# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2022 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ky409_reprocess _database_code_depnum_ccdc_archive 'CCDC 2084378' loop_ _audit_author_name _audit_author_address 'Marina Uzelac' ;University of Edinburgh United Kingdom ; _audit_update_record ; 2021-05-18 deposited with the CCDC. 2022-01-03 downloaded from the CCDC. ; _audit_creation_date 2021-02-24 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C20 H13 B Br N' _chemical_formula_sum 'C20 H13 B Br N' _chemical_formula_weight 358.03 _chemical_absolute_configuration ? _chemical_melting_point ? _chemical_oxdiff_formula 'C20 H13 B Br N' 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' B B 0.0013 0.0007 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_H-M_alt 'P c a 21' _space_group_name_Hall 'P 2c -2ac' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 22.9580(7) _cell_length_b 9.4271(3) _cell_length_c 7.0146(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1518.15(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8543 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 25.2870 _cell_measurement_theta_min 3.7160 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.704 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 720 _exptl_crystal_preparation ? _exptl_crystal_recrystallization_method ? _exptl_crystal_size_max 0.232 _exptl_crystal_size_mid 0.197 _exptl_crystal_size_min 0.11 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.931 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 31855 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.906 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.344 _diffrn_reflns_theta_min 3.404 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0521 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.931 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -87.00 20.00 1.00 17.50 -- -15.66 -16.00 -72.00 107 2 \w -52.00 56.00 1.00 17.50 -- -15.66 16.00 97.00 108 3 \w -54.00 54.00 1.00 17.50 -- 17.38 -16.00 -72.00 108 4 \w -19.00 89.00 1.00 17.50 -- 17.38 16.00 97.00 108 5 \w -83.00 1.00 1.00 17.50 -- -15.66 -57.00 90.00 84 6 \w -39.00 11.00 1.00 17.50 -- -15.66 -77.00-120.00 50 7 \w -9.00 39.00 1.00 17.50 -- 17.38 77.00-120.00 48 8 \w -9.00 39.00 1.00 17.50 -- 17.38 77.00 -90.00 48 9 \w 39.00 90.00 1.00 17.50 -- 17.38 178.00 120.00 51 10 \w -52.00 37.00 1.00 17.50 -- 17.38 -37.00 60.00 89 11 \w -9.00 39.00 1.00 17.50 -- 17.38 77.00 30.00 48 12 \w -9.00 39.00 1.00 17.50 -- 17.38 77.00 150.00 48 13 \w -20.00 56.00 1.00 17.50 -- 17.38 -99.00 -90.00 76 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0062351000 _diffrn_orient_matrix_UB_12 0.0675046000 _diffrn_orient_matrix_UB_13 0.0396748000 _diffrn_orient_matrix_UB_21 -0.0015177000 _diffrn_orient_matrix_UB_22 -0.0308001000 _diffrn_orient_matrix_UB_23 0.0921593000 _diffrn_orient_matrix_UB_31 0.0302129000 _diffrn_orient_matrix_UB_32 0.0124691000 _diffrn_orient_matrix_UB_33 0.0127897000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.804 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.876 _reflns_number_gt 3087 _reflns_number_total 3769 _reflns_odcompleteness_completeness 99.56 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.378 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.071 _refine_ls_abs_structure_details ; Flack x determined using 1186 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.011(4) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3769 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0353 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.6498P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.0679 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 2.a Aromatic/amide H refined with riding coordinates: N1(H1), C18(H18), C3(H3), C13(H13), C19(H19), C6(H6), C7(H7), C14(H14), C5(H5), C16(H16), C17(H17), C8(H8), C2(H2) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.67855(2) 0.15558(4) 0.68689(9) 0.03039(12) Uani 1 1 d . . . . . N1 N 0.61424(13) 0.4020(3) 0.8081(5) 0.0214(7) Uani 1 1 d . . . . . H1 H 0.616236 0.360547 0.917091 0.026 Uiso 1 1 calc R U . . . C10 C 0.62806(15) 0.5697(4) 0.4788(5) 0.0175(8) Uani 1 1 d . . . . . C9 C 0.65179(16) 0.6715(4) 0.3465(5) 0.0190(8) Uani 1 1 d . . . . . C18 C 0.47953(16) 0.8643(4) 0.3953(6) 0.0215(9) Uani 1 1 d . . . . . H18 H 0.471773 0.901657 0.275247 0.026 Uiso 1 1 calc R U . . . C3 C 0.69693(14) 0.4740(4) 0.1711(8) 0.0244(8) Uani 1 1 d . . . . . H3 H 0.715289 0.439283 0.062531 0.029 Uiso 1 1 calc R U . . . C20 C 0.53862(16) 0.7113(4) 0.5969(5) 0.0191(8) Uani 1 1 d . . . . . C1 C 0.64974(16) 0.4305(4) 0.4736(6) 0.0203(8) Uani 1 1 d . . . . . C4 C 0.68366(13) 0.6216(4) 0.1848(10) 0.0228(7) Uani 1 1 d . . . . . C13 C 0.54559(16) 0.5641(4) 0.9466(6) 0.0218(8) Uani 1 1 d . . . . . H13 H 0.548108 0.514590 1.060940 0.026 Uiso 1 1 calc R U . . . C12 C 0.58195(16) 0.5260(4) 0.7917(5) 0.0185(8) Uani 1 1 d . . . . . C19 C 0.52515(16) 0.7712(4) 0.4179(5) 0.0191(8) Uani 1 1 d . . . . . H19 H 0.547693 0.747223 0.312580 0.023 Uiso 1 1 calc R U . . . C6 C 0.70123(18) 0.8629(5) 0.0825(6) 0.0288(10) Uani 1 1 d . . . . . H6 H 0.715261 0.926478 -0.007810 0.035 Uiso 1 1 calc R U . . . C7 C 0.67513(16) 0.9131(5) 0.2511(6) 0.0262(10) Uani 1 1 d . . . . . H7 H 0.674478 1.009845 0.276829 0.031 Uiso 1 1 calc R U . . . C15 C 0.50076(15) 0.7449(4) 0.7513(6) 0.0199(8) Uani 1 1 d . . . . . C14 C 0.50705(17) 0.6726(4) 0.9288(6) 0.0228(9) Uani 1 1 d . . . . . H14 H 0.484644 0.699998 1.032959 0.027 Uiso 1 1 calc R U . . . C11 C 0.58447(15) 0.6060(4) 0.6247(5) 0.0160(8) Uani 1 1 d . . . . . C5 C 0.70582(17) 0.7205(5) 0.0524(6) 0.0281(10) Uani 1 1 d . . . . . H5 H 0.723947 0.687876 -0.057713 0.034 Uiso 1 1 calc R U . . . C16 C 0.45474(16) 0.8425(4) 0.7247(6) 0.0224(11) Uani 1 1 d . . . . . H16 H 0.430889 0.865812 0.827167 0.027 Uiso 1 1 calc R U . . . C17 C 0.44469(16) 0.9034(5) 0.5497(6) 0.0243(9) Uani 1 1 d . . . . . H17 H 0.415087 0.969781 0.534352 0.029 Uiso 1 1 calc R U . . . C8 C 0.65064(16) 0.8193(4) 0.3775(6) 0.0209(9) Uani 1 1 d . . . . . H8 H 0.632765 0.854213 0.486874 0.025 Uiso 1 1 calc R U . . . C2 C 0.68320(15) 0.3848(4) 0.3134(6) 0.0237(9) Uani 1 1 d . . . . . H2 H 0.695768 0.291091 0.307459 0.028 Uiso 1 1 calc R U . . . B1 B 0.64350(18) 0.3426(5) 0.6536(7) 0.0208(11) Uani 1 1 d . . . . . 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 0.0309(2) 0.02320(18) 0.0371(2) 0.0021(3) -0.0016(3) 0.00515(16) N1 0.0246(17) 0.0212(17) 0.0185(17) 0.0030(14) -0.0027(14) -0.0006(14) C10 0.0174(18) 0.023(2) 0.0118(18) -0.0032(15) -0.0049(15) -0.0012(16) C9 0.0131(18) 0.030(2) 0.0135(19) -0.0006(17) -0.0042(14) 0.0019(16) C18 0.0192(19) 0.022(2) 0.023(2) 0.0018(16) -0.0034(15) -0.0038(16) C3 0.0147(15) 0.037(2) 0.022(2) -0.005(2) -0.002(2) 0.0048(14) C20 0.0149(18) 0.0216(19) 0.021(2) -0.0028(17) 0.0001(15) -0.0039(16) C1 0.0156(18) 0.024(2) 0.021(2) -0.0045(17) -0.0026(16) -0.0003(16) C4 0.0112(14) 0.039(2) 0.0179(15) -0.005(3) -0.001(2) 0.0008(14) C13 0.026(2) 0.026(2) 0.0136(19) 0.0010(17) 0.0007(15) -0.0059(17) C12 0.0185(19) 0.019(2) 0.018(2) -0.0029(16) -0.0021(15) -0.0051(15) C19 0.0173(19) 0.022(2) 0.018(2) -0.0020(16) 0.0015(15) -0.0042(16) C6 0.019(2) 0.041(3) 0.026(2) 0.013(2) 0.0027(18) -0.002(2) C7 0.018(2) 0.029(2) 0.031(2) 0.0084(17) -0.0001(17) 0.0013(17) C15 0.0177(19) 0.0194(19) 0.023(2) -0.0043(15) 0.0012(14) -0.0062(16) C14 0.024(2) 0.029(2) 0.0153(19) -0.0045(17) 0.0039(15) -0.0039(17) C11 0.0143(17) 0.0176(18) 0.0161(19) -0.0027(14) -0.0014(13) -0.0039(15) C5 0.018(2) 0.048(3) 0.019(2) 0.003(2) 0.0039(16) 0.003(2) C16 0.0175(17) 0.027(2) 0.023(3) -0.0055(17) 0.0022(15) -0.0006(15) C17 0.019(2) 0.023(2) 0.031(2) -0.0045(18) 0.0006(17) 0.0015(17) C8 0.0139(19) 0.028(2) 0.021(2) 0.0035(17) -0.0017(15) 0.0017(16) C2 0.0186(19) 0.026(2) 0.026(2) -0.0066(17) -0.0022(17) 0.0014(17) B1 0.0173(18) 0.0227(19) 0.022(3) -0.005(2) -0.0052(17) 0.0007(16) _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 B1 1.952(4) . ? N1 H1 0.8600 . ? N1 C12 1.389(5) . ? N1 B1 1.392(5) . ? C10 C9 1.442(5) . ? C10 C1 1.404(5) . ? C10 C11 1.472(5) . ? C9 C4 1.429(7) . ? C9 C8 1.410(6) . ? C18 H18 0.9300 . ? C18 C19 1.375(5) . ? C18 C17 1.396(5) . ? C3 H3 0.9300 . ? C3 C4 1.428(5) . ? C3 C2 1.343(6) . ? C20 C19 1.411(5) . ? C20 C15 1.424(5) . ? C20 C11 1.460(5) . ? C1 C2 1.428(6) . ? C1 B1 1.517(6) . ? C4 C5 1.411(7) . ? C13 H13 0.9300 . ? C13 C12 1.416(5) . ? C13 C14 1.358(6) . ? C12 C11 1.395(5) . ? C19 H19 0.9300 . ? C6 H6 0.9300 . ? C6 C7 1.408(6) . ? C6 C5 1.362(6) . ? C7 H7 0.9300 . ? C7 C8 1.373(5) . ? C15 C14 1.427(5) . ? C15 C16 1.413(5) . ? C14 H14 0.9300 . ? C5 H5 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.375(6) . ? C17 H17 0.9300 . ? C8 H8 0.9300 . ? C2 H2 0.9300 . ? 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 C12 N1 H1 118.9 . . ? C12 N1 B1 122.1(4) . . ? B1 N1 H1 118.9 . . ? C9 C10 C11 123.3(3) . . ? C1 C10 C9 118.1(3) . . ? C1 C10 C11 118.5(3) . . ? C4 C9 C10 119.0(3) . . ? C8 C9 C10 123.4(3) . . ? C8 C9 C4 117.2(4) . . ? C19 C18 H18 119.5 . . ? C19 C18 C17 121.0(4) . . ? C17 C18 H18 119.5 . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C2 C3 C4 120.7(5) . . ? C19 C20 C15 117.0(3) . . ? C19 C20 C11 123.3(3) . . ? C15 C20 C11 119.3(3) . . ? C10 C1 C2 119.6(4) . . ? C10 C1 B1 117.1(3) . . ? C2 C1 B1 122.7(4) . . ? C3 C4 C9 118.9(5) . . ? C5 C4 C9 119.3(4) . . ? C5 C4 C3 121.5(5) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C14 C13 C12 120.3(4) . . ? N1 C12 C13 117.7(4) . . ? N1 C12 C11 120.1(3) . . ? C11 C12 C13 122.1(3) . . ? C18 C19 C20 121.7(4) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C5 C6 C7 119.6(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7 120.0 . . ? C20 C15 C14 119.7(3) . . ? C16 C15 C20 120.0(4) . . ? C16 C15 C14 120.1(3) . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C20 C11 C10 123.8(3) . . ? C12 C11 C10 119.1(3) . . ? C12 C11 C20 116.7(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 C4 121.4(4) . . ? C6 C5 H5 119.3 . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 121.0(4) . . ? C17 C16 H16 119.5 . . ? C18 C17 H17 120.5 . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17 120.5 . . ? C9 C8 H8 119.0 . . ? C7 C8 C9 121.9(4) . . ? C7 C8 H8 119.0 . . ? C3 C2 C1 121.5(4) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? N1 B1 Br1 118.0(3) . . ? N1 B1 C1 118.3(4) . . ? C1 B1 Br1 123.6(3) . . ? 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 N1 C12 C11 C10 -9.2(5) . . . . ? N1 C12 C11 C20 164.0(3) . . . . ? C10 C9 C4 C3 -7.3(6) . . . . ? C10 C9 C4 C5 178.5(3) . . . . ? C10 C9 C8 C7 178.1(3) . . . . ? C10 C1 C2 C3 3.3(6) . . . . ? C10 C1 B1 Br1 -172.5(3) . . . . ? C10 C1 B1 N1 3.3(5) . . . . ? C9 C10 C1 C2 -14.8(5) . . . . ? C9 C10 C1 B1 156.6(3) . . . . ? C9 C10 C11 C20 34.6(5) . . . . ? C9 C10 C11 C12 -152.8(3) . . . . ? C9 C4 C5 C6 4.9(6) . . . . ? C3 C4 C5 C6 -169.1(4) . . . . ? C20 C15 C14 C13 -5.5(6) . . . . ? C20 C15 C16 C17 1.8(6) . . . . ? C1 C10 C9 C4 16.8(5) . . . . ? C1 C10 C9 C8 -156.4(3) . . . . ? C1 C10 C11 C20 -148.5(3) . . . . ? C1 C10 C11 C12 24.1(5) . . . . ? C4 C9 C8 C7 4.9(6) . . . . ? C4 C3 C2 C1 6.6(6) . . . . ? C13 C12 C11 C10 173.0(3) . . . . ? C13 C12 C11 C20 -13.9(5) . . . . ? C12 N1 B1 Br1 -172.0(3) . . . . ? C12 N1 B1 C1 12.0(5) . . . . ? C12 C13 C14 C15 3.1(6) . . . . ? C19 C18 C17 C16 -3.1(6) . . . . ? C19 C20 C15 C14 171.3(4) . . . . ? C19 C20 C15 C16 -4.5(5) . . . . ? C19 C20 C11 C10 11.3(6) . . . . ? C19 C20 C11 C12 -161.5(3) . . . . ? C6 C7 C8 C9 1.5(6) . . . . ? C7 C6 C5 C4 1.6(6) . . . . ? C15 C20 C19 C18 3.6(5) . . . . ? C15 C20 C11 C10 -176.2(3) . . . . ? C15 C20 C11 C12 11.1(5) . . . . ? C15 C16 C17 C18 2.1(6) . . . . ? C14 C13 C12 N1 -170.8(4) . . . . ? C14 C13 C12 C11 7.1(6) . . . . ? C14 C15 C16 C17 -174.0(4) . . . . ? C11 C10 C9 C4 -166.3(4) . . . . ? C11 C10 C9 C8 20.6(5) . . . . ? C11 C10 C1 C2 168.1(3) . . . . ? C11 C10 C1 B1 -20.5(5) . . . . ? C11 C20 C19 C18 176.3(4) . . . . ? C11 C20 C15 C14 -1.7(5) . . . . ? C11 C20 C15 C16 -177.5(3) . . . . ? C5 C6 C7 C8 -4.8(6) . . . . ? C16 C15 C14 C13 170.3(4) . . . . ? C17 C18 C19 C20 0.2(6) . . . . ? C8 C9 C4 C3 166.2(3) . . . . ? C8 C9 C4 C5 -7.9(6) . . . . ? C2 C3 C4 C9 -4.4(6) . . . . ? C2 C3 C4 C5 169.6(4) . . . . ? C2 C1 B1 Br1 -1.4(5) . . . . ? C2 C1 B1 N1 174.4(3) . . . . ? B1 N1 C12 C13 169.0(3) . . . . ? B1 N1 C12 C11 -9.0(5) . . . . ? B1 C1 C2 C3 -167.6(4) . . . . ? _shelx_res_file ; TITL ky409_reprocess_a.res in Pca2(1) ky409_reprocess.res created by SHELXL-2018/3 at 11:40:56 on 24-Feb-2021 REM Old TITL KY409_reprocess in Pca2(1) REM SHELXT solution in Pca2(1): R1 0.075, Rweak 0.017, Alpha 0.014 REM 0.877 for 143 systematic absences, Orientation as input REM Flack x = -0.017 ( 0.004 ) from 1115 Parsons' quotients REM Formula found by SHELXT: C21 N Br CELL 0.71073 22.958 9.4271 7.0146 90 90 90 ZERR 4 0.0007 0.0003 0.0003 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H B N Br UNIT 80 52 4 4 4 L.S. 20 PLAN 5 CONF BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA REM REM REM WGHT 0.026200 0.649800 FVAR 0.44594 BR1 5 0.678554 0.155583 0.686889 11.00000 0.03089 0.02320 = 0.03708 0.00211 -0.00157 0.00515 N1 4 0.614244 0.401970 0.808052 11.00000 0.02462 0.02116 = 0.01849 0.00297 -0.00273 -0.00057 AFIX 43 H1 2 0.616236 0.360547 0.917091 11.00000 -1.20000 AFIX 0 C10 1 0.628065 0.569653 0.478804 11.00000 0.01745 0.02328 = 0.01181 -0.00319 -0.00490 -0.00121 C9 1 0.651787 0.671518 0.346452 11.00000 0.01308 0.03040 = 0.01354 -0.00056 -0.00423 0.00189 C18 1 0.479534 0.864250 0.395268 11.00000 0.01922 0.02225 = 0.02293 0.00178 -0.00338 -0.00385 AFIX 43 H18 2 0.471773 0.901657 0.275247 11.00000 -1.20000 AFIX 0 C3 1 0.696934 0.473999 0.171121 11.00000 0.01466 0.03671 = 0.02175 -0.00512 -0.00197 0.00484 AFIX 43 H3 2 0.715289 0.439283 0.062531 11.00000 -1.20000 AFIX 0 C20 1 0.538617 0.711319 0.596934 11.00000 0.01491 0.02162 = 0.02089 -0.00285 0.00007 -0.00395 C1 1 0.649742 0.430487 0.473588 11.00000 0.01565 0.02405 = 0.02115 -0.00445 -0.00257 -0.00028 C4 1 0.683656 0.621582 0.184776 11.00000 0.01125 0.03909 = 0.01792 -0.00538 -0.00112 0.00078 C13 1 0.545590 0.564099 0.946562 11.00000 0.02572 0.02606 = 0.01365 0.00103 0.00073 -0.00588 AFIX 43 H13 2 0.548108 0.514590 1.060940 11.00000 -1.20000 AFIX 0 C12 1 0.581948 0.525973 0.791725 11.00000 0.01854 0.01854 = 0.01843 -0.00291 -0.00207 -0.00506 C19 1 0.525149 0.771245 0.417895 11.00000 0.01734 0.02153 = 0.01843 -0.00202 0.00149 -0.00417 AFIX 43 H19 2 0.547693 0.747223 0.312580 11.00000 -1.20000 AFIX 0 C6 1 0.701229 0.862859 0.082514 11.00000 0.01924 0.04145 = 0.02569 0.01345 0.00269 -0.00221 AFIX 43 H6 2 0.715261 0.926478 -0.007810 11.00000 -1.20000 AFIX 0 C7 1 0.675129 0.913082 0.251099 11.00000 0.01842 0.02935 = 0.03092 0.00842 -0.00011 0.00132 AFIX 43 H7 2 0.674478 1.009845 0.276829 11.00000 -1.20000 AFIX 0 C15 1 0.500762 0.744923 0.751290 11.00000 0.01771 0.01936 = 0.02258 -0.00431 0.00119 -0.00616 C14 1 0.507053 0.672643 0.928810 11.00000 0.02359 0.02949 = 0.01533 -0.00447 0.00386 -0.00386 AFIX 43 H14 2 0.484644 0.699998 1.032959 11.00000 -1.20000 AFIX 0 C11 1 0.584472 0.605977 0.624699 11.00000 0.01426 0.01759 = 0.01610 -0.00266 -0.00135 -0.00394 C5 1 0.705817 0.720525 0.052430 11.00000 0.01767 0.04781 = 0.01878 0.00260 0.00392 0.00283 AFIX 43 H5 2 0.723947 0.687876 -0.057713 11.00000 -1.20000 AFIX 0 C16 1 0.454744 0.842467 0.724707 11.00000 0.01751 0.02657 = 0.02324 -0.00546 0.00224 -0.00059 AFIX 43 H16 2 0.430889 0.865812 0.827167 11.00000 -1.20000 AFIX 0 C17 1 0.444688 0.903406 0.549672 11.00000 0.01932 0.02263 = 0.03096 -0.00454 0.00063 0.00154 AFIX 43 H17 2 0.415087 0.969781 0.534352 11.00000 -1.20000 AFIX 0 C8 1 0.650635 0.819290 0.377541 11.00000 0.01393 0.02774 = 0.02110 0.00349 -0.00175 0.00172 AFIX 43 H8 2 0.632765 0.854213 0.486874 11.00000 -1.20000 AFIX 0 C2 1 0.683202 0.384772 0.313395 11.00000 0.01862 0.02621 = 0.02613 -0.00662 -0.00223 0.00143 AFIX 43 H2 2 0.695768 0.291091 0.307459 11.00000 -1.20000 AFIX 0 B1 3 0.643497 0.342567 0.653570 11.00000 0.01725 0.02267 = 0.02245 -0.00495 -0.00522 0.00069 HKLF 4 REM ky409_reprocess_a.res in Pca2(1) REM wR2 = 0.0679, GooF = S = 1.035, Restrained GooF = 1.035 for all data REM R1 = 0.0353 for 3087 Fo > 4sig(Fo) and 0.0544 for all 3769 data REM 208 parameters refined using 1 restraints END WGHT 0.0261 0.6477 REM Highest difference peak 0.378, deepest hole -0.342, 1-sigma level 0.071 Q1 1 0.7206 0.1628 0.7334 11.00000 0.05 0.38 Q2 1 0.6824 0.5391 0.1752 11.00000 0.05 0.37 Q3 1 0.6785 0.2532 0.6970 11.00000 0.05 0.35 Q4 1 0.6363 0.1585 0.6107 11.00000 0.05 0.33 Q5 1 0.6774 0.0534 0.7689 11.00000 0.05 0.32 ; _shelx_res_checksum 25156 _shelx_hkl_file ; 0 0 -8 243.13 29.26 0 0 -7 4.91 9.77 0 0 -6 196.87 20.54 0 0 -5 -3.55 7.76 0 0 -4 1064.17 39.34 0 0 -4 1017.42 39.96 0 0 -4 991.72 33.93 0 0 -3 0.22 4.35 0 0 -3 -0.43 4.57 0 0 -3 0.93 3.49 0 0 -2 1917.16 46.92 0 0 -2 1924.33 47.22 0 0 -2 1957.76 46.92 0 0 -2 1887.18 47.31 0 0 -2 1942.91 43.51 0 0 2 2101.22 50.29 0 0 2 2084.08 49.87 0 0 2 2137.09 51.10 0 0 3 2.88 4.82 0 0 3 5.31 4.89 0 0 3 6.67 5.96 0 0 3 0.68 5.40 0 0 4 1014.35 39.16 0 0 4 1027.78 40.85 0 0 5 -1.76 6.44 0 0 5 -5.70 7.85 0 0 6 164.08 19.81 0 0 6 194.52 21.64 