# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jerry L. Atwood' _publ_contact_author_address ; Chemistry University of Missouri - Columbia 125 Chemistry Columbia MO UNITED STATES OF AMERICA ; _publ_contact_author_email ATWOODJ@MISSOURI.EDU _publ_section_title ; Organic crystals absorb hydrogen gas under mild conditions ; loop_ _publ_author_name 'Praveen Kumar Thallapally' 'Gareth O. Lloyd' 'Trevor B. Wirsig' 'Martin W. Bredenkamp' ; J.L.Atwood ; 'Leonard J. Barbour' data_D:\Structures\Octyl\OCTYL.CIF _database_code_depnum_ccdc_archive 'CCDC 280984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Octyl _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H88 O4' _chemical_formula_weight 873.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3633(17) _cell_length_b 38.624(6) _cell_length_c 12.6614(19) _cell_angle_alpha 90.00 _cell_angle_beta 101.881(2) _cell_angle_gamma 90.00 _cell_volume 5438.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9841 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47813 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.14 _reflns_number_total 12034 _reflns_number_gt 6101 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material SHELX-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two of the tert-octyl groups are disordered over two positions each. For each of the disordered groups, the site occupancies of the atoms in each disordered set were assigned a common value which was refined with the sum for the two sets constrained to equal unity. The final refined site occupancies are: C(9B).C(15B), 0.66; C(9E).C(15E), 0.34; C(9C).C(15C), 0.64; C(9F).C(15F), 0.36. The hydroxyl hydrogen atoms were also modelled as disordered and two possibilities are chemically feasible. The hydrogen atoms are involved in a cyclic hydrogen bonded arrangement about the lower rim of the calixarene. For a given calixarene molecule, the four hydrogen atoms must all be directed in the same direction about the hydrogen bonded ring and their site occupancies must therefore be the same. Thus the site occupancies of two orientations were refined with their sum constrained to equal unity. One orientation of the four hydrogen atoms refined to a value of 0.41 for its site occupancy while the second orientation has a value of 0.59. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12034 _refine_ls_number_parameters 738 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2142 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.90706(17) 0.13534(5) 0.42063(16) 0.0410(5) Uani 1 1 d D . . O1D O 0.72296(18) 0.15920(5) 0.50161(14) 0.0410(5) Uani 1 1 d D . . O1C O 0.69557(18) 0.21578(5) 0.37593(15) 0.0429(5) Uani 1 1 d D . . O1B O 0.87137(18) 0.19004(5) 0.28714(15) 0.0414(5) Uani 1 1 d D . . C2D C 0.5082(3) 0.15175(7) 0.4618(2) 0.0338(7) Uani 1 1 d . . . C2A C 0.8086(2) 0.07995(7) 0.4049(2) 0.0322(6) Uani 1 1 d . . . C1A C 0.8737(2) 0.10500(7) 0.3628(2) 0.0326(6) Uani 1 1 d D . . C6D C 0.6414(2) 0.10192(7) 0.49110(19) 0.0336(7) Uani 1 1 d . . . C1B C 0.8362(2) 0.18128(7) 0.1786(2) 0.0313(6) Uani 1 1 d D . . C6B C 0.7547(2) 0.20253(6) 0.1112(2) 0.0312(6) Uani 1 1 d . . . C5B C 0.7241(3) 0.19405(7) 0.0021(2) 0.0368(7) Uani 1 1 d . . . H5B H 0.6682 0.2083 -0.0446 0.044 Uiso 1 1 calc R . . C3A C 0.7791(2) 0.04943(7) 0.3458(2) 0.0351(7) Uani 1 1 d . . . H3A H 0.7345 0.0322 0.3740 