Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680605272X/hy2033sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680605272X/hy2033Isup2.hkl |
CCDC reference: 618419
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.013 Å
- R factor = 0.057
- wR factor = 0.151
- Data-to-parameter ratio = 13.3
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O6 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O7 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mo1 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C40 - C41 ... 1.54 Ang.
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.10 From the CIF: _reflns_number_total 6593 Count of symmetry unique reflns 3534 Completeness (_total/calc) 186.56% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3059 Fraction of Friedel pairs measured 0.866 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1999); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
(C39H36P2)[Mo(C2O4)O(O2)2]·H2O | F(000) = 872.0 |
Mr = 848.59 | Dx = 1.475 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 6593 reflections |
a = 10.9385 (8) Å | θ = 1.8–25.1° |
b = 15.6425 (12) Å | µ = 0.49 mm−1 |
c = 11.8100 (9) Å | T = 296 K |
β = 109.040 (1)° | Plate, yellow |
V = 1910.2 (2) Å3 | 0.34 × 0.28 × 0.15 mm |
Z = 2 |
Bruker SMART APEXII CCD diffractometer | 6593 independent reflections |
Radiation source: fine-focus sealed tube | 5391 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 25.1°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | h = −12→13 |
Tmin = 0.852, Tmax = 0.930 | k = −17→18 |
9549 measured reflections | l = −14→8 |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.057 | w = 1/[σ2(Fo2) + (0.0606P)2 + 3.2002P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.151 | (Δ/σ)max = 0.001 |
S = 1.05 | Δρmax = 0.53 e Å−3 |
6593 reflections | Δρmin = −0.76 e Å−3 |
494 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
3 restraints | Extinction coefficient: 0.0132 (12) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 1458 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.02 (5) |
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 | 0.74619 (6) | 1.04409 (4) | 0.39693 (6) | 0.0512 (2) | |
P1 | 0.85369 (18) | 0.27691 (12) | 0.76147 (16) | 0.0443 (4) | |
P2 | 0.72354 (17) | 0.39688 (12) | 0.29927 (16) | 0.0446 (4) | |
O1 | 0.6088 (5) | 0.9357 (4) | 0.3607 (5) | 0.0568 (14) | |
O2 | 0.5347 (6) | 0.8341 (4) | 0.4553 (6) | 0.0798 (19) | |
O3 | 0.6385 (6) | 0.9300 (5) | 0.6625 (6) | 0.0842 (19) | |
O4 | 0.7246 (5) | 1.0160 (3) | 0.5583 (5) | 0.0614 (15) | |
O5 | 0.8669 (6) | 0.9494 (4) | 0.4208 (7) | 0.077 (2) | |
O6 | 0.8289 (7) | 0.9866 (5) | 0.3013 (7) | 0.090 (2) | |
O7 | 0.6356 (7) | 1.0981 (4) | 0.2580 (6) | 0.086 (2) | |
