Supplementary Material (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Wen Sheng Guo' 'Fang Guo' 'Fumio Toda' _publ_contact_author_name 'Wen Sheng Guo' _publ_contact_author_address ; Institute of Chemical Science & Engineering Liaoning University Shenyang 110036 CHINA ; _publ_contact_author_email WENGSGUO@1NU.EDU.CN _publ_section_title ; Supramolecular stereoisomer - the conformational isomer of 1,1,6,6-tetraphenylhexa-2,4-diyne-1,6-diol in the different inclusion compound. ; data_gws04 _database_code_CSD 177473 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H28 O2.50' _chemical_formula_weight 488.57 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9719(15) _cell_length_b 15.119(2) _cell_length_c 16.799(3) _cell_angle_alpha 100.572(11) _cell_angle_beta 104.897(11) _cell_angle_gamma 113.581(10) _cell_volume 2761.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 7745 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6413 _reflns_number_gt 4068 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.0964P)^2^+0.9282P] 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 6413 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.148 _refine_ls_shift/su_mean 0.010 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 C27A C 0.7421(5) -0.0092(3) -0.2252(3) 0.0925(16) Uani 1 1 d . . . H27A H 0.7664 -0.0493 -0.1976 0.111 Uiso 1 1 calc R . . C28A C 0.6830(4) -0.0447(3) -0.3130(3) 0.0859(15) Uani 1 1 d . . . H28A H 0.6672 -0.1086 -0.3455 0.103 Uiso 1 1 calc R . . C29A C 0.6480(4) 0.0140(3) -0.3520(3) 0.0914(15) Uani 1 1 d . . . H29A H 0.6077 -0.0095 -0.4120 0.110 Uiso 1 1 calc R . . C30A C 0.6714(4) 0.1086(3) -0.3039(2) 0.0778(14) Uani 1 1 d . . . H30A H 0.6455 0.1477 -0.3321 0.093 Uiso 1 1 calc R . . C1B C 0.0750(4) 0.3504(2) 0.71528(19) 0.0427(11) Uani 1 1 d . . . C2B C 0.1206(3) 0.4215(2) 0.66755(19) 0.0473(10) Uani 1 1 d . . . C3B C 0.1541(3) 0.4804(2) 0.6300(2) 0.0501(10) Uani 1 1 d . . . C4B C 0.1968(3) 0.5499(2) 0.5889(2) 0.0504(10) Uani 1 1 d . . . C5B C 0.2355(3) 0.6113(2) 0.55449(19) 0.0500(10) Uani 1 1 d . . . C6B C 0.2862(4) 0.6879(2) 0.51216(17) 0.0453(12) Uani 1 1 d . . . C7B C 0.1569(4) 0.4009(2) 0.8115(2) 0.0438(10) Uani 1 1 d . . . C8B C 0.2596(5) 0.3930(4) 0.8408(3) 0.0989(18) Uani 1 1 d . . . H8BA H 0.2797 0.3565 0.8021 0.119 Uiso 1 1 calc R . . C9B C 0.3344(5) 0.4383(5) 0.9272(3) 0.130(2) Uani 1 1 d . . . H9BA H 0.4035 0.4309 0.9462 0.156 Uiso 1 1 calc R . . C10B C 0.3091(5) 0.4934(4) 0.9850(3) 0.0982(19) Uani 1 1 d . . . H10A H 0.3610 0.5252 1.0430 0.118 Uiso 1 1 calc R . . C11B C 0.2081(5) 0.5010(4) 0.9569(3) 0.0951(17) Uani 1 1 d . . . H11A H 0.1885 0.5373 0.9962 0.114 Uiso 1 1 calc R . . C12B C 0.1315(4) 0.4558(3) 0.8702(2) 0.0760(14) Uani 1 1 d . . . H12A H 0.0622 0.4631 0.8519 0.091 Uiso 1 1 calc R . . C13B C 0.0683(3) 0.2479(2) 0.67731(19) 0.0460(10) Uani 1 1 d . . . C14B C 0.1305(4) 0.2340(3) 0.6272(2) 0.0678(13) Uani 1 1 d . . . H14A H 0.1759 0.2882 0.6113 0.081 Uiso 1 1 calc R . . C15B C 0.1286(4) 0.1407(3) 0.5988(3) 0.0868(15) Uani 1 1 d . . . H15A H 0.1741 0.1335 0.5659 0.104 Uiso 1 1 calc R . . C16B C 0.0600(5) 0.0608(3) 0.6194(3) 0.0914(17) Uani 1 1 d . . . H16A H 0.0584 -0.0018 0.6011 0.110 Uiso 1 1 calc R . . C17B C -0.0063(5) 0.0725(3) 0.6669(4) 0.109(2) Uani 1 1 d . . . H17A H -0.0549 0.0171 0.6800 0.131 Uiso 1 1 calc R . . C18B C -0.0029(4) 0.1653(3) 0.6960(3) 0.0848(15) Uani 1 1 d . . . H18A