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The central atom in the title complex, [Mo(C21H32NO2)O2(C2H6O)], is offset from the equatorial plane of a tetragonally distorted octahedron. This plane is defined by three donor atoms from a tridentate Schiff base auxiliary (O2N) and one oxo ligand. A second oxo ligand and an O donor atom of an ethanol molecule are located in axial positions of the coordination polyhedron. The absolute configuration at Mo is C. There are two molecules in the asymmetric unit.
Supporting information
CCDC reference: 298459
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.033
- wR factor = 0.081
- Data-to-parameter ratio = 19.1
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.88 Ratio
| Author Response: The distances C23-C24 and C45-C46 appear unusually short for
single C(sp^3^)-C(sp^3^) bonds [1.473(6) \%A and 1.492(7) \%A] due to
intense
thermal motion at these fragments. Similar large thermal motion
was observed for the methyl substituent in one of the tert-butyl
substituents.
Splitting of the methyl C atoms in this substituent was associated with an
improvement of the results. It was refrained from splitting the ethanol
C atoms, since this attempt did not improvement of the results.
|
PLAT773_ALERT_2_A Suspect C-C Bond in CIF: C41 -C43B .. 1.72 Ang.
| Author Response: Please refer to _vrf_PLAT220_har88_3_100K. Structure
solution and refinement of the data set of the title compound that was
obtained at 298 K affords the following bond lengths at the tert-butyl
group in question: C41-C42 1.389(15), C41-C43 1.444(14), C41-C44
1.451(13).
Thermal ellipsoids at this entity are significant. Thermal ellipsoids
of the remaining atoms of the title compound, however, were satisfactory
at 298 K. The data set obtained at 100 K was of sufficient quality to
split
the methyl C atoms of this tert-butyl substituent. Although the net effect
of this procdure was a slight improvement of the results, it also
led to unsatisfactory values for one of the conectivities formed between
the quarternary atom C41 and the split methyl C atoms(C42, C43, C44).
It is worth pointing out the second C-C bond obtained from this procedure
is satisfactory as outlined below:
|
C41 C42A 1.559(9) . ?
C41 C43A 1.509(8) . ?
C41 C44B 1.535(12) . ?
C41 C42B 1.480(14) . ?
C41 C43B 1.720(13) . ?
C41 C44A 1.648(8) . ?
In view of these arguments we feel that the compound is structurally
adequately
characterized and appreciate, if it merrits publication in Acta E.
Alert level B
PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.25 Ratio
| Author Response: The distances C23-C24 and C45-C46 appear unusually short for
single C(sp^3^)-C(sp^3^) bonds [1.473(6) \%A and 1.492(7) \%A] due to
intense
thermal motion at these fragments. Similar large thermal motion
was observed for the methyl substituent in one of the tert-butyl
substituents.
Splitting of the methyl C atoms in this substituent was associated with an
improvement of the results. It was refrained from splitting the ethanol
C atoms, since this attempt did not improvement of the results.
|
PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.24 Ratio
PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.85 Ratio
PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O10 .. 2.69 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O5 .. O6 .. 2.77 Ang.
Alert level C
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C45
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C18
PLAT301_ALERT_3_C Main Residue Disorder ......................... 5.00 Perc.
PLAT333_ALERT_2_C Large Average Benzene C-C Dist. C2 -C7 1.44 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact O2 .. C24 .. 2.95 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 123
C22 -O5 -MO1 -O1 153.00 1.30 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 149
C45 -O10 -MO2 -O6 -145.70 0.70 1.555 1.555 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 23.10 Deg.
C42B -C41 -C42A 1.555 1.555 1.555
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 26.38
From the CIF: _reflns_number_total 10881
Count of symmetry unique reflns 6079
Completeness (_total/calc) 178.99%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 4802
Fraction of Friedel pairs measured 0.790
Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem
5 ALERT level B = Potentially serious problem