O8 | 0.5851 (6) | 1.1081 (4) | 0.3567 (6) | 0.0742 (17) | |
O9 | 0.8485 (6) | 1.1221 (4) | 0.4591 (6) | 0.0691 (17) | |
O10 | 0.3728 (8) | 0.2304 (5) | 0.3049 (8) | 0.092 (2) | |
C1 | 1.0914 (8) | 0.2784 (6) | 0.7270 (8) | 0.056 (2) | |
H1 | 1.0563 | 0.3205 | 0.6701 | 0.067* | |
C2 | 1.2174 (8) | 0.2521 (6) | 0.7480 (8) | 0.064 (2) | |
H2 | 1.2664 | 0.2762 | 0.7051 | 0.077* | |
C3 | 1.2701 (9) | 0.1904 (6) | 0.8325 (9) | 0.071 (2) | |
H3 | 1.3542 | 0.1715 | 0.8454 | 0.085* | |
C4 | 1.1988 (9) | 0.1565 (6) | 0.8978 (9) | 0.072 (2) | |
H4 | 1.2359 | 0.1161 | 0.9568 | 0.087* | |
C5 | 1.0715 (8) | 0.1819 (5) | 0.8768 (8) | 0.059 (2) | |
H5 | 1.0237 | 0.1583 | 0.9212 | 0.071* | |
C6 | 1.0162 (7) | 0.2426 (5) | 0.7897 (6) | 0.0487 (17) | |
C7 | 0.7510 (7) | 0.1298 (5) | 0.8188 (7) | 0.0525 (19) | |
H7 | 0.7651 | 0.1062 | 0.7519 | 0.063* | |
C8 | 0.6984 (8) | 0.0806 (6) | 0.8884 (7) | 0.064 (2) | |
H8 | 0.6802 | 0.0231 | 0.8704 | 0.077* | |
C9 | 0.6731 (9) | 0.1171 (7) | 0.9848 (8) | 0.076 (3) | |
H9 | 0.6349 | 0.0842 | 1.0297 | 0.092* | |
C10 | 0.7028 (10) | 0.1997 (6) | 1.0151 (8) | 0.074 (3) | |
H10 | 0.6864 | 0.2228 | 1.0812 | 0.089* | |
C11 | 0.7570 (8) | 0.2494 (5) | 0.9484 (7) | 0.063 (2) | |
H11 | 0.7768 | 0.3063 | 0.9691 | 0.075* | |
C12 | 0.7827 (7) | 0.2148 (5) | 0.8494 (6) | 0.0473 (17) | |
C13 | 0.9598 (8) | 0.4349 (5) | 0.8469 (8) | 0.063 (2) | |
H13 | 1.0403 | 0.4084 | 0.8710 | 0.076* | |
C14 | 0.9494 (9) | 0.5226 (5) | 0.8636 (9) | 0.075 (3) | |
H14 | 1.0235 | 0.5547 | 0.8998 | 0.090* | |
C15 | 0.8317 (9) | 0.5613 (5) | 0.8274 (8) | 0.066 (2) | |
H15 | 0.8261 | 0.6198 | 0.8388 | 0.079* | |
C16 | 0.7208 (9) | 0.5150 (5) | 0.7742 (8) | 0.061 (2) | |
H16 | 0.6406 | 0.5420 | 0.7493 | 0.073* | |
C17 | 0.7298 (7) | 0.4288 (5) | 0.7584 (7) | 0.0540 (19) | |
H17 | 0.6552 | 0.3971 | 0.7232 | 0.065* | |
C18 | 0.8495 (7) | 0.3881 (5) | 0.7945 (6) | 0.0474 (16) | |
C19 | 0.7579 (7) | 0.2617 (5) | 0.6080 (6) | 0.0479 (17) | |
H19A | 0.7657 | 0.2026 | 0.5865 | 0.058* | |
H19B | 0.6679 | 0.2717 | 0.5998 | 0.058* | |
C20 | 0.7948 (7) | 0.3201 (5) | 0.5188 (6) | 0.0523 (18) | |
H20A | 0.8071 | 0.3780 | 0.5497 | 0.063* | |
H20B | 0.8759 | 0.3007 | 0.5110 | 0.063* | |
C21 | 0.6913 (7) | 0.3197 (5) | 0.3967 (6) | 0.0498 (17) | |
H21A | 0.6080 | 0.3318 | 0.4058 | 0.060* | |
H21B | 0.6868 | 0.2633 | 0.3613 | 0.060* | |
C22 | 0.8465 (7) | 0.5315 (6) | 0.4443 (7) | 0.056 (2) | |
H22 | 0.9237 | 0.5023 | 0.4563 | 0.067* | |
C23 | 0.8467 (9) | 0.6076 (6) | 0.5033 (8) | 0.066 (2) | |
H23 | 0.9239 | 0.6298 | 0.5545 | 0.079* | |
C24 | 0.7323 (10) | 0.6506 (6) | 0.4863 (9) | 0.075 (3) | |
H24 | 0.7327 | 0.7022 | 0.5255 | 0.090* | |
C25 | 0.6174 (9) | 0.6179 (6) | 0.4120 (8) | 0.070 (2) | |
H25 | 0.5403 | 0.6468 | 0.4023 | 0.084* | |
