# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name V.Alexander _publ_contact_author_email valexander@rediffmail.com _publ_author_name V.Alexander # Attachment '- Crystal data of compound-2.cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 708245' #TrackingRef '- Crystal data of compound-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H30 O6' _chemical_formula_weight 522.57 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.7707(6) _cell_length_b 16.3646(5) _cell_length_c 18.2805(6) _cell_angle_alpha 83.202(2) _cell_angle_beta 66.0120(10) _cell_angle_gamma 73.704(2) _cell_volume 4137.2(2) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8082 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 21.15 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8988 _exptl_absorpt_correction_T_max 0.9830 _exptl_absorpt_process_details 'SADABS (Bruker 1999)' _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 'bruker axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 73977 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 24.44 _reflns_number_total 13594 _reflns_number_gt 8323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1175P)^2^+1.3869P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13594 _refine_ls_number_parameters 1065 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.2133 _refine_ls_wR_factor_gt 0.1698 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 C1A C 1.1977(2) 0.48471(19) 0.35946(16) 0.0558(7) Uani 1 1 d . . . C2A C 1.1053(2) 0.51405(17) 0.35970(16) 0.0532(7) Uani 1 1 d . . . C3A C 1.03940(18) 0.46520(17) 0.39739(16) 0.0503(6) Uani 1 1 d . . . C4A C 1.06545(19) 0.38678(17) 0.43381(16) 0.0504(6) Uani 1 1 d . . . C5A C 1.1583(2) 0.35797(17) 0.43131(16) 0.0530(7) Uani 1 1 d . . . C6A C 1.22433(19) 0.40720(19) 0.39587(17) 0.0571(7) Uani 1 1 d . . . C7A C 1.2704(2) 0.5360(2) 0.32157(18) 0.0701(9) Uani 1 1 d . . . H7AA H 1.3341 0.4987 0.2962 0.084 Uiso 1 1 calc R . . H7AB H 1.2552 0.5742 0.2813 0.084 Uiso 1 1 calc R . . C8A C 1.3376(2) 0.62207(19) 0.36891(19) 0.0615(7) Uani 1 1 d . . . C9A C 1.4099(2) 0.6252(2) 0.2946(2) 0.0790(10) Uani 1 1 d . . . H9A H 1.4117 0.6006 0.2504 0.095 Uiso 1 1 calc R . . C10A C 1.4787(3) 0.6651(3) 0.2867(2) 0.0969(12) Uani 1 1 d . . . H10A H 1.5275 0.6673 0.2367 0.116 Uiso 1 1 calc R . . C11A C 1.4773(3) 0.7018(3) 0.3508(3) 0.1052(14) Uani 1 1 d . B . C12A C 1.4056(3) 0.6970(3) 0.4253(3) 0.1026(14) Uani 1 1 d . . . H12A H 1.4049 0.7205 0.4695 0.123 Uiso 1 1 calc R . . C13A C 1.3355(2) 0.6580(2) 0.4346(2) 0.0789(10) Uani 1 1 d . . . H13A H 1.2869 0.6557 0.4847 0.095 Uiso 1 1 calc R . . C14A C 1.5548(4) 0.7415(5) 0.3378(4) 0.179(3) Uani 1 1 d D . . H14A H 1.5913 0.7581 0.2869 0.215 Uiso 1 1 calc R A 1 C15A C 0.9381(2) 0.49573(18) 0.40258(19) 0.0606(7) Uani 1 1 d . . . H15A H 0.8933 0.4957 0.4579 0.073 Uiso 1 1 calc R . . H15B H 0.9268 0.5533 0.3817 0.073 Uiso 1 1 calc R . . C16A C 0.8329(2) 0.44688(19) 0.36393(18) 0.0605(7) Uani 1 1 d . . . C17A C 0.7566(2) 0.5147(2) 0.3995(2) 0.0687(8) Uani 1 1 d . . . H17A H 0.7653 0.5592 0.4206 0.082 Uiso 1 1 calc R . . C18A C 0.6676(2) 0.5161(2) 0.4035(2) 0.0795(10) Uani 1 1 d . . . H18A H 0.6160 0.5619 0.4278 0.095 Uiso 1 1 calc R . . C19A C 0.6529(2) 0.4510(2) 0.3724(2) 0.0779(9) Uani 1 1 d . . . C20A C 0.7303(3) 0.3829(2) 0.3372(2) 0.0871(11) Uani 1 1 d . . . H20A H 0.7215 0.3385 0.3159 0.104 Uiso 1 1 calc R . . C21A C 0.8194(2) 0.3801(2) 0.3333(2) 0.0798(10) Uani 1 1 d . . . H21A H 0.8708 0.3337 0.3103 0.096 Uiso 1 1 calc R . . C22A C 0.5575(3) 0.4541(3) 0.3766(3) 0.1074(14) Uani 1 1 d . . . H22A H 0.5072 0.4993 0.4043 0.129 Uiso 1 1 calc R . . C23A C 1.1886(2) 0.27420(19) 0.46915(18) 0.0660(8) Uani 1 1 d . . . H23A H 1.1512 0.2359 0.4697 0.079 Uiso 1 1 calc R . . H23B H 1.2560 0.2476 0.4395 0.079 Uiso 1 1 calc R . . C24A C 1.2097(2) 0.23088(17) 0.59261(18) 0.0567(7) Uani 1 1 d . . . C25A C 1.1873(2) 0.25343(19) 0.67042(18) 0.0636(8) Uani 1 1 d . . . H25A H 1.1487 0.3072 0.6893 0.076 Uiso 1 1 calc R . . C26A C 1.2216(2) 0.1971(2) 0.71920(19) 0.0653(8) Uani 1 1 d . . . H26A H 1.2055 0.2122 0.7716 0.078 Uiso 1 1 calc R . . C27A C 1.2804(2) 0.11743(19) 0.6910(2) 0.0647(8) Uani 1 1 d . . . C28A C 1.3021(3) 0.0966(2) 0.6141(2) 0.0806(10) Uani 1 1 d . . . H28A H 1.3420 0.0433 0.5948 0.097 Uiso 1 1 calc R . . C29A C 1.2667(3) 0.15204(19) 0.5641(2) 0.0730(9) Uani 1 1 d . . . H29A H 1.2812 0.1362 0.5123 0.088 Uiso 1 1 calc R . . C30A C 1.3201(3) 0.0569(3) 0.7415(3) 0.0888(11) Uani 1 1 d . . . H30A H 1.3609 0.0052 0.7186 0.107 Uiso 1 1 calc R . . C31A C 1.3233(2) 0.3779(3) 0.3977(2) 0.0874(11) Uani 1 1 d . . . H31A H 1.3299 0.3240 0.4248 0.131 Uiso 1 1 calc R . . H31B H 1.3320 0.4190 0.4256 0.131 Uiso 1 1 calc R . . H31C H 1.3710 0.3721 0.3439 0.131 Uiso 1 1 calc R . . C32A C 1.0765(3) 0.5979(2) 0.3207(2) 0.0784(9) Uani 1 1 d . . . H32A H 1.1300 0.6228 0.2974 0.118 Uiso 1 1 calc R . . H32B H 1.0240 0.6357 0.3602 0.118 Uiso 1 1 calc R . . H32C H 1.0570 0.5884 0.2796 0.118 Uiso 1 1 calc R . . C33A C 0.9931(2) 0.33533(19) 0.47468(19) 0.0687(8) Uani 1 1 d . . . H33A H 1.0222 0.2841 0.4963 0.103 Uiso 1 1 calc R . . H33B H 0.9720 0.3210 0.4366 0.103 Uiso 1 1 calc R . . H33C H 0.9391 0.3681 0.5172 0.103 Uiso 1 1 calc R . . O1A O 1.26659(14) 0.58354(14) 0.38442(12) 0.0708(6) Uani 1 1 d . . . O2A O 1.5710(9) 0.7529(17) 0.4016(8) 0.211(9) Uani 0.60(3) 1 d PD B 1 O2A' O 1.531(2) 0.8138(15) 0.3771(15) 0.147(11) Uani 0.27(3) 1 d PD B 2 O3A O 0.92449(13) 0.43889(13) 0.35597(12) 0.0662(5) Uani 1 1 d . . . O4A O 0.5387(2) 0.4038(3) 0.3477(2) 0.1395(13) Uani 1 1 d . . . O5A O 1.17199(16) 0.29272(12) 0.54938(12) 0.0709(6) Uani 1 1 d . . . O6A O 1.3052(2) 0.0678(2) 0.8087(2) 0.1186(10) Uani 1 1 d . . . C1B C 0.61935(19) 0.35902(18) 0.01013(17) 0.0548(7) Uani 1 1 d . . . C2B C 0.64811(19) 0.29228(19) -0.04282(17) 0.0561(7) Uani 1 1 d . . . C3B C 0.64284(19) 0.21050(18) -0.01340(17) 0.0559(7) Uani 1 1 d . . . C4B C 0.6065(2) 0.19547(18) 0.06913(18) 0.0567(7) Uani 1 1 d . . . C5B C 0.58237(19) 0.26181(18) 0.12165(16) 0.0553(7) Uani 1 1 d . . . C6B C 0.58933(19) 0.34396(18) 0.09208(17) 0.0556(7) Uani 1 1 d . . . C7B C 0.6208(2) 0.44697(19) -0.0237(2) 0.0676(8) Uani 1 1 d . . . H7BA H 0.5935 0.4582 -0.0639 0.081 Uiso 1 1 calc R . . H7BB H 0.5831 0.4889 0.0184 0.081 Uiso 1 1 calc R . . C8B C 0.7389(2) 0.52064(19) -0.10654(18) 0.0631(8) Uani 1 1 d . . . C9B C 0.6737(3) 0.5839(2) -0.1270(2) 0.0779(9) Uani 1 1 d . . . H9BA H 0.6096 0.5829 -0.1075 0.093 Uiso 1 