0 0 7 -13.99 10.16 0 0 7 -8.51 9.61 0 0 8 267.58 29.80 0 0 8 295.20 31.47 0 -1 -8 23.25 12.77 0 1 -8 9.18 11.01 0 -1 -7 6.77 11.40 0 1 -7 29.02 11.55 0 -1 -6 581.07 35.50 0 1 -6 577.67 35.83 0 1 -5 2.00 7.10 0 1 -5 11.52 8.75 0 -1 -5 9.01 8.04 0 -1 -5 2.95 4.93 0 1 -4 143.08 15.92 0 1 -4 150.52 14.93 0 -1 -4 178.26 15.91 0 1 -4 145.38 13.15 0 1 -4 152.44 13.33 0 -1 -4 150.29 11.01 0 -1 -3 5.86 4.63 0 1 -3 -1.36 5.40 0 -1 -3 -8.05 4.95 0 1 -3 -1.49 5.56 0 -1 -3 3.34 5.44 0 1 -3 10.88 5.00 0 -1 -3 2.48 3.14 0 1 -3 0.12 4.00 0 1 -2 988.06 29.92 0 -1 -2 1003.33 30.70 0 -1 -2 952.78 29.47 0 -1 -2 1007.30 30.16 0 1 -2 942.03 30.36 0 -1 -2 998.74 24.13 0 1 -2 969.93 26.85 0 1 -2 947.93 30.28 0 -1 -1 3.84 2.61 0 1 -1 1.42 3.13 0 -1 -1 1.34 2.54 0 -1 -1 0.07 2.53 0 -1 -1 -1.36 2.79 0 1 -1 -3.81 2.26 0 1 -1 -0.31 1.95 0 -1 -1 -1.45 1.98 0 1 -1 -0.25 2.53 0 -1 1 0.53 2.77 0 1 1 -4.16 2.77 0 -1 1 1.73 2.75 0 1 1 -0.89 2.44 0 -1 1 -0.20 2.73 0 -1 1 0.01 1.84 0 1 1 1.12 2.64 0 -1 1 -1.11 2.10 0 -1 2 916.38 29.06 0 1 2 1021.37 30.47 0 1 2 972.36 29.40 0 1 2 967.33 29.68 0 -1 2 963.39 29.87 0 1 2 959.09 29.79 0 1 2 972.36 23.82 0 -1 2 912.10 30.05 0 1 3 -0.04 5.91 0 -1 3 2.62 5.04 0 1 3 4.12 4.99 0 -1 3 0.94 5.79 0 -1 3 -4.32 5.29 0 1 3 1.28 4.32 0 -1 3 6.41 6.16 0 -1 4 165.27 15.51 0 1 4 164.77 15.30 0 -1 4 169.05 16.90 0 -1 5 8.58 7.66 0 1 5 2.43 7.05 0 1 5 26.75 10.78 0 -1 5 1.11 8.58 0 1 6 775.50 41.38 0 -1 6 683.63 38.80 0 1 6 742.53 41.40 0 -1 6 662.24 39.61 0 1 7 19.28 12.96 0 -1 7 0.50 10.45 0 -1 7 23.10 13.25 0 1 7 17.58 12.48 0 1 8 2.69 10.49 0 -1 8 -1.70 11.09 0 1 8 18.14 13.52 0 -1 8 1.49 11.24 0 2 -8 -2.18 13.38 0 -2 -8 7.71 11.52 0 2 -7 -10.28 11.91 0 -2 -7 -4.46 10.35 0 2 -7 -2.31 6.70 0 2 -6 256.55 24.65 0 2 -6 307.50 26.29 0 2 -6 256.31 19.06 0 2 -5 -6.44 8.44 0 2 -5 2.18 10.01 0 -2 -5 12.81 8.66 0 -2 -4 292.05 20.68 0 2 -4 301.17 21.92 0 2 -4 273.33 16.30 0 2 -4 291.35 17.88 0 -2 -4 300.32 18.93 0 2 -4 274.93 21.63 0 -2 -3 2.93 4.82 0 -2 -3 7.51 5.48 0 2 -3 16.06 7.23 0 2 -3 10.14 6.75 0 2 -3 14.04 6.52 0 -2 -3 -1.40 4.24 0 2 -3 7.96 4.26 0 -2 -3 8.18 4.60 0 2 -3 11.19 5.40 0 2 -3 5.93 3.87 0 -2 -2 157.67 11.76 0 -2 -2 169.37 12.19 0 -2 -2 189.06 13.23 0 -2 -2 177.71 12.31 0 2 -2 201.00 13.45 0 2 -2 177.37 12.38 0 2 -2 191.38 10.45 0 2 -2 202.40 10.60 0 2 -2 181.39 12.76 0 -2 -2 162.79 9.42 0 -2 -1 1.23 3.68 0 2 -1 2.56 3.78 0 -2 -1 -3.60 3.69 0 2 -1 11.72 4.24 0 2 -1 6.51 3.04 0 -2 -1 -1.20 3.90 0 2 -1 4.42 3.64 0 2 -1 7.33 4.52 0 -2 -1 4.23 3.73 0 -2 -1 3.67 3.86 0 -2 0 822.78 26.75 0 2 0 801.08 26.23 0 2 0 806.15 26.63 0 -2 0 823.52 26.39 0 -2 0 853.24 26.22 0 2 0 858.31 26.30 0 2 0 853.87 24.73 0 -2 0 819.18 21.69 0 -2 1 2.83 3.52 0 2 1 0.95 3.79 0 2 1 -3.89 3.46 0 2 1 0.74 3.80 0 2 1 -2.45 3.72 0 -2 1 9.04 4.59 0 -2 1 7.45 3.58 0 2 1 -1.28 3.02 0 -2 1 5.08 3.91 0 -2 1 1.54 2.59 0 2 1 4.58 2.23 0 2 2 202.88 12.82 0 2 2 199.82 13.48 0 -2 2 199.43 13.32 0 2 2 183.30 13.07 0 -2 2 208.51 13.05 0 2 2 182.88 12.93 0 2 2 190.76 7.96 0 -2 2 184.56 12.90 0 -2 2 210.55 10.52 0 -2 3 7.92 5.27 0 -2 3 12.23 5.75 0 2 3 4.95 5.31 0 2 3 10.74 5.65 0 2 3 5.34 6.07 0 2 3 11.10 6.70 0 -2 3 8.58 6.20 0 2 3 6.95 4.82 0 2 3 2.54 3.16 0 -2 3 15.20 5.65 0 2 4 205.02 17.29 0 2 4 241.85 18.95 0 -2 4 215.85 18.91 0 -2 5 7.89 9.30 0 2 5 -9.96 8.73 0 -2 5 2.26 7.21 0 -2 6 292.38 25.69 0 2 6 290.06 25.73 0 -2 6 296.61 26.35 0 2 6 298.76 27.00 0 -2 7 8.24 10.62 0 2 7 -6.97 9.76 0 -2 7 6.44 10.30 0 2 7 -6.76 12.24 0 2 8 -4.05 10.99 0 -2 8 18.39 14.43 0 -2 8 22.10 13.06 0 2 8 4.06 13.13 0 3 -9 -15.85 17.04 0 -3 -8 65.48 17.75 0 3 -8 78.52 18.53 0 -3 -8 78.72 18.44 0 -3 -7 1.07 11.74 0 -3 -7 -5.31 10.79 0 3 -7 15.21 11.47 0 3 -7 7.01 11.29 0 -3 -6 318.21 26.63 0 3 -6 323.83 27.18 0 -3 -6 354.95 29.96 0 3 -6 305.98 20.59 0 3 -6 315.30 28.07 0 -3 -5 -10.68 9.24 0 3 -5 -7.14 9.52 0 -3 -5 -11.71 9.82 0 3 -5 6.11 5.81 0 -3 -4 1183.37 44.85 0 -3 -4 1225.52 48.37 0 3 -4 1121.25 37.45 0 3 -4 1123.96 38.15 0 3 -4 1255.56 47.46 0 -3 -4 1179.14 39.27 0 -3 -3 4.64 6.02 0 3 -3 7.78 6.26 0 -3 -3 2.13 5.90 0 3 -3 -0.25 4.58 0 3 -3 2.00 5.14 0 -3 -3 0.19 3.38 0 -3 -2 1480.44 43.16 0 -3 -2 1449.94 44.54 0 -3 -2 1414.99 42.99 0 -3 -2 1428.96 44.81 0 3 -2 1398.63 44.01 0 -3 -2 1441.76 43.84 0 3 -2 1461.24 42.62 0 3 -2 1422.89 37.48 0 3 -2 1368.11 39.16 0 3 -2 1401.08 42.44 0 -3 -2 1439.04 34.68 0 -3 -1 7.35 4.72 0 3 -1 -2.06 4.50 0 -3 -1 2.47 4.87 0 -3 -1 -3.28 5.05 0 -3 -1 2.34 3.79 0 3 -1 1.25 4.58 0 3 -1 6.39 5.18 0 -3 -1 6.95 4.77 0 3 -1 5.21 3.27 0 3 -1 5.34 4.12 0 3 -1 1.17 2.41 0 -3 0 2829.66 69.54 0 3 0 2755.81 68.74 0 3 0 2719.68 68.99 0 3 0 2814.85 68.36 0 -3 0 2821.80 68.45 0 -3 0 2780.11 69.30 0 3 0 2789.68 65.47 0 -3 0 2759.72 60.21 0 -3 0 2855.54 62.57 0 3 0 2737.55 60.99 0 3 1 7.49 5.41 0 -3 1 1.71 4.70 0 3 1 5.53 4.65 0 3 1 5.75 4.95 0 -3 1 -1.70 2.63 0 -3 1 3.58 3.97 0 3 1 -2.03 3.99 0 -3 1 7.37 4.81 0 3 1 1.73 2.28 0 -3 1 4.15 4.07 0 -3 2 1368.58 42.58 0 3 2 1509.17 44.14 0 3 2 1485.16 44.78 0 3 2 1457.22 45.01 0 3 2 1494.27 44.34 0 -3 2 1492.34 44.64 0 3 2 1593.21 45.26 0 -3 2 1404.19 38.48 0 -3 2 1474.16 43.23 0 -3 2 1417.36 42.61 0 -3 2 1392.55 29.32 0 -3 2 1388.37 36.99 0 3 3 -1.45 6.18 0 3 3 -0.07 4.29 0 3 3 7.22 5.92 0 -3 3 6.66 5.60 0 3 3 0.69 2.51 0 -3 3 3.25 3.72 0 3 4 1278.87 48.00 0 3 4 1301.14 48.09 0 -3 4 1302.22 48.24 0 3 4 1252.04 33.49 0 3 5 4.59 8.50 0 3 5 8.34 8.13 0 -3 5 12.46 9.92 0 -3 6 386.85 30.25 0 3 6 429.43 31.65 0 -3 6 432.28 32.11 0 3 7 -1.05 9.58 0 -3 7 -21.53 14.42 0 -3 7 16.21 11.90 0 3 7 -5.02 11.74 0 3 8 41.89 14.74 0 -3 8 75.59 18.24 0 -3 8 44.55 15.49 0 3 8 81.15 20.19 0 4 -9 14.45 14.09 0 -4 -8 64.40 17.32 0 4 -8 48.99 15.96 0 -4 -8 78.92 19.24 0 4 -7 16.48 12.46 0 -4 -7 1.11 9.24 0 4 -7 12.12 10.37 0 -4 -7 -6.84 11.37 0 -4 -6 247.08 24.75 0 4 -6 284.08 27.45 0 4 -6 269.88 24.54 0 4 -6 287.57 20.70 0 -4 -6 283.99 27.71 0 4 -5 16.67 9.68 0 -4 -5 2.27 7.19 0 -4 -5 8.61 9.12 0 4 -5 -9.56 8.61 0 4 -5 6.38 5.88 0 -4 -4 528.52 29.97 0 -4 -4 557.31 32.37 0 4 -4 488.58 25.73 0 4 -4 492.72 24.36 0 -4 -4 503.98 23.22 0 4 -4 509.02 29.87 0 4 -3 3.36 6.28 0 -4 -3 4.21 5.99 0 -4 -3 14.24 7.73 0 4 -3 2.05 4.88 0 4 -3 5.43 5.20 0 -4 -3 0.79 3.28 0 -4 -2 855.19 33.48 0 -4 -2 857.03 35.98 0 4 -2 844.24 32.63 0 -4 -2 872.31 33.83 0 4 -2 806.70 26.74 0 4 -2 846.30 32.37 0 -4 -1 -8.16 6.48 0 4 -1 5.39 4.92 0 -4 -1 -0.61 5.41 0 4 -1 2.29 6.39 0 -4 -1 -2.19 5.19 0 4 -1 7.32 6.14 0 -4 -1 9.38 8.01 0 -4 -1 2.62 5.20 0 4 -1 1.52 4.91 0 4 -1 1.05 3.60 0 4 -1 5.48 3.65 0 -4 0 3538.93 89.16 0 4 0 3499.02 88.29 0 4 0 3514.60 88.67 0 -4 0 3611.13 89.81 0 4 0 3583.70 88.08 0 -4 0 3656.74 88.20 0 -4 0 3585.39 80.10 0 -4 0 3537.72 77.25 0 4 0 3511.55 84.05 0 4 0 3455.27 80.03 0 4 0 3529.70 78.42 0 4 1 11.42 6.36 0 4 1 -1.17 5.75 0 -4 1 2.88 6.55 0 4 1 13.01 6.73 0 -4 1 12.94 6.01 0 4 1 6.95 5.04 0 -4 1 -2.41 4.89 0 -4 1 -0.65 2.85 0 -4 1 1.86 5.28 0 -4 1 4.42 4.60 0 4 2 884.94 36.35 0 -4 2 882.70 35.50 0 4 2 938.42 36.24 0 4 2 924.80 35.18 0 -4 2 913.50 34.19 0 -4 2 872.60 31.48 0 -4 2 821.67 28.09 0 -4 2 918.41 34.28 0 4 2 879.31 24.90 0 4 3 5.03 6.45 0 4 3 7.38 7.27 0 -4 3 -6.30 6.28 0 -4 3 15.21 5.20 0 -4 3 0.84 4.33 0 4 3 -0.34 2.66 0 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5.76 10.92 0 -6 -5 -0.03 8.78 0 -6 -5 14.23 13.18 0 6 -5 -7.51 7.59 0 -6 -4 851.53 43.29 0 -6 -4 851.25 46.64 0 6 -4 802.28 34.52 0 6 -4 849.77 43.07 0 -6 -3 11.66 9.77 0 6 -3 -0.91 6.84 0 6 -3 6.07 7.82 0 -6 -3 15.84 10.50 0 6 -3 2.59 4.54 0 6 -2 965.37 44.90 0 -6 -2 873.23 41.01 0 -6 -2 912.20 44.46 0 -6 -2 939.63 39.83 0 6 -2 959.72 31.89 0 6 -2 868.08 37.06 0 6 -1 5.28 5.70 0 -6 -1 -0.24 7.21 0 -6 -1 -7.05 8.41 0 6 -1 -4.31 7.52 0 -6 -1 8.70 6.02 0 6 -1 3.72 5.51 0 6 0 539.50 32.29 0 -6 0 592.11 34.19 0 -6 0 525.51 26.02 0 -6 0 522.36 24.12 0 6 0 526.63 26.85 0 6 0 527.83 25.04 0 6 1 4.57 7.64 0 6 1 -1.92 7.19 0 -6 1 5.56 8.14 0 -6 1 11.92 7.49 0 -6 1 2.94 3.96 0 6 1 8.08 6.24 0 6 2 987.79 45.14 0 -6 2 909.95 43.40 0 6 2 981.93 44.57 0 -6 2 1028.28 42.86 0 6 2 956.31 26.89 0 6 3 14.00 9.63 0 -6 3 2.77 9.80 0 6 3 2.92 7.76 0 -6 3 0.83 7.81 0 -6 3 -3.47 5.38 0 6 4 706.74 40.71 0 6 4 738.65 41.48 0 -6 4 754.06 40.17 0 6 4 680.01 22.00 0 -6 4 626.02 29.24 0 6 5 7.63 9.66 0 6 5 6.02 8.41 0 -6 5 5.69 9.77 0 -6 5 3.93 6.32 0 6 6 412.18 34.97 0 -6 6 443.90 35.50 0 6 6 410.58 34.10 0 6 7 23.09 14.97 0 -6 7 7.77 12.59 0 6 7 -5.28 11.03 0 7 -7 -9.11 12.68 0 -7 -7 -5.36 11.97 0 -7 -7 -10.40 14.42 0 -7 -6 60.27 15.24 0 7 -6 55.12 16.24 0 -7 -6 36.13 15.78 0 -7 -5 26.82 12.42 0 -7 -5 4.59 10.84 0 7 -5 5.70 7.64 0 -7 -4 251.02 25.98 0 -7 -4 337.65 30.51 0 7 -4 268.58 28.31 0 7 -4 234.44 18.34 0 7 -4 233.81 24.01 0 7 -3 4.54 7.94 0 7 -3 5.62 10.17 0 -7 -3 -18.80 13.11 0 7 -3 1.55 4.85 0 7 -2 336.98 28.54 0 -7 -2 344.91 27.08 0 -7 -2 396.69 31.09 0 -7 -2 333.35 24.30 0 7 -2 364.26 24.01 0 -7 -1 -3.49 7.51 0 7 -1 1.89 5.83 0 7 -1 3.58 9.11 0 -7 -1 7.31 10.57 0 -7 -1 4.21 6.36 0 -7 -1 -2.96 5.80 0 7 -1 3.61 4.82 0 7 0 1346.60 57.18 0 -7 0 1369.78 57.92 0 -7 0 1220.06 41.75 0 -7 0 1300.24 46.33 0 7 0 1213.97 46.30 0 7 0 1327.23 44.97 0 7 1 0.47 9.39 0 7 1 -8.37 9.60 0 -7 1 3.15 9.28 0 -7 1 2.20 5.55 0 -7 1 3.90 4.66 0 7 1 -1.74 7.32 0 7 2 212.66 23.37 0 7 2 244.22 23.95 0 -7 2 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-3 11.75 6.34 1 1 -3 25.67 7.75 -1 -1 -3 4.98 4.59 -1 1 -3 10.98 4.45 1 1 -3 22.67 5.52 -1 -1 -3 17.87 3.47 1 1 -3 13.62 4.73 1 -1 -3 13.70 3.86 1 -1 -3 8.22 4.68 -1 1 -2 1806.40 45.66 -1 -1 -2 1905.81 46.40 1 1 -2 1807.38 45.83 1 -1 -2 1846.68 46.91 -1 -1 -2 1845.44 46.71 1 -1 -2 1796.88 45.86 1 -1 -2 1774.97 46.05 -1 -1 -2 1848.50 46.18 -1 1 -2 1847.97 46.80 -1 1 -2 1742.84 41.15 -1 1 -2 1784.78 47.23 1 1 -2 1812.50 46.41 1 1 -2 1829.85 43.65 1 -1 -2 1834.27 40.65 -1 -1 -2 1823.05 37.71 1 -1 -2 1815.98 44.29 1 1 -2 1785.90 45.32 -1 -1 -1 303.87 11.73 1 -1 -1 321.74 11.88 -1 -1 -1 303.22 12.25 1 -1 -1 317.61 12.34 1 -1 -1 337.05 12.88 1 1 -1 297.46 12.04 -1 -1 -1 294.13 11.80 -1 1 -1 304.81 12.29 -1 -1 -1 322.26 12.80 1 -1 -1 314.69 11.96 1 1 -1 294.78 11.43 -1 1 -1 294.29 12.22 -1 -1 -1 300.57 12.57 1 1 -1 291.46 11.11 -1 1 -1 309.78 11.27 -1 1 -1 302.72 8.85 1 1 -1 292.02 11.97 1 -1 -1 310.36 10.80 -1 1 -1 319.49 12.86 1 1 -1 294.85 11.63 1 1 -1 282.67 10.87 -1 1 1 441.43 14.41 1 1 1 411.72 14.42 1 1 1 413.96 14.12 1 -1 1 424.66 14.25 -1 -1 1 405.48 14.22 -1 1 1 438.86 14.90 -1 1 1 423.50 14.30 1 1 1 389.16 14.05 1 1 1 386.43 14.90 1 -1 1 438.62 14.93 -1 -1 1 407.39 13.44 1 1 1 410.24 12.99 1 -1 1 398.47 14.54 -1 -1 1 401.60 14.00 1 -1 1 404.06 10.78 -1 1 1 413.39 13.18 -1 -1 1 398.07 13.05 1 1 2 2015.37 48.55 -1 -1 2 1967.71 48.62 1 -1 2 1935.11 48.37 -1 1 2 1976.76 48.35 1 1 2 1958.51 48.71 -1 1 2 1999.75 49.07 1 1 2 1954.83 48.71 -1 1 2 1980.58 48.70 1 1 2 1955.50 49.77 1 -1 2 1957.45 49.51 -1 -1 2 2021.02 48.83 -1 -1 2 1968.11 46.16 1 1 2 1933.21 47.77 -1 1 2 1972.79 48.96 -1 1 2 1947.96 43.18 -1 -1 2 1951.09 49.15 1 -1 2 1900.20 49.48 -1 -1 3 -4.16 5.90 1 1 3 9.44 6.34 -1 1 3 8.62 6.00 1 -1 3 2.68 4.79 -1 1 3 20.81 6.48 1 -1 3 10.89 4.90 -1 -1 3 10.03 5.68 -1 1 3 6.10 5.07 -1 -1 3 10.33 5.64 1 1 3 9.45 5.61 1 -1 3 7.33 5.49 1 1 3 -1.15 4.41 -1 -1 3 8.11 5.81 1 -1 3 10.24 6.33 -1 1 3 14.86 4.68 -1 1 4 778.15 33.72 1 -1 4 760.12 33.54 -1 -1 4 766.39 33.70 1 1 4 795.60 34.04 -1 -1 4 831.91 35.44 1 -1 4 835.98 35.70 1 1 5 440.40 27.45 1 -1 5 398.89 26.71 -1 -1 5 428.84 27.14 -1 1 5 408.94 26.71 1 -1 5 392.65 27.13 1 1 5 388.92 26.91 -1 -1 5 362.48 26.01 -1 -1 6 255.36 24.07 1 -1 6 217.02 21.64 -1 1 6 302.03 25.58 1 1 6 209.15 22.36 1 1 6 299.03 26.31 1 -1 6 258.26 24.85 -1 1 6 245.66 24.71 -1 -1 6 299.38 26.02 1 -1 7 95.27 17.81 -1 -1 7 70.55 16.09 1 1 7 93.32 18.04 -1 1 7 59.60 15.39 -1 -1 7 63.94 15.35 1 1 7 65.84 15.19 1 -1 7 63.39 15.48 -1 1 7 82.47 17.34 -1 -1 8 73.84 17.32 1 -1 8 110.28 20.90 1 1 8 115.04 20.61 -1 1 8 88.47 18.54 1 -1 8 106.34 19.80 -1 1 8 110.38 20.95 1 1 8 66.45 18.31 -1 -1 8 74.16 17.79 1 1 9 35.26 17.49 1 -2 -8 89.39 20.67 -1 -2 -8 85.56 16.94 1 2 -8 67.24 17.53 -1 2 -8 80.87 19.40 -1 2 -7 31.83 15.21 -1 2 -7 15.00 10.19 1 2 -7 30.34 13.93 1 -2 -7 20.02 11.10 -1 -2 -7 26.25 12.24 1 2 -7 31.99 8.51 -1 2 -7 22.39 8.06 1 -2 -6 409.02 29.95 -1 2 -6 400.30 30.08 1 2 -6 404.50 30.51 -1 -2 -6 417.88 30.19 1 2 -6 395.00 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102.98 20.64 13 -5 -6 88.31 18.84 -13 -5 -6 94.96 18.95 -13 5 -5 33.62 15.38 13 -5 -5 79.27 14.96 -13 -5 -5 52.51 12.73 -13 -5 -5 79.18 18.51 13 5 -5 99.82 20.41 13 -5 -5 92.99 18.29 -13 5 -5 77.45 17.25 13 -5 -5 89.39 17.82 -13 -5 -5 63.13 15.25 -13 5 -4 190.73 24.05 -13 -5 -4 236.61 21.39 13 -5 -4 195.79 19.30 13 -5 -4 211.37 22.95 -13 -5 -4 230.28 23.38 13 5 -4 182.85 22.70 13 -5 -4 216.64 21.69 -13 5 -4 213.04 24.38 -13 -5 -4 205.01 25.21 -13 5 -3 193.68 23.79 -13 -5 -3 168.19 17.29 13 -5 -3 180.21 17.41 13 5 -3 185.22 20.12 -13 5 -3 166.38 18.79 13 -5 -3 194.13 20.52 -13 -5 -3 185.23 19.90 13 5 -3 204.65 23.23 -13 -5 -3 227.30 25.26 13 -5 -3 153.75 16.84 -13 5 -3 208.85 23.59 -13 -5 -3 195.10 10.82 13 5 -2 370.87 25.77 -13 5 -2 313.75 23.85 13 -5 -2 357.48 22.79 -13 -5 -2 346.01 22.82 13 -5 -2 356.76 25.68 -13 -5 -2 381.60 26.49 13 -5 -2 350.48 23.32 -13 5 -2 332.08 11.65 -13 -5 -2 325.44 28.94 -13 5 -2 361.51 30.07 13 5 -2 355.19 29.36 -13 5 -2 351.34 30.90 -13 5 -2 306.98 19.40 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25.23 16.87 -28 0 -2 223.52 27.84 28 0 -2 216.12 31.18 -28 0 -2 238.40 30.47 -28 0 -2 191.20 25.80 28 0 -1 18.63 17.89 -28 0 -1 25.84 14.85 -28 0 -1 23.34 13.90 -28 0 -1 3.58 11.05 -28 0 -1 26.20 13.50 28 0 0 134.35 27.00 -28 0 0 181.02 24.50 -28 0 0 169.09 24.59 -28 0 0 178.26 22.50 -28 0 0 163.52 25.52 -28 0 0 168.71 24.53 -28 0 1 25.39 13.02 -28 0 1 -1.46 11.69 -28 0 1 26.78 15.73 -28 0 2 249.08 30.20 -28 0 2 288.17 30.29 -28 0 2 277.53 31.74 -28 0 3 24.82 13.83 -28 1 -4 46.08 17.17 -28 1 -3 -33.22 16.44 28 -1 -3 13.65 17.44 -28 -1 -3 -13.32 16.91 -28 1 -2 38.52 16.03 28 1 -2 45.21 18.53 28 -1 -2 49.49 19.28 -28 1 -2 55.42 19.74 -28 -1 -2 74.98 18.80 -28 -1 -2 50.16 15.89 -28 -1 -2 20.82 11.91 28 1 -1 -15.69 18.46 28 -1 -1 22.63 16.97 -28 -1 -1 4.69 10.92 -28 1 -1 -8.21 12.93 -28 -1 -1 -1.53 11.42 -28 -1 -1 3.84 10.52 -28 -1 -1 -6.34 12.42 -28 1 -1 -16.36 15.67 -28 1 -1 19.02 14.18 -28 -1 -1 37.80 14.15 28 -1 0 8.56 13.96 -28 -1 0 8.53 15.78 -28 1 0 62.95 18.08 -28 -1 0 33.66 12.37 -28 -1 0 38.64 14.48 -28 -1 0 22.24 12.54 -28 1 0 46.08 17.01 -28 -1 0 47.07 12.58 -28 1 0 25.69 13.17 -28 1 0 33.72 16.32 -28 1 1 10.71 11.04 -28 -1 1 -4.23 12.38 -28 -1 1 -2.88 13.42 -28 1 1 -15.97 11.99 -28 1 1 25.43 13.77 -28 -1 1 25.38 14.65 -28 1 1 13.84 12.53 -28 -1 2 74.98 18.36 -28 1 2 49.34 19.33 -28 -1 2 69.06 17.38 -28 1 2 49.32 16.10 -28 -1 2 67.72 18.85 -28 1 2 30.60 14.60 -28 -1 3 -6.21 12.84 -28 2 -3 40.93 16.62 28 -2 -3 -4.56 15.80 -28 -2 -3 2.75 10.51 -28 -2 -3 29.96 15.38 -28 2 -2 78.01 20.68 28 2 -2 88.74 25.95 28 -2 -2 44.73 19.82 -28 -2 -2 61.84 19.21 -28 2 -2 65.26 20.08 -28 -2 -2 67.52 19.11 -28 -2 -2 34.33 12.57 -28 -2 -2 36.94 13.75 -28 -2 -2 38.43 15.42 28 2 -1 4.94 14.33 28 -2 -1 -4.06 13.86 -28 -2 -1 -0.20 11.25 -28 2 -1 25.85 15.64 -28 -2 -1 -16.45 13.23 -28 2 -1 33.70 16.82 -28 -2 -1 5.83 10.81 -28 -2 -1 -9.30 10.95 -28 2 -1 0.39 13.22 -28 -2 -1 5.50 11.52 -28 -2 0 89.92 21.22 -28 2 0 102.99 20.89 -28 -2 0 85.93 18.52 -28 -2 0 93.27 18.47 -28 2 0 81.51 20.93 -28 -2 0 141.93 22.00 -28 2 0 122.10 24.43 -28 2 1 13.37 11.67 -28 -2 1 16.48 14.03 -28 -2 1 15.74 12.09 -28 2 1 21.93 14.57 -28 -2 1 9.57 11.80 -28 2 1 13.82 15.14 -28 -2 2 43.84 16.64 -28 -2 2 49.34 17.39 -28 -2 2 47.41 16.89 28 -3 -3 -1.79 14.44 -28 -3 -3 -21.03 14.54 -28 3 -2 75.54 21.95 28 -3 -2 33.06 16.94 -28 -3 -2 49.12 15.83 -28 -3 -2 54.97 16.47 -28 -3 -2 67.49 17.78 -28 -3 -1 8.62 12.27 -28 3 -1 5.27 13.42 -28 -3 -1 5.70 10.69 -28 -3 -1 -0.20 10.79 -28 -3 -1 -11.56 10.60 -28 3 -1 -18.01 17.19 -28 -3 -1 -5.05 10.46 -28 -3 0 40.15 16.94 -28 3 0 7.18 14.19 -28 -3 0 -4.75 14.35 -28 -3 0 4.29 10.35 -28 -3 0 -2.32 11.08 -28 3 0 5.78 15.04 -28 -3 1 -1.53 13.64 -28 -3 1 -7.07 10.77 -28 -3 1 -15.35 12.97 -28 -3 2 56.14 17.28 -28 -3 2 66.56 17.72 -28 -3 3 -9.84 12.91 -28 -4 -3 5.86 11.78 -28 -4 -2 48.05 18.08 -28 -4 -2 105.59 21.57 -28 -4 -2 75.63 18.90 -28 -4 -1 -2.09 13.32 -28 4 -1 25.28 15.58 -28 -4 -1 30.38 15.97 -28 4 0 67.73 20.19 -28 -4 0 35.80 17.88 -28 -4 0 44.64 16.69 -28 4 0 72.33 22.52 -28 -4 0 43.75 15.85 -28 -4 1 12.90 11.97 -28 -4 1 29.45 13.86 -28 -4 2 79.93 18.33 -28 -5 1 36.04 15.57 29 0 -2 3.44 16.46 -29 0 -2 -1.92 12.41 -29 0 -2 11.57 13.14 -29 0 -2 -10.89 11.89 29 0 -1 -25.52 17.00 -29 0 -1 -35.10 15.88 -29 0 -1 -15.51 15.02 -29 0 -1 -4.36 11.37 -29 0 0 15.96 13.61 -29 0 0 -4.70 12.49 -29 0 0 -2.55 11.76 -29 0 0 1.86 12.57 -29 0 0 -3.85 13.90 -29 0 1 29.31 15.52 -29 0 1 22.29 13.87 -29 0 1 3.13 13.24 -29 0 2 0.15 13.17 -29 1 -3 28.99 20.78 -29 -1 -3 22.28 14.37 -29 1 -2 54.78 18.15 29 -1 -2 70.98 22.77 -29 1 -2 46.40 18.14 -29 -1 -2 90.13 20.27 -29 -1 -2 51.51 16.34 -29 -1 -2 92.44 19.23 29 1 -1 22.16 19.21 29 -1 -1 60.03 22.15 -29 1 -1 55.39 18.26 -29 -1 -1 44.70 16.59 -29 1 -1 37.00 15.45 -29 -1 -1 33.23 13.55 -29 -1 -1 53.71 16.68 -29 1 -1 12.69 13.03 -29 -1 -1 20.82 11.98 -29 -1 0 52.48 