5,11,17,23,29,35-Hexa-tert-butyl-37,38,39,40,41,42-hexa­hydroxy­calix[6]arene dichloro­methane disolvate

Crystallization of the title compound, C₆₆H₈₄O₆·2CH₂Cl₂, from a methanol–dichloro­methane solution yields a 1:2 inclusion compound with dichloro­methane. The host–guest compound crystallizes with one host and two guest mol­ecules in the asymmetric unit. The mol­ecular geometry is stabilized by intra­molecular O—H...O hydrogen bonds, whereas the packing structure is dominated by van der Waals forces.

Key indicators

• Single-crystal X-ray study
• T = 93 K
• Mean [sigma](C-C) = 0.004 Å
• Disorder in main residue
• R factor = 0.054
• wR factor = 0.133
• Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.71 Ratio
PLAT222_ALERT_3_B Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       4.06 Ratio

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        Cl3
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C682
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for       C681
PLAT301_ALERT_3_C Main Residue  Disorder .........................       4.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      25.00 Perc.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C7     ..  C8      ..       3.18 Ang.

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   8 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   5 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Bruker, 2004); cell refinement: SMART; data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

5,11,17,23,29,35-Hexa-tert-butyl-37,38,39,40,41,42-hexahydroxycalix[6]arene dichloromethane disolvate

Crystal data

C66H84O6·2CH2Cl2	Z = 2
Mr = 1143.18	F(000) = 1224
Triclinic, P1	Dx = 1.199 Mg m^−3
a = 12.2406 (10) Å	Mo Kα radiation, λ = 0.71073 Å
b = 17.2407 (6) Å	Cell parameters from 9049 reflections
c = 17.4069 (6) Å	θ = 2.3–25.8°
α = 118.615 (2)°	µ = 0.24 mm^−1
β = 92.644 (2)°	T = 93 K
γ = 97.961 (2)°	Needle, colourless
V = 3166.9 (3) Å^3	0.39 × 0.11 × 0.09 mm

Data collection

Bruker SMART CCD area-detector diffractometer	6703 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.064
Graphite monochromator	θmax = 25.8°, θmin = 1.4°
φ and ω scans	h = −14→14
35059 measured reflections	k = −21→21
12156 independent reflections	l = −21→21

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.055	H-atom parameters constrained
wR(F^2) = 0.133	w = 1/[σ^2(Fo^2) + (0.0595P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.96	(Δ/σ)max = 0.013
12156 reflections	Δρmax = 1.14 e Å^−3
731 parameters	Δρmin = −0.72 e Å^−3
4 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0035 (5)

