Thermal motion of tert-butyl groups III. tert-Butyl substituents in aromatic hydrocarbons, the view from the bottom of the well

The rigidity of the tert-butyl group (TBG) as a substituent in aromatic hydrocarbons is investigated, with a modified Hirshfeld test of anisotropic displacement parameters (ADPs) as a primary criterion. Four new structures are analyzed, along with low-temperature studies of a previously published crowded supermesityl dimer; three of the five structures meet the primary test. Most of the TBGs meet the Hirshfeld test at 100 K, and the ADPs are improved by omitting low-order data in the final refinement. The three most precise structures yield a wide variation in libration amplitudes (and in estimated rotation barriers) for 13 unique TBGs. A similar range of values is found in analyses of structures in the Cambridge Crystallographic Database. The libration amplitudes are calculated with the program THMA14C, with each TBG as an attached rigid group (ARG). Packing analysis suggests that large ADPs, especially for some individual TBG methyl groups, correspond to voids in the crystal. Published barriers to TBG reorientation, determined by solid-state NMR spin-lattice relaxation methods, for six related crystalline compounds are compared with barriers calculated from their crystal structure data.

Computing details

Data collection: Bruker SMART APEX2 for (IIIa), IIIahigh; UCLA Crystallographic Package for (IIIb), (IVa), (I), (IVb); Bruker SMART for (Va), Vahigh, (VI), (VIIa), VIIahigh, (Vb), (Vc), (Vd), (VIIb), (VIIc), (VIId). Cell refinement: Bruker SMART APEX2 for (IIIa), IIIahigh; UCLA Crystallographic Package for (IIIb), (IVa), (I), (IVb); Bruker SMART for (Va), Vahigh, (VI), (VIIa), VIIahigh, (Vb), (Vc), (Vd), (VIIb), (VIIc), (VIId). Data reduction: Bruker SAINT for (IIIa), IIIahigh, (Va), Vahigh, (VI), (VIIa), VIIahigh, (Vb), (Vc), (Vd), (VIIb), (VIIc), (VIId); UCLA Crystallographic Package for (IIIb), (IVa), (I), (IVb). For all structures, 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.

1-(2,4,6-Tri-tert-butylphenyl)-2-(3,5-di-tert-butylphenyl)- 2-methylpropane (IIIa)

Crystal data

C36H58	Z = 4
Mr = 490.82	F(000) = 1096
Triclinic, P1	Dx = 1.015 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 15.7799 (17) Å	Cell parameters from 9886 reflections
b = 19.394 (2) Å	θ = 3.8–29.1°
c = 10.5789 (11) Å	µ = 0.06 mm^−1
α = 94.982 (1)°	T = 100 K
β = 95.188 (1)°	Parallelipiped, colorless
γ = 89.963 (2)°	0.40 × 0.36 × 0.16 mm
V = 3212.1 (6) Å^3

Data collection

CCD area detector diffractometer	16793 independent reflections
Radiation source: fine-focus sealed tube	11868 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.037
phi and ω scans	θmax = 29.2°, θmin = 3.8°
Absorption correction: multi-scan Sadabs (Bruker)	h = −21→21
Tmin = 0.898, Tmax = 0.991	k = −24→26
42208 measured reflections	l = −14→14

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)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.129	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0526P)^2 + 0.967P] where P = (Fo^2 + 2Fc^2)/3
16793 reflections	(Δ/σ)max = 0.001
696 parameters	Δρmax = 0.38 e Å^−3
6 restraints	Δρmin = −0.21 e Å^−3

Special details

Experimental. Cell used is that of published room-temperature structure (Frey, J., Nugiel, D. A. and Rappoport, Z. (1991) J. Org. Chem., 56, 466–469.

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. Refinement includes a twofold disorder model for C34B—C36B (occupancy 0.08) and C34D—C36D (occupancy 0.92) (labelling based on 145 K structure in which C34D—C36D is the major conformer).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.41826 (8)	0.72769 (7)	0.13797 (11)	0.0190 (2)
C2	0.51690 (8)	0.74218 (6)	0.16795 (11)	0.0180 (2)
H2A	0.5474	0.6995	0.1414	0.022*
H2B	0.5331	0.7784	0.1140	0.022*
C3	0.54905 (8)	0.76493 (6)	0.30538 (11)	0.0170 (2)
C4	0.58154 (8)	0.71447 (6)	0.38802 (11)	0.0171 (2)
C5	0.58832 (8)	0.73172 (6)	0.51957 (11)	0.0185 (2)
H5	0.6071	0.6973	0.5741	0.022*
C6	0.56888 (8)	0.79699 (6)	0.57444 (11)	0.0184 (2)
C7	0.54962 (8)	0.84738 (7)	0.49143 (11)	0.0195 (2)
H7	0.5403	0.8932	0.5267	0.023*
C8	0.54312 (8)	0.83465 (6)	0.35803 (11)	0.0175 (2)
C9	0.38686 (8)	0.66759 (6)	0.20767 (11)	0.0178 (2)
C10	0.36577 (8)	0.60295 (7)	0.14549 (11)	0.0189 (2)
H10	0.3723	0.5951	0.0570	0.023*
C11	0.33507 (8)	0.54895 (6)	0.20927 (11)	0.0189 (2)
C12	0.32578 (8)	0.56190 (7)	0.33882 (11)	0.0196 (2)
H12	0.3055	0.5258	0.3836	0.024*
C13	0.34536 (8)	0.62637 (6)	0.40526 (11)	0.0184 (2)
C14	0.37614 (8)	0.67840 (7)	0.33823 (11)	0.0183 (2)
H14	0.3902	0.7223	0.3820	0.022*
C15	0.40536 (9)	0.71142 (7)	−0.00769 (11)	0.0248 (3)
H15A	0.4211	0.7521	−0.0496	0.032*
H15B	0.3455	0.6996	−0.0330	0.032*
H15C	0.4412	0.6723	−0.0331	0.032*
C16	0.36454 (8)	0.79143 (7)	0.17206 (13)	0.0233 (3)
H16A	0.3770	0.8283	0.1186	0.030*
H16B	0.3783	0.8076	0.2619	0.030*
H16C	0.3040	0.7791	0.1574	0.030*
C17	0.62330 (8)	0.64529 (6)	0.33888 (11)	0.0185 (2)
C18	0.69577 (8)	0.66427 (7)	0.25895 (12)	0.0238 (3)
H18A	0.7242	0.6220	0.2280	0.031*
H18B	0.7370	0.6945	0.3119	0.031*
H18C	0.6721	0.6883	0.1862	0.031*
C19	0.56369 (9)	0.59030 (7)	0.26300 (12)	0.0221 (3)
H19A	0.5956	0.5477	0.2451	0.029*
H19B	0.5411	0.6078	0.1826	0.029*
H19C	0.5165	0.5805	0.3132	0.029*
C20	0.66596 (9)	0.60712 (7)	0.44960 (12)	0.0233 (3)
H20A	0.6969	0.5669	0.4151	0.030*
H20B	0.6223	0.5916	0.5012	0.030*
H20C	0.7058	0.6385	0.5028	0.030*
C21	0.57741 (8)	0.81649 (7)	0.71929 (11)	0.0205 (3)
C22	0.59343 (10)	0.75315 (7)	0.79489 (12)	0.0260 (3)
H22A	0.6474	0.7317	0.7744	0.034*
H22B	0.5469	0.7196	0.7723	0.034*
H22C	0.5963	0.7675	0.8863	0.034*
C23	0.49609 (9)	0.85233 (7)	0.76045 (12)	0.0241 (3)
H23A	0.5043	0.8682	0.8513	0.031*
H23B	0.4483	0.8195	0.7455	0.031*
H23C	0.4839	0.8921	0.7108	0.031*
C24	0.65351 (9)	0.86676 (7)	0.75275 (12)	0.0265 (3)
H24A	0.7057	0.8441	0.7275	0.035*
H24B	0.6595	0.8797	0.8448	0.035*
H24C	0.6437	0.9083	0.7072	0.035*
C25	0.54036 (8)	0.90334 (6)	0.28915 (11)	0.0199 (3)
C26	0.46114 (9)	0.94629 (7)	0.31699 (13)	0.0248 (3)
H26A	0.4652	0.9914	0.2827	0.032*
H26B	0.4577	0.9531	0.4093	0.032*
H26C	0.4101	0.9218	0.2767	0.032*
C27	0.62056 (9)	0.94589 (7)	0.34535 (12)	0.0243 (3)
H27A	0.6224	0.9892	0.3043	0.032*
H27B	0.6717	0.9189	0.3299	0.032*
H27C	0.6181	0.9564	0.4373	0.032*
C28	0.54643 (9)	0.89827 (7)	0.14420 (12)	0.0241 (3)
H28A	0.5518	0.9448	0.1164	0.031*
H28B	0.4950	0.8758	0.1005	0.031*
H28C	0.5964	0.8710	0.1234	0.031*
C29	0.31526 (9)	0.47812 (7)	0.13593 (11)	0.0216 (3)
C30	0.26516 (12)	0.43076 (8)	0.21097 (14)	0.0404 (4)
H30A	0.2511	0.3874	0.1586	0.053*
H30B	0.2126	0.4538	0.2335	0.053*
H30C	0.2997	0.4208	0.2889	0.053*
C31	0.39910 (10)	0.44285 (8)	0.10737 (17)	0.0402 (4)
H31A	0.3871	0.3977	0.0600	0.052*
H31B	0.4332	0.4364	0.1876	0.052*
H31C	0.4307	0.4719	0.0563	0.052*
C32	0.26163 (11)	0.48637 (8)	0.01017 (13)	0.0336 (3)
H32A	0.2460	0.4406	−0.0320	0.044*
H32B	0.2946	0.5116	−0.0453	0.044*
H32C	0.2099	0.5122	0.0273	0.044*
C33	0.33533 (9)	0.63749 (7)	0.54882 (11)	0.0219 (3)
C34	0.24885 (10)	0.61032 (9)	0.57878 (13)	0.0344 (4)
H34A	0.2440	0.6176	0.6707	0.045*
H34B	0.2440	0.5608	0.5516	0.045*
H34C	0.2032	0.6352	0.5333	0.045*
C35	0.40693 (10)	0.59781 (8)	0.61941 (13)	0.0329 (3)
H35A	0.4015	0.6038	0.7113	0.043*
H35B	0.4623	0.6159	0.6019	0.043*
H35C	0.4026	0.5485	0.5900	0.043*
C36	0.34260 (10)	0.71390 (7)	0.59858 (13)	0.0303 (3)
H36A	0.3353	0.7187	0.6899	0.039*
H36B	0.2984	0.7402	0.5531	0.039*
H36C	0.3988	0.7317	0.5846	0.039*
C1B	1.09970 (8)	0.69188 (6)	0.08118 (11)	0.0175 (2)
C2B	1.00022 (8)	0.67970 (6)	0.07232 (10)	0.0168 (2)
H2B1	0.9733	0.7098	0.0095	0.020*
H2B2	0.9883	0.6312	0.0383	0.020*
C3B	0.95705 (8)	0.69298 (6)	0.19541 (11)	0.0168 (2)
C4B	0.91398 (8)	0.75670 (6)	0.22073 (11)	0.0176 (2)
C5B	0.90208 (8)	0.77931 (7)	0.34731 (11)	0.0194 (2)
H5B	0.8774	0.8234	0.3646	0.023*
C6B	0.92496 (8)	0.73987 (7)	0.44880 (11)	0.0193 (2)
C7B	0.95051 (8)	0.67272 (7)	0.41713 (11)	0.0194 (2)
H7B	0.9592	0.6427	0.4834	0.023*
C8B	0.96432 (8)	0.64635 (6)	0.29296 (11)	0.0176 (2)
C9B	1.12271 (8)	0.76922 (6)	0.10068 (11)	0.0177 (2)
C10B	1.14845 (8)	0.80569 (7)	0.00257 (11)	0.0191 (2)
H10B	1.1487	0.7826	−0.0804	0.023*
C11B	1.17386 (8)	0.87525 (7)	0.02248 (12)	0.0201 (3)
C12B	1.17146 (9)	0.90802 (7)	0.14463 (12)	0.0238 (3)
H12B	1.1880	0.9553	0.1598	0.029*
C13B	1.14556 (8)	0.87364 (7)	0.24555 (12)	0.0219 (3)
C14B	1.12134 (8)	0.80442 (7)	0.22176 (11)	0.0195 (2)
H14B	1.1034	0.7804	0.2894	0.023*
C15B	1.12832 (9)	0.65875 (7)	−0.04596 (12)	0.0215 (3)
H15D	1.0956	0.6786	−0.1172	0.028*
H15E	1.1184	0.6086	−0.0519	0.028*
H15F	1.1891	0.6680	−0.0495	0.028*
C16B	1.14895 (8)	0.65604 (7)	0.18887 (12)	0.0207 (3)
H16D	1.1436	0.6057	0.1708	0.027*
H16E	1.1255	0.6701	0.2698	0.027*
H16F	1.2091	0.6695	0.1946	0.027*
C17B	0.87035 (8)	0.79911 (7)	0.11406 (11)	0.0202 (3)
C18B	0.81715 (9)	0.74985 (7)	0.01465 (12)	0.0240 (3)
H18D	0.7870	0.7769	−0.0492	0.031*
H18E	0.7758	0.7247	0.0574	0.031*
H18F	0.8549	0.7168	−0.0272	0.031*
C19B	0.93121 (9)	0.84324 (7)	0.04762 (13)	0.0250 (3)
H19D	0.9657	0.8732	0.1118	0.033*
H19E	0.8980	0.8718	−0.0106	0.033*
H19F	0.9686	0.8128	−0.0006	0.033*
C20B	0.80480 (10)	0.84981 (8)	0.16889 (13)	0.0284 (3)
H20D	0.8346	0.8862	0.2261	0.037*
H20E	0.7662	0.8247	0.2164	0.037*
H20F	0.7720	0.8707	0.0990	0.037*
C21B	0.91504 (9)	0.76501 (7)	0.58867 (11)	0.0232 (3)
C22B	0.89521 (11)	0.84234 (8)	0.60649 (13)	0.0324 (3)
H22D	0.8402	0.8513	0.5602	0.042*
H22E	0.9399	0.8688	0.5734	0.042*
H22F	0.8928	0.8564	0.6973	0.042*
C23B	0.99743 (10)	0.75133 (9)	0.67099 (13)	0.0331 (3)
H23D	1.0092	0.7016	0.6645	0.043*
H23E	0.9910	0.7675	0.7600	0.043*
H23F	1.0447	0.7762	0.6410	0.043*
C24B	0.84147 (10)	0.72523 (8)	0.63549 (13)	0.0333 (3)
H24D	0.8532	0.6755	0.6269	0.043*
H24E	0.7884	0.7345	0.5843	0.043*
H24F	0.8358	0.7403	0.7252	0.043*
C25B	0.97552 (8)	0.56601 (6)	0.27976 (11)	0.0190 (2)
C26B	1.05053 (8)	0.54240 (7)	0.36944 (12)	0.0224 (3)
H26D	1.1041	0.5592	0.3428	0.029*
H26E	1.0511	0.4917	0.3655	0.029*
H26F	1.0439	0.5613	0.4569	0.029*
C27B	0.89230 (8)	0.53512 (7)	0.31956 (12)	0.0230 (3)
H27D	0.8440	0.5481	0.2617	0.030*
H27E	0.8837	0.5531	0.4069	0.030*
H27F	0.8965	0.4846	0.3152	0.030*
C28B	0.98489 (9)	0.53036 (7)	0.14653 (12)	0.0218 (3)
H28D	0.9367	0.5426	0.0879	0.028*
H28E	0.9860	0.4801	0.1506	0.028*
H28F	1.0380	0.5456	0.1161	0.028*
C29B	1.20151 (9)	0.91438 (7)	−0.08708 (12)	0.0249 (3)
C30B	1.26462 (12)	0.97284 (9)	−0.03817 (15)	0.0429 (4)
H30D	1.2835	0.9951	−0.1106	0.056*
H30E	1.3139	0.9537	0.0097	0.056*
H30F	1.2368	1.0071	0.0176	0.056*
C31B	1.12195 (11)	0.94577 (8)	−0.15394 (14)	0.0346 (3)
H31D	1.1385	0.9717	−0.2234	0.045*
H31E	1.0944	0.9770	−0.0925	0.045*
H31F	1.0822	0.9086	−0.1886	0.045*
C32B	1.24435 (12)	0.86608 (8)	−0.18458 (15)	0.0388 (4)
H32D	1.2656	0.8933	−0.2491	0.050*
H32E	1.2029	0.8318	−0.2258	0.050*
H32F	1.2919	0.8424	−0.1411	0.050*
C33B	1.14294 (10)	0.91305 (8)	0.37742 (13)	0.0308 (3)
C34D	1.22675 (15)	0.94963 (15)	0.41955 (19)	0.0626 (9)	0.920 (3)
H34J	1.2369	0.9844	0.3607	0.081*	0.920 (3)
H34K	1.2729	0.9158	0.4196	0.081*	0.920 (3)
H34L	1.2247	0.9723	0.5057	0.081*	0.920 (3)
C35D	1.07072 (16)	0.96700 (11)	0.3675 (2)	0.0561 (6)	0.920 (3)
H35J	1.0815	0.9981	0.3024	0.073*	0.920 (3)
H35K	1.0688	0.9940	0.4499	0.073*	0.920 (3)
H35L	1.0161	0.9431	0.3440	0.073*	0.920 (3)
C36D	1.12201 (12)	0.86567 (9)	0.47829 (14)	0.0377 (5)	0.920 (3)
H36J	1.1660	0.8302	0.4862	0.049*	0.920 (3)
H36K	1.0666	0.8433	0.4531	0.049*	0.920 (3)
H36L	1.1200	0.8930	0.5603	0.049*	0.920 (3)
C34B	1.2045 (11)	0.8692 (10)	0.4693 (18)	0.037 (5)*	0.080 (3)
H34D	1.2613	0.8905	0.4813	0.048*	0.080 (3)
H34E	1.2085	0.8217	0.4306	0.048*	0.080 (3)
H34F	1.1813	0.8686	0.5521	0.048*	0.080 (3)
C35B	1.0574 (12)	0.9208 (11)	0.424 (2)	0.050 (6)*	0.080 (3)
H35D	1.0273	0.9586	0.3844	0.065*	0.080 (3)
H35E	1.0634	0.9312	0.5171	0.065*	0.080 (3)
H35F	1.0251	0.8776	0.4027	0.065*	0.080 (3)
C36B	1.1904 (15)	0.9856 (11)	0.381 (3)	0.071 (9)*	0.080 (3)
H36D	1.2031	1.0043	0.4701	0.093*	0.080 (3)
H36E	1.1538	1.0179	0.3357	0.093*	0.080 (3)
H36F	1.2436	0.9794	0.3407	0.093*	0.080 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0185 (6)	0.0216 (6)	0.0167 (5)	−0.0042 (5)	0.0012 (4)	0.0023 (4)
C2	0.0188 (6)	0.0181 (6)	0.0173 (5)	−0.0034 (5)	0.0041 (4)	0.0009 (4)
C3	0.0153 (6)	0.0188 (6)	0.0174 (5)	−0.0036 (5)	0.0053 (4)	−0.0001 (4)
C4	0.0155 (6)	0.0171 (6)	0.0187 (5)	−0.0031 (5)	0.0041 (4)	−0.0003 (4)
C5	0.0178 (6)	0.0184 (6)	0.0193 (5)	−0.0028 (5)	0.0019 (4)	0.0017 (4)
C6	0.0180 (6)	0.0190 (6)	0.0183 (5)	−0.0038 (5)	0.0041 (4)	−0.0006 (4)
C7	0.0207 (6)	0.0182 (6)	0.0198 (6)	−0.0026 (5)	0.0056 (5)	−0.0016 (4)
C8	0.0166 (6)	0.0173 (6)	0.0191 (5)	−0.0023 (5)	0.0042 (4)	0.0012 (4)
C9	0.0158 (6)	0.0195 (6)	0.0182 (5)	−0.0017 (5)	0.0019 (4)	0.0024 (4)
C10	0.0176 (6)	0.0221 (6)	0.0167 (5)	−0.0011 (5)	0.0020 (4)	−0.0007 (4)
C11	0.0177 (6)	0.0182 (6)	0.0203 (6)	−0.0014 (5)	0.0006 (4)	−0.0008 (4)
C12	0.0197 (6)	0.0194 (6)	0.0199 (6)	−0.0032 (5)	0.0021 (4)	0.0019 (4)
C13	0.0176 (6)	0.0205 (6)	0.0168 (5)	−0.0026 (5)	0.0019 (4)	0.0008 (4)
C14	0.0170 (6)	0.0192 (6)	0.0183 (5)	−0.0032 (5)	0.0017 (4)	−0.0005 (4)
C15	0.0261 (7)	0.0301 (7)	0.0184 (6)	−0.0090 (6)	−0.0003 (5)	0.0049 (5)
C16	0.0196 (6)	0.0227 (7)	0.0285 (6)	−0.0021 (5)	0.0025 (5)	0.0065 (5)
C17	0.0181 (6)	0.0175 (6)	0.0196 (5)	−0.0008 (5)	0.0019 (4)	−0.0006 (4)
C18	0.0196 (6)	0.0254 (7)	0.0267 (6)	0.0006 (5)	0.0059 (5)	−0.0003 (5)
C19	0.0226 (7)	0.0185 (6)	0.0245 (6)	−0.0015 (5)	0.0020 (5)	−0.0024 (5)
C20	0.0249 (7)	0.0191 (6)	0.0251 (6)	0.0024 (5)	0.0000 (5)	0.0001 (5)
C21	0.0234 (7)	0.0216 (6)	0.0164 (5)	−0.0029 (5)	0.0031 (5)	−0.0008 (4)
C22	0.0339 (8)	0.0268 (7)	0.0173 (6)	0.0002 (6)	0.0029 (5)	0.0008 (5)
C23	0.0272 (7)	0.0247 (7)	0.0208 (6)	−0.0030 (6)	0.0067 (5)	−0.0014 (5)
C24	0.0261 (7)	0.0293 (7)	0.0233 (6)	−0.0071 (6)	0.0019 (5)	−0.0027 (5)
C25	0.0228 (7)	0.0174 (6)	0.0201 (6)	−0.0035 (5)	0.0046 (5)	0.0017 (4)
C26	0.0270 (7)	0.0196 (7)	0.0284 (6)	0.0005 (5)	0.0055 (5)	0.0026 (5)
C27	0.0260 (7)	0.0212 (7)	0.0259 (6)	−0.0061 (5)	0.0047 (5)	0.0004 (5)
C28	0.0306 (7)	0.0219 (7)	0.0207 (6)	−0.0060 (6)	0.0053 (5)	0.0037 (5)
C29	0.0248 (7)	0.0188 (6)	0.0204 (6)	−0.0021 (5)	0.0003 (5)	−0.0011 (4)
C30	0.0621 (11)	0.0283 (8)	0.0302 (7)	−0.0225 (8)	0.0083 (7)	−0.0060 (6)
C31	0.0333 (9)	0.0270 (8)	0.0565 (10)	0.0040 (7)	−0.0026 (7)	−0.0121 (7)
C32	0.0452 (9)	0.0235 (7)	0.0283 (7)	−0.0013 (7)	−0.0108 (6)	−0.0039 (5)
C33	0.0264 (7)	0.0227 (7)	0.0166 (5)	−0.0073 (5)	0.0037 (5)	−0.0006 (4)
C34	0.0356 (8)	0.0428 (9)	0.0249 (7)	−0.0177 (7)	0.0121 (6)	−0.0070 (6)
C35	0.0415 (9)	0.0354 (8)	0.0211 (6)	−0.0028 (7)	−0.0012 (6)	0.0028 (5)
C36	0.0416 (9)	0.0274 (7)	0.0222 (6)	−0.0081 (6)	0.0100 (6)	−0.0043 (5)
C1B	0.0174 (6)	0.0169 (6)	0.0183 (5)	−0.0021 (5)	0.0044 (4)	0.0000 (4)
C2B	0.0180 (6)	0.0172 (6)	0.0152 (5)	−0.0022 (5)	0.0025 (4)	0.0001 (4)
C3B	0.0153 (6)	0.0188 (6)	0.0160 (5)	−0.0036 (5)	0.0020 (4)	0.0003 (4)
C4B	0.0169 (6)	0.0184 (6)	0.0177 (5)	−0.0036 (5)	0.0024 (4)	0.0022 (4)
C5B	0.0189 (6)	0.0184 (6)	0.0209 (6)	−0.0015 (5)	0.0043 (5)	−0.0006 (4)
C6B	0.0196 (6)	0.0223 (6)	0.0159 (5)	−0.0039 (5)	0.0040 (4)	−0.0009 (4)
C7B	0.0215 (6)	0.0207 (6)	0.0165 (5)	−0.0027 (5)	0.0024 (4)	0.0029 (4)
C8B	0.0159 (6)	0.0190 (6)	0.0179 (5)	−0.0031 (5)	0.0015 (4)	0.0011 (4)
C9B	0.0152 (6)	0.0182 (6)	0.0199 (5)	−0.0018 (5)	0.0030 (4)	0.0007 (4)
C10B	0.0184 (6)	0.0202 (6)	0.0189 (5)	−0.0020 (5)	0.0030 (4)	0.0006 (4)
C11B	0.0183 (6)	0.0194 (6)	0.0231 (6)	−0.0014 (5)	0.0034 (5)	0.0038 (5)
C12B	0.0258 (7)	0.0170 (6)	0.0287 (6)	−0.0046 (5)	0.0070 (5)	−0.0013 (5)
C13B	0.0212 (7)	0.0212 (7)	0.0232 (6)	−0.0027 (5)	0.0060 (5)	−0.0034 (5)
C14B	0.0186 (6)	0.0208 (6)	0.0195 (5)	−0.0030 (5)	0.0044 (4)	0.0007 (4)
C15B	0.0223 (7)	0.0203 (6)	0.0220 (6)	−0.0027 (5)	0.0073 (5)	−0.0024 (5)
C16B	0.0186 (6)	0.0195 (6)	0.0244 (6)	−0.0021 (5)	0.0022 (5)	0.0030 (5)
C17B	0.0197 (6)	0.0216 (6)	0.0202 (6)	0.0013 (5)	0.0039 (5)	0.0042 (4)
C18B	0.0196 (7)	0.0305 (7)	0.0222 (6)	−0.0018 (6)	0.0011 (5)	0.0045 (5)
C19B	0.0251 (7)	0.0241 (7)	0.0274 (6)	−0.0002 (6)	0.0038 (5)	0.0094 (5)
C20B	0.0301 (8)	0.0286 (8)	0.0278 (7)	0.0086 (6)	0.0062 (6)	0.0054 (5)
C21B	0.0270 (7)	0.0259 (7)	0.0165 (5)	−0.0043 (6)	0.0048 (5)	−0.0027 (5)
C22B	0.0433 (9)	0.0288 (8)	0.0246 (7)	−0.0005 (7)	0.0102 (6)	−0.0068 (5)
C23B	0.0358 (8)	0.0418 (9)	0.0201 (6)	−0.0017 (7)	−0.0005 (6)	−0.0039 (6)
C24B	0.0381 (9)	0.0383 (9)	0.0241 (7)	−0.0097 (7)	0.0133 (6)	−0.0049 (6)
C25B	0.0201 (6)	0.0182 (6)	0.0188 (5)	−0.0034 (5)	0.0022 (4)	0.0018 (4)
C26B	0.0233 (7)	0.0208 (7)	0.0234 (6)	−0.0003 (5)	0.0023 (5)	0.0043 (5)
C27B	0.0225 (7)	0.0217 (7)	0.0254 (6)	−0.0037 (5)	0.0034 (5)	0.0042 (5)
C28B	0.0248 (7)	0.0181 (6)	0.0224 (6)	−0.0036 (5)	0.0038 (5)	−0.0006 (4)
C29B	0.0302 (7)	0.0212 (7)	0.0247 (6)	−0.0042 (6)	0.0055 (5)	0.0056 (5)
C30B	0.0517 (11)	0.0435 (10)	0.0347 (8)	−0.0259 (8)	0.0007 (7)	0.0130 (7)
C31B	0.0420 (9)	0.0336 (8)	0.0291 (7)	0.0026 (7)	0.0027 (6)	0.0097 (6)
C32B	0.0501 (10)	0.0334 (9)	0.0382 (8)	0.0033 (7)	0.0250 (7)	0.0119 (6)
C33B	0.0382 (9)	0.0271 (8)	0.0269 (7)	−0.0117 (6)	0.0125 (6)	−0.0095 (5)
C34D	0.0600 (14)	0.0876 (19)	0.0367 (10)	−0.0545 (14)	0.0197 (10)	−0.0307 (11)
C35D	0.0799 (17)	0.0412 (12)	0.0491 (12)	0.0151 (11)	0.0289 (11)	−0.0084 (9)
C36D	0.0483 (11)	0.0423 (10)	0.0218 (7)	−0.0155 (8)	0.0089 (7)	−0.0085 (6)

Geometric parameters (Å, º)

C1—C16	1.5340 (19)	C2B—H2B2	0.9900
C1—C9	1.5376 (17)	C3B—C4B	1.4268 (18)
C1—C15	1.5409 (16)	C3B—C8B	1.4271 (16)
C1—C2	1.5806 (17)	C4B—C5B	1.4014 (16)
C2—C3	1.5235 (16)	C4B—C17B	1.5632 (17)
C2—H2A	0.9900	C5B—C6B	1.3928 (17)
C2—H2B	0.9900	C5B—H5B	0.9500
C3—C8	1.4233 (17)	C6B—C7B	1.3852 (18)
C3—C4	1.4324 (17)	C6B—C21B	1.5389 (16)
C4—C5	1.3972 (16)	C7B—C8B	1.4034 (16)
C4—C17	1.5633 (17)	C7B—H7B	0.9500
C5—C6	1.3920 (17)	C8B—C25B	1.5636 (18)
C5—H5	0.9500	C9B—C10B	1.3953 (16)
C6—C7	1.3854 (17)	C9B—C14B	1.4001 (16)
C6—C21	1.5399 (16)	C10B—C11B	1.4004 (17)
C7—C8	1.4059 (16)	C10B—H10B	0.9500
C7—H7	0.9500	C11B—C12B	1.3933 (17)
C8—C25	1.5718 (17)	C11B—C29B	1.5343 (17)
C9—C10	1.3902 (17)	C12B—C13B	1.3981 (18)
C9—C14	1.4044 (16)	C12B—H12B	0.9500
C10—C11	1.4034 (17)	C13B—C14B	1.3915 (18)
C10—H10	0.9500	C13B—C33B	1.5352 (17)
C11—C12	1.3927 (16)	C14B—H14B	0.9500
C11—C29	1.5355 (17)	C15B—H15D	0.9800
C12—C13	1.4005 (17)	C15B—H15E	0.9800
C12—H12	0.9500	C15B—H15F	0.9800
C13—C14	1.3943 (17)	C16B—H16D	0.9800
C13—C33	1.5377 (16)	C16B—H16E	0.9800
C14—H14	0.9500	C16B—H16F	0.9800
C15—H15A	0.9800	C17B—C19B	1.5417 (18)
C15—H15B	0.9800	C17B—C20B	1.5431 (19)
C15—H15C	0.9800	C17B—C18B	1.5460 (18)
C16—H16A	0.9800	C18B—H18D	0.9800
C16—H16B	0.9800	C18B—H18E	0.9800
C16—H16C	0.9800	C18B—H18F	0.9800
C17—C20	1.5429 (17)	C19B—H19D	0.9800
C17—C19	1.5436 (17)	C19B—H19E	0.9800
C17—C18	1.5453 (18)	C19B—H19F	0.9800
C18—H18A	0.9800	C20B—H20D	0.9800
C18—H18B	0.9800	C20B—H20E	0.9800
C18—H18C	0.9800	C20B—H20F	0.9800
C19—H19A	0.9800	C21B—C22B	1.531 (2)
C19—H19B	0.9800	C21B—C23B	1.534 (2)
C19—H19C	0.9800	C21B—C24B	1.5361 (19)
C20—H20A	0.9800	C22B—H22D	0.9800
C20—H20B	0.9800	C22B—H22E	0.9800
C20—H20C	0.9800	C22B—H22F	0.9800
C21—C22	1.5319 (18)	C23B—H23D	0.9800
C21—C23	1.5385 (19)	C23B—H23E	0.9800
C21—C24	1.5434 (18)	C23B—H23F	0.9800
C22—H22A	0.9800	C24B—H24D	0.9800
C22—H22B	0.9800	C24B—H24E	0.9800
C22—H22C	0.9800	C24B—H24F	0.9800
C23—H23A	0.9800	C25B—C28B	1.5345 (17)
C23—H23B	0.9800	C25B—C26B	1.5435 (18)
C23—H23C	0.9800	C25B—C27B	1.5510 (17)
C24—H24A	0.9800	C26B—H26D	0.9800
C24—H24B	0.9800	C26B—H26E	0.9800
C24—H24C	0.9800	C26B—H26F	0.9800
C25—C26	1.5381 (19)	C27B—H27D	0.9800
C25—C28	1.5396 (17)	C27B—H27E	0.9800
C25—C27	1.5544 (18)	C27B—H27F	0.9800
C26—H26A	0.9800	C28B—H28D	0.9800
C26—H26B	0.9800	C28B—H28E	0.9800
C26—H26C	0.9800	C28B—H28F	0.9800
C27—H27A	0.9800	C29B—C30B	1.533 (2)
C27—H27B	0.9800	C29B—C32B	1.535 (2)
C27—H27C	0.9800	C29B—C31B	1.536 (2)
C28—H28A	0.9800	C30B—H30D	0.9800
C28—H28B	0.9800	C30B—H30E	0.9800
C28—H28C	0.9800	C30B—H30F	0.9800
C29—C30	1.5298 (19)	C31B—H31D	0.9800
C29—C32	1.5313 (18)	C31B—H31E	0.9800
C29—C31	1.531 (2)	C31B—H31F	0.9800
C30—H30A	0.9800	C32B—H32D	0.9800
C30—H30B	0.9800	C32B—H32E	0.9800
C30—H30C	0.9800	C32B—H32F	0.9800
C31—H31A	0.9800	C33B—C35B	1.483
C31—H31B	0.9800	C33B—C34D	1.514 (2)
C31—H31C	0.9800	C33B—C36D	1.525 (2)
C32—H32A	0.9800	C33B—C35D	1.549 (3)
C32—H32B	0.9800	C33B—C36B	1.591
C32—H32C	0.9800	C33B—C34B	1.608
C33—C36	1.5297 (19)	C34D—H34J	0.9800
C33—C34	1.5326 (19)	C34D—H34K	0.9800
C33—C35	1.540 (2)	C34D—H34L	0.9800
C34—H34A	0.9800	C35D—H35J	0.9800
C34—H34B	0.9800	C35D—H35K	0.9800
C34—H34C	0.9800	C35D—H35L	0.9800
C35—H35A	0.9800	C36D—H36J	0.9800
C35—H35B	0.9800	C36D—H36K	0.9800
C35—H35C	0.9800	C36D—H36L	0.9800
C36—H36A	0.9800	C34B—H34D	0.9800
C36—H36B	0.9800	C34B—H34E	0.9800
C36—H36C	0.9800	C34B—H34F	0.9800
C1B—C9B	1.5355 (17)	C35B—H35D	0.9800
C1B—C16B	1.5368 (17)	C35B—H35E	0.9800
C1B—C15B	1.5444 (16)	C35B—H35F	0.9800
C1B—C2B	1.5807 (17)	C36B—H36D	0.9800
C2B—C3B	1.5258 (16)	C36B—H36E	0.9800
C2B—H2B1	0.9900	C36B—H36F	0.9800
C16—C1—C9	107.90 (10)	C1B—C2B—H2B1	108.1
C16—C1—C15	107.47 (11)	C3B—C2B—H2B2	108.1
C9—C1—C15	111.24 (10)	C1B—C2B—H2B2	108.1
C16—C1—C2	112.45 (10)	H2B1—C2B—H2B2	107.3
C9—C1—C2	112.80 (10)	C4B—C3B—C8B	117.74 (10)
C15—C1—C2	104.88 (10)	C4B—C3B—C2B	119.75 (10)
C3—C2—C1	117.41 (10)	C8B—C3B—C2B	122.27 (11)
C3—C2—H2A	107.9	C5B—C4B—C3B	118.71 (11)
C1—C2—H2A	107.9	C5B—C4B—C17B	117.46 (11)
C3—C2—H2B	107.9	C3B—C4B—C17B	123.48 (10)
C1—C2—H2B	107.9	C6B—C5B—C4B	122.80 (12)
H2A—C2—H2B	107.2	C6B—C5B—H5B	118.6
C8—C3—C4	118.01 (10)	C4B—C5B—H5B	118.6
C8—C3—C2	122.15 (11)	C7B—C6B—C5B	116.22 (11)
C4—C3—C2	119.71 (10)	C7B—C6B—C21B	120.15 (11)
C5—C4—C3	118.80 (11)	C5B—C6B—C21B	123.38 (12)
C5—C4—C17	117.32 (11)	C6B—C7B—C8B	123.92 (11)
C3—C4—C17	123.17 (10)	C6B—C7B—H7B	118.0
C6—C5—C4	123.09 (11)	C8B—C7B—H7B	118.0
C6—C5—H5	118.5	C7B—C8B—C3B	117.74 (11)
C4—C5—H5	118.5	C7B—C8B—C25B	113.03 (10)
C7—C6—C5	116.45 (11)	C3B—C8B—C25B	128.82 (10)
C7—C6—C21	119.95 (11)	C10B—C9B—C14B	118.14 (11)
C5—C6—C21	123.25 (11)	C10B—C9B—C1B	122.28 (10)
C6—C7—C8	123.79 (12)	C14B—C9B—C1B	119.54 (10)
C6—C7—H7	118.1	C9B—C10B—C11B	122.08 (11)
C8—C7—H7	118.1	C9B—C10B—H10B	119.0
C7—C8—C3	118.01 (11)	C11B—C10B—H10B	119.0
C7—C8—C25	112.31 (10)	C12B—C11B—C10B	117.65 (11)
C3—C8—C25	129.29 (10)	C12B—C11B—C29B	121.21 (11)
C10—C9—C14	118.15 (11)	C10B—C11B—C29B	121.13 (11)
C10—C9—C1	122.49 (10)	C11B—C12B—C13B	122.22 (12)
C14—C9—C1	119.32 (11)	C11B—C12B—H12B	118.9
C9—C10—C11	122.08 (11)	C13B—C12B—H12B	118.9
C9—C10—H10	119.0	C14B—C13B—C12B	118.24 (11)
C11—C10—H10	119.0	C14B—C13B—C33B	122.09 (11)
C12—C11—C10	117.79 (11)	C12B—C13B—C33B	119.65 (12)
C12—C11—C29	122.65 (11)	C13B—C14B—C9B	121.67 (11)
C10—C11—C29	119.53 (10)	C13B—C14B—H14B	119.2
C11—C12—C13	122.19 (11)	C9B—C14B—H14B	119.2
C11—C12—H12	118.9	C1B—C15B—H15D	109.5
C13—C12—H12	118.9	C1B—C15B—H15E	109.5
C14—C13—C12	118.05 (11)	H15D—C15B—H15E	109.5
C14—C13—C33	121.89 (11)	C1B—C15B—H15F	109.5
C12—C13—C33	120.03 (11)	H15D—C15B—H15F	109.5
C13—C14—C9	121.72 (11)	H15E—C15B—H15F	109.5
C13—C14—H14	119.1	C1B—C16B—H16D	109.5
C9—C14—H14	119.1	C1B—C16B—H16E	109.5
C1—C15—H15A	109.5	H16D—C16B—H16E	109.5
C1—C15—H15B	109.5	C1B—C16B—H16F	109.5
H15A—C15—H15B	109.5	H16D—C16B—H16F	109.5
C1—C15—H15C	109.5	H16E—C16B—H16F	109.5
H15A—C15—H15C	109.5	C19B—C17B—C20B	106.07 (11)
H15B—C15—H15C	109.5	C19B—C17B—C18B	110.32 (10)
C1—C16—H16A	109.5	C20B—C17B—C18B	104.50 (11)
C1—C16—H16B	109.5	C19B—C17B—C4B	115.16 (11)
H16A—C16—H16B	109.5	C20B—C17B—C4B	110.65 (10)
C1—C16—H16C	109.5	C18B—C17B—C4B	109.57 (10)
H16A—C16—H16C	109.5	C17B—C18B—H18D	109.5
H16B—C16—H16C	109.5	C17B—C18B—H18E	109.5
C20—C17—C19	104.06 (10)	H18D—C18B—H18E	109.5
C20—C17—C18	105.94 (11)	C17B—C18B—H18F	109.5
C19—C17—C18	110.41 (10)	H18D—C18B—H18F	109.5
C20—C17—C4	111.71 (10)	H18E—C18B—H18F	109.5
C19—C17—C4	116.87 (10)	C17B—C19B—H19D	109.5
C18—C17—C4	107.36 (10)	C17B—C19B—H19E	109.5
C17—C18—H18A	109.5	H19D—C19B—H19E	109.5
C17—C18—H18B	109.5	C17B—C19B—H19F	109.5
H18A—C18—H18B	109.5	H19D—C19B—H19F	109.5
C17—C18—H18C	109.5	H19E—C19B—H19F	109.5
H18A—C18—H18C	109.5	C17B—C20B—H20D	109.5
H18B—C18—H18C	109.5	C17B—C20B—H20E	109.5
C17—C19—H19A	109.5	H20D—C20B—H20E	109.5
C17—C19—H19B	109.5	C17B—C20B—H20F	109.5
H19A—C19—H19B	109.5	H20D—C20B—H20F	109.5
C17—C19—H19C	109.5	H20E—C20B—H20F	109.5
H19A—C19—H19C	109.5	C22B—C21B—C23B	108.51 (12)
H19B—C19—H19C	109.5	C22B—C21B—C24B	107.81 (12)
C17—C20—H20A	109.5	C23B—C21B—C24B	109.09 (12)
C17—C20—H20B	109.5	C22B—C21B—C6B	112.53 (11)
H20A—C20—H20B	109.5	C23B—C21B—C6B	109.59 (11)
C17—C20—H20C	109.5	C24B—C21B—C6B	109.24 (10)
H20A—C20—H20C	109.5	C21B—C22B—H22D	109.5
H20B—C20—H20C	109.5	C21B—C22B—H22E	109.5
C22—C21—C23	108.50 (11)	H22D—C22B—H22E	109.5
C22—C21—C6	112.09 (10)	C21B—C22B—H22F	109.5
C23—C21—C6	110.32 (11)	H22D—C22B—H22F	109.5
C22—C21—C24	108.16 (11)	H22E—C22B—H22F	109.5
C23—C21—C24	109.03 (11)	C21B—C23B—H23D	109.5
C6—C21—C24	108.68 (10)	C21B—C23B—H23E	109.5
C21—C22—H22A	109.5	H23D—C23B—H23E	109.5
C21—C22—H22B	109.5	C21B—C23B—H23F	109.5
H22A—C22—H22B	109.5	H23D—C23B—H23F	109.5
C21—C22—H22C	109.5	H23E—C23B—H23F	109.5
H22A—C22—H22C	109.5	C21B—C24B—H24D	109.5
H22B—C22—H22C	109.5	C21B—C24B—H24E	109.5
C21—C23—H23A	109.5	H24D—C24B—H24E	109.5
C21—C23—H23B	109.5	C21B—C24B—H24F	109.5
H23A—C23—H23B	109.5	H24D—C24B—H24F	109.5
C21—C23—H23C	109.5	H24E—C24B—H24F	109.5
H23A—C23—H23C	109.5	C28B—C25B—C26B	107.36 (11)
H23B—C23—H23C	109.5	C28B—C25B—C27B	104.46 (10)
C21—C24—H24A	109.5	C26B—C25B—C27B	108.18 (10)
C21—C24—H24B	109.5	C28B—C25B—C8B	117.97 (10)
H24A—C24—H24B	109.5	C26B—C25B—C8B	112.19 (10)
C21—C24—H24C	109.5	C27B—C25B—C8B	106.04 (10)
H24A—C24—H24C	109.5	C25B—C26B—H26D	109.5
H24B—C24—H24C	109.5	C25B—C26B—H26E	109.5
C26—C25—C28	107.59 (11)	H26D—C26B—H26E	109.5
C26—C25—C27	108.28 (11)	C25B—C26B—H26F	109.5
C28—C25—C27	104.18 (10)	H26D—C26B—H26F	109.5
C26—C25—C8	111.50 (10)	H26E—C26B—H26F	109.5
C28—C25—C8	118.47 (10)	C25B—C27B—H27D	109.5
C27—C25—C8	106.19 (10)	C25B—C27B—H27E	109.5
C25—C26—H26A	109.5	H27D—C27B—H27E	109.5
C25—C26—H26B	109.5	C25B—C27B—H27F	109.5
H26A—C26—H26B	109.5	H27D—C27B—H27F	109.5
C25—C26—H26C	109.5	H27E—C27B—H27F	109.5
H26A—C26—H26C	109.5	C25B—C28B—H28D	109.5
H26B—C26—H26C	109.5	C25B—C28B—H28E	109.5
C25—C27—H27A	109.5	H28D—C28B—H28E	109.5
C25—C27—H27B	109.5	C25B—C28B—H28F	109.5
H27A—C27—H27B	109.5	H28D—C28B—H28F	109.5
C25—C27—H27C	109.5	H28E—C28B—H28F	109.5
H27A—C27—H27C	109.5	C30B—C29B—C11B	111.44 (11)
H27B—C27—H27C	109.5	C30B—C29B—C32B	107.75 (13)
C25—C28—H28A	109.5	C11B—C29B—C32B	111.54 (11)
C25—C28—H28B	109.5	C30B—C29B—C31B	108.87 (13)
H28A—C28—H28B	109.5	C11B—C29B—C31B	108.24 (11)
C25—C28—H28C	109.5	C32B—C29B—C31B	108.94 (12)
H28A—C28—H28C	109.5	C29B—C30B—H30D	109.5
H28B—C28—H28C	109.5	C29B—C30B—H30E	109.5
C30—C29—C32	107.00 (12)	H30D—C30B—H30E	109.5
C30—C29—C31	108.71 (13)	C29B—C30B—H30F	109.5
C32—C29—C31	109.05 (12)	H30D—C30B—H30F	109.5
C30—C29—C11	112.36 (11)	H30E—C30B—H30F	109.5
C32—C29—C11	110.74 (11)	C29B—C31B—H31D	109.5
C31—C29—C11	108.91 (11)	C29B—C31B—H31E	109.5
C29—C30—H30A	109.5	H31D—C31B—H31E	109.5
C29—C30—H30B	109.5	C29B—C31B—H31F	109.5
H30A—C30—H30B	109.5	H31D—C31B—H31F	109.5
C29—C30—H30C	109.5	H31E—C31B—H31F	109.5
H30A—C30—H30C	109.5	C29B—C32B—H32D	109.5
H30B—C30—H30C	109.5	C29B—C32B—H32E	109.5
C29—C31—H31A	109.5	H32D—C32B—H32E	109.5
C29—C31—H31B	109.5	C29B—C32B—H32F	109.5
H31A—C31—H31B	109.5	H32D—C32B—H32F	109.5
C29—C31—H31C	109.5	H32E—C32B—H32F	109.5
H31A—C31—H31C	109.5	C34D—C33B—C36D	109.18 (15)
H31B—C31—H31C	109.5	C35B—C33B—C13B	115.6 (10)
C29—C32—H32A	109.5	C34D—C33B—C13B	110.91 (12)
C29—C32—H32B	109.5	C36D—C33B—C13B	112.23 (12)
H32A—C32—H32B	109.5	C34D—C33B—C35D	109.60 (18)
C29—C32—H32C	109.5	C36D—C33B—C35D	107.10 (14)
H32A—C32—H32C	109.5	C13B—C33B—C35D	107.71 (13)
H32B—C32—H32C	109.5	C35B—C33B—C36B	111.7 (10)
C36—C33—C34	108.07 (12)	C13B—C33B—C36B	110.0 (12)
C36—C33—C13	112.17 (10)	C35B—C33B—C34B	111.0 (9)
C34—C33—C13	110.86 (10)	C13B—C33B—C34B	103.7 (7)
C36—C33—C35	108.28 (11)	C36B—C33B—C34B	103.9 (9)
C34—C33—C35	109.40 (12)	C33B—C34D—H34J	109.5
C13—C33—C35	108.02 (11)	C33B—C34D—H34K	109.5
C33—C34—H34A	109.5	C33B—C34D—H34L	109.5
C33—C34—H34B	109.5	C33B—C35D—H35J	109.5
H34A—C34—H34B	109.5	C33B—C35D—H35K	109.5
C33—C34—H34C	109.5	C33B—C35D—H35L	109.5
H34A—C34—H34C	109.5	C33B—C36D—H36J	109.5
H34B—C34—H34C	109.5	C33B—C36D—H36K	109.5
C33—C35—H35A	109.5	C33B—C36D—H36L	109.5
C33—C35—H35B	109.5	C33B—C34B—H34D	109.5
H35A—C35—H35B	109.5	C33B—C34B—H34E	109.5
C33—C35—H35C	109.5	H34D—C34B—H34E	109.5
H35A—C35—H35C	109.5	C33B—C34B—H34F	109.5
H35B—C35—H35C	109.5	H34D—C34B—H34F	109.5
C33—C36—H36A	109.5	H34E—C34B—H34F	109.5
C33—C36—H36B	109.5	C33B—C35B—H35D	109.5
H36A—C36—H36B	109.5	C33B—C35B—H35E	109.5
C33—C36—H36C	109.5	H35D—C35B—H35E	109.5
H36A—C36—H36C	109.5	C33B—C35B—H35F	109.5
H36B—C36—H36C	109.5	H35D—C35B—H35F	109.5
C9B—C1B—C16B	107.57 (10)	H35E—C35B—H35F	109.5
C9B—C1B—C15B	111.12 (10)	C33B—C36B—H36D	109.5
C16B—C1B—C15B	107.28 (10)	C33B—C36B—H36E	109.5
C9B—C1B—C2B	111.67 (10)	H36D—C36B—H36E	109.5
C16B—C1B—C2B	113.69 (10)	C33B—C36B—H36F	109.5
C15B—C1B—C2B	105.45 (9)	H36D—C36B—H36F	109.5
C3B—C2B—C1B	116.97 (9)	H36E—C36B—H36F	109.5
C3B—C2B—H2B1	108.1
C16—C1—C2—C3	59.41 (14)	C1B—C2B—C3B—C4B	99.53 (13)
C9—C1—C2—C3	−62.89 (14)	C1B—C2B—C3B—C8B	−74.75 (15)
C15—C1—C2—C3	175.89 (11)	C8B—C3B—C4B—C5B	17.46 (17)
C1—C2—C3—C8	−80.96 (14)	C2B—C3B—C4B—C5B	−157.08 (11)
C1—C2—C3—C4	94.96 (14)	C8B—C3B—C4B—C17B	−155.65 (11)
C8—C3—C4—C5	13.79 (17)	C2B—C3B—C4B—C17B	29.82 (17)
C2—C3—C4—C5	−162.29 (11)	C3B—C4B—C5B—C6B	−4.81 (18)
C8—C3—C4—C17	−156.21 (11)	C17B—C4B—C5B—C6B	168.71 (11)
C2—C3—C4—C17	27.71 (17)	C4B—C5B—C6B—C7B	−7.96 (18)
C3—C4—C5—C6	−3.26 (18)	C4B—C5B—C6B—C21B	177.90 (12)
C17—C4—C5—C6	167.32 (11)	C5B—C6B—C7B—C8B	8.21 (19)
C4—C5—C6—C7	−5.92 (18)	C21B—C6B—C7B—C8B	−177.45 (12)
C4—C5—C6—C21	−179.15 (11)	C6B—C7B—C8B—C3B	4.36 (19)
C5—C6—C7—C8	4.58 (19)	C6B—C7B—C8B—C25B	−168.91 (12)
C21—C6—C7—C8	178.04 (12)	C4B—C3B—C8B—C7B	−17.15 (17)
C6—C7—C8—C3	5.91 (19)	C2B—C3B—C8B—C7B	157.24 (11)
C6—C7—C8—C25	−167.59 (12)	C4B—C3B—C8B—C25B	154.90 (12)
C4—C3—C8—C7	−14.95 (17)	C2B—C3B—C8B—C25B	−30.71 (19)
C2—C3—C8—C7	161.03 (11)	C16B—C1B—C9B—C10B	130.13 (12)
C4—C3—C8—C25	157.28 (12)	C15B—C1B—C9B—C10B	12.99 (17)
C2—C3—C8—C25	−26.74 (19)	C2B—C1B—C9B—C10B	−104.45 (13)
C16—C1—C9—C10	129.21 (12)	C16B—C1B—C9B—C14B	−47.29 (15)
C15—C1—C9—C10	11.56 (17)	C15B—C1B—C9B—C14B	−164.44 (11)
C2—C1—C9—C10	−105.97 (13)	C2B—C1B—C9B—C14B	78.12 (14)
C16—C1—C9—C14	−48.64 (15)	C14B—C9B—C10B—C11B	1.04 (19)
C15—C1—C9—C14	−166.28 (11)	C1B—C9B—C10B—C11B	−176.41 (12)
C2—C1—C9—C14	76.19 (14)	C9B—C10B—C11B—C12B	−1.01 (19)
C14—C9—C10—C11	−0.45 (19)	C9B—C10B—C11B—C29B	−179.70 (12)
C1—C9—C10—C11	−178.32 (12)	C10B—C11B—C12B—C13B	0.6 (2)
C9—C10—C11—C12	0.20 (19)	C29B—C11B—C12B—C13B	179.24 (13)
C9—C10—C11—C29	−178.30 (12)	C11B—C12B—C13B—C14B	−0.2 (2)
C10—C11—C12—C13	0.47 (19)	C11B—C12B—C13B—C33B	−179.00 (13)
C29—C11—C12—C13	178.92 (12)	C12B—C13B—C14B—C9B	0.2 (2)
C11—C12—C13—C14	−0.84 (19)	C33B—C13B—C14B—C9B	179.01 (13)
C11—C12—C13—C33	−178.98 (12)	C10B—C9B—C14B—C13B	−0.62 (19)
C12—C13—C14—C9	0.57 (19)	C1B—C9B—C14B—C13B	176.91 (12)
C33—C13—C14—C9	178.67 (12)	C5B—C4B—C17B—C19B	107.56 (13)
C10—C9—C14—C13	0.05 (19)	C3B—C4B—C17B—C19B	−79.26 (15)
C1—C9—C14—C13	177.99 (12)	C5B—C4B—C17B—C20B	−12.69 (16)
C5—C4—C17—C20	0.12 (15)	C3B—C4B—C17B—C20B	160.49 (12)
C3—C4—C17—C20	170.26 (11)	C5B—C4B—C17B—C18B	−127.40 (12)
C5—C4—C17—C19	119.79 (12)	C3B—C4B—C17B—C18B	45.79 (15)
C3—C4—C17—C19	−70.08 (15)	C7B—C6B—C21B—C22B	174.21 (12)
C5—C4—C17—C18	−115.60 (12)	C5B—C6B—C21B—C22B	−11.87 (18)
C3—C4—C17—C18	54.53 (15)	C7B—C6B—C21B—C23B	53.38 (16)
C7—C6—C21—C22	176.49 (12)	C5B—C6B—C21B—C23B	−132.70 (14)
C5—C6—C21—C22	−10.51 (17)	C7B—C6B—C21B—C24B	−66.09 (16)
C7—C6—C21—C23	55.46 (15)	C5B—C6B—C21B—C24B	107.83 (15)
C5—C6—C21—C23	−131.53 (13)	C7B—C8B—C25B—C28B	175.88 (11)
C7—C6—C21—C24	−64.02 (15)	C3B—C8B—C25B—C28B	3.52 (19)
C5—C6—C21—C24	108.98 (14)	C7B—C8B—C25B—C26B	−58.56 (14)
C7—C8—C25—C26	−63.09 (14)	C3B—C8B—C25B—C26B	129.08 (13)
C3—C8—C25—C26	124.32 (14)	C7B—C8B—C25B—C27B	59.34 (13)
C7—C8—C25—C28	171.24 (11)	C3B—C8B—C25B—C27B	−113.02 (13)
C3—C8—C25—C28	−1.35 (19)	C12B—C11B—C29B—C30B	29.10 (19)
C7—C8—C25—C27	54.65 (13)	C10B—C11B—C29B—C30B	−152.25 (14)
C3—C8—C25—C27	−117.94 (14)	C12B—C11B—C29B—C32B	149.58 (14)
C12—C11—C29—C30	13.84 (19)	C10B—C11B—C29B—C32B	−31.77 (18)
C10—C11—C29—C30	−167.74 (13)	C12B—C11B—C29B—C31B	−90.58 (15)
C12—C11—C29—C32	133.44 (14)	C10B—C11B—C29B—C31B	88.06 (15)
C10—C11—C29—C32	−48.14 (17)	C14B—C13B—C33B—C35B	−63.2 (9)
C12—C11—C29—C31	−106.65 (15)	C12B—C13B—C33B—C35B	115.6 (9)
C10—C11—C29—C31	71.77 (15)	C14B—C13B—C33B—C34D	129.45 (19)
C14—C13—C33—C36	13.22 (18)	C12B—C13B—C33B—C34D	−51.8 (2)
C12—C13—C33—C36	−168.72 (12)	C14B—C13B—C33B—C36D	7.0 (2)
C14—C13—C33—C34	134.12 (14)	C12B—C13B—C33B—C36D	−174.17 (14)
C12—C13—C33—C34	−47.82 (17)	C14B—C13B—C33B—C35D	−110.62 (17)
C14—C13—C33—C35	−106.04 (14)	C12B—C13B—C33B—C35D	68.18 (18)
C12—C13—C33—C35	72.02 (15)	C14B—C13B—C33B—C36B	169.2 (10)
C9B—C1B—C2B—C3B	−72.14 (13)	C12B—C13B—C33B—C36B	−12.0 (10)
C16B—C1B—C2B—C3B	49.81 (14)	C14B—C13B—C33B—C34B	58.6 (7)
C15B—C1B—C2B—C3B	167.06 (10)	C12B—C13B—C33B—C34B	−122.6 (7)

1-(2,4,6-Tri-tert-butylphenyl)-2-(3,5-di-tert-butylphenyl)- 2-methylpropane (IIIahigh)

Crystal data

C36H58	Z = 4
Mr = 490.82	F(000) = 1096
Triclinic, P1	Dx = 1.015 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 15.7799 (17) Å	Cell parameters from 9886 reflections
b = 19.394 (2) Å	θ = 3.8–29.1°
c = 10.5789 (11) Å	µ = 0.06 mm^−1
α = 94.982 (1)°	T = 100 K
β = 95.188 (1)°	Parallelipiped, colorless
γ = 89.963 (2)°	0.40 × 0.36 × 0.16 mm
V = 3212.1 (6) Å^3

Data collection

CCD area detector diffractometer	10124 independent reflections
Radiation source: fine-focus sealed tube	6146 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.104
phi and ω scans	θmax = 29.2°, θmin = 20.8°
Absorption correction: multi-scan Sadabs (Bruker)	h = −21→21
Tmin = 0.898, Tmax = 0.991	k = −24→26
21193 measured reflections	l = −14→14

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)] = 0.053	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.138	H-atom parameters constrained
S = 0.99	w = 1/[σ^2(Fo^2) + (0.0502P)^2] where P = (Fo^2 + 2Fc^2)/3
10124 reflections	(Δ/σ)max = 0.001
693 parameters	Δρmax = 0.15 e Å^−3
6 restraints	Δρmin = −0.13 e Å^−3

Special details

Experimental. Cell used is that of published room-temperature structure (Frey, J., Nugiel, D. A. and Rappoport, Z. (1991) J. Org. Chem., 56, 466–469.

