data_007b-17085 _vrf_RINTA01_007b-17085 ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: The diffraction data was not ideal due to crystal quality. The crystal was very small and produced weak diffraction. ; _vrf_PLAT020_007b-17085 ; PROBLEM: The value of Rint is greater than 0.12 RESPONSE: See the response to RINTA01 ; _vrf_PLAT341_007b-17085 ; PROBLEM: Low Bond Precision on C-C Bonds RESPONSE: The reflections were weak and streaky, leading to a non-ideal integration ; _vrf_PLAT363_007b-17085 ; PROBLEM: Long C(sp3)-C(sp2) Bond RESPONSE: The model is not of an ideal quality due to the problematic diffraction data. ; _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 Br2 F6 N2 O3' _chemical_formula_sum 'C27 H26 Br2 F6 N2 O3' _chemical_formula_weight 700.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.8852(2) _cell_length_b 24.6027(7) _cell_length_c 26.0792(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5700.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 18494 _cell_measurement_theta_min 3.5660 _cell_measurement_theta_max 64.9360 _exptl_crystal_description Needle _exptl_crystal_colour Colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_F_000 2800 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 4.251 _shelx_estimated_absorpt_T_min 0.362 _shelx_estimated_absorpt_T_max 0.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66725 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'microfocus rotating anode' _diffrn_measurement_device_type 'Rigaku Saturn 944+ CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 22.2 _diffrn_reflns_number 204401 _diffrn_reflns_av_unetI/netI 0.0687 _diffrn_reflns_av_R_equivalents 0.2362 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.469 _diffrn_reflns_theta_max 66.586 _diffrn_reflns_theta_full 66.586 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 10085 _reflns_number_gt 6951 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.790 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ; Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., OLEX2: A complete structure solution, refinement and analysis program (2009). J. Appl. Cryst., 42, 339-341. ; _computing_publication_material 'CIFTAB-2014/2 (Sheldrick, 2014)' _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. The hydrogen atoms were first found in the difference map, then generated geometrically and refined as riding atoms with C-H distances = 0.95 - 0.99 angstroms and Uiso(H) = 1.2 times Ueq(C) for CH, NH, and CH2 groups and Uiso(H) = 1.5 times Ueq(C) for CH3 groups. The two of the four aryl ring with CF3 and Br are disordered. The occupancies of the disordered atoms were freely refined to occupancies of 0.930(5) and 0.070(5). The major component has atom label suffixes of "a"; the minor has "b". Chemically equivalent C-C, F-C, and Br-C bonds were restrained to be similar. The thermal ellipsoids of the entire model were restrained to have similar tensor directions; a requirement due to the poor data quality Additionally, the small occupancy of the disordered aryl required that the thermal ellipsoids be constrained to their chemically equivalent counterparts in the major component. Finally, the tert-butyl group with atoms C24 to C27 is disordered over two positions. The chemically equivalent C-C bonds were restrained to be similar. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+20.1020P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary SHELXT _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_abs_structure_details ; Flack x determined using 2197 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.07(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 10085 _refine_ls_number_parameters 822 _refine_ls_number_restraints 997 _refine_ls_R_factor_all 0.1167 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.068 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7009(13) 0.5602(5) 0.3409(5) 0.025(2) Uani 1 1 d . U . . . O1 O 0.4659(10) 0.5381(3) 0.2995(3) 0.0292(19) Uani 1 1 d . U . . . Br2 Br 0.95075(19) 0.34378(6) 0.50079(7) 0.0522(4) Uani 1 1 d . U . . . N1 N 0.6746(11) 0.4961(4) 0.2704(4) 0.025(2) Uani 1 1 d . U . . . H1 H 0.7734 0.4957 0.2729 0.030 Uiso 1 1 calc R U . A 1 N2 N 0.8303(13) 0.5352(4) 0.4202(4) 0.032(2) Uani 1 1 d . U . . . H2 H 0.8495 0.5703 0.4210 0.039 Uiso 1 1 calc R U . . . O2 O 0.6879(12) 0.4711(4) 0.3796(3) 0.038(2) Uani 1 1 d . U . . . C2 C 0.6144(15) 0.6088(5) 0.3663(5) 0.032(3) Uani 1 1 d . U . . . H2A H 0.5160 0.6149 0.3495 0.038 Uiso 1 1 calc R U . . . H2B H 0.5980 0.6023 0.4034 0.038 Uiso 1 1 calc R U . . . O3 O 0.8589(12) 0.6497(4) 0.3997(4) 0.061(3) Uani 1 1 d . U . . . C3 C 0.7225(18) 0.6575(6) 0.3573(6) 0.063(3) Uani 1 1 d . U . . . H3 H 0.6734 0.6941 0.3574 0.076 Uiso 1 1 calc R U . . . F4 F 1.0363(12) 0.3933(4) 0.6125(3) 0.063(3) Uani 1 1 d . U . . . C4 C 0.8181(18) 0.6480(6) 0.3167(7) 0.062(4) Uani 1 1 d . U . . . H4 H 0.9125 0.6701 0.3174 0.074 Uiso 1 1 calc R U . . . C5 C 0.8442(15) 0.5860(5) 0.3154(5) 0.032(3) Uani 1 1 d . U . . . H5A H 0.9360 0.5763 0.3348 0.038 Uiso 1 1 calc R U . . . H5B H 0.8555 0.5732 0.2796 0.038 Uiso 1 1 calc R U . . . F5 F 1.2068(13) 0.4549(4) 0.6096(4) 0.071(3) Uani 1 1 d . U . . . F6 F 1.2270(12) 0.3837(4) 0.5648(4) 0.075(3) Uani 1 1 d . U . . . C6 C 0.688(2) 0.6687(8) 0.2713(8) 0.085(5) Uani 1 1 d . U . . . H6 H 0.6460 0.7038 0.2757 0.102 Uiso 1 1 calc R U . . . C7 C 0.644(3) 0.6414(10) 0.2322(8) 0.114(8) Uani 1 1 d . U . . . H7A H 0.6828 0.6060 0.2260 0.137 Uiso 1 1 calc R U . . . H7B H 0.5716 0.6565 0.2094 0.137 Uiso 1 1 calc R U . . . C8 C 0.6019(14) 0.5307(5) 0.3015(5) 0.028(2) Uani 1 1 d . U . . . C16 C 0.7400(15) 0.5177(6) 0.3818(5) 0.031(3) Uani 1 1 d . U . . . C17 C 0.8976(15) 0.5033(5) 0.4596(5) 0.032(3) Uani 1 1 d . U . . . C18 C 0.8877(15) 0.4480(6) 0.4614(5) 0.033(3) Uani 1 1 d . U . . . H18 H 0.8305 0.4283 0.4368 0.039 Uiso 1 1 calc R U . . . C19 C 0.9654(14) 0.4212(5) 0.5011(6) 0.035(3) Uani 1 1 d . U . . . C20 C 1.0471(16) 0.4491(5) 0.5390(5) 0.033(3) Uani 1 1 d . U . . . C21 C 1.0552(18) 0.5046(6) 0.5345(6) 0.042(3) Uani 1 1 d . U . . . H21 H 1.1142 0.5246 0.5582 0.050 Uiso 1 1 calc R U . . . C22 C 0.9791(16) 0.5318(5) 0.4961(6) 0.040(3) Uani 1 1 d . U . . . H22 H 0.9826 0.5704 0.4946 0.048 Uiso 1 1 calc R U . . . C23 C 1.1320(19) 0.4208(7) 0.5815(7) 0.052(3) Uani 1 1 d . U . . . C25 C 1.015(2) 0.6845(8) 0.4615(7) 0.074(5) Uani 1 1 d . U . . . H25A H 0.9164 0.6958 0.4742 0.111 Uiso 0.556(17) 1 calc R U P B 1 H25B H 1.0359 0.6471 0.4725 0.111 Uiso 0.556(17) 1 calc R U P B 1 H25C H 1.0929 0.7088 0.4752 0.111 Uiso 0.556(17) 1 calc R U P B 1 H25D H 1.0471 0.7174 0.4796 0.111 Uiso 0.444(17) 1 calc R U P B 2 H25E H 0.9751 0.6582 0.4861 0.111 Uiso 0.444(17) 1 calc R U P B 2 H25F H 1.1019 0.6685 0.4437 0.111 Uiso 0.444(17) 1 calc R U P B 2 C26 C 0.9533(19) 0.7424(6) 0.3869(6) 0.048(3) Uani 1 1 d . U . . . H26A H 0.8638 0.7495 0.4078 0.073 Uiso 0.556(17) 1 calc R U P B 1 H26B H 1.0291 0.7704 0.3936 0.073 Uiso 0.556(17) 1 calc R U P B 1 H26C H 0.9257 0.7431 0.3505 0.073 Uiso 0.556(17) 1 calc R U P B 1 H26D H 0.8707 0.7498 0.3630 0.073 Uiso 0.444(17) 1 calc R U P B 2 H26E H 0.9789 0.7757 0.4055 0.073 Uiso 0.444(17) 1 calc R U P B 2 H26F H 1.0415 0.7298 0.3677 0.073 Uiso 0.444(17) 1 calc R U P B 2 Br1A Br 0.6978(3) 0.30179(8) 0.19759(9) 0.0720(8) Uani 0.889(5) 1 d D U P C 1 F1A F 0.3709(16) 0.3002(7) 0.1539(6) 0.076(4) Uani 0.889(5) 1 d D U P C 1 F2A F 0.5128(17) 0.3285(5) 0.0945(5) 0.075(4) Uani 0.889(5) 1 d D U P C 1 F3A F 0.3050(16) 0.3691(6) 0.1040(5) 0.091(4) Uani 0.889(5) 1 d D U P C 1 C9A C 0.6136(17) 0.4620(6) 0.2359(7) 0.028(3) Uani 0.889(5) 1 d D U P C 1 C10A C 0.4923(14) 0.4772(6) 0.2037(5) 0.028(3) Uani 0.889(5) 1 d D U P C 1 H10A H 0.4507 0.5127 0.2056 0.033 Uiso 0.889(5) 1 calc R U P C 1 C11A C 0.4349(18) 0.4392(6) 0.1694(6) 0.042(3) Uani 0.889(5) 1 d D U P C 1 H11A H 0.3568 0.4502 0.1468 0.050 Uiso 0.889(5) 1 calc R U P C 1 C12A C 0.4861(17) 0.3862(6) 0.1665(6) 0.039(3) Uani 0.889(5) 1 d D U P C 1 C13A C 0.6087(17) 0.3715(6) 0.1968(6) 0.041(3) Uani 0.889(5) 1 d D U P C 1 C14A C 0.6671(18) 0.4092(6) 0.2311(6) 0.035(3) Uani 0.889(5) 1 d D U P C 1 