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	0.88044 (17)	0.25588 (11)	0.47283 (12)	0.0247 (5)
H1O	0.9084	0.2156	0.4761	0.037*
O2	0.96421 (14)	0.14726 (11)	0.50900 (11)	0.0155 (4)
H2O	0.9350	0.1623	0.5556	0.023*
O3	0.83898 (14)	0.20289 (11)	0.63634 (12)	0.0203 (5)
H3O	0.8259	0.2555	0.6621	0.030*
O4	0.84050 (15)	0.37874 (11)	0.73141 (11)	0.0202 (5)
H4O	0.8957	0.4197	0.7446	0.030*
O5	1.01784 (14)	0.49436 (11)	0.74024 (12)	0.0175 (4)
H5O	1.0078	0.4751	0.6856	0.026*
O6	0.91444 (15)	0.42730 (11)	0.57923 (12)	0.0192 (4)
H6O	0.8933	0.3720	0.5446	0.029*
C1	0.9598 (2)	0.10610 (16)	0.32982 (18)	0.0152 (6)
H1A	1.0205	0.1508	0.3756	0.018*
H1B	0.9922	0.0749	0.2742	0.018*
C2	0.9140 (2)	0.03741 (16)	0.35731 (17)	0.0138 (6)
C3	0.8737 (2)	−0.05163 (16)	0.29352 (18)	0.0156 (6)
H3	0.8744	−0.0684	0.2330	0.019*
C4	0.8325 (2)	−0.11675 (16)	0.31560 (17)	0.0147 (6)
C5	0.8299 (2)	−0.08887 (16)	0.40500 (18)	0.0163 (6)
H5	0.7995	−0.1318	0.4213	0.020*
C6	0.8698 (2)	−0.00093 (16)	0.47140 (17)	0.0136 (6)
C7	0.9134 (2)	0.06065 (16)	0.44568 (17)	0.0130 (6)
C8	0.8681 (2)	0.02363 (16)	0.56766 (17)	0.0146 (6)
H8A	0.8766	−0.0296	0.5736	0.018*
H8B	0.9329	0.0716	0.6034	0.018*
C9	0.7636 (2)	0.05539 (16)	0.60480 (17)	0.0145 (6)
C10	0.6777 (2)	−0.00461 (17)	0.60763 (17)	0.0152 (6)
H10	0.6860	−0.0654	0.5852	0.018*
C11	0.5803 (2)	0.02035 (16)	0.64173 (17)	0.0157 (6)
C12	0.5701 (2)	0.10940 (17)	0.67155 (17)	0.0167 (6)
H12	0.5034	0.1280	0.6939	0.020*
C13	0.6528 (2)	0.17228 (16)	0.67023 (17)	0.0137 (6)
C14	0.7500 (2)	0.14417 (16)	0.63750 (17)	0.0136 (6)
C15	0.6355 (2)	0.26803 (15)	0.70131 (17)	0.0148 (6)
H15A	0.5546	0.2684	0.6997	0.018*
H15B	0.6631	0.2867	0.6590	0.018*
C16	0.6922 (2)	0.33729 (15)	0.79349 (17)	0.0140 (6)
C17	0.6446 (2)	0.34519 (16)	0.86790 (18)	0.0165 (6)
H17	0.5778	0.3053	0.8597	0.020*
C18	0.6913 (2)	0.40903 (16)	0.95312 (18)	0.0165 (6)
C19	0.7873 (2)	0.46925 (16)	0.96159 (18)	0.0156 (6)
H19	0.8187	0.5159	1.0190	0.019*
C20	0.8382 (2)	0.46371 (16)	0.89018 (17)	0.0148 (6)
C21	0.7915 (2)	0.39433 (16)	0.80614 (17)	0.0151 (6)
C22	0.9446 (2)	0.52918 (16)	0.90360 (17)	0.0163 (6)
H22A	0.9690	0.5670	0.9678	0.020*
H22B	1.0033	0.4939	0.8774	0.020*
C23	0.9360 (2)	0.59109 (16)	0.86459 (17)	0.0151 (6)
C24	0.8912 (2)	0.66827 (16)	0.90874 (17)	0.0159 (6)
H24	0.8650	0.6816	0.9635	0.019*
C25	0.8831 (2)	0.72737 (16)	0.87573 (17)	0.0163 (6)
C26	0.9231 (2)	0.70613 (16)	0.79589 (18)	0.0163 (6)
H26	0.9196	0.7457	0.7726	0.020*
C27	0.9681 (2)	0.62910 (16)	0.74861 (17)	0.0139 (6)
C28	0.9746 (2)	0.57236 (16)	0.78365 (17)	0.0149 (6)
C29	1.0043 (2)	0.60945 (17)	0.65929 (17)	0.0162 (6)
H29A	1.0417	0.6662	0.6633	0.019*
H29B	1.0589	0.5686	0.6445	0.019*
C30	0.9075 (2)	0.56694 (16)	0.58630 (17)	0.0136 (6)
C31	0.8574 (2)	0.61693 (17)	0.55659 (17)	0.0168 (6)
H31	0.8880	0.6789	0.5807	0.020*
C32	0.7641 (2)	0.57999 (17)	0.49292 (17)	0.0157 (6)
C33	0.7208 (2)	0.48871 (16)	0.46066 (17)	0.0156 (6)
H33	0.6561	0.4621	0.4183	0.019*
C34	0.7675 (2)	0.43559 (16)	0.48740 (17)	0.0139 (6)
C35	0.8628 (2)	0.47538 (16)	0.54887 (17)	0.0131 (6)
C36	0.7097 (2)	0.33851 (16)	0.45321 (17)	0.0165 (6)
H36A	0.7158	0.3249	0.5022	0.020*
H36B	0.6297	0.3338	0.4365	0.020*
C37	0.7536 (2)	0.26736 (15)	0.37500 (17)	0.0129 (6)
C38	0.7088 (2)	0.23963 (16)	0.28854 (17)	0.0154 (6)
H38	0.6531	0.2687	0.2793	0.018*
C39	0.7429 (2)	0.17103 (17)	0.21563 (17)	0.0161 (6)
C40	0.8258 (2)	0.13029 (16)	0.23189 (17)	0.0151 (6)
H40	0.8507	0.0835	0.1830	0.018*
C41	0.8732 (2)	0.15529 (16)	0.31639 (17)	0.0135 (6)
C42	0.8359 (2)	0.22488 (16)	0.38688 (17)	0.0136 (6)
C43	0.7931 (2)	−0.21657 (17)	0.24767 (18)	0.0173 (6)
C44	0.7968 (2)	−0.23455 (18)	0.15344 (18)	0.0249 (7)
H44A	0.7513	−0.1976	0.1423	0.037*
H44B	0.7676	−0.2982	0.1123	0.037*
H44C	0.8738	−0.2195	0.1450	0.037*
C45	0.8678 (2)	−0.27247 (17)	0.26523 (19)	0.0221 (7)
H45A	0.8421	−0.3363	0.2228	0.033*
H45B	0.8642	−0.2626	0.3253	0.033*
H45C	0.9448	−0.2542	0.2588	0.033*