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 between d = 0 and d = 1.0 Angstroms (theta_min 20.82 degrees). The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.41837 (10)	0.72771 (8)	0.13774 (12)	0.0171 (3)
C2	0.51702 (10)	0.74221 (8)	0.16794 (12)	0.0165 (3)
H2A	0.5476	0.6995	0.1415	0.020*
H2B	0.5333	0.7784	0.1140	0.020*
C3	0.54888 (10)	0.76493 (8)	0.30512 (12)	0.0151 (3)
C4	0.58156 (10)	0.71433 (8)	0.38786 (12)	0.0156 (3)
C5	0.58828 (10)	0.73151 (8)	0.51979 (12)	0.0172 (3)
H5	0.6069	0.6970	0.5743	0.021*
C6	0.56892 (10)	0.79697 (8)	0.57475 (13)	0.0172 (3)
C7	0.54946 (11)	0.84780 (8)	0.49167 (13)	0.0183 (3)
H7	0.5400	0.8936	0.5269	0.022*
C8	0.54308 (10)	0.83478 (8)	0.35791 (12)	0.0160 (3)
C9	0.38681 (10)	0.66769 (8)	0.20749 (12)	0.0165 (3)
C10	0.36578 (10)	0.60292 (8)	0.14494 (12)	0.0173 (3)
H10	0.3724	0.5950	0.0565	0.021*
C11	0.33495 (10)	0.54887 (8)	0.20924 (13)	0.0174 (3)
C12	0.32562 (11)	0.56182 (8)	0.33926 (13)	0.0183 (3)
H12	0.3053	0.5258	0.3841	0.022*
C13	0.34535 (10)	0.62640 (8)	0.40550 (12)	0.0168 (3)
C14	0.37628 (10)	0.67866 (8)	0.33854 (12)	0.0172 (3)
H14	0.3905	0.7225	0.3824	0.021*
C15	0.40543 (12)	0.71138 (10)	−0.00824 (13)	0.0234 (3)
H15A	0.4224	0.7516	−0.0502	0.030*
H15B	0.3453	0.7006	−0.0338	0.030*
H15C	0.4403	0.6716	−0.0334	0.030*
C16	0.36466 (11)	0.79152 (9)	0.17195 (15)	0.0218 (3)
H16A	0.3748	0.8275	0.1153	0.028*
H16B	0.3807	0.8092	0.2605	0.028*
H16C	0.3042	0.7786	0.1619	0.028*
C17	0.62335 (10)	0.64519 (8)	0.33878 (13)	0.0166 (3)
C18	0.69603 (11)	0.66425 (9)	0.25889 (14)	0.0222 (3)
H18A	0.7252	0.6220	0.2295	0.029*
H18B	0.7366	0.6953	0.3115	0.029*
H18C	0.6722	0.6875	0.1851	0.029*
C19	0.56349 (11)	0.59024 (9)	0.26281 (14)	0.0208 (3)
H19A	0.5953	0.5477	0.2446	0.027*
H19B	0.5408	0.6078	0.1826	0.027*
H19C	0.5164	0.5804	0.3131	0.027*
C20	0.66602 (12)	0.60695 (9)	0.44990 (14)	0.0217 (3)
H20A	0.6969	0.5667	0.4155	0.028*
H20B	0.6223	0.5915	0.5015	0.028*
H20C	0.7059	0.6384	0.5030	0.028*
C21	0.57740 (11)	0.81644 (9)	0.71931 (13)	0.0189 (3)
C22	0.59343 (13)	0.75289 (10)	0.79515 (13)	0.0246 (3)
H22A	0.6462	0.7304	0.7721	0.032*
H22B	0.5458	0.7202	0.7751	0.032*
H22C	0.5986	0.7675	0.8866	0.032*
C23	0.49599 (12)	0.85240 (9)	0.76054 (13)	0.0225 (3)
H23A	0.5050	0.8699	0.8505	0.029*
H23B	0.4486	0.8191	0.7489	0.029*
H23C	0.4826	0.8910	0.7085	0.029*
C24	0.65367 (12)	0.86682 (10)	0.75299 (15)	0.0250 (3)
H24A	0.7057	0.8445	0.7263	0.032*
H24B	0.6603	0.8791	0.8452	0.032*
H24C	0.6434	0.9088	0.7088	0.032*
C25	0.54042 (11)	0.90333 (8)	0.28904 (13)	0.0182 (3)
C26	0.46096 (12)	0.94628 (9)	0.31701 (15)	0.0233 (3)
H26A	0.4638	0.9907	0.2798	0.030*
H26B	0.4588	0.9546	0.4094	0.030*
H26C	0.4098	0.9209	0.2796	0.030*
C27	0.62087 (12)	0.94598 (9)	0.34563 (14)	0.0231 (3)
H27A	0.6217	0.9900	0.3068	0.030*
H27B	0.6721	0.9197	0.3276	0.030*
H27C	0.6194	0.9550	0.4380	0.030*
C28	0.54642 (12)	0.89827 (9)	0.14398 (14)	0.0229 (3)
H28A	0.5562	0.9445	0.1171	0.030*
H28B	0.4932	0.8791	0.1001	0.030*
H28C	0.5937	0.8680	0.1224	0.030*
C29	0.31530 (12)	0.47811 (9)	0.13607 (14)	0.0203 (3)
C30	0.26544 (19)	0.43043 (12)	0.21140 (18)	0.0386 (5)
H30A	0.2472	0.3888	0.1566	0.050*
H30B	0.2153	0.4548	0.2404	0.050*
H30C	0.3019	0.4173	0.2853	0.050*
C31	0.39941 (16)	0.44298 (12)	0.1061 (2)	0.0376 (5)
H31A	0.3875	0.3969	0.0627	0.049*
H31B	0.4352	0.4387	0.1857	0.049*
H31C	0.4292	0.4710	0.0510	0.049*
C32	0.26108 (16)	0.48625 (10)	0.01005 (17)	0.0320 (4)
H32A	0.2466	0.4404	−0.0329	0.042*
H32B	0.2934	0.5124	−0.0449	0.042*
H32C	0.2088	0.5111	0.0276	0.042*
C33	0.33531 (11)	0.63741 (9)	0.54871 (13)	0.0201 (3)
C34	0.24874 (14)	0.61016 (12)	0.57917 (16)	0.0325 (4)
H34A	0.2436	0.6183	0.6709	0.042*
H34B	0.2443	0.5604	0.5537	0.042*
H34C	0.2030	0.6344	0.5324	0.042*
C35	0.40709 (15)	0.59752 (11)	0.61936 (15)	0.0303 (4)
H35A	0.4015	0.6033	0.7112	0.039*
H35B	0.4624	0.6157	0.6022	0.039*
H35C	0.4029	0.5483	0.5896	0.039*
C36	0.34294 (14)	0.71382 (10)	0.59885 (15)	0.0286 (4)
H36A	0.3353	0.7186	0.6901	0.037*
H36B	0.2991	0.7404	0.5531	0.037*
H36C	0.3993	0.7314	0.5854	0.037*
C1B	1.09960 (10)	0.69189 (8)	0.08112 (12)	0.0156 (3)
C2B	1.00019 (10)	0.67963 (8)	0.07208 (11)	0.0152 (3)
H2B1	0.9732	0.7097	0.0091	0.018*
H2B2	0.9883	0.6311	0.0382	0.018*
C3B	0.95700 (10)	0.69300 (8)	0.19523 (12)	0.0155 (3)
C4B	0.91402 (10)	0.75664 (8)	0.22046 (12)	0.0168 (3)
C5B	0.90189 (10)	0.77967 (8)	0.34750 (13)	0.0179 (3)
H5B	0.8772	0.8238	0.3648	0.022*
C6B	0.92496 (11)	0.73987 (9)	0.44914 (12)	0.0179 (3)
C7B	0.95063 (11)	0.67252 (8)	0.41757 (12)	0.0184 (3)
H7B	0.9594	0.6425	0.4838	0.022*
C8B	0.96444 (10)	0.64623 (8)	0.29294 (12)	0.0161 (3)
C9B	1.12260 (10)	0.76906 (8)	0.10063 (12)	0.0163 (3)
C10B	1.14853 (10)	0.80556 (8)	0.00213 (12)	0.0177 (3)
H10B	1.1490	0.7824	−0.0807	0.021*
C11B	1.17377 (11)	0.87517 (9)	0.02220 (14)	0.0187 (3)
C12B	1.17152 (12)	0.90838 (9)	0.14466 (15)	0.0218 (3)
H12B	1.1879	0.9557	0.1598	0.026*
C13B	1.14559 (12)	0.87357 (9)	0.24579 (14)	0.0207 (3)
C14B	1.12114 (10)	0.80430 (8)	0.22213 (13)	0.0183 (3)
H14B	1.1031	0.7804	0.2897	0.022*
C15B	1.12842 (11)	0.65849 (9)	−0.04612 (13)	0.0202 (3)
H15D	1.0949	0.6774	−0.1175	0.026*
H15E	1.1197	0.6083	−0.0510	0.026*
H15F	1.1889	0.6686	−0.0504	0.026*
C16B	1.14903 (10)	0.65580 (8)	0.18894 (14)	0.0195 (3)
H16D	1.1446	0.6055	0.1699	0.025*
H16E	1.1249	0.6690	0.2697	0.025*
H16F	1.2090	0.6699	0.1958	0.025*
C17B	0.87037 (11)	0.79912 (9)	0.11386 (13)	0.0182 (3)
C18B	0.81698 (11)	0.74969 (10)	0.01453 (14)	0.0226 (3)
H18D	0.7860	0.7767	−0.0486	0.029*
H18E	0.7763	0.7240	0.0576	0.029*
H18F	0.8548	0.7171	−0.0283	0.029*
C19B	0.93125 (12)	0.84328 (9)	0.04737 (15)	0.0235 (3)
H19D	0.9683	0.8710	0.1118	0.031*
H19E	0.8980	0.8741	−0.0065	0.031*
H19F	0.9661	0.8128	−0.0054	0.031*
C20B	0.80448 (13)	0.84986 (10)	0.16893 (16)	0.0272 (4)
H20D	0.8340	0.8854	0.2285	0.035*
H20E	0.7646	0.8244	0.2138	0.035*
H20F	0.7731	0.8720	0.0993	0.035*
C21B	0.91503 (12)	0.76505 (9)	0.58863 (13)	0.0218 (3)
C22B	0.89519 (15)	0.84250 (11)	0.60650 (16)	0.0305 (4)
H22D	0.8405	0.8515	0.5596	0.040*
H22E	0.9401	0.8690	0.5741	0.040*
H22F	0.8923	0.8565	0.6973	0.040*
C23B	0.99748 (14)	0.75111 (12)	0.67155 (15)	0.0310 (4)
H23D	1.0118	0.7020	0.6591	0.040*
H23E	0.9892	0.7633	0.7614	0.040*
H23F	1.0439	0.7792	0.6469	0.040*
C24B	0.84094 (15)	0.72535 (12)	0.63536 (16)	0.0310 (4)
H24D	0.8546	0.6760	0.6335	0.040*
H24E	0.7890	0.7316	0.5796	0.040*
H24F	0.8321	0.7432	0.7227	0.040*
C25B	0.97537 (11)	0.56603 (8)	0.27985 (13)	0.0177 (3)
C26B	1.05078 (11)	0.54224 (9)	0.36948 (14)	0.0208 (3)
H26D	1.1040	0.5616	0.3463	0.027*
H26E	1.0537	0.4916	0.3611	0.027*
H26F	1.0424	0.5584	0.4578	0.027*
C27B	0.89211 (11)	0.53506 (9)	0.31956 (14)	0.0212 (3)
H27D	0.8436	0.5495	0.2637	0.028*
H27E	0.8846	0.5517	0.4080	0.028*
H27F	0.8955	0.4844	0.3122	0.028*
C28B	0.98493 (11)	0.53030 (9)	0.14631 (14)	0.0206 (3)
H28D	0.9366	0.5423	0.0877	0.027*
H28E	0.9865	0.4800	0.1505	0.027*
H28F	1.0379	0.5459	0.1157	0.027*
C29B	1.20149 (13)	0.91455 (10)	−0.08713 (15)	0.0234 (3)
C30B	1.2649 (2)	0.97299 (15)	−0.0381 (2)	0.0427 (6)
H30D	1.2825	0.9962	−0.1104	0.055*
H30E	1.3150	0.9535	0.0074	0.055*
H30F	1.2378	1.0065	0.0198	0.055*
C31B	1.12178 (16)	0.94577 (12)	−0.15418 (18)	0.0332 (4)
H31D	1.1384	0.9724	−0.2227	0.043*
H31E	1.0936	0.9763	−0.0924	0.043*
H31F	1.0826	0.9085	−0.1902	0.043*
C32B	1.24422 (19)	0.86587 (12)	−0.1851 (2)	0.0375 (5)
H32D	1.2621	0.8925	−0.2528	0.049*
H32E	1.2037	0.8298	−0.2220	0.049*
H32F	1.2941	0.8444	−0.1427	0.049*
C33B	1.14261 (15)	0.91295 (11)	0.37721 (17)	0.0290 (4)
C34D	1.2266 (3)	0.9498 (3)	0.4197 (3)	0.0652 (19)	0.89 (3)
H34J	1.2386	0.9825	0.3578	0.085*	0.89 (3)
H34K	1.2724	0.9158	0.4254	0.085*	0.89 (3)
H34L	1.2230	0.9751	0.5034	0.085*	0.89 (3)
C35D	1.0707 (3)	0.96734 (18)	0.3676 (3)	0.0522 (14)	0.89 (3)
H35J	1.0809	0.9976	0.3010	0.068*	0.89 (3)
H35K	1.0699	0.9951	0.4494	0.068*	0.89 (3)
H35L	1.0157	0.9436	0.3463	0.068*	0.89 (3)
C36D	1.12157 (18)	0.86563 (14)	0.47831 (18)	0.0343 (12)	0.89 (3)
H36J	1.1676	0.8322	0.4908	0.045*	0.89 (3)
H36K	1.0682	0.8408	0.4503	0.045*	0.89 (3)
H36L	1.1155	0.8935	0.5588	0.045*	0.89 (3)
C34B	1.2027 (15)	0.8684 (12)	0.470 (2)	0.041 (10)*	0.11 (3)
H34D	1.2597	0.8891	0.4828	0.053*	0.11 (3)
H34E	1.2061	0.8208	0.4312	0.053*	0.11 (3)
H34F	1.1787	0.8681	0.5521	0.053*	0.11 (3)
C35B	1.0523 (17)	0.9192 (17)	0.422 (4)	0.064 (12)*	0.11 (3)
H35D	1.0222	0.9570	0.3818	0.083*	0.11 (3)
H35E	1.0562	0.9287	0.5147	0.083*	0.11 (3)
H35F	1.0210	0.8757	0.3974	0.083*	0.11 (3)
C36B	1.1867 (17)	0.9866 (13)	0.378 (3)	0.053 (11)*	0.11 (3)
H36D	1.1998	1.0060	0.4666	0.068*	0.11 (3)
H36E	1.1480	1.0176	0.3330	0.068*	0.11 (3)
H36F	1.2394	0.9816	0.3362	0.068*	0.11 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0166 (7)	0.0199 (7)	0.0149 (5)	−0.0042 (5)	0.0019 (4)	0.0022 (4)
C2	0.0168 (7)	0.0182 (7)	0.0148 (5)	−0.0040 (5)	0.0038 (4)	0.0002 (4)
C3	0.0150 (6)	0.0152 (6)	0.0153 (5)	−0.0028 (5)	0.0043 (4)	−0.0005 (4)
C4	0.0156 (6)	0.0163 (6)	0.0151 (5)	−0.0023 (5)	0.0040 (4)	−0.0006 (4)
C5	0.0184 (7)	0.0177 (7)	0.0155 (5)	−0.0029 (5)	0.0022 (4)	0.0001 (4)
C6	0.0186 (7)	0.0170 (7)	0.0162 (5)	−0.0036 (5)	0.0040 (4)	−0.0004 (4)
C7	0.0211 (7)	0.0185 (7)	0.0157 (6)	−0.0030 (5)	0.0057 (4)	−0.0006 (4)
C8	0.0173 (7)	0.0154 (6)	0.0156 (5)	−0.0023 (5)	0.0045 (4)	0.0005 (4)
C9	0.0169 (7)	0.0181 (7)	0.0147 (5)	−0.0025 (5)	0.0024 (4)	0.0013 (4)
C10	0.0176 (7)	0.0181 (7)	0.0161 (5)	−0.0019 (5)	0.0023 (4)	0.0000 (4)
C11	0.0182 (7)	0.0167 (7)	0.0171 (6)	−0.0033 (5)	0.0015 (4)	−0.0006 (4)
C12	0.0200 (7)	0.0184 (7)	0.0164 (5)	−0.0037 (5)	0.0022 (4)	0.0001 (4)
C13	0.0183 (7)	0.0181 (7)	0.0141 (5)	−0.0042 (5)	0.0024 (4)	0.0003 (4)
C14	0.0175 (7)	0.0191 (7)	0.0150 (5)	−0.0038 (5)	0.0026 (4)	0.0000 (4)
C15	0.0257 (8)	0.0292 (8)	0.0153 (5)	−0.0095 (6)	0.0001 (5)	0.0041 (5)
C16	0.0187 (7)	0.0201 (7)	0.0276 (6)	−0.0005 (6)	0.0035 (5)	0.0060 (5)
C17	0.0159 (6)	0.0154 (6)	0.0182 (5)	−0.0007 (5)	0.0021 (4)	−0.0008 (4)
C18	0.0167 (7)	0.0254 (8)	0.0250 (6)	−0.0005 (6)	0.0069 (5)	0.0004 (5)
C19	0.0216 (7)	0.0165 (7)	0.0231 (6)	−0.0029 (6)	0.0011 (5)	−0.0035 (4)
C20	0.0238 (8)	0.0178 (7)	0.0229 (6)	0.0030 (6)	−0.0012 (5)	0.0012 (4)
C21	0.0219 (7)	0.0198 (7)	0.0149 (5)	−0.0034 (6)	0.0034 (4)	−0.0014 (4)
C22	0.0330 (9)	0.0245 (8)	0.0166 (5)	−0.0003 (7)	0.0027 (5)	0.0022 (5)
C23	0.0245 (8)	0.0235 (8)	0.0199 (6)	−0.0018 (6)	0.0077 (5)	−0.0017 (5)
C24	0.0231 (8)	0.0276 (8)	0.0233 (6)	−0.0084 (6)	0.0020 (5)	−0.0033 (5)
C25	0.0211 (7)	0.0158 (7)	0.0183 (5)	−0.0032 (5)	0.0047 (4)	0.0022 (4)
C26	0.0245 (8)	0.0183 (7)	0.0281 (7)	0.0023 (6)	0.0068 (5)	0.0030 (5)
C27	0.0233 (8)	0.0213 (7)	0.0248 (6)	−0.0083 (6)	0.0040 (5)	−0.0001 (5)
C28	0.0300 (8)	0.0220 (7)	0.0176 (6)	−0.0065 (6)	0.0052 (5)	0.0035 (4)
C29	0.0238 (8)	0.0173 (7)	0.0190 (6)	−0.0026 (6)	−0.0002 (5)	−0.0011 (4)
C30	0.0596 (15)	0.0279 (9)	0.0281 (7)	−0.0232 (10)	0.0107 (8)	−0.0054 (6)
C31	0.0296 (10)	0.0262 (10)	0.0533 (11)	0.0045 (8)	−0.0011 (8)	−0.0119 (8)
C32	0.0435 (11)	0.0224 (8)	0.0265 (7)	−0.0016 (8)	−0.0121 (7)	−0.0032 (5)
C33	0.0241 (8)	0.0217 (7)	0.0144 (5)	−0.0073 (6)	0.0035 (5)	−0.0008 (4)
C34	0.0316 (10)	0.0410 (11)	0.0248 (7)	−0.0181 (8)	0.0125 (6)	−0.0072 (6)
C35	0.0379 (10)	0.0329 (9)	0.0195 (6)	−0.0021 (8)	−0.0027 (6)	0.0036 (5)
C36	0.0395 (10)	0.0252 (8)	0.0212 (6)	−0.0083 (7)	0.0094 (6)	−0.0047 (5)
C1B	0.0151 (6)	0.0151 (6)	0.0169 (5)	−0.0018 (5)	0.0041 (4)	−0.0001 (4)
C2B	0.0151 (6)	0.0177 (6)	0.0132 (5)	−0.0023 (5)	0.0037 (4)	0.0002 (4)
C3B	0.0155 (6)	0.0174 (7)	0.0140 (5)	−0.0031 (5)	0.0030 (4)	0.0014 (4)
C4B	0.0174 (7)	0.0181 (7)	0.0151 (5)	−0.0019 (5)	0.0028 (4)	0.0020 (4)
C5B	0.0196 (7)	0.0177 (7)	0.0166 (5)	−0.0013 (5)	0.0036 (4)	−0.0002 (4)
C6B	0.0195 (7)	0.0205 (7)	0.0136 (5)	−0.0027 (5)	0.0037 (4)	−0.0003 (4)
C7B	0.0215 (7)	0.0194 (7)	0.0145 (5)	−0.0027 (6)	0.0032 (4)	0.0016 (4)
C8B	0.0162 (6)	0.0173 (7)	0.0149 (5)	−0.0034 (5)	0.0016 (4)	0.0017 (4)
C9B	0.0163 (6)	0.0161 (7)	0.0168 (5)	−0.0035 (5)	0.0040 (4)	0.0004 (4)
C10B	0.0185 (7)	0.0174 (7)	0.0178 (5)	−0.0030 (5)	0.0045 (4)	0.0014 (4)
C11B	0.0190 (7)	0.0174 (7)	0.0203 (6)	−0.0024 (5)	0.0041 (5)	0.0024 (4)
C12B	0.0251 (8)	0.0166 (7)	0.0241 (6)	−0.0056 (6)	0.0069 (5)	−0.0014 (5)
C13B	0.0227 (7)	0.0187 (7)	0.0209 (6)	−0.0043 (6)	0.0074 (5)	−0.0027 (5)
C14B	0.0185 (7)	0.0191 (7)	0.0172 (5)	−0.0036 (5)	0.0043 (4)	−0.0012 (4)
C15B	0.0213 (7)	0.0201 (7)	0.0195 (6)	−0.0022 (6)	0.0079 (5)	−0.0031 (4)
C16B	0.0170 (7)	0.0187 (7)	0.0231 (6)	−0.0011 (5)	0.0017 (5)	0.0041 (4)
C17B	0.0177 (7)	0.0197 (7)	0.0179 (5)	0.0011 (5)	0.0037 (4)	0.0042 (4)
C18B	0.0181 (7)	0.0295 (8)	0.0202 (6)	−0.0028 (6)	0.0006 (5)	0.0034 (5)
C19B	0.0227 (8)	0.0231 (8)	0.0266 (6)	−0.0015 (6)	0.0054 (5)	0.0096 (5)
C20B	0.0288 (9)	0.0274 (9)	0.0270 (7)	0.0106 (7)	0.0077 (6)	0.0053 (5)
C21B	0.0250 (8)	0.0255 (8)	0.0145 (5)	−0.0047 (6)	0.0052 (5)	−0.0036 (4)
C22B	0.0414 (11)	0.0255 (9)	0.0246 (7)	0.0003 (8)	0.0111 (6)	−0.0065 (5)
C23B	0.0322 (9)	0.0405 (10)	0.0185 (6)	−0.0014 (8)	−0.0009 (6)	−0.0039 (5)
C24B	0.0340 (10)	0.0366 (10)	0.0233 (7)	−0.0108 (8)	0.0135 (6)	−0.0044 (6)
C25B	0.0194 (7)	0.0169 (7)	0.0169 (5)	−0.0045 (5)	0.0025 (4)	0.0019 (4)
C26B	0.0216 (7)	0.0194 (7)	0.0219 (6)	0.0005 (6)	0.0015 (5)	0.0044 (4)
C27B	0.0199 (7)	0.0206 (7)	0.0239 (6)	−0.0051 (6)	0.0041 (5)	0.0047 (5)
C28B	0.0238 (8)	0.0184 (7)	0.0196 (5)	−0.0035 (6)	0.0037 (5)	−0.0011 (4)
C29B	0.0282 (9)	0.0201 (7)	0.0231 (6)	−0.0043 (6)	0.0059 (5)	0.0055 (5)
C30B	0.0535 (14)	0.0439 (13)	0.0314 (8)	−0.0304 (12)	0.0002 (8)	0.0116 (7)
C31B	0.0386 (11)	0.0340 (10)	0.0282 (7)	0.0041 (8)	0.0025 (7)	0.0107 (6)
C32B	0.0496 (13)	0.0314 (10)	0.0371 (9)	0.0046 (9)	0.0272 (9)	0.0106 (7)
C33B	0.0361 (10)	0.0260 (9)	0.0247 (7)	−0.0124 (8)	0.0120 (6)	−0.0091 (6)
C34D	0.062 (2)	0.093 (3)	0.0362 (16)	−0.064 (2)	0.0237 (13)	−0.0363 (15)
C35D	0.076 (3)	0.0373 (18)	0.0465 (17)	0.0183 (15)	0.0283 (14)	−0.0052 (10)
C36D	0.0463 (17)	0.0378 (16)	0.0182 (13)	−0.0156 (10)	0.0082 (7)	−0.0065 (6)

Geometric parameters (Å, º)

C1—C16	1.535 (2)	C2B—H2B2	0.9900
C1—C9	1.5375 (19)	C3B—C4B	1.424 (2)
C1—C15	1.5444 (18)	C3B—C8B	1.4304 (18)
C1—C2	1.581 (2)	C4B—C5B	1.4087 (17)
C2—C3	1.5199 (16)	C4B—C17B	1.564 (2)
C2—H2A	0.9900	C5B—C6B	1.3990 (19)
C2—H2B	0.9900	C5B—H5B	0.9500
C3—C8	1.426 (2)	C6B—C7B	1.389 (2)
C3—C4	1.4360 (19)	C6B—C21B	1.5353 (18)
C4—C5	1.4010 (16)	C7B—C8B	1.4074 (17)
C4—C17	1.563 (2)	C7B—H7B	0.9500
C5—C6	1.395 (2)	C8B—C25B	1.560 (2)
C5—H5	0.9500	C9B—C10B	1.4000 (17)
C6—C7	1.393 (2)	C9B—C14B	1.4044 (17)
C6—C21	1.5368 (17)	C10B—C11B	1.401 (2)
C7—C8	1.4101 (17)	C10B—H10B	0.9500
C7—H7	0.9500	C11B—C12B	1.3993 (19)
C8—C25	1.569 (2)	C11B—C29B	1.5355 (19)
C9—C10	1.394 (2)	C12B—C13B	1.4045 (19)
C9—C14	1.4090 (16)	C12B—H12B	0.9500
C10—C11	1.4080 (19)	C13B—C14B	1.393 (2)
C10—H10	0.9500	C13B—C33B	1.532 (2)
C11—C12	1.3976 (17)	C14B—H14B	0.9500
C11—C29	1.533 (2)	C15B—H15D	0.9800
C12—C13	1.4019 (19)	C15B—H15E	0.9800
C12—H12	0.9500	C15B—H15F	0.9800
C13—C14	1.3982 (19)	C16B—H16D	0.9800
C13—C33	1.5340 (17)	C16B—H16E	0.9800
C14—H14	0.9500	C16B—H16F	0.9800
C15—H15A	0.9800	C17B—C19B	1.542 (2)
C15—H15B	0.9800	C17B—C20B	1.548 (2)
C15—H15C	0.9800	C17B—C18B	1.549 (2)
C16—H16A	0.9800	C18B—H18D	0.9800
C16—H16B	0.9800	C18B—H18E	0.9800
C16—H16C	0.9800	C18B—H18F	0.9800
C17—C19	1.5456 (19)	C19B—H19D	0.9800
C17—C20	1.547 (2)	C19B—H19E	0.9800
C17—C18	1.548 (2)	C19B—H19F	0.9800
C18—H18A	0.9800	C20B—H20D	0.9800
C18—H18B	0.9800	C20B—H20E	0.9800
C18—H18C	0.9800	C20B—H20F	0.9800
C19—H19A	0.9800	C21B—C22B	1.533 (3)
C19—H19B	0.9800	C21B—C23B	1.539 (3)
C19—H19C	0.9800	C21B—C24B	1.541 (2)
C20—H20A	0.9800	C22B—H22D	0.9800
C20—H20B	0.9800	C22B—H22E	0.9800
C20—H20C	0.9800	C22B—H22F	0.9800
C21—C22	1.537 (2)	C23B—H23D	0.9800
C21—C23	1.541 (2)	C23B—H23E	0.9800
C21—C24	1.547 (2)	C23B—H23F	0.9800
C22—H22A	0.9800	C24B—H24D	0.9800
C22—H22B	0.9800	C24B—H24E	0.9800
C22—H22C	0.9800	C24B—H24F	0.9800
C23—H23A	0.9800	C25B—C28B	1.5385 (19)
C23—H23B	0.9800	C25B—C26B	1.549 (2)
C23—H23C	0.9800	C25B—C27B	1.552 (2)
C24—H24A	0.9800	C26B—H26D	0.9800
C24—H24B	0.9800	C26B—H26E	0.9800
C24—H24C	0.9800	C26B—H26F	0.9800
C25—C28	1.5407 (18)	C27B—H27D	0.9800
C25—C26	1.541 (2)	C27B—H27E	0.9800
C25—C27	1.560 (2)	C27B—H27F	0.9800
C26—H26A	0.9800	C28B—H28D	0.9800
C26—H26B	0.9800	C28B—H28E	0.9800
C26—H26C	0.9800	C28B—H28F	0.9800
C27—H27A	0.9800	C29B—C30B	1.537 (3)
C27—H27B	0.9800	C29B—C31B	1.537 (3)
C27—H27C	0.9800	C29B—C32B	1.541 (3)
C28—H28A	0.9800	C30B—H30D	0.9800
C28—H28B	0.9800	C30B—H30E	0.9800
C28—H28C	0.9800	C30B—H30F	0.9800
C29—C30	1.534 (2)	C31B—H31D	0.9800
C29—C31	1.537 (3)	C31B—H31E	0.9800
C29—C32	1.538 (2)	C31B—H31F	0.9800
C30—H30A	0.9800	C32B—H32D	0.9800
C30—H30B	0.9800	C32B—H32E	0.9800
C30—H30C	0.9800	C32B—H32F	0.9800
C31—H31A	0.9800	C33B—C34D	1.520 (3)
C31—H31B	0.9800	C33B—C36D	1.527 (3)
C31—H31C	0.9800	C33B—C35B	1.54 (2)
C32—H32A	0.9800	C33B—C35D	1.552 (5)
C32—H32B	0.9800	C33B—C36B	1.59 (2)
C32—H32C	0.9800	C33B—C34B	1.61 (2)
C33—C36	1.531 (2)	C34D—H34J	0.9800
C33—C34	1.536 (2)	C34D—H34K	0.9800
C33—C35	1.545 (3)	C34D—H34L	0.9800
C34—H34A	0.9800	C35D—H35J	0.9800
C34—H34B	0.9800	C35D—H35K	0.9800
C34—H34C	0.9800	C35D—H35L	0.9800
C35—H35A	0.9800	C36D—H36J	0.9800
C35—H35B	0.9800	C36D—H36K	0.9800
C35—H35C	0.9800	C36D—H36L	0.9800
C36—H36A	0.9800	C34B—H34D	0.9800
C36—H36B	0.9800	C34B—H34E	0.9800
C36—H36C	0.9800	C34B—H34F	0.9800
C1B—C9B	1.532 (2)	C35B—H35D	0.9800
C1B—C16B	1.542 (2)	C35B—H35E	0.9800
C1B—C15B	1.5482 (19)	C35B—H35F	0.9800
C1B—C2B	1.580 (2)	C36B—H36D	0.9800
C2B—C3B	1.5266 (17)	C36B—H36E	0.9800
C2B—H2B1	0.9900	C36B—H36F	0.9800
C16—C1—C9	107.78 (12)	C4B—C3B—C8B	117.85 (12)
C16—C1—C15	107.51 (13)	C4B—C3B—C2B	119.79 (12)
C9—C1—C15	111.25 (12)	C8B—C3B—C2B	122.12 (14)
C16—C1—C2	112.38 (12)	C5B—C4B—C3B	118.98 (13)
C9—C1—C2	112.84 (12)	C5B—C4B—C17B	117.12 (14)
C15—C1—C2	104.98 (12)	C3B—C4B—C17B	123.56 (12)
C3—C2—C1	117.35 (11)	C6B—C5B—C4B	122.31 (15)
C3—C2—H2A	108.0	C6B—C5B—H5B	118.8
C1—C2—H2A	108.0	C4B—C5B—H5B	118.8
C3—C2—H2B	108.0	C7B—C6B—C5B	116.50 (13)
C1—C2—H2B	108.0	C7B—C6B—C21B	120.14 (14)
H2A—C2—H2B	107.2	C5B—C6B—C21B	123.10 (15)
C8—C3—C4	118.01 (12)	C6B—C7B—C8B	123.70 (14)
C8—C3—C2	122.24 (13)	C6B—C7B—H7B	118.1
C4—C3—C2	119.65 (12)	C8B—C7B—H7B	118.1
C5—C4—C3	118.81 (14)	C7B—C8B—C3B	117.81 (14)
C5—C4—C17	117.25 (14)	C7B—C8B—C25B	112.83 (12)
C3—C4—C17	123.25 (11)	C3B—C8B—C25B	128.91 (12)
C6—C5—C4	123.00 (14)	C10B—C9B—C14B	118.28 (13)
C6—C5—H5	118.5	C10B—C9B—C1B	122.19 (12)
C4—C5—H5	118.5	C14B—C9B—C1B	119.48 (12)
C7—C6—C5	116.69 (12)	C9B—C10B—C11B	121.92 (13)
C7—C6—C21	119.74 (14)	C9B—C10B—H10B	119.0
C5—C6—C21	123.24 (14)	C11B—C10B—H10B	119.0
C6—C7—C8	123.37 (14)	C12B—C11B—C10B	118.02 (14)
C6—C7—H7	118.3	C12B—C11B—C29B	120.73 (14)
C8—C7—H7	118.3	C10B—C11B—C29B	121.24 (13)
C7—C8—C3	118.23 (14)	C11B—C12B—C13B	121.71 (15)
C7—C8—C25	112.16 (13)	C11B—C12B—H12B	119.1
C3—C8—C25	129.23 (12)	C13B—C12B—H12B	119.1
C10—C9—C14	118.41 (13)	C14B—C13B—C12B	118.57 (14)
C10—C9—C1	122.33 (12)	C14B—C13B—C33B	121.97 (14)
C14—C9—C1	119.24 (13)	C12B—C13B—C33B	119.43 (15)
C9—C10—C11	121.80 (12)	C13B—C14B—C9B	121.49 (13)
C9—C10—H10	119.1	C13B—C14B—H14B	119.3
C11—C10—H10	119.1	C9B—C14B—H14B	119.3
C12—C11—C10	118.00 (13)	C1B—C15B—H15D	109.5
C12—C11—C29	122.59 (13)	C1B—C15B—H15E	109.5
C10—C11—C29	119.38 (12)	H15D—C15B—H15E	109.5
C11—C12—C13	121.99 (13)	C1B—C15B—H15F	109.5
C11—C12—H12	119.0	H15D—C15B—H15F	109.5
C13—C12—H12	119.0	H15E—C15B—H15F	109.5
C14—C13—C12	118.32 (12)	C1B—C16B—H16D	109.5
C14—C13—C33	121.83 (13)	C1B—C16B—H16E	109.5
C12—C13—C33	119.82 (13)	H16D—C16B—H16E	109.5
C13—C14—C9	121.46 (13)	C1B—C16B—H16F	109.5
C13—C14—H14	119.3	H16D—C16B—H16F	109.5
C9—C14—H14	119.3	H16E—C16B—H16F	109.5
C1—C15—H15A	109.5	C19B—C17B—C20B	106.18 (14)
C1—C15—H15B	109.5	C19B—C17B—C18B	110.47 (12)
H15A—C15—H15B	109.5	C20B—C17B—C18B	104.38 (14)
C1—C15—H15C	109.5	C19B—C17B—C4B	115.17 (13)
H15A—C15—H15C	109.5	C20B—C17B—C4B	110.65 (12)
H15B—C15—H15C	109.5	C18B—C17B—C4B	109.42 (13)
C1—C16—H16A	109.5	C17B—C18B—H18D	109.5
C1—C16—H16B	109.5	C17B—C18B—H18E	109.5
H16A—C16—H16B	109.5	H18D—C18B—H18E	109.5
C1—C16—H16C	109.5	C17B—C18B—H18F	109.5
H16A—C16—H16C	109.5	H18D—C18B—H18F	109.5
H16B—C16—H16C	109.5	H18E—C18B—H18F	109.5
C19—C17—C20	104.14 (12)	C17B—C19B—H19D	109.5
C19—C17—C18	110.56 (12)	C17B—C19B—H19E	109.5
C20—C17—C18	105.96 (14)	H19D—C19B—H19E	109.5
C19—C17—C4	116.71 (13)	C17B—C19B—H19F	109.5
C20—C17—C4	111.65 (11)	H19D—C19B—H19F	109.5
C18—C17—C4	107.35 (12)	H19E—C19B—H19F	109.5
C17—C18—H18A	109.5	C17B—C20B—H20D	109.5
C17—C18—H18B	109.5	C17B—C20B—H20E	109.5
H18A—C18—H18B	109.5	H20D—C20B—H20E	109.5
C17—C18—H18C	109.5	C17B—C20B—H20F	109.5
H18A—C18—H18C	109.5	H20D—C20B—H20F	109.5
H18B—C18—H18C	109.5	H20E—C20B—H20F	109.5
C17—C19—H19A	109.5	C22B—C21B—C6B	112.61 (14)
C17—C19—H19B	109.5	C22B—C21B—C23B	108.62 (15)
H19A—C19—H19B	109.5	C6B—C21B—C23B	109.66 (14)
C17—C19—H19C	109.5	C22B—C21B—C24B	107.63 (16)
H19A—C19—H19C	109.5	C6B—C21B—C24B	109.17 (13)
H19B—C19—H19C	109.5	C23B—C21B—C24B	109.06 (16)
C17—C20—H20A	109.5	C21B—C22B—H22D	109.5
C17—C20—H20B	109.5	C21B—C22B—H22E	109.5
H20A—C20—H20B	109.5	H22D—C22B—H22E	109.5
C17—C20—H20C	109.5	C21B—C22B—H22F	109.5
H20A—C20—H20C	109.5	H22D—C22B—H22F	109.5
H20B—C20—H20C	109.5	H22E—C22B—H22F	109.5
C22—C21—C6	112.09 (13)	C21B—C23B—H23D	109.5
C22—C21—C23	108.52 (13)	C21B—C23B—H23E	109.5
C6—C21—C23	110.35 (13)	H23D—C23B—H23E	109.5
C22—C21—C24	108.14 (14)	C21B—C23B—H23F	109.5
C6—C21—C24	108.72 (12)	H23D—C23B—H23F	109.5
C23—C21—C24	108.95 (14)	H23E—C23B—H23F	109.5
C21—C22—H22A	109.5	C21B—C24B—H24D	109.5
C21—C22—H22B	109.5	C21B—C24B—H24E	109.5
H22A—C22—H22B	109.5	H24D—C24B—H24E	109.5
C21—C22—H22C	109.5	C21B—C24B—H24F	109.5
H22A—C22—H22C	109.5	H24D—C24B—H24F	109.5
H22B—C22—H22C	109.5	H24E—C24B—H24F	109.5
C21—C23—H23A	109.5	C28B—C25B—C26B	107.11 (14)
C21—C23—H23B	109.5	C28B—C25B—C27B	104.48 (12)
H23A—C23—H23B	109.5	C26B—C25B—C27B	108.29 (12)
C21—C23—H23C	109.5	C28B—C25B—C8B	117.92 (12)
H23A—C23—H23C	109.5	C26B—C25B—C8B	112.20 (12)
H23B—C23—H23C	109.5	C27B—C25B—C8B	106.24 (13)
C21—C24—H24A	109.5	C25B—C26B—H26D	109.5
C21—C24—H24B	109.5	C25B—C26B—H26E	109.5
H24A—C24—H24B	109.5	H26D—C26B—H26E	109.5
C21—C24—H24C	109.5	C25B—C26B—H26F	109.5
H24A—C24—H24C	109.5	H26D—C26B—H26F	109.5
H24B—C24—H24C	109.5	H26E—C26B—H26F	109.5
C28—C25—C26	107.58 (14)	C25B—C27B—H27D	109.5
C28—C25—C27	104.29 (12)	C25B—C27B—H27E	109.5
C26—C25—C27	108.33 (13)	H27D—C27B—H27E	109.5
C28—C25—C8	118.54 (13)	C25B—C27B—H27F	109.5
C26—C25—C8	111.34 (12)	H27D—C27B—H27F	109.5
C27—C25—C8	106.15 (13)	H27E—C27B—H27F	109.5
C25—C26—H26A	109.5	C25B—C28B—H28D	109.5
C25—C26—H26B	109.5	C25B—C28B—H28E	109.5
H26A—C26—H26B	109.5	H28D—C28B—H28E	109.5
C25—C26—H26C	109.5	C25B—C28B—H28F	109.5
H26A—C26—H26C	109.5	H28D—C28B—H28F	109.5
H26B—C26—H26C	109.5	H28E—C28B—H28F	109.5
C25—C27—H27A	109.5	C11B—C29B—C30B	111.60 (13)
C25—C27—H27B	109.5	C11B—C29B—C31B	108.18 (15)
H27A—C27—H27B	109.5	C30B—C29B—C31B	109.17 (19)
C25—C27—H27C	109.5	C11B—C29B—C32B	111.24 (15)
H27A—C27—H27C	109.5	C30B—C29B—C32B	107.8 (2)
H27B—C27—H27C	109.5	C31B—C29B—C32B	108.76 (16)
C25—C28—H28A	109.5	C29B—C30B—H30D	109.5
C25—C28—H28B	109.5	C29B—C30B—H30E	109.5
H28A—C28—H28B	109.5	H30D—C30B—H30E	109.5
C25—C28—H28C	109.5	C29B—C30B—H30F	109.5
H28A—C28—H28C	109.5	H30D—C30B—H30F	109.5
H28B—C28—H28C	109.5	H30E—C30B—H30F	109.5
C11—C29—C30	112.43 (13)	C29B—C31B—H31D	109.5
C11—C29—C31	109.01 (14)	C29B—C31B—H31E	109.5
C30—C29—C31	108.90 (19)	H31D—C31B—H31E	109.5
C11—C29—C32	110.76 (14)	C29B—C31B—H31F	109.5
C30—C29—C32	106.91 (16)	H31D—C31B—H31F	109.5
C31—C29—C32	108.75 (16)	H31E—C31B—H31F	109.5
C29—C30—H30A	109.5	C29B—C32B—H32D	109.5
C29—C30—H30B	109.5	C29B—C32B—H32E	109.5
H30A—C30—H30B	109.5	H32D—C32B—H32E	109.5
C29—C30—H30C	109.5	C29B—C32B—H32F	109.5
H30A—C30—H30C	109.5	H32D—C32B—H32F	109.5
H30B—C30—H30C	109.5	H32E—C32B—H32F	109.5
C29—C31—H31A	109.5	C34D—C33B—C36D	109.2 (2)
C29—C31—H31B	109.5	C34D—C33B—C13B	110.88 (17)
H31A—C31—H31B	109.5	C36D—C33B—C13B	112.30 (15)
C29—C31—H31C	109.5	C13B—C33B—C35B	113.7 (15)
H31A—C31—H31C	109.5	C34D—C33B—C35D	109.1 (3)
H31B—C31—H31C	109.5	C36D—C33B—C35D	107.2 (2)
C29—C32—H32A	109.5	C13B—C33B—C35D	108.1 (2)
C29—C32—H32B	109.5	C13B—C33B—C36B	109.6 (12)
H32A—C32—H32B	109.5	C35B—C33B—C36B	111.6 (12)
C29—C32—H32C	109.5	C13B—C33B—C34B	103.7 (9)
H32A—C32—H32C	109.5	C35B—C33B—C34B	110.8 (11)
H32B—C32—H32C	109.5	C36B—C33B—C34B	107.0 (10)
C36—C33—C13	112.19 (13)	C33B—C34D—H34J	109.5
C36—C33—C34	108.16 (16)	C33B—C34D—H34K	109.5
C13—C33—C34	111.07 (12)	H34J—C34D—H34K	109.5
C36—C33—C35	108.12 (15)	C33B—C34D—H34L	109.5
C13—C33—C35	107.98 (14)	H34J—C34D—H34L	109.5
C34—C33—C35	109.25 (15)	H34K—C34D—H34L	109.5
C33—C34—H34A	109.5	C33B—C35D—H35J	109.5
C33—C34—H34B	109.5	C33B—C35D—H35K	109.5
H34A—C34—H34B	109.5	H35J—C35D—H35K	109.5
C33—C34—H34C	109.5	C33B—C35D—H35L	109.5
H34A—C34—H34C	109.5	H35J—C35D—H35L	109.5
H34B—C34—H34C	109.5	H35K—C35D—H35L	109.5
C33—C35—H35A	109.5	C33B—C36D—H36J	109.5
C33—C35—H35B	109.5	C33B—C36D—H36K	109.5
H35A—C35—H35B	109.5	H36J—C36D—H36K	109.5
C33—C35—H35C	109.5	C33B—C36D—H36L	109.5
H35A—C35—H35C	109.5	H36J—C36D—H36L	109.5
H35B—C35—H35C	109.5	H36K—C36D—H36L	109.5
C33—C36—H36A	109.5	C33B—C34B—H34D	109.5
C33—C36—H36B	109.5	C33B—C34B—H34E	109.5
H36A—C36—H36B	109.5	H34D—C34B—H34E	109.5
C33—C36—H36C	109.5	C33B—C34B—H34F	109.5
H36A—C36—H36C	109.5	H34D—C34B—H34F	109.5
H36B—C36—H36C	109.5	H34E—C34B—H34F	109.5
C9B—C1B—C16B	107.64 (12)	C33B—C35B—H35D	109.5
C9B—C1B—C15B	111.25 (12)	C33B—C35B—H35E	109.5
C16B—C1B—C15B	106.99 (13)	H35D—C35B—H35E	109.5
C9B—C1B—C2B	111.76 (13)	C33B—C35B—H35F	109.5
C16B—C1B—C2B	113.71 (11)	H35D—C35B—H35F	109.5
C15B—C1B—C2B	105.42 (11)	H35E—C35B—H35F	109.5
C3B—C2B—C1B	116.89 (11)	C33B—C36B—H36D	109.5
C3B—C2B—H2B1	108.1	C33B—C36B—H36E	109.5
C1B—C2B—H2B1	108.1	H36D—C36B—H36E	109.5
C3B—C2B—H2B2	108.1	C33B—C36B—H36F	109.5
C1B—C2B—H2B2	108.1	H36D—C36B—H36F	109.5
H2B1—C2B—H2B2	107.3	H36E—C36B—H36F	109.5
C16—C1—C2—C3	59.32 (17)	C1B—C2B—C3B—C4B	99.45 (16)
C9—C1—C2—C3	−62.81 (17)	C1B—C2B—C3B—C8B	−74.78 (17)
C15—C1—C2—C3	175.88 (13)	C8B—C3B—C4B—C5B	17.4 (2)
C1—C2—C3—C8	−81.12 (18)	C2B—C3B—C4B—C5B	−157.08 (14)
C1—C2—C3—C4	95.15 (17)	C8B—C3B—C4B—C17B	−155.73 (14)
C8—C3—C4—C5	14.1 (2)	C2B—C3B—C4B—C17B	29.8 (2)
C2—C3—C4—C5	−162.37 (14)	C3B—C4B—C5B—C6B	−4.8 (2)
C8—C3—C4—C17	−156.08 (14)	C17B—C4B—C5B—C6B	168.75 (14)
C2—C3—C4—C17	27.5 (2)	C4B—C5B—C6B—C7B	−7.9 (2)
C3—C4—C5—C6	−3.5 (2)	C4B—C5B—C6B—C21B	177.88 (15)
C17—C4—C5—C6	167.20 (14)	C5B—C6B—C7B—C8B	8.2 (2)
C4—C5—C6—C7	−5.7 (2)	C21B—C6B—C7B—C8B	−177.44 (15)
C4—C5—C6—C21	−179.08 (15)	C6B—C7B—C8B—C3B	4.3 (2)
C5—C6—C7—C8	4.4 (2)	C6B—C7B—C8B—C25B	−168.74 (15)
C21—C6—C7—C8	178.01 (15)	C4B—C3B—C8B—C7B	−17.1 (2)
C6—C7—C8—C3	6.1 (2)	C2B—C3B—C8B—C7B	157.28 (14)
C6—C7—C8—C25	−167.48 (15)	C4B—C3B—C8B—C25B	154.69 (15)
C4—C3—C8—C7	−15.2 (2)	C2B—C3B—C8B—C25B	−31.0 (2)
C2—C3—C8—C7	161.12 (14)	C16B—C1B—C9B—C10B	129.99 (16)
C4—C3—C8—C25	157.14 (15)	C15B—C1B—C9B—C10B	13.1 (2)
C2—C3—C8—C25	−26.5 (2)	C2B—C1B—C9B—C10B	−104.47 (16)
C16—C1—C9—C10	129.37 (16)	C16B—C1B—C9B—C14B	−47.43 (19)
C15—C1—C9—C10	11.7 (2)	C15B—C1B—C9B—C14B	−164.34 (15)
C2—C1—C9—C10	−105.95 (17)	C2B—C1B—C9B—C14B	78.12 (17)
C16—C1—C9—C14	−48.78 (18)	C14B—C9B—C10B—C11B	0.9 (2)
C15—C1—C9—C14	−166.42 (15)	C1B—C9B—C10B—C11B	−176.57 (16)
C2—C1—C9—C14	75.90 (18)	C9B—C10B—C11B—C12B	−0.8 (3)
C14—C9—C10—C11	−0.2 (2)	C9B—C10B—C11B—C29B	−179.61 (16)
C1—C9—C10—C11	−178.41 (15)	C10B—C11B—C12B—C13B	0.5 (3)
C9—C10—C11—C12	0.1 (2)	C29B—C11B—C12B—C13B	179.38 (18)
C9—C10—C11—C29	−178.27 (16)	C11B—C12B—C13B—C14B	−0.4 (3)
C10—C11—C12—C13	0.5 (3)	C11B—C12B—C13B—C33B	−178.73 (19)
C29—C11—C12—C13	178.77 (16)	C12B—C13B—C14B—C9B	0.5 (3)
C11—C12—C13—C14	−0.8 (3)	C33B—C13B—C14B—C9B	178.78 (18)
C11—C12—C13—C33	−178.99 (16)	C10B—C9B—C14B—C13B	−0.7 (3)
C12—C13—C14—C9	0.7 (2)	C1B—C9B—C14B—C13B	176.80 (16)
C33—C13—C14—C9	178.80 (16)	C5B—C4B—C17B—C19B	107.51 (16)
C10—C9—C14—C13	−0.2 (2)	C3B—C4B—C17B—C19B	−79.25 (19)
C1—C9—C14—C13	178.07 (15)	C5B—C4B—C17B—C20B	−12.9 (2)
C5—C4—C17—C19	119.71 (15)	C3B—C4B—C17B—C20B	160.35 (15)
C3—C4—C17—C19	−70.01 (18)	C5B—C4B—C17B—C18B	−127.37 (15)
C5—C4—C17—C20	0.10 (19)	C3B—C4B—C17B—C18B	45.87 (19)
C3—C4—C17—C20	170.38 (14)	C7B—C6B—C21B—C22B	174.15 (16)
C5—C4—C17—C18	−115.61 (15)	C5B—C6B—C21B—C22B	−11.9 (2)
C3—C4—C17—C18	54.67 (18)	C7B—C6B—C21B—C23B	53.1 (2)
C7—C6—C21—C22	176.41 (15)	C5B—C6B—C21B—C23B	−132.95 (18)
C5—C6—C21—C22	−10.4 (2)	C7B—C6B—C21B—C24B	−66.4 (2)
C7—C6—C21—C23	55.33 (19)	C5B—C6B—C21B—C24B	107.61 (19)
C5—C6—C21—C23	−131.49 (16)	C7B—C8B—C25B—C28B	176.02 (14)
C7—C6—C21—C24	−64.1 (2)	C3B—C8B—C25B—C28B	3.9 (2)
C5—C6—C21—C24	109.07 (18)	C7B—C8B—C25B—C26B	−58.82 (17)
C7—C8—C25—C28	171.39 (15)	C3B—C8B—C25B—C26B	129.10 (16)
C3—C8—C25—C28	−1.3 (2)	C7B—C8B—C25B—C27B	59.34 (16)
C7—C8—C25—C26	−63.05 (17)	C3B—C8B—C25B—C27B	−112.74 (16)
C3—C8—C25—C26	124.22 (17)	C12B—C11B—C29B—C30B	29.3 (3)
C7—C8—C25—C27	54.64 (17)	C10B—C11B—C29B—C30B	−151.9 (2)
C3—C8—C25—C27	−118.09 (17)	C12B—C11B—C29B—C31B	−90.8 (2)
C12—C11—C29—C30	13.7 (3)	C10B—C11B—C29B—C31B	88.0 (2)
C10—C11—C29—C30	−168.04 (18)	C12B—C11B—C29B—C32B	149.8 (2)
C12—C11—C29—C31	−107.2 (2)	C10B—C11B—C29B—C32B	−31.4 (3)
C10—C11—C29—C31	71.1 (2)	C14B—C13B—C33B—C34D	129.8 (3)
C12—C11—C29—C32	133.20 (18)	C12B—C13B—C33B—C34D	−52.0 (3)
C10—C11—C29—C32	−48.5 (2)	C14B—C13B—C33B—C36D	7.3 (3)
C14—C13—C33—C36	13.0 (2)	C12B—C13B—C33B—C36D	−174.4 (2)
C12—C13—C33—C36	−168.91 (17)	C14B—C13B—C33B—C35B	−62.5 (12)
C14—C13—C33—C34	134.19 (18)	C12B—C13B—C33B—C35B	115.8 (12)
C12—C13—C33—C34	−47.7 (2)	C14B—C13B—C33B—C35D	−110.7 (3)
C14—C13—C33—C35	−106.04 (18)	C12B—C13B—C33B—C35D	67.6 (3)
C12—C13—C33—C35	72.04 (19)	C14B—C13B—C33B—C36B	171.8 (11)
C9B—C1B—C2B—C3B	−72.04 (15)	C12B—C13B—C33B—C36B	−9.9 (11)
C16B—C1B—C2B—C3B	50.08 (18)	C14B—C13B—C33B—C34B	57.9 (9)
C15B—C1B—C2B—C3B	166.97 (13)	C12B—C13B—C33B—C34B	−123.9 (9)

1-(2,4,6-Tri-tert-butylphenyl)-2-(3,5-di-tert-butylphenyl)- 2-methylpropane (IIIb)

Crystal data

C36H58	Z = 4
Mr = 490.82	F(000) = 1096
Triclinic, P1	Dx = 1.005 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71070 Å
a = 15.850 (4) Å	Cell parameters from 23 reflections
b = 19.464 (5) Å	θ = 8.4–21.2°
c = 10.596 (3) Å	µ = 0.06 mm^−1
α = 95.112 (11)°	T = 145 K
β = 95.102 (11)°	Parallelepiped, colorless
γ = 90.084 (9)°	0.60 × 0.34 × 0.23 mm
V = 3243.0 (15) Å^3

Data collection

Modified Picker FACS1 diffractometer	Rint = 0.0000
Radiation source: fine-focus sealed tube	θmax = 27.0°, θmin = 1.1°
Graphite monochromator	h = −20→20
θ/2θ scans	k = −24→24
8738 measured reflections	l = 0→13
8593 independent reflections	3 standard reflections every 97 reflections
4272 reflections with I > 2σ(I)	intensity decay: 2.0%

