data_ic18876 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18 Br N3 O5' _chemical_formula_weight 460.28 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' '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' 'Br' 'Br' -0.6763 1.2805 '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 5.88470(10) _cell_length_b 10.0526(2) _cell_length_c 31.9302(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1888.88(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 75.04 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_F_000 936 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.271 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.081 _exptl_absorpt_coefficient_mu 3.314 _shelx_estimated_absorpt_T_min 0.467 _shelx_estimated_absorpt_T_max 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5660 _exptl_absorpt_correction_T_max 0.7539 _exptl_absorpt_process_details 'SADABS (Bruker, 2016)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10463 _diffrn_reflns_av_unetI/netI 0.0238 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.768 _diffrn_reflns_theta_max 74.982 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 3864 _reflns_number_gt 3832 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.698 _reflns_Friedel_fraction_max 0.983 _reflns_Friedel_fraction_full 0.992 _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 APEX3' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _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^)+(0.0282P)^2^+0.4775P] 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 1548 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.030(5) _chemical_absolute_configuration 'ad' _refine_ls_number_reflns 3864 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.003 _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 1.17364(5) 0.50834(3) 0.98409(2) 0.03705(9) Uani 1 1 d . . . . . O1 O 0.4396(4) 1.07283(19) 0.81275(7) 0.0420(5) Uani 1 1 d . . . . . O2 O 1.0268(4) 0.8558(3) 0.67813(6) 0.0493(5) Uani 1 1 d . . . . . O3 O 1.1953(4) 0.7789(2) 0.73290(6) 0.0420(5) Uani 1 1 d . . . . . O4 O 0.6517(4) 0.56412(18) 0.78194(7) 0.0446(5) Uani 1 1 d . . . . . O5 O 0.3590(4) 0.6101(2) 0.81936(8) 0.0511(6) Uani 1 1 d . . . . . N1 N 0.6132(4) 1.1665(2) 0.87002(7) 0.0294(4) Uani 1 1 d . . . . . N2 N 1.0288(4) 0.8208(2) 0.71491(6) 0.0290(4) Uani 1 1 d . . . . . N3 N 0.5361(4) 0.6406(2) 0.80200(7) 0.0297(4) Uani 1 1 d . . . . . C1 C 0.5847(4) 1.0723(2) 0.83981(8) 0.0284(5) Uani 1 1 d . . . . . C2 C 0.7633(4) 0.9625(2) 0.84665(7) 0.0241(5) Uani 1 1 d . . . . . C3 C 0.8904(4) 1.0142(2) 0.88429(7) 0.0248(4) Uani 1 1 d . . . . . C4 C 1.0760(4) 