8 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
10 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrysAlis CCD (Oxford Diffraction, 2002); cell refinement: CrysAlis RED-CCD (Oxford Diffraction, 2002); data reduction: CrysAlis RED-CCD; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON2002 (Spek, 2003) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
(
C)-(2,4-Di-
tert-butyl-6-{[(2
S)-3,3-dimethyl-1-oxido-2-
butyl]iminomethyl}phenolato)ethanol-
cis-dioxomolybdenum(VI)
top
Crystal data top
[Mo(C21H32NO2)O2(C2H6O)] | F(000) = 2120 |
Mr = 504.48 | Dx = 1.245 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 14425 reflections |
a = 11.5961 (4) Å | θ = 2.4–29.5° |
b = 19.9913 (5) Å | µ = 0.52 mm−1 |
c = 23.2143 (6) Å | T = 100 K |
V = 5381.6 (3) Å3 | Prism, yellow |
Z = 8 | 0.40 × 0.36 × 0.32 mm |
Data collection top
Oxford Diffraction Xcalibur (TM) diffractometer with Sapphire CCD detector | 10881 independent reflections |
Radiation source: fine-focus sealed tube | 10278 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
rotation method data acquisition using ω scans | θmax = 26.4°, θmin = 4.1° |
Absorption correction: analytical (CrysAlis RED-CCD; Oxford Diffraction, 2002) | h = −14→8 |
Tmin = 0.829, Tmax = 0.874 | k = −24→24 |
35088 measured reflections | l = −29→29 |
Refinement top
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)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.081 | w = 1/[σ2(Fo2) + (0.0315P)2 + 6.7957P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max = 0.009 |
10881 reflections | Δρmax = 0.61 e Å−3 |
571 parameters | Δρmin = −0.40 e Å−3 |
71 restraints | Absolute structure: Flack (1983), 4802 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.02 (3) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1 | 0.6597 (3) | 0.21984 (16) | 0.15375 (13) | 0.0168 (6) | |
H1 | 0.7060 | 0.1866 | 0.1716 | 0.020* | |
C2 | 0.5671 (3) | 0.19669 (16) | 0.11583 (13) | 0.0164 (6) | |
C3 | 0.4822 (3) | 0.24387 (16) | 0.09517 (14) | 0.0167 (6) | |
C4 | 0.3867 (3) | 0.21903 (16) | 0.06385 (13) | 0.0178 (6) | |
C5 | 0.3862 (3) | 0.14772 (16) | 0.04829 (13) | 0.0201 (6) | |
H5 | 0.3235 | 0.1319 | 0.0257 | 0.024* | |
C6 | 0.4736 (3) | 0.09995 (16) | 0.06467 (14) | 0.0203 (7) | |
C7 | 0.5603 (3) | 0.12481 (16) | 0.10048 (14) | 0.0202 (7) | |
H7 | 0.6165 | 0.0949 | 0.1154 | 0.024* | |
C8 | 0.7487 (3) | 0.36662 (17) | 0.23752 (14) | 0.0210 (7) | |
H8A | 0.6949 | 0.3578 | 0.2698 | 0.025* | |
H8B | 0.8194 | 0.3871 | 0.2537 | 0.025* | |
C9 | 0.7810 (3) | 0.29788 (17) | 0.20710 (14) | 0.0186 (7) | |
H9 | 0.7798 | 0.2619 | 0.2370 | 0.022* | |
C10 | 0.9035 (3) | 0.29765 (16) | 0.17796 (14) | 0.0205 (7) | |
C11 | 0.9110 (3) | 0.3514 (2) | 0.12895 (16) | 0.0324 (8) | |
H11A | 0.8996 | 0.3961 | 0.1454 | 0.039* | |
H11B | 0.8511 | 0.3427 | 0.1002 | 0.039* | |
H11C | 0.9870 | 0.3491 | 0.1106 | 0.039* | |
C12 | 0.9293 (3) | 0.22365 (19) | 0.15412 (17) | 0.0304 (8) | |
H12A | 0.8726 | 0.2122 | 0.1244 | 0.036* | |
H12B | 0.9240 | 0.1915 | 0.1859 | 0.036* | |
H12C | 1.0069 | 0.2222 | 0.1375 | 0.036* | |
C13 | 0.9938 (3) | 0.3139 (2) | 0.22409 (16) | 0.0313 (9) | |
H13A | 0.9925 | 0.2791 | 0.2539 | 0.038* | |
H13B | 0.9761 | 0.3573 | 0.2415 | 0.038* | |
H13C | 1.0704 | 0.3155 | 0.2064 | 0.038* | |
C14 | 0.2877 (3) | 0.26932 (18) | 0.04773 (15) | 0.0230 (7) | |
C15 | 0.2405 (3) | 0.3040 (2) | 0.10310 (17) | 0.0321 (9) | |
H15A | 0.3035 | 0.3276 | 0.1226 | 0.039* | |
H15B | 0.2082 | 0.2702 | 0.1290 | 0.039* | |
H15C | 0.1803 | 0.3361 | 0.0925 | 0.039* | |
C16 | 0.3316 (4) | 0.3269 (2) | 0.00655 (17) | 0.0343 (9) | |
H16A | 0.3680 | 0.3072 | −0.0275 | 0.041* | |
H16B | 0.3879 | 0.3547 | 0.0270 | 0.041* | |
H16C | 0.2661 | 0.3547 | −0.0054 | 0.041* | |
C17 | 0.1861 (3) | 0.2310 (2) | 0.01902 (18) | 0.0352 (9) | |
H17A | 0.1550 | 0.1981 | 0.0462 | 0.042* | |
H17B | 0.2140 | 0.2079 | −0.0155 | 0.042* | |
H17C | 0.1255 | 0.2628 | 0.0083 | 0.042* | |
C18 | 0.4733 (3) | 0.02277 (18) | 0.04472 (16) | 0.0259 (8) | |
C19 | 0.3741 (5) | 0.0069 (2) | 0.0019 (2) | 0.0499 (12) | |
H19A | 0.3827 | 0.0346 | −0.0326 | 0.060* | |
H19B | 0.2998 | 0.0166 | 0.0203 | 0.060* | |
H19C | 0.3772 | −0.0405 | −0.0088 | 0.060* | |
C20 | 0.4594 (5) | −0.0259 (2) | 0.0959 (2) | 0.0510 (13) | |
H20A | 0.3855 | −0.0176 | 0.1150 | 0.061* | |