C46	0.6718 (2)	−0.24488 (17)	0.25657 (19)	0.0229 (7)
H46A	0.6243	−0.2115	0.2415	0.034*
H46B	0.6662	−0.2317	0.3175	0.034*
H46C	0.6475	−0.3095	0.2164	0.034*
C47	0.4888 (2)	−0.04856 (17)	0.64451 (19)	0.0206 (7)
C481	0.4404 (4)	−0.1195 (3)	0.5495 (3)	0.0426 (12)	0.81
H48A	0.3800	−0.1627	0.5505	0.064*	0.81
H48B	0.4988	−0.1511	0.5185	0.064*	0.81
H48C	0.4113	−0.0900	0.5189	0.064*	0.81
C491	0.5405 (3)	−0.0977 (3)	0.6881 (3)	0.0344 (10)	0.81
H49A	0.5704	−0.0541	0.7496	0.052*	0.81
H49B	0.6006	−0.1253	0.6560	0.052*	0.81
H49C	0.4831	−0.1443	0.6864	0.052*	0.81
C501	0.3964 (3)	−0.0065 (2)	0.6956 (3)	0.0356 (11)	0.81
H50A	0.3571	0.0189	0.6652	0.053*	0.81
H50B	0.4284	0.0413	0.7551	0.053*	0.81
H50C	0.3441	−0.0525	0.6997	0.053*	0.81
C482	0.5203 (13)	−0.1379 (9)	0.6152 (13)	0.0344 (10)	0.19
H48D	0.4654	−0.1746	0.6296	0.052*	0.19
H48E	0.5938	−0.1298	0.6456	0.052*	0.19
H48F	0.5225	−0.1683	0.5514	0.052*	0.19
C492	0.4554 (15)	−0.0040 (10)	0.7382 (10)	0.0356 (11)	0.19
H49D	0.3976	−0.0459	0.7436	0.053*	0.19
H49E	0.4267	0.0503	0.7493	0.053*	0.19
H49F	0.5206	0.0122	0.7813	0.053*	0.19
C502	0.3888 (13)	−0.0594 (12)	0.5797 (11)	0.0426 (12)	0.19
H50D	0.4145	−0.0673	0.5243	0.064*	0.19
H50E	0.3551	−0.0055	0.6065	0.064*	0.19
H50F	0.3335	−0.1120	0.5677	0.064*	0.19
C51	0.6446 (2)	0.41417 (17)	1.03545 (18)	0.0172 (6)
C52	0.7323 (2)	0.3971 (2)	1.0883 (2)	0.0322 (8)
H52A	0.7519	0.3382	1.0511	0.048*
H52B	0.7023	0.3982	1.1400	0.048*
H52C	0.7987	0.4440	1.1077	0.048*
C53	0.5392 (2)	0.34452 (18)	1.01248 (19)	0.0283 (7)
H53A	0.4808	0.3559	0.9808	0.042*
H53B	0.5143	0.3488	1.0668	0.042*
H53C	0.5549	0.2842	0.9751	0.042*
C54	0.6186 (2)	0.50760 (18)	1.09430 (19)	0.0302 (8)
H54A	0.6857	0.5530	1.1095	0.045*
H54B	0.5938	0.5110	1.1484	0.045*
H54C	0.5597	0.5187	1.0627	0.045*
C55	0.8325 (2)	0.81186 (17)	0.92733 (18)	0.0219 (7)
C56	0.7154 (2)	0.78449 (18)	0.94566 (19)	0.0245 (7)
H56A	0.6679	0.7439	0.8896	0.037*
H56B	0.6830	0.8383	0.9786	0.037*
H56C	0.7208	0.7539	0.9804	0.037*
C57	0.9073 (2)	0.87501 (18)	1.01445 (19)	0.0260 (7)
H57A	0.9173	0.8430	1.0472	0.039*
H57B	0.8726	0.9269	1.0496	0.039*
H57C	0.9798	0.8956	1.0024	0.039*
C58	0.8216 (3)	0.86279 (19)	0.8763 (2)	0.0343 (8)
H58A	0.8955	0.8824	0.8654	0.051*
H58B	0.7878	0.9154	0.9110	0.051*
H58C	0.7745	0.8232	0.8198	0.051*
C59	0.7071 (2)	0.63263 (17)	0.45842 (18)	0.0180 (6)
C60	0.7664 (2)	0.73094 (17)	0.5002 (2)	0.0269 (7)
H60A	0.7697	0.7596	0.5646	0.040*
H60B	0.7252	0.7629	0.4785	0.040*
H60C	0.8420	0.7331	0.4843	0.040*
C61	0.5865 (2)	0.63358 (18)	0.4814 (2)	0.0269 (7)
H61A	0.5448	0.5718	0.4531	0.040*
H61B	0.5506	0.6683	0.4601	0.040*
H61C	0.5876	0.6612	0.5455	0.040*
C62	0.7054 (3)	0.58830 (18)	0.35849 (19)	0.0278 (7)
H62A	0.7819	0.5885	0.3442	0.042*
H62B	0.6683	0.6218	0.3362	0.042*
H62C	0.6650	0.5262	0.3310	0.042*
C63	0.6932 (2)	0.13841 (18)	0.12067 (18)	0.0224 (7)
C64	0.6000 (3)	0.1866 (2)	0.1157 (2)	0.0320 (8)
H64A	0.5403	0.1763	0.1472	0.048*
H64B	0.5708	0.1632	0.0538	0.048*
H64C	0.6290	0.2512	0.1430	0.048*
C65	0.7858 (3)	0.1526 (3)	0.0697 (2)	0.0484 (10)
H65A	0.8169	0.2169	0.0970	0.073*
H65B	0.7551	0.1302	0.0083	0.073*
H65C	0.8446	0.1200	0.0714	0.073*
C66	0.6437 (3)	0.03699 (19)	0.0767 (2)	0.0387 (9)
H66A	0.7022	0.0040	0.0780	0.058*
H66B	0.6132	0.0152	0.0153	0.058*
H66C	0.5843	0.0276	0.1088	0.058*
Cl1	0.44597 (8)	0.36311 (6)	0.29167 (6)	0.0522 (3)
Cl2	0.38160 (9)	0.50042 (7)	0.25865 (9)	0.0779 (4)
C67	0.3484 (3)	0.4303 (2)	0.3052 (2)	0.0520 (11)
H67A	0.3442	0.4679	0.3690	0.062*
H67B	0.2745	0.3919	0.2770	0.062*
Cl3	0.83819 (8)	0.04546 (6)	0.82151 (6)	0.0517 (3)
C681	0.8302 (7)	0.1413 (7)	0.8208 (7)	0.0313 (13)	0.43
H68A	0.7505	0.1429	0.8107	0.038*	0.43
H68B	0.8644	0.1387	0.7693	0.038*	0.43
Cl41	0.8892 (4)	0.2394 (3)	0.9106 (2)	0.0438 (8)	0.43
C682	0.7818 (5)	0.1451 (5)	0.8447 (5)	0.0313 (13)	0.57
H68C	0.7314	0.1334	0.7927	0.038*	0.57
H68D	0.7383	0.1610	0.8951	0.038*	0.57
Cl42	0.8937 (3)	0.2367 (2)	0.87067 (18)	0.0512 (7)	0.57