0.9645(3) 0.90557(9) 0.0334(5) Uani 1 1 d . . . . . H4 H 1.1440 0.8829 0.8974 0.040 Uiso 1 1 calc R U . . . C5 C 1.1624(5) 1.0369(3) 0.93957(9) 0.0421(7) Uani 1 1 d . . . . . H5 H 1.2897 1.0039 0.9546 0.050 Uiso 1 1 calc R U . . . C6 C 1.0638(6) 1.1556(3) 0.95126(9) 0.0432(7) Uani 1 1 d . . . . . H6 H 1.1241 1.2031 0.9745 0.052 Uiso 1 1 calc R U . . . C7 C 0.8778(5) 1.2075(3) 0.92981(8) 0.0362(6) Uani 1 1 d . . . . . H7 H 0.8105 1.2895 0.9379 0.043 Uiso 1 1 calc R U . . . C8 C 0.7951(4) 1.1355(2) 0.89641(7) 0.0258(5) Uani 1 1 d . . . . . C9 C 0.9124(5) 0.9439(3) 0.80656(9) 0.0390(6) Uani 1 1 d . . . . . H9A H 0.8943 1.0212 0.7877 0.047 Uiso 1 1 calc R U . . . H9B H 1.0747 0.9363 0.8143 0.047 Uiso 1 1 calc R U . . . C10 C 0.8323(4) 0.8157(2) 0.78452(7) 0.0238(4) Uani 1 1 d . . . . . H10 H 0.9431 0.7429 0.7907 0.029 Uiso 1 1 calc R U . . . C11 C 0.6083(4) 0.7839(2) 0.80605(7) 0.0238(4) Uani 1 1 d . . . . . H11 H 0.4879 0.8401 0.7928 0.029 Uiso 1 1 calc R U . . . C12 C 0.6306(4) 0.8270(2) 0.85210(7) 0.0234(4) Uani 1 1 d . . . . . H12 H 0.4754 0.8472 0.8631 0.028 Uiso 1 1 calc R U . . . C13 C 0.7469(4) 0.7317(2) 0.88222(7) 0.0240(5) Uani 1 1 d . . . . . C14 C 0.9195(5) 0.6456(3) 0.87116(8) 0.0328(6) Uani 1 1 d . . . . . H14 H 0.9550 0.6334 0.8424 0.039 Uiso 1 1 calc R U . . . C15 C 1.0429(5) 0.5760(3) 0.90132(8) 0.0343(6) Uani 1 1 d . . . . . H15 H 1.1628 0.5181 0.8933 0.041 Uiso 1 1 calc R U . . . C16 C 0.9881(5) 0.5927(2) 0.94288(7) 0.0289(5) Uani 1 1 d . . . . . C17 C 0.8082(5) 0.6715(3) 0.95485(8) 0.0376(6) Uani 1 1 d . . . . . H17 H 0.7672 0.6788 0.9835 0.045 Uiso 1 1 calc R U . . . C18 C 0.6884(5) 0.7397(3) 0.92449(8) 0.0330(5) Uani 1 1 d . . . . . H18 H 0.5630 0.7934 0.9326 0.040 Uiso 1 1 calc R U . . . C19 C 0.4796(6) 1.2874(3) 0.87294(11) 0.0435(7) Uani 1 1 d . . . . . H19A H 0.5691 1.3626 0.8625 0.065 Uiso 1 1 calc R U . . . H19B H 0.4380 1.3033 0.9022 0.065 Uiso 1 1 calc R U . . . H19C H 0.3415 1.2780 0.8561 0.065 Uiso 1 1 calc R U . . . C20 C 0.8050(4) 0.8272(2) 0.73743(7) 0.0274(5) Uani 1 1 d . . . . . H20A H 0.7061 0.7543 0.7273 0.033 Uiso 1 1 calc R U . . . H20B H 0.7293 0.9126 0.7307 0.033 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 0.04637(16) 0.03686(14) 0.02792(13) 0.00108(11) -0.00563(10) 0.00798(13) O1 0.0416(11) 0.0340(10) 0.0502(12) 0.0072(9) -0.0222(9) -0.0041(9) O2 0.0488(13) 0.0706(15) 0.0284(10) 0.0054(10) 0.0075(9) -0.0095(12) O3 0.0300(9) 0.0536(12) 0.0424(11) 0.0055(9) 0.0052(9) 0.0097(10) O4 0.0565(13) 0.0279(9) 0.0495(11) -0.0095(8) 0.0065(11) -0.0002(10) O5 0.0425(13) 0.0430(11) 0.0679(15) -0.0066(10) 0.0149(11) -0.0196(10) N1 0.0286(11) 0.0225(9) 