H20B | 0.5225 | −0.0190 | 0.1233 | 0.061* | |
H20C | 0.4613 | −0.0721 | 0.0817 | 0.061* | |
C21 | 0.5861 (5) | 0.0077 (3) | 0.0133 (3) | 0.0727 (19) | |
H21A | 0.6509 | 0.0130 | 0.0400 | 0.087* | |
H21B | 0.5952 | 0.0388 | −0.0190 | 0.087* | |
H21C | 0.5844 | −0.0383 | −0.0013 | 0.087* | |
C22 | 0.4532 (3) | 0.3914 (2) | 0.26769 (17) | 0.0404 (10) | |
H22A | 0.4809 | 0.3756 | 0.3057 | 0.048* | |
H22B | 0.4910 | 0.4348 | 0.2594 | 0.048* | |
C23 | 0.3274 (5) | 0.4010 (3) | 0.2700 (3) | 0.081 (2) | |
H23C | 0.3091 | 0.4371 | 0.2970 | 0.097* | |
H23B | 0.2904 | 0.3595 | 0.2828 | 0.097* | |
H23A | 0.2988 | 0.4129 | 0.2315 | 0.097* | |
C24 | 0.5632 (3) | 0.58389 (16) | 0.10959 (14) | 0.0174 (7) | |
H24 | 0.6260 | 0.5539 | 0.1046 | 0.021* | |
C25 | 0.4902 (3) | 0.59788 (17) | 0.05951 (14) | 0.0199 (7) | |
C26 | 0.3982 (3) | 0.64644 (16) | 0.06085 (13) | 0.0204 (7) | |
C27 | 0.3371 (3) | 0.66161 (19) | 0.00931 (15) | 0.0249 (7) | |
C28 | 0.3660 (3) | 0.6220 (2) | −0.03942 (14) | 0.0313 (8) | |
H28 | 0.3243 | 0.6300 | −0.0740 | 0.038* | |
C29 | 0.4534 (3) | 0.5708 (2) | −0.04069 (15) | 0.0312 (9) | |
C30 | 0.5158 (3) | 0.56023 (19) | 0.00896 (14) | 0.0255 (8) | |
H30 | 0.5758 | 0.5279 | 0.0095 | 0.031* | |
C31 | 0.5554 (3) | 0.6000 (2) | 0.26340 (15) | 0.0286 (8) | |
H31A | 0.5767 | 0.5664 | 0.2929 | 0.034* | |
H31B | 0.5746 | 0.6449 | 0.2786 | 0.034* | |
C32 | 0.6248 (3) | 0.58696 (16) | 0.20805 (13) | 0.0213 (7) | |
H32 | 0.6380 | 0.5377 | 0.2041 | 0.026* | |
C33 | 0.7458 (3) | 0.6236 (2) | 0.20895 (15) | 0.0273 (8) | |
C34 | 0.8159 (3) | 0.6031 (2) | 0.15546 (18) | 0.0377 (10) | |
H34A | 0.7744 | 0.6166 | 0.1206 | 0.045* | |
H34B | 0.8267 | 0.5545 | 0.1553 | 0.045* | |
H34C | 0.8914 | 0.6252 | 0.1564 | 0.045* | |
C35 | 0.8091 (4) | 0.5974 (2) | 0.26288 (19) | 0.0430 (11) | |
H35A | 0.8139 | 0.5485 | 0.2612 | 0.052* | |
H35B | 0.7666 | 0.6107 | 0.2975 | 0.052* | |
H35C | 0.8871 | 0.6163 | 0.2642 | 0.052* | |
C36 | 0.7346 (3) | 0.7044 (2) | 0.21016 (18) | 0.0348 (9) | |
H36A | 0.6926 | 0.7182 | 0.2448 | 0.042* | |
H36B | 0.6926 | 0.7196 | 0.1759 | 0.042* | |
H36C | 0.8117 | 0.7244 | 0.2105 | 0.042* | |
C37 | 0.2439 (3) | 0.72007 (19) | 0.00759 (18) | 0.0321 (9) | |
C38 | 0.3019 (4) | 0.7910 (2) | 0.0221 (2) | 0.0429 (11) | |
H38A | 0.3618 | 0.8009 | −0.0064 | 0.051* | |
H38B | 0.3364 | 0.7894 | 0.0606 | 0.051* | |
H38C | 0.2428 | 0.8260 | 0.0210 | 0.051* | |
C39 | 0.1456 (3) | 0.7056 (2) | 0.05013 (18) | 0.0352 (9) | |
H39A | 0.1773 | 0.7011 | 0.0891 | 0.042* | |
H39B | 0.1068 | 0.6640 | 0.0391 | 0.042* | |
H39C | 0.0902 | 0.7426 | 0.0493 | 0.042* | |
C40 | 0.1898 (4) | 0.7265 (3) | −0.0531 (2) | 0.0493 (12) | |
H40A | 0.1550 | 0.6837 | −0.0642 | 0.059* | |
H40B | 0.2498 | 0.7386 | −0.0810 | 0.059* | |
H40C | 0.1303 | 0.7613 | −0.0526 | 0.059* | |
C41 | 0.4772 (4) | 0.5278 (3) | −0.09598 (17) | 0.0468 (10) | |
C42A | 0.5674 (14) | 0.4706 (8) | −0.0886 (6) | 0.050 (3) | 0.61 (4) |
H42A | 0.5415 | 0.4399 | −0.0584 | 0.060* | 0.61 (4) |
H42B | 0.6421 | 0.4899 | −0.0778 | 0.060* | 0.61 (4) |
H42C | 0.5753 | 0.4462 | −0.1250 | 0.060* | 0.61 (4) |
C42B | 0.519 (3) | 0.4590 (7) | −0.0855 (9) | 0.056 (4) | 0.39 (4) |
H42D | 0.4634 | 0.4351 | −0.0612 | 0.067* | 0.39 (4) |
H42E | 0.5938 | 0.4607 | −0.0660 | 0.067* | 0.39 (4) |
H42F | 0.5272 | 0.4355 | −0.1224 | 0.067* | 0.39 (4) |
C43A | 0.5024 (7) | 0.5730 (4) | −0.1465 (3) | 0.0498 (19) | 0.644 (10) |
H43A | 0.5703 | 0.6005 | −0.1379 | 0.060* | 0.644 (10) |
H43B | 0.4359 | 0.6022 | −0.1535 | 0.060* | 0.644 (10) |
H43C | 0.5174 | 0.5458 | −0.1808 | 0.060* | 0.644 (10) |
C43B | 0.6006 (12) | 0.5686 (6) | −0.1175 (5) | 0.049 (3) | 0.356 (10) |
H43D | 0.6597 | 0.5642 | −0.0875 | 0.059* | 0.356 (10) |
H43E | 0.5835 | 0.6161 | −0.1237 | 0.059* | 0.356 (10) |
H43F | 0.6288 | 0.5488 | −0.1534 | 0.059* | 0.356 (10) |
C44A | 0.3613 (6) | 0.4838 (3) | −0.1118 (3) | 0.0400 (16) | 0.670 (9) |
H44A | 0.2959 | 0.5141 | −0.1179 | 0.048* | 0.670 (9) |
H44B | 0.3438 | 0.4533 | −0.0799 | 0.048* | 0.670 (9) |
H44C | 0.3752 | 0.4579 | −0.1469 | 0.048* | 0.670 (9) |
C44B | 0.4034 (14) | 0.5527 (8) | −0.1465 (5) | 0.056 (3) | 0.330 (9) |
H44D | 0.4227 | 0.5994 | −0.1549 | 0.067* | 0.330 (9) |
H44E | 0.3216 | 0.5494 | −0.1363 | 0.067* | 0.330 (9) |
H44F | 0.4187 | 0.5251 | −0.1806 | 0.067* | 0.330 (9) |
C45 | 0.2230 (3) | 0.52708 (19) | 0.12490 (18) | 0.0332 (9) | |