H14A H 0.7483 0.3983 0.2524 0.042 Uiso 0.889(5) 1 calc R U P C 1 C15A C 0.4191(19) 0.3470(7) 0.1309(6) 0.066(4) Uani 0.889(5) 1 d D U P C 1 C24A C 1.017(4) 0.6873(12) 0.4003(13) 0.062(6) Uani 0.556(17) 1 d . U P B 1 C27A C 1.144(4) 0.6733(15) 0.3728(13) 0.072(8) Uani 0.556(17) 1 d . U P B 1 H27A H 1.1634 0.6344 0.3769 0.109 Uiso 0.556(17) 1 calc R U P B 1 H27B H 1.2301 0.6941 0.3856 0.109 Uiso 0.556(17) 1 calc R U P B 1 H27C H 1.1279 0.6816 0.3365 0.109 Uiso 0.556(17) 1 calc R U P B 1 F1B F 0.348(11) 0.312(6) 0.139(5) 0.076(4) Uani 0.111(5) 1 d D U P C 2 Br1B Br 0.2687(16) 0.4131(8) 0.1435(6) 0.060(5) Uani 0.111(5) 1 d D U P C 2 F2B F 0.486(15) 0.351(5) 0.084(4) 0.075(4) Uani 0.111(5) 1 d D U P C 2 F3B F 0.602(9) 0.285(3) 0.129(3) 0.077(12) Uani 0.111(5) 1 d D U P C 2 C9B C 0.628(10) 0.452(3) 0.232(4) 0.028(3) Uani 0.111(5) 1 d DG U P C 2 C14B C 0.502(8) 0.455(3) 0.201(4) 0.035(3) Uani 0.111(5) 1 d DG U P C 2 H14B H 0.4397 0.4866 0.2016 0.042 Uiso 0.111(5) 1 calc R U P C 2 C13B C 0.467(5) 0.413(4) 0.168(3) 0.041(3) Uani 0.111(5) 1 d DG U P C 2 C12B C 0.558(8) 0.367(3) 0.167(3) 0.039(3) Uani 0.111(5) 1 d DG U P C 2 C11B C 0.684(8) 0.363(3) 0.198(3) 0.042(3) Uani 0.111(5) 1 d DG U P C 2 H11B H 0.7463 0.3320 0.1970 0.050 Uiso 0.111(5) 1 calc R U P C 2 C10B C 0.719(8) 0.406(4) 0.231(3) 0.028(3) Uani 0.111(5) 1 d DG U P C 2 H10B H 0.8052 0.4039 0.2522 0.033 Uiso 0.111(5) 1 calc R U P C 2 C15B C 0.496(10) 0.325(3) 0.130(3) 0.064(6) Uani 0.111(5) 1 d D U P C 2 C24B C 0.904(4) 0.6977(11) 0.4257(11) 0.045(5) Uani 0.444(17) 1 d . U P B 2 C27B C 0.765(4) 0.7254(13) 0.4586(14) 0.063(8) Uani 0.444(17) 1 d . U P B 2 H27D H 0.6828 0.7352 0.4352 0.095 Uiso 0.444(17) 1 calc R U P B 2 H27E H 0.8011 0.7581 0.4761 0.095 Uiso 0.444(17) 1 calc R U P B 2 H27F H 0.7276 0.6993 0.4840 0.095 Uiso 0.444(17) 1 calc R U P B 2 N3 N 0.1845(13) 0.4979(4) 0.2706(4) 0.030(2) Uani 1 1 d . U . . . H3A H 0.2831 0.4971 0.2737 0.036 Uiso 1 1 calc R U . . . N4 N 0.3318(12) 0.4597(5) 0.4179(4) 0.032(2) Uani 1 1 d . U . . . H4A H 0.3600 0.4255 0.4155 0.039 Uiso 1 1 calc R U . . . O4 O -0.0346(10) 0.4562(4) 0.2943(4) 0.038(2) Uani 1 1 d . U . . . Br04 Br 0.4324(2) 0.65019(7) 0.50155(9) 0.0757(6) Uani 1 1 d . U . . . O5 O 0.1709(11) 0.5218(4) 0.3827(4) 0.038(2) Uani 1 1 d . U . . . O6 O 0.4068(8) 0.3473(3) 0.3857(3) 0.0311(18) Uani 1 1 d . U . . . F7A F -0.1777(17) 0.6289(6) 0.1038(5) 0.090(4) Uani 0.930(5) 1 d D U P D 1 F8A F 0.0286(18) 0.6723(7) 0.0977(5) 0.110(5) Uani 0.930(5) 1 d D U P D 1 F9A F -0.1308(14) 0.6956(5) 0.1540(5) 0.077(3) Uani 0.930(5) 1 d D U P D 1 F10 F 0.7181(11) 0.5421(5) 0.6045(4) 0.070(3) Uani 1 1 d . U . . . F11 F 0.5400(13) 0.6005(5) 0.6101(4) 0.077(3) Uani 1 1 d . U . . . F12 F 0.7251(11) 0.6147(4) 0.5587(4) 0.067(3) Uani 1 1 d . U . . . C28 C 0.1955(15) 0.4348(5) 0.3413(5) 0.029(2) Uani 1 1 d . U . . . C29 C 0.3385(13) 0.4082(5) 0.3171(5) 0.025(2) Uani 1 1 d . U . . . H29A H 0.3324 0.4088 0.2792 0.030 Uiso 1 1 calc R U . . . H29B H 0.4304 0.4278 0.3279 0.030 Uiso 1 1 calc R U . . . C30 C 0.3411(13) 0.3500(5) 0.3368(4) 0.029(2) Uani 1 1 d . U . . . H30 H 0.3953 0.3257 0.3123 0.035 Uiso 1 1 calc R U . . . C31 C 0.1658(13) 0.3355(5) 0.3384(5) 0.035(3) Uani 1 1 d . U . . . H31 H 0.1496 0.3037 0.3616 0.043 Uiso 1 1 calc R U . . . C32 C 0.1081(16) 0.3862(6) 0.3642(6) 0.039(3) Uani 1 1 d . U . . . H32A H 0.1248 0.3841 0.4016 0.047 Uiso 1 1 calc R U . . . H32B H -0.0011 0.3904 0.3578 0.047 Uiso 1 1 calc R U . . . C33 C 0.0869(15) 0.3257(5) 0.2888(5) 0.046(3) Uani 1 1 d . U . . . H33 H -0.0194 0.3224 0.2911 0.056 Uiso 1 1 calc R U . . . C34 C 0.139(2) 0.3212(7) 0.2457(7) 0.071(5) Uani 1 1 d . U . . . H34A H 0.2451 0.3241 0.2406 0.085 Uiso 1 1 calc R U . . . H34B H 0.0748 0.3149 0.2173 0.085 Uiso 1 1 calc R U . . . C35 C 0.1018(14) 0.4642(5) 0.3004(5) 0.026(2) Uani 1 1 d . U . . . C37A C 0.0067(15) 0.5193(6) 0.2002(5) 0.038(3) Uani 0.930(5) 1 d D U P D 1 H37A H -0.0261 0.4826 0.1990 0.046 Uiso 0.930(5) 1 calc R U P D 1 C38A C -0.0565(19) 0.5591(6) 0.1686(6) 0.044(4) Uani 0.930(5) 1 d D U P D 1 H38A H -0.1397 0.5500 0.1474 0.053 Uiso 0.930(5) 1 calc R U P D 1 C39A C 0.0007(17) 0.6117(6) 0.1676(7) 0.045(3) Uani 0.930(5) 1 d D U P D 1 C40A C 0.1150(16) 0.6251(6) 0.2013(7) 0.041(3) Uani 0.930(5) 1 d D U P D 1 C41A C 0.1768(16) 0.5884(5) 0.2349(6) 0.032(3) Uani 0.930(5) 1 d D U P D 1 H41A H 0.2550 0.5984 0.2578 0.039 Uiso 0.930(5) 1 calc R U P D 1 C42A C -0.0712(18) 0.6528(7) 0.1305(7) 0.069(4) Uani 0.930(5) 1 d D U P D 1 C43 C 0.2297(14) 0.4780(6) 0.3817(5) 0.030(3) Uani 1 1 d . U . . . C44 C 0.3950(15) 0.4903(6) 0.4579(5) 0.031(3) Uani 1 1 d . U . . . C45 C 0.4845(15) 0.4632(6) 0.4929(6) 0.041(3) Uani 1 1 d . U . . . H45 H 0.4959 0.4249 0.4907 0.049 Uiso 1 1 calc R U . . . C46 C 0.557(2) 0.4919(7) 0.5310(7) 0.054(4) Uani 1 1 d . U . . . H46 H 0.6174 0.4729 0.5553 0.065 Uiso 1 1 calc R U . . . C47 C 0.5448(19) 0.5466(7) 0.5345(5) 0.046(3) Uani 1 1 d . U . . . C48 C 0.4537(17) 0.5746(6) 0.4999(6) 0.043(3) Uani 1 1 d . U . . . C49 C 0.3821(18) 0.5467(6) 0.4625(6) 0.042(3) Uani 1 1 d . U . . . H49 H 0.3214 0.5660 0.4387 0.050 Uiso 1 1 calc R U . . . C50 C 0.6296(19) 0.5760(8) 0.5772(6) 0.056(3) Uani 1 1 d . U . . . C51 C 0.5208(15) 0.3062(5) 0.3953(5) 0.035(3) Uani 1 1 d . U . . . C52 C 0.5530(15) 0.3111(6) 0.4515(5) 0.045(3) Uani 1 1 d . U . . . H52A H 0.5766 0.3489 0.4598 0.068 Uiso 1 1 calc R U . . . H52B H 0.6389 0.2879 0.4603 0.068 Uiso 1 1 calc R U . . . H52C H 0.4645 0.2995 0.4710 0.068 Uiso 1 1 calc R U . . . C53 C 0.4714(19) 0.2497(6) 0.3814(6) 0.051(4) Uani 1 1 d . U . . . H53A H 0.3793 0.2407 0.4002 0.076 Uiso 1 1 calc R U . . . H53B H 0.5509 0.2238 0.3905 0.076 Uiso 1 1 calc R U . . . H53C H 0.4519 0.2479 0.3445 0.076 Uiso 1 1 calc R U . . . C54 C 0.6623(16) 0.3235(6) 0.3641(6) 0.045(3) Uani 1 1 d . U . . . H54A H 0.6428 0.3183 0.3274 0.068 Uiso 1 1 calc R U . . . H54B H 0.7484 0.3011 0.3744 0.068 Uiso 1 1 calc R U . . . H54C H 0.6846 0.3618 0.3707 0.068 Uiso 1 1 calc R U . . . Br3A Br 0.1952(3) 0.69665(8) 0.20509(10) 0.0792(9) Uani 0.930(5) 1 d D U P D 1 C37B C 0.205(9) 0.583(2) 0.232(5) 0.032(3) Uani 0.070(5) 1 d DG U P D 2 H37B H 0.2951 0.5856 0.2512 0.039 Uiso 0.070(5) 1 calc R U P D 2 C36 C 0.1192(14) 0.5358(5) 0.2335(5) 0.033(3) Uani 1 1 d DG U . . . C41B C -0.012(9) 0.532(3) 0.205(4) 0.032(3) Uani 0.070(5) 1 d DG U P D 2 H41B H -0.0710 0.4998 0.2061 0.039 Uiso 0.070(5) 1 calc R U P D 2 C40B C -0.057(12) 0.575(5) 0.174(6) 0.041(3) Uani 0.070(5) 1 d DG U P D 2 C39B C 0.029(13) 0.622(5) 0.172(7) 0.045(3) Uani 0.070(5) 1 d DG U P D 2 C38B C 0.160(13) 0.626(3) 0.201(7) 0.041(3) Uani 0.070(5) 1 d DG U P D 2 H38B H 0.2189 0.6584 0.1997 0.049 Uiso 0.070(5) 1 calc R U P D 2 Br3B Br -0.246(3) 0.5733(12) 0.1392(12) 0.065(9) Uani 0.070(5) 1 d D U P D 2 C42B C -0.018(19) 0.668(4) 0.135(4) 0.080(7) Uani 0.070(5) 1 d D U P D 2 F7B F 0.090(19) 0.699(7) 0.116(7) 0.090(4) Uani 0.070(5) 1 d D U P D 2 F8B F -0.09(2) 0.692(7) 0.175(6) 0.086(13) Uani 0.070(5) 1 d D U P D 2 F9B F -0.080(19) 0.652(6) 0.091(6) 0.077(3) Uani 0.070(5) 1 d D U P D 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 C1 0.007(5) 0.034(5) 0.034(5) 0.001(4) 0.000(4) -0.003(4) O1 0.016(3) 0.032(4) 0.039(5) 0.001(4) -0.006(4) -0.008(3) Br2 0.0618(9) 0.0416(7) 0.0531(9) 0.0122(8) -0.0059(10) 0.0047(7) N1 0.007(4) 0.035(5) 0.034(5) 0.000(3) -0.001(4) -0.008(3) N2 0.031(6) 0.035(5) 0.030(5) 0.005(4) -0.008(4) -0.009(4) O2 0.042(5) 0.034(4) 0.036(5) 0.009(4) -0.013(4) -0.009(4) C2 0.024(6) 0.033(6) 0.038(6) -0.006(5) 0.000(5) 0.002(4) O3 0.081(7) 0.031(5) 0.071(6) 0.003(4) -0.031(5) -0.011(4) C3 0.063(7) 0.042(6) 0.085(8) -0.009(6) 0.010(6) -0.009(6) F4 0.069(6) 0.072(6) 0.048(5) 0.032(4) -0.006(5) 0.002(5) C4 0.047(7) 0.046(7) 0.093(8) 0.000(5) 0.013(6) -0.005(6) C5 0.023(6) 0.033(6) 0.039(7) 0.001(5) 0.006(5) -0.012(4) F5 0.073(6) 0.069(6) 0.070(6) 0.018(4) -0.028(5) 0.009(5) F6 0.065(6) 0.075(6) 0.085(7) 0.017(5) -0.012(5) 0.030(5) C6 0.080(11) 0.075(11) 0.100(10) 0.018(8) -0.024(9) -0.021(9) C7 0.123(18) 0.115(16) 0.104(12) 0.024(10) -0.036(12) -0.043(14) C8 0.015(4) 0.035(5) 0.035(5) 0.005(4) -0.002(4) -0.010(4) C16 0.026(6) 0.038(5) 0.030(5) 