0.0371(11) 0.0012(8) -0.0033(9) 0.0033(8) N2 0.0322(11) 0.0287(10) 0.0260(10) -0.0031(8) 0.0036(9) -0.0034(9) N3 0.0309(11) 0.0275(10) 0.0306(10) -0.0007(8) -0.0036(9) -0.0051(9) C1 0.0276(12) 0.0248(11) 0.0327(12) 0.0045(10) -0.0045(10) -0.0039(10) C2 0.0228(10) 0.0246(10) 0.0248(10) -0.0022(8) 0.0010(8) -0.0017(8) C3 0.0229(10) 0.0249(10) 0.0266(10) 0.0002(9) -0.0001(8) -0.0016(9) C4 0.0255(12) 0.0312(12) 0.0433(14) 0.0016(10) -0.0045(10) 0.0007(10) C5 0.0378(14) 0.0450(14) 0.0434(14) 0.0086(12) -0.0191(12) -0.0092(13) C6 0.0589(19) 0.0412(14) 0.0296(13) 0.0011(11) -0.0154(13) -0.0195(14) C7 0.0493(17) 0.0284(11) 0.0308(12) -0.0036(10) 0.0001(12) -0.0055(11) C8 0.0266(12) 0.0255(10) 0.0253(11) 0.0016(8) 0.0009(9) -0.0012(10) C9 0.0383(14) 0.0428(15) 0.0361(14) -0.0137(12) 0.0138(12) -0.0178(12) C10 0.0212(10) 0.0265(10) 0.0237(10) -0.0013(8) -0.0003(9) -0.0013(10) C11 0.0211(10) 0.0217(10) 0.0287(11) -0.0011(9) -0.0003(9) -0.0010(8) C12 0.0188(11) 0.0250(10) 0.0263(11) -0.0013(9) 0.0011(9) 0.0001(9) C13 0.0241(11) 0.0238(10) 0.0239(11) -0.0007(9) 0.0011(8) -0.0013(8) C14 0.0413(14) 0.0340(12) 0.0232(11) 0.0003(10) 0.0051(10) 0.0126(11) C15 0.0415(15) 0.0324(12) 0.0291(12) -0.0003(10) 0.0057(11) 0.0141(12) C16 0.0367(13) 0.0251(10) 0.0250(11) 0.0012(9) -0.0042(10) 0.0015(10) C17 0.0450(15) 0.0450(14) 0.0229(11) 0.0009(10) 0.0062(11) 0.0091(14) C18 0.0314(13) 0.0383(12) 0.0292(12) -0.0012(10) 0.0074(10) 0.0092(12) C19 0.0404(15) 0.0286(12) 0.0615(19) 0.0015(12) 0.0001(14) 0.0106(12) C20 0.0245(11) 0.0320(11) 0.0258(11) 0.0019(9) -0.0009(9) 0.0001(10) _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 C16 1.909(2) . ? O1 C1 1.215(3) . ? O2 N2 1.226(3) . ? O3 N2 1.211(3) . ? O4 N3 1.210(3) . ? O5 N3 1.220(3) . ? N1 C1 1.362(3) . ? N1 C8 1.397(3) . ? N1 C19 1.450(3) . ? N2 C20 1.502(3) . ? N3 C11 1.507(3) . ? C1 C2 1.540(3) . ? C2 C3 1.508(3) . ? C2 C9 1.563(3) . ? C2 C12 1.579(3) . ? C3 C4 1.380(3) . ? C3 C8 1.398(3) . ? C4 C5 1.402(4) . ? C5 C6 1.379(5) . ? C6 C7 1.392(4) . ? C7 C8 1.378(4) . ? C9 C10 1.542(3) . ? C10 C20 1.517(3) . ? C10 C11 1.520(3) . ? C11 C12 1.539(3) . ? C12 C13 1.520(3) . ? C13 C14 1.381(3) . ? C13 C18 1.395(3) . ? C14 C15 1.394(4) . ? C15 C16 1.376(3) . ? C16 C17 1.376(4) . ? C17 C18 1.381(4) . ? 