H45B | 0.2434 | 0.4906 | 0.0979 | 0.040* | |
H45A | 0.1969 | 0.5658 | 0.1017 | 0.040* | |
C46 | 0.1264 (4) | 0.5044 (3) | 0.1625 (3) | 0.0738 (18) | |
H46A | 0.1109 | 0.5385 | 0.1919 | 0.089* | |
H46B | 0.1476 | 0.4623 | 0.1814 | 0.089* | |
H46C | 0.0571 | 0.4975 | 0.1391 | 0.089* | |
N1 | 0.6854 (2) | 0.28453 (13) | 0.16561 (11) | 0.0159 (5) | |
N2 | 0.5479 (2) | 0.60965 (14) | 0.16034 (11) | 0.0187 (6) | |
O1 | 0.6647 (2) | 0.40652 (13) | 0.07989 (11) | 0.0271 (6) | |
O2 | 0.48581 (19) | 0.44975 (11) | 0.14605 (11) | 0.0230 (5) | |
O3 | 0.4909 (2) | 0.31272 (12) | 0.10568 (10) | 0.0203 (5) | |
O4 | 0.69526 (19) | 0.41334 (11) | 0.19737 (11) | 0.0221 (5) | |
O5 | 0.4860 (2) | 0.34248 (13) | 0.22310 (10) | 0.0237 (5) | |
O6 | 0.4362 (2) | 0.73293 (13) | 0.21548 (11) | 0.0303 (6) | |
O7 | 0.2331 (2) | 0.65882 (14) | 0.21032 (11) | 0.0308 (6) | |
O8 | 0.3693 (2) | 0.67940 (11) | 0.11007 (10) | 0.0244 (5) | |
O9 | 0.4348 (2) | 0.59612 (13) | 0.25234 (10) | 0.0283 (6) | |
O10 | 0.3246 (2) | 0.54603 (12) | 0.15710 (10) | 0.0238 (5) | |
Mo1 | 0.58797 (2) | 0.383517 (13) | 0.139510 (11) | 0.01615 (6) | |
Mo2 | 0.37671 (2) | 0.654983 (15) | 0.191631 (12) | 0.02186 (7) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0137 (14) | 0.0197 (15) | 0.0170 (15) | 0.0042 (12) | 0.0019 (11) | 0.0022 (12) |
C2 | 0.0160 (16) | 0.0185 (15) | 0.0147 (14) | −0.0029 (12) | 0.0010 (12) | 0.0014 (12) |
C3 | 0.0147 (15) | 0.0207 (16) | 0.0148 (15) | −0.0004 (12) | 0.0043 (12) | −0.0015 (13) |
C4 | 0.0158 (16) | 0.0234 (16) | 0.0140 (14) | −0.0012 (13) | 0.0029 (12) | −0.0015 (12) |
C5 | 0.0198 (16) | 0.0240 (16) | 0.0164 (14) | −0.0069 (14) | 0.0030 (12) | −0.0026 (13) |
C6 | 0.0260 (18) | 0.0194 (17) | 0.0156 (15) | −0.0013 (13) | 0.0077 (13) | −0.0014 (13) |
C7 | 0.0236 (17) | 0.0182 (16) | 0.0187 (15) | 0.0001 (13) | 0.0029 (12) | 0.0031 (13) |
C8 | 0.0177 (16) | 0.0276 (19) | 0.0176 (16) | −0.0004 (13) | −0.0038 (13) | −0.0022 (13) |
C9 | 0.0164 (16) | 0.0219 (16) | 0.0174 (16) | −0.0026 (13) | −0.0044 (12) | 0.0017 (13) |
C10 | 0.0134 (15) | 0.0259 (16) | 0.0221 (16) | 0.0010 (13) | −0.0022 (13) | 0.0006 (13) |
C11 | 0.0156 (15) | 0.045 (2) | 0.037 (2) | 0.0000 (17) | 0.0057 (15) | 0.0148 (18) |
C12 | 0.0169 (17) | 0.036 (2) | 0.038 (2) | 0.0019 (15) | 0.0042 (15) | −0.0067 (16) |
C13 | 0.0166 (17) | 0.048 (2) | 0.0294 (19) | 0.0047 (16) | −0.0062 (15) | −0.0058 (18) |
C14 | 0.0173 (16) | 0.0298 (19) | 0.0220 (17) | 0.0025 (14) | −0.0042 (13) | −0.0046 (15) |
C15 | 0.0158 (17) | 0.050 (2) | 0.031 (2) | 0.0058 (16) | 0.0002 (15) | −0.0130 (18) |
C16 | 0.033 (2) | 0.039 (2) | 0.031 (2) | 0.0072 (17) | −0.0080 (16) | 0.0052 (17) |
C17 | 0.0249 (19) | 0.043 (2) | 0.038 (2) | −0.0007 (17) | −0.0138 (17) | −0.0075 (19) |
C18 | 0.033 (2) | 0.0191 (17) | 0.0259 (18) | −0.0033 (15) | −0.0005 (15) | −0.0050 (14) |
C19 | 0.076 (3) | 0.028 (2) | 0.045 (3) | −0.004 (2) | −0.023 (3) | −0.0078 (19) |
C20 | 0.090 (4) | 0.028 (2) | 0.035 (2) | −0.005 (2) | −0.009 (2) | −0.0017 (19) |
C21 | 0.059 (3) | 0.049 (3) | 0.110 (5) | −0.014 (3) | 0.038 (4) | −0.046 (3) |
C22 | 0.043 (2) | 0.050 (3) | 0.0278 (19) | −0.001 (2) | 0.0065 (17) | −0.011 (2) |
C23 | 0.060 (4) | 0.075 (4) | 0.106 (5) | 0.006 (3) | 0.036 (4) | −0.015 (4) |
C24 | 0.0135 (16) | 0.0185 (15) | 0.0203 (16) | −0.0039 (12) | 0.0009 (12) | 0.0011 (13) |
C25 | 0.0224 (17) | 0.0227 (18) | 0.0148 (15) | 0.0013 (13) | 0.0009 (13) | 0.0005 (13) |
C26 | 0.0244 (17) | 0.0178 (15) | 0.0191 (15) | −0.0027 (14) | −0.0020 (13) | 0.0019 (13) |
C27 | 0.0249 (17) | 0.0271 (18) | 0.0228 (17) | 0.0037 (15) | −0.0034 (13) | 0.0059 (15) |
C28 | 0.0340 (19) | 0.043 (2) | 0.0165 (15) | 0.0022 (19) | −0.0073 (14) | 0.0086 (16) |
C29 | 0.0246 (18) | 0.052 (2) | 0.0171 (17) | 0.0058 (17) | 0.0035 (14) | 0.0008 (17) |
C30 | 0.0233 (18) | 0.036 (2) | 0.0176 (16) | 0.0063 (15) | 0.0037 (14) | 0.0007 (15) |
C31 | 0.031 (2) | 0.035 (2) | 0.0195 (17) | −0.0032 (15) | −0.0068 (14) | −0.0005 (15) |
C32 | 0.0220 (16) | 0.0207 (15) | 0.0212 (16) | 0.0009 (14) | −0.0066 (13) | 0.0013 (13) |
C33 | 0.0211 (16) | 0.0317 (19) | 0.0291 (18) | −0.0013 (15) | −0.0066 (14) | −0.0039 (16) |
C34 | 0.0183 (17) | 0.052 (3) | 0.043 (2) | −0.0039 (17) | −0.0021 (16) | −0.0029 (19) |
C35 | 0.036 (2) | 0.050 (3) | 0.043 (2) | −0.0042 (19) | −0.0209 (19) | 0.006 (2) |