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O1	0.0426 (13)	0.0136 (10)	0.0162 (11)	0.0093 (9)	−0.0057 (9)	0.0057 (9)
O2	0.0220 (11)	0.0112 (9)	0.0127 (10)	0.0011 (8)	0.0036 (8)	0.0059 (8)
O3	0.0232 (11)	0.0100 (9)	0.0244 (12)	0.0004 (8)	0.0093 (9)	0.0061 (9)
O4	0.0252 (11)	0.0139 (10)	0.0159 (11)	−0.0023 (8)	0.0090 (9)	0.0038 (8)
O5	0.0200 (10)	0.0162 (10)	0.0152 (10)	0.0035 (8)	0.0036 (9)	0.0067 (9)
O6	0.0248 (11)	0.0108 (9)	0.0183 (11)	0.0022 (8)	−0.0008 (9)	0.0050 (9)
C1	0.0178 (15)	0.0144 (13)	0.0163 (15)	0.0050 (11)	0.0060 (12)	0.0090 (12)
C2	0.0140 (14)	0.0135 (13)	0.0189 (16)	0.0047 (11)	0.0056 (12)	0.0110 (12)
C3	0.0133 (14)	0.0192 (14)	0.0153 (15)	0.0056 (11)	0.0030 (11)	0.0084 (12)
C4	0.0149 (14)	0.0150 (13)	0.0164 (15)	0.0045 (11)	0.0037 (12)	0.0088 (12)
C5	0.0160 (15)	0.0138 (13)	0.0238 (17)	0.0022 (11)	0.0051 (12)	0.0128 (13)
C6	0.0121 (14)	0.0144 (13)	0.0171 (15)	0.0059 (11)	0.0056 (11)	0.0087 (12)
C7	0.0128 (14)	0.0100 (13)	0.0154 (15)	0.0053 (11)	0.0043 (11)	0.0045 (12)
C8	0.0197 (15)	0.0116 (13)	0.0145 (15)	0.0041 (11)	0.0065 (12)	0.0072 (12)
C9	0.0165 (14)	0.0151 (14)	0.0123 (15)	0.0032 (11)	0.0014 (11)	0.0072 (12)
C10	0.0194 (15)	0.0122 (13)	0.0138 (15)	0.0018 (11)	0.0011 (12)	0.0065 (12)
C11	0.0181 (15)	0.0124 (13)	0.0144 (15)	0.0013 (11)	0.0024 (12)	0.0051 (12)
C12	0.0102 (14)	0.0187 (14)	0.0177 (15)	0.0015 (11)	0.0048 (11)	0.0062 (12)
C13	0.0157 (14)	0.0139 (13)	0.0095 (14)	0.0024 (11)	−0.0010 (11)	0.0044 (11)
C14	0.0169 (14)	0.0113 (13)	0.0117 (15)	−0.0012 (11)	0.0010 (11)	0.0060 (12)
C15	0.0151 (14)	0.0121 (13)	0.0163 (15)	0.0006 (11)	0.0040 (12)	0.0065 (12)
C16	0.0166 (14)	0.0072 (12)	0.0173 (15)	0.0034 (11)	0.0023 (12)	0.0050 (12)
C17	0.0175 (15)	0.0099 (13)	0.0225 (16)	0.0001 (11)	0.0043 (12)	0.0086 (12)
C18	0.0200 (15)	0.0123 (13)	0.0203 (16)	0.0030 (11)	0.0044 (12)	0.0102 (12)
C19	0.0193 (15)	0.0110 (13)	0.0154 (15)	0.0004 (11)	−0.0027 (12)	0.0066 (12)
C20	0.0159 (14)	0.0128 (13)	0.0185 (16)	0.0025 (11)	0.0003 (12)	0.0100 (12)
C21	0.0213 (15)	0.0107 (13)	0.0145 (15)	0.0025 (11)	0.0047 (12)	0.0072 (12)
C22	0.0192 (15)	0.0145 (14)	0.0142 (15)	−0.0001 (11)	0.0008 (12)	0.0072 (12)
C23	0.0127 (14)	0.0157 (14)	0.0169 (16)	−0.0038 (11)	−0.0006 (12)	0.0097 (12)
C24	0.0192 (15)	0.0132 (13)	0.0122 (15)	−0.0007 (11)	0.0055 (12)	0.0043 (12)
C25	0.0177 (15)	0.0132 (13)	0.0154 (15)	−0.0016 (11)	0.0036 (12)	0.0060 (12)
C26	0.0172 (15)	0.0119 (13)	0.0200 (16)	−0.0022 (11)	−0.0006 (12)	0.0094 (12)
C27	0.0109 (14)	0.0133 (13)	0.0160 (15)	−0.0035 (11)	0.0000 (11)	0.0076 (12)
C28	0.0120 (14)	0.0099 (13)	0.0177 (16)	−0.0011 (11)	0.0010 (12)	0.0036 (12)
C29	0.0146 (14)	0.0142 (13)	0.0201 (16)	−0.0011 (11)	0.0027 (12)	0.0098 (12)
C30	0.0152 (14)	0.0140 (13)	0.0120 (15)	0.0011 (11)	0.0065 (11)	0.0067 (12)
C31	0.0196 (15)	0.0108 (13)	0.0180 (16)	−0.0015 (11)	0.0043 (12)	0.0065 (12)
C32	0.0167 (14)	0.0164 (14)	0.0156 (15)	0.0035 (11)	0.0080 (12)	0.0085 (12)
C33	0.0145 (14)	0.0150 (13)	0.0132 (15)	−0.0003 (11)	0.0032 (11)	0.0045 (12)
C34	0.0172 (14)	0.0108 (13)	0.0125 (15)	0.0027 (11)	0.0070 (12)	0.0043 (12)
C35	0.0147 (14)	0.0148 (13)	0.0145 (15)	0.0074 (11)	0.0067 (12)	0.0092 (12)
C36	0.0181 (15)	0.0117 (13)	0.0186 (16)	0.0003 (11)	0.0031 (12)	0.0071 (12)
C37	0.0162 (14)	0.0067 (12)	0.0151 (15)	−0.0021 (11)	0.0043 (12)	0.0055 (11)
C38	0.0140 (14)	0.0122 (13)	0.0216 (16)	−0.0013 (11)	0.0002 (12)	0.0107 (12)
C39	0.0168 (15)	0.0157 (14)	0.0149 (15)	−0.0015 (11)	0.0028 (12)	0.0080 (12)
C40	0.0172 (14)	0.0113 (13)	0.0158 (15)	0.0014 (11)	0.0072 (12)	0.0057 (12)
C41	0.0155 (14)	0.0088 (12)	0.0187 (16)	−0.0001 (11)	0.0042 (12)	0.0092 (12)
C42	0.0175 (14)	0.0091 (12)	0.0125 (15)	−0.0023 (11)	−0.0001 (12)	0.0053 (11)
C43	0.0207 (15)	0.0159 (14)	0.0172 (16)	0.0042 (12)	0.0048 (12)	0.0092 (12)
C44	0.0341 (18)	0.0158 (14)	0.0211 (17)	0.0018 (13)	0.0019 (14)	0.0070 (13)
C45	0.0243 (16)	0.0144 (14)	0.0232 (17)	0.0024 (12)	0.0010 (13)	0.0062 (13)
C46	0.0226 (16)	0.0168 (14)	0.0241 (17)	0.0013 (12)	0.0017 (13)	0.0065 (13)
C47	0.0171 (15)	0.0186 (14)	0.0256 (17)	−0.0020 (12)	0.0039 (13)	0.0118 (13)
C481	0.049 (3)	0.030 (2)	0.028 (2)	−0.0261 (19)	0.002 (2)	0.008 (2)
C491	0.026 (2)	0.040 (2)	0.055 (3)	0.0035 (18)	0.010 (2)	0.038 (2)
C501	0.028 (2)	0.0222 (19)	0.058 (3)	0.0008 (18)	0.020 (2)	0.021 (2)
C482	0.026 (2)	0.040 (2)	0.055 (3)	0.0035 (18)	0.010 (2)	0.038 (2)
C492	0.028 (2)	0.0222 (19)	0.058 (3)	0.0008 (18)	0.020 (2)	0.021 (2)
C502	0.049 (3)	0.030 (2)	0.028 (2)	−0.0261 (19)	0.002 (2)	0.008 (2)
C51	0.0205 (15)	0.0152 (14)	0.0152 (15)	−0.0002 (11)	0.0033 (12)	0.0077 (12)
C52	0.0329 (18)	0.0445 (19)	0.0316 (19)	0.0041 (15)	0.0071 (15)	0.0289 (17)
C53	0.0317 (18)	0.0270 (16)	0.0211 (17)	−0.0066 (13)	0.0062 (14)	0.0107 (14)
C54	0.0344 (19)	0.0260 (16)	0.0223 (18)	−0.0010 (14)	0.0114 (14)	0.0067 (14)
C55	0.0301 (17)	0.0168 (14)	0.0198 (17)	0.0077 (12)	0.0069 (13)	0.0085 (13)
C56	0.0228 (16)	0.0236 (15)	0.0227 (17)	0.0066 (13)	0.0042 (13)	0.0073 (14)
C57	0.0289 (17)	0.0165 (14)	0.0260 (18)	0.0024 (12)	0.0073 (14)	0.0052 (13)
C58	0.058 (2)	0.0255 (17)	0.032 (2)	0.0250 (16)	0.0190 (17)	0.0179 (15)
C59	0.0211 (15)	0.0143 (14)	0.0215 (16)	0.0022 (11)	0.0017 (12)	0.0112 (13)
C60	0.0320 (18)	0.0182 (15)	0.0321 (19)	0.0021 (13)	−0.0023 (14)	0.0147 (14)
C61	0.0279 (17)	0.0218 (15)	0.0343 (19)	0.0047 (13)	0.0011 (14)	0.0165 (15)
C62	0.0377 (19)	0.0219 (15)	0.0270 (18)	0.0032 (14)	0.0003 (15)	0.0154 (14)
C63	0.0241 (16)	0.0252 (16)	0.0161 (16)	0.0066 (13)	−0.0010 (13)	0.0085 (13)
C64	0.041 (2)	0.0321 (17)	0.0226 (18)	0.0126 (15)	−0.0044 (15)	0.0126 (15)
C65	0.046 (2)	0.084 (3)	0.031 (2)	0.018 (2)	0.0103 (17)	0.039 (2)
C66	0.044 (2)	0.0276 (17)	0.030 (2)	0.0135 (15)	−0.0115 (16)	0.0027 (16)
Cl1	0.0593 (6)	0.0412 (5)	0.0460 (6)	0.0056 (4)	−0.0164 (5)	0.0165 (5)
Cl2	0.0762 (8)	0.0579 (7)	0.1057 (10)	0.0017 (6)	−0.0338 (7)	0.0513 (7)
C67	0.0282 (19)	0.057 (2)	0.032 (2)	−0.0105 (17)	0.0128 (16)	−0.0048 (18)
Cl3	0.0624 (6)	0.0398 (5)	0.0471 (6)	0.0122 (4)	−0.0043 (5)	0.0171 (5)
C681	0.027 (4)	0.041 (2)	0.032 (4)	0.007 (3)	0.006 (3)	0.022 (3)
Cl41	0.0423 (15)	0.0329 (13)	0.049 (2)	0.0106 (10)	0.0068 (18)	0.0133 (17)
C682	0.027 (4)	0.041 (2)	0.032 (4)	0.007 (3)	0.006 (3)	0.022 (3)
Cl42	0.0352 (11)	0.0492 (13)	0.068 (2)	0.0022 (9)	−0.0059 (16)	0.0307 (17)

