(C)-(2,4-Di-tert-butyl-6-{[(2S)-3,3-dimethyl-1-oxido-2-but­yl]imino­meth­yl}phenolato)ethanol-cis-dioxomolybdenum(VI) at 100 K

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.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](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

---

Computing details

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-{[(2S)-3,3-dimethyl-1-oxido-2- butyl]iminomethyl}phenolato)ethanol-cis-dioxomolybdenum(VI)

Crystal data

[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) Å^3	Prism, yellow
Z = 8	0.40 × 0.36 × 0.32 mm

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.033	H-atom parameters constrained
wR(F^2) = 0.081	w = 1/[σ^2(Fo^2) + (0.0315P)^2 + 6.7957P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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)