C36 | 0.030 (2) | 0.039 (2) | 0.035 (2) | −0.0126 (18) | −0.0069 (17) | 0.0003 (18) |
C37 | 0.033 (2) | 0.0254 (19) | 0.037 (2) | 0.0060 (16) | −0.0101 (17) | 0.0049 (17) |
C38 | 0.039 (2) | 0.024 (2) | 0.065 (3) | 0.0026 (18) | −0.011 (2) | 0.009 (2) |
C39 | 0.028 (2) | 0.032 (2) | 0.045 (2) | 0.0127 (17) | −0.0076 (18) | −0.0040 (18) |
C40 | 0.051 (3) | 0.054 (3) | 0.043 (3) | 0.019 (2) | −0.015 (2) | 0.013 (2) |
C41 | 0.055 (3) | 0.068 (3) | 0.0171 (18) | 0.018 (2) | 0.0019 (18) | −0.0064 (19) |
C42A | 0.053 (5) | 0.072 (6) | 0.026 (4) | 0.019 (5) | 0.000 (5) | −0.016 (4) |
C42B | 0.103 (12) | 0.040 (5) | 0.025 (6) | −0.009 (6) | 0.005 (9) | −0.011 (5) |
C43A | 0.060 (5) | 0.065 (4) | 0.025 (3) | −0.007 (3) | 0.010 (3) | −0.001 (3) |
C43B | 0.072 (6) | 0.048 (6) | 0.027 (6) | 0.005 (6) | 0.003 (5) | −0.004 (5) |
C44A | 0.049 (3) | 0.045 (4) | 0.026 (3) | 0.005 (3) | 0.002 (3) | −0.006 (3) |
C44B | 0.068 (6) | 0.083 (8) | 0.016 (5) | 0.008 (6) | −0.002 (5) | −0.011 (5) |
C45 | 0.0267 (19) | 0.0240 (18) | 0.049 (2) | −0.0027 (15) | −0.0157 (17) | −0.0056 (17) |
C46 | 0.035 (3) | 0.087 (4) | 0.099 (5) | −0.022 (3) | 0.014 (3) | −0.029 (4) |
N1 | 0.0122 (12) | 0.0208 (14) | 0.0148 (12) | −0.0018 (11) | −0.0007 (10) | 0.0009 (11) |
N2 | 0.0192 (13) | 0.0183 (13) | 0.0187 (13) | −0.0040 (11) | −0.0048 (10) | 0.0029 (12) |
O1 | 0.0241 (12) | 0.0324 (14) | 0.0247 (13) | 0.0026 (10) | 0.0015 (10) | 0.0061 (11) |
O2 | 0.0189 (11) | 0.0186 (11) | 0.0316 (13) | 0.0025 (9) | −0.0012 (11) | 0.0001 (10) |
O3 | 0.0177 (11) | 0.0181 (11) | 0.0251 (12) | 0.0008 (9) | −0.0034 (10) | −0.0028 (10) |
O4 | 0.0198 (11) | 0.0196 (11) | 0.0270 (13) | −0.0002 (9) | −0.0062 (10) | 0.0004 (10) |
O5 | 0.0234 (12) | 0.0276 (13) | 0.0201 (11) | 0.0015 (11) | 0.0033 (9) | −0.0049 (11) |
O6 | 0.0321 (14) | 0.0303 (14) | 0.0286 (13) | −0.0010 (11) | 0.0015 (11) | −0.0097 (11) |
O7 | 0.0241 (12) | 0.0321 (14) | 0.0361 (14) | 0.0023 (11) | 0.0025 (10) | −0.0113 (12) |
O8 | 0.0250 (12) | 0.0219 (11) | 0.0264 (12) | 0.0069 (10) | −0.0057 (10) | −0.0033 (10) |
O9 | 0.0262 (14) | 0.0381 (15) | 0.0207 (12) | −0.0040 (11) | 0.0018 (10) | −0.0024 (11) |
O10 | 0.0194 (11) | 0.0217 (12) | 0.0302 (13) | −0.0001 (10) | −0.0010 (10) | −0.0046 (10) |
Mo1 | 0.01465 (12) | 0.01470 (12) | 0.01910 (12) | 0.00059 (10) | −0.00059 (11) | 0.00020 (11) |
Mo2 | 0.02117 (14) | 0.02251 (14) | 0.02191 (14) | 0.00109 (12) | 0.00035 (12) | −0.00763 (12) |
Geometric parameters (Å, º) top
C1—N1 | 1.355 (4) | C29—C41 | 1.569 (6) |
C1—C2 | 1.464 (4) | C30—H30 | 0.9500 |
C1—H1 | 0.9500 | C31—O9 | 1.424 (4) |
C2—C3 | 1.445 (4) | C31—C32 | 1.538 (5) |
C2—C7 | 1.482 (4) | C31—H31A | 0.9900 |
C3—O3 | 1.402 (4) | C31—H31B | 0.9900 |
C3—C4 | 1.415 (4) | C32—N2 | 1.493 (4) |
C4—C5 | 1.471 (4) | C32—C33 | 1.582 (5) |
C4—C14 | 1.571 (5) | C32—H32 | 1.0000 |
C5—C6 | 1.444 (5) | C33—C34 | 1.540 (5) |
C5—H5 | 0.9500 | C33—C35 | 1.544 (5) |
C6—C7 | 1.396 (5) | C33—C36 | 1.621 (6) |
C6—C18 | 1.611 (5) | C34—H34A | 0.9800 |
C7—H7 | 0.9500 | C34—H34B | 0.9800 |
C8—O4 | 1.458 (4) | C34—H34C | 0.9800 |
C8—C9 | 1.590 (5) | C35—H35A | 0.9800 |
C8—H8A | 0.9900 | C35—H35B | 0.9800 |
C8—H8B | 0.9900 | C35—H35C | 0.9800 |
C9—N1 | 1.493 (4) | C36—H36A | 0.9800 |
C9—C10 | 1.573 (4) | C36—H36B | 0.9800 |
C9—H9 | 1.0000 | C36—H36C | 0.9800 |
C10—C13 | 1.532 (5) | C37—C39 | 1.536 (6) |
C10—C11 | 1.568 (5) | C37—C40 | 1.548 (6) |
C10—C12 | 1.607 (5) | C37—C38 | 1.605 (6) |
C11—H11A | 0.9800 | C38—H38A | 0.9800 |
C11—H11B | 0.9800 | C38—H38B | 0.9800 |
C11—H11C | 0.9800 | C38—H38C | 0.9800 |
C12—H12A | 0.9800 | C39—H39A | 0.9800 |
C12—H12B | 0.9800 | C39—H39B | 0.9800 |
C12—H12C | 0.9800 | C39—H39C | 0.9800 |
C13—H13A | 0.9800 | C40—H40A | 0.9800 |
C13—H13B | 0.9800 | C40—H40B | 0.9800 |
C13—H13C | 0.9800 | C40—H40C | 0.9800 |
C14—C17 | 1.555 (5) | C41—C42B | 1.480 (14) |
C14—C15 | 1.560 (5) | C41—C43A | 1.509 (8) |
C14—C16 | 1.581 (5) | C41—C44B | 1.535 (12) |
C15—H15A | 0.9800 | C41—C42A | 1.559 (9) |
C15—H15B | 0.9800 | C41—C44A | 1.648 (8) |
C15—H15C | 0.9800 | C41—C43B | 1.720 (13) |
C16—H16A | 0.9800 | C42A—H42A | 0.9800 |
C16—H16B | 0.9800 | C42A—H42B | 0.9800 |
C16—H16C | 0.9800 | C42A—H42C | 0.9800 |
C17—H17A | 0.9800 | C42B—H42D | 0.9800 |
C17—H17B | 0.9800 | C42B—H42E | 0.9800 |
C17—H17C | 0.9800 | C42B—H42F | 0.9800 |
C18—C21 | 1.527 (6) | C43A—H43A | 0.9800 |
C18—C20 | 1.544 (6) | C43A—H43B | 0.9800 |
