data_minor_P212121 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H21 Br N2 O2' _chemical_formula_sum 'C20 H21 Br N2 O2' _chemical_formula_weight 401.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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 5.8738(7) _cell_length_b 14.1110(17) _cell_length_c 21.502(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1782.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5655 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 32.90 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_F_000 824 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 2.322 _shelx_estimated_absorpt_T_min 0.606 _shelx_estimated_absorpt_T_max 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3723 _exptl_absorpt_correction_T_max 0.4353 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25539 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.726 _diffrn_reflns_theta_max 32.574 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6480 _reflns_number_gt 5782 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.758 _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0490P)^2^+0.2000P] 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_abs_structure_details ; Flack x determined using 2301 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.005(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 6480 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.78963(5) 0.07587(2) -0.05619(2) 0.02854(8) Uani 1 1 d . . . . . O1 O 1.1264(4) 0.10157(13) 0.23337(9) 0.0273(4) Uani 1 1 d . . . . . O2 O 0.7853(4) 0.06158(11) 0.26107(8) 0.0255(3) Uani 1 1 d . . . . . N1 N 0.7633(4) 0.35649(13) 0.31246(9) 0.0217(4) Uani 1 1 d . . . . . N2 N 0.9316(4) 0.12093(14) 0.24862(9) 0.0188(4) Uani 1 1 d . . . . . C1 C 0.8088(4) 0.25522(15) 0.31955(9) 0.0173(4) Uani 1 1 d . . . . . H1 H 0.6662 0.2227 0.3333 0.021 Uiso 1 1 calc R U . . . C2 C 0.8661(4) 0.22402(14) 0.25216(10) 0.0150(4) Uani 1 1 d . . . . . H2 H 0.9955 0.2633 0.2364 0.018 Uiso 1 1 calc R U . . . C3 C 0.6602(4) 0.23803(16) 0.20926(10) 0.0165(4) Uani 1 1 d . . . . . H3 H 0.5331 0.2000 0.2275 0.020 Uiso 1 1 calc R U . . . C4 C 0.5814(4) 0.34333(17) 0.21075(11) 0.0219(5) Uani 1 1 d . . . . . H4 H 0.4287 0.3468 0.1903 0.026 Uiso 1 1 calc R U . . . C5 C 0.5518(5) 0.37254(19) 0.27881(12) 0.0262(5) Uani 1 1 d . . . . . H5A H 0.5098 0.4404 0.2812 0.031 Uiso 1 1 calc R U . . . H5B H 0.4278 0.3350 0.2980 0.031 Uiso 1 1 calc R U . . . C6 C 0.7954(5) 0.41267(16) 0.36849(11) 0.0265(5) Uani 1 1 d . . . . . H6A H 0.7006 0.3870 0.4026 0.032 Uiso 1 1 calc R U . . . H6B H 0.7486 0.4791 0.3608 0.032 Uiso 1 1 calc R U . . . C7 C 1.0437(5) 0.40922(19) 0.38649(13) 0.0300(6) Uani 1 1 d . . . . . H7A H 1.1371 0.4387 0.3534 0.036 Uiso 1 1 calc R U . . . H7B H 1.0677 0.4454 0.4254 0.036 Uiso 1 1 calc R U . . . C8 C 1.1159(5) 