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 C1 N1 C8 111.5(2) . . ? C1 N1 C19 124.1(2) . . ? C8 N1 C19 124.3(2) . . ? O3 N2 O2 124.2(2) . . ? O3 N2 C20 119.8(2) . . ? O2 N2 C20 116.0(2) . . ? O4 N3 O5 124.1(2) . . ? O4 N3 C11 119.6(2) . . ? O5 N3 C11 116.2(2) . . ? O1 C1 N1 126.0(2) . . ? O1 C1 C2 125.7(2) . . ? N1 C1 C2 108.3(2) . . ? C3 C2 C1 101.81(18) . . ? C3 C2 C9 114.6(2) . . ? C1 C2 C9 110.6(2) . . ? C3 C2 C12 117.02(19) . . ? C1 C2 C12 107.24(19) . . ? C9 C2 C12 105.33(18) . . ? C4 C3 C8 119.8(2) . . ? C4 C3 C2 131.3(2) . . ? C8 C3 C2 108.81(19) . . ? C3 C4 C5 118.7(2) . . ? C6 C5 C4 120.4(3) . . ? C5 C6 C7 121.4(3) . . ? C8 C7 C6 117.5(3) . . ? C7 C8 N1 128.4(2) . . ? C7 C8 C3 122.1(2) . . ? N1 C8 C3 109.6(2) . . ? C10 C9 C2 107.6(2) . . ? C20 C10 C11 111.9(2) . . ? C20 C10 C9 114.9(2) . . ? C11 C10 C9 103.54(19) . . ? N3 C11 C10 113.97(19) . . ? N3 C11 C12 112.05(19) . . ? C10 C11 C12 107.38(18) . . ? C13 C12 C11 117.72(19) . . ? C13 C12 C2 113.01(18) . . ? C11 C12 C2 100.37(17) . . ? C14 C13 C18 117.7(2) . . ? C14 C13 C12 124.4(2) . . ? C18 C13 C12 117.7(2) . . ? C13 C14 C15 121.4(2) . . ? C16 C15 C14 118.9(2) . . ? C15 C16 C17 121.2(2) . . ? C15 C16 Br1 118.5(2) . . ? C17 C16 Br1 120.28(19) . . ? C16 C17 C18 118.9(2) . . ? C17 C18 C13 121.6(2) . . ? N2 C20 C10 112.2(2) . . ? _refine_diff_density_max 0.414 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.043 _shelx_res_file ; ic18876.res created by SHELXL-2014/7 TITL ic18876 in P2(1)2(1)2(1) CELL 1.54178 5.88470 10.05260 31.93020 90.0000 90.0000 90.0000 ZERR 4.00 0.00010 0.00020 0.00070 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 72 12 20 4 OMIT -3 150 OMIT 1 0 3 L.S. 10 ACTA BOND FMAP 2 PLAN 20 SIZE 0.081 0.095 0.271 TEMP -73.160 WGHT 0.028200 0.477500 FVAR 0.25053 BR1 5 1.173644 0.508337 0.984088 11.00000 0.04637 0.03686 = 0.02792 0.00108 -0.00563 0.00798 O1 4 0.439568 1.072827 0.812748 11.00000 0.04163 0.03404 = 0.05022 0.00719 -0.02216 -0.00405 O2 4 1.026812 0.855757 0.678134 11.00000 0.04884 0.07061 = 0.02839 0.00540 0.00752 -0.00950 O3 4 1.195308 0.778949 0.732897 11.00000 0.03002 0.05360 = 0.04243 0.00547 0.00525 0.00972 O4 4 0.651727 0.564116 0.781942 11.00000 0.05648 0.02787 = 0.04949 -0.00953 0.00654 -0.00016 O5 4 0.359039 0.610067 0.819357 11.00000 0.04251 0.04300 = 0.06793 -0.00660 0.01488 -0.01958 N1 3 0.613196 1.166484 0.870021 11.00000 0.02865 0.02247 = 0.03714 0.00117 -0.00334 0.00331 N2 3 1.028820 0.820844 0.714910 11.00000 0.03218 0.02872 = 0.02602 -0.00311 0.00356 -0.00338 N3 3 0.536128 0.640587 0.801996 11.00000 0.03092 0.02753 = 0.03057 -0.00072 -0.00364 -0.00506 C1 1 0.584651 1.072349 0.839807 11.00000 0.02765 0.02475 = 0.03266 0.00450 -0.00453 -0.00393 C2 1 0.763302 0.962501 0.846654 11.00000 0.02282 0.02457 = 0.02484 -0.00218 0.00096 -0.00165 C3 1 0.890376 1.014166 0.884289 11.00000 0.02287 0.02485 = 0.02664 0.00021 -0.00015 -0.00158 C4 1 1.076011 0.964506 0.905572 11.00000 0.02553 0.03121 = 0.04331 0.00161 -0.00453 0.00073 AFIX 43 H4 