H -0.0491 0.1720 0.7286 0.102 Uiso 1 1 calc R . . C19B C 0.2958(3) 0.7895(2) 0.56056(19) 0.0489(10) Uani 1 1 d . . . C20B C 0.3514(4) 0.8298(3) 0.6492(2) 0.0779(14) Uani 1 1 d . . . H20A H 0.3807 0.7944 0.6803 0.093 Uiso 1 1 calc R . . C21B C 0.3644(5) 0.9233(3) 0.6932(3) 0.0957(16) Uani 1 1 d . . . H21A H 0.4016 0.9496 0.7535 0.115 Uiso 1 1 calc R . . C22B C 0.3235(5) 0.9766(3) 0.6491(3) 0.0905(16) Uani 1 1 d . . . H22A H 0.3332 1.0394 0.6788 0.109 Uiso 1 1 calc R . . C23B C 0.2686(5) 0.9375(3) 0.5618(3) 0.0929(16) Uani 1 1 d . . . H23A H 0.2396 0.9735 0.5314 0.112 Uiso 1 1 calc R . . C24B C 0.2546(4) 0.8442(3) 0.5167(2) 0.0716(13) Uani 1 1 d . . . H24A H 0.2172 0.8187 0.4563 0.086 Uiso 1 1 calc R . . C25B C 0.4074(4) 0.7006(2) 0.50970(18) 0.0425(11) Uani 1 1 d . . . C26B C 0.4673(5) 0.6552(3) 0.5503(2) 0.0678(14) Uani 1 1 d . . . H26A H 0.4342 0.6153 0.5822 0.081 Uiso 1 1 calc R . . C27B C 0.5762(5) 0.6679(3) 0.5447(3) 0.0811(16) Uani 1 1 d . . . H27B H 0.6158 0.6366 0.5729 0.097 Uiso 1 1 calc R . . C28B C 0.6266(4) 0.7259(3) 0.4982(3) 0.0712(13) Uani 1 1 d . . . H28B H 0.6996 0.7339 0.4939 0.085 Uiso 1 1 calc R . . C29B C 0.5670(5) 0.7722(3) 0.4581(2) 0.0704(15) Uani 1 1 d . . . H29B H 0.6002 0.8123 0.4263 0.085 Uiso 1 1 calc R . . C30B C 0.4591(5) 0.7600(3) 0.4641(2) 0.0602(13) Uani 1 1 d . . . H30B H 0.4203 0.7924 0.4368 0.072 Uiso 1 1 calc R . . C1 C 0.2647(12) 0.9326(7) 0.9265(8) 0.155(3) Uani 1 1 d . . . C2 C 0.1775(9) 0.9349(10) 0.8679(7) 0.227(6) Uani 1 1 d . . . H2A H 0.1419 0.8885 0.8119 0.272 Uiso 1 1 calc R . . C3 C 0.1372(9) 1.0066(11) 0.8888(7) 0.299(8) Uani 1 1 d . . . H3A H 0.0732 1.0062 0.8478 0.358 Uiso 1 1 calc R . . C4 C 0.1924(9) 1.0752(8) 0.9685(6) 0.182(4) Uani 1 1 d . . . C5 C 0.2842(10) 1.0749(6) 1.0263(5) 0.156(3) Uani 1 1 d . . . H5A H 0.3213 1.1228 1.0816 0.187 Uiso 1 1 calc R . . C6 C 0.3257(8) 1.0071(8) 1.0071(6) 0.158(3) Uani 1 1 d . . . H6A H 0.3931 1.0108 1.0472 0.190 Uiso 1 1 calc R . . C7 C 0.3258(9) 0.8601(10) 0.9124(6) 0.202(5) Uani 1 1 d . . . H7A H 0.4033 0.8788 0.9496 0.242 Uiso 1 1 calc R . . C8 C 0.2755(9) 0.7896(8) 0.8593(5) 0.193(5) Uani 1 1 d . . . H8A H 0.1977 0.7708 0.8227 0.231 Uiso 1 1 calc R . . C9 C 0.3387(9) 0.7136(6) 0.8428(5) 0.193(4) Uani 1 1 d . . . H9A H 0.2817 0.6527 0.7947 0.290 Uiso 1 1 calc R . . H9B H 0.3610 0.6957 0.8942 0.290 Uiso 1 1 calc R . . H9C H 0.4094 0.7488 0.8301 0.290 Uiso 1 1 calc R . . C10 C 0.0665(10) 1.1503(11) 0.9457(10) 0.434(15) Uani 1 1 d . . . H10B H 0.0556 1.2051 0.9744 0.650 Uiso 1 1 calc R . . H10C H -0.0041 1.0866 0.9318 0.650 Uiso 1 1 calc R . . H10D H 0.0786 1.1594 0.8932 0.650 Uiso 1 1 calc R . . O1 O 0.1638(7) 1.1499(6) 0.9988(5) 0.262(4) Uani 1 1 d . . . O1A O 1.1903(2) 0.52627(15) 0.28108(12) 0.0557(7) Uani 1 1 d . . . H1AA H 1.1899 0.5584 0.2467 0.084 Uiso 1 1 calc R . . O2A O 0.7981(2) 0.32317(15) -0.20890(13) 0.0532(7) Uani 1 1 d . . . H2AA H 0.8447 0.3115 -0.2286 0.080 Uiso 1 1 calc R . . O1B O -0.0429(3) 0.33589(16) 0.71024(13) 0.0512(8) Uani 1 1 d . . . H1BA H -0.0766 0.3420 0.6646 0.077 Uiso 1 1 calc R . . O2B O 0.2013(2) 0.65423(15) 0.42518(12) 0.0518(7) Uani 1 1 d . . . H2BA H 0.2149 0.6166 0.3924 0.078 Uiso 1 1 calc R . . C1A C 1.1716(4) 0.4267(2) 0.23742(17) 0.0481(12) Uani 1 1 d . . . C2A C 1.0774(3) 0.3880(2) 0.1492(2) 0.0535(11) Uani 1 1 d . . . C3A C 1.0025(3) 0.3574(3) 0.0782(2) 0.0551(11) Uani 1 1 d . . . C4A C 0.9164(3) 