# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_121025_p6c2br _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H72 Br12 O12' _chemical_formula_sum 'C66 H72 Br12 O12' _chemical_formula_weight 2016.16 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9742(4) _cell_length_b 13.6564(5) _cell_length_c 24.0532(9) _cell_angle_alpha 89.320(3) _cell_angle_beta 79.331(3) _cell_angle_gamma 84.985(3) _cell_volume 3850.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 7176 _cell_measurement_theta_min 2.9714 _cell_measurement_theta_max 29.3309 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 6.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2167 _exptl_absorpt_correction_T_max 0.2914 _exptl_absorpt_process_details ; CrysAlis PRO (Agilent Technologies, 2011) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24262 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.35 _reflns_number_total 14080 _reflns_number_gt 9745 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Agilent Technologies, 2011)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0528P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14080 _refine_ls_number_parameters 815 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.001 _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 Br1 Br 0.93578(4) 0.19901(4) 0.03962(2) 0.03679(15) Uani 1 1 d . . . Br6 Br 0.14380(4) 0.36830(4) 0.52732(2) 0.03544(15) Uani 1 1 d . . . Br10 Br 0.12650(4) 0.65020(4) 0.14656(2) 0.03817(16) Uani 1 1 d . . . Br11 Br 0.99411(5) 0.55581(5) -0.09015(2) 0.04445(18) Uani 1 1 d . . . Br3 Br 0.81326(5) -0.15310(5) 0.07153(2) 0.04183(16) Uani 1 1 d . . . Br9 Br 0.95878(5) 0.61050(5) 0.30152(3) 0.04373(17) Uani 1 1 d . . . Br2 Br 0.03370(5) -0.00694(5) 0.15243(2) 0.04116(16) Uani 1 1 d . . . Br8 Br 0.16607(5) 0.70595(4) 0.39531(3) 0.04186(16) Uani 1 1 d . . . Br5 Br 0.93574(5) -0.11028(5) 0.30920(3) 0.04669(18) Uani 1 1 d . . . Br4 Br 0.15272(5) -0.07250(5) 0.47337(3) 0.04931(18) Uani 1 1 d . . . Br7 Br 1.09071(6) 0.28246(6) 0.37233(3) 0.0528(2) Uani 0.8969(12) 1 d P A 1 Br12 Br 0.10629(8) 0.23856(6) 0.21875(4) 0.1013(4) Uani 1 1 d . . . O8 O 0.3745(3) 0.5484(3) 0.38887(14) 0.0267(8) Uani 1 1 d . . . O1 O 0.6731(3) 0.1581(3) 0.07403(15) 0.0287(8) Uani 1 1 d . . . O9 O 0.7450(3) 0.5386(3) 0.26474(13) 0.0289(9) Uani 1 1 d . . . O10 O 0.3521(2) 0.6780(3) 0.19053(13) 0.0261(8) Uani 1 1 d . . . O6 O 0.3562(3) 0.2064(3) 0.51583(14) 0.0266(9) Uani 1 1 d . . . C28 C 0.4449(4) 0.1574(4) 0.47858(19) 0.0212(11) Uani 1 1 d . . . O4 O 0.3080(3) -0.0095(3) 0.36080(14) 0.0299(9) Uani 1 1 d . . . O3 O 0.6382(3) -0.1609(3) 0.18422(13) 0.0260(8) Uani 1 1 d . . . C57 C 0.5325(4) 0.5034(3) 0.08223(18) 0.0166(10) Uani 1 1 d . . . O2 O 0.2881(3) -0.0416(2) 0.08337(14) 0.0236(8) Uani 1 1 d . . . C49 C 0.5386(4) 0.6032(3) 0.17031(19) 0.0167(10) Uani 1 1 d . . . O12 O 0.3399(3) 0.3073(3) 0.08104(14) 0.0301(9) Uani 1 1 d . . . C61 C 0.4361(4) 0.3595(3) 0.07010(19) 0.0188(11) Uani 1 1 d . . . O11 O 0.7196(3) 0.5183(3) 0.03430(14) 0.0296(9) Uani 1 1 d . . . C32 C 0.2472(4) 0.1701(4) 0.5236(2) 0.0292(13) Uani 1 1 d . . . H32A H 0.2499 0.1041 0.5410 0.035 Uiso 1 1 calc R . . H32B H 0.2230 0.1647 0.4867 0.035 Uiso 1 1 calc R . . O5 O 0.7141(3) 0.0221(3) 0.36464(15) 0.0321(9) Uani 1 1 d . . . C60 C 0.5283(4) 0.3207(3) 0.03106(18) 0.0160(10) Uani 1 1 d . . . C2 C 0.5035(4) 0.1372(3) 0.04151(19) 0.0173(11) Uani 1 1 d . . . C48 C 0.6370(4) 0.5665(4) 0.18800(19) 0.0211(11) Uani 1 1 d . . . H48 H 0.6985 0.5369 0.1611 0.025 Uiso 1 1 calc R . . C6 C 0.3838(4) 0.0102(3) 0.07975(19) 