 0.9700 |
Mo4—O12 | 1.958 (3) | C5B—C6 | 1.580 (15) |
Mo4—O8 | 2.203 (3) | C6—N6A | 1.395 (7) |
Mo4—O3 | 2.325 (3) | C6—N6B | 1.411 (11) |
Mo5—O22 | 1.724 (3) | C6—H6A | 0.9700 |
Mo5—O23 | 1.733 (3) | C6—H6B | 0.9700 |
Mo5—O9 | 1.885 (3) | N1—H1C | 0.8900 |
Mo5—O13 | 1.953 (3) | N1—H1D | 0.8900 |
Mo5—O4 | 2.282 (3) | N1—H1E | 0.8900 |
Mo5—O8 | 2.383 (3) | N2—H2C | 0.8900 |
P1—O1 | 1.517 (3) | N2—H2D | 0.8900 |
P1—O4 | 1.545 (3) | N2—H2E | 0.8900 |
P1—O2 | 1.559 (3) | N3A—H3A3 | 0.8900 |
P1—O3 | 1.565 (3) | N3A—H3A4 | 0.8900 |
P2—O5 | 1.518 (3) | N3A—H3A5 | 0.8900 |
P2—O6 | 1.535 (3) | N4A—H4C | 0.8900 |
P2—O7 | 1.566 (3) | N4A—H4D | 0.8900 |
P2—O8 | 1.582 (3) | N4A—H4E | 0.8900 |
O24—H11 | 0.8453 | N5—H5A | 0.8900 |
O24—H12 | 0.8512 | N5—H5B | 0.8900 |
O25—H13 | 0.8493 | N5—H5C | 0.8900 |
O25—H14 | 0.8588 | N6A—H6C | 0.8900 |
O26—H15 | 0.8508 | N6A—H6D | 0.8900 |
O26—H16 | 0.8495 | N6A—H6E | 0.8900 |
O15—Mo1—O14 | 101.59 (14) | P1—O3—Mo3 | 125.77 (14) |
O15—Mo1—O9 | 100.72 (12) | P1—O3—Mo4 | 128.93 (14) |
O14—Mo1—O9 | 97.75 (13) | Mo3—O3—Mo4 | 93.38 (9) |
O15—Mo1—O10 | 103.08 (12) | P1—O4—Mo5 | 123.93 (14) |
O14—Mo1—O10 | 101.04 (13) | P2—O6—Mo1 | 124.73 (14) |
O9—Mo1—O10 | 145.83 (11) | P2—O7—Mo3 | 127.36 (14) |
O15—Mo1—O6 | 87.09 (12) | P2—O7—Mo2 | 128.64 (14) |
O14—Mo1—O6 | 171.31 (11) | Mo3—O7—Mo2 | 92.72 (9) |
O9—Mo1—O6 | 80.05 (11) | P2—O8—Mo4 | 129.27 (14) |
O10—Mo1—O6 | 77.07 (11) | P2—O8—Mo5 | 133.57 (14) |
O15—Mo1—O2 | 171.02 (11) | Mo4—O8—Mo5 | 95.66 (10) |
O14—Mo1—O2 | 85.29 (11) | Mo5—O9—Mo1 | 149.49 (15) |
O9—Mo1—O2 | 83.86 (10) | Mo1—O10—Mo2 | 121.62 (13) |
O10—Mo1—O2 | 69.65 (10) | Mo3—O11—Mo2 | 122.05 (13) |
O6—Mo1—O2 | 86.11 (9) | Mo3—O12—Mo4 | 120.89 (13) |
O16—Mo2—O17 | 103.72 (14) | Mo5—O13—Mo4 | 120.96 (13) |
O16—Mo2—O10 | 100.57 (13) | H11—O24—H12 | 109.4 |
O17—Mo2—O10 | 96.38 (13) | H13—O25—H14 | 109.3 |
O16—Mo2—O11 | 95.39 (13) | H15—O26—H16 | 108.7 |
O17—Mo2—O11 | 100.83 (13) | N1—C1—C2 | 114.7 (3) |
O10—Mo2—O11 | 153.00 (11) | N1—C1—H1A | 108.6 |
O16—Mo2—O2 | 97.77 (12) | C2—C1—H1A | 108.6 |
