A reexamination of the low-temperature crystal structure of the p-tert-butylcalix[4]arene–toluene inclusion compound. Differences in spatial averaging with Cu and Mo Kα radiation

The low-temperature crystal structure of the p-tert-butyl­calix[4]arene–toluene inclusion compound, C₄₄H₅₆O₄·C₇H₈, exhibits significant guest-induced distortion of the host calixarene molecule. This distortion persists long enough to establish a correlation in the orientation of guests in adjacent host molecules. Remarkably, the space group and unit cell that best describe the structure appear to depend on the wavelength of the incident radiation. This behaviour appears to arise from spatial averaging over the different scattering volumes required to establish the diffraction peaks.

Computing details

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

Figures

(newcell)

Crystal data

C51H64O4	F(000) = 1608
Mr = 741.02	Dx = 1.117 Mg m^−3
Monoclinic, P2/c	Mo Kα radiation, λ = 0.71073 Å
a = 17.8141 (18) Å	Cell parameters from all reflections reflections
b = 13.890 (3) Å	θ = 1.5–28.7°
c = 17.8060 (17) Å	µ = 0.07 mm^−1
β = 89.91 (3)°	T = 173 K
V = 4405.9 (15) Å^3	, colorless
Z = 4	0.30 × 0.26 × 0.18 mm

Data collection

Bruker SMART CCD diffractometer	11537 independent reflections
Radiation source: fine-focus sealed tube	9480 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
w scans	θmax = 28.7°, θmin = 1.5°
Absorption correction: empirical (using intensity measurements) (SADABS; bruker,1997) ?	h = −24→23
Tmin = ?, Tmax = ?	k = −18→18
51325 measured reflections	l = −23→24