17.13 -29 1 0 70.54 17.89 -29 1 0 80.33 20.85 -29 -1 0 48.95 16.55 -29 -1 0 46.66 16.53 -29 1 0 44.51 19.66 -29 -1 0 49.01 16.79 -29 1 0 30.00 15.50 -29 -1 1 34.84 16.78 -29 1 1 16.15 13.20 -29 -1 1 56.91 17.97 -29 1 1 50.40 15.65 -29 -1 1 7.57 13.68 -29 -1 2 57.47 17.12 -29 -1 2 61.52 17.97 -29 1 2 47.87 15.56 -29 2 -3 18.73 16.05 -29 2 -2 123.09 25.18 29 -2 -2 94.44 26.04 -29 -2 -2 125.97 22.86 -29 -2 -2 126.62 23.87 -29 -2 -2 142.43 22.54 29 -2 -1 -0.97 15.00 -29 -2 -1 39.97 16.13 -29 2 -1 13.10 13.63 -29 -2 -1 2.06 12.21 -29 -2 -1 44.54 15.44 -29 -2 -1 34.38 15.90 -29 2 -1 50.30 18.65 -29 -2 -1 18.97 12.37 -29 -2 0 52.58 17.45 -29 2 0 68.64 18.53 -29 2 0 49.26 18.39 -29 -2 0 83.15 18.70 -29 -2 0 69.22 16.50 -29 -2 0 78.53 19.36 -29 2 1 29.74 14.75 -29 -2 1 8.79 11.53 -29 -2 1 40.23 18.53 -29 -2 1 55.05 18.29 -29 -2 2 108.29 21.01 -29 -3 -3 10.46 13.86 -29 -3 -2 -6.87 15.37 -29 -3 -2 26.53 15.44 -29 -3 -2 -7.18 12.42 -29 -3 -1 16.34 15.56 -29 3 -1 48.83 19.48 -29 -3 -1 42.57 16.12 -29 3 -1 25.89 17.70 -29 -3 -1 33.76 13.95 -29 -3 0 -24.77 16.48 -29 3 0 -10.55 13.48 -29 -3 0 -0.14 11.50 -29 3 0 29.33 17.31 -29 -3 0 20.75 13.20 -29 -3 0 8.75 11.96 -29 -3 1 36.96 14.33 -29 -3 1 28.20 14.44 -29 -3 1 43.02 17.60 -29 -3 2 6.70 12.94 -29 -4 -2 27.19 15.59 -29 4 0 107.85 23.59 -29 -4 0 110.20 21.12 -29 -4 1 21.48 15.24 -29 -4 2 19.60 12.90 -30 0 -2 29.09 14.47 30 0 -1 52.35 20.82 -30 0 -1 39.59 17.10 -30 0 -1 48.09 16.88 -30 0 -1 77.21 18.72 -30 0 0 182.16 28.25 -30 0 0 226.66 29.47 -30 0 1 82.04 19.62 -30 0 2 92.77 20.96 -30 -1 -3 -14.18 13.00 -30 -1 -2 16.20 17.11 -30 -1 -2 10.97 11.52 -30 -1 -2 -1.51 11.30 30 -1 -1 20.36 16.76 -30 1 -1 34.18 18.51 -30 -1 -1 28.76 15.42 -30 -1 -1 32.03 15.62 -30 1 -1 16.11 14.33 -30 -1 -1 18.53 13.23 -30 1 0 -8.82 12.33 -30 -1 0 -0.40 11.50 -30 -1 0 -6.88 12.82 -30 1 0 8.34 14.22 -30 -1 0 14.91 14.13 -30 -1 1 11.49 13.26 -30 1 2 -10.40 12.83 -30 2 -2 34.21 17.53 30 -2 -2 -3.75 14.61 -30 -2 -2 5.97 13.09 30 -2 -1 -6.78 15.08 -30 -2 -1 39.76 17.23 -30 2 -1 6.90 13.54 -30 -2 -1 -7.78 11.04 -30 -2 -1 11.84 10.99 -30 2 -1 21.88 14.42 -30 -2 -1 19.19 12.71 -30 -2 -1 5.32 10.67 -30 -2 0 0.66 12.80 -30 2 0 -20.55 16.06 -30 -2 0 4.29 13.54 -30 -2 0 -9.27 11.68 -30 2 0 27.59 17.84 -30 -2 0 -4.90 13.02 -30 -2 1 25.64 15.69 -30 -2 1 5.31 14.64 -30 -3 -1 33.31 17.25 -30 -3 -1 39.53 17.52 -30 -3 0 32.12 16.93 -30 3 0 5.61 15.81 -30 -3 0 49.77 16.52 -30 -3 1 2.80 11.53 -30 -4 0 155.74 24.27 -31 0 -1 3.29 13.60 -31 -1 -1 140.17 24.59 -31 1 0 3.16 15.74 -31 -1 1 117.69 21.95 -31 1 1 120.43 25.01 -31 -2 -1 20.91 12.10 -31 -2 -1 33.32 13.91 -31 -2 0 3.98 13.12 -31 2 0 -5.97 13.18 -31 -2 0 20.01 14.79 0 0 0 0.00 0.00 TITL KY409_reprocess in Pca2(1) REM Pca2(1) (#29, found as P2(1)ca in -cba setting) CELL 0.71073 22.957980 9.427088 7.014567 90.0000 90.0000 90.0000 ZERR 4.00 0.000712 0.000304 0.000283 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 B N Br UNIT 80.00 52.00 4.00 4.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 30434 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.317 _oxdiff_exptl_absorpt_empirical_full_min 0.852 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mi21007c _database_code_depnum_ccdc_archive 'CCDC 2084380' loop_ _audit_author_name _audit_author_address 'Marina Uzelac' ;University of Edinburgh United Kingdom ; _audit_update_record ; 2021-05-18 deposited with the CCDC. 2022-01-03 downloaded from the CCDC. ; _audit_creation_date 2021-05-10 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 loop_ _audit_author_email '' g.s.nichol@ed.ac.uk _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '1(C33 H26 B1 N1)' _chemical_formula_sum 'C33 H26 B N' _chemical_formula_weight 447.36 _chemical_melting_point ? _chemical_oxdiff_formula C33H26BN _chemical_oxdiff_usercomment '@ 120 K KY461' 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' B B 0.0090 0.0039 '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' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6409(2) _cell_length_b 12.0504(4) _cell_length_c 15.9138(6) _cell_angle_alpha 78.061(3) _cell_angle_beta 78.902(3) _cell_angle_gamma 79.901(3) _cell_volume 1210.41(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8254 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 76.2060 _cell_measurement_theta_min 3.7780 _shelx_estimated_absorpt_T_max 0.983 _shelx_estimated_absorpt_T_min 0.829 _exptl_absorpt_coefficient_mu 0.528 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 472 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 5 2 0.1368 4 4 5 0.1456 3 -4 -1 0.1655 1 -7 -4 0.1637 -4 -4 -5 0.0919 0 0 -1 0.0165 0 0 1 0.0165 _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of hexane and dichloromethane by slow evaporation' _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.251 _exptl_crystal_size_min 0.033 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -2.5900 5.2296 1.6795 0.1097 0.3135 0.9432 3.8773 4.1187 4.7127 0.2839 0.8019 -0.5257 3.1868 -4.1223 -0.6678 -0.0483 -0.1397 -0.9890 0.5575 -7.2000 -4.0358 -0.2515 -0.7138 -0.6537 -3.8758 -4.1237 -4.7150 -0.2840 -0.8023 0.5250 0.0000 -0.0000 -0.9996 -0.1000 0.0040 -0.0051 -0.0000 0.0000 0.9996 0.1000 -0.0040 0.0051 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_unetI/netI 0.0223 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 19449 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.684 _diffrn_reflns_theta_min 3.787 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1574 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -73.00 -14.00 1.00 1.00 -- 0.00 142.00 26.00 59 2 \w -64.00 -8.00 1.00 1.00 -- 0.00 128.00-145.00 56 3 \w -143.00 -74.00 1.00 3.00 -- -59.00-128.00 140.00 69 4 \w -100.00 -14.00 1.00 3.00 -- -59.00 142.00 26.00 86 5 \w -144.00 -66.00 1.00 3.00 -- -59.00-142.00 -30.00 78 6 \w 36.00 125.00 1.00 3.00 -- 59.00-142.00 -30.00 89 7 \w 30.00 114.00 1.00 3.00 -- 59.00-128.00 140.00 84 8 \w 96.00 143.00 1.00 3.00 -- 59.00 128.00-145.00 47 9 \w 88.00 143.00 1.00 3.00 -- 59.00 142.00 26.00 55 10 \w 36.00 125.00 1.00 3.00 -- 118.00-142.00 -30.00 89 11 \w 96.00 178.00 1.00 3.00 -- 118.00 128.00-145.00 82 12 \w 87.00 172.00 1.00 3.00 -- 118.00 142.00 26.00 85 13 \w 34.00 114.00 1.00 3.00 -- 118.00-128.00 140.00 80 14 \w -96.00 -39.00 1.00 1.00 -- 0.00-178.00 90.00 57 15 \w -95.00 -37.00 1.00 1.00 -- 0.00 178.00 -90.00 58 16 \w -39.00 42.00 1.00 1.00 -- 0.00 77.00 0.00 81 17 \w -151.00 -82.00 1.00 3.00 -- -59.00 -77.00-120.00 69 18 \w -143.00 -22.00 1.00 3.00 -- -59.00 -38.00 -60.00 121 19 \w -151.00 -82.00 1.00 3.00 -- -59.00 -77.00 0.00 69 20 \w 103.00 151.00 1.00 3.00 -- 59.00 77.00 0.00 48 21 \w 97.00 143.00 1.00 3.00 -- 59.00 125.00 -60.00 46 22 \w 97.00 143.00 1.00 3.00 -- 59.00 125.00-180.00 46 23 \w 97.00 143.00 1.00 3.00 -- 59.00 125.00 120.00 46 24 \w 103.00 151.00 1.00 3.00 -- 59.00 77.00 -30.00 48 25 \w 32.00 109.00 1.00 3.00 -- 118.00-111.00 150.00 77 26 \w 82.00 178.00 1.00 3.00 -- 118.00 45.00 -90.00 96 27 \w 81.00 178.00 1.00 3.00 -- 118.00 61.00-150.00 97 28 \w 32.00 109.00 1.00 3.00 -- 118.00-111.00 90.00 77 29 \w 27.00 106.00 1.00 3.00 -- 118.00 -94.00 30.00 79 30 \w 26.00 157.00 1.00 3.00 -- 118.00 -77.00-120.00 131 31 \w 104.00 178.00 1.00 3.00 -- 118.00 111.00 -90.00 74 32 \w 27.00 106.00 1.00 3.00 -- 118.00 -94.00 -60.00 79 33 \w 28.00 178.00 1.00 3.00 -- 118.00 15.00 -90.00 150 34 \w 82.00 178.00 1.00 3.00 -- 118.00 50.00-177.08 96 35 \w 34.00 154.00 1.00 3.00 -- 118.00 -45.00 0.00 120 36 \w 104.00 178.00 1.00 3.00 -- 118.00 111.00 90.00 74 37 \w 103.00 178.00 1.00 3.00 -- 118.00 77.00 -30.00 75 38 \w 27.00 106.00 1.00 3.00 -- 118.00 -94.00-150.00 79 39 \w 33.00 155.00 1.00 3.00 -- 118.00 -61.00 -30.00 122 40 \w 27.00 106.00 1.00 3.00 -- 118.00 -94.00 150.00 79 41 \w 27.00 106.00 1.00 3.00 -- 118.00 -94.00 120.00 79 42 \w 82.00 178.00 1.00 3.00 -- 118.00 45.00 30.00 96 43 \w 27.00 106.00 1.00 3.00 -- 118.00 -94.00-120.00 79 44 \w 32.00 109.00 1.00 3.00 -- 118.00-111.00 120.00 77 45 \w 104.00 178.00 1.00 3.00 -- 118.00 111.00 -30.00 74 46 \w 61.00 146.00 1.00 3.00 -- 118.00 178.00 30.00 85 47 \w 57.00 83.00 1.00 3.00 -- 118.00 -94.00-180.00 26 48 \w 105.00 152.00 1.00 3.00 -- 118.00 30.00 60.00 47 49 \w 72.00 103.00 1.00 3.00 -- 118.00-111.00 30.00 31 50 \w 153.00 178.00 1.00 3.00 -- 118.00 77.00 60.00 25 51 \w 61.00 109.00 1.00 3.00 -- 118.00-111.00-150.00 48 52 \w 74.00 116.00 1.00 3.00 -- 118.00 -61.00-120.00 42 53 \w 37.00 62.00 1.00 3.00 -- 118.00-111.00 30.00 25 54 \w 104.00 134.00 1.00 3.00 -- 118.00 77.00 60.00 30 55 \w 106.00 135.00 1.00 3.00 -- 118.00 77.00 90.00 29 56 \w 87.00 128.00 1.00 3.00 -- 118.00 -77.00 60.00 41 57 \w 124.00 150.00 1.00 3.00 -- 118.00 111.00 150.00 26 58 \w 66.00 108.00 1.00 3.00 -- 118.00 178.00 120.00 42 59 \w 68.00 105.00 1.00 3.00 -- 118.00-111.00 -60.00 37 60 \w 111.00 147.00 1.00 3.00 -- 118.00 45.00 -30.00 36 61 \w 91.00 117.00 1.00 3.00 -- 118.00 -61.00 150.00 26 62 \w 97.00 123.00 1.00 3.00 -- 118.00 -83.00 -64.23 26 63 \w 81.00 134.00 1.00 3.00 -- 118.00 61.00 -30.00 53 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0239555000 _diffrn_orient_matrix_UB_12 -0.0230180000 _diffrn_orient_matrix_UB_13 0.1000672000 _diffrn_orient_matrix_UB_21 0.0960733000 _diffrn_orient_matrix_UB_22 0.1087885000 _diffrn_orient_matrix_UB_23 -0.0039554000 _diffrn_orient_matrix_UB_31 -0.2172990000 _diffrn_orient_matrix_UB_32 0.0711121000 _diffrn_orient_matrix_UB_33 0.0050904000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7191 _reflns_number_total 9193 _reflns_special_details ; _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.184 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.046 _refine_ls_extinction_coef 0.0081(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 592 _refine_ls_number_reflns 9193 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0571 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1596 _refine_ls_wR_factor_ref 0.1660 _refine_special_details ; All of the crystals tested in this sample suffered from quite severe twinning. A detector distance of 65 mm was used. CrysAlisPro was used to apply twin law [-1 0 0 / 0 -1 0 / -0.7746 -0.4716 1] during integration, with refined twin scale fraction 0.2477(13). The structure suffers from whole molecule disorder, with the exception of N1/C1, C4/C17 & C7/C20, three pairs of atoms which were constrained to have identical coordinates and displacement ellipsoid parameters. Some geometric similarity restraints were used. The N-bound H atoms were identified from difference maps and refined using a riding model. #=============================================================================== #>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<< #=============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.55 Note 420_ALERT_2_C D-H Bond Without Acceptor N1 --H1 . Please Check 788_ALERT_4_C Change B1 into B in MoietyFormula Please Do Consequence of whole molecule disorder 906_ALERT_3_C Large K Value in the Analysis of Variance ...... 3.937 Check 918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) . 1 Check No action taken #=============================================================================== ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.7527(12) 0.2473(12) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 3. Shared sites {N1, C1A} {C1, N1A} {C4, C17A} {C17, C4A} {C7, C20A} {C20, C7A} 4. Restrained distances N1A-H1AA 0.83 with sigma of 0.02 N1-H1 0.84 with sigma of 0.02 C26-C31 \\sim C26A-C31A with sigma of 0.02 C29-C30 \\sim C29A-C30A with sigma of 0.02 C25-C26 \\sim C25A-C26A with sigma of 0.02 C25-C30 \\sim C25A-C30A with sigma of 0.02 C26-C27 \\sim C26A-C27A with sigma of 0.02 C25-B1 \\sim C25A-B1 with sigma of 0.02 C25-B1A \\sim C25A-B1A with sigma of 0.02 C30-B1A \\sim C30A-B1A with sigma of 0.04 C27-C29 \\sim C27A-C29A with sigma of 0.04 C27-C32 \\sim C27A-C32A with sigma of 0.04 C28-C29 \\sim C28A-C29A with sigma of 0.02 C28-C30 \\sim C28A-C30A with sigma of 0.04 C29-C32 \\sim C29A-C32A with sigma of 0.04 C27-C28 \\sim C27A-C28A with sigma of 0.02 C27-C31 \\sim C27A-C31A with sigma of 0.04 C28-C32 \\sim C28A-C32A with sigma of 0.02 C29-C33 \\sim C29A-C33A with sigma of 0.04 C30-B1 \\sim C30A-B1 with sigma of 0.04 C25-C27 \\sim C25A-C27A with sigma of 0.04 C25-C29 \\sim C25A-C29A with sigma of 0.04 C25-C31 \\sim C25A-C31A with sigma of 0.04 C25-C33 \\sim C25A-C33A with sigma of 0.04 C30-C33 \\sim C30A-C33A with sigma of 0.02 C26-C28 \\sim C26A-C28A with sigma of 0.04 C26-C30 \\sim C26A-C30A with sigma of 0.04 C26-B1 \\sim C26A-B1 with sigma of 0.04 C26-B1A \\sim C26A-B1A with sigma of 0.04 5. Restrained planarity C26, C27, C28, C29, C30 with sigma of 0.1 C25, C26, C27, C28, C29, C30 with sigma of 0.1 6. Uiso/Uaniso restraints and constraints Uanis(N1) = Uanis(C1A) Uanis(C1) = Uanis(N1A) Uanis(C4) = Uanis(C17A) Uanis(C17) = Uanis(C4A) Uanis(C7) = Uanis(C20A) Uanis(C20) = Uanis(C7A) 7. Rigid body (RIGU) restrains C25, C26, C27, C28, C29, C30 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C26, C27, C28, C29, C30 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 8. Others Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)= Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)= Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C15A)=Sof(C16A)= Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)= Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(C40)= Sof(N1A)=Sof(H1AA)=Sof(B1A)=Sof(C25A)=Sof(C26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)= Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)= Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=Sof(H33A)=Sof(H33B)= Sof(H33C)=1-FVAR(1) Sof(N1)=Sof(H1)=Sof(C1)=Sof(H1B)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)= Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)= Sof(C10)=Sof(H10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)= Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)= Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(C24)=Sof(C25)=Sof(C26)= Sof(C27)=Sof(H27)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(C31)=Sof(H31D)= Sof(H31E)=Sof(H31F)=Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33)=Sof(H33D)= Sof(H33E)=Sof(H33F)=Sof(B1)=FVAR(1) 9.a Aromatic/amide H refined with riding coordinates: C1A(H1A), C1(H1B), C2(H2), C2A(H2A), C4(H4), C4A(H4A), C5(H5), C5A(H5A), C7(H7), C7A(H7A), C8(H8), C8A(H8A), C9(H9), C9A(H9A), C10(H10), C10A(H10A), C16(H16), C16A(H16A), C17(H17), C17A(H17A), C19(H19), C19A(H19A), C20(H20), C20A(H20A), C21(H21), C21A(H21A), C22(H22), C22A(H22A), C27(H27), C29(H29), C27A(H27A), C29A(H29A) 9.b Idealised Me refined as rotating group: C31(H31D,H31E,H31F), C32(H32D,H32E,H32F), C33(H33D,H33E,H33F), C31A(H31A,H31B, H31C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 C1A C 0.9508(2) 0.82928(12) 0.52408(9) 0.0361(3) Uani 0.483(2) 1 d . . P A 2 H1A H 0.992835 0.849461 0.463029 0.043 Uiso 0.483(2) 1 calc R U P A 2 N1 N 0.9508(2) 0.82928(12) 0.52408(9) 0.0361(3) Uani 0.517(2) 1 d D . P A 1 H1 H 1.050(5) 0.861(3) 0.490(2) 0.043 Uiso 0.517(2) 1 d D U P A 1 C1 C 0.5294(2) 0.65730(13) 0.52563(10) 0.0393(4) Uani 0.517(2) 1 d . . P A 1 H1B H 0.531099 0.666305 0.464774 0.047 Uiso 0.517(2) 1 calc R U P A 1 C2 C 0.3870(5) 0.5808(3) 0.5927(3) 0.0386(8) Uani 0.517(2) 1 d . . P A 1 H2 H 0.278649 0.552870 0.575687 0.046 Uiso 0.517(2) 1 calc R U P A 1 C2A C 1.0514(5) 0.8749(2) 0.5820(2) 0.0317(7) Uani 0.483(2) 1 d . . P A 2 H2A H 1.173261 0.910124 0.561719 0.038 Uiso 0.483(2) 1 calc R U P A 2 C3 C 0.4214(5) 0.5537(2) 0.6790(2) 0.0371(7) Uani 0.517(2) 1 d . . P A 1 C3A C 0.9534(6) 0.8624(3) 0.6697(2) 0.0309(7) Uani 0.483(2) 1 d . . P A 2 C4 C 0.3196(3) 0.47446(17) 0.72824(17) 0.0569(5) Uani 0.517(2) 1 d . . P A 1 H4 H 0.225013 0.442677 0.705469 0.068 Uiso 0.517(2) 1 calc R U P A 1 C4A C 1.0095(3) 0.92045(16) 0.72404(14) 0.0488(4) Uani 0.483(2) 1 d . . P A 2 H4A H 1.118466 0.965254 0.700968 0.059 Uiso 0.483(2) 1 calc R U P A 2 C5 C 0.3516(8) 0.4338(3) 0.8200(3) 0.0578(11) Uani 0.517(2) 1 d . . P A 1 H5 H 0.259975 0.388067 0.859955 0.069 Uiso 0.517(2) 1 calc R U P A 1 C5A C 0.9222(6) 0.9198(3) 0.8093(3) 0.0489(9) Uani 0.483(2) 1 d . . P A 2 H5A H 0.986056 0.947021 0.848073 0.059 Uiso 0.483(2) 1 calc R U P A 2 C6 C 0.5252(7) 0.4657(3) 0.8467(2) 0.0465(9) Uani 0.517(2) 1 d . . P A 1 C6A C 0.7283(6) 0.8754(3) 0.8366(3) 0.0366(8) Uani 0.483(2) 1 d . . P A 2 C7 C 0.5846(3) 0.41527(15) 0.92041(13) 0.0537(5) Uani 0.517(2) 1 d . . P A 1 H7 H 0.502943 0.361709 0.957651 0.064 Uiso 0.517(2) 1 calc R U P A 1 C7A C 0.5962(3) 0.89369(15) 0.91760(12) 0.0483(5) Uani 0.483(2) 1 d . . P A 2 H7A H 0.646616 0.930824 0.954852 0.058 Uiso 0.483(2) 1 calc R U P A 2 C8 C 0.7637(7) 0.4352(3) 0.9488(2) 0.0587(11) Uani 0.517(2) 1 d . . P A 1 H8 H 0.798366 0.399649 1.004235 0.070 Uiso 0.517(2) 1 calc R U P A 1 C8A C 0.4121(6) 0.8625(3) 0.9429(2) 0.0429(8) Uani 0.483(2) 1 d . . P A 2 H8A H 0.336675 0.871000 0.998839 0.051 Uiso 0.483(2) 1 calc R U P A 2 C9 C 0.8864(7) 0.5105(3) 0.8900(2) 0.0483(9) Uani 0.517(2) 1 d . . P A 1 H9 H 1.011147 0.524108 0.904433 0.058 Uiso 0.517(2) 1 calc R U P A 1 C9A C 0.3282(6) 0.8162(3) 0.8856(2) 0.0352(7) Uani 0.483(2) 1 d . . P A 2 H9A H 0.190663 0.798256 0.901200 0.042 Uiso 0.483(2) 1 