0.003(4) -0.003(4) -0.003(4) C17 0.026(6) 0.046(6) 0.024(5) 0.004(4) -0.002(5) 0.002(5) C18 0.024(6) 0.043(5) 0.031(6) 0.004(4) -0.002(5) 0.001(5) C19 0.022(5) 0.046(5) 0.038(6) 0.010(5) 0.007(5) 0.008(4) C20 0.027(6) 0.044(5) 0.028(5) 0.012(4) 0.008(4) 0.007(4) C21 0.046(8) 0.049(6) 0.030(6) 0.006(5) -0.006(6) 0.001(5) C22 0.041(7) 0.043(6) 0.036(6) 0.003(5) -0.011(6) -0.002(5) C23 0.043(7) 0.059(7) 0.053(7) 0.025(5) -0.008(5) 0.010(5) C25 0.085(11) 0.067(10) 0.069(8) 0.010(7) -0.026(7) -0.022(8) C26 0.051(8) 0.045(6) 0.049(7) -0.001(5) -0.015(7) -0.017(6) Br1A 0.0885(17) 0.0424(11) 0.0850(15) -0.0229(11) -0.0016(13) 0.0034(12) F1A 0.067(7) 0.084(8) 0.077(9) -0.016(6) 0.014(6) -0.042(6) F2A 0.077(7) 0.090(9) 0.056(6) -0.035(5) 0.010(5) -0.037(6) F3A 0.091(8) 0.102(8) 0.079(8) -0.038(6) -0.034(6) -0.036(6) C9A 0.019(5) 0.037(5) 0.029(5) 0.002(4) 0.002(4) -0.009(4) C10A 0.017(5) 0.040(5) 0.026(6) 0.003(5) 0.002(4) -0.011(4) C11A 0.029(7) 0.055(6) 0.041(7) -0.007(5) -0.004(5) -0.018(5) C12A 0.029(6) 0.050(5) 0.039(6) -0.006(4) 0.003(5) -0.022(4) C13A 0.035(6) 0.046(5) 0.043(7) -0.009(5) 0.004(5) -0.018(5) C14A 0.025(7) 0.042(5) 0.038(7) -0.003(5) -0.003(6) -0.006(5) C15A 0.065(8) 0.081(8) 0.052(7) -0.023(6) 0.005(6) -0.037(6) C24A 0.077(10) 0.036(10) 0.072(11) 0.008(8) -0.024(8) -0.016(8) C27A 0.065(12) 0.079(18) 0.074(15) -0.002(12) -0.035(10) -0.005(11) F1B 0.067(7) 0.084(8) 0.077(9) -0.016(6) 0.014(6) -0.042(6) Br1B 0.029(7) 0.096(12) 0.054(9) 0.011(8) -0.005(6) -0.025(6) F2B 0.077(7) 0.090(9) 0.056(6) -0.035(5) 0.010(5) -0.037(6) F3B 0.070(17) 0.081(15) 0.08(2) -0.038(14) 0.008(15) -0.027(13) C9B 0.019(5) 0.037(5) 0.029(5) 0.002(4) 0.002(4) -0.009(4) C14B 0.025(7) 0.042(5) 0.038(7) -0.003(5) -0.003(6) -0.006(5) C13B 0.035(6) 0.046(5) 0.043(7) -0.009(5) 0.004(5) -0.018(5) C12B 0.029(6) 0.050(5) 0.039(6) -0.006(4) 0.003(5) -0.022(4) C11B 0.029(7) 0.055(6) 0.041(7) -0.007(5) -0.004(5) -0.018(5) C10B 0.017(5) 0.040(5) 0.026(6) 0.003(5) 0.002(4) -0.011(4) C15B 0.058(11) 0.077(11) 0.058(11) -0.032(8) 0.009(8) -0.035(8) C24B 0.059(12) 0.028(8) 0.047(9) 0.001(7) -0.005(8) -0.018(7) C27B 0.074(14) 0.043(14) 0.072(16) -0.001(11) 0.008(11) -0.021(10) N3 0.016(4) 0.037(5) 0.036(5) 0.006(4) 0.001(4) 0.004(4) N4 0.021(5) 0.041(5) 0.035(5) -0.003(4) 0.002(4) 0.003(4) O4 0.014(4) 0.045(5) 0.055(6) -0.002(4) -0.004(4) -0.008(4) Br04 0.0886(14) 0.0660(12) 0.0724(12) -0.0301(11) -0.0183(13) 0.0134(11) O5 0.025(5) 0.044(5) 0.045(5) 0.000(4) 0.004(4) 0.003(4) O6 0.024(4) 0.041(4) 0.029(4) -0.004(3) -0.003(3) 0.012(3) F7A 0.088(7) 0.107(8) 0.074(7) 0.031(6) -0.015(6) 0.029(6) F8A 0.096(9) 0.128(11) 0.107(9) 0.079(8) 0.040(7) 0.054(7) F9A 0.068(7) 0.072(6) 0.091(7) 0.025(5) 0.000(5) 0.043(5) F10 0.057(6) 0.108(7) 0.045(5) 0.001(5) -0.025(4) -0.007(5) F11 0.064(6) 0.121(8) 0.046(5) -0.030(5) 0.003(5) -0.010(6) F12 0.043(5) 0.094(7) 0.062(6) -0.007(5) -0.007(4) -0.018(5) C28 0.017(5) 0.038(5) 0.033(5) 0.006(4) -0.001(4) -0.005(4) C29 0.010(5) 0.034(5) 0.032(6) -0.003(4) -0.005(4) -0.008(4) C30 0.023(5) 0.036(5) 0.027(5) -0.003(4) -0.003(4) -0.001(4) C31 0.025(5) 0.032(5) 0.049(6) 0.004(4) -0.013(4) -0.009(4) C32 0.021(6) 0.041(6) 0.055(7) 0.006(5) 0.004(5) -0.011(4) C33 0.034(7) 0.042(7) 0.063(6) -0.007(5) -0.007(5) -0.015(6) C34 0.070(11) 0.070(11) 0.074(8) -0.006(7) -0.003(7) -0.003(9) C35 0.019(4) 0.029(5) 0.029(5) -0.004(4) -0.002(4) -0.002(4) C37A 0.026(7) 0.051(7) 0.037(7) 0.000(5) 0.004(5) 0.008(5) C38A 0.031(7) 0.063(7) 0.038(8) 0.004(6) 0.003(6) 0.019(6) C39A 0.026(6) 0.057(5) 0.052(6) 0.013(5) 0.009(4) 0.020(4) C40A 0.029(6) 0.043(5) 0.050(7) 0.014(4) 0.012(6) 0.017(4) C41A 0.020(5) 0.037(5) 0.040(6) 0.004(4) 0.009(5) 0.011(4) C42A 0.061(8) 0.084(8) 0.062(8) 0.028(6) 0.013(6) 0.038(6) C43 0.017(5) 0.044(6) 0.030(5) 0.000(4) -0.002(4) -0.006(4) C44 0.016(5) 0.046(6) 0.032(6) -0.002(4) 0.004(5) -0.001(5) C45 0.034(7) 0.051(6) 0.037(6) -0.002(5) -0.005(5) 0.004(5) C46 0.051(9) 0.073(7) 0.039(7) -0.001(5) -0.008(7) -0.005(6) C47 0.044(7) 0.068(6) 0.028(6) -0.004(5) 0.000(5) -0.009(5) C48 0.048(7) 0.050(5) 0.032(6) -0.004(5) 0.004(6) -0.001(5) C49 0.043(8) 0.050(6) 0.033(6) -0.006(5) 0.005(6) 0.005(5) C50 0.046(7) 0.092(8) 0.031(6) -0.008(5) -0.008(5) -0.012(5) C51 0.028(5) 0.034(6) 0.043(6) 0.007(5) -0.003(4) 0.004(4) C52 0.025(6) 0.061(8) 0.049(6) 0.004(5) -0.005(5) 0.017(6) C53 0.056(9) 0.035(6) 0.061(9) 0.009(5) 0.001(7) -0.004(6) C54 0.035(6) 0.036(7) 0.065(8) 0.002(6) 0.012(6) 0.003(5) Br3A 0.0577(13) 0.0414(11) 0.138(2) 0.0320(12) 0.0152(14) 0.0005(10) C37B 0.020(5) 0.037(5) 0.040(6) 0.004(4) 0.009(5) 0.011(4) C36 0.025(5) 0.037(5) 0.036(6) 0.005(4) 0.003(4) 0.005(4) C41B 0.020(5) 0.037(5) 0.040(6) 0.004(4) 0.009(5) 0.011(4) C40B 0.029(6) 0.043(5) 0.050(7) 0.014(4) 0.012(6) 0.017(4) C39B 0.026(6) 0.057(5) 0.052(6) 0.013(5) 0.009(4) 0.020(4) C38B 0.029(6) 0.043(5) 0.050(7) 0.014(4) 0.012(6) 0.017(4) Br3B 0.031(10) 0.072(16) 0.093(18) 0.046(13) -0.011(10) -0.005(9) C42B 0.080(13) 0.073(11) 0.085(10) 0.026(8) -0.003(8) 0.037(9) F7B 0.088(7) 0.107(8) 0.074(7) 0.031(6) -0.015(6) 0.029(6) F8B 0.09(3) 0.074(18) 0.091(16) 0.024(12) 0.002(15) 0.046(16) F9B 0.068(7) 0.072(6) 0.091(7) 0.025(5) 0.000(5) 0.043(5) _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 C16 1.533(18) . ? C1 C8 1.537(17) . ? C1 C2 1.568(18) . ? C1 C5 1.571(17) . ? O1 C8 1.223(14) . ? Br2 C19 1.909(13) . ? N1 C8 1.341(16) . ? N1 C9A 1.344(17) . ? N1 C9B 1.53(5) . ? N1 H1 0.8800 . ? N2 C16 1.354(17) . ? N2 C17 1.425(16) . ? N2 H2 0.8800 . ? O2 C16 1.239(17) . ? C2 C3 1.554(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C24B 1.42(3) . ? O3 C3 1.65(2) . ? O3 C24A 1.68(3) . ? C3 C4 1.38(2) . ? C3 H3 1.0000 . ? F4 C23 1.354(19) . ? C4 C5 1.542(19) . ? C4 C6 1.73(3) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? F5 C23 1.30(2) . ? F6 C23 1.318(19) . ? C6 C7 1.28(3) . ? C6 H6 0.9500 . ? C7 H7A 0.9500 . ? C7 H7B 0.9500 . ? C17 C18 1.363(18) . ? C17 C22 1.386(19) . ? C18 C19 1.408(19) . ? C18 H18 0.9500 . ? C19 C20 1.41(2) . ? C20 C21 1.372(18) . ? C20 C23 1.51(2) . ? C21 C22 1.38(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C25 C24B 1.40(3) . ? C25 C24A 1.60(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? C26 C24A 1.51(3) . ? C26 C24B 1.56(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? Br1A C13A 1.888(16) . ? F1A C15A 1.367(17) . ? F2A C15A 1.342(16) . ? F3A C15A 1.349(17) . ? C9A C14A 1.389(14) . ? C9A C10A 1.415(14) . ? C10A C11A 1.392(14) . ? C10A H10A 0.9500 . ? C11A C12A 1.382(15) . ? C11A H11A 0.9500 . ? C12A C13A 1.394(15) . ? C12A C15A 1.47(2) . ? C13A C14A 1.390(14) . ? C14A H14A 0.9500 . ? C24A C27A 1.38(5) . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? F1B C15B 1.37(2) . ? Br1B C13B 1.87(3) . ? F2B C15B 1.37(2) . ? F3B C15B 1.37(2) . ? C9B C14B 1.3900 . ? C9B C10B 1.3900 . ? C14B C13B 1.3900 . ? C14B H14B 0.9500 . ? C13B C12B 1.3900 . ? C12B C11B 1.3900 . ? C12B C15B 1.49(4) . ? C11B C10B 1.3900 . ? C11B H11B 0.9500 . ? C10B H10B 0.9500 . ? C24B C27B 1.65(5) . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? N3 C35 1.354(16) . ? N3 C36 1.463(16) . ? N3 H3A 0.8800 . ? N4 C43 1.385(17) . ? N4 C44 1.405(17) . ? N4 H4A 0.8800 . ? O4 C35 1.238(14) . ? Br04 C48 1.870(14) . ? O5 C43 1.198(17) . ? O6 C30 1.403(13) . ? O6 C51 1.452(15) . ? F7A C42A 1.315(17) . ? F8A C42A 1.323(16) . ? F9A C42A 1.328(15) . ? F10 C50 1.35(2) . ? F11 C50 1.32(2) . ? F12 C50 1.36(2) . ? C28 C43 1.528(19) . ? C28 C35 1.534(18) . ? C28 C32 1.545(18) . ? C28 C29 1.562(18) . ? C29 C30 1.522(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.598(15) . ? C30 H30 1.0000 . ? C31 C33 1.490(17) . ? C31 C32 1.507(19) . ? C31 H31 1.0000 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.22(2) . ? C33 H33 0.9500 . ? C34 H34A 0.9500 . ? C34 H34B 0.9500 . ? C37A C36 1.385(14) . ? C37A C38A 1.397(14) . ? C37A H37A 0.9500 . ? C38A C39A 1.391(15) . ? C38A H38A 0.9500 . ? C39A C40A 1.384(15) . ? C39A C42A 1.54(2) . ? C40A C41A 1.372(14) . ? C40A Br3A 1.902(16) . ? C41A C36 1.391(14) . ? C41A H41A 0.9500 . ? C44 C45 1.380(19) . ? C44 C49 1.399(19) . ? C45 C46 1.38(2) . ? C45 H45 0.9500 . ? C46 C47 1.35(2) . ? C46 H46 0.9500 . ? C47 C48 1.39(2) . ? C47 C50 1.53(2) . ? C48 C49 1.35(2) . ? C49 H49 0.9500 . ? C51 C52 1.496(19) . ? C51 C53 1.502(19) . ? C51 C54 1.558(18) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C37B C36 1.3900 . ? C37B C38B 1.3900 . ? C37B H37B 0.9500 . ? C36 C41B 1.3900 . ? C41B C40B 1.3900 . ? C41B H41B 0.9500 . ? C40B C39B 1.3900 . ? C40B Br3B 1.91(3) . ? C39B C38B 1.3900 . ? C39B C42B 1.55(4) . ? C38B H38B 0.9500 . ? C42B F7B 1.33(3) . ? C42B F8B 1.33(2) . ? C42B F9B 1.33(2) . ? 