0.3211(2) -0.0041(2) 0.0525(10) Uani 1 1 d . . . C5A C 0.8425(3) 0.2895(2) -0.0757(2) 0.0489(10) Uani 1 1 d . . . C6A C 0.7530(4) 0.2517(2) -0.16510(17) 0.0406(11) Uani 1 1 d . . . C7A C 1.1189(4) 0.3588(2) 0.2898(2) 0.0502(11) Uani 1 1 d . . . C8A C 1.1382(4) 0.2761(3) 0.2929(3) 0.0766(13) Uani 1 1 d . . . H8AA H 1.1844 0.2611 0.2640 0.092 Uiso 1 1 calc R . . C9A C 1.0881(5) 0.2151(4) 0.3397(4) 0.1011(19) Uani 1 1 d . . . H9AA H 1.1008 0.1590 0.3414 0.121 Uiso 1 1 calc R . . C10A C 1.0218(6) 0.2360(4) 0.3825(4) 0.102(2) Uani 1 1 d . . . H10E H 0.9899 0.1948 0.4139 0.123 Uiso 1 1 calc R . . C11A C 1.0014(5) 0.3165(4) 0.3801(3) 0.0965(16) Uani 1 1 d . . . H11B H 0.9554 0.3308 0.4097 0.116 Uiso 1 1 calc R . . C12A C 1.0497(4) 0.3778(3) 0.3331(3) 0.0751(14) Uani 1 1 d . . . H12B H 1.0347 0.4327 0.3310 0.090 Uiso 1 1 calc R . . C13A C 1.2897(4) 0.4322(2) 0.2341(2) 0.0491(12) Uani 1 1 d . . . C14A C 1.2970(6) 0.3772(4) 0.1628(3) 0.0924(18) Uani 1 1 d . . . H14B H 1.2277 0.3362 0.1133 0.111 Uiso 1 1 calc R . . C15A C 1.4047(7) 0.3823(5) 0.1641(3) 0.109(2) Uani 1 1 d . . . H15B H 1.4077 0.3440 0.1156 0.131 Uiso 1 1 calc R . . C16A C 1.5086(5) 0.4429(4) 0.2357(4) 0.0935(16) Uani 1 1 d . . . H16B H 1.5820 0.4465 0.2362 0.112 Uiso 1 1 calc R . . C17A C 1.5012(6) 0.4976(3) 0.3059(3) 0.0790(16) Uani 1 1 d . . . H17B H 1.5709 0.5389 0.3552 0.095 Uiso 1 1 calc R . . C18A C 1.3937(5) 0.4932(3) 0.3059(2) 0.0604(13) Uani 1 1 d . . . H18B H 1.3911 0.5317 0.3547 0.072 Uiso 1 1 calc R . . C19A C 0.6345(4) 0.2463(2) -0.16346(18) 0.0426(11) Uani 1 1 d . . . C20A C 0.5805(5) 0.1953(3) -0.1143(3) 0.0798(15) Uani 1 1 d . . . H20B H 0.6192 0.1676 -0.0801 0.096 Uiso 1 1 calc R . . C21A C 0.4702(6) 0.1841(4) -0.1146(3) 0.0926(17) Uani 1 1 d . . . H21B H 0.4347 0.1481 -0.0813 0.111 Uiso 1 1 calc R . . C22A C 0.4110(4) 0.2254(3) -0.1634(3) 0.0761(13) Uani 1 1 d . . . H22B H 0.3367 0.2187 -0.1629 0.091 Uiso 1 1 calc R . . C23A C 0.4652(6) 0.2764(3) -0.2125(3) 0.0762(15) Uani 1 1 d . . . H23B H 0.4268 0.3044 -0.2464 0.091 Uiso 1 1 calc R . . C24A C 0.5752(5) 0.2871(3) -0.2125(2) 0.0606(13) Uani 1 1 d . . . H24B H 0.6104 0.3226 -0.2462 0.073 Uiso 1 1 calc R . . C25A C 0.7317(3) 0.1466(2) -0.21555(19) 0.0463(10) Uani 1 1 d . . . C26A C 0.7664(4) 0.0868(3) -0.1762(2) 0.0733(13) Uani 1 1 d . . . H26B H 0.8066 0.1101 -0.1162 0.088 Uiso 1 1 calc R . . 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 C27A 0.127(5) 0.069(3) 0.091(3) 0.029(2) 0.032(3) 0.058(3) C28A 0.098(4) 0.054(2) 0.086(3) 0.007(2) 0.035(3) 0.024(2) C29A 0.110(4) 0.078(3) 0.056(2) -0.002(2) 0.015(2) 0.036(3) C30A 0.102(4) 0.070(2) 0.049(2) 0.0138(18) 0.013(2) 0.041(2) C1B 0.039(3) 0.0493(18) 0.0489(18) 0.0226(14) 0.0213(17) 0.0229(17) C2B 0.047(3) 0.0473(18) 0.0478(17) 0.0159(15) 0.0169(16) 0.0226(17) C3B 0.054(3) 0.0506(18) 0.0506(18) 0.0211(15) 0.0227(17) 0.0245(17) C4B 0.053(3) 0.0474(18) 0.0515(18) 0.0209(15) 0.0212(17) 0.0213(17) C5B 0.050(3) 0.0504(18) 0.0473(17) 0.0159(15) 0.0177(17) 0.0213(17) C6B 0.052(3) 0.0413(17) 0.0367(16) 0.0151(13) 0.0121(16) 0.0180(17) C7B 0.042(3) 0.0485(18) 0.0493(18) 0.0168(14) 0.0186(18) 0.0275(17) C8B 0.089(4) 0.143(4) 0.062(3) -0.006(3) 0.004(3) 0.084(4) C9B 0.114(5) 0.189(6) 0.075(3) -0.008(3) -0.015(3) 0.113(5) C10B 0.088(5) 0.123(4) 0.059(3) -0.003(3) 0.001(3) 0.056(3) C11B 0.091(4) 0.109(4) 0.064(3) -0.016(2) 0.010(3) 0.057(3) C12B 0.066(4) 0.083(3) 0.074(3) 0.000(2) 