1 calc R . . C10B C 0.7048(4) 0.6494(2) -0.1772(2) 0.0905(11) Uani 1 1 d . . . H10B H 0.6611 0.6921 -0.1915 0.109 Uiso 1 1 calc R . . C11B C 0.7990(4) 0.6521(3) -0.2060(2) 0.0933(12) Uani 1 1 d . . . C12B C 0.8625(3) 0.5875(3) -0.1855(2) 0.0981(12) Uani 1 1 d . . . H12B H 0.9269 0.5876 -0.2057 0.118 Uiso 1 1 calc R . . C13B C 0.8330(3) 0.5230(2) -0.1361(2) 0.0794(9) Uani 1 1 d . . . H13B H 0.8771 0.4802 -0.1223 0.095 Uiso 1 1 calc R . . C14B C 0.8341(5) 0.7208(4) -0.2580(3) 0.136(2) Uani 1 1 d . . . H14B H 0.8983 0.7191 -0.2724 0.163 Uiso 1 1 calc R . . C15B C 0.6772(2) 0.1397(2) -0.0719(2) 0.0677(8) Uani 1 1 d . . . H15C H 0.7348 0.1458 -0.1172 0.081 Uiso 1 1 calc R . . H15D H 0.6919 0.0851 -0.0465 0.081 Uiso 1 1 calc R . . C16B C 0.6198(2) 0.09107(19) -0.15697(18) 0.0615(7) Uani 1 1 d . . . C17B C 0.7074(2) 0.0381(2) -0.1983(2) 0.0810(10) Uani 1 1 d . . . H17B H 0.7602 0.0369 -0.1872 0.097 Uiso 1 1 calc R . . C18B C 0.7164(3) -0.0133(2) -0.2564(2) 0.0899(11) Uani 1 1 d . . . H18B H 0.7762 -0.0489 -0.2849 0.108 Uiso 1 1 calc R . . C19B C 0.6405(3) -0.0138(2) -0.2737(2) 0.0741(9) Uani 1 1 d . . . C20B C 0.5543(3) 0.0386(3) -0.2325(3) 0.0978(12) Uani 1 1 d . . . H20B H 0.5017 0.0389 -0.2437 0.117 Uiso 1 1 calc R . . C21B C 0.5426(3) 0.0917(3) -0.1743(2) 0.0969(13) Uani 1 1 d . . . H21B H 0.4828 0.1278 -0.1467 0.116 Uiso 1 1 calc R . . C22B C 0.6539(4) -0.0716(3) -0.3350(2) 0.1016(13) Uani 1 1 d . . . H22B H 0.7165 -0.1025 -0.3634 0.122 Uiso 1 1 calc R . . C23B C 0.5544(2) 0.2435(2) 0.20966(17) 0.0674(8) Uani 1 1 d . . . H23C H 0.5124 0.2940 0.2405 0.081 Uiso 1 1 calc R . . H23D H 0.5212 0.1985 0.2255 0.081 Uiso 1 1 calc R . . C24B C 0.6387(2) 0.18675(19) 0.29589(18) 0.0617(7) Uani 1 1 d . . . C25B C 0.7258(3) 0.1622(2) 0.3039(2) 0.0790(9) Uani 1 1 d . . . H25B H 0.7810 0.1690 0.2609 0.095 Uiso 1 1 calc R . . C26B C 0.7321(3) 0.1281(2) 0.3737(2) 0.0837(10) Uani 1 1 d . . . H26B H 0.7916 0.1108 0.3775 0.100 Uiso 1 1 calc R . . C27B C 0.6506(3) 0.1190(2) 0.4392(2) 0.0781(10) Uani 1 1 d . . . C28B C 0.5637(3) 0.1458(2) 0.4314(2) 0.0795(9) Uani 1 1 d . . . H28B H 0.5082 0.1412 0.4752 0.095 Uiso 1 1 calc R . . C29B C 0.5563(2) 0.1792(2) 0.36082(19) 0.0712(8) Uani 1 1 d . . . H29B H 0.4969 0.1964 0.3569 0.085 Uiso 1 1 calc R . . C30B C 0.6553(4) 0.0796(3) 0.5136(3) 0.1043(13) Uani 1 1 d . . . H30B H 0.5978 0.0785 0.5565 0.125 Uiso 1 1 calc R . . C31B C 0.5654(3) 0.4139(2) 0.1497(2) 0.0797(9) Uani 1 1 d . . . H31D H 0.5732 0.4659 0.1205 0.120 Uiso 1 1 calc R . . H31E H 0.6077 0.3984 0.1777 0.120 Uiso 1 1 calc R . . H31F H 0.5002 0.4217 0.1875 0.120 Uiso 1 1 calc R . . C32B C 0.6838(3) 0.3084(3) -0.13239(19) 0.0840(10) Uani 1 1 d . . . H32D H 0.7005 0.2560 -0.1597 0.126 Uiso 1 1 calc R . . H32E H 0.7393 0.3304 -0.1494 0.126 Uiso 1 1 calc R . . H32F H 0.6342 0.3490 -0.1448 0.126 Uiso 1 1 calc R . . C33B C 0.5911(3) 0.1085(2) 0.1010(2) 0.0853(10) Uani 1 1 d . . . H33D H 0.6113 0.0712 0.0569 0.128 Uiso 1 1 calc R . . H33E H 0.5242 0.1140 0.1333 0.128 Uiso 1 1 calc R . . H33F H 0.6280 0.0854 0.1329 0.128 Uiso 1 1 calc R . . O1B O 0.71852(14) 0.45215(13) -0.05879(13) 0.0692(6) Uani 1 1 d . . . O2B O 0.7909(4) 0.7761(3) -0.2826(3) 0.192(2) Uani 1 1 d . . . O3B O 0.60189(14) 0.14457(14) -0.09797(13) 0.0751(6) Uani 1 1 d . . . O4B O 0.5944(3) -0.0828(3) -0.3518(2) 0.1515(14) Uani 1 1 d . . . O5B O 0.64165(14) 0.21747(14) 0.22282(12) 0.0706(6) Uani 1 1 d . . . O6B O 0.7297(3) 0.0480(2) 0.5231(2) 0.1363(12) Uani 1 1 d . . . C1C C 0.1079(2) -0.15342(19) 0.0337(2) 0.0623(8) Uani 1 1 d . . . C2C C 0.12211(18) -0.07633(19) -0.00350(17) 0.0567(7) Uani 1 1 d . . . C3C C 0.10241(19) -0.00610(18) 0.04296(18) 0.0568(7) Uani 1 1 d . . . C4C C 0.0603(2) -0.0109(2) 0.12702(18) 0.0613(8) Uani 1 1 d . . . C5C C 0.0399(2) -0.0871(2) 0.16308(18) 0.0638(8) Uani 1 1 d . . . C6C C 0.0658(2) -0.1594(2) 0.1173(2) 0.0658(8) Uani 1 1 d . . . C7C C 0.1450(2) -0.2326(2) -0.0156(2) 0.0781(10) Uani 1 1 d . . . H7CA H 0.1910 -0.2229 -0.0684 0.094 Uiso 1 1 calc R . . H7CB H 0.1777 -0.2789 0.0095 0.094 Uiso 1 1 calc R . . C8C C 0.0892(2) -0.3310(2) -0.0592(2) 0.0739(9) Uani 1 1 d . . . C9C C 0.1787(3) -0.3810(3) -0.0960(3) 0.1141(16) Uani 1 1 d . . . H9CA H 0.2316 -0.3649 -0.0978 0.137 Uiso 1 1 calc R . . C10C C 0.1912(3) -0.4559(3) -0.1311(3) 0.1202(17) Uani 1 1 d . . . H10C H 0.2532 -0.4899 -0.1556 0.144 Uiso 1 1 calc R . . C11C C 0.1183(3) -0.4817(2) -0.1313(2) 0.0865(10) Uani 1 1 d . . . C12C C 0.0286(3) -0.4333(3) -0.0903(4) 0.135(2) Uani 1 1 d . . . H12C H -0.0241 -0.4516 -0.0858 0.162 Uiso 1 1 calc R . . C13C C 0.0136(3) -0.3576(3) -0.0552(3) 0.131(2) Uani 1 1 d . . . H13C H -0.0486 -0.3248 -0.0288 0.157 Uiso 1 1 calc R . . C14C C 0.1371(4) -0.5613(3) -0.1718(3) 0.1182(15) Uani 1 1 d . . . H14C H 0.2007 -0.5919 -0.1968 0.142 Uiso 1 1 calc R . . C15C C 0.1335(2) 0.07289(19) 0.0047(2) 0.0669(8) Uani 1 1 d . . . H15E H 0.1529 0.0718 -0.0529 0.080 Uiso 1 1 calc R . . H15F H 0.0817 0.1234 0.0258 0.080 Uiso 1 1 calc R . . C16C C 0.2538(2) 0.13801(19) 0.0052(2) 0.0670(8) Uani 1 1 d . . . C17C C 0.2344(3) 0.2040(2) -0.0434(2) 0.0808(10) Uani 1 1 d . . . H17C H 0.1894 0.2070 -0.0650 0.097 Uiso 1 1 calc R . . C18C C 0.2842(3) 0.2673(2) -0.0600(2) 0.0907(11) Uani 1 1 d . . . H18C H 0.2720 0.3129 -0.0930 0.109 Uiso 1 1 calc R . . C19C C 0.3508(3) 0.2629(2) -0.0284(2) 0.0780(10) Uani 1 1 d . . . C20C C 0.3672(3) 0.1971(2) 0.0214(3) 0.0897(11) Uani 1 1 d . . . H20C H 0.4109 0.1946 0.0442 0.108 Uiso 1 1 calc R . . C21C C 0.3197(3) 0.1354(2) 0.0379(3) 0.0881(11) Uani 1 1 d . . . H21C H 0.3316 0.0906 0.0717 0.106 Uiso 1 1 calc R . . C22C C 0.4057(3) 0.3273(3) -0.0481(3) 0.1051(14) Uani 1 1 d . . . H22C H 0.4478 0.3209 -0.0228 0.126 Uiso 1 1 calc R . . C23C C -0.0053(2) -0.0923(3) 0.25261(19) 0.0802(10) Uani 1 1 d . . . H23E H -0.0441 -0.0367 0.2749 0.096 Uiso 1 1 calc R . . H23F H -0.0460 -0.1314 0.2690 0.096 Uiso 1 1 calc R . . C24C C 0.0504(2) -0.1214(2) 0.3601(2) 0.0723(9) Uani 1 1 d . . . C25C C -0.0395(2) -0.0898(2) 0.4173(2) 0.0741(9) Uani 1 1 d . . . H25C H -0.0919 -0.0684 0.4030 0.089 Uiso 1 1 calc R . . C26C C -0.0511(3) -0.0903(2) 0.4962(2) 0.0777(9) Uani 1 1 d . . . H26C H -0.1121 -0.0687 0.5348 0.093 Uiso 1 1 calc R . . C27C C 0.0238(3) -0.1213(2) 0.5199(2) 0.0761(9) Uani 1 1 d . . . C28C C 0.1138(3) -0.1532(3) 0.4612(3) 0.0923(11) Uani 1 1 d . . . H28C H 0.1659 -0.1754 0.4756 0.111 Uiso 1 1 calc R . . C29C C 0.1274(3) -0.1526(3) 0.3822(2) 0.0904(11) Uani 1 1 d . . . H29C H 0.1886 -0.1733 