data_bromo _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H13 Br O4' _chemical_formula_sum 'C13 H13 Br O4' _chemical_formula_weight 313.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 8.848(4) _cell_length_b 12.172(6) _cell_length_c 12.759(6) _cell_angle_alpha 103.682(7) _cell_angle_beta 98.765(5) _cell_angle_gamma 90.185(7) _cell_volume 1318.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2775 _cell_measurement_theta_min 1.6635 _cell_measurement_theta_max 30.9549 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Colorless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_F_000 632 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 3.121 _shelx_estimated_absorpt_T_min 0.465 _shelx_estimated_absorpt_T_max 0.912 _exptl_absorpt_correction_type 'Numerical' _exptl_absorpt_correction_T_min 0.4647 _exptl_absorpt_correction_T_max 0.7664 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method 'dtprofit.ref' _diffrn_detector_area_resol_mean 14.6306 _diffrn_reflns_number 11070 _diffrn_reflns_av_unetI/netI 0.0835 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.723 _diffrn_reflns_theta_max 27.497 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 6015 _reflns_number_gt 3110 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _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^)+(0.0628P)^2^+0.1629P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6015 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Br1 Br 0.81621(9) 0.60589(5) 0.44313(5) 0.0763(3) Uani 1 1 d . . . . . Br2 Br 0.13072(9) -0.11945(5) -0.44517(5) 0.0768(3) Uani 1 1 d . . . . . O1 O 0.7701(4) 0.2500(3) -0.0529(3) 0.0506(9) Uani 1 1 d . . . . . O2 O 0.6992(5) 0.0810(3) -0.1647(4) 0.0695(12) Uani 1 1 d . . . . . O3 O 0.8035(5) 0.2611(3) -0.2956(4) 0.0706(12) Uani 1 1 d . . . . . O4 O 0.5906(4) 0.3430(3) -0.3476(3) 0.0601(11) Uani 1 1 d . . . . . O5 O 0.2903(4) 0.2493(3) 0.0476(3) 0.0531(10) Uani 1 1 d . . . . . O6 O 0.2645(5) 0.4177(3) 0.1572(3) 0.0704(12) Uani 1 1 d . . . . . O7 O 0.4272(4) 0.2461(4) 0.2945(4) 0.0778(13) Uani 1 1 d . . . . . O8 O 0.2401(4) 0.1550(3) 0.3409(3) 0.0580(10) Uani 1 1 d . . . . . C1 C 0.7813(6) 0.5352(4) 0.2922(4) 0.0449(12) Uani 1 1 d . . . . . C2 C 0.6835(6) 0.4425(4) 0.2534(4) 0.0460(12) Uani 1 1 d . . . . . H2 H 0.6301 0.4161 0.3006 0.055 Uiso 1 1 calc R U . . . C3 C 0.6644(6) 0.3887(4) 0.1450(5) 0.0478(13) Uani 1 1 d . . . . . H3 H 0.5983 0.3252 0.1192 0.057 Uiso 1 1 calc R U . . . C4 C 0.7421(5) 0.4269(4) 0.0720(4) 0.0401(11) Uani 1 1 d . . . . . C5 C 0.8369(6) 0.5242(4) 0.1138(5) 0.0491(13) Uani 1 1 d . . . . . H5 H 0.8883 0.5531 0.0672 0.059 Uiso 1 1 calc R U . . . C6 C 0.8554(6) 0.5782(4) 0.2234(5) 0.0509(13) Uani 1 1 d . . . . . H6 H 0.9180 0.6434 0.2502 0.061 Uiso 1 1 calc R U . . . C7 C 0.7278(5) 0.3687(4) -0.0460(4) 0.0403(11) Uani 1 1 d . . . . . H7 H 0.7991 0.4055 -0.0799 0.048 Uiso 1 1 calc R U . . . C8 C 0.5714(5) 0.3571(4) -0.1145(4) 0.0379(11) Uani 1 1 d . . . . . H8 H 0.5495 0.4230 -0.1438 0.045 Uiso 1 1 calc R U . . . H8A H 0.4921 0.3455 -0.0730 0.045 Uiso 1 1 calc R U . . . C9 C 0.5864(5) 0.2514(4) -0.2056(4) 0.0361(11) Uani 1 1 d . . . . . C10 C 0.6883(6) 0.1812(4) -0.1432(5) 0.0461(12) Uani 1 1 d . . . . . C11 C 0.6735(6) 0.2833(4) -0.2873(4) 0.0427(12) Uani 1 1 d . . . . . C12 C 0.4351(6) 0.1878(4) -0.2624(5) 0.0542(14) Uani 1 1 d . . . . . H12 H 0.3702 0.2369 -0.2962 0.081 Uiso 1 1 calc R U . . . H12A H 0.3850 0.1637 -0.2095 0.081 Uiso 1 1 calc R U . . . H12B H 0.4552 0.1229 -0.3172 0.081 Uiso 1 1 calc R U . . . C13 C 0.6641(8) 0.3911(5) -0.4214(5) 0.078(2) Uani 1 1 d . . . . . H13 H 0.6402 0.4693 -0.4123 0.118 Uiso 1 1 calc R U . . . H13A H 0.6281 0.3507 -0.4953 0.118 Uiso 1 1 calc R U . . . H13B H 0.7730 0.3851 -0.4053 0.118 Uiso 1 1 calc R U . . . C14 C 0.1604(6) -0.0438(4) -0.2953(4) 0.0507(14) Uani 1 1 d . . . . . C15 C 0.0775(6) 0.0496(4) -0.2604(5) 0.0491(13) Uani 1 1 d . . . . . H15 H 0.0051 0.0748 -0.3094 0.059 Uiso 1 1 calc R U . . . C16 C 0.1040(6) 0.1053(4) -0.1507(5) 0.0480(13) Uani 1 1 d . . . . . H16 H 0.0479 0.1681 -0.1261 0.058 Uiso 1 1 calc R U . . . C17 C 0.2128(5) 0.0692(4) -0.0769(4) 0.0407(12) Uani 1 1 d . . . . . C18 C 0.2909(6) -0.0269(4) -0.1150(5) 0.0511(14) Uani 1 1 d . . . . . H18 H 0.3620 -0.0538 -0.0665 0.061 Uiso 1 1 calc R U . . . C19 C 0.2646(6) -0.0834(4) -0.2242(5) 0.0566(15) Uani 1 1 d . . . . . H19 H 0.3175 -0.1479 -0.2488 0.068 Uiso 1 1 calc R U . . . C20 C 0.2482(6) 0.1303(4) 0.0409(4) 0.0447(12) Uani 1 1 d . . . . . H20 H 0.3351 0.0956 0.0763 0.054 Uiso 1 1 calc R U . . . C21 C 0.1189(5) 0.1397(4) 0.1085(4) 0.0405(12) Uani 1 1 d . . . . . H21 H 0.1111 0.0738 0.1380 0.049 Uiso 1 1 calc R U . . . H21A H 0.0215 0.1491 0.0657 0.049 Uiso 1 1 calc R U . . . C22 C 0.1694(5) 0.2462(3) 0.1995(4) 0.0388(11) Uani 1 1 d . . . . . C23 C 0.2463(6) 0.3166(4) 0.1365(4) 0.0475(13) Uani 1 1 d . . . . . C24 C 0.2954(6) 0.2184(4) 0.2836(4) 0.0440(12) Uani 1 1 d . . . . . C25 C 0.0423(6) 0.3086(4) 0.2543(5) 0.0562(14) Uani 1 1 d . . . . . H25 H 0.0001 0.2626 0.2952 0.084 Uiso 1 1 calc R U . . . H25A H -0.0366 0.3236 0.1995 0.084 Uiso 1 1 calc R U . . . H25B H 0.0833 0.3787 0.3026 0.084 Uiso 1 1 calc R U . . . C26 C 0.3481(8) 0.1148(5) 0.4188(5) 0.0747(19) Uani 1 1 d . . . . . H26 H 0.4278 0.0769 0.3829 0.112 Uiso 1 1 calc R U . . . H26A H 0.2964 0.0631 0.4491 0.112 Uiso 1 1 calc R U . . . H26B H 0.3918 0.1778 0.4763 0.112 Uiso 1 1 calc R U . . . 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 0.0920(6) 0.0810(5) 0.0458(4) 0.0005(3) 0.0026(4) 0.0054(4) Br2 0.1009(6) 0.0741(4) 0.0495(4) 0.0033(3) 0.0117(4) 0.0033(4) O1 0.053(2) 0.0488(19) 0.047(2) 0.0113(18) -0.0008(18) 0.0247(17) O2 0.096(3) 0.038(2) 0.073(3) 0.014(2) 0.006(3) 0.022(2) O3 0.052(3) 0.095(3) 0.074(3) 0.032(3) 0.020(2) 0.016(2) O4 0.064(3) 0.070(2) 0.060(3) 0.039(2) 0.016(2) 0.012(2) O5 0.061(2) 0.050(2) 0.050(2) 0.0119(18) 0.0137(19) -0.0141(17) O6 0.099(3) 0.038(2) 0.075(3) 0.018(2) 0.012(3) -0.012(2) O7 0.041(2) 0.107(3) 0.091(4) 0.049(3) -0.013(2) -0.007(2) O8 0.066(3) 0.063(2) 0.051(2) 0.030(2) 0.002(2) 0.0056(19) C1 