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 C16 C1 C8 105.8(10) . . ? C16 C1 C2 109.7(10) . . ? C8 C1 C2 111.3(10) . . ? C16 C1 C5 112.8(10) . . ? C8 C1 C5 111.8(10) . . ? C2 C1 C5 105.6(10) . . ? C8 N1 C9A 127.3(11) . . ? C8 N1 C9B 135(4) . . ? C8 N1 H1 116.3 . . ? C9A N1 H1 116.3 . . ? C16 N2 C17 127.4(11) . . ? C16 N2 H2 116.3 . . ? C17 N2 H2 116.3 . . ? C3 C2 C1 102.8(11) . . ? C3 C2 H2A 111.2 . . ? C1 C2 H2A 111.2 . . ? C3 C2 H2B 111.2 . . ? C1 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? C24B O3 C3 115.4(15) . . ? C3 O3 C24A 123.8(13) . . ? C4 C3 C2 111.4(13) . . ? C4 C3 O3 92.4(12) . . ? C2 C3 O3 105.3(12) . . ? C4 C3 H3 115.1 . . ? C2 C3 H3 115.1 . . ? O3 C3 H3 115.1 . . ? C3 C4 C5 106.2(13) . . ? C3 C4 C6 93.8(13) . . ? C5 C4 C6 112.1(13) . . ? C3 C4 H4 114.3 . . ? C5 C4 H4 114.3 . . ? C6 C4 H4 114.3 . . ? C4 C5 C1 105.5(11) . . ? C4 C5 H5A 110.6 . . ? C1 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? C1 C5 H5B 110.6 . . ? H5A C5 H5B 108.8 . . ? C7 C6 C4 127(2) . . ? C7 C6 H6 116.7 . . ? C4 C6 H6 116.7 . . ? C6 C7 H7A 120.0 . . ? C6 C7 H7B 120.0 . . ? H7A C7 H7B 120.0 . . ? O1 C8 N1 123.1(12) . . ? O1 C8 C1 121.5(12) . . ? N1 C8 C1 115.4(11) . . ? O2 C16 N2 123.4(12) . . ? O2 C16 C1 121.0(11) . . ? N2 C16 C1 115.6(12) . . ? C18 C17 C22 121.1(13) . . ? C18 C17 N2 123.2(12) . . ? C22 C17 N2 115.7(11) . . ? C17 C18 C19 117.4(13) . . ? C17 C18 H18 121.3 . . ? C19 C18 H18 121.3 . . ? C20 C19 C18 122.8(12) . . ? C20 C19 Br2 121.7(10) . . ? C18 C19 Br2 115.6(11) . . ? C21 C20 C19 116.9(12) . . ? C21 C20 C23 119.6(15) . . ? C19 C20 C23 123.4(13) . . ? C20 C21 C22 121.2(15) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C17 120.5(13) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? F5 C23 F6 107.8(14) . . ? F5 C23 F4 107.8(15) . . ? F6 C23 F4 104.7(13) . . ? F5 C23 C20 111.9(14) . . ? F6 C23 C20 113.4(15) . . ? F4 C23 C20 110.8(13) . . ? C24A C25 H25A 109.5 . . ? C24A C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24A C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24B C25 H25D 109.5 . . ? C24B C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? C24B C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C24A C26 H26A 109.5 . . ? C24A C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24A C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24B C26 H26D 109.5 . . ? C24B C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? C24B C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? N1 C9A C14A 120.4(12) . . ? N1 C9A C10A 122.6(12) . . ? C14A C9A C10A 117.0(14) . . ? C11A C10A C9A 118.9(14) . . ? C11A C10A H10A 120.6 . . ? C9A C10A H10A 120.6 . . ? C12A C11A C10A 123.3(15) . . ? C12A C11A H11A 118.4 . . ? C10A C11A H11A 118.4 . . ? C11A C12A C13A 118.1(14) . . ? C11A C12A C15A 121.5(14) . . ? C13A C12A C15A 120.3(14) . . ? C14A C13A C12A 118.8(14) . . ? C14A C13A Br1A 116.3(11) . . ? C12A C13A Br1A 124.8(11) . . ? C9A C14A C13A 123.7(14) . . ? C9A C14A H14A 118.1 . . ? C13A C14A H14A 118.1 . . ? F2A C15A F3A 103.6(14) . . ? F2A C15A F1A 102.6(15) . . ? F3A C15A F1A 109.5(15) . . ? F2A C15A C12A 114.8(14) . . ? F3A C15A C12A 111.6(14) . . ? F1A C15A C12A 113.9(14) . . ? C27A C24A C26 114(3) . . ? C27A C24A C25 121(3) . . ? C26 C24A C25 106(2) . . ? C27A C24A O3 123(3) . . ? C26 C24A O3 100(2) . . ? C25 C24A O3 89(2) . . ? C24A C27A H27A 109.5 . . ? C24A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C24A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C14B C9B C10B 120.0 . . ? C14B C9B N1 124(6) . . ? C10B C9B N1 116(6) . . ? C9B C14B C13B 120.0 . . ? C9B C14B H14B 120.0 . . ? C13B C14B H14B 120.0 . . ? C12B C13B C14B 120.0 . . ? C12B C13B Br1B 123(5) . . ? C14B C13B Br1B 114(5) . . ? C11B C12B C13B 120.0 . . ? C11B C12B C15B 129(6) . . ? C13B C12B C15B 111(6) . . ? C12B C11B C10B 120.0 . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C10B C9B 120.0 . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? F2B C15B F3B 110(9) . . ? F2B C15B F1B 101(9) . . ? F3B C15B F1B 120(10) . . ? F2B C15B C12B 106(8) . . ? F3B C15B C12B 105(6) . . ? F1B C15B C12B 115(9) . . ? C25 C24B O3 109(2) . . ? C25 C24B C26 113(2) . . ? O3 C24B C26 111(2) . . ? C25 C24B C27B 106(2) . . ? O3 C24B C27B 112(2) . . ? C26 C24B C27B 105(2) . . ? C24B C27B H27D 109.5 . . ? C24B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C24B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C35 N3 C36 123.7(11) . . ? C35 N3 H3A 118.1 . . ? C36 N3 H3A 118.1 . . ? C43 N4 C44 126.5(12) . . ? C43 N4 H4A 116.8 . . ? C44 N4 H4A 116.8 . . ? C30 O6 C51 118.8(9) . . ? C43 C28 C35 105.0(10) . . ? C43 C28 C32 111.9(11) . . ? C35 C28 C32 111.1(11) . . ? C43 C28 C29 114.1(10) . . ? C35 C28 C29 111.0(10) . . ? C32 C28 C29 103.9(10) . . ? C30 C29 C28 105.7(10) . . ? C30 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? C30 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? O6 C30 C29 110.9(9) . . ? O6 C30 C31 111.8(9) . . ? C29 C30 C31 101.8(9) . . ? O6 C30 H30 110.7 . . ? C29 C30 H30 110.7 . . ? C31 C30 H30 110.7 . . ? C33 C31 C32 111.2(11) . . ? C33 C31 C30 118.2(11) . . ? C32 C31 C30 99.1(9) . . ? C33 C31 H31 109.3 . . ? C32 C31 H31 109.3 . . ? C30 C31 H31 109.3 . . ? C31 C32 C28 107.3(11) . . ? C31 C32 H32A 110.3 . . ? C28 C32 H32A 110.3 . . ? C31 C32 H32B 110.3 . . ? C28 C32 H32B 110.3 . . ? H32A C32 H32B 108.5 . . ? C34 C33 C31 129.2(15) . . ? C34 C33 H33 115.4 . . ? C31 C33 H33 115.4 . . ? C33 C34 H34A 120.0 . . ? C33 C34 H34B 120.0 . . ? H34A C34 H34B 120.0 . . ? O4 C35 N3 123.7(12) . . ? O4 C35 C28 123.0(12) . . ? N3 C35 C28 113.2(11) . . ? C36 C37A C38A 117.1(14) . . ? C36 C37A H37A 121.5 . . ? C38A C37A H37A 121.5 . . ? C39A C38A C37A 121.1(14) . . ? C39A C38A H38A 119.5 . . ? C37A C38A H38A 119.5 . . ? C40A C39A C38A 118.5(14) . . ? C40A C39A C42A 123.2(13) . . ? C38A C39A C42A 118.2(13) . . ? C41A C40A C39A 122.9(14) . . ? C41A C40A Br3A 115.2(11) . . ? C39A C40A Br3A 121.9(10) . . ? C40A C41A C36 116.6(13) . . ? C40A C41A H41A 121.7 . . ? C36 C41A H41A 121.7 . . ? F7A C42A F8A 107.6(16) . . ? F7A C42A F9A 108.2(15) . . ? F8A C42A F9A 106.2(15) . . ? F7A C42A C39A 109.7(14) . . ? F8A C42A C39A 111.5(14) . . ? F9A C42A C39A 113.5(14) . . ? O5 C43 N4 124.3(12) . . ? O5 C43 C28 123.8(12) . . ? N4 C43 C28 111.9(12) . . ? C45 C44 C49 118.1(13) . . ? C45 C44 N4 117.6(12) . . ? C49 C44 N4 124.2(13) . . ? C44 C45 C46 119.9(14) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 121.2(16) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 119.8(15) . . ? C46 C47 C50 118.6(16) . . ? C48 C47 C50 121.6(15) . . ? C49 C48 C47 119.3(14) . . ? C49 C48 Br04 118.2(12) . . ? C47 C48 Br04 122.4(11) . . ? C48 C49 C44 121.8(15) . . ? C48 C49 H49 119.1 . . ? C44 C49 H49 119.1 . . ? F11 C50 F10 106.9(14) . . ? F11 C50 F12 106.7(15) . . ? F10 C50 F12 104.8(13) . . ? F11 C50 C47 113.3(14) . . ? F10 C50 C47 112.4(15) . . ? F12 C50 C47 112.3(13) . . ? O6 C51 C52 104.4(10) . . ? O6 C51 C53 113.4(11) . . ? C52 C51 C53 111.5(12) . . ? O6 C51 C54 106.4(10) . . ? C52 C51 C54 109.7(12) . . ? C53 C51 C54 111.2(12) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C36 C37B C38B 120.00(6) . . ? C36 C37B H37B 120.0 . . ? C38B C37B H37B 120.0 . . ? C37B C36 C41B 120.0 . . ? C37A C36 C41A 123.6(13) . . ? C37A C36 N3 120.9(11) . . ? C37B C36 N3 110(2) . . ? C41B C36 N3 130(2) . . ? C41A C36 N3 115.5(11) . . ? C40B C41B C36 120.0 . . ? C40B C41B H41B 120.0 . . ? C36 C41B H41B 120.0 . . ? C39B C40B C41B 120.00(5) . . ? C39B C40B Br3B 119(4) . . ? C41B C40B Br3B 121(4) . . ? C40B C39B C38B 120.0 . . ? C40B C39B C42B 119(8) . . ? C38B C39B C42B 121(8) . . ? C39B C38B C37B 120.0 . . ? C39B C38B H38B 120.0 . . ? C37B C38B H38B 120.0 . . ? F7B C42B F8B 112(10) . . ? F7B C42B F9B 99(10) . . ? F8B C42B F9B 128(10) . . ? F7B C42B C39B 117(10) . . ? F8B C42B C39B 87(10) . . ? F9B C42B C39B 115(10) . . ? 