0.3435 0.109 Uiso 1 1 calc R . . C30C C 0.0036(4) -0.1212(3) 0.6064(3) 0.1073(14) Uani 1 1 d . . . H30C H -0.0582 -0.0950 0.6413 0.129 Uiso 1 1 calc R . . C31C C 0.1569(2) -0.0684(2) -0.09333(19) 0.0807(10) Uani 1 1 d . . . H31G H 0.1626 -0.0115 -0.1092 0.121 Uiso 1 1 calc R . . H31H H 0.1118 -0.0807 -0.1105 0.121 Uiso 1 1 calc R . . H31I H 0.2184 -0.1079 -0.1175 0.121 Uiso 1 1 calc R . . C32C C 0.0386(3) 0.0653(2) 0.1764(2) 0.0847(10) Uani 1 1 d . . . H32G H 0.0103 0.0516 0.2322 0.127 Uiso 1 1 calc R . . H32H H -0.0053 0.1121 0.1631 0.127 Uiso 1 1 calc R . . H32I H 0.0971 0.0807 0.1655 0.127 Uiso 1 1 calc R . . C33C C 0.0495(3) -0.2429(2) 0.1564(3) 0.1007(12) Uani 1 1 d . . . H33G H 0.0715 -0.2851 0.1159 0.151 Uiso 1 1 calc R . . H33H H -0.0178 -0.2363 0.1877 0.151 Uiso 1 1 calc R . . H33I H 0.0843 -0.2608 0.1905 0.151 Uiso 1 1 calc R . . O1C O 0.06741(15) -0.25539(14) -0.02291(15) 0.0819(7) Uani 1 1 d . . . O2C O 0.0776(3) -0.5887(3) -0.1747(3) 0.1756(18) Uani 1 1 d . . . O3C O 0.21312(15) 0.07192(13) 0.02431(15) 0.0761(6) Uani 1 1 d . . . O4C O 0.4032(3) 0.3849(2) -0.0911(2) 0.1328(13) Uani 1 1 d . . . O5C O 0.07173(16) -0.12220(18) 0.27990(14) 0.0894(7) Uani 1 1 d . . . O6C O 0.0615(3) -0.1525(3) 0.6329(2) 0.1494(13) Uani 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 C1A 0.0534(17) 0.0645(18) 0.0529(16) -0.0033(14) -0.0176(13) -0.0242(14) C2A 0.0629(18) 0.0486(15) 0.0541(16) 0.0000(13) -0.0250(14) -0.0200(13) C3A 0.0515(16) 0.0483(15) 0.0552(16) -0.0053(13) -0.0232(13) -0.0137(12) C4A 0.0536(16) 0.0507(16) 0.0509(15) -0.0066(13) -0.0213(13) -0.0159(12) C5A 0.0560(17) 0.0486(15) 0.0534(16) -0.0076(13) -0.0225(13) -0.0073(13) C6A 0.0471(16) 0.0694(19) 0.0545(16) -0.0126(14) -0.0191(13) -0.0107(14) C7A 0.070(2) 0.092(2) 0.0595(18) -0.0007(17) -0.0226(16) -0.0417(18) C8A 0.0567(18) 0.0601(18) 0.071(2) 0.0016(15) -0.0238(16) -0.0224(14) C9A 0.078(2) 0.105(3) 0.067(2) 0.0092(19) -0.0256(18) -0.052(2) C10A 0.087(3) 0.127(3) 0.080(3) -0.001(2) -0.013(2) -0.063(3) C11A 0.083(3) 0.117(3) 0.116(3) -0.030(3) -0.009(2) -0.060(2) C12A 0.086(3) 0.112(3) 0.113(3) -0.049(3) -0.014(2) -0.048(2) C13A 0.065(2) 0.082(2) 0.083(2) -0.0231(19) -0.0094(17) -0.0296(17) C14A 0.146(5) 0.236(7) 0.183(6) -0.090(5) -0.015(4) -0.129(5) C15A 0.0578(17) 0.0540(17) 0.078(2) -0.0074(15) -0.0339(15) -0.0131(13) C16A 0.0533(17) 0.0668(19) 0.0700(19) -0.0039(15) -0.0308(15) -0.0167(15) C17A 0.0590(19) 0.0629(19) 0.090(2) -0.0162(17) -0.0341(17) -0.0102(15) C18A 0.0537(19) 0.085(2) 0.099(3) -0.019(2) -0.0333(18) -0.0029(16) C19A 0.060(2) 0.098(3) 0.087(2) -0.010(2) -0.0362(18) -0.0223(19) C20A 0.076(2) 0.094(3) 0.109(3) -0.028(2) -0.044(2) -0.025(2) C21A 0.063(2) 0.078(2) 0.105(3) -0.027(2) -0.0366(19) -0.0119(17) C22A 0.074(3) 0.139(4) 0.128(4) -0.025(3) -0.051(3) -0.028(2) C23A 0.077(2) 0.0556(18) 0.0647(19) -0.0097(15) -0.0344(16) -0.0030(15) C24A 0.0580(17) 0.0467(16) 0.0655(19) 0.0009(14) -0.0280(15) -0.0084(13) C25A 0.0628(18) 0.0541(17) 0.066(2) -0.0026(15) -0.0234(15) -0.0050(14) C26A 0.0636(19) 0.068(2) 0.0632(19) 0.0057(16) -0.0247(15) -0.0172(16) C27A 0.069(2) 0.0578(19) 0.078(2) 0.0108(16) -0.0377(17) -0.0234(15) C28A 0.095(3) 0.0450(17) 0.109(3) -0.0076(18) -0.056(2) -0.0014(16) C29A 0.096(2) 0.0485(18) 0.081(2) -0.0119(16) -0.050(2) -0.0009(16) C30A 0.096(3) 0.080(3) 0.095(3) 0.017(2) -0.050(2) -0.018(2) C31A 0.0553(19) 0.107(3) 0.096(3) -0.013(2) -0.0313(18) -0.0072(18) C32A 0.094(2) 0.063(2) 0.086(2) 0.0168(17) -0.042(2) -0.0299(18) C33A 0.076(2) 0.0591(18) 0.074(2) 0.0070(15) -0.0268(17) -0.0291(16) O1A 0.0611(13) 0.0852(15) 0.0705(13) -0.0086(11) -0.0157(10) -0.0373(11) O2A 0.116(8) 0.29(2) 0.224(12) -0.145(12) 0.023(6) -0.118(11) O2A' 0.123(16) 0.165(18) 0.165(15) -0.055(15) -0.016(12) -0.094(13) O3A 0.0508(11) 0.0733(13) 0.0809(14) -0.0225(11) -0.0290(10) -0.0117(9) O4A 0.095(2) 0.179(3) 0.179(3) -0.035(3) -0.067(2) -0.053(2) O5A 0.0872(15) 0.0537(12) 0.0644(13) -0.0073(10) -0.0379(11) 0.0087(10) O6A 0.132(3) 0.121(2) 0.096(2) 0.0301(18) -0.058(2) -0.0141(18) C1B 0.0455(15) 0.0575(17) 0.0615(18) 0.0029(14) -0.0202(13) -0.0157(13) C2B 0.0510(16) 0.0672(19) 0.0564(17) 0.0022(15) -0.0245(13) -0.0203(14) C3B 0.0536(16) 0.0601(18) 0.0610(18) -0.0067(14) -0.0281(14) -0.0140(13) C4B 0.0559(17) 0.0550(17) 0.0662(19) 0.0036(14) -0.0301(15) -0.0169(13) C5B 0.0498(16) 0.0635(18) 0.0540(17) -0.0006(14) -0.0211(13) -0.0153(13) C6B 0.0470(15) 0.0569(17) 0.0637(19) -0.0071(14) -0.0220(14) -0.0111(13) C7B 0.0522(18) 0.0620(19) 0.088(2) 0.0095(16) -0.0280(16) -0.0174(14) C8B 0.0642(19) 0.0566(18) 0.0657(19) 0.0000(15) -0.0195(15) -0.0207(15) C9B 0.078(2) 0.067(2) 0.087(2) 0.0042(19) -0.0335(19) -0.0159(18) C10B 0.129(4) 0.061(2) 0.079(2) 0.0054(19) -0.045(2) -0.018(2) C11B 0.139(4) 0.071(3) 0.068(2) 0.0026(19) -0.026(2) -0.047(3) C12B 0.102(3) 0.091(3) 0.097(3) 0.006(2) -0.021(2) -0.048(3) C13B 0.072(2) 0.076(2) 0.088(2) 0.0053(19) -0.0232(19) -0.0302(18) C14B 0.213(6) 0.084(3) 0.093(3) 0.011(3) -0.038(4) -0.052(4) C15B 0.0615(18) 0.073(2) 0.074(2) -0.0153(16) -0.0335(16) -0.0095(15) C16B 0.0621(19) 0.0619(18) 0.0654(19) -0.0097(15) -0.0256(15) -0.0185(15) C17B 0.070(2) 0.092(2) 0.086(2) -0.030(2) -0.0370(19) -0.0060(19) C18B 0.087(3) 0.090(3) 0.090(3) -0.036(2) -0.038(2) -0.001(2) C19B 0.095(3) 0.066(2) 0.069(2) -0.0059(17) -0.032(2) -0.0311(19) C20B 0.084(3) 0.119(3) 0.110(3) -0.034(3) -0.046(2) -0.030(2) C21B 0.066(2) 0.118(3) 0.116(3) -0.052(3) -0.040(2) -0.009(2) C22B 0.137(4) 0.098(3) 0.095(3) -0.014(2) -0.056(3) -0.048(3) C23B 0.0589(18) 0.082(2) 0.0589(18) 0.0010(16) -0.0211(15) -0.0175(16) C24B 0.067(2) 0.0635(18) 0.0556(19) -0.0086(14) -0.0240(16) -0.0143(15) C25B 0.071(2) 0.098(3) 0.075(2) -0.0057(19) -0.0319(18) -0.0261(19) C26B 0.090(3) 0.088(3) 0.091(3) -0.006(2) -0.056(2) -0.017(2) C27B 0.104(3) 0.068(2) 0.073(2) -0.0058(17) -0.047(2) -0.0156(19) C28B 0.089(3) 0.076(2) 0.066(2) -0.0012(17) -0.0254(19) -0.0164(19) C29B 0.072(2) 0.075(2) 0.063(2) -0.0035(16) -0.0268(17) -0.0111(16) C30B 0.134(4) 0.099(3) 0.092(3) 0.008(2) -0.066(3) -0.019(3) C31B 0.080(2) 0.076(2) 0.080(2) -0.0183(18) -0.0233(18) -0.0193(18) C32B 0.098(3) 0.103(3) 0.061(2) 0.0078(19) -0.0331(19) -0.040(2) C33B 0.104(3) 0.065(2) 0.093(3) 0.0122(19) -0.043(2) -0.0288(19) O1B 0.0547(12) 0.0624(13) 0.0895(15) 0.0150(11) -0.0276(11) -0.0207(10) O2B 0.330(7) 0.079(2) 0.133(3) 0.018(2) -0.066(4) -0.047(3) O3B 0.0611(13) 0.0823(15) 0.0880(15) -0.0329(12) -0.0351(11) -0.0052(11) O4B 0.169(3) 