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)] = 0.051	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.137	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ^2(Fo^2) + (0.056P)^2 + 1.4935P] where P = (Fo^2 + 2Fc^2)/3
11537 reflections	(Δ/σ)max = 0.008
493 parameters	Δρmax = 0.31 e Å^−3
0 restraints	Δρmin = −0.26 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)
O21	0.10052 (4)	−0.05186 (5)	0.21650 (4)	0.03033 (19)
H21A	0.0830	−0.0520	0.2591	0.036*	0.50
H21B	0.0612	−0.0591	0.1909	0.036*	0.50
O1	0.03383 (4)	−0.05566 (5)	0.35386 (4)	0.03050 (19)
H01A	−0.0100	−0.0608	0.3404	0.037*	0.50
H01B	0.0499	−0.0498	0.3037	0.037*	0.50
O61	0.39649 (4)	1.03950 (5)	0.28367 (4)	0.02487 (17)
H61A	0.4179	1.0389	0.2429	0.030*	0.50
H61B	0.4362	1.0535	0.3151	0.030*	0.50
O41	0.468004 (9)	1.036243 (12)	0.150155 (9)	0.02460 (17)
H41A	0.5120	1.0388	0.1634	0.030*	0.50
H41B	0.4472	1.0411	0.1941	0.030*	0.50
C66	0.321408 (10)	0.909306 (13)	0.234150 (10)	0.0208 (2)
C25	0.226042 (12)	0.152584 (12)	0.251338 (9)	0.0245 (2)
C65	0.285143 (11)	0.821346 (13)	0.247556 (10)	0.0221 (2)
C63	0.323436 (12)	0.823548 (12)	0.376313 (9)	0.0242 (2)
C61	0.359727 (11)	0.952647 (12)	0.294445 (10)	0.0194 (2)
C48	0.321546 (9)	0.951915 (13)	0.155733 (12)	0.0209 (2)
C41	0.456691 (9)	0.953684 (12)	0.107445 (9)	0.0202 (2)
C62	0.360854 (12)	0.910155 (12)	0.365532 (9)	0.0207 (2)
C64	0.285370 (11)	0.776204 (12)	0.317803 (10)	0.0232 (2)
C42	0.384832 (9)	0.912995 (13)	0.106740 (12)	0.0196 (2)
C26	0.183795 (12)	0.070356 (12)	0.265479 (9)	0.0222 (2)
C23	0.186116 (12)	0.156665 (12)	0.123382 (9)	0.0238 (2)
C22	0.142886 (12)	0.073969 (12)	0.134684 (10)	0.0236 (2)
C43	0.373599 (9)	0.830853 (13)	0.062362 (12)	0.0212 (2)
C6	−0.015464 (11)	0.076819 (12)	0.427498 (10)	0.0243 (2)
C24	0.228308 (12)	0.197895 (12)	0.181087 (9)	0.0236 (2)
C21	0.142107 (12)	0.031241 (12)	0.205757 (9)	0.0224 (2)
C8	0.179625 (12)	0.028958 (12)	0.344352 (9)	0.0252 (2)
C45	0.500965 (10)	0.833356 (15)	0.021773 (13)	0.0218 (2)
C68	0.404988 (12)	0.954498 (12)	0.430657 (9)	0.0222 (2)
C3	0.125423 (12)	0.161843 (12)	0.424966 (9)	0.0266 (2)
C46	0.515357 (10)	0.913856 (15)	0.065960 (13)	0.0201 (2)
C2	0.115415 (12)	0.073718 (12)	0.388565 (9)	0.0238 (2)
C27	0.278676 (12)	0.286774 (12)	0.169660 (9)	0.0278 (2)
C1	0.043750 (12)	0.032411 (12)	0.390334 (9)	0.0252 (2)