0.011(2) 0.049(2) C13B 0.051(3) 0.0461(18) 0.0442(17) 0.0167(14) 0.0202(17) 0.0228(17) C14B 0.079(4) 0.052(2) 0.079(3) 0.0195(18) 0.043(3) 0.028(2) C15B 0.098(4) 0.068(3) 0.110(3) 0.016(2) 0.067(3) 0.041(3) C16B 0.107(5) 0.053(2) 0.124(4) 0.021(2) 0.058(3) 0.040(3) C17B 0.137(6) 0.058(3) 0.169(5) 0.055(3) 0.099(5) 0.047(3) C18B 0.110(4) 0.063(2) 0.122(3) 0.047(2) 0.080(3) 0.048(3) C19B 0.047(3) 0.0423(17) 0.0507(19) 0.0157(14) 0.0207(16) 0.0125(16) C20B 0.103(4) 0.062(2) 0.051(2) 0.0107(17) 0.018(2) 0.032(2) C21B 0.125(5) 0.072(3) 0.061(2) 0.000(2) 0.035(3) 0.029(3) C22B 0.119(5) 0.051(2) 0.095(3) 0.011(2) 0.054(3) 0.031(3) C23B 0.122(5) 0.062(2) 0.096(3) 0.020(2) 0.033(3) 0.051(3) C24B 0.092(4) 0.059(2) 0.065(2) 0.0174(18) 0.022(2) 0.041(2) C25B 0.034(3) 0.0453(17) 0.0416(17) 0.0137(13) 0.0109(16) 0.0141(16) C26B 0.056(4) 0.081(3) 0.079(3) 0.046(2) 0.027(2) 0.033(2) C27B 0.061(4) 0.095(3) 0.103(3) 0.051(3) 0.029(3) 0.044(3) C28B 0.045(3) 0.083(3) 0.078(3) 0.018(2) 0.023(2) 0.025(2) C29B 0.064(4) 0.082(3) 0.062(2) 0.030(2) 0.028(2) 0.026(3) C30B 0.056(4) 0.073(2) 0.063(2) 0.0345(18) 0.028(2) 0.033(2) C1 0.193(11) 0.131(6) 0.187(10) 0.094(7) 0.109(9) 0.075(7) C2 0.147(9) 0.274(13) 0.161(8) -0.059(7) -0.015(7) 0.107(8) C3 0.144(9) 0.366(16) 0.226(11) -0.139(11) -0.056(7) 0.149(10) C4 0.147(8) 0.207(9) 0.129(6) -0.019(6) 0.007(6) 0.084(7) C5 0.206(10) 0.127(6) 0.117(5) 0.055(5) 0.061(6) 0.055(6) C6 0.197(9) 0.138(7) 0.127(6) 0.072(6) 0.055(6) 0.056(7) C7 0.192(9) 0.190(9) 0.104(6) 0.085(6) 0.016(6) -0.012(8) C8 0.171(9) 0.166(8) 0.102(5) 0.012(5) 0.033(5) -0.026(7) C9 0.316(12) 0.130(6) 0.138(6) 0.039(5) 0.090(7) 0.107(7) C10 0.188(12) 0.48(2) 0.412(19) -0.197(16) -0.144(13) 0.255(14) O1 0.190(7) 0.265(7) 0.227(7) -0.089(6) -0.002(5) 0.130(6) O1A 0.076(2) 0.0459(12) 0.0458(12) 0.0157(9) 0.0187(12) 0.0311(12) O2A 0.0578(19) 0.0564(13) 0.0600(13) 0.0323(10) 0.0304(12) 0.0295(12) O1B 0.045(2) 0.0667(14) 0.0536(13) 0.0309(11) 0.0204(12) 0.0305(13) O2B 0.0561(18) 0.0558(12) 0.0395(11) 0.0119(9) 0.0083(11) 0.0296(12) C1A 0.058(3) 0.0411(17) 0.0358(16) 0.0079(13) 0.0050(16) 0.0238(17) C2A 0.060(3) 0.0552(19) 0.0459(19) 0.0135(15) 0.0153(19) 0.0320(19) C3A 0.058(3) 0.062(2) 0.045(2) 0.0118(15) 0.0126(19) 0.0350(19) C4A 0.057(3) 0.061(2) 0.0414(19) 0.0145(15) 0.0150(19) 0.0333(19) C5A 0.049(3) 0.0515(18) 0.049(2) 0.0160(15) 0.0186(18) 0.0263(17) C6A 0.039(3) 0.0489(18) 0.0398(16) 0.0209(13) 0.0167(16) 0.0223(16) C7A 0.049(3) 0.0425(18) 0.0456(18) 0.0111(14) 0.0045(18) 0.0188(17) C8A 0.070(3) 0.056(2) 0.107(3) 0.035(2) 0.029(2) 0.030(2) C9A 0.090(5) 0.068(3) 0.148(5) 0.062(3) 0.033(4) 0.033(3) C10A 0.092(5) 0.087(4) 0.104(4) 0.058(3) 0.025(3) 0.016(3) C11A 0.105(4) 0.080(3) 0.103(3) 0.040(3) 0.055(3) 0.027(3) C12A 0.086(4) 0.060(2) 0.083(3) 0.027(2) 0.037(3) 0.033(2) C13A 0.038(3) 0.059(2) 0.055(2) 0.0184(17) 0.0144(19) 0.0293(19) C14A 0.068(5) 0.130(4) 0.069(3) -0.004(2) 0.012(3) 0.060(3) C15A 0.086(5) 0.168(5) 0.091(4) 0.017(3) 0.035(4) 0.084(4) C16A 0.061(4) 0.122(4) 0.110(4) 0.045(3) 0.031(4) 0.052(3) C17A 0.060(4) 0.070(3) 0.096(4) 0.027(2) 0.016(3) 0.028(3) C18A 0.054(4) 0.060(2) 0.065(2) 0.0173(17) 0.013(2) 0.031(2) C19A 0.038(3) 0.0536(19) 0.0407(16) 0.0184(14) 0.0156(16) 0.0233(17) C20A 0.069(4) 0.123(4) 0.100(3) 0.076(3) 0.055(3) 0.061(3) C21A 0.087(5) 0.125(4) 0.109(4) 0.075(3) 0.064(3) 0.057(4) C22A 0.056(4) 0.094(3) 0.092(3) 0.025(3) 