O17—Mo2—O2 | 157.66 (12) | N1—C1—H1B | 108.6 |
O10—Mo2—O2 | 73.46 (10) | C2—C1—H1B | 108.6 |
O11—Mo2—O2 | 82.96 (10) | H1A—C1—H1B | 107.6 |
O16—Mo2—O7 | 164.41 (12) | N2—C2—C1 | 112.4 (3) |
O17—Mo2—O7 | 87.06 (12) | N2—C2—H2A | 109.1 |
O10—Mo2—O7 | 89.18 (10) | C1—C2—H2A | 109.1 |
O11—Mo2—O7 | 71.23 (10) | N2—C2—H2B | 109.1 |
O2—Mo2—O7 | 73.21 (9) | C1—C2—H2B | 109.1 |
O19—Mo3—O18 | 103.13 (14) | H2A—C2—H2B | 107.8 |
O19—Mo3—O11 | 102.25 (14) | N3A—C3A—C4 | 121.3 (8) |
O18—Mo3—O11 | 97.50 (12) | N3A—C3A—H3A1 | 107.0 |
O19—Mo3—O12 | 99.16 (13) | C4—C3A—H3A1 | 107.0 |
O18—Mo3—O12 | 100.92 (13) | N3A—C3A—H3A2 | 107.0 |
O11—Mo3—O12 | 147.65 (11) | C4—C3A—H3A2 | 107.0 |
O19—Mo3—O7 | 90.42 (12) | H3A1—C3A—H3A2 | 106.8 |
O18—Mo3—O7 | 165.36 (12) | C4—C3B—N3B | 99.5 (8) |
O11—Mo3—O7 | 73.89 (10) | N4B—C4—C3B | 134.3 (7) |
O12—Mo3—O7 | 82.03 (10) | N4B—C4—N4A | 50.7 (5) |
O19—Mo3—O3 | 168.72 (11) | C3B—C4—N4A | 123.7 (8) |
O18—Mo3—O3 | 86.62 (12) | N4B—C4—C3A | 112.2 (7) |
O11—Mo3—O3 | 81.76 (10) | N4A—C4—C3A | 104.2 (6) |
O12—Mo3—O3 | 73.10 (10) | N4B—C4—H4A | 136.3 |
O7—Mo3—O3 | 80.50 (9) | C3B—C4—H4A | 89.5 |
O20—Mo4—O21 | 104.29 (14) | N4A—C4—H4A | 110.9 |
O20—Mo4—O13 | 97.63 (13) | C3A—C4—H4A | 110.9 |
O21—Mo4—O13 | 99.24 (13) | N4B—C4—H4B | 61.3 |
O20—Mo4—O12 | 100.19 (13) | C3B—C4—H4B | 110.4 |
O21—Mo4—O12 | 93.77 (13) | N4A—C4—H4B | 110.9 |
O13—Mo4—O12 | 154.59 (11) | C3A—C4—H4B | 110.9 |
O20—Mo4—O8 | 156.82 (12) | H4A—C4—H4B | 108.9 |
O21—Mo4—O8 | 98.25 (12) | N5—C5A—C6 | 117.8 (7) |
O13—Mo4—O8 | 73.19 (10) | N5—C5A—H5A1 | 107.9 |
O12—Mo4—O8 | 83.44 (10) | C6—C5A—H5A1 | 107.9 |
O20—Mo4—O3 | 84.81 (12) | N5—C5A—H5A2 | 107.9 |
O21—Mo4—O3 | 164.94 (12) | C6—C5A—H5A2 | 107.9 |
O13—Mo4—O3 | 91.27 (10) | H5A1—C5A—H5A2 | 107.2 |
O12—Mo4—O3 | 72.57 (10) | N6A—C6—N6B | 73.1 (5) |
O8—Mo4—O3 | 74.38 (9) | N6A—C6—C5A | 122.1 (6) |
O22—Mo5—O23 | 102.46 (14) | N6B—C6—C5A | 125.5 (6) |
O22—Mo5—O9 | 102.05 (13) | N6A—C6—C5B | 95.6 (7) |
O23—Mo5—O9 | 99.86 (14) | N6B—C6—C5B | 116.4 (7) |