0.30810(18) 0.39575(11) 0.0234(5) Uani 1 1 d . . . . . C9 C 1.2901(5) 0.2849(2) 0.43721(11) 0.0329(6) Uani 1 1 d . . . . . H9 H 1.3726 0.3343 0.4571 0.039 Uiso 1 1 calc R U . . . C10 C 1.3456(5) 0.1914(3) 0.45012(13) 0.0377(7) Uani 1 1 d . . . . . H10 H 1.4688 0.1770 0.4772 0.045 Uiso 1 1 calc R U . . . C11 C 1.2199(6) 0.1192(2) 0.42323(12) 0.0338(6) Uani 1 1 d . . . . . H11 H 1.2524 0.0550 0.4330 0.041 Uiso 1 1 calc R U . . . C12 C 1.0464(5) 0.14096(19) 0.38196(11) 0.0249(5) Uani 1 1 d . . . . . H12 H 0.9598 0.0911 0.3640 0.030 Uiso 1 1 calc R U . . . C13 C 0.9964(4) 0.23495(17) 0.36623(10) 0.0188(4) Uani 1 1 d . . . . . C14 C 0.6971(4) 0.20048(15) 0.14391(10) 0.0164(4) Uani 1 1 d . . . . . C15 C 0.8981(4) 0.21547(17) 0.11059(11) 0.0197(4) Uani 1 1 d . . . . . H15 H 1.0181 0.2507 0.1291 0.024 Uiso 1 1 calc R U . . . C16 C 0.9258(4) 0.17980(16) 0.05084(11) 0.0203(4) Uani 1 1 d . . . . . H16 H 1.0628 0.1907 0.0285 0.024 Uiso 1 1 calc R U . . . C17 C 0.7500(4) 0.12799(15) 0.02436(10) 0.0192(4) Uani 1 1 d . . . . . C18 C 0.5480(4) 0.11205(17) 0.05588(12) 0.0215(4) Uani 1 1 d . . . . . H18 H 0.4285 0.0767 0.0372 0.026 Uiso 1 1 calc R U . . . C19 C 0.5237(4) 0.14888(17) 0.11556(11) 0.0191(4) Uani 1 1 d . . . . . H19 H 0.3855 0.1386 0.1375 0.023 Uiso 1 1 calc R U . . . C20 C 0.7396(5) 0.41219(16) 0.17675(11) 0.0251(5) Uani 1 1 d . . . . . H20A H 0.6776 0.4765 0.1795 0.038 Uiso 1 1 calc R U . . . H20B H 0.7518 0.3936 0.1330 0.038 Uiso 1 1 calc R U . . . H20C H 0.8908 0.4105 0.1960 0.038 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 0.03296(13) 0.03385(13) 0.01880(10) -0.00548(9) 0.00124(10) 0.00539(11) O1 0.0280(9) 0.0283(9) 0.0256(9) 0.0004(7) 0.0049(7) 0.0114(7) O2 0.0300(9) 0.0177(7) 0.0288(8) 0.0006(6) -0.0052(8) -0.0046(7) N1 0.0302(12) 0.0161(8) 0.0188(8) -0.0021(6) 0.0040(8) 0.0042(8) N2 0.0254(10) 0.0159(8) 0.0151(8) -0.0011(7) -0.0018(7) 0.0022(7) C1 0.0203(10) 0.0159(9) 0.0156(8) -0.0004(7) 0.0032(8) 0.0007(8) C2 0.0179(9) 0.0117(8) 0.0154(9) -0.0008(7) 0.0010(7) 0.0011(7) C3 0.0153(10) 0.0175(9) 0.0167(9) 0.0013(7) 0.0016(7) 0.0010(7) C4 0.0221(11) 0.0218(11) 0.0217(11) 0.0026(8) 0.0024(9) 0.0060(9) C5 0.0321(14) 0.0228(11) 0.0236(11) 0.0026(9) 0.0069(10) 0.0118(10) C6 0.0387(13) 0.0179(10) 0.0228(10) -0.0058(8) 0.0104(10) -0.0005(11) C7 0.0399(15) 0.0252(13) 0.0249(12) -0.0091(10) 0.0096(10) -0.0129(11) C8 0.0251(12) 0.0298(12) 0.0154(10) -0.0062(8) 0.0073(9) -0.0077(9) C9 0.0266(12) 0.0545(17) 0.0176(10) -0.0107(10) 0.0030(11) -0.0117(13) C10 0.0291(14) 0.067(2) 0.0172(11) -0.0036(12) -0.0035(10) 0.0077(13) C11 0.0405(16) 0.0423(15) 0.0185(10) -0.0013(10) -0.0051(11) 0.0127(14) C12 0.0326(13) 0.0266(12) 0.0156(10) 0.0000(9) -0.0027(9) 0.0049(10) C13 0.0215(10) 0.0222(10) 0.0126(9) -0.0011(8) 0.0019(8) -0.0013(8) C14 0.0160(9) 0.0169(9) 0.0163(8) 0.0027(7) -0.0004(8) -0.0002(8) C15 