Geometric parameters (Å, º)

O1—C42	1.378 (3)	C43—C46	1.537 (4)
O1—H1O	0.8400	C44—H44A	0.9800
O2—C7	1.391 (3)	C44—H44B	0.9800
O2—H2O	0.8400	C44—H44C	0.9800
O3—C14	1.388 (3)	C45—H45A	0.9800
O3—H3O	0.8400	C45—H45B	0.9800
O4—C21	1.381 (3)	C45—H45C	0.9800
O4—H4O	0.8400	C46—H46A	0.9800
O5—C28	1.386 (3)	C46—H46B	0.9800
O5—H5O	0.8400	C46—H46C	0.9800
O6—C35	1.379 (3)	C47—C501	1.516 (4)
O6—H6O	0.8400	C47—C481	1.534 (4)
C1—C41	1.521 (4)	C47—C491	1.553 (4)
C1—C2	1.526 (3)	C481—H48A	0.9800
C1—H1A	0.9900	C481—H48B	0.9800
C1—H1B	0.9900	C481—H48C	0.9800
C2—C7	1.392 (4)	C491—H49A	0.9800
C2—C3	1.393 (3)	C491—H49B	0.9800
C3—C4	1.392 (3)	C491—H49C	0.9800
C3—H3	0.9500	C501—H50A	0.9800
C4—C5	1.395 (4)	C501—H50B	0.9800
C4—C43	1.536 (3)	C501—H50C	0.9800
C5—C6	1.392 (3)	C482—H48D	0.9800
C5—H5	0.9500	C482—H48E	0.9800
C6—C7	1.391 (3)	C482—H48F	0.9800
C6—C8	1.521 (3)	C492—H49D	0.9800
C8—C9	1.512 (3)	C492—H49E	0.9800
C8—H8A	0.9900	C492—H49F	0.9800
C8—H8B	0.9900	C502—H50D	0.9800
C9—C10	1.390 (3)	C502—H50E	0.9800
C9—C14	1.393 (3)	C502—H50F	0.9800
C10—C11	1.386 (4)	C51—C53	1.526 (3)
C10—H10	0.9500	C51—C54	1.528 (4)
C11—C12	1.392 (3)	C51—C52	1.530 (4)
C11—C47	1.536 (3)	C52—H52A	0.9800
C12—C13	1.386 (3)	C52—H52B	0.9800
C12—H12	0.9500	C52—H52C	0.9800
C13—C14	1.391 (4)	C53—H53A	0.9800
C13—C15	1.521 (3)	C53—H53B	0.9800
C15—C16	1.522 (3)	C53—H53C	0.9800
C15—H15A	0.9900	C54—H54A	0.9800
C15—H15B	0.9900	C54—H54B	0.9800
C16—C21	1.389 (3)	C54—H54C	0.9800
C16—C17	1.399 (4)	C55—C57	1.529 (4)
C17—C18	1.386 (4)	C55—C58	1.532 (4)
C17—H17	0.9500	C55—C56	1.542 (4)
C18—C19	1.407 (3)	C56—H56A	0.9800
C18—C51	1.535 (4)	C56—H56B	0.9800
C19—C20	1.384 (4)	C56—H56C	0.9800
C19—H19	0.9500	C57—H57A	0.9800
C20—C21	1.398 (3)	C57—H57B	0.9800
C20—C22	1.528 (3)	C57—H57C	0.9800
C22—C23	1.526 (4)	C58—H58A	0.9800
C22—H22A	0.9900	C58—H58B	0.9800
C22—H22B	0.9900	C58—H58C	0.9800
C23—C24	1.387 (3)	C59—C62	1.526 (4)
C23—C28	1.408 (4)	C59—C60	1.536 (3)
C24—C25	1.401 (4)	C59—C61	1.548 (4)
C24—H24	0.9500	C60—H60A	0.9800
C25—C26	1.389 (4)	C60—H60B	0.9799
C25—C55	1.536 (4)	C60—H60C	0.9800
C26—C27	1.394 (3)	C61—H61A	0.9800
C26—H26	0.9500	C61—H61B	0.9800
C27—C28	1.387 (4)	C61—H61C	0.9800
C27—C29	1.526 (4)	C62—H62A	0.9800
C29—C30	1.512 (3)	C62—H62B	0.9800
C29—H29A	0.9900	C62—H62C	0.9800
C29—H29B	0.9900	C63—C64	1.524 (4)
C30—C31	1.389 (4)	C63—C65	1.534 (4)
C30—C35	1.400 (3)	C63—C66	1.547 (4)
C31—C32	1.394 (3)	C64—H64A	0.9800
C31—H31	0.9500	C64—H64B	0.9800
C32—C33	1.403 (3)	C64—H64C	0.9800
C32—C59	1.526 (4)	C65—H65A	0.9800
C33—C34	1.382 (4)	C65—H65B	0.9800
C33—H33	0.9500	C65—H65C	0.9800
C34—C35	1.392 (3)	C66—H66A	0.9800
C34—C36	1.528 (3)	C66—H66B	0.9800
C36—C37	1.516 (3)	C66—H66C	0.9800
C36—H36A	0.9900	Cl1—C67	1.723 (4)
C36—H36B	0.9900	Cl2—C67	1.765 (4)
C37—C42	1.387 (4)	C67—H67A	0.9900
C37—C38	1.399 (4)	C67—H67B	0.9900
C38—C39	1.390 (4)	Cl3—C681	1.675 (10)
C38—H38	0.9500	Cl3—C682	1.812 (7)
C39—C40	1.402 (4)	C681—Cl41	1.688 (11)
C39—C63	1.530 (4)	C681—H68A	0.9900
C40—C41	1.389 (4)	C681—H68B	0.9900
C40—H40	0.9500	C682—Cl42	1.798 (7)
C41—C42	1.395 (3)	C682—H68C	0.9900
C43—C44	1.521 (4)	C682—H68D	0.9900
C43—C45	1.536 (4)
C42—O1—H1O	109.5	H44B—C44—H44C	109.5
C7—O2—H2O	109.5	C43—C45—H45A	109.4
C14—O3—H3O	109.5	C43—C45—H45B	109.5
C21—O4—H4O	109.5	H45A—C45—H45B	109.5
C28—O5—H5O	109.5	C43—C45—H45C	109.5
C35—O6—H6O	109.5	H45A—C45—H45C	109.5
C41—C1—C2	113.9 (2)	H45B—C45—H45C	109.5
C41—C1—H1A	108.8	C43—C46—H46A	109.5
C2—C1—H1A	108.8	C43—C46—H46B	109.5
C41—C1—H1B	108.8	H46A—C46—H46B	109.5