0.180(4) 0.141(3) -0.054(3) -0.059(3) -0.079(3) O5B 0.0603(13) 0.0957(16) 0.0563(13) 0.0003(11) -0.0236(10) -0.0198(11) O6B 0.162(3) 0.148(3) 0.124(3) 0.025(2) -0.093(3) -0.034(2) C1C 0.0447(16) 0.0631(19) 0.083(2) -0.0117(16) -0.0256(15) -0.0139(13) C2C 0.0432(15) 0.0671(19) 0.0627(18) -0.0091(15) -0.0207(13) -0.0150(13) C3C 0.0478(16) 0.0588(17) 0.0673(19) -0.0049(14) -0.0253(14) -0.0125(13) C4C 0.0495(16) 0.070(2) 0.066(2) -0.0121(16) -0.0238(15) -0.0100(14) C5C 0.0459(16) 0.081(2) 0.0627(19) 0.0026(17) -0.0194(14) -0.0180(15) C6C 0.0501(17) 0.067(2) 0.082(2) 0.0028(17) -0.0259(16) -0.0188(14) C7C 0.0538(18) 0.071(2) 0.113(3) -0.0257(19) -0.0278(18) -0.0181(15) C8C 0.065(2) 0.067(2) 0.100(2) -0.0196(18) -0.0392(19) -0.0136(16) C9C 0.070(2) 0.102(3) 0.173(4) -0.065(3) -0.043(3) -0.008(2) C10C 0.082(3) 0.106(3) 0.171(5) -0.068(3) -0.045(3) 0.000(2) C11C 0.095(3) 0.078(2) 0.099(3) -0.022(2) -0.047(2) -0.017(2) C12C 0.091(3) 0.129(4) 0.200(5) -0.078(4) -0.049(3) -0.032(3) C13C 0.071(3) 0.120(4) 0.207(5) -0.082(4) -0.046(3) -0.014(2) C14C 0.134(4) 0.119(4) 0.127(4) -0.032(3) -0.059(3) -0.046(3) C15C 0.070(2) 0.0601(18) 0.077(2) 0.0019(16) -0.0377(17) -0.0138(15) C16C 0.069(2) 0.0471(17) 0.081(2) -0.0043(16) -0.0242(17) -0.0154(15) C17C 0.100(3) 0.069(2) 0.082(2) 0.0025(19) -0.039(2) -0.0306(19) C18C 0.121(3) 0.062(2) 0.077(2) 0.0087(18) -0.028(2) -0.025(2) C19C 0.071(2) 0.074(2) 0.078(2) -0.0184(19) -0.0084(19) -0.0258(18) C20C 0.084(3) 0.079(2) 0.115(3) 0.000(2) -0.041(2) -0.030(2) C21C 0.086(2) 0.075(2) 0.121(3) 0.014(2) -0.054(2) -0.032(2) C22C 0.112(3) 0.080(3) 0.102(3) -0.023(3) -0.005(2) -0.040(2) C23C 0.062(2) 0.107(3) 0.069(2) 0.0070(19) -0.0232(17) -0.0247(19) C24C 0.070(2) 0.078(2) 0.071(2) 0.0107(17) -0.0286(18) -0.0239(17) C25C 0.068(2) 0.081(2) 0.077(2) 0.0109(18) -0.0291(18) -0.0268(17) C26C 0.086(2) 0.075(2) 0.074(2) 0.0041(18) -0.0274(19) -0.0304(19) C27C 0.094(3) 0.065(2) 0.084(2) 0.0063(18) -0.042(2) -0.0331(19) C28C 0.096(3) 0.098(3) 0.102(3) 0.013(2) -0.058(3) -0.028(2) C29C 0.071(2) 0.112(3) 0.085(3) 0.007(2) -0.032(2) -0.019(2) C30C 0.140(4) 0.102(3) 0.123(4) 0.015(3) -0.092(3) -0.041(3) C31C 0.074(2) 0.101(3) 0.070(2) -0.0166(19) -0.0239(18) -0.0276(19) C32C 0.081(2) 0.092(3) 0.080(2) -0.028(2) -0.0276(19) -0.0154(19) C33C 0.091(3) 0.088(3) 0.121(3) 0.021(2) -0.036(2) -0.039(2) O1C 0.0594(13) 0.0694(14) 0.126(2) -0.0334(13) -0.0424(13) -0.0071(10) O2C 0.165(4) 0.153(3) 0.219(5) -0.087(3) -0.057(3) -0.049(3) O3C 0.0716(14) 0.0580(13) 0.1125(18) 0.0132(12) -0.0486(13) -0.0242(11) O4C 0.184(3) 0.079(2) 0.114(2) 0.0022(18) -0.019(2) -0.063(2) O5C 0.0628(14) 0.128(2) 0.0692(15) 0.0063(14) -0.0264(12) -0.0143(13) O6C 0.161(3) 0.189(4) 0.109(2) -0.009(2) -0.061(2) -0.044(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 C1A C2A 1.399(4) . ? C1A C6A 1.399(4) . ? C1A C7A 1.501(4) . ? C2A C3A 1.396(4) . ? C2A C32A 1.510(4) . ? C3A C4A 1.408(4) . ? C3A C15A 1.501(4) . ? C4A C5A 1.390(4) . ? C4A C33A 1.505(4) . ? C5A C6A 1.397(4) . ? C5A C23A 1.504(4) . ? C6A C31A 1.513(4) . ? C7A O1A 1.435(3) . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C8A O1A 1.353(3) . ? C8A C9A 1.380(4) . ? C8A C13A 1.383(4) . ? C9A C10A 1.368(5) . ? C9A H9A 0.9300 . ? C10A C11A 1.368(5) . ? C10A H10A 0.9300 . ? C11A C12A 1.383(5) . ? C11A C14A 1.463(6) . ? C12A C13A 1.369(5) . ? C12A H12A 0.9300 . ? C13A H13A 0.9300 . ? C14A O2A 1.336(12) . ? C14A O2A' 1.337(14) . ? C14A H14A 0.9300 . ? C15A O3A 1.444(3) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A O3A 1.361(3) . ? C16A C17A 1.374(4) . ? C16A C21A 1.386(4) . ? C17A C18A 1.368(4) . ? C17A H17A 0.9300 . ? C18A C19A 1.379(5) . ? C18A H18A 0.9300 . ? C19A C20A 1.383(5) . ? C19A C22A 1.461(5) . ? C20A C21A 1.367(4) . ? C20A H20A 0.9300 . ? C21A H21A 0.9300 . ? C22A O4A 1.187(5) . ? C22A H22A 0.9300 . ? C23A O5A 1.435(3) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A O5A 1.363(3) . ? C24A C29A 1.368(4) . ? C24A C25A 1.388(4) . ? C25A C26A 1.362(4) . ? C25A H25A 0.9300 . ? C26A C27A 1.384(4) . ? C26A H26A 0.9300 . ? C27A C28A 1.367(5) . ? C27A C30A 1.460(5) . ? C28A C29A 1.380(4) . ? C28A H28A 0.9300 . ? C29A H29A 0.9300 . ? C30A O6A 1.179(4) . ? C30A H30A 0.9300 . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C1B C6B 1.390(4) . ? C1B C2B 1.397(4) . ? C1B C7B 1.500(4) . ? C2B C3B 1.394(4) . ? C2B C32B 1.516(4) . ? C3B C4B 1.398(4) . ? C3B C15B 1.500(4) . ? C4B C5B 1.401(4) . ? C4B C33B 1.518(4) . ? C5B C6B 1.405(4) . ? C5B C23B 1.502(4) . ? C6B C31B 1.510(4) . ? C7B O1B 1.432(3) . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C8B O1B 1.365(3) . ? C8B C13B 1.368(4) . ? C8B C9B 1.376(4) . ? C9B C10B 1.388(5) . ? C9B H9BA 0.9300 . ? C10B C11B 1.371(6) . ? C10B H10B 0.9300 . ? C11B C12B 1.371(6) . ? C11B C14B 1.464(6) . ? C12B C13B 1.362(5) . ? C12B H12B 0.9300 . ? C13B H13B 0.9300 . ? C14B O2B 1.137(7) . ? C14B H14B 0.9300 . ? C15B O3B 1.429(3) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B O3B 1.359(3) . ? C16B C17B 1.365(4) . ? C16B C21B 1.373(4) . ? C17B C18B 1.371(5) . ? C17B H17B 0.9300 . ? C18B C19B 1.357(5) . ? C18B H18B 0.9300 . ? C19B C20B 1.348(5) . ? C19B C22B 1.463(5) . ? C20B C21B 1.375(5) . ? C20B H20B 0.9300 . ? C21B H21B 0.9300 . ? C22B O4B 1.165(5) . ? C22B H22B 0.9300 . ? C23B O5B 1.431(3) . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? C24B O5B 1.357(3) . ? C24B C25B 1.382(4) . ? C24B C29B 1.383(4) . ? C25B C26B 1.361(5) . ? C25B H25B 0.9300 . ? C26B C27B 1.386(5) . ? C26B H26B 0.9300 . ? C27B C28B 1.379(5) . ? C27B C30B 1.454(5) . ? C28B C29B 1.377(5) . ? C28B H28B 0.9300 . ? C29B H29B 0.9300 . ? C30B O6B 1.216(5) . ? C30B H30B 0.9300 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33B H33D 0.9600 . ? C33B H33E 0.9600 . ? C33B H33F 0.9600 . ? C1C C2C 1.392(4) . ? C1C C6C 1.400(4) . ? C1C C7C 1.502(4) . ? C2C C3C 1.398(4) . ? C2C C31C 1.507(4) . ? C3C C4C 1.407(4) . ? C3C C15C 1.505(4) . ? C4C C5C 1.397(4) . ? C4C C32C 1.504(4) . ? C5C C6C 1.397(4) . ? C5C C23C 1.499(4) . ? C6C C33C 1.504(5) . ? C7C O1C 1.434(4) . ? C7C H7CA 0.9700 . ? C7C H7CB 0.9700 . ? C8C C9C 1.351(5) . ? C8C C13C 1.352(5) . ? C8C O1C 1.364(4) . ? C9C C10C 1.378(5) . ? C9C H9CA 0.9300 . ? C10C C11C 1.333(5) . ? C10C H10C 0.9300 . ? C11C C12C 1.356(6) . ? C11C C14C 1.471(6) . ? C12C C13C 1.378(6) . ? C12C H12C 0.9300 . ? C13C H13C 0.9300 . ? C14C O2C 1.170(5) . ? C14C H14C 0.9300 . ? C15C O3C 1.435(3) . ? C15C H15E 0.9700 . ? C15C H15F 0.9700 . ? C16C O3C 1.349(4) . ? C16C C17C 1.363(5) . ? C16C C21C 1.383(5) . ? C17C C18C 1.403(5) . ? C17C H17C 0.9300 . ? C18C C19C 1.372(5) . ? C18C H18C 0.9300 . ? C19C C20C 1.364(5) . ? C19C C22C 1.469(5) . ? C20C C21C 1.358(5) . ? C20C H20C 0.9300 . ? C21C H21C 0.9300 . ? C22C O4C 1.156(5) . ? C22C H22C 0.9300 . ? C23C O5C 1.437(4) . ? C23C H23E 0.9700 . ? C23C H23F 0.9700 . ? C24C O5C 1.366(4) . ? C24C C25C 1.372(5) . ? C24C C29C 1.380(5) . ? C25C C26C 1.378(5) . ? C25C H25C 0.9300 . ? C26C C27C 1.366(5) . ? C26C H26C 0.9300 . ? C27C C28C 1.384(5) . ? C27C C30C 1.481(6) . ? C28C C29C 1.369(5) . ? C28C H28C 0.9300 . ? C29C H29C 0.9300 . ? C30C O6C 1.170(5) . ? C30C H30C 0.9300 . ? C31C H31G 0.9600 . ? C31C H31H 0.9600 . ? C31C H31I 0.9600 . ? C32C H32G 0.9600 . ? C32C H32H 0.9600 . ? C32C H32I 0.9600 . ? C33C H33G 0.9600 . ? C33C H33H 0.9600 . ? C33C H33I 0.9600 . ? 