0.044(3) 0.046(3) 0.042(3) 0.007(2) 0.001(2) 0.006(2) C2 0.039(3) 0.061(3) 0.040(3) 0.014(3) 0.006(2) 0.007(2) C3 0.041(3) 0.045(3) 0.058(4) 0.016(3) 0.008(3) 0.001(2) C4 0.034(3) 0.045(3) 0.042(3) 0.014(2) 0.002(2) 0.008(2) C5 0.051(3) 0.050(3) 0.051(4) 0.019(3) 0.013(3) 0.003(2) C6 0.047(3) 0.047(3) 0.055(4) 0.008(3) 0.004(3) -0.001(2) C7 0.038(3) 0.038(2) 0.046(3) 0.012(2) 0.007(2) 0.010(2) C8 0.032(3) 0.039(2) 0.046(3) 0.016(2) 0.008(2) 0.013(2) C9 0.032(3) 0.036(2) 0.043(3) 0.016(2) 0.004(2) 0.006(2) C10 0.046(3) 0.042(3) 0.051(3) 0.013(3) 0.007(3) 0.012(2) C11 0.041(3) 0.044(3) 0.043(3) 0.013(2) 0.004(2) 0.008(2) C12 0.046(3) 0.055(3) 0.063(4) 0.018(3) 0.006(3) -0.005(3) C13 0.106(6) 0.085(4) 0.058(4) 0.039(4) 0.020(4) -0.005(4) C14 0.059(4) 0.051(3) 0.042(3) 0.008(3) 0.011(3) -0.008(3) C15 0.052(3) 0.051(3) 0.045(3) 0.014(3) 0.006(3) 0.004(3) C16 0.044(3) 0.049(3) 0.054(4) 0.014(3) 0.014(3) 0.009(2) C17 0.038(3) 0.041(3) 0.044(3) 0.011(2) 0.008(2) -0.003(2) C18 0.051(3) 0.050(3) 0.054(4) 0.016(3) 0.007(3) 0.008(3) C19 0.052(4) 0.051(3) 0.067(4) 0.016(3) 0.008(3) 0.009(3) C20 0.040(3) 0.036(2) 0.057(3) 0.012(2) 0.005(3) -0.002(2) C21 0.040(3) 0.035(2) 0.048(3) 0.013(2) 0.007(2) 0.000(2) C22 0.042(3) 0.033(2) 0.043(3) 0.013(2) 0.007(2) 0.005(2) C23 0.052(3) 0.043(3) 0.047(3) 0.012(3) 0.002(3) -0.004(2) C24 0.045(3) 0.043(3) 0.042(3) 0.009(2) 0.005(2) 0.009(2) C25 0.050(3) 0.056(3) 0.063(4) 0.013(3) 0.011(3) 0.015(3) C26 0.096(5) 0.075(4) 0.055(4) 0.032(3) -0.005(4) 0.020(4) _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 C1 1.891(5) . ? Br2 C14 1.893(5) . ? O1 C10 1.356(6) . ? O1 C7 1.480(5) . ? O2 C10 1.193(5) . ? O3 C11 1.197(6) . ? O4 C11 1.325(6) . ? O4 C13 1.447(6) . ? O5 C23 1.344(6) . ? O5 C20 1.474(5) . ? O6 C23 1.200(5) . ? O7 C24 1.191(6) . ? O8 C24 1.320(5) . ? O8 C26 1.444(6) . ? C1 C6 1.365(7) . ? C1 C2 1.367(6) . ? C2 C3 1.368(7) . ? C3 C4 1.399(6) . ? C4 C5 1.395(7) . ? C4 C7 1.490(7) . ? C5 C6 1.383(7) . ? C7 C8 1.507(7) . ? C8 C9 1.537(6) . ? C9 C11 1.504(6) . ? C9 C10 1.512(6) . ? C9 C12 1.533(7) . ? C14 C19 1.364(8) . ? C14 C15 1.376(7) . ? C15 C16 1.388(7) . ? C16 C17 1.388(7) . ? C17 C18 1.386(7) . ? C17 C20 1.495(7) . ? C18 C19 1.384(8) . ? C20 C21 1.523(7) . ? C21 C22 1.534(6) . ? C22 C24 1.524(7) . ? C22 C25 1.524(7) . ? C22 C23 1.527(6) . ? 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 C10 O1 C7 109.9(4) . . ? C11 O4 C13 118.4(4) . . ? C23 O5 C20 109.9(3) . . ? C24 O8 C26 117.2(4) . . ? C6 C1 C2 121.0(5) . . ? C6 C1 Br1 119.0(4) . . ? C2 C1 Br1 120.1(4) . . ? C1 C2 C3 119.7(4) . . ? C2 C3 C4 121.5(5) . . ? C5 C4 C3 117.2(5) . . ? C5 C4 C7 119.8(4) . . ? C3 C4 C7 123.0(4) . . ? C6 C5 C4 120.9(4) . . ? C1 C6 C5 119.6(5) . . ? O1 C7 C4 107.6(4) . . ? O1 C7 C8 103.3(3) . . ? C4 C7 C8 118.1(4) . . ? C7 C8 C9 101.9(4) . . ? C11 C9 C10 107.9(4) . . ? C11 C9 C12 111.0(4) . . ? C10 C9 C12 111.8(4) . . ? C11 C9 C8 109.3(3) . . ? C10 C9 C8 101.1(4) . . ? C12 C9 C8 115.1(4) . . ? O2 C10 O1 122.3(5) . . ? O2 C10 C9 128.2(5) . . ? O1 C10 C9 109.5(4) . . ? O3 