calc R U P A 2 C10 C 0.8276(8) 0.5646(6) 0.8117(5) 0.0394(12) Uani 0.517(2) 1 d . . P A 1 H10 H 0.913986 0.613983 0.772346 0.047 Uiso 0.517(2) 1 calc R U P A 1 C10A C 0.4437(11) 0.7966(9) 0.8066(7) 0.0292(13) Uani 0.483(2) 1 d . . P A 2 H10A H 0.384022 0.766245 0.768069 0.035 Uiso 0.483(2) 1 calc R U P A 2 C11 C 0.6414(9) 0.5482(4) 0.7886(4) 0.0330(10) Uani 0.517(2) 1 d . . P A 1 C11A C 0.6524(15) 0.8214(8) 0.7822(5) 0.0282(14) Uani 0.483(2) 1 d . . P A 2 C12 C 0.5726(6) 0.6021(5) 0.7066(5) 0.0283(8) Uani 0.517(2) 1 d . . P A 1 C12A C 0.7759(8) 0.8029(4) 0.6988(4) 0.0223(8) Uani 0.483(2) 1 d . . P A 2 C13 C 0.6594(8) 0.6958(6) 0.6464(3) 0.0241(6) Uani 0.517(2) 1 d . . P A 1 C13A C 0.7326(7) 0.7377(5) 0.6411(3) 0.0217(6) Uani 0.483(2) 1 d . . P A 2 C14 C 0.6464(4) 0.7085(2) 0.55729(19) 0.0271(6) Uani 0.517(2) 1 d . . P A 1 C15 C 0.9091(4) 0.8336(2) 0.61209(18) 0.0274(6) Uani 0.517(2) 1 d . . P A 1 C15A C 0.5019(4) 0.6168(2) 0.6089(2) 0.0276(6) Uani 0.483(2) 1 d . . P A 2 C16 C 1.0335(6) 0.9009(3) 0.6383(3) 0.0362(7) Uani 0.517(2) 1 d . . P A 1 H16 H 1.137880 0.934267 0.595919 0.043 Uiso 0.517(2) 1 calc R U P A 1 C16A C 0.3566(6) 0.5380(3) 0.6354(3) 0.0352(8) Uani 0.483(2) 1 d . . P A 2 H16A H 0.281098 0.524947 0.594226 0.042 Uiso 0.483(2) 1 calc R U P A 2 C17 C 1.0095(3) 0.92045(16) 0.72404(14) 0.0488(4) Uani 0.517(2) 1 d . . P A 1 H17 H 1.107872 0.953279 0.743763 0.059 Uiso 0.517(2) 1 calc R U P A 1 C17A C 0.3196(3) 0.47446(17) 0.72824(17) 0.0569(5) Uani 0.483(2) 1 d . . P A 2 H17A H 0.210240 0.429767 0.750444 0.068 Uiso 0.483(2) 1 calc R U P A 2 C18 C 0.8208(5) 0.8861(2) 0.7804(2) 0.0365(7) Uani 0.517(2) 1 d . . P A 1 C18A C 0.4590(5) 0.4877(3) 0.7769(2) 0.0349(7) Uani 0.483(2) 1 d . . P A 2 C19 C 0.7628(6) 0.9208(4) 0.8623(3) 0.0499(9) Uani 0.517(2) 1 d . . P A 1 H19 H 0.848205 0.965825 0.878381 0.060 Uiso 0.517(2) 1 calc R U P A 1 C19A C 0.4503(7) 0.4146(3) 0.8599(3) 0.0421(9) Uani 0.483(2) 1 d . . P A 2 H19A H 0.350855 0.362969 0.875870 0.050 Uiso 0.483(2) 1 calc R U P A 2 C20 C 0.5962(3) 0.89369(15) 0.91760(12) 0.0483(5) Uani 0.517(2) 1 d . . P A 1 H20 H 0.568703 0.913108 0.974004 0.058 Uiso 0.517(2) 1 calc R U P A 1 C20A C 0.5846(3) 0.41527(15) 0.92041(13) 0.0537(5) Uani 0.483(2) 1 d . . P A 2 H20A H 0.573761 0.369372 0.976893 0.064 Uiso 0.483(2) 1 calc R U P A 2 C21 C 0.4541(6) 0.8329(3) 0.8901(2) 0.0389(7) Uani 0.517(2) 1 d . . P A 1 H21 H 0.325438 0.819795 0.925939 0.047 Uiso 0.517(2) 1 calc R U P A 1 C21A C 0.7350(6) 0.4907(3) 0.8882(2) 0.0395(8) Uani 0.483(2) 1 d . . P A 2 H21A H 0.834982 0.490304 0.923764 0.047 Uiso 0.483(2) 1 calc R U P A 2 C22 C 0.5093(9) 0.7949(8) 0.8115(6) 0.0288(13) Uani 0.517(2) 1 d . . P A 1 H22 H 0.419307 0.753044 0.794971 0.035 Uiso 0.517(2) 1 calc R U P A 1 C22A C 0.7467(10) 0.5645(5) 0.8093(4) 0.0289(11) Uani 0.483(2) 1 d . . P A 2 H22A H 0.851081 0.613243 0.792536 0.035 Uiso 0.483(2) 1 calc R U P A 2 C23 C 0.6966(12) 0.8165(6) 0.7549(4) 0.0265(15) Uani 0.517(2) 1 d . . P A 1 C23A C 0.6024(7) 0.5679(4) 0.7526(5) 0.0245(9) Uani 0.483(2) 1 d . . P A 2 C24 C 0.7607(6) 0.7784(4) 0.6720(4) 0.0232(9) Uani 0.517(2) 1 d . . P A 1 C24A C 0.6075(7) 0.6436(6) 0.6691(4) 0.0231(7) Uani 0.483(2) 1 d . . P A 2 C25 C 0.8193(6) 0.7885(3) 0.3870(3) 0.0279(8) Uani 0.517(2) 1 d D . P A 1 C26 C 0.6649(11) 0.8569(6) 0.3431(5) 0.0305(13) Uani 0.517(2) 1 d D . P A 1 C27 C 0.690(2) 0.8705(14) 0.2534(7) 0.036(2) Uani 0.517(2) 1 d D . P A 1 H27 H 0.584579 0.917475 0.224615 0.043 Uiso 0.517(2) 1 calc R U P A 1 C28 C 0.8614(16) 0.8196(8) 0.2034(4) 0.034(3) Uani 0.517(2) 1 d D . P A 1 C29 C 1.0153(16) 0.7446(8) 0.2464(5) 0.027(2) Uani 0.517(2) 1 d D . P A 1 H29 H 1.128835 0.702674 0.214788 0.033 Uiso 0.517(2) 1 calc R U P A 1 C30 C 0.9942(11) 0.7345(6) 0.3370(5) 0.0270(13) Uani 0.517(2) 1 d D . P A 1 C31 C 0.4750(9) 0.9215(5) 0.3909(5) 0.0419(12) Uani 0.517(2) 1 d D . P A 1 H31D H 0.424966 0.872633 0.445660 0.063 Uiso 0.517(2) 1 calc R U P A 1 H31E H 0.365939 0.942483 0.354584 0.063 Uiso 0.517(2) 1 calc R U P A 1 H31F H 0.511706 0.991026 0.403465 0.063 Uiso 0.517(2) 1 calc R U P A 1 C32 C 0.888(2) 0.8354(16) 0.1044(8) 0.052(2) Uani 0.517(2) 1 d D . P A 1 H32D H 0.755638 0.832325 0.087051 0.078 Uiso 0.517(2) 1 calc R U P A 1 H32E H 0.992275 0.774224 0.084040 0.078 Uiso 0.517(2) 1 calc R U P A 1 H32F H 0.933646 0.909869 0.078400 0.078 Uiso 0.517(2) 1 calc R U P A 1 C33 C 1.1578(13) 0.6509(8) 0.3826(8) 0.0473(19) Uani 0.517(2) 1 d D . P A 1 H33D H 1.126033 0.651276 0.445325 0.071 Uiso 0.517(2) 1 calc R U P A 1 H33E H 1.294850 0.674198 0.359515 0.071 Uiso 0.517(2) 1 calc R U P A 1 H33F H 1.157429 0.573513 0.372294 0.071 Uiso 0.517(2) 1 calc R U P A 1 C40 C 0.8115(4) 0.7646(2) 0.5510(2) 0.0236(6) Uani 0.483(2) 1 d . . P A 2 N1A N 0.5294(2) 0.65730(13) 0.52563(10) 0.0393(4) Uani 0.483(2) 1 d D . P A 2 H1AA H 0.471(6) 0.642(4) 0.488(2) 0.047 Uiso 0.483(2) 1 d D U P A 2 B1 B 0.7995(5) 0.7766(3) 0.4893(2) 0.0280(7) Uani 0.517(2) 1 d . . P A 1 B1A B 0.7095(5) 0.7273(3) 0.4842(2) 0.0255(7) Uani 0.483(2) 1 d . . P A 2 C25A C 0.7689(7) 0.7604(4) 0.3821(3) 0.0270(8) Uani 0.483(2) 1 d D . P A 2 C26A C 0.6358(12) 0.8383(6) 0.3305(6) 0.0311(14) Uani 0.483(2) 1 d D . P A 2 C27A C 0.687(2) 0.8633(15) 0.2409(8) 0.033(2) Uani 0.483(2) 1 d D . P A 2 H27A H 0.591924 0.913090 0.207509 0.039 Uiso 0.483(2) 1 calc R U P A 2 C28A C 0.878(2) 0.8153(10) 0.1990(6) 0.045(3) Uani 0.483(2) 1 d D . P A 2 C29A C 1.011(2) 0.7466(12) 0.2523(7) 0.048(4) Uani 0.483(2) 1 d D . P A 2 H29A H 1.148513 0.722742 0.225977 0.058 Uiso 0.483(2) 1 calc R U P A 2 C30A C 0.9584(12) 0.7106(6) 0.3403(6) 0.0276(14) Uani 0.483(2) 1 d D . P A 2 C31A C 0.4344(10) 0.8978(6) 0.3737(5) 0.0448(14) Uani 0.483(2) 1 d D . P A 2 H31A H 0.402015 0.858789 0.434139 0.067 Uiso 0.483(2) 1 calc R U P A 2 H31B H 0.322561 0.895516 0.342227 0.067 Uiso 0.483(2) 1 calc R U P A 2 H31C H 0.448245 0.977728 0.372819 0.067 Uiso 0.483(2) 1 calc R U P A 2 C32A C 0.936(3) 0.8451(18) 0.1024(8) 0.055(3) Uani 0.483(2) 1 d D . P A 2 H32A H 0.883737 0.792724 0.074887 0.083 Uiso 0.483(2) 1 calc R U P A 2 H32B H 1.087334 0.837989 0.086768 0.083 Uiso 0.483(2) 1 calc R U P A 2 H32C H 0.875127 0.923984 0.082234 0.083 Uiso 0.483(2) 1 calc R U P A 2 C33A C 1.1089(14) 0.6258(8) 0.3889(8) 0.0422(17) Uani 0.483(2) 1 d D . P A 2 H33A H 1.099989 0.643722 0.446893 0.063 Uiso 0.483(2) 1 calc R U P A 2 H33B H 1.249906 0.629872 0.356917 0.063 Uiso 0.483(2) 1 calc R U P A 2 H33C H 1.075023 0.548349 0.394471 0.063 Uiso 0.483(2) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0422(8) 0.0321(6) 0.0303(7) -0.0038(5) -0.0040(6) 0.0005(6) N1 0.0422(8) 0.0321(6) 0.0303(7) -0.0038(5) -0.0040(6) 0.0005(6) C1 0.0434(8) 0.0390(7) 0.0393(8) -0.0170(6) -0.0143(6) 0.0046(6) C2 0.0290(15) 0.0334(16) 0.058(2) -0.0159(17) -0.0029(16) -0.0132(13) C2A 0.0278(14) 0.0262(13) 0.0422(19) -0.0039(13) -0.0043(13) -0.0112(11) C3 0.0351(14) 0.0277(13) 0.0488(19) -0.0121(13) 0.0056(14) -0.0123(11) C3A 0.0307(15) 0.0259(13) 0.0380(18) -0.0051(13) -0.0069(14) -0.0086(13) C4 0.0527(11) 0.0430(9) 0.0818(15) -0.0192(10) -0.0046(10) -0.0221(8) C4A 0.0552(11) 0.0445(9) 0.0543(11) -0.0134(8) -0.0079(8) -0.0230(8) C5 0.063(2) 0.0428(19) 0.064(3) -0.0035(19) 0.013(2) -0.0293(19) C5A 0.060(2) 0.0518(19) 0.048(2) -0.0173(17) -0.0186(19) -0.0228(17) C6 0.061(2) 0.0293(15) 0.0390(19) -0.0040(14) 0.0144(16) -0.0059(17) C6A 0.052(2) 0.0292(15) 0.035(2) -0.0118(14) -0.0141(18) -0.0070(14) C7 0.0719(13) 0.0338(8) 0.0434(10) -0.0016(7) 0.0122(9) -0.0054(8) C7A 0.0748(13) 0.0405(8) 0.0326(8) -0.0137(7) -0.0141(8) -0.0016(8) C8 0.094(3) 0.0377(17) 0.0290(17) 0.0022(14) 0.0015(18) 0.0114(18) C8A 0.067(2) 0.0329(15) 0.0261(16) -0.0081(13) -0.0027(15) -0.0020(15) C9 0.063(2) 0.0390(16) 0.0339(16) -0.0042(13) -0.0059(16) 0.0124(16) C9A 0.0440(19) 0.0279(14) 0.0286(15) -0.0025(11) -0.0008(14) -0.0005(13) C10 0.042(3) 0.0316(18) 0.036(2) -0.0049(13) -0.002(3) 0.011(3) C10A 0.032(4) 0.0243(17) 0.028(2) -0.0034(14) -0.004(3) 0.002(3) C11 0.039(3) 0.0229(18) 0.031(3) -0.004(2) 0.005(2) -0.0003(16) C11A 0.043(4) 0.0208(16) 0.021(3) -0.006(3) -0.007(3) 0.001(2) C12 0.0297(16) 0.019(2) 0.032(3) -0.0036(18) 0.004(2) -0.0038(15) C12A 0.0303(18) 0.0180(17) 0.020(3) -0.0077(15) -0.004(2) -0.0013(14) C13 0.0248(17) 0.0185(18) 0.0280(18) -0.0043(18) -0.0014(15) -0.0031(14) C13A 0.0238(16) 0.0158(16) 0.026(2) -0.0044(16) -0.0035(15) -0.0043(15) C14 0.0246(11) 0.0245(11) 0.0331(15) -0.0073(10) -0.0045(10) -0.0037(9) C15 0.0286(13) 0.0238(11) 0.0298(14) -0.0021(10) -0.0067(11) -0.0052(10) C15A 0.0269(13) 0.0247(12) 0.0322(15) -0.0100(11) -0.0005(11) -0.0054(11) C16 0.0332(16) 0.0335(15) 0.044(2) -0.0041(15) -0.0092(15) -0.0103(14) C16A 0.0355(17) 0.0348(18) 0.038(2) -0.0115(16) 0.0032(16) -0.0157(15) C17 0.0552(11) 0.0445(9) 0.0543(11) -0.0134(8) -0.0079(8) -0.0230(8) C17A 0.0527(11) 0.0430(9) 0.0818(15) -0.0192(10) -0.0046(10) -0.0221(8) C18 0.0447(17) 0.0320(14) 0.0364(18) -0.0057(12) -0.0140(15) -0.0070(12) C18A 0.0413(17) 0.0283(14) 0.0319(16) -0.0078(12) 0.0081(13) -0.0088(13) C19 0.060(2) 0.052(2) 0.043(2) -0.0159(18) -0.0156(18) -0.0044(18) C19A 0.051(2) 0.0270(17) 0.041(2) -0.0017(15) 0.0123(18) -0.0140(18) C20 0.0748(13) 0.0405(8) 0.0326(8) -0.0137(7) -0.0141(8) -0.0016(8) C20A 0.0719(13) 0.0338(8) 0.0434(10) -0.0016(7) 0.0122(9) -0.0054(8) C21 0.053(2) 0.0295(14) 0.0307(18) -0.0047(12) -0.0056(15) 0.0025(14) C21A 0.050(2) 0.0290(14) 0.0340(18) -0.0043(13) -0.0038(14) 0.0034(14) C22 0.035(4) 0.0212(15) 0.028(2) -0.0039(13) -0.003(3) 0.000(3) C22A 0.036(3) 0.0217(16) 0.0245(18) -0.0018(12) -0.004(3) 0.004(3) C23 0.037(4) 0.0212(17) 0.025(4) -0.005(3) -0.014(3) -0.004(2) C23A 0.029(2) 0.019(2) 0.024(3) -0.004(2) 0.001(2) -0.0047(14) C24 0.0285(17) 0.022(2) 0.020(3) -0.0074(15) -0.0019(16) -0.0030(16) C24A 0.0266(18) 0.018(2) 0.023(3) -0.0032(17) -0.0003(15) -0.0047(17) C25 0.0259(18) 0.0268(18) 0.0319(17) -0.0048(14) -0.0064(14) -0.0045(13) C26 0.033(2) 0.032(3) 0.029(3) -0.0043(16) -0.0068(17) -0.0090(17) C27 0.045(3) 0.028(3) 0.038(4) -0.002(3) -0.019(3) -0.009(2) C28 0.058(5) 0.034(4) 0.016(3) 0.004(2) -0.018(3) -0.017(3) C29 0.039(5) 0.028(4) 0.014(3) -0.005(2) 0.006(2) -0.012(3) C30 0.025(2) 0.026(3) 0.031(2) -0.007(2) -0.0019(17) -0.0082(18) C31 0.035(2) 0.035(3) 0.049(3) -0.0016(18) -0.0062(19) 0.0049(17) C32 0.090(6) 0.040(3) 0.031(3) -0.002(2) -0.018(3) -0.021(4) C33 0.040(4) 0.056(4) 0.045(3) -0.021(3) -0.013(3) 0.016(3) C40 0.0224(12) 0.0195(11) 0.0278(17) -0.0042(10) -0.0017(10) -0.0030(9) N1A 0.0434(8) 0.0390(7) 0.0393(8) -0.0170(6) -0.0143(6) 0.0046(6) B1 0.0259(14) 0.0271(14) 0.032(2) -0.0071(12) -0.0074(12) -0.0013(13) B1A 0.0237(14) 0.0260(14) 0.0260(17) -0.0060(12) -0.0017(12) -0.0020(13) C25A 0.028(2) 0.0272(19) 0.0265(17) -0.0046(14) -0.0024(15) -0.0083(14) C26A 0.030(2) 0.028(3) 0.036(3) -0.003(2) -0.0120(19) -0.0021(19) C27A 0.041(4) 0.034(4) 0.027(3) 0.000(2) -0.014(3) -0.010(3) C28A 0.052(5) 0.032(4) 0.052(5) -0.018(3) 0.010(3) -0.014(3) C29A 0.041(6) 0.049(6) 0.061(8) -0.025(4) -0.013(5) -0.001(4) C30A 0.030(3) 0.024(3) 0.029(2) -0.0036(19) -0.0008(19) -0.0119(18) C31A 0.039(3) 0.038(3) 0.048(3) 0.003(2) -0.004(2) 0.003(2) C32A 0.097(7) 0.044(4) 0.030(3) -0.008(2) -0.010(3) -0.021(5) C33A 0.038(4) 0.047(4) 0.040(3) -0.015(3) -0.008(3) 0.009(2) _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 C1A H1A 0.9500 . ? C1A C2A 1.474(4) . ? C1A C40 1.268(3) . ? N1 H1 0.86(2) . ? N1 C15 1.384(3) . ? N1 B1 1.517(4) . ? C1 H1B 0.9500 . ? C1 C2 1.548(5) . ? C1 C14 1.298(3) . ? C2 H2 0.9500 . ? C2 C3 1.397(6) . ? C2A H2A 0.9500 . ? C2A C3A 1.412(5) . ? C3 C4 1.302(4) . ? C3 C12 1.422(6) . ? C3A C4A 1.357(4) . ? C3A C12A 1.437(7) . ? C4 H4 0.9500 . ? C4 C5 1.484(6) . ? C4A H4A 0.9500 . ? C4A C5A 1.367(5) . ? C5 H5 0.9500 . ? C5 C6 1.438(6) . ? C5A H5A 0.9500 . ? C5A C6A 1.436(5) . ? C6 C7 1.304(4) . ? C6 C11 1.432(7) . ? C6A C7A 1.447(4) . ? C6A C11A 1.394(12) . ? C7 H7 0.9500 . ? C7 C8 1.424(5) . ? C7A H7A 0.9500 . ? C7A C8A 1.306(5) . ? C8 H8 0.9500 . ? C8 C9 1.406(6) . ? C8A H8A 0.9500 . ? C8A C9A 1.402(5) . ? C9 H9 0.9500 . ? C9 C10 1.375(8) . ? C9A H9A 0.9500 . ? C9A C10A 1.384(11) . ? C10 H10 0.9500 . ? C10 C11 1.412(7) . ? C10A H10A 0.9500 . ? C10A C11A 1.432(12) . ? C11 C12 1.453(7) . ? C11A C12A 1.456(6) . ? C12 C13 1.447(7) . ? C12A C13A 1.423(6) . ? C13 C14 1.413(4) . ? C13 C24 1.454(6) . ? C13A C24A 1.468(7) . ? C13A C40 1.418(5) . ? C14 B1 1.543(4) . ? C15 C16 1.423(4) . ? C15 C24 1.389(5) . ? C15A C16A 1.418(5) . ? C15A C24A 1.408(5) . ? C15A N1A 1.303(3) . ? C16 H16 0.9500 . ? C16 C17 1.406(4) . ? C16A H16A 0.9500 . ? C16A C17A 1.512(5) . ? C17 H17 0.9500 . ? C17 C18 1.464(4) . ? C17A H17A 0.9500 . ? C17A C18A 1.364(4) . ? C18 C19 1.413(5) . ? C18 C23 1.436(9) . ? C18A C19A 1.424(5) . ? C18A C23A 1.420(5) . ? C19 H19 0.9500 . ? C19 C20 1.318(5) . ? C19A H19A 0.9500 . ? C19A C20A 1.435(6) . ? C20 H20 0.9500 . ? C20 C21 1.467(4) . ? C20A H20A 0.9500 . ? C20A C21A 1.420(4) . ? C21 H21 0.9500 . ? C21 C22 1.382(9) . ? C21A H21A 0.9500 . ? C21A C22A 1.379(7) . ? C22 H22 0.9500 . ? C22 C23 1.418(10) . ? C22A H22A 0.9500 . ? C22A C23A 1.428(7) . ? C23 C24 1.449(7) . ? C23A C24A 1.446(7) . ? C25 C26 1.400(8) . ? C25 C30 1.413(8) . ? C25 B1 1.586(6) . ? C26 C27 1.383(11) . ? C26 C31 1.519(9) . ? C27 H27 0.9500 . ? C27 C28 1.381(12) . ? C28 C29 1.421(10) . ? C28 C32 1.528(11) . ? C29 H29 0.9500 . ? C29 C30 1.404(10) . ? C30 C33 1.530(10) . ? C31 H31D 0.9800 . ? C31 H31E 0.9800 . ? C31 H31F 0.9800 . ? C32 H32D 0.9800 . ? C32 H32E 0.9800 . ? C32 H32F 0.9800 . ? C33 H33D 0.9800 . ? C33 H33E 0.9800 . ? C33 H33F 0.9800 . ? C40 B1A 1.542(4) . ? N1A H1AA 0.84(2) . ? N1A B1A 1.548(4) . ? B1A C25A 1.578(6) . ? C25A C26A 1.416(9) . ? C25A C30A 1.402(9) . ? C26A C27A 1.383(11) . ? C26A C31A 1.513(9) . ? C27A H27A 0.9500 . ? C27A C28A 1.404(12) . ? C28A C29A 1.386(12) . ? C28A C32A 1.494(13) . ? C29A H29A 0.9500 . ? C29A C30A 1.373(12) . ? C30A C33A 1.501(11) . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 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 C2A C1A H1A 118.1 . . ? C40 C1A H1A 118.1 . . ? C40 C1A C2A 123.8(2) . . ? C15 N1 H1 121(3) . . ? C15 N1 B1 116.5(2) . . ? B1 N1 H1 122(3) . . ? C2 C1 H1B 121.9 . . ? C14 C1 H1B 121.9 . . ? C14 C1 C2 116.1(2) . . ? C1 C2 H2 120.8 . . ? C3 C2 C1 118.5(3) . . ? C3 C2 H2 120.8 . . ? C1A C2A H2A 122.4 . . ? C3A C2A C1A 115.1(2) . . ? C3A C2A H2A 122.4 . . ? C2 C3 C12 121.1(4) . . ? C4 C3 C2 114.9(3) . . ? C4 C3 C12 123.7(4) . . ? C2A C3A C12A 120.8(4) . . ? C4A C3A C2A 119.3(3) . . ? C4A C3A C12A 119.3(4) . . ? C3 C4 H4 120.0 . . ? C3 C4 C5 119.9(3) . . ? C5 C4 H4 120.0 . . ? C3A C4A H4A 117.3 . . ? C3A C4A C5A 125.4(3) . . ? C5A C4A H4A 117.3 . . ? C4 C5 H5 120.9 . . ? C6 C5 C4 118.1(3) . . ? C6 C5 H5 120.9 . . ? C4A C5A H5A 122.0 . . ? C4A C5A C6A 116.0(3) . . ? C6A C5A H5A 122.0 . . ? C7 C6 C5 120.6(4) . . ? C7 C6 C11 120.1(5) . . ? C11 C6 C5 119.2(5) . . ? C5A C6A C7A 121.6(3) . . ? C11A C6A C5A 120.7(5) . . ? C11A C6A C7A 117.4(4) . . ? C6 C7 H7 117.8 . . ? C6 C7 C8 124.3(3) . . ? C8 C7 H7 117.8 . . ? C6A C7A H7A 117.8 . . ? C8A C7A C6A 124.3(3) . . ? C8A C7A H7A 117.8 . . ? C7 C8 H8 121.9 . . ? C9 C8 C7 116.2(3) . . ? C9 C8 H8 121.9 . . ? C7A C8A H8A 120.7 . . ? C7A C8A C9A 118.6(3) . . ? C9A C8A H8A 120.7 . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.6(5) . . ? C10 C9 H9 119.7 . . ? C8A C9A H9A 119.7 . . ? C10A C9A C8A 120.7(4) . . ? C10A C9A H9A 119.7 . . ? C9 C10 H10 119.3 . . ? C9 C10 C11 121.3(7) . . ? C11 C10 H10 119.3 . . ? C9A C10A H10A 119.7 . . ? C9A C10A C11A 120.7(7) . . ? C11A C10A H10A 119.7 . . ? C6 C11 C12 118.8(6) . . ? C10 C11 C6 117.3(7) . . ? C10 C11 C12 123.7(6) . . ? C6A C11A C10A 118.0(6) . . ? C6A C11A C12A 120.0(8) . . ? C10A C11A C12A 121.6(9) . . ? C3 C12 C11 118.2(6) . . ? C3 C12 C13 116.8(6) . . ? C13 C12 C11 124.8(5) . . ? C3A C12A C11A 116.4(6) . . ? C13A C12A C3A 116.7(5) . . ? C13A C12A C11A 126.8(8) . . ? C12 C13 C24 124.0(3) . . ? C14 C13 C12 118.5(6) . . ? C14 C13 C24 117.5(6) . . ? C12A C13A C24A 123.6(4) . . ? C40 C13A C12A 119.1(5) . . ? C40 C13A C24A 117.3(5) . . ? C1 C14 C13 125.4(4) . . ? C1 C14 B1 115.4(2) . . ? C13 C14 B1 118.9(4) . . ? N1 C15 C16 114.2(3) . . ? N1 C15 C24 124.8(4) . . ? C24 C15 C16 121.0(4) . . ? C24A C15A C16A 121.1(4) . . ? N1A C15A C16A 113.9(3) . . ? N1A C15A C24A 125.0(4) . . ? C15 C16 H16 118.4 . . ? C17 C16 C15 123.1(3) . . ? C17 C16 H16 118.4 . . ? C15A C16A H16A 119.5 . . ? C15A C16A C17A 121.1(3) . . ? C17A C16A H16A 119.5 . . ? C16 C17 H17 122.7 . . ? C16 C17 C18 114.6(2) . . ? C18 C17 H17 122.7 . . ? C16A C17A H17A 123.3 . . ? C18A C17A C16A 113.3(2) . . ? C18A C17A H17A 123.3 . . ? C19 C18 C17 118.9(3) . . ? C19 C18 C23 119.7(4) . . ? C23 C18 C17 121.4(4) . . ? C17A C18A C19A 114.8(3) . . ? C17A C18A C23A 125.8(4) . . ? C23A C18A C19A 119.4(5) . . ? C18 C19 H19 118.4 . . ? C20 C19 C18 123.3(4) . . ? C20 C19 H19 118.4 . . ? C18A C19A H19A 118.4 . . ? C18A C19A C20A 123.2(4) . . ? C20A C19A H19A 118.4 . . ? C19 C20 H20 120.7 . . ? C19 C20 C21 118.5(3) . . ? C21 C20 H20 120.7 . . ? C19A C20A H20A 123.0 . . ? C21A C20A C19A 113.9(3) . . ? C21A C20A H20A 123.0 . . ? C20 C21 H21 120.3 . . ? C22 C21 C20 119.3(4) . . ? C22 C21 H21 120.3 . . ? C20A C21A H21A 117.6 . . ? C22A C21A C20A 124.8(4) . . ? C22A C21A H21A 117.6 . . ? C21 C22 H22 119.0 . . ? C21 C22 C23 121.9(6) . . ? C23 C22 H22 119.0 . . ? C21A C22A H22A 119.9 . . ? C21A C22A C23A 120.1(6) . . ? C23A C22A H22A 119.9 . . ? C18 C23 C24 119.3(6) . . ? C22 C23 C18 116.8(6) . . ? C22 C23 C24 123.8(8) . . ? C18A C23A C22A 118.1(6) . . ? C18A C23A C24A 119.2(6) . . ? C22A C23A C24A 122.5(4) . . ? C15 C24 C13 119.8(6) . . ? C15 C24 C23 117.3(6) . . ? C23 C24 C13 122.6(5) . . ? C15A C24A C13A 118.8(6) . . ? C15A C24A C23A 116.9(6) . . ? C23A C24A C13A 123.9(3) . . ? C26 C25 C30 117.9(6) . . ? C26 C25 B1 120.3(4) . . ? C30 C25 B1 121.8(4) . . ? C25 C26 C31 121.7(6) . . ? C27 C26 C25 119.2(8) . . ? C27 C26 C31 119.0(8) . . ? C26 C27 H27 118.2 . . ? C28 C27 C26 123.6(11) . . ? C28 C27 H27 118.2 . . ? C27 C28 C29 118.5(8) . . ? C27 C28 C32 123.2(9) . . ? C29 C28 C32 118.2(10) . . ? C28 C29 H29 121.1 . . ? C30 C29 C28 117.8(8) . . ? C30 C29 H29 121.1 . . ? C25 C30 C33 119.8(7) . . ? C29 C30 C25 122.6(7) . . ? C29 C30 C33 117.2(8) . . ? C26 C31 H31D 109.5 . . ? C26 C31 H31E 109.5 . . ? C26 C31 H31F 109.5 . . ? H31D C31 H31E 109.5 . . ? H31D C31 H31F 109.5 . . ? H31E C31 H31F 109.5 . . ? C28 C32 H32D 109.5 . . ? C28 C32 H32E 109.5 . . ? C28 C32 H32F 109.5 . . ? H32D C32 H32E 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? C30 C33 H33D 109.5 . . ? C30 C33 H33E 109.5 . . ? C30 C33 H33F 109.5 . . ? H33D C33 H33E 109.5 . . ? H33D C33 H33F 109.5 . . ? H33E C33 H33F 109.5 . . ? C1A C40 C13A 120.7(4) . . ? C1A C40 B1A 119.1(3) . . ? C13A C40 B1A 119.8(4) . . ? C15A N1A H1AA 128(3) . . ? C15A N1A B1A 120.0(2) . . ? B1A N1A H1AA 112(3) . . ? N1 B1 C14 116.8(3) . . ? N1 B1 C25 118.2(3) . . ? C14 B1 C25 124.9(3) . . ? C40 B1A N1A 113.9(2) . . ? C40 B1A C25A 125.0(3) . . ? N1A B1A C25A 121.1(3) . . ? C26A C25A B1A 122.3(5) . . ? C30A C25A B1A 119.4(5) . . ? C30A C25A C26A 118.3(6) . . ? C25A C26A C31A 119.8(7) . . ? C27A C26A C25A 121.6(9) . . ? C27A C26A C31A 118.6(8) . . ? C26A C27A H27A 119.9 . . ? C26A C27A C28A 120.1(12) . . ? C28A C27A H27A 119.9 . . ? C27A C28A C32A 120.1(11) . . ? C29A C28A C27A 116.5(10) . . ? C29A C28A C32A 123.2(11) . . ? C28A C29A H29A 117.6 . . ? C30A C29A C28A 124.8(10) . . ? C30A C29A H29A 117.6 . . ? C25A C30A C33A 122.5(8) . . ? C29A C30A C25A 117.9(8) . . ? C29A C30A C33A 119.5(9) . . ? C26A C31A H31A 109.5 . . ? C26A C31A H31B 109.5 . . ? C26A C31A H31C 109.5 . . ? H31A C31A H31B 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C28A C32A H32A 109.5 . . ? C28A C32A H32B 109.5 . . ? C28A C32A H32C 109.5 . . ? H32A C32A H32B 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30A C33A H33A 109.5 . . ? C30A C33A H33B 109.5 . . ? C30A C33A H33C 109.5 . . ? H33A C33A H33B 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 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 C1A C2A C3A C4A -167.4(2) . . . . ? C1A C2A C3A C12A 3.5(4) . . . . ? C1A C40 B1A N1A -175.0(2) . . . . ? C1A C40 B1A C25A 1.9(4) . . . . ? N1 C15 C16 C17 177.1(2) . . . . ? N1 C15 C24 C13 9.7(4) . . . . ? N1 C15 C24 C23 -163.2(4) . . . . ? C1 C2 C3 C4 -169.1(2) . . . . ? C1 C2 C3 C12 4.9(4) . . . . ? C1 C14 B1 N1 -175.07(19) . . . . ? C1 C14 B1 C25 0.8(4) . . . . ? C2 C1 C14 C13 2.8(3) . . . . ? C2 C1 C14 B1 175.4(2) . . . . ? C2 C3 C4 C5 176.8(3) . . . . ? C2 C3 C12 C11 -163.3(3) . . . . ? C2 C3 C12 C13 11.5(4) . . . . ? C2A C1A C40 C13A 4.2(4) . . . . ? C2A C1A C40 B1A 176.8(2) . . . . ? C2A C3A C4A C5A 177.3(3) . . . . ? C2A C3A C12A C11A -163.5(4) . . . . ? C2A C3A C12A C13A 12.9(5) . . . . ? C3 C4 C5 C6 -12.8(5) . . . . ? C3 C12 C13 C14 -21.0(4) . . . . ? C3 C12 C13 C24 159.3(3) . . . . ? C3A C4A C5A C6A -14.6(5) . . . . ? C3A C12A C13A C24A 158.8(3) . . . . ? C3A C12A C13A C40 -21.9(5) . . . . ? C4 C3 C12 C11 10.1(5) . . . . ? C4 C3 C12 C13 -175.1(3) . . . . ? C4 C5 C6 C7 -166.6(3) . . . . ? C4 C5 C6 C11 9.2(5) . . . . ? C4A C3A C12A C11A 7.4(5) . . . . ? C4A C3A C12A C13A -176.1(3) . . . . ? C4A C5A C6A C7A -165.4(3) . . . . ? C4A C5A C6A C11A 9.0(6) . . . . ? C5 C6 C7 C8 175.0(3) . . . . ? C5 C6 C11 C10 -170.9(4) . . . . ? C5 C6 C11 C12 3.5(5) . . . . ? C5A C6A C7A C8A 174.9(3) . . . . ? C5A C6A C11A C10A -169.6(6) . . . . ? C5A C6A C11A C12A 3.9(8) . . . . ? C6 C7 C8 C9 -3.2(4) . . . . ? C6 C11 C12 C3 -13.2(5) . . . . ? C6 C11 C12 C13 172.5(3) . . . . ? C6A C7A C8A C9A -5.2(4) . . . . ? C6A C11A C12A C3A -12.1(8) . . . . ? C6A C11A C12A C13A 171.9(5) . . . . ? C7 C6 C11 C10 4.9(6) . . . . ? C7 C6 C11 C12 179.3(3) . . . . ? C7 C8 C9 C10 2.9(5) . . . . ? C7A C6A C11A C10A 5.1(9) . . . . ? C7A C6A C11A C12A 178.5(4) . . . . ? C7A C8A C9A C10A 4.5(6) . . . . ? C8 C9 C10 C11 1.2(8) . . . . ? C8A C9A C10A C11A 0.9(10) . . . . ? C9 C10 C11 C6 -5.1(8) . . . . ? C9 C10 C11 C12 -179.3(4) . . . . ? C9A C10A C11A C6A -5.7(12) . . . . ? C9A C10A C11A C12A -179.1(6) . . . . ? C10 C11 C12 C3 160.9(4) . . . . ? C10 C11 C12 C13 -13.5(6) . . . . ? C10A C11A C12A C3A 161.2(7) . . . . ? C10A C11A C12A C13A -14.9(10) . . . . ? C11 C6 C7 C8 -0.8(5) . . . . ? C11 C12 C13 C14 153.4(3) . . . . ? C11 C12 C13 C24 -26.3(5) . . . . ? C11A C6A C7A C8A 0.4(5) . . . . ? C11A C12A C13A C24A -25.2(6) . . . . ? C11A C12A C13A C40 154.1(5) . . . . ? C12 C3 C4 C5 3.0(4) . . . . ? C12 C13 C14 C1 14.0(4) . . . . ? C12 C13 C14 B1 -158.3(3) . . . . ? C12 C13 C24 C15 153.6(3) . . . . ? C12 C13 C24 C23 -34.0(5) . . . . ? C12A C3A C4A C5A 6.3(5) . . . . ? C12A C13A C24A C15A 153.7(3) . . . . ? C12A C13A C24A C23A -33.2(5) . . . . ? C12A C13A C40 C1A 13.9(4) . . . . ? C12A C13A C40 B1A -158.7(3) . . . . ? C13 C14 B1 N1 -2.0(4) . . . . ? C13 C14 B1 C25 173.9(3) . . . . ? C13A C40 B1A N1A -2.4(3) . . . . ? C13A C40 B1A C25A 174.5(3) . . . . ? C14 C1 C2 C3 -12.4(3) . . . . ? C14 C13 C24 C15 -26.2(4) . . . . ? C14 C13 C24 C23 146.3(4) . . . . ? C15 N1 B1 C14 -13.9(3) . . . . ? C15 N1 B1 C25 170.0(2) . . . . ? C15 C16 C17 C18 -11.8(4) . . . . ? C15A C16A C17A C18A -9.4(4) . . . . ? C15A N1A B1A C40 -12.9(3) . . . . ? C15A N1A B1A C25A 170.1(3) . . . . ? C16 C15 C24 C13 -170.1(3) . . . . ? C16 C15 C24 C23 17.0(5) . . . . ? C16 C17 C18 C19 -168.6(3) . . . . ? C16 C17 C18 C23 12.6(5) . . . . ? C16A C15A C24A C13A -171.1(3) . . . . ? C16A C15A C24A C23A 15.3(4) . . . . ? C16A C15A N1A B1A -169.4(2) . . . . ? C16A C17A C18A C19A -170.2(3) . . . . ? C16A C17A C18A C23A 11.5(4) . . . . ? C17 C18 C19 C20 -179.7(3) . . . . ? C17 C18 C23 C22 -175.7(5) . . . . ? C17 C18 C23 C24 0.7(7) . . . . ? C17A C18A C19A C20A 179.8(3) . . . . ? C17A C18A C23A C22A -175.8(4) . . . . ? C17A C18A C23A C24A -0.4(5) . . . . ? C18 C19 C20 C21 -5.3(5) . . . . ? C18 C23 C24 C13 171.7(4) . . . . ? C18 C23 C24 C15 -15.7(7) . . . . ? C18A C19A C20A C21A -3.4(4) . . . . ? C18A C23A C24A C13A 173.2(3) . . . . ? C18A C23A C24A C15A -13.5(4) . . . . ? C19 C18 C23 C22 5.5(8) . . . . ? C19 C18 C23 C24 -178.1(4) . . . . ? C19 C20 C21 C22 7.0(5) . . . . ? C19A C18A C23A C22A 5.9(5) . . . . ? C19A C18A C23A C24A -178.6(3) . . . . ? C19A C20A C21A C22A 4.8(5) . . . . ? C20 C21 C22 C23 -2.4(9) . . . . ? C20A C21A C22A C23A -0.8(7) . . . . ? C21 C22 C23 C18 -3.7(10) . . . . ? C21 C22 C23 C24 180.0(5) . . . . ? C21A C22A C23A C18A -4.8(7) . . . . ? C21A C22A C23A C24A 180.0(4) . . . . ? C22 C23 C24 C13 -12.1(8) . . . . ? C22 C23 C24 C15 160.5(6) . . . . ? C22A C23A C24A C13A -11.6(5) . . . . ? C22A C23A C24A C15A 161.7(4) . . . . ? C23 C18 C19 C20 -0.9(6) . . . . ? C23A C18A C19A C20A -1.8(5) . . . . ? C24 C13 C14 C1 -166.2(3) . . . . ? C24 C13 C14 B1 21.4(4) . . . . ? C24 C15 C16 C17 -3.0(4) . . . . ? C24A C13A C40 C1A -166.8(2) . . . . ? C24A C13A C40 B1A 20.6(4) . . . . ? C24A C15A C16A C17A -3.9(4) . . . . ? C24A C15A N1A B1A 8.9(4) . . . . ? C25 C26 C27 C28 0.3(16) . . . . ? C26 C25 C30 C29 -1.8(8) . . . . ? C26 C25 C30 C33 -174.8(5) . . . . ? C26 C25 B1 N1 -111.7(4) . . . . ? C26 C25 B1 C14 72.5(5) . . . . ? C26 C27 C28 C29 3.2(17) . . . . ? C26 C27 C28 C32 -179.9(13) . . . . ? C27 C28 C29 C30 -5.7(14) . . . . ? C28 C29 C30 C25 5.1(12) . . . . ? C28 C29 C30 C33 178.3(8) . . . . ? C30 C25 C26 C27 -1.0(9) . . . . ? C30 C25 C26 C31 -177.9(5) . . . . ? C30 C25 B1 N1 66.0(5) . . . . ? C30 C25 B1 C14 -109.8(4) . . . . ? C31 C26 C27 C28 177.2(11) . . . . ? C32 C28 C29 C30 177.2(10) . . . . ? C40 C1A C2A C3A -12.9(3) . . . . ? C40 C13A C24A C15A -25.7(4) . . . . ? C40 C13A C24A C23A 147.5(3) . . . . ? C40 B1A C25A C26A -109.2(5) . . . . ? C40 B1A C25A C30A 71.5(5) . . . . ? N1A C15A C16A C17A 174.4(2) . . . . ? N1A C15A C24A C13A 10.8(4) . . . . ? N1A C15A C24A C23A -162.9(3) . . . . ? N1A B1A C25A C26A 67.5(5) . . . . ? N1A B1A C25A C30A -111.8(4) . . . . ? B1 N1 C15 C16 -169.7(2) . . . . ? B1 N1 C15 C24 10.5(3) . . . . ? B1 C25 C26 C27 176.8(8) . . . . ? B1 C25 C26 C31 -0.1(8) . . . . ? B1 C25 C30 C29 -179.5(6) . . . . ? B1 C25 C30 C33 7.5(7) . . . . ? B1A C25A C26A C27A -177.6(9) . . . . ? B1A C25A C26A C31A 3.5(8) . . . . ? B1A C25A C30A C29A -176.0(8) . . . . ? B1A C25A C30A C33A 0.2(8) . . . . ? C25A C26A C27A C28A -2.9(18) . . . . ? C26A C25A C30A C29A 4.7(10) . . . . ? C26A C25A C30A C33A -179.1(6) . . . . ? C26A C27A C28A C29A -2.1(19) . . . . ? C26A C27A C28A C32A -178.1(14) . . . . ? C27A C28A C29A C30A 9(2) . . . . ? C28A C29A C30A C25A -10.5(18) . . . . ? C28A C29A C30A C33A 173.2(11) . . . . ? C30A C25A C26A C27A 1.6(12) . . . . ? C30A C25A C26A C31A -177.3(5) . . . . ? C31A C26A C27A C28A 175.9(11) . . . . ? C32A C28A C29A C30A -175.0(13) . . . . ? _shelx_res_file ; TITL p-1_a.res in P-1 mi21007c.res created by SHELXL-2018/3 at 17:10:54 on 10-May-2021 REM Old TITL p-1 in P-1 REM SHELXT solution in P-1 REM R1 0.351, Rweak 0.068, Alpha 0.142, Orientation as input REM Formula found by SHELXT: C8 B6 N12 CELL 1.54184 6.640859 12.050433 15.913779 78.0611 78.9022 79.9008 ZERR 2 0.000215 0.000411 0.000613 0.0031 0.003 0.0028 LATT 1 SFAC C H B N UNIT 66 52 2 2 EADP N1 C1A SADI C26 C31 C26A C31A FLAT C26 C27 C28 C29 C30 SADI C29 C30 C29A C30A FLAT C25 C26 C27 C28 C29 C30 SADI C25 C26 C25A C26A EADP C1 N1A RIGU C25 C26 C27 C28 C29 C30 SADI C25 C30 C25A C30A RIGU C26 C27 C28 C29 C30 SADI C26 C27 C26A C27A EADP C4 C17A SADI C25 B1 C25A B1 EADP C17 C4A SADI C25 B1A C25A B1A EADP C7 C20A EADP C20 C7A SADI 0.04 C30 B1A C30A B1A SADI 0.04 C27 C29 C27A C29A DFIX 0.83 N1A H1Aa DFIX 0.84 N1 H1 SADI 0.04 C27 C32 C27A C32A SADI C28 C29 C28A C29A SADI 0.04 C28 C30 C28A C30A SADI 0.04 C29 C32 C29A C32A SADI C27 C28 C27A C28A SADI 0.04 C27 C31 C27A C31A SADI C28 C32 C28A C32A SADI 0.04 C29 C33 C29A C33A SADI 0.04 C30 B1 C30A B1 SADI 0.04 C25 C27 C25A C27A SADI 0.04 C25 C29 C25A C29A SADI 0.04 C25 C31 C25A C31A SADI 0.04 C25 C33 C25A C33A SADI C30 C33 C30A C33A SADI 0.04 C26 C28 C26A C28A SADI 0.04 C26 C30 C26A C30A SADI 0.04 C26 B1 C26A B1 SADI 0.04 C26 B1A C26A B1A EXYZ N1 C1A EXYZ C1 N1A EXYZ C4 C17A EXYZ C17 C4A EXYZ C7 C20A EXYZ C20 C7A L.S. 16 PLAN 1 SIZE 0.033 0.251 0.368 TEMP -153.15(10) CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.115100 EXTI 0.008083 BASF 0.24725 FVAR 7.46428 0.51692 PART 2 C1A 1 0.950847 0.829275 0.524078 -21.00000 0.04219 0.03212 = 0.03025 -0.00383 -0.00396 0.00045 AFIX 43 H1A 2 0.992835 0.849461 0.463029 -21.00000 -1.20000 AFIX 0 PART 1 N1 4 0.950847 0.829275 0.524078 21.00000 0.04219 0.03212 = 0.03025 -0.00383 -0.00396 0.00045 H1 2 1.049779 0.861250 0.490176 21.00000 -1.20000 C1 1 0.529412 0.657299 0.525628 21.00000 0.04336 0.03903 = 0.03933 -0.01704 -0.01434 0.00462 AFIX 43 H1B 2 0.531099 0.666305 0.464774 21.00000 -1.20000 AFIX 0 C2 1 0.387006 0.580782 0.592747 21.00000 0.02901 0.03338 = 0.05845 -0.01594 -0.00290 -0.01319 AFIX 43 H2 2 0.278649 0.552870 0.575687 21.00000 -1.20000 AFIX 0 PART 2 C2A 1 1.051398 0.874892 0.581960 -21.00000 0.02777 0.02620 = 0.04220 -0.00392 -0.00432 -0.01116 AFIX 43 H2A 2 1.173261 0.910124 0.561719 -21.00000 -1.20000 AFIX 0 PART 1 C3 1 0.421410 0.553677 0.679009 21.00000 0.03506 0.02766 = 0.04882 -0.01214 0.00565 -0.01228 PART 2 C3A 1 0.953382 0.862409 0.669701 -21.00000 0.03067 0.02589 = 0.03800 -0.00513 -0.00689 -0.00861 PART 1 C4 1 0.319649 0.474461 0.728241 21.00000 0.05271 0.04304 = 0.08178 -0.01923 -0.00465 -0.02213 AFIX 43 H4 2 0.225013 0.442677 0.705469 21.00000 -1.20000 AFIX 0 PART 2 C4A 1 1.009522 0.920447 0.724043 -21.00000 0.05518 0.04451 = 0.05433 -0.01336 -0.00792 -0.02296 AFIX 43 H4A 2 1.118466 0.965254 0.700968 -21.00000 -1.20000 AFIX 0 PART 1 C5 1 0.351605 0.433834 0.819991 21.00000 0.06282 0.04279 = 0.06382 -0.00349 0.01282 -0.02931 AFIX 43 H5 2 0.259975 0.388067 0.859955 21.00000 -1.20000 AFIX 0 PART 2 C5A 1 0.922231 0.919759 0.809266 -21.00000 0.06043 0.05182 = 0.04777 -0.01734 -0.01855 -0.02277 AFIX 43 H5A 2 0.986056 0.947021 0.848073 -21.00000 -1.20000 AFIX 0 PART 1 C6 1 0.525219 0.465725 0.846663 21.00000 0.06086 0.02929 = 0.03896 -0.00400 0.01436 -0.00592 PART 2 C6A 1 0.728340 0.875382 0.836636 -21.00000 0.05202 0.02921 = 0.03462 -0.01181 -0.01414 -0.00699 PART 1 C7 1 0.584575 0.415269 0.920406 21.00000 0.07194 0.03385 = 0.04342 -0.00159 0.01217 -0.00544 AFIX 43 H7 2 0.502943 0.361709 0.957651 21.00000 -1.20000 AFIX 0 PART 2 C7A 1 0.596187 0.893687 0.917605 -21.00000 0.07482 0.04053 = 0.03263 -0.01375 -0.01410 -0.00158 AFIX 43 H7A 2 0.646616 0.930824 0.954852 -21.00000 -1.20000 AFIX 0 PART 1 C8 1 0.763746 0.435190 0.948772 21.00000 0.09354 0.03765 = 0.02901 0.00215 0.00151 0.01137 AFIX 43 H8 2 0.798366 0.399649 1.004235 21.00000 -1.20000 AFIX 0 PART 2 C8A 1 0.412083 0.862513 0.942872 -21.00000 0.06699 0.03293 = 0.02606 -0.00810 -0.00265 -0.00200 AFIX 43 H8A 2 0.336675 0.871000 0.998839 -21.00000 -1.20000 AFIX 0 PART 1 C9 1 0.886445 0.510490 0.889960 21.00000 0.06286 0.03902 = 0.03392 -0.00416 -0.00591 0.01244 AFIX 43 H9 2 1.011147 0.524108 0.904433 21.00000 -1.20000 AFIX 0 PART 2 C9A 1 0.328177 0.816249 0.885592 -21.00000 0.04404 0.02795 = 0.02865 -0.00248 -0.00081 -0.00051 AFIX 43 H9A 2 0.190663 0.798256 0.901200 -21.00000 -1.20000 AFIX 0 PART 1 C10 1 0.827604 0.564599 0.811688 21.00000 0.04178 0.03160 = 0.03640 -0.00489 -0.00235 0.01139 AFIX 43 H10 2 0.913986 0.613983 0.772346 21.00000 -1.20000 AFIX 0 PART 2 C10A 1 0.443726 0.796551 0.806555 -21.00000 0.03188 0.02431 = 0.02825 -0.00340 -0.00426 0.00229 AFIX 43 H10A 2 0.384022 0.766245 0.768069 -21.00000 -1.20000 AFIX 0 PART 1 C11 1 0.641414 0.548216 0.788645 21.00000 0.03890 0.02288 = 0.03083 -0.00355 0.00465 -0.00026 PART 2 C11A 1 0.652377 0.821392 0.782206 -21.00000 0.04286 0.02079 = 0.02091 -0.00600 -0.00723 0.00067 PART 1 C12 1 0.572636 0.602057 0.706566 21.00000 0.02973 0.01939 = 0.03182 -0.00365 0.00418 -0.00380 PART 2 C12A 1 0.775903 0.802936 0.698847 -21.00000 0.03032 0.01804 = 0.01966 -0.00773 -0.00432 -0.00134 PART 1 C13 1 0.659364 0.695809 0.646435 21.00000 0.02484 0.01846 = 0.02796 -0.00426 -0.00145 -0.00311 PART 2 C13A 1 0.732608 0.737748 0.641073 -21.00000 0.02380 0.01581 = 0.02608 -0.00443 -0.00353 -0.00429 PART 1 C14 1 0.646428 0.708467 0.557285 21.00000 0.02465 0.02448 = 0.03309 -0.00728 -0.00455 -0.00368 C15 1 0.909063 0.833599 0.612086 21.00000 0.02861 0.02380 = 0.02984 -0.00207 -0.00670 -0.00518 PART 2 C15A 1 0.501924 0.616795 0.608875 -21.00000 0.02686 0.02469 = 0.03223 -0.00996 -0.00050 -0.00544 PART 1 C16 1 1.033545 0.900917 0.638330 21.00000 0.03321 0.03349 = 0.04388 -0.00415 -0.00920 -0.01031 AFIX 43 H16 2 1.137880 0.934267 0.595919 21.00000 -1.20000 AFIX 0 PART 2 C16A 1 0.356553 0.538019 0.635420 -21.00000 0.03545 0.03480 = 0.03792 -0.01148 0.00319 -0.01569 AFIX 43 H16A 2 0.281098 0.524947 0.594226 -21.00000 -1.20000 AFIX 0 PART 1 C17 1 1.009522 0.920447 0.724043 21.00000 0.05518 0.04451 = 0.05433 -0.01336 -0.00792 -0.02296 AFIX 43 H17 2 1.107872 0.953279 0.743763 21.00000 -1.20000 AFIX 0 PART 2 C17A 1 0.319649 0.474461 0.728241 -21.00000 0.05271 0.04304 = 0.08178 -0.01923 -0.00465 -0.02213 AFIX 43 H17A 2 0.210240 0.429767 0.750444 -21.00000 -1.20000 AFIX 0 PART 1 C18 1 0.820766 0.886116 0.780446 21.00000 0.04470 0.03199 = 0.03640 -0.00572 -0.01396 -0.00704 PART 2 C18A 1 0.459020 0.487658 0.776935 -21.00000 0.04127 0.02826 = 0.03188 -0.00782 0.00811 -0.00884 PART 1 C19 1 0.762815 0.920766 0.862346 21.00000 0.06046 0.05152 = 0.04280 -0.01593 -0.01557 -0.00444 AFIX 43 H19 2 0.848205 0.965825 0.878381 21.00000 -1.20000 AFIX 0 PART 2 C19A 1 0.450324 0.414623 0.859853 -21.00000 0.05138 0.02701 = 0.04086 -0.00170 0.01229 -0.01400 AFIX 43 H19A 2 0.350855 0.362969 0.875870 -21.00000 -1.20000 AFIX 0 PART 1 C20 1 0.596187 0.893687 0.917605 21.00000 0.07482 0.04053 = 0.03263 -0.01375 -0.01410 -0.00158 AFIX 43 H20 2 0.568703 0.913108 0.974004 21.00000 -1.20000 AFIX 0 PART 2 C20A 1 0.584575 0.415269 0.920406 -21.00000 0.07194 0.03385 = 0.04342 -0.00159 0.01217 -0.00544 AFIX 43 H20A 2 0.573761 0.369372 0.976893 -21.00000 -1.20000 AFIX 0 PART 1 C21 1 0.454083 0.832891 0.890101 21.00000 0.05276 0.02947 = 0.03070 -0.00468 -0.00564 0.00250 AFIX 43 H21 2 0.325438 0.819795 0.925939 21.00000 -1.20000 AFIX 0 PART 2 C21A 1 0.735009 0.490715 0.888242 -21.00000 0.05034 0.02901 = 0.03398 -0.00430 -0.00383 0.00342 AFIX 43 H21A 2 0.834982 0.490304 0.923764 -21.00000 -1.20000 AFIX 0 PART 1 C22 1 0.509345 0.794888 0.811522 21.00000 0.03499 0.02122 = 0.02785 -0.00385 -0.00309 -0.00034 AFIX 43 H22 2 0.419307 0.753044 0.794971 21.00000 -1.20000 AFIX 0 PART 