O22—Mo5—O13 | 99.50 (13) | N6A—C6—H6A | 106.8 |
O23—Mo5—O13 | 100.32 (14) | N6B—C6—H6A | 118.3 |
O9—Mo5—O13 | 146.37 (11) | C5A—C6—H6A | 106.8 |
O22—Mo5—O4 | 84.66 (12) | C5B—C6—H6A | 124.7 |
O23—Mo5—O4 | 172.75 (12) | N6A—C6—H6B | 106.8 |
O9—Mo5—O4 | 79.76 (10) | C5A—C6—H6B | 106.8 |
O13—Mo5—O4 | 76.88 (11) | C5B—C6—H6B | 114.1 |
O22—Mo5—O8 | 166.87 (12) | H6A—C6—H6B | 106.7 |
O23—Mo5—O8 | 86.54 (12) | C1—N1—H1C | 109.5 |
O9—Mo5—O8 | 85.54 (10) | C1—N1—H1D | 109.5 |
O13—Mo5—O8 | 69.18 (10) | H1C—N1—H1D | 109.5 |
O4—Mo5—O8 | 86.21 (9) | C1—N1—H1E | 109.5 |
O1—P1—O4 | 111.93 (15) | H1C—N1—H1E | 109.5 |
O1—P1—O2 | 111.61 (15) | H1D—N1—H1E | 109.5 |
O4—P1—O2 | 107.26 (14) | C2—N2—H2C | 109.5 |
O1—P1—O3 | 108.60 (15) | C2—N2—H2D | 109.5 |
O4—P1—O3 | 107.75 (14) | H2C—N2—H2D | 109.5 |
O2—P1—O3 | 109.59 (14) | C2—N2—H2E | 109.5 |
O5—P2—O6 | 112.17 (16) | H2C—N2—H2E | 109.5 |
O5—P2—O7 | 110.13 (15) | H2D—N2—H2E | 109.5 |
O6—P2—O7 | 108.86 (15) | C4—N4A—H4C | 109.5 |
O5—P2—O8 | 110.32 (16) | C4—N4A—H4D | 109.5 |
O6—P2—O8 | 106.07 (14) | C4—N4A—H4E | 109.5 |
O7—P2—O8 | 109.16 (14) | C6—N6A—H6C | 109.5 |
P1—O2—Mo2 | 129.46 (14) | C6—N6A—H6D | 109.5 |
P1—O2—Mo1 | 134.59 (14) | C6—N6A—H6E | 109.5 |
Mo2—O2—Mo1 | 94.87 (9) | ||
O1—P1—O2—Mo2 | −67.7 (2) | O11—Mo2—O7—Mo3 | 2.21 (9) |
O4—P1—O2—Mo2 | 169.35 (17) | O2—Mo2—O7—Mo3 | 90.34 (10) |
O3—P1—O2—Mo2 | 52.6 (2) | O5—P2—O8—Mo4 | −70.7 (2) |
O1—P1—O2—Mo1 | 127.3 (2) | O6—P2—O8—Mo4 | 167.59 (17) |
O4—P1—O2—Mo1 | 4.4 (2) | O7—P2—O8—Mo4 | 50.4 (2) |
O3—P1—O2—Mo1 | −112.3 (2) | O5—P2—O8—Mo5 | 126.76 (19) |
O16—Mo2—O2—P1 | 87.8 (2) | O6—P2—O8—Mo5 | 5.1 (2) |
O17—Mo2—O2—P1 | −108.2 (3) | O7—P2—O8—Mo5 | −112.09 (19) |
O10—Mo2—O2—P1 | −173.5 (2) | O20—Mo4—O8—P2 | −104.6 (3) |
O11—Mo2—O2—P1 | −6.76 (19) | O21—Mo4—O8—P2 | 88.8 (2) |
O7—Mo2—O2—P1 | −79.21 (19) | O13—Mo4—O8—P2 | −174.0 (2) |
O16—Mo2—O2—Mo1 | −102.92 (12) | O12—Mo4—O8—P2 | −4.04 (19) |
O17—Mo2—O2—Mo1 | 61.2 (3) | O3—Mo4—O8—P2 | −77.73 (19) |
O10—Mo2—O2—Mo1 | −4.14 (10) | O20—Mo4—O8—Mo5 | 62.7 (3) |
O11—Mo2—O2—Mo1 | 162.57 (11) | O21—Mo4—O8—Mo5 | −103.80 (12) |