C11 O4 123.2(5) . . ? O3 C11 C9 124.9(5) . . ? O4 C11 C9 111.9(4) . . ? C19 C14 C15 121.4(5) . . ? C19 C14 Br2 118.9(4) . . ? C15 C14 Br2 119.7(5) . . ? C14 C15 C16 118.7(5) . . ? C15 C16 C17 121.3(5) . . ? C18 C17 C16 118.1(5) . . ? C18 C17 C20 119.4(5) . . ? C16 C17 C20 122.4(5) . . ? C19 C18 C17 121.0(5) . . ? C14 C19 C18 119.5(5) . . ? O5 C20 C17 108.5(4) . . ? O5 C20 C21 103.2(4) . . ? C17 C20 C21 117.6(4) . . ? C20 C21 C22 102.2(4) . . ? C24 C22 C25 111.1(4) . . ? C24 C22 C23 106.3(4) . . ? C25 C22 C23 112.3(4) . . ? C24 C22 C21 109.9(4) . . ? C25 C22 C21 116.0(4) . . ? C23 C22 C21 100.4(4) . . ? O6 C23 O5 121.9(4) . . ? O6 C23 C22 127.7(5) . . ? O5 C23 C22 110.4(4) . . ? O7 C24 O8 124.0(5) . . ? O7 C24 C22 125.2(5) . . ? O8 C24 C22 110.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.0(8) . . . . ? Br1 C1 C2 C3 -176.9(4) . . . . ? C1 C2 C3 C4 -0.6(8) . . . . ? C2 C3 C4 C5 -1.7(8) . . . . ? C2 C3 C4 C7 178.2(5) . . . . ? C3 C4 C5 C6 1.6(8) . . . . ? C7 C4 C5 C6 -178.3(5) . . . . ? C2 C1 C6 C5 -3.0(8) . . . . ? Br1 C1 C6 C5 176.9(4) . . . . ? C4 C5 C6 C1 0.7(8) . . . . ? C10 O1 C7 C4 147.7(4) . . . . ? C10 O1 C7 C8 22.1(5) . . . . ? C5 C4 C7 O1 123.6(5) . . . . ? C3 C4 C7 O1 -56.3(6) . . . . ? C5 C4 C7 C8 -120.2(5) . . . . ? C3 C4 C7 C8 60.0(6) . . . . ? O1 C7 C8 C9 -35.5(4) . . . . ? C4 C7 C8 C9 -154.0(4) . . . . ? C7 C8 C9 C11 -78.0(4) . . . . ? C7 C8 C9 C10 35.6(4) . . . . ? C7 C8 C9 C12 156.3(4) . . . . ? C7 O1 C10 O2 -177.8(5) . . . . ? C7 O1 C10 C9 1.5(5) . . . . ? C11 C9 C10 O2 -89.8(6) . . . . ? C12 C9 C10 O2 32.5(7) . . . . ? C8 C9 C10 O2 155.4(5) . . . . ? C11 C9 C10 O1 91.0(5) . . . . ? C12 C9 C10 O1 -146.7(4) . . . . ? C8 C9 C10 O1 -23.7(5) . . . . ? C13 O4 C11 O3 -4.8(8) . . . . ? C13 O4 C11 C9 173.0(4) . . . . ? C10 C9 C11 O3 -3.7(7) . . . . ? C12 C9 C11 O3 -126.6(6) . . . . ? C8 C9 C11 O3 105.4(6) . . . . ? C10 C9 C11 O4 178.5(4) . . . . ? C12 C9 C11 O4 55.6(5) . . . . ? C8 C9 C11 O4 -72.4(5) . . . . ? C19 C14 C15 C16 1.5(7) . . . . ? Br2 C14 C15 C16 -178.4(3) . . . . ? C14 C15 C16 C17 0.6(7) . . . . ? C15 C16 C17 C18 -2.3(7) . . . . ? C15 C16 C17 C20 177.5(4) . . . . ? C16 C17 C18 C19 1.9(7) . . . . ? C20 C17 C18 C19 -177.9(4) . . . . ? C15 C14 C19 C18 -1.8(7) . . . . ? Br2 C14 C19 C18 178.0(4) . . . . ? C17 C18 C19 C14 0.1(7) . . . . ? C23 O5 C20 C17 148.0(4) . . . . ? C23 O5 C20 C21 22.5(5) . . . . ? C18 C17 C20 O5 124.4(4) . . . . ? C16 C17 C20 O5 -55.4(6) . . . . ? C18 C17 C20 C21 -119.1(5) . . . . ? C16 C17 C20 C21 61.1(6) . . . . ? O5 C20 C21 C22 -35.4(5) . . . . ? C17 C20 C21 C22 -154.8(4) . . . . ? C20 C21 C22 C24 -77.1(5) . . . . ? C20 C21 C22 C25 155.8(4) . . . . ? C20 C21 C22 C23 34.5(5) . . . . ? C20 O5 C23 O6 -177.7(5) . . . . ? C20 O5 C23 C22 0.3(6) . . . . ? C24 C22 C23 O6 -90.3(6) . . . . ? C25 C22 C23 O6 31.4(8) . . . . ? C21 C22 C23 O6 155.3(6) . . . . ? C24 C22 C23 O5 91.8(5) . . . . ? C25 C22 C23 O5 -146.5(5) . . . . ? C21 C22 C23 O5 -22.6(5) . . . . ? C26 O8 C24 O7 -1.9(8) . . . . ? C26 O8 C24 C22 175.7(4) . . . . ? C25 C22 C24 O7 -123.5(6) . . . . ? C23 C22 C24 O7 -1.1(7) . . . . ? C21 C22 C24 O7 106.8(6) . . . . ? C25 C22 C24 O8 59.0(5) . . . . ? C23 C22 C24 O8 -178.6(4) . . . . ? C21 C22 C24 O8 -70.8(5) . . . . ? _refine_diff_density_max 0.461 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.079 _shelx_res_file ; bromo.res created by SHELXL-2014/7 TITL _bromo REM Yadorkari-X generated CELL 0.71075 8.8478 12.1721 12.7585 103.6816 98.7648 90.1845 ZERR 4.0 0.0039 0.0055 0.0059 0.0068 0.0051 0.0068 LATT 1 REM SPGR P-1 triclinic SFAC C H O Br UNIT 52 52 16 4 SIZE 0.29 0.29 0.03 TEMP 20.1 L.S. 10 FMAP 2 PLAN -25 ACTA CONF LIST 4 MERG 2 OMIT -10.000000 55.000000 WGHT 0.062800 0.162900 FVAR 2.74912 BR1 4 0.816210 0.605893 0.443135 11.00000 0.09199 0.08102 = 0.04583 0.00053 0.00256 0.00540 BR2 4 0.130720 -0.119446 -0.445171 11.00000 0.10095 0.07412 = 0.04953 0.00332 0.01173 0.00334 O1 3 0.770066 0.249972 -0.052907 11.00000 0.05316 0.04878 = 0.04705 0.01132 -0.00080 0.02468 O2 3 0.699214 0.080954 -0.164659 11.00000 0.09625 0.03816 = 0.07257 0.01423 0.00648 0.02233 O3 3 0.803457 0.261137 -0.295570 11.00000 0.05238 0.09492 = 0.07394 0.03250 0.02006 0.01567 O4 3 0.590592 0.342989 -0.347639 11.00000 0.06436 0.07031 = 0.05977 0.03945 0.01621 0.01242 O5 3 0.290267 0.249274 0.047573 11.00000 0.06070 0.04991 = 0.05025 0.01191 0.01367 -0.01410 O6 3 0.264537 0.417670 0.157210 11.00000 0.09938 0.03832 = 0.07530 0.01825 0.01217 -0.01244 O7 3 0.427160 0.246130 0.294491 11.00000 0.04069 0.10702 = 0.09112 0.04905 -0.01254 -0.00675 O8 3 0.240061 0.155014 0.340900 11.00000 0.06614 0.06260 = 0.05116 0.02992 0.00173 0.00561 C1 1 0.781333 0.535210 0.292210 11.00000 0.04355 0.04617 = 0.04171 0.00747 0.00092 0.00604 C2 1 0.683473 0.442481 0.253437 11.00000 0.03854 0.06109 = 0.03961 0.01423 0.00627 0.00701 AFIX 43 H2 2 0.630075 0.416083 0.300561 11.00000 -1.20000 AFIX 0 C3 1 0.664412 0.388661 0.144993 11.00000 0.04148 0.04530 = 0.05840 0.01564 0.00835 0.00126 AFIX 43 H3 2 0.598320 0.325210 0.119249 11.00000 -1.20000 AFIX 0 C4 1 0.742122 0.426946 0.071967 11.00000 0.03403 0.04526 = 0.04176 0.01391 0.00239 0.00783 C5 1 0.836855 0.524214 0.113757 11.00000 0.05141 0.04990 = 0.05103 0.01888 0.01317 0.00342 AFIX 43 H5 2 0.888264 0.553147 0.067155 11.00000 -1.20000 AFIX 0 C6 1 0.855382 0.578185 0.223446 11.00000 0.04689 0.04692 = 0.05529 0.00797 0.00387 -0.00057 AFIX 43 H6 2 0.917959 0.643416 0.250226 11.00000 -1.20000 AFIX 0 C7 1 0.727794 0.368690 -0.045980 11.00000 0.03804 0.03780 = 0.04641 0.01199 0.00749 0.01034 AFIX 13 H7 2 0.799148 0.405486 -0.079950 11.00000 -1.20000 AFIX 0 C8 1 0.571390 0.357062 -0.114529 11.00000 0.03247 0.03887 = 0.04620 0.01644 0.00814 0.01280 AFIX 23 H8 2 0.549510 0.422961 -0.143790 11.00000 -1.20000 H8A 2 0.492089 0.345516 -0.072987 11.00000 -1.20000 AFIX 0 C9 1 0.586407 0.251429 -0.205642 11.00000 0.03204 0.03618 = 0.04278 0.01583 0.00377 0.00609 C10 1 0.688274 0.181186 -0.143200 11.00000 0.04621 0.04169 = 0.05099 0.01263 0.00725 0.01215 C11 1 0.673457 0.283287 -0.287298 11.00000 0.04069 0.04425 = 0.04332 0.01251 