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)] = 0.086	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.258	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.099P)^2 + 3.3833P] where P = (Fo^2 + 2Fc^2)/3
8593 reflections	(Δ/σ)max = 0.001
652 parameters	Δρmax = 0.35 e Å^−3
18 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. Total number of reflections listed, 8593, is number greater than 0; a room temperature structure had been reported (J. Org. Chem. 56, 466–469,(1991)) with the unit cell used in the present study. The final model includes a threefold disorder at the tert-butyl group C33B(C34B—C35B—C36B). Distances and angles within the group were constrained. Standard uncertainties for distances and angles in the disordered group have been deleted.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.4183 (3)	0.7266 (3)	0.1407 (5)	0.0246 (13)
C2	0.5167 (3)	0.7412 (3)	0.1690 (5)	0.0251 (13)
H2A	0.5469	0.6985	0.1429	0.030*
H2B	0.5326	0.7768	0.1143	0.030*
C3	0.5495 (3)	0.7648 (3)	0.3067 (5)	0.0231 (13)
C4	0.5825 (3)	0.7152 (3)	0.3891 (5)	0.0226 (12)
C5	0.5891 (4)	0.7321 (3)	0.5205 (5)	0.0253 (13)
H5	0.6075	0.6978	0.5750	0.030*
C6	0.5692 (3)	0.7986 (3)	0.5753 (5)	0.0247 (13)
C7	0.5496 (4)	0.8474 (3)	0.4926 (5)	0.0268 (13)
H7	0.5396	0.8930	0.5275	0.032*
C8	0.5432 (3)	0.8347 (3)	0.3591 (5)	0.0237 (13)
C9	0.3874 (4)	0.6677 (3)	0.2094 (5)	0.0270 (13)
C10	0.3658 (3)	0.6032 (3)	0.1478 (5)	0.0273 (13)
H10	0.3726	0.5954	0.0595	0.033*
C11	0.3348 (3)	0.5496 (3)	0.2091 (5)	0.0244 (13)
C12	0.3254 (4)	0.5619 (3)	0.3393 (5)	0.0264 (13)
H12	0.3050	0.5258	0.3834	0.032*
C13	0.3455 (3)	0.6264 (3)	0.4065 (5)	0.0255 (13)
C14	0.3763 (3)	0.6776 (3)	0.3392 (5)	0.0231 (12)
H14	0.3905	0.7214	0.3833	0.028*
C15	0.4057 (4)	0.7115 (3)	−0.0052 (6)	0.0382 (16)
H15A	0.4263	0.7509	−0.0457	0.057*
H15B	0.3453	0.7039	−0.0316	0.057*
H15C	0.4373	0.6702	−0.0310	0.057*
C16	0.3656 (4)	0.7913 (3)	0.1748 (6)	0.0298 (14)
H16A	0.3848	0.8298	0.1307	0.045*
H16B	0.3729	0.8034	0.2669	0.045*
H16C	0.3056	0.7815	0.1484	0.045*
C17	0.6228 (4)	0.6462 (3)	0.3404 (6)	0.0305 (14)
C18	0.6944 (4)	0.6650 (3)	0.2593 (6)	0.0319 (14)
H18A	0.7212	0.6227	0.2258	0.048*
H18B	0.7367	0.6940	0.3123	0.048*
H18C	0.6706	0.6901	0.1885	0.048*
C19	0.5634 (4)	0.5910 (3)	0.2649 (6)	0.0297 (14)
H19A	0.5963	0.5503	0.2399	0.045*
H19B	0.5366	0.6098	0.1886	0.045*
H19C	0.5196	0.5780	0.3182	0.045*
C20	0.6660 (4)	0.6083 (3)	0.4511 (6)	0.0332 (15)
H20A	0.6898	0.5649	0.4169	0.050*
H20B	0.6241	0.5987	0.5100	0.050*
H20C	0.7114	0.6375	0.4964	0.050*
C21	0.5775 (4)	0.8173 (3)	0.7203 (5)	0.0290 (14)
C22	0.5939 (4)	0.7538 (3)	0.7964 (5)	0.0361 (15)
H22A	0.6455	0.7308	0.7712	0.054*
H22B	0.5458	0.7217	0.7787	0.054*
H22C	0.6009	0.7687	0.8875	0.054*
C23	0.4964 (4)	0.8520 (3)	0.7612 (6)	0.0360 (15)
H23A	0.5023	0.8638	0.8534	0.054*
H23B	0.4482	0.8204	0.7384	0.054*
H23C	0.4869	0.8941	0.7178	0.054*
C24	0.6531 (4)	0.8677 (3)	0.7544 (6)	0.0379 (16)
H24A	0.7050	0.8457	0.7277	0.057*
H24B	0.6594	0.8798	0.8465	0.057*
H24C	0.6428	0.9095	0.7105	0.057*
C25	0.5407 (4)	0.9023 (3)	0.2908 (6)	0.0279 (13)
C26	0.4620 (4)	0.9456 (3)	0.3185 (6)	0.0355 (15)
H26A	0.4625	0.9876	0.2741	0.053*
H26B	0.4627	0.9581	0.4103	0.053*
H26C	0.4106	0.9186	0.2888	0.053*
C27	0.6207 (4)	0.9452 (3)	0.3459 (6)	0.0342 (15)
H27A	0.6218	0.9885	0.3053	0.051*
H27B	0.6717	0.9188	0.3291	0.051*
H27C	0.6190	0.9555	0.4379	0.051*
C28	0.5463 (4)	0.8973 (3)	0.1443 (5)	0.0331 (15)
H28A	0.5440	0.9436	0.1151	0.050*
H28B	0.4988	0.8695	0.1016	0.050*
H28C	0.5998	0.8755	0.1241	0.050*
C29	0.3150 (4)	0.4782 (3)	0.1371 (6)	0.0304 (14)
C30	0.2631 (5)	0.4318 (3)	0.2093 (7)	0.059 (2)
H30A	0.2526	0.3874	0.1591	0.088*
H30B	0.2089	0.4538	0.2246	0.088*
H30C	0.2943	0.4243	0.2909	0.088*
C31	0.3991 (4)	0.4430 (3)	0.1101 (8)	0.058 (2)
H31A	0.3875	0.3975	0.0645	0.087*
H31B	0.4329	0.4378	0.1907	0.087*
H31C	0.4306	0.4713	0.0580	0.087*
C32	0.2632 (5)	0.4874 (3)	0.0098 (6)	0.0497 (19)
H32A	0.2505	0.4421	−0.0360	0.075*
H32B	0.2960	0.5151	−0.0417	0.075*
H32C	0.2102	0.5110	0.0263	0.075*
C33	0.3343 (4)	0.6371 (3)	0.5494 (5)	0.0279 (14)
C34	0.2491 (4)	0.6094 (4)	0.5795 (6)	0.049 (2)
H34A	0.2443	0.6168	0.6713	0.074*
H34B	0.2448	0.5600	0.5525	0.074*
H34C	0.2034	0.6338	0.5341	0.074*
C35	0.4059 (5)	0.5981 (4)	0.6191 (6)	0.0479 (19)
H35A	0.4006	0.6039	0.7108	0.072*
H35B	0.4608	0.6166	0.6015	0.072*
H35C	0.4020	0.5490	0.5893	0.072*
C36	0.3422 (5)	0.7131 (3)	0.5996 (6)	0.053 (2)
H36A	0.3351	0.7178	0.6908	0.079*
H36B	0.2984	0.7395	0.5545	0.079*
H36C	0.3983	0.7306	0.5855	0.079*
C1B	1.1001 (4)	0.6924 (3)	0.0819 (5)	0.0242 (13)
C2B	1.0011 (3)	0.6806 (3)	0.0738 (5)	0.0216 (12)
H2B1	0.9746	0.7108	0.0114	0.026*
H2B2	0.9890	0.6323	0.0391	0.026*
C3B	0.9571 (3)	0.6935 (3)	0.1971 (5)	0.0212 (12)
C4B	0.9144 (3)	0.7569 (3)	0.2220 (5)	0.0244 (13)
C5B	0.9029 (3)	0.7801 (3)	0.3500 (5)	0.0237 (13)
H5B	0.8791	0.8242	0.3683	0.028*
C6B	0.9252 (4)	0.7402 (3)	0.4485 (5)	0.0263 (13)
C7B	0.9506 (3)	0.6723 (3)	0.4173 (5)	0.0273 (13)
H7B	0.9587	0.6422	0.4831	0.033*
C8B	0.9647 (3)	0.6470 (3)	0.2931 (5)	0.0246 (13)
C9B	1.1234 (3)	0.7695 (3)	0.1016 (5)	0.0237 (13)
C10B	1.1492 (3)	0.8060 (3)	0.0038 (5)	0.0257 (13)
H10B	1.1492	0.7830	−0.0792	0.031*
C11B	1.1752 (4)	0.8755 (3)	0.0235 (5)	0.0280 (14)
C12B	1.1734 (4)	0.9073 (3)	0.1470 (6)	0.0309 (14)
H12B	1.1908	0.9542	0.1631	0.037*
C13B	1.1474 (4)	0.8737 (3)	0.2470 (5)	0.0288 (14)
C14B	1.1220 (3)	0.8048 (3)	0.2227 (5)	0.0259 (13)
H14B	1.1033	0.7811	0.2899	0.031*
C15B	1.1282 (4)	0.6597 (3)	−0.0455 (5)	0.0308 (14)
H15D	1.0977	0.6814	−0.1159	0.046*
H15E	1.1153	0.6101	−0.0540	0.046*
H15F	1.1892	0.6668	−0.0475	0.046*
C16B	1.1488 (4)	0.6572 (3)	0.1885 (5)	0.0298 (14)
H16D	1.1353	0.6077	0.1786	0.045*
H16E	1.1325	0.6773	0.2708	0.045*
H16F	1.2097	0.6639	0.1844	0.045*
C17B	0.8705 (4)	0.7992 (3)	0.1157 (6)	0.0304 (14)
C18B	0.8179 (4)	0.7502 (3)	0.0173 (5)	0.0309 (14)
H18D	0.7908	0.7766	−0.0494	0.046*
H18E	0.7744	0.7273	0.0592	0.046*
H18F	0.8551	0.7155	−0.0206	0.046*
C19B	0.9320 (4)	0.8434 (3)	0.0486 (6)	0.0343 (15)
H19D	0.9649	0.8745	0.1124	0.051*
H19E	0.8992	0.8706	−0.0118	0.051*
H19F	0.9705	0.8130	0.0029	0.051*
C20B	0.8054 (4)	0.8502 (3)	0.1709 (6)	0.0347 (15)
H20D	0.8348	0.8837	0.2344	0.052*
H20E	0.7633	0.8247	0.2110	0.052*
H20F	0.7770	0.8745	0.1021	0.052*
C21B	0.9155 (4)	0.7652 (3)	0.5899 (6)	0.0343 (15)
C22B	0.8954 (5)	0.8424 (3)	0.6085 (7)	0.0491 (19)
H22D	0.8428	0.8518	0.5572	0.074*
H22E	0.9419	0.8693	0.5817	0.074*
H22F	0.8886	0.8555	0.6985	0.074*
C23B	0.9985 (4)	0.7517 (4)	0.6708 (6)	0.0471 (18)
H23D	1.0115	0.7025	0.6611	0.071*
H23E	0.9920	0.7660	0.7605	0.071*
H23F	1.0447	0.7782	0.6424	0.071*
C24B	0.8431 (5)	0.7245 (4)	0.6380 (6)	0.051 (2)
H24D	0.8549	0.6750	0.6272	0.077*
H24E	0.7896	0.7339	0.5892	0.077*
H24F	0.8388	0.7387	0.7283	0.077*
C25B	0.9754 (4)	0.5671 (3)	0.2804 (5)	0.0278 (13)
C26B	1.0494 (4)	0.5430 (3)	0.3681 (6)	0.0320 (14)
H26D	1.1026	0.5622	0.3450	0.048*
H26E	1.0518	0.4925	0.3587	0.048*
H26F	1.0413	0.5589	0.4565	0.048*
C27B	0.8923 (4)	0.5357 (3)	0.3196 (6)	0.0344 (15)
H27D	0.8439	0.5507	0.2650	0.052*
H27E	0.8852	0.5513	0.4085	0.052*
H27F	0.8954	0.4852	0.3100	0.052*
C28B	0.9840 (4)	0.5310 (3)	0.1466 (5)	0.0311 (14)
H28D	0.9375	0.5451	0.0875	0.047*
H28E	0.9818	0.4809	0.1500	0.047*
H28F	1.0382	0.5441	0.1173	0.047*
C29B	1.2024 (4)	0.9150 (3)	−0.0838 (6)	0.0347 (15)
C30B	1.2659 (5)	0.9738 (4)	−0.0356 (7)	0.067 (3)
H30D	1.2814	0.9978	−0.1078	0.100*
H30E	1.3167	0.9544	0.0067	0.100*
H30F	1.2397	1.0064	0.0247	0.100*
C31B	1.1237 (5)	0.9449 (4)	−0.1521 (6)	0.0490 (19)
H31D	1.1405	0.9707	−0.2213	0.074*
H31E	1.0953	0.9759	−0.0917	0.074*
H31F	1.0850	0.9073	−0.1871	0.074*
C32B	1.2455 (5)	0.8664 (4)	−0.1818 (7)	0.053 (2)
H32D	1.2626	0.8928	−0.2500	0.079*
H32E	1.2056	0.8298	−0.2179	0.079*
H32F	1.2956	0.8458	−0.1396	0.079*
C33B	1.1448 (4)	0.9127 (3)	0.3809 (6)	0.0411 (17)
C34B	1.2176 (8)	0.9621 (8)	0.4130 (17)	0.048 (3)*	0.46
H34D	1.2240	0.9892	0.3408	0.072*	0.46
H34E	1.2696	0.9363	0.4315	0.072*	0.46
H34F	1.2068	0.9931	0.4877	0.072*	0.46
C35B	1.0618 (8)	0.9580 (8)	0.3690 (18)	0.048 (3)*	0.46
H35D	1.0671	0.9907	0.3047	0.072*	0.46
H35E	1.0545	0.9836	0.4512	0.072*	0.46
H35F	1.0125	0.9279	0.3436	0.072*	0.46
C36B	1.1353 (11)	0.8643 (8)	0.4840 (17)	0.048 (3)*	0.46
H36D	1.0852	0.8348	0.4606	0.072*	0.46
H36E	1.1289	0.8915	0.5649	0.072*	0.46
H36F	1.1858	0.8356	0.4928	0.072*	0.46
C34D	1.2353 (8)	0.9364 (9)	0.4314 (18)	0.041 (3)*	0.39
H34J	1.2579	0.9661	0.3722	0.061*	0.39
H34K	1.2716	0.8960	0.4392	0.061*	0.39
H34L	1.2341	0.9622	0.5150	0.061*	0.39
C35D	1.0867 (10)	0.9755 (8)	0.3726 (19)	0.041 (3)*	0.39
H35J	1.1063	1.0052	0.3109	0.061*	0.39
H35K	1.0881	1.0016	0.4563	0.061*	0.39
H35L	1.0286	0.9599	0.3453	0.061*	0.39
C36D	1.1113 (11)	0.8680 (9)	0.4742 (19)	0.041 (3)*	0.39
H36J	1.1478	0.8278	0.4824	0.061*	0.39
H36K	1.0536	0.8527	0.4437	0.061*	0.39
H36L	1.1108	0.8945	0.5572	0.061*	0.39
C34C	1.203 (2)	0.8701 (17)	0.471 (3)	0.042 (7)*	0.15
H34G	1.2563	0.8604	0.4342	0.062*	0.15
H34H	1.1742	0.8265	0.4818	0.062*	0.15
H34I	1.2137	0.8965	0.5541	0.062*	0.15
C36C	1.0601 (13)	0.9212 (19)	0.428 (4)	0.042 (7)*	0.15
H36G	1.0656	0.9452	0.5133	0.062*	0.15
H36H	1.0339	0.8757	0.4303	0.062*	0.15
H36I	1.0245	0.9483	0.3704	0.062*	0.15
C35C	1.191 (2)	0.9826 (13)	0.379 (4)	0.042 (7)*	0.15
H35G	1.2516	0.9746	0.3731	0.062*	0.15
H35H	1.1831	1.0115	0.4578	0.062*	0.15
H35I	1.1677	1.0059	0.3059	0.062*	0.15

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.024 (3)	0.025 (3)	0.026 (3)	−0.004 (2)	0.008 (2)	0.005 (2)
C2	0.028 (3)	0.025 (3)	0.023 (3)	−0.001 (2)	0.009 (2)	−0.001 (2)
C3	0.016 (3)	0.029 (3)	0.023 (3)	−0.005 (2)	0.006 (2)	−0.006 (2)
C4	0.023 (3)	0.022 (3)	0.023 (3)	−0.002 (2)	0.005 (2)	0.000 (2)
C5	0.033 (3)	0.022 (3)	0.021 (3)	−0.002 (2)	0.006 (3)	0.001 (2)
C6	0.021 (3)	0.030 (3)	0.023 (3)	0.001 (2)	0.005 (2)	−0.001 (3)
C7	0.030 (3)	0.027 (3)	0.023 (3)	−0.001 (3)	0.006 (3)	−0.004 (3)
C8	0.021 (3)	0.023 (3)	0.027 (3)	0.001 (2)	0.003 (2)	0.003 (2)
C9	0.027 (3)	0.027 (3)	0.027 (3)	−0.001 (3)	0.003 (3)	0.001 (3)
C10	0.026 (3)	0.037 (4)	0.019 (3)	−0.001 (3)	0.002 (2)	−0.002 (3)
C11	0.021 (3)	0.019 (3)	0.032 (3)	0.001 (2)	0.002 (2)	−0.004 (2)
C12	0.033 (3)	0.017 (3)	0.029 (3)	−0.001 (2)	0.002 (3)	0.001 (2)
C13	0.020 (3)	0.031 (3)	0.026 (3)	0.000 (2)	0.008 (2)	0.001 (3)
C14	0.015 (3)	0.025 (3)	0.028 (3)	−0.001 (2)	−0.001 (2)	−0.001 (2)
C15	0.034 (4)	0.046 (4)	0.036 (4)	−0.011 (3)	0.003 (3)	0.009 (3)
C16	0.028 (3)	0.028 (3)	0.034 (4)	0.002 (3)	0.003 (3)	0.007 (3)
C17	0.027 (3)	0.031 (3)	0.033 (4)	0.001 (3)	0.008 (3)	−0.002 (3)
C18	0.027 (3)	0.025 (3)	0.042 (4)	−0.001 (3)	0.002 (3)	−0.007 (3)
C19	0.030 (3)	0.024 (3)	0.034 (4)	0.003 (3)	0.002 (3)	−0.003 (3)
C20	0.034 (4)	0.022 (3)	0.042 (4)	0.005 (3)	0.004 (3)	−0.006 (3)
C21	0.033 (3)	0.034 (4)	0.022 (3)	−0.004 (3)	0.011 (3)	0.002 (3)
C22	0.051 (4)	0.035 (4)	0.022 (3)	−0.002 (3)	0.008 (3)	−0.002 (3)
C23	0.048 (4)	0.038 (4)	0.022 (3)	−0.003 (3)	0.012 (3)	−0.004 (3)
C24	0.043 (4)	0.045 (4)	0.025 (4)	−0.010 (3)	0.004 (3)	−0.004 (3)
C25	0.028 (3)	0.025 (3)	0.032 (3)	0.006 (3)	0.009 (3)	0.001 (3)
C26	0.043 (4)	0.027 (3)	0.038 (4)	0.003 (3)	0.003 (3)	0.007 (3)
C27	0.039 (4)	0.033 (4)	0.032 (4)	−0.011 (3)	0.010 (3)	0.001 (3)
C28	0.041 (4)	0.030 (3)	0.029 (3)	−0.004 (3)	0.011 (3)	0.000 (3)
C29	0.043 (4)	0.020 (3)	0.027 (3)	−0.002 (3)	0.003 (3)	−0.004 (3)
C30	0.091 (6)	0.036 (4)	0.048 (5)	−0.031 (4)	0.021 (4)	−0.018 (3)
C31	0.051 (5)	0.032 (4)	0.086 (6)	0.015 (3)	0.003 (4)	−0.016 (4)
C32	0.068 (5)	0.032 (4)	0.043 (4)	0.005 (3)	−0.019 (4)	−0.005 (3)
C33	0.035 (3)	0.023 (3)	0.026 (3)	−0.007 (3)	0.008 (3)	0.002 (3)
C34	0.045 (4)	0.062 (5)	0.038 (4)	−0.029 (4)	0.014 (3)	−0.014 (3)
C35	0.069 (5)	0.046 (4)	0.030 (4)	−0.001 (4)	0.008 (4)	0.003 (3)
C36	0.082 (6)	0.041 (4)	0.038 (4)	−0.013 (4)	0.028 (4)	−0.008 (3)
C1B	0.030 (3)	0.021 (3)	0.021 (3)	−0.003 (2)	0.009 (2)	−0.003 (2)
C2B	0.023 (3)	0.024 (3)	0.018 (3)	0.000 (2)	0.004 (2)	−0.001 (2)
C3B	0.020 (3)	0.024 (3)	0.019 (3)	0.001 (2)	0.004 (2)	0.000 (2)
C4B	0.020 (3)	0.032 (3)	0.023 (3)	−0.004 (2)	0.000 (2)	0.008 (3)
C5B	0.025 (3)	0.018 (3)	0.027 (3)	−0.003 (2)	0.005 (2)	−0.002 (2)
C6B	0.028 (3)	0.028 (3)	0.023 (3)	−0.009 (3)	0.003 (2)	0.002 (3)
C7B	0.022 (3)	0.033 (3)	0.028 (3)	0.002 (3)	0.004 (2)	0.008 (3)
C8B	0.027 (3)	0.026 (3)	0.021 (3)	−0.002 (2)	0.002 (2)	−0.001 (2)
C9B	0.023 (3)	0.020 (3)	0.029 (3)	0.000 (2)	0.005 (2)	0.002 (2)
C10B	0.025 (3)	0.028 (3)	0.023 (3)	0.001 (2)	0.002 (2)	−0.002 (2)
C11B	0.036 (4)	0.027 (3)	0.020 (3)	0.003 (3)	0.002 (3)	0.001 (3)
C12B	0.036 (4)	0.019 (3)	0.038 (4)	−0.006 (3)	0.010 (3)	−0.001 (3)
C13B	0.029 (3)	0.030 (3)	0.028 (3)	−0.003 (3)	0.010 (3)	−0.003 (3)
C14B	0.027 (3)	0.026 (3)	0.026 (3)	−0.003 (2)	0.005 (2)	0.004 (3)
C15B	0.038 (4)	0.028 (3)	0.028 (3)	−0.003 (3)	0.014 (3)	0.002 (3)
C16B	0.029 (3)	0.030 (3)	0.030 (3)	−0.004 (3)	0.002 (3)	−0.001 (3)
C17B	0.029 (3)	0.034 (4)	0.030 (3)	0.001 (3)	0.006 (3)	0.008 (3)
C18B	0.025 (3)	0.042 (4)	0.026 (3)	−0.001 (3)	0.004 (3)	0.010 (3)
C19B	0.036 (4)	0.038 (4)	0.029 (4)	0.003 (3)	0.001 (3)	0.006 (3)
C20B	0.036 (4)	0.032 (4)	0.039 (4)	0.016 (3)	0.010 (3)	0.009 (3)
C21B	0.043 (4)	0.038 (4)	0.022 (3)	0.001 (3)	0.010 (3)	−0.001 (3)
C22B	0.068 (5)	0.037 (4)	0.041 (4)	−0.005 (4)	0.017 (4)	−0.011 (3)
C23B	0.052 (5)	0.060 (5)	0.025 (4)	0.004 (4)	−0.002 (3)	−0.015 (3)
C24B	0.070 (5)	0.055 (5)	0.029 (4)	−0.009 (4)	0.019 (4)	−0.007 (3)
C25B	0.033 (3)	0.023 (3)	0.028 (3)	−0.002 (3)	0.004 (3)	0.002 (3)
C26B	0.027 (3)	0.034 (4)	0.033 (4)	−0.005 (3)	0.005 (3)	−0.005 (3)
C27B	0.033 (4)	0.032 (3)	0.040 (4)	−0.008 (3)	0.006 (3)	0.009 (3)
C28B	0.036 (4)	0.024 (3)	0.032 (3)	−0.007 (3)	0.003 (3)	−0.006 (3)
C29B	0.045 (4)	0.031 (4)	0.029 (4)	0.002 (3)	0.006 (3)	0.007 (3)
C30B	0.082 (6)	0.074 (6)	0.047 (5)	−0.039 (5)	0.010 (4)	0.017 (4)
C31B	0.062 (5)	0.049 (5)	0.036 (4)	0.000 (4)	0.003 (4)	0.009 (3)
C32B	0.071 (5)	0.044 (4)	0.051 (5)	0.005 (4)	0.038 (4)	0.015 (4)
C33B	0.054 (4)	0.034 (4)	0.033 (4)	−0.012 (3)	0.012 (3)	−0.016 (3)

Geometric parameters (Å, º)

C1—C9	1.516 (7)	C5B—H5B	0.9500
C1—C15	1.543 (8)	C6B—C7B	1.403 (8)
C1—C16	1.545 (8)	C6B—C21B	1.554 (8)
C1—C2	1.582 (7)	C7B—C8B	1.400 (8)
C2—C3	1.534 (7)	C7B—H7B	0.9500
C2—H2A	0.9900	C8B—C25B	1.559 (8)
C2—H2B	0.9900	C9B—C10B	1.399 (7)
C3—C4	1.428 (8)	C9B—C14B	1.403 (8)
C3—C8	1.430 (7)	C10B—C11B	1.405 (8)
C4—C5	1.396 (7)	C10B—H10B	0.9500
C4—C17	1.555 (8)	C11B—C12B	1.400 (8)
C5—C6	1.418 (7)	C11B—C29B	1.521 (8)
C5—H5	0.9500	C12B—C13B	1.386 (8)
C6—C7	1.367 (8)	C12B—H12B	0.9500
C6—C21	1.541 (8)	C13B—C14B	1.395 (7)
C7—C8	1.409 (8)	C13B—C33B	1.552 (8)
C7—H7	0.9500	C14B—H14B	0.9500
C8—C25	1.555 (8)	C15B—H15D	0.9800
C9—C10	1.390 (8)	C15B—H15E	0.9800
C9—C14	1.399 (8)	C15B—H15F	0.9800
C10—C11	1.389 (8)	C16B—H16D	0.9800
C10—H10	0.9500	C16B—H16E	0.9800
C11—C12	1.400 (8)	C16B—H16F	0.9800
C11—C29	1.542 (7)	C17B—C18B	1.534 (8)
C12—C13	1.408 (7)	C17B—C20B	1.549 (8)
C12—H12	0.9500	C17B—C19B	1.558 (8)
C13—C14	1.389 (7)	C18B—H18D	0.9800
C13—C33	1.536 (8)	C18B—H18E	0.9800
C14—H14	0.9500	C18B—H18F	0.9800
C15—H15A	0.9800	C19B—H19D	0.9800
C15—H15B	0.9800	C19B—H19E	0.9800
C15—H15C	0.9800	C19B—H19F	0.9800
C16—H16A	0.9800	C20B—H20D	0.9800
C16—H16B	0.9800	C20B—H20E	0.9800
C16—H16C	0.9800	C20B—H20F	0.9800
C17—C18	1.546 (8)	C21B—C22B	1.537 (8)
C17—C19	1.545 (8)	C21B—C24B	1.541 (9)
C17—C20	1.549 (8)	C21B—C23B	1.542 (9)
C18—H18A	0.9800	C22B—H22D	0.9800
C18—H18B	0.9800	C22B—H22E	0.9800
C18—H18C	0.9800	C22B—H22F	0.9800
C19—H19A	0.9800	C23B—H23D	0.9800
C19—H19B	0.9800	C23B—H23E	0.9800
C19—H19C	0.9800	C23B—H23F	0.9800
C20—H20A	0.9800	C24B—H24D	0.9800
C20—H20B	0.9800	C24B—H24E	0.9800
C20—H20C	0.9800	C24B—H24F	0.9800
C21—C23	1.531 (8)	C25B—C26B	1.532 (8)
C21—C22	1.544 (8)	C25B—C28B	1.542 (8)
C21—C24	1.545 (8)	C25B—C27B	1.557 (8)
C22—H22A	0.9800	C26B—H26D	0.9800
C22—H22B	0.9800	C26B—H26E	0.9800
C22—H22C	0.9800	C26B—H26F	0.9800
C23—H23A	0.9800	C27B—H27D	0.9800
C23—H23B	0.9800	C27B—H27E	0.9800
C23—H23C	0.9800	C27B—H27F	0.9800
C24—H24A	0.9800	C28B—H28D	0.9800
C24—H24B	0.9800	C28B—H28E	0.9800
C24—H24C	0.9800	C28B—H28F	0.9800
C25—C26	1.542 (8)	C29B—C31B	1.527 (9)
C25—C28	1.557 (8)	C29B—C30B	1.543 (9)
C25—C27	1.558 (8)	C29B—C32B	1.546 (8)
C26—H26A	0.9800	C30B—H30D	0.9800
C26—H26B	0.9800	C30B—H30E	0.9800
C26—H26C	0.9800	C30B—H30F	0.9800
C27—H27A	0.9800	C31B—H31D	0.9800
C27—H27B	0.9800	C31B—H31E	0.9800
C27—H27C	0.9800	C31B—H31F	0.9800
C28—H28A	0.9800	C32B—H32D	0.9800
C28—H28B	0.9800	C32B—H32E	0.9800
C28—H28C	0.9800	C32B—H32F	0.9800
C29—C30	1.520 (8)	C33B—C36C	1.476
C29—C31	1.538 (8)	C33B—C34B	1.497
C29—C32	1.539 (8)	C33B—C36D	1.503
C30—H30A	0.9800	C33B—C36B	1.521
C30—H30B	0.9800	C33B—C35D	1.536
C30—H30C	0.9800	C33B—C34D	1.542
C31—H31A	0.9800	C33B—C35C	1.547
C31—H31B	0.9800	C33B—C34C	1.559
C31—H31C	0.9800	C33B—C35B	1.587
C32—H32A	0.9800	C34B—H34D	0.9800
C32—H32B	0.9800	C34B—H34E	0.9800
C32—H32C	0.9800	C34B—H34F	0.9800
C33—C34	1.524 (8)	C35B—H35D	0.9800
C33—C36	1.528 (8)	C35B—H35E	0.9800
C33—C35	1.536 (9)	C35B—H35F	0.9800
C34—H34A	0.9800	C36B—H36D	0.9800
C34—H34B	0.9800	C36B—H36E	0.9800
C34—H34C	0.9800	C36B—H36F	0.9800
C35—H35A	0.9800	C34D—H34J	0.9800
C35—H35B	0.9800	C34D—H34K	0.9800
C35—H35C	0.9800	C34D—H34L	0.9800
C36—H36A	0.9800	C35D—H35J	0.9800
C36—H36B	0.9800	C35D—H35K	0.9800
C36—H36C	0.9800	C35D—H35L	0.9800
C1B—C16B	1.524 (8)	C36D—H36J	0.9800
C1B—C9B	1.535 (7)	C36D—H36K	0.9800
C1B—C15B	1.543 (7)	C36D—H36L	0.9800
C1B—C2B	1.579 (7)	C34C—H34G	0.9800
C2B—C3B	1.537 (7)	C34C—H34H	0.9800
C2B—H2B1	0.9900	C34C—H34I	0.9800
C2B—H2B2	0.9900	C36C—H36G	0.9800
C3B—C8B	1.418 (7)	C36C—H36H	0.9800
C3B—C4B	1.424 (7)	C36C—H36I	0.9800
C4B—C5B	1.419 (7)	C35C—H35G	0.9800
C4B—C17B	1.568 (8)	C35C—H35H	0.9800
C5B—C6B	1.376 (7)	C35C—H35I	0.9800
C9—C1—C15	112.2 (5)	C8B—C7B—C6B	122.7 (5)
C9—C1—C16	108.5 (4)	C8B—C7B—H7B	118.6
C15—C1—C16	106.7 (5)	C6B—C7B—H7B	118.6
C9—C1—C2	113.2 (5)	C7B—C8B—C3B	118.0 (5)
C15—C1—C2	104.1 (4)	C7B—C8B—C25B	111.9 (5)
C16—C1—C2	111.9 (4)	C3B—C8B—C25B	129.5 (5)
C3—C2—C1	117.3 (4)	C10B—C9B—C14B	117.9 (5)
C3—C2—H2A	108.0	C10B—C9B—C1B	122.5 (5)
C1—C2—H2A	108.0	C14B—C9B—C1B	119.6 (5)
C3—C2—H2B	108.0	C9B—C10B—C11B	122.5 (5)
C1—C2—H2B	108.0	C9B—C10B—H10B	118.8
H2A—C2—H2B	107.2	C11B—C10B—H10B	118.8
C4—C3—C8	118.0 (5)	C12B—C11B—C10B	116.7 (5)
C4—C3—C2	119.6 (5)	C12B—C11B—C29B	121.2 (5)
C8—C3—C2	122.3 (5)	C10B—C11B—C29B	122.1 (5)
C5—C4—C3	119.3 (5)	C13B—C12B—C11B	123.2 (5)
C5—C4—C17	117.0 (5)	C13B—C12B—H12B	118.4
C3—C4—C17	123.3 (5)	C11B—C12B—H12B	118.4
C4—C5—C6	122.2 (5)	C12B—C13B—C14B	118.1 (5)
C4—C5—H5	118.9	C12B—C13B—C33B	120.5 (5)
C6—C5—H5	118.9	C14B—C13B—C33B	121.4 (5)
C7—C6—C5	116.5 (5)	C13B—C14B—C9B	121.7 (5)
C7—C6—C21	121.2 (5)	C13B—C14B—H14B	119.2
C5—C6—C21	122.1 (5)	C9B—C14B—H14B	119.2
C6—C7—C8	124.5 (5)	C1B—C15B—H15D	109.5
C6—C7—H7	117.8	C1B—C15B—H15E	109.5
C8—C7—H7	117.8	H15D—C15B—H15E	109.5
C7—C8—C3	117.6 (5)	C1B—C15B—H15F	109.5
C7—C8—C25	112.6 (5)	H15D—C15B—H15F	109.5
C3—C8—C25	129.4 (5)	H15E—C15B—H15F	109.5
C10—C9—C14	117.0 (5)	C1B—C16B—H16D	109.5
C10—C9—C1	122.7 (5)	C1B—C16B—H16E	109.5
C14—C9—C1	120.2 (5)	H16D—C16B—H16E	109.5
C11—C10—C9	123.2 (5)	C1B—C16B—H16F	109.5
C11—C10—H10	118.4	H16D—C16B—H16F	109.5
C9—C10—H10	118.4	H16E—C16B—H16F	109.5
C10—C11—C12	117.6 (5)	C18B—C17B—C20B	104.8 (5)
C10—C11—C29	121.0 (5)	C18B—C17B—C19B	110.4 (5)
C12—C11—C29	121.4 (5)	C20B—C17B—C19B	106.0 (5)
C11—C12—C13	121.8 (5)	C18B—C17B—C4B	109.5 (5)
C11—C12—H12	119.1	C20B—C17B—C4B	111.0 (5)
C13—C12—H12	119.1	C19B—C17B—C4B	114.7 (5)
C14—C13—C12	117.5 (5)	C17B—C18B—H18D	109.5
C14—C13—C33	122.8 (5)	C17B—C18B—H18E	109.5
C12—C13—C33	119.7 (5)	H18D—C18B—H18E	109.5
C13—C14—C9	122.9 (5)	C17B—C18B—H18F	109.5
C13—C14—H14	118.6	H18D—C18B—H18F	109.5
C9—C14—H14	118.6	H18E—C18B—H18F	109.5
C1—C15—H15A	109.5	C17B—C19B—H19D	109.5
C1—C15—H15B	109.5	C17B—C19B—H19E	109.5
H15A—C15—H15B	109.5	H19D—C19B—H19E	109.5
C1—C15—H15C	109.5	C17B—C19B—H19F	109.5
H15A—C15—H15C	109.5	H19D—C19B—H19F	109.5
H15B—C15—H15C	109.5	H19E—C19B—H19F	109.5
C1—C16—H16A	109.5	C17B—C20B—H20D	109.5
C1—C16—H16B	109.5	C17B—C20B—H20E	109.5
H16A—C16—H16B	109.5	H20D—C20B—H20E	109.5
C1—C16—H16C	109.5	C17B—C20B—H20F	109.5
H16A—C16—H16C	109.5	H20D—C20B—H20F	109.5
H16B—C16—H16C	109.5	H20E—C20B—H20F	109.5
C18—C17—C19	110.0 (5)	C22B—C21B—C24B	108.3 (5)
C18—C17—C20	106.0 (5)	C22B—C21B—C23B	108.6 (5)
C19—C17—C20	104.2 (5)	C24B—C21B—C23B	108.8 (5)
C18—C17—C4	106.7 (5)	C22B—C21B—C6B	112.4 (5)
C19—C17—C4	117.6 (5)	C24B—C21B—C6B	109.5 (5)
C20—C17—C4	111.9 (5)	C23B—C21B—C6B	109.2 (5)
C17—C18—H18A	109.5	C21B—C22B—H22D	109.5
C17—C18—H18B	109.5	C21B—C22B—H22E	109.5
H18A—C18—H18B	109.5	H22D—C22B—H22E	109.5
C17—C18—H18C	109.5	C21B—C22B—H22F	109.5
H18A—C18—H18C	109.5	H22D—C22B—H22F	109.5
H18B—C18—H18C	109.5	H22E—C22B—H22F	109.5
C17—C19—H19A	109.5	C21B—C23B—H23D	109.5
C17—C19—H19B	109.5	C21B—C23B—H23E	109.5
H19A—C19—H19B	109.5	H23D—C23B—H23E	109.5
C17—C19—H19C	109.5	C21B—C23B—H23F	109.5
H19A—C19—H19C	109.5	H23D—C23B—H23F	109.5
H19B—C19—H19C	109.5	H23E—C23B—H23F	109.5
C17—C20—H20A	109.5	C21B—C24B—H24D	109.5
C17—C20—H20B	109.5	C21B—C24B—H24E	109.5
H20A—C20—H20B	109.5	H24D—C24B—H24E	109.5
C17—C20—H20C	109.5	C21B—C24B—H24F	109.5
H20A—C20—H20C	109.5	H24D—C24B—H24F	109.5
H20B—C20—H20C	109.5	H24E—C24B—H24F	109.5
C23—C21—C6	110.0 (5)	C26B—C25B—C28B	107.0 (5)
C23—C21—C22	108.3 (5)	C26B—C25B—C27B	108.1 (5)
C6—C21—C22	112.8 (5)	C28B—C25B—C27B	103.5 (5)
C23—C21—C24	109.3 (5)	C26B—C25B—C8B	112.9 (5)
C6—C21—C24	108.5 (4)	C28B—C25B—C8B	117.9 (5)
C22—C21—C24	107.9 (5)	C27B—C25B—C8B	106.7 (5)
C21—C22—H22A	109.5	C25B—C26B—H26D	109.5
C21—C22—H22B	109.5	C25B—C26B—H26E	109.5
H22A—C22—H22B	109.5	H26D—C26B—H26E	109.5
C21—C22—H22C	109.5	C25B—C26B—H26F	109.5
H22A—C22—H22C	109.5	H26D—C26B—H26F	109.5
H22B—C22—H22C	109.5	H26E—C26B—H26F	109.5
C21—C23—H23A	109.5	C25B—C27B—H27D	109.5
C21—C23—H23B	109.5	C25B—C27B—H27E	109.5
H23A—C23—H23B	109.5	H27D—C27B—H27E	109.5
C21—C23—H23C	109.5	C25B—C27B—H27F	109.5
H23A—C23—H23C	109.5	H27D—C27B—H27F	109.5
H23B—C23—H23C	109.5	H27E—C27B—H27F	109.5
C21—C24—H24A	109.5	C25B—C28B—H28D	109.5
C21—C24—H24B	109.5	C25B—C28B—H28E	109.5
H24A—C24—H24B	109.5	H28D—C28B—H28E	109.5
C21—C24—H24C	109.5	C25B—C28B—H28F	109.5
H24A—C24—H24C	109.5	H28D—C28B—H28F	109.5
H24B—C24—H24C	109.5	H28E—C28B—H28F	109.5
C26—C25—C8	111.8 (5)	C11B—C29B—C31B	108.7 (5)
C26—C25—C28	107.1 (5)	C11B—C29B—C30B	112.4 (5)
C8—C25—C28	118.8 (5)	C31B—C29B—C30B	109.6 (6)
C26—C25—C27	108.0 (5)	C11B—C29B—C32B	110.7 (5)
C8—C25—C27	106.6 (5)	C31B—C29B—C32B	108.0 (5)
C28—C25—C27	103.9 (5)	C30B—C29B—C32B	107.4 (6)
C25—C26—H26A	109.5	C29B—C30B—H30D	109.5
C25—C26—H26B	109.5	C29B—C30B—H30E	109.5
H26A—C26—H26B	109.5	H30D—C30B—H30E	109.5
C25—C26—H26C	109.5	C29B—C30B—H30F	109.5
H26A—C26—H26C	109.5	H30D—C30B—H30F	109.5
H26B—C26—H26C	109.5	H30E—C30B—H30F	109.5
C25—C27—H27A	109.5	C29B—C31B—H31D	109.5
C25—C27—H27B	109.5	C29B—C31B—H31E	109.5
H27A—C27—H27B	109.5	H31D—C31B—H31E	109.5
C25—C27—H27C	109.5	C29B—C31B—H31F	109.5
H27A—C27—H27C	109.5	H31D—C31B—H31F	109.5
H27B—C27—H27C	109.5	H31E—C31B—H31F	109.5
C25—C28—H28A	109.5	C29B—C32B—H32D	109.5
C25—C28—H28B	109.5	C29B—C32B—H32E	109.5
H28A—C28—H28B	109.5	H32D—C32B—H32E	109.5
C25—C28—H28C	109.5	C29B—C32B—H32F	109.5
H28A—C28—H28C	109.5	H32D—C32B—H32F	109.5
H28B—C28—H28C	109.5	H32E—C32B—H32F	109.5
C30—C29—C31	109.6 (6)	C36C—C33B—C13B	116.0
C30—C29—C32	107.0 (6)	C34B—C33B—C13B	112.1
C31—C29—C32	109.0 (6)	C36D—C33B—C13B	112.1
C30—C29—C11	113.2 (5)	C36B—C33B—C13B	112.7
C31—C29—C11	108.5 (5)	C35D—C33B—C13B	109.9
C32—C29—C11	109.3 (5)	C34D—C33B—C13B	108.9
C29—C30—H30A	109.5	C35C—C33B—C13B	107.3
C29—C30—H30B	109.5	C13B—C33B—C34C	104.7
H30A—C30—H30B	109.5	C13B—C33B—C35B	104.4
C29—C30—H30C	109.5	C34B—C33B—C35B	106.5
H30A—C30—H30C	109.5	C36B—C33B—C35B	107.9
H30B—C30—H30C	109.5	C34B—C33B—C36B	112.6
C29—C31—H31A	109.5	C36D—C33B—C35D	107.7
C29—C31—H31B	109.5	C36D—C33B—C34D	108.4
H31A—C31—H31B	109.5	C35D—C33B—C34D	109.9
C29—C31—H31C	109.5	C36C—C33B—C35C	112.1
H31A—C31—H31C	109.5	C36C—C33B—C34C	110.3
H31B—C31—H31C	109.5	C35C—C33B—C34C	105.7
C29—C32—H32A	109.5	C33B—C34B—H34D	109.5
C29—C32—H32B	109.5	C33B—C34B—H34E	109.5
H32A—C32—H32B	109.5	H34D—C34B—H34E	109.5
C29—C32—H32C	109.5	C33B—C34B—H34F	109.5
H32A—C32—H32C	109.5	H34D—C34B—H34F	109.5
H32B—C32—H32C	109.5	H34E—C34B—H34F	109.5
C34—C33—C36	108.8 (5)	C33B—C35B—H35D	109.5
C34—C33—C13	111.7 (5)	C33B—C35B—H35E	109.5
C36—C33—C13	111.8 (5)	H35D—C35B—H35E	109.5
C34—C33—C35	109.4 (5)	C33B—C35B—H35F	109.5
C36—C33—C35	107.7 (5)	H35D—C35B—H35F	109.5
C13—C33—C35	107.4 (5)	H35E—C35B—H35F	109.5
C33—C34—H34A	109.5	C33B—C36B—H36D	109.5
C33—C34—H34B	109.5	C33B—C36B—H36E	109.5
H34A—C34—H34B	109.5	H36D—C36B—H36E	109.5
C33—C34—H34C	109.5	C33B—C36B—H36F	109.5
H34A—C34—H34C	109.5	H36D—C36B—H36F	109.5
H34B—C34—H34C	109.5	H36E—C36B—H36F	109.5
C33—C35—H35A	109.5	C33B—C34D—H34J	109.5
C33—C35—H35B	109.5	C33B—C34D—H34K	109.5
H35A—C35—H35B	109.5	H34J—C34D—H34K	109.5
C33—C35—H35C	109.5	C33B—C34D—H34L	109.5
H35A—C35—H35C	109.5	H34J—C34D—H34L	109.5
H35B—C35—H35C	109.5	H34K—C34D—H34L	109.5
C33—C36—H36A	109.5	C33B—C35D—H35J	109.5
C33—C36—H36B	109.5	C33B—C35D—H35K	109.5
H36A—C36—H36B	109.5	H35J—C35D—H35K	109.5
C33—C36—H36C	109.5	C33B—C35D—H35L	109.5
H36A—C36—H36C	109.5	H35J—C35D—H35L	109.5
H36B—C36—H36C	109.5	H35K—C35D—H35L	109.5
C16B—C1B—C9B	107.4 (4)	C33B—C36D—H36J	109.5
C16B—C1B—C15B	107.7 (5)	C33B—C36D—H36K	109.5
C9B—C1B—C15B	110.9 (4)	H36J—C36D—H36K	109.5
C16B—C1B—C2B	113.7 (4)	C33B—C36D—H36L	109.5
C9B—C1B—C2B	111.5 (4)	H36J—C36D—H36L	109.5
C15B—C1B—C2B	105.5 (4)	H36K—C36D—H36L	109.5
C3B—C2B—C1B	117.8 (4)	C33B—C34C—H34G	109.5
C3B—C2B—H2B1	107.9	C33B—C34C—H34H	109.5
C1B—C2B—H2B1	107.9	H34G—C34C—H34H	109.5
C3B—C2B—H2B2	107.9	C33B—C34C—H34I	109.5
C1B—C2B—H2B2	107.9	H34G—C34C—H34I	109.5
H2B1—C2B—H2B2	107.2	H34H—C34C—H34I	109.5
C8B—C3B—C4B	118.5 (5)	C33B—C36C—H36G	109.5
C8B—C3B—C2B	121.8 (5)	C33B—C36C—H36H	109.5
C4B—C3B—C2B	119.4 (5)	H36G—C36C—H36H	109.5
C5B—C4B—C3B	118.5 (5)	C33B—C36C—H36I	109.5
C5B—C4B—C17B	117.3 (5)	H36G—C36C—H36I	109.5
C3B—C4B—C17B	123.9 (5)	H36H—C36C—H36I	109.5
C6B—C5B—C4B	121.8 (5)	C33B—C35C—H35G	109.5
C6B—C5B—H5B	119.1	C33B—C35C—H35H	109.5
C4B—C5B—H5B	119.1	H35G—C35C—H35H	109.5
C5B—C6B—C7B	117.6 (5)	C33B—C35C—H35I	109.5
C5B—C6B—C21B	122.8 (5)	H35G—C35C—H35I	109.5
C7B—C6B—C21B	119.3 (5)	H35H—C35C—H35I	109.5
C9—C1—C2—C3	−63.5 (6)	C2B—C3B—C4B—C5B	−156.1 (5)
C15—C1—C2—C3	174.4 (5)	C8B—C3B—C4B—C17B	−155.3 (5)
C16—C1—C2—C3	59.5 (6)	C2B—C3B—C4B—C17B	30.8 (7)
C1—C2—C3—C4	95.5 (6)	C3B—C4B—C5B—C6B	−5.6 (8)
C1—C2—C3—C8	−80.4 (6)	C17B—C4B—C5B—C6B	167.9 (5)
C8—C3—C4—C5	14.6 (8)	C4B—C5B—C6B—C7B	−7.4 (8)
C2—C3—C4—C5	−161.5 (5)	C4B—C5B—C6B—C21B	178.3 (5)
C8—C3—C4—C17	−157.3 (5)	C5B—C6B—C7B—C8B	8.6 (8)
C2—C3—C4—C17	26.7 (7)	C21B—C6B—C7B—C8B	−176.9 (5)
C3—C4—C5—C6	−4.2 (8)	C6B—C7B—C8B—C3B	3.5 (8)
C17—C4—C5—C6	168.2 (5)	C6B—C7B—C8B—C25B	−169.1 (5)
C4—C5—C6—C7	−5.1 (8)	C4B—C3B—C8B—C7B	−16.6 (8)
C4—C5—C6—C21	−179.3 (5)	C2B—C3B—C8B—C7B	157.1 (5)
C5—C6—C7—C8	3.9 (8)	C4B—C3B—C8B—C25B	154.5 (5)
C21—C6—C7—C8	178.2 (5)	C2B—C3B—C8B—C25B	−31.9 (8)
C6—C7—C8—C3	6.4 (8)	C16B—C1B—C9B—C10B	130.1 (5)
C6—C7—C8—C25	−166.8 (5)	C15B—C1B—C9B—C10B	12.7 (7)
C4—C3—C8—C7	−15.5 (7)	C2B—C1B—C9B—C10B	−104.6 (6)
C2—C3—C8—C7	160.4 (5)	C16B—C1B—C9B—C14B	−47.5 (7)
C4—C3—C8—C25	156.5 (5)	C15B—C1B—C9B—C14B	−164.9 (5)
C2—C3—C8—C25	−27.6 (8)	C2B—C1B—C9B—C14B	77.8 (6)
C15—C1—C9—C10	11.6 (8)	C14B—C9B—C10B—C11B	1.4 (8)
C16—C1—C9—C10	129.3 (6)	C1B—C9B—C10B—C11B	−176.2 (5)
C2—C1—C9—C10	−105.8 (6)	C9B—C10B—C11B—C12B	−0.5 (8)
C15—C1—C9—C14	−165.9 (5)	C9B—C10B—C11B—C29B	−179.4 (5)
C16—C1—C9—C14	−48.2 (7)	C10B—C11B—C12B—C13B	−0.2 (9)
C2—C1—C9—C14	76.7 (6)	C29B—C11B—C12B—C13B	178.7 (6)
C14—C9—C10—C11	−0.2 (9)	C11B—C12B—C13B—C14B	0.1 (9)
C1—C9—C10—C11	−177.8 (5)	C11B—C12B—C13B—C33B	−178.3 (6)
C9—C10—C11—C12	−0.2 (8)	C12B—C13B—C14B—C9B	0.9 (9)
C9—C10—C11—C29	−177.7 (5)	C33B—C13B—C14B—C9B	179.3 (5)
C10—C11—C12—C13	0.8 (8)	C10B—C9B—C14B—C13B	−1.6 (8)
C29—C11—C12—C13	178.2 (5)	C1B—C9B—C14B—C13B	176.1 (5)
C11—C12—C13—C14	−0.8 (8)	C5B—C4B—C17B—C18B	−127.8 (5)
C11—C12—C13—C33	−179.8 (5)	C3B—C4B—C17B—C18B	45.4 (7)
C12—C13—C14—C9	0.3 (8)	C5B—C4B—C17B—C20B	−12.5 (7)
C33—C13—C14—C9	179.3 (5)	C3B—C4B—C17B—C20B	160.6 (5)
C10—C9—C14—C13	0.2 (8)	C5B—C4B—C17B—C19B	107.5 (6)
C1—C9—C14—C13	177.8 (5)	C3B—C4B—C17B—C19B	−79.3 (7)
C5—C4—C17—C18	−116.8 (6)	C5B—C6B—C21B—C22B	−11.1 (8)
C3—C4—C17—C18	55.3 (7)	C7B—C6B—C21B—C22B	174.6 (5)
C5—C4—C17—C19	119.1 (6)	C5B—C6B—C21B—C24B	109.3 (6)
C3—C4—C17—C19	−68.8 (7)	C7B—C6B—C21B—C24B	−65.0 (7)
C5—C4—C17—C20	−1.3 (7)	C5B—C6B—C21B—C23B	−131.7 (6)
C3—C4—C17—C20	170.7 (5)	C7B—C6B—C21B—C23B	54.0 (7)
C7—C6—C21—C23	55.1 (7)	C7B—C8B—C25B—C26B	−59.3 (6)
C5—C6—C21—C23	−131.0 (6)	C3B—C8B—C25B—C26B	129.2 (6)
C7—C6—C21—C22	176.1 (5)	C7B—C8B—C25B—C28B	175.1 (5)
C5—C6—C21—C22	−9.9 (8)	C3B—C8B—C25B—C28B	3.6 (9)
C7—C6—C21—C24	−64.4 (7)	C7B—C8B—C25B—C27B	59.3 (6)
C5—C6—C21—C24	109.5 (6)	C3B—C8B—C25B—C27B	−112.2 (6)
C7—C8—C25—C26	−62.9 (6)	C12B—C11B—C29B—C31B	−92.7 (7)
C3—C8—C25—C26	124.8 (6)	C10B—C11B—C29B—C31B	86.2 (7)
C7—C8—C25—C28	171.6 (5)	C12B—C11B—C29B—C30B	28.8 (9)
C3—C8—C25—C28	−0.7 (9)	C10B—C11B—C29B—C30B	−152.4 (6)
C7—C8—C25—C27	54.9 (6)	C12B—C11B—C29B—C32B	148.9 (6)
C3—C8—C25—C27	−117.4 (6)	C10B—C11B—C29B—C32B	−32.3 (8)
C10—C11—C29—C30	−166.5 (6)	C12B—C13B—C33B—C36C	115.1
C12—C11—C29—C30	16.1 (8)	C14B—C13B—C33B—C36C	−63.3
C10—C11—C29—C31	71.5 (7)	C12B—C13B—C33B—C34B	−38.1
C12—C11—C29—C31	−105.9 (6)	C14B—C13B—C33B—C34B	143.6
C10—C11—C29—C32	−47.3 (7)	C12B—C13B—C33B—C36D	177.5
C12—C11—C29—C32	135.3 (6)	C14B—C13B—C33B—C36D	−0.9
C14—C13—C33—C34	134.5 (6)	C12B—C13B—C33B—C36B	−166.3
C12—C13—C33—C34	−46.5 (8)	C14B—C13B—C33B—C36B	15.3
C14—C13—C33—C36	12.4 (8)	C12B—C13B—C33B—C35D	57.8
C12—C13—C33—C36	−168.7 (5)	C14B—C13B—C33B—C35D	−120.6
C14—C13—C33—C35	−105.5 (6)	C12B—C13B—C33B—C34D	−62.6
C12—C13—C33—C35	73.4 (7)	C14B—C13B—C33B—C34D	119.0
C16B—C1B—C2B—C3B	49.3 (6)	C12B—C13B—C33B—C35C	−11.1
C9B—C1B—C2B—C3B	−72.4 (6)	C14B—C13B—C33B—C35C	170.5
C15B—C1B—C2B—C3B	167.1 (5)	C12B—C13B—C33B—C34C	−123.1
C1B—C2B—C3B—C8B	−74.0 (7)	C14B—C13B—C33B—C34C	58.5
C1B—C2B—C3B—C4B	99.6 (6)	C12B—C13B—C33B—C35B	76.8
C8B—C3B—C4B—C5B	17.7 (8)	C14B—C13B—C33B—C35B	−101.5

2,5-bis(3,5-di-tert-butylphenyl)-2,5-dimethylhexane (IVa)

Crystal data

C36H58	Z = 1
Mr = 490.82	F(000) = 274
Triclinic, P1	Dx = 0.997 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71070 Å
a = 9.8680 (7) Å	Cell parameters from 27 reflections
b = 9.9061 (7) Å	θ = 4.2–9.3°
c = 9.9285 (7) Å	µ = 0.06 mm^−1
α = 77.626 (3)°	T = 128 K
β = 60.758 (3)°	Cut plate, colourless
γ = 76.286 (3)°	0.45 × 0.4 × 0.2 mm
V = 817.15 (10) Å^3

Data collection

Modified Picker FACS1 diffractometer	Rint = 0.0000
Radiation source: fine-focus sealed tube	θmax = 30.0°, θmin = 2.1°
Graphite monochromator	h = 0→13
θ/2θ scans	k = −13→13
4751 measured reflections	l = −11→13
4751 independent reflections	3 standard reflections every 97 reflections
2086 reflections with I > 2σ(I)	intensity decay: 1.5%

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)] = 0.077	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.228	H-atom parameters constrained
S = 1.06	w = 1/[σ^2(Fo^2) + (0.P)^2 + 1.5116P] where P = (Fo^2 + 2Fc^2)/3
4751 reflections	(Δ/σ)max = 0.004
171 parameters	Δρmax = 0.39 e Å^−3
0 restraints	Δρmin = −0.42 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
C1	0.3502 (3)	0.7202 (2)	0.8850 (3)	0.0178 (5)
C2	0.2005 (3)	0.7226 (3)	1.0140 (3)	0.0197 (5)
H2	0.1920	0.7097	1.1153	0.024*
C3	0.0641 (3)	0.7432 (3)	0.9983 (3)	0.0187 (5)
C4	0.0799 (3)	0.7642 (3)	0.8474 (3)	0.0206 (5)
H4	−0.0119	0.7798	0.8343	0.025*
C5	0.2257 (3)	0.7628 (3)	0.7163 (3)	0.0193 (5)
C6	0.3600 (3)	0.7404 (3)	0.7379 (3)	0.0208 (5)
H6	0.4605	0.7389	0.6494	0.025*
C11	0.4950 (3)	0.7001 (3)	0.9107 (3)	0.0217 (5)
C12	0.4972 (3)	0.5682 (3)	1.0261 (3)	0.0212 (5)
H12A	0.5899	0.5596	1.0432	0.025*
H12B	0.4022	0.5812	1.1270	0.025*
C13	0.4841 (4)	0.8276 (3)	0.9832 (4)	0.0320 (7)
H13A	0.3870	0.8354	1.0816	0.048*
H13B	0.4835	0.9126	0.9116	0.048*
H13C	0.5748	0.8157	1.0026	0.048*
C14	0.6502 (3)	0.6896 (3)	0.7594 (3)	0.0290 (6)
H14A	0.7387	0.6717	0.7832	0.044*
H14B	0.6539	0.7777	0.6910	0.044*
H14C	0.6571	0.6129	0.7072	0.044*
C31	−0.0992 (3)	0.7456 (3)	1.1368 (3)	0.0239 (5)
C32	−0.1781 (4)	0.6314 (3)	1.1326 (4)	0.0336 (7)
H32A	−0.1821	0.6460	1.0337	0.050*
H32B	−0.2852	0.6358	1.2186	0.050*
H32C	−0.1175	0.5394	1.1428	0.050*
C33	−0.0959 (4)	0.7196 (4)	1.2929 (4)	0.0429 (9)
H33A	−0.0323	0.6287	1.3006	0.064*
H33B	−0.2034	0.7198	1.3777	0.064*
H33C	−0.0501	0.7936	1.3002	0.064*
C34	−0.1987 (3)	0.8888 (3)	1.1279 (4)	0.0348 (7)
H34A	−0.2028	0.9074	1.0289	0.052*
H34B	−0.1514	0.9617	1.1354	0.052*
H34C	−0.3055	0.8888	1.2139	0.052*
C51	0.2438 (3)	0.7838 (3)	0.5511 (3)	0.0264 (6)
C52	0.3164 (4)	0.9184 (4)	0.4640 (4)	0.0403 (8)
H52A	0.4187	0.9094	0.4614	0.060*
H52B	0.2462	0.9989	0.5178	0.060*
H52C	0.3304	0.9321	0.3575	0.060*
C53	0.0878 (4)	0.7984 (5)	0.5480 (4)	0.0483 (10)
H53A	0.0419	0.7125	0.5993	0.073*
H53C	0.1059	0.8143	0.4400	0.073*
H53B	0.0154	0.8778	0.6026	0.073*
C54	0.3538 (4)	0.6588 (4)	0.4650 (4)	0.0416 (8)
H54A	0.3650	0.6725	0.3596	0.062*
H54B	0.3097	0.5728	0.5209	0.062*
H54C	0.4572	0.6513	0.4596	0.062*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0193 (11)	0.0145 (11)	0.0225 (12)	−0.0013 (9)	−0.0127 (10)	−0.0012 (9)
C2	0.0219 (12)	0.0188 (12)	0.0182 (12)	−0.0006 (9)	−0.0096 (10)	−0.0037 (9)
C3	0.0193 (11)	0.0181 (12)	0.0197 (12)	−0.0011 (9)	−0.0097 (10)	−0.0039 (9)
C4	0.0192 (12)	0.0207 (12)	0.0246 (13)	−0.0027 (9)	−0.0126 (10)	−0.0019 (10)
C5	0.0219 (12)	0.0189 (12)	0.0186 (11)	−0.0047 (9)	−0.0107 (10)	0.0000 (9)
C6	0.0188 (12)	0.0223 (12)	0.0194 (12)	−0.0024 (10)	−0.0083 (10)	−0.0012 (10)
C11	0.0230 (13)	0.0195 (12)	0.0272 (13)	−0.0036 (10)	−0.0164 (11)	0.0007 (10)
C12	0.0233 (12)	0.0199 (12)	0.0229 (12)	−0.0009 (10)	−0.0135 (10)	−0.0027 (10)
C13	0.0366 (16)	0.0258 (15)	0.0460 (18)	−0.0080 (12)	−0.0282 (15)	−0.0015 (13)
C14	0.0225 (13)	0.0336 (16)	0.0296 (15)	−0.0071 (11)	−0.0123 (12)	0.0027 (12)
C31	0.0205 (12)	0.0228 (13)	0.0243 (13)	−0.0006 (10)	−0.0077 (10)	−0.0044 (10)
C32	0.0267 (15)	0.0294 (15)	0.0362 (17)	−0.0094 (12)	−0.0055 (13)	−0.0049 (13)
C33	0.0294 (16)	0.074 (3)	0.0213 (15)	−0.0070 (16)	−0.0071 (13)	−0.0099 (15)
C34	0.0233 (14)	0.0301 (15)	0.0405 (18)	−0.0012 (12)	−0.0061 (13)	−0.0088 (13)
C51	0.0291 (14)	0.0305 (15)	0.0192 (12)	−0.0030 (11)	−0.0119 (11)	−0.0017 (11)
C52	0.056 (2)	0.0403 (19)	0.0258 (15)	−0.0150 (16)	−0.0207 (15)	0.0080 (13)
C53	0.041 (2)	0.083 (3)	0.0285 (17)	−0.0111 (19)	−0.0243 (16)	0.0010 (17)
C54	0.052 (2)	0.045 (2)	0.0275 (16)	−0.0009 (16)	−0.0181 (15)	−0.0112 (14)

Geometric parameters (Å, º)

C1—C6	1.389 (3)	C31—C33	1.531 (4)
C1—C2	1.404 (3)	C31—C34	1.534 (4)
C1—C11	1.532 (3)	C31—C32	1.536 (4)
C2—C3	1.392 (3)	C32—H32A	0.9800
C2—H2	0.9500	C32—H32B	0.9800
C3—C4	1.402 (3)	C32—H32C	0.9800
C3—C31	1.523 (4)	C33—H33A	0.9800
C4—C5	1.390 (4)	C33—H33B	0.9800
C4—H4	0.9500	C33—H33C	0.9800
C5—C6	1.403 (3)	C34—H34A	0.9800
C5—C51	1.533 (4)	C34—H34B	0.9800
C6—H6	0.9500	C34—H34C	0.9800
C11—C14	1.535 (4)	C51—C53	1.527 (4)
C11—C13	1.541 (4)	C51—C54	1.534 (4)
C11—C12	1.545 (4)	C51—C52	1.547 (4)
C12—C12^i	1.528 (5)	C52—H52A	0.9800
C12—H12A	0.9900	C52—H52B	0.9800
C12—H12B	0.9900	C52—H52C	0.9800
C13—H13A	0.9800	C53—H53A	0.9800
C13—H13B	0.9800	C53—H53C	0.9800
C13—H13C	0.9800	C53—H53B	0.9800
C14—H14A	0.9800	C54—H54A	0.9800
C14—H14B	0.9800	C54—H54B	0.9800
C14—H14C	0.9800	C54—H54C	0.9800
C6—C1—C2	118.0 (2)	C3—C31—C32	109.4 (2)
C6—C1—C11	122.6 (2)	C33—C31—C32	107.9 (3)
C2—C1—C11	119.4 (2)	C34—C31—C32	109.2 (2)
C3—C2—C1	122.2 (2)	C31—C32—H32A	109.5
C3—C2—H2	118.9	C31—C32—H32B	109.5
C1—C2—H2	118.9	H32A—C32—H32B	109.5
C2—C3—C4	117.7 (2)	C31—C32—H32C	109.5
C2—C3—C31	123.0 (2)	H32A—C32—H32C	109.5
C4—C3—C31	119.3 (2)	H32B—C32—H32C	109.5
C5—C4—C3	122.1 (2)	C31—C33—H33A	109.5
C5—C4—H4	118.9	C31—C33—H33B	109.5
C3—C4—H4	118.9	H33A—C33—H33B	109.5
C4—C5—C6	118.2 (2)	C31—C33—H33C	109.5
C4—C5—C51	122.3 (2)	H33A—C33—H33C	109.5
C6—C5—C51	119.5 (2)	H33B—C33—H33C	109.5
C1—C6—C5	121.8 (2)	C31—C34—H34A	109.5
C1—C6—H6	119.1	C31—C34—H34B	109.5
C5—C6—H6	119.1	H34A—C34—H34B	109.5
C1—C11—C14	113.0 (2)	C31—C34—H34C	109.5
C1—C11—C13	108.2 (2)	H34A—C34—H34C	109.5
C14—C11—C13	107.7 (2)	H34B—C34—H34C	109.5
C1—C11—C12	110.3 (2)	C53—C51—C5	113.0 (2)
C14—C11—C12	109.5 (2)	C53—C51—C54	108.1 (3)
C13—C11—C12	107.9 (2)	C5—C51—C54	109.7 (2)
C12^i—C12—C11	114.7 (3)	C53—C51—C52	108.3 (3)
C12^i—C12—H12A	108.6	C5—C51—C52	108.6 (2)
C11—C12—H12A	108.6	C54—C51—C52	109.0 (3)
C12^i—C12—H12B	108.6	C51—C52—H52A	109.5
C11—C12—H12B	108.6	C51—C52—H52B	109.5
H12A—C12—H12B	107.6	H52A—C52—H52B	109.5
C11—C13—H13A	109.5	C51—C52—H52C	109.5
C11—C13—H13B	109.5	H52A—C52—H52C	109.5
H13A—C13—H13B	109.5	H52B—C52—H52C	109.5
C11—C13—H13C	109.5	C51—C53—H53A	109.5
H13A—C13—H13C	109.5	C51—C53—H53C	109.5
H13B—C13—H13C	109.5	H53A—C53—H53C	109.5
C11—C14—H14A	109.5	C51—C53—H53B	109.5
C11—C14—H14B	109.5	H53A—C53—H53B	109.5
H14A—C14—H14B	109.5	H53C—C53—H53B	109.5
C11—C14—H14C	109.5	C51—C54—H54A	109.5
H14A—C14—H14C	109.5	C51—C54—H54B	109.5
H14B—C14—H14C	109.5	H54A—C54—H54B	109.5
C3—C31—C33	112.8 (2)	C51—C54—H54C	109.5
C3—C31—C34	109.4 (2)	H54A—C54—H54C	109.5
C33—C31—C34	108.1 (3)	H54B—C54—H54C	109.5
C6—C1—C2—C3	0.5 (4)	C2—C1—C11—C12	53.0 (3)
C11—C1—C2—C3	178.7 (2)	C1—C11—C12—C12^i	60.2 (4)
C1—C2—C3—C4	−1.0 (4)	C14—C11—C12—C12^i	−64.8 (3)
C1—C2—C3—C31	179.8 (2)	C13—C11—C12—C12^i	178.2 (3)
C2—C3—C4—C5	0.9 (4)	C2—C3—C31—C33	−1.4 (4)
C31—C3—C4—C5	−179.8 (2)	C4—C3—C31—C33	179.4 (3)
C3—C4—C5—C6	−0.3 (4)	C2—C3—C31—C34	119.0 (3)
C3—C4—C5—C51	179.2 (2)	C4—C3—C31—C34	−60.2 (3)
C2—C1—C6—C5	0.1 (4)	C2—C3—C31—C32	−121.5 (3)
C11—C1—C6—C5	−178.1 (2)	C4—C3—C31—C32	59.3 (3)
C4—C5—C6—C1	−0.2 (4)	C4—C5—C51—C53	−2.9 (4)
C51—C5—C6—C1	−179.7 (2)	C6—C5—C51—C53	176.6 (3)
C6—C1—C11—C14	−5.8 (3)	C4—C5—C51—C54	−123.6 (3)
C2—C1—C11—C14	176.0 (2)	C6—C5—C51—C54	55.9 (3)
C6—C1—C11—C13	113.4 (3)	C4—C5—C51—C52	117.4 (3)
C2—C1—C11—C13	−64.8 (3)	C6—C5—C51—C52	−63.1 (3)
C6—C1—C11—C12	−128.8 (3)

Symmetry code: (i) −x+1, −y+1, −z+2.