C26 | 0.6165 (6) | 0.5428 (7) | 0.3522 (6) | 0.0576 (18) | |
H26 | 0.5387 | 0.5212 | 0.3014 | 0.069* | |
C27 | 0.7312 (7) | 0.4981 (5) | 0.3667 (7) | 0.0487 (18) | |
C28 | 0.9389 (8) | 0.4353 (6) | 0.2361 (8) | 0.064 (2) | |
H28 | 0.9113 | 0.4918 | 0.2317 | 0.077* | |
C29 | 1.0470 (9) | 0.4150 (7) | 0.2058 (9) | 0.079 (3) | |
H29 | 1.0918 | 0.4573 | 0.1804 | 0.095* | |
C30 | 1.0877 (9) | 0.3316 (8) | 0.2137 (9) | 0.079 (3) | |
H30 | 1.1616 | 0.3176 | 0.1952 | 0.095* | |
C31 | 1.0214 (10) | 0.2694 (7) | 0.2484 (9) | 0.082 (3) | |
H31 | 1.0486 | 0.2130 | 0.2503 | 0.098* | |
C32 | 0.9140 (9) | 0.2883 (6) | 0.2808 (8) | 0.060 (2) | |
H32 | 0.8711 | 0.2454 | 0.3075 | 0.072* | |
C33 | 0.8711 (7) | 0.3728 (5) | 0.2728 (6) | 0.0482 (17) | |
C34 | 0.4815 (8) | 0.3557 (5) | 0.1431 (7) | 0.058 (2) | |
H34 | 0.4677 | 0.3269 | 0.2067 | 0.070* | |
C35 | 0.3838 (8) | 0.3580 (6) | 0.0308 (8) | 0.068 (2) | |
H35 | 0.3059 | 0.3297 | 0.0197 | 0.082* | |
C36 | 0.4031 (9) | 0.4011 (6) | −0.0604 (8) | 0.069 (2) | |
H36 | 0.3369 | 0.4041 | −0.1336 | 0.083* | |
C37 | 0.5181 (9) | 0.4403 (6) | −0.0474 (8) | 0.068 (2) | |
H37 | 0.5313 | 0.4679 | −0.1122 | 0.081* | |
C38 | 0.6148 (8) | 0.4389 (5) | 0.0621 (6) | 0.0543 (19) | |
H38 | 0.6924 | 0.4670 | 0.0713 | 0.065* | |
C39 | 0.5981 (6) | 0.3961 (4) | 0.1588 (6) | 0.0416 (15) | |
C40 | 0.5950 (7) | 0.9012 (6) | 0.4523 (8) | 0.058 (2) | |
C41 | 0.6554 (8) | 0.9516 (5) | 0.5693 (7) | 0.057 (2) | |
H10D | 0.439 (6) | 0.197 (5) | 0.322 (8) | 0.100* | |
H10E | 0.375 (9) | 0.260 (6) | 0.367 (6) | 0.100* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo1 | 0.0506 (3) | 0.0450 (3) | 0.0630 (4) | −0.0057 (3) | 0.0255 (3) | −0.0096 (3) |
P1 | 0.0493 (11) | 0.0413 (10) | 0.0436 (10) | 0.0002 (9) | 0.0170 (9) | 0.0015 (8) |
P2 | 0.0447 (10) | 0.0432 (10) | 0.0442 (10) | 0.0009 (8) | 0.0122 (8) | 0.0028 (8) |
O1 | 0.060 (3) | 0.057 (3) | 0.052 (3) | −0.008 (3) | 0.017 (3) | −0.002 (3) |
O2 | 0.074 (4) | 0.058 (4) | 0.109 (5) | −0.017 (3) | 0.032 (4) | 0.005 (3) |
O3 | 0.092 (5) | 0.105 (5) | 0.068 (4) | 0.005 (4) | 0.042 (4) | 0.020 (4) |
O4 | 0.063 (3) | 0.057 (4) | 0.058 (3) | −0.004 (3) | 0.012 (3) | −0.011 (2) |
O5 | 0.058 (4) | 0.066 (4) | 0.106 (5) | 0.001 (3) | 0.023 (4) | −0.026 (4) |
O6 | 0.087 (5) | 0.092 (5) | 0.105 (6) | −0.013 (4) | 0.052 (4) | −0.029 (4) |
O7 | 0.108 (5) | 0.082 (5) | 0.066 (4) | −0.009 (4) | 0.026 (4) | 0.012 (3) |
O8 | 0.073 (4) | 0.067 (4) | 0.081 (4) | 0.004 (3) | 0.024 (3) | 0.006 (3) |
O9 | 0.059 (4) | 0.055 (4) | 0.103 (5) | −0.011 (3) | 0.039 (3) | −0.028 (3) |
O10 | 0.090 (5) | 0.081 (5) | 0.116 (6) | 0.007 (4) | 0.049 (5) | 0.003 (4) |
C1 | 0.054 (5) | 0.050 (5) | 0.062 (5) | −0.005 (4) | 0.016 (4) | 0.000 (4) |