0.00422 0.00761 C12 1 0.435053 0.187797 -0.262444 11.00000 0.04612 0.05479 = 0.06253 0.01776 0.00582 -0.00500 AFIX 137 H12 2 0.370217 0.236949 -0.296223 11.00000 -1.50000 H12A 2 0.384993 0.163745 -0.209523 11.00000 -1.50000 H12B 2 0.455177 0.122852 -0.317154 11.00000 -1.50000 AFIX 0 C13 1 0.664135 0.391053 -0.421364 11.00000 0.10589 0.08481 = 0.05784 0.03893 0.02047 -0.00539 AFIX 137 H13 2 0.640156 0.469271 -0.412342 11.00000 -1.50000 H13A 2 0.628072 0.350679 -0.495324 11.00000 -1.50000 H13B 2 0.772956 0.385090 -0.405326 11.00000 -1.50000 AFIX 0 C14 1 0.160378 -0.043790 -0.295329 11.00000 0.05883 0.05092 = 0.04180 0.00831 0.01085 -0.00840 C15 1 0.077453 0.049573 -0.260429 11.00000 0.05230 0.05130 = 0.04478 0.01408 0.00649 0.00428 AFIX 43 H15 2 0.005079 0.074803 -0.309404 11.00000 -1.20000 AFIX 0 C16 1 0.104021 0.105318 -0.150657 11.00000 0.04409 0.04864 = 0.05379 0.01359 0.01358 0.00856 AFIX 43 H16 2 0.047887 0.168056 -0.126059 11.00000 -1.20000 AFIX 0 C17 1 0.212768 0.069241 -0.076865 11.00000 0.03782 0.04128 = 0.04364 0.01057 0.00812 -0.00319 C18 1 0.290881 -0.026884 -0.114994 11.00000 0.05055 0.04999 = 0.05440 0.01634 0.00702 0.00778 AFIX 43 H18 2 0.362015 -0.053781 -0.066479 11.00000 -1.20000 AFIX 0 C19 1 0.264571 -0.083392 -0.224159 11.00000 0.05219 0.05080 = 0.06707 0.01557 0.00795 0.00862 AFIX 43 H19 2 0.317500 -0.147874 -0.248838 11.00000 -1.20000 AFIX 0 C20 1 0.248179 0.130292 0.040862 11.00000 0.04022 0.03644 = 0.05695 0.01195 0.00478 -0.00197 AFIX 13 H20 2 0.335076 0.095613 0.076321 11.00000 -1.20000 AFIX 0 C21 1 0.118940 0.139749 0.108531 11.00000 0.03990 0.03538 = 0.04752 0.01265 0.00706 -0.00038 AFIX 23 H21 2 0.111086 0.073833 0.138045 11.00000 -1.20000 H21A 2 0.021526 0.149119 0.065716 11.00000 -1.20000 AFIX 0 C22 1 0.169355 0.246246 0.199473 11.00000 0.04233 0.03303 = 0.04284 0.01253 0.00656 0.00524 C23 1 0.246336 0.316617 0.136513 11.00000 0.05182 0.04256 = 0.04716 0.01237 0.00240 -0.00447 C24 1 0.295420 0.218406 0.283647 11.00000 0.04541 0.04344 = 0.04213 0.00944 0.00461 0.00862 C25 1 0.042271 0.308566 0.254273 11.00000 0.05021 0.05615 = 0.06252 0.01327 0.01143 0.01482 AFIX 137 H25 2 0.000103 0.262623 0.295247 11.00000 -1.50000 H25A 2 -0.036642 0.323608 0.199526 11.00000 -1.50000 H25B 2 0.083302 0.378723 0.302566 11.00000 -1.50000 AFIX 0 C26 1 0.348069 0.114837 0.418815 11.00000 0.09641 0.07523 = 0.05543 0.03227 -0.00522 0.01959 AFIX 137 H26 2 0.427789 0.076899 0.382867 11.00000 -1.50000 H26A 2 0.296415 0.063071 0.449053 11.00000 -1.50000 H26B 2 0.391827 0.177822 0.476336 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM _bromo REM R1 = 0.0685 for 3110 Fo > 4sig(Fo) and 0.1384 for all 6015 data REM 329 parameters refined using 0 restraints END WGHT 0.0628 0.1629 REM Highest difference peak 0.461, deepest hole -0.517, 1-sigma level 0.079 Q1 1 0.8617 0.5378 0.3845 11.00000 0.05 0.46 Q2 1 0.8188 0.1888 -0.4937 11.00000 0.05 0.45 Q3 1 0.7649 0.6667 0.5024 11.00000 0.05 0.43 Q4 1 0.0977 -0.0570 -0.3838 11.00000 0.05 0.40 Q5 1 0.7753 0.2849 -0.4651 11.00000 0.05 0.37 Q6 1 