0.042 Uiso 1 1 calc R . . C5D C 0.5399(3) 0.08060(7) 0.4749(2) 0.0338(7) Uani 1 1 d . . . H5D H 0.5512 0.0563 0.4813 0.041 Uiso 1 1 calc R . . C2C C 0.5832(3) 0.22348(6) 0.1941(2) 0.0336(7) Uani 1 1 d . . . C1D C 0.6237(3) 0.13751(7) 0.4842(2) 0.0341(7) Uani 1 1 d D . . C5A C 0.8771(2) 0.06947(7) 0.2095(2) 0.0362(7) Uani 1 1 d . . . H5A H 0.9012 0.0660 0.1427 0.043 Uiso 1 1 calc R . . C1C C 0.5865(3) 0.21421(6) 0.3011(2) 0.0339(7) Uani 1 1 d D . . C2B C 0.8862(2) 0.15236(7) 0.1396(2) 0.0340(7) Uani 1 1 d . . . C8D C 0.3123(3) 0.07015(7) 0.4207(2) 0.0386(7) Uani 1 1 d . . . C4D C 0.4230(2) 0.09343(7) 0.4497(2) 0.0329(6) Uani 1 1 d . . . C3B C 0.8524(3) 0.14503(7) 0.0300(2) 0.0389(7) Uani 1 1 d . . . H3B H 0.8857 0.1252 0.0028 0.047 Uiso 1 1 calc R . . C3D C 0.4111(3) 0.12938(7) 0.4452(2) 0.0332(7) Uani 1 1 d . . . H3D H 0.3324 0.1390 0.4301 0.040 Uiso 1 1 calc R . . C7B C 0.6965(2) 0.23321(7) 0.1535(2) 0.0359(7) Uani 1 1 d . . . H7B1 H 0.6754 0.2506 0.0954 0.043 Uiso 1 1 calc R . . H7B2 H 0.7551 0.2439 0.2133 0.043 Uiso 1 1 calc R . . C6A C 0.9082(2) 0.10043(7) 0.2644(2) 0.0338(7) Uani 1 1 d . . . C4A C 0.8123(2) 0.04316(7) 0.2474(2) 0.0333(7) Uani 1 1 d . . . C4C C 0.3668(3) 0.21144(7) 0.1510(2) 0.0388(7) Uani 1 1 d . B . C7D C 0.7651(2) 0.08565(7) 0.5096(2) 0.0355(7) Uani 1 1 d . . . H7D1 H 0.7632 0.0631 0.5466 0.043 Uiso 1 1 calc R . . H7D2 H 0.8230 0.1008 0.5577 0.043 Uiso 1 1 calc R . . C5C C 0.3761(3) 0.20232(7) 0.2599(2) 0.0398(7) Uani 1 1 d . . . H5C H 0.3057 0.1951 0.2832 0.048 Uiso 1 1 calc R . . C3C C 0.4728(3) 0.22235(7) 0.1222(2) 0.0371(7) Uani 1 1 d . . . H3C H 0.4694 0.2294 0.0497 0.045 Uiso 1 1 calc R . . C7A C 0.9716(3) 0.12834(7) 0.2137(2) 0.0404(7) Uani 1 1 d . . . H7A1 H 1.0260 0.1173 0.1720 0.048 Uiso 1 1 calc R . . H7A2 H 1.0217 0.1423 0.2718 0.048 Uiso 1 1 calc R . . C7C C 0.4885(3) 0.19070(7) 0.4501(2) 0.0393(7) Uani 1 1 d . . . H7C1 H 0.5542 0.2028 0.5000 0.047 Uiso 1 1 calc R . . H7C2 H 0.4119 0.1967 0.4713 0.047 Uiso 1 1 calc R . . C6C C 0.4844(3) 0.20346(7) 0.3352(2) 0.0366(7) Uani 1 1 d . . . C4B C 0.7719(3) 0.16550(7) -0.0415(2) 0.0396(7) Uani 1 1 d . A . C11D C 0.2554(3) 0.07382(8) 0.2989(2) 0.0397(7) Uani 1 1 d . . . H11A H 0.1886 0.0569 0.2836 0.048 Uiso 1 1 calc R . . H11B H 0.2178 0.0971 0.2898 0.048 Uiso 1 1 calc R . . C8C C 0.2486(3) 0.20816(8) 0.0672(3) 0.0459(8) Uani 1 1 d . . . C8A C 0.7777(3) 0.01058(7) 0.1799(2) 0.0402(7) Uani 1 1 d . . . C11A C 0.8892(3) -0.00820(8) 0.1544(2) 0.0425(7) Uani 1 1 d . . . H11C H 0.8591 -0.0238 0.0927 0.051 Uiso 1 1 calc R . . H11D H 0.9382 0.0097 0.1279 0.051 Uiso 1 1 calc R . . C12D C 0.3257(3) 0.06981(8) 0.2067(2) 0.0435(8) Uani 1 1 d . . . C10D C 0.3412(3) 0.03215(8) 0.4530(3) 0.0546(9) Uani 1 1 d . . . H10A H 0.2678 0.0182 0.4336 0.082 Uiso 1 1 calc R . . H10B H 0.3722 0.0308 0.5310 0.082 Uiso 1 1 calc R . . H10C H 0.4018 0.0233 0.4149 0.082 Uiso 1 1 calc R . . C8B C 0.7421(3) 0.15806(8) -0.1629(2) 0.0482(8) Uani 1 1 d . . . C9D C 0.2162(3) 0.08220(9) 0.4828(2) 0.0514(8) Uani 1 1 d . . . H9D1 H 0.1455 0.0671 0.4646 0.077 Uiso 1 1 calc R . . H9D2 H 0.1928 0.1061 0.4625 0.077 Uiso 1 1 calc R . . H9D3 H 0.2492 0.0810 0.5605 0.077 Uiso 1 1 calc R . . C9A C 0.7000(3) -0.01434(8) 0.2314(3) 0.0526(9) Uani 1 1 d . . . H9A1 H 0.6795 -0.0347 0.1850 0.079 Uiso 1 1 calc R . . H9A2 H 0.6261 -0.0025 0.2397 0.079 Uiso 1 1 calc R . . H9A3 