2 C22A 1 0.746737 0.564536 0.809266 -21.00000 0.03630 0.02170 = 0.02455 -0.00184 -0.00403 0.00367 AFIX 43 H22A 2 0.851081 0.613243 0.792536 -21.00000 -1.20000 AFIX 0 PART 1 C23 1 0.696552 0.816525 0.754857 21.00000 0.03702 0.02118 = 0.02544 -0.00522 -0.01354 -0.00447 PART 2 C23A 1 0.602352 0.567925 0.752567 -21.00000 0.02874 0.01906 = 0.02388 -0.00396 0.00128 -0.00469 PART 1 C24 1 0.760666 0.778359 0.671964 21.00000 0.02852 0.02196 = 0.01960 -0.00741 -0.00189 -0.00296 PART 2 C24A 1 0.607456 0.643635 0.669113 -21.00000 0.02655 0.01846 = 0.02303 -0.00323 -0.00034 -0.00473 PART 1 C25 1 0.819292 0.788463 0.387012 21.00000 0.02587 0.02681 = 0.03190 -0.00476 -0.00640 -0.00450 C26 1 0.664926 0.856898 0.343111 21.00000 0.03288 0.03175 = 0.02884 -0.00431 -0.00677 -0.00895 C27 1 0.690476 0.870506 0.253439 21.00000 0.04502 0.02827 = 0.03803 -0.00161 -0.01863 -0.00931 AFIX 43 H27 2 0.584579 0.917475 0.224615 21.00000 -1.20000 AFIX 0 C28 1 0.861371 0.819617 0.203448 21.00000 0.05779 0.03398 = 0.01627 0.00413 -0.01791 -0.01688 C29 1 1.015300 0.744632 0.246385 21.00000 0.03858 0.02815 = 0.01383 -0.00489 0.00596 -0.01229 AFIX 43 H29 2 1.128835 0.702674 0.214788 21.00000 -1.20000 AFIX 0 C30 1 0.994200 0.734547 0.337011 21.00000 0.02517 0.02588 = 0.03125 -0.00689 -0.00194 -0.00815 C31 1 0.475043 0.921489 0.390948 21.00000 0.03527 0.03523 = 0.04867 -0.00158 -0.00620 0.00485 AFIX 137 H31D 2 0.424966 0.872633 0.445660 21.00000 -1.50000 H31E 2 0.365939 0.942483 0.354584 21.00000 -1.50000 H31F 2 0.511706 0.991026 0.403465 21.00000 -1.50000 AFIX 0 C32 1 0.888131 0.835426 0.104350 21.00000 0.09046 0.03960 = 0.03140 -0.00151 -0.01775 -0.02119 AFIX 137 H32D 2 0.755638 0.832325 0.087051 21.00000 -1.50000 H32E 2 0.992275 0.774224 0.084040 21.00000 -1.50000 H32F 2 0.933646 0.909869 0.078400 21.00000 -1.50000 AFIX 0 C33 1 1.157838 0.650861 0.382638 21.00000 0.04001 0.05602 = 0.04491 -0.02057 -0.01297 0.01619 AFIX 137 H33D 2 1.126033 0.651276 0.445325 21.00000 -1.50000 H33E 2 1.294850 0.674198 0.359515 21.00000 -1.50000 H33F 2 1.157429 0.573513 0.372294 21.00000 -1.50000 AFIX 0 PART 2 C40 1 0.811509 0.764633 0.551017 -21.00000 0.02243 0.01950 = 0.02784 -0.00424 -0.00173 -0.00305 N1A 4 0.529412 0.657299 0.525628 -21.00000 0.04336 0.03903 = 0.03933 -0.01704 -0.01434 0.00462 H1AA 2 0.471204 0.642291 0.487695 -21.00000 -1.20000 PART 1 B1 3 0.799488 0.776615 0.489322 21.00000 0.02586 0.02714 = 0.03191 -0.00714 -0.00738 -0.00134 PART 2 B1A 3 0.709453 0.727297 0.484153 -21.00000 0.02369 0.02600 = 0.02596 -0.00597 -0.00165 -0.00200 C25A 1 0.768887 0.760419 0.382130 -21.00000 0.02812 0.02719 = 0.02653 -0.00461 -0.00245 -0.00830 C26A 1 0.635837 0.838291 0.330527 -21.00000 0.03009 0.02784 = 0.03603 -0.00282 -0.01204 -0.00208 C27A 1 0.686747 0.863311 0.240859 -21.00000 0.04090 0.03351 = 0.02705 -0.00008 -0.01410 -0.00972 AFIX 43 H27A 2 0.591924 0.913090 0.207509 -21.00000 -1.20000 AFIX 0 C28A 1 0.878328 0.815267 0.199035 -21.00000 0.05179 0.03164 = 0.05166 -0.01841 0.01012 -0.01381 C29A 1 1.011017 0.746618 0.252302 -21.00000 0.04054 0.04901 = 0.06105 -0.02530 -0.01301 -0.00083 AFIX 43 H29A 2 1.148513 0.722742 0.225977 -21.00000 -1.20000 AFIX 0 C30A 1 0.958417 0.710574 0.340301 -21.00000 0.03040 0.02416 = 0.02899 -0.00360 -0.00075 -0.01193 C31A 1 0.434419 0.897826 0.373735 -21.00000 0.03925 0.03828 = 0.04762 0.00254 -0.00356 0.00349 AFIX 137 H31A 2 0.402015 0.858789 0.434139 -21.00000 -1.50000 H31B 2 0.322561 0.895516 0.342227 -21.00000 -1.50000 H31C 2 0.448245 0.977728 0.372819 -21.00000 -1.50000 AFIX 0 C32A 1 0.936103 0.845054 0.102417 -21.00000 0.09688 0.04377 = 0.03014 -0.00840 -0.00975 -0.02088 AFIX 137 H32A 2 0.883737 0.792724 0.074887 -21.00000 -1.50000 H32B 2 1.087334 0.837989 0.086768 -21.00000 -1.50000 H32C 2 0.875127 0.923984 0.082234 -21.00000 -1.50000 AFIX 0 C33A 1 1.108887 0.625773 0.388858 -21.00000 0.03767 0.04734 = 0.03957 -0.01479 -0.00759 0.00926 AFIX 137 H33A 2 1.099989 0.643722 0.446893 -21.00000 -1.50000 H33B 2 1.249906 0.629872 0.356917 -21.00000 -1.50000 H33C 2 1.075023 0.548349 0.394471 -21.00000 -1.50000 AFIX 0 HKLF 5 REM p-1_a.res in P-1 REM wR2 = 0.1660, GooF = S = 1.053, Restrained GooF = 1.052 for all data REM R1 = 0.0571 for 7191 Fo > 4sig(Fo) and 0.0683 for all 9193 data REM 592 parameters refined using 64 restraints END WGHT 0.1151 0.0000 REM Highest difference peak 0.184, deepest hole -0.208, 1-sigma level 0.046 Q1 1 0.2083 0.4257 0.7242 11.00000 0.05 0.18 ; _shelx_res_checksum 77693 _shelx_hkl_file ; 0 0 2 184771. 753.240 -2 0 0 2 184771. 753.240 1 0 0 3 6303.82 178.868 -2 0 0 3 6303.82 178.868 1 0 0 4 58108.4 602.861 -2 0 0 4 58108.4 602.861 1 0 0 -5 208.691 37.7593 -2 0 0 -5 208.691 37.7593 1 0 0 6 9554.68 120.000 -2 0 0 6 9554.68 120.000 1 0 0 7 138746. 523.129 -2 0 0 7 138746. 523.129 1 0 0 8 8581.35 151.332 -2 0 0 8 8581.35 151.332 1 0 0 9 2111.09 88.6371 -2 0 0 9 2111.09 88.6371 1 0 0 -10 2312.46 98.8182 -2 0 0 -10 2312.46 98.8182 1 0 0 -11 4113.30 133.409 -2 0 0 -11 4113.30 133.409 1 0 0 -12 57.3151 55.7708 -2 0 0 -12 57.3151 55.7708 1 0 0 -13 100.128 48.8589 -2 0 0 -13 100.128 48.8589 1 0 0 -14 5105.45 100.772 -2 0 0 -14 5105.45 100.772 1 0 0 15 2212.14 76.3913 -2 0 0 15 2212.14 76.3913 1 0 0 -16 114.357 40.0554 -2 0 0 -16 114.357 40.0554 1 0 0 17 95.8632 40.8559 -2 0 0 17 95.8632 40.8559 1 0 0 -18 78.7689 37.2447 -2 0 0 -18 78.7689 37.2447 1 0 0 -19 44.8768 49.7646 -2 0 0 -19 44.8768 49.7646 1 0 1 -19 0.07158 41.1970 1 0 -1 18 324.504 36.3537 1 0 1 -17 1.63271 27.5006 1 0 -1 16 707.523 47.6784 1 0 1 -15 81.9336 41.0336 1 0 1 -14 8.02557 37.6614 1 0 -1 13 842.967 64.9936 1 0 1 -12 518.375 81.0997 1 0 1 -11 2103.98 111.706 1 0 1 -10 22.0039 40.3413 1 0 -1 9 541.072 50.7450 1 0 -1 8 728.404 59.6137 1 0 -1 7 20359.7 188.361 1 0 1 -6 23997.7 183.835 1 0 -1 5 1283.85 48.7914 1 0 -1 4 10028.0 76.5836 1 0 -1 3 2381.03 60.1833 1 0 1 -2 90.4056 24.9227 1 0 -1 1 12263.5 111.982 1 0 -1 0 3393.24 45.9650 1 0 -1 -1 18757.6 148.197 1 0 1 2 771.514 41.5125 1 0 1 3 54.8408 28.0077 1 0 1 4 12357.7 129.157 1 0 1 5 5676.04 117.564 1 0 1 6 9786.99 164.716 1 0 1 7 41794.0 424.056 1 0 1 8 3828.43 107.867 1 0 1 9 4955.26 129.571 1 0 -1 -10 29.9448 49.1019 1 0 1 11 849.315 78.0524 1 0 1 12 106.345 62.3861 1 0 -1 -13 772.106 71.1497 1 0 1 14 285.759 33.6600 1 0 1 15 165.167 37.6846 1 0 -1 -16 380.283 40.0712 1 0 1 17 164.326 34.4495 1 0 -1 -18 571.287 34.5826 1 0 -1 -19 17.8298 26.7312 1 0 -2 -19 122.368 49.9042 -2 0 2 -18 122.368 49.9042 1 0 -2 -18 56.6801 44.6678 -2 0 2 -17 56.6801 44.6678 1 0 -2 -17 195.179 48.7457 -2 0 2 -16 195.179 48.7457 1 0 2 16 373.681 61.5798 -2 0 -2 15 373.681 61.5798 1 0 -2 -15 2446.74 105.165 -2 0 2 -14 2446.74 105.165 1 0 -2 -14 999.166 68.7085 -2 0 2 -13 999.166 68.7085 1 0 -2 -13 3473.11 274.390 -2 0 2 -12 3473.11 274.390 1 0 -2 -12 481.681 103.218 -2 0 2 -11 481.681 103.218 1 0 -2 -11 619.419 99.8212 -2 0 2 -10 619.419 99.8212 1 0 -2 -10 10311.8 262.166 -2 0 2 -9 10311.8 262.166 1 0 -2 -9 4911.63 175.660 -2 0 2 -8 4911.63 175.660 1 0 -2 -8 23306.1 332.792 -2 0 2 -7 23306.1 332.792 1 0 -2 -7 30893.6 240.346 -2 0 2 -6 30893.6 240.346 1 0 2 6 5145.82 97.9665 -2 0 -2 5 5145.82 97.9665 1 0 2 5 207.784 39.6668 -2 0 -2 4 207.784 39.6668 1 0 2 4 18412.4 192.220 -2 0 -2 3 18412.4 192.220 1 0 2 3 31472.0 266.228 -2 0 -2 2 31472.0 266.228 1 0 -2 -2 234936. 774.788 -2 0 2 -1 234936. 774.788 1 0 -2 -1 30412.1 182.026 -2 0 2 0 30412.1 182.026 1 0 -2 0 43060.1 240.841 -2 0 2 1 43060.1 240.841 1 0 -2 1 207487. 613.640 -2 0 2 2 207487. 613.640 1 0 -2 2 32492.3 311.704 -2 0 2 3 32492.3 311.704 1 0 -2 3 20889.9 205.534 -2 0 2 4 20889.9 205.534 1 0 -2 4 511.728 52.3626 -2 0 2 5 511.728 52.3626 1 0 -2 5 7205.07 137.610 -2 0 2 6 7205.07 137.610 1 0 -2 6 27645.6 484.526 -2 0 2 7 27645.6 484.526 1 0 -2 7 16759.6 408.330 -2 0 2 8 16759.6 408.330 1 0 -2 8 9007.00 325.964 -2 0 2 9 9007.00 325.964 1 0 2 -9 8965.06 240.020 -2 0 -2 -10 8965.06 240.020 1 0 2 -10 863.805 105.084 -2 0 -2 -11 863.805 105.084 1 0 2 -11 469.170 99.8584 -2 0 -2 -12 469.170 99.8584 1 0 2 -12 2502.83 163.411 -2 0 -2 -13 2502.83 163.411 1 0 2 -13 1508.46 63.2272 -2 0 -2 -14 1508.46 63.2272 1 0 2 -14 1893.77 71.5533 -2 0 -2 -15 1893.77 71.5533 1 0 -2 15 457.770 45.7235 -2 0 2 16 457.770 45.7235 1 0 -2 16 17.0809 49.7837 -2 0 2 17 17.0809 49.7837 1 0 -2 17 25.3693 48.8334 -2 0 2 18 25.3693 48.8334 1 0 2 -18 169.446 34.7132 -2 0 -2 -19 169.446 34.7132 1 0 -3 18 477.123 37.8746 1 0 -3 17 41.8097 28.3645 1 0 3 -16 32.1347 31.3492 1 0 3 -15 811.514 50.1598 1 0 3 -14 64.0470 41.9281 1 0 3 -13 3420.75 77.0222 1 0 3 -12 147.323 39.6087 1 0 3 -11 805.464 139.520 1 0 3 -10 5098.38 161.416 1 0 3 -9 7905.28 187.538 1 0 3 -8 100.163 57.3179 1 0 3 -7 4946.91 133.866 1 0 3 -6 14354.3 202.931 1 0 3 -5 2128.64 82.1571 1 0 3 -4 26.4658 21.7393 1 0 3 -3 1179.45 38.0839 1 0 3 -2 30355.0 176.996 1 0 3 -1 2554.66 68.3343 1 0 -3 0 392132. 777.743 1 0 3 1 148289. 385.270 1 0 -3 -2 89153.0 355.051 1 0 3 3 83031.2 430.034 1 0 3 4 1353.48 44.2895 1 0 3 5 770.808 34.8372 1 0 3 6 5667.67 105.298 1 0 3 7 14600.7 271.967 1 0 3 8 63.0783 69.6470 1 0 3 9 1906.14 131.407 1 0 3 10 6401.30 227.057 1 0 3 11 759.626 79.4037 1 0 3 12 334.323 71.4996 1 0 -3 -13 137.020 46.6918 1 0 -3 -14 6612.11 88.8397 1 0 3 15 175.311 37.0282 1 0 3 16 178.098 40.0873 1 0 -3 -17 412.276 38.1202 1 0 -3 -18 32.6142 30.4985 1 0 3 19 1641.22 35.8270 1 0 -4 17 410.299 55.8442 1 0 4 19 349.665 51.9578 -2 0 -4 17 349.665 51.9578 1 0 -4 -18 1835.49 62.6168 -2 0 4 -16 1835.49 62.6168 1 0 -4 -17 754.684 53.3383 -2 0 4 -15 754.684 53.3383 1 0 -4 -16 198.872 52.6225 -2 0 4 -14 198.872 52.6225 1 0 -4 -15 8123.53 137.336 -2 0 4 -13 8123.53 137.336 1 0 -4 -14 79.4292 50.4539 -2 0 4 -12 79.4292 50.4539 1 0 -4 -13 3394.17 91.1419 -2 0 4 -11 3394.17 91.1419 1 0 -4 -12 4421.07 271.672 -2 0 4 -10 4421.07 271.672 1 0 -4 -11 5214.86 276.121 -2 0 4 -9 5214.86 276.121 1 0 -4 -10 1532.65 114.533 -2 0 4 -8 1532.65 114.533 1 0 -4 -9 918.706 94.5551 -2 0 4 -7 918.706 94.5551 1 0 -4 -8 236.100 73.9096 -2 0 4 -6 236.100 73.9096 1 0 -4 -7 982.942 88.2185 -2 0 4 -5 982.942 88.2185 1 0 -4 -6 30161.7 143.757 -2 0 4 -4 30161.7 143.757 1 0 -4 -5 2479.44 56.8869 -2 0 4 -3 2479.44 56.8869 1 0 -4 -4 2537.17 56.4236 -2 0 4 -2 2537.17 56.4236 1 0 -4 -3 6417.02 65.6178 -2 0 4 -1 6417.02 65.6178 1 0 -4 -2 82825.4 224.320 -2 0 4 0 82825.4 224.320 1 0 4 1 135.777 24.2796 -2 0 -4 -1 135.777 24.2796 1 0 -4 0 80179.2 238.838 -2 0 4 2 80179.2 238.838 1 0 -4 1 12972.6 103.049 -2 0 4 3 12972.6 103.049 1 0 -4 2 954.468 39.9572 -2 0 4 4 954.468 39.9572 1 0 -4 3 1207.01 44.4583 -2 0 4 5 1207.01 44.4583 1 0 -4 4 25725.9 132.676 -2 0 4 6 25725.9 132.676 1 0 -4 5 1934.49 98.4604 -2 0 4 7 1934.49 98.4604 1 0 -4 6 209.343 71.0570 -2 0 4 8 209.343 71.0570 1 0 -4 7 595.795 85.5195 -2 0 4 9 595.795 85.5195 1 0 -4 8 842.222 95.2159 -2 0 4 10 842.222 95.2159 1 0 -4 9 7205.19 208.570 -2 0 4 11 7205.19 208.570 1 0 -4 10 4593.25 126.950 -2 0 4 12 4593.25 126.950 1 0 -4 11 1095.15 64.6498 -2 0 4 13 1095.15 64.6498 1 0 4 -12 32.8788 60.2445 -2 0 -4 -14 32.8788 60.2445 1 0 4 -13 9296.40 146.075 -2 0 -4 -15 9296.40 146.075 1 0 -4 14 116.480 51.2634 -2 0 4 16 116.480 51.2634 1 0 4 -15 399.223 48.6184 -2 0 -4 -17 399.223 48.6184 1 0 4 -16 1148.61 64.3954 -2 0 -4 -18 1148.61 64.3954 1 0 4 19 11.1785 20.4098 1 0 -4 17 114.512 76.8638 -2 0 4 19 114.512 76.8638 1 0 -5 17-4.39958 37.8301 1 0 5 -16 2483.21 63.3935 1 0 -5 15 70.4395 33.1386 1 0 -5 14 981.156 48.5788 1 0 -5 13 311.117 42.4459 1 0 5 -12 4512.68 88.3442 1 0 5 -11 827.064 52.7576 1 0 5 -10 22929.8 226.158 1 0 5 -9 5697.06 276.425 1 0 5 -8 4024.44 222.332 1 0 5 -7 122.183 57.0756 1 0 5 -6 2480.46 109.671 1 0 5 -5 613.479 65.1085 1 0 5 -4 23.2354 24.9226 1 0 5 -3 22050.1 126.308 1 0 5 -2 139.592 27.8558 1 0 5 -1 1677.31 41.3286 1 0 5 0 81.7308 25.3898 1 0 5 1 227.193 26.9322 1 0 5 2 659.691 31.7430 1 0 5 3 188.470 28.0616 1 0 5 4 3085.20 53.5153 1 0 5 5 19051.7 114.067 1 0 5 6 569.196 31.2678 1 0 5 7 152.164 36.4845 1 0 5 8 3596.87 114.934 1 0 5 9 982.750 76.5033 1 0 5 10 3625.04 187.364 1 0 5 11 2446.46 116.018 1 0 5 12 25211.8 335.765 1 0 5 13 5534.49 111.848 1 0 -5 -14 6164.70 115.985 1 0 5 15 3256.51 94.8893 1 0 5 16 212.685 44.8221 1 0 5 17 401.388 38.2636 1 0 5 18 365.414 32.2903 1 0 5 19 661.618 28.5300 1 0 -6 16 1828.01 85.4841 1 0 -6 15 346.051 38.4071 1 0 6 -14 3491.28 85.4828 1 0 -6 -17 4008.92 163.862 -2 0 6 -14 4008.92 163.862 1 0 -6 13 246.785 59.1675 1 0 -6 -16 467.330 63.0476 -2 0 6 -13 467.330 63.0476 1 0 6 -12 904.449 117.112 1 0 -6 -15 693.930 73.1546 -2 0 6 -12 693.930 73.1546 1 0 6 -11 1099.15 130.372 1 0 -6 -14 1443.82 81.8941 -2 0 6 -11 1443.82 81.8941 1 0 -6 -13 5032.50 99.3228 -2 0 6 -10 5032.50 99.3228 1 0 -6 -12 19171.3 189.964 -2 0 6 -9 19171.3 189.964 1 0 -6 -11 1537.16 126.647 -2 0 6 -8 1537.16 126.647 1 0 -6 -10 267.087 92.7731 -2 0 6 -7 267.087 92.7731 1 0 -6 -9 5688.76 136.153 -2 0 6 -6 5688.76 136.153 1 0 -6 -8 3269.64 106.142 -2 0 6 -5 3269.64 106.142 1 0 -6 -7 5332.39 72.4375 -2 0 6 -4 5332.39 72.4375 1 0 -6 -6 43398.0 213.905 -2 0 6 -3 43398.0 213.905 1 0 -6 -5 10451.4 109.736 -2 0 6 -2 10451.4 109.736 1 0 6 -1 2379.50 97.4823 1 0 -6 -4 2032.64 59.1975 -2 0 6 -1 2032.64 59.1975 1 0 6 0 2017.89 95.8440 1 0 -6 -3 2953.84 75.4224 -2 0 6 0 2953.84 75.4224 1 0 -6 -2 5906.46 90.4451 -2 0 6 1 5906.46 90.4451 1 0 -6 -1 3800.82 77.1433 -2 0 6 2 3800.82 77.1433 1 0 -6 0 4021.19 91.2093 -2 0 6 3 4021.19 91.2093 1 0 -6 1 1547.26 57.9375 -2 0 6 4 1547.26 57.9375 1 0 -6 2 18697.9 145.207 -2 0 6 5 18697.9 145.207 1 0 -6 3 37440.0 205.180 -2 0 6 6 37440.0 205.180 1 0 6 7 4237.02 139.324 1 0 -6 4 5573.62 87.5778 -2 0 6 7 5573.62 87.5778 1 0 -6 5 2021.14 150.433 -2 0 6 8 2021.14 150.433 1 0 -6 6 5968.51 231.642 -2 0 6 9 5968.51 231.642 1 0 -6 7 832.421 96.2356 -2 0 6 10 832.421 96.2356 1 0 -6 8 891.586 106.370 -2 0 6 11 891.586 106.370 1 0 6 12 2469.49 175.511 1 0 -6 9 7464.83 143.292 -2 0 6 12 7464.83 143.292 1 0 -6 10 5209.40 125.621 -2 0 6 13 5209.40 125.621 1 0 -6 11 512.379 59.0714 -2 0 6 14 512.379 59.0714 1 0 6 -12 214.922 61.8495 -2 0 -6 -15 214.922 61.8495 1 0 6 16 912.803 78.6912 1 0 -6 13 997.511 77.6902 -2 0 6 16 997.511 77.6902 1 0 6 17 1989.93 57.0828 1 0 -6 -18 308.586 29.6159 1 0 6 19 3421.30 51.0528 1 0 -7 15 888.233 69.4909 1 0 -7 14 0.74177 31.7908 1 0 7 -13 248.603 36.5510 1 0 7 -12 872.696 75.7411 1 0 7 -11 433.522 47.9503 1 0 7 -10 6464.36 128.934 1 0 7 -9 10294.3 161.039 1 0 7 -8 8403.83 114.894 1 0 7 -7 3266.18 217.470 1 0 7 -6 158.956 92.3048 1 0 7 -5 130.290 96.1589 1 0 7 -4 732.329 38.7696 1 0 -7 -7 935.588 122.970 -2 0 7 -4 935.588 122.970 1 0 7 -3 461.648 35.6028 1 0 -7 -6 527.702 112.889 -2 0 7 -3 527.702 112.889 1 0 7 -2 1621.75 58.1691 1 0 -7 -5 2356.00 154.268 -2 0 7 -2 2356.00 154.268 1 0 7 -1 2812.26 82.5728 1 0 -7 -4 3199.91 122.527 -2 0 7 -1 3199.91 122.527 1 0 7 0 2255.00 56.1706 1 0 -7 -3 2675.54 155.618 -2 0 7 0 2675.54 155.618 1 0 7 1 791.063 42.7712 1 0 -7 -2 1093.31 124.628 -2 0 7 1 1093.31 124.628 1 0 7 2 908.757 41.4634 1 0 7 3 507.319 41.2793 1 0 7 4 400.043 38.7775 1 0 7 5 1017.75 49.9116 1 0 7 6 8.25664 32.5700 1 0 7 7 757.559 36.4082 1 0 7 8 189.203 59.6293 1 0 7 9 1847.37 104.230 1 0 7 10 5675.30 168.018 1 0 7 11 2566.03 67.2595 1 0 7 12 17415.3 141.316 1 0 7 13 5706.66 85.3405 1 0 7 14 906.631 55.6185 1 0 7 15 530.981 41.0406 1 0 -7 -16 448.964 36.6769 1 0 7 17 185.295 30.8628 1 0 -7 -18 262.190 23.6776 1 0 -8 14 559.635 64.1221 1 0 -8 13 39.7141 26.9532 1 0 8 -12 57.2807 39.6336 1 0 8 -11 574.527 45.2534 1 0 8 -10 4896.63 101.865 1 0 8 -9 1598.42 102.667 1 0 -8 -13 3250.98 191.828 -2 0 8 -9 3250.98 191.828 1 0 8 -8 21234.9 200.759 1 0 -8 -12 21880.8 328.240 -2 0 8 -8 21880.8 328.240 1 0 8 -7 2822.69 101.888 1 0 -8 -11 4601.83 136.299 -2 0 8 -7 4601.83 136.299 1 0 8 -6 516.289 123.802 1 0 -8 -10 848.666 67.2904 -2 0 8 -6 848.666 67.2904 1 0 -8 -9 246.371 135.458 -2 0 8 -5 246.371 135.458 1 0 8 -4 5609.77 137.312 1 0 -8 -8 5266.53 263.796 -2 0 8 -4 5266.53 263.796 1 0 8 -3 9260.76 125.297 1 0 -8 -7 12381.2 245.908 -2 0 8 -3 12381.2 245.908 1 0 8 -2 552.060 46.3075 1 0 -8 -6 2680.65 136.431 -2 0 8 -2 2680.65 136.431 1 0 8 -1 10093.3 133.691 1 0 -8 -5 12194.4 251.419 -2 0 8 -1 12194.4 251.419 1 0 8 0 1907.28 77.5827 1 0 -8 -4 2583.63 180.132 -2 0 8 0 2583.63 180.132 1 0 8 1 356.147 41.0613 1 0 -8 -3 2165.21 168.723 -2 0 8 1 2165.21 168.723 1 0 8 2 10684.9 137.502 1 0 8 3 4468.80 93.7971 1 0 8 4 1247.21 58.4631 1 0 8 5 3777.92 79.3546 1 0 8 6 6316.08 98.1552 1 0 8 7 9963.03 119.737 1 0 8 8 2226.45 165.333 1 0 8 9 540.076 104.678 1 0 8 10 1327.84 67.6733 1 0 -8 6 1387.70 121.912 -2 0 8 10 1387.70 121.912 1 0 8 11 5867.09 139.048 1 0 -8 7 5717.18 99.3798 -2 0 8 11 5717.18 99.3798 1 0 8 12 8654.34 127.605 1 0 8 -8 12808.5 200.797 -2 0 -8 -12 12808.5 200.797 1 0 8 13 5005.80 108.021 1 0 -8 9 5126.75 168.944 -2 0 8 13 5126.75 168.944 1 0 -8 -14 1312.98 57.8968 1 0 8 15 18.0425 28.8919 1 0 -8 -16 99.5147 34.1245 1 0 8 17 92.2661 26.0846 1 0 8 18 1306.09 32.0767 1 0 9 -13 33.9816 29.5712 1 0 9 -12 27.8772 31.3611 1 0 9 -11 45.2648 35.0733 1 0 9 -10 336.086 41.1672 1 0 9 -9 4579.52 98.3082 1 0 9 -8 3832.37 90.3664 1 0 -9 -12 4765.41 219.327 -2 0 9 -8 4765.41 219.327 1 0 9 -7 622.153 50.1841 1 0 -9 -11 785.649 98.8047 -2 0 9 -7 785.649 