0.8560 0.6578 0.4222 11.00000 0.05 0.32 Q7 1 0.2692 0.2762 0.0772 11.00000 0.05 0.29 Q8 1 -0.0750 -0.0155 -0.3060 11.00000 0.05 0.28 Q9 1 1.1886 0.4781 0.2199 11.00000 0.05 0.28 Q10 1 1.0283 0.3631 0.3166 11.00000 0.05 0.28 Q11 1 0.1228 0.2029 0.1579 11.00000 0.05 0.27 Q12 1 0.7305 0.5264 0.4971 11.00000 0.05 0.26 Q13 1 0.6206 0.7106 0.5788 11.00000 0.05 0.25 Q14 1 0.7918 0.2217 -0.1033 11.00000 0.05 0.25 Q15 1 0.3429 0.3789 0.1346 11.00000 0.05 0.25 Q16 1 0.4480 0.4770 0.2413 11.00000 0.05 0.24 Q17 1 0.4300 0.4378 0.2254 11.00000 0.05 0.24 Q18 1 0.2706 0.1113 0.4871 11.00000 0.05 0.24 Q19 1 0.9882 0.4381 0.1762 11.00000 0.05 0.24 Q20 1 0.6046 0.1010 -0.1049 11.00000 0.05 0.24 Q21 1 -0.0794 0.1222 -0.3245 11.00000 0.05 0.23 Q22 1 0.3981 0.2139 -0.2653 11.00000 0.05 0.23 Q23 1 0.2076 0.2978 0.1505 11.00000 0.05 0.23 Q24 1 0.6275 0.1204 -0.0848 11.00000 0.05 0.23 Q25 1 0.9559 0.4920 0.3515 11.00000 0.05 0.23 ; _shelx_res_checksum 2298 _shelx_hkl_file ; 0 0 -2 678.31 96.55 0 0 2 564.85 105.75 0 0 -320294.20 530.82 0 0 318043.00 482.58 0 0 318963.50 390.57 0 0 -4 515.12 125.16 0 0 4 27.08 118.28 0 0 4 292.10 54.18 0 0 -4 286.78 50.23 0 0 -5 9938.04 410.85 0 0 510196.50 429.04 0 0 510881.40 327.13 0 0 -510097.70 290.45 0 0 625437.00 814.68 0 0 627473.50 679.20 0 0 -626202.20 645.55 0 0 741037.40 1382.63 0 0 741647.00 1195.91 0 0 -739962.30 1209.50 0 0 835040.90 1130.10 0 0 834449.10 840.27 0 0 -834544.20 810.79 0 0 9 9917.82 464.47 0 0 1021435.60 729.54 0 0 11 2526.26 322.56 0 0 12 3394.57 347.57 0 0 -13 37.13 186.99 0 0 -14 639.24 256.69 0 0 -15 263.06 131.01 0 0 -16 893.87 337.64 0 1 -17 89.55 151.74 0 1 -16 234.31 160.56 0 1 -15 334.07 172.88 0 1 -14 -34.90 169.00 0 1 -13 139.35 172.38 0 1 -12 196.09 147.66 0 1 -11 152.57 189.16 0 -1 9 100.51 151.40 0 -1 8 62.42 145.33 0 1 -8 79.41 28.04 0 -1 7 49.39 134.90 0 1 -7 25.23 32.48 0 -1 6 162.97 170.13 0 -1 6 55.83 35.73 0 1 -6 39.57 33.95 0 1 -5 2.19 102.39 0 -1 5 -2.97 102.95 0 -1 5 72.14 42.09 0 1 -5 67.18 45.75 0 1 -4 113.21 93.31 0 -1 4 -7.67 82.56 0 -1 4 56.70 33.79 0 1 -4 29.48 20.28 0 1 -4 12.53 25.27 0 1 -3 -50.70 84.82 0 -1 3 273.26 93.14 0 -1 3 51.77 30.56 0 1 -3 75.95 52.02 0 -1 3 90.89 48.57 0 1 -3 149.51 59.76 0 1 -2 94.31 56.56 0 1 -2 111.73 59.84 0 -1 2 102.90 53.22 0 1 -2 129.86 53.73 0 -1 2 94.93 46.15 0 1 -2 94.92 54.40 0 -1 1 201.32 85.06 0 1 0 -20.09 16.73 0 -1 0 57.66 25.65 0 1 0 -10.97 23.27 0 1 0 -24.26 17.81 0 -1 -1 56.91 63.91 0 1 1 186.19 75.00 0 -1 -2 18.41 89.86 0 1 2 422.76 109.06 0 -1 -3 114.56 97.36 0 1 3 -136.05 121.14 0 -1 -4 253.16 150.91 0 1 4 260.39 157.20 0 1 5 294.92 168.19 0 1 6 701.27 160.41 0 1 7 291.60 220.21 0 1 7 196.49 46.76 0 1 8 157.99 154.08 0 1 8 38.97 33.68 0 -1 -8 35.73 25.04 0 1 9 453.76 242.69 0 1 9 241.59 42.50 0 -1 -9 165.37 37.24 0 1 10 317.69 278.13 0 1 11 22.54 166.23 0 1 12 233.04 185.31 0 1 13 -121.04 168.75 0 -1 -14 95.94 223.53 0 -1 -15 -5.74 250.26 0 -1 -16 -95.12 220.41 0 2 -17 152.39 214.02 0 2 -16 11.97 143.54 0 2 -15 2167.31 664.39 0 2 -14 744.53 310.49 0 2 -13 2704.91 683.56 