O7—Mo2—O2—Mo1 | 90.11 (10) | O13—Mo4—O8—Mo5 | −6.58 (10) |
O14—Mo1—O2—P1 | −83.7 (2) | O12—Mo4—O8—Mo5 | 163.33 (11) |
O9—Mo1—O2—P1 | 14.6 (2) | O3—Mo4—O8—Mo5 | 89.64 (10) |
O10—Mo1—O2—P1 | 172.7 (2) | O22—Mo5—O8—P2 | 141.8 (5) |
O6—Mo1—O2—P1 | 95.0 (2) | O23—Mo5—O8—P2 | −84.3 (2) |
O14—Mo1—O2—Mo2 | 107.88 (12) | O9—Mo5—O8—P2 | 15.8 (2) |
O9—Mo1—O2—Mo2 | −153.79 (11) | O13—Mo5—O8—P2 | 173.2 (2) |
O10—Mo1—O2—Mo2 | 4.25 (10) | O4—Mo5—O8—P2 | 95.8 (2) |
O6—Mo1—O2—Mo2 | −73.39 (10) | O22—Mo5—O8—Mo4 | −24.7 (6) |
O1—P1—O3—Mo3 | 85.50 (19) | O23—Mo5—O8—Mo4 | 109.16 (14) |
O4—P1—O3—Mo3 | −153.07 (15) | O9—Mo5—O8—Mo4 | −150.65 (11) |
O2—P1—O3—Mo3 | −36.7 (2) | O13—Mo5—O8—Mo4 | 6.75 (10) |
O1—P1—O3—Mo4 | −142.00 (17) | O4—Mo5—O8—Mo4 | −70.65 (10) |
O4—P1—O3—Mo4 | −20.6 (2) | O22—Mo5—O9—Mo1 | −143.0 (3) |
O2—P1—O3—Mo4 | 95.84 (18) | O23—Mo5—O9—Mo1 | 111.9 (3) |
O19—Mo3—O3—P1 | 95.8 (6) | O13—Mo5—O9—Mo1 | −14.3 (4) |
O18—Mo3—O3—P1 | −114.03 (19) | O4—Mo5—O9—Mo1 | −60.8 (3) |
O11—Mo3—O3—P1 | −15.94 (17) | O8—Mo5—O9—Mo1 | 26.2 (3) |
O12—Mo3—O3—P1 | 143.47 (19) | O15—Mo1—O9—Mo5 | −139.5 (3) |
O7—Mo3—O3—P1 | 58.98 (17) | O14—Mo1—O9—Mo5 | 117.1 (3) |
O19—Mo3—O3—Mo4 | −49.2 (6) | O10—Mo1—O9—Mo5 | −5.9 (4) |
O18—Mo3—O3—Mo4 | 101.03 (12) | O6—Mo1—O9—Mo5 | −54.4 (3) |
O11—Mo3—O3—Mo4 | −160.88 (10) | O2—Mo1—O9—Mo5 | 32.7 (3) |
O12—Mo3—O3—Mo4 | −1.46 (9) | O15—Mo1—O10—Mo2 | 168.83 (16) |
O7—Mo3—O3—Mo4 | −85.95 (9) | O14—Mo1—O10—Mo2 | −86.37 (18) |
O20—Mo4—O3—P1 | 115.9 (2) | O9—Mo1—O10—Mo2 | 35.8 (3) |
O21—Mo4—O3—P1 | −116.1 (4) | O6—Mo1—O10—Mo2 | 84.96 (16) |
O13—Mo4—O3—P1 | 18.31 (19) | O2—Mo1—O10—Mo2 | −5.66 (13) |
O12—Mo4—O3—P1 | −141.7 (2) | O16—Mo2—O10—Mo1 | 101.02 (18) |
O8—Mo4—O3—P1 | −53.84 (17) | O17—Mo2—O10—Mo1 | −153.69 (17) |
O20—Mo4—O3—Mo3 | −100.95 (12) | O11—Mo2—O10—Mo1 | −24.2 (3) |
O21—Mo4—O3—Mo3 | 27.1 (5) | O2—Mo2—O10—Mo1 | 5.97 (14) |
O13—Mo4—O3—Mo3 | 161.50 (10) | O7—Mo2—O10—Mo1 | −66.74 (16) |
O12—Mo4—O3—Mo3 | 1.45 (9) | O19—Mo3—O11—Mo2 | −83.67 (17) |