0.0158(10) Uani 1 1 d . . . C51 C 0.4587(4) 0.6480(3) 0.26702(19) 0.0183(11) Uani 1 1 d . . . H51 H 0.3959 0.6748 0.2942 0.022 Uiso 1 1 calc R . . C24 C 0.5257(4) 0.0239(4) 0.41472(19) 0.0213(11) Uani 1 1 d . . . C40 C 0.4673(4) 0.4254(4) 0.4433(2) 0.0205(11) Uani 1 1 d . . . H40 H 0.3961 0.4023 0.4598 0.025 Uiso 1 1 calc R . . C25 C 0.6265(4) 0.0683(4) 0.40365(19) 0.0217(11) Uani 1 1 d . . . C62 C 0.4386(4) 0.4493(3) 0.0953(2) 0.0208(11) Uani 1 1 d . . . H62 H 0.3745 0.4746 0.1221 0.025 Uiso 1 1 calc R . . C1 C 0.5263(4) 0.2228(3) 0.00194(19) 0.0214(11) Uani 1 1 d . . . H1A H 0.4668 0.2296 -0.0218 0.026 Uiso 1 1 calc R . . H1B H 0.6006 0.2077 -0.0236 0.026 Uiso 1 1 calc R . . C34 C 0.5620(4) 0.2950(4) 0.4983(2) 0.0221(11) Uani 1 1 d . . . H34A H 0.4973 0.3091 0.5301 0.026 Uiso 1 1 calc R . . H34B H 0.6331 0.2873 0.5140 0.026 Uiso 1 1 calc R . . C12 C 0.4279(4) -0.1020(4) 0.1586(2) 0.0256(12) Uani 1 1 d . . . H12A H 0.3458 -0.1115 0.1625 0.031 Uiso 1 1 calc R . . H12B H 0.4713 -0.1627 0.1415 0.031 Uiso 1 1 calc R . . C7 C 0.4084(4) 0.0864(3) 0.04188(19) 0.0167(10) Uani 1 1 d . . . H7 H 0.3592 0.1038 0.0159 0.020 Uiso 1 1 calc R . . C14 C 0.5605(4) -0.1204(4) 0.2294(2) 0.0222(11) Uani 1 1 d . . . C59 C 0.6234(4) 0.3735(3) 0.01903(19) 0.0198(11) Uani 1 1 d . . . H59 H 0.6880 0.3471 -0.0072 0.024 Uiso 1 1 calc R . . C50 C 0.4475(4) 0.6430(4) 0.2111(2) 0.0211(11) Uani 1 1 d . . . C13 C 0.4542(4) -0.0902(4) 0.2172(2) 0.0207(11) Uani 1 1 d . . . C5 C 0.4546(4) -0.0176(3) 0.11795(18) 0.0166(11) Uani 1 1 d . . . C29 C 0.4344(4) 0.0698(4) 0.45216(19) 0.0212(11) Uani 1 1 d . . . H29 H 0.3639 0.0409 0.4598 0.025 Uiso 1 1 calc R . . C58 C 0.6272(4) 0.4630(4) 0.04399(19) 0.0199(11) Uani 1 1 d . . . C27 C 0.5473(4) 0.2000(4) 0.46954(19) 0.0203(11) Uani 1 1 d . . . C15 C 0.5821(4) -0.1114(4) 0.28405(19) 0.0205(11) Uani 1 1 d . . . H15 H 0.6562 -0.1306 0.2914 0.025 Uiso 1 1 calc R . . C63 C 0.8049(4) 0.4942(4) -0.0149(2) 0.0294(13) Uani 1 1 d . . . H63A H 0.7694 0.4844 -0.0483 0.035 Uiso 1 1 calc R . . H63B H 0.8528 0.4336 -0.0088 0.035 Uiso 1 1 calc R . . C38 C 0.5730(4) 0.5400(3) 0.38223(19) 0.0200(11) Uani 1 1 d . . . O7 O 0.7680(3) 0.3702(3) 0.44813(15) 0.0400(10) Uani 1 1 d . . . C56 C 0.5319(4) 0.6044(3) 0.10768(18) 0.0191(11) Uani 1 1 d . . . H56A H 0.4613 0.6440 0.1026 0.023 Uiso 1 1 calc R . . H56B H 0.5974 0.6372 0.0867 0.023 Uiso 1 1 calc R . . C46 C 0.5587(4) 0.6152(3) 0.28455(19) 0.0179(11) Uani 1 1 d . . . C26 C 0.6382(4) 0.1549(4) 0.4315(2) 0.0246(12) Uani 1 1 d . . . H26 H 0.7092 0.1833 0.4243 0.029 Uiso 1 1 calc R . . C54 C 0.2514(4) 0.7098(4) 0.2291(2) 0.0251(12) Uani 1 1 d . . . H54A H 0.2673 0.7615 0.2544 0.030 Uiso 1 1 calc R . . H54B H 0.2231 0.6540 0.2527 0.030 Uiso 1 1 calc R . . C45 C 0.5744(4) 0.6300(4) 0.34536(19) 0.0231(12) Uani 1 1 d . . . H45A H 0.6481 0.6585 0.3442 0.028 Uiso 1 1 calc R . . H45B H 0.5134 0.6791 0.3637 0.028 Uiso 1 1 calc R . . C16 C 0.4969(4) -0.0747(3) 0.3277(2) 0.0205(11) Uani 1 1 d . . . C3 C 0.5762(4) 0.1071(4) 0.0785(2) 0.0221(12) Uani 1 1 d . . . C41 C 0.8680(4) 0.3690(4) 0.4083(2) 0.0380(15) Uani 1 1 d . A . H41A H 0.8974 0.4348 0.4054 0.046 Uiso 1 1 calc R . . H41B H 0.8541 0.3504 0.3706 0.046 Uiso 1 1 calc R . . C35 C 0.5674(4) 0.3804(3) 0.45769(19) 0.0197(11) Uani 1 1 d . . . C37 C 0.6721(4) 0.4952(4) 0.3962(2) 0.0238(12) Uani 1 1 d . . . H37 H 0.7433 0.5191 0.3805 0.029 Uiso 1 1 calc R . . C53 C 0.9428(4) 0.4959(4) 0.2568(2) 0.0299(13) Uani 1 1 d . . . H53A H 1.0148 0.4789 0.2298 0.036 Uiso 1 1 calc R . . H53B H 0.9272 0.4391 0.2821 0.036 Uiso 1 1 calc R . . C18 C 0.3685(4) -0.0513(4) 0.2618(2) 0.0264(12) Uani 1 1 d . . . H18 H 0.2950 -0.0297 0.2546 0.032 Uiso 1 1 calc R . . C17 C 0.3909(4) -0.0446(4) 0.3157(2) 0.0224(11) Uani 1 1 d . . . C23 C 0.5169(4) -0.0756(4) 0.38848(19) 0.0225(11) Uani 1 1 d . . . H23A H 0.5882 -0.1174 0.3899 0.027 Uiso 1 1 calc R . . H23B H 0.4537 -0.1073 0.4124 0.027 Uiso 1 1 calc R . . C47 C 0.6485(4) 0.5717(4) 0.2443(2) 0.0213(11) Uani 1 1 d . . . C39 C 0.4693(4) 0.5020(4) 0.4059(2) 0.0212(12) Uani 1 1 d . . . C9 C 0.8236(4) 0.2200(4) 0.1095(2) 0.0375(15) Uani 1 1 d . . . H9A H 0.8635 0.2174 0.1421 0.045 Uiso 1 1 calc R . . H9B H 0.7830 0.2862 0.1088 0.045 Uiso 1 1 calc R . . C19 C 0.7518(4) -0.1858(4) 0.1910(2) 0.0313(13) Uani 1 1 d . . . H19A H 0.7533 -0.2303 0.2238 0.038 Uiso 1 1 calc R . . H19B H 0.7883 -0.1259 0.1979 0.038 Uiso 1 1 calc R . . C10 C 0.2033(4) -0.0066(4) 0.0518(2) 0.0249(12) Uani 1 1 d . . . H10A H 0.2286 -0.0244 0.0114 0.030 Uiso 1 1 calc R . . H10B H 0.1897 0.0658 0.0549 0.030 Uiso 1 1 calc R . . C4 C 0.5524(4) 0.0318(4) 0.1159(2) 0.0234(12) Uani 1 1 d . . . H4 H 0.6034 0.0132 0.1409 0.028 Uiso 1 1 calc R . . C21 C 0.1926(4) -0.0145(5) 0.3562(2) 0.0381(15) Uani 1 1 d . . . H21A H 0.1802 -0.0819 0.3456 0.046 Uiso 1 1 calc R . . H21B H 0.1727 0.0312 0.3266 0.046 Uiso 1 1 calc R . . C31 C 0.8815(5) 0.0239(4) 0.2958(2) 0.0395(15) Uani 1 1 d . . . H31A H 0.9476 0.0620 0.2818 0.047 Uiso 1 1 calc R . . H31B H 0.8341 0.0247 0.2661 0.047 Uiso 1 1 calc R . . C20 C 0.8143(5) -0.2360(4) 0.1378(2) 0.0355(14) Uani 1 1 d . . . H20A H 0.7786 -0.2970 0.1324 0.043 Uiso 1 1 calc R . . H20B H 0.8942 -0.2546 0.1418 0.043 Uiso 1 1 calc R . . C52 C 0.8473(4) 0.5172(4) 0.2249(2) 0.0276(12) Uani 1 1 d . . . H52A H 0.8625 0.5740 0.1995 0.033 Uiso 1 1 calc R . . H52B H 0.8404 0.4595 0.2016 0.033 Uiso 1 1 calc R . . C36 C 0.6692(4) 0.4160(4) 0.4329(2) 0.0229(12) Uani 1 1 d . . . C64 C 0.8748(4) 0.5815(4) -0.0231(2) 0.0342(14) Uani 1 1 d . . . H64A H 0.9094 0.5908 0.0106 0.041 Uiso 1 1 calc R . . H64B H 0.8258 0.6418 -0.0285 0.041 Uiso 1 1 calc R . . C11 C 0.0959(4) -0.0536(4) 0.0757(2) 0.0259(12) Uani 1 1 d . . . H11A H 0.1124 -0.1259 0.0760 0.031 Uiso 1 1 calc R . . H11B H 0.0387 -0.0379 0.0512 0.031 Uiso 1 1 calc R . . C55 C 0.1653(4) 0.7489(4) 0.1963(2) 0.0306(13) Uani 1 1 d . . . H55A H 0.1946 0.8048 0.1732 0.037 Uiso 1 1 calc R . . H55B H 0.0954 0.7740 0.2227 0.037 Uiso 1 1 calc R . . C65 C 0.2762(5) 0.3134(4) 0.1368(2) 0.0460(18) Uani 1 1 d . . . H65A H 0.2296 0.3772 0.1427 0.055 Uiso 1 1 calc R . . H65B H 0.3281 0.3080 0.1645 0.055 Uiso 1 1 calc R . . C30 C 0.8131(4) 0.0716(4) 0.3478(2) 0.0382(15) Uani 1 1 d . . . H30A H 0.8585 0.0686 0.3784 0.046 Uiso 1 1 calc R . . H30B H 0.7919 0.1416 0.3403 0.046 Uiso 1 1 calc R . . C43 C 0.2670(4) 0.5145(4) 0.4139(2) 0.0296(13) Uani 1 1 d . . . H43A H 0.2486 0.5313 0.4547 0.035 Uiso 1 1 calc R . . H43B H 0.2695 0.4423 0.4099 0.035 Uiso 1 1 calc R . . C66 C 0.2009(5) 0.2309(5) 0.1444(3) 0.0482(18) Uani 1 1 d . . . H66A H 0.2481 0.1673 0.1398 0.058 Uiso 1 1 calc R . . H66B H 0.1521 0.2348 0.1152 0.058 Uiso 1 1 calc R . . C8 C 0.7388(4) 0.1447(4) 0.1171(2) 0.0317(13) Uani 1 1 d . . . H8A H 0.7787 0.0779 0.1145 0.038 Uiso 1 1 calc R . . H8B H 0.6888 0.1525 0.1547 0.038 Uiso 1 1 calc R . . C42 C 0.9520(4) 0.2946(5) 0.4279(2) 0.0397(15) Uani 1 1 d . . . H42A H 0.9194 0.2303 0.4333 0.048 Uiso 0.8969(12) 1 calc PR A 1 H42B H 0.9684 0.3156 0.4646 0.048 Uiso 0.8969(12) 1 calc PR A 1 H42C H 0.9161 0.2465 0.4551 0.048 Uiso 0.1031(12) 1 calc PR A 2 H42D H 1.0138 0.3240 0.4423 0.048 Uiso 0.1031(12) 