0 2 -1213958.00 2496.75 0 2 -11 107.53 168.41 0 2 -10 5179.37 1365.73 0 2 -9 16.74 128.16 0 2 -8 7077.46 572.31 0 2 -722405.90 994.86 0 2 -722743.70 760.28 0 2 -633262.20 1264.41 0 2 -636030.30 1003.25 0 2 -5117776.3 1079.88 0 2 -5117511.8 1054.41 0 2 -461660.80 1299.32 0 2 -460432.80 1283.29 0 2 -346399.80 959.34 0 -2 346027.10 942.52 0 2 -2102347.1 1917.51 0 -2 298739.90 1883.78 0 -2 110044.10 237.65 0 2 -110007.30 244.31 0 -2 110628.10 284.63 0 2 -1 9780.67 260.77 0 -2 1 9607.17 252.53 0 2 -1 9410.71 360.63 0 -2 0 3520.91 125.80 0 2 0 3859.13 148.65 0 -2 0 3350.11 139.86 0 2 0 3641.86 148.60 0 2 0 3729.41 330.20 0 -2 -130744.50 650.70 0 2 129306.10 628.81 0 -2 -2183606.8 3419.96 0 2 2180669.1 3365.21 0 -2 -3190559.2 3583.44 0 2 3181128.1 3433.64 0 -2 -410489.20 420.57 0 2 410107.30 405.02 0 2 568008.00 962.83 0 2 6 7154.44 434.91 0 2 7 6154.37 416.44 0 2 8 9167.29 466.90 0 2 9 4887.08 390.24 0 2 9 3755.15 264.36 0 2 10 7236.36 490.44 0 2 11 2687.85 374.59 0 2 12 4350.90 613.05 0 2 13 7556.09 567.25 0 2 14 2340.62 591.62 0 -2 -15 415.92 200.39 0 3 -17 201.44 99.46 0 3 -16 -311.23 209.94 0 3 -15 270.86 101.14 0 3 -14 161.63 145.02 0 3 -13 -141.59 187.89 0 3 -12 207.38 97.05 0 3 -11 84.40 140.34 0 3 -10 -271.90 158.53 0 3 -9 0.54 99.66 0 3 -8 78.78 104.31 0 3 -8 44.65 62.87 0 3 -7 426.79 81.58 0 3 -7 433.03 142.51 0 -3 7 465.79 173.75 0 3 -6 96.21 151.22 0 3 -6 154.32 106.04 0 3 -6 52.45 47.63 0 -3 6 143.19 71.13 0 3 -5 388.42 150.34 0 3 -5 507.82 119.71 0 3 -5 333.34 141.13 0 -3 5 240.54 129.01 0 -3 4 165.01 52.46 0 3 -4 305.68 113.46 0 3 -4 -15.44 79.97 0 -3 4 344.86 83.95 0 -3 3 9.15 37.49 0 3 -3 29.35 36.41 0 3 -3 -94.68 84.89 0 -3 3 67.77 50.15 0 -3 2 170.03 70.91 0 3 -2 50.45 48.76 0 3 -2 131.86 72.66 0 -3 2 -48.38 79.61 0 -3 2 83.30 90.89 0 -3 1 641.47 77.70 0 3 -1 740.16 81.36 0 -3 1 652.13 161.91 0 3 -1 744.71 192.05 0 -3 1 656.34 125.29 0 3 -1 650.65 151.58 0 -3 0 944.54 93.46 0 3 0 804.14 84.65 0 -3 0 823.42 227.13 0 3 0 859.81 191.12 0 -3 -1 1374.87 109.88 0 3 1 1471.03 117.56 0 -3 -2 1139.86 118.46 0 3 2 1156.06 130.80 0 -3 -3 957.06 129.37 0 3 3 675.31 151.03 0 3 4 1955.91 172.57 0 3 5 42.41 137.13 0 3 6 67.51 139.10 0 3 7 67.47 145.40 0 3 8 524.22 179.45 0 3 9 396.50 188.84 0 3 10 463.63 220.98 0 3 11 385.83 212.35 0 3 12 228.69 213.17 0 3 13 -67.53 197.47 0 3 14 160.18 212.44 0 -3 -15 -136.89 230.38 0 4 -17 521.10 257.43 0 4 -16 207.85 277.56 0 4 -15 -11.33 136.51 0 4 -14 221.19 202.78 0 4 -13 1384.13 386.84 0 4 -12 -35.92 195.05 0 4 -11 1512.63 323.24 0 4 -1039583.10 1209.07 0 4 -1042895.10 737.53 0 4 -924921.20 1119.97 0 4 -927270.40 671.82 0 -4 929306.70 626.70 0 4 -8 6678.68 682.97 0 4 -8 7277.50 368.50 0 -4 8 6725.66 749.19 0 4 -719211.30 1084.36 0 4 -718236.30 789.32 0 -4 717755.40 801.62 0 4 -6 47.91 82.02 0 4 -6 28.33 85.26 0 4 -6 108.64 54.15 0 -4 6 42.48 32.04 0 -4 5 79.02 82.55 0 4 -5 89.45 102.50 0 4 -5 69.85 70.89 0 -4 5 17.87 42.49 0 -4 4 1001.12 312.35 0 4 -4 645.35 129.31 0 4 -4 639.51 110.01 0 -4 4 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