C2—C1—H1B	108.8	C43—C46—H46C	109.5
H1A—C1—H1B	107.7	H46A—C46—H46C	109.5
C7—C2—C3	118.2 (2)	H46B—C46—H46C	109.5
C7—C2—C1	121.7 (2)	C501—C47—C481	109.8 (3)
C3—C2—C1	120.1 (2)	C501—C47—C11	113.0 (2)
C4—C3—C2	122.1 (3)	C481—C47—C11	108.6 (2)
C4—C3—H3	119.0	C501—C47—C491	108.3 (3)
C2—C3—H3	119.0	C481—C47—C491	107.4 (3)
C3—C4—C5	117.2 (2)	C11—C47—C491	109.5 (2)
C3—C4—C43	123.7 (2)	C47—C481—H48A	109.4
C5—C4—C43	119.0 (2)	C47—C481—H48B	109.6
C6—C5—C4	123.0 (2)	H48A—C481—H48B	109.5
C6—C5—H5	118.5	C47—C481—H48C	109.5
C4—C5—H5	118.5	H48A—C481—H48C	109.5
C7—C6—C5	117.3 (2)	H48B—C481—H48C	109.5
C7—C6—C8	122.7 (2)	C47—C491—H49A	109.3
C5—C6—C8	119.9 (2)	C47—C491—H49B	109.7
C6—C7—O2	120.0 (2)	H49A—C491—H49B	109.5
C6—C7—C2	122.1 (2)	C47—C491—H49C	109.5
O2—C7—C2	117.7 (2)	H49A—C491—H49C	109.5
C9—C8—C6	114.3 (2)	H49B—C491—H49C	109.5
C9—C8—H8A	108.7	C47—C501—H50A	109.6
C6—C8—H8A	108.7	C47—C501—H50B	109.4
C9—C8—H8B	108.7	H50A—C501—H50B	109.5
C6—C8—H8B	108.7	C47—C501—H50C	109.4
H8A—C8—H8B	107.6	H50A—C501—H50C	109.5
C10—C9—C14	118.0 (2)	H50B—C501—H50C	109.5
C10—C9—C8	120.0 (2)	H48D—C482—H48E	109.5
C14—C9—C8	122.1 (2)	H48D—C482—H48F	109.5
C11—C10—C9	122.9 (2)	H48E—C482—H48F	109.5
C11—C10—H10	118.6	H49D—C492—H49E	109.5
C9—C10—H10	118.6	H49D—C492—H49F	109.5
C10—C11—C12	116.7 (2)	H49E—C492—H49F	109.5
C10—C11—C47	120.6 (2)	H50D—C502—H50E	109.5
C12—C11—C47	122.7 (2)	H50D—C502—H50F	109.5
C13—C12—C11	123.1 (2)	H50E—C502—H50F	109.5
C13—C12—H12	118.5	C53—C51—C54	108.7 (2)
C11—C12—H12	118.5	C53—C51—C52	108.1 (2)
C12—C13—C14	117.8 (2)	C54—C51—C52	108.1 (2)
C12—C13—C15	120.7 (2)	C53—C51—C18	112.4 (2)
C14—C13—C15	121.5 (2)	C54—C51—C18	110.5 (2)
O3—C14—C13	122.0 (2)	C52—C51—C18	108.8 (2)
O3—C14—C9	116.4 (2)	C51—C52—H52A	109.5
C13—C14—C9	121.5 (2)	C51—C52—H52B	109.5
C13—C15—C16	115.3 (2)	H52A—C52—H52B	109.5
C13—C15—H15A	108.5	C51—C52—H52C	109.4
C16—C15—H15A	108.5	H52A—C52—H52C	109.5
C13—C15—H15B	108.5	H52B—C52—H52C	109.5
C16—C15—H15B	108.5	C51—C53—H53A	109.4
H15A—C15—H15B	107.5	C51—C53—H53B	109.5
C21—C16—C17	118.4 (2)	H53A—C53—H53B	109.5
C21—C16—C15	121.3 (2)	C51—C53—H53C	109.5
C17—C16—C15	120.4 (2)	H53A—C53—H53C	109.5
C18—C17—C16	122.5 (2)	H53B—C53—H53C	109.5
C18—C17—H17	118.7	C51—C54—H54A	109.5
C16—C17—H17	118.7	C51—C54—H54B	109.5
C17—C18—C19	116.6 (2)	H54A—C54—H54B	109.5
C17—C18—C51	123.0 (2)	C51—C54—H54C	109.5
C19—C18—C51	120.4 (2)	H54A—C54—H54C	109.5
C20—C19—C18	123.1 (2)	H54B—C54—H54C	109.5
C20—C19—H19	118.5	C57—C55—C58	108.2 (2)
C18—C19—H19	118.5	C57—C55—C25	109.1 (2)
C19—C20—C21	117.8 (2)	C58—C55—C25	112.2 (2)
C19—C20—C22	120.8 (2)	C57—C55—C56	109.9 (2)
C21—C20—C22	121.4 (2)	C58—C55—C56	108.1 (2)
O4—C21—C16	116.3 (2)	C25—C55—C56	109.3 (2)
O4—C21—C20	122.3 (2)	C55—C56—H56A	109.6
C16—C21—C20	121.4 (2)	C55—C56—H56B	109.4
C23—C22—C20	116.0 (2)	H56A—C56—H56B	109.5
C23—C22—H22A	108.3	C55—C56—H56C	109.4
C20—C22—H22A	108.3	H56A—C56—H56C	109.5
C23—C22—H22B	108.3	H56B—C56—H56C	109.5
C20—C22—H22B	108.3	C55—C57—H57A	109.5
H22A—C22—H22B	107.4	C55—C57—H57B	109.5
C24—C23—C28	118.1 (2)	H57A—C57—H57B	109.5
C24—C23—C22	120.8 (2)	C55—C57—H57C	109.5
C28—C23—C22	121.1 (2)	H57A—C57—H57C	109.5
C23—C24—C25	122.5 (3)	H57B—C57—H57C	109.5
C23—C24—H24	118.7	C55—C58—H58A	109.5
C25—C24—H24	118.7	C55—C58—H58B	109.4
C26—C25—C24	117.1 (2)	H58A—C58—H58B	109.5
C26—C25—C55	122.5 (2)	C55—C58—H58C	109.5
C24—C25—C55	120.4 (2)	H58A—C58—H58C	109.5
C25—C26—C27	122.6 (3)	H58B—C58—H58C	109.5
C25—C26—H26	118.7	C62—C59—C32	109.4 (2)
C27—C26—H26	118.7	C62—C59—C60	108.9 (2)
C28—C27—C26	118.4 (2)	C32—C59—C60	112.1 (2)