H 0.7450 -0.0217 0.3024 0.079 Uiso 1 1 calc R . . C13A C 1.0069(3) -0.01216(8) 0.3501(3) 0.0572(9) Uani 1 1 d . . . H13A H 1.0377 0.0112 0.3425 0.086 Uiso 1 1 calc R . . H13B H 1.0681 -0.0258 0.3985 0.086 Uiso 1 1 calc R . . H13C H 0.9341 -0.0108 0.3801 0.086 Uiso 1 1 calc R . . C12A C 0.9767(3) -0.02976(8) 0.2383(3) 0.0455(8) Uani 1 1 d . . . C14A C 0.9290(3) -0.06618(8) 0.2498(3) 0.0575(9) Uani 1 1 d . . . H14A H 0.9861 -0.0789 0.3047 0.086 Uiso 1 1 calc R . . H14B H 0.9189 -0.0783 0.1806 0.086 Uiso 1 1 calc R . . H14C H 0.8512 -0.0647 0.2716 0.086 Uiso 1 1 calc R . . C10A C 0.7008(3) 0.02213(9) 0.0708(3) 0.0662(10) Uani 1 1 d . . . H10D H 0.6762 0.0018 0.0254 0.099 Uiso 1 1 calc R . . H10E H 0.7480 0.0377 0.0345 0.099 Uiso 1 1 calc R . . H10F H 0.6291 0.0343 0.0831 0.099 Uiso 1 1 calc R . . C14D C 0.4136(3) 0.09971(9) 0.2023(2) 0.0578(9) Uani 1 1 d . . . H14D H 0.3708 0.1218 0.2000 0.087 Uiso 1 1 calc R . . H14E H 0.4476 0.0974 0.1375 0.087 Uiso 1 1 calc R . . H14F H 0.4785 0.0990 0.2666 0.087 Uiso 1 1 calc R . . C13D C 0.3933(3) 0.03552(9) 0.2105(3) 0.0684(11) Uani 1 1 d . . . H13D H 0.3376 0.0163 0.2132 0.103 Uiso 1 1 calc R . . H13E H 0.4581 0.0349 0.2749 0.103 Uiso 1 1 calc R . . H13F H 0.4276 0.0333 0.1459 0.103 Uiso 1 1 calc R . . C13B C 0.5613(10) 0.1097(3) -0.0560(8) 0.0419(18) Uani 0.659(6) 1 d P A 1 H13G H 0.5546 0.1343 -0.0398 0.063 Uiso 0.659(6) 1 calc PR A 1 H13H H 0.6316 0.0999 -0.0074 0.063 Uiso 0.659(6) 1 calc PR A 1 H13I H 0.4886 0.0976 -0.0459 0.063 Uiso 0.659(6) 1 calc PR A 1 C15D C 0.2299(3) 0.07080(10) 0.1008(2) 0.0611(10) Uani 1 1 d . . . H15A H 0.1718 0.0521 0.1011 0.092 Uiso 1 1 calc R . . H15B H 0.2690 0.0679 0.0393 0.092 Uiso 1 1 calc R . . H15C H 0.1879 0.0931 0.0949 0.092 Uiso 1 1 calc R . . C14B C 0.5842(6) 0.06615(17) -0.1986(6) 0.0579(18) Uani 0.659(6) 1 d P A 1 H14G H 0.6556 0.0563 -0.1515 0.087 Uiso 0.659(6) 1 calc PR A 1 H14H H 0.5905 0.0633 -0.2742 0.087 Uiso 0.659(6) 1 calc PR A 1 H14I H 0.5121 0.0542 -0.1864 0.087 Uiso 0.659(6) 1 calc PR A 1 C11B C 0.6945(4) 0.12125(10) -0.1925(3) 0.0330(13) Uani 0.659(6) 1 d P A 1 H11E H 0.7588 0.1054 -0.1564 0.040 Uiso 0.659(6) 1 calc PR A 1 H11F H 0.6911 0.1188 -0.2709 0.040 Uiso 0.659(6) 1 calc PR A 1 C15A C 1.0930(3) -0.03353(10) 0.1957(3) 0.0735(11) Uani 1 1 d . . . H15D H 1.1265 -0.0105 0.1875 0.110 Uiso 1 1 calc R . . H15E H 1.0754 -0.0453 0.1256 0.110 Uiso 1 1 calc R . . H15F H 1.1513 -0.0472 0.2469 0.110 Uiso 1 1 calc R . . C11C C 0.2029(4) 0.24283(13) 0.0154(4) 0.0501(16) Uani 0.643(5) 1 d P B 3 H11G H 0.1436 0.2369 -0.0511 0.060 Uiso 0.643(5) 1 calc PR B 3 H11H H 0.2721 0.2535 -0.0086 0.060 Uiso 0.643(5) 1 calc PR B 3 C10B C 0.6409(6) 0.18462(14) -0.2257(4) 0.0615(18) Uani 0.659(6) 1 d P A 1 H10G H 0.5663 0.1816 -0.1993 0.092 Uiso 0.659(6) 1 calc PR A 1 H10H H 0.6257 0.1799 -0.3033 0.092 Uiso 0.659(6) 1 calc PR A 1 H10I H 0.6695 0.2085 -0.2123 0.092 Uiso 0.659(6) 1 calc PR A 1 C13C C 0.230(3) 0.2792(7) 0.1749(19) 0.161(14) Uani 0.643(5) 1 d P B 3 H13J H 0.1968 0.2970 0.2159 0.242 Uiso 0.643(5) 1 calc PR B 3 H13K H 0.3066 0.2873 0.1599 0.242 Uiso 0.643(5) 1 calc PR B 3 H13L H 0.2429 0.2578 0.2171 0.242 Uiso 0.643(5) 1 calc PR B 3 C12B C 0.5752(9) 0.1055(2) -0.1728(8) 0.0417(19) Uani 0.659(6) 1 d P A 1 C12C C 0.1439(10) 0.2726(4) 0.0713(13) 0.062(4) Uani 0.643(5) 1 d P B 3 C14C C 0.1403(9) 0.3043(2) -0.0018(10) 