C18—C19 | 1.553 (6) | C43A—H43C | 0.9800 |
C19—H19A | 0.9800 | C43B—H43D | 0.9800 |
C19—H19B | 0.9800 | C43B—H43E | 0.9800 |
C19—H19C | 0.9800 | C43B—H43F | 0.9800 |
C20—H20A | 0.9800 | C44A—H44A | 0.9800 |
C20—H20B | 0.9800 | C44A—H44B | 0.9800 |
C20—H20C | 0.9800 | C44A—H44C | 0.9800 |
C21—H21A | 0.9800 | C44B—H44D | 0.9800 |
C21—H21B | 0.9800 | C44B—H44E | 0.9800 |
C21—H21C | 0.9800 | C44B—H44F | 0.9800 |
C22—C23 | 1.473 (6) | C45—O10 | 1.445 (4) |
C22—O5 | 1.474 (4) | C45—C46 | 1.492 (7) |
C22—H22A | 0.9900 | C45—H45B | 0.9900 |
C22—H22B | 0.9900 | C45—H45A | 0.9900 |
C23—H23C | 0.9800 | C46—H46A | 0.9800 |
C23—H23B | 0.9800 | C46—H46B | 0.9800 |
C23—H23A | 0.9800 | C46—H46C | 0.9800 |
C24—N2 | 1.298 (4) | N1—Mo1 | 2.358 (3) |
C24—C25 | 1.465 (5) | N2—Mo2 | 2.300 (3) |
C24—H24 | 0.9500 | O1—Mo1 | 1.709 (2) |
C25—C30 | 1.425 (5) | O2—Mo1 | 1.783 (2) |
C25—C26 | 1.443 (5) | O3—Mo1 | 1.971 (2) |
C26—O8 | 1.361 (4) | O4—Mo1 | 1.925 (2) |
C26—C27 | 1.423 (4) | O5—Mo1 | 2.416 (2) |
C27—C28 | 1.420 (5) | O6—Mo2 | 1.792 (3) |
C27—C37 | 1.592 (5) | O7—Mo2 | 1.723 (2) |
C28—C29 | 1.441 (5) | O8—Mo2 | 1.957 (2) |
C28—H28 | 0.9500 | O9—Mo2 | 1.956 (3) |
C29—C30 | 1.377 (5) | O10—Mo2 | 2.398 (2) |
| | | |
N1—C1—C2 | 125.8 (3) | C32—C33—C36 | 113.0 (3) |
N1—C1—H1 | 117.1 | C33—C34—H34A | 109.5 |
C2—C1—H1 | 117.1 | C33—C34—H34B | 109.5 |
C3—C2—C1 | 119.5 (3) | H34A—C34—H34B | 109.5 |
C3—C2—C7 | 121.1 (3) | C33—C34—H34C | 109.5 |
C1—C2—C7 | 119.3 (3) | H34A—C34—H34C | 109.5 |
O3—C3—C4 | 119.4 (3) | H34B—C34—H34C | 109.5 |
O3—C3—C2 | 122.3 (3) | C33—C35—H35A | 109.5 |
C4—C3—C2 | 118.3 (3) | C33—C35—H35B | 109.5 |
C3—C4—C5 | 118.0 (3) | H35A—C35—H35B | 109.5 |
C3—C4—C14 | 118.0 (3) | C33—C35—H35C | 109.5 |
C5—C4—C14 | 124.0 (3) | H35A—C35—H35C | 109.5 |
C6—C5—C4 | 125.0 (3) | H35B—C35—H35C | 109.5 |
C6—C5—H5 | 117.5 | C33—C36—H36A | 109.5 |
C4—C5—H5 | 117.5 | C33—C36—H36B | 109.5 |
C7—C6—C5 | 115.3 (3) | H36A—C36—H36B | 109.5 |
C7—C6—C18 | 120.9 (3) | C33—C36—H36C | 109.5 |
C5—C6—C18 | 123.8 (3) | H36A—C36—H36C | 109.5 |
C6—C7—C2 | 121.8 (3) | H36B—C36—H36C | 109.5 |
C6—C7—H7 | 119.1 | C39—C37—C40 | 107.5 (3) |
C2—C7—H7 | 119.1 | C39—C37—C27 | 110.5 (3) |
O4—C8—C9 | 111.7 (3) | C40—C37—C27 | 111.0 (3) |
O4—C8—H8A | 109.3 | C39—C37—C38 | 110.0 (3) |
C9—C8—H8A | 109.3 | C40—C37—C38 | 106.7 (3) |
O4—C8—H8B | 109.3 | C27—C37—C38 | 111.1 (3) |
C9—C8—H8B | 109.3 | C37—C38—H38A | 109.5 |
H8A—C8—H8B | 107.9 | C37—C38—H38B | 109.5 |
N1—C9—C10 | 113.1 (2) | H38A—C38—H38B | 109.5 |
N1—C9—C8 | 105.4 (2) | C37—C38—H38C | 109.5 |
C10—C9—C8 | 114.0 (3) | H38A—C38—H38C | 109.5 |
N1—C9—H9 | 108.0 | H38B—C38—H38C | 109.5 |
C10—C9—H9 | 108.0 | C37—C39—H39A | 109.5 |
C8—C9—H9 | 108.0 | C37—C39—H39B | 109.5 |
C13—C10—C11 | 108.9 (3) | H39A—C39—H39B | 109.5 |
C13—C10—C9 | 108.4 (3) | C37—C39—H39C | 109.5 |
C11—C10—C9 | 111.1 (3) | H39A—C39—H39C | 109.5 |
C13—C10—C12 | 108.0 (3) | H39B—C39—H39C | 109.5 |
C11—C10—C12 | 111.8 (3) | C37—C40—H40A | 109.5 |
C9—C10—C12 | 108.6 (3) | C37—C40—H40B | 109.5 |
C10—C11—H11A | 109.5 | H40A—C40—H40B | 109.5 |
C10—C11—H11B | 109.5 | C37—C40—H40C | 109.5 |
H11A—C11—H11B | 109.5 | H40A—C40—H40C | 109.5 |
C10—C11—H11C | 109.5 | H40B—C40—H40C | 109.5 |
H11A—C11—H11C | 109.5 | C42B—C41—C43A | 128.4 (11) |
H11B—C11—H11C | 109.5 | C42B—C41—C44B | 127.5 (12) |
C10—C12—H12A | 109.5 | C43A—C41—C44B | 47.2 (7) |
C10—C12—H12B | 109.5 | C42B—C41—C42A | 23.1 (9) |
H12A—C12—H12B | 109.5 | C43A—C41—C42A | 113.3 (8) |
C10—C12—H12C | 109.5 | C44B—C41—C42A | 134.1 (8) |
H12A—C12—H12C | 109.5 | C42B—C41—C29 | 115.6 (9) |
H12B—C12—H12C | 109.5 | C43A—C41—C29 | 110.0 (5) |
C10—C13—H13A | 109.5 | C44B—C41—C29 | 110.5 (6) |
C10—C13—H13B | 109.5 | C42A—C41—C29 | 115.4 (6) |
H13A—C13—H13B | 109.5 | C42B—C41—C44A | 78.8 (14) |
C10—C13—H13C | 109.5 | C43A—C41—C44A | 107.8 (5) |
H13A—C13—H13C | 109.5 | C44B—C41—C44A | 63.1 (7) |
H13B—C13—H13C | 109.5 | C42A—C41—C44A | 100.4 (8) |
C17—C14—C15 | 107.9 (3) | C29—C41—C44A | 109.3 (4) |
C17—C14—C4 | 109.9 (3) | C42B—C41—C43B | 102.5 (15) |
C15—C14—C4 | 110.1 (3) | C43A—C41—C43B | 47.9 (5) |
C17—C14—C16 | 110.1 (3) | C44B—C41—C43B | 95.1 (8) |
C15—C14—C16 | 106.7 (3) | C42A—C41—C43B | 79.7 (9) |
C4—C14—C16 | 112.0 (3) | C29—C41—C43B | 97.2 (5) |
C14—C15—H15A | 109.5 | C44A—C41—C43B | 150.1 (5) |
C14—C15—H15B | 109.5 | C41—C42A—H42A | 109.5 |