C2 | 0.062 (5) | 0.066 (6) | 0.073 (6) | −0.010 (4) | 0.031 (4) | −0.014 (5) |
C3 | 0.058 (5) | 0.061 (6) | 0.095 (7) | 0.008 (4) | 0.025 (5) | −0.010 (5) |
C4 | 0.063 (5) | 0.062 (6) | 0.083 (7) | 0.009 (4) | 0.012 (5) | 0.007 (5) |
C5 | 0.059 (5) | 0.048 (5) | 0.072 (5) | 0.008 (4) | 0.025 (4) | 0.017 (4) |
C6 | 0.050 (4) | 0.045 (4) | 0.051 (4) | −0.004 (3) | 0.017 (3) | 0.001 (3) |
C7 | 0.059 (5) | 0.048 (5) | 0.052 (4) | −0.006 (4) | 0.021 (4) | −0.005 (3) |
C8 | 0.069 (5) | 0.054 (5) | 0.066 (5) | −0.019 (4) | 0.018 (4) | 0.004 (4) |
C9 | 0.084 (7) | 0.085 (7) | 0.068 (6) | −0.030 (6) | 0.034 (5) | 0.001 (5) |
C10 | 0.110 (8) | 0.068 (6) | 0.066 (5) | −0.020 (6) | 0.057 (6) | −0.002 (5) |
C11 | 0.089 (6) | 0.045 (5) | 0.061 (5) | −0.015 (4) | 0.034 (5) | −0.006 (4) |
C12 | 0.054 (4) | 0.048 (4) | 0.041 (4) | −0.002 (3) | 0.016 (3) | −0.008 (3) |
C13 | 0.055 (5) | 0.049 (5) | 0.083 (6) | −0.001 (4) | 0.019 (4) | −0.007 (4) |
C14 | 0.070 (6) | 0.053 (7) | 0.102 (7) | −0.013 (4) | 0.028 (5) | −0.022 (5) |
C15 | 0.085 (6) | 0.036 (5) | 0.090 (6) | −0.007 (4) | 0.046 (5) | −0.005 (4) |
C16 | 0.065 (5) | 0.049 (5) | 0.071 (5) | 0.007 (4) | 0.025 (4) | 0.004 (4) |
C17 | 0.048 (4) | 0.043 (4) | 0.071 (5) | 0.005 (3) | 0.020 (4) | 0.000 (4) |
C18 | 0.053 (4) | 0.039 (4) | 0.051 (4) | −0.004 (3) | 0.017 (3) | 0.001 (3) |
C19 | 0.056 (4) | 0.041 (4) | 0.051 (4) | −0.001 (3) | 0.023 (3) | 0.003 (3) |
C20 | 0.049 (4) | 0.058 (5) | 0.049 (4) | −0.006 (4) | 0.015 (3) | 0.005 (3) |
C21 | 0.060 (4) | 0.046 (4) | 0.045 (4) | 0.002 (4) | 0.019 (4) | −0.001 (3) |
C22 | 0.042 (4) | 0.054 (5) | 0.063 (4) | −0.005 (4) | 0.006 (3) | −0.006 (4) |
C23 | 0.061 (5) | 0.061 (5) | 0.070 (6) | −0.007 (4) | 0.014 (4) | −0.016 (4) |
C24 | 0.088 (7) | 0.067 (6) | 0.079 (6) | −0.003 (5) | 0.038 (6) | −0.021 (5) |
C25 | 0.054 (5) | 0.076 (6) | 0.081 (6) | 0.003 (4) | 0.022 (5) | −0.023 (5) |
C26 | 0.045 (3) | 0.059 (4) | 0.067 (4) | 0.006 (5) | 0.016 (3) | −0.020 (5) |
C27 | 0.050 (4) | 0.048 (4) | 0.048 (4) | −0.004 (3) | 0.016 (3) | 0.005 (3) |
C28 | 0.052 (5) | 0.061 (5) | 0.085 (6) | 0.007 (4) | 0.029 (4) | 0.007 (4) |
C29 | 0.060 (5) | 0.091 (8) | 0.097 (8) | 0.000 (5) | 0.041 (5) | 0.004 (6) |
C30 | 0.058 (6) | 0.113 (9) | 0.067 (6) | 0.021 (6) | 0.022 (5) | −0.004 (6) |
C31 | 0.089 (7) | 0.078 (7) | 0.089 (7) | 0.042 (6) | 0.045 (6) | 0.016 (6) |
C32 | 0.071 (6) | 0.057 (5) | 0.058 (5) | 0.015 (4) | 0.029 (4) | 0.009 (4) |
C33 | 0.047 (4) | 0.051 (4) | 0.047 (4) | 0.002 (3) | 0.016 (3) | 0.006 (3) |
C34 | 0.065 (5) | 0.066 (5) | 0.043 (4) | −0.011 (4) | 0.017 (4) | −0.001 (4) |
C35 | 0.054 (5) | 0.079 (6) | 0.059 (5) | −0.018 (4) | 0.001 (4) | −0.004 (5) |
C36 | 0.071 (5) | 0.075 (6) | 0.050 (5) | 0.002 (5) | 0.003 (4) | 0.003 (4) |