0.039(3) 0.042(3) C23A 0.064(4) 0.087(3) 0.096(3) 0.044(2) 0.035(3) 0.044(3) C24A 0.051(4) 0.072(2) 0.071(2) 0.0373(19) 0.029(2) 0.031(2) C25A 0.043(3) 0.0487(18) 0.0475(18) 0.0182(14) 0.0209(16) 0.0181(16) C26A 0.095(4) 0.063(2) 0.059(2) 0.0204(18) 0.014(2) 0.043(2) _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 C27A C28A 1.360(6) . ? C27A C26A 1.395(5) . ? C28A C29A 1.344(6) . ? C29A C30A 1.376(5) . ? C30A C25A 1.369(4) . ? C1B O1B 1.433(4) . ? C1B C2B 1.483(4) . ? C1B C13B 1.522(5) . ? C1B C7B 1.530(4) . ? C2B C3B 1.190(4) . ? C3B C4B 1.373(4) . ? C4B C5B 1.192(4) . ? C5B C6B 1.487(4) . ? C6B O2B 1.434(4) . ? C6B C25B 1.519(5) . ? C6B C19B 1.540(5) . ? C7B C8B 1.358(5) . ? C7B C12B 1.361(5) . ? C8B C9B 1.377(6) . ? C9B C10B 1.352(7) . ? C10B C11B 1.333(6) . ? C11B C12B 1.387(6) . ? C13B C14B 1.350(5) . ? C13B C18B 1.372(5) . ? C14B C15B 1.391(5) . ? C15B C16B 1.350(6) . ? C16B C17B 1.354(6) . ? C17B C18B 1.377(6) . ? C19B C20B 1.369(4) . ? C19B C24B 1.375(5) . ? C20B C21B 1.392(6) . ? C21B C22B 1.355(6) . ? C22B C23B 1.347(6) . ? C23B C24B 1.389(5) . ? C25B C26B 1.366(5) . ? C25B C30B 1.370(5) . ? C26B C27B 1.379(6) . ? C27B C28B 1.364(6) . ? C28B C29B 1.372(6) . ? C29B C30B 1.370(5) . ? C1 C2 1.312(11) . ? C1 C6 1.380(11) . ? C1 C7 1.607(14) . ? C2 C3 1.408(12) . ? C3 C4 1.335(11) . ? C4 C5 1.331(10) . ? C4 O1 1.376(10) . ? C5 C6 1.362(10) . ? C7 C8 1.074(10) . ? C8 C9 1.679(13) . ? C10 O1 1.348(10) . ? O1A C1A 1.441(4) . ? O2A C6A 1.435(3) . ? C1A C2A 1.486(4) . ? C1A C13A 1.517(5) . ? C1A C7A 1.541(5) . ? C2A C3A 1.193(4) . ? C3A C4A 1.378(5) . ? C4A C5A 1.194(4) . ? C5A C6A 1.479(4) . ? C6A C19A 1.514(5) . ? C6A C25A 1.534(4) . ? C7A C12A 1.372(5) . ? C7A C8A 1.378(5) . ? C8A C9A 1.393(6) . ? C9A C10A 1.345(7) . ? C10A C11A 1.351(7) . ? C11A C12A 1.391(6) . ? C13A C18A 1.373(5) . ? C13A C14A 1.374(6) . ? C14A C15A 1.362(6) . ? C15A C16A 1.369(7) . ? C16A C17A 1.360(7) . ? C17A C18A 1.370(6) . ? C19A C20A 1.366(5) . ? C19A C24A 1.376(5) . ? C20A C21A 1.371(6) . ? C21A C22A 1.377(6) . ? C22A C23A 1.366(6) . ? C23A C24A 1.370(5) . ? C25A C26A 1.360(5) . ? 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 C28A C27A C26A 120.6(4) . . ? C29A C28A C27A 119.0(4) . . ? C28A C29A C30A 120.5(4) . . ? C25A C30A C29A 121.6(4) . . ? O1B C1B C2B 108.7(3) . . ? O1B C1B C13B 109.6(3) . . ? C2B C1B C13B 111.5(3) . . ? O1B C1B C7B 106.8(3) . . ? C2B C1B C7B 108.5(3) . . ? C13B C1B C7B 111.7(3) . . ? C3B C2B C1B 177.2(4) . . ? C2B C3B C4B 178.0(4) . . ? C5B C4B C3B 178.9(4) . . ? C4B C5B C6B 178.8(4) . . ? O2B C6B C5B 108.0(3) . . ? O2B C6B C25B 109.8(3) . . ? C5B C6B C25B 111.7(3) . . ? O2B C6B C19B 106.9(3) . . ? C5B C6B C19B 108.7(3) . . ? C25B C6B C19B 111.6(3) . . ? C8B C7B C12B 117.7(4) . . ? C8B C7B C1B 120.1(3) . . ? C12B C7B C1B 122.2(4) . . ? C7B C8B C9B 120.7(4) . . ? C10B C9B C8B 121.2(5) . . ? C11B C10B C9B 118.4(5) . . ? C10B C11B C12B 121.2(5) . . ? C7B C12B C11B 120.7(4) . . ? C14B C13B C18B 117.9(3) . . ? C14B C13B C1B 123.6(3) . . ? C18B C13B C1B 118.6(4) . . ? C13B C14B C15B 121.8(4) . . ? C16B C15B C14B 119.5(4) . . ? C17B C16B C15B 119.4(4) . . ? C16B C17B C18B 121.0(4) . . ? C17B C18B C13B 120.4(4) . . ? C20B C19B C24B 118.3(3) . . ? C20B C19B C6B 120.0(3) . . ? C24B C19B C6B 121.7(3) . . ? C19B C20B C21B 120.3(4) . . ? C22B C21B C20B 120.8(4) . . ? C23B C22B C21B 119.2(4) . . ? C22B C23B C24B 120.9(4) . . ? C19B C24B