Single-crystal-to-single-crystal E → Z isomerization of tiglic acid in a supramolecular framework

The single-crystal-to-single-crystal E → Z photoisomerization of tiglic acid (2,3-dimethylacrylic acid) occurs in the supramolecular crystals CECR–HTA·2MeOH·1.5H₂O (1) (where HTA = tiglic acid, CECR = C-ethylcalix[4]resorcinarene) with the preservation of the crystal lattice, indicating the `scaffolding effect' of the molecular framework, which holds the crystal together notwithstanding the change in shape of the embedded guest molecules. A photostationary state is reached at a concentration of ca 30% of the Z isomers. A kinetic analysis shows the Z → E back-reaction to proceed with a larger rate constant than the E → Z isomerization.

Computing details

For all compounds, data collection: Bruker APEXII; cell refinement: Bruker APEXII; data reduction: Bruker SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.

(CECR-HTA-2MeOH-1.5H2O@200k)

Crystal data

C43H59O13.50	F(000) = 850
Mr = 791.90	Dx = 1.257 Mg m^−3
Triclinic, P1	Melting point: not measured K
a = 11.3467 (14) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.1629 (18) Å	Cell parameters from 865 reflections
c = 14.8100 (19) Å	θ = 2.5–25°
α = 108.886 (4)°	µ = 0.09 mm^−1
β = 109.437 (4)°	T = 200 K
γ = 92.483 (4)°	Block, pale yellow
V = 2092.9 (5) Å^3	0.14 × 0.10 × 0.08 mm
Z = 2

Data collection

CCD area detector diffractometer	7230 independent reflections
Radiation source: fine-focus sealed tube	4698 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
phi and ω scans	θmax = 25.0°, θmin = 1.9°
Absorption correction: empirical (using intensity measurements) Blessing, R. (1995) Acta Crystallogr., A51, 33-38	h = −13→13
Tmin = 0.987, Tmax = 0.993	k = −16→15
14548 measured reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.072	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.219	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.1228P)^2 + 0.8046P] where P = (Fo^2 + 2Fc^2)/3
7230 reflections	(Δ/σ)max < 0.001
523 parameters	Δρmax = 0.78 e Å^−3
18 restraints	Δρmin = −0.44 e Å^−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)
O1	−0.2332 (2)	0.46448 (17)	−0.05463 (18)	0.0342 (6)
O2	0.1340 (2)	0.46745 (17)	0.22049 (19)	0.0383 (6)
O3	0.2614 (2)	0.40897 (17)	0.39493 (17)	0.0339 (6)
O4	0.0100 (2)	0.36441 (19)	0.57901 (17)	0.0396 (6)
O5	−0.2392 (2)	0.39128 (17)	0.51725 (17)	0.0334 (6)
O6	−0.6188 (2)	0.39090 (17)	0.25489 (17)	0.0334 (6)
O7	−0.7338 (2)	0.34660 (17)	0.04919 (18)	0.0341 (6)
O8	−0.4913 (2)	0.39190 (18)	−0.15083 (18)	0.0367 (6)
C1	−0.2073 (3)	0.3098 (2)	−0.0169 (2)	0.0257 (7)
C2	−0.1650 (3)	0.4116 (2)	0.0032 (2)	0.0282 (7)
C3	−0.0525 (3)	0.4647 (2)	0.0814 (3)	0.0294 (7)
H3A	−0.0267	0.5338	0.0933	0.035*
C4	0.0228 (3)	0.4178 (2)	0.1425 (2)	0.0293 (7)
C5	−0.0140 (3)	0.3160 (2)	0.1253 (2)	0.0248 (7)
C6	−0.1287 (3)	0.2651 (2)	0.0458 (2)	0.0252 (7)
H6A	−0.1546	0.1960	0.0339	0.030*
C7	0.0704 (3)	0.2653 (2)	0.1917 (2)	0.0260 (7)
H7A	0.1597	0.2935	0.2056	0.031*
C8	0.0565 (3)	0.2939 (2)	0.2965 (2)	0.0257 (7)
C9	0.1477 (3)	0.3594 (2)	0.3874 (2)	0.0284 (7)
C10	0.1303 (3)	0.3828 (2)	0.4804 (2)	0.0313 (8)
H10A	0.1930	0.4290	0.5416	0.038*
C11	0.0208 (3)	0.3382 (3)	0.4835 (2)	0.0309 (8)
C12	−0.0715 (3)	0.2697 (2)	0.3956 (2)	0.0268 (7)
C13	−0.0522 (3)	0.2510 (2)	0.3040 (2)	0.0262 (7)
H13A	−0.1164	0.2064	0.2426	0.031*
C14	−0.1886 (3)	0.2129 (2)	0.3984 (2)	0.0287 (7)
H14A	−0.1735	0.2273	0.4724	0.034*
C15	−0.3055 (3)	0.2558 (2)	0.3569 (2)	0.0249 (7)
C16	−0.3264 (3)	0.3463 (2)	0.4191 (2)	0.0266 (7)
C17	−0.4318 (3)	0.3888 (2)	0.3830 (2)	0.0289 (7)
H17A	−0.4453	0.4498	0.4266	0.035*
C18	−0.5170 (3)	0.3425 (2)	0.2836 (3)	0.0272 (7)
C19	−0.5003 (3)	0.2520 (2)	0.2178 (2)	0.0249 (7)
C20	−0.3945 (3)	0.2114 (2)	0.2574 (2)	0.0252 (7)
H20A	−0.3819	0.1497	0.2142	0.030*
C21	−0.5938 (3)	0.2023 (2)	0.1081 (2)	0.0253 (7)
H21A	−0.6794	0.2150	0.1095	0.030*
C22	−0.5673 (3)	0.2532 (2)	0.0383 (2)	0.0248 (7)
C23	−0.6389 (3)	0.3230 (2)	0.0100 (2)	0.0270 (7)
C24	−0.6165 (3)	0.3693 (2)	−0.0536 (3)	0.0309 (8)
H24A	−0.6673	0.4164	−0.0725	0.037*
C25	−0.5182 (3)	0.3457 (2)	−0.0893 (2)	0.0291 (7)
C26	−0.4425 (3)	0.2775 (2)	−0.0629 (2)	0.0255 (7)
C27	−0.4699 (3)	0.2325 (2)	0.0009 (2)	0.0248 (7)
H27A	−0.4193	0.1852	0.0197	0.030*
C28	−0.3337 (3)	0.2529 (2)	−0.1012 (2)	0.0277 (7)
H28A	−0.3462	0.2799	−0.1578	0.033*
C29	0.0549 (3)	0.1498 (2)	0.1392 (3)	0.0314 (8)
H29A	−0.0307	0.1183	0.1284	0.038*
H29B	0.0612	0.1347	0.0711	0.038*
C30	0.1535 (4)	0.1027 (3)	0.2011 (3)	0.0449 (9)
H30A	0.2386	0.1364	0.2159	0.067*
H30B	0.1437	0.0305	0.1616	0.067*
H30C	0.1417	0.1109	0.2657	0.067*
C31	−0.2009 (3)	0.0981 (3)	0.3487 (3)	0.0361 (8)
H31A	−0.2800	0.0647	0.3478	0.043*
H31B	−0.2070	0.0809	0.2768	0.043*
C32	−0.0885 (4)	0.0576 (3)	0.4058 (4)	0.0585 (12)
H32A	−0.0101	0.0894	0.4056	0.088*
H32B	−0.1001	−0.0159	0.3716	0.088*
H32C	−0.0830	0.0734	0.4767	0.088*
C33	−0.6024 (3)	0.0867 (2)	0.0650 (3)	0.0294 (7)
H33A	−0.5215	0.0711	0.0568	0.035*
H33B	−0.6138	0.0582	0.1150	0.035*
C34	−0.7103 (4)	0.0358 (3)	−0.0373 (3)	0.0417 (9)
H34A	−0.7910	0.0495	−0.0294	0.063*
H34B	−0.7110	−0.0374	−0.0609	0.063*
H34C	−0.6987	0.0625	−0.0877	0.063*
C35	−0.3378 (3)	0.1391 (2)	−0.1478 (3)	0.0316 (8)
H35A	−0.2651	0.1274	−0.1704	0.038*
H35B	−0.3283	0.1094	−0.0943	0.038*
C36	−0.4596 (4)	0.0851 (3)	−0.2385 (3)	0.0450 (9)
H36A	−0.5315	0.0911	−0.2155	0.067*
H36B	−0.4543	0.0134	−0.2678	0.067*
H36C	−0.4716	0.1160	−0.2907	0.067*
O1S	0.0032 (4)	0.8416 (4)	0.2508 (4)	0.1019 (13)
H1S	−0.0504	0.7932	0.2602	0.153*
C1S	−0.0288 (6)	0.8037 (5)	0.1485 (5)	0.098 (2)
H1S1	0.0147	0.8493	0.1276	0.147*
H1S2	−0.1207	0.7972	0.1149	0.147*
H1S3	−0.0037	0.7370	0.1284	0.147*
O2S	0.8518 (4)	0.7362 (5)	0.3045 (4)	0.1189 (17)
H2S	0.9073	0.7074	0.3490	0.178*
C2S	0.7661 (6)	0.7790 (6)	0.3497 (6)	0.105 (2)
H2S1	0.8132	0.8316	0.4168	0.158*
H2S2	0.7171	0.7262	0.3584	0.158*
H2S3	0.7084	0.8090	0.3053	0.158*
O1W	0.2558 (4)	0.5515 (3)	0.7716 (3)	0.0472 (11)	0.60
H1WA	0.1900	0.5022	0.7213	0.071*	0.60
H1WB	0.2435	0.5851	0.8319	0.071*	0.60
O2W	0.3127 (10)	0.4692 (6)	0.7567 (5)	0.124 (4)	0.60
H2WA	0.2658	0.4102	0.7368	0.187*	0.60
H2WB	0.3172	0.4875	0.7030	0.187*	0.60
O3W	0.3713 (7)	0.5325 (6)	0.8288 (7)	0.047 (2)	0.30
H3WA	0.2922	0.5217	0.8325	0.070*	0.30
H3WB	0.3724	0.5583	0.7791	0.070*	0.30
H1O	−0.3158	0.4367	−0.1016	0.070*
H2O	0.1527	0.5357	0.2269	0.070*
H3O	0.2676	0.3926	0.3303	0.070*
H4O	−0.0713	0.3816	0.5741	0.070*
H5O	−0.2477	0.4595	0.5497	0.070*
H6O	−0.6561	0.3735	0.1835	0.070*
H7O	−0.7703	0.3941	0.0215	0.070*
H8O	−0.5697	0.3787	−0.2036	0.070*
O9	0.1931 (4)	0.6731 (2)	0.2666 (2)	0.0700 (9)
O10	0.2268 (4)	0.8366 (3)	0.3589 (3)	0.0871 (12)
H10O	0.1514	0.8278	0.3006	0.131*
C41	0.2644 (5)	0.7480 (3)	0.3384 (3)	0.0550 (12)
C42	0.3932 (4)	0.7459 (3)	0.4036 (3)	0.0533 (11)
C43	0.4584 (5)	0.8289 (4)	0.4851 (4)	0.0740 (15)
H43A	0.4202	0.8879	0.4955	0.089*
C44	0.5875 (6)	0.8348 (6)	0.5607 (5)	0.107 (2)
H44A	0.5802	0.8327	0.6241	0.161*
H44B	0.6412	0.8982	0.5756	0.161*
H44C	0.6255	0.7773	0.5317	0.161*
C45	0.4399 (5)	0.6482 (4)	0.3743 (4)	0.0644 (13)
H45A	0.4796	0.6463	0.3244	0.097*
H45B	0.3685	0.5921	0.3438	0.097*
H45C	0.5023	0.6419	0.4354	0.097*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0394 (14)	0.0292 (13)	0.0426 (14)	0.0098 (10)	0.0186 (11)	0.0198 (11)
O2	0.0369 (14)	0.0256 (12)	0.0460 (15)	−0.0032 (10)	0.0094 (12)	0.0119 (11)
O3	0.0316 (13)	0.0363 (13)	0.0312 (12)	−0.0015 (10)	0.0174 (10)	0.0037 (10)
O4	0.0418 (14)	0.0492 (15)	0.0261 (12)	0.0005 (12)	0.0182 (11)	0.0064 (11)
O5	0.0388 (13)	0.0289 (12)	0.0298 (13)	0.0026 (10)	0.0164 (11)	0.0036 (10)
O6	0.0336 (13)	0.0298 (13)	0.0372 (13)	0.0132 (10)	0.0180 (11)	0.0064 (10)
O7	0.0399 (14)	0.0311 (13)	0.0483 (15)	0.0144 (10)	0.0317 (12)	0.0186 (11)
O8	0.0448 (14)	0.0419 (14)	0.0420 (14)	0.0126 (11)	0.0276 (12)	0.0257 (12)
C1	0.0332 (18)	0.0227 (16)	0.0271 (16)	0.0068 (13)	0.0201 (14)	0.0069 (13)
C2	0.0375 (19)	0.0254 (17)	0.0333 (18)	0.0109 (14)	0.0239 (15)	0.0134 (14)
C3	0.0336 (18)	0.0228 (16)	0.0364 (18)	0.0014 (14)	0.0174 (15)	0.0123 (14)
C4	0.0336 (18)	0.0264 (17)	0.0329 (18)	0.0046 (14)	0.0193 (15)	0.0097 (14)
C5	0.0284 (17)	0.0241 (16)	0.0254 (16)	0.0053 (13)	0.0157 (14)	0.0071 (13)
C6	0.0310 (17)	0.0212 (16)	0.0300 (17)	0.0055 (13)	0.0201 (14)	0.0083 (13)
C7	0.0290 (17)	0.0223 (16)	0.0289 (17)	0.0034 (13)	0.0156 (14)	0.0071 (13)
C8	0.0314 (17)	0.0208 (16)	0.0302 (17)	0.0083 (13)	0.0177 (14)	0.0089 (13)
C9	0.0256 (16)	0.0281 (17)	0.0341 (18)	0.0034 (13)	0.0163 (14)	0.0088 (14)
C10	0.0339 (18)	0.0286 (18)	0.0265 (17)	0.0017 (14)	0.0123 (14)	0.0031 (14)
C11	0.0365 (19)	0.0348 (19)	0.0275 (17)	0.0079 (15)	0.0197 (15)	0.0103 (14)
C12	0.0333 (18)	0.0239 (16)	0.0298 (17)	0.0079 (14)	0.0169 (14)	0.0122 (14)
C13	0.0286 (17)	0.0242 (16)	0.0262 (16)	0.0045 (13)	0.0121 (14)	0.0074 (13)
C14	0.0358 (18)	0.0276 (17)	0.0270 (17)	0.0027 (14)	0.0170 (15)	0.0102 (14)
C15	0.0325 (17)	0.0210 (16)	0.0277 (17)	0.0034 (13)	0.0190 (14)	0.0089 (13)
C16	0.0307 (17)	0.0257 (16)	0.0255 (16)	−0.0002 (14)	0.0164 (14)	0.0062 (13)
C17	0.0345 (18)	0.0235 (16)	0.0314 (18)	0.0059 (14)	0.0212 (15)	0.0037 (14)
C18	0.0320 (18)	0.0234 (16)	0.0369 (18)	0.0076 (14)	0.0242 (15)	0.0121 (14)
C19	0.0331 (18)	0.0210 (16)	0.0278 (16)	0.0047 (13)	0.0199 (14)	0.0086 (13)
C20	0.0351 (18)	0.0179 (15)	0.0299 (17)	0.0055 (13)	0.0213 (15)	0.0079 (13)
C21	0.0285 (17)	0.0221 (16)	0.0302 (17)	0.0031 (13)	0.0180 (14)	0.0080 (13)
C22	0.0316 (17)	0.0173 (15)	0.0265 (16)	0.0005 (13)	0.0157 (14)	0.0044 (13)
C23	0.0316 (17)	0.0201 (16)	0.0331 (18)	0.0058 (13)	0.0188 (15)	0.0071 (14)
C24	0.0377 (19)	0.0280 (17)	0.0361 (19)	0.0130 (15)	0.0193 (16)	0.0161 (15)
C25	0.0401 (19)	0.0253 (17)	0.0281 (17)	0.0057 (14)	0.0180 (15)	0.0119 (14)
C26	0.0310 (17)	0.0201 (16)	0.0248 (16)	0.0004 (13)	0.0138 (14)	0.0043 (13)
C27	0.0298 (17)	0.0197 (15)	0.0247 (16)	0.0041 (13)	0.0128 (13)	0.0048 (13)
C28	0.0382 (19)	0.0271 (17)	0.0269 (17)	0.0091 (14)	0.0202 (15)	0.0123 (14)
C29	0.0398 (19)	0.0240 (17)	0.0307 (18)	0.0071 (14)	0.0169 (15)	0.0059 (14)
C30	0.056 (2)	0.035 (2)	0.053 (2)	0.0175 (18)	0.028 (2)	0.0179 (18)
C31	0.042 (2)	0.0271 (18)	0.041 (2)	0.0055 (15)	0.0171 (17)	0.0129 (16)
C32	0.066 (3)	0.040 (2)	0.066 (3)	0.015 (2)	0.015 (2)	0.024 (2)
C33	0.0373 (19)	0.0216 (16)	0.0343 (18)	0.0049 (14)	0.0208 (15)	0.0085 (14)
C34	0.047 (2)	0.0293 (19)	0.042 (2)	0.0011 (16)	0.0168 (18)	0.0045 (16)
C35	0.0378 (19)	0.0282 (18)	0.0312 (18)	0.0056 (14)	0.0199 (15)	0.0062 (14)
C36	0.049 (2)	0.037 (2)	0.041 (2)	0.0030 (17)	0.0151 (18)	0.0051 (17)
O1S	0.091 (3)	0.112 (3)	0.104 (4)	0.023 (2)	0.040 (3)	0.036 (3)
C1S	0.077 (4)	0.108 (5)	0.083 (5)	−0.001 (4)	0.003 (3)	0.030 (4)
O2S	0.084 (3)	0.189 (5)	0.117 (4)	0.039 (3)	0.035 (3)	0.099 (4)
C2S	0.072 (4)	0.106 (5)	0.126 (6)	−0.003 (4)	0.023 (4)	0.043 (4)
O1W	0.055 (3)	0.049 (3)	0.039 (2)	0.009 (2)	0.029 (2)	0.004 (2)
O2W	0.211 (9)	0.096 (5)	0.057 (4)	0.113 (6)	0.027 (5)	0.028 (4)
O3W	0.022 (4)	0.034 (5)	0.070 (7)	0.009 (4)	−0.006 (4)	0.024 (5)
O9	0.097 (3)	0.0436 (18)	0.0571 (19)	−0.0041 (17)	0.0191 (18)	0.0143 (16)
O10	0.095 (3)	0.048 (2)	0.110 (3)	0.0156 (18)	0.043 (2)	0.0123 (19)
C41	0.087 (3)	0.035 (2)	0.056 (3)	0.002 (2)	0.045 (3)	0.015 (2)
C42	0.062 (3)	0.058 (3)	0.044 (2)	−0.002 (2)	0.027 (2)	0.017 (2)
C43	0.086 (4)	0.065 (3)	0.062 (3)	0.005 (3)	0.030 (3)	0.009 (3)
C44	0.084 (4)	0.112 (5)	0.080 (4)	0.004 (4)	0.001 (3)	0.006 (4)
C45	0.080 (3)	0.072 (3)	0.055 (3)	0.013 (3)	0.042 (3)	0.022 (2)

Geometric parameters (Å, º)