98.8047 1 0 9 -6 2750.69 102.067 1 0 -9 -10 3222.83 117.661 -2 0 9 -6 3222.83 117.661 1 0 9 -5 803.169 83.0536 1 0 -9 -9 777.173 64.5050 -2 0 9 -5 777.173 64.5050 1 0 9 -4 1202.60 86.2949 1 0 -9 -8 1622.09 84.6019 -2 0 9 -4 1622.09 84.6019 1 0 9 -3 7600.00 120.044 1 0 -9 -7 9465.96 347.015 -2 0 9 -3 9465.96 347.015 1 0 9 -2 93.1893 37.6953 1 0 9 -1 10176.2 144.094 1 0 -9 -5 17679.1 394.948 -2 0 9 -1 17679.1 394.948 1 0 9 0 131.385 39.2891 1 0 -9 -4 303.512 123.974 -2 0 9 0 303.512 123.974 1 0 9 1 9726.44 143.068 1 0 9 2 271.086 37.7626 1 0 9 3 11644.2 138.308 1 0 9 4 236.702 39.1188 1 0 9 5 10399.3 132.394 1 0 9 6 37.3623 36.1946 1 0 9 7 8743.41 119.408 1 0 9 8 1035.76 134.139 1 0 -9 4 1506.01 72.5073 -2 0 9 8 1506.01 72.5073 1 0 9 9 307.220 91.1376 1 0 -9 5 452.361 60.3746 -2 0 9 9 452.361 60.3746 1 0 9 10 940.399 89.3499 1 0 -9 6 1557.52 82.9234 -2 0 9 10 1557.52 82.9234 1 0 9 11 326.795 60.4924 1 0 -9 7 481.877 79.7579 -2 0 9 11 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3797.28 153.962 2 2 6 -15 90.5071 27.0898 2 2 6 -14 13.0023 25.0943 2 2 6 -13 2.46955 30.8041 2 -2 -6 12 302.333 40.7181 2 -2 -6 11 24.4108 42.4954 2 2 6 -10 795.935 55.8908 2 2 6 -9 143.095 42.4156 2 -2 -6 8 222.742 46.2014 2 2 6 -7 710.115 91.6158 2 2 6 -6 6095.19 185.294 2 2 6 -5 1150.22 92.2211 2 2 6 -4 223.434 65.7607 2 2 6 -3 589.303 98.4122 2 2 6 -2 3628.01 164.026 2 2 6 -1 32.4811 67.1821 2 2 6 0 2632.22 95.2962 2 2 6 1 2877.19 96.9533 2 -2 -6 -2 13803.5 303.776 2 -2 -6 -3 5997.48 212.119 2 -2 -6 -4 1737.38 86.6454 2 -2 -6 -5 774.876 68.6048 2 -2 -6 -6 3845.47 124.017 2 -2 -6 -7-2.64668 56.5066 2 2 6 8 184.703 46.0750 2 -2 -6 -9 308.496 67.9729 2 -2 -6 -10 4806.78 163.001 2 -2 -6 -11 1883.49 118.251 2 -2 -6 -12 936.376 102.215 2 -2 -6 -13 459.944 42.1159 2 -2 -6 -14 1260.42 54.2332 2 -2 -6 -15 12.0931 59.6920 2 2 6 16 201.525 42.2455 2 2 6 17 225.193 36.3473 2 2 6 18 181.699 31.1852 2 2 6 19 112.570 27.0476 2 2 7 -14 346.845 29.9534 2 2 7 -13 1268.15 39.5058 2 -2 -7 12 41.8966 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891.490 55.4658 2 3 -6 -2 890.852 54.9046 2 3 -6 -1 680.732 51.0631 2 3 -6 0 52.9854 38.8582 2 3 -6 1 35.7175 39.1999 2 3 -6 2 1030.52 58.1375 2 3 -6 3 1432.45 63.6258 2 3 -6 4 1108.48 53.9125 2 3 -6 5 1843.10 80.3391 2 3 -6 6 690.302 45.3882 2 3 -6 7 2268.23 52.3640 2 3 -6 8 94.7700 36.3160 2 3 -6 9 142.652 34.0777 2 3 -6 10 193.334 37.2281 2 3 -6 11 20.0145 31.8073 2 3 -6 12-0.44085 28.9354 2 -3 6 -13 426.381 32.5184 2 -3 6 -14 91.3229 30.1485 2 3 -6 15 44.3901 27.6425 2 -3 4 16 56.6875 27.2461 2 3 -4 -15 278.225 39.6660 2 3 -4 -14 326.221 39.7279 2 3 -4 -13 42.0442 35.3988 2 3 -4 -12 432.080 52.3311 2 3 -4 -11 393.796 62.5116 2 3 -4 -10 1203.86 69.6944 2 3 -4 -9 931.564 65.7456 2 3 -4 -8 68.3956 110.350 2 3 -4 -7 559.787 126.951 2 3 -4 -6 76.6882 102.049 2 3 -4 -5 128.757 35.6084 2 3 -4 -4 2614.01 72.0265 2 3 -4 -3 596.610 39.1940 2 3 -4 -2 2583.59 63.0573 2 3 -4 -1 2091.10 61.1539 2 3 -4 0 71.3042 31.1838 2 3 -4 1 792.294 44.2512 2 3 -4 2 3112.95 72.5962 2 3 -4 3 167.336 35.6375 2 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1031.84 168.961 2 -5 -7 -9 298.696 94.9804 2 5 7 15 707.871 83.5491 2 5 7 16-5.34946 53.5317 2 5 7 17 14.1364 24.5104 2 -5 -8 9 674.209 33.9700 2 5 8 -8 286.193 26.2523 2 -5 -8 7 221.289 28.8975 2 -5 -8 6 23.3511 29.3506 2 -5 -8 5 42.8112 33.3058 2 -5 -8 4-3.78963 35.4881 2 -5 -8 3 190.850 54.8520 2 -5 -8 2 100.836 52.1819 2 -5 -8 1 91.5003 43.8482 2 5 8 0 92.2787 46.6225 2 5 8 1 714.487 43.8825 2 5 8 2 56.7376 34.6096 2 5 8 3 79.2946 33.8636 2 5 8 4 36.9648 34.4640 2 5 8 5 182.665 33.1419 2 5 8 6 64.4258 33.0093 2 5 8 7 1155.89 53.1831 2 5 8 8 107.791 39.5247 2 5 8 9 205.551 38.8986 2 5 8 10 112.162 47.3763 2 -5 -8 -11 0.51716 32.6664 2 5 8 12-20.3175 36.2608 2 5 8 13 166.445 36.5328 2 5 8 14-7.68401 30.4336 2 5 8 15 61.9460 32.6917 2 5 8 16 1625.28 46.4841 2 5 9 10 396.652 87.7343 2 5 10 -6 12.9137 22.1240 2 -5 -10 5 30.3006 20.6412 2 -5 -10 4-5.03699 23.0080 2 -5 -10 3 15.2860 24.9725 2 -5 -10 2 371.479 32.4106 2 5 10 -1 223.791 31.2457 2 -5 -10 0-8.70757 33.2312 2 -5 -10 -1-2.04763 34.8938 2 -5 -10 -2 434.715 45.4337 2 5 10 3 42.0169 38.0650 2 -5 -10 -4 45.7386 39.7653 2 -5 -10 -5 203.914 40.9859 2 5 10 6 333.942 39.8544 2 5 10 7 179.934 41.1980 2 5 10 8 18.6648 28.3608 2 5 10 9 82.8228 28.4758 2 5 10 10 414.932 32.1173 2 -5 -10 -11 82.6225 29.2887 2 5 10 12 52.7880 30.1789 2 5 10 13-10.8146 27.0489 2 5 10 14 60.6287 33.3411 2 -5 -10 -15 395.545 35.5842 2 5 12 -2 693.717 45.2330 2 -5 -12 1 25.3870 28.6199 2 -5 -12 0 283.539 23.1328 2 5 12 1 48.3199 21.2768 2 5 12 2 405.034 32.8500 2 -5 -12 -3 327.975 33.6420 2 5 12 4 693.018 40.2478 2 5 12 5 224.917 32.9149 2 5 12 6 505.119 43.8090 2 5 12 7 153.843 36.2508 2 5 12 8 295.600 28.7231 2 5 12 9 277.320 23.4252 2 5 12 10 125.711 18.2238 2 -5 -12 -11 407.034 26.8536 2 5 12 12 387.618 47.2465 2 6 -7 -6 269.478 49.0811 2 6 -7 -5 17.6528 27.5062 2 6 -7 -4 192.654 33.3927 2 6 -7 -3 258.237 34.7913 2 6 -7 -2 378.369 33.1525 2 6 -7 -1-3.09032 27.7109 2 6 -7 0 11.3972 26.2562 2 6 -7 1 28.3052 30.2258 2 6 -7 2 30.9002 29.9992 2 6 -7 3 180.080 44.9621 2 6 -7 4 138.094 56.3429 2 6 -7 5 527.739 60.3501 2 6 -5 -8 49.5482 28.3824 2 6 -5 -7 57.3898 23.4605 2 6 -5 -6 195.535 32.4479 2 6 -5 -5 30.1593 36.4659 2 6 -5 -4 4.91063 40.6639 2 6 -5 -3 1284.44 50.5656 2 6 -5 -2 214.375 36.5243 2 6 -5 -1 637.915 37.3190 2 6 -5 0 94.5643 26.9242 2 6 -5 1-6.26354 28.5415 2 6 -5 2 26.4400 31.2066 2 6 -5 3 813.553 38.2728 2 6 -5 4 18.5997 30.1099 2 6 -5 5 1190.39 54.3229 2 6 -5 6-4.83365 66.5690 2 6 -5 7 15.6579 67.3864 2 6 -5 8 165.521 69.2581 2 6 -5 9 75.1473 44.5885 2 6 -5 10 5.37352 36.2385 2 6 -5 11 65.5866 31.3087 2 6 -4 -9 171.798 28.9011 2 6 -4 -8 50.4391 24.5510 2 6 -4 -7 27.4066 61.6037 2 6 -4 -6 70.7003 31.3750 2 6 -4 -5 577.777 50.8941 2 6 -4 -4 920.384 58.4414 2 6 -4 -3 434.992 46.4107 2 6 -4 -2 68.8239 44.9160 2 6 -4 -1 15.0690 36.4808 2 6 -4 0-24.3969 35.5486 2 6 -4 1 424.457 54.8766 2 6 -4 2 305.628 36.8605 2 6 -4 3 6.27097 44.2288 2 6 -4 4 114.782 46.7454 2 6 -4 5 21.5436 81.1740 2 6 -4 6 1058.31 62.4193 2 6 -4 7 396.300 87.7621 2 6 -4 8 482.738 63.3127 2 6 -4 9 12.0846 64.1684 2 6 -4 10 57.1967 65.1738 2 6 -4 11 20.8042 38.3644 2 6 -4 12 120.185 27.4732 2 6 -3 -10 83.9894 30.7971 2 6 -3 -9 72.5835 21.2169 2 6 -3 -8 676.098 41.0153 2 6 -3 -7 111.330 46.9769 2 6 -3 -6 163.224 41.0156 2 6 -3 -5 102.666 50.7670 2 6 -3 -4 84.9219 43.2999 2 6 -3 -3 205.286 87.2907 2 6 -3 -2 196.441 63.7336 2 6 -3 -1 59.1038 72.4726 2 6 -3 0 70.7796 96.5309 2 6 -3 1 186.975 61.2300 2 6 -3 2 152.209 62.7536 2 6 -3 3 176.701 62.9780 2 6 -3 4 123.559 58.2476 2 6 -3 5 107.450 89.6578 2 6 -3 6 87.9897 59.9896 2 6 -3 7 14.8243 47.2323 2 6 -3 8 211.123 85.1584 2 6 -3 9 34.2852 55.2161 2 6 -3 10-16.7714 50.5663 2 6 -3 11 755.963 50.6836 2 6 -3 12 132.990 33.8060 2 6 -3 13 85.8236 34.1245 2 6 -2 -10 172.594 26.0223 2 6 -2 -9 100.754 25.9954 2 6 -2 -8 2.88044 28.9370 2 6 -2 -7 46.3094 31.8823 2 6 -2 -6 1452.24 66.4118 2 6 -2 -5 282.923 38.9743 2 6 -2 -4 12.5545 40.4045 2 6 -2 -3 209.839 36.7396 2 6 -2 -2 90.8283 34.6086 2 6 -2 -1 143.159 34.3717 2 6 -2 0 70.5681 31.7398 2 6 -2 1 110.908 32.2361 2 6 -2 2 556.737 34.2216 2 6 -2 3 210.948 31.7003 2 6 -2 4 24.1415 34.1334 2 6 -2 5 157.871 41.0138 2 6 -2 6 0.79542 36.2510 2 6 -2 7 12.4131 34.6140 2 6 -2 8-6.25441 42.8810 2 6 -2 9 672.174 52.1178 2 6 -2 10 1111.66 50.4612 2 6 -2 11 112.755 32.7430 2 6 -2 12 6.53908 28.3496 2 6 -2 13 14.7171 24.1964 2 6 -2 14 187.390 50.7423 2 6 -1 -10-17.4886 35.7114 2 6 -1 -9 465.731 69.8199 2 6 -1 8 39.5914 59.6830 2 6 -1 11 230.857 80.5673 2 6 -1 14 15.2886 38.4653 2 6 0 -10 13.4983 29.6478 2 6 0 -9-8.39446 25.3403 2 6 0 -8 39.3825 24.7690 2 6 0 -7 166.192 29.1775 2 6 0 -6 263.129 33.0885 2 6 0 -5 1790.77 63.8111 2 6 0 -4 150.511 52.0042 2 6 0 -3 1459.84 59.9151 2 6 0 -2 143.498 39.9568 2 6 0 -1 188.915 38.6364 2 6 0 0 281.058 37.6117 2 6 0 1 792.375 50.3832 2 6 0 2 2752.54 65.6557 2 6 0 3 816.048 46.5701 2 6 0 4 868.961 46.1325 2 6 0 5 149.107 36.1828 2 6 0 6 116.841 35.1094 2 6 0 7 520.137 38.6692 2 6 0 8 1871.88 52.6671 2 6 0 9 341.173 38.4015 2 6 0 10 1590.55 51.3820 2 6 0 11 111.513 41.5625 2 6 0 12 44.0206 37.7114 2 6 0 13-5.72131 33.2279 2 6 0 14 16.5302 28.2539 2 6 0 15 42.7091 28.9513 2 6 2 -10 79.2131 23.6866 2 6 2 -9 95.7276 27.0668 2 6 2 -8 16.2382 29.2090 2 6 2 -7 28.1014 29.2042 2 6 2 -6-3.72725 31.4300 2 6 2 -5 368.755 43.8429 2 6 2 -4 103.916 41.2798 2 6 2 -3 413.095 52.5347 2 6 2 -2 283.400 42.9576 2 6 2 -1 3.21714 32.7833 2 6 2 0 649.287 42.6040 2 6 2 1 199.915 35.0818 2 6 2 2 702.029 42.0868 2 6 2 3 3132.86 62.0591 2 6 2 4 161.484 31.1364 2 6 2 5 652.229 33.4677 2 6 2 6 173.590 30.6248 2 6 2 7 490.811 33.3235 2 6 2 8 20.2113 32.9180 2 6 2 9 592.153 44.4462 2 6 2 10 242.901 35.0326 2 6 2 11 133.862 39.9767 2 6 2 12 10.7099 34.8969 2 6 2 13-0.40255 34.6737 2 6 2 14 41.5619 27.1012 2 6 2 15 276.812 31.2419 2 6 2 16 67.2052 32.7459 2 -6 -4 9 81.3463 24.0881 2 -6 -4 8 88.4177 29.0019 2 6 4 -7 62.0240 31.7426 2 6 4 -6 25.1724 34.5568 2 6 4 -5 28.2829 43.0559 2 6 4 -4 67.3156 48.6393 2 6 4 -3 519.982 61.5156 2 6 4 -2 860.865 57.2831 2 6 4 -1 184.039 43.3372 2 6 4 0 376.968 38.8457 2 6 4 1 640.188 43.6147 2 6 4 2 3307.13 59.4770 2 6 4 3 46.2891 30.8681 2 6 4 4 869.406 40.0770 2 6 4 5 2836.07 52.9556 2 6 4 6 553.049 33.5704 2 6 4 7 129.817 34.0729 2 6 4 8 1317.76 54.2242 2 6 4 9 106.520 33.0589 2 6 4 10 241.595 42.1850 2 6 4 11-4.21952 36.1225 2 6 4 12 106.599 31.3776 2 6 4 13 30.1565 30.8028 2 6 4 14-0.86241 33.1617 2 6 4 15 66.0041 34.9218 2 6 4 16 5.02389 33.2653 2 -6 -6 8 50.7390 23.0637 2 6 6 -7 129.633 28.0620 2 -6 -6 6 249.099 29.9811 2 -6 -6 5 5.54287 27.2180 2 6 6 -4 86.4206 36.4946 2 6 6 -3 38.0832 37.9779 2 6 6 -2 260.092 36.4500 2 6 6 -1 1530.71 53.7153 2 6 6 0 27.7795 35.2718 2 6 6 1 83.3888 33.5419 2 6 6 2-10.5014 36.8982 2 6 6 3 23.2548 31.6862 2 6 6 4 58.0577 30.6502 2 6 6 5-16.5755 33.9592 2 6 6 6-2.17410 35.6117 2 6 6 7 71.3115 38.8939 2 6 6 8 652.668 48.1840 2 6 6 9 902.733 45.6084 2 6 6 10 40.7121 46.5437 2 6 6 11-9.99834 35.8817 2 6 6 12 61.2342 31.8514 2 6 6 13 67.9709 29.0997 2 6 6 14 499.475 36.4781 2 6 6 15 19.3159 30.3565 2 -6 -6 -16-0.46158 39.7206 2 -6 -8 6 231.664 29.1894 2 -6 -8 5 66.3625 20.9325 2 -6 -8 4 285.213 29.3985 2 -6 -8 3 106.810 33.7289 2 -6 -8 2 15.9560 30.3671 2 -6 -8 1 29.9558 28.1886 2 -6 -8 0 13.7771 29.9139 2 6 8 1 35.0330 30.7307 2 -6 -8 -2 113.819 35.2355 2 -6 -8 -3-5.58473 35.8029 2 -6 -8 -4 4.00841 34.9000 2 6 8 5 1.53062 37.5826 2 6 8 6 27.2458 39.1788 2 6 8 7 248.626 37.6030 2 6 8 8 5.23461 32.3690 2 6 8 9 35.4147 36.4125 2 6 8 10 19.6551 29.7761 2 6 8 11 44.4898 38.4440 2 6 8 12 362.375 41.4667 2 6 8 13 30.1502 27.1193 2 -6 -8 -14 451.102 33.4956 2 6 9 -5 225.419 48.6447 2 -6 -10 3 77.5673 26.5000 2 -6 -10 2 422.727 29.8167 2 -6 -10 1 190.126 33.1865 2 -6 -10 0 27.6967 30.2113 2 -6 -10 -1 20.0616 33.5191 2 -6 -10 -2 55.2586 36.2798 2 -6 -10 -3-7.34895 36.4133 2 6 10 4 183.392 41.2992 2 6 10 5 384.502 44.4479 2 -6 -10 -6-6.03756 37.3696 2 6 10 7 71.3820 27.7289 2 6 10 8 4.85659 26.6045 2 6 10 9 50.7919 24.8477 2 -6 -10 -10 130.282 22.5043 2 6 10 11 816.247 41.5517 2 6 10 12 27.8395 33.0761 2 6 10 13 552.003 52.1752 2 -6 -11 1 697.651 58.8651 2 6 12 3 15.2546 21.9543 2 6 12 4 374.844 24.9600 2 6 12 5 293.499 24.7377 2 6 12 6 402.326 26.0046 2 6 12 7 20.7284 19.7629 2 6 12 8 111.766 37.4648 2 7 -4 -5 24.8413 42.7817 2 7 -4 -4 27.0185 35.4797 2 7 -4 -3 52.9110 31.3100 2 7 -4 -2 93.7114 59.6444 2 7 -4 -1-14.7262 42.7193 2 7 -4 0 31.3987 64.7681 2 7 -4 1-21.0665 41.6112 2 7 -4 2 17.2654 33.8665 2 7 -4 3 35.7485 35.0090 2 7 -4 4-30.0858 33.7788 2 7 -4 5 53.9304 39.1904 2 7 -4 6 174.818 53.5747 2 7 -4 7 86.1360 47.1179 2 7 -4 8 67.3881 45.4679 2 7 -2 -6 27.9745 34.7116 2 7 -2 -5 813.439 55.3097 2 7 -2 -4 444.432 32.8634 2 7 -2 -3 3.49515 31.9459 2 7 -2 -2 112.970 31.7157 2 7 -2 -1 81.4104 35.2926 2 7 -2 0 22.3479 29.8552 2 7 -2 1-6.59737 33.7825 2 7 -2 2 12.9721 33.9108 2 7 -2 3 71.2951 34.5005 2 7 -2 4 220.848 29.9790 2 7 -2 5 29.4959 25.3022 2 7 -2 6-1.73351 25.9526 2 7 -2 7 75.0919 25.6117 2 7 -2 8 218.774 35.0897 2 7 -2 9 765.187 45.6156 2 7 -2 10 297.993 41.0582 2 7 -2 11 129.921 32.2446 2 7 0 -7 141.610 34.8631 2 7 0 -6 105.199 26.2205 2 7 0 -5 11.3191 29.1544 2 7 0 -4 42.1784 33.4466 2 7 0 -3 5.63084 30.8451 2 7 0 -2 260.668 36.0333 2 7 0 -1 4.32796 30.3254 2 7 0 0 58.0934 31.1629 2 7 0 1 1723.31 50.0922 2 7 0 2 202.727 35.4481 2 7 0 3 17.3348 30.0105 2 7 0 4 1191.94 45.6304 2 7 0 5 780.619 40.8891 2 7 0 6 102.881 27.9820 2 7 0 7 223.570 27.7094 2 7 0 8 159.849 25.1889 2 7 0 9 41.4939 26.6942 2 7 0 10 12.0756 25.7732 2 7 0 11 10.7098 25.6242 2 7 0 12 328.018 29.5406 2 7 1 -7 2.59726 37.9555 2 7 2 -7 113.640 26.5440 2 7 2 -6 36.6168 29.4892 2 7 2 -5 835.184 40.4129 2 7 2 -4 125.250 33.0665 2 7 2 -3 551.408 48.8620 2 7 2 -2 61.5730 34.6748 2 7 2 -1 285.418 36.6677 2 7 2 0 381.280 45.3114 2 7 2 1 14.1957 42.3756 2 7 2 2 1416.26 58.8828 2 7 2 3 350.296 43.1888 2 7 2 4 1658.84 61.1980 2 7 2 5 185.771 44.9258 2 7 2 6 119.900 31.9915 2 7 2 7 367.918 34.0172 2 7 2 8 165.329 30.5624 2 7 2 9 146.351 25.1828 2 7 2 10 571.406 38.2844 2 7 2 11 378.730 30.0595 2 7 2 12 115.323 23.8255 2 7 2 13 36.8115 24.6091 2 7 3 -7 42.7298 37.7932 2 7 3 -6 61.0313 41.8112 2 7 3 12 137.213 57.5172 2 7 3 13 9.30607 27.3369 2 7 4 -6 5.05239 25.3101 2 7 4 -5 102.077 32.7101 2 7 4 -4 6.56840 34.7608 2 7 4 -3 41.9047 38.4228 2 7 4 -2 61.6495 38.2814 2 7 4 -1 95.7277 47.5620 2 7 4 0 91.0227 40.3925 2 7 4 1 226.452 58.6169 2 7 4 2 72.8323 46.9161 2 7 4 3 24.3711 38.0591 2 7 4 4 28.0571 39.4626 2 7 4 5 47.8002 40.3468 2 7 4 6 151.110 35.8430 2 7 4 7 264.090 33.3900 2 7 4 8 57.5596 29.9243 2 7 4 9 16.9566 26.0637 2 7 4 10 6.55156 29.5730 2 7 4 11 49.0125 27.3340 2 7 4 12 93.6180 24.8889 2 7 4 13 22.9954 21.9827 2 7 5 -5 102.083 54.7190 2 7 5 -4 36.6748 60.3340 2 7 5 -1 127.713 66.5125 2 7 5 9 185.450 65.9876 2 7 5 10 133.861 63.6371 2 7 5 11 61.8241 30.7262 2 7 5 12 0.95312 32.0468 2 7 5 13 14.1715 27.7883 2 -7 -6 5 82.4284 29.1180 2 7 6 -4 24.9226 24.0453 2 -7 -6 3 18.2016 31.4171 2 7 6 -1 135.125 43.5901 2 7 6 0 43.5113 45.2442 2 7 6 1 118.680 50.2270 2 7 6 2 85.6682 51.7821 2 7 6 3 16.0114 40.3496 2 7 6 4 1.65036 40.1424 2 7 6 5-0.46138 41.3097 2 7 6 6 119.301 77.0797 2 7 6 7 194.828 53.4028 2 7 6 8 25.2555 38.0747 2 7 6 9 35.4662 44.0126 2 7 6 10 280.875 64.9949 2 7 6 11 36.1758 42.7298 2 7 6 12 47.4353 35.9901 2 7 6 13 141.397 34.5189 2 -7 -7 4 50.2195 28.5957 2 -7 -7 3 70.8476 34.9340 2 7 7 -2-6.98799 55.9611 2 7 7 -1 158.388 34.1543 2 7 7 0 64.2489 39.6704 2 7 7 1 102.592 45.0786 2 7 7 2 90.6006 47.4624 2 7 7 3 288.417 51.2055 2 7 7 4 237.867 42.6571 2 7 7 5 19.9817 32.8742 2 7 7 6 361.202 46.9756 2 7 7 7-7.68839 32.5409 2 7 7 8 142.534 28.2978 2 7 7 9 106.456 35.2620 2 7 7 10 76.0699 33.1269 2 7 7 11 33.0971 25.9838 2 7 7 12 37.2163 26.0947 2 7 8 0 35.4929 48.7384 2 -7 -8 -6 48.0978 52.1541 2 7 8 9-5.55077 52.8059 2 7 8 12 425.011 52.5843 2 -7 -9 1 25.9361 35.9738 2 7 9 1 18.3077 31.0584 2 7 9 2 68.8415 34.5854 2 7 9 3 81.3305 29.9303 2 7 9 4 443.659 37.8577 2 7 9 5 1192.77 40.5234 2 7 9 6 32.2318 25.9917 2 7 9 7 97.4842 30.8339 2 7 9 8 10.2305 21.0976 2 7 9 9 32.2808 19.9459 2 7 9 10 59.4738 23.9226 2 8 -1 1 359.222 57.0325 2 8 -1 2 104.320 52.3180 2 8 -1 3 15.1631 32.7258 2 8 -1 4 83.9276 35.4375 2 8 -1 5 488.638 41.1346 2 8 -1 6 487.272 54.2162 2 8 0 0 13.2092 44.5061 2 8 0 1 34.3200 48.3504 2 8 1 -1 95.5410 44.8260 2 8 1 0 22.7844 33.6990 2 8 1 1 96.6881 30.7451 2 8 1 2 18.7505 27.1731 2 8 1 3-16.8379 27.8535 2 8 1 4 3.41812 27.9980 2 8 1 5-6.51647 27.6232 2 8 1 6 61.3457 23.4108 2 8 1 7 39.6948 21.5846 2 8 1 8 50.9629 22.8690 2 8 3 -1 53.9264 31.8149 2 8 3 0 253.387 26.7315 2 8 3 1 294.575 28.6096 2 8 3 2 8.16635 23.9180 2 8 3 3 111.433 28.5263 2 8 3 4 23.6501 27.9854 2 8 3 5 47.6617 24.3195 2 8 3 6 163.385 25.6792 2 8 3 7 330.022 20.7497 2 8 3 8 88.1888 22.3034 2 8 3 9 50.5868 24.6457 2 8 5 0-0.70614 29.9956 2 8 5 1 33.6903 25.8194 2 8 5 2 115.631 25.1303 2 8 5 3 60.0532 25.8534 2 8 5 4 73.5286 26.5491 2 8 5 5 126.640 21.0804 2 8 5 6 32.5018 19.8626 2 8 5 7 41.1123 19.0869 2 8 5 8 52.0852 19.7284 2 ; _shelx_hkl_checksum 80918 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in Paratone oil.' _olex2_submission_original_sample_id KY-461 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.639 _oxdiff_exptl_absorpt_empirical_full_min 0.719 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.7527(12) 13221 12078 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.2473(12) 13198 12078 nmt -1.0003 -0.0001 -0.0000 -0.0005 -0.9998 -0.0000 -0.7746 -0.4716 0.9999 _twin_special_details ; Component 2 rotated by -179.9876\% around [-0.00 0.00 1.00] (reciprocal) or [-0.35 -0.21 0.91] (direct) ; ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_ky463_reprocess _database_code_depnum_ccdc_archive 'CCDC 2084379' loop_ _audit_author_name _audit_author_address 'Marina Uzelac' ;University of Edinburgh United Kingdom ; _audit_update_record ; 2021-05-18 deposited with the CCDC. 2022-01-03 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT910_ky463_reprocess ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 11 Note RESPONSE: Reduction of beam stop mask did not yield significant improvement. Most of these missing reflections appeared to be very strong and were treated as overflows. ; # Added during the CSD deposition process: Tuesday 18 May 2021 09:15 AM # end Validation Reply Form _audit_creation_date 2021-04-30 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C34 H30 B N' _chemical_formula_sum 'C34 H30 B N' _chemical_formula_weight 463.40 _chemical_melting_point ? _chemical_oxdiff_formula 'C34 H30 B N' _chemical_oxdiff_usercomment '@ 120 K ' 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' B B 0.0013 0.0007 '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' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0461(6) _cell_length_b 17.1985(5) _cell_length_c 13.0700(6) _cell_angle_alpha 90 _cell_angle_beta 109.463(5) _cell_angle_gamma 90 _cell_volume 2553.