C28—C27—C29	123.0 (2)	C62—C59—C61	109.6 (2)
C26—C27—C29	118.5 (2)	C32—C59—C61	109.7 (2)
O5—C28—C27	121.7 (2)	C60—C59—C61	107.2 (2)
O5—C28—C23	117.1 (2)	C59—C60—H60A	109.5
C27—C28—C23	121.2 (2)	C59—C60—H60B	109.5
C30—C29—C27	112.3 (2)	H60A—C60—H60B	109.5
C30—C29—H29A	109.1	C59—C60—H60C	109.5
C27—C29—H29A	109.1	H60A—C60—H60C	109.5
C30—C29—H29B	109.1	H60B—C60—H60C	109.5
C27—C29—H29B	109.1	C59—C61—H61A	109.5
H29A—C29—H29B	107.9	C59—C61—H61B	109.5
C31—C30—C35	117.9 (2)	H61A—C61—H61B	109.5
C31—C30—C29	121.9 (2)	C59—C61—H61C	109.5
C35—C30—C29	120.1 (2)	H61A—C61—H61C	109.5
C30—C31—C32	122.8 (2)	H61B—C61—H61C	109.5
C30—C31—H31	118.6	C59—C62—H62A	109.4
C32—C31—H31	118.6	C59—C62—H62B	109.5
C31—C32—C33	116.4 (2)	H62A—C62—H62B	109.5
C31—C32—C59	124.2 (2)	C59—C62—H62C	109.5
C33—C32—C59	119.3 (2)	H62A—C62—H62C	109.5
C34—C33—C32	123.3 (2)	H62B—C62—H62C	109.5
C34—C33—H33	118.3	C64—C63—C39	112.6 (2)
C32—C33—H33	118.3	C64—C63—C65	109.6 (3)
C33—C34—C35	117.7 (2)	C39—C63—C65	109.0 (2)
C33—C34—C36	119.4 (2)	C64—C63—C66	107.6 (2)
C35—C34—C36	122.8 (2)	C39—C63—C66	108.9 (2)
O6—C35—C34	121.4 (2)	C65—C63—C66	109.2 (3)
O6—C35—C30	116.7 (2)	C63—C64—H64A	109.5
C34—C35—C30	121.8 (2)	C63—C64—H64B	109.5
C37—C36—C34	116.1 (2)	H64A—C64—H64B	109.5
C37—C36—H36A	108.3	C63—C64—H64C	109.5
C34—C36—H36A	108.3	H64A—C64—H64C	109.5
C37—C36—H36B	108.3	H64B—C64—H64C	109.5
C34—C36—H36B	108.3	C63—C65—H65A	109.5
H36A—C36—H36B	107.4	C63—C65—H65B	109.5
C42—C37—C38	117.9 (2)	H65A—C65—H65B	109.5
C42—C37—C36	121.1 (2)	C63—C65—H65C	109.5
C38—C37—C36	120.9 (2)	H65A—C65—H65C	109.5
C39—C38—C37	122.3 (2)	H65B—C65—H65C	109.5
C39—C38—H38	118.9	C63—C66—H66A	109.5
C37—C38—H38	118.9	C63—C66—H66B	109.5
C38—C39—C40	117.2 (2)	H66A—C66—H66B	109.5
C38—C39—C63	123.1 (2)	C63—C66—H66C	109.5
C40—C39—C63	119.7 (2)	H66A—C66—H66C	109.5
C41—C40—C39	122.9 (2)	H66B—C66—H66C	109.5
C41—C40—H40	118.5	Cl1—C67—Cl2	111.67 (19)
C39—C40—H40	118.5	Cl1—C67—H67A	109.3
C40—C41—C42	117.3 (2)	Cl2—C67—H67A	109.3
C40—C41—C1	120.4 (2)	Cl1—C67—H67B	109.3
C42—C41—C1	122.3 (2)	Cl2—C67—H67B	109.3
O1—C42—C37	116.2 (2)	H67A—C67—H67B	107.9
O1—C42—C41	121.3 (2)	Cl3—C681—Cl41	118.3 (6)
C37—C42—C41	122.5 (2)	Cl3—C681—H68A	107.7
C44—C43—C45	109.0 (2)	Cl41—C681—H68A	107.7
C44—C43—C4	112.1 (2)	Cl3—C681—H68B	107.7
C45—C43—C4	109.1 (2)	Cl41—C681—H68B	107.7
C44—C43—C46	107.5 (2)	H68A—C681—H68B	107.1
C45—C43—C46	110.3 (2)	Cl42—C682—Cl3	109.5 (3)
C4—C43—C46	108.8 (2)	Cl42—C682—H68C	109.8
C43—C44—H44A	109.5	Cl3—C682—H68C	109.8
C43—C44—H44B	109.4	Cl42—C682—H68D	109.8
H44A—C44—H44B	109.5	Cl3—C682—H68D	109.8
C43—C44—H44C	109.5	H68C—C682—H68D	108.2
H44A—C44—H44C	109.5
C41—C1—C2—C7	−90.2 (3)	C26—C27—C29—C30	−80.3 (3)
C41—C1—C2—C3	91.2 (3)	C27—C29—C30—C31	98.9 (3)
C7—C2—C3—C4	0.6 (4)	C27—C29—C30—C35	−78.6 (3)
C1—C2—C3—C4	179.2 (2)	C35—C30—C31—C32	1.3 (4)
C2—C3—C4—C5	1.8 (4)	C29—C30—C31—C32	−176.2 (2)
C2—C3—C4—C43	−176.6 (2)	C30—C31—C32—C33	1.2 (4)
C3—C4—C5—C6	−2.3 (4)	C30—C31—C32—C59	−179.7 (3)
C43—C4—C5—C6	176.2 (2)	C31—C32—C33—C34	−1.5 (4)
C4—C5—C6—C7	0.3 (4)	C59—C32—C33—C34	179.3 (2)
C4—C5—C6—C8	−177.7 (2)	C32—C33—C34—C35	−0.6 (4)
C5—C6—C7—O2	−173.9 (2)	C32—C33—C34—C36	175.8 (2)
C8—C6—C7—O2	4.0 (4)	C33—C34—C35—O6	179.8 (2)
C5—C6—C7—C2	2.4 (4)	C36—C34—C35—O6	3.5 (4)
C8—C6—C7—C2	−179.7 (2)	C33—C34—C35—C30	3.2 (4)
C3—C2—C7—C6	−2.8 (4)	C36—C34—C35—C30	−173.1 (2)
C1—C2—C7—C6	178.6 (2)	C31—C30—C35—O6	179.7 (2)
C3—C2—C7—O2	173.5 (2)	C29—C30—C35—O6	−2.8 (4)
C1—C2—C7—O2	−5.1 (4)	C31—C30—C35—C34	−3.6 (4)