0.0163(10) 0.0229(11) 0.0199(10) 0.0012(8) 0.0012(8) -0.0031(8) C16 0.0179(10) 0.0243(10) 0.0186(10) 0.0041(9) 0.0031(8) -0.0002(8) C17 0.0238(13) 0.0190(9) 0.0147(8) 0.0010(7) -0.0003(7) 0.0048(8) C18 0.0206(10) 0.0223(10) 0.0216(10) -0.0006(9) -0.0018(10) -0.0018(8) C19 0.0161(10) 0.0222(11) 0.0191(10) 0.0018(8) 0.0010(8) 0.0002(8) C20 0.0344(14) 0.0190(10) 0.0219(10) 0.0038(8) 0.0011(9) 0.0017(9) _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 C17 1.896(2) . ? O1 N2 1.221(3) . ? O2 N2 1.229(3) . ? N1 C6 1.455(3) . ? N1 C5 1.455(4) . ? N1 C1 1.462(3) . ? N2 C2 1.507(3) . ? C1 C13 1.517(3) . ? C1 C2 1.551(3) . ? C1 H1 1.0000 . ? C2 C3 1.534(3) . ? C2 H2 1.0000 . ? C3 C14 1.517(3) . ? C3 C4 1.557(3) . ? C3 H3 1.0000 . ? C4 C20 1.530(3) . ? C4 C5 1.530(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.510(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.502(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.396(4) . ? C8 C13 1.400(3) . ? C9 C10 1.387(5) . ? C9 H9 0.9500 . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 C13 1.400(3) . ? C12 H12 0.9500 . ? C14 C19 1.393(3) . ? C14 C15 1.397(3) . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 C18 1.385(3) . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 C6 N1 C5 116.0(2) . . ? C6 N1 C1 115.00(19) . . ? C5 N1 C1 111.1(2) . . ? O1 N2 O2 124.1(2) . . ? O1 N2 C2 117.9(2) . . ? O2 N2 C2 117.9(2) . . ? N1 C1 C13 112.72(19) . . ? N1 C1 C2 102.69(16) . . ? C13 C1 C2 114.02(19) . . ? N1 C1 H1 109.1 . . ? C13 C1 H1 109.1 . . ? C2 C1 H1 109.1 . . ? N2 C2 C3 107.18(17) . . ? N2 C2 C1 112.12(17) . . ? C3 C2 C1 110.75(18) . . ? N2 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? C1 C2 H2 108.9 . . ? C14 C3 C2 113.53(18) . . ? C14 C3 C4 113.25(18) . . ? C2 C3 C4 110.18(18) . . ? C14 C3 H3 106.4 . . ? C2 C3 H3 106.4 . . ? C4 C3 H3 106.4 . . ? C20 C4 C5 110.8(2) . . ? C20 C4 C3 114.6(2) . . ? C5 C4 C3 108.09(19) . . ? C20 C4 H4 107.7 . . ? C5 C4 H4 107.7 . . ? C3 C4 H4 107.7 . . ? N1 C5 C4 109.7(2) . . ? N1 C5 H5A 109.7 . . ? C4 C5 H5A 109.7 . . ? N1 C5 H5B 109.7 . . ? C4 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N1 C6 C7 108.7(2) . . ? N1 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? N1 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? C8 C7 C6 109.7(2) . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C9 C8 C13 118.9(2) . . ? C9 C8 C7 121.0(2) . . ? C13 C8 C7 119.9(2) . . ? C10 C9 C8 121.6(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 119.8(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 121.3(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C12 C13 C8 118.9(2) . . ? C12 C13 C1 119.4(2) . . ? C8 C13 C1 121.6(2) . . ? C19 C14 C15 118.2(2) . . ? C19 C14 C3 118.9(2) . . ? C15 C14 C3 122.9(2) . . ? C16 C15 C14 121.2(2) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 