1 calc PR A 2 C22 C 0.1176(5) 0.0139(5) 0.4137(2) 0.0403(15) Uani 1 1 d . . . H22A H 0.0364 0.0115 0.4109 0.048 Uiso 1 1 calc R . . H22B H 0.1290 0.0822 0.4232 0.048 Uiso 1 1 calc R . . C44 C 0.1796(4) 0.5637(4) 0.3841(2) 0.0333(13) Uani 1 1 d . . . H44A H 0.1049 0.5379 0.3984 0.040 Uiso 1 1 calc R . . H44B H 0.2007 0.5486 0.3431 0.040 Uiso 1 1 calc R . . C33 C 0.1650(4) 0.2397(4) 0.5613(2) 0.0338(14) Uani 1 1 d . . . H33A H 0.1928 0.2475 0.5971 0.041 Uiso 1 1 calc R . . H33B H 0.0904 0.2115 0.5705 0.041 Uiso 1 1 calc R . . Br7A Br 0.9960(5) 0.2455(5) 0.3524(3) 0.0528(2) Uani 0.1031(12) 1 d P A 2 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 Br1 0.0318(3) 0.0406(3) 0.0375(3) -0.0044(3) -0.0003(2) -0.0127(3) Br6 0.0307(3) 0.0382(3) 0.0350(3) 0.0012(3) 0.0001(2) -0.0027(2) Br10 0.0304(3) 0.0466(4) 0.0383(3) -0.0129(3) -0.0081(2) -0.0024(3) Br11 0.0364(3) 0.0544(4) 0.0381(3) -0.0133(3) 0.0149(3) -0.0244(3) Br3 0.0396(3) 0.0567(4) 0.0267(3) 0.0067(3) 0.0027(2) -0.0094(3) Br9 0.0330(3) 0.0608(4) 0.0380(3) -0.0086(3) -0.0027(3) -0.0147(3) Br2 0.0371(3) 0.0533(4) 0.0288(3) 0.0014(3) 0.0026(2) 0.0012(3) Br8 0.0317(3) 0.0345(3) 0.0544(4) 0.0029(3) 0.0007(3) 0.0060(2) Br5 0.0447(3) 0.0428(4) 0.0436(4) -0.0026(3) 0.0087(3) 0.0100(3) Br4 0.0575(4) 0.0462(4) 0.0378(4) 0.0032(3) 0.0107(3) -0.0108(3) Br7 0.0394(4) 0.0619(5) 0.0473(4) 0.0052(4) 0.0088(3) 0.0141(3) Br12 0.1245(7) 0.0718(6) 0.0813(6) -0.0336(5) 0.0748(6) -0.0588(5) O8 0.0154(16) 0.033(2) 0.029(2) 0.0108(17) -0.0002(14) -0.0012(15) O1 0.0237(18) 0.030(2) 0.039(2) 0.0156(17) -0.0161(16) -0.0161(16) O9 0.0163(17) 0.051(2) 0.0166(18) 0.0009(17) 0.0009(14) 0.0021(16) O10 0.0143(16) 0.042(2) 0.0205(18) 0.0066(17) -0.0025(14) 0.0042(15) O6 0.0209(17) 0.034(2) 0.0227(19) -0.0078(17) 0.0013(14) -0.0017(16) C28 0.026(3) 0.026(3) 0.010(2) 0.003(2) -0.002(2) 0.004(2) O4 0.0174(17) 0.043(2) 0.028(2) -0.0030(18) -0.0009(15) -0.0008(16) O3 0.0242(18) 0.035(2) 0.0179(18) 0.0003(16) -0.0037(14) -0.0007(16) C57 0.022(2) 0.016(2) 0.011(2) 0.001(2) -0.0047(19) 0.003(2) O2 0.0188(17) 0.0252(19) 0.030(2) 0.0081(16) -0.0093(15) -0.0116(15) C49 0.020(2) 0.015(2) 0.015(2) 0.000(2) -0.0010(19) -0.008(2) O12 0.0254(18) 0.032(2) 0.031(2) -0.0039(18) 0.0063(15) -0.0134(16) C61 0.019(2) 0.020(3) 0.017(3) 0.004(2) -0.002(2) -0.004(2) O11 0.0200(17) 0.036(2) 0.031(2) -0.0120(18) 0.0075(15) -0.0157(16) C32 0.022(3) 0.031(3) 0.034(3) 0.000(3) -0.002(2) -0.004(2) O5 0.0219(18) 0.037(2) 0.034(2) -0.0143(19) 0.0048(16) -0.0001(16) C60 0.020(2) 0.019(3) 0.009(2) 0.003(2) -0.0033(18) 0.000(2) C2 0.020(2) 0.017(3) 0.014(2) 0.001(2) 0.0008(19) -0.002(2) C48 0.019(2) 0.027(3) 0.016(3) -0.004(2) 0.000(2) -0.002(2) C6 0.018(2) 0.016(3) 0.014(2) -0.004(2) -0.0032(19) -0.002(2) C51 0.019(2) 0.017(3) 0.017(3) 0.000(2) 0.002(2) -0.001(2) C24 0.026(3) 0.022(3) 0.017(3) 0.002(2) -0.009(2) 0.001(2) C40 0.020(2) 0.024(3) 0.017(3) -0.001(2) -0.001(2) -0.004(2) C25 0.017(2) 0.032(3) 0.015(3) 0.003(2) -0.0024(19) 0.005(2) C62 0.016(2) 0.024(3) 0.020(3) 0.002(2) 0.003(2) -0.003(2) C1 0.025(3) 0.021(3) 0.016(3) 0.000(2) 0.002(2) -0.002(2) C34 0.023(2) 0.026(3) 0.017(3) -0.001(2) -0.003(2) -0.004(2) C12 0.025(3) 0.031(3) 0.024(3) 0.007(2) -0.008(2) -0.013(2) C7 0.020(2) 0.017(3) 0.013(2) 0.001(2) -0.0034(19) 0.001(2) C14 0.025(3) 0.021(3) 0.019(3) 0.003(2) 0.002(2) -0.006(2) C59 0.016(2) 0.022(3) 0.019(3) -0.001(2) 0.0026(19) -0.003(2) C50 0.021(2) 0.018(3) 0.025(3) 0.004(2) -0.003(2) -0.007(2) C13 0.027(3) 0.020(3) 0.018(3) 0.010(2) -0.005(2) -0.012(2) C5 0.019(2) 0.020(3) 0.010(2) 