C28	0.094974 (11)	0.034443 (12)	0.071060 (10)	0.0261 (2)
C47	0.417206 (14)	0.702467 (12)	−0.032647 (10)	0.0292 (3)
C5	−0.002755 (11)	0.164842 (12)	0.462863 (10)	0.0269 (2)
C4	0.067374 (12)	0.210234 (12)	0.462061 (9)	0.0275 (2)
C44	0.430403 (13)	0.789923 (12)	0.019079 (11)	0.0225 (2)
C67	0.245285 (11)	0.680191 (12)	0.332768 (10)	0.0304 (3)
C30	0.361193 (12)	0.253583 (12)	0.172023 (9)	0.0365 (3)
H30A	0.3710	0.2224	0.2191	0.055*
H30B	0.3936	0.3084	0.1667	0.055*
H30C	0.3704	0.2093	0.1317	0.055*
C7	0.08252 (6)	0.30768 (9)	0.49979 (7)	0.0356 (3)
C31	0.26512 (7)	0.36024 (8)	0.23360 (7)	0.0368 (3)
H31A	0.2741	0.3299	0.2812	0.055*
H31B	0.2142	0.3826	0.2317	0.055*
H31C	0.2987	0.4138	0.2276	0.055*
C51	0.42079 (8)	0.73705 (9)	−0.11471 (6)	0.0394 (3)
H51A	0.4130	0.6834	−0.1477	0.059*
H51B	0.4691	0.7649	−0.1245	0.059*
H51C	0.3825	0.7844	−0.1231	0.059*
C11	0.01055 (7)	0.35453 (11)	0.52912 (8)	0.0500 (4)
H11A	−0.0132	0.3124	0.5647	0.075*
H11B	−0.0230	0.3662	0.4880	0.075*
H11C	0.0226	0.4144	0.5532	0.075*
C71	0.21560 (9)	0.63488 (9)	0.26014 (7)	0.0478 (4)
H71A	0.1810	0.6783	0.2366	0.072*
H71B	0.1904	0.5756	0.2717	0.072*
H71C	0.2568	0.6224	0.2267	0.072*
C50	0.47849 (7)	0.62637 (8)	−0.02080 (7)	0.0379 (3)
H50A	0.4695	0.5726	−0.0535	0.057*
H50B	0.4776	0.6050	0.0305	0.057*
H50C	0.5267	0.6539	−0.0319	0.057*
C29	0.26440 (8)	0.33645 (10)	0.09456 (7)	0.0480 (4)
H29A	0.2132	0.3578	0.0925	0.072*
H29B	0.2737	0.2919	0.0544	0.072*
H29C	0.2973	0.3908	0.0896	0.072*
C49	0.34133 (8)	0.65502 (10)	−0.01842 (9)	0.0566 (4)
H49A	0.3355	0.6010	−0.0515	0.085*
H49B	0.3020	0.7008	−0.0275	0.085*
H49C	0.3388	0.6334	0.0327	0.085*
C10	0.13604 (8)	0.29153 (11)	0.56629 (7)	0.0466 (4)
H10A	0.1816	0.2623	0.5486	0.070*
H10B	0.1125	0.2499	0.6024	0.070*
H10C	0.1474	0.3522	0.5894	0.070*
C9	0.11872 (8)	0.37769 (10)	0.44324 (8)	0.0439 (3)
H9A	0.1644	0.3502	0.4242	0.066*
H9B	0.1296	0.4376	0.4678	0.066*
H9C	0.0847	0.3889	0.4024	0.066*
C70	0.30010 (8)	0.60778 (9)	0.36842 (8)	0.0408 (3)
H70A	0.3415	0.5969	0.3349	0.061*
H70B	0.2745	0.5481	0.3775	0.061*
H70C	0.3184	0.6332	0.4150	0.061*
C69	0.17951 (7)	0.69785 (10)	0.38619 (8)	0.0457 (4)
H69A	0.1455	0.7433	0.3640	0.068*
H69B	0.1980	0.7231	0.4328	0.068*
H69C	0.1537	0.6383	0.3953	0.068*
H28A	0.1214 (7)	0.0535 (9)	0.0215 (7)	0.032 (3)*
H43	0.3205 (6)	0.8034 (8)	0.0594 (6)	0.023 (3)*