O1—C2	1.385 (4)	C28—C35	1.526 (4)
O1—H1O	0.9354	C28—H28A	1.0000
O2—C4	1.360 (4)	C29—C30	1.521 (5)
O2—H2O	0.9479	C29—H29A	0.9900
O3—C9	1.394 (4)	C29—H29B	0.9900
O3—H3O	0.9369	C30—H30A	0.9800
O4—C11	1.391 (4)	C30—H30B	0.9800
O4—H4O	0.9501	C30—H30C	0.9800
O5—C16	1.373 (4)	C31—C32	1.526 (6)
O5—H5O	0.9554	C31—H31A	0.9900
O6—C18	1.384 (4)	C31—H31B	0.9900
O6—H6O	0.9390	C32—H32A	0.9800
O7—C23	1.389 (4)	C32—H32B	0.9800
O7—H7O	0.9389	C32—H32C	0.9800
O8—C25	1.380 (4)	C33—C34	1.515 (5)
O8—H8O	0.9302	C33—H33A	0.9900
C1—C6	1.393 (5)	C33—H33B	0.9900
C1—C2	1.401 (4)	C34—H34A	0.9800
C1—C28	1.524 (5)	C34—H34B	0.9800
C2—C3	1.380 (5)	C34—H34C	0.9800
C3—C4	1.383 (5)	C35—C36	1.519 (5)
C3—H3A	0.9500	C35—H35A	0.9900
C4—C5	1.400 (4)	C35—H35B	0.9900
C5—C6	1.396 (4)	C36—H36A	0.9800
C5—C7	1.513 (4)	C36—H36B	0.9800
C6—H6A	0.9500	C36—H36C	0.9800
C7—C8	1.537 (4)	O1S—C1S	1.343 (7)
C7—C29	1.540 (4)	O1S—H1S	0.9707
C7—H7A	1.0000	C1S—H1S1	0.9800
C8—C9	1.388 (5)	C1S—H1S2	0.9800
C8—C13	1.404 (4)	C1S—H1S3	0.9800
C9—C10	1.392 (4)	O2S—C2S	1.408 (8)
C10—C11	1.389 (5)	O2S—H2S	0.9578
C10—H10A	0.9500	C2S—H2S1	0.9800
C11—C12	1.386 (5)	C2S—H2S2	0.9800
C12—C13	1.389 (4)	C2S—H2S3	0.9800
C12—C14	1.543 (4)	O1W—H1WA	0.9209
C13—H13A	0.9500	O1W—H1WB	0.9255
C14—C15	1.509 (5)	O1W—H3WA	1.0849
C14—C31	1.530 (5)	O1W—H3WB	1.2867
C14—H14A	1.0000	O2W—H1WA	1.4696
C15—C20	1.393 (4)	O2W—H2WA	0.8753
C15—C16	1.397 (4)	O2W—H2WB	0.9268
C16—C17	1.388 (5)	O2W—H3WA	1.2321
C17—C18	1.380 (5)	O2W—H3WB	1.2910
C17—H17A	0.9500	O3W—H3WA	0.9260
C18—C19	1.401 (4)	O3W—H3WB	0.9264
C19—C20	1.388 (5)	O9—C41	1.238 (5)
C19—C21	1.518 (4)	O10—C41	1.317 (5)
C20—H20A	0.9500	O10—H10O	0.9600
C21—C22	1.534 (4)	C41—C42	1.467 (7)
C21—C33	1.539 (4)	C42—C43	1.341 (6)
C21—H21A	1.0000	C42—C45	1.487 (7)
C22—C23	1.387 (4)	C43—C44	1.498 (8)
C22—C27	1.394 (4)	C43—H43A	0.9500
C23—C24	1.388 (5)	C44—H44A	0.9800
C24—C25	1.395 (5)	C44—H44B	0.9800
C24—H24A	0.9500	C44—H44C	0.9800
C25—C26	1.384 (5)	C45—H45A	0.9800
C26—C27	1.401 (4)	C45—H45B	0.9800
C26—C28	1.531 (4)	C45—H45C	0.9800
C27—H27A	0.9500
C2—O1—H1O	120.5	C26—C28—H28A	106.6
C4—O2—H2O	112.5	C30—C29—C7	113.0 (3)
C9—O3—H3O	110.9	C30—C29—H29A	109.0
C11—O4—H4O	109.7	C7—C29—H29A	109.0
C16—O5—H5O	113.1	C30—C29—H29B	109.0
C18—O6—H6O	112.8	C7—C29—H29B	109.0
C23—O7—H7O	104.2	H29A—C29—H29B	107.8
C25—O8—H8O	102.0	C29—C30—H30A	109.5
C6—C1—C2	116.2 (3)	C29—C30—H30B	109.5
C6—C1—C28	122.4 (3)	H30A—C30—H30B	109.5
C2—C1—C28	121.4 (3)	C29—C30—H30C	109.5
C3—C2—O1	116.1 (3)	H30A—C30—H30C	109.5
C3—C2—C1	121.9 (3)	H30B—C30—H30C	109.5
O1—C2—C1	121.9 (3)	C32—C31—C14	112.1 (3)
C2—C3—C4	120.3 (3)	C32—C31—H31A	109.2
C2—C3—H3A	119.9	C14—C31—H31A	109.2
C4—C3—H3A	119.9	C32—C31—H31B	109.2
O2—C4—C3	122.2 (3)	C14—C31—H31B	109.2
O2—C4—C5	117.5 (3)	H31A—C31—H31B	107.9
C3—C4—C5	120.4 (3)	C31—C32—H32A	109.5
C6—C5—C4	117.6 (3)	C31—C32—H32B	109.5
C6—C5—C7	122.7 (3)	H32A—C32—H32B	109.5
C4—C5—C7	119.7 (3)	C31—C32—H32C	109.5
C1—C6—C5	123.7 (3)	H32A—C32—H32C	109.5
C1—C6—H6A	118.2	H32B—C32—H32C	109.5
C5—C6—H6A	118.2	C34—C33—C21	113.1 (3)
C5—C7—C8	111.5 (2)	C34—C33—H33A	109.0
C5—C7—C29	114.0 (3)	C21—C33—H33A	109.0
C8—C7—C29	111.7 (3)	C34—C33—H33B	109.0
C5—C7—H7A	106.4	C21—C33—H33B	109.0
C8—C7—H7A	106.4	H33A—C33—H33B	107.8
C29—C7—H7A	106.4	C33—C34—H34A	109.5
C9—C8—C13	116.5 (3)	C33—C34—H34B	109.5
C9—C8—C7	123.7 (3)	H34A—C34—H34B	109.5
C13—C8—C7	119.8 (3)	C33—C34—H34C	109.5
C8—C9—C10	121.4 (3)	H34A—C34—H34C	109.5
C8—C9—O3	124.5 (3)	H34B—C34—H34C	109.5
C10—C9—O3	114.1 (3)	C36—C35—C28	113.3 (3)
C11—C10—C9	119.8 (3)	C36—C35—H35A	108.9
C11—C10—H10A	120.1	C28—C35—H35A	108.9
C9—C10—H10A	120.1	C36—C35—H35B	108.9
C12—C11—C10	121.3 (3)	C28—C35—H35B	108.9
C12—C11—O4	121.9 (3)	H35A—C35—H35B	107.7
C10—C11—O4	116.7 (3)	C35—C36—H36A	109.5
C11—C12—C13	117.0 (3)	C35—C36—H36B	109.5
C11—C12—C14	122.2 (3)	H36A—C36—H36B	109.5
C13—C12—C14	120.7 (3)	C35—C36—H36C	109.5
C12—C13—C8	124.0 (3)	H36A—C36—H36C	109.5
C12—C13—H13A	118.0	H36B—C36—H36C	109.5
C8—C13—H13A	118.0	C1S—O1S—H1S	101.0
C15—C14—C31	114.9 (3)	O1S—C1S—H1S1	109.5
C15—C14—C12	110.5 (3)	O1S—C1S—H1S2	109.5
C31—C14—C12	111.7 (3)	H1S1—C1S—H1S2	109.5
C15—C14—H14A	106.4	O1S—C1S—H1S3	109.5
C31—C14—H14A	106.4	H1S1—C1S—H1S3	109.5
C12—C14—H14A	106.4	H1S2—C1S—H1S3	109.5
C20—C15—C16	117.0 (3)	C2S—O2S—H2S	108.2
C20—C15—C14	123.5 (3)	O2S—C2S—H2S1	109.5
C16—C15—C14	119.5 (3)	O2S—C2S—H2S2	109.5
O5—C16—C17	121.2 (3)	H2S1—C2S—H2S2	109.5
O5—C16—C15	117.7 (3)	O2S—C2S—H2S3	109.5
C17—C16—C15	121.1 (3)	H2S1—C2S—H2S3	109.5
C18—C17—C16	119.9 (3)	H2S2—C2S—H2S3	109.5
C18—C17—H17A	120.0	H1WA—O1W—H1WB	116.3
C16—C17—H17A	120.0	H1WA—O1W—H3WA	104.9
C17—C18—O6	115.5 (3)	H1WB—O1W—H3WA	64.1
C17—C18—C19	121.4 (3)	H1WA—O1W—H3WB	125.6
O6—C18—C19	123.2 (3)	H1WB—O1W—H3WB	114.8
C20—C19—C18	116.8 (3)	H3WA—O1W—H3WB	81.7
C20—C19—C21	122.3 (3)	H1WA—O2W—H2WA	83.8
C18—C19—C21	120.9 (3)	H1WA—O2W—H2WB	77.9
C19—C20—C15	123.8 (3)	H2WA—O2W—H2WB	113.8
C19—C20—H20A	118.1	H1WA—O2W—H3WA	71.7
C15—C20—H20A	118.1	H2WA—O2W—H3WA	104.4
C19—C21—C22	111.1 (2)	H2WB—O2W—H3WA	127.4
C19—C21—C33	113.4 (3)	H1WA—O2W—H3WB	90.9
C22—C21—C33	112.2 (2)	H2WA—O2W—H3WB	174.0
C19—C21—H21A	106.5	H2WB—O2W—H3WB	62.2
C22—C21—H21A	106.5	H3WA—O2W—H3WB	76.2
C33—C21—H21A	106.5	H3WA—O3W—H3WB	114.5
C23—C22—C27	116.8 (3)	C41—O10—H10O	104.6
C23—C22—C21	121.3 (3)	O9—C41—O10	120.0 (5)
C27—C22—C21	121.9 (3)	O9—C41—C42	123.9 (4)
C22—C23—C24	121.9 (3)	O10—C41—C42	116.0 (4)
C22—C23—O7	117.4 (3)	C43—C42—C41	119.2 (5)
C24—C23—O7	120.7 (3)	C43—C42—C45	124.9 (5)
C23—C24—C25	119.1 (3)	C41—C42—C45	115.9 (4)
C23—C24—H24A	120.5	C42—C43—C44	124.3 (5)
C25—C24—H24A	120.5	C42—C43—H43A	117.8
O8—C25—C26	117.6 (3)	C44—C43—H43A	117.8
O8—C25—C24	120.7 (3)	C43—C44—H44A	109.5
C26—C25—C24	121.7 (3)	C43—C44—H44B	109.5
C25—C26—C27	116.9 (3)	H44A—C44—H44B	109.5
C25—C26—C28	121.5 (3)	C43—C44—H44C	109.5
C27—C26—C28	121.7 (3)	H44A—C44—H44C	109.5
C22—C27—C26	123.6 (3)	H44B—C44—H44C	109.5
C22—C27—H27A	118.2	C42—C45—H45A	109.5
C26—C27—H27A	118.2	C42—C45—H45B	109.5
C1—C28—C35	114.0 (3)	H45A—C45—H45B	109.5
C1—C28—C26	110.3 (2)	C42—C45—H45C	109.5
C35—C28—C26	112.2 (3)	H45A—C45—H45C	109.5
C1—C28—H28A	106.6	H45B—C45—H45C	109.5
C35—C28—H28A	106.6
C6—C1—C2—C3	−0.6 (4)	C16—C17—C18—C19	0.7 (5)
C28—C1—C2—C3	177.9 (3)	C17—C18—C19—C20	0.1 (4)
C6—C1—C2—O1	178.9 (3)	O6—C18—C19—C20	−179.3 (3)
C28—C1—C2—O1	−2.5 (4)	C17—C18—C19—C21	−179.2 (3)
O1—C2—C3—C4	−179.2 (3)	O6—C18—C19—C21	1.4 (4)
C1—C2—C3—C4	0.3 (5)	C18—C19—C20—C15	−0.6 (4)
C2—C3—C4—O2	−179.8 (3)	C21—C19—C20—C15	178.7 (3)
C2—C3—C4—C5	0.3 (5)	C16—C15—C20—C19	0.3 (4)
O2—C4—C5—C6	179.5 (3)	C14—C15—C20—C19	−178.1 (3)
C3—C4—C5—C6	−0.6 (4)	C20—C19—C21—C22	−98.8 (3)
O2—C4—C5—C7	−0.9 (4)	C18—C19—C21—C22	80.5 (3)
C3—C4—C5—C7	179.0 (3)	C20—C19—C21—C33	28.8 (4)
C2—C1—C6—C5	0.3 (4)	C18—C19—C21—C33	−152.0 (3)
C28—C1—C6—C5	−178.3 (3)	C19—C21—C22—C23	−100.7 (3)
C4—C5—C6—C1	0.3 (4)	C33—C21—C22—C23	131.1 (3)
C7—C5—C6—C1	−179.3 (3)	C19—C21—C22—C27	78.7 (3)
C6—C5—C7—C8	−101.9 (3)	C33—C21—C22—C27	−49.5 (4)
C4—C5—C7—C8	78.5 (3)	C27—C22—C23—C24	0.9 (5)
C6—C5—C7—C29	25.7 (4)	C21—C22—C23—C24	−179.7 (3)
C4—C5—C7—C29	−153.9 (3)	C27—C22—C23—O7	−178.1 (3)
C5—C7—C8—C9	−106.7 (3)	C21—C22—C23—O7	1.3 (4)
C29—C7—C8—C9	124.5 (3)	C22—C23—C24—C25	−0.6 (5)
C5—C7—C8—C13	74.9 (4)	O7—C23—C24—C25	178.3 (3)
C29—C7—C8—C13	−54.0 (4)	C23—C24—C25—O8	−178.6 (3)
C13—C8—C9—C10	−1.5 (5)	C23—C24—C25—C26	−0.1 (5)
C7—C8—C9—C10	−180.0 (3)	O8—C25—C26—C27	179.0 (3)
C13—C8—C9—O3	180.0 (3)	C24—C25—C26—C27	0.5 (5)
C7—C8—C9—O3	1.5 (5)	O8—C25—C26—C28	−0.7 (4)
C8—C9—C10—C11	1.4 (5)	C24—C25—C26—C28	−179.2 (3)
O3—C9—C10—C11	−179.9 (3)	C23—C22—C27—C26	−0.4 (5)
C9—C10—C11—C12	0.7 (5)	C21—C22—C27—C26	−179.9 (3)
C9—C10—C11—O4	179.6 (3)	C25—C26—C27—C22	−0.3 (5)
C10—C11—C12—C13	−2.7 (5)	C28—C26—C27—C22	179.5 (3)
O4—C11—C12—C13	178.6 (3)	C6—C1—C28—C35	−29.7 (4)
C10—C11—C12—C14	175.0 (3)	C2—C1—C28—C35	151.8 (3)
O4—C11—C12—C14	−3.7 (5)	C6—C1—C28—C26	97.5 (3)
C11—C12—C13—C8	2.7 (5)	C2—C1—C28—C26	−81.0 (3)
C14—C12—C13—C8	−175.0 (3)	C25—C26—C28—C1	101.5 (3)
C9—C8—C13—C12	−0.6 (5)	C27—C26—C28—C1	−78.3 (4)
C7—C8—C13—C12	177.9 (3)	C25—C26—C28—C35	−130.4 (3)
C11—C12—C14—C15	105.9 (3)	C27—C26—C28—C35	49.9 (4)
C13—C12—C14—C15	−76.5 (4)	C5—C7—C29—C30	171.7 (3)
C11—C12—C14—C31	−124.8 (3)	C8—C7—C29—C30	−60.8 (4)
C13—C12—C14—C31	52.8 (4)	C15—C14—C31—C32	−170.4 (3)
C31—C14—C15—C20	−27.6 (4)	C12—C14—C31—C32	62.7 (4)
C12—C14—C15—C20	99.9 (3)	C19—C21—C33—C34	170.7 (3)
C31—C14—C15—C16	154.0 (3)	C22—C21—C33—C34	−62.4 (4)
C12—C14—C15—C16	−78.5 (3)	C1—C28—C35—C36	−174.4 (3)
C20—C15—C16—O5	−179.7 (3)	C26—C28—C35—C36	59.4 (4)
C14—C15—C16—O5	−1.2 (4)	O9—C41—C42—C43	−174.1 (4)
C20—C15—C16—C17	0.5 (4)	O10—C41—C42—C43	7.2 (6)
C14—C15—C16—C17	179.0 (3)	O9—C41—C42—C45	4.3 (6)
O5—C16—C17—C18	179.2 (3)	O10—C41—C42—C45	−174.4 (4)
C15—C16—C17—C18	−1.0 (5)	C41—C42—C43—C44	176.5 (5)
C16—C17—C18—O6	−179.9 (3)	C45—C42—C43—C44	−1.7 (8)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O···O8	0.94	1.88	2.771 (3)	159
O2—H2O···O9	0.95	1.83	2.764 (4)	168
O3—H3O···O6^i	0.94	1.96	2.789 (3)	146
O3—H3O···O2	0.94	2.38	2.907 (3)	115
O4—H4O···O5	0.95	1.84	2.752 (3)	160
O5—H5O···O3^ii	0.96	1.81	2.767 (3)	176
O6—H6O···O7	0.94	1.79	2.725 (3)	176
O7—H7O···O1^iii	0.94	1.90	2.697 (3)	142
O10—H10O···O1S	0.96	1.65	2.528 (6)	151
O1S—H1S···O2S^iv	0.97	1.75	2.697 (7)	164
O2S—H2S···O4^v	0.96	1.78	2.730 (5)	170

Symmetry codes: (i) x+1, y, z; (ii) −x, −y+1, −z+1; (iii) −x−1, −y+1, −z; (iv) x−1, y, z; (v) −x+1, −y+1, −z+1.

(CECR-HTA-2MeOH-1.5H2O@90k)

Crystal data

C43H59O13.50	F(000) = 850
Mr = 791.90	Dx = 1.272 Mg m^−3
Triclinic, P1	Melting point: not measured K
a = 11.2958 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.0716 (3) Å	Cell parameters from 865 reflections
c = 14.7200 (3) Å	θ = 2.5–25°
α = 108.7556 (8)°	µ = 0.09 mm^−1
β = 108.6284 (7)°	T = 90 K
γ = 93.0151 (7)°	Block, pale yellow
V = 2067.74 (7) Å^3	0.14 × 0.10 × 0.08 mm
Z = 2

Data collection

CCD area detector diffractometer	7281 independent reflections
Radiation source: fine-focus sealed tube	6643 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.016
phi and ω scans	θmax = 25.0°, θmin = 1.6°
Absorption correction: empirical (using intensity measurements) Blessing, R. (1995) Acta Crystallogr., A51, 33-38	h = −13→13
Tmin = 0.987, Tmax = 0.993	k = −16→16
27003 measured reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.113	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0601P)^2 + 1.1813P] where P = (Fo^2 + 2Fc^2)/3
7281 reflections	(Δ/σ)max < 0.001
559 parameters	Δρmax = 0.66 e Å^−3
0 restraints	Δρmin = −0.39 e Å^−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)
O1	−0.22998 (10)	0.46677 (8)	−0.05402 (8)	0.0164 (2)
O2	0.13347 (10)	0.47083 (9)	0.22290 (8)	0.0185 (2)
O3	0.26210 (9)	0.40822 (8)	0.39604 (8)	0.0162 (2)
O4	0.00608 (11)	0.36479 (8)	0.58011 (8)	0.0182 (2)
O5	−0.24177 (10)	0.39233 (8)	0.51778 (8)	0.0160 (2)
O6	−0.61956 (10)	0.39039 (8)	0.25631 (8)	0.0155 (2)
O7	−0.73266 (10)	0.34638 (8)	0.05154 (8)	0.0161 (2)
O8	−0.48714 (10)	0.39475 (8)	−0.14894 (8)	0.0170 (2)
C1	−0.20490 (13)	0.31144 (11)	−0.01629 (11)	0.0129 (3)
C2	−0.16318 (13)	0.41400 (11)	0.00394 (11)	0.0137 (3)
C3	−0.05137 (14)	0.46823 (11)	0.08296 (11)	0.0153 (3)
H3A	−0.0255	0.5380	0.0954	0.018*
C4	0.02274 (13)	0.42044 (11)	0.14395 (11)	0.0144 (3)
C5	−0.01374 (13)	0.31731 (11)	0.12612 (11)	0.0129 (3)
C6	−0.12729 (13)	0.26625 (11)	0.04654 (11)	0.0128 (3)
H6A	−0.1535	0.1966	0.0343	0.015*
C7	0.07143 (13)	0.26648 (11)	0.19271 (11)	0.0132 (3)
H7A	0.1608	0.2953	0.2063	0.016*
C8	0.05618 (13)	0.29406 (10)	0.29716 (11)	0.0133 (3)
C9	0.14794 (13)	0.35985 (11)	0.38877 (11)	0.0140 (3)
C10	0.12874 (14)	0.38282 (11)	0.48143 (11)	0.0161 (3)
H10A	0.1914	0.4288	0.5427	0.019*
C11	0.01825 (14)	0.33882 (11)	0.48465 (11)	0.0148 (3)
C12	−0.07410 (13)	0.26938 (11)	0.39647 (11)	0.0137 (3)
C13	−0.05329 (13)	0.25138 (11)	0.30444 (11)	0.0134 (3)
H13A	−0.1175	0.2074	0.2429	0.016*
C14	−0.19080 (13)	0.21275 (11)	0.40005 (11)	0.0139 (3)
H14A	−0.1767	0.2275	0.4742	0.017*
C15	−0.30821 (13)	0.25533 (11)	0.35772 (11)	0.0130 (3)
C16	−0.32885 (13)	0.34673 (11)	0.41999 (11)	0.0136 (3)
C17	−0.43315 (14)	0.38956 (11)	0.38419 (11)	0.0145 (3)
H17A	−0.4465	0.4511	0.4278	0.017*
C18	−0.51847 (13)	0.34234 (11)	0.28426 (11)	0.0130 (3)
C19	−0.50207 (13)	0.25097 (10)	0.21877 (11)	0.0124 (3)
C20	−0.39591 (13)	0.21019 (10)	0.25867 (11)	0.0127 (3)
H20A	−0.3830	0.1481	0.2156	0.015*
C21	−0.59496 (13)	0.20089 (10)	0.10856 (11)	0.0125 (3)
H21A	−0.6810	0.2129	0.1098	0.015*
C22	−0.56706 (13)	0.25221 (10)	0.03865 (11)	0.0127 (3)
C23	−0.63825 (13)	0.32340 (11)	0.01146 (11)	0.0136 (3)
C24	−0.61416 (14)	0.37049 (11)	−0.05192 (11)	0.0153 (3)
H24A	−0.6646	0.4180	−0.0704	0.018*
C25	−0.51578 (14)	0.34771 (11)	−0.08815 (11)	0.0141 (3)
C26	−0.44072 (13)	0.27785 (10)	−0.06230 (10)	0.0128 (3)
C27	−0.46875 (13)	0.23210 (10)	0.00123 (11)	0.0128 (3)
H27A	−0.4182	0.1848	0.0199	0.015*
C28	−0.33086 (13)	0.25458 (11)	−0.10083 (11)	0.0131 (3)
H28A	−0.3423	0.2825	−0.1570	0.016*
C29	0.05522 (14)	0.15027 (11)	0.13877 (11)	0.0153 (3)
H29A	−0.0308	0.1183	0.1277	0.018*
H29B	0.0628	0.1360	0.0706	0.018*
C30	0.15303 (15)	0.10269 (12)	0.20029 (13)	0.0213 (3)
H30A	0.2385	0.1369	0.2150	0.032*
H30B	0.1432	0.0301	0.1605	0.032*
H30C	0.1403	0.1105	0.2650	0.032*
C31	−0.20351 (14)	0.09672 (11)	0.35023 (12)	0.0170 (3)
H31A	−0.2833	0.0629	0.3492	0.020*
H31B	−0.2079	0.0793	0.2784	0.020*
C32	−0.09184 (16)	0.05736 (12)	0.40852 (13)	0.0261 (4)
H32A	−0.0129	0.0895	0.4083	0.039*
H32B	−0.1029	−0.0167	0.3753	0.039*
H32C	−0.0879	0.0739	0.4795	0.039*
C33	−0.60216 (13)	0.08488 (11)	0.06603 (11)	0.0143 (3)
H33A	−0.5208	0.0699	0.0578	0.017*
H33B	−0.6144	0.0559	0.1161	0.017*
C34	−0.70982 (15)	0.03365 (12)	−0.03689 (12)	0.0200 (3)
H34A	−0.7908	0.0474	−0.0290	0.030*
H34B	−0.7110	−0.0401	−0.0606	0.030*
H34C	−0.6969	0.0606	−0.0873	0.030*
C35	−0.33435 (14)	0.13949 (11)	−0.14849 (11)	0.0152 (3)
H35A	−0.2614	0.1284	−0.1717	0.018*
H35B	−0.3253	0.1088	−0.0953	0.018*
C36	−0.45691 (15)	0.08578 (12)	−0.23931 (12)	0.0209 (3)
H36A	−0.5290	0.0920	−0.2157	0.031*
H36B	−0.4526	0.0136	−0.2692	0.031*
H36C	−0.4678	0.1173	−0.2913	0.031*
O1S	0.00003 (12)	0.84570 (10)	0.25216 (10)	0.0340 (3)
H1S	−0.0536	0.7973	0.2616	0.051*
C1S	−0.02719 (18)	0.80817 (15)	0.14516 (14)	0.0345 (4)
H1S1	0.0184	0.8562	0.1270	0.052*
H1S2	−0.1186	0.8004	0.1092	0.052*
H1S3	−0.0003	0.7419	0.1250	0.052*
O2S	0.84865 (13)	0.73058 (12)	0.30161 (11)	0.0437 (4)
H2S	0.9041	0.7018	0.3461	0.066*
C2S	0.76339 (19)	0.77579 (16)	0.34844 (17)	0.0405 (5)
H2S1	0.8115	0.8283	0.4154	0.061*
H2S2	0.7125	0.7234	0.3576	0.061*
H2S3	0.7072	0.8069	0.3046	0.061*
O1W	0.25549 (16)	0.55184 (13)	0.77055 (13)	0.0167 (4)	0.60
H1WA	0.1897	0.5025	0.7203	0.025*	0.60
H1WB	0.2431	0.5854	0.8308	0.025*	0.60
O2W	0.3184 (3)	0.4704 (2)	0.76223 (18)	0.0524 (8)	0.60
H2WA	0.2715	0.4114	0.7423	0.079*	0.60
H2WB	0.3228	0.4887	0.7086	0.079*	0.60
O3W	0.3707 (3)	0.5348 (3)	0.8301 (3)	0.0186 (7)	0.30
H3WA	0.2916	0.5241	0.8338	0.028*	0.30
H3WB	0.3718	0.5607	0.7803	0.028*	0.30
H1O	−0.307 (2)	0.4342 (17)	−0.0913 (17)	0.037 (6)*
H2O	0.149 (2)	0.5311 (18)	0.2284 (17)	0.037 (6)*
H3O	0.265 (2)	0.3996 (16)	0.3375 (18)	0.037 (6)*
H4O	−0.069 (2)	0.3710 (17)	0.5704 (17)	0.041 (6)*
H5O	−0.255 (2)	0.4522 (18)	0.5458 (18)	0.041 (6)*
H6O	−0.655 (2)	0.3713 (16)	0.1877 (18)	0.036 (6)*
H7O	−0.758 (2)	0.3967 (18)	0.0409 (17)	0.037 (6)*
H8O	−0.544 (2)	0.4305 (19)	−0.1672 (18)	0.048 (7)*
O9	0.18977 (12)	0.67752 (9)	0.26827 (9)	0.0284 (3)
O10	0.22897 (13)	0.84265 (9)	0.36301 (10)	0.0312 (3)
H10O	0.145 (2)	0.8388 (17)	0.3177 (17)	0.040 (6)*
C41	0.26148 (16)	0.75158 (12)	0.33918 (12)	0.0216 (3)
C42	0.39046 (16)	0.74682 (12)	0.40423 (12)	0.0221 (3)
C43	0.45669 (17)	0.82825 (14)	0.48710 (13)	0.0287 (4)
H43A	0.4187	0.8875	0.4990	0.034*
C44	0.58458 (19)	0.83480 (16)	0.56256 (15)	0.0391 (5)
H44A	0.5762	0.8326	0.6261	0.059*
H44B	0.6384	0.8988	0.5773	0.059*
H44C	0.6232	0.7772	0.5338	0.059*
C45	0.43718 (17)	0.64779 (13)	0.37251 (13)	0.0260 (4)
H45A	0.4769	0.6470	0.3221	0.039*
H45B	0.3656	0.5912	0.3419	0.039*
H45C	0.4995	0.6406	0.4328	0.039*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0150 (5)	0.0144 (5)	0.0207 (6)	0.0037 (4)	0.0043 (4)	0.0094 (4)
O2	0.0157 (5)	0.0141 (5)	0.0205 (6)	−0.0012 (4)	0.0005 (4)	0.0058 (4)
O3	0.0135 (5)	0.0184 (5)	0.0143 (5)	−0.0006 (4)	0.0057 (4)	0.0025 (4)
O4	0.0153 (6)	0.0256 (6)	0.0127 (5)	0.0024 (4)	0.0058 (4)	0.0047 (4)
O5	0.0156 (5)	0.0152 (5)	0.0126 (5)	0.0026 (4)	0.0029 (4)	0.0013 (4)
O6	0.0142 (5)	0.0160 (5)	0.0152 (5)	0.0066 (4)	0.0047 (4)	0.0040 (4)
O7	0.0165 (5)	0.0163 (5)	0.0213 (6)	0.0080 (4)	0.0103 (4)	0.0098 (4)
O8	0.0174 (5)	0.0212 (6)	0.0195 (5)	0.0075 (4)	0.0086 (4)	0.0135 (5)
C1	0.0140 (7)	0.0144 (7)	0.0125 (7)	0.0040 (6)	0.0079 (6)	0.0042 (6)
C2	0.0149 (7)	0.0160 (7)	0.0151 (7)	0.0067 (6)	0.0090 (6)	0.0076 (6)
C3	0.0170 (7)	0.0121 (7)	0.0185 (7)	0.0021 (6)	0.0088 (6)	0.0052 (6)
C4	0.0124 (7)	0.0157 (7)	0.0147 (7)	0.0018 (6)	0.0060 (6)	0.0040 (6)
C5	0.0137 (7)	0.0150 (7)	0.0127 (7)	0.0042 (6)	0.0080 (6)	0.0048 (6)
C6	0.0139 (7)	0.0124 (7)	0.0139 (7)	0.0035 (5)	0.0075 (6)	0.0042 (6)
C7	0.0114 (7)	0.0140 (7)	0.0137 (7)	0.0023 (5)	0.0044 (6)	0.0044 (6)
C8	0.0135 (7)	0.0123 (7)	0.0149 (7)	0.0055 (5)	0.0049 (6)	0.0058 (6)
C9	0.0114 (7)	0.0133 (7)	0.0183 (7)	0.0036 (5)	0.0057 (6)	0.0064 (6)
C10	0.0143 (7)	0.0159 (7)	0.0142 (7)	0.0022 (6)	0.0029 (6)	0.0027 (6)
C11	0.0158 (7)	0.0163 (7)	0.0133 (7)	0.0052 (6)	0.0056 (6)	0.0057 (6)
C12	0.0129 (7)	0.0140 (7)	0.0166 (7)	0.0059 (6)	0.0056 (6)	0.0074 (6)
C13	0.0126 (7)	0.0122 (7)	0.0135 (7)	0.0032 (5)	0.0026 (6)	0.0043 (6)
C14	0.0136 (7)	0.0150 (7)	0.0129 (7)	0.0021 (6)	0.0042 (6)	0.0053 (6)
C15	0.0133 (7)	0.0133 (7)	0.0153 (7)	0.0018 (5)	0.0076 (6)	0.0066 (6)
C16	0.0134 (7)	0.0152 (7)	0.0127 (7)	−0.0003 (6)	0.0054 (6)	0.0055 (6)
C17	0.0163 (7)	0.0128 (7)	0.0162 (7)	0.0031 (6)	0.0095 (6)	0.0037 (6)
C18	0.0115 (7)	0.0137 (7)	0.0171 (7)	0.0028 (5)	0.0075 (6)	0.0075 (6)
C19	0.0132 (7)	0.0117 (7)	0.0144 (7)	0.0005 (5)	0.0067 (6)	0.0056 (6)
C20	0.0144 (7)	0.0111 (7)	0.0146 (7)	0.0022 (5)	0.0077 (6)	0.0045 (6)
C21	0.0115 (7)	0.0128 (7)	0.0138 (7)	0.0031 (5)	0.0051 (6)	0.0047 (6)
C22	0.0132 (7)	0.0110 (7)	0.0113 (7)	0.0001 (5)	0.0027 (5)	0.0024 (5)
C23	0.0117 (7)	0.0137 (7)	0.0141 (7)	0.0020 (5)	0.0047 (6)	0.0031 (6)
C24	0.0151 (7)	0.0150 (7)	0.0169 (7)	0.0053 (6)	0.0050 (6)	0.0074 (6)
C25	0.0149 (7)	0.0146 (7)	0.0120 (7)	0.0012 (6)	0.0031 (6)	0.0055 (6)
C26	0.0120 (7)	0.0122 (7)	0.0110 (7)	0.0004 (5)	0.0027 (5)	0.0018 (5)
C27	0.0125 (7)	0.0109 (7)	0.0122 (7)	0.0023 (5)	0.0022 (5)	0.0028 (5)
C28	0.0142 (7)	0.0141 (7)	0.0122 (7)	0.0031 (6)	0.0053 (6)	0.0057 (6)
C29	0.0158 (7)	0.0147 (7)	0.0150 (7)	0.0045 (6)	0.0059 (6)	0.0038 (6)
C30	0.0227 (8)	0.0196 (8)	0.0242 (8)	0.0091 (6)	0.0093 (7)	0.0092 (7)
C31	0.0168 (7)	0.0149 (7)	0.0188 (7)	0.0029 (6)	0.0054 (6)	0.0065 (6)
C32	0.0274 (9)	0.0190 (8)	0.0303 (9)	0.0093 (7)	0.0058 (7)	0.0104 (7)
C33	0.0151 (7)	0.0121 (7)	0.0159 (7)	0.0022 (5)	0.0061 (6)	0.0050 (6)
C34	0.0198 (8)	0.0154 (7)	0.0201 (8)	0.0015 (6)	0.0041 (6)	0.0036 (6)
C35	0.0155 (7)	0.0148 (7)	0.0153 (7)	0.0039 (6)	0.0058 (6)	0.0048 (6)
C36	0.0213 (8)	0.0184 (8)	0.0183 (8)	0.0021 (6)	0.0047 (6)	0.0031 (6)
O1S	0.0334 (7)	0.0371 (7)	0.0322 (7)	0.0110 (6)	0.0127 (6)	0.0116 (6)
C1S	0.0294 (10)	0.0390 (11)	0.0310 (10)	0.0037 (8)	0.0059 (8)	0.0125 (8)
O2S	0.0350 (8)	0.0623 (10)	0.0430 (8)	0.0170 (7)	0.0118 (6)	0.0314 (7)
C2S	0.0298 (10)	0.0415 (11)	0.0506 (12)	0.0034 (8)	0.0106 (9)	0.0210 (10)
O1W	0.0158 (8)	0.0197 (9)	0.0123 (8)	0.0041 (7)	0.0055 (7)	0.0019 (7)
O2W	0.0645 (17)	0.0438 (15)	0.0306 (13)	0.0402 (14)	−0.0068 (12)	0.0086 (12)
O3W	0.0132 (17)	0.0103 (16)	0.023 (2)	0.0015 (14)	−0.0047 (15)	0.0048 (16)
O9	0.0348 (7)	0.0196 (6)	0.0232 (6)	−0.0003 (5)	0.0032 (5)	0.0058 (5)
O10	0.0318 (7)	0.0218 (6)	0.0302 (7)	0.0063 (5)	0.0041 (6)	0.0033 (5)
C41	0.0302 (9)	0.0181 (8)	0.0187 (8)	0.0008 (7)	0.0119 (7)	0.0067 (7)
C42	0.0266 (8)	0.0230 (8)	0.0198 (8)	0.0015 (7)	0.0118 (7)	0.0086 (7)
C43	0.0304 (9)	0.0283 (9)	0.0253 (9)	0.0040 (7)	0.0094 (7)	0.0075 (7)
C44	0.0328 (10)	0.0389 (11)	0.0332 (10)	0.0044 (8)	0.0042 (8)	0.0047 (9)
C45	0.0289 (9)	0.0283 (9)	0.0236 (8)	0.0059 (7)	0.0129 (7)	0.0090 (7)