0.002(2) -0.0015(19) -0.006(2) C29 0.017(2) 0.027(3) 0.019(3) 0.002(2) -0.002(2) -0.004(2) C58 0.021(2) 0.025(3) 0.014(2) 0.005(2) -0.002(2) -0.005(2) C27 0.023(3) 0.023(3) 0.016(3) 0.004(2) -0.007(2) 0.001(2) C15 0.020(2) 0.023(3) 0.021(3) 0.002(2) -0.007(2) -0.003(2) C63 0.025(3) 0.037(3) 0.023(3) -0.007(3) 0.007(2) -0.008(2) C38 0.024(3) 0.020(3) 0.015(2) -0.004(2) 0.001(2) -0.007(2) O7 0.0181(18) 0.073(3) 0.029(2) 0.019(2) -0.0046(16) -0.0049(19) C56 0.023(2) 0.020(3) 0.015(2) 0.003(2) -0.004(2) -0.003(2) C46 0.023(2) 0.015(2) 0.016(2) 0.002(2) -0.002(2) -0.008(2) C26 0.023(3) 0.030(3) 0.019(3) -0.003(2) -0.001(2) 0.000(2) C54 0.018(2) 0.026(3) 0.029(3) -0.006(2) 0.001(2) 0.000(2) C45 0.026(3) 0.030(3) 0.015(3) 0.000(2) -0.002(2) -0.011(2) C16 0.027(3) 0.018(3) 0.020(3) 0.007(2) -0.009(2) -0.009(2) C3 0.020(2) 0.024(3) 0.023(3) 0.000(2) -0.002(2) -0.009(2) C41 0.027(3) 0.040(4) 0.043(4) 0.008(3) 0.004(3) 0.002(3) C35 0.025(3) 0.016(3) 0.017(3) -0.007(2) -0.001(2) -0.003(2) C37 0.024(3) 0.030(3) 0.016(3) -0.005(2) 0.000(2) -0.004(2) C53 0.023(3) 0.035(3) 0.029(3) -0.001(3) -0.001(2) 0.004(2) C18 0.017(2) 0.033(3) 0.031(3) 0.007(3) -0.006(2) -0.011(2) C17 0.024(3) 0.021(3) 0.022(3) 0.004(2) -0.002(2) -0.003(2) C23 0.025(3) 0.026(3) 0.015(3) 0.003(2) -0.002(2) 0.001(2) C47 0.017(2) 0.028(3) 0.021(3) 0.003(2) -0.006(2) -0.006(2) C39 0.019(2) 0.024(3) 0.020(3) -0.007(2) 0.000(2) 0.000(2) C9 0.024(3) 0.055(4) 0.033(3) -0.012(3) 0.004(2) -0.018(3) C19 0.029(3) 0.040(3) 0.025(3) 0.000(3) -0.003(2) 0.000(2) C10 0.023(3) 0.030(3) 0.025(3) -0.001(2) -0.010(2) -0.011(2) C4 0.020(2) 0.027(3) 0.024(3) 0.002(2) -0.009(2) -0.001(2) C21 0.023(3) 0.053(4) 0.037(3) -0.002(3) -0.003(2) -0.006(3) C31 0.037(3) 0.036(3) 0.038(3) -0.005(3) 0.011(3) -0.001(3) C20 0.035(3) 0.038(3) 0.032(3) 0.005(3) -0.006(2) 0.003(3) C52 0.027(3) 0.035(3) 0.019(3) -0.001(2) -0.001(2) -0.001(2) C36 0.020(3) 0.031(3) 0.018(3) -0.002(2) -0.004(2) -0.003(2) C64 0.029(3) 0.037(3) 0.033(3) -0.008(3) 0.008(2) -0.016(3) C11 0.021(2) 0.029(3) 0.028(3) -0.004(2) -0.003(2) -0.007(2) C55 0.021(3) 0.029(3) 0.041(3) -0.009(3) -0.005(2) -0.001(2) C65 0.047(3) 0.041(4) 0.042(4) -0.011(3) 0.022(3) -0.020(3) C30 0.032(3) 0.041(4) 0.036(3) -0.009(3) 0.008(3) -0.004(3) C43 0.023(3) 0.037(3) 0.027(3) 0.005(3) 0.002(2) -0.005(2) C66 0.051(4) 0.042(4) 0.043(4) -0.007(3) 0.021(3) -0.019(3) C8 0.032(3) 0.039(3) 0.028(3) 0.005(3) -0.010(2) -0.013(3) C42 0.033(3) 0.050(4) 0.034(3) 0.009(3) -0.004(3) 0.003(3) C22 0.033(3) 0.052(4) 0.037(3) -0.006(3) -0.012(3) 0.008(3) C44 0.024(3) 0.034(3) 0.044(4) 0.006(3) -0.012(2) -0.005(2) C33 0.029(3) 0.041(3) 0.027(3) 0.003(3) 0.004(2) -0.001(3) Br7A 0.0394(4) 0.0619(5) 0.0473(4) 0.0052(4) 0.0088(3) 0.0141(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 Br1 C9 1.954(5) . ? Br6 C33 1.944(6) . ? Br10 C55 1.953(5) . ? Br11 C64 1.959(4) . ? Br3 C20 1.946(6) . ? Br9 C53 1.952(5) . ? Br2 C11 1.951(4) . ? Br8 C44 1.953(5) . ? Br5 C31 1.934(6) . ? Br4 C22 1.930(6) . ? Br7 C42 1.926(5) . ? Br12 C66 1.930(5) . ? O8 C39 1.378(6) . ? O8 C43 1.430(6) . ? O1 C3 1.392(5) . ? O1 C8 1.412(6) . ? O9 C47 1.377(6) . ? O9 C52 1.419(5) . ? O10 C50 1.374(6) . ? O10 C54 1.416(5) . ? O6 C28 1.384(5) . ? O6 C32 1.415(6) . ? C28 C27 1.383(7) . ? C28 C29 1.388(6) . ? O4 C17 1.386(5) . ? O4 C21 1.413(6) . ? O3 C14 1.379(5) . ? O3 C19 1.412(6) . ? C57 C62 1.384(6) . ? C57 C58 1.397(6) . ? C57 C56 1.514(6) . ? O2 C6 1.387(5) . ? O2 C10 1.424(6) . ? C49 C48 1.378(7) . ? C49 C50 1.401(6) . ? C49 C56 1.523(6) . ? O12 C61 1.390(5) . ? O12 C65 1.414(6) . ? C61 C62 