2,15-di-(tert-butyl)-hexahelicene (Va)

Crystal data

C34H31.98I0.02	F(000) = 1896
Mr = 443.11	Dx = 1.197 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 6810 reflections
a = 9.7668 (8) Å	θ = 2.5–28.0°
b = 16.5318 (14) Å	µ = 0.09 mm^−1
c = 30.463 (3) Å	T = 100 K
V = 4918.7 (7) Å^3	Parallelipip, colourless
Z = 8	0.58 × 0.15 × 0.15 mm

Data collection

CCD area detector diffractometer	6020 independent reflections
Radiation source: fine-focus sealed tube	4289 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
phi and ω scans	θmax = 28.3°, θmin = 2.5°
Absorption correction: multi-scan SADABS (Bruker)	h = −12→13
Tmin = 0.776, Tmax = 0.99	k = −17→21
30137 measured reflections	l = −33→40

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.127	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0466P)^2 + 2.971P] where P = (Fo^2 + 2Fc^2)/3
6020 reflections	(Δ/σ)max = 0.006
331 parameters	Δρmax = 0.30 e Å^−3
0 restraints	Δρmin = −0.21 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. After solution and refinement of the carbon and hydrogen framework, two peaks of about the same size remained in the difference map. The distance from each peak to nearby carbon atoms suggested iodine,and since iodine had been present in the synthesis, the peaks were refined as iodine atoms. The final occupancy of each iodine was 0.01 and that of the two H atoms (H4 and H13,bound to the respective C4 and C13 atoms near I1 and I2) was 0.99.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.42143 (15)	0.98285 (8)	0.38360 (5)	0.0198 (3)
H1	0.4796	0.9421	0.3720	0.024*
C2	0.39361 (15)	1.05009 (8)	0.35827 (5)	0.0200 (3)
C3	0.30555 (16)	1.11013 (9)	0.37592 (5)	0.0247 (3)
H3	0.2807	1.1554	0.3584	0.030*
C4	0.25612 (17)	1.10373 (9)	0.41761 (5)	0.0270 (3)
H4	0.1986	1.1451	0.4289	0.032*	0.99
C5	0.25472 (19)	1.03573 (10)	0.48991 (5)	0.0312 (4)
H5	0.1962	1.0762	0.5017	0.037*
C6	0.30583 (18)	0.97723 (10)	0.51624 (5)	0.0316 (4)
H6	0.2921	0.9810	0.5470	0.038*
C7	0.44053 (17)	0.85303 (10)	0.52800 (5)	0.0298 (4)
H7	0.4271	0.8582	0.5588	0.036*
C8	0.51721 (17)	0.79146 (10)	0.51217 (5)	0.0298 (4)
H8	0.5669	0.7581	0.5319	0.036*
C9	0.60791 (17)	0.71216 (10)	0.45051 (6)	0.0315 (4)
H9	0.6560	0.6791	0.4708	0.038*
C10	0.62009 (17)	0.69759 (10)	0.40712 (6)	0.0306 (4)
H10	0.6866	0.6601	0.3969	0.037*
C11	0.54135 (16)	0.71870 (9)	0.33095 (6)	0.0290 (4)
H11	0.6114	0.6834	0.3209	0.035*
C12	0.45160 (16)	0.74935 (9)	0.30182 (5)	0.0273 (3)
H12	0.4645	0.7402	0.2713	0.033*
C13	0.22956 (17)	0.81765 (9)	0.28812 (5)	0.0269 (3)
H13	0.2384	0.8069	0.2576	0.032*	0.99
C14	0.11324 (17)	0.85404 (9)	0.30331 (5)	0.0263 (3)
H14	0.0438	0.8695	0.2831	0.032*
C15	0.09462 (15)	0.86914 (9)	0.34870 (5)	0.0226 (3)
C16	0.20096 (15)	0.85015 (8)	0.37659 (5)	0.0207 (3)
H16	0.1901	0.8604	0.4071	0.025*
C17	0.32570 (15)	0.81603 (8)	0.36183 (5)	0.0201 (3)
C18	0.33681 (16)	0.79572 (9)	0.31671 (5)	0.0235 (3)
C19	0.43738 (15)	0.79571 (8)	0.39147 (5)	0.0214 (3)
C20	0.53386 (15)	0.73804 (9)	0.37651 (5)	0.0253 (3)
C21	0.45044 (15)	0.82558 (9)	0.43629 (5)	0.0227 (3)
C22	0.52428 (16)	0.77624 (9)	0.46641 (5)	0.0268 (3)
C23	0.39589 (15)	0.90128 (9)	0.45302 (5)	0.0221 (3)
C24	0.37987 (16)	0.90996 (9)	0.49897 (5)	0.0257 (3)
C25	0.36659 (15)	0.97226 (9)	0.42623 (5)	0.0214 (3)
C26	0.28896 (16)	1.03659 (9)	0.44440 (5)	0.0253 (3)
C27	0.45715 (15)	1.06326 (9)	0.31291 (5)	0.0214 (3)
C28	0.55188 (18)	1.13719 (10)	0.31516 (6)	0.0323 (4)
H28A	0.4981	1.1853	0.3226	0.048*
H28B	0.5961	1.1452	0.2866	0.048*
H28C	0.6220	1.1283	0.3377	0.048*
C29	0.34299 (17)	1.07848 (11)	0.27917 (5)	0.0313 (4)
H29A	0.2833	1.0309	0.2776	0.047*
H29B	0.3838	1.0885	0.2503	0.047*
H29C	0.2891	1.1257	0.2881	0.047*
C30	0.54063 (17)	0.99063 (9)	0.29742 (5)	0.0269 (3)
H30A	0.6180	0.9821	0.3174	0.040*
H30B	0.5750	1.0008	0.2677	0.040*
H30C	0.4825	0.9423	0.2972	0.040*
C31	−0.03966 (16)	0.90579 (10)	0.36487 (5)	0.0273 (3)
C32	−0.05637 (19)	0.99029 (10)	0.34504 (7)	0.0382 (4)
H32A	0.0203	1.0246	0.3543	0.057*
H32B	−0.1426	1.0141	0.3552	0.057*
H32C	−0.0575	0.9863	0.3129	0.057*
C33	−0.0433 (2)	0.91473 (17)	0.41459 (7)	0.0622 (7)
H33A	−0.0345	0.8613	0.4283	0.093*
H33B	−0.1303	0.9393	0.4234	0.093*
H33C	0.0326	0.9493	0.4241	0.093*
C34	−0.16002 (19)	0.85290 (12)	0.35022 (9)	0.0519 (6)
H34A	−0.1639	0.8516	0.3181	0.078*
H34B	−0.2456	0.8754	0.3618	0.078*
H34C	−0.1476	0.7978	0.3614	0.078*
I1	0.1778 (13)	1.1569 (8)	0.4690 (4)	0.044 (3)	0.01
I2	0.2492 (15)	0.8070 (8)	0.2351 (4)	0.046 (3)	0.01

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0212 (7)	0.0168 (7)	0.0213 (7)	0.0002 (5)	0.0003 (5)	−0.0020 (5)
C2	0.0222 (7)	0.0173 (7)	0.0206 (7)	−0.0019 (5)	−0.0032 (5)	−0.0018 (5)
C3	0.0313 (8)	0.0176 (7)	0.0252 (8)	0.0040 (6)	−0.0035 (6)	0.0004 (6)
C4	0.0342 (8)	0.0207 (7)	0.0262 (8)	0.0073 (6)	0.0009 (6)	−0.0030 (6)
C5	0.0404 (9)	0.0276 (8)	0.0256 (8)	0.0070 (7)	0.0078 (7)	−0.0023 (6)
C6	0.0412 (10)	0.0322 (9)	0.0213 (8)	0.0023 (7)	0.0056 (7)	−0.0003 (6)
C7	0.0324 (9)	0.0337 (9)	0.0232 (8)	−0.0017 (7)	−0.0001 (6)	0.0069 (7)
C8	0.0291 (8)	0.0303 (8)	0.0302 (8)	−0.0004 (7)	−0.0036 (7)	0.0112 (7)
C9	0.0251 (8)	0.0253 (8)	0.0442 (10)	0.0042 (6)	−0.0013 (7)	0.0077 (7)
C10	0.0237 (8)	0.0227 (8)	0.0454 (10)	0.0044 (6)	0.0034 (7)	0.0012 (7)
C11	0.0254 (8)	0.0207 (7)	0.0410 (9)	−0.0009 (6)	0.0088 (7)	−0.0068 (7)
C12	0.0304 (8)	0.0227 (7)	0.0290 (8)	−0.0057 (6)	0.0088 (6)	−0.0069 (6)
C13	0.0340 (9)	0.0250 (8)	0.0218 (7)	−0.0068 (7)	0.0023 (6)	−0.0027 (6)
C14	0.0288 (8)	0.0234 (8)	0.0266 (8)	−0.0049 (6)	−0.0042 (6)	0.0020 (6)
C15	0.0239 (7)	0.0168 (7)	0.0273 (8)	−0.0019 (6)	0.0006 (6)	0.0042 (6)
C16	0.0245 (7)	0.0156 (6)	0.0221 (7)	−0.0004 (5)	0.0029 (6)	0.0018 (5)
C17	0.0217 (7)	0.0135 (6)	0.0251 (7)	−0.0031 (5)	0.0019 (6)	0.0005 (5)
C18	0.0265 (8)	0.0171 (7)	0.0269 (8)	−0.0059 (6)	0.0043 (6)	−0.0019 (6)
C19	0.0200 (7)	0.0156 (6)	0.0286 (8)	−0.0005 (5)	0.0036 (6)	0.0024 (6)
C20	0.0214 (7)	0.0178 (7)	0.0366 (9)	−0.0007 (6)	0.0042 (6)	−0.0006 (6)
C21	0.0197 (7)	0.0209 (7)	0.0275 (8)	−0.0007 (6)	0.0016 (6)	0.0046 (6)
C22	0.0232 (8)	0.0241 (8)	0.0331 (9)	0.0002 (6)	0.0000 (6)	0.0061 (6)
C23	0.0212 (7)	0.0233 (7)	0.0219 (7)	0.0005 (6)	0.0005 (6)	0.0024 (6)
C24	0.0269 (8)	0.0265 (8)	0.0238 (8)	−0.0012 (6)	0.0024 (6)	0.0038 (6)
C25	0.0239 (7)	0.0192 (7)	0.0211 (7)	0.0002 (6)	−0.0005 (6)	−0.0004 (6)
C26	0.0303 (8)	0.0225 (7)	0.0233 (8)	0.0028 (6)	0.0021 (6)	−0.0014 (6)
C27	0.0250 (7)	0.0200 (7)	0.0191 (7)	−0.0017 (6)	−0.0019 (6)	0.0022 (5)
C28	0.0392 (9)	0.0258 (8)	0.0319 (9)	−0.0102 (7)	−0.0006 (7)	0.0052 (7)
C29	0.0331 (9)	0.0379 (9)	0.0228 (8)	0.0051 (7)	−0.0055 (7)	−0.0016 (7)
C30	0.0298 (8)	0.0269 (8)	0.0239 (8)	0.0006 (6)	0.0063 (6)	0.0035 (6)
C31	0.0243 (8)	0.0261 (8)	0.0314 (8)	0.0052 (6)	0.0000 (6)	0.0052 (6)
C32	0.0370 (10)	0.0244 (8)	0.0531 (11)	0.0055 (7)	−0.0020 (8)	0.0052 (8)
C33	0.0466 (12)	0.104 (2)	0.0356 (11)	0.0478 (13)	0.0114 (9)	0.0134 (12)
C34	0.0262 (9)	0.0311 (10)	0.0985 (18)	−0.0015 (8)	0.0081 (10)	−0.0052 (10)
I1	0.041 (7)	0.043 (7)	0.048 (7)	0.005 (6)	−0.002 (5)	−0.006 (6)
I2	0.057 (8)	0.045 (7)	0.038 (6)	0.008 (6)	−0.006 (6)	−0.016 (5)

Geometric parameters (Å, º)

C1—C2	1.3802 (19)	C16—C17	1.416 (2)
C1—C25	1.416 (2)	C16—H16	0.9500
C1—H1	0.9500	C17—C18	1.419 (2)
C2—C3	1.419 (2)	C17—C19	1.455 (2)
C2—C27	1.530 (2)	C19—C20	1.416 (2)
C3—C4	1.363 (2)	C19—C21	1.458 (2)
C3—H3	0.9500	C21—C22	1.424 (2)
C4—C26	1.415 (2)	C21—C23	1.452 (2)
C4—H4	0.9500	C23—C24	1.416 (2)
C5—C6	1.352 (2)	C23—C25	1.458 (2)
C5—C26	1.426 (2)	C25—C26	1.418 (2)
C5—H5	0.9500	C27—C30	1.526 (2)
C6—C24	1.427 (2)	C27—C28	1.535 (2)
C6—H6	0.9500	C27—C29	1.537 (2)
C7—C8	1.352 (2)	C28—H28A	0.9800
C7—C24	1.421 (2)	C28—H28B	0.9800
C7—H7	0.9500	C28—H28C	0.9800
C8—C22	1.418 (2)	C29—H29A	0.9800
C8—H8	0.9500	C29—H29B	0.9800
C9—C10	1.349 (2)	C29—H29C	0.9800
C9—C22	1.423 (2)	C30—H30A	0.9800
C9—H9	0.9500	C30—H30B	0.9800
C10—C20	1.423 (2)	C30—H30C	0.9800
C10—H10	0.9500	C31—C33	1.522 (3)
C11—C12	1.346 (2)	C31—C32	1.531 (2)
C11—C20	1.426 (2)	C31—C34	1.531 (2)
C11—H11	0.9500	C32—H32A	0.9800
C12—C18	1.432 (2)	C32—H32B	0.9800
C12—H12	0.9500	C32—H32C	0.9800
C13—C14	1.366 (2)	C33—H33A	0.9800
C13—C18	1.410 (2)	C33—H33B	0.9800
C13—H13	0.9500	C33—H33C	0.9800
C14—C15	1.417 (2)	C34—H34A	0.9800
C14—H14	0.9500	C34—H34B	0.9800
C15—C16	1.378 (2)	C34—H34C	0.9800
C15—C31	1.526 (2)
C2—C1—C25	122.55 (13)	C15—C16—C17	122.92 (14)
C2—C1—H1	118.7	C15—C16—H16	118.5
C25—C1—H1	118.7	C17—C16—H16	118.5
C1—C2—C3	118.09 (13)	C16—C17—C18	117.88 (13)
C1—C2—C27	122.66 (13)	C16—C17—C19	122.68 (13)
C3—C2—C27	119.23 (13)	C18—C17—C19	119.27 (13)
C4—C3—C2	120.89 (14)	C13—C18—C17	118.74 (14)
C4—C3—H3	119.6	C13—C18—C12	121.57 (14)
C2—C3—H3	119.6	C17—C18—C12	119.57 (14)
C3—C4—C26	121.21 (14)	C20—C19—C17	117.04 (13)
C3—C4—H4	119.4	C20—C19—C21	118.13 (14)
C26—C4—H4	119.4	C17—C19—C21	124.65 (13)
C6—C5—C26	119.82 (15)	C19—C20—C10	119.95 (15)
C6—C5—H5	120.1	C19—C20—C11	119.89 (14)
C26—C5—H5	120.1	C10—C20—C11	120.13 (14)
C5—C6—C24	121.72 (15)	C22—C21—C23	116.96 (14)
C5—C6—H6	119.1	C22—C21—C19	116.99 (13)
C24—C6—H6	119.1	C23—C21—C19	126.05 (13)
C8—C7—C24	120.51 (15)	C8—C22—C9	119.65 (15)
C8—C7—H7	119.7	C8—C22—C21	120.47 (15)
C24—C7—H7	119.7	C9—C22—C21	119.87 (15)
C7—C8—C22	120.72 (15)	C24—C23—C21	118.35 (13)
C7—C8—H8	119.6	C24—C23—C25	116.76 (13)
C22—C8—H8	119.6	C21—C23—C25	124.69 (13)
C10—C9—C22	121.15 (15)	C23—C24—C7	120.13 (14)
C10—C9—H9	119.4	C23—C24—C6	119.97 (14)
C22—C9—H9	119.4	C7—C24—C6	119.88 (15)
C9—C10—C20	120.39 (15)	C1—C25—C26	117.86 (13)
C9—C10—H10	119.8	C1—C25—C23	122.61 (13)
C20—C10—H10	119.8	C26—C25—C23	119.35 (13)
C12—C11—C20	121.58 (14)	C4—C26—C25	118.98 (14)
C12—C11—H11	119.2	C4—C26—C5	121.02 (14)
C20—C11—H11	119.2	C25—C26—C5	119.81 (14)
C11—C12—C18	120.16 (15)	C30—C27—C2	112.57 (12)
C11—C12—H12	119.9	C30—C27—C28	108.56 (13)
C18—C12—H12	119.9	C2—C27—C28	108.50 (12)
C14—C13—C18	121.44 (14)	C30—C27—C29	108.04 (12)
C14—C13—H13	119.3	C2—C27—C29	109.45 (12)
C18—C13—H13	119.3	C28—C27—C29	109.68 (13)
C13—C14—C15	121.00 (15)	C33—C31—C15	112.31 (13)
C13—C14—H14	119.5	C33—C31—C32	107.55 (16)
C15—C14—H14	119.5	C15—C31—C32	109.06 (13)
C16—C15—C14	117.70 (14)	C33—C31—C34	109.12 (18)
C16—C15—C31	122.62 (14)	C15—C31—C34	109.81 (13)
C14—C15—C31	119.68 (14)	C32—C31—C34	108.92 (15)
C25—C1—C2—C3	−0.5 (2)	C10—C9—C22—C21	0.8 (2)
C25—C1—C2—C27	177.57 (13)	C23—C21—C22—C8	14.0 (2)
C1—C2—C3—C4	3.6 (2)	C19—C21—C22—C8	−166.41 (14)
C27—C2—C3—C4	−174.54 (14)	C23—C21—C22—C9	−164.78 (14)
C2—C3—C4—C26	−1.0 (2)	C19—C21—C22—C9	14.8 (2)
C26—C5—C6—C24	−7.9 (3)	C22—C21—C23—C24	−19.8 (2)
C24—C7—C8—C22	−8.2 (3)	C19—C21—C23—C24	160.67 (14)
C22—C9—C10—C20	−9.5 (2)	C22—C21—C23—C25	154.85 (14)
C20—C11—C12—C18	−6.6 (2)	C19—C21—C23—C25	−24.7 (2)
C18—C13—C14—C15	−1.7 (2)	C21—C23—C24—C7	12.3 (2)
C13—C14—C15—C16	3.7 (2)	C25—C23—C24—C7	−162.75 (14)
C13—C14—C15—C31	−176.75 (14)	C21—C23—C24—C6	−169.43 (14)
C14—C15—C16—C17	−0.5 (2)	C25—C23—C24—C6	15.5 (2)
C31—C15—C16—C17	179.90 (13)	C8—C7—C24—C23	1.9 (2)
C15—C16—C17—C18	−4.4 (2)	C8—C7—C24—C6	−176.40 (16)
C15—C16—C17—C19	−179.67 (13)	C5—C6—C24—C23	−2.9 (3)
C14—C13—C18—C17	−3.4 (2)	C5—C6—C24—C7	175.34 (17)
C14—C13—C18—C12	172.68 (14)	C2—C1—C25—C26	−5.0 (2)
C16—C17—C18—C13	6.2 (2)	C2—C1—C25—C23	180.00 (14)
C19—C17—C18—C13	−178.32 (13)	C24—C23—C25—C1	157.25 (14)
C16—C17—C18—C12	−169.89 (13)	C21—C23—C25—C1	−17.4 (2)
C19—C17—C18—C12	5.6 (2)	C24—C23—C25—C26	−17.7 (2)
C11—C12—C18—C13	−169.70 (15)	C21—C23—C25—C26	167.60 (14)
C11—C12—C18—C17	6.3 (2)	C3—C4—C26—C25	−4.6 (2)
C16—C17—C19—C20	158.54 (13)	C3—C4—C26—C5	170.40 (16)
C18—C17—C19—C20	−16.68 (19)	C1—C25—C26—C4	7.4 (2)
C16—C17—C19—C21	−16.4 (2)	C23—C25—C26—C4	−177.39 (14)
C18—C17—C19—C21	168.36 (13)	C1—C25—C26—C5	−167.65 (15)
C17—C19—C20—C10	−161.40 (14)	C23—C25—C26—C5	7.5 (2)
C21—C19—C20—C10	13.9 (2)	C6—C5—C26—C4	−169.49 (17)
C17—C19—C20—C11	16.6 (2)	C6—C5—C26—C25	5.5 (3)
C21—C19—C20—C11	−168.11 (13)	C1—C2—C27—C30	6.0 (2)
C9—C10—C20—C19	1.9 (2)	C3—C2—C27—C30	−175.89 (13)
C9—C10—C20—C11	−176.10 (15)	C1—C2—C27—C28	−114.14 (15)
C12—C11—C20—C19	−5.2 (2)	C3—C2—C27—C28	63.93 (17)
C12—C11—C20—C10	172.80 (15)	C1—C2—C27—C29	126.20 (15)
C20—C19—C21—C22	−21.8 (2)	C3—C2—C27—C29	−55.72 (17)
C17—C19—C21—C22	153.08 (14)	C16—C15—C31—C33	−2.6 (2)
C20—C19—C21—C23	157.73 (14)	C14—C15—C31—C33	177.84 (17)
C17—C19—C21—C23	−27.4 (2)	C16—C15—C31—C32	116.52 (16)
C7—C8—C22—C9	178.70 (15)	C14—C15—C31—C32	−63.04 (18)
C7—C8—C22—C21	−0.1 (2)	C16—C15—C31—C34	−124.20 (17)
C10—C9—C22—C8	−178.02 (16)	C14—C15—C31—C34	56.24 (19)

2,15-di-(tert-butyl)-hexahelicene (Vahigh)

Crystal data

C34H31.98I0.02	F(000) = 1896
Mr = 443.11	Dx = 1.197 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 6810 reflections
a = 9.7668 (8) Å	θ = 2.5–28.0°
b = 16.5318 (14) Å	µ = 0.09 mm^−1
c = 30.463 (3) Å	T = 100 K
V = 4918.7 (7) Å^3	Parallelipip, colourless
Z = 8	0.58 × 0.15 × 0.15 mm

Data collection

CCD area detector diffractometer	4540 independent reflections
Radiation source: fine-focus sealed tube	2945 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.082
phi and ω scans	θmax = 28.3°, θmin = 17.2°
Absorption correction: multi-scan SADABS (Bruker)	h = −12→13
Tmin = 0.776, Tmax = 0.99	k = −17→21
19817 measured reflections	l = −33→40

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.131	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0328P)^2 + 2.4391P] where P = (Fo^2 + 2Fc^2)/3
4540 reflections	(Δ/σ)max = 0.001
331 parameters	Δρmax = 0.19 e Å^−3
0 restraints	Δρmin = −0.17 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 reflections with d= 1.2 to 0 (theta_min 17.23, 331 parameters). The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.42158 (17)	0.98265 (10)	0.38346 (6)	0.0169 (3)
H1	0.4797	0.9419	0.3718	0.020*
C2	0.39352 (17)	1.05013 (10)	0.35828 (5)	0.0172 (3)
C3	0.3053 (2)	1.11030 (10)	0.37581 (6)	0.0217 (4)
H3	0.2806	1.1555	0.3583	0.026*
C4	0.2556 (2)	1.10393 (11)	0.41764 (6)	0.0240 (4)
H4	0.1981	1.1453	0.4289	0.029*	0.99
C5	0.2543 (2)	1.03582 (12)	0.48990 (7)	0.0279 (4)
H5	0.1955	1.0762	0.5016	0.033*
C6	0.3059 (2)	0.97709 (13)	0.51645 (6)	0.0285 (4)
H6	0.2927	0.9808	0.5473	0.034*
C7	0.4403 (2)	0.85291 (13)	0.52824 (6)	0.0264 (4)
H7	0.4266	0.8581	0.5590	0.032*
C8	0.5175 (2)	0.79128 (12)	0.51230 (7)	0.0266 (4)
H8	0.5675	0.7579	0.5320	0.032*
C9	0.6083 (2)	0.71176 (12)	0.45050 (8)	0.0283 (4)
H9	0.6561	0.6786	0.4708	0.034*
C10	0.6204 (2)	0.69749 (12)	0.40711 (8)	0.0279 (4)
H10	0.6871	0.6602	0.3969	0.033*
C11	0.5418 (2)	0.71847 (11)	0.33087 (7)	0.0258 (4)
H11	0.6119	0.6831	0.3209	0.031*
C12	0.4515 (2)	0.74940 (11)	0.30160 (6)	0.0245 (4)
H12	0.4642	0.7404	0.2711	0.029*
C13	0.2296 (2)	0.81750 (11)	0.28789 (6)	0.0237 (4)
H13	0.2385	0.8066	0.2574	0.028*	0.99
C14	0.1126 (2)	0.85413 (11)	0.30327 (6)	0.0234 (4)
H14	0.0430	0.8696	0.2832	0.028*
C15	0.09460 (18)	0.86909 (10)	0.34863 (6)	0.0200 (4)
C16	0.20106 (18)	0.85020 (10)	0.37674 (6)	0.0178 (3)
H16	0.1902	0.8605	0.4072	0.021*
C17	0.32575 (17)	0.81602 (9)	0.36185 (6)	0.0174 (3)
C18	0.33696 (19)	0.79576 (10)	0.31673 (6)	0.0206 (4)
C19	0.43737 (17)	0.79575 (10)	0.39145 (6)	0.0186 (3)
C20	0.53392 (18)	0.73793 (10)	0.37654 (7)	0.0223 (4)
C21	0.45040 (17)	0.82555 (10)	0.43633 (6)	0.0201 (4)
C22	0.52427 (19)	0.77628 (11)	0.46630 (7)	0.0239 (4)
C23	0.39582 (17)	0.90123 (11)	0.45306 (6)	0.0192 (3)
C24	0.37973 (19)	0.90993 (11)	0.49889 (6)	0.0227 (4)
C25	0.36647 (17)	0.97222 (10)	0.42623 (6)	0.0184 (3)
C26	0.28865 (19)	1.03647 (11)	0.44437 (6)	0.0224 (4)
C27	0.45714 (18)	1.06330 (10)	0.31286 (5)	0.0185 (3)
C28	0.5522 (2)	1.13709 (12)	0.31513 (7)	0.0288 (4)
H28A	0.4986	1.1853	0.3226	0.043*
H28B	0.5966	1.1450	0.2866	0.043*
H28C	0.6222	1.1281	0.3377	0.043*
C29	0.3429 (2)	1.07870 (13)	0.27907 (6)	0.0282 (4)
H29A	0.2821	1.0316	0.2778	0.042*
H29B	0.3836	1.0878	0.2501	0.042*
H29C	0.2901	1.1265	0.2878	0.042*
C30	0.5408 (2)	0.99042 (11)	0.29738 (6)	0.0236 (4)
H30A	0.6194	0.9827	0.3169	0.035*
H30B	0.5733	1.0000	0.2674	0.035*
H30C	0.4832	0.9419	0.2979	0.035*
C31	−0.03960 (19)	0.90577 (12)	0.36484 (6)	0.0240 (4)
C32	−0.0560 (2)	0.99037 (13)	0.34489 (9)	0.0345 (5)
H32A	0.0195	1.0250	0.3547	0.052*
H32B	−0.1433	1.0138	0.3544	0.052*
H32C	−0.0546	0.9864	0.3128	0.052*
C33	−0.0429 (3)	0.9152 (3)	0.41466 (9)	0.0572 (10)
H33A	−0.0399	0.8617	0.4284	0.086*
H33B	−0.1273	0.9430	0.4233	0.086*
H33C	0.0364	0.9470	0.4242	0.086*
C34	−0.1603 (2)	0.85274 (15)	0.35004 (13)	0.0469 (7)
H34A	−0.1688	0.8551	0.3180	0.070*
H34B	−0.2450	0.8726	0.3635	0.070*
H34C	−0.1442	0.7967	0.3591	0.070*
I1	0.1771 (15)	1.1587 (9)	0.4689 (5)	0.035 (3)	0.01
I2	0.2481 (17)	0.8073 (8)	0.2348 (4)	0.035 (3)	0.01

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0185 (7)	0.0136 (7)	0.0186 (8)	0.0005 (5)	0.0006 (5)	−0.0012 (5)
C2	0.0199 (7)	0.0148 (7)	0.0170 (7)	−0.0014 (6)	−0.0030 (6)	−0.0013 (5)
C3	0.0283 (8)	0.0141 (7)	0.0226 (8)	0.0043 (6)	−0.0029 (6)	0.0002 (6)
C4	0.0318 (9)	0.0174 (8)	0.0228 (8)	0.0075 (6)	0.0006 (7)	−0.0026 (6)
C5	0.0380 (10)	0.0235 (8)	0.0220 (9)	0.0072 (7)	0.0073 (7)	−0.0011 (7)
C6	0.0384 (10)	0.0288 (9)	0.0185 (8)	0.0032 (8)	0.0055 (7)	0.0005 (7)
C7	0.0303 (9)	0.0292 (9)	0.0198 (8)	−0.0007 (7)	−0.0002 (6)	0.0061 (7)
C8	0.0265 (9)	0.0265 (9)	0.0266 (9)	0.0002 (7)	−0.0032 (7)	0.0106 (7)
C9	0.0221 (8)	0.0227 (8)	0.0403 (11)	0.0045 (7)	−0.0015 (7)	0.0069 (7)
C10	0.0216 (8)	0.0196 (8)	0.0425 (11)	0.0047 (6)	0.0032 (7)	0.0010 (7)
C11	0.0224 (8)	0.0188 (8)	0.0363 (10)	−0.0006 (6)	0.0077 (7)	−0.0062 (7)
C12	0.0266 (8)	0.0201 (8)	0.0268 (9)	−0.0050 (7)	0.0082 (7)	−0.0072 (6)
C13	0.0301 (9)	0.0222 (8)	0.0188 (8)	−0.0058 (7)	0.0023 (6)	−0.0029 (6)
C14	0.0254 (8)	0.0207 (8)	0.0242 (9)	−0.0043 (6)	−0.0039 (6)	0.0016 (6)
C15	0.0204 (8)	0.0150 (7)	0.0246 (9)	−0.0012 (6)	0.0004 (6)	0.0040 (6)
C16	0.0207 (8)	0.0134 (7)	0.0191 (7)	0.0003 (6)	0.0025 (6)	0.0024 (5)
C17	0.0188 (7)	0.0120 (7)	0.0213 (8)	−0.0024 (5)	0.0017 (6)	0.0003 (5)
C18	0.0235 (8)	0.0150 (7)	0.0234 (8)	−0.0049 (6)	0.0046 (6)	−0.0020 (6)
C19	0.0168 (7)	0.0130 (7)	0.0259 (8)	0.0004 (5)	0.0031 (6)	0.0018 (6)
C20	0.0187 (8)	0.0155 (7)	0.0328 (9)	0.0005 (6)	0.0040 (6)	−0.0010 (6)
C21	0.0177 (7)	0.0178 (7)	0.0247 (8)	−0.0003 (6)	0.0012 (6)	0.0040 (6)
C22	0.0212 (8)	0.0211 (8)	0.0294 (9)	0.0016 (6)	0.0002 (6)	0.0051 (7)
C23	0.0191 (7)	0.0198 (8)	0.0187 (8)	0.0008 (6)	0.0006 (6)	0.0024 (6)
C24	0.0244 (8)	0.0233 (8)	0.0203 (8)	−0.0005 (7)	0.0022 (6)	0.0041 (6)
C25	0.0212 (7)	0.0168 (7)	0.0173 (8)	0.0009 (6)	0.0000 (6)	−0.0001 (6)
C26	0.0278 (8)	0.0193 (8)	0.0202 (8)	0.0034 (6)	0.0022 (6)	−0.0008 (6)
C27	0.0217 (8)	0.0173 (7)	0.0164 (7)	−0.0017 (6)	−0.0017 (6)	0.0021 (5)
C28	0.0359 (10)	0.0219 (8)	0.0286 (9)	−0.0105 (7)	0.0000 (7)	0.0046 (7)
C29	0.0298 (9)	0.0350 (10)	0.0198 (8)	0.0049 (7)	−0.0058 (7)	−0.0011 (7)
C30	0.0270 (8)	0.0232 (8)	0.0206 (8)	0.0010 (7)	0.0067 (6)	0.0033 (6)
C31	0.0209 (8)	0.0232 (8)	0.0280 (9)	0.0050 (7)	−0.0001 (6)	0.0045 (6)
C32	0.0337 (10)	0.0205 (9)	0.0494 (12)	0.0055 (7)	−0.0009 (9)	0.0060 (8)
C33	0.0429 (13)	0.100 (3)	0.0289 (12)	0.0463 (16)	0.0100 (9)	0.0126 (13)
C34	0.0224 (9)	0.0270 (10)	0.091 (2)	−0.0020 (8)	0.0073 (11)	−0.0069 (11)
I1	0.032 (6)	0.037 (7)	0.037 (7)	0.004 (5)	−0.002 (5)	−0.007 (5)
I2	0.049 (7)	0.029 (6)	0.027 (6)	0.009 (5)	−0.006 (5)	−0.005 (5)

Geometric parameters (Å, º)

C1—C2	1.381 (2)	C16—C17	1.417 (2)
C1—C25	1.420 (2)	C16—H16	0.9500
C1—H1	0.9500	C17—C18	1.419 (3)
C2—C3	1.420 (2)	C17—C19	1.454 (2)
C2—C27	1.532 (2)	C19—C20	1.417 (2)
C3—C4	1.368 (3)	C19—C21	1.459 (3)
C3—H3	0.9500	C21—C22	1.420 (3)
C4—C26	1.418 (3)	C21—C23	1.452 (2)
C4—H4	0.9500	C23—C24	1.412 (3)
C5—C6	1.361 (3)	C23—C25	1.459 (2)
C5—C26	1.427 (3)	C25—C26	1.418 (2)
C5—H5	0.9500	C27—C30	1.530 (3)
C6—C24	1.428 (3)	C27—C28	1.535 (2)
C6—H6	0.9500	C27—C29	1.540 (2)
C7—C8	1.357 (3)	C28—H28A	0.9800
C7—C24	1.427 (3)	C28—H28B	0.9800
C7—H7	0.9500	C28—H28C	0.9800
C8—C22	1.425 (3)	C29—H29A	0.9800
C8—H8	0.9500	C29—H29B	0.9800
C9—C10	1.348 (4)	C29—H29C	0.9800
C9—C22	1.429 (3)	C30—H30A	0.9800
C9—H9	0.9500	C30—H30B	0.9800
C10—C20	1.424 (3)	C30—H30C	0.9800
C10—H10	0.9500	C31—C33	1.526 (3)
C11—C12	1.354 (3)	C31—C32	1.533 (3)
C11—C20	1.430 (3)	C31—C34	1.537 (3)
C11—H11	0.9500	C32—H32A	0.9800
C12—C18	1.433 (3)	C32—H32B	0.9800
C12—H12	0.9500	C32—H32C	0.9800
C13—C14	1.376 (3)	C33—H33A	0.9800
C13—C18	1.414 (3)	C33—H33B	0.9800
C13—H13	0.9500	C33—H33C	0.9800
C14—C15	1.415 (3)	C34—H34A	0.9800
C14—H14	0.9500	C34—H34B	0.9800
C15—C16	1.383 (3)	C34—H34C	0.9800
C15—C31	1.526 (2)
C2—C1—C25	122.16 (15)	C15—C16—C17	122.54 (16)
C2—C1—H1	118.9	C15—C16—H16	118.7
C25—C1—H1	118.9	C17—C16—H16	118.7
C1—C2—C3	118.51 (16)	C16—C17—C18	118.07 (16)
C1—C2—C27	122.40 (15)	C16—C17—C19	122.52 (15)
C3—C2—C27	119.08 (15)	C18—C17—C19	119.25 (16)
C4—C3—C2	120.79 (16)	C13—C18—C17	118.99 (17)
C4—C3—H3	119.6	C13—C18—C12	121.01 (17)
C2—C3—H3	119.6	C17—C18—C12	119.88 (18)
C3—C4—C26	120.99 (17)	C20—C19—C17	117.09 (16)
C3—C4—H4	119.5	C20—C19—C21	118.04 (16)
C26—C4—H4	119.5	C17—C19—C21	124.67 (15)
C6—C5—C26	119.71 (18)	C19—C20—C10	120.09 (18)
C6—C5—H5	120.1	C19—C20—C11	119.97 (17)
C26—C5—H5	120.1	C10—C20—C11	119.91 (17)
C5—C6—C24	121.31 (18)	C22—C21—C23	117.06 (17)
C5—C6—H6	119.3	C22—C21—C19	116.94 (16)
C24—C6—H6	119.3	C23—C21—C19	126.00 (16)
C8—C7—C24	120.13 (18)	C21—C22—C8	120.59 (18)
C8—C7—H7	119.9	C21—C22—C9	120.21 (19)
C24—C7—H7	119.9	C8—C22—C9	119.19 (18)
C7—C8—C22	120.54 (17)	C24—C23—C21	118.38 (16)
C7—C8—H8	119.7	C24—C23—C25	116.76 (16)
C22—C8—H8	119.7	C21—C23—C25	124.66 (16)
C10—C9—C22	120.75 (18)	C23—C24—C7	120.38 (17)
C10—C9—H9	119.6	C23—C24—C6	120.37 (17)
C22—C9—H9	119.6	C7—C24—C6	119.22 (18)
C9—C10—C20	120.48 (18)	C26—C25—C1	118.02 (16)
C9—C10—H10	119.8	C26—C25—C23	119.31 (16)
C20—C10—H10	119.8	C1—C25—C23	122.50 (15)
C12—C11—C20	121.36 (17)	C4—C26—C25	119.14 (17)
C12—C11—H11	119.3	C4—C26—C5	120.70 (17)
C20—C11—H11	119.3	C25—C26—C5	119.96 (17)
C11—C12—C18	119.92 (18)	C30—C27—C2	112.52 (14)
C11—C12—H12	120.0	C30—C27—C28	108.46 (16)
C18—C12—H12	120.0	C2—C27—C28	108.53 (14)
C14—C13—C18	121.07 (17)	C30—C27—C29	108.12 (15)
C14—C13—H13	119.5	C2—C27—C29	109.47 (15)
C18—C13—H13	119.5	C28—C27—C29	109.71 (16)
C13—C14—C15	120.85 (17)	C15—C31—C33	112.35 (16)
C13—C14—H14	119.6	C15—C31—C32	108.90 (16)
C15—C14—H14	119.6	C33—C31—C32	107.4 (2)
C16—C15—C14	118.17 (17)	C15—C31—C34	109.72 (17)
C16—C15—C31	122.36 (17)	C33—C31—C34	109.5 (3)
C14—C15—C31	119.47 (16)	C32—C31—C34	108.91 (19)

Trans-1-(3, 5-di-t-butylphenyl)-2-(3, 4-benzo-5, 7-di-t-butylphenanthrenyl)-ethylene (VI)

Crystal data

C42H50	F(000) = 1208
Mr = 554.82	Dx = 1.077 Mg m^−3
Monoclinic, P21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 4545 reflections
a = 9.7954 (7) Å	θ = 2.2–27.8°
b = 28.071 (2) Å	µ = 0.06 mm^−1
c = 12.5190 (9) Å	T = 100 K
β = 96.349 (1)°	Irregular, colourless
V = 3421.2 (4) Å^3	0.3 × 0.2 × 0.1 mm
Z = 4

Data collection

CCD area detector diffractometer	8320 independent reflections
Radiation source: fine-focus sealed tube	4267 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.066
phi and ω scans	θmax = 28.3°, θmin = 1.8°
Absorption correction: multi-scan SADABS (Bruker)	h = −12→12
Tmin = 0.511, Tmax = 1.0	k = −24→36
22479 measured reflections	l = −16→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)] = 0.066	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.186	H-atom parameters constrained
S = 1.00	w = 1/[σ^2(Fo^2) + (0.0629P)^2 + 2.2848P] where P = (Fo^2 + 2Fc^2)/3
8320 reflections	(Δ/σ)max = 0.003
761 parameters	Δρmax = 0.49 e Å^−3
49 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. Although both enantiomers are present, no center could be found; F²(hkl) and F²(-h-k-l) were merged (HKLF 4). The tert-butyl groups at C35, C39, C35C and C39C are clearly disordered. A twofold disorder model for all four groups (as suggested by the "may be split" statement in SHELXL97) was tested. First, occupancies were fixed at 0.5 and U(iso) at 0.05 for all methyl C in the four groups, while the quaternary carbons were treated as ordered with anisotropic displacement parameters. C—C and C···C distances were restrained. Next, occupancies were allowed to refine (converging at x = 0.60656 for C36A—C38A, 0.38726 for C40A—C42A, 0.69179 for C36D—C38D and 0.48804 for C40D—C42D, 1 - x for C36B—C38B etc.) while U(iso) was held at 0.05. Finally, occupancies were fixed at 0.61/0.39, 0.39/0.61, 0.69/0.31 and 0.49/0.51 for the four twofold disordered regions, and U(iso) for methyl C was allowed to refine. The final U(iso) values vary from 0.038 (4) (C38E) to 0.099 (8) (C37B) and restrained C—CH3 distances from 1.470 (C35—C36B) to 1.639 (C35—C38A). Highest peak in the final difference map is 0.49, in a disordered region 0.55 A from H36D. The deepest hole is -0.32, in the same region, 0.52 A from C36A. All su values have been deleted for distances and angles involving disordered atoms.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	1.0421 (6)	0.2626 (2)	0.3036 (4)	0.0342 (14)
C2	1.1824 (6)	0.2535 (2)	0.3034 (5)	0.0376 (14)
H2	1.2242	0.2606	0.2403	0.045*
C3	1.2631 (6)	0.2346 (2)	0.3905 (5)	0.0395 (15)
C4	1.2004 (7)	0.2241 (2)	0.4818 (5)	0.0463 (17)
H4	1.2537	0.2103	0.5420	0.056*
C5	1.0052 (7)	0.2230 (2)	0.5893 (5)	0.0491 (17)
H5	1.0622	0.2040	0.6388	0.059*
C6	0.8895 (6)	0.2360 (2)	0.6214 (5)	0.0363 (14)
H6	0.8317	0.2547	0.5719	0.044*
C7	0.9090 (7)	0.1979 (2)	0.8033 (5)	0.0457 (16)
H7	0.9996	0.1879	0.7939	0.055*
C8	0.8524 (6)	0.1848 (2)	0.8936 (5)	0.0391 (15)
H8	0.9032	0.1651	0.9453	0.047*
C9	0.6508 (6)	0.1817 (2)	0.9980 (4)	0.0350 (14)
H9	0.6993	0.1616	1.0503	0.042*
C10	0.5179 (6)	0.1926 (2)	1.0050 (5)	0.0346 (14)
H10	0.4712	0.1776	1.0584	0.042*
C11	0.3014 (6)	0.2334 (2)	0.9359 (5)	0.0478 (17)
H11	0.2551	0.2186	0.9899	0.057*
C12	0.2316 (6)	0.2607 (2)	0.8614 (5)	0.0469 (17)
H12	0.1341	0.2610	0.8561	0.056*
C13	0.2231 (6)	0.3182 (2)	0.7128 (5)	0.0400 (15)
H13	0.1257	0.3158	0.7053	0.048*
C14	0.2830 (5)	0.3490 (2)	0.6492 (4)	0.0342 (14)
C15	0.4268 (5)	0.35509 (18)	0.6727 (4)	0.0261 (12)
H15	0.4703	0.3780	0.6319	0.031*
C16	0.5081 (5)	0.33017 (17)	0.7504 (4)	0.0236 (11)
C17	0.4468 (5)	0.29018 (18)	0.7984 (4)	0.0258 (12)
C18	0.3000 (5)	0.2896 (2)	0.7896 (4)	0.0304 (13)
C19	0.5156 (5)	0.25124 (18)	0.8588 (4)	0.0233 (12)
C20	0.4458 (6)	0.2262 (2)	0.9344 (4)	0.0335 (13)
C21	0.6488 (5)	0.23287 (18)	0.8385 (4)	0.0243 (11)
C22	0.7179 (5)	0.20040 (18)	0.9117 (4)	0.0285 (12)
C23	0.7078 (5)	0.24270 (17)	0.7434 (4)	0.0247 (12)
H23	0.6578	0.2618	0.6899	0.030*
C24	0.8356 (6)	0.2258 (2)	0.7243 (5)	0.0337 (13)
C25	0.9836 (6)	0.2522 (2)	0.3964 (5)	0.0376 (15)
H25	0.8884	0.2581	0.3985	0.045*
C26	1.0613 (7)	0.2332 (2)	0.4879 (5)	0.0422 (16)
C27	0.2052 (6)	0.3811 (3)	0.5641 (5)	0.0472 (18)
C28	0.0488 (6)	0.3709 (3)	0.5562 (6)	0.068 (2)
H28A	0.0150	0.3783	0.6251	0.102*
H28B	0.0320	0.3372	0.5390	0.102*
H28C	0.0007	0.3908	0.4996	0.102*
C29	0.2539 (7)	0.3702 (3)	0.4536 (5)	0.061 (2)
H29A	0.2076	0.3917	0.3994	0.092*
H29B	0.2315	0.3371	0.4337	0.092*
H29C	0.3534	0.3749	0.4575	0.092*
C30	0.2316 (7)	0.4333 (3)	0.5915 (6)	0.064 (2)
H30A	0.2070	0.4397	0.6639	0.096*
H30B	0.1757	0.4533	0.5395	0.096*
H30C	0.3290	0.4405	0.5888	0.096*
C31	0.6446 (5)	0.35622 (19)	0.7938 (4)	0.0280 (12)
C32	0.7426 (6)	0.3622 (2)	0.7058 (4)	0.0357 (14)
H32A	0.7802	0.3311	0.6889	0.054*
H32B	0.8179	0.3837	0.7319	0.054*
H32C	0.6918	0.3757	0.6409	0.054*
C33	0.7264 (6)	0.3347 (2)	0.8944 (4)	0.0356 (14)
H33A	0.7737	0.3058	0.8743	0.053*
H33B	0.6634	0.3267	0.9472	0.053*
H33C	0.7942	0.3579	0.9255	0.053*
C34	0.6015 (6)	0.4063 (2)	0.8278 (5)	0.0403 (15)
H34A	0.6830	0.4241	0.8578	0.060*
H34B	0.5373	0.4034	0.8822	0.060*
H34C	0.5567	0.4233	0.7650	0.060*
C35	1.4185 (6)	0.2263 (2)	0.3869 (5)	0.058 (2)
C36A	1.4884 (14)	0.1948 (4)	0.4758 (8)	0.077 (4)*	0.61
H36A	1.4517	0.1623	0.4677	0.115*	0.61
H36B	1.4709	0.2075	0.5459	0.115*	0.61
H36C	1.5876	0.1942	0.4711	0.115*	0.61
C37A	1.4543 (11)	0.2130 (4)	0.2766 (6)	0.047 (3)*	0.61
H37A	1.5523	0.2051	0.2807	0.070*	0.61
H37B	1.4342	0.2398	0.2274	0.070*	0.61
H37C	1.3998	0.1853	0.2502	0.070*	0.61
C38A	1.4941 (11)	0.2779 (3)	0.4112 (8)	0.056 (3)*	0.61
H38A	1.4692	0.2907	0.4792	0.085*	0.61
H38B	1.4644	0.3001	0.3528	0.085*	0.61
H38C	1.5939	0.2737	0.4159	0.085*	0.61
C36B	1.422 (2)	0.1699 (3)	0.3776 (13)	0.072 (6)*	0.39
H36D	1.3769	0.1558	0.4358	0.109*	0.39
H36E	1.5181	0.1592	0.3830	0.109*	0.39
H36F	1.3746	0.1601	0.3082	0.109*	0.39
C37B	1.466 (2)	0.2469 (7)	0.2846 (10)	0.099 (8)*	0.39
H37D	1.5619	0.2377	0.2800	0.148*	0.39
H37E	1.4595	0.2818	0.2862	0.148*	0.39
H37F	1.4082	0.2346	0.2219	0.148*	0.39
C38B	1.4975 (15)	0.2416 (5)	0.4877 (8)	0.042 (4)*	0.39
H38D	1.4789	0.2753	0.5006	0.063*	0.39
H38E	1.5958	0.2373	0.4823	0.063*	0.39
H38F	1.4707	0.2225	0.5474	0.063*	0.39
C39	0.9592 (5)	0.28517 (18)	0.2048 (4)	0.0371 (14)
C40A	0.8155 (11)	0.2630 (5)	0.1829 (13)	0.052 (5)*	0.39
H40A	0.7686	0.2650	0.2479	0.078*	0.39
H40B	0.8240	0.2295	0.1623	0.078*	0.39
H40C	0.7623	0.2803	0.1244	0.078*	0.39
C41A	0.9406 (16)	0.3393 (3)	0.2318 (13)	0.054 (5)*	0.39
H41A	0.8906	0.3422	0.2950	0.081*	0.39
H41B	0.8887	0.3552	0.1704	0.081*	0.39
H41C	1.0310	0.3543	0.2466	0.081*	0.39
C42A	1.0337 (16)	0.2826 (6)	0.1033 (11)	0.064 (5)*	0.39
H42A	0.9775	0.2981	0.0435	0.096*	0.39
H42B	1.0486	0.2492	0.0852	0.096*	0.39
H42C	1.1224	0.2989	0.1164	0.096*	0.39
C40B	0.8032 (7)	0.2824 (4)	0.2136 (9)	0.047 (3)*	0.61
H40D	0.7778	0.2495	0.2279	0.071*	0.61
H40E	0.7525	0.2931	0.1460	0.071*	0.61
H40F	0.7804	0.3029	0.2724	0.071*	0.61
C41B	1.0025 (11)	0.3368 (3)	0.1947 (9)	0.052 (3)*	0.61
H41D	0.9414	0.3525	0.1381	0.079*	0.61
H41E	1.0972	0.3381	0.1764	0.079*	0.61
H41F	0.9971	0.3532	0.2632	0.079*	0.61
C42B	0.9857 (10)	0.2574 (3)	0.1014 (7)	0.045 (3)*	0.61
H42D	0.9579	0.2241	0.1081	0.067*	0.61
H42E	1.0837	0.2588	0.0922	0.067*	0.61
H42F	0.9323	0.2718	0.0389	0.067*	0.61
C1C	−0.3043 (6)	0.5476 (2)	0.4364 (5)	0.0350 (14)
C2C	−0.4457 (6)	0.5520 (2)	0.4346 (4)	0.0319 (13)
H2C	−0.4864	0.5440	0.4978	0.038*
C3C	−0.5309 (6)	0.5675 (2)	0.3449 (4)	0.0323 (13)
C4C	−0.4696 (6)	0.5798 (2)	0.2545 (5)	0.0338 (13)
H4C	−0.5250	0.5918	0.1933	0.041*
C5C	−0.2725 (6)	0.5875 (2)	0.1503 (5)	0.0417 (16)
H5C	−0.3293	0.6069	0.1016	0.050*
C6C	−0.1526 (6)	0.5750 (2)	0.1195 (5)	0.0349 (14)
H6C	−0.0954	0.5563	0.1694	0.042*
C7C	−0.1656 (6)	0.6181 (2)	−0.0595 (5)	0.0345 (14)
H7C	−0.2542	0.6299	−0.0496	0.041*
C8C	−0.1047 (6)	0.6312 (2)	−0.1474 (5)	0.0385 (15)
H8C	−0.1503	0.6532	−0.1967	0.046*
C9C	0.0923 (6)	0.6306 (2)	−0.2543 (5)	0.0352 (14)
H9C	0.0461	0.6517	−0.3055	0.042*
C10C	0.2231 (7)	0.6171 (2)	−0.2636 (5)	0.0406 (16)
H10C	0.2702	0.6309	−0.3184	0.049*
C11C	0.4347 (7)	0.5750 (2)	−0.1942 (5)	0.0441 (16)
H11C	0.4812	0.5890	−0.2490	0.053*
C12C	0.5052 (6)	0.5481 (2)	−0.1186 (5)	0.0412 (16)
H12C	0.6028	0.5481	−0.1119	0.049*
C13C	0.5119 (6)	0.4893 (2)	0.0275 (5)	0.0337 (14)
H13C	0.6093	0.4910	0.0349	0.040*
C14C	0.4476 (6)	0.45760 (19)	0.0901 (5)	0.0308 (13)
C15C	0.30484 (18)	0.45260 (6)	0.06430 (14)	0.0277 (12)
H15C	0.2598	0.4293	0.1030	0.033*
C16C	0.22451 (18)	0.47858 (6)	−0.01245 (14)	0.0265 (12)
C17C	0.28846 (18)	0.51862 (6)	−0.05878 (14)	0.0241 (11)
C18C	0.43459 (18)	0.51912 (6)	−0.04746 (14)	0.0301 (13)
C19C	0.22049 (18)	0.55851 (6)	−0.11848 (14)	0.0287 (13)
C20C	0.29171 (18)	0.58272 (6)	−0.19352 (14)	0.0322 (13)
C21C	0.09129 (18)	0.57821 (6)	−0.09598 (14)	0.0251 (12)
C22C	0.02414 (18)	0.61309 (6)	−0.16735 (14)	0.0317 (13)
C23C	0.02835 (18)	0.56741 (6)	−0.00204 (14)	0.0257 (12)
H23C	0.0741	0.5462	0.0492	0.031*
C24C	−0.0961 (5)	0.5863 (2)	0.0182 (4)	0.0297 (12)
C25C	−0.2474 (6)	0.5596 (2)	0.3427 (5)	0.0405 (16)
H25C	−0.1508	0.5571	0.3415	0.049*
C26C	−0.3283 (6)	0.5751 (2)	0.2509 (4)	0.0358 (14)
C27C	0.5255 (6)	0.4252 (2)	0.1740 (5)	0.0404 (15)
C28C	0.4782 (7)	0.4349 (3)	0.2837 (5)	0.0521 (18)
H28D	0.5261	0.4134	0.3369	0.078*
H28E	0.3789	0.4295	0.2803	0.078*
H28F	0.4990	0.4680	0.3045	0.078*
C29C	0.4948 (8)	0.3729 (2)	0.1442 (7)	0.065 (2)
H29D	0.5159	0.3670	0.0706	0.098*
H29E	0.3974	0.3662	0.1490	0.098*
H29F	0.5514	0.3521	0.1939	0.098*
C30C	0.6802 (7)	0.4331 (3)	0.1817 (8)	0.081 (3)
H30D	0.7149	0.4216	0.1158	0.121*
H30E	0.7252	0.4156	0.2436	0.121*
H30F	0.7002	0.4672	0.1906	0.121*
C31C	0.0875 (6)	0.4543 (2)	−0.0558 (5)	0.0328 (13)
C32C	−0.0116 (6)	0.4496 (2)	0.0297 (5)	0.0380 (15)
H32D	0.0354	0.4341	0.0936	0.057*
H32E	−0.0909	0.4304	0.0013	0.057*
H32F	−0.0428	0.4813	0.0490	0.057*
C33C	0.0108 (6)	0.4761 (2)	−0.1577 (5)	0.0426 (16)
H33D	−0.0386	0.5047	−0.1386	0.064*
H33E	−0.0548	0.4528	−0.1917	0.064*
H33F	0.0769	0.4847	−0.2078	0.064*
C34C	0.1282 (7)	0.4036 (2)	−0.0908 (5)	0.0428 (16)
H34D	0.1936	0.4061	−0.1444	0.064*
H34E	0.0459	0.3866	−0.1220	0.064*
H34F	0.1707	0.3860	−0.0280	0.064*
C35C	−0.6881 (5)	0.57089 (18)	0.3494 (4)	0.0346 (13)
C36D	−0.7623 (10)	0.5664 (3)	0.2387 (5)	0.054 (3)*	0.69
H36G	−0.8616	0.5661	0.2431	0.080*	0.69
H36H	−0.7350	0.5367	0.2058	0.080*	0.69
H36I	−0.7389	0.5935	0.1949	0.080*	0.69
C37D	−0.7169 (9)	0.6191 (2)	0.4018 (6)	0.040 (2)*	0.69
H37G	−0.6688	0.6203	0.4746	0.060*	0.69
H37H	−0.8159	0.6225	0.4051	0.060*	0.69
H37I	−0.6844	0.6451	0.3588	0.060*	0.69
C38D	−0.7356 (10)	0.5312 (3)	0.4240 (7)	0.057 (3)*	0.69
H38G	−0.7015	0.5383	0.4989	0.086*	0.69
H38H	−0.6990	0.5004	0.4037	0.086*	0.69
H38I	−0.8362	0.5298	0.4165	0.086*	0.69
C36E	−0.7512 (18)	0.6026 (5)	0.2520 (10)	0.041 (5)*	0.31
H36J	−0.8517	0.6015	0.2473	0.062*	0.31
H36K	−0.7210	0.5904	0.1851	0.062*	0.31
H36L	−0.7200	0.6356	0.2632	0.062*	0.31
C37E	−0.727 (2)	0.5928 (6)	0.4531 (10)	0.067 (7)*	0.31
H37J	−0.7066	0.5702	0.5124	0.100*	0.31
H37K	−0.8259	0.6000	0.4449	0.100*	0.31
H37L	−0.6751	0.6222	0.4686	0.100*	0.31
C38E	−0.7597 (18)	0.5214 (4)	0.3312 (13)	0.038 (4)*	0.31
H38J	−0.7098	0.4976	0.3777	0.057*	0.31
H38K	−0.7598	0.5120	0.2559	0.057*	0.31
H38L	−0.8546	0.5236	0.3488	0.057*	0.31
C39C	−0.2144 (5)	0.5289 (2)	0.5370 (4)	0.0468 (17)
C40D	−0.2981 (12)	0.5177 (5)	0.6280 (9)	0.057 (4)*	0.49
H40G	−0.3692	0.4943	0.6038	0.086*	0.49
H40H	−0.3416	0.5469	0.6505	0.086*	0.49
H40I	−0.2380	0.5046	0.6887	0.086*	0.49
C41D	−0.0978 (11)	0.5631 (4)	0.5634 (10)	0.054 (4)*	0.49
H41G	−0.0468	0.5666	0.5008	0.081*	0.49
H41H	−0.0363	0.5508	0.6242	0.081*	0.49
H41I	−0.1342	0.5941	0.5823	0.081*	0.49
C42D	−0.1518 (13)	0.4798 (3)	0.5006 (10)	0.055 (4)*	0.49
H42G	−0.2266	0.4581	0.4748	0.082*	0.49
H42H	−0.0959	0.4653	0.5619	0.082*	0.49
H42I	−0.0943	0.4858	0.4427	0.082*	0.49
C40E	−0.2478 (11)	0.5612 (4)	0.6366 (8)	0.047 (3)*	0.51
H40J	−0.3451	0.5579	0.6469	0.071*	0.51
H40K	−0.2277	0.5947	0.6219	0.071*	0.51
H40L	−0.1910	0.5509	0.7018	0.071*	0.51
C41E	−0.0605 (8)	0.5342 (4)	0.5328 (10)	0.049 (3)*	0.51
H41J	−0.0389	0.5677	0.5198	0.073*	0.51
H41K	−0.0321	0.5145	0.4746	0.073*	0.51
H41L	−0.0113	0.5240	0.6014	0.073*	0.51
C42E	−0.2544 (13)	0.4783 (3)	0.5640 (11)	0.057 (4)*	0.51
H42J	−0.3484	0.4782	0.5839	0.085*	0.51
H42K	−0.1912	0.4664	0.6242	0.085*	0.51
H42L	−0.2494	0.4578	0.5011	0.085*	0.51