H15A—C15—H15B | 109.5 | C41—C42A—H42B | 109.5 |
C14—C15—H15C | 109.5 | H42A—C42A—H42B | 109.5 |
H15A—C15—H15C | 109.5 | C41—C42A—H42C | 109.5 |
H15B—C15—H15C | 109.5 | H42A—C42A—H42C | 109.5 |
C14—C16—H16A | 109.5 | H42B—C42A—H42C | 109.5 |
C14—C16—H16B | 109.5 | C41—C42B—H42D | 109.5 |
H16A—C16—H16B | 109.5 | C41—C42B—H42E | 109.5 |
C14—C16—H16C | 109.5 | H42D—C42B—H42E | 109.5 |
H16A—C16—H16C | 109.5 | C41—C42B—H42F | 109.5 |
H16B—C16—H16C | 109.5 | H42D—C42B—H42F | 109.5 |
C14—C17—H17A | 109.5 | H42E—C42B—H42F | 109.5 |
C14—C17—H17B | 109.5 | C41—C43A—H43A | 109.5 |
H17A—C17—H17B | 109.5 | C41—C43A—H43B | 109.5 |
C14—C17—H17C | 109.5 | H43A—C43A—H43B | 109.5 |
H17A—C17—H17C | 109.5 | C41—C43A—H43C | 109.5 |
H17B—C17—H17C | 109.5 | H43A—C43A—H43C | 109.5 |
C21—C18—C20 | 109.4 (4) | H43B—C43A—H43C | 109.5 |
C21—C18—C19 | 106.8 (4) | C41—C43B—H43D | 109.5 |
C20—C18—C19 | 106.6 (3) | C41—C43B—H43E | 109.5 |
C21—C18—C6 | 108.9 (3) | H43D—C43B—H43E | 109.5 |
C20—C18—C6 | 112.5 (3) | C41—C43B—H43F | 109.5 |
C19—C18—C6 | 112.4 (3) | H43D—C43B—H43F | 109.5 |
C18—C19—H19A | 109.5 | H43E—C43B—H43F | 109.5 |
C18—C19—H19B | 109.5 | C41—C44A—H44A | 109.5 |
H19A—C19—H19B | 109.5 | C41—C44A—H44B | 109.5 |
C18—C19—H19C | 109.5 | H44A—C44A—H44B | 109.5 |
H19A—C19—H19C | 109.5 | C41—C44A—H44C | 109.5 |
H19B—C19—H19C | 109.5 | H44A—C44A—H44C | 109.5 |
C18—C20—H20A | 109.5 | H44B—C44A—H44C | 109.5 |
C18—C20—H20B | 109.5 | C41—C44B—H44D | 109.5 |
H20A—C20—H20B | 109.5 | C41—C44B—H44E | 109.5 |
C18—C20—H20C | 109.5 | H44D—C44B—H44E | 109.5 |
H20A—C20—H20C | 109.5 | C41—C44B—H44F | 109.5 |
H20B—C20—H20C | 109.5 | H44D—C44B—H44F | 109.5 |
C18—C21—H21A | 109.5 | H44E—C44B—H44F | 109.5 |
C18—C21—H21B | 109.5 | O10—C45—C46 | 112.9 (4) |
H21A—C21—H21B | 109.5 | O10—C45—H45B | 109.0 |
C18—C21—H21C | 109.5 | C46—C45—H45B | 109.0 |
H21A—C21—H21C | 109.5 | O10—C45—H45A | 109.0 |
H21B—C21—H21C | 109.5 | C46—C45—H45A | 109.0 |
C23—C22—O5 | 111.5 (4) | H45B—C45—H45A | 107.8 |
C23—C22—H22A | 109.3 | C45—C46—H46A | 109.5 |
O5—C22—H22A | 109.3 | C45—C46—H46B | 109.5 |
C23—C22—H22B | 109.3 | H46A—C46—H46B | 109.5 |
O5—C22—H22B | 109.3 | C45—C46—H46C | 109.5 |
H22A—C22—H22B | 108.0 | H46A—C46—H46C | 109.5 |
C22—C23—H23C | 109.5 | H46B—C46—H46C | 109.5 |
C22—C23—H23B | 109.5 | C1—N1—C9 | 117.7 (3) |
H23C—C23—H23B | 109.5 | C1—N1—Mo1 | 130.1 (2) |
C22—C23—H23A | 109.5 | C9—N1—Mo1 | 111.81 (19) |
H23C—C23—H23A | 109.5 | C24—N2—C32 | 118.1 (3) |
H23B—C23—H23A | 109.5 | C24—N2—Mo2 | 124.1 (2) |
N2—C24—C25 | 124.4 (3) | C32—N2—Mo2 | 113.7 (2) |
N2—C24—H24 | 117.8 | C3—O3—Mo1 | 144.7 (2) |
C25—C24—H24 | 117.8 | C8—O4—Mo1 | 121.49 (19) |
C30—C25—C26 | 121.8 (3) | C22—O5—Mo1 | 117.7 (2) |
C30—C25—C24 | 115.6 (3) | C26—O8—Mo2 | 132.9 (2) |
C26—C25—C24 | 122.6 (3) | C31—O9—Mo2 | 115.8 (2) |
O8—C26—C27 | 118.7 (3) | C45—O10—Mo2 | 128.1 (2) |
O8—C26—C25 | 121.7 (3) | O1—Mo1—O2 | 102.43 (12) |
C27—C26—C25 | 119.6 (3) | O1—Mo1—O4 | 98.34 (11) |
C28—C27—C26 | 115.7 (3) | O2—Mo1—O4 | 98.05 (10) |
C28—C27—C37 | 123.3 (3) | O1—Mo1—O3 | 99.67 (11) |
C26—C27—C37 | 121.0 (3) | O2—Mo1—O3 | 100.83 (10) |
C27—C28—C29 | 125.3 (3) | O4—Mo1—O3 | 150.35 (10) |
C27—C28—H28 | 117.3 | O1—Mo1—N1 | 100.63 (11) |
C29—C28—H28 | 117.3 | O2—Mo1—N1 | 156.87 (10) |
C30—C29—C28 | 117.5 (3) | O4—Mo1—N1 | 76.77 (9) |
C30—C29—C41 | 120.6 (4) | O3—Mo1—N1 | 76.89 (9) |
C28—C29—C41 | 122.0 (3) | O1—Mo1—O5 | 175.56 (10) |
C29—C30—C25 | 119.9 (3) | O2—Mo1—O5 | 81.87 (10) |
C29—C30—H30 | 120.0 | O4—Mo1—O5 | 82.02 (9) |
C25—C30—H30 | 120.0 | O3—Mo1—O5 | 78.28 (9) |
O9—C31—C32 | 110.8 (3) | N1—Mo1—O5 | 75.11 (9) |
O9—C31—H31A | 109.5 | O7—Mo2—O6 | 104.82 (12) |
C32—C31—H31A | 109.5 | O7—Mo2—O9 | 100.27 (12) |
O9—C31—H31B | 109.5 | O6—Mo2—O9 | 99.67 (11) |
C32—C31—H31B | 109.5 | O7—Mo2—O8 | 100.95 (11) |
H31A—C31—H31B | 108.1 | O6—Mo2—O8 | 95.68 (11) |
N2—C32—C31 | 104.8 (3) | O9—Mo2—O8 | 149.58 (10) |
N2—C32—C33 | 113.5 (3) | O7—Mo2—N2 | 158.67 (11) |
C31—C32—C33 | 112.0 (3) | O6—Mo2—N2 | 96.18 (11) |
N2—C32—H32 | 108.8 | O9—Mo2—N2 | 72.13 (10) |
C31—C32—H32 | 108.8 | O8—Mo2—N2 | 80.26 (10) |
C33—C32—H32 | 108.8 | O7—Mo2—O10 | 83.16 (10) |
C34—C33—C35 | 108.2 (3) | O6—Mo2—O10 | 171.93 (10) |
C34—C33—C32 | 109.5 (3) | O9—Mo2—O10 | 77.37 (9) |
C35—C33—C32 | 106.0 (3) | O8—Mo2—O10 | 83.80 (9) |
C34—C33—C36 | 108.8 (3) | N2—Mo2—O10 | 75.78 (9) |