0.086(3) Uani 0.643(5) 1 d P B 3 H14J H 0.0887 0.2994 -0.0723 0.130 Uiso 0.643(5) 1 calc PR B 3 H14K H 0.2219 0.3097 -0.0112 0.130 Uiso 0.643(5) 1 calc PR B 3 H14L H 0.1081 0.3242 0.0313 0.130 Uiso 0.643(5) 1 calc PR B 3 C9C C 0.2745(5) 0.18403(15) -0.0232(4) 0.0613(18) Uani 0.643(5) 1 d P B 3 H9C1 H 0.2010 0.1812 -0.0786 0.092 Uiso 0.643(5) 1 calc PR B 3 H9C2 H 0.3013 0.1614 0.0076 0.092 Uiso 0.643(5) 1 calc PR B 3 H9C3 H 0.3375 0.1943 -0.0557 0.092 Uiso 0.643(5) 1 calc PR B 3 C15B C 0.4620(7) 0.11892(17) -0.2479(6) 0.0628(18) Uani 0.659(6) 1 d P A 1 H15G H 0.4524 0.1437 -0.2346 0.094 Uiso 0.659(6) 1 calc PR A 1 H15H H 0.3919 0.1063 -0.2342 0.094 Uiso 0.659(6) 1 calc PR A 1 H15I H 0.4689 0.1154 -0.3230 0.094 Uiso 0.659(6) 1 calc PR A 1 C9B C 0.8503(6) 0.16452(19) -0.2092(4) 0.069(2) Uani 0.659(6) 1 d P A 1 H9B1 H 0.8314 0.1595 -0.2867 0.104 Uiso 0.659(6) 1 calc PR A 1 H9B2 H 0.9161 0.1495 -0.1735 0.104 Uiso 0.659(6) 1 calc PR A 1 H9B3 H 0.8746 0.1888 -0.1977 0.104 Uiso 0.659(6) 1 calc PR A 1 C15C C 0.0130(8) 0.2651(2) 0.0763(11) 0.128(4) Uani 0.643(5) 1 d P B 3 H15J H -0.0322 0.2591 0.0040 0.192 Uiso 0.643(5) 1 calc PR B 3 H15K H -0.0227 0.2856 0.1026 0.192 Uiso 0.643(5) 1 calc PR B 3 H15L H 0.0100 0.2456 0.1254 0.192 Uiso 0.643(5) 1 calc PR B 3 C10C C 0.1490(5) 0.18994(15) 0.1158(5) 0.0575(17) Uani 0.643(5) 1 d P B 3 H10J H 0.0749 0.1882 0.0605 0.086 Uiso 0.643(5) 1 calc PR B 3 H10K H 0.1334 0.2035 0.1769 0.086 Uiso 0.643(5) 1 calc PR B 3 H10L H 0.1760 0.1667 0.1406 0.086 Uiso 0.643(5) 1 calc PR B 3 C9F C 0.2637(8) 0.2186(3) -0.0488(8) 0.057(3) Uani 0.357(5) 1 d P B 4 H9F1 H 0.3307 0.2055 -0.0673 0.085 Uiso 0.357(5) 1 calc PR B 4 H9F2 H 0.2805 0.2434 -0.0506 0.085 Uiso 0.357(5) 1 calc PR B 4 H9F3 H 0.1895 0.2133 -0.1010 0.085 Uiso 0.357(5) 1 calc PR B 4 C11F C 0.1471(9) 0.2284(3) 0.0986(8) 0.070(4) Uani 0.357(5) 1 d P B 4 H11I H 0.1395 0.2200 0.1708 0.084 Uiso 0.357(5) 1 calc PR B 4 H11J H 0.0724 0.2216 0.0477 0.084 Uiso 0.357(5) 1 calc PR B 4 C11E C 0.6169(12) 0.1516(3) -0.2035(7) 0.068(4) Uani 0.341(6) 1 d P A 2 H1 H 0.6068 0.1500 -0.2829 0.082 Uiso 0.341(6) 1 calc PR A 2 H2 H 0.5744 0.1729 -0.1892 0.082 Uiso 0.341(6) 1 calc PR A 2 C9E C 0.8263(11) 0.1249(3) -0.1855(7) 0.071(4) Uani 0.341(6) 1 d P A 2 H9E1 H 0.9109 0.1298 -0.1545 0.107 Uiso 0.341(6) 1 calc PR A 2 H9E2 H 0.8162 0.1212 -0.2634 0.107 Uiso 0.341(6) 1 calc PR A 2 H9E3 H 0.8015 0.1040 -0.1519 0.107 Uiso 0.341(6) 1 calc PR A 2 C10F C 0.2104(11) 0.1692(3) 0.0607(10) 0.083(4) Uani 0.357(5) 1 d P B 4 H10M H 0.2737 0.1552 0.0395 0.125 Uiso 0.357(5) 1 calc PR B 4 H10N H 0.1353 0.1664 0.0071 0.125 Uiso 0.357(5) 1 calc PR B 4 H10O H 0.1981 0.1615 0.1314 0.125 Uiso 0.357(5) 1 calc PR B 4 C10E C 0.7912(18) 0.1894(3) -0.2138(8) 0.100(7) Uani 0.341(6) 1 d P A 2 H3 H 0.8766 0.1924 -0.1813 0.150 Uiso 0.341(6) 1 calc PR A 2 H4 H 0.7467 0.2101 -0.2011 0.150 Uiso 0.341(6) 1 calc PR A 2 H5 H 0.7818 0.1856 -0.2916 0.150 Uiso 0.341(6) 1 calc PR A 2 C12E C 0.546(2) 0.1219(6) -0.1705(17) 0.076(6) Uani 0.341(6) 1 d P A 2 C13E C 0.551(3) 0.1212(7) -0.047(3) 0.126(13) Uani 0.341(6) 1 d P A 2 H6 H 0.6269 0.1111 -0.0095 0.190 Uiso 0.341(6) 1 calc PR A 2 H7 H 0.4836 0.1073 -0.0321 0.190 Uiso 0.341(6) 1 calc PR A 2 H8 H 0.5442 0.1449 -0.0208 0.190 Uiso 0.341(6) 1 calc PR A 2 C15E C 0.414(2) 0.1335(7) -0.2235(15) 0.162(11) Uani 0.341(6) 1 d P A 2 H9 H 0.3570 0.1159 -0.2097 0.244 Uiso 0.341(6) 1 calc PR A 2 H10 H 0.4069 0.1362 -0.3016 0.244 Uiso 0.341(6) 1 calc PR A 2 H11 H 0.3962 0.1556 -0.1923 0.244 Uiso 0.341(6) 1 calc PR A 2 C14E C 0.5700(18) 0.0867(5) -0.2153(16) 0.097(7) Uani 0.341(6) 1 d P A 2 H12 H 0.6457 0.0773 -0.1739 0.146 Uiso 0.341(6) 1 calc PR A 2 H13 H 0.5756 0.0891 -0.2912 0.146 Uiso 0.341(6) 1 calc PR A 2 H14 H 0.5040 0.0709 -0.2099 0.146 Uiso 0.341(6) 1 calc PR A 2 C14F C 0.0408(17) 0.2765(6) 0.1645(14) 0.128(7) Uani 0.357(5) 1 d P B 4 H14M H -0.0301 0.2630 0.1313 0.193 Uiso 0.357(5) 1 calc PR B 4 H14N H 0.0211 0.3013 0.1588 0.193 Uiso 0.357(5) 1 calc PR B 4 H14O H 0.0657 0.2702 0.2408 0.193 Uiso 0.357(5) 1 calc PR B 4 C13F C 0.246(3) 0.2869(10) 0.169(2) 0.072(6) Uani 0.357(5) 1 d PU B 4 H13M H 0.3200 0.2818 0.1438 0.108 Uiso 0.357(5) 1 calc PR B 4 H13N H 0.2544 0.2796 0.2440 0.108 Uiso 0.357(5) 1 calc PR B 4 H13O H 0.2298 0.3119 0.1630 0.108 Uiso 0.357(5) 1 calc PR B 4 C15F C 0.1058(18) 0.2853(5) -0.0096(17) 0.094(6) Uani 0.357(5) 1 d P B 4 H15M H 0.1711 0.2842 -0.0495 0.141 Uiso 0.357(5) 1 calc PR B 4 H15N H 0.0836 0.3095 -0.0014 0.141 Uiso 0.357(5) 1 calc PR B 4 H15O H 0.0359 0.2726 -0.0494 0.141 Uiso 0.357(5) 1 calc PR B 4 C12F C 0.148(4) 0.2687(7) 0.103(3) 0.096(11) Uani 0.357(5) 1 d P B 4 HA1 H 0.8487(14) 0.1372(5) 0.4678(16) 0.006(17) Uiso 0.41(5) 1 d PD C 5 HD1 H 0.6914(17) 0.1817(3) 0.4715(17) 0.006(17) Uiso 0.41(5) 1 d PD C 5 HB1 H 0.905(2) 0.1683(4) 0.3213(11) 0.021(19) Uiso 0.41(5) 1 d PD C 5 HC1 H 0.7561(9) 0.2150(6) 0.3299(15) 0.03(2) Uiso 0.41(5) 1 d PD C 5 HA1' H 0.7898(11) 0.1440(5) 0.492(2) 0.12(3) Uiso 0.59(5) 1 d PD C 6 HD1' H 0.7100(17) 0.1911(4) 0.3968(17) 0.26(6) Uiso 0.59(5) 1 d PD C 6 HC1' H 0.7937(14) 0.1910(7) 0.3112(14) 0.15(4) Uiso 0.59(5) 1 d PD C 6 HB1' H 0.922(2) 0.1516(3) 0.3637(14) 0.37(9) Uiso 0.59(5) 1 d PD C 6 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.0390(12) 0.0381(12) 0.0424(12) -0.0037(10) 0.0003(10) -0.0028(9) O1D 0.0489(13) 0.0417(12) 0.0303(11) -0.0049(9) 0.0031(9) -0.0034(11) O1C 0.0518(14) 0.0365(12) 0.0389(12) -0.0094(9) 0.0058(11) -0.0047(10) O1B 0.0446(13) 0.0405(12) 0.0346(11) -0.0048(9) -0.0020(10) -0.0033(10) C2D 0.0480(19) 0.0331(16) 0.0210(14) -0.0026(12) 0.0090(13) 0.0045(14) C2A 0.0295(15) 0.0361(16) 0.0274(15) 0.0039(12) -0.0024(12) 0.0038(12) C1A 0.0291(15) 0.0325(16) 0.0314(16) 0.0011(12) -0.0043(12) 0.0028(12) C6D 0.0418(17) 0.0396(17) 0.0175(14) 0.0027(12) 0.0013(12) 0.0016(14) C1B 0.0326(16) 0.0292(15) 0.0317(15) -0.0015(12) 0.0056(12) -0.0042(12) C6B 0.0369(16) 0.0228(14) 0.0357(16) 0.0004(12) 0.0115(13) -0.0052(12) C5B 0.0441(18) 0.0277(15) 0.0391(17) 0.0042(13) 0.0098(14) -0.0009(13) C3A 0.0346(16) 0.0364(17) 0.0328(16) 0.0068(13) 0.0034(13) 0.0022(13) C5D 0.0472(18) 0.0304(15) 0.0230(14) 0.0038(11) 0.0050(13) 0.0030(14) C2C 0.0450(18) 0.0187(14) 0.0401(17) -0.0009(12) 0.0158(14) 0.0037(12) C1D 0.0416(18) 0.0435(18) 0.0156(13) -0.0038(12) 0.0020(12) -0.0018(14) C5A 0.0374(17) 0.0383(17) 0.0333(16) 0.0032(13) 0.0078(13) 0.0101(13) C1C 0.0410(18) 0.0228(14) 0.0376(17) -0.0057(12) 0.0072(14) 0.0034(12) C2B 0.0353(16) 0.0268(15) 0.0426(18) 0.0072(13) 0.0141(13) 0.0010(12) C8D 0.0428(18) 0.0359(17) 0.0367(17) 0.0028(13) 0.0072(14) -0.0002(14) C4D 0.0416(17) 0.0347(16) 0.0218(14) 0.0027(12) 0.0053(12) 0.0018(13) C3B 0.0528(19) 0.0256(15) 0.0427(18) 0.0036(13) 0.0202(15) 