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.040 (4)	0.031 (3)	0.032 (3)	0.011 (3)	0.005 (3)	0.008 (3)
C2	0.032 (3)	0.046 (4)	0.037 (3)	0.010 (3)	0.010 (3)	0.011 (3)
C3	0.032 (3)	0.052 (4)	0.036 (3)	0.016 (3)	0.006 (3)	0.006 (3)
C4	0.051 (4)	0.057 (4)	0.031 (3)	0.024 (3)	0.007 (3)	0.015 (3)
C5	0.055 (4)	0.054 (4)	0.040 (4)	0.009 (3)	0.016 (3)	0.004 (3)
C6	0.032 (3)	0.029 (3)	0.049 (4)	0.010 (3)	0.008 (3)	0.003 (3)
C7	0.041 (4)	0.039 (4)	0.059 (4)	0.015 (3)	0.016 (3)	0.014 (3)
C8	0.037 (4)	0.039 (4)	0.041 (3)	0.014 (3)	0.004 (3)	0.013 (3)
C9	0.038 (4)	0.032 (3)	0.034 (3)	−0.001 (3)	−0.004 (3)	0.009 (3)
C10	0.033 (3)	0.039 (4)	0.032 (3)	−0.007 (3)	0.005 (2)	0.006 (3)
C11	0.038 (4)	0.058 (4)	0.051 (4)	0.001 (3)	0.020 (3)	0.021 (3)
C12	0.026 (3)	0.061 (5)	0.056 (4)	0.004 (3)	0.016 (3)	0.026 (4)
C13	0.017 (3)	0.060 (4)	0.043 (3)	0.002 (3)	0.003 (3)	0.010 (3)
C14	0.024 (3)	0.047 (4)	0.033 (3)	0.006 (3)	0.005 (2)	0.006 (3)
C15	0.023 (3)	0.032 (3)	0.024 (3)	0.000 (2)	0.005 (2)	0.002 (2)
C16	0.019 (3)	0.026 (3)	0.027 (3)	−0.001 (2)	0.006 (2)	−0.003 (2)
C17	0.028 (3)	0.027 (3)	0.023 (3)	0.000 (2)	0.006 (2)	−0.003 (2)
C18	0.023 (3)	0.038 (3)	0.031 (3)	0.000 (2)	0.006 (2)	0.007 (3)
C19	0.023 (3)	0.025 (3)	0.021 (3)	−0.007 (2)	0.001 (2)	−0.003 (2)
C20	0.033 (3)	0.034 (3)	0.035 (3)	0.000 (3)	0.011 (3)	0.000 (3)
C21	0.022 (3)	0.022 (3)	0.029 (3)	−0.006 (2)	0.003 (2)	−0.004 (2)
C22	0.033 (3)	0.022 (3)	0.031 (3)	0.002 (2)	0.005 (2)	0.003 (2)
C23	0.025 (3)	0.020 (3)	0.029 (3)	−0.002 (2)	0.002 (2)	0.000 (2)
C24	0.029 (3)	0.028 (3)	0.045 (3)	0.003 (2)	0.008 (3)	0.002 (3)
C25	0.032 (3)	0.044 (4)	0.039 (3)	0.010 (3)	0.013 (3)	0.002 (3)
C26	0.052 (4)	0.047 (4)	0.029 (3)	0.007 (3)	0.012 (3)	0.009 (3)
C27	0.026 (3)	0.069 (5)	0.046 (4)	0.012 (3)	0.003 (3)	0.026 (3)
C28	0.025 (4)	0.101 (6)	0.077 (5)	0.010 (4)	0.003 (3)	0.055 (5)
C29	0.047 (4)	0.099 (6)	0.035 (4)	−0.002 (4)	−0.005 (3)	0.024 (4)
C30	0.047 (4)	0.074 (6)	0.072 (5)	0.026 (4)	0.015 (4)	0.033 (4)
C31	0.031 (3)	0.024 (3)	0.027 (3)	0.002 (2)	−0.003 (2)	0.000 (2)
C32	0.029 (3)	0.033 (3)	0.044 (3)	−0.007 (3)	0.001 (3)	0.002 (3)
C33	0.041 (4)	0.027 (3)	0.036 (3)	−0.008 (3)	−0.010 (3)	−0.002 (3)
C34	0.051 (4)	0.027 (3)	0.041 (3)	−0.002 (3)	−0.001 (3)	−0.008 (3)
C35	0.036 (4)	0.089 (6)	0.050 (4)	0.029 (4)	0.006 (3)	0.009 (4)
C39	0.030 (3)	0.043 (4)	0.038 (3)	0.009 (3)	0.001 (3)	0.013 (3)
C1C	0.026 (3)	0.046 (4)	0.034 (3)	0.012 (3)	0.006 (3)	0.011 (3)
C2C	0.025 (3)	0.040 (3)	0.032 (3)	0.008 (2)	0.009 (2)	0.009 (3)
C3C	0.025 (3)	0.036 (3)	0.036 (3)	0.003 (2)	0.002 (2)	0.004 (3)
C4C	0.027 (3)	0.037 (3)	0.038 (3)	0.008 (2)	0.003 (2)	0.009 (3)
C5C	0.031 (3)	0.054 (4)	0.040 (3)	−0.005 (3)	0.003 (3)	0.019 (3)
C6C	0.023 (3)	0.032 (3)	0.049 (4)	0.000 (2)	0.001 (3)	0.009 (3)
C7C	0.021 (3)	0.033 (3)	0.048 (4)	−0.003 (2)	−0.002 (2)	0.014 (3)
C8C	0.033 (3)	0.043 (4)	0.037 (3)	−0.009 (3)	−0.004 (3)	0.013 (3)
C9C	0.046 (4)	0.026 (3)	0.033 (3)	−0.003 (3)	−0.001 (3)	0.006 (2)
C10C	0.066 (5)	0.031 (3)	0.028 (3)	−0.005 (3)	0.017 (3)	0.003 (3)
C11C	0.054 (4)	0.033 (3)	0.051 (4)	0.007 (3)	0.031 (3)	0.011 (3)
C12C	0.039 (4)	0.031 (3)	0.059 (4)	0.000 (3)	0.032 (3)	−0.001 (3)
C13C	0.028 (3)	0.029 (3)	0.048 (4)	−0.003 (2)	0.018 (3)	−0.001 (3)
C14C	0.027 (3)	0.026 (3)	0.041 (3)	0.006 (2)	0.011 (2)	−0.003 (3)
C15C	0.026 (3)	0.027 (3)	0.032 (3)	−0.002 (2)	0.015 (2)	−0.004 (2)
C16C	0.034 (3)	0.024 (3)	0.022 (3)	−0.004 (2)	0.003 (2)	−0.004 (2)
C17C	0.030 (3)	0.022 (3)	0.021 (3)	0.000 (2)	0.007 (2)	−0.005 (2)
C18C	0.031 (3)	0.021 (3)	0.040 (3)	−0.002 (2)	0.015 (3)	−0.002 (2)
C19C	0.042 (4)	0.019 (3)	0.025 (3)	−0.006 (2)	0.006 (3)	−0.001 (2)
C20C	0.045 (4)	0.024 (3)	0.030 (3)	0.000 (3)	0.012 (3)	−0.002 (2)
C21C	0.029 (3)	0.017 (3)	0.028 (3)	−0.010 (2)	−0.002 (2)	−0.001 (2)
C22C	0.037 (3)	0.026 (3)	0.031 (3)	−0.008 (2)	−0.003 (3)	0.005 (2)
C23C	0.022 (3)	0.026 (3)	0.028 (3)	−0.002 (2)	0.001 (2)	0.004 (2)
C24C	0.023 (3)	0.031 (3)	0.035 (3)	−0.002 (2)	0.000 (2)	0.007 (2)
C25C	0.025 (3)	0.057 (4)	0.040 (3)	0.007 (3)	0.006 (3)	0.013 (3)
C26C	0.027 (3)	0.044 (4)	0.036 (3)	0.001 (3)	0.005 (3)	0.012 (3)
C27C	0.024 (3)	0.039 (4)	0.060 (4)	0.010 (3)	0.012 (3)	0.014 (3)
C28C	0.044 (4)	0.071 (5)	0.039 (4)	0.005 (4)	−0.003 (3)	0.018 (3)
C29C	0.076 (5)	0.034 (4)	0.091 (6)	0.023 (4)	0.029 (4)	0.020 (4)
C30C	0.029 (4)	0.089 (6)	0.123 (8)	0.012 (4)	0.005 (4)	0.053 (6)
C31C	0.035 (3)	0.024 (3)	0.038 (3)	−0.010 (2)	−0.003 (3)	0.000 (2)
C32C	0.030 (3)	0.037 (3)	0.045 (4)	−0.015 (3)	−0.002 (3)	0.007 (3)
C33C	0.049 (4)	0.030 (3)	0.044 (4)	−0.015 (3)	−0.017 (3)	0.003 (3)
C34C	0.062 (4)	0.025 (3)	0.039 (3)	−0.013 (3)	−0.008 (3)	−0.003 (3)
C35C	0.026 (3)	0.038 (3)	0.040 (3)	0.008 (2)	0.003 (2)	−0.001 (3)
C39C	0.035 (4)	0.065 (5)	0.040 (4)	0.019 (3)	0.003 (3)	0.019 (3)

Geometric parameters (Å, º)

C1—C25	1.383 (8)	C1C—C2C	1.388 (7)
C1—C2	1.399 (8)	C1C—C25C	1.395 (8)
C1—C39	1.539 (7)	C1C—C39C	1.547 (7)
C2—C3	1.380 (8)	C2C—C3C	1.393 (7)
C2—H2	0.9500	C2C—H2C	0.9500
C3—C4	1.388 (8)	C3C—C4C	1.382 (8)
C3—C35	1.545 (8)	C3C—C35C	1.550 (7)
C4—C26	1.398 (9)	C4C—C26C	1.397 (7)
C4—H4	0.9500	C4C—H4C	0.9500
C5—C6	1.296 (8)	C5C—C6C	1.323 (8)
C5—C26	1.466 (8)	C5C—C26C	1.468 (8)
C5—H5	0.9500	C5C—H5C	0.9500
C6—C24	1.473 (8)	C6C—C24C	1.474 (8)
C6—H6	0.9500	C6C—H6C	0.9500
C7—C8	1.364 (8)	C7C—C8C	1.359 (8)
C7—C24	1.396 (8)	C7C—C24C	1.435 (7)
C7—H7	0.9500	C7C—H7C	0.9500
C8—C22	1.430 (7)	C8C—C22C	1.408 (7)
C8—H8	0.9500	C8C—H8C	0.9500
C9—C10	1.350 (8)	C9C—C10C	1.353 (8)
C9—C22	1.426 (7)	C9C—C22C	1.426 (6)
C9—H9	0.9500	C9C—H9C	0.9500
C10—C20	1.425 (8)	C10C—C20C	1.423 (6)
C10—H10	0.9500	C10C—H10C	0.9500
C11—C12	1.336 (8)	C11C—C12C	1.341 (9)
C11—C20	1.430 (8)	C11C—C20C	1.419 (7)
C11—H11	0.9500	C11C—H11C	0.9500
C12—C18	1.430 (7)	C12C—C18C	1.438 (6)
C12—H12	0.9500	C12C—H12C	0.9500
C13—C14	1.354 (8)	C13C—C14C	1.382 (8)
C13—C18	1.406 (8)	C13C—C18C	1.414 (6)
C13—H13	0.9500	C13C—H13C	0.9500
C14—C15	1.417 (7)	C14C—C15C	1.407 (6)
C14—C27	1.533 (8)	C14C—C27C	1.528 (8)
C15—C16	1.378 (7)	C15C—C16C	1.3809
C15—H15	0.9500	C15C—H15C	0.9500
C16—C17	1.436 (7)	C16C—C17C	1.4394
C16—C31	1.567 (7)	C16C—C31C	1.548 (6)
C17—C18	1.430 (7)	C17C—C18C	1.4227
C17—C19	1.452 (7)	C17C—C19C	1.4649
C19—C20	1.414 (7)	C19C—C20C	1.4057
C19—C21	1.451 (7)	C19C—C21C	1.4372
C21—C23	1.407 (7)	C21C—C23C	1.4196
C21—C22	1.411 (7)	C21C—C22C	1.4351
C23—C24	1.384 (7)	C23C—C24C	1.378 (6)
C23—H23	0.9500	C23C—H23C	0.9500
C25—C26	1.408 (8)	C25C—C26C	1.392 (8)
C25—H25	0.9500	C25C—H25C	0.9500
C27—C30	1.520 (11)	C27C—C28C	1.521 (9)
C27—C29	1.543 (9)	C27C—C29C	1.538 (10)
C27—C28	1.550 (8)	C27C—C30C	1.525 (8)
C28—H28A	0.9800	C28C—H28D	0.9800
C28—H28B	0.9800	C28C—H28E	0.9800
C28—H28C	0.9800	C28C—H28F	0.9800
C29—H29A	0.9800	C29C—H29D	0.9800
C29—H29B	0.9800	C29C—H29E	0.9800
C29—H29C	0.9800	C29C—H29F	0.9800
C30—H30A	0.9800	C30C—H30D	0.9800
C30—H30B	0.9800	C30C—H30E	0.9800
C30—H30C	0.9800	C30C—H30F	0.9800
C31—C33	1.540 (7)	C31C—C32C	1.528 (8)
C31—C34	1.542 (8)	C31C—C33C	1.534 (8)
C31—C32	1.549 (7)	C31C—C34C	1.556 (8)
C32—H32A	0.9800	C32C—H32D	0.9800
C32—H32B	0.9800	C32C—H32E	0.9800
C32—H32C	0.9800	C32C—H32F	0.9800
C33—H33A	0.9800	C33C—H33D	0.9800
C33—H33B	0.9800	C33C—H33E	0.9800
C33—H33C	0.9800	C33C—H33F	0.9800
C34—H34A	0.9800	C34C—H34D	0.9800
C34—H34B	0.9800	C34C—H34E	0.9800
C34—H34C	0.9800	C34C—H34F	0.9800
C35—C38B	1.470	C35C—C36D	1.497
C35—C37A	1.509	C35C—C37E	1.524
C35—C37B	1.525	C35C—C37D	1.543
C35—C36A	1.525	C35C—C38D	1.559
C35—C36B	1.587	C35C—C38E	1.561
C35—C38A	1.639	C35C—C36E	1.579
C36A—H36A	0.9800	C36D—H36G	0.9800
C36A—H36B	0.9800	C36D—H36H	0.9800
C36A—H36C	0.9800	C36D—H36I	0.9800
C37A—H37A	0.9800	C37D—H37G	0.9800
C37A—H37B	0.9800	C37D—H37H	0.9800
C37A—H37C	0.9800	C37D—H37I	0.9800
C38A—H38A	0.9800	C38D—H38G	0.9800
C38A—H38B	0.9800	C38D—H38H	0.9800
C38A—H38C	0.9800	C38D—H38I	0.9800
C36B—H36D	0.9800	C36E—H36J	0.9800
C36B—H36E	0.9800	C36E—H36K	0.9800
C36B—H36F	0.9800	C36E—H36L	0.9800
C37B—H37D	0.9800	C37E—H37J	0.9800
C37B—H37E	0.9800	C37E—H37K	0.9800
C37B—H37F	0.9800	C37E—H37L	0.9800
C38B—H38D	0.9800	C38E—H38J	0.9800
C38B—H38E	0.9800	C38E—H38K	0.9800
C38B—H38F	0.9800	C38E—H38L	0.9800
C39—C41B	1.520	C39C—C41D	1.500
C39—C42A	1.535	C39C—C40D	1.508
C39—C40A	1.536	C39C—C42E	1.520
C39—C40B	1.546	C39C—C41E	1.521
C39—C42B	1.557	C39C—C42D	1.595
C39—C41A	1.572	C39C—C40E	1.605
C40A—H40A	0.9800	C40D—H40G	0.9800
C40A—H40B	0.9800	C40D—H40H	0.9800
C40A—H40C	0.9800	C40D—H40I	0.9800
C41A—H41A	0.9800	C41D—H41G	0.9800
C41A—H41B	0.9800	C41D—H41H	0.9800
C41A—H41C	0.9800	C41D—H41I	0.9800
C42A—H42A	0.9800	C42D—H42G	0.9800
C42A—H42B	0.9800	C42D—H42H	0.9800
C42A—H42C	0.9800	C42D—H42I	0.9800
C40B—H40D	0.9800	C40E—H40J	0.9800
C40B—H40E	0.9800	C40E—H40K	0.9800
C40B—H40F	0.9800	C40E—H40L	0.9800
C41B—H41D	0.9800	C41E—H41J	0.9800
C41B—H41E	0.9800	C41E—H41K	0.9800
C41B—H41F	0.9800	C41E—H41L	0.9800
C42B—H42D	0.9800	C42E—H42J	0.9800
C42B—H42E	0.9800	C42E—H42K	0.9800
C42B—H42F	0.9800	C42E—H42L	0.9800
C25—C1—C2	117.5 (5)	H42D—C42B—H42E	109.5
C25—C1—C39	122.1 (5)	C39—C42B—H42F	109.5
C2—C1—C39	120.4 (5)	H42D—C42B—H42F	109.5
C3—C2—C1	123.1 (5)	H42E—C42B—H42F	109.5
C3—C2—H2	118.4	C2C—C1C—C25C	117.1 (5)
C1—C2—H2	118.4	C2C—C1C—C39C	121.4 (5)
C2—C3—C4	117.7 (6)	C25C—C1C—C39C	121.5 (5)
C2—C3—C35	121.0 (5)	C1C—C2C—C3C	123.2 (5)
C4—C3—C35	121.3 (5)	C1C—C2C—H2C	118.4
C3—C4—C26	121.9 (5)	C3C—C2C—H2C	118.4
C3—C4—H4	119.0	C4C—C3C—C2C	117.6 (5)
C26—C4—H4	119.0	C4C—C3C—C35C	122.5 (5)
C6—C5—C26	129.6 (6)	C2C—C3C—C35C	119.9 (5)
C6—C5—H5	115.2	C3C—C4C—C26C	121.7 (5)
C26—C5—H5	115.2	C3C—C4C—H4C	119.2
C5—C6—C24	128.8 (6)	C26C—C4C—H4C	119.2
C5—C6—H6	115.6	C6C—C5C—C26C	127.8 (6)
C24—C6—H6	115.6	C6C—C5C—H5C	116.1
C8—C7—C24	120.9 (6)	C26C—C5C—H5C	116.1
C8—C7—H7	119.6	C5C—C6C—C24C	128.6 (5)
C24—C7—H7	119.6	C5C—C6C—H6C	115.7
C7—C8—C22	121.1 (5)	C24C—C6C—H6C	115.7
C7—C8—H8	119.5	C8C—C7C—C24C	120.0 (6)
C22—C8—H8	119.5	C8C—C7C—H7C	120.0
C10—C9—C22	119.6 (5)	C24C—C7C—H7C	120.0
C10—C9—H9	120.2	C7C—C8C—C22C	121.9 (5)
C22—C9—H9	120.2	C7C—C8C—H8C	119.1
C9—C10—C20	121.7 (5)	C22C—C8C—H8C	119.1
C9—C10—H10	119.1	C10C—C9C—C22C	119.8 (5)
C20—C10—H10	119.1	C10C—C9C—H9C	120.1
C12—C11—C20	120.1 (5)	C22C—C9C—H9C	120.1
C12—C11—H11	119.9	C9C—C10C—C20C	121.6 (5)
C20—C11—H11	119.9	C9C—C10C—H10C	119.2
C11—C12—C18	121.6 (5)	C20C—C10C—H10C	119.2
C11—C12—H12	119.2	C12C—C11C—C20C	120.9 (5)
C18—C12—H12	119.2	C12C—C11C—H11C	119.5
C14—C13—C18	122.2 (5)	C20C—C11C—H11C	119.5
C14—C13—H13	118.9	C11C—C12C—C18C	120.7 (5)
C18—C13—H13	118.9	C11C—C12C—H12C	119.7
C13—C14—C15	116.2 (5)	C18C—C12C—H12C	119.7
C13—C14—C27	124.8 (5)	C14C—C13C—C18C	120.9 (5)
C15—C14—C27	118.7 (5)	C14C—C13C—H13C	119.5
C16—C15—C14	124.7 (5)	C18C—C13C—H13C	119.5
C16—C15—H15	117.7	C13C—C14C—C15C	115.9 (5)
C14—C15—H15	117.7	C13C—C14C—C27C	123.2 (5)
C15—C16—C17	117.1 (5)	C15C—C14C—C27C	120.5 (5)
C15—C16—C31	114.3 (4)	C16C—C15C—C14C	125.6 (2)
C17—C16—C31	126.9 (4)	C16C—C15C—H15C	117.2
C18—C17—C16	116.2 (4)	C14C—C15C—H15C	117.2
C18—C17—C19	115.8 (4)	C15C—C16C—C17C	116.9
C16—C17—C19	127.9 (5)	C15C—C16C—C31C	114.6 (2)
C13—C18—C12	120.0 (5)	C17C—C16C—C31C	126.9 (2)
C13—C18—C17	120.3 (5)	C18C—C17C—C16C	116.5
C12—C18—C17	119.7 (5)	C18C—C17C—C19C	116.0
C20—C19—C17	119.4 (5)	C16C—C17C—C19C	127.5
C20—C19—C21	116.9 (5)	C13C—C18C—C17C	121.3 (2)
C17—C19—C21	123.4 (4)	C13C—C18C—C12C	119.1 (4)
C19—C20—C10	120.0 (5)	C17C—C18C—C12C	119.4 (3)
C19—C20—C11	119.4 (5)	C20C—C19C—C21C	117.3
C10—C20—C11	120.5 (5)	C20C—C19C—C17C	118.6
C23—C21—C22	117.6 (5)	C21C—C19C—C17C	123.7
C23—C21—C19	122.7 (4)	C19C—C20C—C11C	119.5 (3)
C22—C21—C19	119.4 (4)	C19C—C20C—C10C	120.3 (3)
C21—C22—C9	120.1 (5)	C11C—C20C—C10C	120.0 (4)
C21—C22—C8	118.6 (5)	C23C—C21C—C22C	116.8
C9—C22—C8	121.2 (5)	C23C—C21C—C19C	123.5
C24—C23—C21	122.9 (5)	C22C—C21C—C19C	119.6
C24—C23—H23	118.6	C8C—C22C—C9C	121.0 (4)
C21—C23—H23	118.6	C8C—C22C—C21C	119.6 (2)
C23—C24—C7	118.4 (5)	C9C—C22C—C21C	119.3 (3)
C23—C24—C6	120.2 (5)	C24C—C23C—C21C	122.9 (2)
C7—C24—C6	121.4 (5)	C24C—C23C—H23C	118.5
C1—C25—C26	121.8 (6)	C21C—C23C—H23C	118.5
C1—C25—H25	119.1	C23C—C24C—C7C	118.5 (5)
C26—C25—H25	119.1	C23C—C24C—C6C	120.0 (4)
C4—C26—C25	117.9 (5)	C7C—C24C—C6C	121.5 (5)
C4—C26—C5	118.1 (6)	C26C—C25C—C1C	121.7 (5)
C25—C26—C5	123.9 (6)	C26C—C25C—H25C	119.1
C30—C27—C14	110.5 (6)	C1C—C25C—H25C	119.1
C30—C27—C29	109.4 (6)	C25C—C26C—C4C	118.6 (5)
C14—C27—C29	109.1 (5)	C25C—C26C—C5C	123.4 (5)
C30—C27—C28	109.5 (6)	C4C—C26C—C5C	118.0 (5)
C14—C27—C28	110.3 (5)	C28C—C27C—C14C	109.6 (5)
C29—C27—C28	107.9 (6)	C28C—C27C—C29C	108.6 (6)
C27—C28—H28A	109.5	C14C—C27C—C29C	109.4 (6)
C27—C28—H28B	109.5	C28C—C27C—C30C	108.5 (6)
H28A—C28—H28B	109.5	C14C—C27C—C30C	112.0 (5)
C27—C28—H28C	109.5	C29C—C27C—C30C	108.7 (6)
H28A—C28—H28C	109.5	C27C—C28C—H28D	109.5
H28B—C28—H28C	109.5	C27C—C28C—H28E	109.5
C27—C29—H29A	109.5	H28D—C28C—H28E	109.5
C27—C29—H29B	109.5	C27C—C28C—H28F	109.5
H29A—C29—H29B	109.5	H28D—C28C—H28F	109.5
C27—C29—H29C	109.5	H28E—C28C—H28F	109.5
H29A—C29—H29C	109.5	C27C—C29C—H29D	109.5
H29B—C29—H29C	109.5	C27C—C29C—H29E	109.5
C27—C30—H30A	109.5	H29D—C29C—H29E	109.5
C27—C30—H30B	109.5	C27C—C29C—H29F	109.5
H30A—C30—H30B	109.5	H29D—C29C—H29F	109.5
C27—C30—H30C	109.5	H29E—C29C—H29F	109.5
H30A—C30—H30C	109.5	C27C—C30C—H30D	109.5
H30B—C30—H30C	109.5	C27C—C30C—H30E	109.5
C33—C31—C34	105.4 (4)	H30D—C30C—H30E	109.5
C33—C31—C32	108.5 (5)	C27C—C30C—H30F	109.5
C34—C31—C32	107.9 (5)	H30D—C30C—H30F	109.5
C33—C31—C16	116.6 (4)	H30E—C30C—H30F	109.5
C34—C31—C16	105.8 (4)	C32C—C31C—C33C	109.1 (5)
C32—C31—C16	112.2 (4)	C32C—C31C—C16C	112.7 (4)
C31—C32—H32A	109.5	C33C—C31C—C16C	116.2 (4)
C31—C32—H32B	109.5	C32C—C31C—C34C	108.7 (5)
H32A—C32—H32B	109.5	C33C—C31C—C34C	104.3 (5)
C31—C32—H32C	109.5	C16C—C31C—C34C	105.2 (4)
H32A—C32—H32C	109.5	C31C—C32C—H32D	109.5
H32B—C32—H32C	109.5	C31C—C32C—H32E	109.5
C31—C33—H33A	109.5	H32D—C32C—H32E	109.5
C31—C33—H33B	109.5	C31C—C32C—H32F	109.5
H33A—C33—H33B	109.5	H32D—C32C—H32F	109.5
C31—C33—H33C	109.5	H32E—C32C—H32F	109.5
H33A—C33—H33C	109.5	C31C—C33C—H33D	109.5
H33B—C33—H33C	109.5	C31C—C33C—H33E	109.5
C31—C34—H34A	109.5	H33D—C33C—H33E	109.5
C31—C34—H34B	109.5	C31C—C33C—H33F	109.5
H34A—C34—H34B	109.5	H33D—C33C—H33F	109.5
C31—C34—H34C	109.5	H33E—C33C—H33F	109.5
H34A—C34—H34C	109.5	C31C—C34C—H34D	109.5
H34B—C34—H34C	109.5	C31C—C34C—H34E	109.5
C38B—C35—C37B	115.3	H34D—C34C—H34E	109.5
C37A—C35—C36A	113.1	C31C—C34C—H34F	109.5
C38B—C35—C3	111.0	H34D—C34C—H34F	109.5
C37A—C35—C3	113.2	H34E—C34C—H34F	109.5
C37B—C35—C3	111.3	C36D—C35C—C37D	111.9
C36A—C35—C3	115.5	C36D—C35C—C3C	110.1
C38B—C35—C36B	109.9	C37E—C35C—C3C	113.7
C37B—C35—C36B	107.7	C37D—C35C—C3C	107.4
C3—C35—C36B	100.6	C36D—C35C—C38D	110.4
C37A—C35—C38A	104.1	C37D—C35C—C38D	106.9
C36A—C35—C38A	102.7	C3C—C35C—C38D	110.0
C3—C35—C38A	106.8	C37E—C35C—C38E	109.3
C35—C36A—H36A	109.5	C3C—C35C—C38E	111.9
C35—C36A—H36B	109.5	C37E—C35C—C36E	108.4
C35—C36A—H36C	109.5	C3C—C35C—C36E	108.2
C35—C37A—H37A	109.5	C38E—C35C—C36E	105.0
C35—C37A—H37B	109.5	C35C—C36D—H36G	109.5
C35—C37A—H37C	109.5	C35C—C36D—H36H	109.5
C35—C38A—H38A	109.5	C35C—C36D—H36I	109.5
C35—C38A—H38B	109.5	C35C—C37D—H37G	109.5
C35—C38A—H38C	109.5	C35C—C37D—H37H	109.5
C35—C36B—H36D	109.5	C35C—C37D—H37I	109.5
C35—C36B—H36E	109.5	C35C—C38D—H38G	109.5
H36D—C36B—H36E	109.5	C35C—C38D—H38H	109.5
C35—C36B—H36F	109.5	C35C—C38D—H38I	109.5
H36D—C36B—H36F	109.5	C35C—C36E—H36J	109.5
H36E—C36B—H36F	109.5	C35C—C36E—H36K	109.5
C35—C37B—H37D	109.5	H36J—C36E—H36K	109.5
C35—C37B—H37E	109.5	C35C—C36E—H36L	109.5
H37D—C37B—H37E	109.5	H36J—C36E—H36L	109.5
C35—C37B—H37F	109.5	H36K—C36E—H36L	109.5
H37D—C37B—H37F	109.5	C35C—C37E—H37J	109.5
H37E—C37B—H37F	109.5	C35C—C37E—H37K	109.5
C35—C38B—H38D	109.5	H37J—C37E—H37K	109.5
C35—C38B—H38E	109.5	C35C—C37E—H37L	109.5
H38D—C38B—H38E	109.5	H37J—C37E—H37L	109.5
C35—C38B—H38F	109.5	H37K—C37E—H37L	109.5
H38D—C38B—H38F	109.5	C35C—C38E—H38J	109.5
H38E—C38B—H38F	109.5	C35C—C38E—H38K	109.5
C42A—C39—C40A	110.1	H38J—C38E—H38K	109.5
C41B—C39—C1	109.4	C35C—C38E—H38L	109.5
C42A—C39—C1	112.9	H38J—C38E—H38L	109.5
C40A—C39—C1	111.6	H38K—C38E—H38L	109.5
C41B—C39—C40B	109.9	C41D—C39C—C40D	115.6
C1—C39—C40B	111.1	C42E—C39C—C41E	112.4
C41B—C39—C42B	109.6	C41D—C39C—C1C	108.2
C1—C39—C42B	109.9	C40D—C39C—C1C	112.2
C40B—C39—C42B	106.9	C42E—C39C—C1C	111.1
C42A—C39—C41A	107.5	C41E—C39C—C1C	114.5
C40A—C39—C41A	107.8	C41D—C39C—C42D	107.9
C1—C39—C41A	106.8	C40D—C39C—C42D	107.1
C39—C40A—H40A	109.5	C1C—C39C—C42D	105.2
C39—C40A—H40B	109.5	C42E—C39C—C40E	106.0
C39—C40A—H40C	109.5	C41E—C39C—C40E	105.0
C39—C41A—H41A	109.5	C1C—C39C—C40E	107.1
C39—C41A—H41B	109.5	C39C—C40D—H40G	109.5
C39—C41A—H41C	109.5	C39C—C40D—H40H	109.5
C39—C42A—H42A	109.5	C39C—C40D—H40I	109.5
C39—C42A—H42B	109.5	C39C—C41D—H41G	109.5
C39—C42A—H42C	109.5	C39C—C41D—H41H	109.5
C39—C40B—H40D	109.5	C39C—C41D—H41I	109.5
C39—C40B—H40E	109.5	C39C—C42D—H42G	109.5
H40D—C40B—H40E	109.5	C39C—C42D—H42H	109.5
C39—C40B—H40F	109.5	C39C—C42D—H42I	109.5
H40D—C40B—H40F	109.5	C39C—C40E—H40J	109.5
H40E—C40B—H40F	109.5	C39C—C40E—H40K	109.5
C39—C41B—H41D	109.5	C39C—C40E—H40L	109.5
C39—C41B—H41E	109.5	C39C—C41E—H41J	109.5
H41D—C41B—H41E	109.5	C39C—C41E—H41K	109.5
C39—C41B—H41F	109.5	C39C—C41E—H41L	109.5
H41D—C41B—H41F	109.5	C39C—C42E—H42J	109.5
H41E—C41B—H41F	109.5	C39C—C42E—H42K	109.5
C39—C42B—H42D	109.5	C39C—C42E—H42L	109.5
C39—C42B—H42E	109.5
C25—C1—C2—C3	0.4 (9)	C25C—C1C—C2C—C3C	0.1 (9)
C39—C1—C2—C3	178.1 (6)	C39C—C1C—C2C—C3C	−178.3 (6)
C1—C2—C3—C4	0.4 (10)	C1C—C2C—C3C—C4C	−1.3 (9)
C1—C2—C3—C35	−178.5 (6)	C1C—C2C—C3C—C35C	179.4 (5)
C2—C3—C4—C26	−1.6 (10)	C2C—C3C—C4C—C26C	2.8 (9)
C35—C3—C4—C26	177.3 (6)	C35C—C3C—C4C—C26C	−178.0 (5)
C26—C5—C6—C24	−179.3 (6)	C26C—C5C—C6C—C24C	178.6 (6)
C24—C7—C8—C22	−1.9 (10)	C24C—C7C—C8C—C22C	2.4 (8)
C22—C9—C10—C20	−6.2 (9)	C22C—C9C—C10C—C20C	5.0 (8)
C20—C11—C12—C18	−10.2 (10)	C20C—C11C—C12C—C18C	12.0 (9)
C18—C13—C14—C15	−7.2 (9)	C18C—C13C—C14C—C15C	8.3 (7)
C18—C13—C14—C27	179.9 (6)	C18C—C13C—C14C—C27C	−178.7 (5)
C13—C14—C15—C16	3.7 (8)	C13C—C14C—C15C—C16C	−4.4 (6)
C27—C14—C15—C16	177.0 (5)	C27C—C14C—C15C—C16C	−177.6 (4)
C14—C15—C16—C17	10.6 (8)	C14C—C15C—C16C—C17C	−9.5 (3)
C14—C15—C16—C31	−155.9 (5)	C14C—C15C—C16C—C31C	157.5 (4)
C15—C16—C17—C18	−20.7 (7)	C15C—C16C—C17C—C18C	18.9
C31—C16—C17—C18	143.8 (5)	C31C—C16C—C17C—C18C	−146.2 (3)
C15—C16—C17—C19	162.2 (5)	C15C—C16C—C17C—C19C	−162.6
C31—C16—C17—C19	−33.3 (8)	C31C—C16C—C17C—C19C	32.3 (3)
C14—C13—C18—C12	174.3 (6)	C14C—C13C—C18C—C17C	1.8 (6)
C14—C13—C18—C17	−3.8 (9)	C14C—C13C—C18C—C12C	−173.8 (5)
C11—C12—C18—C13	−179.5 (6)	C16C—C17C—C18C—C13C	−15.7 (3)
C11—C12—C18—C17	−1.3 (10)	C19C—C17C—C18C—C13C	165.6 (3)
C16—C17—C18—C13	17.9 (7)	C16C—C17C—C18C—C12C	159.9 (3)
C19—C17—C18—C13	−164.6 (5)	C19C—C17C—C18C—C12C	−18.8 (3)
C16—C17—C18—C12	−160.2 (5)	C11C—C12C—C18C—C13C	176.6 (5)
C19—C17—C18—C12	17.3 (7)	C11C—C12C—C18C—C17C	0.9 (7)
C18—C17—C19—C20	−22.3 (7)	C18C—C17C—C19C—C20C	24.7
C16—C17—C19—C20	154.8 (5)	C16C—C17C—C19C—C20C	−153.9
C18—C17—C19—C21	151.1 (5)	C18C—C17C—C19C—C21C	−147.6
C16—C17—C19—C21	−31.7 (8)	C16C—C17C—C19C—C21C	33.9
C17—C19—C20—C10	−171.1 (5)	C21C—C19C—C20C—C11C	159.8 (3)
C21—C19—C20—C10	15.1 (7)	C17C—C19C—C20C—C11C	−12.9 (3)
C17—C19—C20—C11	11.8 (8)	C21C—C19C—C20C—C10C	−16.0 (3)
C21—C19—C20—C11	−162.1 (5)	C17C—C19C—C20C—C10C	171.2 (3)
C9—C10—C20—C19	−3.9 (8)	C12C—C11C—C20C—C19C	−5.8 (7)
C9—C10—C20—C11	173.2 (6)	C12C—C11C—C20C—C10C	170.1 (5)
C12—C11—C20—C19	4.8 (9)	C9C—C10C—C20C—C19C	5.9 (7)
C12—C11—C20—C10	−172.3 (6)	C9C—C10C—C20C—C11C	−169.9 (5)
C20—C19—C21—C23	157.6 (5)	C20C—C19C—C21C—C23C	−160.2
C17—C19—C21—C23	−16.0 (7)	C17C—C19C—C21C—C23C	12.2
C20—C19—C21—C22	−16.6 (7)	C20C—C19C—C21C—C22C	15.7
C17—C19—C21—C22	169.8 (5)	C17C—C19C—C21C—C22C	−172.0
C23—C21—C22—C9	−167.4 (5)	C7C—C8C—C22C—C9C	−174.0 (5)
C19—C21—C22—C9	7.1 (7)	C7C—C8C—C22C—C21C	2.7 (6)
C23—C21—C22—C8	9.1 (7)	C10C—C9C—C22C—C8C	171.6 (5)
C19—C21—C22—C8	−176.4 (5)	C10C—C9C—C22C—C21C	−5.2 (6)
C10—C9—C22—C21	4.5 (8)	C23C—C21C—C22C—C8C	−6.1 (3)
C10—C9—C22—C8	−171.9 (6)	C19C—C21C—C22C—C8C	177.8 (3)
C7—C8—C22—C21	−5.2 (9)	C23C—C21C—C22C—C9C	170.8 (3)
C7—C8—C22—C9	171.2 (6)	C19C—C21C—C22C—C9C	−5.3 (3)
C22—C21—C23—C24	−6.6 (7)	C22C—C21C—C23C—C24C	4.6 (3)
C19—C21—C23—C24	179.2 (5)	C19C—C21C—C23C—C24C	−179.5 (3)
C21—C23—C24—C7	−0.3 (8)	C21C—C23C—C24C—C7C	0.4 (6)
C21—C23—C24—C6	178.0 (5)	C21C—C23C—C24C—C6C	−177.5 (3)
C8—C7—C24—C23	4.6 (9)	C8C—C7C—C24C—C23C	−4.0 (8)
C8—C7—C24—C6	−173.6 (6)	C8C—C7C—C24C—C6C	173.8 (5)
C5—C6—C24—C23	−179.5 (6)	C5C—C6C—C24C—C23C	−176.0 (6)
C5—C6—C24—C7	−1.3 (10)	C5C—C6C—C24C—C7C	6.2 (9)
C2—C1—C25—C26	0.1 (9)	C2C—C1C—C25C—C26C	−0.3 (10)
C39—C1—C25—C26	−177.6 (6)	C39C—C1C—C25C—C26C	178.1 (6)
C3—C4—C26—C25	2.0 (10)	C1C—C25C—C26C—C4C	1.7 (10)
C3—C4—C26—C5	−177.3 (6)	C1C—C25C—C26C—C5C	−179.3 (6)
C1—C25—C26—C4	−1.3 (10)	C3C—C4C—C26C—C25C	−3.0 (9)
C1—C25—C26—C5	178.0 (6)	C3C—C4C—C26C—C5C	178.0 (6)
C6—C5—C26—C4	166.1 (7)	C6C—C5C—C26C—C25C	19.4 (11)
C6—C5—C26—C25	−13.2 (12)	C6C—C5C—C26C—C4C	−161.6 (6)
C13—C14—C27—C30	117.7 (7)	C13C—C14C—C27C—C28C	122.0 (6)
C15—C14—C27—C30	−55.0 (7)	C15C—C14C—C27C—C28C	−65.3 (7)
C13—C14—C27—C29	−122.0 (7)	C13C—C14C—C27C—C29C	−119.1 (6)
C15—C14—C27—C29	65.3 (8)	C15C—C14C—C27C—C29C	53.6 (7)
C13—C14—C27—C28	−3.6 (10)	C13C—C14C—C27C—C30C	1.5 (9)
C15—C14—C27—C28	−176.3 (6)	C15C—C14C—C27C—C30C	174.2 (6)
C15—C16—C31—C33	169.2 (5)	C15C—C16C—C31C—C32C	66.3 (5)
C17—C16—C31—C33	4.3 (7)	C17C—C16C—C31C—C32C	−128.3 (4)
C15—C16—C31—C34	52.5 (6)	C15C—C16C—C31C—C33C	−166.8 (4)
C17—C16—C31—C34	−112.5 (5)	C17C—C16C—C31C—C33C	−1.3 (6)
C15—C16—C31—C32	−64.9 (6)	C15C—C16C—C31C—C34C	−51.9 (4)
C17—C16—C31—C32	130.1 (5)	C17C—C16C—C31C—C34C	113.5 (3)
C2—C3—C35—C38B	136.8	C4C—C3C—C35C—C36D	26.1
C4—C3—C35—C38B	−42.1	C2C—C3C—C35C—C36D	−154.6
C2—C3—C35—C37A	−33.3	C4C—C3C—C35C—C37E	−135.8
C4—C3—C35—C37A	147.9	C2C—C3C—C35C—C37E	43.5
C2—C3—C35—C37B	6.9	C4C—C3C—C35C—C37D	−96.0
C4—C3—C35—C37B	−171.9	C2C—C3C—C35C—C37D	83.3
C2—C3—C35—C36A	−165.9	C4C—C3C—C35C—C38D	148.0
C4—C3—C35—C36A	15.3	C2C—C3C—C35C—C38D	−32.7
C2—C3—C35—C36B	−107.0	C4C—C3C—C35C—C38E	99.8
C4—C3—C35—C36B	74.2	C2C—C3C—C35C—C38E	−81.0
C2—C3—C35—C38A	80.6	C4C—C3C—C35C—C36E	−15.3
C4—C3—C35—C38A	−98.2	C2C—C3C—C35C—C36E	163.9
C25—C1—C39—C41B	107.5	C2C—C1C—C39C—C41D	−129.6
C2—C1—C39—C41B	−70.1	C25C—C1C—C39C—C41D	52.0
C25—C1—C39—C42A	−166.3	C2C—C1C—C39C—C40D	−0.9
C2—C1—C39—C42A	16.1	C25C—C1C—C39C—C40D	−179.3
C25—C1—C39—C40A	−41.7	C2C—C1C—C39C—C42E	61.4
C2—C1—C39—C40A	140.7	C25C—C1C—C39C—C42E	−117.0
C25—C1—C39—C40B	−14.1	C2C—C1C—C39C—C41E	−170.0
C2—C1—C39—C40B	168.3	C25C—C1C—C39C—C41E	11.7
C25—C1—C39—C42B	−132.2	C2C—C1C—C39C—C42D	115.2
C2—C1—C39—C42B	50.2	C25C—C1C—C39C—C42D	−63.2
C25—C1—C39—C41A	75.8	C2C—C1C—C39C—C40E	−54.0
C2—C1—C39—C41A	−101.8	C25C—C1C—C39C—C40E	127.6

Trans-1-(para-tert-butylphenyl)-2-(2-benzo[c]phenanthrenyl)ethylene (VIIa)

Crystal data

C30H26	F(000) = 824
Mr = 386.51	Dx = 1.222 Mg m^−3
Monoclinic, p_21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -p_2ybc	Cell parameters from 2542 reflections
a = 15.8912 (15) Å	θ = 2.6–27.4°
b = 15.3430 (14) Å	µ = 0.07 mm^−1
c = 8.6285 (8) Å	T = 100 K
β = 92.680 (2)°	Plate, colorless
V = 2101.5 (3) Å^3	0.6 × 0.18 × 0.10 mm
Z = 4

Data collection

CCD area detector diffractometer	5024 independent reflections
Radiation source: fine-focus sealed tube	3123 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
phi and ω scans	θmax = 28.3°, θmin = 1.9°
Absorption correction: multi-scan SADABS (Bruker)	h = −20→17
Tmin = 0.630, Tmax = 0.993	k = −20→20
13315 measured reflections	l = −11→10

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)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.136	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0543P)^2 + 0.7071P] where P = (Fo^2 + 2Fc^2)/3
5024 reflections	(Δ/σ)max = 0.001
274 parameters	Δρmax = 0.27 e Å^−3
0 restraints	Δρmin = −0.24 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
C1	1.02198 (11)	0.16465 (11)	0.5018 (2)	0.0231 (4)
H1	1.0055	0.1949	0.4093	0.028*
C2	1.09900 (10)	0.12008 (11)	0.5102 (2)	0.0210 (4)
C3	1.12025 (12)	0.07772 (12)	0.6485 (2)	0.0292 (4)
H3	1.1722	0.0472	0.6588	0.035*
C4	1.06748 (12)	0.07883 (12)	0.7721 (2)	0.0301 (4)
H4	1.0843	0.0492	0.8652	0.036*
C5	0.93667 (11)	0.12099 (11)	0.8967 (2)	0.0244 (4)
H5	0.9626	0.1030	0.9929	0.029*
C6	0.85515 (11)	0.14239 (11)	0.8978 (2)	0.0212 (4)
H6	0.8288	0.1609	0.8022	0.025*
C7	0.83737 (11)	0.13522 (11)	1.1870 (2)	0.0248 (4)
H7	0.8966	0.1297	1.2051	0.030*
C8	0.78617 (11)	0.13856 (11)	1.3093 (2)	0.0242 (4)
H8	0.8107	0.1380	1.4119	0.029*
C9	0.64633 (12)	0.15586 (11)	1.4167 (2)	0.0237 (4)
H9	0.6709	0.1547	1.5192	0.028*
C10	0.56257 (12)	0.16985 (10)	1.3932 (2)	0.0231 (4)
H10	0.5300	0.1853	1.4786	0.028*
C11	0.43346 (11)	0.17359 (11)	1.2248 (2)	0.0245 (4)
H11	0.4029	0.1912	1.3116	0.029*
C12	0.39183 (11)	0.16023 (11)	1.0871 (2)	0.0251 (4)
H12	0.3333	0.1727	1.0764	0.030*
C13	0.38848 (11)	0.10532 (11)	0.8189 (2)	0.0249 (4)
H13	0.3298	0.1170	0.8097	0.030*
C14	0.42694 (11)	0.06720 (11)	0.6977 (2)	0.0255 (4)
H14	0.3959	0.0548	0.6035	0.031*
C15	0.51288 (11)	0.04670 (11)	0.7146 (2)	0.0225 (4)
H15	0.5394	0.0173	0.6331	0.027*
C16	0.55917 (11)	0.06848 (10)	0.84675 (19)	0.0196 (4)
H16	0.6171	0.0530	0.8556	0.023*
C17	0.52290 (10)	0.11358 (10)	0.97094 (19)	0.0183 (4)
C18	0.43429 (11)	0.12777 (10)	0.9578 (2)	0.0217 (4)
C19	0.56909 (10)	0.13854 (10)	1.11370 (19)	0.0182 (4)
C20	0.52243 (11)	0.16184 (10)	1.2428 (2)	0.0208 (4)
C21	0.66043 (11)	0.13952 (10)	1.13461 (19)	0.0191 (4)
C22	0.69769 (11)	0.14285 (10)	1.2873 (2)	0.0210 (4)
C23	0.71603 (10)	0.14315 (10)	1.0104 (2)	0.0193 (4)
H23	0.6927	0.1480	0.9074	0.023*
C24	0.80267 (11)	0.13990 (10)	1.0332 (2)	0.0210 (4)
C25	0.96928 (11)	0.16571 (11)	0.6248 (2)	0.0231 (4)
H25	0.9176	0.1967	0.6149	0.028*
C26	0.99039 (11)	0.12227 (11)	0.7632 (2)	0.0221 (4)
C27	1.15873 (11)	0.12334 (11)	0.3756 (2)	0.0233 (4)
C28	1.21849 (12)	0.04492 (13)	0.3785 (2)	0.0342 (5)
H28A	1.1855	−0.0091	0.3726	0.051*
H28B	1.2535	0.0455	0.4750	0.051*
H28C	1.2546	0.0481	0.2897	0.051*
C29	1.10993 (12)	0.12261 (14)	0.2183 (2)	0.0348 (5)
H29A	1.0753	0.1753	0.2080	0.052*
H29B	1.0736	0.0710	0.2113	0.052*
H29C	1.1497	0.1210	0.1349	0.052*
C30	1.21013 (14)	0.20751 (14)	0.3917 (3)	0.0456 (6)
H30A	1.2475	0.2123	0.3049	0.068*
H30B	1.2439	0.2065	0.4896	0.068*
H30C	1.1719	0.2576	0.3909	0.068*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0193 (9)	0.0264 (9)	0.0237 (9)	0.0023 (7)	−0.0002 (7)	0.0000 (7)
C2	0.0166 (9)	0.0192 (8)	0.0272 (9)	−0.0034 (7)	0.0014 (7)	−0.0025 (7)
C3	0.0187 (10)	0.0332 (10)	0.0359 (11)	0.0073 (8)	0.0037 (8)	0.0066 (8)
C4	0.0226 (10)	0.0352 (10)	0.0326 (11)	0.0039 (8)	0.0039 (8)	0.0106 (8)
C5	0.0197 (9)	0.0273 (9)	0.0265 (10)	−0.0030 (7)	0.0030 (7)	0.0012 (8)
C6	0.0197 (9)	0.0200 (8)	0.0240 (9)	−0.0018 (7)	0.0011 (7)	−0.0008 (7)
C7	0.0188 (9)	0.0259 (9)	0.0295 (10)	−0.0022 (7)	−0.0019 (7)	0.0015 (8)
C8	0.0263 (10)	0.0245 (9)	0.0212 (9)	−0.0035 (7)	−0.0029 (7)	0.0010 (7)
C9	0.0334 (11)	0.0179 (8)	0.0200 (9)	−0.0037 (7)	0.0031 (8)	0.0001 (7)
C10	0.0302 (10)	0.0160 (8)	0.0239 (9)	−0.0013 (7)	0.0095 (8)	−0.0018 (7)
C11	0.0258 (10)	0.0197 (8)	0.0290 (10)	0.0038 (7)	0.0117 (8)	0.0007 (7)
C12	0.0192 (9)	0.0209 (8)	0.0358 (11)	0.0043 (7)	0.0069 (8)	0.0027 (8)
C13	0.0193 (9)	0.0229 (9)	0.0326 (11)	0.0008 (7)	0.0006 (8)	0.0050 (8)
C14	0.0249 (10)	0.0245 (9)	0.0268 (10)	−0.0026 (8)	−0.0025 (8)	0.0012 (7)
C15	0.0235 (10)	0.0203 (8)	0.0240 (9)	−0.0042 (7)	0.0045 (7)	−0.0001 (7)
C16	0.0167 (9)	0.0177 (8)	0.0247 (9)	−0.0024 (7)	0.0043 (7)	0.0020 (7)
C17	0.0179 (9)	0.0148 (7)	0.0223 (9)	−0.0011 (6)	0.0039 (7)	0.0037 (6)
C18	0.0194 (9)	0.0168 (8)	0.0294 (10)	0.0009 (7)	0.0043 (7)	0.0039 (7)
C19	0.0188 (9)	0.0132 (7)	0.0229 (9)	0.0001 (6)	0.0043 (7)	0.0024 (6)
C20	0.0238 (9)	0.0132 (7)	0.0259 (9)	−0.0002 (7)	0.0068 (7)	0.0010 (7)
C21	0.0221 (9)	0.0125 (7)	0.0229 (9)	−0.0013 (6)	0.0033 (7)	−0.0001 (6)
C22	0.0251 (10)	0.0145 (8)	0.0233 (9)	−0.0031 (7)	0.0020 (7)	0.0017 (7)
C23	0.0190 (9)	0.0175 (8)	0.0213 (9)	−0.0002 (7)	0.0019 (7)	−0.0004 (7)
C24	0.0200 (9)	0.0167 (8)	0.0264 (9)	−0.0012 (7)	0.0019 (7)	−0.0006 (7)
C25	0.0161 (9)	0.0257 (9)	0.0275 (10)	0.0017 (7)	0.0000 (7)	−0.0019 (7)
C26	0.0165 (9)	0.0223 (8)	0.0274 (9)	−0.0024 (7)	0.0009 (7)	−0.0016 (7)
C27	0.0176 (9)	0.0230 (9)	0.0297 (10)	−0.0002 (7)	0.0049 (7)	−0.0018 (7)
C28	0.0308 (11)	0.0405 (11)	0.0316 (11)	0.0117 (9)	0.0060 (9)	−0.0010 (9)
C29	0.0290 (11)	0.0471 (12)	0.0288 (10)	0.0074 (9)	0.0067 (8)	0.0072 (9)
C30	0.0411 (13)	0.0358 (12)	0.0625 (16)	−0.0162 (10)	0.0305 (11)	−0.0177 (11)

Geometric parameters (Å, º)

C1—C25	1.382 (2)	C13—C18	1.416 (2)
C1—C2	1.401 (2)	C13—H13	0.9500
C1—H1	0.9500	C14—C15	1.402 (2)
C2—C3	1.386 (2)	C14—H14	0.9500
C2—C27	1.535 (2)	C15—C16	1.369 (2)
C3—C4	1.387 (2)	C15—H15	0.9500
C3—H3	0.9500	C16—C17	1.420 (2)
C4—C26	1.394 (2)	C16—H16	0.9500
C4—H4	0.9500	C17—C18	1.424 (2)
C5—C6	1.337 (2)	C17—C19	1.455 (2)
C5—C26	1.466 (2)	C19—C20	1.413 (2)
C5—H5	0.9500	C19—C21	1.454 (2)
C6—C24	1.468 (2)	C21—C22	1.420 (2)
C6—H6	0.9500	C21—C23	1.421 (2)
C7—C8	1.363 (2)	C23—C24	1.383 (2)
C7—C24	1.415 (2)	C23—H23	0.9500
C7—H7	0.9500	C25—C26	1.395 (2)
C8—C22	1.412 (2)	C25—H25	0.9500
C8—H8	0.9500	C27—C30	1.531 (3)
C9—C10	1.354 (2)	C27—C29	1.532 (3)
C9—C22	1.428 (2)	C27—C28	1.532 (2)
C9—H9	0.9500	C28—H28A	0.9800
C10—C20	1.425 (2)	C28—H28B	0.9800
C10—H10	0.9500	C28—H28C	0.9800
C11—C12	1.348 (3)	C29—H29A	0.9800
C11—C20	1.426 (2)	C29—H29B	0.9800
C11—H11	0.9500	C29—H29C	0.9800
C12—C18	1.421 (2)	C30—H30A	0.9800
C12—H12	0.9500	C30—H30B	0.9800
C13—C14	1.367 (2)	C30—H30C	0.9800
C25—C1—C2	121.68 (17)	C13—C18—C12	120.39 (16)
C25—C1—H1	119.2	C13—C18—C17	119.84 (16)
C2—C1—H1	119.2	C12—C18—C17	119.69 (16)
C3—C2—C1	116.77 (16)	C20—C19—C21	117.21 (15)
C3—C2—C27	122.14 (15)	C20—C19—C17	118.12 (15)
C1—C2—C27	120.98 (16)	C21—C19—C17	124.66 (15)
C2—C3—C4	121.61 (17)	C19—C20—C10	120.73 (16)
C2—C3—H3	119.2	C19—C20—C11	120.03 (16)
C4—C3—H3	119.2	C10—C20—C11	119.18 (16)
C3—C4—C26	121.65 (18)	C22—C21—C23	116.81 (16)
C3—C4—H4	119.2	C22—C21—C19	119.08 (15)
C26—C4—H4	119.2	C23—C21—C19	123.98 (16)
C6—C5—C26	127.03 (17)	C8—C22—C21	119.52 (16)
C6—C5—H5	116.5	C8—C22—C9	120.24 (16)
C26—C5—H5	116.5	C21—C22—C9	120.13 (16)
C5—C6—C24	125.86 (17)	C24—C23—C21	122.77 (16)
C5—C6—H6	117.1	C24—C23—H23	118.6
C24—C6—H6	117.1	C21—C23—H23	118.6
C8—C7—C24	120.23 (17)	C23—C24—C7	118.51 (16)
C8—C7—H7	119.9	C23—C24—C6	119.00 (16)
C24—C7—H7	119.9	C7—C24—C6	122.49 (16)
C7—C8—C22	121.63 (17)	C1—C25—C26	121.43 (16)
C7—C8—H8	119.2	C1—C25—H25	119.3
C22—C8—H8	119.2	C26—C25—H25	119.3
C10—C9—C22	119.92 (17)	C4—C26—C25	116.84 (16)
C10—C9—H9	120.0	C4—C26—C5	119.55 (17)
C22—C9—H9	120.0	C25—C26—C5	123.61 (16)
C9—C10—C20	121.20 (16)	C30—C27—C29	109.41 (17)
C9—C10—H10	119.4	C30—C27—C28	109.46 (16)
C20—C10—H10	119.4	C29—C27—C28	107.23 (15)
C12—C11—C20	121.31 (16)	C30—C27—C2	107.77 (14)
C12—C11—H11	119.3	C29—C27—C2	111.42 (15)
C20—C11—H11	119.3	C28—C27—C2	111.53 (15)
C11—C12—C18	120.91 (17)	C27—C28—H28A	109.5
C11—C12—H12	119.5	C27—C28—H28B	109.5
C18—C12—H12	119.5	H28A—C28—H28B	109.5
C14—C13—C18	121.41 (17)	C27—C28—H28C	109.5
C14—C13—H13	119.3	H28A—C28—H28C	109.5
C18—C13—H13	119.3	H28B—C28—H28C	109.5
C13—C14—C15	119.00 (17)	C27—C29—H29A	109.5
C13—C14—H14	120.5	C27—C29—H29B	109.5
C15—C14—H14	120.5	H29A—C29—H29B	109.5
C16—C15—C14	120.94 (16)	C27—C29—H29C	109.5
C16—C15—H15	119.5	H29A—C29—H29C	109.5
C14—C15—H15	119.5	H29B—C29—H29C	109.5
C15—C16—C17	121.74 (16)	C27—C30—H30A	109.5
C15—C16—H16	119.1	C27—C30—H30B	109.5
C17—C16—H16	119.1	H30A—C30—H30B	109.5
C16—C17—C18	116.69 (15)	C27—C30—H30C	109.5
C16—C17—C19	124.08 (15)	H30A—C30—H30C	109.5
C18—C17—C19	119.00 (15)	H30B—C30—H30C	109.5
C25—C1—C2—C3	−0.6 (3)	C20—C19—C21—C22	14.8 (2)
C25—C1—C2—C27	−176.94 (16)	C17—C19—C21—C22	−163.81 (15)
C1—C2—C3—C4	0.5 (3)	C20—C19—C21—C23	−160.84 (15)
C27—C2—C3—C4	176.80 (17)	C17—C19—C21—C23	20.5 (2)
C2—C3—C4—C26	0.3 (3)	C7—C8—C22—C21	3.0 (2)
C26—C5—C6—C24	179.53 (16)	C7—C8—C22—C9	−173.14 (16)
C24—C7—C8—C22	2.8 (3)	C23—C21—C22—C8	−7.8 (2)
C22—C9—C10—C20	7.4 (2)	C19—C21—C22—C8	176.21 (15)
C20—C11—C12—C18	4.7 (3)	C23—C21—C22—C9	168.34 (15)
C18—C13—C14—C15	2.7 (3)	C19—C21—C22—C9	−7.6 (2)
C13—C14—C15—C16	−3.5 (3)	C10—C9—C22—C8	172.48 (16)
C14—C15—C16—C17	−0.9 (2)	C10—C9—C22—C21	−3.6 (2)
C15—C16—C17—C18	5.8 (2)	C22—C21—C23—C24	7.4 (2)
C15—C16—C17—C19	−179.83 (15)	C19—C21—C23—C24	−176.89 (15)
C14—C13—C18—C12	−174.44 (16)	C21—C23—C24—C7	−1.8 (2)
C14—C13—C18—C17	2.3 (2)	C21—C23—C24—C6	178.86 (15)
C11—C12—C18—C13	173.32 (16)	C8—C7—C24—C23	−3.4 (2)
C11—C12—C18—C17	−3.5 (2)	C8—C7—C24—C6	175.88 (16)
C16—C17—C18—C13	−6.4 (2)	C5—C6—C24—C23	−164.41 (17)
C19—C17—C18—C13	178.91 (15)	C5—C6—C24—C7	16.3 (3)
C16—C17—C18—C12	170.37 (15)	C2—C1—C25—C26	−0.1 (3)
C19—C17—C18—C12	−4.3 (2)	C3—C4—C26—C25	−0.9 (3)
C16—C17—C19—C20	−163.56 (15)	C3—C4—C26—C5	179.59 (18)
C18—C17—C19—C20	10.7 (2)	C1—C25—C26—C4	0.8 (3)
C16—C17—C19—C21	15.1 (2)	C1—C25—C26—C5	−179.71 (16)
C18—C17—C19—C21	−170.70 (15)	C6—C5—C26—C4	−164.65 (18)
C21—C19—C20—C10	−11.4 (2)	C6—C5—C26—C25	15.9 (3)
C17—C19—C20—C10	167.33 (15)	C3—C2—C27—C30	−93.4 (2)
C21—C19—C20—C11	171.59 (15)	C1—C2—C27—C30	82.8 (2)
C17—C19—C20—C11	−9.7 (2)	C3—C2—C27—C29	146.57 (17)
C9—C10—C20—C19	0.3 (2)	C1—C2—C27—C29	−37.3 (2)
C9—C10—C20—C11	177.37 (16)	C3—C2—C27—C28	26.8 (2)
C12—C11—C20—C19	2.1 (2)	C1—C2—C27—C28	−157.08 (16)
C12—C11—C20—C10	−174.94 (16)