H23	0.1829 (6)	0.1824 (8)	0.0755 (6)	0.019 (3)*
H48B	0.2744 (6)	0.9364 (8)	0.1341 (6)	0.019 (3)*
H45	0.5416 (6)	0.8057 (7)	−0.0092 (5)	0.013 (2)*
H28B	0.0904 (7)	−0.0348 (9)	0.0699 (7)	0.039 (4)*
H3	0.1817 (8)	0.1894 (10)	0.4273 (8)	0.045 (4)*
H8A	0.2266 (6)	0.0434 (8)	0.3691 (6)	0.020 (3)*
H8B	0.1721 (7)	−0.0423 (9)	0.3471 (7)	0.034 (3)*
H5	−0.0428 (6)	0.1934 (9)	0.4895 (6)	0.026 (3)*
H48A	0.3263 (6)	1.0208 (8)	0.1545 (6)	0.019 (3)*
H25	0.2569 (7)	0.1734 (10)	0.2939 (7)	0.038 (3)*
H63	0.3292 (6)	0.7971 (8)	0.4235 (6)	0.021 (3)*
H65	0.2603 (7)	0.7906 (9)	0.2034 (7)	0.034 (3)*
H68B	0.4078 (7)	1.0236 (9)	0.4314 (7)	0.029 (3)*
H68B	0.3754 (7)	0.9383 (9)	0.4789 (7)	0.025 (3)*
C102	0.50678 (7)	0.46499 (4)	0.25823 (6)	0.0436 (6)	0.50
H102	0.5088	0.3982	0.2614	0.052*	0.50
C107	0.54903 (7)	0.52135 (4)	0.30734 (6)	0.0464 (7)	0.50
H107	0.5793	0.4921	0.3433	0.056*	0.50
C106	0.54595 (7)	0.62152 (4)	0.30254 (6)	0.0383 (7)	0.50
H106	0.5741	0.6591	0.3353	0.046*	0.50
C105	0.50061 (7)	0.66532 (4)	0.24864 (6)	0.0253 (3)
C104	0.45836 (7)	0.60896 (4)	0.19954 (6)	0.0262 (6)	0.50
H104	0.4281	0.6382	0.1636	0.031*	0.50
C103	0.46144 (7)	0.50880 (4)	0.20433 (6)	0.0377 (7)	0.50
H103	0.4333	0.4712	0.1716	0.045*	0.50
C101	0.49722 (7)	0.77554 (4)	0.24337 (6)	0.0284 (4)	0.50
H10D	0.5293	0.8032	0.2809	0.043*	0.25
H10E	0.4466	0.7967	0.2515	0.043*	0.25
H10F	0.5137	0.7956	0.1944	0.043*	0.25
H10G	0.4637	0.7938	0.2037	0.043*	0.25
H10H	0.5465	0.8003	0.2330	0.043*	0.25
H10I	0.4794	0.8014	0.2901	0.043*	0.25
C202	0.01455 (7)	0.53028 (4)	0.22937 (6)	0.0752 (12)	0.50
H202	0.0181	0.5966	0.2233	0.090*	0.50
C203	0.06026 (7)	0.46922 (4)	0.18713 (6)	0.0688 (11)	0.50
H203	0.0943	0.4949	0.1529	0.083*	0.50
C204	0.05488 (7)	0.36971 (4)	0.19623 (6)	0.0424 (7)	0.50
H204	0.0854	0.3290	0.1681	0.051*	0.50
C205	0.00380 (7)	0.33125 (4)	0.24756 (6)	0.0339 (4)	0.50
C206	−0.04190 (7)	0.39232 (4)	0.28980 (6)	0.0484 (8)	0.50
H206	−0.0760	0.3667	0.3240	0.058*	0.50
C207	−0.03653 (7)	0.49183 (4)	0.28070 (6)	0.0731 (10)	0.50
H207	−0.0670	0.5325	0.3089	0.088*	0.50
C201	−0.00211 (7)	0.22175 (4)	0.25756 (6)	0.0432 (5)	0.50
H20A	−0.0396	0.2074	0.2947	0.065*	0.25
H20B	0.0455	0.1967	0.2736	0.065*	0.25
H20C	−0.0159	0.1927	0.2107	0.065*	0.25
H20D	0.0329	0.1905	0.2246	0.065*	0.25
H20E	−0.0521	0.2012	0.2457	0.065*	0.25
H20F	0.0092	0.2052	0.3086	0.065*	0.25