Geometric parameters (Å, º)

O1—C2	1.3798 (17)	C27—H27A	0.9500
O1—H1O	0.87 (2)	C28—C35	1.5367 (19)
O2—C4	1.3661 (18)	C28—H28A	1.0000
O2—H2O	0.83 (2)	C29—C30	1.522 (2)
O3—C9	1.3820 (18)	C29—H29A	0.9900
O3—H3O	0.84 (2)	C29—H29B	0.9900
O4—C11	1.3876 (18)	C30—H30A	0.9800
O4—H4O	0.83 (2)	C30—H30B	0.9800
O5—C16	1.3734 (17)	C30—H30C	0.9800
O5—H5O	0.85 (2)	C31—C32	1.524 (2)
O6—C18	1.3749 (17)	C31—H31A	0.9900
O6—H6O	0.90 (2)	C31—H31B	0.9900
O7—C23	1.3804 (17)	C32—H32A	0.9800
O7—H7O	0.82 (2)	C32—H32B	0.9800
O8—C25	1.3735 (18)	C32—H32C	0.9800
O8—H8O	0.86 (3)	C33—C34	1.524 (2)
C1—C6	1.395 (2)	C33—H33A	0.9900
C1—C2	1.399 (2)	C33—H33B	0.9900
C1—C28	1.5237 (19)	C34—H34A	0.9800
C2—C3	1.385 (2)	C34—H34B	0.9800
C3—C4	1.388 (2)	C34—H34C	0.9800
C3—H3A	0.9500	C35—C36	1.527 (2)
C4—C5	1.403 (2)	C35—H35A	0.9900
C5—C6	1.391 (2)	C35—H35B	0.9900
C5—C7	1.5228 (19)	C36—H36A	0.9800
C6—H6A	0.9500	C36—H36B	0.9800
C7—C8	1.5286 (19)	C36—H36C	0.9800
C7—C29	1.5423 (19)	O1S—C1S	1.412 (2)
C7—H7A	1.0000	O1S—H1S	0.9599
C8—C13	1.396 (2)	C1S—H1S1	0.9800
C8—C9	1.398 (2)	C1S—H1S2	0.9800
C9—C10	1.387 (2)	C1S—H1S3	0.9800
C10—C11	1.385 (2)	O2S—C2S	1.419 (3)
C10—H10A	0.9500	O2S—H2S	0.9599
C11—C12	1.393 (2)	C2S—H2S1	0.9800
C12—C13	1.394 (2)	C2S—H2S2	0.9800
C12—C14	1.529 (2)	C2S—H2S3	0.9800
C13—H13A	0.9500	O1W—H1WA	0.9197
C14—C15	1.517 (2)	O1W—H1WB	0.9198
C14—C31	1.537 (2)	O1W—H3WA	1.0919
C14—H14A	1.0000	O1W—H3WB	1.2702
C15—C20	1.388 (2)	O2W—H2WA	0.8684
C15—C16	1.400 (2)	O2W—H2WB	0.9200
C16—C17	1.382 (2)	O2W—H3WA	1.2195
C17—C18	1.390 (2)	O2W—H3WB	1.2847
C17—H17A	0.9500	O3W—H3WA	0.9197
C18—C19	1.400 (2)	O3W—H3WB	0.9200
C19—C20	1.397 (2)	O9—C41	1.226 (2)
C19—C21	1.5260 (19)	O10—C41	1.320 (2)
C20—H20A	0.9500	O10—H10O	0.96 (2)
C21—C22	1.5301 (19)	C41—C42	1.485 (2)
C21—C33	1.5361 (19)	C42—C43	1.337 (2)
C21—H21A	1.0000	C42—C45	1.502 (2)
C22—C27	1.393 (2)	C43—C44	1.491 (3)
C22—C23	1.395 (2)	C43—H43A	0.9500
C23—C24	1.387 (2)	C44—H44A	0.9800
C24—C25	1.389 (2)	C44—H44B	0.9800
C24—H24A	0.9500	C44—H44C	0.9800
C25—C26	1.397 (2)	C45—H45A	0.9800
C26—C27	1.394 (2)	C45—H45B	0.9800
C26—C28	1.5303 (19)	C45—H45C	0.9800
C2—O1—H1O	111.3 (14)	C1—C28—H28A	106.7
C4—O2—H2O	111.9 (15)	C26—C28—H28A	106.7
C9—O3—H3O	111.4 (15)	C35—C28—H28A	106.7
C11—O4—H4O	106.0 (16)	C30—C29—C7	112.55 (12)
C16—O5—H5O	110.7 (15)	C30—C29—H29A	109.1
C18—O6—H6O	111.4 (14)	C7—C29—H29A	109.1
C23—O7—H7O	109.1 (16)	C30—C29—H29B	109.1
C25—O8—H8O	111.1 (16)	C7—C29—H29B	109.1
C6—C1—C2	116.50 (13)	H29A—C29—H29B	107.8
C6—C1—C28	122.67 (12)	C29—C30—H30A	109.5
C2—C1—C28	120.80 (12)	C29—C30—H30B	109.5
O1—C2—C3	116.12 (13)	H30A—C30—H30B	109.5
O1—C2—C1	122.11 (13)	C29—C30—H30C	109.5
C3—C2—C1	121.77 (13)	H30A—C30—H30C	109.5
C2—C3—C4	119.85 (13)	H30B—C30—H30C	109.5
C2—C3—H3A	120.1	C32—C31—C14	111.35 (12)
C4—C3—H3A	120.1	C32—C31—H31A	109.4
O2—C4—C3	121.96 (13)	C14—C31—H31A	109.4
O2—C4—C5	117.29 (13)	C32—C31—H31B	109.4
C3—C4—C5	120.74 (13)	C14—C31—H31B	109.4
C6—C5—C4	117.34 (13)	H31A—C31—H31B	108.0
C6—C5—C7	123.25 (13)	C31—C32—H32A	109.5
C4—C5—C7	119.41 (13)	C31—C32—H32B	109.5
C5—C6—C1	123.79 (13)	H32A—C32—H32B	109.5
C5—C6—H6A	118.1	C31—C32—H32C	109.5
C1—C6—H6A	118.1	H32A—C32—H32C	109.5
C5—C7—C8	111.43 (11)	H32B—C32—H32C	109.5
C5—C7—C29	113.20 (12)	C34—C33—C21	112.45 (12)
C8—C7—C29	111.95 (11)	C34—C33—H33A	109.1
C5—C7—H7A	106.6	C21—C33—H33A	109.1
C8—C7—H7A	106.6	C34—C33—H33B	109.1
C29—C7—H7A	106.6	C21—C33—H33B	109.1
C13—C8—C9	116.63 (13)	H33A—C33—H33B	107.8
C13—C8—C7	119.81 (12)	C33—C34—H34A	109.5
C9—C8—C7	123.55 (13)	C33—C34—H34B	109.5
O3—C9—C10	114.40 (13)	H34A—C34—H34B	109.5
O3—C9—C8	124.47 (13)	C33—C34—H34C	109.5
C10—C9—C8	121.13 (13)	H34A—C34—H34C	109.5
C11—C10—C9	120.08 (13)	H34B—C34—H34C	109.5
C11—C10—H10A	120.0	C36—C35—C28	112.64 (12)
C9—C10—H10A	120.0	C36—C35—H35A	109.1
C10—C11—O4	116.84 (13)	C28—C35—H35A	109.1
C10—C11—C12	121.29 (13)	C36—C35—H35B	109.1
O4—C11—C12	121.84 (13)	C28—C35—H35B	109.1
C11—C12—C13	116.74 (13)	H35A—C35—H35B	107.8
C11—C12—C14	122.02 (13)	C35—C36—H36A	109.5
C13—C12—C14	121.21 (13)	C35—C36—H36B	109.5
C12—C13—C8	124.01 (13)	H36A—C36—H36B	109.5
C12—C13—H13A	118.0	C35—C36—H36C	109.5
C8—C13—H13A	118.0	H36A—C36—H36C	109.5
C15—C14—C12	110.55 (11)	H36B—C36—H36C	109.5
C15—C14—C31	114.45 (12)	C1S—O1S—H1S	103.3
C12—C14—C31	111.63 (12)	O1S—C1S—H1S1	109.5
C15—C14—H14A	106.6	O1S—C1S—H1S2	109.5
C12—C14—H14A	106.6	H1S1—C1S—H1S2	109.5
C31—C14—H14A	106.6	O1S—C1S—H1S3	109.5
C20—C15—C16	117.33 (13)	H1S1—C1S—H1S3	109.5
C20—C15—C14	123.67 (13)	H1S2—C1S—H1S3	109.5
C16—C15—C14	118.98 (13)	C2S—O2S—H2S	108.5
O5—C16—C17	121.25 (13)	O2S—C2S—H2S1	109.5
O5—C16—C15	117.63 (13)	O2S—C2S—H2S2	109.5
C17—C16—C15	121.11 (13)	H2S1—C2S—H2S2	109.5
C16—C17—C18	119.84 (13)	O2S—C2S—H2S3	109.5
C16—C17—H17A	120.1	H2S1—C2S—H2S3	109.5
C18—C17—H17A	120.1	H2S2—C2S—H2S3	109.5
O6—C18—C17	115.39 (12)	H1WA—O1W—H1WB	116.7
O6—C18—C19	123.28 (13)	H1WA—O1W—H3WA	106.7
C17—C18—C19	121.32 (13)	H1WB—O1W—H3WA	62.3
C20—C19—C18	116.74 (13)	H1WA—O1W—H3WB	127.4
C20—C19—C21	122.39 (12)	H1WB—O1W—H3WB	112.8
C18—C19—C21	120.85 (12)	H3WA—O1W—H3WB	81.0
C15—C20—C19	123.65 (13)	H2WA—O2W—H2WB	113.2
C15—C20—H20A	118.2	H2WA—O2W—H3WA	104.5
C19—C20—H20A	118.2	H2WB—O2W—H3WA	124.6
C19—C21—C22	111.17 (11)	H2WA—O2W—H3WB	170.2
C19—C21—C33	112.92 (11)	H2WB—O2W—H3WB	60.4
C22—C21—C33	112.21 (11)	H3WA—O2W—H3WB	75.9
C19—C21—H21A	106.7	H3WA—O3W—H3WB	113.7
C22—C21—H21A	106.7	C41—O10—H10O	109.3 (13)
C33—C21—H21A	106.7	O9—C41—O10	121.83 (16)
C27—C22—C23	117.09 (13)	O9—C41—C42	123.36 (15)
C27—C22—C21	122.01 (12)	O10—C41—C42	114.81 (14)
C23—C22—C21	120.89 (12)	C43—C42—C41	119.34 (15)
O7—C23—C24	121.19 (13)	C43—C42—C45	124.03 (16)
O7—C23—C22	117.26 (13)	C41—C42—C45	116.61 (14)
C24—C23—C22	121.55 (13)	C42—C43—C44	126.16 (17)
C23—C24—C25	119.50 (13)	C42—C43—H43A	116.9
C23—C24—H24A	120.3	C44—C43—H43A	116.9
C25—C24—H24A	120.3	C43—C44—H44A	109.5
O8—C25—C24	121.10 (13)	C43—C44—H44B	109.5
O8—C25—C26	117.65 (13)	H44A—C44—H44B	109.5
C24—C25—C26	121.23 (13)	C43—C44—H44C	109.5
C27—C26—C25	117.26 (13)	H44A—C44—H44C	109.5
C27—C26—C28	121.76 (12)	H44B—C44—H44C	109.5
C25—C26—C28	120.98 (12)	C42—C45—H45A	109.5
C22—C27—C26	123.36 (13)	C42—C45—H45B	109.5
C22—C27—H27A	118.3	H45A—C45—H45B	109.5
C26—C27—H27A	118.3	C42—C45—H45C	109.5
C1—C28—C26	110.36 (11)	H45A—C45—H45C	109.5
C1—C28—C35	113.65 (11)	H45B—C45—H45C	109.5
C26—C28—C35	112.13 (11)
C6—C1—C2—O1	178.62 (12)	C16—C17—C18—C19	0.8 (2)
C28—C1—C2—O1	−3.2 (2)	O6—C18—C19—C20	−178.78 (12)
C6—C1—C2—C3	−0.7 (2)	C17—C18—C19—C20	−0.3 (2)
C28—C1—C2—C3	177.49 (13)	O6—C18—C19—C21	2.6 (2)
O1—C2—C3—C4	−178.93 (12)	C17—C18—C19—C21	−178.82 (12)
C1—C2—C3—C4	0.4 (2)	C16—C15—C20—C19	0.0 (2)
C2—C3—C4—O2	−179.80 (13)	C14—C15—C20—C19	−178.10 (13)
C2—C3—C4—C5	0.5 (2)	C18—C19—C20—C15	−0.2 (2)
O2—C4—C5—C6	179.22 (12)	C21—C19—C20—C15	178.38 (12)
C3—C4—C5—C6	−1.0 (2)	C20—C19—C21—C22	−98.70 (15)
O2—C4—C5—C7	−1.31 (19)	C18—C19—C21—C22	79.78 (16)
C3—C4—C5—C7	178.45 (13)	C20—C19—C21—C33	28.45 (18)
C4—C5—C6—C1	0.7 (2)	C18—C19—C21—C33	−153.06 (13)
C7—C5—C6—C1	−178.70 (13)	C19—C21—C22—C27	78.50 (16)
C2—C1—C6—C5	0.1 (2)	C33—C21—C22—C27	−49.04 (18)
C28—C1—C6—C5	−178.07 (13)	C19—C21—C22—C23	−100.09 (15)
C6—C5—C7—C8	−102.09 (15)	C33—C21—C22—C23	132.37 (14)
C4—C5—C7—C8	78.48 (16)	C27—C22—C23—O7	−177.62 (12)
C6—C5—C7—C29	25.16 (19)	C21—C22—C23—O7	1.0 (2)
C4—C5—C7—C29	−154.27 (13)	C27—C22—C23—C24	1.4 (2)
C5—C7—C8—C13	73.45 (16)	C21—C22—C23—C24	−179.94 (13)
C29—C7—C8—C13	−54.46 (17)	O7—C23—C24—C25	177.99 (13)
C5—C7—C8—C9	−107.58 (15)	C22—C23—C24—C25	−1.0 (2)
C29—C7—C8—C9	124.51 (14)	C23—C24—C25—O8	−178.35 (13)
C13—C8—C9—O3	179.55 (13)	C23—C24—C25—C26	0.2 (2)
C7—C8—C9—O3	0.5 (2)	O8—C25—C26—C27	178.66 (12)
C13—C8—C9—C10	−1.5 (2)	C24—C25—C26—C27	0.0 (2)
C7—C8—C9—C10	179.54 (13)	O8—C25—C26—C28	−0.2 (2)
O3—C9—C10—C11	−179.64 (13)	C24—C25—C26—C28	−178.84 (13)
C8—C9—C10—C11	1.3 (2)	C23—C22—C27—C26	−1.1 (2)
C9—C10—C11—O4	179.53 (13)	C21—C22—C27—C26	−179.79 (13)
C9—C10—C11—C12	1.5 (2)	C25—C26—C27—C22	0.5 (2)
C10—C11—C12—C13	−3.8 (2)	C28—C26—C27—C22	179.30 (12)
O4—C11—C12—C13	178.25 (13)	C6—C1—C28—C26	96.84 (15)
C10—C11—C12—C14	174.30 (13)	C2—C1—C28—C26	−81.25 (16)
O4—C11—C12—C14	−3.6 (2)	C6—C1—C28—C35	−30.11 (18)
C11—C12—C13—C8	3.7 (2)	C2—C1—C28—C35	151.79 (13)
C14—C12—C13—C8	−174.46 (13)	C27—C26—C28—C1	−77.50 (16)
C9—C8—C13—C12	−1.1 (2)	C25—C26—C28—C1	101.30 (15)
C7—C8—C13—C12	177.95 (13)	C27—C26—C28—C35	50.29 (17)
C11—C12—C14—C15	106.44 (15)	C25—C26—C28—C35	−130.90 (14)
C13—C12—C14—C15	−75.52 (16)	C5—C7—C29—C30	172.23 (12)
C11—C12—C14—C31	−124.93 (14)	C8—C7—C29—C30	−60.80 (16)
C13—C12—C14—C31	53.10 (17)	C15—C14—C31—C32	−170.16 (13)
C12—C14—C15—C20	99.64 (15)	C12—C14—C31—C32	63.33 (16)
C31—C14—C15—C20	−27.43 (19)	C19—C21—C33—C34	170.73 (12)
C12—C14—C15—C16	−78.47 (16)	C22—C21—C33—C34	−62.67 (16)
C31—C14—C15—C16	154.46 (13)	C1—C28—C35—C36	−174.84 (12)
C20—C15—C16—O5	−179.39 (12)	C26—C28—C35—C36	59.14 (16)
C14—C15—C16—O5	−1.16 (19)	O9—C41—C42—C43	−172.39 (16)
C20—C15—C16—C17	0.5 (2)	O10—C41—C42—C43	7.9 (2)
C14—C15—C16—C17	178.75 (13)	O9—C41—C42—C45	6.4 (2)
O5—C16—C17—C18	178.97 (12)	O10—C41—C42—C45	−173.24 (14)
C15—C16—C17—C18	−0.9 (2)	C41—C42—C43—C44	177.34 (17)
C16—C17—C18—O6	179.44 (12)	C45—C42—C43—C44	−1.4 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1O···O8	0.87 (2)	1.91 (2)	2.7575 (15)	164 (2)
O2—H2O···O9	0.83 (2)	1.94 (2)	2.7557 (16)	169 (2)
O3—H3O···O6^i	0.84 (2)	2.01 (2)	2.7460 (15)	145 (2)
O3—H3O···O2	0.84 (2)	2.39 (2)	2.9318 (15)	122.6 (18)
O4—H4O···O5	0.83 (2)	1.93 (2)	2.7445 (15)	165 (2)
O5—H5O···O3^ii	0.85 (2)	1.89 (2)	2.7393 (15)	171 (2)
O6—H6O···O7	0.90 (2)	1.82 (2)	2.7123 (15)	174 (2)
O7—H7O···O1^iii	0.82 (2)	1.88 (2)	2.6754 (15)	162 (2)
O10—H10O···O1S	0.96 (2)	1.64 (2)	2.5909 (18)	173 (2)
O1S—H1S···O2S^iv	0.96	1.76	2.709 (2)	168
O2S—H2S···O4^v	0.96	1.77	2.7265 (18)	173

Symmetry codes: (i) x+1, y, z; (ii) −x, −y+1, −z+1; (iii) −x−1, −y+1, −z; (iv) x−1, y, z; (v) −x+1, −y+1, −z+1.

(CECR-HTA-2MeOH-1.5H2O@90k-1h-exposure)

Crystal data

C43H59O13.50	F(000) = 850
Mr = 791.90	Dx = 1.268 Mg m^−3
Triclinic, P1	Melting point: not measured K
a = 11.2954 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.0883 (3) Å	Cell parameters from 865 reflections
c = 14.7549 (3) Å	θ = 2.5–25°
α = 108.6380 (5)°	µ = 0.09 mm^−1
β = 108.8086 (5)°	T = 90 K
γ = 92.9259 (6)°	Block, pale yellow
V = 2074.74 (7) Å^3	0.14 × 0.10 × 0.08 mm
Z = 2