1.379(6) . ? C61 C60 1.381(6) . ? O11 C58 1.377(5) . ? O11 C63 1.435(5) . ? C32 C33 1.490(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O5 C25 1.383(5) . ? O5 C30 1.408(6) . ? C60 C59 1.385(6) . ? C60 C1 1.520(6) . ? C2 C7 1.383(6) . ? C2 C3 1.390(7) . ? C2 C1 1.510(7) . ? C48 C47 1.390(7) . ? C48 H48 0.9500 . ? C6 C5 1.389(7) . ? C6 C7 1.390(7) . ? C51 C46 1.378(7) . ? C51 C50 1.379(7) . ? C51 H51 0.9500 . ? C24 C25 1.378(7) . ? C24 C29 1.388(6) . ? C24 C23 1.526(6) . ? C40 C39 1.370(7) . ? C40 C35 1.398(7) . ? C40 H40 0.9500 . ? C25 C26 1.397(7) . ? C62 H62 0.9500 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C34 C35 1.511(7) . ? C34 C27 1.517(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C12 C13 1.513(7) . ? C12 C5 1.519(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C7 H7 0.9500 . ? C14 C13 1.386(7) . ? C14 C15 1.395(7) . ? C59 C58 1.376(6) . ? C59 H59 0.9500 . ? C13 C18 1.414(6) . ? C5 C4 1.396(6) . ? C29 H29 0.9500 . ? C27 C26 1.389(6) . ? C15 C16 1.386(6) . ? C15 H15 0.9500 . ? C63 C64 1.506(7) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C38 C37 1.384(7) . ? C38 C39 1.406(6) . ? C38 C45 1.507(7) . ? O7 C41 1.387(6) . ? O7 C36 1.396(6) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C46 C47 1.401(6) . ? C46 C45 1.527(6) . ? C26 H26 0.9500 . ? C54 C55 1.472(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C16 C17 1.381(7) . ? C16 C23 1.523(7) . ? C3 C4 1.373(7) . ? C41 C42 1.501(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C35 C36 1.381(6) . ? C37 C36 1.386(7) . ? C37 H37 0.9500 . ? C53 C52 1.496(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C18 C17 1.377(7) . ? C18 H18 0.9500 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C9 C8 1.493(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C19 C20 1.498(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C10 C11 1.502(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C4 H4 0.9500 . ? C21 C22 1.536(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C31 C30 1.486(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C65 C66 1.492(7) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C43 C44 1.486(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C42 Br7A 1.906(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 H42C 0.9900 . ? C42 H42D 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 C39 O8 C43 116.3(4) . . ? C3 O1 C8 117.9(4) . . ? C47 O9 C52 117.7(4) . . ? C50 O10 C54 119.2(4) . . ? C28 O6 C32 118.5(3) . . ? C27 C28 O6 116.0(4) . . ? C27 C28 C29 121.0(4) . . ? O6 C28 C29 123.0(4) . . ? C17 O4 C21 117.6(4) . . ? C14 O3 C19 118.9(4) . . ? C62 C57 C58 118.1(4) . . ? C62 C57 C56 121.1(4) . . ? C58 C57 C56 120.8(4) . . ? C6 O2 C10 118.0(4) . . ? C48 C49 C50 118.2(4) . . ? C48 C49 C56 120.5(4) . . ? C50 C49 C56 121.3(4) . . ? C61 O12 C65 116.5(4) . . ? C62 C61 C60 120.5(4) . . ? C62 C61 O12 121.6(4) . . ? C60 C61 O12 117.8(4) . . ? C58 O11 C63 117.0(3) . . ? O6 C32 C33 108.3(4) . . ? O6 C32 H32A 110.0 . . ? C33 C32 H32A 110.0 . . ? O6 C32 H32B 110.0 . . ? C33 C32 H32B 110.0 . . ? H32A C32 H32B 108.4 . . ? C25 O5 C30 117.7(4) . . ? C61 C60 C59 118.1(4) . . ? C61 C60 C1 121.3(4) . . ? C59 C60 C1 120.6(4) . . ? C7 C2 C3 118.0(5) . . ? C7 C2 C1 120.3(4) . . ? C3 C2 C1 121.7(4) . . ? C49 C48 C47 121.6(4) . . ? C49 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? O2 C6 C5 115.4(4) . . ? O2 C6 C7 123.6(4) . . ? C5 C6 C7 121.0(4) . . ? C46 C51 C50 121.8(4) . . ? C46 C51 H51 119.1 . . ? C50 C51 H51 119.1 . . ? C25 C24 C29 118.4(4) . . ? C25 C24 C23 120.5(4) . . ? C29 C24 C23 