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 C16 C1 C2 C3 116.9(12) . . . . ? C8 C1 C2 C3 -126.3(12) . . . . ? C5 C1 C2 C3 -4.8(14) . . . . ? C1 C2 C3 C4 22.7(17) . . . . ? C1 C2 C3 O3 -76.2(12) . . . . ? C24B O3 C3 C4 110.6(18) . . . . ? C24A O3 C3 C4 58(2) . . . . ? C24B O3 C3 C2 -136.4(17) . . . . ? C24A O3 C3 C2 171.2(18) . . . . ? C2 C3 C4 C5 -30.8(18) . . . . ? O3 C3 C4 C5 76.6(12) . . . . ? C2 C3 C4 C6 83.5(14) . . . . ? O3 C3 C4 C6 -169.1(10) . . . . ? C3 C4 C5 C1 26.1(17) . . . . ? C6 C4 C5 C1 -75.0(15) . . . . ? C16 C1 C5 C4 -131.5(13) . . . . ? C8 C1 C5 C4 109.4(13) . . . . ? C2 C1 C5 C4 -11.7(14) . . . . ? C3 C4 C6 C7 -126(2) . . . . ? C5 C4 C6 C7 -17(3) . . . . ? C9A N1 C8 O1 -5(2) . . . . ? C9B N1 C8 O1 -11(6) . . . . ? C9A N1 C8 C1 173.9(13) . . . . ? C9B N1 C8 C1 169(6) . . . . ? C16 C1 C8 O1 105.0(14) . . . . ? C2 C1 C8 O1 -14.1(17) . . . . ? C5 C1 C8 O1 -131.8(13) . . . . ? C16 C1 C8 N1 -74.1(13) . . . . ? C2 C1 C8 N1 166.8(11) . . . . ? C5 C1 C8 N1 49.0(14) . . . . ? C17 N2 C16 O2 9(2) . . . . ? C17 N2 C16 C1 -172.3(12) . . . . ? C8 C1 C16 O2 -2.9(17) . . . . ? C2 C1 C16 O2 117.2(14) . . . . ? C5 C1 C16 O2 -125.4(13) . . . . ? C8 C1 C16 N2 178.8(11) . . . . ? C2 C1 C16 N2 -61.1(14) . . . . ? C5 C1 C16 N2 56.3(15) . . . . ? C16 N2 C17 C18 5(2) . . . . ? C16 N2 C17 C22 -176.7(14) . . . . ? C22 C17 C18 C19 -1(2) . . . . ? N2 C17 C18 C19 177.1(12) . . . . ? C17 C18 C19 C20 2(2) . . . . ? C17 C18 C19 Br2 -178.7(11) . . . . ? C18 C19 C20 C21 -3(2) . . . . ? Br2 C19 C20 C21 177.6(11) . . . . ? C18 C19 C20 C23 -179.5(13) . . . . ? Br2 C19 C20 C23 1.3(19) . . . . ? C19 C20 C21 C22 4(2) . . . . ? C23 C20 C21 C22 180.0(14) . . . . ? C20 C21 C22 C17 -3(2) . . . . ? C18 C17 C22 C21 2(2) . . . . ? N2 C17 C22 C21 -176.8(13) . . . . ? C21 C20 C23 F5 -1(2) . . . . ? C19 C20 C23 F5 175.6(14) . . . . ? C21 C20 C23 F6 -122.8(16) . . . . ? C19 C20 C23 F6 53(2) . . . . ? C21 C20 C23 F4 119.9(16) . . . . ? C19 C20 C23 F4 -64(2) . . . . ? C8 N1 C9A C14A -137.5(15) . . . . ? C8 N1 C9A C10A 41(2) . . . . ? N1 C9A C10A C11A -179.4(16) . . . . ? C14A C9A C10A C11A 0(2) . . . . ? C9A C10A C11A C12A 3(2) . . . . ? C10A C11A C12A C13A -5(2) . . . . ? C10A C11A C12A C15A 177.9(15) . . . . ? C11A C12A C13A C14A 4(2) . . . . ? C15A C12A C13A C14A -178.4(15) . . . . ? C11A C12A C13A Br1A -178.8(13) . . . . ? C15A C12A C13A Br1A -2(2) . . . . ? N1 C9A C14A C13A 179.1(17) . . . . ? C10A C9A C14A C13A 0(2) . . . . ? C12A C13A C14A C9A -2(2) . . . . ? Br1A C13A C14A C9A -179.2(13) . . . . ? C11A C12A C15A F2A 116.3(18) . . . . ? C13A C12A C15A F2A -61(2) . . . . ? C11A C12A C15A F3A -1(2) . . . . ? C13A C12A C15A F3A -178.2(15) . . . . ? C11A C12A C15A F1A -125.7(18) . . . . ? C13A C12A C15A F1A 57(2) . . . . ? C3 O3 C24A C27A -88(3) . . . . ? C3 O3 C24A C26 39(3) . . . . ? C3 O3 C24A C25 144.8(14) . . . . ? C8 N1 C9B C14B 36(10) . . . . ? C8 N1 C9B C10B -143(4) . . . . ? C10B C9B C14B C13B 0.0 . . . . ? N1 C9B C14B C13B -179(10) . . . . ? C9B C14B C13B C12B 0.0 . . . . ? C9B C14B C13B Br1B 162(7) . . . . ? C14B C13B C12B C11B 0.0 . . . . ? Br1B C13B C12B C11B -161(7) . . . . ? C14B C13B C12B C15B 178(9) . . . . ? Br1B C13B C12B C15B 17(8) . . . . ? C13B C12B C11B C10B 0.0 . . . . ? C15B C12B C11B C10B -177(10) . . . . ? C12B C11B C10B C9B 0.0 . . . . ? C14B C9B C10B C11B 0.0 . . . . ? N1 C9B C10B C11B 179(9) . . . . ? C11B C12B C15B F2B -125(9) . . . . ? C13B C12B C15B F2B 57(10) . . . . ? C11B C12B C15B F3B -8(12) . . . . ? C13B C12B C15B F3B 174(7) . . . . ? C11B C12B C15B F1B 125(9) . . . . ? C13B C12B C15B F1B -53(11) . . . . ? C3 O3 C24B C25 177.7(17) . . . . ? C3 O3 C24B C26 -57(3) . . . . ? C3 O3 C24B C27B 60(3) . . . . ? C43 C28 C29 C30 110.6(11) . . . . ? C35 C28 C29 C30 -131.0(10) . . . . ? C32 C28 C29 C30 -11.5(13) . . . . ? C51 O6 C30 C29 -132.4(11) . . . . ? C51 O6 C30 C31 114.8(11) . . . . ? C28 C29 C30 O6 -83.3(11) . . . . ? C28 C29 C30 C31 35.8(11) . . . . ? O6 C30 C31 C33 -167.9(10) . . . . ? C29 C30 C31 C33 73.6(12) . . . . ? O6 C30 C31 C32 72.0(12) . . . . ? C29 C30 C31 C32 -46.4(11) . . . . ? C33 C31 C32 C28 -84.8(13) . . . . ? C30 C31 C32 C28 40.3(12) . . . . ? C43 C28 C32 C31 -142.8(11) . . . . ? C35 C28 C32 C31 100.2(12) . . . . ? C29 C28 C32 C31 -19.2(14) . . . . ? C32 C31 C33 C34 122.3(17) . . . . ? C30 C31 C33 C34 9(2) . . . . ? C36 N3 C35 O4 10.7(19) . . . . ? C36 N3 C35 C28 -171.6(11) . . . . ? C43 C28 C35 O4 -108.1(13) . . . . ? C32 C28 C35 O4 13.0(18) . . . . ? C29 C28 C35 O4 128.1(13) . . . . ? C43 C28 C35 N3 74.2(13) . . . . ? C32 C28 C35 N3 -164.7(11) . . . . ? C29 C28 C35 N3 -49.6(14) . . . . ? C36 C37A C38A C39A 5(2) . . . . ? C37A C38A C39A C40A -4(2) . . . . ? C37A C38A C39A C42A 178.1(15) . . . . ? C38A C39A C40A C41A 2(2) . . . . ? C42A C39A C40A C41A 178.8(16) . . . . ? C38A C39A C40A Br3A -177.3(14) . . . . ? C42A C39A C40A Br3A 0(2) . . . . ? C39A C40A C41A C36 0(2) . . . . ? Br3A C40A C41A C36 179.2(12) . . . . ? C40A C39A C42A F7A -179.1(15) . . . . ? C38A C39A C42A F7A -2(2) . . . . ? C40A C39A C42A F8A 62(2) . . . . ? C38A C39A C42A F8A -120.9(18) . . . . ? C40A C39A C42A F9A -58(2) . . . . ? C38A C39A C42A F9A 119.3(18) . . . . ? C44 N4 C43 O5 -7(2) . . . . ? C44 N4 C43 C28 175.3(11) . . . . ? C35 C28 C43 O5 10.9(17) . . . . ? C32 C28 C43 O5 -109.8(15) . . . . ? C29 C28 C43 O5 132.6(13) . . . . ? C35 C28 C43 N4 -171.5(10) . . . . ? C32 C28 C43 N4 67.9(14) . . . . ? C29 C28 C43 N4 -49.8(14) . . . . ? C43 N4 C44 C45 174.2(13) . . . . ? C43 N4 C44 C49 -11(2) . . . . ? C49 C44 C45 C46 0(2) . . . . ? N4 C44 C45 C46 175.7(13) . . . . ? C44 C45 C46 C47 -1(2) . . . . ? C45 C46 C47 C48 2(3) . . . . ? C45 C46 C47 C50 -179.3(15) . . . . ? C46 C47 C48 C49 -2(2) . . . . ? C50 C47 C48 C49 179.4(14) . . . . ? C46 C47 C48 Br04 -179.2(13) . . . . ? C50 C47 C48 Br04 2(2) . . . . ? C47 C48 C49 C44 1(2) . . . . ? Br04 C48 C49 C44 178.6(11) . . . . ? C45 C44 C49 C48 0(2) . . . . ? N4 C44 C49 C48 -175.4(13) . . . . ? C46 C47 C50 F11 -116.5(19) . . . . ? C48 C47 C50 F11 62(2) . . . . ? C46 C47 C50 F10 5(2) . . . . ? C48 C47 C50 F10 -176.4(14) . . . . ? C46 C47 C50 F12 122.6(18) . . . . ? C48 C47 C50 F12 -59(2) . . . . ? C30 O6 C51 C52 -174.1(11) . . . . ? C30 O6 C51 C53 -52.6(15) . . . . ? C30 O6 C51 C54 70.0(13) . . . . ? C38A C37A C36 C41A -4(2) . . . . ? C38A C37A C36 N3 175.7(13) . . . . ? C38B C37B C36 C41B 0.0 . . . . ? C38B C37B C36 N3 -176(5) . . . . ? C40A C41A C36 C37A 1(2) . . . . ? C40A C41A C36 N3 -178.5(12) . . . . ? C35 N3 C36 C37A -45.9(19) . . . . ? C35 N3 C36 C37B 145(7) . . . . ? C35 N3 C36 C41B -31(8) . . . . ? C35 N3 C36 C41A 133.5(13) . . . . ? C37B C36 C41B C40B 0.0 . . . . ? N3 C36 C41B C40B 176(6) . . . . ? C36 C41B C40B C39B 0.0 . . . . ? C36 C41B C40B Br3B -174(14) . . . . ? C41B C40B C39B C38B 0.0 . . . . ? Br3B C40B C39B C38B 175(14) . . . . ? C41B C40B C39B C42B 176(16) . . . . ? Br3B C40B C39B C42B -9(14) . . . . ? C40B C39B C38B C37B 0.0 . . . . ? C42B C39B C38B C37B -176(16) . . . . ? C36 C37B C38B C39B 0.0 . . . . ? C40B C39B C42B F7B -150(14) . . . . ? C38B C39B C42B F7B 26(21) . . . . ? C40B C39B C42B F8B 97(15) . . . . ? C38B C39B C42B F8B -87(16) . . . . ? C40B C39B C42B F9B -34(20) . . . . ? C38B C39B C42B F9B 142(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O4 0.88 2.04 2.834(14) 149.2 1_655 N2 H2 O3 0.88 2.03 2.880(14) 160.8 . N3 H3A O1 0.88 2.03 2.792(14) 144.7 . N4 H4A O6 0.88 2.12 2.967(14) 161.9 . _refine_diff_density_max 0.786 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.091 _shelx_res_file ; 007b-17085.res created by SHELXL-2014/7 TITL 007b-17085 CELL 1.54184 8.8852 24.6027 26.0792 90 90 90 ZERR 8 0.0002 0.0007 0.0007 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Br F N O UNIT 216 208 16 48 16 24 SADI C10B C11B C14A C13A C11B C12B C11A C12A C13A C12A C13B C12B C14B C13B = C10A C11A C9B C14B C9A C10A C9B C10B C9A C14A SADI Br1A C13A Br1B C13B SADI C12B C15B C12A C15A SADI F3B C15B F2B C15B F1B C15B F1A C15A F2A C15A F3A