Data collection

CCD area detector diffractometer	7308 independent reflections
Radiation source: fine-focus sealed tube	6443 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.014
phi and ω scans	θmax = 25.0°, θmin = 1.6°
Absorption correction: empirical (using intensity measurements) Blessing, R. (1995) Acta Crystallogr., A51, 33-38	h = −12→13
Tmin = 0.987, Tmax = 0.993	k = −16→14
16740 measured reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.119	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0601P)^2 + 1.1813P] where P = (Fo^2 + 2Fc^2)/3
7308 reflections	(Δ/σ)max = 0.001
581 parameters	Δρmax = 0.58 e Å^−3
7 restraints	Δρmin = −0.32 e Å^−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)
O1	−0.23014 (11)	0.46641 (9)	−0.05381 (9)	0.0175 (3)
O2	0.13478 (11)	0.47033 (9)	0.22257 (9)	0.0198 (3)
O3	0.26240 (10)	0.40939 (9)	0.39637 (9)	0.0177 (3)
O4	0.00699 (12)	0.36466 (9)	0.57970 (9)	0.0201 (3)
O5	−0.24132 (10)	0.39135 (9)	0.51760 (8)	0.0173 (3)
O6	−0.61963 (10)	0.38985 (9)	0.25596 (9)	0.0173 (3)
O7	−0.73338 (11)	0.34628 (9)	0.05119 (9)	0.0174 (3)
O8	−0.48786 (11)	0.39468 (9)	−0.14847 (9)	0.0186 (3)
C1	−0.20473 (14)	0.31151 (12)	−0.01558 (12)	0.0137 (3)
C2	−0.16301 (15)	0.41368 (12)	0.00414 (12)	0.0145 (3)
C3	−0.05099 (15)	0.46766 (12)	0.08284 (12)	0.0162 (3)
H3A	−0.0252	0.5372	0.0950	0.019*
C4	0.02370 (15)	0.42010 (12)	0.14397 (12)	0.0153 (3)
C5	−0.01290 (15)	0.31732 (12)	0.12668 (12)	0.0141 (3)
C6	−0.12661 (14)	0.26659 (12)	0.04751 (12)	0.0135 (3)
H6A	−0.1528	0.1971	0.0356	0.016*
C7	0.07266 (14)	0.26671 (12)	0.19365 (12)	0.0144 (3)
H7A	0.1621	0.2956	0.2073	0.017*
C8	0.05733 (15)	0.29437 (12)	0.29778 (12)	0.0143 (3)
C9	0.14867 (15)	0.36052 (12)	0.38916 (12)	0.0150 (3)
C10	0.12926 (15)	0.38333 (12)	0.48139 (12)	0.0175 (3)
H10A	0.1916	0.4296	0.5425	0.021*
C11	0.01921 (15)	0.33878 (12)	0.48457 (12)	0.0160 (3)
C12	−0.07284 (15)	0.26942 (12)	0.39662 (12)	0.0149 (3)
C13	−0.05207 (15)	0.25137 (12)	0.30487 (12)	0.0144 (3)
H13A	−0.1161	0.2072	0.2435	0.017*
C14	−0.18951 (15)	0.21245 (12)	0.39990 (12)	0.0149 (3)
H14A	−0.1752	0.2267	0.4739	0.018*
C15	−0.30737 (14)	0.25510 (12)	0.35775 (12)	0.0141 (3)
C16	−0.32835 (15)	0.34585 (12)	0.41969 (12)	0.0147 (3)
C17	−0.43294 (15)	0.38873 (12)	0.38391 (12)	0.0157 (3)
H17A	−0.4464	0.4500	0.4274	0.019*
C18	−0.51833 (14)	0.34175 (12)	0.28392 (12)	0.0141 (3)
C19	−0.50183 (14)	0.25084 (12)	0.21866 (12)	0.0134 (3)
C20	−0.39521 (14)	0.20987 (12)	0.25862 (12)	0.0133 (3)
H20A	−0.3822	0.1480	0.2158	0.016*
C21	−0.59477 (14)	0.20109 (12)	0.10871 (12)	0.0134 (3)
H21A	−0.6808	0.2131	0.1099	0.016*
C22	−0.56710 (14)	0.25233 (11)	0.03891 (12)	0.0134 (3)
C23	−0.63877 (14)	0.32333 (12)	0.01151 (12)	0.0147 (3)
C24	−0.61473 (15)	0.37049 (12)	−0.05177 (12)	0.0167 (3)
H24A	−0.6652	0.4179	−0.0704	0.020*
C25	−0.51612 (15)	0.34770 (12)	−0.08766 (12)	0.0154 (3)
C26	−0.44086 (14)	0.27806 (12)	−0.06163 (12)	0.0140 (3)
C27	−0.46872 (14)	0.23233 (11)	0.00172 (12)	0.0134 (3)
H27A	−0.4180	0.1851	0.0205	0.016*
C28	−0.33094 (14)	0.25478 (12)	−0.09984 (12)	0.0141 (3)
H28A	−0.3426	0.2826	−0.1560	0.017*
C29	0.05695 (15)	0.15082 (12)	0.14042 (12)	0.0171 (3)
H29A	−0.0291	0.1188	0.1293	0.020*
H29B	0.0645	0.1364	0.0725	0.020*
C30	0.15491 (17)	0.10365 (14)	0.20218 (14)	0.0236 (4)
H30A	0.2403	0.1378	0.2169	0.035*
H30B	0.1453	0.0312	0.1628	0.035*
H30C	0.1423	0.1115	0.2667	0.035*
C31	−0.20190 (16)	0.09678 (12)	0.34978 (13)	0.0188 (3)
H31A	−0.2817	0.0628	0.3484	0.023*
H31B	−0.2064	0.0799	0.2781	0.023*
C32	−0.08988 (18)	0.05699 (14)	0.40768 (15)	0.0287 (4)
H32A	−0.0110	0.0891	0.4074	0.043*
H32B	−0.1010	−0.0169	0.3743	0.043*
H32C	−0.0856	0.0731	0.4785	0.043*
C33	−0.60205 (15)	0.08510 (12)	0.06626 (12)	0.0153 (3)
H33A	−0.5206	0.0701	0.0582	0.018*
H33B	−0.6143	0.0561	0.1161	0.018*
C34	−0.70980 (16)	0.03433 (13)	−0.03647 (13)	0.0210 (4)
H34A	−0.7908	0.0481	−0.0287	0.031*
H34B	−0.7110	−0.0392	−0.0602	0.031*
H34C	−0.6969	0.0615	−0.0867	0.031*
C35	−0.33411 (15)	0.13991 (12)	−0.14711 (12)	0.0163 (3)
H35A	−0.2613	0.1289	−0.1704	0.020*
H35B	−0.3245	0.1093	−0.0939	0.020*
C36	−0.45689 (17)	0.08624 (13)	−0.23745 (13)	0.0233 (4)
H36A	−0.5288	0.0926	−0.2138	0.035*
H36B	−0.4525	0.0142	−0.2670	0.035*
H36C	−0.4682	0.1175	−0.2895	0.035*
O2S	0.84850 (15)	0.73131 (14)	0.30213 (13)	0.0490 (4)
H2S	0.9056	0.7017	0.3479	0.074*
C2S	0.76245 (13)	0.77647 (11)	0.34741 (11)	0.0442 (5)
H2S1	0.8100	0.8289	0.4143	0.066*
H2S2	0.7111	0.7243	0.3563	0.066*
H2S3	0.7068	0.8074	0.3030	0.066*
O1W	0.25498 (13)	0.55221 (11)	0.77025 (11)	0.0180 (4)	0.60
H1WA	0.1892	0.5028	0.7200	0.027*	0.60
H1WB	0.2426	0.5858	0.8305	0.027*	0.60
O2W	0.3166 (3)	0.4696 (2)	0.7622 (2)	0.0528 (8)	0.60
H2WA	0.2696	0.4106	0.7423	0.079*	0.60
H2WB	0.3210	0.4879	0.7086	0.079*	0.60
O3W	0.3709 (4)	0.5350 (3)	0.8301 (3)	0.0188 (8)	0.30
H3WA	0.2918	0.5243	0.8338	0.028*	0.30
H3WB	0.3720	0.5609	0.7803	0.028*	0.30
H1O	−0.306 (2)	0.4341 (18)	−0.0926 (18)	0.036 (6)*
H2O	0.150 (2)	0.530 (2)	0.2258 (18)	0.039 (7)*
H3O	0.263 (2)	0.4015 (19)	0.337 (2)	0.047 (7)*
H4O	−0.068 (3)	0.3720 (19)	0.571 (2)	0.050 (8)*
H5O	−0.258 (2)	0.450 (2)	0.5469 (19)	0.042 (7)*
H6O	−0.655 (2)	0.3717 (17)	0.1881 (19)	0.034 (6)*
H7O	−0.758 (2)	0.396 (2)	0.0397 (19)	0.044 (7)*
H8O	−0.544 (3)	0.429 (2)	−0.167 (2)	0.051 (8)*
O9	0.1884 (2)	0.67794 (18)	0.26746 (19)	0.0285 (5)	0.869 (4)
O10	0.2286 (4)	0.8430 (3)	0.3627 (3)	0.0373 (6)	0.869 (4)
H10O	0.1450	0.8387	0.3166	0.056*	0.869 (4)
C41	0.2603 (3)	0.7516 (2)	0.3389 (3)	0.0247 (7)	0.869 (4)
C42	0.3893 (2)	0.7463 (2)	0.4040 (2)	0.0253 (7)	0.869 (4)
C43	0.4552 (3)	0.8270 (2)	0.48719 (19)	0.0327 (6)	0.869 (4)
H43A	0.4169	0.8861	0.4993	0.039*	0.869 (4)
C44	0.5832 (2)	0.8333 (2)	0.5629 (2)	0.0436 (7)	0.869 (4)
H44A	0.5747	0.8311	0.6263	0.065*	0.869 (4)
H44B	0.6373	0.8971	0.5777	0.065*	0.869 (4)
H44C	0.6218	0.7757	0.5344	0.065*	0.869 (4)
C45	0.4378 (4)	0.6478 (2)	0.3706 (3)	0.0297 (7)	0.869 (4)
H45A	0.4769	0.6487	0.3205	0.045*	0.869 (4)
H45B	0.3669	0.5907	0.3395	0.045*	0.869 (4)
H45C	0.5010	0.6400	0.4303	0.045*	0.869 (4)
O1S	0.00176 (16)	0.84474 (13)	0.25257 (13)	0.0365 (5)	0.888 (4)
H1S	−0.0594	0.7958	0.2617	0.055*	0.888 (4)
C1S	−0.0269 (4)	0.8062 (3)	0.1431 (2)	0.0374 (9)	0.888 (4)
H1S1	0.0224	0.8518	0.1251	0.056*	0.888 (4)
H1S2	−0.1177	0.8026	0.1075	0.056*	0.888 (4)
H1S3	−0.0050	0.7382	0.1224	0.056*	0.888 (4)
O9B	0.2230 (18)	0.6643 (15)	0.2675 (16)	0.0285 (5)	0.131 (4)
O10B	0.242 (3)	0.823 (2)	0.369 (3)	0.0373 (6)	0.131 (4)
H10P	0.1686	0.8263	0.3308	0.056*	0.131 (4)
C41B	0.288 (2)	0.739 (2)	0.340 (2)	0.0247 (7)	0.131 (4)
C42B	0.416 (2)	0.7311 (18)	0.3978 (19)	0.0253 (7)	0.131 (4)
C43B	0.5028 (19)	0.8071 (12)	0.4747 (13)	0.0327 (6)	0.131 (4)
H43B	0.5803	0.7890	0.5084	0.039*	0.131 (4)
C44B	0.4925 (17)	0.9190 (12)	0.5152 (13)	0.0436 (7)	0.131 (4)
H44D	0.4703	0.9450	0.4587	0.065*	0.131 (4)
H44E	0.5741	0.9575	0.5673	0.065*	0.131 (4)
H44F	0.4266	0.9266	0.5456	0.065*	0.131 (4)
C45B	0.431 (3)	0.6222 (19)	0.376 (2)	0.0297 (7)	0.131 (4)
H45D	0.3591	0.5844	0.3798	0.045*	0.131 (4)
H45E	0.5102	0.6176	0.4259	0.045*	0.131 (4)
H45F	0.4340	0.5932	0.3066	0.045*	0.131 (4)
O1SB	−0.026 (3)	0.8228 (15)	0.169 (2)	0.0365 (5)	0.112 (4)
H1SP	−0.0631	0.8462	0.2113	0.055*	0.112 (4)
C1SB	−0.0389 (19)	0.7250 (13)	0.1745 (14)	0.0374 (9)	0.112 (4)
H1S4	−0.1269	0.7027	0.1653	0.056*	0.112 (4)
H1S5	0.0176	0.7269	0.2415	0.056*	0.112 (4)
H1S6	−0.0161	0.6772	0.1205	0.056*	0.112 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0163 (6)	0.0159 (6)	0.0220 (6)	0.0040 (5)	0.0052 (5)	0.0105 (5)
O2	0.0166 (6)	0.0154 (6)	0.0227 (6)	−0.0016 (5)	0.0011 (5)	0.0072 (5)
O3	0.0144 (6)	0.0208 (6)	0.0158 (6)	−0.0006 (5)	0.0063 (5)	0.0035 (5)
O4	0.0169 (6)	0.0279 (7)	0.0145 (6)	0.0023 (5)	0.0067 (5)	0.0053 (5)
O5	0.0161 (6)	0.0180 (6)	0.0133 (6)	0.0026 (5)	0.0032 (5)	0.0020 (5)
O6	0.0150 (6)	0.0186 (6)	0.0168 (6)	0.0073 (5)	0.0050 (5)	0.0042 (5)
O7	0.0178 (6)	0.0177 (6)	0.0235 (6)	0.0083 (5)	0.0115 (5)	0.0111 (5)
O8	0.0192 (6)	0.0229 (6)	0.0220 (6)	0.0078 (5)	0.0098 (5)	0.0156 (5)
C1	0.0148 (8)	0.0151 (8)	0.0137 (8)	0.0037 (6)	0.0088 (6)	0.0045 (6)
C2	0.0164 (8)	0.0165 (8)	0.0162 (8)	0.0074 (6)	0.0095 (6)	0.0086 (6)
C3	0.0182 (8)	0.0130 (8)	0.0193 (8)	0.0016 (6)	0.0094 (7)	0.0057 (7)
C4	0.0136 (8)	0.0165 (8)	0.0156 (8)	0.0012 (6)	0.0064 (6)	0.0043 (6)
C5	0.0146 (8)	0.0164 (8)	0.0147 (8)	0.0041 (6)	0.0091 (6)	0.0058 (6)
C6	0.0148 (8)	0.0125 (7)	0.0156 (8)	0.0036 (6)	0.0087 (6)	0.0047 (6)
C7	0.0122 (7)	0.0151 (8)	0.0155 (8)	0.0022 (6)	0.0047 (6)	0.0052 (6)
C8	0.0143 (8)	0.0135 (8)	0.0165 (8)	0.0060 (6)	0.0054 (6)	0.0069 (6)
C9	0.0123 (7)	0.0145 (8)	0.0194 (8)	0.0037 (6)	0.0060 (6)	0.0069 (6)
C10	0.0150 (8)	0.0187 (8)	0.0156 (8)	0.0024 (6)	0.0032 (6)	0.0042 (7)
C11	0.0171 (8)	0.0180 (8)	0.0148 (8)	0.0053 (6)	0.0067 (6)	0.0068 (6)
C12	0.0138 (8)	0.0146 (8)	0.0180 (8)	0.0053 (6)	0.0056 (6)	0.0077 (6)
C13	0.0139 (8)	0.0134 (8)	0.0145 (8)	0.0036 (6)	0.0029 (6)	0.0052 (6)
C14	0.0149 (8)	0.0163 (8)	0.0145 (8)	0.0029 (6)	0.0053 (6)	0.0066 (6)
C15	0.0144 (8)	0.0154 (8)	0.0166 (8)	0.0021 (6)	0.0082 (6)	0.0086 (6)
C16	0.0140 (8)	0.0172 (8)	0.0139 (8)	−0.0006 (6)	0.0056 (6)	0.0066 (6)
C17	0.0177 (8)	0.0144 (8)	0.0164 (8)	0.0033 (6)	0.0094 (7)	0.0036 (6)
C18	0.0123 (7)	0.0158 (8)	0.0184 (8)	0.0034 (6)	0.0078 (6)	0.0090 (6)
C19	0.0135 (7)	0.0130 (8)	0.0151 (8)	0.0000 (6)	0.0067 (6)	0.0058 (6)
C20	0.0150 (8)	0.0123 (7)	0.0154 (8)	0.0025 (6)	0.0084 (6)	0.0057 (6)
C21	0.0122 (7)	0.0135 (8)	0.0156 (8)	0.0025 (6)	0.0059 (6)	0.0055 (6)
C22	0.0142 (7)	0.0115 (7)	0.0124 (7)	0.0004 (6)	0.0031 (6)	0.0032 (6)
C23	0.0126 (7)	0.0147 (8)	0.0162 (8)	0.0019 (6)	0.0055 (6)	0.0045 (6)
C24	0.0166 (8)	0.0175 (8)	0.0180 (8)	0.0061 (6)	0.0056 (6)	0.0088 (7)
C25	0.0164 (8)	0.0164 (8)	0.0131 (8)	0.0011 (6)	0.0035 (6)	0.0067 (6)
C26	0.0138 (8)	0.0131 (8)	0.0121 (7)	0.0002 (6)	0.0033 (6)	0.0024 (6)
C27	0.0132 (7)	0.0115 (7)	0.0137 (7)	0.0020 (6)	0.0029 (6)	0.0041 (6)
C28	0.0149 (8)	0.0163 (8)	0.0133 (8)	0.0038 (6)	0.0056 (6)	0.0072 (6)
C29	0.0186 (8)	0.0156 (8)	0.0177 (8)	0.0049 (6)	0.0081 (7)	0.0050 (7)
C30	0.0256 (9)	0.0213 (9)	0.0289 (10)	0.0107 (7)	0.0125 (8)	0.0117 (8)
C31	0.0191 (8)	0.0160 (8)	0.0209 (8)	0.0028 (7)	0.0055 (7)	0.0076 (7)
C32	0.0291 (10)	0.0216 (9)	0.0338 (10)	0.0094 (8)	0.0057 (8)	0.0125 (8)
C33	0.0162 (8)	0.0129 (8)	0.0177 (8)	0.0019 (6)	0.0067 (6)	0.0059 (6)
C34	0.0201 (8)	0.0163 (8)	0.0219 (9)	0.0013 (7)	0.0047 (7)	0.0039 (7)
C35	0.0169 (8)	0.0162 (8)	0.0166 (8)	0.0042 (6)	0.0068 (6)	0.0058 (7)
C36	0.0241 (9)	0.0202 (9)	0.0213 (9)	0.0019 (7)	0.0054 (7)	0.0046 (7)
O2S	0.0405 (9)	0.0711 (12)	0.0479 (10)	0.0210 (8)	0.0150 (7)	0.0365 (9)
C2S	0.0331 (12)	0.0445 (13)	0.0541 (14)	0.0033 (10)	0.0107 (10)	0.0217 (11)
O1W	0.0169 (9)	0.0214 (10)	0.0145 (9)	0.0037 (8)	0.0064 (8)	0.0036 (8)
O2W	0.0655 (19)	0.0444 (16)	0.0343 (15)	0.0386 (15)	−0.0030 (14)	0.0124 (13)
O3W	0.0146 (18)	0.0091 (18)	0.022 (2)	0.0010 (15)	−0.0053 (16)	0.0037 (17)
O9	0.0326 (14)	0.0208 (10)	0.0254 (7)	0.0027 (8)	0.0044 (10)	0.0060 (7)
O10	0.0438 (14)	0.0221 (18)	0.0359 (10)	0.0072 (10)	0.0054 (10)	0.0060 (11)
C41	0.0328 (17)	0.0222 (17)	0.0229 (10)	0.0020 (12)	0.0141 (13)	0.0093 (10)
C42	0.0295 (16)	0.0282 (14)	0.0233 (10)	0.0017 (10)	0.0144 (11)	0.0109 (10)
C43	0.0324 (15)	0.0349 (13)	0.0293 (12)	0.0050 (11)	0.0115 (11)	0.0094 (10)
C44	0.0358 (14)	0.0457 (15)	0.0368 (14)	0.0057 (11)	0.0051 (11)	0.0067 (12)
C45	0.0346 (12)	0.033 (2)	0.0272 (11)	−0.0005 (16)	0.0155 (9)	0.0152 (13)
O1S	0.0414 (10)	0.0371 (10)	0.0322 (10)	0.0110 (7)	0.0165 (8)	0.0098 (7)
C1S	0.0382 (13)	0.0418 (17)	0.027 (2)	0.0040 (13)	0.0100 (15)	0.0080 (14)
O9B	0.0326 (14)	0.0208 (10)	0.0254 (7)	0.0027 (8)	0.0044 (10)	0.0060 (7)
O10B	0.0438 (14)	0.0221 (18)	0.0359 (10)	0.0072 (10)	0.0054 (10)	0.0060 (11)
C41B	0.0328 (17)	0.0222 (17)	0.0229 (10)	0.0020 (12)	0.0141 (13)	0.0093 (10)
C42B	0.0295 (16)	0.0282 (14)	0.0233 (10)	0.0017 (10)	0.0144 (11)	0.0109 (10)
C43B	0.0324 (15)	0.0349 (13)	0.0293 (12)	0.0050 (11)	0.0115 (11)	0.0094 (10)
C44B	0.0358 (14)	0.0457 (15)	0.0368 (14)	0.0057 (11)	0.0051 (11)	0.0067 (12)
C45B	0.0346 (12)	0.033 (2)	0.0272 (11)	−0.0005 (16)	0.0155 (9)	0.0152 (13)
O1SB	0.0414 (10)	0.0371 (10)	0.0322 (10)	0.0110 (7)	0.0165 (8)	0.0098 (7)
C1SB	0.0382 (13)	0.0418 (17)	0.027 (2)	0.0040 (13)	0.0100 (15)	0.0080 (14)

Geometric parameters (Å, º)

O1—C2	1.3796 (19)	C32—H32B	0.9800
O1—H1O	0.87 (2)	C32—H32C	0.9800
O2—C4	1.366 (2)	C33—C34	1.523 (2)
O2—H2O	0.84 (3)	C33—H33A	0.9900
O3—C9	1.3821 (19)	C33—H33B	0.9900
O3—H3O	0.85 (3)	C34—H34A	0.9800
O4—C11	1.3876 (19)	C34—H34B	0.9800
O4—H4O	0.83 (3)	C34—H34C	0.9800
O5—C16	1.3756 (19)	C35—C36	1.526 (2)
O5—H5O	0.87 (3)	C35—H35A	0.9900
O6—C18	1.3756 (19)	C35—H35B	0.9900
O6—H6O	0.89 (2)	C36—H36A	0.9800
O7—C23	1.3809 (19)	C36—H36B	0.9800
O7—H7O	0.82 (3)	C36—H36C	0.9800
O8—C25	1.3739 (19)	O2S—C2S	1.416 (2)
O8—H8O	0.84 (3)	O2S—H2S	0.9869
C1—C6	1.396 (2)	C2S—H2S1	0.9800
C1—C2	1.398 (2)	C2S—H2S2	0.9800
C1—C28	1.524 (2)	C2S—H2S3	0.9800
C2—C3	1.385 (2)	O1W—H1WA	0.9208
C3—C4	1.388 (2)	O1W—H1WB	0.9229
C3—H3A	0.9500	O1W—H2WB	1.4776
C4—C5	1.403 (2)	O1W—H3WA	1.0990
C5—C6	1.389 (2)	O1W—H3WB	1.2759
C5—C7	1.524 (2)	O2W—H2WA	0.8699
C6—H6A	0.9500	O2W—H2WB	0.9215
C7—C8	1.529 (2)	O2W—H3WA	1.2165
C7—C29	1.541 (2)	O2W—H3WB	1.3065
C7—H7A	1.0000	O3W—H3WA	0.9201
C8—C9	1.397 (2)	O3W—H3WB	0.9214
C8—C13	1.397 (2)	O9—C41	1.229 (3)
C9—C10	1.387 (2)	O10—C41	1.323 (3)
C10—C11	1.385 (2)	O10—H10O	0.9549
C10—H10A	0.9500	O10—H10P	0.6665
C11—C12	1.391 (2)	C41—C42	1.485 (4)
C12—C13	1.394 (2)	C41—H10P	1.5199
C12—C14	1.530 (2)	C42—C43	1.336 (3)
C13—H13A	0.9500	C42—C45	1.512 (4)
C14—C15	1.519 (2)	C43—C44	1.494 (4)
C14—C31	1.537 (2)	C43—H43A	0.9500
C14—H14A	1.0000	C44—H44A	0.9800
C15—C20	1.391 (2)	C44—H44B	0.9800
C15—C16	1.396 (2)	C44—H44C	0.9800
C16—C17	1.383 (2)	C45—H45A	0.9800
C17—C18	1.392 (2)	C45—H45B	0.9800
C17—H17A	0.9500	C45—H45C	0.9800
C18—C19	1.398 (2)	O1S—C1S	1.447 (4)
C19—C20	1.401 (2)	O1S—H1S	1.0203
C19—C21	1.525 (2)	O1S—H1SP	0.7937
C20—H20A	0.9500	C1S—H1S1	0.9800
C21—C22	1.529 (2)	C1S—H1S2	0.9800
C21—C33	1.539 (2)	C1S—H1S3	0.9800
C21—H21A	1.0000	C1S—H1SP	1.1931
C22—C27	1.394 (2)	O9B—C41B	1.225 (18)
C22—C23	1.396 (2)	O10B—C41B	1.319 (17)
C23—C24	1.389 (2)	O10B—H10O	1.1923
C24—C25	1.390 (2)	O10B—H10P	0.8481
C24—H24A	0.9500	C41B—C42B	1.455 (18)
C25—C26	1.396 (2)	C42B—C43B	1.338 (17)
C26—C27	1.393 (2)	C42B—C45B	1.492 (17)
C26—C28	1.530 (2)	C43B—C44B	1.523 (16)
C27—H27A	0.9500	C43B—H43B	0.9500
C28—C35	1.537 (2)	C44B—H44D	0.9800
C28—H28A	1.0000	C44B—H44E	0.9800
C29—C30	1.519 (2)	C44B—H44F	0.9800
C29—H29A	0.9900	C45B—H45D	0.9800
C29—H29B	0.9900	C45B—H45E	0.9800
C30—H30A	0.9800	C45B—H45F	0.9800
C30—H30B	0.9800	O1SB—C1SB	1.409 (17)
C30—H30C	0.9800	O1SB—H1SP	0.8521
C31—C32	1.525 (2)	C1SB—H1S	1.4497
C31—H31A	0.9900	C1SB—H1S4	0.9800
C31—H31B	0.9900	C1SB—H1S5	0.9800
C32—H32A	0.9800	C1SB—H1S6	0.9800
C2—O1—H1O	112.3 (15)	H32A—C32—H32C	109.5
C4—O2—H2O	110.7 (16)	H32B—C32—H32C	109.5
C9—O3—H3O	110.3 (17)	C34—C33—C21	112.40 (13)
C11—O4—H4O	107.4 (18)	C34—C33—H33A	109.1
C16—O5—H5O	110.3 (16)	C21—C33—H33A	109.1
C18—O6—H6O	111.6 (14)	C34—C33—H33B	109.1
C23—O7—H7O	107.9 (18)	C21—C33—H33B	109.1
C25—O8—H8O	110.6 (18)	H33A—C33—H33B	107.9
C6—C1—C2	116.39 (14)	C33—C34—H34A	109.5
C6—C1—C28	122.77 (14)	C33—C34—H34B	109.5
C2—C1—C28	120.82 (14)	H34A—C34—H34B	109.5
O1—C2—C3	116.12 (14)	C33—C34—H34C	109.5
O1—C2—C1	122.16 (14)	H34A—C34—H34C	109.5
C3—C2—C1	121.72 (14)	H34B—C34—H34C	109.5
C2—C3—C4	120.01 (14)	C36—C35—C28	112.61 (13)
C2—C3—H3A	120.0	C36—C35—H35A	109.1
C4—C3—H3A	120.0	C28—C35—H35A	109.1
O2—C4—C3	122.06 (14)	C36—C35—H35B	109.1
O2—C4—C5	117.32 (14)	C28—C35—H35B	109.1
C3—C4—C5	120.62 (14)	H35A—C35—H35B	107.8
C6—C5—C4	117.30 (14)	C35—C36—H36A	109.5
C6—C5—C7	123.36 (14)	C35—C36—H36B	109.5
C4—C5—C7	119.33 (14)	H36A—C36—H36B	109.5
C5—C6—C1	123.95 (14)	C35—C36—H36C	109.5
C5—C6—H6A	118.0	H36A—C36—H36C	109.5
C1—C6—H6A	118.0	H36B—C36—H36C	109.5
C5—C7—C8	111.41 (12)	C2S—O2S—H2S	109.2
C5—C7—C29	113.28 (13)	O2S—C2S—H2S1	109.5
C8—C7—C29	111.92 (13)	O2S—C2S—H2S2	109.5
C5—C7—H7A	106.6	H2S1—C2S—H2S2	109.5
C8—C7—H7A	106.6	O2S—C2S—H2S3	109.5
C29—C7—H7A	106.6	H2S1—C2S—H2S3	109.5
C9—C8—C13	116.64 (14)	H2S2—C2S—H2S3	109.5
C9—C8—C7	123.60 (14)	H1WA—O1W—H1WB	116.8
C13—C8—C7	119.75 (14)	H1WA—O1W—H2WB	77.8
O3—C9—C10	114.51 (14)	H1WB—O1W—H2WB	154.0
O3—C9—C8	124.39 (14)	H1WA—O1W—H3WA	106.8
C10—C9—C8	121.09 (14)	H1WB—O1W—H3WA	62.4
C11—C10—C9	120.15 (15)	H2WB—O1W—H3WA	93.5
C11—C10—H10A	119.9	H1WA—O1W—H3WB	127.3
C9—C10—H10A	119.9	H1WB—O1W—H3WB	112.7
C10—C11—O4	116.85 (14)	H2WB—O1W—H3WB	49.4
C10—C11—C12	121.25 (15)	H3WA—O1W—H3WB	80.7
O4—C11—C12	121.87 (14)	H2WA—O2W—H2WB	113.2
C11—C12—C13	116.84 (14)	H2WA—O2W—H3WA	105.7
C11—C12—C14	122.08 (14)	H2WB—O2W—H3WA	124.2
C13—C12—C14	121.05 (14)	H2WA—O2W—H3WB	170.6
C12—C13—C8	123.93 (15)	H2WB—O2W—H3WB	60.2
C12—C13—H13A	118.0	H3WA—O2W—H3WB	75.3
C8—C13—H13A	118.0	H3WA—O3W—H3WB	113.9
C15—C14—C12	110.54 (12)	C41—O10—H10O	108.3
C15—C14—C31	114.47 (13)	C41—O10—H10P	93.7
C12—C14—C31	111.57 (13)	H10O—O10—H10P	16.8
C15—C14—H14A	106.6	O9—C41—O10	122.0 (3)
C12—C14—H14A	106.6	O9—C41—C42	123.4 (2)
C31—C14—H14A	106.6	O10—C41—C42	114.6 (3)
C20—C15—C16	117.45 (14)	O9—C41—H10P	96.3
C20—C15—C14	123.39 (14)	O10—C41—H10P	25.9
C16—C15—C14	119.14 (14)	C42—C41—H10P	140.2
O5—C16—C17	121.05 (14)	C43—C42—C41	119.3 (2)
O5—C16—C15	117.73 (14)	C43—C42—C45	124.0 (3)
C17—C16—C15	121.21 (14)	C41—C42—C45	116.7 (3)
C16—C17—C18	119.74 (14)	C42—C43—C44	126.2 (3)
C16—C17—H17A	120.1	C42—C43—H43A	116.9
C18—C17—H17A	120.1	C44—C43—H43A	116.9
O6—C18—C17	115.29 (14)	C43—C44—H44A	109.5
O6—C18—C19	123.31 (14)	C43—C44—H44B	109.5
C17—C18—C19	121.38 (14)	H44A—C44—H44B	109.5
C18—C19—C20	116.78 (14)	C43—C44—H44C	109.5
C18—C19—C21	120.88 (14)	H44A—C44—H44C	109.5
C20—C19—C21	122.32 (14)	H44B—C44—H44C	109.5
C15—C20—C19	123.42 (14)	C42—C45—H45A	109.5
C15—C20—H20A	118.3	C42—C45—H45B	109.5
C19—C20—H20A	118.3	H45A—C45—H45B	109.5
C19—C21—C22	111.24 (12)	C42—C45—H45C	109.5
C19—C21—C33	112.95 (13)	H45A—C45—H45C	109.5
C22—C21—C33	112.18 (13)	H45B—C45—H45C	109.5
C19—C21—H21A	106.7	C1S—O1S—H1S	102.8
C22—C21—H21A	106.7	C1S—O1S—H1SP	55.5
C33—C21—H21A	106.7	H1S—O1S—H1SP	79.6
C27—C22—C23	117.13 (14)	O1S—C1S—H1S1	109.5
C27—C22—C21	122.05 (14)	O1S—C1S—H1S2	109.5
C23—C22—C21	120.81 (14)	H1S1—C1S—H1S2	109.5
O7—C23—C24	121.11 (14)	O1S—C1S—H1S3	109.5
O7—C23—C22	117.42 (14)	H1S1—C1S—H1S3	109.5
C24—C23—C22	121.46 (14)	H1S2—C1S—H1S3	109.5
C23—C24—C25	119.43 (15)	O1S—C1S—H1SP	33.3
C23—C24—H24A	120.3	H1S1—C1S—H1SP	115.9
C25—C24—H24A	120.3	H1S2—C1S—H1SP	76.9
O8—C25—C24	120.96 (14)	H1S3—C1S—H1SP	128.8
O8—C25—C26	117.71 (14)	C41B—O10B—H10O	123.2
C24—C25—C26	121.33 (14)	C41B—O10B—H10P	118.0
C27—C26—C25	117.26 (14)	H10O—O10B—H10P	7.8
C27—C26—C28	121.69 (14)	O9B—C41B—O10B	121 (3)
C25—C26—C28	121.04 (14)	O9B—C41B—C42B	118 (2)
C26—C27—C22	123.38 (14)	O10B—C41B—C42B	121 (2)
C26—C27—H27A	118.3	C43B—C42B—C41B	126 (2)
C22—C27—H27A	118.3	C43B—C42B—C45B	123 (2)
C1—C28—C26	110.48 (12)	C41B—C42B—C45B	111 (2)
C1—C28—C35	113.56 (13)	C42B—C43B—C44B	128.2 (19)
C26—C28—C35	112.21 (13)	C42B—C43B—H43B	115.9
C1—C28—H28A	106.7	C44B—C43B—H43B	115.9
C26—C28—H28A	106.7	C43B—C44B—H44D	109.5
C35—C28—H28A	106.7	C43B—C44B—H44E	109.5
C30—C29—C7	112.61 (14)	H44D—C44B—H44E	109.5
C30—C29—H29A	109.1	C43B—C44B—H44F	109.5
C7—C29—H29A	109.1	H44D—C44B—H44F	109.5
C30—C29—H29B	109.1	H44E—C44B—H44F	109.5
C7—C29—H29B	109.1	C42B—C45B—H45D	109.5
H29A—C29—H29B	107.8	C42B—C45B—H45E	109.5
C29—C30—H30A	109.5	H45D—C45B—H45E	109.5
C29—C30—H30B	109.5	C42B—C45B—H45F	109.5
H30A—C30—H30B	109.5	H45D—C45B—H45F	109.5
C29—C30—H30C	109.5	H45E—C45B—H45F	109.5
H30A—C30—H30C	109.5	C1SB—O1SB—H1SP	93.0
H30B—C30—H30C	109.5	O1SB—C1SB—H1S	71.8
C32—C31—C14	111.49 (14)	O1SB—C1SB—H1S4	109.5
C32—C31—H31A	109.3	H1S—C1SB—H1S4	75.1
C14—C31—H31A	109.3	O1SB—C1SB—H1S5	109.5
C32—C31—H31B	109.3	H1S—C1SB—H1S5	64.9
C14—C31—H31B	109.3	H1S4—C1SB—H1S5	109.5
H31A—C31—H31B	108.0	O1SB—C1SB—H1S6	109.5
C31—C32—H32A	109.5	H1S—C1SB—H1S6	174.0
C31—C32—H32B	109.5	H1S4—C1SB—H1S6	109.5
H32A—C32—H32B	109.5	H1S5—C1SB—H1S6	109.5
C31—C32—H32C	109.5