C23B 120.4(4) . . ? C26B C25B C30B 118.3(5) . . ? C26B C25B C6B 123.2(3) . . ? C30B C25B C6B 118.5(4) . . ? C25B C26B C27B 120.8(4) . . ? C28B C27B C26B 120.8(4) . . ? C27B C28B C29B 118.5(5) . . ? C30B C29B C28B 120.7(4) . . ? C25B C30B C29B 121.0(4) . . ? C2 C1 C6 119.9(10) . . ? C2 C1 C7 127.1(11) . . ? C6 C1 C7 112.4(11) . . ? C1 C2 C3 120.7(10) . . ? C4 C3 C2 118.9(10) . . ? C5 C4 C3 119.7(11) . . ? C5 C4 O1 114.4(9) . . ? C3 C4 O1 125.9(11) . . ? C4 C5 C6 122.3(9) . . ? C5 C6 C1 118.0(9) . . ? C8 C7 C1 118.8(13) . . ? C7 C8 C9 119.4(13) . . ? C10 O1 C4 117.5(8) . . ? O1A C1A C2A 107.9(3) . . ? O1A C1A C13A 110.3(3) . . ? C2A C1A C13A 112.4(3) . . ? O1A C1A C7A 105.2(3) . . ? C2A C1A C7A 107.7(3) . . ? C13A C1A C7A 112.9(3) . . ? C3A C2A C1A 179.4(5) . . ? C2A C3A C4A 179.3(4) . . ? C5A C4A C3A 179.3(4) . . ? C4A C5A C6A 178.8(4) . . ? O2A C6A C5A 108.4(3) . . ? O2A C6A C19A 107.0(3) . . ? C5A C6A C19A 110.8(3) . . ? O2A C6A C25A 109.5(3) . . ? C5A C6A C25A 111.0(3) . . ? C19A C6A C25A 109.9(3) . . ? C12A C7A C8A 118.2(4) . . ? C12A C7A C1A 121.1(3) . . ? C8A C7A C1A 120.7(4) . . ? C7A C8A C9A 119.6(5) . . ? C10A C9A C8A 121.1(5) . . ? C11A C10A C9A 120.3(5) . . ? C10A C11A C12A 119.4(5) . . ? C7A C12A C11A 121.3(4) . . ? C18A C13A C14A 118.4(5) . . ? C18A C13A C1A 118.7(4) . . ? C14A C13A C1A 122.8(4) . . ? C15A C14A C13A 120.6(5) . . ? C14A C15A C16A 121.2(5) . . ? C17A C16A C15A 118.1(6) . . ? C18A C17A C16A 121.5(5) . . ? C17A C18A C13A 120.2(4) . . ? C20A C19A C24A 117.8(5) . . ? C20A C19A C6A 119.3(4) . . ? C24A C19A C6A 122.8(3) . . ? C19A C20A C21A 121.1(4) . . ? C20A C21A C22A 121.1(4) . . ? C23A C22A C21A 117.7(5) . . ? C24A C23A C22A 121.2(4) . . ? C23A C24A C19A 121.1(4) . . ? C26A C25A C30A 117.7(3) . . ? C26A C25A C6A 123.0(3) . . ? C30A C25A C6A 119.3(3) . . ? C25A C26A C27A 120.5(3) . . ? _diffrn_measured_fraction_theta_max 0.661 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.661 _refine_diff_density_max 0.265 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.041 data_samp304 _database_code_CSD 195761 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37.50 N O2' _chemical_formula_weight 384.06 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' N N 0.0061 0.0033 '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 ? _symmetry_space_group_name_H-M ? 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 13.220(3) _cell_length_b 10.568(4) _cell_length_c 15.517(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.954(17) _cell_angle_gamma 90.00 _cell_volume 2084.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 4403 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3469 _reflns_number_gt 1870 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.0543P)^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 3469 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.004 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 O1 O 0.74778(16) 0.86360(19) 0.19251(12) 0.0492(6) Uani 1 1 d . . . H1O H 0.770(3) 0.939(4) 0.172(2) 0.090(12) Uiso 1 1 d . . . C1 C 0.6823(2) 0.7972(2) 0.11812(16) 0.0395(7) Uani 1 1 d . . . C2 C 0.6016(2) 0.8851(3) 0.06497(18) 0.0433(7) Uani 1 1 d . . . C3 C 0.5376(2) 0.9571(3) 0.02394(19) 0.0450(7) Uani 1 1 d . . . C7 C 0.6291(2) 0.6905(2) 0.15614(17) 0.0400(7) Uani 1 1 d . . . C8 C 0.5345(3) 0.6400(3) 0.1078(2) 0.0567(9) Uani 1 1 d . . . H8 H 0.506(2) 0.672(3) 0.0499(19) 