C37 | 0.072 (6) | 0.078 (6) | 0.051 (5) | 0.010 (5) | 0.016 (4) | 0.011 (4) |
C38 | 0.056 (4) | 0.058 (5) | 0.047 (4) | −0.005 (4) | 0.013 (4) | 0.011 (4) |
C39 | 0.046 (4) | 0.041 (4) | 0.037 (3) | −0.003 (3) | 0.013 (3) | 0.000 (3) |
C40 | 0.041 (4) | 0.056 (5) | 0.075 (5) | 0.003 (4) | 0.017 (4) | 0.002 (4) |
C41 | 0.054 (5) | 0.061 (5) | 0.058 (5) | 0.018 (4) | 0.020 (4) | 0.005 (4) |
Mo1—O9 | 1.657 (6) | C14—H14 | 0.9300 |
Mo1—O6 | 1.890 (7) | C15—C16 | 1.376 (11) |
Mo1—O7 | 1.890 (7) | C15—H15 | 0.9300 |
Mo1—O5 | 1.943 (6) | C16—C17 | 1.370 (10) |
Mo1—O8 | 1.945 (7) | C16—H16 | 0.9300 |
Mo1—O4 | 2.043 (6) | C17—C18 | 1.392 (10) |
Mo1—O1 | 2.213 (5) | C17—H17 | 0.9300 |
P1—C12 | 1.775 (7) | C19—C20 | 1.544 (9) |
P1—C6 | 1.781 (8) | C19—H19A | 0.9700 |
P1—C18 | 1.787 (8) | C19—H19B | 0.9700 |
P1—C19 | 1.789 (7) | C20—C21 | 1.515 (10) |
P2—C27 | 1.762 (8) | C20—H20A | 0.9700 |
P2—C39 | 1.775 (6) | C20—H20B | 0.9700 |
P2—C33 | 1.781 (7) | C21—H21A | 0.9700 |
P2—C21 | 1.781 (7) | C21—H21B | 0.9700 |
O1—C40 | 1.262 (9) | C22—C23 | 1.379 (12) |
O2—C40 | 1.246 (10) | C22—C27 | 1.396 (10) |
O3—C41 | 1.221 (9) | C22—H22 | 0.9300 |
O4—C41 | 1.293 (10) | C23—C24 | 1.377 (12) |
O5—O6 | 1.456 (10) | C23—H23 | 0.9300 |
O7—O8 | 1.451 (9) | C24—C25 | 1.376 (12) |
O10—H10D | 0.86 (8) | C24—H24 | 0.9300 |
O10—H10E | 0.86 (8) | C25—C26 | 1.369 (12) |
C1—C2 | 1.380 (12) | C25—H25 | 0.9300 |
C1—C6 | 1.392 (11) | C26—C27 | 1.396 (10) |
C1—H1 | 0.9300 | C26—H26 | 0.9300 |
C2—C3 | 1.373 (13) | C28—C33 | 1.380 (11) |
C2—H2 | 0.9300 | C28—C29 | 1.380 (11) |
C3—C4 | 1.369 (13) | C28—H28 | 0.9300 |
C3—H3 | 0.9300 | C29—C30 | 1.371 (14) |
C4—C5 | 1.390 (12) | C29—H29 | 0.9300 |
C4—H4 | 0.9300 | C30—C31 | 1.354 (15) |
C5—C6 | 1.385 (10) | C30—H30 | 0.9300 |
C5—H5 | 0.9300 | C31—C32 | 1.381 (12) |
C7—C8 | 1.380 (10) | C31—H31 | 0.9300 |
C7—C12 | 1.392 (10) | C32—C33 | 1.396 (11) |
C7—H7 | 0.9300 | C32—H32 | 0.9300 |
C8—C9 | 1.380 (12) | C34—C39 | 1.380 (10) |
C8—H8 | 0.9300 | C34—C35 | 1.406 (11) |
C9—C10 | 1.352 (12) | C34—H34 | 0.9300 |
C9—H9 | 0.9300 | C35—C36 | 1.345 (12) |
C10—C11 | 1.372 (11) | C35—H35 | 0.9300 |
C10—H10 | 0.9300 | C36—C37 | 1.363 (12) |
C11—C12 | 1.398 (10) | C36—H36 | 0.9300 |
C11—H11 | 0.9300 | C37—C38 | 1.378 (11) |
C13—C18 | 1.373 (10) | C37—H37 | 0.9300 |
C13—C14 | 1.396 (11) | C38—C39 | 1.386 (9) |
C13—H13 | 0.9300 | C38—H38 | 0.9300 |
C14—C15 | 1.360 (12) | C40—C41 | 1.540 (12) |
O9—Mo1—O6 | 103.3 (3) | C17—C16—H16 | 120.4 |
O9—Mo1—O7 | 101.8 (3) | C15—C16—H16 | 120.4 |
O6—Mo1—O7 | 89.4 (4) | C16—C17—C18 | 120.7 (8) |
O9—Mo1—O5 | 99.7 (3) | C16—C17—H17 | 119.6 |
O6—Mo1—O5 | 44.6 (3) | C18—C17—H17 | 119.6 |
O7—Mo1—O5 | 132.7 (3) | C13—C18—C17 | 119.7 (7) |
O9—Mo1—O8 | 99.0 (3) | C13—C18—P1 | 122.4 (6) |