2 1.143963 0.882855 0.897353 11.00000 -1.20000 AFIX 0 C5 1 1.162388 1.036911 0.939566 11.00000 0.03779 0.04500 = 0.04341 0.00857 -0.01913 -0.00923 AFIX 43 H5 2 1.289678 1.003930 0.954634 11.00000 -1.20000 AFIX 0 C6 1 1.063823 1.155632 0.951265 11.00000 0.05894 0.04120 = 0.02959 0.00106 -0.01535 -0.01946 AFIX 43 H6 2 1.124101 1.203097 0.974470 11.00000 -1.20000 AFIX 0 C7 1 0.877836 1.207504 0.929812 11.00000 0.04933 0.02838 = 0.03078 -0.00355 0.00009 -0.00552 AFIX 43 H7 2 0.810530 1.289463 0.937907 11.00000 -1.20000 AFIX 0 C8 1 0.795063 1.135541 0.896409 11.00000 0.02657 0.02551 = 0.02526 0.00157 0.00094 -0.00123 C9 1 0.912356 0.943883 0.806561 11.00000 0.03829 0.04278 = 0.03606 -0.01367 0.01383 -0.01775 AFIX 23 H9A 2 0.894288 1.021215 0.787654 11.00000 -1.20000 H9B 2 1.074690 0.936314 0.814342 11.00000 -1.20000 AFIX 0 C10 1 0.832276 0.815666 0.784518 11.00000 0.02121 0.02653 = 0.02369 -0.00125 -0.00031 -0.00126 AFIX 13 H10 2 0.943079 0.742873 0.790732 11.00000 -1.20000 AFIX 0 C11 1 0.608301 0.783882 0.806045 11.00000 0.02107 0.02166 = 0.02874 -0.00108 -0.00026 -0.00098 AFIX 13 H11 2 0.487896 0.840134 0.792825 11.00000 -1.20000 AFIX 0 C12 1 0.630645 0.827039 0.852105 11.00000 0.01878 0.02500 = 0.02632 -0.00126 0.00111 0.00009 AFIX 13 H12 2 0.475388 0.847183 0.863144 11.00000 -1.20000 AFIX 0 C13 1 0.746906 0.731701 0.882221 11.00000 0.02410 0.02384 = 0.02392 -0.00067 0.00114 -0.00130 C14 1 0.919518 0.645563 0.871163 11.00000 0.04127 0.03401 = 0.02316 0.00029 0.00513 0.01257 AFIX 43 H14 2 0.954954 0.633423 0.842389 11.00000 -1.20000 AFIX 0 C15 1 1.042890 0.576035 0.901320 11.00000 0.04148 0.03242 = 0.02905 -0.00029 0.00573 0.01408 AFIX 43 H15 2 1.162806 0.518101 0.893314 11.00000 -1.20000 AFIX 0 C16 1 0.988077 0.592722 0.942877 11.00000 0.03671 0.02507 = 0.02499 0.00121 -0.00423 0.00150 C17 1 0.808249 0.671488 0.954850 11.00000 0.04498 0.04505 = 0.02286 0.00088 0.00622 0.00906 AFIX 43 H17 2 0.767201 0.678823 0.983531 11.00000 -1.20000 AFIX 0 C18 1 0.688358 0.739726 0.924492 11.00000 0.03137 0.03833 = 0.02915 -0.00120 0.00738 0.00924 AFIX 43 H18 2 0.562995 0.793427 0.932589 11.00000 -1.20000 AFIX 0 C19 1 0.479616 1.287385 0.872936 11.00000 0.04041 0.02863 = 0.06155 0.00145 0.00013 0.01060 AFIX 137 H19A 2 0.569149 1.362603 0.862500 11.00000 -1.50000 H19B 2 0.437956 1.303265 0.902229 11.00000 -1.50000 H19C 2 0.341485 1.277974 0.856050 11.00000 -1.50000 AFIX 0 C20 1 0.805022 0.827229 0.737428 11.00000 0.02449 0.03202 = 0.02577 0.00193 -0.00089 0.00006 AFIX 23 H20A 2 0.706107 0.754302 0.727337 11.00000 -1.20000 H20B 2 0.729341 0.912572 0.730732 11.00000 -1.20000 AFIX 0 HKLF 4 REM ic18876 in