C15A SADI C38A C37A C41B C40B C40B C39B C39A C38A C40A C39A C39B C38B C41A C40A = C38B C37B C41A C36 C37A C36 SADI Br3A C40A Br3B C40B SADI C42B C39B C42A C39A SADI F8A C42A F9B C42B F7A C42A F9A C42A F7B C42B F8B C42B RIGU EADP C12A C12B EADP C13A C13B EADP C14A C14B EADP C9A C9B EADP F1A F1B EADP F2A F2B EADP C11A C11B EADP C10A C10B EADP C39A C39B EADP C40A C40B EADP C41A C41B EADP F9A F9B EADP F7A F7B EADP C41B C37B EADP C40B C38B EQIV $1 x+1, y, z HTAB N1 O4_$1 HTAB N2 O3 HTAB N3 O1 HTAB N4 O6 L.S. 10 SIZE 0.3 0.01 0.01 TEMP -180 BOND $H MORE -1 CONF ACTA WGHT 0.043300 20.102003 FVAR 0.19964 0.55570 0.88923 0.07016 C1 1 0.700927 0.560226 0.340922 11.00000 0.00702 0.03399 = 0.03434 0.00111 0.00034 -0.00307 O1 6 0.465948 0.538110 0.299496 11.00000 0.01646 0.03175 = 0.03936 0.00083 -0.00642 -0.00757 BR2 3 0.950748 0.343784 0.500785 11.00000 0.06179 0.04162 = 0.05314 0.01216 -0.00590 0.00469 N1 5 0.674626 0.496093 0.270384 11.00000 0.00720 0.03503 = 0.03361 0.00050 -0.00057 -0.00787 AFIX 43 H1 2 0.773391 0.495654 0.272865 11.00000 -1.20000 AFIX 0 N2 5 0.830278 0.535207 0.420227 11.00000 0.03125 0.03548 = 0.03027 0.00453 -0.00830 -0.00855 AFIX 43 H2 2 0.849548 0.570283 0.420980 11.00000 -1.20000 AFIX 0 O2 6 0.687932 0.471083 0.379554 11.00000 0.04227 0.03418 = 0.03605 0.00853 -0.01256 -0.00933 C2 1 0.614374 0.608803 0.366303 11.00000 0.02429 0.03340 = 0.03817 -0.00582 -0.00032 0.00193 AFIX 23 H2A 2 0.515983 0.614927 0.349451 11.00000 -1.20000 H2B 2 0.597976 0.602338 0.403352 11.00000 -1.20000 AFIX 0 O3 6 0.858892 0.649745 0.399674 11.00000 0.08105 0.03087 = 0.07124 0.00298 -0.03090 -0.01071 C3 1 0.722503 0.657530 0.357338 11.00000 0.06325 0.04242 = 0.08483 -0.00864 0.01049 -0.00946 AFIX 13 H3 2 0.673359 0.694096 0.357407 11.00000 -1.20000 AFIX 0 F4 4 1.036337 0.393313 0.612489 11.00000 0.06929 0.07170 = 0.04796 0.03206 -0.00603 0.00175 C4 1 0.818064 0.647979 0.316694 11.00000 0.04722 0.04582 = 0.09260 0.00001 0.01335 -0.00486 AFIX 13 H4 2 0.912523 0.670067 0.317360 11.00000 -1.20000 AFIX 0 C5 1 0.844206 0.586033 0.315364 11.00000 0.02315 0.03350 = 0.03900 0.00064 0.00603 -0.01166 AFIX 23 H5A 2 0.936014 0.576270 0.334802 11.00000 -1.20000 H5B 2 0.855463 0.573168 0.279600 11.00000 -1.20000 AFIX 0 F5 4 1.206774 0.454875 0.609606 11.00000 0.07324 0.06939 = 0.06977 0.01838 -0.02759 0.00890 F6 4 1.227002 0.383676 0.564792 11.00000 0.06508 0.07470 = 0.08483 0.01737 -0.01204 0.03025 C6 1 0.688441 0.668682 0.271310 11.00000 0.08002 0.07534 = 0.10023 0.01750 -0.02377 -0.02060 AFIX 43 H6 2 0.645970 0.703806 0.275744 11.00000 -1.20000 AFIX 0 C7 1 0.643724 0.641386 0.232195 11.00000 0.12270 0.11510 = 0.10438 0.02396 -0.03561 -0.04306 AFIX 93 H7A 2 0.682770 0.606037 0.226036 11.00000 -1.20000 H7B 2 0.571599 0.656544 0.209421 11.00000 -1.20000 AFIX 0 C8 1 0.601907 0.530664 0.301468 11.00000 0.01479 0.03498 = 0.03477 0.00484 -0.00184 -0.00952 C16 1 0.740010 0.517736 0.381783 11.00000 0.02612 0.03793 = 0.02990 0.00259 -0.00255 -0.00346 C17 1 0.897636 0.503255 0.459613 11.00000 0.02566 0.04611 = 0.02374 0.00365 -0.00239 0.00168 C18 1 0.887683 0.447999 0.461410 11.00000 0.02443 0.04310 = 0.03115 0.00361 -0.00223 0.00131 AFIX 43 H18 2 0.830498 0.428344 0.436842 11.00000 -1.20000 AFIX 0 C19 1 0.965386 0.421176 0.501063 11.00000 0.02164 0.04650 = 0.03833 0.00981 0.00701 0.00781 C20 1 1.047120 0.449051 0.538960 11.00000 0.02736 0.04416 = 0.02781 0.01155 0.00767 0.00675 C21 1 1.055207 0.504558 0.534481 11.00000 0.04581 0.04925 = 0.03047 0.00600 -0.00618 0.00110 AFIX 43 H21 2 1.114235 0.524630 0.558229 11.00000 -1.20000 AFIX 0 C22 1 0.979051 0.531808 0.496055 11.00000 0.04125 0.04257 = 0.03602 0.00321 -0.01084 -0.00158 AFIX 43 H22 2 0.982568 0.570371 0.494626 11.00000 -1.20000 AFIX 0 C23 1 1.131981 0.420800 0.581474 11.00000 0.04265 0.05925 = 0.05311 0.02476 -0.00772 0.00978 C25 1 1.015375 0.684466 0.461469 11.00000 0.08520 0.06741 = 0.06900 0.01027 -0.02608 -0.02238 PART 1 AFIX 33 H25A 2 0.916438 0.695777 0.474197 21.00000 -1.50000 H25B 2 1.035889 0.647125 0.472530 21.00000 -1.50000 H25C 2 1.092899 0.708762 0.475222 21.00000 -1.50000 AFIX 33 PART 0 PART 2 H25D 2 1.047146 0.717394 0.479634 -21.00000 -1.50000 H25E 2 0.975112 0.658177 0.486144 -21.00000 -1.50000 H25F 2 1.101943 0.668535 0.443684 -21.00000 -1.50000 AFIX 0 PART 0 C26 1 0.953304 0.742402 0.386862 11.00000 0.05131 0.04501 = 0.04915 -0.00054 -0.01484 -0.01737 PART 1 AFIX 33 H26A 2 0.863825 0.749464 0.407799 21.00000 -1.50000 H26B 2 1.029141 0.770432 0.393587 21.00000 -1.50000 H26C 2 0.925705 0.743079 0.350485 21.00000 -1.50000 AFIX 33 PART 0 PART 2 H26D 2 0.870723 0.749831 0.362959 -21.00000 -1.50000 H26E 2 0.978888 0.775725 0.405512 -21.00000 -1.50000 H26F 2 1.041475 0.729754 0.367697 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 BR1A 3 0.697793 0.301792 0.197588 31.00000 0.08846 0.04240 = 0.08499 -0.02294 -0.00158 0.00343 F1A 4 0.370874 0.300194 0.153935 31.00000 0.06722 0.08417 = 0.07666 -0.01583 0.01359 -0.04186 F2A 4 0.512770 0.328453 0.094534 31.00000 0.07748 0.08981 = 0.05640 -0.03517 0.00984 -0.03700 F3A 4 0.304951 0.369128 0.104015 31.00000 0.09100 0.10214 = 0.07946 -0.03800 -0.03427 -0.03599 C9A 1 0.613598 0.462031 0.235858 31.00000 0.01889 0.03744 = 0.02882 0.00155 0.00181 -0.00895 C10A 1 0.492285 0.477210 0.203726 31.00000 0.01705 0.03994 = 0.02612 0.00313 0.00247 -0.01113 AFIX 43 H10A 2 0.450726 0.512733 0.205575 31.00000 -1.20000 AFIX 0 C11A 1 0.434947 0.439196 0.169378 31.00000 0.02864 0.05518 = 0.04107 -0.00686 -0.00401 -0.01751 AFIX 43 H11A 2 0.356762 0.450198 0.146803 31.00000 -1.20000 AFIX 0 C12A 1 0.486086 0.386240 0.166477 31.00000 0.02889 0.04981 = 0.03926 -0.00648 0.00338 -0.02177 C13A 1 0.608665 0.371461 0.196789 31.00000 0.03466 0.04624 = 0.04264 -0.00943 0.00449 -0.01819 C14A 1 0.667115 0.409221 0.231057 31.00000 0.02532 0.04153 = 0.03764 -0.00343 -0.00276 -0.00562 AFIX 43 H14A 2 0.748282 0.398298 0.252412 31.00000 -1.20000 AFIX 0 C15A 1 0.419096 0.346976 0.130938 31.00000 0.06484 0.08149 = 0.05219 -0.02265 0.00494 -0.03703 C24A 1 1.016842 0.687291 0.400289 21.00000 0.07679 0.03643 = 0.07245 0.00798 -0.02420 -0.01585 C27A 1 1.143744 0.673329 0.372825 21.00000 0.06483 0.07898 = 0.07367 -0.00215 -0.03512 -0.00469 AFIX 137 H27A 2 1.163373 0.634366 0.376860 21.00000 -1.50000 H27B 2 1.230086 0.694066 0.385631 21.00000 -1.50000 H27C 2 1.127939 0.681634 0.336470 21.00000 -1.50000 AFIX 0 PART 0 PART 2 F1B 4 0.348125 0.312025 0.138577 -31.00000 0.06722 0.08417 = 0.07666 -0.01583 0.01359 -0.04186 BR1B 3 0.268729 0.413139 0.143454 -31.00000 0.02928 0.09578 = 0.05417 0.01092 -0.00508 -0.02525 F2B 4 0.486109 0.350698 0.083903 -31.00000 0.07748 0.08981 = 0.05640 -0.03517 0.00984 -0.03700 F3B 4 0.602271 0.285047 0.128682 -31.00000 0.06971 0.08143 = 0.07868 -0.03821 0.00765 -0.02749 AFIX 66 C9B 1 0.628006 0.452009 0.232123 -31.00000 0.01889 0.03744 = 0.02882 0.00155 0.00181 -0.00895 C14B 1 0.501968 0.455234 0.200697 -31.00000 0.02532 0.04153 = 0.03764 -0.00343 -0.00276 -0.00562 AFIX 43 H14B 2 0.439739 0.486617 0.201642 -31.00000 -1.20000 AFIX 65 C13B 1 0.466981 0.412539 0.167888 -31.00000 0.03466 0.04624 = 0.04264 -0.00943 0.00449 -0.01819 C12B 1 0.558031 0.366620 0.166505 -31.00000 0.02889 0.04981 = 0.03926 -0.00648 0.00338 -0.02177 C11B 1 0.684069 0.363395 0.197931 -31.00000 0.02864 0.05518 = 0.04107 -0.00686 -0.00401 -0.01751 AFIX 43 H11B 2 0.746298 0.332011 0.196985 -31.00000 -1.20000 AFIX 65 C10B 1 0.719059 0.406089 0.230739 -31.00000 0.01705 0.03994 = 0.02612 0.00313 0.00247 -0.01113 AFIX 43 H10B 2 0.805200 0.403885 0.252217 -31.00000 -1.20000 AFIX 0 C15B 1 0.495980 0.325256 0.130321 -31.00000 0.05778 0.07657 = 0.05824 -0.03214 0.00947 -0.03526 C24B 1 0.903774 0.697749 0.425658 -21.00000 0.05910 0.02782 = 0.04734 0.00103 -0.00535 -0.01757 C27B 1 0.764677 0.725399 0.458596 -21.00000 0.07417 0.04262 = 0.07223 -0.00126 0.00839 -0.02099 AFIX 137 H27D 2 0.682773 0.735219 0.435196 -21.00000 -1.50000 H27E 2 0.801110 0.758087 0.476119 -21.00000 -1.50000 H27F 2 0.727618 0.699295 0.484017 -21.00000 -1.50000 AFIX 0 PART 0 N3 5 0.184527 0.497950 0.270617 11.00000 0.01603 0.03720 = 0.03569 0.00552 0.00146 0.00424 AFIX 43 H3A 2 0.283112 0.497073 