O6—Mo1—O8 | 132.1 (3) | C17—C18—P1 | 117.8 (6) |
O7—Mo1—O8 | 44.4 (3) | C20—C19—P1 | 114.5 (5) |
O5—Mo1—O8 | 161.1 (3) | C20—C19—H19A | 108.6 |
O9—Mo1—O4 | 90.7 (3) | P1—C19—H19A | 108.6 |
O6—Mo1—O4 | 132.7 (3) | C20—C19—H19B | 108.6 |
O7—Mo1—O4 | 132.0 (3) | P1—C19—H19B | 108.6 |
O5—Mo1—O4 | 88.9 (3) | H19A—C19—H19B | 107.6 |
O8—Mo1—O4 | 88.1 (3) | C21—C20—C19 | 111.5 (6) |
O9—Mo1—O1 | 165.5 (3) | C21—C20—H20A | 109.3 |
O6—Mo1—O1 | 86.9 (3) | C19—C20—H20A | 109.3 |
O7—Mo1—O1 | 88.4 (3) | C21—C20—H20B | 109.3 |
O5—Mo1—O1 | 80.2 (3) | C19—C20—H20B | 109.3 |
O8—Mo1—O1 | 81.0 (3) | H20A—C20—H20B | 108.0 |
O4—Mo1—O1 | 74.8 (2) | C20—C21—P2 | 111.6 (5) |
C12—P1—C6 | 109.0 (3) | C20—C21—H21A | 109.3 |
C12—P1—C18 | 111.0 (3) | P2—C21—H21A | 109.3 |
C6—P1—C18 | 110.4 (3) | C20—C21—H21B | 109.3 |
C12—P1—C19 | 107.2 (3) | P2—C21—H21B | 109.3 |
C6—P1—C19 | 111.6 (3) | H21A—C21—H21B | 108.0 |
C18—P1—C19 | 107.6 (3) | C23—C22—C27 | 120.5 (8) |
C27—P2—C39 | 109.7 (3) | C23—C22—H22 | 119.8 |
C27—P2—C33 | 111.0 (4) | C27—C22—H22 | 119.8 |
C39—P2—C33 | 107.7 (3) | C24—C23—C22 | 119.7 (8) |
C27—P2—C21 | 107.9 (3) | C24—C23—H23 | 120.1 |
C39—P2—C21 | 110.1 (3) | C22—C23—H23 | 120.1 |
C33—P2—C21 | 110.6 (4) | C25—C24—C23 | 120.6 (9) |
C40—O1—Mo1 | 115.2 (5) | C25—C24—H24 | 119.7 |
C41—O4—Mo1 | 120.8 (5) | C23—C24—H24 | 119.7 |
O6—O5—Mo1 | 65.7 (4) | C26—C25—C24 | 119.9 (8) |
O5—O6—Mo1 | 69.6 (4) | C26—C25—H25 | 120.0 |
O8—O7—Mo1 | 69.8 (4) | C24—C25—H25 | 120.0 |
O7—O8—Mo1 | 65.8 (4) | C25—C26—C27 | 120.8 (7) |
H10D—O10—H10E | 109 (10) | C25—C26—H26 | 119.6 |
C2—C1—C6 | 120.9 (8) | C27—C26—H26 | 119.6 |
C2—C1—H1 | 119.6 | C26—C27—C22 | 118.4 (8) |
C6—C1—H1 | 119.6 | C26—C27—P2 | 119.1 (6) |
C3—C2—C1 | 119.9 (8) | C22—C27—P2 | 122.2 (6) |
C3—C2—H2 | 120.1 | C33—C28—C29 | 120.8 (9) |
C1—C2—H2 | 120.1 | C33—C28—H28 | 119.6 |
C4—C3—C2 | 119.9 (8) | C29—C28—H28 | 119.6 |
C4—C3—H3 | 120.0 | C30—C29—C28 | 119.2 (10) |
C2—C3—H3 | 120.0 | C30—C29—H29 | 120.4 |
C3—C4—C5 | 120.7 (8) | C28—C29—H29 | 120.4 |
C3—C4—H4 | 119.6 | C31—C30—C29 | 120.7 (9) |
C5—C4—H4 | 119.6 | C31—C30—H30 | 119.7 |
C6—C5—C4 | 119.8 (8) | C29—C30—H30 | 119.7 |
C6—C5—H5 | 120.1 | C30—C31—C32 | 121.2 (10) |
C4—C5—H5 | 120.1 | C30—C31—H31 | 119.4 |
C5—C6—C1 | 118.7 (7) | C32—C31—H31 | 119.4 |
C5—C6—P1 | 120.9 (6) | C31—C32—C33 | 118.8 (9) |
C1—C6—P1 | 120.4 (6) | C31—C32—H32 | 120.6 |
C8—C7—C12 | 119.7 (7) | C33—C32—H32 | 120.6 |
C8—C7—H7 | 120.1 | C28—C33—C32 | 119.3 (7) |
C12—C7—H7 | 120.1 | C28—C33—P2 | 121.0 (6) |
C7—C8—C9 | 119.7 (8) | C32—C33—P2 | 119.5 (6) |
C7—C8—H8 | 120.2 | C39—C34—C35 | 120.0 (7) |
C9—C8—H8 | 120.2 | C39—C34—H34 | 120.0 |
C10—C9—C8 | 121.2 (8) | C35—C34—H34 | 120.0 |
C10—C9—H9 | 119.4 | C36—C35—C34 | 119.9 (8) |