118.9(2) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C18 C17 C16 121.5(2) . . ? C18 C17 Br1 119.27(18) . . ? C16 C17 Br1 119.21(18) . . ? C17 C18 C19 118.6(2) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C18 C19 C14 121.6(2) . . ? C18 C19 H19 119.2 . . ? C14 C19 H19 119.2 . . ? C4 C20 H20A 109.5 . . ? C4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C1 C13 -32.8(3) . . . . ? C5 N1 C1 C13 -167.07(19) . . . . ? C6 N1 C1 C2 -156.0(2) . . . . ? C5 N1 C1 C2 69.8(2) . . . . ? O1 N2 C2 C3 123.7(2) . . . . ? O2 N2 C2 C3 -56.1(2) . . . . ? O1 N2 C2 C1 -114.6(2) . . . . ? O2 N2 C2 C1 65.6(3) . . . . ? N1 C1 C2 N2 177.11(19) . . . . ? C13 C1 C2 N2 54.9(3) . . . . ? N1 C1 C2 C3 -63.2(2) . . . . ? C13 C1 C2 C3 174.51(18) . . . . ? N2 C2 C3 C14 -52.1(2) . . . . ? C1 C2 C3 C14 -174.67(17) . . . . ? N2 C2 C3 C4 179.68(18) . . . . ? C1 C2 C3 C4 57.1(2) . . . . ? C14 C3 C4 C20 -55.6(3) . . . . ? C2 C3 C4 C20 72.7(2) . . . . ? C14 C3 C4 C5 -179.7(2) . . . . ? C2 C3 C4 C5 -51.3(3) . . . . ? C6 N1 C5 C4 156.6(2) . . . . ? C1 N1 C5 C4 -69.6(2) . . . . ? C20 C4 C5 N1 -70.0(3) . . . . ? C3 C4 C5 N1 56.3(3) . . . . ? C5 N1 C6 C7 -163.6(2) . . . . ? C1 N1 C6 C7 64.4(3) . . . . ? N1 C6 C7 C8 -57.5(3) . . . . ? C6 C7 C8 C9 -151.0(2) . . . . ? C6 C7 C8 C13 24.1(3) . . . . ? C13 C8 C9 C10 -0.6(4) . . . . ? C7 C8 C9 C10 174.5(3) . . . . ? C8 C9 C10 C11 -2.6(4) . . . . ? C9 C10 C11 C12 2.5(4) . . . . ? C10 C11 C12 C13 0.6(4) . . . . ? C11 C12 C13 C8 -3.8(4) . . . . ? C11 C12 C13 C1 178.4(2) . . . . ? C9 C8 C13 C12 3.7(3) . . . . ? C7 C8 C13 C12 -171.4(2) . . . . ? C9 C8 C13 C1 -178.6(2) . . . . ? C7 C8 C13 C1 6.3(3) . . . . ? N1 C1 C13 C12 174.7(2) . . . . ? C2 C1 C13 C12 -68.7(3) . . . . ? N1 C1 C13 C8 -3.1(3) . . . . ? C2 C1 C13 C8 113.5(2) . . . . ? C2 C3 C14 C19 136.2(2) . . . . ? C4 C3 C14 C19 -97.1(2) . . . . ? C2 C3 C14 C15 -43.9(3) . . . . ? C4 C3 C14 C15 82.8(3) . . . . ? C19 C14 C15 C16 -0.2(3) . . . . ? C3 C14 C15 C16 179.9(2) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C15 C16 C17 Br1 -178.16(17) . . . . ? C16 C17 C18 C19 -0.3(3) . . . . ? Br1 C17 C18 C19 178.48(17) . . . . ? C17 C18 C19 C14 -0.3(3) . . . . ? C15 C14 C19 C18 0.6(3) . . . . ? C3 C14 C19 C18 -179.5(2) . . . . ? _refine_diff_density_max 0.887 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.085 _shelxl_version_number 2013-4 _shelx_res_file ; TITL minor_P212121 in P2(1)2(1)2(1) CELL 0.71073 5.87380 14.11100 21.50220 90.0000 90.0000 90.0000 ZERR 4.00 0.00070 0.00170 0.00260 0.0000 0.0000 0.0000 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 N O Br UNIT 80 84 8 8 4 L.S. 12 BOND $H acta conf FMAP 2 PLAN 33 SIZE 0.10 0.20 0.24 TEMP -173.0 WGHT 0.049000 0.200000 FVAR 0.17324 MOLE 1 BR1 5 0.789633 0.075873 -0.056187 11.00000 0.03296 0.03385 = 0.01880 -0.00548 0.00124 0.00539 O1 4 1.126398 0.101568 0.233368 