O8—Mo4—O3—Mo3 | 89.35 (10) | O18—Mo3—O11—Mo2 | 171.08 (16) |
O1—P1—O4—Mo5 | 179.44 (15) | O12—Mo3—O11—Mo2 | 46.7 (3) |
O2—P1—O4—Mo5 | −57.8 (2) | O7—Mo3—O11—Mo2 | 3.19 (13) |
O3—P1—O4—Mo5 | 60.10 (19) | O3—Mo3—O11—Mo2 | 85.62 (15) |
O22—Mo5—O4—P1 | 175.24 (19) | O16—Mo2—O11—Mo3 | −174.91 (16) |
O9—Mo5—O4—P1 | 71.94 (18) | O17—Mo2—O11—Mo3 | 79.98 (17) |
O13—Mo5—O4—P1 | −83.69 (18) | O10—Mo2—O11—Mo3 | −48.7 (3) |
O8—Mo5—O4—P1 | −14.20 (17) | O2—Mo2—O11—Mo3 | −77.72 (16) |
O5—P2—O6—Mo1 | 179.03 (16) | O7—Mo2—O11—Mo3 | −3.12 (13) |
O7—P2—O6—Mo1 | 56.9 (2) | O19—Mo3—O12—Mo4 | 173.59 (16) |
O8—P2—O6—Mo1 | −60.5 (2) | O18—Mo3—O12—Mo4 | −81.01 (17) |
O15—Mo1—O6—P2 | 174.8 (2) | O11—Mo3—O12—Mo4 | 42.6 (3) |
O9—Mo1—O6—P2 | 73.41 (18) | O7—Mo3—O12—Mo4 | 84.45 (15) |
O10—Mo1—O6—P2 | −81.03 (18) | O3—Mo3—O12—Mo4 | 2.02 (13) |
O2—Mo1—O6—P2 | −11.03 (17) | O20—Mo4—O12—Mo3 | 79.19 (17) |
O5—P2—O7—Mo3 | 84.1 (2) | O21—Mo4—O12—Mo3 | −175.56 (16) |
O6—P2—O7—Mo3 | −152.54 (16) | O13—Mo4—O12—Mo3 | −54.7 (3) |
O8—P2—O7—Mo3 | −37.2 (2) | O8—Mo4—O12—Mo3 | −77.67 (15) |
O5—P2—O7—Mo2 | −142.54 (18) | O3—Mo4—O12—Mo3 | −2.02 (13) |
O6—P2—O7—Mo2 | −19.2 (2) | O22—Mo5—O13—Mo4 | 164.26 (17) |
O8—P2—O7—Mo2 | 96.20 (19) | O23—Mo5—O13—Mo4 | −91.09 (18) |
O19—Mo3—O7—P2 | −114.2 (2) | O9—Mo5—O13—Mo4 | 34.9 (3) |
O18—Mo3—O7—P2 | 87.7 (5) | O4—Mo5—O13—Mo4 | 82.08 (16) |
O11—Mo3—O7—P2 | 143.1 (2) | O8—Mo5—O13—Mo4 | −8.84 (13) |
O12—Mo3—O7—P2 | −15.05 (18) | O20—Mo4—O13—Mo5 | −148.85 (17) |
O3—Mo3—O7—P2 | 59.04 (17) | O21—Mo4—O13—Mo5 | 105.24 (18) |
O19—Mo3—O7—Mo2 | 100.41 (12) | O12—Mo4—O13—Mo5 | −14.6 (4) |
O18—Mo3—O7—Mo2 | −57.6 (5) | O8—Mo4—O13—Mo5 | 9.34 (14) |
O11—Mo3—O7—Mo2 | −2.22 (9) | O3—Mo4—O13—Mo5 | −63.92 (16) |
O12—Mo3—O7—Mo2 | −160.40 (11) | N1—C1—C2—N2 | 72.2 (4) |
O3—Mo3—O7—Mo2 | −86.31 (9) | N3B—C3B—C4—N4B | 7.4 (18) |
O16—Mo2—O7—P2 | −110.5 (4) | N3B—C3B—C4—N4A | 73.1 (12) |
O17—Mo2—O7—P2 | 115.07 (19) | N3B—C3B—C4—C3A | 33.9 (14) |
O10—Mo2—O7—P2 | 18.64 (18) | N3A—C3A—C4—N4B | 95.1 (13) |
O11—Mo2—O7—P2 | −142.4 (2) | N3A—C3A—C4—C3B | −64.8 (18) |