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
O21	0.0297 (4)	0.0261 (3)	0.0351 (4)	−0.0033 (3)	−0.0005 (3)	−0.0008 (3)
O1	0.0322 (4)	0.0228 (3)	0.0365 (4)	0.0010 (3)	−0.0002 (3)	0.0050 (3)
O61	0.0294 (3)	0.0184 (3)	0.0268 (3)	−0.0009 (3)	−0.0028 (3)	−0.0013 (3)
O41	0.0303 (4)	0.0191 (3)	0.0245 (3)	0.0007 (3)	−0.0032 (3)	−0.0020 (3)
C66	0.0195 (4)	0.0212 (4)	0.0217 (4)	0.0054 (4)	−0.0007 (3)	−0.0028 (4)
C25	0.0220 (4)	0.0288 (5)	0.0227 (4)	0.0021 (4)	−0.0020 (4)	−0.0023 (4)
C65	0.0209 (4)	0.0248 (4)	0.0206 (4)	0.0018 (4)	−0.0013 (3)	−0.0023 (4)
C63	0.0239 (4)	0.0276 (5)	0.0211 (4)	0.0016 (4)	−0.0026 (4)	0.0013 (4)
C61	0.0186 (4)	0.0172 (4)	0.0226 (4)	0.0036 (3)	−0.0013 (3)	−0.0034 (3)
C48	0.0198 (4)	0.0213 (4)	0.0216 (4)	0.0046 (3)	−0.0038 (3)	−0.0005 (4)
C41	0.0264 (4)	0.0168 (4)	0.0174 (4)	0.0005 (4)	−0.0047 (3)	0.0018 (3)
C62	0.0184 (4)	0.0233 (4)	0.0205 (4)	0.0026 (4)	−0.0014 (3)	−0.0043 (4)
C64	0.0231 (4)	0.0222 (4)	0.0245 (4)	−0.0006 (4)	−0.0019 (4)	−0.0002 (4)
C42	0.0224 (4)	0.0180 (4)	0.0186 (4)	0.0042 (3)	−0.0034 (3)	0.0035 (3)
C26	0.0199 (4)	0.0225 (4)	0.0243 (4)	0.0072 (4)	0.0010 (3)	0.0001 (4)
C23	0.0265 (4)	0.0250 (4)	0.0199 (4)	0.0043 (4)	−0.0009 (4)	−0.0025 (4)
C22	0.0187 (4)	0.0253 (5)	0.0268 (5)	0.0032 (4)	−0.0016 (4)	−0.0061 (4)
C43	0.0221 (4)	0.0209 (4)	0.0206 (4)	−0.0009 (4)	−0.0042 (3)	0.0017 (4)
C6	0.0210 (4)	0.0317 (5)	0.0202 (4)	0.0000 (4)	−0.0015 (4)	0.0075 (4)
C24	0.0237 (4)	0.0223 (4)	0.0248 (4)	0.0018 (4)	−0.0007 (4)	−0.0041 (4)
C21	0.0188 (4)	0.0201 (4)	0.0284 (5)	0.0028 (4)	0.0009 (4)	−0.0043 (4)
C8	0.0216 (4)	0.0286 (5)	0.0253 (5)	0.0059 (4)	−0.0021 (4)	0.0025 (4)
C45	0.0238 (4)	0.0226 (4)	0.0191 (4)	0.0048 (4)	−0.0012 (4)	0.0001 (4)
C68	0.0235 (4)	0.0216 (4)	0.0214 (4)	0.0017 (4)	−0.0037 (4)	−0.0037 (4)
C3	0.0222 (4)	0.0347 (5)	0.0228 (4)	−0.0002 (4)	−0.0027 (4)	0.0025 (4)
C46	0.0220 (4)	0.0208 (4)	0.0176 (4)	0.0001 (4)	−0.0023 (3)	0.0044 (3)
C2	0.0226 (4)	0.0276 (5)	0.0211 (4)	0.0054 (4)	−0.0026 (4)	0.0075 (4)
C27	0.0329 (5)	0.0231 (4)	0.0275 (5)	−0.0021 (4)	−0.0009 (4)	0.0004 (4)
C1	0.0263 (5)	0.0247 (4)	0.0245 (5)	0.0006 (4)	−0.0036 (4)	0.0072 (4)
C28	0.0228 (5)	0.0283 (5)	0.0271 (5)	0.0014 (4)	−0.0011 (4)	−0.0081 (4)
C47	0.0310 (5)	0.0234 (5)	0.0331 (5)	0.0015 (4)	−0.0010 (4)	−0.0084 (4)