11.00000 0.02801 0.02826 = 0.02560 0.00042 0.00487 0.01139 O2 4 0.785341 0.061580 0.261074 11.00000 0.02999 0.01769 = 0.02879 0.00059 -0.00521 -0.00463 N1 3 0.763273 0.356489 0.312455 11.00000 0.03022 0.01607 = 0.01875 -0.00205 0.00405 0.00416 N2 3 0.931562 0.120930 0.248617 11.00000 0.02540 0.01585 = 0.01511 -0.00109 -0.00179 0.00222 C1 1 0.808847 0.255223 0.319547 11.00000 0.02028 0.01593 = 0.01563 -0.00043 0.00324 0.00069 AFIX 13 H1 2 0.666210 0.222658 0.333257 11.00000 -1.20000 AFIX 0 C2 1 0.866095 0.224020 0.252156 11.00000 0.01787 0.01171 = 0.01540 -0.00075 0.00098 0.00114 AFIX 13 H2 2 0.995507 0.263303 0.236390 11.00000 -1.20000 AFIX 0 C3 1 0.660198 0.238027 0.209261 11.00000 0.01526 0.01752 = 0.01667 0.00132 0.00156 0.00096 AFIX 13 H3 2 0.533141 0.199954 0.227535 11.00000 -1.20000 AFIX 0 C4 1 0.581426 0.343333 0.210747 11.00000 0.02211 0.02178 = 0.02171 0.00261 0.00241 0.00603 AFIX 13 H4 2 0.428659 0.346795 0.190346 11.00000 -1.20000 AFIX 0 C5 1 0.551808 0.372543 0.278809 11.00000 0.03213 0.02283 = 0.02361 0.00260 0.00694 0.01183 AFIX 23 H5A 2 0.509837 0.440396 0.281163 11.00000 -1.20000 H5B 2 0.427834 0.335042 0.297973 11.00000 -1.20000 AFIX 0 C6 1 0.795366 0.412674 0.368493 11.00000 0.03867 0.01794 = 0.02277 -0.00580 0.01042 -0.00051 AFIX 23 H6A 2 0.700601 0.386953 0.402622 11.00000 -1.20000 H6B 2 0.748610 0.479052 0.360802 11.00000 -1.20000 AFIX 0 C7 1 1.043674 0.409220 0.386489 11.00000 0.03988 0.02518 = 0.02485 -0.00911 0.00956 -0.01291 AFIX 23 H7A 2 1.137063 0.438662 0.353388 11.00000 -1.20000 H7B 2 1.067666 0.445380 0.425397 11.00000 -1.20000 AFIX 0 C8 1 1.115897 0.308101 0.395746 11.00000 0.02506 0.02981 = 0.01538 -0.00619 0.00732 -0.00773 C9 1 1.290138 0.284863 0.437214 11.00000 0.02657 0.05454 = 0.01762 -0.01071 0.00304 -0.01167 AFIX 43 H9 2 1.372620 0.334258 0.457053 11.00000 -1.20000 AFIX 0 C10 1 1.345623 0.191366 0.450122 11.00000 0.02906 0.06671 = 0.01718 -0.00364 -0.00349 0.00769 AFIX 43 H10 2 1.468768 0.176980 0.477164 11.00000 -1.20000 AFIX 0 C11 1 1.219861 0.119196 0.423230 11.00000 0.04053 0.04234 = 0.01848 -0.00134 -0.00511 0.01275 AFIX 43 H11 2 1.252396 0.054966 0.433041 11.00000 -1.20000 AFIX 0 C12 1 1.046412 0.140964 0.381963 11.00000 0.03259 0.02664 = 0.01559 -0.00004 -0.00267 0.00493 AFIX 43 H12 2 0.959763 0.091144 0.363997 11.00000 -1.20000 AFIX 0 C13 1 0.996373 0.234949 0.366229 11.00000 0.02154 0.02222 = 0.01257 -0.00105 0.00189 -0.00127 C14 1 0.697115 0.200481 0.143911 11.00000 0.01597 0.01691 = 0.01633 0.00272 -0.00036 -0.00020 C15 1 0.898125 0.215474 0.110593 11.00000 0.01625 0.02291 = 0.01990 0.00121 0.00124 -0.00306 AFIX 43 H15 2 1.018081 0.250704 0.129132 11.00000 -1.20000 AFIX 0 C16 1 0.925786 0.179797 0.050839 11.00000 0.01791 0.02431 = 0.01856 0.00406 0.00305 -0.00024 AFIX 43 H16 2 1.062810 0.190704 0.028485 11.00000 -1.20000 AFIX 0 C17 1 