Trans-1-(para-tert-butylphenyl)-2-(2-benzo[c]phenanthrenyl)ethylene (VIIahigh)

Crystal data

C30H26	F(000) = 824
Mr = 386.51	Dx = 1.222 Mg m^−3
Monoclinic, p_21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -p_2ybc	Cell parameters from 2542 reflections
a = 15.8912 (15) Å	θ = 2.6–27.4°
b = 15.3430 (14) Å	µ = 0.07 mm^−1
c = 8.6285 (8) Å	T = 100 K
β = 92.680 (2)°	Plate, colourless
V = 2101.5 (3) Å^3	0.6 × 0.18 × 0.10 mm
Z = 4

Data collection

CCD area detector diffractometer	3750 independent reflections
Radiation source: fine-focus sealed tube	2057 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.081
phi and ω scans	θmax = 28.3°, θmin = 17.2°
Absorption correction: multi-scan SADABS (Bruker)	h = −20→17
Tmin = 0.630, Tmax = 0.993	k = −20→20
8635 measured reflections	l = −11→10

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full with fixed elements per cycle	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.057	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.160	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0542P)^2 + 0.5056P] where P = (Fo^2 + 2Fc^2)/3
3750 reflections	(Δ/σ)max < 0.001
181 parameters	Δρmax = 0.19 e Å^−3
0 restraints	Δρmin = −0.18 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 with d 1.2–0 (theta_min 17.24) (181 parameters, U only refined). 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
C1	1.0220	0.1647	0.5018	0.0216 (5)
H1	1.0055	0.1949	0.4093	0.026*
C2	1.0990	0.1201	0.5102	0.0197 (5)
C3	1.1202	0.0777	0.6485	0.0274 (6)
H3	1.1722	0.0472	0.6588	0.033*
C4	1.0675	0.0788	0.7721	0.0286 (6)
H4	1.0843	0.0492	0.8652	0.034*
C5	0.9367	0.1210	0.8967	0.0229 (5)
H5	0.9626	0.1030	0.9929	0.027*
C6	0.8552	0.1424	0.8978	0.0191 (5)
H6	0.8288	0.1609	0.8022	0.023*
C7	0.8374	0.1352	1.1870	0.0234 (5)
H7	0.8966	0.1297	1.2051	0.028*
C8	0.7862	0.1386	1.3093	0.0227 (5)
H8	0.8107	0.1380	1.4119	0.027*
C9	0.6463	0.1559	1.4167	0.0224 (5)
H9	0.6709	0.1547	1.5192	0.027*
C10	0.5626	0.1698	1.3932	0.0215 (5)
H10	0.5300	0.1853	1.4786	0.026*
C11	0.4335	0.1736	1.2248	0.0227 (5)
H11	0.4029	0.1912	1.3116	0.027*
C12	0.3918	0.1602	1.0871	0.0236 (5)
H12	0.3333	0.1727	1.0764	0.028*
C13	0.3885	0.1053	0.8189	0.0237 (5)
H13	0.3298	0.1170	0.8097	0.028*
C14	0.4269	0.0672	0.6977	0.0236 (5)
H14	0.3959	0.0548	0.6035	0.028*
C15	0.5129	0.0467	0.7146	0.0211 (5)
H15	0.5394	0.0173	0.6331	0.025*
C16	0.5592	0.0685	0.8467	0.0181 (5)
H16	0.6171	0.0530	0.8556	0.022*
C17	0.5229	0.1136	0.9709	0.0172 (5)
C18	0.4343	0.1278	0.9578	0.0205 (5)
C19	0.5691	0.1385	1.1137	0.0170 (5)
C20	0.5224	0.1618	1.2428	0.0196 (5)
C21	0.6604	0.1395	1.1346	0.0180 (5)
C22	0.6977	0.1429	1.2873	0.0200 (5)
C23	0.7160	0.1431	1.0104	0.0176 (5)
H23	0.6927	0.1480	0.9074	0.021*
C24	0.8027	0.1399	1.0332	0.0200 (5)
C25	0.9693	0.1657	0.6248	0.0218 (5)
H25	0.9176	0.1967	0.6149	0.026*
C26	0.9904	0.1223	0.7632	0.0212 (5)
C27	1.1587	0.1233	0.3756	0.0219 (5)
C28	1.2185	0.0449	0.3785	0.0323 (6)
H28A	1.1855	−0.0091	0.3726	0.048*
H28B	1.2535	0.0455	0.4750	0.048*
H28C	1.2546	0.0481	0.2897	0.048*
C29	1.1099	0.1226	0.2183	0.0327 (6)
H29A	1.0753	0.1753	0.2080	0.049*
H29B	1.0736	0.0710	0.2113	0.049*
H29C	1.1497	0.1210	0.1349	0.049*
C30	1.2101	0.2075	0.3917	0.0426 (8)
H30A	1.2475	0.2123	0.3049	0.064*
H30B	1.2439	0.2065	0.4896	0.064*
H30C	1.1719	0.2576	0.3909	0.064*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0178 (11)	0.0246 (10)	0.0222 (11)	0.0022 (8)	0.0000 (8)	−0.0002 (8)
C2	0.0151 (10)	0.0182 (9)	0.0259 (11)	−0.0035 (7)	0.0021 (8)	−0.0027 (8)
C3	0.0179 (11)	0.0305 (11)	0.0340 (13)	0.0075 (9)	0.0032 (9)	0.0064 (10)
C4	0.0212 (12)	0.0339 (12)	0.0309 (13)	0.0035 (9)	0.0034 (10)	0.0101 (10)
C5	0.0185 (11)	0.0257 (10)	0.0246 (11)	−0.0031 (8)	0.0025 (8)	0.0017 (9)
C6	0.0180 (10)	0.0184 (9)	0.0211 (11)	−0.0014 (8)	0.0014 (8)	−0.0009 (7)
C7	0.0182 (10)	0.0242 (10)	0.0277 (12)	−0.0026 (8)	−0.0023 (8)	0.0019 (9)
C8	0.0251 (12)	0.0233 (10)	0.0194 (11)	−0.0032 (9)	−0.0028 (8)	0.0003 (8)
C9	0.0317 (13)	0.0171 (9)	0.0184 (11)	−0.0035 (8)	0.0033 (9)	−0.0005 (7)
C10	0.0286 (12)	0.0152 (9)	0.0215 (11)	−0.0014 (8)	0.0090 (9)	−0.0012 (8)
C11	0.0250 (12)	0.0183 (9)	0.0259 (12)	0.0039 (8)	0.0118 (9)	0.0009 (8)
C12	0.0178 (10)	0.0194 (9)	0.0340 (13)	0.0040 (8)	0.0065 (9)	0.0021 (9)
C13	0.0178 (11)	0.0225 (10)	0.0308 (13)	0.0010 (8)	0.0004 (9)	0.0045 (9)
C14	0.0234 (12)	0.0226 (10)	0.0246 (11)	−0.0025 (8)	−0.0021 (9)	0.0010 (8)
C15	0.0232 (12)	0.0186 (9)	0.0220 (11)	−0.0043 (8)	0.0044 (8)	−0.0004 (8)
C16	0.0158 (10)	0.0166 (9)	0.0221 (11)	−0.0015 (7)	0.0039 (8)	0.0019 (8)
C17	0.0167 (10)	0.0137 (8)	0.0214 (11)	−0.0013 (7)	0.0042 (8)	0.0033 (7)
C18	0.0178 (11)	0.0161 (9)	0.0279 (12)	0.0010 (8)	0.0042 (8)	0.0033 (8)
C19	0.0181 (10)	0.0121 (8)	0.0211 (10)	0.0005 (7)	0.0043 (8)	0.0020 (7)
C20	0.0225 (11)	0.0129 (8)	0.0239 (11)	−0.0002 (7)	0.0064 (9)	0.0014 (7)
C21	0.0211 (11)	0.0121 (8)	0.0209 (10)	−0.0018 (7)	0.0035 (8)	−0.0002 (7)
C22	0.0241 (11)	0.0138 (9)	0.0221 (11)	−0.0027 (8)	0.0021 (8)	0.0019 (7)
C23	0.0173 (10)	0.0164 (9)	0.0194 (10)	−0.0002 (7)	0.0025 (8)	−0.0004 (7)
C24	0.0186 (10)	0.0163 (9)	0.0255 (11)	−0.0014 (8)	0.0031 (8)	−0.0008 (8)
C25	0.0153 (10)	0.0239 (10)	0.0261 (12)	0.0015 (8)	−0.0003 (8)	−0.0015 (8)
C26	0.0162 (10)	0.0208 (10)	0.0266 (12)	−0.0022 (8)	0.0014 (8)	−0.0016 (8)
C27	0.0166 (10)	0.0217 (10)	0.0277 (12)	−0.0006 (8)	0.0048 (8)	−0.0017 (8)
C28	0.0302 (14)	0.0379 (13)	0.0293 (13)	0.0128 (11)	0.0057 (10)	−0.0012 (10)
C29	0.0267 (13)	0.0460 (15)	0.0259 (12)	0.0072 (11)	0.0056 (10)	0.0073 (11)
C30	0.0389 (16)	0.0330 (13)	0.058 (2)	−0.0164 (12)	0.0295 (15)	−0.0185 (13)

Geometric parameters (Å, º)

C1—C25	1.3824	C13—C18	1.4155
C1—C2	1.4009	C13—H13	0.9500
C1—H1	0.9500	C14—C15	1.4024
C2—C3	1.3863	C14—H14	0.9500
C2—C27	1.5348	C15—C16	1.3694
C3—C4	1.3874	C15—H15	0.9500
C3—H3	0.9500	C16—C17	1.4202
C4—C26	1.3936	C16—H16	0.9500
C4—H4	0.9500	C17—C18	1.4241
C5—C6	1.3368	C17—C19	1.4554
C5—C26	1.4656	C19—C20	1.4126
C5—H5	0.9500	C19—C21	1.4542
C6—C24	1.4679	C21—C22	1.4200
C6—H6	0.9500	C21—C23	1.4214
C7—C8	1.3633	C23—C24	1.3825
C7—C24	1.4147	C23—H23	0.9500
C7—H7	0.9500	C25—C26	1.3946
C8—C22	1.4116	C25—H25	0.9500
C8—H8	0.9500	C27—C30	1.5309
C9—C10	1.3542	C27—C29	1.5317
C9—C22	1.4277	C27—C28	1.5323
C9—H9	0.9500	C28—H28A	0.9800
C10—C20	1.4246	C28—H28B	0.9800
C10—H10	0.9500	C28—H28C	0.9800
C11—C12	1.3480	C29—H29A	0.9800
C11—C20	1.4265	C29—H29B	0.9800
C11—H11	0.9500	C29—H29C	0.9800
C12—C18	1.4209	C30—H30A	0.9800
C12—H12	0.9500	C30—H30B	0.9800
C13—C14	1.3669	C30—H30C	0.9800
C25—C1—C2	121.7	C13—C18—C12	120.4
C25—C1—H1	119.2	C13—C18—C17	119.8
C2—C1—H1	119.2	C12—C18—C17	119.7
C3—C2—C1	116.8	C20—C19—C21	117.2
C3—C2—C27	122.1	C20—C19—C17	118.1
C1—C2—C27	121.0	C21—C19—C17	124.7
C2—C3—C4	121.6	C19—C20—C10	120.7
C2—C3—H3	119.2	C19—C20—C11	120.0
C4—C3—H3	119.2	C10—C20—C11	119.2
C3—C4—C26	121.7	C22—C21—C23	116.8
C3—C4—H4	119.2	C22—C21—C19	119.1
C26—C4—H4	119.2	C23—C21—C19	124.0
C6—C5—C26	127.0	C8—C22—C21	119.5
C6—C5—H5	116.5	C8—C22—C9	120.2
C26—C5—H5	116.5	C21—C22—C9	120.1
C5—C6—C24	125.9	C24—C23—C21	122.8
C5—C6—H6	117.1	C24—C23—H23	118.6
C24—C6—H6	117.1	C21—C23—H23	118.6
C8—C7—C24	120.2	C23—C24—C7	118.5
C8—C7—H7	119.9	C23—C24—C6	119.0
C24—C7—H7	119.9	C7—C24—C6	122.5
C7—C8—C22	121.6	C1—C25—C26	121.4
C7—C8—H8	119.2	C1—C25—H25	119.3
C22—C8—H8	119.2	C26—C25—H25	119.3
C10—C9—C22	119.9	C4—C26—C25	116.8
C10—C9—H9	120.0	C4—C26—C5	119.5
C22—C9—H9	120.0	C25—C26—C5	123.6
C9—C10—C20	121.2	C30—C27—C29	109.4
C9—C10—H10	119.4	C30—C27—C28	109.5
C20—C10—H10	119.4	C29—C27—C28	107.2
C12—C11—C20	121.3	C30—C27—C2	107.8
C12—C11—H11	119.3	C29—C27—C2	111.4
C20—C11—H11	119.3	C28—C27—C2	111.5
C11—C12—C18	120.9	C27—C28—H28A	109.5
C11—C12—H12	119.5	C27—C28—H28B	109.5
C18—C12—H12	119.5	H28A—C28—H28B	109.5
C14—C13—C18	121.4	C27—C28—H28C	109.5
C14—C13—H13	119.3	H28A—C28—H28C	109.5
C18—C13—H13	119.3	H28B—C28—H28C	109.5
C13—C14—C15	119.0	C27—C29—H29A	109.5
C13—C14—H14	120.5	C27—C29—H29B	109.5
C15—C14—H14	120.5	H29A—C29—H29B	109.5
C16—C15—C14	120.9	C27—C29—H29C	109.5
C16—C15—H15	119.5	H29A—C29—H29C	109.5
C14—C15—H15	119.5	H29B—C29—H29C	109.5
C15—C16—C17	121.7	C27—C30—H30A	109.5
C15—C16—H16	119.1	C27—C30—H30B	109.5
C17—C16—H16	119.1	H30A—C30—H30B	109.5
C16—C17—C18	116.7	C27—C30—H30C	109.5
C16—C17—C19	124.1	H30A—C30—H30C	109.5
C18—C17—C19	119.0	H30B—C30—H30C	109.5
C25—C1—C2—C3	−0.6	C20—C19—C21—C22	14.8
C25—C1—C2—C27	−176.9	C17—C19—C21—C22	−163.8
C1—C2—C3—C4	0.5	C20—C19—C21—C23	−160.8
C27—C2—C3—C4	176.8	C17—C19—C21—C23	20.5
C2—C3—C4—C26	0.3	C7—C8—C22—C21	3.0
C26—C5—C6—C24	179.5	C7—C8—C22—C9	−173.1
C24—C7—C8—C22	2.8	C23—C21—C22—C8	−7.8
C22—C9—C10—C20	7.4	C19—C21—C22—C8	176.2
C20—C11—C12—C18	4.7	C23—C21—C22—C9	168.3
C18—C13—C14—C15	2.7	C19—C21—C22—C9	−7.6
C13—C14—C15—C16	−3.5	C10—C9—C22—C8	172.5
C14—C15—C16—C17	−0.9	C10—C9—C22—C21	−3.6
C15—C16—C17—C18	5.8	C22—C21—C23—C24	7.4
C15—C16—C17—C19	−179.8	C19—C21—C23—C24	−176.9
C14—C13—C18—C12	−174.4	C21—C23—C24—C7	−1.8
C14—C13—C18—C17	2.3	C21—C23—C24—C6	178.9
C11—C12—C18—C13	173.3	C8—C7—C24—C23	−3.4
C11—C12—C18—C17	−3.5	C8—C7—C24—C6	175.9
C16—C17—C18—C13	−6.4	C5—C6—C24—C23	−164.4
C19—C17—C18—C13	178.9	C5—C6—C24—C7	16.3
C16—C17—C18—C12	170.4	C2—C1—C25—C26	−0.1
C19—C17—C18—C12	−4.3	C3—C4—C26—C25	−0.9
C16—C17—C19—C20	−163.6	C3—C4—C26—C5	179.6
C18—C17—C19—C20	10.7	C1—C25—C26—C4	0.8
C16—C17—C19—C21	15.1	C1—C25—C26—C5	−179.7
C18—C17—C19—C21	−170.7	C6—C5—C26—C4	−164.7
C21—C19—C20—C10	−11.4	C6—C5—C26—C25	15.9
C17—C19—C20—C10	167.3	C3—C2—C27—C30	−93.4
C21—C19—C20—C11	171.6	C1—C2—C27—C30	82.8
C17—C19—C20—C11	−9.7	C3—C2—C27—C29	146.6
C9—C10—C20—C19	0.3	C1—C2—C27—C29	−37.3
C9—C10—C20—C11	177.4	C3—C2—C27—C28	26.8
C12—C11—C20—C19	2.1	C1—C2—C27—C28	−157.1
C12—C11—C20—C10	−174.9

2,2",4,4",6,6"-hexa-tert-butyl-azobenzene (I)

Crystal data

C36H58N2	V = 6588.7 (18) Å^3
Mr = 518.84	Z = 8
Orthorhombic, Pbca	F(000) = 2304
Hall symbol: -P 2ac 2ab	Dx = 1.046 Mg m^−3
a = 16.495 (3) Å	Mo Kα radiation, λ = 0.71070 Å
b = 17.360 (3) Å	µ = 0.06 mm^−1
c = 23.009 (4) Å	T = 100 K

Data collection

Modified Huber diffractometer	Rint = 0.087
Radiation source: fine-focus sealed tube	θmax = 25.0°, θmin = 1.8°
Graphite monochromator	h = 0→19
θ/2θ scans	k = −20→20
10284 measured reflections	l = −27→27
5809 independent reflections	3 standard reflections every 97 reflections
3646 reflections with I > 2σ(I)

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)] = 0.085	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.240	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0853P)^2 + 11.3428P] where P = (Fo^2 + 2Fc^2)/3
5809 reflections	(Δ/σ)max < 0.001
361 parameters	Δρmax = 0.26 e Å^−3
0 restraints	Δρmin = −0.34 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. This is a re-refinement of the published structure (Acta Cryst. 1991, B47, 272–280) on F², all reflections, C—H distances 0.93–0.96 A.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
N1	0.41112 (19)	0.24037 (16)	0.18838 (12)	0.0261 (7)
C2	0.3767 (2)	0.23520 (19)	0.24644 (15)	0.0239 (8)
C3	0.3106 (2)	0.27733 (19)	0.26937 (15)	0.0252 (8)
C4	0.2734 (2)	0.2474 (2)	0.31858 (15)	0.0253 (8)
H4	0.2286	0.2732	0.3335	0.030*
C5	0.2995 (2)	0.18072 (19)	0.34681 (15)	0.0246 (8)
C6	0.3707 (2)	0.14709 (19)	0.32712 (15)	0.0261 (8)
H6	0.3914	0.1050	0.3472	0.031*
C7	0.4124 (2)	0.17384 (19)	0.27837 (15)	0.0254 (8)
C8	0.2851 (2)	0.35924 (18)	0.24896 (16)	0.0260 (8)
C9	0.3626 (2)	0.4071 (2)	0.23767 (17)	0.0296 (8)
H9A	0.3478	0.4569	0.2229	0.044*
H9B	0.3960	0.3810	0.2097	0.044*
H9C	0.3921	0.4131	0.2734	0.044*
C10	0.2286 (2)	0.3586 (2)	0.19571 (17)	0.0313 (9)
H10A	0.1821	0.3271	0.2038	0.047*
H10B	0.2571	0.3381	0.1628	0.047*
H10C	0.2112	0.4102	0.1873	0.047*
C11	0.2391 (3)	0.4027 (2)	0.29704 (17)	0.0373 (10)
H11A	0.2704	0.4016	0.3322	0.056*
H11B	0.1877	0.3784	0.3036	0.056*
H11C	0.2307	0.4551	0.2853	0.056*
C12	0.2539 (2)	0.1504 (2)	0.40020 (15)	0.0264 (8)
C13	0.2574 (3)	0.2114 (2)	0.44836 (17)	0.0400 (10)
H13A	0.3130	0.2238	0.4566	0.060*
H13B	0.2321	0.1916	0.4828	0.060*
H13C	0.2294	0.2570	0.4358	0.060*
C14	0.1648 (2)	0.1348 (2)	0.38444 (17)	0.0343 (9)
H14A	0.1407	0.1810	0.3693	0.051*
H14B	0.1359	0.1188	0.4185	0.051*
H14C	0.1622	0.0950	0.3556	0.051*
C15	0.2902 (3)	0.0757 (2)	0.42398 (17)	0.0379 (10)
H15A	0.2902	0.0372	0.3940	0.057*
H15B	0.2584	0.0580	0.4563	0.057*
H15C	0.3448	0.0849	0.4366	0.057*
C16	0.4950 (2)	0.13587 (19)	0.26302 (16)	0.0265 (8)
C17	0.5608 (2)	0.1976 (2)	0.25561 (17)	0.0306 (8)
H17A	0.6123	0.1731	0.2499	0.046*
H17B	0.5629	0.2292	0.2898	0.046*
H17C	0.5482	0.2290	0.2225	0.046*
C18	0.4893 (2)	0.0847 (2)	0.20869 (17)	0.0315 (9)
H18A	0.4742	0.1156	0.1758	0.047*
H18B	0.4493	0.0454	0.2148	0.047*
H18C	0.5410	0.0612	0.2015	0.047*
C19	0.5242 (2)	0.0836 (2)	0.31278 (17)	0.0322 (9)
H19A	0.5782	0.0662	0.3047	0.048*
H19B	0.4887	0.0400	0.3161	0.048*
H19C	0.5238	0.1120	0.3486	0.048*
N20	0.35918 (18)	0.24434 (16)	0.14848 (12)	0.0252 (7)
C21	0.3911 (2)	0.22619 (19)	0.09122 (15)	0.0225 (7)
C22	0.4538 (2)	0.26518 (19)	0.06144 (15)	0.0230 (7)
C23	0.4851 (2)	0.23003 (19)	0.01156 (15)	0.0242 (8)
H23	0.5272	0.2544	−0.0080	0.029*
C24	0.4563 (2)	0.16028 (19)	−0.01039 (15)	0.0252 (8)
C25	0.3885 (2)	0.12832 (19)	0.01690 (15)	0.0247 (8)
H25	0.3655	0.0841	0.0011	0.030*
C26	0.3539 (2)	0.15991 (19)	0.06682 (15)	0.0232 (8)
C27	0.4823 (2)	0.34874 (19)	0.07562 (15)	0.0248 (8)
C28	0.4068 (2)	0.39958 (19)	0.08468 (17)	0.0296 (8)
H28A	0.3746	0.3789	0.1157	0.044*
H28B	0.3753	0.4005	0.0496	0.044*
H28C	0.4234	0.4510	0.0944	0.044*
C29	0.5384 (2)	0.3516 (2)	0.12872 (16)	0.0287 (8)
H29A	0.5830	0.3169	0.1231	0.043*
H29B	0.5087	0.3368	0.1628	0.043*
H29C	0.5588	0.4031	0.1335	0.043*
C30	0.5293 (3)	0.3848 (2)	0.02473 (17)	0.0338 (9)
H30A	0.5397	0.4381	0.0329	0.051*
H30B	0.4978	0.3805	−0.0102	0.051*
H30C	0.5799	0.3581	0.0197	0.051*
C31	0.4940 (2)	0.12560 (19)	−0.06557 (16)	0.0271 (8)
C32	0.5858 (2)	0.1141 (2)	−0.05645 (17)	0.0335 (9)
H32A	0.6109	0.1630	−0.0489	0.050*
H32B	0.6091	0.0918	−0.0908	0.050*
H32C	0.5946	0.0803	−0.0240	0.050*
C33	0.4814 (3)	0.1822 (2)	−0.11645 (16)	0.0360 (9)
H33A	0.4244	0.1898	−0.1227	0.054*
H33B	0.5054	0.1613	−0.1510	0.054*
H33C	0.5064	0.2306	−0.1073	0.054*
C34	0.4561 (3)	0.0481 (2)	−0.08220 (17)	0.0340 (9)
H34A	0.4632	0.0122	−0.0509	0.051*
H34B	0.4822	0.0285	−0.1165	0.051*
H34C	0.3993	0.0549	−0.0897	0.051*
C35	0.2735 (2)	0.1246 (2)	0.09037 (16)	0.0273 (8)
C36	0.2066 (2)	0.1862 (2)	0.09135 (17)	0.0303 (8)
H36A	0.2005	0.2078	0.0532	0.045*
H36B	0.2211	0.2261	0.1183	0.045*
H36C	0.1564	0.1631	0.1032	0.045*
C37	0.2427 (2)	0.0593 (2)	0.05100 (18)	0.0346 (9)
H37A	0.2817	0.0182	0.0505	0.052*
H37B	0.2353	0.0785	0.0122	0.052*
H37C	0.1920	0.0404	0.0656	0.052*
C38	0.2836 (2)	0.0891 (2)	0.15117 (17)	0.0341 (9)
H38A	0.2354	0.0612	0.1613	0.051*
H38B	0.2927	0.1293	0.1791	0.051*
H38C	0.3291	0.0546	0.1511	0.051*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
N1	0.0296 (16)	0.0242 (14)	0.0246 (15)	−0.0001 (13)	0.0022 (14)	−0.0002 (12)
C2	0.0256 (18)	0.0228 (16)	0.0232 (17)	−0.0030 (15)	0.0002 (15)	−0.0011 (14)
C3	0.0251 (18)	0.0231 (16)	0.0274 (18)	−0.0014 (15)	−0.0016 (16)	−0.0007 (14)
C4	0.0218 (17)	0.0263 (17)	0.0279 (18)	0.0001 (15)	0.0012 (15)	−0.0010 (14)
C5	0.0260 (19)	0.0256 (17)	0.0222 (17)	−0.0061 (15)	−0.0007 (15)	−0.0030 (14)
C6	0.0270 (19)	0.0211 (16)	0.0302 (19)	−0.0016 (15)	−0.0074 (16)	0.0007 (14)
C7	0.0270 (19)	0.0234 (17)	0.0259 (18)	−0.0011 (16)	−0.0004 (16)	−0.0034 (14)
C8	0.0261 (19)	0.0198 (16)	0.0321 (19)	0.0001 (15)	0.0057 (17)	0.0013 (14)
C9	0.034 (2)	0.0210 (16)	0.034 (2)	−0.0013 (16)	−0.0010 (18)	−0.0017 (15)
C10	0.033 (2)	0.0206 (16)	0.040 (2)	0.0022 (16)	−0.0024 (18)	0.0031 (15)
C11	0.048 (3)	0.0254 (18)	0.039 (2)	0.0049 (18)	0.010 (2)	0.0006 (16)
C12	0.0284 (19)	0.0264 (17)	0.0243 (17)	−0.0035 (16)	0.0006 (16)	0.0005 (14)
C13	0.052 (3)	0.039 (2)	0.029 (2)	−0.009 (2)	0.004 (2)	0.0012 (17)
C14	0.035 (2)	0.036 (2)	0.032 (2)	−0.0043 (18)	0.0018 (18)	0.0048 (16)
C15	0.046 (2)	0.035 (2)	0.033 (2)	0.0016 (19)	0.002 (2)	0.0090 (17)
C16	0.029 (2)	0.0197 (16)	0.030 (2)	0.0029 (15)	0.0028 (17)	−0.0004 (14)
C17	0.0240 (19)	0.0296 (18)	0.038 (2)	0.0017 (16)	0.0002 (17)	−0.0038 (16)
C18	0.028 (2)	0.0316 (19)	0.035 (2)	0.0029 (16)	0.0017 (17)	−0.0040 (16)
C19	0.029 (2)	0.0266 (18)	0.041 (2)	0.0079 (16)	0.0017 (18)	0.0016 (16)
N20	0.0284 (16)	0.0241 (14)	0.0232 (15)	−0.0007 (13)	−0.0011 (14)	0.0000 (12)
C21	0.0212 (17)	0.0232 (16)	0.0230 (17)	0.0042 (14)	0.0018 (15)	−0.0025 (14)
C22	0.0208 (17)	0.0236 (16)	0.0244 (18)	−0.0002 (14)	−0.0014 (15)	0.0014 (14)
C23	0.0203 (18)	0.0225 (16)	0.0296 (19)	−0.0004 (14)	0.0013 (16)	0.0031 (14)
C24	0.0279 (19)	0.0241 (17)	0.0237 (18)	0.0055 (15)	−0.0024 (16)	0.0038 (14)
C25	0.0239 (18)	0.0213 (16)	0.0291 (18)	−0.0035 (15)	−0.0029 (16)	0.0001 (14)
C26	0.0215 (18)	0.0204 (16)	0.0279 (18)	0.0003 (14)	−0.0039 (15)	0.0029 (14)
C27	0.0250 (18)	0.0213 (16)	0.0281 (18)	−0.0023 (15)	0.0004 (16)	−0.0014 (14)
C28	0.033 (2)	0.0199 (16)	0.036 (2)	0.0009 (16)	−0.0015 (18)	−0.0043 (15)
C29	0.0246 (19)	0.0245 (17)	0.037 (2)	−0.0011 (15)	0.0024 (17)	−0.0040 (15)
C30	0.041 (2)	0.0220 (17)	0.038 (2)	−0.0064 (17)	0.0041 (19)	−0.0012 (15)
C31	0.031 (2)	0.0227 (17)	0.0272 (19)	0.0024 (16)	−0.0013 (16)	0.0005 (14)
C32	0.033 (2)	0.037 (2)	0.031 (2)	0.0036 (18)	−0.0001 (18)	−0.0061 (16)
C33	0.049 (3)	0.035 (2)	0.0246 (19)	0.0039 (19)	0.0028 (19)	0.0019 (16)
C34	0.037 (2)	0.0278 (19)	0.037 (2)	−0.0022 (17)	0.0060 (19)	−0.0072 (16)
C35	0.0243 (19)	0.0234 (17)	0.034 (2)	−0.0023 (15)	0.0014 (16)	0.0022 (15)
C36	0.0226 (19)	0.0309 (18)	0.037 (2)	−0.0003 (16)	0.0039 (17)	0.0000 (16)
C37	0.026 (2)	0.0330 (19)	0.045 (2)	−0.0008 (17)	0.0026 (18)	−0.0043 (18)
C38	0.028 (2)	0.036 (2)	0.038 (2)	−0.0065 (17)	0.0002 (18)	0.0091 (17)

Geometric parameters (Å, º)

N1—N20	1.258 (4)	N20—C21	1.453 (4)
N1—C2	1.455 (5)	C21—C22	1.413 (5)
C2—C3	1.414 (5)	C21—C26	1.420 (5)
C2—C7	1.422 (5)	C22—C23	1.398 (5)
C3—C4	1.389 (5)	C22—C27	1.559 (5)
C3—C8	1.556 (5)	C23—C24	1.395 (5)
C4—C5	1.395 (5)	C23—H23	0.9300
C4—H4	0.9300	C24—C25	1.398 (5)
C5—C6	1.387 (5)	C24—C31	1.536 (5)
C5—C12	1.533 (5)	C25—C26	1.395 (5)
C6—C7	1.396 (5)	C25—H25	0.9300
C6—H6	0.9300	C26—C35	1.558 (5)
C7—C16	1.553 (5)	C27—C29	1.534 (5)
C8—C11	1.538 (5)	C27—C30	1.537 (5)
C8—C10	1.540 (5)	C27—C28	1.541 (5)
C8—C9	1.547 (5)	C28—H28A	0.9600
C9—H9A	0.9600	C28—H28B	0.9600
C9—H9B	0.9600	C28—H28C	0.9600
C9—H9C	0.9600	C29—H29A	0.9600
C10—H10A	0.9600	C29—H29B	0.9600
C10—H10B	0.9600	C29—H29C	0.9600
C10—H10C	0.9600	C30—H30A	0.9600
C11—H11A	0.9600	C30—H30B	0.9600
C11—H11B	0.9600	C30—H30C	0.9600
C11—H11C	0.9600	C31—C34	1.532 (5)
C12—C15	1.530 (5)	C31—C32	1.542 (5)
C12—C13	1.534 (5)	C31—C33	1.542 (5)
C12—C14	1.538 (5)	C32—H32A	0.9600
C13—H13A	0.9600	C32—H32B	0.9600
C13—H13B	0.9600	C32—H32C	0.9600
C13—H13C	0.9600	C33—H33A	0.9600
C14—H14A	0.9600	C33—H33B	0.9600
C14—H14B	0.9600	C33—H33C	0.9600
C14—H14C	0.9600	C34—H34A	0.9600
C15—H15A	0.9600	C34—H34B	0.9600
C15—H15B	0.9600	C34—H34C	0.9600
C15—H15C	0.9600	C35—C36	1.537 (5)
C16—C17	1.535 (5)	C35—C37	1.537 (5)
C16—C18	1.536 (5)	C35—C38	1.538 (5)
C16—C19	1.538 (5)	C36—H36A	0.9600
C17—H17A	0.9600	C36—H36B	0.9600
C17—H17B	0.9600	C36—H36C	0.9600
C17—H17C	0.9600	C37—H37A	0.9600
C18—H18A	0.9600	C37—H37B	0.9600
C18—H18B	0.9600	C37—H37C	0.9600
C18—H18C	0.9600	C38—H38A	0.9600
C19—H19A	0.9600	C38—H38B	0.9600
C19—H19B	0.9600	C38—H38C	0.9600
C19—H19C	0.9600
N20—N1—C2	114.1 (3)	N1—N20—C21	113.7 (3)
C3—C2—C7	120.9 (3)	C22—C21—C26	120.9 (3)
C3—C2—N1	127.7 (3)	C22—C21—N20	126.9 (3)
C7—C2—N1	111.0 (3)	C26—C21—N20	112.2 (3)
C4—C3—C2	116.8 (3)	C23—C22—C21	117.3 (3)
C4—C3—C8	117.9 (3)	C23—C22—C27	117.8 (3)
C2—C3—C8	124.7 (3)	C21—C22—C27	124.4 (3)
C3—C4—C5	123.6 (3)	C24—C23—C22	123.4 (3)
C3—C4—H4	118.2	C24—C23—H23	118.3
C5—C4—H4	118.2	C22—C23—H23	118.3
C6—C5—C4	117.3 (3)	C23—C24—C25	117.0 (3)
C6—C5—C12	122.2 (3)	C23—C24—C31	120.1 (3)
C4—C5—C12	120.4 (3)	C25—C24—C31	122.6 (3)
C5—C6—C7	122.7 (3)	C26—C25—C24	122.8 (3)
C5—C6—H6	118.7	C26—C25—H25	118.6
C7—C6—H6	118.7	C24—C25—H25	118.6
C6—C7—C2	117.4 (3)	C25—C26—C21	117.8 (3)
C6—C7—C16	118.3 (3)	C25—C26—C35	118.7 (3)
C2—C7—C16	124.3 (3)	C21—C26—C35	123.3 (3)
C11—C8—C10	106.1 (3)	C29—C27—C30	106.8 (3)
C11—C8—C9	105.3 (3)	C29—C27—C28	111.2 (3)
C10—C8—C9	111.8 (3)	C30—C27—C28	106.1 (3)
C11—C8—C3	111.4 (3)	C29—C27—C22	112.3 (3)
C10—C8—C3	113.4 (3)	C30—C27—C22	111.8 (3)
C9—C8—C3	108.5 (3)	C28—C27—C22	108.5 (3)
C8—C9—H9A	109.5	C27—C28—H28A	109.5
C8—C9—H9B	109.5	C27—C28—H28B	109.5
H9A—C9—H9B	109.5	H28A—C28—H28B	109.5
C8—C9—H9C	109.5	C27—C28—H28C	109.5
H9A—C9—H9C	109.5	H28A—C28—H28C	109.5
H9B—C9—H9C	109.5	H28B—C28—H28C	109.5
C8—C10—H10A	109.5	C27—C29—H29A	109.5
C8—C10—H10B	109.5	C27—C29—H29B	109.5
H10A—C10—H10B	109.5	H29A—C29—H29B	109.5
C8—C10—H10C	109.5	C27—C29—H29C	109.5
H10A—C10—H10C	109.5	H29A—C29—H29C	109.5
H10B—C10—H10C	109.5	H29B—C29—H29C	109.5
C8—C11—H11A	109.5	C27—C30—H30A	109.5
C8—C11—H11B	109.5	C27—C30—H30B	109.5
H11A—C11—H11B	109.5	H30A—C30—H30B	109.5
C8—C11—H11C	109.5	C27—C30—H30C	109.5
H11A—C11—H11C	109.5	H30A—C30—H30C	109.5
H11B—C11—H11C	109.5	H30B—C30—H30C	109.5
C15—C12—C13	108.2 (3)	C34—C31—C24	112.7 (3)
C15—C12—C5	112.7 (3)	C34—C31—C32	108.7 (3)
C13—C12—C5	108.9 (3)	C24—C31—C32	109.6 (3)
C15—C12—C14	108.0 (3)	C34—C31—C33	108.3 (3)
C13—C12—C14	109.2 (3)	C24—C31—C33	108.9 (3)
C5—C12—C14	109.9 (3)	C32—C31—C33	108.6 (3)
C12—C13—H13A	109.5	C31—C32—H32A	109.5
C12—C13—H13B	109.5	C31—C32—H32B	109.5
H13A—C13—H13B	109.5	H32A—C32—H32B	109.5
C12—C13—H13C	109.5	C31—C32—H32C	109.5
H13A—C13—H13C	109.5	H32A—C32—H32C	109.5
H13B—C13—H13C	109.5	H32B—C32—H32C	109.5
C12—C14—H14A	109.5	C31—C33—H33A	109.5
C12—C14—H14B	109.5	C31—C33—H33B	109.5
H14A—C14—H14B	109.5	H33A—C33—H33B	109.5
C12—C14—H14C	109.5	C31—C33—H33C	109.5
H14A—C14—H14C	109.5	H33A—C33—H33C	109.5
H14B—C14—H14C	109.5	H33B—C33—H33C	109.5
C12—C15—H15A	109.5	C31—C34—H34A	109.5
C12—C15—H15B	109.5	C31—C34—H34B	109.5
H15A—C15—H15B	109.5	H34A—C34—H34B	109.5
C12—C15—H15C	109.5	C31—C34—H34C	109.5
H15A—C15—H15C	109.5	H34A—C34—H34C	109.5
H15B—C15—H15C	109.5	H34B—C34—H34C	109.5
C17—C16—C18	110.8 (3)	C36—C35—C37	106.5 (3)
C17—C16—C19	105.8 (3)	C36—C35—C38	110.1 (3)
C18—C16—C19	106.5 (3)	C37—C35—C38	106.0 (3)
C17—C16—C7	110.4 (3)	C36—C35—C26	110.0 (3)
C18—C16—C7	112.2 (3)	C37—C35—C26	111.5 (3)
C19—C16—C7	110.8 (3)	C38—C35—C26	112.4 (3)
C16—C17—H17A	109.5	C35—C36—H36A	109.5
C16—C17—H17B	109.5	C35—C36—H36B	109.5
H17A—C17—H17B	109.5	H36A—C36—H36B	109.5
C16—C17—H17C	109.5	C35—C36—H36C	109.5
H17A—C17—H17C	109.5	H36A—C36—H36C	109.5
H17B—C17—H17C	109.5	H36B—C36—H36C	109.5
C16—C18—H18A	109.5	C35—C37—H37A	109.5
C16—C18—H18B	109.5	C35—C37—H37B	109.5
H18A—C18—H18B	109.5	H37A—C37—H37B	109.5
C16—C18—H18C	109.5	C35—C37—H37C	109.5
H18A—C18—H18C	109.5	H37A—C37—H37C	109.5
H18B—C18—H18C	109.5	H37B—C37—H37C	109.5
C16—C19—H19A	109.5	C35—C38—H38A	109.5
C16—C19—H19B	109.5	C35—C38—H38B	109.5
H19A—C19—H19B	109.5	H38A—C38—H38B	109.5
C16—C19—H19C	109.5	C35—C38—H38C	109.5
H19A—C19—H19C	109.5	H38A—C38—H38C	109.5
H19B—C19—H19C	109.5	H38B—C38—H38C	109.5
N20—N1—C2—C3	−42.8 (5)	N1—N20—C21—C22	−60.5 (4)
N20—N1—C2—C7	130.6 (3)	N1—N20—C21—C26	117.2 (3)
C7—C2—C3—C4	−11.5 (5)	C26—C21—C22—C23	−8.7 (5)
N1—C2—C3—C4	161.2 (3)	N20—C21—C22—C23	168.7 (3)
C7—C2—C3—C8	159.5 (3)	C26—C21—C22—C27	162.9 (3)
N1—C2—C3—C8	−27.8 (5)	N20—C21—C22—C27	−19.6 (5)
C2—C3—C4—C5	2.3 (5)	C21—C22—C23—C24	1.4 (5)
C8—C3—C4—C5	−169.3 (3)	C27—C22—C23—C24	−170.8 (3)
C3—C4—C5—C6	5.8 (5)	C22—C23—C24—C25	5.4 (5)
C3—C4—C5—C12	−178.7 (3)	C22—C23—C24—C31	179.9 (3)
C4—C5—C6—C7	−5.0 (5)	C23—C24—C25—C26	−5.2 (5)
C12—C5—C6—C7	179.6 (3)	C31—C24—C25—C26	−179.6 (3)
C5—C6—C7—C2	−3.8 (5)	C24—C25—C26—C21	−1.7 (5)
C5—C6—C7—C16	175.3 (3)	C24—C25—C26—C35	174.1 (3)
C3—C2—C7—C6	12.3 (5)	C22—C21—C26—C25	8.9 (5)
N1—C2—C7—C6	−161.6 (3)	N20—C21—C26—C25	−168.9 (3)
C3—C2—C7—C16	−166.8 (3)	C22—C21—C26—C35	−166.7 (3)
N1—C2—C7—C16	19.4 (5)	N20—C21—C26—C35	15.5 (5)
C4—C3—C8—C11	16.0 (5)	C23—C22—C27—C29	−109.2 (4)
C2—C3—C8—C11	−155.0 (4)	C21—C22—C27—C29	79.2 (4)
C4—C3—C8—C10	−103.7 (4)	C23—C22—C27—C30	10.8 (4)
C2—C3—C8—C10	85.4 (4)	C21—C22—C27—C30	−160.8 (3)
C4—C3—C8—C9	131.5 (3)	C23—C22—C27—C28	127.5 (3)
C2—C3—C8—C9	−39.5 (5)	C21—C22—C27—C28	−44.1 (4)
C6—C5—C12—C15	−6.3 (5)	C23—C24—C31—C34	178.6 (3)
C4—C5—C12—C15	178.4 (3)	C25—C24—C31—C34	−7.2 (5)
C6—C5—C12—C13	113.7 (4)	C23—C24—C31—C32	57.4 (4)
C4—C5—C12—C13	−61.6 (4)	C25—C24—C31—C32	−128.4 (4)
C6—C5—C12—C14	−126.8 (4)	C23—C24—C31—C33	−61.2 (4)
C4—C5—C12—C14	57.9 (4)	C25—C24—C31—C33	113.0 (4)
C6—C7—C16—C17	−127.7 (3)	C25—C26—C35—C36	−120.3 (3)
C2—C7—C16—C17	51.3 (4)	C21—C26—C35—C36	55.3 (4)
C6—C7—C16—C18	108.1 (4)	C25—C26—C35—C37	−2.3 (4)
C2—C7—C16—C18	−72.9 (4)	C21—C26—C35—C37	173.2 (3)
C6—C7—C16—C19	−10.8 (4)	C25—C26—C35—C38	116.6 (4)
C2—C7—C16—C19	168.3 (3)	C21—C26—C35—C38	−67.8 (4)
C2—N1—N20—C21	−162.4 (3)

2,5-bis(3,5-di-tert-butylphenyl)-2,5-dimethylhexane (IVb)

Crystal data

C36H58	Z = 1
Mr = 490.82	F(000) = 274
Triclinic, P_1	Dx = 0.964 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.0239 (7) Å	Cell parameters from 65 reflections
b = 10.0397 (7) Å	θ = 4.0–10.2°
c = 9.9982 (7) Å	µ = 0.05 mm^−1
α = 77.364 (2)°	T = 293 K
β = 60.735 (2)°	Fragment, colourless
γ = 76.060 (3)°	0.4 × 0.3 × 0.25 mm
V = 845.83 (10) Å^3

Data collection

Modified Huber diffractometer	Rint = 0.0000
Radiation source: fine-focus sealed tube	θmax = 30.0°, θmin = 2.1°
Graphite monochromator	h = −13→14
θ/2θ scans	k = 0→14
4925 measured reflections	l = −13→14
4925 independent reflections	3 standard reflections every 97 reflections
2874 reflections with I > 2σ(I)	intensity decay: none

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)] = 0.085	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.298	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.1386P)^2 + 0.2807P] where P = (Fo^2 + 2Fc^2)/3
4925 reflections	(Δ/σ)max = 0.001
171 parameters	Δρmax = 0.45 e Å^−3
0 restraints	Δρmin = −0.28 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
C1	0.3536 (2)	0.71666 (18)	0.8802 (2)	0.0395 (4)
C2	0.2064 (2)	0.72029 (19)	1.0077 (2)	0.0423 (4)
H2	0.1979	0.7082	1.1063	0.051*
C3	0.0724 (2)	0.74137 (19)	0.9916 (2)	0.0411 (4)
C4	0.0882 (2)	0.76036 (19)	0.8426 (2)	0.0432 (4)
H4	−0.0005	0.7749	0.8301	0.052*
C5	0.2310 (2)	0.75837 (19)	0.7121 (2)	0.0423 (4)
C6	0.3638 (2)	0.7359 (2)	0.7340 (2)	0.0430 (4)
H6	0.4608	0.7339	0.6481	0.052*
C11	0.4967 (2)	0.6970 (2)	0.9064 (2)	0.0468 (4)
C12	0.4986 (2)	0.5680 (2)	1.0231 (2)	0.0456 (4)
H12A	0.5888	0.5596	1.0384	0.055*
H12B	0.4077	0.5825	1.1214	0.055*
C13	0.4853 (3)	0.8251 (2)	0.9758 (4)	0.0676 (7)
H13A	0.3904	0.8348	1.0701	0.101*
H13B	0.4869	0.9063	0.9037	0.101*
H13C	0.5715	0.8139	0.9967	0.101*
C14	0.6498 (2)	0.6837 (3)	0.7558 (3)	0.0657 (7)
H14B	0.6539	0.7678	0.6871	0.099*
H14C	0.6557	0.6081	0.7077	0.099*
H14A	0.7353	0.6670	0.7787	0.099*
C31	−0.0895 (2)	0.7449 (2)	1.1310 (2)	0.0525 (5)
C32	−0.1707 (3)	0.6361 (3)	1.1260 (4)	0.0860 (9)
H32B	−0.2741	0.6420	1.2096	0.129*
H32C	−0.1142	0.5457	1.1357	0.129*
H32A	−0.1745	0.6525	1.0296	0.129*
C33	−0.0872 (4)	0.7207 (6)	1.2828 (3)	0.1176 (16)
H33C	−0.0365	0.7887	1.2865	0.176*
H33A	−0.0321	0.6301	1.2946	0.176*
H33B	−0.1915	0.7279	1.3648	0.176*
C34	−0.1878 (3)	0.8878 (3)	1.1180 (4)	0.0948 (11)
H34B	−0.1437	0.9587	1.1261	0.142*
H34C	−0.2919	0.8883	1.1997	0.142*
H34A	−0.1887	0.9047	1.0201	0.142*
C51	0.2490 (3)	0.7807 (3)	0.5480 (2)	0.0579 (6)
C52	0.3183 (6)	0.9113 (4)	0.4624 (4)	0.1158 (15)
H52C	0.3425	0.9188	0.3558	0.174*
H52A	0.4111	0.9075	0.4698	0.174*
H52B	0.2452	0.9902	0.5075	0.174*
C53	0.0949 (5)	0.7930 (7)	0.5471 (4)	0.143 (2)
H53A	0.0471	0.7133	0.6069	0.214*
H53B	0.1124	0.7985	0.4428	0.214*
H53C	0.0281	0.8748	0.5911	0.214*
C54	0.3587 (5)	0.6590 (4)	0.4621 (4)	0.1126 (14)
H54B	0.3156	0.5756	0.5137	0.169*
H54C	0.4570	0.6504	0.4604	0.169*
H54A	0.3726	0.6744	0.3582	0.169*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0378 (8)	0.0396 (8)	0.0421 (9)	−0.0054 (6)	−0.0208 (7)	−0.0019 (6)
C2	0.0435 (9)	0.0462 (9)	0.0372 (8)	−0.0058 (7)	−0.0200 (7)	−0.0026 (7)
C3	0.0377 (8)	0.0422 (9)	0.0410 (9)	−0.0052 (6)	−0.0164 (7)	−0.0059 (7)
C4	0.0402 (9)	0.0463 (9)	0.0473 (10)	−0.0039 (7)	−0.0247 (8)	−0.0054 (7)
C5	0.0466 (9)	0.0447 (9)	0.0389 (8)	−0.0054 (7)	−0.0242 (7)	−0.0019 (7)
C6	0.0385 (8)	0.0479 (10)	0.0379 (8)	−0.0047 (7)	−0.0162 (7)	−0.0018 (7)
C11	0.0449 (9)	0.0490 (10)	0.0556 (11)	−0.0100 (8)	−0.0315 (9)	0.0003 (8)
C12	0.0492 (10)	0.0484 (10)	0.0511 (10)	−0.0057 (8)	−0.0332 (9)	−0.0055 (8)
C13	0.0776 (16)	0.0511 (12)	0.102 (2)	−0.0112 (11)	−0.0629 (16)	−0.0085 (12)
C14	0.0401 (10)	0.0784 (16)	0.0727 (15)	−0.0165 (10)	−0.0261 (10)	0.0105 (12)
C31	0.0394 (9)	0.0591 (12)	0.0488 (10)	−0.0072 (8)	−0.0111 (8)	−0.0107 (9)
C32	0.0634 (15)	0.088 (2)	0.0837 (19)	−0.0320 (14)	−0.0053 (14)	−0.0156 (15)
C33	0.0646 (18)	0.220 (5)	0.0464 (14)	−0.024 (2)	−0.0075 (13)	−0.018 (2)
C34	0.0565 (15)	0.0694 (17)	0.110 (3)	0.0047 (12)	−0.0042 (15)	−0.0209 (16)
C51	0.0659 (13)	0.0715 (14)	0.0404 (10)	−0.0084 (11)	−0.0309 (10)	−0.0011 (9)
C52	0.187 (4)	0.106 (3)	0.0662 (19)	−0.053 (3)	−0.069 (2)	0.0286 (17)
C53	0.105 (3)	0.275 (7)	0.072 (2)	−0.035 (3)	−0.066 (2)	0.002 (3)
C54	0.157 (4)	0.120 (3)	0.0668 (19)	0.012 (3)	−0.062 (2)	−0.0335 (19)

Geometric parameters (Å, º)

C1—C6	1.387 (2)	C31—C33	1.495 (4)
C1—C2	1.400 (2)	C31—C32	1.533 (4)
C1—C11	1.541 (2)	C31—C34	1.552 (4)
C2—C3	1.390 (3)	C32—H32B	0.9600
C2—H2	0.9300	C32—H32C	0.9600
C3—C4	1.393 (3)	C32—H32A	0.9600
C3—C31	1.536 (3)	C33—H33C	0.9600
C4—C5	1.387 (3)	C33—H33A	0.9600
C4—H4	0.9300	C33—H33B	0.9600
C5—C6	1.411 (3)	C34—H34B	0.9600
C5—C51	1.531 (3)	C34—H34C	0.9600
C6—H6	0.9300	C34—H34A	0.9600
C11—C14	1.540 (3)	C51—C52	1.517 (4)
C11—C12	1.545 (3)	C51—C53	1.524 (4)
C11—C13	1.547 (3)	C51—C54	1.525 (4)
C12—C12^i	1.524 (4)	C52—H52C	0.9600
C12—H12A	0.9700	C52—H52A	0.9600
C12—H12B	0.9700	C52—H52B	0.9600
C13—H13A	0.9600	C53—H53A	0.9600
C13—H13B	0.9600	C53—H53B	0.9600
C13—H13C	0.9600	C53—H53C	0.9600
C14—H14B	0.9600	C54—H54B	0.9600
C14—H14C	0.9600	C54—H54C	0.9600
C14—H14A	0.9600	C54—H54A	0.9600
C6—C1—C2	118.10 (16)	C33—C31—C34	108.9 (3)
C6—C1—C11	122.58 (16)	C32—C31—C34	106.9 (2)
C2—C1—C11	119.28 (16)	C3—C31—C34	108.81 (19)
C3—C2—C1	122.08 (16)	C31—C32—H32B	109.5
C3—C2—H2	119.0	C31—C32—H32C	109.5
C1—C2—H2	119.0	H32B—C32—H32C	109.5
C2—C3—C4	117.83 (16)	C31—C32—H32A	109.5
C2—C3—C31	122.40 (17)	H32B—C32—H32A	109.5
C4—C3—C31	119.76 (17)	H32C—C32—H32A	109.5
C5—C4—C3	122.57 (16)	C31—C33—H33C	109.5
C5—C4—H4	118.7	C31—C33—H33A	109.5
C3—C4—H4	118.7	H33C—C33—H33A	109.5
C4—C5—C6	117.65 (16)	C31—C33—H33B	109.5
C4—C5—C51	122.85 (17)	H33C—C33—H33B	109.5
C6—C5—C51	119.49 (17)	H33A—C33—H33B	109.5
C1—C6—C5	121.76 (16)	C31—C34—H34B	109.5
C1—C6—H6	119.1	C31—C34—H34C	109.5
C5—C6—H6	119.1	H34B—C34—H34C	109.5
C14—C11—C1	112.60 (17)	C31—C34—H34A	109.5
C14—C11—C12	109.18 (17)	H34B—C34—H34A	109.5
C1—C11—C12	110.56 (15)	H34C—C34—H34A	109.5
C14—C11—C13	108.39 (19)	C52—C51—C53	109.0 (3)
C1—C11—C13	107.82 (16)	C52—C51—C54	108.4 (3)
C12—C11—C13	108.17 (17)	C53—C51—C54	108.3 (3)
C12^i—C12—C11	115.42 (19)	C52—C51—C5	109.4 (2)
C12^i—C12—H12A	108.4	C53—C51—C5	112.1 (2)
C11—C12—H12A	108.4	C54—C51—C5	109.5 (2)
C12^i—C12—H12B	108.4	C51—C52—H52C	109.5
C11—C12—H12B	108.4	C51—C52—H52A	109.5
H12A—C12—H12B	107.5	H52C—C52—H52A	109.5
C11—C13—H13A	109.5	C51—C52—H52B	109.5
C11—C13—H13B	109.5	H52C—C52—H52B	109.5
H13A—C13—H13B	109.5	H52A—C52—H52B	109.5
C11—C13—H13C	109.5	C51—C53—H53A	109.5
H13A—C13—H13C	109.5	C51—C53—H53B	109.5
H13B—C13—H13C	109.5	H53A—C53—H53B	109.5
C11—C14—H14B	109.5	C51—C53—H53C	109.5
C11—C14—H14C	109.5	H53A—C53—H53C	109.5
H14B—C14—H14C	109.5	H53B—C53—H53C	109.5
C11—C14—H14A	109.5	C51—C54—H54B	109.5
H14B—C14—H14A	109.5	C51—C54—H54C	109.5
H14C—C14—H14A	109.5	H54B—C54—H54C	109.5
C33—C31—C32	109.2 (3)	C51—C54—H54A	109.5
C33—C31—C3	113.4 (2)	H54B—C54—H54A	109.5
C32—C31—C3	109.45 (18)	H54C—C54—H54A	109.5

Symmetry code: (i) −x+1, −y+1, −z+2.