0.0009(13) C3D 0.0417(17) 0.0353(16) 0.0218(14) 0.0015(12) 0.0047(12) 0.0054(13) C7B 0.0412(17) 0.0242(15) 0.0421(17) -0.0009(12) 0.0086(14) 0.0001(12) C6A 0.0286(15) 0.0333(16) 0.0387(17) 0.0079(13) 0.0051(13) 0.0080(12) C4A 0.0337(16) 0.0324(16) 0.0311(16) 0.0049(12) 0.0004(13) 0.0059(12) C4C 0.0420(18) 0.0301(16) 0.0455(18) 0.0070(13) 0.0118(15) 0.0042(13) C7D 0.0389(17) 0.0389(17) 0.0247(15) 0.0061(12) -0.0026(12) 0.0003(13) C5C 0.0426(19) 0.0329(16) 0.0479(19) 0.0059(14) 0.0184(16) 0.0045(14) C3C 0.0428(18) 0.0302(15) 0.0394(17) 0.0065(13) 0.0110(15) 0.0057(13) C7A 0.0385(17) 0.0346(16) 0.0507(19) 0.0061(14) 0.0150(15) 0.0066(14) C7C 0.0531(19) 0.0349(16) 0.0329(16) -0.0032(13) 0.0158(14) 0.0034(14) C6C 0.0510(19) 0.0248(15) 0.0385(17) -0.0023(12) 0.0198(15) 0.0062(13) C4B 0.061(2) 0.0266(16) 0.0354(17) 0.0027(13) 0.0188(15) -0.0054(14) C11D 0.0373(17) 0.0411(17) 0.0383(17) -0.0029(13) 0.0020(14) 0.0011(13) C8C 0.0364(18) 0.053(2) 0.0478(19) 0.0133(16) 0.0063(15) -0.0002(15) C8A 0.0414(18) 0.0417(18) 0.0336(16) -0.0050(13) -0.0015(14) 0.0018(14) C11A 0.0477(19) 0.0387(17) 0.0405(17) -0.0034(14) 0.0079(15) 0.0031(14) C12D 0.0408(18) 0.0513(19) 0.0361(17) -0.0142(14) 0.0029(14) 0.0066(15) C10D 0.047(2) 0.049(2) 0.064(2) 0.0121(17) 0.0030(17) -0.0068(16) C8B 0.078(3) 0.0399(18) 0.0306(17) 0.0012(14) 0.0193(17) -0.0052(17) C9D 0.052(2) 0.064(2) 0.0389(18) 0.0025(16) 0.0122(16) -0.0040(17) C9A 0.045(2) 0.0459(19) 0.068(2) -0.0127(17) 0.0123(17) -0.0041(15) C13A 0.055(2) 0.049(2) 0.056(2) -0.0061(17) -0.0152(17) 0.0132(17) C12A 0.0443(19) 0.0379(18) 0.053(2) -0.0030(15) 0.0068(16) 0.0065(14) C14A 0.067(2) 0.0399(19) 0.065(2) 0.0008(17) 0.0101(18) 0.0096(17) C10A 0.075(3) 0.062(2) 0.048(2) -0.0041(18) -0.0179(19) 0.0128(19) C14D 0.065(2) 0.082(3) 0.0287(17) -0.0022(17) 0.0156(16) -0.006(2) C13D 0.062(2) 0.073(3) 0.068(2) -0.021(2) 0.011(2) 0.022(2) C13B 0.048(4) 0.052(4) 0.026(4) 0.001(3) 0.008(3) -0.016(3) C15D 0.055(2) 0.090(3) 0.0333(18) -0.0173(18) -0.0019(16) 0.0100(19) C14B 0.068(4) 0.046(4) 0.057(4) -0.005(4) 0.007(3) -0.011(4) C11B 0.041(3) 0.037(3) 0.020(2) 0.0012(18) 0.0063(19) 0.001(2) C15A 0.059(2) 0.059(2) 0.108(3) 0.002(2) 0.030(2) 0.0144(19) C11C 0.037(3) 0.058(3) 0.054(3) 0.021(3) 0.007(3) -0.007(3) C10B 0.100(5) 0.047(3) 0.031(3) 0.010(2) -0.003(3) -0.006(3) C13C 0.25(3) 0.090(17) 0.128(16) -0.015(11) 0.003(14) 0.090(16) C12B 0.045(4) 0.045(5) 0.034(4) -0.002(4) 0.007(3) -0.011(4) C12C 0.040(5) 0.063(6) 0.082(11) 0.024(6) 0.006(5) 0.009(4) C14C 0.058(5) 0.073(6) 0.127(7) 0.043(6) 0.014(5) 0.019(5) C9C 0.064(4) 0.059(4) 0.053(3) -0.002(3) -0.007(3) -0.004(3) C15B 0.066(5) 0.069(4) 0.050(4) 0.004(3) 0.002(4) -0.006(4) C9B 0.091(5) 0.085(5) 0.040(3) -0.008(3) 0.034(3) -0.043(4) C15C 0.069(7) 0.111(7) 0.221(13) 0.071(8) 0.074(8) 0.027(5) C10C 0.047(3) 0.054(4) 0.069(4) 0.018(3) 0.008(3) -0.010(3) C9F 0.037(5) 0.076(8) 0.056(6) 0.008(5) 0.006(5) -0.004(5) C11F 0.063(7) 0.084(9) 0.057(7) 0.020(6) -0.001(6) 0.021(6) C11E 0.116(11) 0.057(8) 0.025(5) -0.015(5) 0.000(6) 0.025(7) C9E 0.102(10) 0.091(9) 0.023(5) -0.007(5) 0.018(5) 0.047(7) C10F 0.072(8) 0.078(9) 0.081(9) 0.027(7) -0.025(7) -0.020(7) C10E 0.25(2) 0.039(7) 0.033(6) 0.006(5) 0.070(9) -0.012(9) C12E 0.080(15) 0.112(18) 0.039(9) -0.028(12) 0.021(9) -0.029(13) C13E 0.15(2) 0.18(3) 0.069(12) -0.051(16) 0.063(12) -0.08(2) C15E 0.13(2) 0.29(3) 