0.750039 0.127995 0.024363 11.00000 0.02379 0.01901 = 0.01470 0.00097 -0.00032 0.00478 C18 1 0.547982 0.112045 0.055877 11.00000 0.02062 0.02229 = 0.02156 -0.00059 -0.00179 -0.00175 AFIX 43 H18 2 0.428542 0.076727 0.037163 11.00000 -1.20000 AFIX 0 C19 1 0.523718 0.148884 0.115557 11.00000 0.01606 0.02223 = 0.01909 0.00185 0.00104 0.00016 AFIX 43 H19 2 0.385501 0.138578 0.137480 11.00000 -1.20000 AFIX 0 C20 1 0.739632 0.412192 0.176753 11.00000 0.03440 0.01901 = 0.02189 0.00376 0.00110 0.00174 AFIX 137 H20A 2 0.677614 0.476526 0.179531 11.00000 -1.50000 H20B 2 0.751773 0.393621 0.132961 11.00000 -1.50000 H20C 2 0.890820 0.410525 0.195997 11.00000 -1.50000 AFIX 0 HKLF 4 REM minor_P212121 in P2(1)2(1)2(1) REM R1 = 0.0352 for 5782 Fo > 4sig(Fo) and 0.0420 for all 6480 data REM 227 parameters refined using 0 restraints END WGHT 0.0486 0.0000 REM Highest difference peak 0.887, deepest hole -0.229, 1-sigma level 0.085 Q1 1 0.9246 0.0746 -0.0531 11.00000 0.05 0.89 Q2 1 0.6654 0.0743 -0.0509 11.00000 0.05 0.84 Q3 1 0.7930 0.0697 -0.0846 11.00000 0.05 0.77 Q4 1 0.8345 0.0224 -0.0556 11.00000 0.05 0.73 Q5 1 0.7916 0.0763 -0.0204 11.00000 0.05 0.71 Q6 1 0.8648 0.1206 -0.0561 11.00000 0.05 0.70 Q7 1 0.9284 0.4206 0.3748 11.00000 0.05 0.42 Q8 1 1.0775 0.3567 0.3880 11.00000 0.05 0.41 Q9 1 1.2320 0.1637 0.4388 11.00000 0.05 0.40 Q10 1 0.6607 0.3628 0.2908 11.00000 0.05 0.40 Q11 1 0.7870 0.2228 0.2234 11.00000 0.05 0.39 Q12 1 0.5716 0.3534 0.2467 11.00000 0.05 0.39 Q13 1 0.7872 0.2175 0.1195 11.00000 0.05 0.38 Q14 1 1.0670 0.2758 0.3736 11.00000 0.05 0.38 Q15 1 0.6135 0.1817 0.1271 11.00000 0.05 0.38 Q16 1 0.7566 0.2379 0.2385 11.00000 0.05 0.37 Q17 1 0.8881 0.1796 0.2492 11.00000 0.05 0.36 Q18 1 1.2536 0.2258 0.4508 11.00000 0.05 0.36 Q19 1 0.6729 0.1020 0.0432 11.00000 0.05 0.35 Q20 1 1.3245 0.2373 0.4512 11.00000 0.05 0.34 Q21 1 1.1370 0.1373 0.4042 11.00000 0.05 0.34 Q22 1 0.6462 0.1359 0.0363 11.00000 0.05 0.34 Q23 1 0.8310 0.2355 0.2867 11.00000 0.05 0.34 Q24 1 0.8853 0.2065 0.0778 11.00000 0.05 0.33 Q25 1 1.2439 0.2977 0.4030 11.00000 0.05 0.32 Q26 1 0.6893 0.2184 0.1771 11.00000 0.05 0.32 Q27 1 0.7932 0.3103 0.3197 11.00000 0.05 0.32 Q28 1 0.5364 0.1240 0.0870 11.00000 0.05 0.32 Q29 1 0.8803 0.0825 0.2610 11.00000 0.05 0.31 Q30 1 1.0115 0.1939 0.3805 11.00000 0.05 0.31 Q31 1 0.8506 0.1428 0.0415 11.00000 0.05 0.31 Q32 1 0.6386 0.3811 0.1910 11.00000 0.05 0.30 Q33 1 0.9861 0.2349 0.2468 11.00000 0.05 0.30 ; _shelx_res_checksum 30585 _shelx_hkl_file ; 1 0 0 0.21 0.12 1 0 0 -0.11 0.08 1 0 0 -0.07 0.08 -2 0 0 400.42 14.34 2 0 0 425.18 15.60 2 0 0 444.50 14.83 3 0 0 0.19 0.16 -3 0 0 -0.07 0.16 3 0 0 0.47 0.21 4 0 0 82.70 3.09 -4 0 0 82.53 2.97 4 0 0 80.86 3.34 -5 0 0 -0.10 0.27 5 0 0 -0.02 0.26 5 0 0 0.16 0.35 6 0 0 9.46 0.96 -6 0 0 7.10 0.60 6 0 0 5.90 0.65 7 0 0 0.15 0.63 7 0 0 -0.53 0.40 8 0 0 3.04 