2,15-di-(tert-butyl)-hexahelicene (Vb)

Crystal data

C34H31.98I0.02	F(000) = 1896
Mr = 443.11	Dx = 1.197 Mg m^−3
Orthorhombic, Pbca	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 9979 reflections
a = 9.7674 (2) Å	θ = 2.9–67.3°
b = 16.5340 (3) Å	µ = 0.70 mm^−1
c = 30.4455 (5) Å	T = 100 K
V = 4916.77 (16) Å^3	Rod, colourless
Z = 8	0.60 × 0.20 × 0.20 mm

Data collection

CCD area detector diffractometer	4366 independent reflections
Radiation source: fine-focus sealed tube	4061 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.026
phi and ω scans	θmax = 67.8°, θmin = 2.9°
Absorption correction: multi-scan SADABS (Bruker)	h = −10→11
Tmin = 0.744, Tmax = 0.870	k = −19→18
47333 measured reflections	l = −36→36

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.095	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0393P)^2 + 2.3993P] where P = (Fo^2 + 2Fc^2)/3
4366 reflections	(Δ/σ)max < 0.001
331 parameters	Δρmax = 0.20 e Å^−3
0 restraints	Δρmin = −0.19 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. Two peaks found after all C and H atoms had been located were refined as I atoms since iodine had been used in synthesis. Occupancies for the two I atoms refined to about 0.008 and 0.009; they were rounded to 0.01 and were held constant in the final cycles. Occupancies for the nearby H atoms H4 and H13 were held to 0.99.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.42132 (12)	0.98293 (7)	0.38364 (4)	0.0218 (3)
H1	0.4794	0.9422	0.3720	0.026*
C2	0.39367 (12)	1.05012 (7)	0.35837 (4)	0.0223 (3)
C3	0.30549 (14)	1.10999 (7)	0.37590 (4)	0.0268 (3)
H3	0.2804	1.1552	0.3584	0.032*
C4	0.25633 (14)	1.10354 (8)	0.41758 (4)	0.0293 (3)
H4	0.1988	1.1450	0.4289	0.035*	0.99
C5	0.25467 (15)	1.03562 (8)	0.48995 (4)	0.0334 (3)
H5	0.1960	1.0760	0.5017	0.040*
C6	0.30579 (15)	0.97724 (8)	0.51628 (4)	0.0340 (3)
H6	0.2922	0.9811	0.5471	0.041*
C7	0.44031 (14)	0.85311 (9)	0.52807 (4)	0.0319 (3)
H7	0.4269	0.8583	0.5588	0.038*
C8	0.51714 (14)	0.79156 (8)	0.51219 (4)	0.0315 (3)
H8	0.5669	0.7582	0.5319	0.038*
C9	0.60759 (14)	0.71231 (8)	0.45056 (5)	0.0335 (3)
H9	0.6555	0.6792	0.4709	0.040*
C10	0.61996 (14)	0.69766 (8)	0.40721 (5)	0.0326 (3)
H10	0.6866	0.6602	0.3971	0.039*
C11	0.54118 (14)	0.71867 (8)	0.33101 (5)	0.0312 (3)
H11	0.6112	0.6833	0.3210	0.037*
C12	0.45158 (13)	0.74931 (8)	0.30188 (4)	0.0296 (3)
H12	0.4646	0.7402	0.2714	0.035*
C13	0.22938 (14)	0.81754 (8)	0.28817 (4)	0.0293 (3)
H13	0.2380	0.8067	0.2577	0.035*	0.99
C14	0.11338 (14)	0.85397 (8)	0.30335 (4)	0.0283 (3)
H14	0.0440	0.8694	0.2832	0.034*
C15	0.09475 (13)	0.86912 (7)	0.34871 (4)	0.0250 (3)
C16	0.20093 (12)	0.85011 (7)	0.37659 (4)	0.0231 (3)
H16	0.1900	0.8603	0.4071	0.028*
C17	0.32561 (12)	0.81606 (7)	0.36189 (4)	0.0224 (3)
C18	0.33665 (13)	0.79564 (7)	0.31671 (4)	0.0255 (3)
C19	0.43740 (12)	0.79573 (7)	0.39150 (4)	0.0235 (3)
C20	0.53365 (13)	0.73802 (7)	0.37654 (5)	0.0281 (3)
C21	0.45042 (12)	0.82560 (7)	0.43628 (4)	0.0245 (3)
C22	0.52419 (13)	0.77635 (8)	0.46644 (4)	0.0289 (3)
C23	0.39574 (13)	0.90127 (7)	0.45304 (4)	0.0243 (3)
C24	0.37967 (14)	0.90992 (8)	0.49899 (4)	0.0286 (3)
C25	0.36669 (13)	0.97228 (7)	0.42625 (4)	0.0239 (3)
C26	0.28899 (14)	1.03659 (8)	0.44441 (4)	0.0276 (3)
C27	0.45697 (13)	1.06314 (7)	0.31294 (4)	0.0237 (3)
C28	0.55186 (15)	1.13718 (8)	0.31517 (5)	0.0343 (3)
H28A	0.6213	1.1286	0.3379	0.051*
H28B	0.4979	1.1854	0.3223	0.051*
H28C	0.5969	1.1447	0.2867	0.051*
C29	0.34308 (15)	1.07851 (9)	0.27911 (4)	0.0332 (3)
H29A	0.2895	1.1259	0.2880	0.050*
H29B	0.2831	1.0311	0.2775	0.050*
H29C	0.3841	1.0884	0.2502	0.050*
C30	0.54069 (14)	0.99070 (8)	0.29741 (4)	0.0290 (3)
H30A	0.4826	0.9424	0.2971	0.043*
H30B	0.6178	0.9821	0.3175	0.043*
H30C	0.5754	1.0011	0.2677	0.043*
C31	−0.03979 (14)	0.90583 (8)	0.36488 (4)	0.0296 (3)
C32	−0.05666 (16)	0.99028 (9)	0.34500 (5)	0.0395 (4)
H32A	−0.0583	0.9862	0.3129	0.059*
H32B	0.0202	1.0245	0.3541	0.059*
H32C	−0.1427	1.0142	0.3553	0.059*
C33	−0.04320 (19)	0.91479 (14)	0.41458 (5)	0.0646 (6)
H33A	−0.1301	0.9395	0.4234	0.097*
H33B	0.0329	0.9492	0.4241	0.097*
H33C	−0.0346	0.8614	0.4283	0.097*
C34	−0.15985 (16)	0.85276 (10)	0.35027 (7)	0.0545 (5)
H34A	−0.1637	0.8513	0.3181	0.082*
H34B	−0.2455	0.8752	0.3618	0.082*
H34C	−0.1472	0.7978	0.3616	0.082*
I1	0.1778 (10)	1.1575 (5)	0.4689 (3)	0.036 (2)	0.01
I2	0.2493 (13)	0.8073 (7)	0.2358 (4)	0.052 (3)	0.01

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0220 (6)	0.0197 (6)	0.0237 (6)	−0.0008 (5)	0.0002 (5)	−0.0028 (5)
C2	0.0236 (6)	0.0185 (6)	0.0248 (6)	−0.0025 (5)	−0.0031 (5)	−0.0020 (5)
C3	0.0338 (7)	0.0196 (6)	0.0270 (6)	0.0030 (5)	−0.0038 (5)	0.0004 (5)
C4	0.0351 (7)	0.0226 (6)	0.0301 (7)	0.0058 (5)	0.0009 (6)	−0.0043 (5)
C5	0.0411 (8)	0.0302 (7)	0.0290 (7)	0.0069 (6)	0.0075 (6)	−0.0025 (6)
C6	0.0439 (8)	0.0339 (8)	0.0240 (6)	0.0025 (6)	0.0059 (6)	0.0002 (6)
C7	0.0337 (7)	0.0362 (8)	0.0259 (7)	−0.0024 (6)	0.0008 (6)	0.0073 (6)
C8	0.0301 (7)	0.0313 (7)	0.0332 (7)	−0.0010 (6)	−0.0034 (6)	0.0107 (6)
C9	0.0275 (7)	0.0267 (7)	0.0464 (8)	0.0039 (5)	−0.0018 (6)	0.0078 (6)
C10	0.0253 (7)	0.0242 (7)	0.0482 (8)	0.0044 (5)	0.0037 (6)	0.0010 (6)
C11	0.0279 (7)	0.0210 (6)	0.0447 (8)	−0.0005 (5)	0.0087 (6)	−0.0056 (6)
C12	0.0333 (7)	0.0236 (6)	0.0317 (7)	−0.0067 (5)	0.0089 (6)	−0.0071 (5)
C13	0.0361 (7)	0.0258 (7)	0.0260 (6)	−0.0078 (6)	0.0020 (6)	−0.0030 (5)
C14	0.0304 (7)	0.0241 (6)	0.0304 (7)	−0.0055 (5)	−0.0045 (5)	0.0023 (5)
C15	0.0265 (6)	0.0180 (6)	0.0304 (7)	−0.0029 (5)	0.0005 (5)	0.0041 (5)
C16	0.0256 (6)	0.0175 (6)	0.0260 (6)	−0.0010 (5)	0.0029 (5)	0.0017 (5)
C17	0.0242 (6)	0.0138 (6)	0.0291 (6)	−0.0035 (5)	0.0025 (5)	0.0011 (5)
C18	0.0280 (7)	0.0179 (6)	0.0306 (7)	−0.0065 (5)	0.0039 (5)	−0.0015 (5)
C19	0.0221 (6)	0.0161 (6)	0.0324 (7)	−0.0022 (5)	0.0039 (5)	0.0036 (5)
C20	0.0231 (6)	0.0188 (6)	0.0423 (8)	−0.0020 (5)	0.0056 (6)	−0.0003 (5)
C21	0.0207 (6)	0.0229 (6)	0.0300 (7)	−0.0014 (5)	0.0022 (5)	0.0056 (5)
C22	0.0256 (7)	0.0251 (7)	0.0361 (7)	−0.0012 (5)	−0.0001 (6)	0.0072 (5)
C23	0.0233 (6)	0.0245 (6)	0.0251 (6)	−0.0002 (5)	0.0007 (5)	0.0016 (5)
C24	0.0292 (7)	0.0290 (7)	0.0275 (6)	−0.0016 (5)	0.0025 (5)	0.0038 (5)
C25	0.0258 (6)	0.0213 (6)	0.0246 (6)	−0.0008 (5)	−0.0005 (5)	−0.0004 (5)
C26	0.0314 (7)	0.0251 (6)	0.0264 (6)	0.0027 (5)	0.0028 (5)	−0.0013 (5)
C27	0.0261 (6)	0.0217 (6)	0.0233 (6)	−0.0018 (5)	−0.0022 (5)	0.0018 (5)
C28	0.0415 (8)	0.0276 (7)	0.0339 (7)	−0.0094 (6)	−0.0012 (6)	0.0055 (6)
C29	0.0347 (7)	0.0393 (8)	0.0258 (7)	0.0049 (6)	−0.0049 (6)	−0.0015 (6)
C30	0.0316 (7)	0.0282 (7)	0.0271 (6)	0.0008 (5)	0.0058 (5)	0.0034 (5)
C31	0.0265 (7)	0.0278 (7)	0.0346 (7)	0.0049 (5)	0.0004 (5)	0.0062 (6)
C32	0.0373 (8)	0.0267 (7)	0.0546 (9)	0.0049 (6)	−0.0031 (7)	0.0038 (7)
C33	0.0498 (10)	0.1044 (16)	0.0396 (9)	0.0485 (11)	0.0129 (8)	0.0145 (10)
C34	0.0279 (8)	0.0333 (9)	0.1023 (15)	−0.0007 (7)	0.0098 (9)	−0.0041 (9)
I1	0.040 (5)	0.028 (4)	0.039 (5)	0.008 (4)	−0.002 (4)	−0.001 (4)
I2	0.054 (6)	0.051 (6)	0.051 (6)	0.016 (5)	−0.009 (5)	−0.015 (5)

Geometric parameters (Å, º)

C1—C2	1.3780 (17)	C16—C17	1.4143 (17)
C1—C25	1.4135 (17)	C16—H16	0.9500
C1—H1	0.9500	C17—C18	1.4205 (17)
C2—C3	1.4166 (17)	C17—C19	1.4553 (17)
C2—C27	1.5302 (17)	C19—C20	1.4148 (17)
C3—C4	1.3608 (18)	C19—C21	1.4556 (18)
C3—H3	0.9500	C21—C22	1.4233 (18)
C4—C26	1.4123 (18)	C21—C23	1.4529 (17)
C4—H4	0.9500	C23—C24	1.4150 (18)
C5—C6	1.3503 (19)	C23—C25	1.4574 (17)
C5—C26	1.4265 (18)	C25—C26	1.4187 (17)
C5—H5	0.9500	C27—C30	1.5254 (18)
C6—C24	1.4272 (19)	C27—C28	1.5371 (17)
C6—H6	0.9500	C27—C29	1.5372 (17)
C7—C8	1.354 (2)	C28—H28A	0.9800
C7—C24	1.4202 (19)	C28—H28B	0.9800
C7—H7	0.9500	C28—H28C	0.9800
C8—C22	1.4170 (19)	C29—H29A	0.9800
C8—H8	0.9500	C29—H29B	0.9800
C9—C10	1.347 (2)	C29—H29C	0.9800
C9—C22	1.4208 (19)	C30—H30A	0.9800
C9—H9	0.9500	C30—H30B	0.9800
C10—C20	1.4241 (19)	C30—H30C	0.9800
C10—H10	0.9500	C31—C33	1.521 (2)
C11—C12	1.345 (2)	C31—C32	1.5306 (19)
C11—C20	1.4243 (19)	C31—C34	1.531 (2)
C11—H11	0.9500	C32—H32A	0.9800
C12—C18	1.4320 (18)	C32—H32B	0.9800
C12—H12	0.9500	C32—H32C	0.9800
C13—C14	1.3639 (19)	C33—H33A	0.9800
C13—C18	1.4085 (19)	C33—H33B	0.9800
C13—H13	0.9500	C33—H33C	0.9800
C14—C15	1.4154 (18)	C34—H34A	0.9800
C14—H14	0.9500	C34—H34B	0.9800
C15—C16	1.3765 (18)	C34—H34C	0.9800
C15—C31	1.5289 (18)
C2—C1—C25	122.60 (11)	C8—C22—C9	119.64 (12)
C2—C1—H1	118.7	C8—C22—C21	120.54 (12)
C25—C1—H1	118.7	C9—C22—C21	119.81 (13)
C1—C2—C3	118.17 (11)	C24—C23—C21	118.36 (11)
C1—C2—C27	122.61 (11)	C24—C23—C25	116.77 (11)
C3—C2—C27	119.20 (11)	C21—C23—C25	124.66 (11)
C4—C3—C2	120.74 (12)	C23—C24—C7	120.22 (12)
C4—C3—H3	119.6	C23—C24—C6	119.97 (12)
C2—C3—H3	119.6	C7—C24—C6	119.78 (12)
C3—C4—C26	121.40 (12)	C1—C25—C26	117.80 (11)
C3—C4—H4	119.3	C1—C25—C23	122.71 (11)
C26—C4—H4	119.3	C26—C25—C23	119.32 (11)
C6—C5—C26	119.87 (12)	C4—C26—C25	118.87 (11)
C6—C5—H5	120.1	C4—C26—C5	121.20 (12)
C26—C5—H5	120.1	C25—C26—C5	119.75 (12)
C5—C6—C24	121.71 (12)	C30—C27—C2	112.73 (10)
C5—C6—H6	119.1	C30—C27—C28	108.41 (11)
C24—C6—H6	119.1	C2—C27—C28	108.41 (10)
C8—C7—C24	120.38 (12)	C30—C27—C29	108.07 (10)
C8—C7—H7	119.8	C2—C27—C29	109.67 (10)
C24—C7—H7	119.8	C28—C27—C29	109.52 (11)
C7—C8—C22	120.75 (12)	C27—C28—H28A	109.5
C7—C8—H8	119.6	C27—C28—H28B	109.5
C22—C8—H8	119.6	H28A—C28—H28B	109.5
C10—C9—C22	121.25 (13)	C27—C28—H28C	109.5
C10—C9—H9	119.4	H28A—C28—H28C	109.5
C22—C9—H9	119.4	H28B—C28—H28C	109.5
C9—C10—C20	120.34 (12)	C27—C29—H29A	109.5
C9—C10—H10	119.8	C27—C29—H29B	109.5
C20—C10—H10	119.8	H29A—C29—H29B	109.5
C12—C11—C20	121.56 (12)	C27—C29—H29C	109.5
C12—C11—H11	119.2	H29A—C29—H29C	109.5
C20—C11—H11	119.2	H29B—C29—H29C	109.5
C11—C12—C18	120.25 (12)	C27—C30—H30A	109.5
C11—C12—H12	119.9	C27—C30—H30B	109.5
C18—C12—H12	119.9	H30A—C30—H30B	109.5
C14—C13—C18	121.50 (12)	C27—C30—H30C	109.5
C14—C13—H13	119.3	H30A—C30—H30C	109.5
C18—C13—H13	119.3	H30B—C30—H30C	109.5
C13—C14—C15	121.04 (12)	C33—C31—C15	112.20 (11)
C13—C14—H14	119.5	C33—C31—C32	107.59 (13)
C15—C14—H14	119.5	C15—C31—C32	109.11 (11)
C16—C15—C14	117.68 (12)	C33—C31—C34	109.16 (15)
C16—C15—C31	122.66 (11)	C15—C31—C34	109.71 (11)
C14—C15—C31	119.66 (11)	C32—C31—C34	109.00 (12)
C15—C16—C17	122.98 (12)	C31—C32—H32A	109.5
C15—C16—H16	118.5	C31—C32—H32B	109.5
C17—C16—H16	118.5	H32A—C32—H32B	109.5
C16—C17—C18	117.81 (11)	C31—C32—H32C	109.5
C16—C17—C19	122.81 (11)	H32A—C32—H32C	109.5
C18—C17—C19	119.21 (11)	H32B—C32—H32C	109.5
C13—C18—C17	118.67 (12)	C31—C33—H33A	109.5
C13—C18—C12	121.75 (12)	C31—C33—H33B	109.5
C17—C18—C12	119.46 (12)	H33A—C33—H33B	109.5
C20—C19—C17	117.06 (11)	C31—C33—H33C	109.5
C20—C19—C21	118.18 (11)	H33A—C33—H33C	109.5
C17—C19—C21	124.56 (11)	H33B—C33—H33C	109.5
C19—C20—C10	119.88 (13)	C31—C34—H34A	109.5
C19—C20—C11	119.94 (12)	C31—C34—H34B	109.5
C10—C20—C11	120.15 (12)	H34A—C34—H34B	109.5
C22—C21—C23	116.88 (12)	C31—C34—H34C	109.5
C22—C21—C19	117.03 (11)	H34A—C34—H34C	109.5
C23—C21—C19	126.09 (11)	H34B—C34—H34C	109.5
C25—C1—C2—C3	−0.82 (18)	C10—C9—C22—C21	0.9 (2)
C25—C1—C2—C27	177.69 (11)	C23—C21—C22—C8	13.93 (18)
C1—C2—C3—C4	3.94 (19)	C19—C21—C22—C8	−166.39 (12)
C27—C2—C3—C4	−174.63 (12)	C23—C21—C22—C9	−164.92 (12)
C2—C3—C4—C26	−1.3 (2)	C19—C21—C22—C9	14.76 (18)
C26—C5—C6—C24	−8.2 (2)	C22—C21—C23—C24	−19.74 (17)
C24—C7—C8—C22	−8.2 (2)	C19—C21—C23—C24	160.61 (12)
C22—C9—C10—C20	−9.6 (2)	C22—C21—C23—C25	154.72 (12)
C20—C11—C12—C18	−6.73 (19)	C19—C21—C23—C25	−24.9 (2)
C18—C13—C14—C15	−1.82 (19)	C21—C23—C24—C7	12.30 (19)
C13—C14—C15—C16	3.68 (18)	C25—C23—C24—C7	−162.59 (12)
C13—C14—C15—C31	−176.66 (12)	C21—C23—C24—C6	−169.57 (12)
C14—C15—C16—C17	−0.42 (18)	C25—C23—C24—C6	15.53 (19)
C31—C15—C16—C17	179.93 (11)	C8—C7—C24—C23	1.9 (2)
C15—C16—C17—C18	−4.54 (17)	C8—C7—C24—C6	−176.26 (13)
C15—C16—C17—C19	−179.73 (11)	C5—C6—C24—C23	−2.8 (2)
C14—C13—C18—C17	−3.30 (18)	C5—C6—C24—C7	175.35 (14)
C14—C13—C18—C12	172.80 (12)	C2—C1—C25—C26	−4.81 (18)
C16—C17—C18—C13	6.28 (17)	C2—C1—C25—C23	179.98 (12)
C19—C17—C18—C13	−178.35 (11)	C24—C23—C25—C1	157.31 (12)
C16—C17—C18—C12	−169.90 (11)	C21—C23—C25—C1	−17.23 (19)
C19—C17—C18—C12	5.47 (17)	C24—C23—C25—C26	−17.83 (18)
C11—C12—C18—C13	−169.61 (12)	C21—C23—C25—C26	167.63 (12)
C11—C12—C18—C17	6.46 (18)	C3—C4—C26—C25	−4.5 (2)
C16—C17—C19—C20	158.41 (11)	C3—C4—C26—C5	170.52 (13)
C18—C17—C19—C20	−16.71 (16)	C1—C25—C26—C4	7.35 (18)
C16—C17—C19—C21	−16.46 (18)	C23—C25—C26—C4	−177.27 (12)
C18—C17—C19—C21	168.42 (11)	C1—C25—C26—C5	−167.76 (12)
C17—C19—C20—C10	−161.44 (11)	C23—C25—C26—C5	7.62 (19)
C21—C19—C20—C10	13.77 (17)	C6—C5—C26—C4	−169.44 (14)
C17—C19—C20—C11	16.70 (17)	C6—C5—C26—C25	5.6 (2)
C21—C19—C20—C11	−168.09 (11)	C1—C2—C27—C30	5.70 (16)
C9—C10—C20—C19	2.05 (19)	C3—C2—C27—C30	−175.80 (11)
C9—C10—C20—C11	−176.08 (13)	C1—C2—C27—C28	−114.32 (13)
C12—C11—C20—C19	−5.23 (19)	C3—C2—C27—C28	64.18 (14)
C12—C11—C20—C10	172.90 (12)	C1—C2—C27—C29	126.15 (13)
C20—C19—C21—C22	−21.77 (17)	C3—C2—C27—C29	−55.36 (15)
C17—C19—C21—C22	153.05 (12)	C16—C15—C31—C33	−2.51 (19)
C20—C19—C21—C23	157.88 (12)	C14—C15—C31—C33	177.85 (14)
C17—C19—C21—C23	−27.30 (19)	C16—C15—C31—C32	116.63 (13)
C7—C8—C22—C9	178.83 (13)	C14—C15—C31—C32	−63.02 (15)
C7—C8—C22—C21	0.0 (2)	C16—C15—C31—C34	−124.03 (14)
C10—C9—C22—C8	−177.98 (13)	C14—C15—C31—C34	56.33 (16)

2,15-di-(tert-butyl)-hexahelicene (Vc)

Crystal data

C34H31.98I0.02	F(000) = 1896
Mr = 443.11	Dx = 1.166 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 7816 reflections
a = 9.8880 (6) Å	θ = 2.4–26.1°
b = 16.6917 (10) Å	µ = 0.09 mm^−1
c = 30.5802 (18) Å	T = 298 K
V = 5047.2 (5) Å^3	Cut-prism, colourless
Z = 8	0.6 × 0.4 × 0.3 mm

Data collection

CCD area detector diffractometer	6166 independent reflections
Radiation source: fine-focus sealed tube	3865 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
phi and ω scans	θmax = 28.3°, θmin = 2.4°
Absorption correction: multi-scan SADABS (Bruker)	h = −10→12
Tmin = 0.811, Tmax = 1.0	k = −12→22
29923 measured reflections	l = −38→39

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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.161	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0704P)^2 + 1.1583P] where P = (Fo^2 + 2Fc^2)/3
6166 reflections	(Δ/σ)max = 0.009
331 parameters	Δρmax = 0.19 e Å^−3
0 restraints	Δρmin = −0.17 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. As in the 100 K structure, residual peaks were refined as I1 and I2 to an occupancy of about 0.008, rounded to 0.010 in the final cycles.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.41881 (16)	0.98463 (8)	0.38390 (5)	0.0427 (3)
H1	0.4740	0.9448	0.3723	0.051*
C2	0.39318 (16)	1.05154 (8)	0.35907 (5)	0.0450 (4)
C3	0.30813 (19)	1.11104 (10)	0.37712 (6)	0.0582 (4)
H3	0.2849	1.1555	0.3604	0.070*
C4	0.2600 (2)	1.10446 (10)	0.41834 (6)	0.0640 (5)
H4	0.2058	1.1451	0.4296	0.077*	0.99
C5	0.2559 (2)	1.03590 (13)	0.48977 (6)	0.0753 (6)
H5	0.2007	1.0756	0.5015	0.090*
C6	0.3033 (2)	0.97711 (14)	0.51540 (6)	0.0755 (6)
H6	0.2884	0.9800	0.5454	0.091*
C7	0.4343 (2)	0.85338 (14)	0.52669 (7)	0.0751 (6)
H7	0.4199	0.8574	0.5567	0.090*
C8	0.5102 (2)	0.79391 (14)	0.51102 (7)	0.0753 (6)
H8	0.5578	0.7614	0.5303	0.090*
C9	0.6031 (2)	0.71742 (12)	0.44940 (9)	0.0825 (7)
H9	0.6506	0.6856	0.4691	0.099*
C10	0.6156 (2)	0.70336 (12)	0.40635 (9)	0.0797 (6)
H10	0.6808	0.6675	0.3964	0.096*
C11	0.5365 (2)	0.72418 (11)	0.33082 (8)	0.0751 (6)
H11	0.6046	0.6903	0.3209	0.090*
C12	0.4482 (2)	0.75348 (12)	0.30216 (7)	0.0704 (6)
H12	0.4604	0.7443	0.2724	0.084*
C13	0.2283 (2)	0.82066 (11)	0.28870 (6)	0.0670 (5)
H13	0.2369	0.8103	0.2589	0.080*	0.99
C14	0.1133 (2)	0.85627 (11)	0.30371 (6)	0.0635 (5)
H14	0.0461	0.8710	0.2840	0.076*
C15	0.09474 (17)	0.87103 (9)	0.34867 (5)	0.0515 (4)
C16	0.20021 (16)	0.85243 (8)	0.37621 (5)	0.0449 (4)
H16	0.1897	0.8624	0.4059	0.054*
C17	0.32332 (16)	0.81910 (8)	0.36173 (5)	0.0452 (4)
C18	0.33413 (19)	0.79918 (9)	0.31685 (6)	0.0553 (4)
C19	0.43393 (16)	0.79943 (9)	0.39096 (6)	0.0487 (4)
C20	0.52996 (18)	0.74291 (10)	0.37584 (7)	0.0630 (5)
C21	0.44665 (16)	0.82837 (9)	0.43556 (6)	0.0511 (4)
C22	0.51947 (19)	0.77937 (11)	0.46550 (7)	0.0650 (5)
C23	0.39252 (17)	0.90270 (9)	0.45248 (5)	0.0486 (4)
C24	0.3754 (2)	0.91058 (11)	0.49824 (6)	0.0606 (5)
C25	0.36506 (17)	0.97362 (9)	0.42625 (5)	0.0461 (4)
C26	0.28999 (19)	1.03752 (10)	0.44455 (5)	0.0562 (4)
C27	0.45497 (18)	1.06466 (9)	0.31386 (5)	0.0515 (4)
C28	0.5487 (3)	1.13743 (13)	0.31565 (8)	0.0919 (8)
H28A	0.4979	1.1838	0.3244	0.138*
H28B	0.5873	1.1464	0.2873	0.138*
H28C	0.6196	1.1278	0.3364	0.138*
C29	0.3420 (3)	1.07973 (15)	0.28066 (7)	0.0886 (7)
H29A	0.2849	1.0333	0.2789	0.133*
H29B	0.3809	1.0903	0.2525	0.133*
H29C	0.2893	1.1251	0.2898	0.133*
C30	0.5367 (2)	0.99312 (12)	0.29801 (6)	0.0751 (6)
H30A	0.6096	0.9831	0.3180	0.113*
H30B	0.5726	1.0043	0.2695	0.113*
H30C	0.4793	0.9468	0.2966	0.113*
C31	−0.03779 (19)	0.90633 (11)	0.36511 (6)	0.0631 (5)
C32	−0.0526 (3)	0.99118 (15)	0.34807 (11)	0.1130 (10)
H32A	−0.1361	1.0136	0.3584	0.170*
H32B	−0.0527	0.9905	0.3167	0.170*
H32C	0.0216	1.0232	0.3583	0.170*
C33	−0.0442 (3)	0.9103 (3)	0.41400 (9)	0.184 (2)
H33A	−0.0352	0.8573	0.4259	0.276*
H33B	−0.1294	0.9327	0.4228	0.276*
H33C	0.0280	0.9435	0.4247	0.276*
C34	−0.1568 (3)	0.85794 (18)	0.34776 (14)	0.1481 (15)
H34A	−0.1503	0.8038	0.3581	0.222*
H34B	−0.1552	0.8583	0.3164	0.222*
H34C	−0.2398	0.8813	0.3579	0.222*
I1	0.180 (2)	1.1555 (14)	0.4684 (7)	0.122 (7)	0.01
I2	0.252 (3)	0.8037 (13)	0.2373 (7)	0.123 (7)	0.01

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0475 (9)	0.0343 (7)	0.0462 (8)	0.0001 (6)	−0.0014 (7)	−0.0010 (6)
C2	0.0521 (9)	0.0361 (7)	0.0468 (8)	−0.0021 (6)	−0.0054 (7)	−0.0001 (6)
C3	0.0728 (12)	0.0407 (8)	0.0611 (10)	0.0113 (8)	−0.0073 (9)	0.0015 (7)
C4	0.0765 (13)	0.0485 (9)	0.0670 (11)	0.0173 (9)	0.0033 (10)	−0.0110 (8)
C5	0.0903 (15)	0.0740 (13)	0.0615 (11)	0.0094 (11)	0.0205 (11)	−0.0103 (10)
C6	0.0911 (16)	0.0874 (15)	0.0479 (10)	−0.0035 (12)	0.0129 (10)	−0.0019 (10)
C7	0.0732 (14)	0.0966 (16)	0.0554 (11)	−0.0139 (12)	−0.0046 (10)	0.0263 (11)
C8	0.0662 (13)	0.0838 (14)	0.0759 (14)	−0.0077 (11)	−0.0149 (11)	0.0370 (11)
C9	0.0602 (13)	0.0647 (13)	0.123 (2)	0.0127 (10)	−0.0060 (13)	0.0302 (13)
C10	0.0557 (12)	0.0540 (11)	0.129 (2)	0.0160 (9)	0.0057 (13)	0.0101 (12)
C11	0.0656 (13)	0.0501 (10)	0.1098 (18)	0.0028 (9)	0.0246 (12)	−0.0159 (11)
C12	0.0781 (14)	0.0571 (11)	0.0759 (13)	−0.0133 (10)	0.0262 (11)	−0.0213 (10)
C13	0.0848 (14)	0.0646 (11)	0.0516 (10)	−0.0178 (10)	0.0040 (10)	−0.0087 (8)
C14	0.0730 (13)	0.0605 (11)	0.0569 (10)	−0.0113 (9)	−0.0136 (9)	0.0051 (8)
C15	0.0527 (10)	0.0444 (8)	0.0576 (10)	−0.0049 (7)	−0.0037 (8)	0.0081 (7)
C16	0.0486 (9)	0.0385 (7)	0.0477 (8)	−0.0012 (6)	0.0018 (7)	0.0032 (6)
C17	0.0487 (9)	0.0315 (7)	0.0554 (9)	−0.0051 (6)	0.0066 (7)	0.0013 (6)
C18	0.0651 (11)	0.0414 (8)	0.0594 (10)	−0.0123 (8)	0.0111 (9)	−0.0083 (7)
C19	0.0445 (9)	0.0337 (7)	0.0679 (10)	−0.0013 (6)	0.0068 (7)	0.0063 (7)
C20	0.0503 (10)	0.0406 (8)	0.0982 (14)	0.0015 (7)	0.0134 (10)	0.0015 (9)
C21	0.0425 (9)	0.0463 (8)	0.0644 (10)	−0.0017 (7)	0.0002 (7)	0.0161 (7)
C22	0.0508 (10)	0.0578 (11)	0.0862 (14)	−0.0030 (8)	−0.0069 (9)	0.0263 (9)
C23	0.0468 (9)	0.0513 (9)	0.0478 (8)	−0.0042 (7)	0.0008 (7)	0.0085 (7)
C24	0.0613 (11)	0.0703 (11)	0.0502 (9)	−0.0103 (9)	0.0020 (8)	0.0104 (8)
C25	0.0504 (9)	0.0422 (8)	0.0456 (8)	−0.0016 (7)	0.0002 (7)	−0.0007 (6)
C26	0.0645 (11)	0.0529 (9)	0.0513 (9)	0.0033 (8)	0.0058 (8)	−0.0066 (7)
C27	0.0611 (10)	0.0447 (8)	0.0488 (9)	−0.0046 (7)	−0.0045 (7)	0.0092 (7)
C28	0.115 (2)	0.0730 (14)	0.0874 (15)	−0.0389 (13)	0.0041 (14)	0.0131 (11)
C29	0.0940 (17)	0.1143 (19)	0.0575 (12)	0.0148 (14)	−0.0171 (11)	0.0051 (11)
C30	0.0921 (16)	0.0693 (12)	0.0639 (12)	0.0099 (11)	0.0262 (11)	0.0117 (9)
C31	0.0524 (10)	0.0626 (11)	0.0743 (12)	0.0095 (8)	−0.0049 (9)	0.0117 (9)
C32	0.107 (2)	0.0645 (14)	0.168 (3)	0.0204 (14)	0.0034 (19)	0.0081 (16)
C33	0.114 (2)	0.349 (6)	0.0885 (19)	0.144 (3)	0.0345 (17)	0.042 (3)
C34	0.0589 (16)	0.096 (2)	0.289 (5)	−0.0077 (14)	0.007 (2)	−0.045 (2)
I1	0.122 (17)	0.127 (16)	0.116 (14)	0.021 (13)	−0.011 (12)	−0.002 (12)
I2	0.146 (18)	0.118 (15)	0.106 (13)	−0.005 (13)	0.015 (13)	−0.034 (11)

Geometric parameters (Å, º)

C1—C2	1.374 (2)	C16—C17	1.410 (2)
C1—C25	1.412 (2)	C16—H16	0.9300
C1—H1	0.9300	C17—C18	1.416 (2)
C2—C3	1.414 (2)	C17—C19	1.450 (2)
C2—C27	1.527 (2)	C19—C20	1.416 (2)
C3—C4	1.352 (3)	C19—C21	1.452 (2)
C3—H3	0.9300	C21—C22	1.423 (2)
C4—C26	1.407 (3)	C21—C23	1.447 (2)
C4—H4	0.9300	C23—C24	1.416 (2)
C5—C6	1.341 (3)	C23—C25	1.455 (2)
C5—C26	1.424 (2)	C25—C26	1.415 (2)
C5—H5	0.9300	C27—C30	1.521 (3)
C6—C24	1.420 (3)	C27—C28	1.529 (3)
C6—H6	0.9300	C27—C29	1.530 (3)
C7—C8	1.333 (3)	C28—H28A	0.9600
C7—C24	1.417 (3)	C28—H28B	0.9600
C7—H7	0.9300	C28—H28C	0.9600
C8—C22	1.416 (3)	C29—H29A	0.9600
C8—H8	0.9300	C29—H29B	0.9600
C9—C10	1.343 (3)	C29—H29C	0.9600
C9—C22	1.413 (3)	C30—H30A	0.9600
C9—H9	0.9300	C30—H30B	0.9600
C10—C20	1.423 (3)	C30—H30C	0.9600
C10—H10	0.9300	C31—C33	1.498 (3)
C11—C12	1.331 (3)	C31—C32	1.516 (3)
C11—C20	1.413 (3)	C31—C34	1.522 (3)
C11—H11	0.9300	C32—H32A	0.9600
C12—C18	1.434 (3)	C32—H32B	0.9600
C12—H12	0.9300	C32—H32C	0.9600
C13—C14	1.363 (3)	C33—H33A	0.9600
C13—C18	1.401 (3)	C33—H33B	0.9600
C13—H13	0.9300	C33—H33C	0.9600
C14—C15	1.409 (2)	C34—H34A	0.9600
C14—H14	0.9300	C34—H34B	0.9600
C15—C16	1.376 (2)	C34—H34C	0.9600
C15—C31	1.522 (3)
C2—C1—C25	122.90 (14)	C15—C16—C17	123.44 (15)
C2—C1—H1	118.5	C15—C16—H16	118.3
C25—C1—H1	118.5	C17—C16—H16	118.3
C1—C2—C3	117.71 (14)	C16—C17—C18	117.54 (15)
C1—C2—C27	122.89 (14)	C16—C17—C19	123.15 (14)
C3—C2—C27	119.38 (13)	C18—C17—C19	119.17 (15)
C4—C3—C2	121.10 (15)	C13—C18—C17	118.62 (16)
C4—C3—H3	119.4	C13—C18—C12	122.06 (17)
C2—C3—H3	119.4	C17—C18—C12	119.21 (18)
C3—C4—C26	121.42 (16)	C20—C19—C17	117.07 (16)
C3—C4—H4	119.3	C20—C19—C21	118.05 (16)
C26—C4—H4	119.3	C17—C19—C21	124.67 (14)
C6—C5—C26	119.93 (18)	C11—C20—C19	119.75 (18)
C6—C5—H5	120.0	C11—C20—C10	120.60 (19)
C26—C5—H5	120.0	C19—C20—C10	119.61 (19)
C5—C6—C24	122.14 (17)	C22—C21—C23	116.74 (16)
C5—C6—H6	118.9	C22—C21—C19	117.17 (16)
C24—C6—H6	118.9	C23—C21—C19	126.08 (14)
C8—C7—C24	120.81 (19)	C9—C22—C8	120.40 (19)
C8—C7—H7	119.6	C9—C22—C21	119.5 (2)
C24—C7—H7	119.6	C8—C22—C21	120.06 (19)
C7—C8—C22	121.16 (18)	C24—C23—C21	118.51 (15)
C7—C8—H8	119.4	C24—C23—C25	116.54 (15)
C22—C8—H8	119.4	C21—C23—C25	124.71 (14)
C10—C9—C22	121.57 (19)	C23—C24—C7	119.69 (19)
C10—C9—H9	119.2	C23—C24—C6	119.85 (17)
C22—C9—H9	119.2	C7—C24—C6	120.44 (18)
C9—C10—C20	120.45 (19)	C1—C25—C26	117.52 (14)
C9—C10—H10	119.8	C1—C25—C23	122.76 (14)
C20—C10—H10	119.8	C26—C25—C23	119.55 (14)
C12—C11—C20	122.02 (18)	C4—C26—C25	118.97 (15)
C12—C11—H11	119.0	C4—C26—C5	121.23 (16)
C20—C11—H11	119.0	C25—C26—C5	119.61 (16)
C11—C12—C18	120.37 (19)	C30—C27—C2	112.85 (13)
C11—C12—H12	119.8	C30—C27—C28	108.26 (18)
C18—C12—H12	119.8	C2—C27—C28	108.91 (15)
C14—C13—C18	121.84 (17)	C30—C27—C29	107.78 (16)
C14—C13—H13	119.1	C2—C27—C29	109.40 (16)
C18—C13—H13	119.1	C28—C27—C29	109.60 (17)
C13—C14—C15	120.90 (18)	C33—C31—C32	107.3 (2)
C13—C14—H14	119.6	C33—C31—C34	109.8 (3)
C15—C14—H14	119.6	C32—C31—C34	107.5 (2)
C16—C15—C14	117.35 (16)	C33—C31—C15	112.52 (16)
C16—C15—C31	122.52 (15)	C32—C31—C15	109.34 (18)
C14—C15—C31	120.13 (16)	C34—C31—C15	110.17 (18)
C25—C1—C2—C3	−0.5 (2)	C7—C8—C22—C21	−0.3 (3)
C25—C1—C2—C27	177.98 (14)	C23—C21—C22—C9	−164.04 (17)
C1—C2—C3—C4	3.7 (3)	C19—C21—C22—C9	15.8 (2)
C27—C2—C3—C4	−174.87 (17)	C23—C21—C22—C8	14.6 (2)
C2—C3—C4—C26	−1.4 (3)	C19—C21—C22—C8	−165.61 (16)
C26—C5—C6—C24	−6.9 (3)	C22—C21—C23—C24	−20.1 (2)
C24—C7—C8—C22	−8.7 (3)	C19—C21—C23—C24	160.10 (16)
C22—C9—C10—C20	−9.2 (3)	C22—C21—C23—C25	154.04 (16)
C20—C11—C12—C18	−6.3 (3)	C19—C21—C23—C25	−25.7 (3)
C18—C13—C14—C15	−1.7 (3)	C21—C23—C24—C7	12.0 (3)
C13—C14—C15—C16	3.7 (2)	C25—C23—C24—C7	−162.65 (17)
C13—C14—C15—C31	−176.38 (17)	C21—C23—C24—C6	−170.06 (17)
C14—C15—C16—C17	−0.6 (2)	C25—C23—C24—C6	15.3 (3)
C31—C15—C16—C17	179.46 (14)	C8—C7—C24—C23	2.7 (3)
C15—C16—C17—C18	−4.3 (2)	C8—C7—C24—C6	−175.3 (2)
C15—C16—C17—C19	−179.82 (14)	C5—C6—C24—C23	−3.6 (3)
C14—C13—C18—C17	−3.4 (3)	C5—C6—C24—C7	174.3 (2)
C14—C13—C18—C12	172.57 (17)	C2—C1—C25—C26	−4.7 (2)
C16—C17—C18—C13	6.2 (2)	C2—C1—C25—C23	−179.95 (15)
C19—C17—C18—C13	−178.11 (14)	C24—C23—C25—C1	158.04 (16)
C16—C17—C18—C12	−169.89 (14)	C21—C23—C25—C1	−16.2 (3)
C19—C17—C18—C12	5.8 (2)	C24—C23—C25—C26	−17.1 (2)
C11—C12—C18—C13	−170.12 (18)	C21—C23—C25—C26	168.64 (16)
C11—C12—C18—C17	5.8 (3)	C3—C4—C26—C25	−4.1 (3)
C16—C17—C19—C20	158.91 (14)	C3—C4—C26—C5	170.8 (2)
C18—C17—C19—C20	−16.5 (2)	C1—C25—C26—C4	6.9 (2)
C16—C17—C19—C21	−15.8 (2)	C23—C25—C26—C4	−177.71 (17)
C18—C17—C19—C21	168.77 (14)	C1—C25—C26—C5	−168.06 (17)
C12—C11—C20—C19	−5.2 (3)	C23—C25—C26—C5	7.3 (3)
C12—C11—C20—C10	172.52 (19)	C6—C5—C26—C4	−169.9 (2)
C17—C19—C20—C11	16.4 (2)	C6—C5—C26—C25	4.9 (3)
C21—C19—C20—C11	−168.60 (16)	C1—C2—C27—C30	5.0 (2)
C17—C19—C20—C10	−161.35 (16)	C3—C2—C27—C30	−176.47 (16)
C21—C19—C20—C10	13.7 (2)	C1—C2—C27—C28	−115.20 (19)
C9—C10—C20—C11	−175.6 (2)	C3—C2—C27—C28	63.3 (2)
C9—C10—C20—C19	2.1 (3)	C1—C2—C27—C29	125.02 (18)
C20—C19—C21—C22	−22.2 (2)	C3—C2—C27—C29	−56.5 (2)
C17—C19—C21—C22	152.40 (15)	C16—C15—C31—C33	−5.7 (3)
C20—C19—C21—C23	157.53 (16)	C14—C15—C31—C33	174.4 (3)
C17—C19—C21—C23	−27.8 (2)	C16—C15—C31—C32	113.4 (2)
C10—C9—C22—C8	−178.7 (2)	C14—C15—C31—C32	−66.5 (2)
C10—C9—C22—C21	−0.1 (3)	C16—C15—C31—C34	−128.6 (2)
C7—C8—C22—C9	178.3 (2)	C14—C15—C31—C34	51.5 (3)

2,15-di-(tert-butyl)-hexahelicene (Vd)

Crystal data

C34H31.98I0.02	F(000) = 1896
Mr = 443.11	Dx = 1.166 Mg m^−3
Orthorhombic, Pbca	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 8561 reflections
a = 9.8836 (3) Å	θ = 2.9–63.6°
b = 16.7096 (5) Å	µ = 0.68 mm^−1
c = 30.5719 (10) Å	T = 298 K
V = 5049.0 (3) Å^3	Rod, colourless
Z = 8	0.60 × 0.20 × 0.20 mm

Data collection

CCD area detector diffractometer	4162 independent reflections
Radiation source: fine-focus sealed tube	3221 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.032
phi and ω scans	θmax = 64.5°, θmin = 2.9°
Absorption correction: multi-scan SADABS (Bruker)	h = −10→11
Tmin = 0.690, Tmax = 0.990	k = −19→16
24764 measured reflections	l = −30→34

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)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.143	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0711P)^2 + 1.0652P] where P = (Fo^2 + 2Fc^2)/3
4162 reflections	(Δ/σ)max = 0.008
331 parameters	Δρmax = 0.16 e Å^−3
0 restraints	Δρmin = −0.18 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. Two peaks found after all C and H atoms had been located were refined as I atoms since iodine had been used in synthesis. Occupancies for the two I atoms refined to about 0.008 and 0.009; they were rounded to 0.01 and were held constant in the final cycles. Occupancies for the nearby H atoms H4 and H13 were held to 0.99.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.41854 (17)	0.98452 (9)	0.38396 (5)	0.0450 (4)
H1	0.4735	0.9447	0.3723	0.054*
C2	0.39299 (17)	1.05168 (9)	0.35911 (5)	0.0472 (4)
C3	0.3080 (2)	1.11086 (11)	0.37715 (6)	0.0613 (5)
H3	0.2845	1.1551	0.3604	0.074*
C4	0.2602 (2)	1.10445 (11)	0.41829 (7)	0.0666 (6)
H4	0.2062	1.1451	0.4296	0.080*	0.99
C5	0.2558 (3)	1.03573 (14)	0.48969 (7)	0.0795 (6)
H5	0.2004	1.0753	0.5014	0.095*
C6	0.3031 (2)	0.97699 (15)	0.51547 (7)	0.0795 (7)
H6	0.2881	0.9799	0.5455	0.095*
C7	0.4342 (2)	0.85346 (16)	0.52675 (7)	0.0794 (7)
H7	0.4200	0.8576	0.5567	0.095*
C8	0.5098 (2)	0.79391 (15)	0.51101 (8)	0.0782 (7)
H8	0.5572	0.7613	0.5303	0.094*
C9	0.6024 (2)	0.71769 (13)	0.44942 (10)	0.0856 (7)
H9	0.6498	0.6859	0.4691	0.103*
C10	0.6153 (2)	0.70341 (13)	0.40637 (10)	0.0839 (7)
H10	0.6805	0.6676	0.3965	0.101*
C11	0.5360 (2)	0.72417 (12)	0.33082 (9)	0.0797 (7)
H11	0.6040	0.6903	0.3210	0.096*
C12	0.4477 (2)	0.75341 (13)	0.30221 (8)	0.0742 (6)
H12	0.4600	0.7442	0.2725	0.089*
C13	0.2281 (2)	0.82067 (12)	0.28875 (7)	0.0705 (6)
H13	0.2367	0.8105	0.2590	0.085*	0.99
C14	0.1132 (2)	0.85630 (12)	0.30381 (6)	0.0663 (5)
H14	0.0460	0.8712	0.2841	0.080*
C15	0.09462 (19)	0.87093 (10)	0.34869 (6)	0.0541 (5)
C16	0.19997 (17)	0.85244 (9)	0.37627 (6)	0.0483 (4)
H16	0.1895	0.8624	0.4060	0.058*
C17	0.32298 (17)	0.81918 (9)	0.36173 (6)	0.0481 (4)
C18	0.3335 (2)	0.79905 (10)	0.31689 (6)	0.0579 (5)
C19	0.43405 (17)	0.79941 (9)	0.39099 (6)	0.0511 (4)
C20	0.5293 (2)	0.74314 (11)	0.37581 (8)	0.0669 (6)
C21	0.44660 (17)	0.82844 (10)	0.43558 (6)	0.0537 (5)
C22	0.5194 (2)	0.77923 (12)	0.46550 (7)	0.0677 (6)
C23	0.39239 (18)	0.90272 (10)	0.45257 (6)	0.0518 (4)
C24	0.3753 (2)	0.91048 (13)	0.49824 (6)	0.0645 (5)
C25	0.36511 (18)	0.97354 (10)	0.42623 (5)	0.0493 (4)
C26	0.2902 (2)	1.03752 (11)	0.44461 (6)	0.0595 (5)
C27	0.45498 (19)	1.06453 (10)	0.31387 (6)	0.0542 (5)
C28	0.5478 (3)	1.13731 (14)	0.31569 (8)	0.0949 (8)
H28A	0.6193	1.1277	0.3363	0.142*
H28B	0.4967	1.1833	0.3247	0.142*
H28C	0.5858	1.1467	0.2873	0.142*
C29	0.3417 (3)	1.07964 (16)	0.28061 (7)	0.0923 (8)
H29A	0.2897	1.1254	0.2895	0.138*
H29B	0.2839	1.0335	0.2791	0.138*
H29C	0.3805	1.0895	0.2523	0.138*
C30	0.5364 (2)	0.99317 (13)	0.29806 (7)	0.0781 (7)
H30A	0.4796	0.9466	0.2974	0.117*
H30B	0.6109	0.9841	0.3176	0.117*
H30C	0.5703	1.0037	0.2692	0.117*
C31	−0.0377 (2)	0.90642 (12)	0.36511 (7)	0.0663 (5)
C32	−0.0525 (3)	0.99102 (16)	0.34811 (11)	0.1169 (10)
H32A	−0.0489	0.9906	0.3167	0.175*
H32B	0.0196	1.0235	0.3594	0.175*
H32C	−0.1378	1.0126	0.3575	0.175*
C33	−0.0439 (4)	0.9101 (3)	0.41396 (10)	0.189 (2)
H33A	−0.1323	0.9274	0.4229	0.283*
H33B	0.0227	0.9472	0.4245	0.283*
H33C	−0.0261	0.8579	0.4258	0.283*
C34	−0.1571 (3)	0.85795 (19)	0.34797 (15)	0.1539 (16)
H34A	−0.1575	0.8594	0.3166	0.231*
H34B	−0.2399	0.8804	0.3589	0.231*
H34C	−0.1490	0.8035	0.3577	0.231*
I1	0.1821 (19)	1.1575 (10)	0.4685 (6)	0.090 (5)	0.01
I2	0.2520 (19)	0.8048 (11)	0.2375 (5)	0.096 (5)	0.01

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0487 (10)	0.0355 (8)	0.0508 (10)	−0.0009 (7)	−0.0006 (7)	−0.0014 (7)
C2	0.0533 (11)	0.0355 (9)	0.0529 (10)	−0.0012 (7)	−0.0062 (8)	−0.0007 (7)
C3	0.0766 (14)	0.0418 (10)	0.0654 (13)	0.0121 (9)	−0.0072 (10)	0.0011 (8)
C4	0.0786 (14)	0.0491 (11)	0.0719 (14)	0.0174 (10)	0.0027 (11)	−0.0102 (9)
C5	0.0931 (17)	0.0786 (15)	0.0668 (14)	0.0093 (13)	0.0198 (12)	−0.0104 (11)
C6	0.0979 (18)	0.0882 (16)	0.0525 (12)	−0.0021 (13)	0.0129 (11)	−0.0010 (11)
C7	0.0773 (16)	0.0985 (18)	0.0623 (14)	−0.0130 (14)	−0.0044 (11)	0.0275 (12)
C8	0.0689 (15)	0.0839 (16)	0.0817 (17)	−0.0091 (12)	−0.0137 (12)	0.0375 (12)
C9	0.0626 (15)	0.0640 (14)	0.130 (2)	0.0118 (11)	−0.0054 (14)	0.0303 (14)
C10	0.0581 (14)	0.0534 (13)	0.140 (2)	0.0161 (10)	0.0052 (14)	0.0100 (13)
C11	0.0711 (16)	0.0502 (12)	0.118 (2)	0.0042 (10)	0.0258 (14)	−0.0169 (12)
C12	0.0834 (17)	0.0560 (13)	0.0832 (15)	−0.0141 (11)	0.0261 (12)	−0.0206 (11)
C13	0.0895 (17)	0.0659 (13)	0.0561 (12)	−0.0186 (12)	0.0051 (11)	−0.0072 (9)
C14	0.0764 (15)	0.0613 (13)	0.0613 (13)	−0.0110 (11)	−0.0129 (10)	0.0054 (9)
C15	0.0556 (12)	0.0438 (10)	0.0628 (12)	−0.0058 (8)	−0.0045 (9)	0.0091 (8)
C16	0.0523 (11)	0.0379 (9)	0.0548 (10)	−0.0003 (7)	0.0016 (8)	0.0033 (7)
C17	0.0512 (11)	0.0304 (9)	0.0627 (11)	−0.0065 (7)	0.0065 (8)	0.0015 (7)
C18	0.0673 (13)	0.0423 (10)	0.0642 (12)	−0.0118 (9)	0.0108 (10)	−0.0079 (8)
C19	0.0461 (11)	0.0327 (9)	0.0744 (12)	−0.0007 (7)	0.0069 (8)	0.0065 (8)
C20	0.0508 (12)	0.0412 (10)	0.1088 (17)	0.0016 (8)	0.0148 (11)	0.0023 (10)
C21	0.0414 (10)	0.0491 (10)	0.0708 (13)	−0.0028 (8)	0.0008 (8)	0.0176 (8)
C22	0.0525 (12)	0.0585 (13)	0.0920 (16)	−0.0027 (9)	−0.0071 (10)	0.0259 (10)
C23	0.0488 (11)	0.0529 (11)	0.0537 (11)	−0.0038 (8)	0.0000 (8)	0.0087 (8)
C24	0.0643 (13)	0.0734 (13)	0.0559 (12)	−0.0112 (10)	0.0022 (9)	0.0118 (10)
C25	0.0540 (11)	0.0432 (9)	0.0507 (10)	−0.0022 (8)	−0.0003 (8)	−0.0009 (7)
C26	0.0664 (13)	0.0562 (11)	0.0561 (11)	0.0035 (9)	0.0069 (9)	−0.0073 (8)
C27	0.0649 (12)	0.0453 (10)	0.0525 (11)	−0.0040 (8)	−0.0039 (8)	0.0091 (8)
C28	0.118 (2)	0.0755 (16)	0.0914 (17)	−0.0400 (14)	0.0054 (15)	0.0128 (12)
C29	0.0984 (19)	0.116 (2)	0.0622 (14)	0.0162 (16)	−0.0179 (12)	0.0043 (12)
C30	0.0948 (17)	0.0701 (14)	0.0695 (14)	0.0087 (12)	0.0263 (12)	0.0120 (10)
C31	0.0552 (13)	0.0627 (12)	0.0810 (14)	0.0103 (9)	−0.0043 (10)	0.0110 (10)
C32	0.109 (2)	0.0656 (16)	0.176 (3)	0.0205 (15)	0.002 (2)	0.0077 (17)
C33	0.121 (3)	0.351 (6)	0.095 (2)	0.148 (4)	0.0357 (19)	0.043 (3)
C34	0.0611 (18)	0.100 (2)	0.300 (5)	−0.0078 (16)	0.009 (2)	−0.048 (3)
I1	0.104 (13)	0.076 (10)	0.091 (11)	0.016 (9)	0.001 (9)	−0.005 (8)
I2	0.099 (12)	0.105 (13)	0.084 (11)	0.002 (10)	0.005 (9)	−0.023 (9)

Geometric parameters (Å, º)

C1—C2	1.378 (2)	C16—C17	1.409 (2)
C1—C25	1.408 (2)	C16—H16	0.9300
C1—H1	0.9300	C17—C18	1.415 (2)
C2—C3	1.410 (2)	C17—C19	1.454 (2)
C2—C27	1.528 (2)	C19—C20	1.409 (3)
C3—C4	1.348 (3)	C19—C21	1.452 (3)
C3—H3	0.9300	C21—C22	1.425 (2)
C4—C26	1.409 (3)	C21—C23	1.448 (3)
C4—H4	0.9300	C23—C24	1.413 (3)
C5—C6	1.343 (3)	C23—C25	1.457 (2)
C5—C26	1.420 (3)	C25—C26	1.417 (2)
C5—H5	0.9300	C27—C30	1.518 (3)
C6—C24	1.422 (3)	C27—C28	1.524 (3)
C6—H6	0.9300	C27—C29	1.533 (3)
C7—C8	1.334 (3)	C28—H28A	0.9600
C7—C24	1.416 (3)	C28—H28B	0.9600
C7—H7	0.9300	C28—H28C	0.9600
C8—C22	1.416 (3)	C29—H29A	0.9600
C8—H8	0.9300	C29—H29B	0.9600
C9—C10	1.344 (3)	C29—H29C	0.9600
C9—C22	1.404 (3)	C30—H30A	0.9600
C9—H9	0.9300	C30—H30B	0.9600
C10—C20	1.427 (3)	C30—H30C	0.9600
C10—H10	0.9300	C31—C33	1.496 (4)
C11—C12	1.329 (3)	C31—C32	1.513 (3)
C11—C20	1.413 (3)	C31—C34	1.524 (4)
C11—H11	0.9300	C32—H32A	0.9600
C12—C18	1.434 (3)	C32—H32B	0.9600
C12—H12	0.9300	C32—H32C	0.9600
C13—C14	1.363 (3)	C33—H33A	0.9600
C13—C18	1.398 (3)	C33—H33B	0.9600
C13—H13	0.9300	C33—H33C	0.9600
C14—C15	1.406 (3)	C34—H34A	0.9600
C14—H14	0.9300	C34—H34B	0.9600
C15—C16	1.375 (2)	C34—H34C	0.9600
C15—C31	1.521 (3)
C2—C1—C25	122.90 (16)	C9—C22—C8	120.7 (2)
C2—C1—H1	118.6	C9—C22—C21	119.5 (2)
C25—C1—H1	118.6	C8—C22—C21	119.8 (2)
C1—C2—C3	117.69 (16)	C24—C23—C21	118.52 (16)
C1—C2—C27	122.67 (15)	C24—C23—C25	116.73 (16)
C3—C2—C27	119.63 (15)	C21—C23—C25	124.51 (16)
C4—C3—C2	121.21 (17)	C23—C24—C7	119.8 (2)
C4—C3—H3	119.4	C23—C24—C6	119.85 (18)
C2—C3—H3	119.4	C7—C24—C6	120.3 (2)
C3—C4—C26	121.47 (17)	C1—C25—C26	117.49 (15)
C3—C4—H4	119.3	C1—C25—C23	122.94 (15)
C26—C4—H4	119.3	C26—C25—C23	119.39 (16)
C6—C5—C26	120.1 (2)	C4—C26—C25	118.85 (17)
C6—C5—H5	119.9	C4—C26—C5	121.36 (18)
C26—C5—H5	119.9	C25—C26—C5	119.62 (18)
C5—C6—C24	121.91 (19)	C30—C27—C28	108.62 (19)
C5—C6—H6	119.0	C30—C27—C2	112.99 (14)
C24—C6—H6	119.0	C28—C27—C2	108.68 (16)
C8—C7—C24	120.7 (2)	C30—C27—C29	107.80 (17)
C8—C7—H7	119.7	C28—C27—C29	109.40 (18)
C24—C7—H7	119.7	C2—C27—C29	109.31 (17)
C7—C8—C22	121.4 (2)	C27—C28—H28A	109.5
C7—C8—H8	119.3	C27—C28—H28B	109.5
C22—C8—H8	119.3	H28A—C28—H28B	109.5
C10—C9—C22	121.9 (2)	C27—C28—H28C	109.5
C10—C9—H9	119.0	H28A—C28—H28C	109.5
C22—C9—H9	119.0	H28B—C28—H28C	109.5
C9—C10—C20	120.1 (2)	C27—C29—H29A	109.5
C9—C10—H10	119.9	C27—C29—H29B	109.5
C20—C10—H10	119.9	H29A—C29—H29B	109.5
C12—C11—C20	121.9 (2)	C27—C29—H29C	109.5
C12—C11—H11	119.1	H29A—C29—H29C	109.5
C20—C11—H11	119.1	H29B—C29—H29C	109.5
C11—C12—C18	120.4 (2)	C27—C30—H30A	109.5
C11—C12—H12	119.8	C27—C30—H30B	109.5
C18—C12—H12	119.8	H30A—C30—H30B	109.5
C14—C13—C18	121.72 (19)	C27—C30—H30C	109.5
C14—C13—H13	119.1	H30A—C30—H30C	109.5
C18—C13—H13	119.1	H30B—C30—H30C	109.5
C13—C14—C15	120.96 (19)	C33—C31—C32	107.5 (3)
C13—C14—H14	119.5	C33—C31—C15	112.35 (17)
C15—C14—H14	119.5	C32—C31—C15	109.51 (19)
C16—C15—C14	117.44 (18)	C33—C31—C34	109.5 (3)
C16—C15—C31	122.43 (17)	C32—C31—C34	107.7 (2)
C14—C15—C31	120.13 (17)	C15—C31—C34	110.18 (19)
C15—C16—C17	123.27 (16)	C31—C32—H32A	109.5
C15—C16—H16	118.4	C31—C32—H32B	109.5
C17—C16—H16	118.4	H32A—C32—H32B	109.5
C16—C17—C18	117.57 (16)	C31—C32—H32C	109.5
C16—C17—C19	123.15 (16)	H32A—C32—H32C	109.5
C18—C17—C19	119.11 (16)	H32B—C32—H32C	109.5
C13—C18—C17	118.69 (18)	C31—C33—H33A	109.5
C13—C18—C12	122.05 (19)	C31—C33—H33B	109.5
C17—C18—C12	119.16 (19)	H33A—C33—H33B	109.5
C20—C19—C21	118.36 (17)	C31—C33—H33C	109.5
C20—C19—C17	116.95 (18)	H33A—C33—H33C	109.5
C21—C19—C17	124.48 (15)	H33B—C33—H33C	109.5
C19—C20—C11	120.1 (2)	C31—C34—H34A	109.5
C19—C20—C10	119.5 (2)	C31—C34—H34B	109.5
C11—C20—C10	120.3 (2)	H34A—C34—H34B	109.5
C22—C21—C23	116.82 (18)	C31—C34—H34C	109.5
C22—C21—C19	116.93 (17)	H34A—C34—H34C	109.5
C23—C21—C19	126.25 (15)	H34B—C34—H34C	109.5
C25—C1—C2—C3	−0.8 (3)	C7—C8—C22—C21	−0.4 (3)
C25—C1—C2—C27	177.93 (16)	C23—C21—C22—C9	−164.12 (18)
C1—C2—C3—C4	4.1 (3)	C19—C21—C22—C9	15.8 (3)
C27—C2—C3—C4	−174.74 (18)	C23—C21—C22—C8	14.5 (3)
C2—C3—C4—C26	−1.6 (3)	C19—C21—C22—C8	−165.62 (17)
C26—C5—C6—C24	−7.2 (4)	C22—C21—C23—C24	−20.0 (2)
C24—C7—C8—C22	−8.4 (3)	C19—C21—C23—C24	160.07 (17)
C22—C9—C10—C20	−9.2 (4)	C22—C21—C23—C25	154.11 (17)
C20—C11—C12—C18	−6.5 (3)	C19—C21—C23—C25	−25.8 (3)
C18—C13—C14—C15	−1.6 (3)	C21—C23—C24—C7	12.1 (3)
C13—C14—C15—C16	3.9 (3)	C25—C23—C24—C7	−162.52 (18)
C13—C14—C15—C31	−176.51 (18)	C21—C23—C24—C6	−170.08 (18)
C14—C15—C16—C17	−0.7 (2)	C25—C23—C24—C6	15.3 (3)
C31—C15—C16—C17	179.67 (16)	C8—C7—C24—C23	2.4 (3)
C15—C16—C17—C18	−4.5 (2)	C8—C7—C24—C6	−175.5 (2)
C15—C16—C17—C19	−179.77 (15)	C5—C6—C24—C23	−3.6 (3)
C14—C13—C18—C17	−3.8 (3)	C5—C6—C24—C7	174.3 (2)
C14—C13—C18—C12	172.68 (18)	C2—C1—C25—C26	−4.6 (3)
C16—C17—C18—C13	6.6 (2)	C2—C1—C25—C23	−179.80 (16)
C19—C17—C18—C13	−177.91 (16)	C24—C23—C25—C1	158.13 (17)
C16—C17—C18—C12	−169.93 (16)	C21—C23—C25—C1	−16.1 (3)
C19—C17—C18—C12	5.5 (2)	C24—C23—C25—C26	−16.9 (3)
C11—C12—C18—C13	−170.3 (2)	C21—C23—C25—C26	168.82 (17)
C11—C12—C18—C17	6.1 (3)	C3—C4—C26—C25	−4.1 (3)
C16—C17—C19—C20	158.80 (16)	C3—C4—C26—C5	171.2 (2)
C18—C17—C19—C20	−16.4 (2)	C1—C25—C26—C4	7.0 (3)
C16—C17—C19—C21	−15.8 (2)	C23—C25—C26—C4	−177.69 (18)
C18—C17—C19—C21	168.97 (15)	C1—C25—C26—C5	−168.37 (18)
C21—C19—C20—C11	−168.65 (17)	C23—C25—C26—C5	7.0 (3)
C17—C19—C20—C11	16.4 (3)	C6—C5—C26—C4	−170.0 (2)
C21—C19—C20—C10	13.6 (3)	C6—C5—C26—C25	5.3 (3)
C17—C19—C20—C10	−161.35 (17)	C1—C2—C27—C30	4.9 (2)
C12—C11—C20—C19	−5.2 (3)	C3—C2—C27—C30	−176.36 (18)
C12—C11—C20—C10	172.5 (2)	C1—C2—C27—C28	−115.7 (2)
C9—C10—C20—C19	2.2 (3)	C3—C2—C27—C28	63.0 (2)
C9—C10—C20—C11	−175.5 (2)	C1—C2—C27—C29	124.92 (19)
C20—C19—C21—C22	−22.3 (2)	C3—C2—C27—C29	−56.3 (2)
C17—C19—C21—C22	152.30 (16)	C16—C15—C31—C33	−6.1 (3)
C20—C19—C21—C23	157.65 (17)	C14—C15—C31—C33	174.3 (3)
C17—C19—C21—C23	−27.8 (3)	C16—C15—C31—C32	113.3 (2)
C10—C9—C22—C8	−178.7 (2)	C14—C15—C31—C32	−66.3 (3)
C10—C9—C22—C21	−0.2 (3)	C16—C15—C31—C34	−128.5 (2)
C7—C8—C22—C9	178.2 (2)	C14—C15—C31—C34	51.9 (3)