O2—Mo2—O7—P2 | −54.31 (17) | N3A—C3A—C4—N4A | 148.0 (11) |
O16—Mo2—O7—Mo3 | 34.1 (4) | N5—C5A—C6—N6A | 85.2 (9) |
O17—Mo2—O7—Mo3 | −100.28 (12) | N5—C5A—C6—N6B | −6.2 (12) |
O10—Mo2—O7—Mo3 | 163.30 (10) | N5—C5A—C6—C5B | 72.5 (15) |
D—H···A | D—H | H···A | D···A | D—H···A |
N6A—H6E···O14i | 0.89 | 1.97 | 2.773 (6) | 149 |
N6A—H6D···O19ii | 0.89 | 1.95 | 2.739 (6) | 147 |
N6A—H6C···O4i | 0.89 | 1.89 | 2.772 (6) | 172 |
N5—H5C···O10 | 0.89 | 2.04 | 2.865 (5) | 153 |
N5—H5B···O14iii | 0.89 | 2.41 | 3.002 (5) | 124 |
N5—H5B···O25iv | 0.89 | 2.23 | 3.003 (5) | 145 |
N5—H5A···O1i | 0.89 | 1.89 | 2.733 (4) | 159 |
N4A—H4E···O22i | 0.89 | 2.54 | 3.016 (6) | 114 |
N4A—H4E···O13i | 0.89 | 2.24 | 3.047 (7) | 151 |
N4A—H4E···O4i | 0.89 | 2.22 | 2.922 (6) | 136 |
N4A—H4D···O5 | 0.89 | 1.80 | 2.678 (6) | 168 |
N4A—H4C···O26v | 0.89 | 2.06 | 2.898 (8) | 156 |
N3A—H3A5···O22vi | 0.89 | 2.24 | 3.014 (10) | 145 |
N3A—H3A4···O24vii | 0.89 | 1.96 | 2.756 (8) | 149 |
N3A—H3A3···O21vii | 0.89 | 2.41 | 3.204 (9) | 149 |
N3A—H3A4···O21 | 0.89 | 2.52 | 3.140 (9) | 127 |
N3A—H3A3···O12vii | 0.89 | 2.08 | 2.762 (7) | 133 |
N2—H2E···O18i | 0.89 | 2.52 | 3.171 (5) | 130 |
N2—H2E···O15viii | 0.89 | 2.44 | 3.087 (5) | 130 |
N2—H2D···O17iv | 0.89 | 2.09 | 2.945 (5) | 160 |
N2—H2C···O1i | 0.89 | 1.92 | 2.769 (4) | 159 |
N1—H1E···O5 | 0.89 | 1.98 | 2.838 (4) | 161 |
N1—H1D···O20i | 0.89 | 2.58 | 3.069 (5) | 116 |
N1—H1D···O24 | 0.89 | 2.09 | 2.904 (5) | 151 |
N1—H1C···O1i | 0.89 | 2.57 | 3.138 (4) | 122 |
N1—H1C···O3i | 0.89 | 2.20 | 3.068 (4) | 165 |
O24—H12···O13vii | 0.85 | 2.15 | 2.977 (4) | 165 |
O24—H11···O23viii | 0.85 | 1.98 | 2.818 (4) | 175 |
O25—H14···O16ix | 0.86 | 2.04 | 2.891 (5) | 172 |
O25—H13···O17 | 0.85 | 2.36 | 3.042 (5) | 137 |
O26—H15···O18i | 0.85 | 2.36 | 2.818 (7) | 114 |
Symmetry codes: (i) x+1, y, z; (ii) x+1, y−1, z; (iii) −x+1, −y, −z+1; (iv) −x+1, −y+1, −z+1; (v) x, y−1, z; (vi) −x+1, −y, −z; (vii) −x+1, −y+1, −z; (viii) x, y+1, z; (ix) −x, −y+1, −z+1. |
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