0.054(10) -0.049(14) 0.002(11) 0.043(17) C14E 0.152(17) 0.065(13) 0.086(13) -0.022(11) 0.051(12) -0.024(13) C14F 0.096(13) 0.20(2) 0.096(12) -0.007(13) 0.038(11) 0.018(12) C13F 0.118(15) 0.045(9) 0.036(8) -0.004(6) -0.021(9) 0.043(9) C15F 0.092(15) 0.089(14) 0.094(12) 0.031(12) 0.002(10) 0.045(11) C12F 0.18(3) 0.049(12) 0.051(14) 0.005(10) 0.004(12) 0.058(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A C1A 1.392(3) . ? O1D C1D 1.386(3) . ? O1C C1C 1.398(3) . ? O1B C1B 1.392(3) . ? C2D C3D 1.383(4) . ? C2D C1D 1.397(4) . ? C2D C7C 1.524(4) . ? C2A C1A 1.389(4) . ? C2A C3A 1.399(4) . ? C2A C7D 1.523(4) . ? C1A C6A 1.392(4) . ? C6D C1D 1.389(4) . ? C6D C5D 1.397(4) . ? C6D C7D 1.514(4) . ? C1B C6B 1.390(4) . ? C1B C2B 1.389(4) . ? C6B C5B 1.392(4) . ? C6B C7B 1.509(4) . ? C5B C4B 1.393(4) . ? C3A C4A 1.395(4) . ? C5D C4D 1.392(4) . ? C2C C3C 1.392(4) . ? C2C C1C 1.394(4) . ? C2C C7B 1.528(4) . ? C5A C6A 1.392(4) . ? C5A C4A 1.396(4) . ? C1C C6C 1.382(4) . ? C2B C3B 1.390(4) . ? C2B C7A 1.519(4) . ? C8D C4D 1.528(4) . ? C8D C10D 1.541(4) . ? C8D C9D 1.543(4) . ? C8D C11D 1.551(4) . ? C4D C3D 1.395(4) . ? C3B C4B 1.393(4) . ? C6A C7A 1.511(4) . ? C4A C8A 1.527(4) . ? C4C C3C 1.394(4) . ? C4C C5C 1.406(4) . ? C4C C8C 1.536(4) . ? C5C C6C 1.393(4) . ? C7C C6C 1.528(4) . ? C4B C8B 1.532(4) . ? C11D C12D 1.552(4) . ? C8C C11F 1.512(10) . ? C8C C11C 1.534(6) . ? C8C C9C 1.550(6) . ? C8C C10C 1.563(6) . ? C8C C10F 1.565(11) . ? C8C C9F 1.565(10) . ? C8A C10A 1.541(4) . ? C8A C9A 1.539(4) . ? C8A C11A 1.550(4) . ? C11A C12A 1.541(4) . ? C12D C13D 1.527(4) . ? C12D C14D 1.535(4) . ? C12D C15D 1.544(4) . ? C8B C11E 1.431(12) . ? C8B C9B 1.487(6) . ? C8B C10E 1.528(11) . ? C8B C11B 1.540(5) . ? C8B C10B 1.622(6) . ? C8B C9E 1.659(10) . ? C13A C12A 1.543(4) . ? C12A C14A 1.525(4) . ? C12A C15A 1.534(4) . ? C13B C12B 1.528(15) . ? C14B C12B 1.564(9) . ? C11B C12B 1.552(10) . ? C11C C12C 1.571(16) . ? C13C C12C 1.49(3) . ? C12B C15B 1.524(12) . ? C12C C15C 1.530(16) . ? C12C C14C 1.530(15) . ? C11F C12F 1.56(3) . ? C11E C12E 1.51(3) . ? C12E C14E 1.52(2) . ? C12E C13E 1.56(4) . ? C12E C15E 1.58(3) . ? C14F C12F 1.60(4) . ? C13F C12F 1.42(6) . ? C15F C12F 1.55(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3D C2D C1D 118.2(3) . . ? C3D C2D C7C 120.3(3) . . ? C1D C2D C7C 121.4(3) . . ? C1A C2A C3A 118.0(2) . . ? C1A C2A C7D 121.8(2) . . ? C3A C2A C7D 120.2(2) . . ? C2A C1A O1A 119.6(2) . . ? C2A C1A C6A 121.7(3) . . ? O1A C1A C6A 118.7(2) . . ? C1D C6D C5D 118.0(3) . . ? C1D C6D C7D 122.5(3) . . ? C5D C6D C7D 119.4(2) . . ? C6B C1B C2B 121.7(2) . . ? C6B C1B O1B 118.8(2) . . ? C2B C1B O1B 119.4(2) . . ? C1B C6B C5B 117.9(2) . . ? C1B C6B C7B 122.1(2) . . ? C5B C6B C7B 119.9(2) . . ? C4B C5B C6B 122.8(3) . . ? C4A C3A C2A 123.0(3) . . ? C4D C5D C6D 122.9(3) . . ? C3C C2C C1C 117.9(3) . . ? C3C C2C C7B 119.7(3) . . ? C1C C2C C7B 122.3(3) . . ? O1D C1D C6D 119.1(3) . . ? O1D C1D C2D 119.6(3) . . ? C6D C1D C2D 121.3(3) . . ? C6A C5A C4A 123.4(3) . . ? C6C C1C C2C 121.6(3) . . ? C6C C1C O1C 119.1(3) . . ? C2C C1C O1C 119.3(3) . . ? C1B C2B C3B 118.0(3) . . ? C1B C2B C7A 121.8(3) . . ? C3B C2B C7A 120.1(3) . . ? C4D C8D C10D 112.1(2) . . ? C4D C8D C9D 109.5(2) . . ? C10D C8D C9D 106.6(2) . . ? C4D C8D C11D 109.8(2) . . ? C10D C8D C11D 111.9(2) . . ? C9D C8D C11D 106.6(2) . . ? C5D C4D C3D 116.3(3) . . ? C5D C4D C8D 