0.88 1 1 0 230.94 8.13 -1 -1 0 230.51 7.86 1 -1 0 234.72 8.12 1 -1 0 235.64 8.53 1 1 0 225.93 8.54 2 1 0 20.15 0.89 2 1 0 18.87 0.80 2 -1 0 20.21 0.78 2 -1 0 18.13 0.87 2 -1 0 19.23 0.77 -2 -1 0 19.49 0.74 3 1 0 41.43 1.58 -3 1 0 40.15 1.52 3 -1 0 40.24 1.71 -3 -1 0 41.08 1.47 3 1 0 36.85 1.71 3 -1 0 38.92 1.54 4 -1 0 58.53 2.33 4 1 0 60.60 2.36 4 1 0 63.54 2.59 -4 1 0 61.21 2.27 -4 -1 0 60.74 2.23 4 -1 0 60.66 2.56 5 1 0 15.13 1.05 -5 -1 0 15.64 0.78 5 -1 0 16.61 1.05 5 1 0 15.50 0.88 -5 1 0 15.63 0.84 5 -1 0 14.43 0.82 6 -1 0 4.18 0.52 6 1 0 4.08 0.55 6 1 0 5.10 0.76 -6 1 0 3.80 0.50 6 -1 0 3.95 0.73 7 1 0 3.34 0.76 7 1 0 1.81 0.58 7 -1 0 2.77 0.72 8 -1 0 10.12 1.21 -8 -1 0 9.00 1.18 0 -2 0 188.69 6.40 0 2 0 184.19 6.61 0 -2 0 189.48 6.95 1 2 0 179.00 6.42 1 -2 0 187.85 6.73 -1 -2 0 179.81 6.74 -1 2 0 181.25 6.39 2 -2 0 133.35 5.59 2 -2 0 163.06 5.30 2 2 0 144.93 5.62 -2 -2 0 151.47 5.08 2 -2 0 147.03 5.15 2 2 0 154.07 5.33 3 2 0 86.30 3.12 3 -2 0 68.41 3.29 3 -2 0 87.93 3.08 -3 -2 0 89.93 2.94 3 -2 0 86.13 3.02 4 2 0 45.45 2.04 -4 -2 0 47.31 1.69 4 -2 0 45.84 1.80 -4 2 0 44.42 1.78 4 2 0 44.48 1.84 4 -2 0 44.44 2.00 5 2 0 13.63 0.77 5 -2 0 13.07 0.74 5 -2 0 11.16 0.89 -5 -2 0 10.95 0.63 -5 2 0 11.61 0.73 5 2 0 11.26 0.94 -6 2 0 5.71 0.59 6 2 0 6.90 0.85 6 -2 0 5.81 0.60 6 -2 0 5.41 0.78 6 2 0 5.96 0.68 7 2 0 28.28 1.52 7 -2 0 27.98 1.71 8 -2 0 0.68 0.70 -8 -2 0 0.87 0.77 0 -3 0 -0.30 0.13 0 -3 0 -0.57 0.10 0 3 0 -0.30 0.11 -1 3 0 1.77 0.17 -1 -3 0 2.23 0.27 1 -3 0 1.63 0.20 1 -3 0 2.15 0.23 1 3 0 1.63 0.20 -2 -3 0 0.98 0.09 2 -3 0 1.17 0.16 2 -3 0 0.93 0.20 -2 -3 0 1.70 0.26 2 3 0 1.02 0.21 2 -3 0 0.90 0.19 -3 -3 0 30.29 1.12 3 -3 0 31.67 1.24 3 3 0 30.39 1.29 3 -3 0 31.49 1.24 3 -3 0 30.72 1.39 -4 3 0 158.09 5.34 4 -3 0 139.91 5.82 4 -3 0 147.80 5.44 -4 -3 0 153.17 5.18 4 3 0 146.19 5.86 4 3 0 154.65 5.51 5 -3 0 0.07 0.38 5 3 0 -0.03 0.29 5 -3 0 0.23 0.28 -5 3 0 -0.01 0.32 -6 3 0 31.45 1.53 -6 -3 0 35.09 1.88 6 3 0 35.21 1.65 6 -3 0 34.95 1.85 7 3 0 -0.41 0.48 -7 3 0 -0.76 0.41 7 -3 0 0.02 0.61 -7 -3 0 -0.36 0.63 -8 -3 0 10.00 1.17 8 -3 0 9.88 1.19 0 4 0 778.97 27.40 0 -4 0 795.18 26.52 0 -4 0 781.99 28.76 1 -4 0 0.18 0.14 -1 -4 0 0.12 0.17 1 4 0 -0.04 0.14 1 -4 0 0.26 0.15 -1 4 0 0.51 0.12 -1 -4 0 0.14 0.07 2 -4 0 0.97 0.22 -2 4 0 0.96 0.15 -2 -4 0 0.84 0.23 2 -4 0 1.00 0.21 2 4 0 1.18 0.21 3 -4 0 190.34 7.35 -3 -4 0 194.26 6.61 -3 -4 0 198.42 7.40 3 4 0 195.66 7.00 -4 -4 0 31.76 1.56 4 -4 0 30.64 1.34 -4 -4 0 32.96 1.17 4 4 0 30.57 1.39 4 -4 0 30.14 1.52 -4 4 0 33.78 1.40 -5 4 0 94.18 3.47 5 -4 0 90.42 3.48 5 4 0 91.55 3.57 5 -4 0 87.98 3.82 -5 -4 0 96.82 3.89 6 4 0 21.86 1.26 -6 4 0 22.82 1.20 6 -4 0 20.59 1.38 -6 -4 0 21.86 1.46 -7 4 0 6.94 0.78 7 4 0 7.93 0.88 -7 -4 0 7.42 1.03 7 -4 0 8.55 0.97 8 4 0 1.73 0.69 8 -4 0 1.31 0.73 -8 -4 0 0.29 0.72 0 -5 0 -0.05 0.13 0 5 0 -0.14 0.10 