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 C2A C1A C6A 120.7(2) . . ? C2A C1A C7A 121.1(3) . . ? C6A C1A C7A 118.2(3) . . ? C3A C2A C1A 119.1(2) . . ? C3A C2A C32A 120.2(3) . . ? C1A C2A C32A 120.7(3) . . ? C2A C3A C4A 120.8(2) . . ? C2A C3A C15A 121.2(2) . . ? C4A C3A C15A 118.0(2) . . ? C5A C4A C3A 119.1(2) . . ? C5A C4A C33A 120.9(3) . . ? C3A C4A C33A 120.0(2) . . ? C4A C5A C6A 120.8(3) . . ? C4A C5A C23A 120.4(3) . . ? C6A C5A C23A 118.7(3) . . ? C5A C6A C1A 119.4(2) . . ? C5A C6A C31A 120.5(3) . . ? C1A C6A C31A 120.1(3) . . ? O1A C7A C1A 106.9(2) . . ? O1A C7A H7AA 110.3 . . ? C1A C7A H7AA 110.3 . . ? O1A C7A H7AB 110.3 . . ? C1A C7A H7AB 110.3 . . ? H7AA C7A H7AB 108.6 . . ? O1A C8A C9A 124.6(3) . . ? O1A C8A C13A 115.1(3) . . ? C9A C8A C13A 120.4(3) . . ? C10A C9A C8A 119.1(3) . . ? C10A C9A H9A 120.5 . . ? C8A C9A H9A 120.5 . . ? C9A C10A C11A 121.5(3) . . ? C9A C10A H10A 119.3 . . ? C11A C10A H10A 119.3 . . ? C10A C11A C12A 119.0(3) . . ? C10A C11A C14A 118.1(4) . . ? C12A C11A C14A 122.9(4) . . ? C13A C12A C11A 120.6(4) . . ? C13A C12A H12A 119.7 . . ? C11A C12A H12A 119.7 . . ? C12A C13A C8A 119.5(3) . . ? C12A C13A H13A 120.3 . . ? C8A C13A H13A 120.3 . . ? O2A C14A O2A' 51.9(10) . . ? O2A C14A C11A 117.6(8) . . ? O2A' C14A C11A 116.9(11) . . ? O2A C14A H14A 121.2 . . ? O2A' C14A H14A 99.1 . . ? C11A C14A H14A 121.2 . . ? O3A C15A C3A 108.0(2) . . ? O3A C15A H15A 110.1 . . ? C3A C15A H15A 110.1 . . ? O3A C15A H15B 110.1 . . ? C3A C15A H15B 110.1 . . ? H15A C15A H15B 108.4 . . ? O3A C16A C17A 124.5(3) . . ? O3A C16A C21A 115.3(3) . . ? C17A C16A C21A 120.2(3) . . ? C18A C17A C16A 119.4(3) . . ? C18A C17A H17A 120.3 . . ? C16A C17A H17A 120.3 . . ? C17A C18A C19A 121.4(3) . . ? C17A C18A H18A 119.3 . . ? C19A C18A H18A 119.3 . . ? C18A C19A C20A 118.6(3) . . ? C18A C19A C22A 120.6(3) . . ? C20A C19A C22A 120.8(3) . . ? C21A C20A C19A 120.7(3) . . ? C21A C20A H20A 119.6 . . ? C19A C20A H20A 119.6 . . ? C20A C21A C16A 119.7(3) . . ? C20A C21A H21A 120.1 . . ? C16A C21A H21A 120.1 . . ? O4A C22A C19A 125.6(4) . . ? O4A C22A H22A 117.2 . . ? C19A C22A H22A 117.2 . . ? O5A C23A C5A 106.5(2) . . ? O5A C23A H23A 110.4 . . ? C5A C23A H23A 110.4 . . ? O5A C23A H23B 110.4 . . ? C5A C23A H23B 110.4 . . ? H23A C23A H23B 108.6 . . ? O5A C24A C29A 124.7(3) . . ? O5A C24A C25A 114.9(2) . . ? C29A C24A C25A 120.4(3) . . ? C26A C25A C24A 120.3(3) . . ? C26A C25A H25A 119.9 . . ? C24A C25A H25A 119.9 . . ? C25A C26A C27A 120.2(3) . . ? C25A C26A H26A 119.9 . . ? C27A C26A H26A 119.9 . . ? C28A C27A C26A 118.7(3) . . ? C28A C27A C30A 120.2(3) . . ? C26A C27A C30A 121.1(3) . . ? C27A C28A C29A 122.1(3) . . ? C27A C28A H28A 118.9 . . ? C29A C28A H28A 118.9 . . ? C24A C29A C28A 118.3(3) . . ? C24A C29A H29A 120.8 . . ? C28A C29A H29A 120.8 . . ? O6A C30A C27A 125.8(4) . . ? O6A C30A H30A 117.1 . . ? C27A C30A H30A 117.1 . . ? C6A C31A H31A 109.5 . . ? C6A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C6A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C2A C32A H32A 109.5 . . ? C2A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C2A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C4A C33A H33A 109.5 . . ? C4A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C4A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C8A O1A C7A 118.4(2) . . ? C16A O3A C15A 117.0(2) . . ? C24A O5A C23A 118.9(2) . . ? C6B C1B C2B 120.5(3) . . ? C6B C1B C7B 121.2(3) . . ? C2B C1B C7B 118.3(3) . . ? C3B C2B C1B 120.0(3) . . ? C3B C2B C32B 119.6(3) . . ? C1B C2B C32B 120.4(3) . . ? C2B C3B C4B 120.1(3) . . ? C2B C3B C15B 118.7(3) . . ? C4B C3B C15B 121.1(3) . . ? C3B C4B C5B 119.4(3) . . ? C3B C4B C33B 119.9(3) . . ? C5B C4B C33B 120.7(3) . . ? C4B C5B C6B 120.5(3) . . ? C4B C5B C23B 119.5(3) . . ? C6B C5B C23B 119.9(3) . . ? C1B C6B C5B 119.3(3) . . ? C1B C6B C31B 121.2(3) . . ? C5B C6B C31B 119.5(3) . . ? O1B C7B C1B 108.1(2) . . ? O1B C7B H7BA 110.1 . . ? C1B C7B H7BA 110.1 . . ? O1B C7B H7BB 110.1 . . ? C1B C7B H7BB 110.1 . . ? H7BA C7B H7BB 108.4 . . ? O1B C8B C13B 114.9(3) . . ? O1B C8B C9B 125.3(3) . . ? C13B C8B C9B 119.7(3) . . ? C8B C9B C10B 119.1(4) . . ? C8B C9B H9BA 120.4 . . ? C10B C9B H9BA 120.4 . . ? C11B C10B C9B 121.1(4) . . ? C11B C10B H10B 119.5 . . ? C9B C10B H10B 119.5 . . ? C12B C11B C10B 118.4(4) . . ? C12B C11B C14B 119.0(5) . . ? C10B C11B C14B 122.6(5) . . ? C13B C12B C11B 121.3(4) . . ? C13B C12B H12B 119.4 . . ? C11B C12B H12B 119.4 . . ? C12B C13B C8B 120.4(4) . . ? C12B C13B H13B 119.8 . . ? C8B C13B H13B 119.8 . . ? O2B C14B C11B 126.6(7) . . ? O2B C14B H14B 116.7 . . ? C11B C14B H14B 116.7 . . ? O3B C15B C3B 107.3(2) . . ? O3B C15B H15C 110.3 . . ? C3B C15B H15C 110.3 . . ? O3B C15B H15D 110.3 . . ? C3B C15B H15D 110.3 . . ? H15C C15B H15D 108.5 . . ? O3B C16B C17B 124.5(3) . . ? O3B C16B C21B 116.0(3) . . ? C17B C16B C21B 119.5(3) . . ? C16B C17B C18B 119.1(3) . . ? C16B C17B H17B 120.4 . . ? C18B C17B H17B 120.4 . . ? C19B C18B C17B 122.0(3) . . ? C19B C18B H18B 119.0 . . ? C17B C18B H18B 119.0 . . ? C20B C19B C18B 118.5(3) . . ? C20B C19B C22B 122.0(4) . . ? C18B C19B C22B 119.5(4) . . ? C19B C20B C21B 121.2(3) . . ? C19B C20B H20B 119.4 . . ? C21B C20B H20B 119.4 . . ? C16B C21B C20B 119.7(3) . . ? C16B C21B H21B 120.2 . . ? C20B C21B H21B 120.2 . . ? O4B C22B C19B 126.7(5) . . ? O4B C22B H22B 116.6 . . ? C19B C22B H22B 116.6 . . ? O5B C23B C5B 106.6(2) . . ? O5B C23B H23C 110.4 . . ? C5B C23B H23C 110.4 . . ? O5B C23B H23D 110.4 . . ? C5B C23B H23D 110.4 . . ? H23C C23B H23D 108.6 . . ? O5B C24B C25B 115.8(3) . . ? O5B C24B C29B 124.9(3) . . ? C25B C24B C29B 119.3(3) . . ? C26B C25B