(CECR-HTA-2MeOH-1.5H2O@90k-3h-exposure)

Crystal data

C43H59O13.50	F(000) = 850
Mr = 791.90	Dx = 1.263 Mg m^−3
Triclinic, P1	Melting point: not measured K
a = 11.2902 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.1299 (6) Å	Cell parameters from 865 reflections
c = 14.7991 (6) Å	θ = 2.5–25°
α = 108.5839 (13)°	µ = 0.09 mm^−1
β = 109.2657 (12)°	T = 90 K
γ = 92.5600 (13)°	Block, pale yellow
V = 2082.65 (14) Å^3	0.14 × 0.10 × 0.08 mm
Z = 2

Data collection

CCD area detector diffractometer	7340 independent reflections
Radiation source: fine-focus sealed tube	5019 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
phi and ω scans	θmax = 25.0°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements) Blessing, R. (1995) Acta Crystallogr., A51, 33-38	h = −13→13
Tmin = 0.987, Tmax = 0.993	k = −16→16
16761 measured reflections	l = −17→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.056	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.157	H atoms treated by a mixture of independent and constrained refinement
S = 1.17	w = 1/[σ^2(Fo^2) + (0.0601P)^2 + 1.1813P] where P = (Fo^2 + 2Fc^2)/3
7340 reflections	(Δ/σ)max = 0.003
581 parameters	Δρmax = 0.48 e Å^−3
7 restraints	Δρmin = −0.41 e Å^−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)
O1	−0.2315 (2)	0.46510 (15)	−0.05426 (16)	0.0238 (5)
O2	0.13606 (18)	0.46880 (16)	0.22163 (15)	0.0266 (5)
O3	0.26250 (18)	0.41100 (15)	0.39645 (16)	0.0252 (5)
O4	0.0091 (2)	0.36463 (16)	0.57923 (14)	0.0279 (5)
O5	−0.24026 (18)	0.38947 (17)	0.51763 (15)	0.0247 (5)
O6	−0.61908 (18)	0.38957 (15)	0.25527 (16)	0.0250 (5)
O7	−0.73433 (18)	0.34642 (16)	0.05029 (15)	0.0240 (5)
O8	−0.4898 (2)	0.39368 (16)	−0.14886 (16)	0.0270 (5)
C1	−0.2051 (2)	0.3110 (2)	−0.01534 (19)	0.0179 (6)
C2	−0.1641 (2)	0.4121 (2)	0.0037 (2)	0.0193 (6)
C3	−0.0511 (2)	0.4660 (2)	0.0818 (2)	0.0212 (6)
H3A	−0.0255	0.5351	0.0931	0.025*
C4	0.0248 (2)	0.4189 (2)	0.1435 (2)	0.0204 (6)
C5	−0.0116 (2)	0.3166 (2)	0.1269 (2)	0.0187 (6)
C6	−0.1259 (2)	0.2660 (2)	0.04806 (19)	0.0178 (6)
H6A	−0.1518	0.1969	0.0365	0.021*
C7	0.0744 (2)	0.2665 (2)	0.1943 (2)	0.0193 (6)
H7A	0.1639	0.2953	0.2083	0.023*
C8	0.0589 (2)	0.29459 (19)	0.2981 (2)	0.0189 (6)
C9	0.1491 (2)	0.3611 (2)	0.3889 (2)	0.0209 (6)
C10	0.1303 (3)	0.3841 (2)	0.4812 (2)	0.0237 (6)
H10A	0.1925	0.4306	0.5422	0.028*
C11	0.0208 (3)	0.3390 (2)	0.4840 (2)	0.0215 (6)
C12	−0.0705 (2)	0.2695 (2)	0.3964 (2)	0.0201 (6)
C13	−0.0498 (2)	0.2512 (2)	0.3053 (2)	0.0198 (6)
H13A	−0.1135	0.2065	0.2440	0.024*
C14	−0.1869 (2)	0.2118 (2)	0.3990 (2)	0.0204 (6)
H14A	−0.1718	0.2253	0.4728	0.024*
C15	−0.3052 (2)	0.2549 (2)	0.3579 (2)	0.0188 (6)
C16	−0.3270 (2)	0.3445 (2)	0.4196 (2)	0.0196 (6)
C17	−0.4322 (2)	0.3872 (2)	0.3835 (2)	0.0215 (6)
H17A	−0.4463	0.4477	0.4271	0.026*
C18	−0.5174 (2)	0.3415 (2)	0.2834 (2)	0.0190 (6)
C19	−0.5005 (2)	0.25107 (19)	0.21841 (19)	0.0172 (6)
C20	−0.3936 (2)	0.2105 (2)	0.2585 (2)	0.0185 (6)
H20A	−0.3803	0.1490	0.2156	0.022*
C21	−0.5937 (2)	0.20157 (19)	0.10869 (19)	0.0175 (6)
H21A	−0.6798	0.2138	0.1098	0.021*
C22	−0.5674 (2)	0.25265 (19)	0.03860 (19)	0.0169 (6)
C23	−0.6392 (2)	0.3233 (2)	0.0109 (2)	0.0193 (6)
C24	−0.6162 (3)	0.3694 (2)	−0.0525 (2)	0.0233 (6)
H24A	−0.6677	0.4163	−0.0718	0.028*
C25	−0.5174 (2)	0.3469 (2)	−0.0879 (2)	0.0211 (6)
C26	−0.4415 (2)	0.27777 (19)	−0.06123 (19)	0.0177 (6)
C27	−0.4690 (2)	0.23274 (19)	0.00200 (19)	0.0175 (6)
H27A	−0.4177	0.1858	0.0213	0.021*
C28	−0.3320 (2)	0.25415 (19)	−0.0995 (2)	0.0187 (6)
H28A	−0.3446	0.2815	−0.1560	0.022*
C29	0.0596 (3)	0.1514 (2)	0.1419 (2)	0.0234 (6)
H29A	−0.0264	0.1194	0.1304	0.028*
H29B	0.0674	0.1369	0.0743	0.028*
C30	0.1589 (3)	0.1050 (2)	0.2051 (2)	0.0315 (7)
H30A	0.2443	0.1390	0.2199	0.047*
H30B	0.1499	0.0327	0.1666	0.047*
H30C	0.1464	0.1135	0.2695	0.047*
C31	−0.1986 (3)	0.0971 (2)	0.3487 (2)	0.0257 (6)
H31A	−0.2778	0.0630	0.3476	0.031*
H31B	−0.2044	0.0809	0.2770	0.031*
C32	−0.0853 (3)	0.0570 (2)	0.4055 (3)	0.0389 (8)
H32A	−0.0069	0.0892	0.4051	0.058*
H32B	−0.0963	−0.0165	0.3716	0.058*
H32C	−0.0798	0.0724	0.4763	0.058*
C33	−0.6016 (2)	0.08657 (19)	0.0663 (2)	0.0200 (6)
H33A	−0.5201	0.0713	0.0583	0.024*
H33B	−0.6132	0.0578	0.1162	0.024*
C34	−0.7098 (3)	0.0356 (2)	−0.0363 (2)	0.0267 (7)
H34A	−0.7910	0.0492	−0.0287	0.040*
H34B	−0.7104	−0.0376	−0.0595	0.040*
H34C	−0.6977	0.0624	−0.0867	0.040*
C35	−0.3350 (3)	0.1399 (2)	−0.1459 (2)	0.0221 (6)
H35A	−0.2621	0.1286	−0.1689	0.026*
H35B	−0.3247	0.1099	−0.0923	0.026*
C36	−0.4574 (3)	0.0860 (2)	−0.2358 (2)	0.0304 (7)
H36A	−0.5293	0.0922	−0.2124	0.046*
H36B	−0.4521	0.0143	−0.2647	0.046*
H36C	−0.4696	0.1168	−0.2882	0.046*
O2S	0.8495 (3)	0.7326 (3)	0.3028 (2)	0.0752 (9)
H2S	0.9066	0.7029	0.3486	0.113*
C2S	0.7624 (2)	0.77789 (19)	0.34678 (19)	0.0601 (11)
H2S1	0.8095	0.8303	0.4136	0.090*
H2S2	0.7109	0.7261	0.3554	0.090*
H2S3	0.7067	0.8085	0.3017	0.090*
O1W	0.2549 (2)	0.55362 (19)	0.76962 (19)	0.0256 (7)	0.60
H1WA	0.1892	0.5043	0.7193	0.038*	0.60
H1WB	0.2426	0.5872	0.8299	0.038*	0.60
O2W	0.3117 (5)	0.4678 (4)	0.7609 (3)	0.0612 (13)	0.60
H2WA	0.2648	0.4088	0.7410	0.092*	0.60
H2WB	0.3162	0.4861	0.7073	0.092*	0.60
O3W	0.3705 (5)	0.5356 (5)	0.8311 (5)	0.0202 (13)	0.30
H3WA	0.2914	0.5248	0.8348	0.030*	0.30
H3WB	0.3716	0.5614	0.7813	0.030*	0.30
H1O	−0.302 (3)	0.435 (2)	−0.089 (2)	0.030 (9)*
H2O	0.149 (3)	0.530 (3)	0.228 (3)	0.052 (12)*
H3O	0.261 (4)	0.405 (3)	0.341 (3)	0.060 (13)*
H4O	−0.072 (5)	0.375 (3)	0.568 (4)	0.091 (16)*
H5O	−0.254 (4)	0.442 (3)	0.545 (3)	0.052 (13)*
H6O	−0.651 (3)	0.374 (2)	0.191 (3)	0.029 (9)*
H7O	−0.757 (4)	0.394 (3)	0.037 (3)	0.064 (14)*
H8O	−0.545 (4)	0.424 (3)	−0.170 (3)	0.064 (13)*
O9	0.1867 (4)	0.6778 (3)	0.2663 (4)	0.0409 (10)	0.743 (6)
O10	0.2246 (7)	0.8403 (6)	0.3626 (8)	0.0658 (16)	0.743 (6)
H10O	0.1410	0.8360	0.3165	0.099*	0.743 (6)
C41	0.2632 (9)	0.7510 (4)	0.3366 (6)	0.0445 (17)	0.743 (6)
C42	0.3895 (7)	0.7450 (7)	0.4046 (8)	0.049 (2)	0.743 (6)
C43	0.4514 (6)	0.8251 (5)	0.4860 (5)	0.0627 (18)	0.743 (6)
H43A	0.4122	0.8837	0.4975	0.075*	0.743 (6)
C44	0.5810 (6)	0.8295 (5)	0.5624 (5)	0.0808 (19)	0.743 (6)
H44A	0.5725	0.8274	0.6255	0.121*	0.743 (6)
H44B	0.6360	0.8925	0.5775	0.121*	0.743 (6)
H44C	0.6186	0.7715	0.5337	0.121*	0.743 (6)
C45	0.4391 (13)	0.6457 (7)	0.3673 (9)	0.053 (2)	0.743 (6)
H45A	0.4774	0.6491	0.3176	0.080*	0.743 (6)
H45B	0.3682	0.5888	0.3349	0.080*	0.743 (6)
H45C	0.5032	0.6362	0.4257	0.080*	0.743 (6)
O1S	0.0062 (4)	0.8433 (3)	0.2536 (3)	0.0604 (12)	0.737 (5)
H1S	−0.0550	0.7944	0.2627	0.091*	0.737 (5)
C1S	−0.0244 (9)	0.8007 (5)	0.1417 (6)	0.0561 (19)	0.737 (5)
H1S1	0.0236	0.8447	0.1218	0.084*	0.737 (5)
H1S2	−0.1158	0.7960	0.1059	0.084*	0.737 (5)
H1S3	−0.0012	0.7330	0.1233	0.084*	0.737 (5)
O9B	0.2292 (14)	0.6585 (11)	0.2658 (13)	0.0409 (10)	0.257 (6)
O10B	0.262 (3)	0.826 (2)	0.370 (3)	0.0658 (16)	0.257 (6)
H10P	0.1884	0.8293	0.3322	0.099*	0.257 (6)
C41B	0.278 (3)	0.7294 (16)	0.3462 (19)	0.0445 (17)	0.257 (6)
C42B	0.415 (3)	0.731 (2)	0.396 (3)	0.049 (2)	0.257 (6)
C43B	0.505 (2)	0.8013 (14)	0.4719 (16)	0.0627 (18)	0.257 (6)
H43B	0.5833	0.7806	0.5012	0.075*	0.257 (6)
C44B	0.4958 (18)	0.9141 (14)	0.5187 (14)	0.0808 (19)	0.257 (6)
H44D	0.4735	0.9437	0.4649	0.121*	0.257 (6)
H44E	0.5779	0.9506	0.5717	0.121*	0.257 (6)
H44F	0.4301	0.9196	0.5490	0.121*	0.257 (6)
C45B	0.436 (4)	0.621 (3)	0.376 (3)	0.053 (2)	0.257 (6)
H45D	0.3644	0.5823	0.3798	0.080*	0.257 (6)
H45E	0.5152	0.6188	0.4277	0.080*	0.257 (6)
H45F	0.4399	0.5916	0.3077	0.080*	0.257 (6)
O1SB	−0.030 (2)	0.8260 (11)	0.1607 (15)	0.0604 (12)	0.263 (5)
H1SP	−0.0672	0.8494	0.2031	0.091*	0.263 (5)
C1SB	−0.0403 (15)	0.7261 (10)	0.1728 (12)	0.0561 (19)	0.263 (5)
H1S4	−0.1282	0.7037	0.1637	0.084*	0.263 (5)
H1S5	0.0166	0.7319	0.2413	0.084*	0.263 (5)
H1S6	−0.0160	0.6767	0.1212	0.084*	0.263 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0225 (11)	0.0211 (11)	0.0301 (12)	0.0048 (9)	0.0065 (10)	0.0148 (9)
O2	0.0224 (11)	0.0195 (12)	0.0318 (12)	−0.0019 (9)	0.0030 (9)	0.0089 (10)
O3	0.0210 (10)	0.0300 (12)	0.0235 (11)	−0.0001 (8)	0.0100 (9)	0.0065 (9)
O4	0.0254 (11)	0.0392 (13)	0.0190 (10)	0.0027 (9)	0.0097 (9)	0.0087 (9)
O5	0.0249 (11)	0.0264 (12)	0.0175 (10)	0.0039 (9)	0.0056 (9)	0.0028 (9)
O6	0.0213 (10)	0.0278 (11)	0.0226 (11)	0.0107 (8)	0.0065 (9)	0.0054 (9)
O7	0.0243 (11)	0.0252 (12)	0.0322 (12)	0.0114 (9)	0.0166 (9)	0.0150 (10)
O8	0.0283 (11)	0.0339 (12)	0.0309 (12)	0.0123 (10)	0.0140 (10)	0.0228 (10)
C1	0.0199 (14)	0.0203 (14)	0.0180 (14)	0.0052 (11)	0.0121 (12)	0.0071 (12)
C2	0.0241 (14)	0.0208 (14)	0.0199 (14)	0.0084 (11)	0.0125 (12)	0.0109 (12)
C3	0.0246 (14)	0.0168 (14)	0.0253 (15)	0.0038 (11)	0.0124 (13)	0.0083 (12)
C4	0.0194 (14)	0.0210 (15)	0.0221 (14)	0.0026 (11)	0.0106 (12)	0.0063 (12)
C5	0.0195 (14)	0.0228 (15)	0.0180 (14)	0.0065 (11)	0.0115 (12)	0.0072 (12)
C6	0.0209 (14)	0.0175 (14)	0.0212 (14)	0.0054 (11)	0.0124 (12)	0.0094 (12)
C7	0.0184 (13)	0.0205 (14)	0.0211 (14)	0.0043 (11)	0.0092 (12)	0.0078 (12)
C8	0.0197 (14)	0.0194 (14)	0.0201 (14)	0.0076 (11)	0.0068 (12)	0.0100 (12)
C9	0.0164 (13)	0.0228 (15)	0.0244 (15)	0.0046 (11)	0.0081 (12)	0.0085 (12)
C10	0.0206 (14)	0.0246 (15)	0.0221 (15)	0.0027 (12)	0.0051 (12)	0.0061 (12)
C11	0.0226 (14)	0.0245 (15)	0.0205 (14)	0.0074 (12)	0.0099 (12)	0.0091 (12)
C12	0.0186 (14)	0.0228 (15)	0.0230 (15)	0.0070 (11)	0.0084 (12)	0.0118 (12)
C13	0.0176 (13)	0.0211 (14)	0.0205 (14)	0.0066 (11)	0.0050 (12)	0.0087 (12)
C14	0.0201 (14)	0.0234 (15)	0.0189 (14)	0.0032 (11)	0.0057 (12)	0.0106 (12)
C15	0.0188 (13)	0.0215 (15)	0.0208 (14)	0.0022 (11)	0.0099 (12)	0.0108 (12)
C16	0.0199 (14)	0.0222 (15)	0.0169 (14)	−0.0002 (11)	0.0077 (12)	0.0066 (12)
C17	0.0219 (14)	0.0221 (15)	0.0215 (15)	0.0054 (12)	0.0118 (12)	0.0046 (12)
C18	0.0165 (13)	0.0217 (15)	0.0227 (14)	0.0041 (11)	0.0086 (12)	0.0111 (12)
C19	0.0179 (13)	0.0174 (14)	0.0194 (14)	0.0008 (11)	0.0090 (12)	0.0086 (11)
C20	0.0215 (14)	0.0178 (14)	0.0199 (14)	0.0043 (11)	0.0110 (12)	0.0080 (11)
C21	0.0160 (13)	0.0177 (14)	0.0202 (14)	0.0025 (10)	0.0082 (11)	0.0069 (11)
C22	0.0176 (13)	0.0170 (14)	0.0152 (13)	0.0015 (11)	0.0050 (11)	0.0058 (11)
C23	0.0180 (13)	0.0188 (14)	0.0230 (14)	0.0030 (11)	0.0094 (12)	0.0078 (12)
C24	0.0222 (14)	0.0230 (15)	0.0288 (16)	0.0089 (12)	0.0092 (13)	0.0139 (13)
C25	0.0213 (14)	0.0231 (15)	0.0212 (14)	0.0027 (12)	0.0074 (12)	0.0113 (12)
C26	0.0173 (13)	0.0178 (14)	0.0151 (13)	0.0017 (11)	0.0038 (11)	0.0045 (11)
C27	0.0183 (13)	0.0153 (14)	0.0163 (13)	0.0025 (10)	0.0035 (11)	0.0052 (11)
C28	0.0205 (14)	0.0203 (14)	0.0181 (14)	0.0058 (11)	0.0087 (12)	0.0083 (12)
C29	0.0262 (15)	0.0214 (15)	0.0250 (15)	0.0067 (12)	0.0112 (13)	0.0088 (12)
C30	0.0329 (17)	0.0300 (17)	0.0410 (19)	0.0157 (14)	0.0187 (15)	0.0178 (15)
C31	0.0258 (15)	0.0240 (16)	0.0267 (16)	0.0045 (12)	0.0067 (13)	0.0112 (13)
C32	0.0402 (19)	0.0289 (18)	0.045 (2)	0.0114 (14)	0.0064 (16)	0.0177 (16)
C33	0.0218 (14)	0.0162 (14)	0.0232 (14)	0.0036 (11)	0.0092 (12)	0.0074 (12)
C34	0.0267 (15)	0.0230 (15)	0.0275 (16)	0.0039 (12)	0.0086 (13)	0.0066 (13)
C35	0.0237 (14)	0.0215 (15)	0.0204 (14)	0.0032 (11)	0.0077 (12)	0.0070 (12)
C36	0.0333 (17)	0.0268 (16)	0.0260 (16)	0.0031 (13)	0.0077 (14)	0.0061 (13)
O2S	0.0633 (18)	0.111 (3)	0.073 (2)	0.0332 (18)	0.0253 (16)	0.057 (2)
C2S	0.044 (2)	0.062 (3)	0.067 (3)	0.005 (2)	0.008 (2)	0.027 (2)
O1W	0.0276 (18)	0.0258 (18)	0.0209 (17)	0.0055 (14)	0.0105 (15)	0.0032 (14)
O2W	0.084 (3)	0.057 (3)	0.042 (3)	0.046 (3)	0.009 (3)	0.025 (2)
O3W	0.013 (3)	0.019 (3)	0.021 (3)	0.001 (3)	−0.004 (3)	0.009 (3)
O9	0.052 (3)	0.026 (2)	0.0396 (15)	0.0113 (17)	0.015 (2)	0.0062 (16)
O10	0.073 (5)	0.049 (3)	0.066 (3)	0.018 (2)	0.018 (4)	0.015 (2)
C41	0.080 (4)	0.022 (4)	0.037 (3)	−0.002 (3)	0.022 (2)	0.019 (3)
C42	0.052 (5)	0.061 (4)	0.040 (3)	−0.004 (3)	0.021 (3)	0.022 (3)
C43	0.063 (5)	0.071 (4)	0.048 (3)	−0.010 (3)	0.022 (3)	0.015 (3)
C44	0.063 (4)	0.095 (5)	0.066 (4)	−0.004 (3)	0.008 (3)	0.022 (4)
C45	0.061 (3)	0.067 (7)	0.044 (3)	−0.008 (5)	0.028 (2)	0.030 (4)
O1S	0.079 (3)	0.055 (2)	0.053 (2)	0.0196 (19)	0.035 (2)	0.015 (2)
C1S	0.059 (3)	0.044 (4)	0.054 (4)	0.011 (3)	0.016 (3)	0.006 (3)
O9B	0.052 (3)	0.026 (2)	0.0396 (15)	0.0113 (17)	0.015 (2)	0.0062 (16)
O10B	0.073 (5)	0.049 (3)	0.066 (3)	0.018 (2)	0.018 (4)	0.015 (2)
C41B	0.080 (4)	0.022 (4)	0.037 (3)	−0.002 (3)	0.022 (2)	0.019 (3)
C42B	0.052 (5)	0.061 (4)	0.040 (3)	−0.004 (3)	0.021 (3)	0.022 (3)
C43B	0.063 (5)	0.071 (4)	0.048 (3)	−0.010 (3)	0.022 (3)	0.015 (3)
C44B	0.063 (4)	0.095 (5)	0.066 (4)	−0.004 (3)	0.008 (3)	0.022 (4)
C45B	0.061 (3)	0.067 (7)	0.044 (3)	−0.008 (5)	0.028 (2)	0.030 (4)
O1SB	0.079 (3)	0.055 (2)	0.053 (2)	0.0196 (19)	0.035 (2)	0.015 (2)
C1SB	0.059 (3)	0.044 (4)	0.054 (4)	0.011 (3)	0.016 (3)	0.006 (3)

Geometric parameters (Å, º)