0 -5 0 -0.14 0.10 -1 -5 0 3.17 0.32 1 5 0 3.22 0.28 -1 -5 0 3.76 0.20 1 -5 0 3.17 0.27 1 -5 0 3.39 0.31 -1 5 0 3.05 0.24 -2 -5 0 96.82 3.76 2 -5 0 93.87 3.43 -2 5 0 98.19 3.46 2 5 0 96.37 3.55 2 -5 0 95.45 3.72 3 -5 0 37.46 1.50 -3 -5 0 34.69 1.65 3 -5 0 35.55 1.63 -3 5 0 38.00 1.43 3 5 0 37.74 1.55 4 5 0 26.90 1.26 -4 -5 0 27.33 1.39 4 -5 0 25.71 1.33 -5 5 0 11.14 0.77 -5 -5 0 10.89 0.93 5 -5 0 9.94 0.85 5 5 0 10.42 0.76 -6 5 0 35.43 1.66 -6 -5 0 35.79 1.93 6 -5 0 35.18 1.89 6 5 0 34.28 1.72 -7 -5 0 5.29 0.93 -7 5 0 5.39 0.74 7 -5 0 6.33 0.92 7 5 0 6.46 0.80 -8 -5 0 4.52 0.95 8 -5 0 5.35 0.98 8 5 0 5.54 0.87 0 6 0 740.31 26.11 0 -6 0 754.84 27.43 0 -6 0 746.15 25.27 1 -6 0 3.10 0.34 1 6 0 3.30 0.31 -1 -6 0 3.61 0.22 -1 -6 0 2.83 0.35 -1 6 0 2.82 0.26 1 -6 0 3.12 0.31 -2 -6 0 302.54 11.06 2 6 0 297.51 10.51 2 -6 0 289.29 11.01 2 -6 0 296.12 10.18 -2 6 0 293.89 10.40 3 -6 0 0.31 0.24 3 6 0 0.32 0.26 -3 6 0 0.48 0.19 -3 -6 0 -0.15 0.29 3 -6 0 0.59 0.28 -4 6 0 30.93 1.24 -4 -6 0 27.61 1.53 4 6 0 30.18 1.38 4 -6 0 29.22 1.48 -5 6 0 7.62 0.74 5 -6 0 7.30 0.82 5 6 0 7.71 0.74 -5 -6 0 8.18 0.91 6 6 0 4.08 0.66 -6 -6 0 3.35 0.75 -6 6 0 3.63 0.63 6 -6 0 4.71 0.77 7 -6 0 1.58 0.65 -7 -6 0 1.60 0.72 7 6 0 1.48 0.60 -7 6 0 1.58 0.63 8 6 0 -0.60 0.60 -8 -6 0 0.56 0.78 -8 6 0 0.99 0.62 8 -6 0 0.22 0.72 0 -7 0 0.46 0.23 0 7 0 -0.03 0.17 0 -7 0 0.13 0.15 -1 -7 0 520.89 19.46 1 -7 0 536.37 17.93 -1 7 0 523.46 18.46 1 -7 0 511.05 19.44 1 7 0 542.28 18.53 -1 -7 0 527.17 17.84 2 7 0 0.31 0.23 -2 -7 0 0.59 0.28 2 -7 0 1.27 0.28 -2 -7 0 0.69 0.11 2 -7 0 0.62 0.25 -2 7 0 0.90 0.19 3 7 0 46.77 2.00 -3 -7 0 46.80 2.13 3 -7 0 51.15 2.11 3 -7 0 47.50 1.94 -3 7 0 49.76 1.85 -4 -7 0 6.26 0.67 4 7 0 6.32 0.59 4 -7 0 5.04 0.57 -4 7 0 6.47 0.46 5 7 0 6.74 0.66 -5 7 0 5.21 0.63 5 -7 0 5.16 0.70 -5 -7 0 6.57 0.82 6 7 0 0.78 0.51 -6 7 0 0.78 0.49 -6 -7 0 0.17 0.54 6 -7 0 1.24 0.60 -7 7 0 0.02 0.57 7 -7 0 0.76 0.65 -7 -7 0 0.20 0.70 7 7 0 0.87 0.59 8 7 0 2.23 0.74 -8 7 0 0.72 0.65 -8 -7 0 2.19 0.90 8 -7 0 2.52 0.83 0 -8 0 20.66 1.04 0 8 0 21.24 0.94 0 -8 0 20.32 0.88 -1 -8 0 2.57 0.38 -1 8 0 2.81 0.30 -1 -8 0 2.40 0.24 1 -8 0 2.75 0.38 1 -8 0 2.19 0.31 1 8 0 1.88 0.32 2 -8 0 116.92 4.15 -2 -8 0 112.52 4.53 2 -8 0 115.30 4.49 2 8 0 117.72 4.30 -2 8 0 113.09 4.16 3 -8 0 24.37 1.21 3 -8 0 27.05 1.30 3 8 0 26.39 1.26 -3 -8 0 27.37 1.37 -3 8 0 24.90 1.07 -4 -8 0 1.56 0.51 4 -8 0 1.74 0.46 4 8 0 2.85 0.51 -5 8 0 11.95 0.92 5 8 0 11.43 0.86 -5 -8 0 11.24 1.00 5 -8 0 9.64 0.93 -6 -8 0 2.13 0.73 6 8 0 2.22 0.60 -6 8 0 1.37 0.59 6 -8 0 0.67 0.60 -7 -8 0 0.71 0.75 -7 8 0 0.70 0.60 7 -8 0 0.49 0.62 7 8 0 -0.06 0.57 8 -8 0 2.09 0.78 -8 8 0 -0.43 0.61 -8 -8 0 0.57 0.82 8 8 0 0.89 0.68 0 9 0 0.19 0.23 0 -9 0 -0.01 0.25 0 -9 0 -0.25 0.19 -1 9 0 16.13 0.77 1 9 0 15.49 0.83 -1 -9 0 16.51 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