C24B 121.0(3) . . ? C26B C25B H25B 119.5 . . ? C24B C25B H25B 119.5 . . ? C25B C26B C27B 120.6(3) . . ? C25B C26B H26B 119.7 . . ? C27B C26B H26B 119.7 . . ? C28B C27B C26B 117.9(3) . . ? C28B C27B C30B 119.9(4) . . ? C26B C27B C30B 122.1(4) . . ? C29B C28B C27B 122.1(3) . . ? C29B C28B H28B 119.0 . . ? C27B C28B H28B 119.0 . . ? C28B C29B C24B 119.0(3) . . ? C28B C29B H29B 120.5 . . ? C24B C29B H29B 120.5 . . ? O6B C30B C27B 124.0(5) . . ? O6B C30B H30B 118.0 . . ? C27B C30B H30B 118.0 . . ? C6B C31B H31D 109.5 . . ? C6B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C6B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C2B C32B H32D 109.5 . . ? C2B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C2B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C4B C33B H33D 109.5 . . ? C4B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C4B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C8B O1B C7B 118.0(2) . . ? C16B O3B C15B 118.0(2) . . ? C24B O5B C23B 119.1(2) . . ? C2C C1C C6C 120.7(3) . . ? C2C C1C C7C 119.8(3) . . ? C6C C1C C7C 119.4(3) . . ? C1C C2C C3C 119.6(3) . . ? C1C C2C C31C 120.0(3) . . ? C3C C2C C31C 120.3(3) . . ? C2C C3C C4C 120.3(3) . . ? C2C C3C C15C 120.8(3) . . ? C4C C3C C15C 118.7(3) . . ? C5C C4C C3C 119.0(3) . . ? C5C C4C C32C 121.2(3) . . ? C3C C4C C32C 119.9(3) . . ? C4C C5C C6C 121.0(3) . . ? C4C C5C C23C 119.1(3) . . ? C6C C5C C23C 119.8(3) . . ? C5C C6C C1C 119.1(3) . . ? C5C C6C C33C 121.1(3) . . ? C1C C6C C33C 119.9(3) . . ? O1C C7C C1C 110.3(2) . . ? O1C C7C H7CA 109.6 . . ? C1C C7C H7CA 109.6 . . ? O1C C7C H7CB 109.6 . . ? C1C C7C H7CB 109.6 . . ? H7CA C7C H7CB 108.1 . . ? C9C C8C C13C 118.7(3) . . ? C9C C8C O1C 125.2(3) . . ? C13C C8C O1C 116.0(3) . . ? C8C C9C C10C 119.6(4) . . ? C8C C9C H9CA 120.2 . . ? C10C C9C H9CA 120.2 . . ? C11C C10C C9C 122.9(4) . . ? C11C C10C H10C 118.6 . . ? C9C C10C H10C 118.6 . . ? C10C C11C C12C 116.8(4) . . ? C10C C11C C14C 120.0(4) . . ? C12C C11C C14C 123.2(4) . . ? C11C C12C C13C 121.7(4) . . ? C11C C12C H12C 119.2 . . ? C13C C12C H12C 119.2 . . ? C8C C13C C12C 120.1(4) . . ? C8C C13C H13C 119.9 . . ? C12C C13C H13C 119.9 . . ? O2C C14C C11C 124.5(5) . . ? O2C C14C H14C 117.7 . . ? C11C C14C H14C 117.7 . . ? O3C C15C C3C 105.3(2) . . ? O3C C15C H15E 110.7 . . ? C3C C15C H15E 110.7 . . ? O3C C15C H15F 110.7 . . ? C3C C15C H15F 110.7 . . ? H15E C15C H15F 108.8 . . ? O3C C16C C17C 124.4(3) . . ? O3C C16C C21C 115.5(3) . . ? C17C C16C C21C 120.1(3) . . ? C16C C17C C18C 118.2(4) . . ? C16C C17C H17C 120.9 . . ? C18C C17C H17C 120.9 . . ? C19C C18C C17C 121.1(4) . . ? C19C C18C H18C 119.5 . . ? C17C C18C H18C 119.5 . . ? C20C C19C C18C 119.5(3) . . ? C20C C19C C22C 119.3(4) . . ? C18C C19C C22C 121.2(4) . . ? C21C C20C C19C 120.1(4) . . ? C21C C20C H20C 119.9 . . ? C19C C20C H20C 119.9 . . ? C20C C21C C16C 121.1(4) . . ? C20C C21C H21C 119.5 . . ? C16C C21C H21C 119.5 . . ? O4C C22C C19C 128.1(5) . . ? O4C C22C H22C 116.0 . . ? C19C C22C H22C 116.0 . . ? O5C C23C C5C 106.9(2) . . ? O5C C23C H23E 110.3 . . ? C5C C23C H23E 110.3 . . ? O5C C23C H23F 110.3 . . ? C5C C23C H23F 110.3 . . ? H23E C23C H23F 108.6 . . ? O5C C24C C25C 124.7(3) . . ? O5C C24C C29C 115.5(3) . . ? C25C C24C C29C 119.8(3) . . ? C24C C25C C26C 119.0(3) . . ? C24C C25C H25C 120.5 . . ? C26C C25C H25C 120.5 . . ? C27C C26C C25C 122.4(3) . . ? C27C C26C H26C 118.8 . . ? C25C C26C H26C 118.8 . . ? C26C C27C C28C 117.5(3) . . ? C26C C27C C30C 118.3(4) . . ? C28C C27C C30C 124.2(4) . . ? C29C C28C C27C 121.3(4) . . ? C29C C28C H28C 119.4 . . ? C27C C28C H28C 119.4 . . ? C28C C29C C24C 120.0(4) . . ? C28C C29C H29C 120.0 . . ? C24C C29C H29C 120.0 . . ? O6C C30C C27C 123.2(5) . . ? O6C C30C H30C 118.4 . . ? C27C C30C H30C 118.4 . . ? C2C C31C H31G 109.5 . . ? C2C C31C H31H 109.5 . . ? H31G C31C H31H 109.5 . . ? C2C C31C H31I 109.5 . . ? H31G C31C H31I 109.5 . . ? H31H C31C H31I 109.5 . . ? C4C C32C H32G 109.5 . . ? C4C C32C H32H 109.5 . . ? H32G C32C H32H 109.5 . . ? C4C C32C H32I 109.5 . . ? H32G C32C H32I 109.5 . . ? H32H C32C H32I 109.5 . . ? C6C C33C H33G 109.5 . . ? C6C C33C H33H 109.5 . . ? H33G C33C H33H 109.5 . . ? C6C C33C H33I 109.5 . . ? H33G C33C H33I 109.5 . . ? H33H C33C H33I 109.5 . . ? C8C O1C C7C 116.7(2) . . ? C16C O3C C15C 121.2(2) . . ? C24C O5C C23C 118.6(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A C1A C2A C3A 0.5(4) . . . . ? C7A C1A C2A C3A -178.4(3) . . . . ? C6A C1A C2A C32A 179.8(3) . . . . ? C7A C1A C2A C32A 0.9(4) . . . . ? C1A C2A C3A C4A -0.9(4) . . . . ? C32A C2A C3A C4A 179.8(3) . . . . ? C1A C2A C3A C15A 177.2(2) . . . . ? C32A C2A C3A C15A -2.1(4) . . . . ? C2A C3A C4A C5A -0.5(4) . . . . ? C15A C3A C4A C5A -178.6(2) . . . . ? C2A C3A C4A C33A 179.6(3) . . . . ? C15A C3A C4A C33A 1.4(4) . . . . ? C3A C4A C5A C6A 2.4(4) . . . . ? C33A C4A C5A C6A -177.7(3) . . . . ? C3A C4A C5A C23A -179.6(2) . . . . ? C33A C4A C5A C23A 0.4(4) . . . . ? C4A C5A C6A C1A -2.8(4) . . . . ? C23A C5A C6A C1A 179.1(2) . . . . ? C4A C5A C6A C31A 176.3(3) . . . . ? C23A C5A C6A C31A -1.8(4) . . . . ? C2A C1A C6A C5A 1.4(4) . . . . ? C7A C1A C6A C5A -179.7(2) . . . . ? C2A C1A C6A C31A -177.8(3) . . . . ? C7A C1A C6A C31A 1.1(4) . . . . ? C2A C1A C7A O1A 96.1(3) . . . . ? C6A C1A C7A O1A -82.9(3) . . . . ? O1A C8A C9A C10A -179.0(4) . . . . ? C13A C8A C9A C10A -0.6(5) . . . . ? C8A C9A C10A C11A -0.1(7) . . . . ? C9A C10A C11A C12A 1.2(7) . . . . ? C9A C10A C11A C14A 178.6(5) . . . . ? C10A C11A C12A C13A -1.6(7) . . . . ? C14A C11A C12A C13A -178.9(6) . . . . ? C11A C12A C13A C8A 0.9(7) . . . . ? O1A C8A C13A C12A 178.7(3) . . . . ? C9A C8A C13A C12A 0.2(6) . . . . ? C10A C11A C14A O2A -159.4(13) . . . . ? C12A C11A C14A O2A 17.9(15) . . . . ? C10A C11A C14A O2A' 141.6(18) . . . . ? C12A C11A C14A O2A' -41(2) . . . . ? C2A C3A C15A O3A 114.6(3) . . . . ? C4A C3A C15A O3A -67.3(3) . . . . ? O3A C16A C17A C18A 179.5(3) . . . . ? C21A C16A C17A C18A -0.7(5) . . . . ? C16A C17A C18A C19A -0.3(5) . . . . ? C17A C18A C19A C20A 0.6(6) . . . . ? C17A C18A C19A C22A -179.4(4) . . . . ? C18A C19A C20A C21A 0.1(6) . . . . ? C22A C19A C20A C21A 180.0(4) . . . . ? C19A C20A C21A C16A -1.0(6) . . . . ? O3A C16A C21A C20A -178.9(3) . . . . ? C17A C16A C21A C20A 1.3(5) . . . . ? C18A C19A C22A O4A 175.5(5) . . . . ? C20A C19A C22A O4A -4.5(7) . . . . ? C4A C5A C23A O5A -92.5(3) . . . . ? C6A C5A C23A O5A 85.6(3) . . . . ? O5A C24A C25A C26A -179.4(3) . . . . ? C29A C24A C25A C26A -0.2(5) . . . . ? C24A