C8—C9—H9 | 119.4 | C36—C35—H35 | 120.1 |
C9—C10—C11 | 120.1 (8) | C34—C35—H35 | 120.1 |
C9—C10—H10 | 119.9 | C35—C36—C37 | 121.1 (8) |
C11—C10—H10 | 119.9 | C35—C36—H36 | 119.5 |
C10—C11—C12 | 120.2 (8) | C37—C36—H36 | 119.5 |
C10—C11—H11 | 119.9 | C36—C37—C38 | 119.7 (8) |
C12—C11—H11 | 119.9 | C36—C37—H37 | 120.1 |
C7—C12—C11 | 119.1 (7) | C38—C37—H37 | 120.1 |
C7—C12—P1 | 119.4 (5) | C37—C38—C39 | 120.9 (8) |
C11—C12—P1 | 121.5 (6) | C37—C38—H38 | 119.5 |
C18—C13—C14 | 119.1 (8) | C39—C38—H38 | 119.5 |
C18—C13—H13 | 120.4 | C34—C39—C38 | 118.3 (6) |
C14—C13—H13 | 120.4 | C34—C39—P2 | 121.8 (5) |
C15—C14—C13 | 120.4 (8) | C38—C39—P2 | 119.8 (5) |
C15—C14—H14 | 119.8 | O2—C40—O1 | 126.7 (8) |
C13—C14—H14 | 119.8 | O2—C40—C41 | 118.8 (8) |
C14—C15—C16 | 120.8 (8) | O1—C40—C41 | 114.5 (7) |
C14—C15—H15 | 119.6 | O3—C41—O4 | 124.9 (8) |
C16—C15—H15 | 119.6 | O3—C41—C40 | 121.3 (8) |
C17—C16—C15 | 119.2 (8) | O4—C41—C40 | 113.7 (7) |
O9—Mo1—O1—C40 | −8.2 (14) | C16—C17—C18—C13 | 0.3 (12) |
O6—Mo1—O1—C40 | 127.2 (6) | C16—C17—C18—P1 | −175.9 (6) |
O7—Mo1—O1—C40 | −143.3 (6) | C12—P1—C18—C13 | 114.2 (7) |
O5—Mo1—O1—C40 | 82.8 (6) | C6—P1—C18—C13 | −6.8 (8) |
O8—Mo1—O1—C40 | −99.2 (6) | C19—P1—C18—C13 | −128.8 (7) |
O4—Mo1—O1—C40 | −8.7 (5) | C12—P1—C18—C17 | −69.8 (7) |
O9—Mo1—O4—C41 | −175.8 (6) | C6—P1—C18—C17 | 169.3 (6) |
O6—Mo1—O4—C41 | −66.9 (7) | C19—P1—C18—C17 | 47.3 (7) |
O7—Mo1—O4—C41 | 77.6 (6) | C12—P1—C19—C20 | 172.5 (5) |
O5—Mo1—O4—C41 | −76.1 (6) | C6—P1—C19—C20 | −68.2 (6) |
O8—Mo1—O4—C41 | 85.3 (6) | C18—P1—C19—C20 | 53.0 (6) |
O1—Mo1—O4—C41 | 4.1 (5) | P1—C19—C20—C21 | −166.0 (5) |
O9—Mo1—O5—O6 | −99.1 (4) | C19—C20—C21—P2 | 172.6 (5) |
O7—Mo1—O5—O6 | 17.0 (6) | C27—P2—C21—C20 | −58.9 (6) |
O8—Mo1—O5—O6 | 89.4 (10) | C39—P2—C21—C20 | −178.5 (5) |
O4—Mo1—O5—O6 | 170.4 (4) | C33—P2—C21—C20 | 62.6 (6) |
O1—Mo1—O5—O6 | 95.6 (4) | C27—C22—C23—C24 | 0.5 (13) |
O9—Mo1—O6—O5 | 90.4 (4) | C22—C23—C24—C25 | 0.7 (15) |
O7—Mo1—O6—O5 | −167.6 (4) | C23—C24—C25—C26 | −1.3 (15) |
O8—Mo1—O6—O5 | −154.1 (4) | C24—C25—C26—C27 | 0.7 (15) |
O4—Mo1—O6—O5 | −13.2 (5) | C25—C26—C27—C22 | 0.5 (13) |
O1—Mo1—O6—O5 | −79.2 (4) | C25—C26—C27—P2 | 174.1 (7) |
O9—Mo1—O7—O8 | −90.9 (4) | C23—C22—C27—C26 | −1.1 (12) |
O6—Mo1—O7—O8 | 165.7 (4) | C23—C22—C27—P2 | −174.4 (7) |
O5—Mo1—O7—O8 | 153.8 (4) | C39—P2—C27—C26 | 36.1 (7) |
O4—Mo1—O7—O8 | 10.9 (5) | C33—P2—C27—C26 | 154.9 (6) |
O1—Mo1—O7—O8 | 78.7 (4) | C21—P2—C27—C26 | −83.8 (7) |
O9—Mo1—O8—O7 | 97.7 (4) | C39—P2—C27—C22 | −150.6 (6) |
O6—Mo1—O8—O7 | −19.5 (6) | C33—P2—C27—C22 | −31.7 (7) |
O5—Mo1—O8—O7 | −90.8 (10) | C21—P2—C27—C22 | 89.5 (7) |
O4—Mo1—O8—O7 | −171.9 (4) | C33—C28—C29—C30 | −0.7 (15) |
O1—Mo1—O8—O7 | −97.0 (4) | C28—C29—C30—C31 | 1.4 (16) |