0.273744 11.00000 -1.20000 AFIX 0 N4 5 0.331821 0.459708 0.417854 11.00000 0.02121 0.04097 = 0.03468 -0.00327 0.00156 0.00250 AFIX 43 H4A 2 0.359964 0.425505 0.415502 11.00000 -1.20000 AFIX 0 O4 6 -0.034605 0.456165 0.294336 11.00000 0.01383 0.04515 = 0.05511 -0.00196 -0.00376 -0.00762 BR04 3 0.432380 0.650194 0.501548 11.00000 0.08863 0.06597 = 0.07238 -0.03008 -0.01827 0.01343 O5 6 0.170862 0.521844 0.382723 11.00000 0.02493 0.04406 = 0.04512 0.00048 0.00411 0.00289 O6 6 0.406820 0.347267 0.385658 11.00000 0.02388 0.04069 = 0.02858 -0.00388 -0.00281 0.01204 PART 1 F7A 4 -0.177749 0.628921 0.103786 -41.00000 0.08833 0.10728 = 0.07362 0.03078 -0.01533 0.02891 F8A 4 0.028649 0.672310 0.097708 -41.00000 0.09550 0.12825 = 0.10729 0.07877 0.03997 0.05405 F9A 4 -0.130838 0.695615 0.153997 -41.00000 0.06791 0.07207 = 0.09089 0.02477 -0.00040 0.04326 PART 0 F10 4 0.718122 0.542141 0.604491 11.00000 0.05726 0.10823 = 0.04484 0.00136 -0.02490 -0.00675 F11 4 0.540040 0.600527 0.610145 11.00000 0.06383 0.12113 = 0.04629 -0.02991 0.00329 -0.01024 F12 4 0.725102 0.614654 0.558709 11.00000 0.04342 0.09386 = 0.06239 -0.00652 -0.00732 -0.01818 C28 1 0.195496 0.434776 0.341292 11.00000 0.01715 0.03806 = 0.03260 0.00609 -0.00063 -0.00520 C29 1 0.338499 0.408168 0.317126 11.00000 0.01016 0.03373 = 0.03207 -0.00254 -0.00467 -0.00774 AFIX 23 H29A 2 0.332369 0.408759 0.279226 11.00000 -1.20000 H29B 2 0.430428 0.427836 0.327889 11.00000 -1.20000 AFIX 0 C30 1 0.341059 0.349964 0.336834 11.00000 0.02328 0.03587 = 0.02723 -0.00287 -0.00330 -0.00056 AFIX 13 H30 2 0.395293 0.325681 0.312255 11.00000 -1.20000 AFIX 0 C31 1 0.165805 0.335487 0.338410 11.00000 0.02482 0.03243 = 0.04903 0.00428 -0.01344 -0.00888 AFIX 13 H31 2 0.149646 0.303650 0.361603 11.00000 -1.20000 AFIX 0 C32 1 0.108103 0.386191 0.364160 11.00000 0.02109 0.04104 = 0.05539 0.00566 0.00362 -0.01065 AFIX 23 H32A 2 0.124765 0.384099 0.401643 11.00000 -1.20000 H32B 2 -0.001108 0.390438 0.357793 11.00000 -1.20000 AFIX 0 C33 1 0.086896 0.325661 0.288841 11.00000 0.03397 0.04186 = 0.06316 -0.00663 -0.00697 -0.01493 AFIX 43 H33 2 -0.019435 0.322377 0.291071 11.00000 -1.20000 AFIX 0 C34 1 0.139495 0.321219 0.245682 11.00000 0.06959 0.06978 = 0.07404 -0.00627 -0.00336 -0.00253 AFIX 93 H34A 2 0.245057 0.324059 0.240555 11.00000 -1.20000 H34B 2 0.074770 0.314929 0.217301 11.00000 -1.20000 AFIX 0 C35 1 0.101850 0.464152 0.300394 11.00000 0.01949 0.02949 = 0.02868 -0.00396 -0.00161 -0.00157 PART 1 C37A 1 0.006702 0.519340 0.200230 -41.00000 0.02571 0.05061 = 0.03748 0.00000 0.00401 0.00818 AFIX 43 H37A 2 -0.026085 0.482611 0.198970 -41.00000 -1.20000 AFIX 0 C38A 1 -0.056460 0.559069 0.168563 -41.00000 0.03102 0.06276 = 0.03782 0.00351 0.00251 0.01926 AFIX 43 H38A 2 -0.139740 0.549989 0.147385 -41.00000 -1.20000 AFIX 0 C39A 1 0.000652 0.611706 0.167551 -41.00000 0.02605 0.05655 = 0.05212 0.01326 0.00921 0.02004 C40A 1 0.114996 0.625101 0.201276 -41.00000 0.02922 0.04284 = 0.05012 0.01372 0.01187 0.01745 C41A 1 0.176798 0.588416 0.234857 -41.00000 0.01968 0.03701 = 0.03986 0.00431 0.00898 0.01062 AFIX 43 H41A 2 0.254976 0.598412 0.257848 -41.00000 -1.20000 AFIX 0 C42A 1 -0.071212 0.652833 0.130533 -41.00000 0.06100 0.08402 = 0.06219 0.02771 0.01311 0.03787 PART 0 C43 1 0.229657 0.478037 0.381670 11.00000 0.01713 0.04419 = 0.02997 0.00044 -0.00169 -0.00639 C44 1 0.395025 0.490276 0.457945 11.00000 0.01599 0.04627 = 0.03213 -0.00216 0.00355 -0.00078 C45 1 0.484491 0.463196 0.492869 11.00000 0.03426 0.05062 = 0.03733 -0.00248 -0.00460 0.00352 AFIX 43 H45 2 0.495942 0.424875 0.490673 11.00000 -1.20000 AFIX 0 C46 1 0.557364 0.491925 0.531028 11.00000 0.05098 0.07288 = 0.03912 -0.00091 -0.00797 -0.00500 AFIX 43 H46 2 0.617351 0.472939 0.555286 11.00000 -1.20000 AFIX 0 C47 1 0.544825 0.546596 0.534465 11.00000 0.04366 0.06771 = 0.02803 -0.00414 -0.00005 -0.00868 C48 1 0.453690 0.574601 0.499911 11.00000 0.04801 0.04955 = 0.03237 -0.00432 0.00440 -0.00085 C49 1 0.382127 0.546748 0.462505 11.00000 0.04306 0.04985 = 0.03304 -0.00599 0.00477 0.00462 AFIX 43 H49 2 0.321424 0.566024 0.438661 11.00000 -1.20000 AFIX 0 C50 1 0.629615 0.575983 0.577191 11.00000 0.04562 0.09239 = 0.03088 -0.00809 -0.00831 -0.01200 C51 1 0.520775 0.306223 0.395330 11.00000 0.02831 0.03380 = 0.04311 0.00732 -0.00321 0.00405 C52 1 0.552967 0.311053 0.451466 11.00000 0.02535 0.06100 = 0.04881 0.00363 -0.00471 0.01727 AFIX 137 H52A 2 0.576631 0.348944 0.459793 11.00000 -1.50000 H52B 2 0.638891 0.287909 0.460322 11.00000 -1.50000 H52C 2 0.464463 0.299468 0.471048 11.00000 -1.50000 AFIX 0 C53 1 0.471418 0.249749 0.381399 11.00000 0.05588 0.03454 = 0.06123 0.00937 0.00109 -0.00355 AFIX 137 H53A 2 0.379263 0.240694 0.400196 11.00000 -1.50000 H53B 2 0.550854 0.223835 0.390453 11.00000 -1.50000 H53C 2 0.451925 0.247862 0.344456 11.00000 -1.50000 AFIX 0 C54 1 0.662287 0.323474 0.364057 11.00000 0.03454 0.03624 = 0.06501 0.00220 0.01176 0.00328 AFIX 137 H54A 2 0.642850 0.318309 0.327389 11.00000 -1.50000 H54B 2 0.748402 0.301128 0.374396 11.00000 -1.50000 H54C 2 0.684642 0.361837 0.370709 11.00000 -1.50000 AFIX 0 PART 1 BR3A 3 0.195246 0.696648 0.205085 -41.00000 0.05768 0.04142 = 0.13837 0.03200 0.01524 0.00053 PART 0 PART 2 AFIX 66 C37B 1 0.205314 0.582964 0.231622 41.00000 0.01968 0.03701 = 0.03986 0.00431 0.00898 0.01062 AFIX 43 H37B 2 0.295096 0.585610 0.251245 41.00000 -1.20000 AFIX 65 PART 0 C36 1 0.119200 0.535840 0.233539 11.00000 0.02459 0.03680 = 0.03643 0.00519 0.00290 0.00533 PART 2 C41B 1 -0.012165 0.531970 0.204827 41.00000 0.01968 0.03701 = 0.03986 0.00431 0.00898 0.01062 AFIX 43 H41B 2 -0.071020 0.499763 0.206138 41.00000 -1.20000 AFIX 65 C40B 1 -0.057417 0.575223 0.174199 41.00000 0.02922 0.04284 = 0.05012 0.01372 0.01187 0.01745 C39B 1 0.028696 0.622347 0.172282 41.00000 0.02605 0.05655 = 0.05212 0.01326 0.00921 0.02004 C38B 1 0.160061 0.626218 0.200993 41.00000 0.02922 0.04284 = 0.05012 0.01372 0.01187 0.01745 AFIX 43 H38B 2 0.218915 0.658426 0.199683 41.00000 -1.20000 AFIX 0 BR3B 3 -0.245727 0.573330 0.139243 41.00000 0.03115 0.07160 = 0.09317 0.04578 -0.01108 -0.00522 C42B 1 -0.018422 0.668393 0.135174 41.00000 0.08044 0.07327 = 0.08497 0.02621 -0.00296 0.03730 F7B 4 0.090445 0.699406 0.115940 41.00000 0.08833 0.10728 = 0.07362 0.03078 -0.01533 0.02891 F8B 4 -0.087355 0.691732 0.174790 41.00000 0.09305 0.07373 = 0.09064 0.02380 0.00234 0.04570 F9B 4 -0.080242 0.651549 0.091426 41.00000 0.06791 0.07207 = 0.09089 0.02477 -0.00040 0.04326 HKLF 4 REM 007b-17085 REM R1 = 0.0750 for 6951 Fo > 4sig(Fo) and 0.1167 for all 10085 data REM 822 parameters refined using 997 restraints END WGHT 0.0432 20.1260 REM Highest difference peak 0.786, deepest hole -0.647, 1-sigma level 0.091 Q1 1 0.1005 0.6993 0.1972 11.00000 0.05 0.79 Q2 1 0.5991 0.3017 0.1966 11.00000 0.05 0.75 Q3 1 0.0331 0.3375 0.2496 11.00000 0.05 0.54 Q4 1 0.5304 0.6666 0.2533 11.00000 0.05 0.47 Q5 1 0.5941 0.6765 0.2977 11.00000 0.05 0.42 Q6 1 0.2224 0.6805 0.1744 11.00000 0.05 0.41 Q7 1 0.9911 0.3174 0.5479 11.00000 0.05 0.39 Q8 1 0.6574 0.6613 0.3316 11.00000 0.05 0.38 Q9 1 0.4827 0.7036 0.1974 11.00000 0.05 0.34 Q10 1 1.1372 0.3591 0.5014 11.00000 0.05 0.34 Q11 1 0.5811 0.6524 0.4976 11.00000 0.05 0.34 Q12 1 0.1198 0.3141 0.2055 11.00000 0.05 0.33 Q13 1 1.0513 0.3444 0.4985 11.00000 0.05 0.33 Q14 1 0.3128 0.3030 0.4603 11.00000 0.05 0.32 Q15 1 0.0113 0.4776 0.3885 11.00000 0.05 0.32 Q16 1 0.6632 0.6424 0.6113 11.00000 0.05 0.30 Q17 1 1.0547 0.5211 0.4510 11.00000 0.05 0.29 Q18 1 0.0000 0.6406 0.0794 11.00000 0.05 0.29 Q19 1 0.7280 0.3161 0.1702 11.00000 0.05 0.29 Q20 1 0.8687 0.6449 0.3495 11.00000 0.05 0.29 ; _shelx_res_checksum 81372 _shelx_hkl_file ; 0 0 -31 -8.31 15.57 0 0 -31 -15.60 13.90 0 0 -30 132.74 18.72 0 0 -30 109.17 19.58 0 0 -30 103.51 20.85 0 0 -29 33.79 18.45 0 0 -29 -25.64 13.28 0 0 -29 15.38 17.89 0 0 -29 9.54 16.01 0 0 -28 46.17 21.73 0 0 -28 30.86 18.27 0 0 -28 2.25 18.67 0 0 -28 39.94 15.57 0 0 -27 14.92 15.63 0 0 -27 -10.36 20.38 0 0 -27 9.77 22.12 0 0 -27 -35.41 20.72 0 0 -26 525.62 44.61 0 0 -26 518.38 45.87 0 0 -26 518.66 43.77 0 0 -25 13.67 17.48 0 0 -25 1.24 22.35 0 0 -25 -13.94 21.51 0 0 -25 18.08 21.81 0 0 -24 420.90 29.62 0 0 -24 342.09 34.73 0 0 -24 414.45 33.01 0 0 -24 357.80 32.91 0 0 -23 -12.23 17.81 0 0 -23 -32.42 25.06 0 0 -23 -1.76 21.85 0 0 -23 -31.85 112.90 0 0 -23 11.11 17.17 0 0 -23 19.03 96.23 0 0 -23 -24.56 85.72 0 0 -23 9.33 22.15 0 0 -22 9.80 15.71 0 0 -22 -59.60 87.56 0 0 -22 44.39 22.42 0 0 -22 0.76 24.03 0 0 -22 23.27 20.87 0 0 -22 51.63 17.84 0 0 -22 12.67 17.46 0 0 -22 58.50 95.46 0 0 -22 42.06 87.13 0 0 -21 -21.02 89.33 0 0 -21 105.80 82.55 0 0 -21 -9.21 17.18 0 0 -21 96.17 84.01 0 0 -21 13.29 21.63 0 0 -21 2.06 21.08 0 0 -21 -7.93 15.54 0 0 -21 -2.87 21.02 0 0 -21 -0.76 17.32 0 0 -20 982.44 116.25 0 0 -20 1075.30 116.38 0 0 -20 935.94 64.39 0 0 -20 952.00 65.10 0 0 -20 1151.95 63.63 0 0 -20 868.79 65.15 0 0 -20 896.95 63.55 0 0 -20 901.02 65.18 0 0 -20 1138.14 110.16 0 0 -20 918.25 63.06 0 0 -19 65.90 72.92 0 0 -19 -7.59 19.82 0 0 -19 9.39 19.22 0 0 -19 8.36 15.96 0 0 -19 27.11 56.48 0 0 -19 -10.31 15.51 0 0 -19 7.24 17.11 0 0 -19 -54.90 67.30 0 0 -19 0.42 19.68 0 0 -19 -79.90 76.66 0 0 -19 -25.38 21.66 0 0 -18 744.46 46.49 0 0 -18 689.45 85.30 0 0 -18 631.74 89.32 0 0 -18 625.71 46.38 0 0 -18 633.47 47.35 0 0 -18 622.43 45.22 0 0 -18 674.38 44.68 0 0 -18 720.48 45.05 0 0 -18 613.37 47.67 0 0 -18 517.39 77.42 0 0 -18 614.78 43.68 0 0 -18 630.13 90.89 0 0 -17 24.05 19.50 0 0 -17 95.00 48.37 0 0 -17 17.05 17.53 0 0 -17 4.16 12.45 0 0 -17 -10.52 11.25 0 0 -17 -18.87 17.18 0 0 -17 5.43 18.00 0 0 -17 7.23 63.81 0 0 -17 -22.85 65.41 0 0 -17 23.58 15.55 0 0 -17 22.32 20.16 0 0 -17 33.61 57.30 0 0 -17 -12.08 14.63 0 0 -16 344.49 32.85 0 0 -16 365.03 58.69 0 0 -16 406.92 67.78 0 0 -16 361.67 27.62 0 0 -16 378.47 28.26 0 0 -16 370.83 30.97 0 0 -16 365.79 32.19 0 0 -16 417.86 29.09 0 0 -16 422.73 31.39 0 0 -16 466.99 29.87 0 0 -16 426.05 75.03 0 0 -16 407.54 30.89 0 0 -16 492.18 74.28 0 0 -15 1.15 12.51 0 0 -15 -3.65 14.61 0 0 -15 -11.35 53.38 0 0 -15 13.09 19.22 0 0 -15 -10.71 13.60 0 0 -15 9.41 16.42 0 0 -15 -1.20 46.48 0 0 -15 74.85 57.74 0 0 -15 3.26 11.32 0 0 -15 28.96 60.93 0 0 -15 -1.55 18.22 0 0 -15 2.23 15.94 0 0 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57.98 -2 0 7 542.16 62.51 2 0 7 652.37 60.03 -2 0 7 574.68 53.74 2 0 7 586.37 54.84 -2 0 7 567.24 62.90 -2 0 7 574.75 44.09 2 0 7 478.17 36.13 2 0 7 574.16 44.86 2 0 7 600.83 57.95 2 0 7 534.87 36.46 2 0 8 1367.90 101.05 2 0 8 1314.10 86.94 -2 0 8 1268.82 102.83 -2 0 8 1252.10 100.49 2 0 8 1323.28 91.75 2 0 8 1448.61 101.71 -2 0 8 1365.07 96.18 -2 0 8 1228.54 100.91 -2 0 8 1324.23 104.80 2 0 8 1340.64 99.77 -2 0 8 1295.08 91.14 -2 0 8 1375.73 101.75 -2 0 9 980.37 81.36 -2 0 9 913.81 81.93 2 0 9 828.25 77.86 -2 0 9 887.88 82.79 2 0 9 947.02 64.96 -2 0 9 902.06 69.58 2 0 9 946.45 79.84 -2 0 9 945.02 82.42 -2 0 9 911.16 81.08 2 0 9 873.76 70.80 -2 0 10 936.54 96.73 -2 0 10 1058.27 96.56 2 0 10 1136.43 93.59 2 0 10 1158.91 82.03 -2 0 10 1186.09 86.03 2 0 10 1293.08 95.23 -2 0 10 1129.90 94.83 -2 0 10 1246.30 99.00 -2 0 10 1160.63 96.45 2 0 10 1252.00 87.37 -2 0 11 1607.64 129.81 2 0 11 1582.04 127.08 -2 0 11 1650.92 126.58 2 0 11 1819.73 121.60 -2 0 11 1559.99 127.81 -2 0 11 1640.47 129.00 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0 14 12.08 56.52 -2 0 14 0.13 55.75 2 0 14 29.08 14.30 -2 0 14 57.45 16.94 2 0 14 31.39 12.68 2 0 14 27.94 46.78 -2 0 14 17.26 41.64 2 0 15 474.75 61.43 2 0 15 298.28 63.85 -2 0 15 482.34 74.20 2 0 15 364.54 30.02 -2 0 15 467.26 56.23 -2 0 15 484.48 64.23 -2 0 15 455.42 72.55 2 0 15 511.48 68.29 -2 0 15 408.47 30.33 -2 0 15 424.57 28.55 -2 0 15 455.59 74.87 2 0 15 470.38 29.53 -2 0 15 382.19 29.96 2 0 15 481.54 68.10 -2 0 15 334.45 32.42 2 0 15 384.72 29.05 -2 0 15 405.54 69.27 -2 0 15 347.96 31.59 -2 0 16 82.55 13.34 2 0 16 99.59 15.39 -2 0 16 130.37 64.09 -2 0 16 207.75 68.23 -2 0 16 113.42 57.39 2 0 16 125.36 58.12 -2 0 16 18.89 67.87 2 0 16 151.38 54.91 -2 0 16 191.00 52.40 2 0 16 106.51 59.13 -2 0 16 68.33 15.55 2 0 16 -53.88 59.66 2 0 16 74.45 15.64 -2 0 16 80.42 15.98 -2 0 16 69.17 20.56 -2 0 16 78.29 19.27 -2 0 16 89.41 66.02 2 0 16 64.55 14.54 -2 0 17 90.95 69.12 2 0 17 95.01 60.61 -2 0 17 99.40 14.55 2 0 17 39.09 59.27 2 0 17 81.83 61.14 -2 0 17 72.57 72.35 -2 0 17 145.88 21.00 -2 0 17 152.75 66.50 2 0 17 86.85 17.03 -2 0 17 79.99 61.34 -2 0 17 78.83 18.35 2 0 17 248.22 63.01 -2 0 17 115.68 17.34 2 0 17 121.40 15.80 -2 0 17 94.29 55.22 -2 0 17 155.32 22.71 2 0 17 104.42 16.39 -2 0 18 308.00 80.10 -2 0 18 263.12 76.71 2 0 18 314.68 68.19 2 0 18 199.96 73.02 -2 0 18 216.96 25.72 -2 0 18 261.48 64.09 -2 0 18 221.29 27.14 2 0 18 296.05 68.91 2 0 18 282.26 22.19 -2 0 18 257.51 20.61 -2 0 18 228.54 23.12 2 0 18 233.16 21.58 2 0 18 197.95 22.41 -2 0 18 241.96 23.22 -2 0 18 197.35 80.98 -2 0 18 281.28 76.25 2 0 18 143.50 66.66 2 0 19 27.73 16.26 -2 0 19 114.57 82.66 2 0 19 89.07 70.83 -2 0 19 46.74 17.41 -2 0 19 23.37 21.23 2 0 19 37.68 68.29 2 0 19 48.67 70.19 -2 0 19 45.80 17.18 -2 0 19 147.77 75.61 -2 0 19 116.91 78.74 -2 0 19 37.09 21.63 -2 0 19 37.59 13.98 2 0 19 76.19 16.68 -2 0 19 95.96 78.39 2 0 19 59.07 15.31 -2 0 20 268.38 25.75 -2 0 20 274.91 89.14 2 0 20 249.77 24.55 -2 0 20 238.93 29.04 -2 0 20 300.14 23.04 -2 0 20 300.88 28.66 2 0 20 258.19 23.92 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20.22 10 -7 1 13.18 13.28 10 7 1 -2.46 13.50 10 -7 1 36.08 16.71 -10 7 2 -0.99 18.80 -10 -7 2 8.51 18.63 -10 -7 2 -14.68 17.49 -10 7 2 -1.10 15.34 -10 -7 2 38.64 19.46 10 -7 2 19.99 12.59 10 7 2 10.53 13.48 10 -7 2 3.89 14.36 -10 7 3 -27.63 18.87 -10 -7 3 21.86 18.75 -10 -7 3 -26.18 17.50 -10 7 3 16.86 15.59 10 -7 3 -7.17 12.58 -10 -7 3 11.43 18.17 10 7 3 -19.43 13.96 10 -7 3 2.37 15.70 -10 7 4 34.05 16.51 -10 -7 4 44.31 16.04 -10 -7 4 3.90 16.54 -10 7 4 16.58 15.48 10 -7 4 10.23 13.18 -10 -7 4 -1.79 18.87 10 7 4 0.28 13.60 10 -7 4 -13.76 14.67 -10 7 5 14.78 14.89 -10 -7 5 9.16 18.47 -10 -7 5 7.64 14.59 -10 7 5 -25.29 15.91 10 -7 5 8.24 11.49 -10 -7 5 16.46 20.02 10 7 5 4.02 12.15 10 -7 5 -5.03 13.35 -10 7 6 -4.46 14.69 -10 -7 6 5.07 15.91 -10 -7 6 30.99 15.50 -10 7 6 14.48 16.36 10 -7 6 24.60 12.59 -10 -7 6 23.26 18.92 10 7 6 31.83 13.50 -10 8 -5 7.26 16.28 -10 -8 -5 21.71 16.31 -10 -8 -5 14.86 19.45 10 8 -5 34.85 15.13 -10 -8 -5 3.69 16.14 10 -8 -5 -12.09 16.57 10 8 -5 0.03 14.37 -10 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2 25.28 15.66 -10 -8 2 -23.09 16.80 -10 8 2 6.48 14.79 -10 -8 2 -10.30 20.57 10 -8 2 7.79 11.93 10 8 2 8.96 11.76 10 -8 2 10.77 15.26 -10 8 3 15.93 15.75 -10 -8 3 -9.75 17.19 -10 -8 3 28.08 16.43 -10 8 3 14.44 15.49 10 -8 3 -8.26 12.69 -10 -8 3 31.90 20.53 10 8 3 4.08 12.03 10 -8 3 9.16 13.86 -10 8 4 12.40 15.15 -10 -8 4 -6.44 18.11 -10 -8 4 -31.39 16.66 -10 8 4 -37.99 16.04 10 -8 4 9.08 12.73 -10 -8 4 26.32 19.60 10 8 4 -11.21 12.23 -10 8 5 13.31 15.13 -10 -8 5 -4.28 14.98 -10 -8 5 28.87 15.61 -10 8 5 11.94 15.00 10 -8 5 -23.31 12.20 -10 -8 5 -11.58 17.43 10 8 5 10.27 12.56 -10 9 -3 21.61 18.54 -10 -9 -3 4.96 16.94 -10 -9 -3 -33.62 19.53 10 -9 -3 13.81 12.16 10 9 -3 19.77 14.15 10 -9 -3 41.93 14.84 10 9 -3 10.86 14.16 -10 -9 -3 -1.40 14.64 -10 9 -2 47.74 18.68 -10 -9 -2 -40.66 15.05 -10 -9 -2 4.15 19.87 10 -9 -2 -9.74 12.61 10 9 -2 28.79 14.82 10 -9 -2 20.79 15.20 10 9 -2 14.11 14.36 -10 -9 -2 25.83 16.62 -10 9 -1 12.23 16.62 -10 -9 -1 24.41 16.98 -10 -9 -1 8.75 19.22 10 -9 -1 -6.51 12.86 10 9 -1 28.16 14.81 10 -9 -1 42.07 14.79 -10 -9 -1 15.78 17.36 -10 9 0 34.10 17.11 -10 -9 0 12.94 15.25 -10 -9 0 47.60 17.16 -10 -9 0 -5.50 17.98 10 -9 0 19.87 13.03 10 9 0 -11.45 15.10 10 -9 0 -5.75 14.07 -10 9 1 -19.85 17.99 -10 -9 1 21.85 16.45 -10 -9 1 27.95 16.56 -10 -9 1 15.66 17.53 10 -9 1 6.30 12.54 10 9 1 -13.98 15.09 -10 9 2 17.16 16.71 -10 -9 2 -3.25 15.77 -10 -9 2 -8.65 17.52 10 -9 2 -14.51 11.23 -10 9 3 17.36 14.59 -10 -9 3 40.52 15.20 -10 -9 3 38.73 15.76 -10 -9 3 2.93 18.27 0 0 0 0.00 0.00 TITL 007b-1708 in Pca2(1) REM Pca2(1) (#29 in standard setting) CELL 1.54184 8.885214 24.602710 26.079249 90.0000 90.0000 90.0000 ZERR 1.00 0.000242 0.000652 0.000718 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y, z SYMM -x+1/2, y, z+1/2 SFAC C H N O Br UNIT 1.00 1.00 1.00 1.00 1.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 19744