121.0(4) . . ? C39 C40 C35 121.6(4) . . ? C39 C40 H40 119.2 . . ? C35 C40 H40 119.2 . . ? C24 C25 O5 116.7(4) . . ? C24 C25 C26 120.8(4) . . ? O5 C25 C26 122.5(4) . . ? C61 C62 C57 121.5(4) . . ? C61 C62 H62 119.2 . . ? C57 C62 H62 119.2 . . ? C2 C1 C60 114.8(4) . . ? C2 C1 H1A 108.6 . . ? C60 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? C60 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? C35 C34 C27 111.6(4) . . ? C35 C34 H34A 109.3 . . ? C27 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C27 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C13 C12 C5 116.1(4) . . ? C13 C12 H12A 108.3 . . ? C5 C12 H12A 108.3 . . ? C13 C12 H12B 108.3 . . ? C5 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? C2 C7 C6 120.9(5) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? O3 C14 C13 114.6(4) . . ? O3 C14 C15 124.7(4) . . ? C13 C14 C15 120.7(4) . . ? C58 C59 C60 122.0(4) . . ? C58 C59 H59 119.0 . . ? C60 C59 H59 119.0 . . ? O10 C50 C51 124.7(4) . . ? O10 C50 C49 115.0(4) . . ? C51 C50 C49 120.2(5) . . ? C14 C13 C18 118.0(4) . . ? C14 C13 C12 121.6(4) . . ? C18 C13 C12 120.4(5) . . ? C6 C5 C4 117.7(5) . . ? C6 C5 C12 120.5(4) . . ? C4 C5 C12 121.7(4) . . ? C28 C29 C24 120.8(4) . . ? C28 C29 H29 119.6 . . ? C24 C29 H29 119.6 . . ? C59 C58 O11 124.7(4) . . ? C59 C58 C57 119.8(4) . . ? O11 C58 C57 115.6(4) . . ? C28 C27 C26 118.2(4) . . ? C28 C27 C34 122.3(4) . . ? C26 C27 C34 119.5(4) . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O11 C63 C64 104.5(4) . . ? O11 C63 H63A 110.9 . . ? C64 C63 H63A 110.9 . . ? O11 C63 H63B 110.9 . . ? C64 C63 H63B 110.9 . . ? H63A C63 H63B 108.9 . . ? C37 C38 C39 117.9(5) . . ? C37 C38 C45 121.4(4) . . ? C39 C38 C45 120.6(5) . . ? C41 O7 C36 117.2(4) . . ? C57 C56 C49 114.1(4) . . ? C57 C56 H56A 108.7 . . ? C49 C56 H56A 108.7 . . ? C57 C56 H56B 108.7 . . ? C49 C56 H56B 108.7 . . ? H56A C56 H56B 107.6 . . ? C51 C46 C47 118.2(4) . . ? C51 C46 C45 121.4(4) . . ? C47 C46 C45 120.3(4) . . ? C27 C26 C25 120.7(4) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? O10 C54 C55 108.1(4) . . ? O10 C54 H54A 110.1 . . ? C55 C54 H54A 110.1 . . ? O10 C54 H54B 110.1 . . ? C55 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? C38 C45 C46 116.6(4) . . ? C38 C45 H45A 108.1 . . ? C46 C45 H45A 108.1 . . ? C38 C45 H45B 108.1 . . ? C46 C45 H45B 108.1 . . ? H45A C45 H45B 107.3 . . ? C17 C16 C15 118.6(4) . . ? C17 C16 C23 120.6(4) . . ? C15 C16 C23 120.6(4) . . ? C4 C3 C2 121.3(4) . . ? C4 C3 O1 123.5(5) . . ? C2 C3 O1 115.1(4) . . ? O7 C41 C42 106.7(5) . . ? O7 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? O7 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? C36 C35 C40 117.6(5) . . ? C36 C35 C34 122.3(5) . . ? C40 C35 C34 120.1(4) . . ? C38 C37 C36 121.0(5) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C52 C53 Br9 110.1(3) . . ? C52 C53 H53A 109.6 . . ? Br9 C53 H53A 109.6 . . ? C52 C53 H53B 109.6 . . ? Br9 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C17 C18 C13 120.5(5) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C18 C17 C16 121.4(4) . . ? C18 C17 O4 122.0(4) . . ? C16 C17 O4 116.6(4) . . ? C16 C23 C24 116.5(4) . . ? C16 C23 H23A 108.2 . . ? C24 C23 H23A 108.2 . . ? C16 C23 H23B 108.2 . . ? C24 C23 H23B 108.2 . . ? H23A C23 H23B 107.3 . . ? O9 C47 C48 124.7(4) . . ? O9 C47 C46 115.3(4) . . ? C48 C47 C46 119.9(5) . . ? C40 C39 O8 124.8(4) . . ? C40 C39 C38 120.5(5) . . ? O8 C39 C38 114.7(5) . . ? C8 C9 Br1 112.0(3) . . ? C8 C9 H9A 109.2 . . ? Br1 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? Br1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? O3 