C6—C1—C2—C3 | −0.5 (13) | C29—C30—C31—C32 | −2.4 (16) |
C1—C2—C3—C4 | −1.7 (13) | C30—C31—C32—C33 | 2.6 (15) |
C2—C3—C4—C5 | 2.2 (14) | C29—C28—C33—C32 | 0.9 (13) |
C3—C4—C5—C6 | −0.5 (14) | C29—C28—C33—P2 | −174.4 (7) |
C4—C5—C6—C1 | −1.6 (13) | C31—C32—C33—C28 | −1.8 (13) |
C4—C5—C6—P1 | −179.6 (7) | C31—C32—C33—P2 | 173.5 (7) |
C2—C1—C6—C5 | 2.1 (13) | C27—P2—C33—C28 | −38.1 (8) |
C2—C1—C6—P1 | −179.9 (6) | C39—P2—C33—C28 | 81.9 (7) |
C12—P1—C6—C5 | −5.4 (8) | C21—P2—C33—C28 | −157.8 (7) |
C18—P1—C6—C5 | 116.8 (7) | C27—P2—C33—C32 | 146.7 (6) |
C19—P1—C6—C5 | −123.6 (7) | C39—P2—C33—C32 | −93.3 (7) |
C12—P1—C6—C1 | 176.7 (6) | C21—P2—C33—C32 | 27.0 (8) |
C18—P1—C6—C1 | −61.1 (7) | C39—C34—C35—C36 | −1.3 (14) |
C19—P1—C6—C1 | 58.4 (8) | C34—C35—C36—C37 | 2.4 (15) |
C12—C7—C8—C9 | 2.6 (13) | C35—C36—C37—C38 | −2.6 (15) |
C7—C8—C9—C10 | −2.3 (15) | C36—C37—C38—C39 | 1.7 (13) |
C8—C9—C10—C11 | 1.2 (17) | C35—C34—C39—C38 | 0.5 (12) |
C9—C10—C11—C12 | −0.5 (15) | C35—C34—C39—P2 | 178.8 (7) |
C8—C7—C12—C11 | −1.9 (12) | C37—C38—C39—C34 | −0.6 (12) |
C8—C7—C12—P1 | 178.6 (6) | C37—C38—C39—P2 | −179.0 (6) |
C10—C11—C12—C7 | 0.8 (12) | C27—P2—C39—C34 | −104.5 (7) |
C10—C11—C12—P1 | −179.6 (7) | C33—P2—C39—C34 | 134.6 (6) |
C6—P1—C12—C7 | −72.3 (7) | C21—P2—C39—C34 | 14.0 (7) |
C18—P1—C12—C7 | 165.9 (6) | C27—P2—C39—C38 | 73.8 (7) |
C19—P1—C12—C7 | 48.7 (7) | C33—P2—C39—C38 | −47.0 (7) |
C6—P1—C12—C11 | 108.1 (7) | C21—P2—C39—C38 | −167.6 (6) |
C18—P1—C12—C11 | −13.6 (8) | Mo1—O1—C40—O2 | −171.5 (7) |
C19—P1—C12—C11 | −130.9 (7) | Mo1—O1—C40—C41 | 11.2 (8) |
C18—C13—C14—C15 | −0.6 (14) | Mo1—O4—C41—O3 | 179.3 (6) |
C13—C14—C15—C16 | 0.3 (14) | Mo1—O4—C41—C40 | 0.2 (8) |
C14—C15—C16—C17 | 0.3 (13) | O2—C40—C41—O3 | −4.6 (12) |
C15—C16—C17—C18 | −0.6 (13) | O1—C40—C41—O3 | 172.8 (7) |
C14—C13—C18—C17 | 0.3 (13) | O2—C40—C41—O4 | 174.6 (7) |
C14—C13—C18—P1 | 176.3 (7) | O1—C40—C41—O4 | −8.0 (10) |
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H10D···O8i | 0.86 (8) | 2.06 (8) | 2.916 (10) | 174 (9) |
O10—H10E···O2ii | 0.86 (8) | 2.32 (4) | 3.131 (11) | 158 (9) |
C7—H7···O4i | 0.93 | 2.60 | 3.484 (9) | 159 |
C19—H19A···O9i | 0.97 | 2.36 | 3.159 (9) | 140 |
C16—H16···O8ii | 0.93 | 2.59 | 3.511 (11) | 170 |
C19—H19B···O2ii | 0.97 | 2.31 | 3.243 (9) | 161 |
C26—H26···O3ii | 0.93 | 2.55 | 3.257 (11) | 133 |
C34—H34···O10 | 0.93 | 2.34 | 3.224 (11) | 158 |
C36—H36···O6iii | 0.93 | 2.56 | 3.408 (11) | 152 |
C1—H1···O5iv | 0.93 | 2.55 | 3.306 (11) | 139 |
C22—H22···O5iv | 0.93 | 2.42 | 3.280 (10) | 153 |
C23—H23···O9iv | 0.93 | 2.55 | 3.225 (10) | 130 |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, y−1/2, −z+1; (iii) −x+1, y−1/2, −z; (iv) −x+2, y−1/2, −z+1. |
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