C5	0.0235 (5)	0.0347 (5)	0.0223 (4)	0.0053 (4)	0.0004 (4)	−0.0006 (4)
C4	0.0275 (5)	0.0329 (5)	0.0220 (4)	0.0009 (4)	−0.0048 (4)	−0.0011 (4)
C44	0.0257 (4)	0.0196 (4)	0.0222 (4)	0.0019 (4)	−0.0038 (4)	−0.0012 (4)
C67	0.0338 (5)	0.0271 (5)	0.0302 (5)	−0.0098 (4)	−0.0026 (4)	0.0029 (4)
C30	0.0321 (5)	0.0290 (5)	0.0482 (6)	−0.0047 (5)	0.0088 (5)	−0.0036 (5)
C7	0.0267 (5)	0.0435 (6)	0.0365 (6)	0.0007 (5)	0.0000 (4)	−0.0105 (5)
C31	0.0399 (6)	0.0250 (5)	0.0454 (6)	−0.0004 (5)	−0.0003 (5)	−0.0079 (5)
C51	0.0537 (7)	0.0339 (6)	0.0306 (5)	0.0083 (5)	−0.0122 (5)	−0.0095 (5)
C11	0.0374 (6)	0.0513 (7)	0.0614 (8)	0.0049 (6)	0.0010 (6)	−0.0252 (6)
C71	0.0672 (8)	0.0335 (6)	0.0429 (7)	−0.0224 (6)	−0.0167 (6)	0.0047 (5)
C50	0.0513 (7)	0.0268 (5)	0.0357 (6)	0.0110 (5)	−0.0035 (5)	−0.0043 (5)
C29	0.0646 (8)	0.0392 (6)	0.0403 (6)	−0.0155 (6)	−0.0119 (6)	0.0123 (5)
C49	0.0475 (7)	0.0451 (6)	0.0773 (9)	−0.0198 (6)	0.0152 (7)	−0.0358 (6)
C10	0.0450 (7)	0.0589 (8)	0.0358 (6)	−0.0020 (6)	−0.0069 (5)	−0.0114 (6)
C9	0.0436 (7)	0.0385 (6)	0.0497 (7)	−0.0024 (6)	−0.0037 (6)	−0.0057 (6)
C70	0.0484 (7)	0.0277 (5)	0.0464 (7)	−0.0030 (5)	−0.0064 (6)	0.0070 (5)
C69	0.0379 (6)	0.0484 (7)	0.0507 (7)	−0.0098 (6)	0.0079 (6)	0.0073 (6)
C102	0.0807 (14)	0.0188 (7)	0.0313 (11)	0.0080 (18)	0.0099 (13)	0.0033 (11)
C107	0.0611 (16)	0.0445 (14)	0.0337 (12)	0.0111 (13)	0.0011 (12)	−0.0051 (11)
C106	0.0494 (14)	0.0222 (10)	0.0432 (13)	0.0021 (10)	−0.0039 (11)	0.0061 (10)
C105	0.0245 (6)	0.0242 (6)	0.0271 (6)	0.006 (3)	0.0050 (7)	0.0226 (14)
C104	0.0300 (11)	0.0241 (9)	0.0245 (11)	−0.0068 (9)	0.0009 (9)	0.0029 (9)
C103	0.0636 (16)	0.0150 (9)	0.0346 (12)	−0.0106 (11)	−0.0014 (11)	−0.0102 (9)
C101	0.0358 (8)	0.0228 (6)	0.0266 (8)	−0.0160 (15)	−0.0056 (9)	−0.0082 (10)
C202	0.086 (2)	0.0453 (13)	0.094 (3)	0.0169 (18)	−0.0415 (18)	−0.0063 (15)
C203	0.0629 (18)	0.0421 (15)	0.101 (3)	−0.0126 (15)	−0.0219 (18)	0.0215 (16)
C204	0.0284 (11)	0.0474 (14)	0.0516 (14)	0.0011 (11)	−0.0006 (11)	0.0133 (12)
C205	0.0270 (7)	0.0401 (8)	0.0346 (8)	0.0167 (18)	−0.0112 (8)	−0.010 (3)
C206	0.0291 (12)	0.0767 (19)	0.0395 (13)	0.0073 (13)	−0.0036 (11)	−0.0129 (14)
C207	0.081 (2)	0.0693 (19)	0.0693 (19)	0.0362 (17)	−0.0396 (15)	−0.0330 (16)
C201	0.0644 (11)	0.0414 (8)	0.0237 (10)	−0.021 (2)	−0.0046 (11)	−0.0033 (12)