0.068(10) Uiso 1 1 d . . . C9 C 0.4866(3) 0.5431(4) 0.1420(3) 0.0719(11) Uani 1 1 d . . . H9 H 0.421(3) 0.515(4) 0.108(2) 0.105(14) Uiso 1 1 d . . . C10 C 0.5333(4) 0.4962(4) 0.2257(3) 0.0715(11) Uani 1 1 d . . . H10 H 0.496(3) 0.427(4) 0.247(2) 0.096(12) Uiso 1 1 d . . . C11 C 0.6271(4) 0.5434(3) 0.2735(3) 0.0736(11) Uani 1 1 d . . . H11 H 0.661(2) 0.508(3) 0.333(2) 0.077(10) Uiso 1 1 d . . . C12 C 0.6765(3) 0.6391(3) 0.2396(2) 0.0574(9) Uani 1 1 d . . . H12 H 0.742(2) 0.674(2) 0.2736(16) 0.046(8) Uiso 1 1 d . . . C13 C 0.7475(2) 0.7401(2) 0.05977(17) 0.0370(7) Uani 1 1 d . . . C14 C 0.8522(2) 0.7117(3) 0.0975(2) 0.0515(8) Uani 1 1 d . . . H14 H 0.881(2) 0.733(2) 0.1614(18) 0.054(8) Uiso 1 1 d . . . C15 C 0.9106(3) 0.6554(3) 0.0474(3) 0.0648(10) Uani 1 1 d . . . H15 H 0.982(3) 0.635(3) 0.076(2) 0.090(12) Uiso 1 1 d . . . C16 C 0.8661(3) 0.6262(3) -0.0412(3) 0.0648(10) Uani 1 1 d . . . H16 H 0.907(2) 0.587(3) -0.078(2) 0.077(10) Uiso 1 1 d . . . C17 C 0.7614(3) 0.6535(3) -0.0798(2) 0.0575(9) Uani 1 1 d . . . H17 H 0.728(2) 0.638(3) -0.1458(19) 0.065(9) Uiso 1 1 d . . . C18 C 0.7029(3) 0.7112(3) -0.02951(19) 0.0466(8) Uani 1 1 d . . . H18 H 0.630(2) 0.735(3) -0.0561(18) 0.055(9) Uiso 1 1 d . . . C1A C 0.7675(2) 0.2132(3) 0.19226(19) 0.0499(8) Uani 1 1 d . . . O2A O 0.81189(16) 0.10606(17) 0.15632(12) 0.0527(6) Uani 1 1 d . . . C3A C 0.8692(2) 0.1410(3) 0.09157(19) 0.0494(8) Uani 1 1 d . . . C4A C 0.9171(4) 0.3455(4) 0.1741(3) 0.0701(10) Uani 1 1 d . . . H2A H 0.996(3) 0.328(4) 0.193(2) 0.104(13) Uiso 1 1 d . . . H4A H 0.908(3) 0.437(4) 0.167(2) 0.103(14) Uiso 1 1 d . . . C5A C 0.8571(3) 0.3013(4) 0.2391(2) 0.0675(10) Uani 1 1 d . . . H5B H 0.904(3) 0.250(3) 0.284(2) 0.080(12) Uiso 1 1 d . . . H5A H 0.823(3) 0.378(4) 0.266(2) 0.103(13) Uiso 1 1 d . . . C6A C 0.6938(3) 0.2816(4) 0.1133(3) 0.0657(10) Uani 1 1 d . . . H6A H 0.632(3) 0.216(3) 0.082(2) 0.096(12) Uiso 1 1 d . . . H6B H 0.662(3) 0.354(3) 0.139(2) 0.084(11) Uiso 1 1 d . . . C7A C 0.7548(3) 0.3313(4) 0.0500(3) 0.0690(10) Uani 1 1 d . . . H7B H 0.755(3) 0.413(3) 0.056(2) 0.070(12) Uiso 1 1 d . . . H7A H 0.720(3) 0.292(3) -0.015(2) 0.092(12) Uiso 1 1 d . . . C8A C 0.8678(3) 0.2848(3) 0.0827(2) 0.0571(9) Uani 1 1 d . . . H8A H 0.910(3) 0.305(3) 0.032(2) 0.104(12) Uiso 1 1 d . . . C9A C 0.7122(4) 0.1588(4) 0.2561(3) 0.0811(13) Uani 1 1 d . . . H9B H 0.771(3) 0.109(3) 0.308(2) 0.084(12) Uiso 1 1 d . . . H9A H 0.650(3) 0.107(4) 0.219(2) 0.105(14) Uiso 1 1 d . . . H9C H 0.675(3) 0.223(4) 0.280(2) 0.106(14) Uiso 1 1 d . . . C10A C 0.8151(5) 0.0750(4) 0.0041(3) 0.0785(12) Uani 1 1 d . . . H10A H 0.829(3) -0.019(4) 0.015(2) 0.101(13) Uiso 1 1 d . . . H10C H 0.848(3) 0.097(3) -0.041(2) 0.086(12) Uiso 1 1 d . . . H10B H 0.734(4) 0.091(4) -0.015(3) 0.128(18) Uiso 1 1 d . . . C11A C 0.9800(4) 0.0880(5) 0.1266(4) 0.0858(13) Uani 1 1 d . . . H11C H 1.012(3) 0.126(4) 0.185(3) 0.119(17) Uiso 1 1 d . . . H11B H 1.029(4) 0.110(5) 0.085(3) 0.150(19) Uiso 1 1 d . . . H11A H 0.974(3) -0.007(5) 0.128(3) 0.133(18) Uiso 1 1 d . . . 