C7—C6—C8—C9	91.0 (3)	C29—C30—C35—C34	174.0 (2)
C5—C6—C8—C9	−91.1 (3)	C33—C34—C36—C37	97.4 (3)
C6—C8—C9—C10	96.6 (3)	C35—C34—C36—C37	−86.4 (3)
C6—C8—C9—C14	−83.9 (3)	C34—C36—C37—C42	92.2 (3)
C14—C9—C10—C11	−0.3 (4)	C34—C36—C37—C38	−90.7 (3)
C8—C9—C10—C11	179.2 (2)	C42—C37—C38—C39	0.9 (4)
C9—C10—C11—C12	1.8 (4)	C36—C37—C38—C39	−176.3 (2)
C9—C10—C11—C47	−179.0 (2)	C37—C38—C39—C40	−0.5 (4)
C10—C11—C12—C13	−1.6 (4)	C37—C38—C39—C63	178.7 (2)
C47—C11—C12—C13	179.2 (3)	C38—C39—C40—C41	0.4 (4)
C11—C12—C13—C14	−0.1 (4)	C63—C39—C40—C41	−178.8 (2)
C11—C12—C13—C15	178.2 (2)	C39—C40—C41—C42	−0.7 (4)
C12—C13—C14—O3	−177.7 (2)	C39—C40—C41—C1	177.7 (2)
C15—C13—C14—O3	4.0 (4)	C2—C1—C41—C40	−101.2 (3)
C12—C13—C14—C9	1.7 (4)	C2—C1—C41—C42	77.2 (3)
C15—C13—C14—C9	−176.6 (2)	C38—C37—C42—O1	178.1 (2)
C10—C9—C14—O3	177.9 (2)	C36—C37—C42—O1	−4.7 (3)
C8—C9—C14—O3	−1.6 (4)	C38—C37—C42—C41	−1.3 (4)
C10—C9—C14—C13	−1.5 (4)	C36—C37—C42—C41	175.9 (2)
C8—C9—C14—C13	179.0 (2)	C40—C41—C42—O1	−178.1 (2)
C12—C13—C15—C16	101.8 (3)	C1—C41—C42—O1	3.5 (4)
C14—C13—C15—C16	−80.0 (3)	C40—C41—C42—C37	1.2 (4)
C13—C15—C16—C21	101.0 (3)	C1—C41—C42—C37	−177.2 (2)
C13—C15—C16—C17	−79.4 (3)	C3—C4—C43—C44	−4.1 (4)
C21—C16—C17—C18	1.6 (4)	C5—C4—C43—C44	177.5 (2)
C15—C16—C17—C18	−178.0 (2)	C3—C4—C43—C45	116.8 (3)
C16—C17—C18—C19	2.9 (4)	C5—C4—C43—C45	−61.6 (3)
C16—C17—C18—C51	−175.6 (2)	C3—C4—C43—C46	−122.9 (3)
C17—C18—C19—C20	−3.6 (4)	C5—C4—C43—C46	58.8 (3)
C51—C18—C19—C20	175.0 (2)	C10—C11—C47—C501	171.7 (3)
C18—C19—C20—C21	−0.4 (4)	C12—C11—C47—C501	−9.1 (4)
C18—C19—C20—C22	−178.0 (2)	C10—C11—C47—C481	−66.2 (4)
C17—C16—C21—O4	174.3 (2)	C12—C11—C47—C481	113.0 (3)
C15—C16—C21—O4	−6.1 (4)	C10—C11—C47—C491	50.8 (4)
C17—C16—C21—C20	−5.9 (4)	C12—C11—C47—C491	−130.0 (3)
C15—C16—C21—C20	173.7 (2)	C17—C18—C51—C53	−2.6 (4)
C19—C20—C21—O4	−174.9 (2)	C19—C18—C51—C53	178.9 (2)
C22—C20—C21—O4	2.7 (4)	C17—C18—C51—C54	−124.3 (3)
C19—C20—C21—C16	5.3 (4)	C19—C18—C51—C54	57.3 (3)
C22—C20—C21—C16	−177.1 (2)	C17—C18—C51—C52	117.1 (3)
C19—C20—C22—C23	−116.5 (3)	C19—C18—C51—C52	−61.3 (3)
C21—C20—C22—C23	66.0 (3)	C26—C25—C55—C57	−114.3 (3)
C20—C22—C23—C24	80.6 (3)	C24—C25—C55—C57	65.3 (3)
C20—C22—C23—C28	−100.3 (3)	C26—C25—C55—C58	5.6 (4)
C28—C23—C24—C25	0.1 (4)	C24—C25—C55—C58	−174.8 (2)
C22—C23—C24—C25	179.2 (2)	C26—C25—C55—C56	125.5 (3)
C23—C24—C25—C26	−0.5 (4)	C24—C25—C55—C56	−55.0 (3)
C23—C24—C25—C55	179.9 (2)	C31—C32—C59—C62	122.4 (3)
C24—C25—C26—C27	1.0 (4)	C33—C32—C59—C62	−58.6 (3)
C55—C25—C26—C27	−179.4 (2)	C31—C32—C59—C60	1.5 (4)
C25—C26—C27—C28	−1.0 (4)	C33—C32—C59—C60	−179.4 (2)
C25—C26—C27—C29	176.9 (2)	C31—C32—C59—C61	−117.4 (3)
C26—C27—C28—O5	179.7 (2)	C33—C32—C59—C61	61.7 (3)
C29—C27—C28—O5	1.8 (4)	C38—C39—C63—C64	−2.4 (4)
C26—C27—C28—C23	0.6 (4)	C40—C39—C63—C64	176.8 (2)
C29—C27—C28—C23	−177.3 (2)	C38—C39—C63—C65	119.4 (3)
C24—C23—C28—O5	−179.3 (2)	C40—C39—C63—C65	−61.4 (3)
C22—C23—C28—O5	1.7 (3)	C38—C39—C63—C66	−121.5 (3)
C24—C23—C28—C27	−0.2 (4)	C40—C39—C63—C66	57.6 (3)
C22—C23—C28—C27	−179.2 (2)	C682—Cl3—C681—Cl41	83.5 (13)
C28—C27—C29—C30	97.6 (3)	C681—Cl3—C682—Cl42	−37.3 (10)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6O···O1	0.84	1.76	2.585 (2)	167
O5—H5O···O6	0.84	1.87	2.638 (3)	151
O4—H4O···O5	0.84	1.86	2.681 (2)	164
O3—H3O···O4	0.84	1.85	2.666 (2)	163
O2—H2O···O3	0.84	1.81	2.621 (3)	161
O1—H1O···O2	0.84	1.74	2.561 (3)	167
C67—H67B···C26^i	0.99	2.62	3.606 (4)	179
C29—H29A···C42^ii	0.99	2.73	3.664 (3)	158

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+2, −y+1, −z+1.