C25A C26A C27A 1.0(5) . . . . ? C25A C26A C27A C28A -0.7(5) . . . . ? C25A C26A C27A C30A 178.3(3) . . . . ? C26A C27A C28A C29A -0.5(5) . . . . ? C30A C27A C28A C29A -179.5(3) . . . . ? O5A C24A C29A C28A 178.2(3) . . . . ? C25A C24A C29A C28A -1.0(5) . . . . ? C27A C28A C29A C24A 1.4(5) . . . . ? C28A C27A C30A O6A -178.9(4) . . . . ? C26A C27A C30A O6A 2.2(6) . . . . ? C9A C8A O1A C7A 5.8(5) . . . . ? C13A C8A O1A C7A -172.6(3) . . . . ? C1A C7A O1A C8A 167.3(3) . . . . ? C17A C16A O3A C15A 13.8(4) . . . . ? C21A C16A O3A C15A -166.0(3) . . . . ? C3A C15A O3A C16A 169.1(2) . . . . ? C29A C24A O5A C23A 2.9(4) . . . . ? C25A C24A O5A C23A -177.9(3) . . . . ? C5A C23A O5A C24A -167.7(2) . . . . ? C6B C1B C2B C3B 2.8(4) . . . . ? C7B C1B C2B C3B -176.5(2) . . . . ? C6B C1B C2B C32B -178.1(3) . . . . ? C7B C1B C2B C32B 2.6(4) . . . . ? C1B C2B C3B C4B 1.6(4) . . . . ? C32B C2B C3B C4B -177.5(3) . . . . ? C1B C2B C3B C15B -178.1(2) . . . . ? C32B C2B C3B C15B 2.8(4) . . . . ? C2B C3B C4B C5B -4.8(4) . . . . ? C15B C3B C4B C5B 174.9(2) . . . . ? C2B C3B C4B C33B 173.6(3) . . . . ? C15B C3B C4B C33B -6.7(4) . . . . ? C3B C4B C5B C6B 3.6(4) . . . . ? C33B C4B C5B C6B -174.7(3) . . . . ? C3B C4B C5B C23B -172.8(2) . . . . ? C33B C4B C5B C23B 8.8(4) . . . . ? C2B C1B C6B C5B -4.0(4) . . . . ? C7B C1B C6B C5B 175.3(2) . . . . ? C2B C1B C6B C31B 175.1(3) . . . . ? C7B C1B C6B C31B -5.5(4) . . . . ? C4B C5B C6B C1B 0.8(4) . . . . ? C23B C5B C6B C1B 177.2(2) . . . . ? C4B C5B C6B C31B -178.4(3) . . . . ? C23B C5B C6B C31B -2.0(4) . . . . ? C6B C1B C7B O1B 104.8(3) . . . . ? C2B C1B C7B O1B -75.8(3) . . . . ? O1B C8B C9B C10B -179.1(3) . . . . ? C13B C8B C9B C10B -0.3(5) . . . . ? C8B C9B C10B C11B -0.4(5) . . . . ? C9B C10B C11B C12B 1.4(6) . . . . ? C9B C10B C11B C14B -179.0(4) . . . . ? C10B C11B C12B C13B -1.7(6) . . . . ? C14B C11B C12B C13B 178.7(4) . . . . ? C11B C12B C13B C8B 1.0(6) . . . . ? O1B C8B C13B C12B 178.9(3) . . . . ? C9B C8B C13B C12B 0.0(5) . . . . ? C12B C11B C14B O2B 176.2(5) . . . . ? C10B C11B C14B O2B -3.4(8) . . . . ? C2B C3B C15B O3B -80.7(3) . . . . ? C4B C3B C15B O3B 99.6(3) . . . . ? O3B C16B C17B C18B 179.7(3) . . . . ? C21B C16B C17B C18B 0.1(6) . . . . ? C16B C17B C18B C19B -0.7(6) . . . . ? C17B C18B C19B C20B 0.6(6) . . . . ? C17B C18B C19B C22B -178.5(4) . . . . ? C18B C19B C20B C21B 0.0(6) . . . . ? C22B C19B C20B C21B 179.1(4) . . . . ? O3B C16B C21B C20B -179.2(4) . . . . ? C17B C16B C21B C20B 0.4(6) . . . . ? C19B C20B C21B C16B -0.5(7) . . . . ? C20B C19B C22B O4B -4.7(7) . . . . ? C18B C19B C22B O4B 174.4(5) . . . . ? C4B C5B C23B O5B 87.0(3) . . . . ? C6B C5B C23B O5B -89.5(3) . . . . ? O5B C24B C25B C26B -178.1(3) . . . . ? C29B C24B C25B C26B 2.2(5) . . . . ? C24B C25B C26B C27B -1.4(5) . . . . ? C25B C26B C27B C28B -0.4(5) . . . . ? C25B C26B C27B C30B 177.3(4) . . . . ? C26B C27B C28B C29B 1.4(5) . . . . ? C30B C27B C28B C29B -176.4(3) . . . . ? C27B C28B C29B C24B -0.6(5) . . . . ? O5B C24B C29B C28B 179.1(3) . . . . ? C25B C24B C29B C28B -1.2(5) . . . . ? C28B C27B C30B O6B 173.7(4) . . . . ? C26B C27B C30B O6B -3.9(6) . . . . ? C13B C8B O1B C7B 178.1(3) . . . . ? C9B C8B O1B C7B -3.1(4) . . . . ? C1B C7B O1B C8B 167.6(2) . . . . ? C17B C16B O3B C15B -6.2(5) . . . . ? C21B C16B O3B C15B 173.4(3) . . . . ? C3B C15B O3B C16B 174.3(3) . . . . ? C25B C24B O5B C23B 179.4(3) . . . . ? C29B C24B O5B C23B -0.9(4) . . . . ? C5B C23B O5B C24B -171.9(2) . . . . ? C6C C1C C2C C3C 5.9(4) . . . . ? C7C C1C C2C C3C -169.1(3) . . . . ? C6C C1C C2C C31C -173.0(3) . . . . ? C7C C1C C2C C31C 11.9(4) . . . . ? C1C C2C C3C C4C -5.7(4) . . . . ? C31C C2C C3C C4C 173.2(3) . . . . ? C1C C2C C3C C15C 168.9(2) . . . . ? C31C C2C C3C C15C -12.2(4) . . . . ? C2C C3C C4C C5C 0.9(4) . . . . ? C15C C3C C4C C5C -173.8(3) . . . . ? C2C C3C C4C C32C -179.5(3) . . . . ? C15C C3C C4C C32C 5.8(4) . . . . ? C3C C4C C5C C6C 3.8(4) . . . . ? C32C C4C C5C C6C -175.7(3) . . . . ? C3C C4C C5C C23C -179.8(3) . . . . ? C32C C4C C5C C23C 0.6(4) . . . . ? C4C C5C C6C C1C -3.7(4) . . . . ? C23C C5C C6C C1C 179.9(3) . . . . ? C4C C5C C6C C33C 176.2(3) . . . . ? C23C C5C C6C C33C -0.2(4) . . . . ? C2C C1C C6C C5C -1.2(4) . . . . ? C7C C1C C6C C5C 173.8(3) . . . . ? C2C C1C C6C C33C 178.9(3) . . . . ? C7C C1C C6C C33C -6.0(4) . . . . ? C2C C1C C7C O1C -105.4(3) . . . . ? C6C C1C C7C O1C 79.5(4) . . . . ? C13C C8C C9C C10C 2.3(8) . . . . ? O1C C8C C9C C10C -179.5(4) . . . . ? C8C C9C C10C C11C 0.8(9) . . . . ? C9C C10C C11C C12C -4.3(8) . . . . ? C9C C10C C11C C14C 178.3(5) . . . . ? C10C C11C C12C C13C 4.8(9) . . . . ? C14C C11C C12C C13C -177.9(5) . . . . ? C9C C8C C13C C12C -1.8(8) . . . . ? O1C C8C C13C C12C 179.9(5) . . . . ? C11C C12C C13C C8C -1.9(10) . . . . ? C10C C11C C14C O2C 179.8(6) . . . . ? C12C C11C C14C O2C 2.5(9) . . . . ? C2C C3C C15C O3C -106.3(3) . . . . ? C4C C3C C15C O3C 68.3(3) . . . . ? O3C C16C C17C C18C -178.2(3) . . . . ? C21C C16C C17C C18C 1.2(5) . . . . ? C16C C17C C18C C19C 0.1(5) . . . . ? C17C C18C C19C C20C -1.5(6) . . . . ? C17C C18C C19C C22C 177.6(3) . . . . ? C18C C19C C20C C21C 1.6(6) . . . . ? C22C C19C C20C C21C -177.5(4) . . . . ? C19C C20C C21C C16C -0.4(6) . . . . ? O3C C16C C21C C20C 178.4(3) . . . . ? C17C C16C C21C C20C -1.1(6) . . . . ? C20C C19C C22C O4C 177.0(4) . . . . ? C18C C19C C22C O4C -2.1(6) . . . . ? C4C C5C C23C O5C -91.1(3) . . . . ? C6C C5C C23C O5C 85.3(4) . . . . ? O5C C24C C25C C26C -178.0(3) . . . . ? C29C C24C C25C C26C -0.2(5) . . . . ? C24C C25C C26C C27C -0.2(5) . . . . ? C25C C26C C27C C28C -0.1(5) . . . . ? C25C C26C C27C C30C -178.3(3) . . . . ? C26C C27C C28C C29C 0.8(5) . . . . ? C30C C27C C28C C29C 178.9(4) . . . . ? C27C C28C C29C C24C -1.3(6) . . . . ? O5C C24C C29C C28C 178.9(3) . . . . ? C25C C24C C29C C28C 0.9(6) . . . . ? C26C C27C C30C O6C 173.8(4) . . . . ? C28C C27C C30C O6C -4.3(7) . . . . ? C9C C8C O1C C7C -7.6(6) . . . . ? C13C C8C O1C C7C 170.6(4) . . . . ? C1C C7C O1C C8C -173.4(3) . . . . ? C17C C16C O3C C15C -10.2(5) . . . . ? C21C C16C O3C C15C 170.4(3) . . . . ? C3C C15C O3C C16C -174.1(3) . . . . ? C25C C24C O5C C23C -3.5(5) . . . . ? C29C C24C O5C C23C 178.7(3) . . . . ? C5C C23C O5C C24C 171.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.707 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.043 data_shelxl1 _database_code_depnum_ccdc_archive 'CCDC 765840' #TrackingRef '- Crystal data of Compound-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 Br3' _chemical_formula_weight 398.97 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.454(2) _cell_length_b 9.478(4) _cell_length_c 9.573(2) _cell_angle_alpha 116.53(2) _cell_angle_beta 109.705(14) _cell_angle_gamma 101.293(18) _cell_volume 658.