O1—C2	1.381 (3)	C32—H32B	0.9800
O1—H1O	0.80 (3)	C32—H32C	0.9800
O2—C4	1.362 (3)	C33—C34	1.522 (4)
O2—H2O	0.84 (4)	C33—H33A	0.9900
O3—C9	1.388 (3)	C33—H33B	0.9900
O3—H3O	0.80 (4)	C34—H34A	0.9800
O4—C11	1.391 (3)	C34—H34B	0.9800
O4—H4O	0.91 (5)	C34—H34C	0.9800
O5—C16	1.374 (3)	C35—C36	1.518 (4)
O5—H5O	0.77 (4)	C35—H35A	0.9900
O6—C18	1.374 (3)	C35—H35B	0.9900
O6—H6O	0.85 (3)	C36—H36A	0.9800
O7—C23	1.386 (3)	C36—H36B	0.9800
O7—H7O	0.78 (4)	C36—H36C	0.9800
O8—C25	1.376 (3)	O2S—C2S	1.418 (4)
O8—H8O	0.80 (4)	O2S—H2S	0.9834
C1—C2	1.390 (4)	C2S—H2S1	0.9800
C1—C6	1.401 (4)	C2S—H2S2	0.9800
C1—C28	1.527 (4)	C2S—H2S3	0.9800
C2—C3	1.387 (4)	O1W—H1WA	0.9218
C3—C4	1.391 (4)	O1W—H1WB	0.9264
C3—H3A	0.9500	O1W—H2WB	1.4689
C4—C5	1.405 (4)	O1W—H3WA	1.1261
C5—C6	1.389 (4)	O1W—H3WB	1.2654
C5—C7	1.520 (4)	O2W—H2WA	0.8738
C6—H6A	0.9500	O2W—H2WB	0.9244
C7—C8	1.532 (4)	O2W—H3WA	1.2321
C7—C29	1.536 (4)	O2W—H3WB	1.3520
C7—H7A	1.0000	O3W—H3WA	0.9212
C8—C9	1.390 (4)	O3W—H3WB	0.9240
C8—C13	1.398 (4)	O9—C41	1.240 (6)
C9—C10	1.388 (4)	O10—C41	1.335 (7)
C10—C11	1.385 (4)	O10—H10O	0.9506
C10—H10A	0.9500	O10—H10P	0.4710
C11—C12	1.387 (4)	C41—C42	1.473 (8)
C12—C13	1.390 (4)	C41—H10P	1.4271
C12—C14	1.533 (4)	C42—C43	1.314 (8)
C13—H13A	0.9500	C42—C45	1.538 (8)
C14—C15	1.517 (4)	C43—C44	1.510 (8)
C14—C31	1.531 (4)	C43—H43A	0.9500
C14—H14A	1.0000	C44—H44A	0.9800
C15—C16	1.391 (4)	C44—H44B	0.9800
C15—C20	1.393 (4)	C44—H44C	0.9800
C16—C17	1.382 (4)	C45—H45A	0.9800
C17—C18	1.389 (4)	C45—H45B	0.9800
C17—H17A	0.9500	C45—H45C	0.9800
C18—C19	1.397 (4)	O1S—C1S	1.481 (8)
C19—C20	1.394 (4)	O1S—H1S	1.0253
C19—C21	1.522 (4)	O1S—H1SP	0.9432
C20—H20A	0.9500	C1S—H1S1	0.9800
C21—C33	1.531 (4)	C1S—H1S2	0.9800
C21—C22	1.532 (4)	C1S—H1S3	0.9800
C21—H21A	1.0000	C1S—H1SP	1.2060
C22—C27	1.391 (4)	O9B—C41B	1.217 (16)
C22—C23	1.391 (4)	O10B—C41B	1.339 (16)
C23—C24	1.382 (4)	O10B—H10O	1.3701
C24—C25	1.390 (4)	O10B—H10P	0.8441
C24—H24A	0.9500	C41B—C42B	1.476 (18)
C25—C26	1.393 (4)	C42B—C43B	1.312 (17)
C26—C27	1.389 (4)	C42B—C45B	1.535 (18)
C26—C28	1.530 (4)	C43B—C44B	1.547 (17)
C27—H27A	0.9500	C43B—H43B	0.9500
C28—C35	1.534 (4)	C44B—H44D	0.9800
C28—H28A	1.0000	C44B—H44E	0.9800
C29—C30	1.525 (4)	C44B—H44F	0.9800
C29—H29A	0.9900	C45B—H45D	0.9800
C29—H29B	0.9900	C45B—H45E	0.9800
C30—H30A	0.9800	C45B—H45F	0.9800
C30—H30B	0.9800	O1SB—C1SB	1.482 (15)
C30—H30C	0.9800	O1SB—H1SP	0.8551
C31—C32	1.524 (4)	C1SB—H1S	1.4395
C31—H31A	0.9900	C1SB—H1S4	0.9800
C31—H31B	0.9900	C1SB—H1S5	0.9800
C32—H32A	0.9800	C1SB—H1S6	0.9800
C2—O1—H1O	111 (2)	H32A—C32—H32C	109.5
C4—O2—H2O	111 (3)	H32B—C32—H32C	109.5
C9—O3—H3O	110 (3)	C34—C33—C21	113.1 (2)
C11—O4—H4O	105 (3)	C34—C33—H33A	109.0
C16—O5—H5O	112 (3)	C21—C33—H33A	109.0
C18—O6—H6O	111 (2)	C34—C33—H33B	109.0
C23—O7—H7O	106 (3)	C21—C33—H33B	109.0
C25—O8—H8O	112 (3)	H33A—C33—H33B	107.8
C2—C1—C6	116.6 (2)	C33—C34—H34A	109.5
C2—C1—C28	120.9 (2)	C33—C34—H34B	109.5
C6—C1—C28	122.5 (2)	H34A—C34—H34B	109.5
O1—C2—C3	115.5 (2)	C33—C34—H34C	109.5
O1—C2—C1	122.6 (2)	H34A—C34—H34C	109.5
C3—C2—C1	121.9 (2)	H34B—C34—H34C	109.5
C2—C3—C4	119.9 (2)	C36—C35—C28	113.0 (2)
C2—C3—H3A	120.1	C36—C35—H35A	109.0
C4—C3—H3A	120.1	C28—C35—H35A	109.0
O2—C4—C3	122.1 (2)	C36—C35—H35B	109.0
O2—C4—C5	117.4 (2)	C28—C35—H35B	109.0
C3—C4—C5	120.5 (2)	H35A—C35—H35B	107.8
C6—C5—C4	117.4 (2)	C35—C36—H36A	109.5
C6—C5—C7	123.3 (2)	C35—C36—H36B	109.5
C4—C5—C7	119.3 (2)	H36A—C36—H36B	109.5
C5—C6—C1	123.7 (2)	C35—C36—H36C	109.5
C5—C6—H6A	118.1	H36A—C36—H36C	109.5
C1—C6—H6A	118.1	H36B—C36—H36C	109.5
C5—C7—C8	111.3 (2)	C2S—O2S—H2S	109.6
C5—C7—C29	113.4 (2)	O2S—C2S—H2S1	109.5
C8—C7—C29	112.0 (2)	O2S—C2S—H2S2	109.5
C5—C7—H7A	106.6	H2S1—C2S—H2S2	109.5
C8—C7—H7A	106.6	O2S—C2S—H2S3	109.5
C29—C7—H7A	106.6	H2S1—C2S—H2S3	109.5
C9—C8—C13	116.4 (2)	H2S2—C2S—H2S3	109.5
C9—C8—C7	123.7 (2)	H1WA—O1W—H1WB	116.8
C13—C8—C7	119.9 (2)	H1WA—O1W—H2WB	75.4
O3—C9—C10	114.2 (2)	H1WB—O1W—H2WB	154.4
O3—C9—C8	124.4 (2)	H1WA—O1W—H3WA	105.9
C10—C9—C8	121.4 (2)	H1WB—O1W—H3WA	61.9
C11—C10—C9	119.8 (3)	H2WB—O1W—H3WA	93.7
C11—C10—H10A	120.1	H1WA—O1W—H3WB	127.4
C9—C10—H10A	120.1	H1WB—O1W—H3WB	112.1
C10—C11—C12	121.3 (2)	H2WB—O1W—H3WB	52.0
C10—C11—O4	116.7 (2)	H3WA—O1W—H3WB	80.6
C12—C11—O4	122.0 (2)	H2WA—O2W—H2WB	113.4
C11—C12—C13	116.9 (2)	H2WA—O2W—H3WA	107.6
C11—C12—C14	122.3 (2)	H2WB—O2W—H3WA	123.9
C13—C12—C14	120.8 (2)	H2WA—O2W—H3WB	172.2
C12—C13—C8	124.1 (3)	H2WB—O2W—H3WB	61.0
C12—C13—H13A	118.0	H3WA—O2W—H3WB	73.6
C8—C13—H13A	118.0	H3WA—O3W—H3WB	114.4
C15—C14—C31	114.8 (2)	C41—O10—H10O	109.7
C15—C14—C12	110.4 (2)	C41—O10—H10P	91.5
C31—C14—C12	111.8 (2)	H10O—O10—H10P	20.4
C15—C14—H14A	106.4	O9—C41—O10	118.7 (8)
C31—C14—H14A	106.4	O9—C41—C42	125.0 (6)
C12—C14—H14A	106.4	O10—C41—C42	115.7 (7)
C16—C15—C20	117.2 (2)	O9—C41—H10P	100.0
C16—C15—C14	119.8 (2)	O10—C41—H10P	19.3
C20—C15—C14	123.0 (2)	C42—C41—H10P	134.8
O5—C16—C17	121.0 (2)	C43—C42—C41	118.2 (7)
O5—C16—C15	117.8 (2)	C43—C42—C45	126.5 (9)
C17—C16—C15	121.2 (2)	C41—C42—C45	115.1 (8)
C16—C17—C18	120.0 (2)	C42—C43—C44	123.9 (8)
C16—C17—H17A	120.0	C42—C43—H43A	118.1
C18—C17—H17A	120.0	C44—C43—H43A	118.1
O6—C18—C17	115.4 (2)	C43—C44—H44A	109.5
O6—C18—C19	123.4 (2)	C43—C44—H44B	109.5
C17—C18—C19	121.1 (2)	H44A—C44—H44B	109.5
C20—C19—C18	116.8 (2)	C43—C44—H44C	109.5
C20—C19—C21	122.3 (2)	H44A—C44—H44C	109.5
C18—C19—C21	121.0 (2)	H44B—C44—H44C	109.5
C15—C20—C19	123.7 (2)	C42—C45—H45A	109.5
C15—C20—H20A	118.2	C42—C45—H45B	109.5
C19—C20—H20A	118.2	H45A—C45—H45B	109.5
C19—C21—C33	113.4 (2)	C42—C45—H45C	109.5
C19—C21—C22	111.4 (2)	H45A—C45—H45C	109.5
C33—C21—C22	112.2 (2)	H45B—C45—H45C	109.5
C19—C21—H21A	106.4	C1S—O1S—H1S	101.3
C33—C21—H21A	106.4	C1S—O1S—H1SP	54.4
C22—C21—H21A	106.4	H1S—O1S—H1SP	84.8
C27—C22—C23	117.0 (2)	O1S—C1S—H1S1	109.5
C27—C22—C21	121.8 (2)	O1S—C1S—H1S2	109.5
C23—C22—C21	121.2 (2)	H1S1—C1S—H1S2	109.5
C24—C23—O7	121.2 (2)	O1S—C1S—H1S3	109.5
C24—C23—C22	121.5 (2)	H1S1—C1S—H1S3	109.5
O7—C23—C22	117.4 (2)	H1S2—C1S—H1S3	109.5
C23—C24—C25	119.6 (2)	O1S—C1S—H1SP	39.5
C23—C24—H24A	120.2	H1S1—C1S—H1SP	111.3
C25—C24—H24A	120.2	H1S2—C1S—H1SP	72.2
O8—C25—C24	121.0 (2)	H1S3—C1S—H1SP	135.7
O8—C25—C26	117.9 (2)	C41B—O10B—H10O	111.8
C24—C25—C26	121.1 (2)	C41B—O10B—H10P	108.8
C27—C26—C25	117.2 (2)	H10O—O10B—H10P	5.1
C27—C26—C28	122.0 (2)	O9B—C41B—O10B	130 (3)
C25—C26—C28	120.8 (2)	O9B—C41B—C42B	113 (2)
C26—C27—C22	123.6 (2)	O10B—C41B—C42B	106 (3)
C26—C27—H27A	118.2	C43B—C42B—C41B	132 (3)
C22—C27—H27A	118.2	C43B—C42B—C45B	117 (3)
C1—C28—C26	110.3 (2)	C41B—C42B—C45B	107 (3)
C1—C28—C35	113.7 (2)	C42B—C43B—C44B	126 (2)
C26—C28—C35	112.1 (2)	C42B—C43B—H43B	117.0
C1—C28—H28A	106.8	C44B—C43B—H43B	117.0
C26—C28—H28A	106.8	C43B—C44B—H44D	109.5
C35—C28—H28A	106.8	C43B—C44B—H44E	109.5
C30—C29—C7	112.4 (2)	H44D—C44B—H44E	109.5
C30—C29—H29A	109.1	C43B—C44B—H44F	109.5
C7—C29—H29A	109.1	H44D—C44B—H44F	109.5
C30—C29—H29B	109.1	H44E—C44B—H44F	109.5
C7—C29—H29B	109.1	C42B—C45B—H45D	109.5
H29A—C29—H29B	107.9	C42B—C45B—H45E	109.5
C29—C30—H30A	109.5	H45D—C45B—H45E	109.5
C29—C30—H30B	109.5	C42B—C45B—H45F	109.5
H30A—C30—H30B	109.5	H45D—C45B—H45F	109.5
C29—C30—H30C	109.5	H45E—C45B—H45F	109.5
H30A—C30—H30C	109.5	C1SB—O1SB—H1SP	90.9
H30B—C30—H30C	109.5	O1SB—C1SB—H1S	76.2
C32—C31—C14	111.7 (2)	O1SB—C1SB—H1S4	109.5
C32—C31—H31A	109.3	H1S—C1SB—H1S4	76.6
C14—C31—H31A	109.3	O1SB—C1SB—H1S5	109.5
C32—C31—H31B	109.3	H1S—C1SB—H1S5	59.2
C14—C31—H31B	109.3	H1S4—C1SB—H1S5	109.5
H31A—C31—H31B	107.9	O1SB—C1SB—H1S6	109.5
C31—C32—H32A	109.5	H1S—C1SB—H1S6	168.7
C31—C32—H32B	109.5	H1S4—C1SB—H1S6	109.5
H32A—C32—H32B	109.5	H1S5—C1SB—H1S6	109.5
C31—C32—H32C	109.5

(CECR-HTA-2MeOH-1.5H2O@90k-6h-exposure)

Crystal data

C43H59O13.50	F(000) = 850
Mr = 791.90	Dx = 1.261 Mg m^−3
Triclinic, P1	Melting point: not measured K
a = 11.2988 (6) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.1506 (8) Å	Cell parameters from 865 reflections
c = 14.8012 (9) Å	θ = 2.5–25°
α = 108.5606 (18)°	µ = 0.09 mm^−1
β = 109.4747 (18)°	T = 90 K
γ = 92.4244 (19)°	Block, pale yellow
V = 2085.7 (2) Å^3	0.14 × 0.10 × 0.08 mm
Z = 2

Data collection

CCD area detector diffractometer	7340 independent reflections
Radiation source: fine-focus sealed tube	4384 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
phi and ω scans	θmax = 25.0°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements) Blessing, R. (1995) Acta Crystallogr., A51, 33-38	h = −13→13
Tmin = 0.987, Tmax = 0.993	k = −16→16
17425 measured reflections	l = −17→17

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.063	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.176	H atoms treated by a mixture of independent and constrained refinement
S = 1.21	w = 1/[σ^2(Fo^2) + (0.0601P)^2 + 1.1813P] where P = (Fo^2 + 2Fc^2)/3
7340 reflections	(Δ/σ)max < 0.001
581 parameters	Δρmax = 0.46 e Å^−3
7 restraints	Δρmin = −0.38 e Å^−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)
O1	−0.2330 (2)	0.46436 (19)	−0.05524 (19)	0.0279 (6)
O2	0.1360 (2)	0.4684 (2)	0.22139 (19)	0.0305 (6)
O3	0.2626 (2)	0.41125 (19)	0.3964 (2)	0.0293 (6)
O4	0.0102 (2)	0.3651 (2)	0.57968 (18)	0.0330 (6)
O5	−0.2398 (2)	0.3892 (2)	0.51811 (18)	0.0290 (6)
O6	−0.6188 (2)	0.38916 (18)	0.2552 (2)	0.0288 (6)
O7	−0.7341 (2)	0.3468 (2)	0.0504 (2)	0.0286 (6)
O8	−0.4913 (2)	0.3931 (2)	−0.1498 (2)	0.0317 (6)
C1	−0.2056 (3)	0.3108 (2)	−0.0159 (2)	0.0209 (7)
C2	−0.1645 (3)	0.4118 (3)	0.0034 (3)	0.0229 (8)
C3	−0.0517 (3)	0.4654 (3)	0.0811 (3)	0.0247 (8)
H3A	−0.0261	0.5343	0.0923	0.030*
C4	0.0242 (3)	0.4181 (3)	0.1428 (3)	0.0236 (8)
C5	−0.0116 (3)	0.3163 (2)	0.1267 (2)	0.0211 (7)
C6	−0.1260 (3)	0.2659 (2)	0.0477 (2)	0.0215 (7)
H6A	−0.1518	0.1969	0.0362	0.026*
C7	0.0740 (3)	0.2664 (2)	0.1943 (2)	0.0213 (7)
H7A	0.1635	0.2951	0.2085	0.026*
C8	0.0591 (3)	0.2948 (2)	0.2982 (2)	0.0219 (8)
C9	0.1491 (3)	0.3614 (3)	0.3889 (3)	0.0242 (8)
C10	0.1304 (3)	0.3844 (3)	0.4813 (3)	0.0279 (8)
H10A	0.1923	0.4311	0.5424	0.034*
C11	0.0217 (3)	0.3391 (3)	0.4839 (3)	0.0261 (8)
C12	−0.0696 (3)	0.2696 (3)	0.3967 (3)	0.0231 (8)
C13	−0.0493 (3)	0.2511 (2)	0.3053 (3)	0.0228 (8)
H13A	−0.1128	0.2062	0.2440	0.027*
C14	−0.1856 (3)	0.2119 (3)	0.3990 (3)	0.0243 (8)
H14A	−0.1703	0.2251	0.4728	0.029*
C15	−0.3043 (3)	0.2549 (2)	0.3579 (2)	0.0212 (7)
C16	−0.3261 (3)	0.3445 (3)	0.4199 (2)	0.0227 (8)
C17	−0.4320 (3)	0.3868 (3)	0.3833 (3)	0.0246 (8)
H17A	−0.4464	0.4471	0.4269	0.030*
C18	−0.5170 (3)	0.3412 (3)	0.2834 (3)	0.0229 (8)
C19	−0.5000 (3)	0.2513 (2)	0.2184 (2)	0.0200 (7)
C20	−0.3930 (3)	0.2109 (2)	0.2585 (2)	0.0210 (7)
H20A	−0.3796	0.1497	0.2154	0.025*
C21	−0.5935 (3)	0.2019 (2)	0.1083 (2)	0.0210 (7)
H21A	−0.6796	0.2142	0.1093	0.025*
C22	−0.5673 (3)	0.2527 (2)	0.0386 (2)	0.0202 (7)
C23	−0.6391 (3)	0.3228 (2)	0.0107 (2)	0.0223 (8)
C24	−0.6166 (3)	0.3694 (3)	−0.0530 (3)	0.0275 (8)
H24A	−0.6682	0.4162	−0.0722	0.033*
C25	−0.5178 (3)	0.3470 (3)	−0.0883 (2)	0.0245 (8)
C26	−0.4421 (3)	0.2775 (2)	−0.0614 (2)	0.0205 (7)
C27	−0.4695 (3)	0.2328 (2)	0.0015 (2)	0.0199 (7)
H27A	−0.4184	0.1856	0.0205	0.024*
C28	−0.3326 (3)	0.2538 (2)	−0.0996 (2)	0.0225 (8)
H28A	−0.3457	0.2808	−0.1564	0.027*
C29	0.0600 (3)	0.1518 (3)	0.1423 (3)	0.0273 (8)
H29A	−0.0259	0.1196	0.1307	0.033*
H29B	0.0676	0.1373	0.0746	0.033*
C30	0.1598 (3)	0.1055 (3)	0.2057 (3)	0.0347 (9)
H30A	0.2451	0.1394	0.2204	0.052*
H30B	0.1509	0.0333	0.1672	0.052*
H30C	0.1476	0.1140	0.2702	0.052*
C31	−0.1974 (3)	0.0978 (3)	0.3486 (3)	0.0301 (9)
H31A	−0.2035	0.0817	0.2768	0.036*
H31B	−0.2766	0.0638	0.3475	0.036*
C32	−0.0838 (4)	0.0576 (3)	0.4055 (3)	0.0428 (10)
H32A	−0.0055	0.0898	0.4051	0.064*
H32B	−0.0948	−0.0158	0.3716	0.064*
H32C	−0.0780	0.0729	0.4764	0.064*
C33	−0.6013 (3)	0.0872 (2)	0.0664 (3)	0.0243 (8)
H33A	−0.5198	0.0718	0.0586	0.029*
H33B	−0.6129	0.0588	0.1165	0.029*
C34	−0.7094 (3)	0.0363 (3)	−0.0362 (3)	0.0310 (9)
H34A	−0.7907	0.0498	−0.0288	0.047*
H34B	−0.7097	−0.0368	−0.0593	0.047*
H34C	−0.6976	0.0630	−0.0867	0.047*
C35	−0.3359 (3)	0.1395 (2)	−0.1459 (2)	0.0252 (8)
H35A	−0.2630	0.1279	−0.1687	0.030*
H35B	−0.3258	0.1096	−0.0922	0.030*
C36	−0.4580 (3)	0.0863 (3)	−0.2357 (3)	0.0350 (9)
H36A	−0.5300	0.0924	−0.2124	0.053*
H36B	−0.4529	0.0147	−0.2649	0.053*
H36C	−0.4704	0.1173	−0.2880	0.053*
O2S	0.8497 (4)	0.7332 (3)	0.3025 (3)	0.0901 (13)
H2S	0.9068	0.7036	0.3483	0.135*
C2S	0.7625 (3)	0.7784 (2)	0.3470 (2)	0.0709 (15)
H2S1	0.8098	0.8308	0.4138	0.106*
H2S2	0.7116	0.7266	0.3559	0.106*
H2S3	0.7061	0.8089	0.3020	0.106*
O1W	0.2550 (3)	0.5541 (2)	0.7699 (2)	0.0306 (10)	0.60
H1WA	0.1893	0.5048	0.7196	0.046*	0.60
H1WB	0.2427	0.5877	0.8301	0.046*	0.60
O2W	0.3081 (6)	0.4669 (4)	0.7599 (4)	0.0688 (17)	0.60
H2WA	0.2611	0.4079	0.7400	0.103*	0.60
H2WB	0.3125	0.4852	0.7063	0.103*	0.60
O3W	0.3706 (7)	0.5352 (6)	0.8305 (6)	0.0262 (18)	0.30
H3WA	0.2915	0.5245	0.8342	0.039*	0.30
H3WB	0.3716	0.5611	0.7807	0.039*	0.30
H1O	−0.302 (4)	0.428 (3)	−0.092 (3)	0.039 (12)*
H2O	0.144 (4)	0.532 (4)	0.225 (4)	0.071 (16)*
H3O	0.254 (4)	0.409 (3)	0.336 (3)	0.059 (15)*
H4O	−0.075 (6)	0.370 (4)	0.566 (5)	0.12 (2)*
H5O	−0.253 (5)	0.444 (4)	0.548 (4)	0.076 (18)*
H6O	−0.653 (4)	0.374 (3)	0.192 (3)	0.037 (12)*
H7O	−0.760 (5)	0.384 (4)	0.030 (4)	0.07 (2)*
H8O	−0.547 (5)	0.427 (4)	−0.173 (4)	0.10 (2)*
O9	0.1853 (6)	0.6768 (5)	0.2653 (6)	0.0489 (15)	0.720 (7)
O10	0.2261 (18)	0.8400 (10)	0.3618 (18)	0.085 (3)	0.720 (7)
H10O	0.1425	0.8357	0.3157	0.127*	0.720 (7)
C41	0.2632 (11)	0.7496 (6)	0.3351 (7)	0.050 (2)	0.720 (7)
C42	0.3890 (9)	0.7442 (10)	0.4035 (13)	0.058 (3)	0.720 (7)
C43	0.4504 (8)	0.8246 (8)	0.4852 (7)	0.082 (3)	0.720 (7)
H43A	0.4109	0.8829	0.4970	0.099*	0.720 (7)
C44	0.5819 (7)	0.8284 (7)	0.5614 (6)	0.100 (3)	0.720 (7)
H44A	0.5744	0.8263	0.6249	0.150*	0.720 (7)
H44B	0.6369	0.8911	0.5763	0.150*	0.720 (7)
H44C	0.6188	0.7703	0.5322	0.150*	0.720 (7)
C45	0.4418 (18)	0.6451 (8)	0.3686 (14)	0.063 (3)	0.720 (7)
H45A	0.4802	0.6480	0.3189	0.094*	0.720 (7)
H45B	0.3722	0.5874	0.3367	0.094*	0.720 (7)
H45C	0.5064	0.6373	0.4281	0.094*	0.720 (7)
O1S	0.0074 (5)	0.8428 (4)	0.2534 (3)	0.0698 (17)	0.732 (7)
H1S	−0.0538	0.7938	0.2625	0.105*	0.732 (7)
C1S	−0.0244 (15)	0.7981 (7)	0.1421 (8)	0.075 (3)	0.732 (7)
H1S1	0.0227	0.8411	0.1206	0.112*	0.732 (7)
H1S2	−0.1160	0.7930	0.1065	0.112*	0.732 (7)
H1S3	−0.0009	0.7306	0.1250	0.112*	0.732 (7)
O9B	0.2285 (19)	0.6575 (15)	0.2670 (17)	0.0489 (15)	0.280 (7)
O10B	0.256 (5)	0.823 (3)	0.368 (5)	0.085 (3)	0.280 (7)
H10P	0.1593	0.8298	0.3212	0.127*	0.280 (7)
C41B	0.283 (3)	0.7279 (19)	0.348 (2)	0.050 (2)	0.280 (7)
C42B	0.419 (3)	0.729 (3)	0.399 (4)	0.058 (3)	0.280 (7)
C43B	0.510 (3)	0.7992 (18)	0.474 (2)	0.082 (3)	0.280 (7)
H43B	0.5891	0.7792	0.5022	0.099*	0.280 (7)
C44B	0.499 (2)	0.9123 (16)	0.5197 (17)	0.100 (3)	0.280 (7)
H44D	0.4755	0.9411	0.4653	0.150*	0.280 (7)
H44E	0.5817	0.9494	0.5722	0.150*	0.280 (7)
H44F	0.4344	0.9178	0.5506	0.150*	0.280 (7)
C45B	0.434 (6)	0.616 (3)	0.370 (4)	0.063 (3)	0.280 (7)
H45D	0.3636	0.5771	0.3754	0.094*	0.280 (7)
H45E	0.5150	0.6088	0.4176	0.094*	0.280 (7)
H45F	0.4324	0.5896	0.3002	0.094*	0.280 (7)
O1SB	−0.027 (3)	0.8250 (15)	0.1567 (19)	0.0698 (17)	0.268 (7)
H1SP	−0.0641	0.8484	0.1991	0.105*	0.268 (7)
C1SB	−0.0389 (19)	0.7285 (14)	0.1755 (16)	0.075 (3)	0.268 (7)
H1S4	−0.1274	0.7079	0.1661	0.112*	0.268 (7)
H1S5	0.0166	0.7381	0.2458	0.112*	0.268 (7)
H1S6	−0.0137	0.6760	0.1272	0.112*	0.268 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0265 (14)	0.0262 (14)	0.0325 (15)	0.0053 (12)	0.0074 (13)	0.0157 (12)
O2	0.0249 (13)	0.0257 (15)	0.0350 (15)	−0.0002 (11)	0.0052 (12)	0.0098 (12)
O3	0.0241 (13)	0.0345 (15)	0.0264 (14)	−0.0002 (11)	0.0096 (12)	0.0071 (12)
O4	0.0291 (15)	0.0463 (17)	0.0212 (13)	0.0024 (12)	0.0092 (12)	0.0091 (12)
O5	0.0269 (14)	0.0335 (16)	0.0199 (13)	0.0046 (12)	0.0056 (11)	0.0039 (12)
O6	0.0224 (13)	0.0329 (15)	0.0267 (15)	0.0124 (11)	0.0070 (12)	0.0056 (12)
O7	0.0289 (14)	0.0304 (15)	0.0363 (16)	0.0132 (12)	0.0183 (13)	0.0168 (13)
O8	0.0346 (15)	0.0386 (16)	0.0378 (15)	0.0143 (13)	0.0200 (13)	0.0260 (13)
C1	0.0226 (17)	0.0235 (19)	0.0202 (17)	0.0045 (14)	0.0112 (15)	0.0089 (15)
C2	0.0265 (18)	0.025 (2)	0.0245 (18)	0.0089 (15)	0.0143 (16)	0.0120 (16)
C3	0.0262 (19)	0.0220 (19)	0.030 (2)	0.0043 (15)	0.0137 (17)	0.0112 (16)
C4	0.0213 (18)	0.025 (2)	0.0255 (19)	0.0053 (15)	0.0104 (16)	0.0088 (16)
C5	0.0217 (17)	0.0244 (19)	0.0203 (18)	0.0058 (14)	0.0124 (15)	0.0067 (15)
C6	0.0268 (18)	0.0195 (18)	0.0238 (18)	0.0062 (15)	0.0150 (16)	0.0087 (15)
C7	0.0196 (17)	0.0222 (19)	0.0249 (18)	0.0056 (14)	0.0102 (15)	0.0094 (15)
C8	0.0201 (17)	0.0240 (19)	0.0239 (18)	0.0084 (15)	0.0077 (15)	0.0113 (16)
C9	0.0187 (17)	0.028 (2)	0.0264 (19)	0.0049 (15)	0.0086 (16)	0.0104 (16)
C10	0.0247 (19)	0.029 (2)	0.0245 (19)	0.0026 (16)	0.0065 (16)	0.0050 (16)
C11	0.0247 (19)	0.032 (2)	0.0247 (19)	0.0087 (16)	0.0113 (16)	0.0110 (17)
C12	0.0223 (18)	0.0245 (19)	0.0259 (19)	0.0075 (15)	0.0097 (16)	0.0121 (16)
C13	0.0205 (17)	0.0213 (18)	0.0235 (18)	0.0058 (14)	0.0054 (15)	0.0065 (15)
C14	0.0250 (18)	0.029 (2)	0.0205 (18)	0.0046 (15)	0.0080 (16)	0.0112 (16)
C15	0.0223 (17)	0.0232 (19)	0.0225 (18)	0.0031 (14)	0.0107 (15)	0.0114 (15)
C16	0.0233 (18)	0.027 (2)	0.0180 (17)	0.0006 (15)	0.0075 (15)	0.0083 (15)
C17	0.0225 (18)	0.0252 (19)	0.0246 (19)	0.0047 (15)	0.0110 (16)	0.0042 (16)
C18	0.0201 (17)	0.027 (2)	0.0270 (19)	0.0056 (15)	0.0113 (16)	0.0128 (16)
C19	0.0212 (17)	0.0191 (18)	0.0235 (18)	0.0017 (14)	0.0108 (15)	0.0099 (15)
C20	0.0235 (18)	0.0212 (18)	0.0219 (18)	0.0046 (14)	0.0119 (15)	0.0084 (15)
C21	0.0189 (17)	0.0205 (18)	0.0245 (18)	0.0039 (14)	0.0087 (15)	0.0081 (15)
C22	0.0195 (17)	0.0192 (18)	0.0200 (17)	0.0027 (14)	0.0052 (15)	0.0066 (15)
C23	0.0197 (17)	0.0244 (19)	0.0248 (18)	0.0047 (14)	0.0102 (16)	0.0091 (16)
C24	0.0256 (19)	0.029 (2)	0.031 (2)	0.0103 (16)	0.0101 (17)	0.0133 (17)
C25	0.0267 (19)	0.028 (2)	0.0214 (18)	0.0035 (15)	0.0094 (16)	0.0114 (16)
C26	0.0200 (17)	0.0205 (18)	0.0192 (17)	0.0042 (14)	0.0051 (15)	0.0067 (15)
C27	0.0194 (17)	0.0188 (18)	0.0198 (17)	0.0031 (14)	0.0049 (15)	0.0072 (15)
C28	0.0253 (18)	0.0252 (19)	0.0209 (18)	0.0072 (15)	0.0107 (15)	0.0105 (15)
C29	0.0305 (19)	0.026 (2)	0.029 (2)	0.0082 (16)	0.0135 (17)	0.0104 (16)
C30	0.036 (2)	0.032 (2)	0.046 (2)	0.0166 (17)	0.021 (2)	0.0181 (19)
C31	0.0283 (19)	0.031 (2)	0.031 (2)	0.0062 (16)	0.0076 (17)	0.0142 (17)
C32	0.044 (2)	0.034 (2)	0.049 (3)	0.0160 (19)	0.008 (2)	0.021 (2)
C33	0.0252 (18)	0.0220 (19)	0.0267 (19)	0.0040 (15)	0.0104 (16)	0.0088 (16)
C34	0.032 (2)	0.027 (2)	0.032 (2)	0.0054 (16)	0.0111 (17)	0.0080 (17)
C35	0.0260 (18)	0.027 (2)	0.0232 (18)	0.0048 (15)	0.0098 (16)	0.0081 (16)
C36	0.037 (2)	0.031 (2)	0.033 (2)	0.0069 (17)	0.0106 (18)	0.0090 (18)
O2S	0.074 (2)	0.134 (4)	0.087 (3)	0.039 (2)	0.029 (2)	0.069 (3)
C2S	0.050 (3)	0.075 (4)	0.082 (4)	0.010 (3)	0.014 (3)	0.031 (3)
O1W	0.029 (2)	0.033 (2)	0.025 (2)	0.0069 (19)	0.0102 (19)	0.0035 (19)
O2W	0.101 (5)	0.060 (4)	0.044 (3)	0.053 (4)	0.013 (3)	0.026 (3)
O3W	0.021 (4)	0.028 (5)	0.023 (4)	0.004 (4)	−0.003 (4)	0.013 (4)
O9	0.065 (5)	0.027 (3)	0.0429 (19)	0.009 (3)	0.011 (3)	0.006 (2)
O10	0.107 (10)	0.059 (5)	0.082 (4)	0.021 (3)	0.032 (7)	0.018 (4)
C41	0.095 (6)	0.025 (5)	0.041 (4)	0.007 (4)	0.027 (4)	0.023 (3)
C42	0.055 (7)	0.075 (6)	0.043 (3)	−0.005 (4)	0.014 (6)	0.027 (4)
C43	0.074 (7)	0.100 (7)	0.055 (4)	−0.031 (6)	0.019 (5)	0.015 (5)
C44	0.071 (5)	0.119 (8)	0.076 (6)	−0.010 (5)	−0.001 (5)	0.023 (5)
C45	0.085 (5)	0.061 (9)	0.056 (4)	−0.010 (7)	0.041 (3)	0.024 (7)
O1S	0.091 (4)	0.062 (3)	0.056 (3)	0.022 (3)	0.036 (3)	0.011 (3)
C1S	0.072 (5)	0.056 (7)	0.078 (7)	0.002 (6)	0.016 (5)	0.014 (6)
O9B	0.065 (5)	0.027 (3)	0.0429 (19)	0.009 (3)	0.011 (3)	0.006 (2)
O10B	0.107 (10)	0.059 (5)	0.082 (4)	0.021 (3)	0.032 (7)	0.018 (4)
C41B	0.095 (6)	0.025 (5)	0.041 (4)	0.007 (4)	0.027 (4)	0.023 (3)
C42B	0.055 (7)	0.075 (6)	0.043 (3)	−0.005 (4)	0.014 (6)	0.027 (4)
C43B	0.074 (7)	0.100 (7)	0.055 (4)	−0.031 (6)	0.019 (5)	0.015 (5)
C44B	0.071 (5)	0.119 (8)	0.076 (6)	−0.010 (5)	−0.001 (5)	0.023 (5)
C45B	0.085 (5)	0.061 (9)	0.056 (4)	−0.010 (7)	0.041 (3)	0.024 (7)
O1SB	0.091 (4)	0.062 (3)	0.056 (3)	0.022 (3)	0.036 (3)	0.011 (3)
C1SB	0.072 (5)	0.056 (7)	0.078 (7)	0.002 (6)	0.016 (5)	0.014 (6)