P2(1)2(1)2(1) REM R1 = 0.0230 for 3832 Fo > 4sig(Fo) and 0.0232 for all 3864 data REM 263 parameters refined using 0 restraints END WGHT 0.0281 0.4762 REM Highest difference peak 0.414, deepest hole -0.293, 1-sigma level 0.043 Q1 1 1.3125 0.5027 0.9764 11.00000 0.05 0.41 Q2 1 0.8502 0.9807 0.8657 11.00000 0.05 0.22 Q3 1 1.1698 0.5869 0.9935 11.00000 0.05 0.22 Q4 1 1.0222 0.5050 0.9781 11.00000 0.05 0.21 Q5 1 1.0102 1.0008 0.7977 11.00000 0.05 0.21 Q6 1 0.7368 0.7884 0.7977 11.00000 0.05 0.20 Q7 1 0.7043 0.7746 0.8665 11.00000 0.05 0.18 Q8 1 0.8106 1.0592 0.8981 11.00000 0.05 0.18 Q9 1 0.8773 1.0889 0.8887 11.00000 0.05 0.17 Q10 1 0.7886 0.6611 0.8762 11.00000 0.05 0.17 Q11 1 0.5687 1.0666 0.8045 11.00000 0.05 0.17 Q12 1 0.6915 0.6589 0.9361 11.00000 0.05 0.16 Q13 1 0.4620 0.7830 0.7955 11.00000 0.05 0.16 Q14 1 1.0391 0.7790 0.6848 11.00000 0.05 0.16 Q15 1 0.6918 1.0115 0.8410 11.00000 0.05 0.16 Q16 1 0.2900 0.5398 0.8020 11.00000 0.05 0.16 Q17 1 0.8194 0.5885 0.9442 11.00000 0.05 0.16 Q18 1 0.3354 1.2796 0.8819 11.00000 0.05 0.16 Q19 1 0.8362 0.9592 0.8275 11.00000 0.05 0.16 Q20 1 0.7483 1.1842 0.8749 11.00000 0.05 0.16 ; _shelx_res_checksum 47985 _shelx_hkl_file ; 0 -2 -39 1.00 0.18 1 -2 -39 10.14 0.57 0 -1 -39 6.69 0.48 1 -1 -39 0.81 0.16 -1 0 -39 2.44 0.28 0 0 -39 -0.04 0.08 1 0 -39 2.87 0.28 -1 1 -39 0.89 0.19 0 1 -39 6.50 0.47 0 2 -39 0.94 0.18 0 -3 -38 11.22 0.62 1 -3 -38 24.80 1.08 -1 -2 -38 22.86 1.08 0 -2 -38 39.83 1.78 1 -2 -38 24.03 1.11 -2 -1 -38 10.11 0.78 -1 -1 -38 15.56 1.13 0 -1 -38 33.09 1.46 1 -1 -38 15.91 0.87 2 -1 -38 9.35 0.54 -2 0 -38 4.67 0.38 -1 0 -38 6.44 0.52 0 0 -38 12.08 0.75 1 0 -38 6.27 0.48 2 0 -38 4.34 0.35 -2 1 -38 9.80 0.58 -1 1 -38 16.69 0.98 0 1 -38 29.82 1.42 1 1 -38 14.07 0.82 2 1 -38 7.25 0.45 -1 2 -38 23.28 1.12 0 2 -38 36.91 1.59 1 2 -38 23.13 1.04 -1 3 -38 24.54 1.11 0 3 -38 12.45 0.82 1 -4 -37 5.81 0.39 -1 -3 -37 4.78 0.38 0 -3 -37 7.23 0.52 1 -3 -37 5.06 0.41 2 -3 -37 7.93 0.48 -2 -2 -37 26.36 1.37 -1 -2 -37 2.14 0.27 0 -2 -37 3.51 0.37 1 -2 -37 1.45 0.25 2 -2 -37 24.98 1.15 -2 -1 -37 1.68 0.24 -1 -1 -37 5.44 0.49 0 -1 -37 0.74 0.21 1 -1 -37 5.45 0.48 2 -1 -37 1.69 0.26 -2 0 -37 21.68 1.41 -1 0 -37 11.58 0.81 0 0 -37 0.19 0.11 1 0 -37 12.13 0.77 2 0 -37 20.08 1.03 -1 1 -37 5.31 0.50 0 1 -37 0.60 0.20 1 1 -37 5.10 0.46 2 1 -37 1.99 0.23 -1 2 -37 1.41 0.25 0 2 -37 3.08 0.34 1 2 -37 1.64 0.38 -2 3 -37 7.50 0.49 -1 3 -37 5.88 0.43 0 3 -37 6.26 0.46 0 -4 -36 24.80 1.11 1 -4 -36 13.47 0.73 2 -4 -36 10.32 0.63 -1 -3 -36 32.11 1.52 0 -3 -36 28.85 1.37 1 -3 -36 28.51 1.38 2 -3 -36 7.14 0.50 -2 -2 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