C19 C20 107.7(4) . . ? O3 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O3 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? O2 C10 C11 107.7(4) . . ? O2 C10 H10A 110.2 . . ? C11 C10 H10A 110.2 . . ? O2 C10 H10B 110.2 . . ? C11 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C3 C4 C5 121.0(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? O4 C21 C22 108.4(4) . . ? O4 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? O4 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? C30 C31 Br5 112.0(4) . . ? C30 C31 H31A 109.2 . . ? Br5 C31 H31A 109.2 . . ? C30 C31 H31B 109.2 . . ? Br5 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C19 C20 Br3 112.4(4) . . ? C19 C20 H20A 109.1 . . ? Br3 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? Br3 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? O9 C52 C53 108.2(4) . . ? O9 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? O9 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C35 C36 C37 121.3(5) . . ? C35 C36 O7 116.6(5) . . ? C37 C36 O7 122.1(4) . . ? C63 C64 Br11 107.6(3) . . ? C63 C64 H64A 110.2 . . ? Br11 C64 H64A 110.2 . . ? C63 C64 H64B 110.2 . . ? Br11 C64 H64B 110.2 . . ? H64A C64 H64B 108.5 . . ? C10 C11 Br2 111.0(3) . . ? C10 C11 H11A 109.4 . . ? Br2 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? Br2 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C54 C55 Br10 112.6(3) . . ? C54 C55 H55A 109.1 . . ? Br10 C55 H55A 109.1 . . ? C54 C55 H55B 109.1 . . ? Br10 C55 H55B 109.1 . . ? H55A C55 H55B 107.8 . . ? O12 C65 C66 107.7(4) . . ? O12 C65 H65A 110.2 . . ? C66 C65 H65A 110.2 . . ? O12 C65 H65B 110.2 . . ? C66 C65 H65B 110.2 . . ? H65A C65 H65B 108.5 . . ? O5 C30 C31 108.8(4) . . ? O5 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 . . ? O5 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? O8 C43 C44 107.4(4) . . ? O8 C43 H43A 110.2 . . ? C44 C43 H43A 110.2 . . ? O8 C43 H43B 110.2 . . ? C44 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? C65 C66 Br12 109.8(4) . . ? C65 C66 H66A 109.7 . . ? Br12 C66 H66A 109.7 . . ? C65 C66 H66B 109.7 . . ? Br12 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? O1 C8 C9 108.2(5) . . ? O1 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? O1 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C41 C42 Br7A 89.5(4) . . ? C41 C42 Br7 109.4(4) . . ? Br7A C42 Br7 44.2(2) . . ? C41 C42 H42A 109.8 . . ? Br7A C42 H42A 81.0 . . ? Br7 C42 H42A 109.8 . . ? C41 C42 H42B 109.8 . . ? Br7A C42 H42B 153.0 . . ? Br7 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C41 C42 H42C 113.7 . . ? Br7A C42 H42C 113.7 . . ? Br7 C42 H42C 131.0 . . ? H42A C42 H42C 33.2 . . ? H42B C42 H42C 76.4 . . ? C41 C42 H42D 113.7 . . ? Br7A C42 H42D 113.7 . . ? Br7 C42 H42D 69.6 . . ? H42A C42 H42D 133.7 . . ? H42B C42 H42D 41.8 . . ? H42C C42 H42D 111.0 . . ? C21 C22 Br4 112.0(4) . . ? C21 C22 H22A 109.2 . . ? Br4 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? Br4 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C43 C44 Br8 111.1(4) . . ? C43 C44 H44A 109.4 . . ? Br8 C44 H44A 109.4 . . ? C43 C44 H44B 109.4 . . ? Br8 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C32 C33 Br6 112.8(4) . . ? C32 C33 H33A 109.0 . . ? Br6 C33 H33A 109.0 . . ? C32 C33 H33B 109.0 . . ? Br6 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.358 _refine_diff_density_min -1.407 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.502 0.713 0.732 211 40 ' ' 2 0.498 0.287 0.268 211 40 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 946657'