Geometric parameters (Å, º)

O1—C2	1.384 (4)	C32—H32B	0.9800
O1—H1O	0.82 (4)	C32—H32C	0.9800
O2—C4	1.369 (4)	C33—C34	1.520 (5)
O2—H2O	0.88 (5)	C33—H33A	0.9900
O3—C9	1.391 (4)	C33—H33B	0.9900
O3—H3O	0.86 (4)	C34—H34A	0.9800
O4—C11	1.398 (4)	C34—H34B	0.9800
O4—H4O	0.92 (6)	C34—H34C	0.9800
O5—C16	1.372 (4)	C35—C36	1.514 (5)
O5—H5O	0.81 (5)	C35—H35A	0.9900
O6—C18	1.372 (4)	C35—H35B	0.9900
O6—H6O	0.84 (4)	C36—H36A	0.9800
O7—C23	1.392 (4)	C36—H36B	0.9800
O7—H7O	0.72 (5)	C36—H36C	0.9800
O8—C25	1.375 (4)	O2S—C2S	1.425 (5)
O8—H8O	0.85 (5)	O2S—H2S	0.9818
C1—C2	1.391 (5)	C2S—H2S1	0.9800
C1—C6	1.402 (4)	C2S—H2S2	0.9800
C1—C28	1.524 (4)	C2S—H2S3	0.9800
C2—C3	1.382 (5)	O1W—H1WA	0.9221
C3—C4	1.391 (5)	O1W—H1WB	0.9272
C3—H3A	0.9500	O1W—H2WB	1.4615
C4—C5	1.401 (5)	O1W—H3WA	1.1219
C5—C6	1.390 (4)	O1W—H3WB	1.2688
C5—C7	1.516 (4)	O2W—H1WA	1.4747
C6—H6A	0.9500	O2W—H2WA	0.8756
C7—C8	1.529 (4)	O2W—H2WB	0.9249
C7—C29	1.533 (4)	O2W—H3WA	1.2199
C7—H7A	1.0000	O2W—H3WB	1.3770
C8—C9	1.388 (5)	O3W—H3WA	0.9224
C8—C13	1.399 (4)	O3W—H3WB	0.9243
C9—C10	1.391 (5)	O9—C41	1.242 (8)
C10—C11	1.379 (5)	O10—C41	1.342 (9)
C10—H10A	0.9500	O10—H10O	0.9490
C11—C12	1.384 (5)	O10—H10P	0.7650
C12—C13	1.393 (4)	C41—C42	1.466 (11)
C12—C14	1.530 (5)	C42—C43	1.317 (10)
C13—H13A	0.9500	C42—C45	1.550 (11)
C14—C15	1.517 (4)	C43—C44	1.523 (12)
C14—C31	1.526 (5)	C43—H43A	0.9500
C14—H14A	1.0000	C44—H44A	0.9800
C15—C20	1.393 (4)	C44—H44B	0.9800
C15—C16	1.395 (5)	C44—H44C	0.9800
C16—C17	1.385 (5)	C45—H45A	0.9800
C17—C18	1.385 (5)	C45—H45B	0.9800
C17—H17A	0.9500	C45—H45C	0.9800
C18—C19	1.396 (5)	O1S—C1S	1.472 (11)
C19—C20	1.391 (4)	O1S—H1S	1.0277
C19—C21	1.524 (4)	O1S—H1SP	0.9583
C20—H20A	0.9500	C1S—H1S1	0.9800
C21—C22	1.526 (4)	C1S—H1S2	0.9800
C21—C33	1.528 (4)	C1S—H1S3	0.9800
C21—H21A	1.0000	C1S—H1SP	1.1478
C22—C23	1.386 (4)	O9B—C41B	1.228 (17)
C22—C27	1.390 (4)	O10B—C41B	1.358 (17)
C23—C24	1.388 (5)	O10B—H10O	1.3106
C24—C25	1.390 (5)	O10B—H10P	1.1077
C24—H24A	0.9500	C41B—C42B	1.470 (19)
C25—C26	1.396 (5)	C42B—C43B	1.312 (17)
C26—C27	1.385 (4)	C42B—C45B	1.551 (18)
C26—C28	1.531 (4)	C43B—C44B	1.55 (2)
C27—H27A	0.9500	C43B—H43B	0.9500
C28—C35	1.536 (4)	C44B—H44D	0.9800
C28—H28A	1.0000	C44B—H44E	0.9800
C29—C30	1.527 (5)	C44B—H44F	0.9800
C29—H29A	0.9900	C45B—H45D	0.9800
C29—H29B	0.9900	C45B—H45E	0.9800
C30—H30A	0.9800	C45B—H45F	0.9800
C30—H30B	0.9800	O1SB—C1SB	1.487 (17)
C30—H30C	0.9800	O1SB—H1SP	0.8563
C31—C32	1.526 (5)	C1SB—H1S	1.3921
C31—H31A	0.9900	C1SB—H1S4	0.9800
C31—H31B	0.9900	C1SB—H1S5	0.9800
C32—H32A	0.9800	C1SB—H1S6	0.9800
C2—O1—H1O	107 (3)	H32A—C32—H32C	109.5
C4—O2—H2O	108 (3)	H32B—C32—H32C	109.5
C9—O3—H3O	107 (3)	C34—C33—C21	113.1 (3)
C11—O4—H4O	104 (4)	C34—C33—H33A	109.0
C16—O5—H5O	113 (4)	C21—C33—H33A	109.0
C18—O6—H6O	113 (3)	C34—C33—H33B	109.0
C23—O7—H7O	103 (4)	C21—C33—H33B	109.0
C25—O8—H8O	115 (4)	H33A—C33—H33B	107.8
C2—C1—C6	116.4 (3)	C33—C34—H34A	109.5
C2—C1—C28	121.4 (3)	C33—C34—H34B	109.5
C6—C1—C28	122.2 (3)	H34A—C34—H34B	109.5
C3—C2—O1	115.8 (3)	C33—C34—H34C	109.5
C3—C2—C1	122.1 (3)	H34A—C34—H34C	109.5
O1—C2—C1	122.1 (3)	H34B—C34—H34C	109.5
C2—C3—C4	119.7 (3)	C36—C35—C28	112.9 (3)
C2—C3—H3A	120.2	C36—C35—H35A	109.0
C4—C3—H3A	120.2	C28—C35—H35A	109.0
O2—C4—C3	121.8 (3)	C36—C35—H35B	109.0
O2—C4—C5	117.3 (3)	C28—C35—H35B	109.0
C3—C4—C5	120.9 (3)	H35A—C35—H35B	107.8
C6—C5—C4	117.1 (3)	C35—C36—H36A	109.5
C6—C5—C7	123.2 (3)	C35—C36—H36B	109.5
C4—C5—C7	119.7 (3)	H36A—C36—H36B	109.5
C5—C6—C1	123.8 (3)	C35—C36—H36C	109.5
C5—C6—H6A	118.1	H36A—C36—H36C	109.5
C1—C6—H6A	118.1	H36B—C36—H36C	109.5
C5—C7—C8	111.4 (2)	C2S—O2S—H2S	109.3
C5—C7—C29	113.5 (3)	O2S—C2S—H2S1	109.5
C8—C7—C29	112.3 (3)	O2S—C2S—H2S2	109.5
C5—C7—H7A	106.3	H2S1—C2S—H2S2	109.5
C8—C7—H7A	106.3	O2S—C2S—H2S3	109.5
C29—C7—H7A	106.3	H2S1—C2S—H2S3	109.5
C9—C8—C13	116.5 (3)	H2S2—C2S—H2S3	109.5
C9—C8—C7	123.9 (3)	H1WA—O1W—H1WB	116.7
C13—C8—C7	119.6 (3)	H1WA—O1W—H2WB	73.8
C8—C9—O3	124.3 (3)	H1WB—O1W—H2WB	155.2
C8—C9—C10	121.3 (3)	H1WA—O1W—H3WA	105.3
O3—C9—C10	114.4 (3)	H1WB—O1W—H3WA	62.6
C11—C10—C9	119.8 (3)	H2WB—O1W—H3WA	93.4
C11—C10—H10A	120.1	H1WA—O1W—H3WB	126.7
C9—C10—H10A	120.1	H1WB—O1W—H3WB	112.8
C10—C11—C12	121.6 (3)	H2WB—O1W—H3WB	52.9
C10—C11—O4	116.5 (3)	H3WA—O1W—H3WB	80.8
C12—C11—O4	121.8 (3)	H1WA—O2W—H2WA	87.4
C11—C12—C13	116.7 (3)	H1WA—O2W—H2WB	73.1
C11—C12—C14	122.7 (3)	H2WA—O2W—H2WB	113.6
C13—C12—C14	120.5 (3)	H1WA—O2W—H3WA	73.7
C12—C13—C8	123.9 (3)	H2WA—O2W—H3WA	109.0
C12—C13—H13A	118.0	H2WB—O2W—H3WA	123.6
C8—C13—H13A	118.0	H1WA—O2W—H3WB	87.0
C15—C14—C31	114.6 (3)	H2WA—O2W—H3WB	173.1
C15—C14—C12	110.5 (3)	H2WB—O2W—H3WB	60.8
C31—C14—C12	112.0 (3)	H3WA—O2W—H3WB	73.2
C15—C14—H14A	106.4	H3WA—O3W—H3WB	114.6
C31—C14—H14A	106.4	C41—O10—H10O	108.9
C12—C14—H14A	106.4	C41—O10—H10P	101.9
C20—C15—C16	117.1 (3)	H10O—O10—H10P	7.0
C20—C15—C14	123.1 (3)	O9—C41—O10	118.9 (12)
C16—C15—C14	119.7 (3)	O9—C41—C42	125.8 (7)
O5—C16—C17	121.0 (3)	O10—C41—C42	114.6 (11)
O5—C16—C15	118.1 (3)	C43—C42—C41	118.2 (9)
C17—C16—C15	120.9 (3)	C43—C42—C45	125.5 (12)
C16—C17—C18	120.1 (3)	C41—C42—C45	116.1 (11)
C16—C17—H17A	119.9	C42—C43—C44	123.1 (11)
C18—C17—H17A	119.9	C42—C43—H43A	118.5
O6—C18—C17	115.4 (3)	C44—C43—H43A	118.5
O6—C18—C19	123.4 (3)	C43—C44—H44A	109.5
C17—C18—C19	121.2 (3)	C43—C44—H44B	109.5
C20—C19—C18	116.7 (3)	H44A—C44—H44B	109.5
C20—C19—C21	122.3 (3)	C43—C44—H44C	109.5
C18—C19—C21	121.0 (3)	H44A—C44—H44C	109.5
C19—C20—C15	123.9 (3)	H44B—C44—H44C	109.5
C19—C20—H20A	118.1	C42—C45—H45A	109.5
C15—C20—H20A	118.1	C42—C45—H45B	109.5
C19—C21—C22	111.4 (3)	H45A—C45—H45B	109.5
C19—C21—C33	113.2 (3)	C42—C45—H45C	109.5
C22—C21—C33	112.4 (3)	H45A—C45—H45C	109.5
C19—C21—H21A	106.4	H45B—C45—H45C	109.5
C22—C21—H21A	106.4	C1S—O1S—H1S	100.1
C33—C21—H21A	106.4	C1S—O1S—H1SP	51.2
C23—C22—C27	116.7 (3)	H1S—O1S—H1SP	87.4
C23—C22—C21	121.2 (3)	O1S—C1S—H1S1	109.5
C27—C22—C21	122.1 (3)	O1S—C1S—H1S2	109.5
C22—C23—C24	121.8 (3)	H1S1—C1S—H1S2	109.5
C22—C23—O7	117.5 (3)	O1S—C1S—H1S3	109.5
C24—C23—O7	120.7 (3)	H1S1—C1S—H1S3	109.5
C23—C24—C25	119.5 (3)	H1S2—C1S—H1S3	109.5
C23—C24—H24A	120.3	O1S—C1S—H1SP	40.6
C25—C24—H24A	120.3	H1S1—C1S—H1SP	109.0
O8—C25—C24	121.0 (3)	H1S2—C1S—H1SP	71.9
O8—C25—C26	118.2 (3)	H1S3—C1S—H1SP	138.1
C24—C25—C26	120.8 (3)	C41B—O10B—H10O	118.0
C27—C26—C25	117.2 (3)	C41B—O10B—H10P	115.2
C27—C26—C28	122.0 (3)	H10O—O10B—H10P	2.9
C25—C26—C28	120.7 (3)	O9B—C41B—O10B	124 (4)
C26—C27—C22	124.0 (3)	O9B—C41B—C42B	116 (3)
C26—C27—H27A	118.0	O10B—C41B—C42B	111 (4)
C22—C27—H27A	118.0	C43B—C42B—C41B	132 (3)
C1—C28—C26	110.6 (3)	C43B—C42B—C45B	121 (4)
C1—C28—C35	114.0 (3)	C41B—C42B—C45B	105 (3)
C26—C28—C35	112.0 (3)	C42B—C43B—C44B	126 (3)
C1—C28—H28A	106.6	C42B—C43B—H43B	117.1
C26—C28—H28A	106.6	C44B—C43B—H43B	117.1
C35—C28—H28A	106.6	C43B—C44B—H44D	109.5
C30—C29—C7	112.5 (3)	C43B—C44B—H44E	109.5
C30—C29—H29A	109.1	H44D—C44B—H44E	109.5
C7—C29—H29A	109.1	C43B—C44B—H44F	109.5
C30—C29—H29B	109.1	H44D—C44B—H44F	109.5
C7—C29—H29B	109.1	H44E—C44B—H44F	109.5
H29A—C29—H29B	107.8	C42B—C45B—H45D	109.5
C29—C30—H30A	109.5	C42B—C45B—H45E	109.5
C29—C30—H30B	109.5	H45D—C45B—H45E	109.5
H30A—C30—H30B	109.5	C42B—C45B—H45F	109.5
C29—C30—H30C	109.5	H45D—C45B—H45F	109.5
H30A—C30—H30C	109.5	H45E—C45B—H45F	109.5
H30B—C30—H30C	109.5	C1SB—O1SB—H1SP	87.0
C14—C31—C32	111.6 (3)	O1SB—C1SB—H1S	80.7
C14—C31—H31A	109.3	O1SB—C1SB—H1S4	109.5
C32—C31—H31A	109.3	H1S—C1SB—H1S4	75.7
C14—C31—H31B	109.3	O1SB—C1SB—H1S5	109.5
C32—C31—H31B	109.3	H1S—C1SB—H1S5	56.1
H31A—C31—H31B	108.0	H1S4—C1SB—H1S5	109.5
C31—C32—H32A	109.5	O1SB—C1SB—H1S6	109.5
C31—C32—H32B	109.5	H1S—C1SB—H1S6	165.2
H32A—C32—H32B	109.5	H1S4—C1SB—H1S6	109.5
C31—C32—H32C	109.5	H1S5—C1SB—H1S6	109.5

(CECR-HTA-2MeOH-1.5H2O@90k-12h-exposure)

Crystal data

C43H59O13.50	F(000) = 850
Mr = 791.90	Dx = 1.258 Mg m^−3
Triclinic, P1	Melting point: not measured K
a = 11.3096 (12) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.1748 (16) Å	Cell parameters from 865 reflections
c = 14.8116 (17) Å	θ = 2.5–25°
α = 108.570 (3)°	µ = 0.09 mm^−1
β = 109.632 (4)°	T = 90 K
γ = 92.276 (4)°	Block, pale yellow
V = 2091.2 (4) Å^3	0.14 × 0.10 × 0.08 mm
Z = 2

Data collection

CCD area detector diffractometer	7351 independent reflections
Radiation source: fine-focus sealed tube	3760 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.049
phi and ω scans	θmax = 25.0°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements) Blessing, R. (1995) Acta Crystallogr., A51, 33-38	h = −13→13
Tmin = 0.987, Tmax = 0.993	k = −16→16
15054 measured reflections	l = −17→12