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5698 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.64 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 9.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1698 _exptl_absorpt_correction_T_max 0.2618 _exptl_absorpt_process_details 'SADABS (Bruker 1999)' _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 'bruker axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14861 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.56 _reflns_number_total 3337 _reflns_number_gt 2428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004)' _computing_structure_solution 'SIR92 (Altornare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0346P)^2^+0.5949P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0089(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3337 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 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 C1 C 0.6242(4) 0.4423(4) -0.1810(4) 0.0322(6) Uani 1 1 d . . . C2 C 0.5880(4) 0.3532(4) -0.1051(4) 0.0334(7) Uani 1 1 d . . . C3 C 0.7011(4) 0.4127(4) 0.0678(4) 0.0337(7) Uani 1 1 d . . . C4 C 0.8537(4) 0.5524(4) 0.1612(4) 0.0354(7) Uani 1 1 d . . . C5 C 0.8925(4) 0.6332(4) 0.0786(4) 0.0345(7) Uani 1 1 d . . . C6 C 0.7766(4) 0.5831(4) -0.0888(4) 0.0336(7) Uani 1 1 d . . . C7 C 0.4993(4) 0.3861(4) -0.3612(4) 0.0386(7) Uani 1 1 d . . . H7A H 0.5045 0.4868 -0.3663 0.046 Uiso 1 1 calc R . . H7B H 0.3901 0.3302 -0.3818 0.046 Uiso 1 1 calc R . . C8 C 0.4292(4) 0.1944(5) -0.2100(5) 0.0493(9) Uani 1 1 d . . . H8A H 0.4441 0.1202 -0.1686 0.074 Uiso 1 1 calc R . . H8B H 0.3987 0.1336 -0.3343 0.074 Uiso 1 1 calc R . . H8C H 0.3437 0.2284 -0.1940 0.074 Uiso 1 1 calc R . . C9 C 0.6580(4) 0.3256(5) 0.1549(5) 0.0441(8) Uani 1 1 d . . . H9A H 0.5391 0.2724 0.1025 0.053 Uiso 1 1 calc R . . H9B H 0.7031 0.4114 0.2810 0.053 Uiso 1 1 calc R . . C10 C 0.9743(5) 0.6177(5) 0.3484(5) 0.0564(10) Uani 1 1 d . . . H10A H 0.9165 0.5857 0.4023 0.085 Uiso 1 1 calc R . . H10B H 1.0304 0.7414 0.4163 0.085 Uiso 1 1 calc R . . H10C H 1.0532 0.5677 0.3464 0.085 Uiso 1 1 calc R . . C11 C 1.0573(4) 0.7750(4) 0.1709(5) 0.0444(8) Uani 1 1 d . . . H11A H 1.0907 0.7692 0.0839 0.053 Uiso 1 1 calc R . . H11B H 1.1376 0.7609 0.2529 0.053 Uiso 1 1 calc R . . C12 C 0.8122(5) 0.6791(5) -0.1720(5) 0.0519(9) Uani 1 1 d . . . H12A H 0.7648 0.7623 -0.1505 0.078 Uiso 1 1 calc R . . H12B H 0.7653 0.5984 -0.2982 0.078 Uiso 1 1 calc R . . H12C H 0.9293 0.7375 -0.1201 0.078 Uiso 1 1 calc R . . Br1 Br 0.53528(5) 0.22553(6) -0.54926(5) 0.05986(15) Uani 1 1 d . . . Br2 Br 0.74445(5) 0.14906(5) 0.12550(6) 0.05757(15) Uani 1 1 d . . . Br3 Br 1.05247(5) 1.00100(5) 0.30288(6) 0.06531(16) Uani 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 C1 0.0331(15) 0.0353(16) 0.0348(16) 0.0214(14) 0.0180(14) 0.0183(13) C2 0.0347(15) 0.0329(16) 0.0431(18) 0.0238(15) 0.0234(14) 0.0177(13) C3 0.0423(17) 0.0370(17) 0.0430(18) 0.0286(15) 0.0282(15) 0.0246(14) C4 0.0392(16) 0.0369(17) 0.0355(17) 0.0216(15) 0.0180(14) 0.0219(14) C5 0.0327(15) 0.0321(16) 0.0419(18) 0.0209(15) 0.0196(14) 0.0151(13) C6 0.0367(16) 0.0352(16) 0.0423(18) 0.0260(15) 0.0241(14) 0.0184(13) C7 0.0395(17) 0.0445(19) 0.0393(18) 0.0277(16) 0.0186(15) 0.0207(15) C8 0.0439(19) 0.044(2) 0.060(2) 0.0334(19) 0.0233(18) 0.0118(16) C9 0.054(2) 0.054(2) 0.055(2) 0.0400(19) 0.0372(18) 0.0318(18) C10 0.062(2) 0.057(2) 0.042(2) 0.0300(19) 0.0147(19) 0.022(2) C11 0.0344(17) 0.0428(19) 0.053(2) 0.0263(17) 0.0192(16) 0.0153(15) C12 0.053(2) 0.055(2) 0.057(2) 0.040(2) 0.0278(19) 0.0155(18) Br1 0.0698(3) 0.0688(3) 0.0413(2) 0.0271(2) 0.0277(2) 0.0364(2) Br2 0.0640(3) 0.0599(3) 0.0895(3) 0.0598(2) 0.0465(2) 0.0357(2) Br3 0.0558(3) 0.0364(2) 0.0755(3) 0.0209(2) 0.0224(2) 0.01039(17) _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 C1 C2 1.400(4) . ? C1 C6 1.404(4) . ? C1 C7 1.488(4) . ? C2 C3 1.392(4) . ? C2 C8 1.508(5) . ? C3 C4 1.399(4) . ? C3 C9 1.502(4) . ? C4 C5 1.405(4) . ? C4 C10 1.500(5) . ? C5 C6 1.388(4) . ? C5 C11 1.484(4) . ? C6 C12 1.511(5) . ? C7 Br1 1.959(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 Br2 1.954(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 Br3 1.961(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 C2 C1 C6 120.7(3) . . ? C2 C1 C7 119.2(3) . . ? C6 C1 C7 120.1(3) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 C8 120.6(3) . . ? C1 C2 C8 120.4(3) . . ? C2 C3 C4 120.9(3) . . ? C2 C3 C9 119.3(3) . . ? C4 C3 C9 119.8(3) . . ? C3 C4 C5 119.3(3) . . ? C3 C4 C10 120.8(3) . . ? C5 C4 C10 120.0(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 C11 119.4(3) . . ? C4 C5 C11 120.2(3) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C12 120.7(3) . . ? C1 C6 C12 119.8(3) . . ? C1 C7 Br1 111.7(2) . . ? C1 C7 H7A 109.3 . . ? Br1 C7 H7A 109.3 . . ? C1 C7 H7B 109.3 . . ? Br1 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 Br2 111.2(2) . . ? C3 C9 H9A 109.4 . . ? Br2 C9 H9A 109.4 . . ? C3 C9 H9B 109.4 . . ? Br2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 Br3 110.7(2) . . ? C5 C11 H11A 109.5 . . ? Br3 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? Br3 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.9(4) . . . . ? C7 C1 C2 C3 -176.2(3) . . . . ? C6 C1 C2 C8 -175.6(3) . . . . ? C7 C1 C2 C8 4.3(4) . . . . ? C1 C2 C3 C4 -4.1(4) . . . . ? C8 C2 C3 C4 175.4(3) . . . . ? C1 C2 C3 C9 175.7(3) . . . . ? C8 C2 C3 C9 -4.8(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C9 C3 C4 C5 -179.8(3) . . . . ? C2 C3 C4 C10 179.1(3) . . . . ? C9 C3 C4 C10 -0.6(5) . . . . ? C3 C4 C5 C6 4.5(4) . . . . ? C10 C4 C5 C6 -174.7(3) . . . . ? C3 C4 C5 C11 -176.4(3) . . . . ? C10 C4 C5 C11 4.4(5) . . . . ? C4 C5 C6 C1 -4.7(4) . . . . ? C11 C5 C6 C1 176.2(3) . . . . ? C4 C5 C6 C12 174.9(3) . . . . ? C11 C5 C6 C12 -4.2(5) . . . . ? C2 C1 C6 C5 0.5(4) . . . . ? C7 C1 C6 C5 -179.4(3) . . . . ? C2 C1 C6 C12 -179.1(3) . . . . ? C7 C1 C6 C12 1.0(4) . . . . ? C2 C1 C7 Br1 -94.3(3) . . . . ? C6 C1 C7 Br1 85.7(3) . . . . ? C2 C3 C9 Br2 95.1(3) . . . . ? C4 C3 C9 Br2 -85.1(3) . . . . ? C6 C5 C11 Br3 85.4(3) . . . . ? C4 C5 C11 Br3 -93.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.836 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.087