Trans-1-(para-tert-butylphenyl)-2-(2-benzo[c]phenanthrenyl)ethylene (VIIb)

Crystal data

C30H26	F(000) = 824
Mr = 386.51	Dx = 1.221 Mg m^−3
Monoclinic, p_21/c	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -p_2ybc	Cell parameters from 9890 reflections
a = 15.8991 (5) Å	θ = 2.8–67.7°
b = 15.3550 (5) Å	µ = 0.52 mm^−1
c = 8.6220 (3) Å	T = 100 K
β = 92.677 (2)°	Rod, colourless
V = 2102.60 (12) Å^3	0.60 × 0.10 × 0.10 mm
Z = 4

Data collection

CCD area detector diffractometer	3653 independent reflections
Radiation source: fine-focus sealed tube	3122 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.030
phi and ω scans	θmax = 68.1°, θmin = 2.8°
Absorption correction: multi-scan SADABS (Bruker)	h = −18→19
Tmin = 0.855, Tmax = 0.950	k = −18→17
22369 measured reflections	l = −10→9

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.103	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0568P)^2 + 0.4277P] where P = (Fo^2 + 2Fc^2)/3
3653 reflections	(Δ/σ)max = 0.002
274 parameters	Δρmax = 0.16 e Å^−3
0 restraints	Δρmin = −0.20 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
C1	0.62021 (8)	0.42258 (9)	0.64883 (17)	0.0336 (3)
H1	0.6721	0.4532	0.6592	0.040*
C2	0.59893 (8)	0.37994 (8)	0.50999 (15)	0.0257 (3)
C3	0.52233 (8)	0.33516 (8)	0.50169 (16)	0.0276 (3)
H3	0.5062	0.3045	0.4093	0.033*
C4	0.46933 (8)	0.33427 (8)	0.62457 (16)	0.0277 (3)
H4	0.4176	0.3034	0.6145	0.033*
C5	0.43668 (8)	0.37920 (8)	0.89683 (16)	0.0286 (3)
H5	0.4625	0.3974	0.9930	0.034*
C6	0.35525 (8)	0.35750 (8)	0.89793 (15)	0.0265 (3)
H6	0.3291	0.3387	0.8024	0.032*
C7	0.33753 (8)	0.36490 (8)	1.18708 (16)	0.0290 (3)
H7	0.3967	0.3706	1.2051	0.035*
C8	0.28626 (8)	0.36131 (8)	1.30947 (16)	0.0289 (3)
H8	0.3108	0.3617	1.4121	0.035*
C9	0.14639 (8)	0.34415 (8)	1.41692 (15)	0.0282 (3)
H9	0.1709	0.3454	1.5195	0.034*
C10	0.06258 (8)	0.33003 (8)	1.39369 (15)	0.0278 (3)
H10	0.0300	0.3145	1.4791	0.033*
C11	−0.06643 (8)	0.32619 (8)	1.22533 (16)	0.0292 (3)
H11	−0.0968	0.3085	1.3123	0.035*
C12	−0.10820 (8)	0.33957 (8)	1.08702 (16)	0.0295 (3)
H12	−0.1667	0.3270	1.0761	0.035*
C13	−0.11138 (8)	0.39468 (8)	0.81882 (16)	0.0294 (3)
H13	−0.1700	0.3829	0.8095	0.035*
C14	−0.07299 (8)	0.43297 (8)	0.69797 (16)	0.0302 (3)
H14	−0.1041	0.4456	0.6039	0.036*
C15	0.01288 (8)	0.45336 (8)	0.71444 (15)	0.0268 (3)
H15	0.0393	0.4827	0.6328	0.032*
C16	0.05929 (8)	0.43152 (8)	0.84683 (15)	0.0244 (3)
H16	0.1172	0.4470	0.8557	0.029*
C17	0.02302 (8)	0.38640 (7)	0.97091 (14)	0.0234 (3)
C18	−0.06545 (8)	0.37224 (8)	0.95770 (15)	0.0262 (3)
C19	0.06923 (8)	0.36148 (7)	1.11381 (14)	0.0231 (3)
C20	0.02255 (8)	0.33817 (8)	1.24275 (15)	0.0255 (3)
C21	0.16045 (8)	0.36050 (7)	1.13432 (15)	0.0235 (3)
C22	0.19780 (8)	0.35709 (8)	1.28807 (15)	0.0259 (3)
C23	0.21598 (8)	0.35688 (8)	1.01037 (15)	0.0241 (3)
H23	0.1926	0.3521	0.9073	0.029*
C24	0.30260 (8)	0.36006 (8)	1.03312 (15)	0.0259 (3)
C25	0.56743 (8)	0.42134 (9)	0.77224 (17)	0.0343 (3)
H25	0.5842	0.4509	0.8654	0.041*
C26	0.49046 (8)	0.37788 (8)	0.76316 (15)	0.0269 (3)
C27	0.65886 (8)	0.37682 (8)	0.37563 (15)	0.0279 (3)
C28	0.60999 (9)	0.37769 (11)	0.21802 (17)	0.0394 (4)
H28A	0.6497	0.3806	0.1346	0.059*
H28B	0.5728	0.4286	0.2120	0.059*
H28C	0.5762	0.3245	0.2067	0.059*
C29	0.71881 (9)	0.45485 (10)	0.37838 (17)	0.0384 (3)
H29A	0.7543	0.4538	0.4744	0.058*
H29B	0.6861	0.5089	0.3736	0.058*
H29C	0.7545	0.4518	0.2889	0.058*
C30	0.71012 (11)	0.29240 (11)	0.3915 (2)	0.0509 (5)
H30A	0.7473	0.2875	0.3044	0.076*
H30B	0.6718	0.2424	0.3910	0.076*
H30C	0.7441	0.2934	0.4893	0.076*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0256 (6)	0.0365 (8)	0.0390 (8)	−0.0065 (5)	0.0054 (6)	−0.0074 (6)
C2	0.0241 (6)	0.0220 (6)	0.0309 (7)	0.0032 (5)	0.0016 (5)	0.0024 (5)
C3	0.0264 (6)	0.0284 (7)	0.0279 (7)	−0.0012 (5)	−0.0007 (5)	0.0003 (5)
C4	0.0228 (6)	0.0283 (7)	0.0321 (7)	−0.0016 (5)	0.0008 (5)	0.0025 (5)
C5	0.0265 (6)	0.0295 (7)	0.0299 (7)	0.0025 (5)	0.0018 (5)	−0.0018 (5)
C6	0.0268 (6)	0.0250 (6)	0.0278 (7)	0.0034 (5)	0.0015 (5)	0.0010 (5)
C7	0.0266 (6)	0.0286 (7)	0.0316 (7)	0.0015 (5)	−0.0007 (5)	−0.0016 (5)
C8	0.0332 (7)	0.0268 (7)	0.0264 (7)	0.0033 (5)	−0.0030 (5)	−0.0013 (5)
C9	0.0382 (7)	0.0225 (6)	0.0241 (7)	0.0042 (5)	0.0020 (5)	0.0002 (5)
C10	0.0376 (7)	0.0192 (6)	0.0272 (7)	0.0022 (5)	0.0092 (5)	0.0015 (5)
C11	0.0325 (7)	0.0228 (6)	0.0333 (7)	−0.0033 (5)	0.0109 (6)	0.0005 (5)
C12	0.0261 (6)	0.0236 (6)	0.0391 (8)	−0.0043 (5)	0.0067 (5)	−0.0029 (5)
C13	0.0261 (6)	0.0249 (6)	0.0370 (8)	−0.0005 (5)	−0.0002 (5)	−0.0048 (5)
C14	0.0336 (7)	0.0265 (7)	0.0302 (7)	0.0039 (5)	−0.0017 (5)	−0.0019 (5)
C15	0.0309 (7)	0.0229 (6)	0.0270 (7)	0.0033 (5)	0.0044 (5)	−0.0002 (5)
C16	0.0249 (6)	0.0210 (6)	0.0277 (7)	0.0024 (5)	0.0045 (5)	−0.0029 (5)
C17	0.0264 (6)	0.0176 (6)	0.0266 (7)	0.0011 (5)	0.0046 (5)	−0.0038 (4)
C18	0.0277 (6)	0.0187 (6)	0.0327 (7)	0.0001 (5)	0.0049 (5)	−0.0043 (5)
C19	0.0278 (6)	0.0158 (6)	0.0261 (7)	−0.0006 (5)	0.0049 (5)	−0.0026 (4)
C20	0.0316 (7)	0.0170 (6)	0.0285 (7)	0.0003 (5)	0.0074 (5)	−0.0010 (5)
C21	0.0282 (6)	0.0159 (6)	0.0264 (7)	0.0004 (5)	0.0029 (5)	−0.0009 (4)
C22	0.0325 (7)	0.0191 (6)	0.0263 (7)	0.0031 (5)	0.0026 (5)	−0.0011 (5)
C23	0.0274 (6)	0.0207 (6)	0.0245 (6)	0.0010 (5)	0.0020 (5)	0.0003 (5)
C24	0.0272 (6)	0.0201 (6)	0.0305 (7)	0.0015 (5)	0.0026 (5)	0.0002 (5)
C25	0.0283 (7)	0.0392 (8)	0.0357 (8)	−0.0042 (6)	0.0040 (6)	−0.0104 (6)
C26	0.0233 (6)	0.0256 (6)	0.0318 (7)	0.0038 (5)	0.0015 (5)	0.0011 (5)
C27	0.0245 (6)	0.0275 (7)	0.0321 (7)	0.0003 (5)	0.0041 (5)	0.0017 (5)
C28	0.0365 (8)	0.0510 (9)	0.0313 (8)	−0.0070 (6)	0.0062 (6)	−0.0066 (6)
C29	0.0376 (8)	0.0440 (9)	0.0340 (8)	−0.0110 (6)	0.0064 (6)	0.0014 (6)
C30	0.0511 (9)	0.0404 (9)	0.0639 (11)	0.0162 (7)	0.0329 (8)	0.0158 (8)

Geometric parameters (Å, º)

C1—C25	1.3856 (19)	C13—C18	1.4156 (19)
C1—C2	1.3923 (19)	C13—H13	0.9500
C1—H1	0.9500	C14—C15	1.4015 (18)
C2—C3	1.3975 (18)	C14—H14	0.9500
C2—C27	1.5347 (17)	C15—C16	1.3715 (19)
C3—C4	1.3843 (18)	C15—H15	0.9500
C3—H3	0.9500	C16—C17	1.4193 (17)
C4—C26	1.3971 (19)	C16—H16	0.9500
C4—H4	0.9500	C17—C18	1.4227 (17)
C5—C6	1.3372 (18)	C17—C19	1.4560 (18)
C5—C26	1.4670 (17)	C19—C20	1.4113 (17)
C5—H5	0.9500	C19—C21	1.4528 (17)
C6—C24	1.4670 (17)	C21—C23	1.4188 (17)
C6—H6	0.9500	C21—C22	1.4280 (19)
C7—C8	1.3643 (18)	C23—C24	1.3827 (17)
C7—C24	1.4168 (19)	C23—H23	0.9500
C7—H7	0.9500	C25—C26	1.3928 (18)
C8—C22	1.4115 (18)	C25—H25	0.9500
C8—H8	0.9500	C27—C29	1.5305 (18)
C9—C10	1.3556 (19)	C27—C30	1.5340 (19)
C9—C22	1.4236 (18)	C27—C28	1.534 (2)
C9—H9	0.9500	C28—H28A	0.9800
C10—C20	1.427 (2)	C28—H28B	0.9800
C10—H10	0.9500	C28—H28C	0.9800
C11—C12	1.353 (2)	C29—H29A	0.9800
C11—C20	1.4276 (18)	C29—H29B	0.9800
C11—H11	0.9500	C29—H29C	0.9800
C12—C18	1.4239 (18)	C30—H30A	0.9800
C12—H12	0.9500	C30—H30B	0.9800
C13—C14	1.3650 (19)	C30—H30C	0.9800
C25—C1—C2	121.49 (12)	C13—C18—C17	119.97 (12)
C25—C1—H1	119.3	C13—C18—C12	120.13 (12)
C2—C1—H1	119.3	C17—C18—C12	119.83 (12)
C1—C2—C3	116.85 (12)	C20—C19—C21	117.40 (12)
C1—C2—C27	121.95 (11)	C20—C19—C17	118.04 (11)
C3—C2—C27	121.08 (12)	C21—C19—C17	124.55 (11)
C4—C3—C2	121.73 (12)	C19—C20—C10	120.80 (12)
C4—C3—H3	119.1	C19—C20—C11	120.32 (12)
C2—C3—H3	119.1	C10—C20—C11	118.82 (12)
C3—C4—C26	121.28 (12)	C23—C21—C22	116.84 (11)
C3—C4—H4	119.4	C23—C21—C19	124.16 (12)
C26—C4—H4	119.4	C22—C21—C19	118.87 (11)
C6—C5—C26	127.03 (13)	C8—C22—C9	120.62 (12)
C6—C5—H5	116.5	C8—C22—C21	119.23 (12)
C26—C5—H5	116.5	C9—C22—C21	120.04 (12)
C5—C6—C24	125.98 (12)	C24—C23—C21	122.85 (12)
C5—C6—H6	117.0	C24—C23—H23	118.6
C24—C6—H6	117.0	C21—C23—H23	118.6
C8—C7—C24	120.03 (12)	C23—C24—C7	118.62 (12)
C8—C7—H7	120.0	C23—C24—C6	119.20 (12)
C24—C7—H7	120.0	C7—C24—C6	122.18 (12)
C7—C8—C22	121.90 (12)	C1—C25—C26	121.69 (13)
C7—C8—H8	119.1	C1—C25—H25	119.2
C22—C8—H8	119.1	C26—C25—H25	119.2
C10—C9—C22	120.22 (12)	C25—C26—C4	116.96 (12)
C10—C9—H9	119.9	C25—C26—C5	119.48 (12)
C22—C9—H9	119.9	C4—C26—C5	123.56 (12)
C9—C10—C20	120.93 (12)	C29—C27—C30	109.41 (12)
C9—C10—H10	119.5	C29—C27—C28	107.23 (11)
C20—C10—H10	119.5	C30—C27—C28	109.36 (13)
C12—C11—C20	121.08 (12)	C29—C27—C2	111.84 (11)
C12—C11—H11	119.5	C30—C27—C2	107.76 (11)
C20—C11—H11	119.5	C28—C27—C2	111.22 (11)
C11—C12—C18	120.73 (12)	C27—C28—H28A	109.5
C11—C12—H12	119.6	C27—C28—H28B	109.5
C18—C12—H12	119.6	H28A—C28—H28B	109.5
C14—C13—C18	121.28 (12)	C27—C28—H28C	109.5
C14—C13—H13	119.4	H28A—C28—H28C	109.5
C18—C13—H13	119.4	H28B—C28—H28C	109.5
C13—C14—C15	119.15 (13)	C27—C29—H29A	109.5
C13—C14—H14	120.4	C27—C29—H29B	109.5
C15—C14—H14	120.4	H29A—C29—H29B	109.5
C16—C15—C14	120.89 (12)	C27—C29—H29C	109.5
C16—C15—H15	119.6	H29A—C29—H29C	109.5
C14—C15—H15	119.6	H29B—C29—H29C	109.5
C15—C16—C17	121.67 (12)	C27—C30—H30A	109.5
C15—C16—H16	119.2	C27—C30—H30B	109.5
C17—C16—H16	119.2	H30A—C30—H30B	109.5
C16—C17—C18	116.69 (12)	C27—C30—H30C	109.5
C16—C17—C19	124.02 (11)	H30A—C30—H30C	109.5
C18—C17—C19	119.05 (11)	H30B—C30—H30C	109.5
C25—C1—C2—C3	−0.6 (2)	C20—C19—C21—C23	160.77 (11)
C25—C1—C2—C27	−176.75 (13)	C17—C19—C21—C23	−20.49 (18)
C1—C2—C3—C4	1.01 (19)	C20—C19—C21—C22	−14.85 (16)
C27—C2—C3—C4	177.15 (12)	C17—C19—C21—C22	163.88 (11)
C2—C3—C4—C26	−0.38 (19)	C7—C8—C22—C9	173.32 (12)
C26—C5—C6—C24	−179.47 (12)	C7—C8—C22—C21	−2.80 (19)
C24—C7—C8—C22	−3.16 (19)	C10—C9—C22—C8	−172.30 (12)
C22—C9—C10—C20	−7.58 (18)	C10—C9—C22—C21	3.79 (18)
C20—C11—C12—C18	−4.69 (19)	C23—C21—C22—C8	7.78 (17)
C18—C13—C14—C15	−2.46 (19)	C19—C21—C22—C8	−176.28 (11)
C13—C14—C15—C16	3.21 (19)	C23—C21—C22—C9	−168.36 (11)
C14—C15—C16—C17	1.06 (19)	C19—C21—C22—C9	7.58 (17)
C15—C16—C17—C18	−5.80 (17)	C22—C21—C23—C24	−7.35 (17)
C15—C16—C17—C19	179.89 (11)	C19—C21—C23—C24	176.94 (11)
C14—C13—C18—C17	−2.47 (18)	C21—C23—C24—C7	1.66 (18)
C14—C13—C18—C12	174.39 (12)	C21—C23—C24—C6	−178.91 (11)
C16—C17—C18—C13	6.43 (17)	C8—C7—C24—C23	3.76 (18)
C19—C17—C18—C13	−178.96 (11)	C8—C7—C24—C6	−175.66 (11)
C16—C17—C18—C12	−170.43 (11)	C5—C6—C24—C23	164.06 (12)
C19—C17—C18—C12	4.17 (17)	C5—C6—C24—C7	−16.5 (2)
C11—C12—C18—C13	−173.28 (12)	C2—C1—C25—C26	−0.4 (2)
C11—C12—C18—C17	3.59 (18)	C1—C25—C26—C4	1.0 (2)
C16—C17—C19—C20	163.54 (11)	C1—C25—C26—C5	−179.52 (13)
C18—C17—C19—C20	−10.64 (16)	C3—C4—C26—C25	−0.63 (19)
C16—C17—C19—C21	−15.19 (18)	C3—C4—C26—C5	179.91 (12)
C18—C17—C19—C21	170.63 (11)	C6—C5—C26—C25	164.88 (14)
C21—C19—C20—C10	11.43 (17)	C6—C5—C26—C4	−15.7 (2)
C17—C19—C20—C10	−167.39 (11)	C1—C2—C27—C29	−26.55 (17)
C21—C19—C20—C11	−171.43 (11)	C3—C2—C27—C29	157.51 (12)
C17—C19—C20—C11	9.75 (17)	C1—C2—C27—C30	93.73 (16)
C9—C10—C20—C19	−0.25 (18)	C3—C2—C27—C30	−82.21 (16)
C9—C10—C20—C11	−177.43 (11)	C1—C2—C27—C28	−146.42 (13)
C12—C11—C20—C19	−2.18 (19)	C3—C2—C27—C28	37.64 (16)
C12—C11—C20—C10	175.02 (12)

Trans-1-(para-tert-butylphenyl)-2-(2-benzo[c]phenanthrenyl)ethylene (VIIc)

Crystal data

C30H26	F(000) = 824
Mr = 386.51	Dx = 1.180 Mg m^−3
Monoclinic, p_21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -p_2ybc	Cell parameters from 5437 reflections
a = 15.990 (2) Å	θ = 3.8–27.6°
b = 15.712 (2) Å	µ = 0.07 mm^−1
c = 8.6656 (11) Å	T = 293 K
β = 92.544 (2)°	Needle, colourless
V = 2175.0 (5) Å^3	0.60 × 0.10 × 0.10 mm
Z = 4

Data collection

CCD area detector diffractometer	5390 independent reflections
Radiation source: fine-focus sealed tube	3017 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.039
phi and ω scans	θmax = 28.3°, θmin = 3.8°
Absorption correction: multi-scan SADABS (Bruker)	h = −21→21
Tmin = 0.961, Tmax = 0.993	k = −20→20
19272 measured reflections	l = −11→11

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)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.160	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0694P)^2 + 0.2605P] where P = (Fo^2 + 2Fc^2)/3
5390 reflections	(Δ/σ)max = 0.002
274 parameters	Δρmax = 0.24 e Å^−3
0 restraints	Δρmin = −0.21 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
C1	0.62421 (11)	0.42050 (14)	0.6594 (2)	0.0656 (5)
H1	0.6747	0.4497	0.6704	0.079*
C2	0.60409 (10)	0.37960 (11)	0.5212 (2)	0.0493 (4)
C3	0.52823 (11)	0.33626 (13)	0.5132 (2)	0.0596 (5)
H3	0.5128	0.3068	0.4233	0.072*
C4	0.47501 (11)	0.33551 (12)	0.6343 (2)	0.0589 (5)
H4	0.4246	0.3061	0.6235	0.071*
C5	0.44087 (11)	0.37873 (12)	0.9042 (2)	0.0579 (5)
H5	0.4658	0.3954	0.9984	0.069*
C6	0.36029 (10)	0.35861 (11)	0.9045 (2)	0.0549 (4)
H6	0.3349	0.3419	0.8107	0.066*
C7	0.34099 (11)	0.36330 (13)	1.1917 (2)	0.0619 (5)
H7	0.3985	0.3681	1.2100	0.074*
C8	0.28980 (12)	0.35921 (12)	1.3126 (2)	0.0622 (5)
H8	0.3135	0.3588	1.4126	0.075*
C9	0.14999 (13)	0.34211 (11)	1.4185 (2)	0.0590 (5)
H9	0.1733	0.3426	1.5188	0.071*
C10	0.06775 (12)	0.32867 (11)	1.3944 (2)	0.0595 (5)
H10	0.0357	0.3134	1.4770	0.071*
C11	−0.05944 (12)	0.32435 (12)	1.2248 (3)	0.0651 (5)
H11	−0.0893	0.3062	1.3084	0.078*
C12	−0.10022 (12)	0.33771 (13)	1.0881 (3)	0.0658 (5)
H12	−0.1568	0.3245	1.0764	0.079*
C13	−0.10287 (12)	0.39500 (13)	0.8243 (2)	0.0674 (5)
H13	−0.1598	0.3830	0.8141	0.081*
C14	−0.06522 (13)	0.43440 (13)	0.7065 (2)	0.0695 (5)
H14	−0.0956	0.4478	0.6157	0.083*
C15	0.01929 (12)	0.45446 (12)	0.7234 (2)	0.0601 (5)
H15	0.0450	0.4834	0.6448	0.072*
C16	0.06517 (11)	0.43218 (11)	0.85410 (19)	0.0508 (4)
H16	0.1214	0.4475	0.8633	0.061*
C17	0.02965 (10)	0.38653 (10)	0.97573 (19)	0.0457 (4)
C18	−0.05815 (11)	0.37167 (11)	0.9616 (2)	0.0548 (5)
C19	0.07512 (10)	0.36146 (10)	1.11728 (19)	0.0458 (4)
C20	0.02833 (11)	0.33737 (10)	1.2444 (2)	0.0520 (4)
C21	0.16562 (10)	0.36058 (10)	1.13855 (19)	0.0457 (4)
C22	0.20204 (11)	0.35564 (11)	1.2912 (2)	0.0518 (4)
C23	0.22144 (10)	0.35824 (10)	1.01601 (19)	0.0485 (4)
H23	0.1990	0.3552	0.9153	0.058*
C24	0.30721 (10)	0.36024 (11)	1.0387 (2)	0.0518 (4)
C25	0.57164 (11)	0.41926 (14)	0.7815 (2)	0.0666 (5)
H25	0.5880	0.4471	0.8726	0.080*
C26	0.49506 (10)	0.37763 (11)	0.7719 (2)	0.0521 (4)
C27	0.66384 (11)	0.37694 (12)	0.3880 (2)	0.0551 (5)
C28	0.61596 (16)	0.3800 (2)	0.2314 (3)	0.1036 (9)
H28A	0.6550	0.3811	0.1504	0.155*
H28B	0.5819	0.4304	0.2256	0.155*
H28C	0.5809	0.3306	0.2199	0.155*
C29	0.72353 (16)	0.4523 (2)	0.3911 (3)	0.1142 (10)
H29A	0.7583	0.4506	0.4843	0.171*
H29B	0.6920	0.5043	0.3876	0.171*
H29C	0.7580	0.4495	0.3034	0.171*
C30	0.71294 (17)	0.29478 (18)	0.3982 (3)	0.1261 (12)
H30A	0.7504	0.2921	0.3149	0.189*
H30B	0.6750	0.2474	0.3914	0.189*
H30C	0.7446	0.2926	0.4950	0.189*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0463 (10)	0.0802 (14)	0.0709 (13)	−0.0150 (9)	0.0091 (9)	−0.0137 (10)
C2	0.0398 (9)	0.0533 (10)	0.0548 (10)	0.0018 (7)	0.0044 (7)	0.0023 (8)
C3	0.0488 (10)	0.0737 (13)	0.0562 (11)	−0.0072 (9)	0.0017 (8)	−0.0057 (9)
C4	0.0399 (9)	0.0718 (12)	0.0650 (12)	−0.0086 (8)	0.0041 (8)	−0.0008 (10)
C5	0.0491 (10)	0.0663 (12)	0.0588 (11)	0.0044 (8)	0.0085 (8)	−0.0027 (9)
C6	0.0470 (10)	0.0599 (11)	0.0583 (11)	0.0061 (8)	0.0080 (8)	0.0016 (8)
C7	0.0481 (10)	0.0709 (13)	0.0665 (12)	0.0032 (9)	0.0018 (9)	0.0007 (10)
C8	0.0630 (12)	0.0704 (13)	0.0526 (11)	0.0056 (9)	−0.0027 (9)	−0.0006 (9)
C9	0.0771 (13)	0.0538 (11)	0.0466 (10)	0.0063 (9)	0.0101 (9)	0.0019 (8)
C10	0.0744 (13)	0.0508 (10)	0.0552 (11)	0.0010 (9)	0.0252 (10)	0.0050 (8)
C11	0.0614 (12)	0.0572 (12)	0.0792 (14)	−0.0091 (9)	0.0305 (10)	0.0030 (10)
C12	0.0491 (10)	0.0625 (12)	0.0870 (15)	−0.0139 (9)	0.0163 (10)	−0.0048 (11)
C13	0.0513 (11)	0.0674 (13)	0.0833 (15)	−0.0026 (9)	0.0004 (10)	−0.0104 (11)
C14	0.0682 (13)	0.0710 (14)	0.0685 (13)	0.0071 (10)	−0.0058 (11)	−0.0037 (10)
C15	0.0642 (12)	0.0607 (12)	0.0559 (11)	0.0086 (9)	0.0088 (9)	−0.0007 (9)
C16	0.0487 (9)	0.0494 (10)	0.0553 (10)	0.0043 (7)	0.0116 (8)	−0.0032 (8)
C17	0.0453 (9)	0.0401 (9)	0.0525 (10)	0.0007 (7)	0.0118 (7)	−0.0072 (7)
C18	0.0501 (10)	0.0470 (10)	0.0679 (12)	−0.0019 (8)	0.0108 (9)	−0.0097 (8)
C19	0.0503 (9)	0.0367 (8)	0.0517 (10)	−0.0017 (7)	0.0146 (8)	−0.0043 (7)
C20	0.0596 (11)	0.0401 (9)	0.0579 (11)	−0.0009 (8)	0.0212 (9)	−0.0009 (8)
C21	0.0508 (9)	0.0381 (8)	0.0491 (9)	0.0001 (7)	0.0116 (7)	−0.0020 (7)
C22	0.0604 (11)	0.0449 (9)	0.0508 (10)	0.0038 (8)	0.0098 (8)	−0.0005 (7)
C23	0.0478 (9)	0.0494 (10)	0.0491 (9)	0.0020 (7)	0.0087 (7)	−0.0010 (7)
C24	0.0480 (10)	0.0510 (10)	0.0569 (11)	0.0043 (8)	0.0085 (8)	0.0009 (8)
C25	0.0531 (11)	0.0838 (14)	0.0636 (12)	−0.0119 (10)	0.0089 (9)	−0.0186 (10)
C26	0.0394 (9)	0.0582 (11)	0.0590 (11)	0.0056 (7)	0.0050 (8)	0.0008 (8)
C27	0.0469 (9)	0.0634 (12)	0.0554 (11)	−0.0012 (8)	0.0073 (8)	0.0031 (8)
C28	0.0852 (17)	0.161 (3)	0.0653 (15)	−0.0060 (17)	0.0125 (13)	0.0034 (15)
C29	0.112 (2)	0.137 (2)	0.0974 (18)	−0.0621 (18)	0.0466 (16)	−0.0227 (17)
C30	0.122 (2)	0.113 (2)	0.150 (3)	0.0576 (18)	0.086 (2)	0.0428 (19)

Geometric parameters (Å, º)

C1—C25	1.380 (2)	C13—C18	1.409 (3)
C1—C2	1.385 (2)	C13—H13	0.9300
C1—H1	0.9300	C14—C15	1.389 (3)
C2—C3	1.390 (2)	C14—H14	0.9300
C2—C27	1.531 (2)	C15—C16	1.367 (2)
C3—C4	1.380 (2)	C15—H15	0.9300
C3—H3	0.9300	C16—C17	1.415 (2)
C4—C26	1.389 (2)	C16—H16	0.9300
C4—H4	0.9300	C17—C18	1.423 (2)
C5—C6	1.327 (2)	C17—C19	1.452 (2)
C5—C26	1.467 (2)	C19—C20	1.411 (2)
C5—H5	0.9300	C19—C21	1.451 (2)
C6—C24	1.470 (2)	C21—C23	1.418 (2)
C6—H6	0.9300	C21—C22	1.423 (2)
C7—C8	1.359 (2)	C23—C24	1.377 (2)
C7—C24	1.410 (3)	C23—H23	0.9300
C7—H7	0.9300	C25—C26	1.388 (2)
C8—C22	1.408 (2)	C25—H25	0.9300
C8—H8	0.9300	C27—C30	1.511 (3)
C9—C10	1.339 (3)	C27—C29	1.520 (3)
C9—C22	1.427 (2)	C27—C28	1.529 (3)
C9—H9	0.9300	C28—H28A	0.9600
C10—C20	1.425 (2)	C28—H28B	0.9600
C10—H10	0.9300	C28—H28C	0.9600
C11—C12	1.343 (3)	C29—H29A	0.9600
C11—C20	1.421 (3)	C29—H29B	0.9600
C11—H11	0.9300	C29—H29C	0.9600
C12—C18	1.416 (3)	C30—H30A	0.9600
C12—H12	0.9300	C30—H30B	0.9600
C13—C14	1.357 (3)	C30—H30C	0.9600
C25—C1—C2	122.03 (17)	C13—C18—C12	120.73 (17)
C25—C1—H1	119.0	C13—C18—C17	119.45 (17)
C2—C1—H1	119.0	C12—C18—C17	119.73 (18)
C1—C2—C3	116.03 (16)	C20—C19—C21	117.32 (15)
C1—C2—C27	122.41 (15)	C20—C19—C17	117.99 (15)
C3—C2—C27	121.44 (16)	C21—C19—C17	124.68 (14)
C4—C3—C2	122.19 (17)	C19—C20—C11	120.02 (17)
C4—C3—H3	118.9	C19—C20—C10	120.61 (16)
C2—C3—H3	118.9	C11—C20—C10	119.33 (16)
C3—C4—C26	121.47 (16)	C23—C21—C22	116.69 (15)
C3—C4—H4	119.3	C23—C21—C19	124.25 (15)
C26—C4—H4	119.3	C22—C21—C19	118.90 (14)
C6—C5—C26	127.29 (18)	C8—C22—C21	118.99 (16)
C6—C5—H5	116.4	C8—C22—C9	121.05 (17)
C26—C5—H5	116.4	C21—C22—C9	119.86 (16)
C5—C6—C24	126.31 (18)	C24—C23—C21	123.26 (16)
C5—C6—H6	116.8	C24—C23—H23	118.4
C24—C6—H6	116.8	C21—C23—H23	118.4
C8—C7—C24	120.28 (17)	C23—C24—C7	118.21 (16)
C8—C7—H7	119.9	C23—C24—C6	119.52 (16)
C24—C7—H7	119.9	C7—C24—C6	122.27 (16)
C7—C8—C22	122.08 (18)	C1—C25—C26	121.79 (18)
C7—C8—H8	119.0	C1—C25—H25	119.1
C22—C8—H8	119.0	C26—C25—H25	119.1
C10—C9—C22	120.32 (17)	C25—C26—C4	116.45 (16)
C10—C9—H9	119.8	C25—C26—C5	119.86 (17)
C22—C9—H9	119.8	C4—C26—C5	123.68 (16)
C9—C10—C20	121.26 (16)	C30—C27—C29	109.9 (2)
C9—C10—H10	119.4	C30—C27—C28	108.5 (2)
C20—C10—H10	119.4	C29—C27—C28	106.29 (19)
C12—C11—C20	121.43 (17)	C30—C27—C2	108.60 (15)
C12—C11—H11	119.3	C29—C27—C2	112.19 (16)
C20—C11—H11	119.3	C28—C27—C2	111.31 (15)
C11—C12—C18	120.86 (17)	C27—C28—H28A	109.5
C11—C12—H12	119.6	C27—C28—H28B	109.5
C18—C12—H12	119.6	H28A—C28—H28B	109.5
C14—C13—C18	121.88 (18)	C27—C28—H28C	109.5
C14—C13—H13	119.1	H28A—C28—H28C	109.5
C18—C13—H13	119.1	H28B—C28—H28C	109.5
C13—C14—C15	119.10 (19)	C27—C29—H29A	109.5
C13—C14—H14	120.4	C27—C29—H29B	109.5
C15—C14—H14	120.5	H29A—C29—H29B	109.5
C16—C15—C14	120.85 (18)	C27—C29—H29C	109.5
C16—C15—H15	119.6	H29A—C29—H29C	109.5
C14—C15—H15	119.6	H29B—C29—H29C	109.5
C15—C16—C17	121.91 (16)	C27—C30—H30A	109.5
C15—C16—H16	119.0	C27—C30—H30B	109.5
C17—C16—H16	119.0	H30A—C30—H30B	109.5
C16—C17—C18	116.50 (16)	C27—C30—H30C	109.5
C16—C17—C19	124.35 (15)	H30A—C30—H30C	109.5
C18—C17—C19	118.90 (15)	H30B—C30—H30C	109.5
C25—C1—C2—C3	−0.8 (3)	C20—C19—C21—C23	160.70 (15)
C25—C1—C2—C27	−176.94 (18)	C17—C19—C21—C23	−20.3 (2)
C1—C2—C3—C4	1.5 (3)	C20—C19—C21—C22	−14.6 (2)
C27—C2—C3—C4	177.66 (17)	C17—C19—C21—C22	164.41 (15)
C2—C3—C4—C26	−0.7 (3)	C7—C8—C22—C21	−3.1 (3)
C26—C5—C6—C24	−179.97 (17)	C7—C8—C22—C9	173.15 (18)
C24—C7—C8—C22	−2.9 (3)	C23—C21—C22—C8	7.6 (2)
C22—C9—C10—C20	−7.5 (3)	C19—C21—C22—C8	−176.76 (15)
C20—C11—C12—C18	−5.0 (3)	C23—C21—C22—C9	−168.67 (15)
C18—C13—C14—C15	−1.8 (3)	C19—C21—C22—C9	7.0 (2)
C13—C14—C15—C16	2.5 (3)	C10—C9—C22—C8	−171.95 (17)
C14—C15—C16—C17	1.4 (3)	C10—C9—C22—C21	4.2 (3)
C15—C16—C17—C18	−5.6 (2)	C22—C21—C23—C24	−6.8 (2)
C15—C16—C17—C19	−179.74 (16)	C19—C21—C23—C24	177.82 (15)
C14—C13—C18—C12	174.21 (19)	C21—C23—C24—C7	1.1 (3)
C14—C13—C18—C17	−2.6 (3)	C21—C23—C24—C6	−179.25 (15)
C11—C12—C18—C13	−172.47 (19)	C8—C7—C24—C23	3.9 (3)
C11—C12—C18—C17	4.3 (3)	C8—C7—C24—C6	−175.77 (18)
C16—C17—C18—C13	6.1 (2)	C5—C6—C24—C23	164.10 (18)
C19—C17—C18—C13	−179.43 (15)	C5—C6—C24—C7	−16.3 (3)
C16—C17—C18—C12	−170.75 (16)	C2—C1—C25—C26	−0.7 (3)
C19—C17—C18—C12	3.8 (2)	C1—C25—C26—C4	1.5 (3)
C16—C17—C19—C20	163.10 (15)	C1—C25—C26—C5	−179.41 (18)
C18—C17—C19—C20	−10.9 (2)	C3—C4—C26—C25	−0.8 (3)
C16—C17—C19—C21	−15.9 (2)	C3—C4—C26—C5	−179.88 (17)
C18—C17—C19—C21	170.05 (15)	C6—C5—C26—C25	164.57 (19)
C21—C19—C20—C11	−170.42 (15)	C6—C5—C26—C4	−16.4 (3)
C17—C19—C20—C11	10.5 (2)	C1—C2—C27—C30	95.3 (2)
C21—C19—C20—C10	11.7 (2)	C3—C2—C27—C30	−80.6 (2)
C17—C19—C20—C10	−167.35 (15)	C1—C2—C27—C29	−26.3 (3)
C12—C11—C20—C19	−2.7 (3)	C3—C2—C27—C29	157.8 (2)
C12—C11—C20—C10	175.21 (18)	C1—C2—C27—C28	−145.3 (2)
C9—C10—C20—C19	−0.7 (3)	C3—C2—C27—C28	38.8 (3)
C9—C10—C20—C11	−178.60 (17)

Trans-1-(para-tert-butylphenyl)-2-(2-benzo[c]phenanthrenyl)ethylene (VIId)

Crystal data

C30H26	F(000) = 824
Mr = 386.51	Dx = 1.182 Mg m^−3
Monoclinic, p_21/c	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -p_2ybc	Cell parameters from 4797 reflections
a = 15.9882 (3) Å	θ = 2.8–63.7°
b = 15.7045 (3) Å	µ = 0.50 mm^−1
c = 8.6555 (2) Å	T = 296 K
β = 92.549 (1)°	Rod, colourless
V = 2171.13 (8) Å^3	0.60 × 0.20 × 0.20 mm
Z = 4

Data collection

CCD area detector diffractometer	3354 independent reflections
Radiation source: fine-focus sealed tube	2528 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.032
phi and ω scans	θmax = 64.7°, θmin = 2.8°
Absorption correction: multi-scan SADABS (Bruker)	h = −18→18
Tmin = 0.803, Tmax = 0.907	k = −16→18
11417 measured reflections	l = −8→10

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)] = 0.046	H-atom parameters constrained
wR(F^2) = 0.137	w = 1/[σ^2(Fo^2) + (0.0698P)^2 + 0.2621P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max < 0.001
3354 reflections	Δρmax = 0.29 e Å^−3
272 parameters	Δρmin = −0.21 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0015 (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
C1	0.62417 (12)	0.42062 (15)	0.6595 (2)	0.0691 (6)
H1	0.6747	0.4498	0.6706	0.083*
C2	0.60417 (10)	0.37973 (12)	0.5209 (2)	0.0536 (5)
C3	0.52814 (11)	0.33634 (14)	0.5126 (2)	0.0625 (5)
H3	0.5126	0.3071	0.4224	0.075*
C4	0.47510 (11)	0.33544 (13)	0.6342 (2)	0.0626 (5)
H4	0.4248	0.3058	0.6237	0.075*
C5	0.44099 (11)	0.37864 (13)	0.9039 (2)	0.0622 (5)
H5	0.4660	0.3950	0.9983	0.075*
C6	0.36031 (11)	0.35872 (12)	0.9041 (2)	0.0578 (5)
H6	0.3348	0.3422	0.8101	0.069*
C7	0.34079 (12)	0.36343 (14)	1.1915 (2)	0.0652 (5)
H7	0.3983	0.3685	1.2098	0.078*
C8	0.28995 (13)	0.35924 (13)	1.3123 (2)	0.0653 (5)
H8	0.3137	0.3587	1.4123	0.078*
C9	0.15037 (13)	0.34220 (13)	1.4187 (2)	0.0631 (5)
H9	0.1738	0.3427	1.5190	0.076*
C10	0.06777 (13)	0.32875 (12)	1.3941 (2)	0.0638 (5)
H10	0.0357	0.3135	1.4767	0.077*
C11	−0.05951 (13)	0.32447 (13)	1.2249 (3)	0.0687 (6)
H11	−0.0894	0.3065	1.3086	0.082*
C12	−0.10010 (12)	0.33770 (14)	1.0882 (3)	0.0692 (6)
H12	−0.1567	0.3243	1.0765	0.083*
C13	−0.10295 (12)	0.39511 (14)	0.8237 (3)	0.0704 (6)
H13	−0.1599	0.3833	0.8136	0.085*
C14	−0.06533 (13)	0.43433 (15)	0.7059 (3)	0.0731 (6)
H14	−0.0956	0.4475	0.6148	0.088*
C15	0.01926 (12)	0.45456 (13)	0.7233 (2)	0.0638 (5)
H15	0.0450	0.4838	0.6449	0.077*
C16	0.06494 (11)	0.43204 (12)	0.8537 (2)	0.0547 (5)
H16	0.1212	0.4472	0.8628	0.066*
C17	0.02957 (11)	0.38634 (11)	0.9757 (2)	0.0504 (4)
C18	−0.05829 (11)	0.37166 (12)	0.9612 (2)	0.0586 (5)
C19	0.07501 (11)	0.36138 (11)	1.1170 (2)	0.0499 (4)
C20	0.02854 (12)	0.33736 (11)	1.2445 (2)	0.0560 (5)
C21	0.16586 (11)	0.36066 (11)	1.1387 (2)	0.0496 (4)
C22	0.20186 (12)	0.35568 (12)	1.2912 (2)	0.0552 (5)
C23	0.22121 (11)	0.35810 (11)	1.0159 (2)	0.0521 (4)
H23	0.1987	0.3548	0.9151	0.063*
C24	0.30728 (11)	0.36026 (12)	1.0389 (2)	0.0552 (5)
C25	0.57164 (12)	0.41944 (15)	0.7812 (3)	0.0710 (6)
H25	0.5879	0.4473	0.8724	0.085*
C26	0.49497 (11)	0.37774 (12)	0.7717 (2)	0.0562 (5)
C27	0.66379 (11)	0.37705 (13)	0.3878 (2)	0.0595 (5)
C28	0.61602 (17)	0.3799 (2)	0.2310 (3)	0.1063 (10)
H28A	0.6550	0.3781	0.1499	0.159*
H28B	0.5841	0.4316	0.2229	0.159*
H28C	0.5790	0.3319	0.2217	0.159*
C29	0.72360 (18)	0.4522 (2)	0.3908 (3)	0.1178 (11)
H29A	0.7600	0.4479	0.3058	0.177*
H29B	0.7564	0.4521	0.4864	0.177*
H29C	0.6922	0.5043	0.3821	0.177*
C30	0.71286 (18)	0.2947 (2)	0.3980 (4)	0.1299 (13)
H30A	0.7506	0.2921	0.3149	0.195*
H30B	0.6749	0.2473	0.3905	0.195*
H30C	0.7442	0.2923	0.4952	0.195*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0497 (10)	0.0843 (16)	0.0737 (15)	−0.0140 (10)	0.0076 (10)	−0.0132 (11)
C2	0.0437 (9)	0.0579 (12)	0.0591 (12)	0.0020 (8)	0.0033 (8)	0.0013 (8)
C3	0.0509 (10)	0.0783 (14)	0.0582 (13)	−0.0070 (9)	0.0014 (9)	−0.0069 (9)
C4	0.0431 (9)	0.0770 (14)	0.0678 (14)	−0.0073 (9)	0.0044 (9)	−0.0008 (10)
C5	0.0528 (11)	0.0700 (14)	0.0642 (13)	0.0034 (9)	0.0083 (9)	−0.0026 (9)
C6	0.0510 (10)	0.0629 (13)	0.0600 (13)	0.0070 (9)	0.0074 (9)	0.0026 (8)
C7	0.0534 (11)	0.0742 (14)	0.0678 (14)	0.0041 (10)	0.0011 (10)	0.0009 (10)
C8	0.0688 (12)	0.0722 (14)	0.0546 (13)	0.0060 (10)	−0.0022 (10)	0.0003 (9)
C9	0.0806 (14)	0.0591 (13)	0.0505 (12)	0.0073 (10)	0.0112 (10)	0.0024 (8)
C10	0.0787 (13)	0.0553 (12)	0.0595 (13)	0.0017 (10)	0.0256 (11)	0.0056 (8)
C11	0.0642 (12)	0.0619 (13)	0.0823 (16)	−0.0102 (10)	0.0290 (11)	0.0042 (10)
C12	0.0539 (11)	0.0674 (14)	0.0875 (17)	−0.0131 (10)	0.0149 (11)	−0.0045 (11)
C13	0.0549 (11)	0.0698 (15)	0.0861 (17)	−0.0012 (10)	−0.0026 (11)	−0.0107 (11)
C14	0.0715 (13)	0.0773 (16)	0.0697 (15)	0.0064 (11)	−0.0047 (11)	−0.0027 (10)
C15	0.0680 (12)	0.0650 (13)	0.0588 (13)	0.0089 (10)	0.0082 (10)	0.0003 (9)
C16	0.0522 (10)	0.0555 (12)	0.0573 (12)	0.0044 (8)	0.0115 (9)	−0.0022 (8)
C17	0.0504 (9)	0.0462 (10)	0.0552 (11)	0.0018 (8)	0.0109 (8)	−0.0069 (7)
C18	0.0544 (10)	0.0510 (12)	0.0712 (14)	−0.0024 (9)	0.0109 (9)	−0.0090 (8)
C19	0.0551 (10)	0.0404 (10)	0.0554 (11)	−0.0015 (8)	0.0144 (8)	−0.0052 (7)
C20	0.0627 (11)	0.0459 (11)	0.0609 (13)	−0.0002 (9)	0.0194 (9)	−0.0006 (8)
C21	0.0548 (10)	0.0422 (10)	0.0525 (11)	0.0000 (8)	0.0108 (8)	−0.0015 (7)
C22	0.0644 (11)	0.0499 (11)	0.0519 (12)	0.0055 (9)	0.0088 (9)	0.0002 (8)
C23	0.0528 (10)	0.0531 (11)	0.0509 (11)	0.0019 (8)	0.0082 (8)	−0.0014 (7)
C24	0.0522 (10)	0.0540 (12)	0.0598 (12)	0.0040 (8)	0.0087 (9)	0.0014 (8)
C25	0.0563 (11)	0.0911 (17)	0.0664 (14)	−0.0141 (11)	0.0101 (10)	−0.0186 (11)
C26	0.0442 (9)	0.0632 (13)	0.0617 (13)	0.0059 (8)	0.0063 (8)	0.0017 (9)
C27	0.0495 (10)	0.0690 (13)	0.0605 (13)	−0.0019 (9)	0.0071 (9)	0.0027 (9)
C28	0.0875 (17)	0.165 (3)	0.0671 (17)	−0.0071 (17)	0.0105 (14)	0.0025 (16)
C29	0.117 (2)	0.140 (3)	0.101 (2)	−0.060 (2)	0.0457 (18)	−0.0212 (18)
C30	0.126 (2)	0.117 (3)	0.154 (3)	0.057 (2)	0.086 (2)	0.042 (2)

Geometric parameters (Å, º)

C1—C25	1.376 (3)	C13—C18	1.409 (3)
C1—C2	1.385 (3)	C13—H13	0.9300
C1—H1	0.9300	C14—C15	1.391 (3)
C2—C3	1.393 (2)	C14—H14	0.9300
C2—C27	1.529 (3)	C15—C16	1.364 (3)
C3—C4	1.381 (3)	C15—H15	0.9300
C3—H3	0.9300	C16—C17	1.415 (2)
C4—C26	1.387 (3)	C16—H16	0.9300
C4—H4	0.9300	C17—C18	1.424 (2)
C5—C6	1.327 (3)	C17—C19	1.449 (3)
C5—C26	1.464 (3)	C19—C20	1.408 (2)
C5—H5	0.9300	C19—C21	1.456 (2)
C6—C24	1.473 (3)	C21—C23	1.413 (2)
C6—H6	0.9300	C21—C22	1.419 (3)
C7—C8	1.354 (3)	C23—C24	1.382 (2)
C7—C24	1.404 (3)	C23—H23	0.9300
C7—H7	0.9300	C25—C26	1.389 (3)
C8—C22	1.413 (3)	C25—H25	0.9300
C8—H8	0.9300	C27—C30	1.514 (3)
C9—C10	1.345 (3)	C27—C29	1.519 (3)
C9—C22	1.422 (3)	C27—C28	1.528 (3)
C9—H9	0.9300	C28—H28A	0.9600
C10—C20	1.420 (3)	C28—H28B	0.9600
C10—H10	0.9300	C28—H28C	0.9600
C11—C12	1.340 (3)	C29—H29A	0.9600
C11—C20	1.425 (3)	C29—H29B	0.9600
C11—H11	0.9300	C29—H29C	0.9600
C12—C18	1.416 (3)	C30—H30A	0.9600
C12—H12	0.9300	C30—H30B	0.9600
C13—C14	1.355 (3)	C30—H30C	0.9600
C25—C1—C2	122.09 (18)	C13—C18—C12	120.99 (18)
C25—C1—H1	119.0	C13—C18—C17	119.55 (18)
C2—C1—H1	119.0	C12—C18—C17	119.39 (19)
C1—C2—C3	116.02 (18)	C20—C19—C17	118.13 (16)
C1—C2—C27	122.55 (16)	C20—C19—C21	117.08 (17)
C3—C2—C27	121.32 (17)	C17—C19—C21	124.78 (16)
C4—C3—C2	122.01 (19)	C19—C20—C10	120.83 (17)
C4—C3—H3	119.0	C19—C20—C11	119.85 (19)
C2—C3—H3	119.0	C10—C20—C11	119.28 (18)
C3—C4—C26	121.59 (18)	C23—C21—C22	117.15 (16)
C3—C4—H4	119.2	C23—C21—C19	123.91 (17)
C26—C4—H4	119.2	C22—C21—C19	118.75 (16)
C6—C5—C26	127.3 (2)	C8—C22—C21	118.61 (17)
C6—C5—H5	116.4	C8—C22—C9	120.91 (19)
C26—C5—H5	116.4	C21—C22—C9	120.37 (18)
C5—C6—C24	126.2 (2)	C24—C23—C21	122.94 (18)
C5—C6—H6	116.9	C24—C23—H23	118.5
C24—C6—H6	116.9	C21—C23—H23	118.5
C8—C7—C24	120.50 (18)	C23—C24—C7	118.16 (17)
C8—C7—H7	119.8	C23—C24—C6	119.36 (18)
C24—C7—H7	119.8	C7—C24—C6	122.48 (17)
C7—C8—C22	122.1 (2)	C1—C25—C26	121.9 (2)
C7—C8—H8	118.9	C1—C25—H25	119.1
C22—C8—H8	118.9	C26—C25—H25	119.1
C10—C9—C22	119.9 (2)	C4—C26—C25	116.40 (18)
C10—C9—H9	120.0	C4—C26—C5	123.69 (17)
C22—C9—H9	120.0	C25—C26—C5	119.90 (19)
C9—C10—C20	121.36 (18)	C30—C27—C29	109.8 (2)
C9—C10—H10	119.3	C30—C27—C28	108.4 (2)
C20—C10—H10	119.3	C29—C27—C28	106.4 (2)
C12—C11—C20	121.34 (19)	C30—C27—C2	108.55 (17)
C12—C11—H11	119.3	C29—C27—C2	112.26 (18)
C20—C11—H11	119.3	C28—C27—C2	111.41 (16)
C11—C12—C18	121.12 (18)	C27—C28—H28A	109.5
C11—C12—H12	119.4	C27—C28—H28B	109.5
C18—C12—H12	119.4	H28A—C28—H28B	109.5
C14—C13—C18	121.94 (19)	C27—C28—H28C	109.5
C14—C13—H13	119.0	H28A—C28—H28C	109.5
C18—C13—H13	119.0	H28B—C28—H28C	109.5
C13—C14—C15	119.0 (2)	C27—C29—H29A	109.5
C13—C14—H14	120.5	C27—C29—H29B	109.5
C15—C14—H14	120.5	H29A—C29—H29B	109.5
C16—C15—C14	120.8 (2)	C27—C29—H29C	109.5
C16—C15—H15	119.6	H29A—C29—H29C	109.5
C14—C15—H15	119.6	H29B—C29—H29C	109.5
C15—C16—C17	122.15 (18)	C27—C30—H30A	109.5
C15—C16—H16	118.9	C27—C30—H30B	109.5
C17—C16—H16	118.9	H30A—C30—H30B	109.5
C16—C17—C18	116.21 (18)	C27—C30—H30C	109.5
C16—C17—C19	124.42 (16)	H30A—C30—H30C	109.5
C18—C17—C19	119.11 (17)	H30B—C30—H30C	109.5
C25—C1—C2—C3	−0.8 (3)	C20—C19—C21—C23	160.59 (17)
C25—C1—C2—C27	−177.0 (2)	C17—C19—C21—C23	−20.6 (3)
C1—C2—C3—C4	1.2 (3)	C20—C19—C21—C22	−14.4 (2)
C27—C2—C3—C4	177.45 (18)	C17—C19—C21—C22	164.45 (16)
C2—C3—C4—C26	−0.1 (3)	C7—C8—C22—C21	−3.0 (3)
C26—C5—C6—C24	−179.90 (18)	C7—C8—C22—C9	173.25 (19)
C24—C7—C8—C22	−3.1 (3)	C23—C21—C22—C8	7.8 (2)
C22—C9—C10—C20	−7.4 (3)	C19—C21—C22—C8	−176.92 (17)
C20—C11—C12—C18	−5.2 (3)	C23—C21—C22—C9	−168.47 (17)
C18—C13—C14—C15	−2.2 (3)	C19—C21—C22—C9	6.8 (3)
C13—C14—C15—C16	3.0 (3)	C10—C9—C22—C8	−171.96 (19)
C14—C15—C16—C17	1.0 (3)	C10—C9—C22—C21	4.2 (3)
C15—C16—C17—C18	−5.4 (3)	C22—C21—C23—C24	−7.1 (3)
C15—C16—C17—C19	−179.54 (17)	C19—C21—C23—C24	177.83 (17)
C14—C13—C18—C12	174.3 (2)	C21—C23—C24—C7	1.3 (3)
C14—C13—C18—C17	−2.5 (3)	C21—C23—C24—C6	−179.02 (17)
C11—C12—C18—C13	−172.3 (2)	C8—C7—C24—C23	3.9 (3)
C11—C12—C18—C17	4.5 (3)	C8—C7—C24—C6	−175.73 (19)
C16—C17—C18—C13	6.0 (3)	C5—C6—C24—C23	164.4 (2)
C19—C17—C18—C13	−179.51 (17)	C5—C6—C24—C7	−15.9 (3)
C16—C17—C18—C12	−170.76 (18)	C2—C1—C25—C26	−0.6 (4)
C19—C17—C18—C12	3.7 (3)	C3—C4—C26—C25	−1.3 (3)
C16—C17—C19—C20	163.03 (17)	C3—C4—C26—C5	−179.92 (19)
C18—C17—C19—C20	−10.9 (2)	C1—C25—C26—C4	1.6 (3)
C16—C17—C19—C21	−15.8 (3)	C1—C25—C26—C5	−179.7 (2)
C18—C17—C19—C21	170.25 (16)	C6—C5—C26—C4	−17.0 (3)
C17—C19—C20—C10	−167.30 (16)	C6—C5—C26—C25	164.3 (2)
C21—C19—C20—C10	11.6 (2)	C1—C2—C27—C30	95.4 (3)
C17—C19—C20—C11	10.4 (3)	C3—C2—C27—C30	−80.7 (3)
C21—C19—C20—C11	−170.71 (17)	C1—C2—C27—C29	−26.2 (3)
C9—C10—C20—C19	−0.8 (3)	C3—C2—C27—C29	157.8 (2)
C9—C10—C20—C11	−178.48 (19)	C1—C2—C27—C28	−145.4 (2)
C12—C11—C20—C19	−2.4 (3)	C3—C2—C27—C28	38.6 (3)
C12—C11—C20—C10	175.3 (2)