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.071	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.194	H atoms treated by a mixture of independent and constrained refinement
S = 1.20	w = 1/[σ^2(Fo^2) + (0.0601P)^2 + 1.1813P] where P = (Fo^2 + 2Fc^2)/3
7351 reflections	(Δ/σ)max = 0.002
581 parameters	Δρmax = 0.49 e Å^−3
7 restraints	Δρmin = −0.41 e Å^−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)
O1	−0.2338 (3)	0.4636 (2)	−0.0560 (3)	0.0315 (8)
O2	0.1359 (3)	0.4678 (3)	0.2207 (2)	0.0335 (8)
O3	0.2620 (3)	0.4116 (2)	0.3960 (2)	0.0316 (8)
O4	0.0109 (3)	0.3650 (2)	0.5797 (2)	0.0357 (8)
O5	−0.2392 (3)	0.3892 (3)	0.5184 (2)	0.0324 (8)
O6	−0.6187 (3)	0.3890 (2)	0.2551 (2)	0.0309 (8)
O7	−0.7342 (3)	0.3471 (2)	0.0499 (2)	0.0314 (8)
O8	−0.4924 (3)	0.3930 (2)	−0.1503 (2)	0.0331 (8)
C1	−0.2062 (4)	0.3105 (3)	−0.0163 (3)	0.0234 (10)
C2	−0.1650 (4)	0.4110 (3)	0.0027 (3)	0.0256 (10)
C3	−0.0515 (4)	0.4653 (3)	0.0812 (3)	0.0267 (10)
H3A	−0.0262	0.5341	0.0927	0.032*
C4	0.0243 (4)	0.4176 (3)	0.1427 (3)	0.0265 (10)
C5	−0.0116 (4)	0.3162 (3)	0.1266 (3)	0.0221 (10)
C6	−0.1263 (4)	0.2656 (3)	0.0476 (3)	0.0230 (10)
H6A	−0.1521	0.1969	0.0363	0.028*
C7	0.0739 (4)	0.2663 (3)	0.1943 (3)	0.0227 (10)
H7A	0.1633	0.2950	0.2087	0.027*
C8	0.0592 (4)	0.2947 (3)	0.2979 (3)	0.0216 (10)
C9	0.1490 (4)	0.3620 (3)	0.3890 (3)	0.0267 (10)
C10	0.1308 (4)	0.3849 (3)	0.4812 (3)	0.0304 (11)
H10A	0.1925	0.4319	0.5422	0.037*
C11	0.0220 (4)	0.3391 (3)	0.4839 (3)	0.0285 (11)
C12	−0.0696 (4)	0.2695 (3)	0.3968 (3)	0.0250 (10)
C13	−0.0488 (4)	0.2513 (3)	0.3057 (3)	0.0239 (10)
H13A	−0.1123	0.2064	0.2445	0.029*
C14	−0.1851 (4)	0.2120 (3)	0.3989 (3)	0.0268 (10)
H14A	−0.1696	0.2253	0.4728	0.032*
C15	−0.3035 (4)	0.2549 (3)	0.3581 (3)	0.0233 (10)
C16	−0.3259 (4)	0.3446 (3)	0.4202 (3)	0.0254 (10)
C17	−0.4321 (4)	0.3867 (3)	0.3837 (3)	0.0271 (10)
H17A	−0.4471	0.4467	0.4271	0.033*
C18	−0.5164 (4)	0.3410 (3)	0.2835 (3)	0.0239 (10)
C19	−0.4997 (4)	0.2517 (3)	0.2183 (3)	0.0200 (9)
C20	−0.3924 (4)	0.2110 (3)	0.2583 (3)	0.0229 (10)
H20A	−0.3791	0.1500	0.2152	0.027*
C21	−0.5934 (4)	0.2021 (3)	0.1084 (3)	0.0219 (10)
H21A	−0.6794	0.2148	0.1094	0.026*
C22	−0.5676 (4)	0.2525 (3)	0.0384 (3)	0.0217 (10)
C23	−0.6387 (4)	0.3229 (3)	0.0107 (3)	0.0239 (10)
C24	−0.6170 (4)	0.3692 (3)	−0.0535 (3)	0.0287 (11)
H24A	−0.6690	0.4157	−0.0730	0.034*
C25	−0.5186 (4)	0.3466 (3)	−0.0887 (3)	0.0267 (10)
C26	−0.4425 (4)	0.2772 (3)	−0.0618 (3)	0.0225 (10)
C27	−0.4702 (4)	0.2329 (3)	0.0016 (3)	0.0221 (10)
H27A	−0.4189	0.1860	0.0210	0.026*
C28	−0.3332 (4)	0.2536 (3)	−0.0999 (3)	0.0242 (10)
H28A	−0.3467	0.2806	−0.1568	0.029*
C29	0.0605 (4)	0.1519 (3)	0.1425 (3)	0.0303 (11)
H29A	−0.0254	0.1198	0.1305	0.036*
H29B	0.0682	0.1375	0.0749	0.036*
C30	0.1603 (4)	0.1054 (3)	0.2060 (4)	0.0374 (12)
H30A	0.2456	0.1391	0.2209	0.056*
H30B	0.1512	0.0333	0.1675	0.056*
H30C	0.1481	0.1139	0.2704	0.056*
C31	−0.1968 (4)	0.0983 (3)	0.3489 (3)	0.0318 (11)
H31A	−0.2754	0.0645	0.3484	0.038*
H31B	−0.2040	0.0820	0.2769	0.038*
C32	−0.0828 (5)	0.0578 (4)	0.4049 (4)	0.0478 (14)
H32A	−0.0050	0.0900	0.4043	0.072*
H32B	−0.0939	−0.0154	0.3705	0.072*
H32C	−0.0763	0.0726	0.4758	0.072*
C33	−0.6017 (4)	0.0876 (3)	0.0663 (3)	0.0237 (10)
H33A	−0.5202	0.0719	0.0587	0.028*
H33B	−0.6135	0.0592	0.1163	0.028*
C34	−0.7098 (4)	0.0371 (3)	−0.0365 (3)	0.0322 (11)
H34A	−0.7910	0.0506	−0.0291	0.048*
H34B	−0.7100	−0.0359	−0.0598	0.048*
H34C	−0.6980	0.0640	−0.0867	0.048*
C35	−0.3365 (4)	0.1397 (3)	−0.1462 (3)	0.0276 (10)
H35A	−0.2638	0.1283	−0.1689	0.033*
H35B	−0.3260	0.1101	−0.0924	0.033*
C36	−0.4580 (4)	0.0861 (3)	−0.2357 (3)	0.0365 (12)
H36A	−0.5299	0.0921	−0.2125	0.055*
H36B	−0.4522	0.0146	−0.2643	0.055*
H36C	−0.4708	0.1165	−0.2884	0.055*
O2S	0.8505 (4)	0.7343 (4)	0.3031 (4)	0.1045 (17)
H2S	0.9076	0.7047	0.3489	0.157*
C2S	0.7623 (3)	0.7795 (3)	0.3473 (3)	0.080 (2)
H2S1	0.8092	0.8319	0.4141	0.121*
H2S2	0.7117	0.7278	0.3561	0.121*
H2S3	0.7058	0.8097	0.3019	0.121*
O1W	0.2548 (3)	0.5553 (3)	0.7702 (3)	0.0343 (13)	0.60
H1WA	0.1891	0.5059	0.7199	0.051*	0.60
H1WB	0.2425	0.5888	0.8304	0.051*	0.60
O2W	0.3061 (7)	0.4666 (5)	0.7591 (5)	0.069 (2)	0.60
H2WA	0.2592	0.4076	0.7392	0.103*	0.60
H2WB	0.3106	0.4849	0.7055	0.103*	0.60
O3W	0.3698 (9)	0.5356 (8)	0.8302 (7)	0.028 (2)	0.30
H3WA	0.2907	0.5249	0.8338	0.043*	0.30
H3WB	0.3709	0.5615	0.7804	0.043*	0.30
H1O	−0.303 (4)	0.429 (4)	−0.091 (4)	0.044 (16)*
H2O	0.149 (5)	0.529 (4)	0.225 (4)	0.07 (2)*
H3O	0.253 (5)	0.410 (4)	0.331 (4)	0.08 (2)*
H4O	−0.070 (9)	0.380 (7)	0.568 (7)	0.20 (4)*
H5O	−0.252 (5)	0.448 (4)	0.551 (4)	0.07 (2)*
H6O	−0.657 (5)	0.371 (4)	0.187 (4)	0.059 (17)*
H7O	−0.763 (6)	0.392 (5)	0.034 (5)	0.10 (3)*
H8O	−0.554 (7)	0.425 (5)	−0.184 (5)	0.12 (3)*
O9	0.1845 (10)	0.6766 (7)	0.2660 (9)	0.060 (2)	0.715 (9)
O10	0.2246 (15)	0.8397 (10)	0.3625 (18)	0.095 (3)	0.715 (9)
H10O	0.1409	0.8354	0.3164	0.142*	0.715 (9)
C41	0.2636 (14)	0.7488 (8)	0.3357 (12)	0.059 (3)	0.715 (9)
C42	0.3906 (12)	0.7447 (11)	0.4035 (17)	0.065 (4)	0.715 (9)
C43	0.4501 (12)	0.8253 (13)	0.4851 (11)	0.108 (6)	0.715 (9)
H43A	0.4108	0.8836	0.4977	0.130*	0.715 (9)
C44	0.5831 (10)	0.8258 (10)	0.5606 (8)	0.122 (4)	0.715 (9)
H44A	0.5766	0.8237	0.6243	0.183*	0.715 (9)
H44B	0.6400	0.8874	0.5755	0.183*	0.715 (9)
H44C	0.6174	0.7667	0.5300	0.183*	0.715 (9)
C45	0.441 (2)	0.6429 (10)	0.3734 (17)	0.070 (4)	0.715 (9)
H45A	0.4811	0.6415	0.3235	0.105*	0.715 (9)
H45B	0.3706	0.5866	0.3431	0.105*	0.715 (9)
H45C	0.5046	0.6368	0.4347	0.105*	0.715 (9)
O1S	0.0077 (6)	0.8424 (5)	0.2535 (4)	0.070 (2)	0.689 (8)
H1S	−0.0535	0.7935	0.2626	0.105*	0.689 (8)
C1S	−0.024 (2)	0.7939 (10)	0.1421 (12)	0.102 (6)	0.689 (8)
H1S1	0.0213	0.8353	0.1186	0.153*	0.689 (8)
H1S2	−0.1163	0.7874	0.1062	0.153*	0.689 (8)
H1S3	0.0003	0.7268	0.1276	0.153*	0.689 (8)
O9B	0.226 (3)	0.656 (2)	0.263 (3)	0.060 (2)	0.285 (9)
O10B	0.262 (4)	0.823 (3)	0.367 (5)	0.095 (3)	0.285 (9)
H10P	0.1652	0.8292	0.3200	0.142*	0.285 (9)
C41B	0.286 (4)	0.725 (3)	0.345 (3)	0.059 (3)	0.285 (9)
C42B	0.421 (4)	0.723 (3)	0.399 (5)	0.065 (4)	0.285 (9)
C43B	0.509 (4)	0.796 (3)	0.472 (3)	0.108 (6)	0.285 (9)
H43B	0.5888	0.7770	0.5012	0.130*	0.285 (9)
C44B	0.502 (3)	0.911 (2)	0.519 (2)	0.122 (4)	0.285 (9)
H44D	0.4786	0.9396	0.4642	0.183*	0.285 (9)
H44E	0.5859	0.9467	0.5703	0.183*	0.285 (9)
H44F	0.4388	0.9185	0.5508	0.183*	0.285 (9)
C45B	0.439 (7)	0.610 (4)	0.355 (5)	0.070 (4)	0.285 (9)
H45D	0.3720	0.5659	0.3576	0.105*	0.285 (9)
H45E	0.5223	0.6011	0.3964	0.105*	0.285 (9)
H45F	0.4323	0.5937	0.2840	0.105*	0.285 (9)
O1SB	−0.022 (3)	0.8228 (16)	0.1522 (18)	0.070 (2)	0.311 (8)
H1SP	−0.0592	0.8462	0.1946	0.105*	0.311 (8)
C1SB	−0.039 (2)	0.7276 (16)	0.174 (2)	0.102 (6)	0.311 (8)
H1S4	−0.1284	0.7097	0.1639	0.153*	0.311 (8)
H1S5	0.0148	0.7382	0.2451	0.153*	0.311 (8)
H1S6	−0.0146	0.6727	0.1275	0.153*	0.311 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0306 (18)	0.0294 (19)	0.039 (2)	0.0087 (16)	0.0109 (17)	0.0193 (17)
O2	0.0236 (16)	0.030 (2)	0.038 (2)	−0.0012 (15)	0.0032 (15)	0.0101 (17)
O3	0.0252 (16)	0.038 (2)	0.0290 (18)	−0.0006 (14)	0.0128 (15)	0.0061 (16)
O4	0.0355 (19)	0.049 (2)	0.0227 (17)	0.0053 (16)	0.0135 (16)	0.0105 (16)
O5	0.0281 (17)	0.038 (2)	0.0227 (18)	0.0054 (15)	0.0073 (15)	0.0022 (16)
O6	0.0227 (16)	0.035 (2)	0.0288 (19)	0.0118 (14)	0.0073 (15)	0.0046 (16)
O7	0.0311 (17)	0.033 (2)	0.041 (2)	0.0148 (15)	0.0206 (16)	0.0174 (17)
O8	0.0333 (18)	0.043 (2)	0.0394 (19)	0.0139 (15)	0.0192 (16)	0.0286 (17)
C1	0.024 (2)	0.028 (3)	0.025 (2)	0.0073 (19)	0.015 (2)	0.011 (2)
C2	0.033 (2)	0.027 (3)	0.028 (2)	0.013 (2)	0.019 (2)	0.015 (2)
C3	0.027 (2)	0.024 (3)	0.031 (3)	0.0044 (19)	0.012 (2)	0.009 (2)
C4	0.024 (2)	0.027 (3)	0.029 (2)	0.007 (2)	0.013 (2)	0.008 (2)
C5	0.022 (2)	0.028 (3)	0.019 (2)	0.0078 (19)	0.012 (2)	0.008 (2)
C6	0.027 (2)	0.021 (2)	0.028 (2)	0.0074 (19)	0.016 (2)	0.011 (2)
C7	0.021 (2)	0.027 (3)	0.022 (2)	0.0057 (18)	0.012 (2)	0.008 (2)
C8	0.020 (2)	0.026 (2)	0.022 (2)	0.0095 (18)	0.009 (2)	0.010 (2)
C9	0.022 (2)	0.031 (3)	0.028 (3)	0.0055 (19)	0.012 (2)	0.009 (2)
C10	0.026 (2)	0.031 (3)	0.026 (3)	0.002 (2)	0.004 (2)	0.005 (2)
C11	0.024 (2)	0.037 (3)	0.025 (2)	0.006 (2)	0.010 (2)	0.012 (2)
C12	0.022 (2)	0.029 (3)	0.028 (2)	0.0091 (19)	0.011 (2)	0.013 (2)
C13	0.018 (2)	0.025 (2)	0.023 (2)	0.0049 (18)	0.0036 (19)	0.004 (2)
C14	0.026 (2)	0.032 (3)	0.024 (2)	0.007 (2)	0.008 (2)	0.012 (2)
C15	0.023 (2)	0.027 (3)	0.026 (2)	0.0050 (19)	0.013 (2)	0.013 (2)
C16	0.023 (2)	0.032 (3)	0.018 (2)	−0.0029 (19)	0.008 (2)	0.006 (2)
C17	0.023 (2)	0.031 (3)	0.027 (2)	0.0069 (19)	0.012 (2)	0.005 (2)
C18	0.020 (2)	0.032 (3)	0.026 (2)	0.0081 (19)	0.012 (2)	0.013 (2)
C19	0.021 (2)	0.019 (2)	0.024 (2)	0.0017 (18)	0.014 (2)	0.008 (2)
C20	0.026 (2)	0.025 (2)	0.023 (2)	0.0046 (19)	0.014 (2)	0.009 (2)
C21	0.020 (2)	0.023 (2)	0.025 (2)	0.0039 (18)	0.012 (2)	0.008 (2)
C22	0.020 (2)	0.022 (2)	0.019 (2)	0.0025 (18)	0.0057 (19)	0.0024 (19)
C23	0.021 (2)	0.027 (3)	0.026 (2)	0.0062 (19)	0.013 (2)	0.008 (2)
C24	0.027 (2)	0.032 (3)	0.032 (3)	0.012 (2)	0.011 (2)	0.016 (2)
C25	0.027 (2)	0.028 (3)	0.024 (2)	0.004 (2)	0.010 (2)	0.008 (2)
C26	0.022 (2)	0.022 (2)	0.021 (2)	0.0050 (18)	0.0052 (19)	0.007 (2)
C27	0.020 (2)	0.023 (2)	0.020 (2)	0.0022 (18)	0.0029 (19)	0.010 (2)
C28	0.027 (2)	0.027 (3)	0.022 (2)	0.0065 (19)	0.011 (2)	0.010 (2)
C29	0.034 (2)	0.031 (3)	0.031 (3)	0.011 (2)	0.017 (2)	0.011 (2)
C30	0.038 (3)	0.033 (3)	0.050 (3)	0.017 (2)	0.021 (3)	0.019 (3)
C31	0.028 (2)	0.033 (3)	0.035 (3)	0.007 (2)	0.007 (2)	0.017 (2)
C32	0.047 (3)	0.040 (3)	0.049 (3)	0.013 (2)	0.004 (3)	0.020 (3)
C33	0.025 (2)	0.022 (2)	0.025 (2)	0.0039 (18)	0.013 (2)	0.005 (2)
C34	0.032 (2)	0.029 (3)	0.031 (3)	0.006 (2)	0.011 (2)	0.006 (2)
C35	0.029 (2)	0.029 (3)	0.025 (2)	0.005 (2)	0.012 (2)	0.008 (2)
C36	0.039 (3)	0.033 (3)	0.032 (3)	0.004 (2)	0.010 (2)	0.007 (2)
O2S	0.079 (3)	0.157 (5)	0.104 (4)	0.040 (3)	0.029 (3)	0.082 (4)
C2S	0.052 (4)	0.085 (5)	0.101 (6)	0.016 (4)	0.017 (4)	0.040 (5)
O1W	0.031 (3)	0.042 (3)	0.027 (3)	0.009 (2)	0.014 (3)	0.006 (3)
O2W	0.104 (6)	0.059 (5)	0.040 (4)	0.054 (4)	0.012 (4)	0.024 (4)
O3W	0.024 (5)	0.033 (6)	0.022 (6)	0.004 (5)	0.001 (5)	0.010 (5)
O9	0.088 (8)	0.030 (5)	0.052 (3)	0.007 (4)	0.024 (5)	0.003 (3)
O10	0.103 (11)	0.079 (6)	0.099 (4)	0.033 (4)	0.037 (8)	0.025 (5)
C41	0.106 (8)	0.027 (7)	0.057 (5)	0.014 (6)	0.036 (5)	0.024 (5)
C42	0.053 (8)	0.093 (9)	0.054 (5)	0.003 (5)	0.014 (7)	0.037 (7)
C43	0.105 (13)	0.138 (13)	0.056 (6)	−0.057 (10)	0.024 (8)	0.018 (8)
C44	0.083 (8)	0.171 (13)	0.076 (8)	−0.006 (7)	0.001 (6)	0.031 (8)
C45	0.106 (6)	0.058 (13)	0.054 (9)	0.011 (11)	0.055 (7)	0.003 (9)
O1S	0.088 (4)	0.062 (4)	0.058 (4)	0.018 (3)	0.038 (4)	0.006 (3)
C1S	0.102 (8)	0.059 (10)	0.105 (11)	−0.021 (9)	0.004 (7)	0.019 (9)
O9B	0.088 (8)	0.030 (5)	0.052 (3)	0.007 (4)	0.024 (5)	0.003 (3)
O10B	0.103 (11)	0.079 (6)	0.099 (4)	0.033 (4)	0.037 (8)	0.025 (5)
C41B	0.106 (8)	0.027 (7)	0.057 (5)	0.014 (6)	0.036 (5)	0.024 (5)
C42B	0.053 (8)	0.093 (9)	0.054 (5)	0.003 (5)	0.014 (7)	0.037 (7)
C43B	0.105 (13)	0.138 (13)	0.056 (6)	−0.057 (10)	0.024 (8)	0.018 (8)
C44B	0.083 (8)	0.171 (13)	0.076 (8)	−0.006 (7)	0.001 (6)	0.031 (8)
C45B	0.106 (6)	0.058 (13)	0.054 (9)	0.011 (11)	0.055 (7)	0.003 (9)
O1SB	0.088 (4)	0.062 (4)	0.058 (4)	0.018 (3)	0.038 (4)	0.006 (3)
C1SB	0.102 (8)	0.059 (10)	0.105 (11)	−0.021 (9)	0.004 (7)	0.019 (9)

Geometric parameters (Å, º)

O1—C2	1.385 (5)	C32—H32B	0.9800
O1—H1O	0.82 (5)	C32—H32C	0.9800
O2—C4	1.363 (5)	C33—C34	1.520 (5)
O2—H2O	0.85 (6)	C33—H33A	0.9900
O3—C9	1.389 (5)	C33—H33B	0.9900
O3—H3O	0.93 (6)	C34—H34A	0.9800
O4—C11	1.399 (5)	C34—H34B	0.9800
O4—H4O	0.91 (9)	C34—H34C	0.9800
O5—C16	1.373 (5)	C35—C36	1.508 (6)
O5—H5O	0.86 (5)	C35—H35A	0.9900
O6—C18	1.378 (5)	C35—H35B	0.9900
O6—H6O	0.90 (5)	C36—H36A	0.9800
O7—C23	1.394 (5)	C36—H36B	0.9800
O7—H7O	0.80 (6)	C36—H36C	0.9800
O8—C25	1.379 (5)	O2S—C2S	1.434 (6)
O8—H8O	0.94 (7)	O2S—H2S	0.9811
C1—C2	1.389 (6)	C2S—H2S1	0.9800
C1—C6	1.404 (5)	C2S—H2S2	0.9800
C1—C28	1.524 (6)	C2S—H2S3	0.9800
C2—C3	1.393 (6)	O1W—H1WA	0.9230
C3—C4	1.391 (6)	O1W—H1WB	0.9280
C3—H3A	0.9500	O1W—H2WB	1.4685
C4—C5	1.400 (6)	O1W—H3WA	1.1206
C5—C6	1.392 (5)	O1W—H3WB	1.2660
C5—C7	1.515 (5)	O2W—H1WA	1.4659
C6—H6A	0.9500	O2W—H2WA	0.8778
C7—C8	1.526 (5)	O2W—H2WB	0.9259
C7—C29	1.533 (6)	O2W—H3WA	1.2232
C7—H7A	1.0000	O2W—H3WB	1.3935
C8—C9	1.394 (6)	O3W—H3WA	0.9238
C8—C13	1.401 (5)	O3W—H3WB	0.9253
C9—C10	1.388 (6)	O9—C41	1.244 (10)
C10—C11	1.387 (6)	O10—C41	1.360 (10)
C10—H10A	0.9500	O10—H10O	0.9482
C11—C12	1.385 (6)	O10—H10P	0.7196
C12—C13	1.393 (6)	C41—C42	1.466 (12)
C12—C14	1.527 (6)	C42—C43	1.316 (12)
C13—H13A	0.9500	C42—C45	1.562 (12)
C14—C15	1.511 (5)	C43—C44	1.542 (18)
C14—C31	1.524 (6)	C43—H43A	0.9500
C14—H14A	1.0000	C44—H44A	0.9800
C15—C20	1.396 (5)	C44—H44B	0.9800
C15—C16	1.401 (6)	C44—H44C	0.9800
C16—C17	1.385 (6)	C45—H45A	0.9800
C17—C18	1.385 (6)	C45—H45B	0.9800
C17—H17A	0.9500	C45—H45C	0.9800
C18—C19	1.389 (5)	O1S—C1S	1.478 (14)
C19—C20	1.396 (5)	O1S—H1S	1.0305
C19—C21	1.523 (5)	O1S—H1SP	0.9621
C20—H20A	0.9500	C1S—H1S1	0.9800
C21—C22	1.526 (6)	C1S—H1S2	0.9800
C21—C33	1.529 (5)	C1S—H1S3	0.9800
C21—H21A	1.0000	C1S—H1SP	1.0819
C22—C23	1.383 (5)	O9B—C41B	1.239 (18)
C22—C27	1.385 (5)	O10B—C41B	1.376 (18)
C23—C24	1.392 (6)	O10B—H10O	1.3710
C24—C25	1.388 (6)	O10B—H10P	1.1067
C24—H24A	0.9500	C41B—C42B	1.471 (19)
C25—C26	1.397 (6)	C42B—C43B	1.316 (19)
C26—C27	1.390 (5)	C42B—C45B	1.565 (19)
C26—C28	1.531 (5)	C43B—C44B	1.57 (2)
C27—H27A	0.9500	C43B—H43B	0.9500
C28—C35	1.533 (5)	C44B—H44D	0.9800
C28—H28A	1.0000	C44B—H44E	0.9800
C29—C30	1.529 (6)	C44B—H44F	0.9800
C29—H29A	0.9900	C45B—H45D	0.9800
C29—H29B	0.9900	C45B—H45E	0.9800
C30—H30A	0.9800	C45B—H45F	0.9800
C30—H30B	0.9800	O1SB—C1SB	1.504 (18)
C30—H30C	0.9800	O1SB—H1SP	0.8574
C31—C32	1.524 (6)	C1SB—H1S	1.4123
C31—H31A	0.9900	C1SB—H1S4	0.9800
C31—H31B	0.9900	C1SB—H1S5	0.9800
C32—H32A	0.9800	C1SB—H1S6	0.9800
C2—O1—H1O	107 (3)	H32A—C32—H32C	109.5
C4—O2—H2O	111 (4)	H32B—C32—H32C	109.5
C9—O3—H3O	108 (3)	C34—C33—C21	113.1 (3)
C11—O4—H4O	104 (6)	C34—C33—H33A	109.0
C16—O5—H5O	114 (4)	C21—C33—H33A	109.0
C18—O6—H6O	113 (3)	C34—C33—H33B	109.0
C23—O7—H7O	108 (5)	C21—C33—H33B	109.0
C25—O8—H8O	120 (4)	H33A—C33—H33B	107.8
C2—C1—C6	116.3 (4)	C33—C34—H34A	109.5
C2—C1—C28	121.5 (4)	C33—C34—H34B	109.5
C6—C1—C28	122.1 (4)	H34A—C34—H34B	109.5
O1—C2—C1	122.1 (4)	C33—C34—H34C	109.5
O1—C2—C3	115.7 (4)	H34A—C34—H34C	109.5
C1—C2—C3	122.3 (4)	H34B—C34—H34C	109.5
C4—C3—C2	119.3 (4)	C36—C35—C28	113.4 (3)
C4—C3—H3A	120.3	C36—C35—H35A	108.9
C2—C3—H3A	120.3	C28—C35—H35A	108.9
O2—C4—C3	121.4 (4)	C36—C35—H35B	108.9
O2—C4—C5	117.6 (4)	C28—C35—H35B	108.9
C3—C4—C5	121.0 (4)	H35A—C35—H35B	107.7
C6—C5—C4	117.4 (4)	C35—C36—H36A	109.5
C6—C5—C7	123.0 (4)	C35—C36—H36B	109.5
C4—C5—C7	119.6 (4)	H36A—C36—H36B	109.5
C5—C6—C1	123.7 (4)	C35—C36—H36C	109.5
C5—C6—H6A	118.2	H36A—C36—H36C	109.5
C1—C6—H6A	118.2	H36B—C36—H36C	109.5
C5—C7—C8	111.5 (3)	C2S—O2S—H2S	109.4
C5—C7—C29	113.7 (3)	O2S—C2S—H2S1	109.5
C8—C7—C29	112.3 (3)	O2S—C2S—H2S2	109.5
C5—C7—H7A	106.2	H2S1—C2S—H2S2	109.5
C8—C7—H7A	106.2	O2S—C2S—H2S3	109.5
C29—C7—H7A	106.2	H2S1—C2S—H2S3	109.5
C9—C8—C13	116.1 (4)	H2S2—C2S—H2S3	109.5
C9—C8—C7	123.9 (4)	H1WA—O1W—H1WB	116.6
C13—C8—C7	120.0 (4)	H1WA—O1W—H2WB	72.9
C10—C9—O3	114.4 (4)	H1WB—O1W—H2WB	155.5
C10—C9—C8	121.5 (4)	H1WA—O1W—H3WA	104.5
O3—C9—C8	124.1 (4)	H1WB—O1W—H3WA	63.0
C11—C10—C9	119.7 (4)	H2WB—O1W—H3WA	93.2
C11—C10—H10A	120.1	H1WA—O1W—H3WB	126.2
C9—C10—H10A	120.1	H1WB—O1W—H3WB	113.3
C12—C11—C10	121.9 (4)	H2WB—O1W—H3WB	53.4
C12—C11—O4	121.7 (4)	H3WA—O1W—H3WB	81.2
C10—C11—O4	116.5 (4)	H1WA—O2W—H2WA	88.3
C11—C12—C13	116.2 (4)	H1WA—O2W—H2WB	72.9
C11—C12—C14	123.0 (4)	H2WA—O2W—H2WB	113.7
C13—C12—C14	120.8 (4)	H1WA—O2W—H3WA	73.5
C12—C13—C8	124.6 (4)	H2WA—O2W—H3WA	109.6
C12—C13—H13A	117.7	H2WB—O2W—H3WA	123.2
C8—C13—H13A	117.7	H1WA—O2W—H3WB	86.4
C15—C14—C31	114.8 (3)	H2WA—O2W—H3WB	173.3
C15—C14—C12	110.5 (3)	H2WB—O2W—H3WB	60.8
C31—C14—C12	112.1 (3)	H3WA—O2W—H3WB	72.7
C15—C14—H14A	106.3	H3WA—O3W—H3WB	114.7
C31—C14—H14A	106.3	C41—O10—H10O	109.4
C12—C14—H14A	106.3	C41—O10—H10P	99.5
C20—C15—C16	116.9 (4)	H10O—O10—H10P	11.7
C20—C15—C14	123.0 (4)	O9—C41—O10	117.7 (12)
C16—C15—C14	120.0 (4)	O9—C41—C42	127.0 (9)
O5—C16—C17	121.1 (4)	O10—C41—C42	114.7 (11)
O5—C16—C15	117.8 (4)	C43—C42—C41	117.7 (12)
C17—C16—C15	121.1 (4)	C43—C42—C45	125.8 (15)
C16—C17—C18	119.7 (4)	C41—C42—C45	116.4 (14)
C16—C17—H17A	120.2	C42—C43—C44	120.5 (15)
C18—C17—H17A	120.2	C42—C43—H43A	119.7
O6—C18—C17	114.9 (4)	C44—C43—H43A	119.7
O6—C18—C19	123.1 (4)	C43—C44—H44A	109.5
C17—C18—C19	121.9 (4)	C43—C44—H44B	109.5
C18—C19—C20	116.7 (4)	H44A—C44—H44B	109.5
C18—C19—C21	121.4 (3)	C43—C44—H44C	109.5
C20—C19—C21	122.0 (4)	H44A—C44—H44C	109.5
C19—C20—C15	123.7 (4)	H44B—C44—H44C	109.5
C19—C20—H20A	118.1	C42—C45—H45A	109.5
C15—C20—H20A	118.1	C42—C45—H45B	109.5
C19—C21—C22	111.3 (3)	H45A—C45—H45B	109.5
C19—C21—C33	113.6 (3)	C42—C45—H45C	109.5
C22—C21—C33	112.2 (3)	H45A—C45—H45C	109.5
C19—C21—H21A	106.4	H45B—C45—H45C	109.5
C22—C21—H21A	106.4	C1S—O1S—H1S	98.5
C33—C21—H21A	106.4	C1S—O1S—H1SP	47.0
C23—C22—C27	116.4 (4)	H1S—O1S—H1SP	90.8
C23—C22—C21	121.3 (4)	O1S—C1S—H1S1	109.5
C27—C22—C21	122.3 (4)	O1S—C1S—H1S2	109.5
C22—C23—C24	122.1 (4)	H1S1—C1S—H1S2	109.5
C22—C23—O7	117.7 (4)	O1S—C1S—H1S3	109.5
C24—C23—O7	120.2 (4)	H1S1—C1S—H1S3	109.5
C25—C24—C23	119.3 (4)	H1S2—C1S—H1S3	109.5
C25—C24—H24A	120.4	O1S—C1S—H1SP	40.6
C23—C24—H24A	120.4	H1S1—C1S—H1SP	105.9
O8—C25—C24	120.8 (4)	H1S2—C1S—H1SP	73.3
O8—C25—C26	118.3 (4)	H1S3—C1S—H1SP	140.7
C24—C25—C26	120.9 (4)	C41B—O10B—H10O	116.7
C27—C26—C25	116.8 (4)	C41B—O10B—H10P	113.8
C27—C26—C28	122.5 (4)	H10O—O10B—H10P	4.8
C25—C26—C28	120.7 (4)	O9B—C41B—O10B	123 (4)
C22—C27—C26	124.4 (4)	O9B—C41B—C42B	119 (4)
C22—C27—H27A	117.8	O10B—C41B—C42B	111 (4)
C26—C27—H27A	117.8	C43B—C42B—C41B	129 (4)
C1—C28—C26	110.6 (3)	C43B—C42B—C45B	126 (4)
C1—C28—C35	114.1 (3)	C41B—C42B—C45B	106 (4)
C26—C28—C35	111.8 (3)	C42B—C43B—C44B	129 (4)
C1—C28—H28A	106.6	C42B—C43B—H43B	115.3
C26—C28—H28A	106.6	C44B—C43B—H43B	115.3
C35—C28—H28A	106.6	C43B—C44B—H44D	109.5
C30—C29—C7	112.8 (4)	C43B—C44B—H44E	109.5
C30—C29—H29A	109.0	H44D—C44B—H44E	109.5
C7—C29—H29A	109.0	C43B—C44B—H44F	109.5
C30—C29—H29B	109.0	H44D—C44B—H44F	109.5
C7—C29—H29B	109.0	H44E—C44B—H44F	109.5
H29A—C29—H29B	107.8	C42B—C45B—H45D	109.5
C29—C30—H30A	109.5	C42B—C45B—H45E	109.5
C29—C30—H30B	109.5	H45D—C45B—H45E	109.5
H30A—C30—H30B	109.5	C42B—C45B—H45F	109.5
C29—C30—H30C	109.5	H45D—C45B—H45F	109.5
H30A—C30—H30C	109.5	H45E—C45B—H45F	109.5
H30B—C30—H30C	109.5	C1SB—O1SB—H1SP	83.9
C32—C31—C14	112.0 (4)	O1SB—C1SB—H1S	83.6
C32—C31—H31A	109.2	O1SB—C1SB—H1S4	109.5
C14—C31—H31A	109.2	H1S—C1SB—H1S4	75.2
C32—C31—H31B	109.2	O1SB—C1SB—H1S5	109.5
C14—C31—H31B	109.2	H1S—C1SB—H1S5	54.1
H31A—C31—H31B	107.9	H1S4—C1SB—H1S5	109.5
C31—C32—H32A	109.5	O1SB—C1SB—H1S6	109.5
C31—C32—H32B	109.5	H1S—C1SB—H1S6	162.6
H32A—C32—H32B	109.5	H1S4—C1SB—H1S6	109.5
C31—C32—H32C	109.5	H1S5—C1SB—H1S6	109.5