123.0(2) . . ? C3D C4D C8D 120.5(3) . . ? C2B C3B C4B 122.9(3) . . ? C2D C3D C4D 123.2(3) . . ? C6B C7B C2C 112.8(2) . . ? C5A C6A C1A 117.8(3) . . ? C5A C6A C7A 119.7(3) . . ? C1A C6A C7A 122.4(3) . . ? C3A C4A C5A 116.1(3) . . ? C3A C4A C8A 123.9(3) . . ? C5A C4A C8A 120.0(2) . . ? C3C C4C C5C 116.0(3) . . ? C3C C4C C8C 121.5(3) . . ? C5C C4C C8C 122.4(3) . . ? C6D C7D C2A 112.5(2) . . ? C6C C5C C4C 122.7(3) . . ? C2C C3C C4C 123.3(3) . . ? C6A C7A C2B 113.5(2) . . ? C2D C7C C6C 112.7(2) . . ? C1C C6C C5C 118.5(3) . . ? C1C C6C C7C 122.1(3) . . ? C5C C6C C7C 119.3(3) . . ? C3B C4B C5B 116.7(3) . . ? C3B C4B C8B 121.7(3) . . ? C5B C4B C8B 121.5(3) . . ? C12D C11D C8D 124.4(2) . . ? C11F C8C C11C 56.7(4) . . ? C11F C8C C4C 112.4(5) . . ? C11C C8C C4C 113.2(3) . . ? C11F C8C C9C 140.8(5) . . ? C11C C8C C9C 108.0(3) . . ? C4C C8C C9C 106.8(3) . . ? C11F C8C C10C 58.4(5) . . ? C11C C8C C10C 110.6(3) . . ? C4C C8C C10C 111.5(3) . . ? C9C C8C C10C 106.4(4) . . ? C11F C8C C10F 107.0(7) . . ? C11C C8C C10F 138.7(5) . . ? C4C C8C C10F 108.0(4) . . ? C9C C8C C10F 58.4(6) . . ? C10C C8C C10F 51.1(5) . . ? C11F C8C C9F 110.5(6) . . ? C11C C8C C9F 57.9(4) . . ? C4C C8C C9F 112.2(4) . . ? C9C C8C C9F 52.3(4) . . ? C10C C8C C9F 135.5(4) . . ? C10F C8C C9F 106.3(7) . . ? C4A C8A C10A 107.3(2) . . ? C4A C8A C9A 112.4(2) . . ? C10A C8A C9A 107.0(3) . . ? C4A C8A C11A 112.0(2) . . ? C10A C8A C11A 106.7(2) . . ? C9A C8A C11A 111.1(2) . . ? C12A C11A C8A 123.3(2) . . ? C13D C12D C14D 109.1(3) . . ? C13D C12D C15D 108.0(3) . . ? C14D C12D C15D 107.3(3) . . ? C13D C12D C11D 113.4(3) . . ? C14D C12D C11D 113.1(2) . . ? C15D C12D C11D 105.7(2) . . ? C11E C8B C9B 136.8(5) . . ? C11E C8B C10E 114.1(8) . . ? C9B C8B C10E 45.4(6) . . ? C11E C8B C4B 113.0(4) . . ? C9B C8B C4B 109.5(3) . . ? C10E C8B C4B 104.5(5) . . ? C11E C8B C11B 58.5(5) . . ? C9B C8B C11B 109.7(4) . . ? C10E C8B C11B 140.2(5) . . ? C4B C8B C11B 114.3(2) . . ? C11E C8B C10B 51.8(5) . . ? C9B C8B C10B 105.2(4) . . ? C10E C8B C10B 65.0(7) . . ? C4B C8B C10B 111.2(3) . . ? C11B C8B C10B 106.7(3) . . ? C11E C8B C9E 111.7(6) . . ? C9B C8B C9E 60.6(5) . . ? C10E C8B C9E 105.4(8) . . ? C4B C8B C9E 107.5(4) . . ? C11B C8B C9E 55.3(5) . . ? C10B C8B C9E 141.3(4) . . ? C14A C12A C15A 107.2(3) . . ? C14A C12A C11A 111.9(3) . . ? C15A C12A C11A 106.8(3) . . ? C14A C12A C13A 109.6(3) . . ? C15A C12A C13A 108.6(3) . . ? C11A C12A C13A 112.6(2) . . ? C8B C11B C12B 126.7(5) . . ? C8C C11C C12C 125.8(6) . . ? C15B C12B C13B 109.0(7) . . ? C15B C12B C11B 114.8(6) . . ? C13B C12B C11B 112.5(8) . . ? C15B C12B C14B 106.4(7) . . ? C13B C12B C14B 109.2(7) . . ? C11B C12B C14B 104.5(6) . . ? C13C C12C C15C 117.7(17) . . ? C13C C12C C14C 109.0(14) . . ? C15C C12C C14C 105.8(9) . . ? C13C C12C C11C 105.0(13) . . ? C15C C12C C11C 112.8(10) . . ? C14C C12C C11C 105.9(10) . . ? C8C C11F C12F 121.7(16) . . ? C8B C11E C12E 125.5(12) . . ? C11E C12E C14E 115.6(17) . . ? C11E C12E C13E 112.4(18) . . ? C14E C12E C13E 113(2) . . ? C11E C12E C15E 100.4(18) . . ? C14E C12E C15E 108.8(18) . . ? C13E C12E C15E 105.3(18) . . ? C13F C12F C15F 113(3) . . ? C13F C12F C11F 121(2) . . ? C15F C12F C11F 112(2) . . ? C13F C12F C14F 102(2) . . ? C15F C12F C14F 104(2) . . ? C11F C12F C14F 102(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.223 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.048