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 O1 0.0628(14) 0.0384(12) 0.0405(11) -0.0018(10) 0.0043(10) -0.0056(10) C1 0.0436(16) 0.0321(14) 0.0367(14) 0.0009(13) 0.0007(13) 0.0025(14) C2 0.0477(18) 0.0350(16) 0.0468(17) 0.0019(14) 0.0124(15) 0.0050(15) C3 0.0464(19) 0.0359(16) 0.0506(18) 0.0028(14) 0.0096(15) 0.0020(14) C7 0.0449(18) 0.0324(15) 0.0440(16) 0.0005(13) 0.0144(14) 0.0061(14) C8 0.051(2) 0.053(2) 0.063(2) 0.0142(18) 0.0110(18) 0.0009(17) C9 0.052(2) 0.066(2) 0.100(3) 0.013(2) 0.025(2) -0.009(2) C10 0.088(3) 0.047(2) 0.100(3) 0.013(2) 0.060(3) 0.004(2) C11 0.110(3) 0.055(2) 0.059(2) 0.014(2) 0.028(2) 0.003(2) C12 0.073(2) 0.0455(18) 0.0478(19) 0.0047(16) 0.0064(19) 0.0006(18) C13 0.0418(18) 0.0262(14) 0.0419(16) 0.0041(12) 0.0095(14) 0.0025(12) C14 0.0444(19) 0.0524(19) 0.055(2) 0.0005(17) 0.0095(17) 0.0061(16) C15 0.049(2) 0.064(2) 0.086(3) 0.002(2) 0.026(2) 0.0031(19) C16 0.072(3) 0.053(2) 0.087(3) -0.005(2) 0.051(3) -0.0061(19) C17 0.080(3) 0.0502(19) 0.050(2) -0.0034(16) 0.031(2) -0.0094(19) C18 0.051(2) 0.0439(17) 0.0418(18) 0.0007(15) 0.0077(16) -0.0017(16) C1A 0.061(2) 0.0395(17) 0.0570(18) -0.0074(15) 0.0287(17) -0.0031(16) O2A 0.0687(14) 0.0368(11) 0.0621(13) 0.0017(10) 0.0339(11) -0.0013(10) C3A 0.053(2) 0.0503(18) 0.0493(17) 0.0032(15) 0.0204(16) -0.0024(16) C4A 0.071(3) 0.059(2) 0.076(3) -0.005(2) 0.013(2) -0.020(2) C5A 0.083(3) 0.054(2) 0.062(2) -0.008(2) 0.015(2) -0.010(2) C6A 0.054(2) 0.062(2) 0.080(2) 0.002(2) 0.017(2) 0.007(2) C7A 0.069(3) 0.060(3) 0.073(3) 0.015(2) 0.011(2) 0.007(2) C8A 0.057(2) 0.055(2) 0.060(2) 0.0114(17) 0.0166(18) -0.0068(17) C9A 0.109(4) 0.067(3) 0.089(3) -0.007(2) 0.065(3) -0.009(3) C10A 0.106(4) 0.074(3) 0.066(3) -0.012(2) 0.041(3) -0.015(3) C11A 0.071(3) 0.084(3) 0.107(4) 0.016(3) 0.031(3) 0.023(3) _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 O1 C1 1.423(3) . ? C1 C2 1.482(4) . ? C1 C7 1.531(4) . ? C1 C13 1.535(4) . ? C2 C3 1.185(3) . ? C3 C3 1.399(6) 3_675 ? C7 C8 1.377(4) . ? C7 C12 1.385(4) . ? C8 C9 1.383(5) . ? C9 C10 1.369(5) . ? C10 C11 1.353(5) . ? C11 C12 1.383(5) . ? C13 C14 1.379(4) . ? C13 C18 1.383(4) . ? C14 C15 1.373(4) . ? C15 C16 1.372(5) . ? C16 C17 1.379(5) . ? C17 C18 1.382(4) . ? C1A O2A 1.455(3) . ? C1A C9A 1.498(4) . ? C1A C6A 1.521(4) . ? C1A C5A 1.525(4) . ? O2A C3A 1.462(3) . ? C3A C10A 1.519(5) . ? C3A C11A 1.522(5) . ? C3A C8A 1.525(4) . ? C4A C5A 1.518(5) . ? C4A C8A 1.529(5) . ? C6A C7A 1.526(5) . ? C7A C8A 1.521(5) . ? 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 O1 C1 C2 109.1(2) . . ? O1 C1 C7 107.0(2) . . ? C2 C1 C7 109.8(2) . . ? O1 C1 C13 110.9(2) . . ? C2 C1 C13 110.7(2) . . ? C7 C1 C13 109.2(2) . . ? C3 C2 C1 178.6(3) . . ? C2 C3 C3 179.5(4) . 3_675 ? C8 C7 C12 117.8(3) . . ? C8 C7 C1 121.4(2) . . ? C12 C7 C1 120.8(3) . . ? C7 C8 C9 121.4(3) . . ? C10 C9 C8 119.8(4) . . ? C11 C10 C9 119.6(4) . . ? C10 C11 C12 121.2(4) . . ? C11 C12 C7 120.2(4) . . ? C14 C13 C18 118.6(3) . . ? C14 C13 C1 119.7(2) . . ? C18 C13 C1 121.6(3) . . ? C15 C14 C13 120.6(3) . . ? C16 C15 C14 120.8(4) . . ? C15 C16 C17 119.4(4) . . ? C16 C17 C18 119.8(3) . . ? C17 C18 C13 120.8(3) . . ? O2A C1A C9A 106.1(3) . . ? O2A C1A C6A 107.3(2) . . ? C9A C1A C6A 113.2(3) . . ? O2A C1A C5A 108.4(3) . . ? C9A C1A C5A 112.0(3) . . ? C6A C1A C5A 109.6(3) . . ? C1A O2A C3A 114.0(2) . . ? O2A C3A C10A 107.0(3) . . ? O2A C3A C11A 106.9(3) . . ? C10A C3A C11A 108.7(4) . . ? O2A C3A C8A 108.5(2) . . ? C10A C3A C8A 112.7(3) . . ? C11A C3A C8A 112.7(3) . . ? C5A C4A C8A 108.6(3) . . ? C4A C5A C1A 110.5(3) . . ? C1A C6A C7A 110.3(3) . . ? C8A C7A C6A 108.5(3) . . ? C7A C8A C3A 109.8(3) . . ? C7A C8A C4A 107.7(3) . . ? C3A C8A C4A 110.1(3) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.152 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.043