C35—C33—C36 | 111.3 (3) | | |
| | | |
N1—C1—C2—C3 | −10.3 (5) | C30—C29—C41—C42A | 4.5 (11) |
N1—C1—C2—C7 | 171.2 (3) | C28—C29—C41—C42A | −175.1 (9) |
C1—C2—C3—O3 | 6.1 (4) | C30—C29—C41—C44A | 116.7 (5) |
C7—C2—C3—O3 | −175.5 (3) | C28—C29—C41—C44A | −62.9 (5) |
C1—C2—C3—C4 | −173.2 (3) | C30—C29—C41—C43B | −77.5 (6) |
C7—C2—C3—C4 | 5.2 (4) | C28—C29—C41—C43B | 102.9 (6) |
O3—C3—C4—C5 | 173.7 (3) | C2—C1—N1—C9 | 178.0 (3) |
C2—C3—C4—C5 | −7.0 (4) | C2—C1—N1—Mo1 | 6.2 (5) |
O3—C3—C4—C14 | −6.2 (4) | C10—C9—N1—C1 | 84.7 (3) |
C2—C3—C4—C14 | 173.1 (3) | C8—C9—N1—C1 | −150.1 (3) |
C3—C4—C5—C6 | 2.8 (5) | C10—C9—N1—Mo1 | −102.1 (2) |
C14—C4—C5—C6 | −177.3 (3) | C8—C9—N1—Mo1 | 23.1 (3) |
C4—C5—C6—C7 | 3.5 (5) | C25—C24—N2—C32 | 175.9 (3) |
C4—C5—C6—C18 | −177.4 (3) | C25—C24—N2—Mo2 | 20.2 (4) |
C5—C6—C7—C2 | −5.4 (4) | C31—C32—N2—C24 | −155.5 (3) |
C18—C6—C7—C2 | 175.4 (3) | C33—C32—N2—C24 | 82.0 (4) |
C3—C2—C7—C6 | 1.4 (5) | C31—C32—N2—Mo2 | 2.6 (3) |
C1—C2—C7—C6 | 179.8 (3) | C33—C32—N2—Mo2 | −119.9 (2) |
O4—C8—C9—N1 | −37.3 (3) | C4—C3—O3—Mo1 | −176.8 (2) |
O4—C8—C9—C10 | 87.3 (3) | C2—C3—O3—Mo1 | 3.9 (5) |
N1—C9—C10—C13 | 178.3 (3) | C9—C8—O4—Mo1 | 38.7 (3) |
C8—C9—C10—C13 | 57.9 (3) | C23—C22—O5—Mo1 | 111.3 (4) |
N1—C9—C10—C11 | 58.7 (4) | C27—C26—O8—Mo2 | 150.9 (3) |
C8—C9—C10—C11 | −61.7 (3) | C25—C26—O8—Mo2 | −30.4 (5) |
N1—C9—C10—C12 | −64.6 (3) | C32—C31—O9—Mo2 | −55.7 (3) |
C8—C9—C10—C12 | 175.0 (3) | C46—C45—O10—Mo2 | −92.4 (4) |
C3—C4—C14—C17 | −174.4 (3) | C8—O4—Mo1—O1 | −117.8 (2) |
C5—C4—C14—C17 | 5.7 (4) | C8—O4—Mo1—O2 | 138.3 (2) |
C3—C4—C14—C15 | −55.7 (4) | C8—O4—Mo1—O3 | 9.1 (4) |
C5—C4—C14—C15 | 124.4 (3) | C8—O4—Mo1—N1 | −18.7 (2) |
C3—C4—C14—C16 | 62.9 (4) | C8—O4—Mo1—O5 | 57.8 (2) |
C5—C4—C14—C16 | −117.0 (3) | C3—O3—Mo1—O1 | 92.4 (4) |
C7—C6—C18—C21 | −58.1 (5) | C3—O3—Mo1—O2 | −162.8 (3) |
C5—C6—C18—C21 | 122.8 (4) | C3—O3—Mo1—O4 | −34.2 (5) |
C7—C6—C18—C20 | 63.4 (5) | C3—O3—Mo1—N1 | −6.3 (3) |
C5—C6—C18—C20 | −115.7 (4) | C3—O3—Mo1—O5 | −83.6 (4) |
C7—C6—C18—C19 | −176.3 (3) | C1—N1—Mo1—O1 | −96.7 (3) |
C5—C6—C18—C19 | 4.6 (5) | C9—N1—Mo1—O1 | 91.2 (2) |
N2—C24—C25—C30 | −174.9 (3) | C1—N1—Mo1—O2 | 87.8 (4) |
N2—C24—C25—C26 | 5.0 (5) | C9—N1—Mo1—O2 | −84.4 (3) |
C30—C25—C26—O8 | 175.9 (3) | C1—N1—Mo1—O4 | 167.1 (3) |
C24—C25—C26—O8 | −4.0 (5) | C9—N1—Mo1—O4 | −4.98 (19) |
C30—C25—C26—C27 | −5.4 (5) | C1—N1—Mo1—O3 | 0.9 (3) |
C24—C25—C26—C27 | 174.7 (3) | C9—N1—Mo1—O3 | −171.3 (2) |
O8—C26—C27—C28 | −175.7 (3) | C1—N1—Mo1—O5 | 82.0 (3) |
C25—C26—C27—C28 | 5.6 (5) | C9—N1—Mo1—O5 | −90.1 (2) |
O8—C26—C27—C37 | 5.0 (5) | C22—O5—Mo1—O1 | 153.0 (13) |
C25—C26—C27—C37 | −173.7 (3) | C22—O5—Mo1—O2 | −41.3 (2) |
C26—C27—C28—C29 | −2.4 (6) | C22—O5—Mo1—O4 | 58.0 (2) |
C37—C27—C28—C29 | 176.9 (4) | C22—O5—Mo1—O3 | −144.2 (2) |
C27—C28—C29—C30 | −1.5 (6) | C22—O5—Mo1—N1 | 136.4 (2) |
C27—C28—C29—C41 | 178.1 (4) | C31—O9—Mo2—O7 | −158.5 (2) |
C28—C29—C30—C25 | 2.0 (6) | C31—O9—Mo2—O6 | −51.4 (2) |
C41—C29—C30—C25 | −177.6 (4) | C31—O9—Mo2—O8 | 67.9 (3) |
C26—C25—C30—C29 | 1.4 (5) | C31—O9—Mo2—N2 | 42.1 (2) |
C24—C25—C30—C29 | −178.7 (3) | C31—O9—Mo2—O10 | 121.0 (2) |
O9—C31—C32—N2 | 28.4 (4) | C26—O8—Mo2—O7 | −118.4 (3) |
O9—C31—C32—C33 | 151.9 (3) | C26—O8—Mo2—O6 | 135.3 (3) |
N2—C32—C33—C34 | −67.2 (4) | C26—O8—Mo2—O9 | 15.1 (4) |
C31—C32—C33—C34 | 174.3 (3) | C26—O8—Mo2—N2 | 40.0 (3) |
N2—C32—C33—C35 | 176.3 (3) | C26—O8—Mo2—O10 | −36.6 (3) |
C31—C32—C33—C35 | 57.9 (4) | C24—N2—Mo2—O7 | 61.4 (4) |
N2—C32—C33—C36 | 54.2 (4) | C32—N2—Mo2—O7 | −95.3 (4) |
C31—C32—C33—C36 | −64.2 (4) | C24—N2—Mo2—O6 | −128.5 (3) |
C28—C27—C37—C39 | 120.0 (4) | C32—N2—Mo2—O6 | 74.8 (2) |
C26—C27—C37—C39 | −60.8 (4) | C24—N2—Mo2—O9 | 133.3 (3) |
C28—C27—C37—C40 | 0.8 (5) | C32—N2—Mo2—O9 | −23.4 (2) |
C26—C27—C37—C40 | −180.0 (4) | C24—N2—Mo2—O8 | −33.8 (3) |
C28—C27—C37—C38 | −117.7 (4) | C32—N2—Mo2—O8 | 169.5 (2) |
C26—C27—C37—C38 | 61.5 (5) | C24—N2—Mo2—O10 | 52.2 (3) |
C30—C29—C41—C42B | 30.1 (17) | C32—N2—Mo2—O10 | −104.4 (2) |
C28—C29—C41—C42B | −149.5 (16) | C45—O10—Mo2—O7 | 42.9 (3) |
C30—C29—C41—C43A | −125.2 (5) | C45—O10—Mo2—O6 | −145.7 (7) |
C28—C29—C41—C43A | 55.2 (6) | C45—O10—Mo2—O9 | 145.1 (3) |
C30—C29—C41—C44B | −175.7 (8) | C45—O10—Mo2—O8 | −58.9 (3) |
C28—C29—C41—C44B | 4.7 (9) | C45—O10—Mo2—N2 | −140.4 (3) |
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