Geometric parameters (Å, º)

O21—C21	1.3847	C3—C2	1.3966
O1—C1	1.3964	C3—C4	1.3983
O61—C61	1.3859	C46—C68^ii	1.5284
O41—C41	1.3909	C2—C1	1.4000
C66—C65	1.4023	C27—C29	1.5265 (13)
C66—C61	1.4083	C27—C30	1.5412
C66—C48	1.5165	C27—C31	1.5476 (12)
C25—C26	1.3906	C28—C6^i	1.5340
C25—C24	1.4008	C47—C49	1.5247 (14)
C65—C64	1.3992	C47—C50	1.5343 (13)
C63—C62	1.3885	C47—C51	1.5394 (12)
C63—C64	1.4071	C47—C44	1.5427
C61—C62	1.3968	C5—C4	1.3994
C48—C42	1.5235	C4—C7	1.5352 (13)
C41—C46	1.3933	C67—C69	1.5278 (14)
C41—C42	1.3994	C67—C71	1.5331 (13)
C62—C68	1.5314	C67—C70	1.5395 (13)
C64—C67	1.5359	C7—C11	1.5290 (18)
C42—C43	1.4024	C7—C10	1.5379 (18)
C26—C21	1.4072	C7—C9	1.5406 (19)
C26—C8	1.5193	C102—C103	1.3950
C23—C24	1.3968	C102—C107	1.3950
C23—C22	1.3973	C107—C106	1.3950
C22—C21	1.3978	C106—C105	1.3950
C22—C28	1.5220	C105—C104	1.3950
C43—C44	1.3924	C105—C101	1.5350
C6—C1	1.3888	C104—C103	1.3950
C6—C5	1.3940	C202—C203	1.3950
C6—C28^i	1.5340	C202—C207	1.3950
C24—C27	1.5395	C203—C204	1.3950
C8—C2	1.5205	C204—C205	1.3950
C45—C46	1.3913	C205—C206	1.3950
C45—C44	1.3952	C205—C201	1.5349
C68—C46^ii	1.5284	C206—C207	1.3950
C65—C66—C61	117.8	C29—C27—C30	108.62 (6)
C65—C66—C48	119.8	C24—C27—C30	108.2
C61—C66—C48	122.3	C29—C27—C31	108.69 (7)
C26—C25—C24	123.1	C24—C27—C31	110.0
C64—C65—C66	122.7	C30—C27—C31	109.0
C62—C63—C64	122.3	C6—C1—O1	120.9
O61—C61—C62	119.1	C6—C1—C2	121.4
O61—C61—C66	119.7	O1—C1—C2	117.7
C62—C61—C66	121.2	C22—C28—C6^i	111.6
C66—C48—C42	112.9	C49—C47—C50	108.07 (8)
O41—C41—C46	120.5	C49—C47—C51	109.15 (8)
O41—C41—C42	118.1	C50—C47—C51	108.48 (7)
C46—C41—C42	121.3	C49—C47—C44	112.16 (6)
C63—C62—C61	118.9	C50—C47—C44	110.6
C63—C62—C68	119.4	C51—C47—C44	108.4
C61—C62—C68	121.6	C6—C5—C4	122.4
C65—C64—C63	117.0	C3—C4—C5	116.6
C65—C64—C67	122.8	C3—C4—C7	120.0
C63—C64—C67	120.1	C5—C4—C7	123.4
C41—C42—C43	117.7	C43—C44—C45	117.3
C41—C42—C48	121.8	C43—C44—C47	122.7
C43—C42—C48	120.3	C45—C44—C47	119.9
C25—C26—C21	117.8	C69—C67—C71	109.02 (8)
C25—C26—C8	120.3	C69—C67—C64	108.94 (6)
C21—C26—C8	121.8	C71—C67—C64	111.8
C24—C23—C22	121.9	C69—C67—C70	109.54 (8)
C23—C22—C21	119.0	C71—C67—C70	107.43 (7)
C23—C22—C28	119.9	C64—C67—C70	110.1
C21—C22—C28	121.1	C11—C7—C4	112.15 (9)
C44—C43—C42	122.7	C11—C7—C10	108.64 (11)
C1—C6—C5	118.8	C4—C7—C10	108.54 (10)
C1—C6—C28^i	122.6	C11—C7—C9	107.73 (11)
C5—C6—C28^i	118.7	C4—C7—C9	110.13 (9)
C23—C24—C25	117.3	C10—C7—C9	109.63 (10)
C23—C24—C27	123.1	C103—C102—C107	120.0
C25—C24—C27	119.6	C102—C107—C106	120.0
O21—C21—C22	118.9	C107—C106—C105	120.0
O21—C21—C26	120.0	C104—C105—C106	120.0
C22—C21—C26	121.0	C104—C105—C101	120.0
C26—C8—C2	111.1	C106—C105—C101	120.0
C46—C45—C44	122.3	C105—C104—C103	120.0
C46^ii—C68—C62	111.0	C102—C103—C104	120.0
C2—C3—C4	123.1	C203—C202—C207	120.0
C45—C46—C41	118.7	C202—C203—C204	120.0
C45—C46—C68^ii	119.4	C203—C204—C205	120.0
C41—C46—C68^ii	121.9	C206—C205—C204	120.0
C3—C2—C1	117.8	C206—C205—C201	120.0
C3—C2—C8	120.1	C204—C205—C201	120.0
C1—C2—C8	122.0	C207—C206—C205	120.0
C29—C27—C24	112.36 (6)	C206—C207—C202	120.0

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