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7492 _cell_measurement_temperature 120.1(4) _cell_measurement_theta_max 23.9510 _cell_measurement_theta_min 3.6690 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 984 _exptl_crystal_recrystallization_method ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.101 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_unetI/netI 0.0768 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.924 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 55926 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.924 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.485 _diffrn_reflns_theta_min 3.406 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.1(4) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0521 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.924 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -45.00 43.00 1.00 20.00 -- -15.82 81.00 -68.00 88 2 \w -10.00 42.00 1.00 20.00 -- 17.54 81.00 -68.00 52 3 \w -43.00 46.00 1.00 20.00 -- 17.54 -81.00 169.00 89 4 \w -88.00 -39.00 1.00 20.00 -- -15.82-178.00 -30.00 49 5 \w -39.00 11.00 1.00 20.00 -- -15.82 -77.00 90.00 50 6 \w -20.00 56.00 1.00 20.00 -- 17.54 -99.00 -90.00 76 7 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00 30.00 48 8 \w -52.00 36.00 1.00 20.00 -- 17.54 -38.00 120.00 88 9 \w -50.00 34.00 1.00 20.00 -- 17.54 -57.00 30.00 84 10 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00 90.00 48 11 \w -1.00 87.00 1.00 20.00 -- 17.54 38.00 90.00 88 12 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00 -30.00 48 13 \w 1.00 85.00 1.00 20.00 -- 17.54 57.00-150.00 84 14 \w -20.00 29.00 1.00 20.00 -- 17.54 -99.00 90.00 49 15 \w -9.00 39.00 1.00 20.00 -- 17.54 77.00-120.00 48 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0520943000 _diffrn_orient_matrix_UB_12 0.0227106000 _diffrn_orient_matrix_UB_13 0.0141777000 _diffrn_orient_matrix_UB_21 -0.0289719000 _diffrn_orient_matrix_UB_22 0.0275127000 _diffrn_orient_matrix_UB_23 -0.0405494000 _diffrn_orient_matrix_UB_31 -0.0186615000 _diffrn_orient_matrix_UB_32 0.0206868000 _diffrn_orient_matrix_UB_33 0.0383074000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3743 _reflns_number_total 6564 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.201 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.044 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 6564 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0623 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.8045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1182 _refine_ls_wR_factor_ref 0.1424 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C8(H8), C18(H18), C19(H19), C3(H3), C13(H13), C2(H2), C7(H7), C5(H5), C14(H14), C21(H21), C30(H30), C6(H6), C28(H28), C20(H20) 2.b Idealised Me refined as rotating group: C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C25(H25A,H25B, H25C), C33(H33A,H33B,H33C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 N1 N 0.26932(15) 0.21893(9) 0.86238(14) 0.0357(4) Uani 1 1 d . . . . . C10 C 0.41235(16) 0.30656(10) 0.83249(14) 0.0283(4) Uani 1 1 d . . . . . C4 C 0.61543(17) 0.29850(10) 0.96340(15) 0.0319(4) Uani 1 1 d . . . . . C9 C 0.53602(17) 0.32302(9) 0.86076(15) 0.0286(4) Uani 1 1 d . . . . . C8 C 0.58694(17) 0.35801(10) 0.78863(15) 0.0309(4) Uani 1 1 d . . . . . H8 H 0.538194 0.373065 0.720028 0.037 Uiso 1 1 calc R U . . . C1 C 0.37884(17) 0.25401(10) 0.89852(15) 0.0308(4) Uani 1 1 d . . . . . C16 C 0.32318(16) 0.40724(10) 0.68429(15) 0.0294(4) Uani 1 1 d . . . . . C11 C 0.32182(16) 0.33406(10) 0.73348(15) 0.0287(4) Uani 1 1 d . . . . . C15 C 0.24284(17) 0.42341(10) 0.58059(15) 0.0317(4) Uani 1 1 d . . . . . C17 C 0.38679(17) 0.48047(10) 0.72703(15) 0.0301(4) Uani 1 1 d . . . . . C12 C 0.22146(17) 0.28591(10) 0.68498(15) 0.0307(4) Uani 1 1 d . . . . . C18 C 0.45735(17) 0.50207(10) 0.83116(16) 0.0318(4) Uani 1 1 d . . . . . H18 H 0.478869 0.465644 0.886927 0.038 Uiso 1 1 calc R U . . . C19 C 0.49494(18) 0.57820(10) 0.85057(17) 0.0355(5) Uani 1 1 d . . . . . H19 H 0.540967 0.593207 0.920137 0.043 Uiso 1 1 calc R U . . . C26 C 0.09091(17) 0.15873(11) 0.71804(15) 0.0326(5) Uani 1 1 d . . . . . C3 C 0.57152(18) 0.25557(10) 1.03391(16) 0.0355(5) Uani 1 1 d . . . . . H3 H 0.621334 0.243174 1.103276 0.043 Uiso 1 1 calc R U . . . C13 C 0.14031(17) 0.30585(11) 0.58394(15) 0.0334(5) Uani 1 1 d . . . . . H13 H 0.076061 0.273505 0.552642 0.040 Uiso 1 1 calc R U . . . C2 C 0.45774(18) 0.23233(10) 1.00146(15) 0.0354(5) Uani 1 1 d . . . . . H2 H 0.431151 0.201810 1.047297 0.043 Uiso 1 1 calc R U . . . C22 C 0.35190(18) 0.53651(11) 0.64456(16) 0.0347(5) Uani 1 1 d . . . . . C7 C 0.70543(18) 0.37028(11) 0.81690(17) 0.0367(5) Uani 1 1 d . . . . . H7 H 0.735931 0.392774 0.767243 0.044 Uiso 1 1 calc R U . . . C5 C 0.73673(18) 0.31355(11) 0.99042(17) 0.0379(5) Uani 1 1 d . . . . . H5 H 0.787550 0.298629 1.058247 0.045 Uiso 1 1 calc R U . . . C14 C 0.15298(17) 0.37248(11) 0.52916(16) 0.0346(5) Uani 1 1 d . . . . . H14 H 0.102136 0.382628 0.459393 0.042 Uiso 1 1 calc R U . . . C27 C 0.11226(17) 0.09029(11) 0.66830(16) 0.0357(5) Uani 1 1 d . . . . . C21 C 0.3934(2) 0.61204(11) 0.66490(18) 0.0414(5) Uani 1 1 d . . . . . H21 H 0.373123 0.648718 0.609439 0.050 Uiso 1 1 calc R U . . . C23 C 0.26459(18) 0.50354(11) 0.54167(16) 0.0371(5) Uani 1 1 d . . . . . C31 C -0.01327(18) 0.16341(12) 0.74329(16) 0.0362(5) Uani 1 1 d . . . . . C30 C -0.08954(18) 0.10018(13) 0.72311(16) 0.0403(5) Uani 1 1 d . . . . . H30 H -0.157840 0.103766 0.741090 0.048 Uiso 1 1 calc R U . . . C6 C 0.78144(19) 0.34925(11) 0.92009(18) 0.0412(5) Uani 1 1 d . . . . . H6 H 0.861616 0.359657 0.940135 0.049 Uiso 1 1 calc R U . . . C28 C 0.03338(19) 0.02884(12) 0.64924(17) 0.0415(5) Uani 1 1 d . . . . . H28 H 0.048875 -0.015995 0.616563 0.050 Uiso 1 1 calc R U . . . C29 C -0.06694(19) 0.03207(12) 0.67708(17) 0.0418(5) Uani 1 1 d . . . . . C20 C 0.46472(19) 0.63255(11) 0.76730(17) 0.0410(5) Uani 1 1 d . . . . . H20 H 0.492923 0.683177 0.780926 0.049 Uiso 1 1 calc R U . . . C34 C -0.0425(2) 0.23744(13) 0.79100(18) 0.0508(6) Uani 1 1 d . . . . . H34A H 0.026210 0.255699 0.847482 0.076 Uiso 1 1 calc R U . . . H34B H -0.104137 0.227431 0.820596 0.076 Uiso 1 1 calc R U . . . H34C H -0.068197 0.276244 0.735271 0.076 Uiso 1 1 calc R U . . . C24 C 0.3196(2) 0.49611(13) 0.45148(17) 0.0493(6) Uani 1 1 d . . . . . H24A H 0.387998 0.463465 0.476054 0.074 Uiso 1 1 calc R U . . . H24B H 0.341757 0.546686 0.433929 0.074 Uiso 1 1 calc R U . . . H24C H 0.263245 0.473546 0.388164 0.074 Uiso 1 1 calc R U . . . C32 C 0.2229(2) 0.08212(13) 0.64026(19) 0.0482(6) Uani 1 1 d . . . . . H32A H 0.229526 0.125208 0.595945 0.072 Uiso 1 1 calc R U . . . H32B H 0.220192 0.034475 0.601211 0.072 Uiso 1 1 calc R U . . . H32C H 0.289827 0.081439 0.705697 0.072 Uiso 1 1 calc R U . . . C25 C 0.1518(2) 0.55243(12) 0.50141(19) 0.0512(6) Uani 1 1 d . . . . . H25A H 0.096864 0.528055 0.438858 0.077 Uiso 1 1 calc R U . . . H25B H 0.170484 0.603506 0.482355 0.077 Uiso 1 1 calc R U . . . H25C H 0.117519 0.556320 0.557812 0.077 Uiso 1 1 calc R U . . . B1 B 0.1932(2) 0.22112(13) 0.75391(18) 0.0328(5) Uani 1 1 d . . . . . C33 C -0.1489(2) -0.03683(15) 0.6595(2) 0.0666(8) Uani 1 1 d . . . . . H33A H -0.139985 -0.060970 0.728003 0.100 Uiso 1 1 calc R U . . . H33B H -0.130001 -0.073673 0.612612 0.100 Uiso 1 1 calc R U . . . H33C H -0.228729 -0.019647 0.626704 0.100 Uiso 1 1 calc R U . . . H1 H 0.2559(19) 0.1886(12) 0.9146(18) 0.051(7) Uiso 1 1 d . . . . . 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 N1 0.0438(11) 0.0313(9) 0.0313(10) 0.0013(7) 0.0117(8) -0.0053(8) C10 0.0385(11) 0.0198(9) 0.0247(10) -0.0037(7) 0.0079(8) 0.0022(8) C4 0.0411(12) 0.0197(9) 0.0298(11) -0.0058(8) 0.0050(9) 0.0018(8) C9 0.0401(12) 0.0171(8) 0.0254(10) -0.0044(7) 0.0066(9) 0.0036(7) C8 0.0371(12) 0.0222(9) 0.0293(11) -0.0057(8) 0.0056(9) 0.0024(8) C1 0.0399(12) 0.0237(9) 0.0267(10) -0.0022(8) 0.0082(9) 0.0003(8) C16 0.0345(11) 0.0280(10) 0.0264(10) -0.0009(8) 0.0111(9) 0.0031(8) C11 0.0336(11) 0.0263(9) 0.0258(10) -0.0030(7) 0.0095(8) 0.0041(8) C15 0.0373(11) 0.0295(10) 0.0295(11) 0.0015(8) 0.0128(9) 0.0074(8) C17 0.0368(11) 0.0229(9) 0.0323(11) 0.0023(8) 0.0138(9) 0.0052(8) C12 0.0340(11) 0.0275(10) 0.0303(11) -0.0018(8) 0.0104(9) 0.0035(8) C18 0.0385(11) 0.0228(9) 0.0354(11) 0.0019(8) 0.0140(9) 0.0022(8) C19 0.0421(12) 0.0272(10) 0.0396(12) -0.0049(8) 0.0167(10) -0.0016(9) C26 0.0348(11) 0.0341(10) 0.0268(11) 0.0039(8) 0.0072(9) 0.0012(8) C3 0.0486(13) 0.0251(10) 0.0255(11) -0.0026(8) 0.0026(9) 0.0029(9) C13 0.0338(11) 0.0352(11) 0.0291(11) -0.0028(8) 0.0076(9) 0.0014(9) C2 0.0533(14) 0.0246(9) 0.0261(11) 0.0003(8) 0.0101(10) -0.0015(9) C22 0.0431(12) 0.0285(10) 0.0357(12) 0.0046(8) 0.0174(10) 0.0069(9) C7 0.0405(12) 0.0286(10) 0.0399(13) -0.0045(9) 0.0120(10) -0.0001(9) C5 0.0435(13) 0.0271(10) 0.0332(12) -0.0036(8) -0.0006(10) 0.0022(9) C14 0.0378(12) 0.0382(11) 0.0246(10) 0.0011(8) 0.0062(9) 0.0075(9) C27 0.0364(12) 0.0348(11) 0.0354(12) -0.0005(9) 0.0115(9) -0.0008(9) C21 0.0604(15) 0.0268(10) 0.0424(13) 0.0096(9) 0.0245(11) 0.0052(9) C23 0.0466(13) 0.0322(10) 0.0315(11) 0.0074(8) 0.0116(10) 0.0059(9) C31 0.0355(12) 0.0431(12) 0.0262(11) 0.0028(8) 0.0050(9) 0.0073(9) C30 0.0290(11) 0.0561(13) 0.0350(12) 0.0066(10) 0.0097(9) -0.0009(10) C6 0.0361(12) 0.0331(11) 0.0484(14) -0.0074(10) 0.0060(10) -0.0011(9) C28 0.0474(13) 0.0336(11) 0.0457(14) -0.0017(9) 0.0185(11) -0.0035(9) C29 0.0404(13) 0.0444(12) 0.0388(13) 0.0040(10) 0.0110(10) -0.0077(10) C20 0.0553(14) 0.0239(10) 0.0487(14) 0.0017(9) 0.0240(11) -0.0024(9) C34 0.0500(14) 0.0570(14) 0.0453(14) -0.0028(11) 0.0157(11) 0.0131(11) C24 0.0704(17) 0.0434(12) 0.0371(13) 0.0072(10) 0.0221(12) -0.0022(11) C32 0.0513(14) 0.0416(12) 0.0589(16) -0.0072(11) 0.0278(12) -0.0042(10) C25 0.0586(15) 0.0381(12) 0.0496(15) 0.0108(10) 0.0081(12) 0.0118(11) B1 0.0370(13) 0.0291(11) 0.0326(13) -0.0014(9) 0.0120(11) 0.0050(9) C33 0.0613(17) 0.0670(17) 0.0745(19) -0.0057(14) 0.0269(15) -0.0286(14) _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 N1 C1 1.383(2) . ? N1 B1 1.409(3) . ? N1 H1 0.91(2) . ? C10 C9 1.438(3) . ? C10 C1 1.399(3) . ? C10 C11 1.465(2) . ? C4 C9 1.427(3) . ? C4 C3 1.414(3) . ? C4 C5 1.408(3) . ? C9 C8 1.419(3) . ? C8 H8 0.9300 . ? C8 C7 1.366(3) . ? C1 C2 1.414(3) . ? C16 C11 1.416(2) . ? C16 C15 1.406(3) . ? C16 C17 1.483(2) . ? C11 C12 1.428(3) . ? C15 C14 1.381(3) . ? C15 C23 1.522(3) . ? C17 C18 1.393(3) . ? C17 C22 1.402(3) . ? C12 C13 1.399(3) . ? C12 B1 1.541(3) . ? C18 H18 0.9300 . ? C18 C19 1.381(2) . ? C19 H19 0.9300 . ? C19 C20 1.388(3) . ? C26 C27 1.409(3) . ? C26 C31 1.402(3) . ? C26 B1 1.582(3) . ? C3 H3 0.9300 . ? C3 C2 1.353(3) . ? C13 H13 0.9300 . ? C13 C14 1.386(3) . ? C2 H2 0.9300 . ? C22 C21 1.386(3) . ? C22 C23 1.514(3) . ? C7 H7 0.9300 . ? C7 C6 1.402(3) . ? C5 H5 0.9300 . ? C5 C6 1.357(3) . ? C14 H14 0.9300 . ? C27 C28 1.387(3) . ? C27 C32 1.502(3) . ? C21 H21 0.9300 . ? C21 C20 1.374(3) . ? C23 C24 1.538(3) . ? C23 C25 1.534(3) . ? C31 C30 1.391(3) . ? C31 C34 1.510(3) . ? C30 H30 0.9300 . ? C30 C29 1.385(3) . ? C6 H6 0.9300 . ? C28 H28 0.9300 . ? C28 C29 1.374(3) . ? C29 C33 1.510(3) . ? C20 H20 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 B1 123.99(18) . . ? C1 N1 H1 112.3(14) . . ? B1 N1 H1 123.2(14) . . ? C9 C10 C11 124.45(17) . . ? C1 C10 C9 117.11(16) . . ? C1 C10 C11 118.07(17) . . ? C3 C4 C9 119.19(18) . . ? C5 C4 C9 119.73(19) . . ? C5 C4 C3 120.99(18) . . ? C4 C9 C10 119.72(17) . . ? C8 C9 C10 123.56(17) . . ? C8 C9 C4 116.56(18) . . ? C9 C8 H8 119.0 . . ? C7 C8 C9 121.99(18) . . ? C7 C8 H8 119.0 . . ? N1 C1 C10 120.64(17) . . ? N1 C1 C2 118.18(17) . . ? C10 C1 C2 121.10(18) . . ? C11 C16 C17 131.79(17) . . ? C15 C16 C11 120.34(17) . . ? C15 C16 C17 107.36(15) . . ? C16 C11 C10 124.76(17) . . ? C16 C11 C12 116.76(17) . . ? C12 C11 C10 118.40(16) . . ? C16 C15 C23 111.19(16) . . ? C14 C15 C16 121.34(17) . . ? C14 C15 C23 127.32(17) . . ? C18 C17 C16 131.65(16) . . ? C18 C17 C22 119.78(17) . . ? C22 C17 C16 108.01(16) . . ? C11 C12 B1 118.65(17) . . ? C13 C12 C11 119.92(17) . . ? C13 C12 B1 120.54(18) . . ? C17 C18 H18 120.4 . . ? C19 C18 C17 119.21(18) . . ? C19 C18 H18 120.4 . . ? C18 C19 H19 119.7 . . ? C18 C19 C20 120.68(19) . . ? C20 C19 H19 119.7 . . ? C27 C26 B1 117.35(17) . . ? C31 C26 C27 118.16(18) . . ? C31 C26 B1 124.10(18) . . ? C4 C3 H3 119.7 . . ? C2 C3 C4 120.65(18) . . ? C2 C3 H3 119.7 . . ? C12 C13 H13 119.1 . . ? C14 C13 C12 121.85(18) . . ? C14 C13 H13 119.1 . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.65(18) . . ? C3 C2 H2 119.7 . . ? C17 C22 C23 111.52(16) . . ? C21 C22 C17 120.03(19) . . ? C21 C22 C23 128.38(18) . . ? C8 C7 H7 119.7 . . ? C8 C7 C6 120.6(2) . . ? C6 C7 H7 119.7 . . ? C4 C5 H5 119.1 . . ? C6 C5 C4 121.74(19) . . ? C6 C5 H5 119.1 . . ? C15 C14 C13 118.45(18) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C26 C27 C32 120.26(18) . . ? C28 C27 C26 119.99(19) . . ? C28 C27 C32 119.69(18) . . ? C22 C21 H21 120.1 . . ? C20 C21 C22 119.75(18) . . ? C20 C21 H21 120.1 . . ? C15 C23 C24 110.31(16) . . ? C15 C23 C25 112.31(18) . . ? C22 C23 C15 100.85(15) . . ? C22 C23 C24 111.27(18) . . ? C22 C23 C25 111.90(17) . . ? C25 C23 C24 109.93(17) . . ? C26 C31 C34 119.73(19) . . ? C30 C31 C26 119.79(18) . . ? C30 C31 C34 120.5(2) . . ? C31 C30 H30 119.0 . . ? C29 C30 C31 122.1(2) . . ? C29 C30 H30 119.0 . . ? C7 C6 H6 120.4 . . ? C5 C6 C7 119.3(2) . . ? C5 C6 H6 120.4 . . ? C27 C28 H28 118.9 . . ? C29 C28 C27 122.1(2) . . ? C29 C28 H28 118.9 . . ? C30 C29 C33 121.1(2) . . ? C28 C29 C30 117.82(19) . . ? C28 C29 C33 121.1(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.43(18) . . ? C21 C20 H20 119.8 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 B1 C12 114.26(18) . . ? N1 B1 C26 117.48(18) . . ? C12 B1 C26 128.26(18) . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 N1 C1 C2 C3 169.93(17) . . . . ? C10 C9 C8 C7 -177.61(17) . . . . ? C10 C1 C2 C3 -6.9(3) . . . . ? C10 C11 C12 C13 -172.53(16) . . . . ? C10 C11 C12 B1 18.2(2) . . . . ? C4 C9 C8 C7 -2.2(2) . . . . ? C4 C3 C2 C1 -3.4(3) . . . . ? C4 C5 C6 C7 -1.4(3) . . . . ? C9 C10 C1 N1 -162.37(16) . . . . ? C9 C10 C1 C2 14.4(3) . . . . ? C9 C10 C11 C16 -35.9(3) . . . . ? C9 C10 C11 C12 147.30(17) . . . . ? C9 C4 C3 C2 5.4(3) . . . . ? C9 C4 C5 C6 -1.7(3) . . . . ? C9 C8 C7 C6 -0.8(3) . . . . ? C8 C7 C6 C5 2.7(3) . . . . ? C1 N1 B1 C12 -18.4(3) . . . . ? C1 N1 B1 C26 161.85(17) . . . . ? C1 C10 C9 C4 -12.1(2) . . . . ? C1 C10 C9 C8 163.11(16) . . . . ? C1 C10 C11 C16 151.25(18) . . . . ? C1 C10 C11 C12 -25.5(2) . . . . ? C16 C11 C12 C13 10.5(3) . . . . ? C16 C11 C12 B1 -158.84(17) . . . . ? C16 C15 C14 C13 2.6(3) . . . . ? C16 C15 C23 C22 -10.2(2) . . . . ? C16 C15 C23 C24 107.51(19) . . . . ? C16 C15 C23 C25 -129.47(19) . . . . ? C16 C17 C18 C19 -172.41(19) . . . . ? C16 C17 C22 C21 176.43(18) . . . . ? C16 C17 C22 C23 -0.9(2) . . . . ? C11 C10 C9 C4 175.01(16) . . . . ? C11 C10 C9 C8 -9.8(3) . . . . ? C11 C10 C1 N1 11.0(3) . . . . ? C11 C10 C1 C2 -172.23(16) . . . . ? C11 C16 C15 C14 7.1(3) . . . . ? C11 C16 C15 C23 -177.02(16) . . . . ? C11 C16 C17 C18 -6.1(4) . . . . ? C11 C16 C17 C22 -177.36(19) . . . . ? C11 C12 C13 C14 -1.1(3) . . . . ? C11 C12 B1 N1 2.8(3) . . . . ? C11 C12 B1 C26 -177.50(18) . . . . ? C15 C16 C11 C10 169.81(17) . . . . ? C15 C16 C11 C12 -13.4(3) . . . . ? C15 C16 C17 C18 165.5(2) . . . . ? C15 C16 C17 C22 -5.7(2) . . . . ? C17 C16 C11 C10 -19.4(3) . . . . ? C17 C16 C11 C12 157.35(19) . . . . ? C17 C16 C15 C14 -165.65(17) . . . . ? C17 C16 C15 C23 10.2(2) . . . . ? C17 C18 C19 C20 -1.1(3) . . . . ? C17 C22 C21 C20 -2.8(3) . . . . ? C17 C22 C23 C15 6.5(2) . . . . ? C17 C22 C23 C24 -110.52(19) . . . . ? C17 C22 C23 C25 126.06(19) . . . . ? C12 C13 C14 C15 -5.6(3) . . . . ? C18 C17 C22 C21 4.0(3) . . . . ? C18 C17 C22 C23 -173.34(17) . . . . ? C18 C19 C20 C21 2.3(3) . . . . ? C26 C27 C28 C29 0.2(3) . . . . ? C26 C31 C30 C29 -0.8(3) . . . . ? C3 C4 C9 C10 2.5(2) . . . . ? C3 C4 C9 C8 -173.03(16) . . . . ? C3 C4 C5 C6 174.69(18) . . . . ? C13 C12 B1 N1 -166.44(17) . . . . ? C13 C12 B1 C26 13.3(3) . . . . ? C22 C17 C18 C19 -2.0(3) . . . . ? C22 C21 C20 C19 -0.3(3) . . . . ? C5 C4 C9 C10 179.02(16) . . . . ? C5 C4 C9 C8 3.5(2) . . . . ? C5 C4 C3 C2 -171.05(17) . . . . ? C14 C15 C23 C22 165.35(19) . . . . ? C14 C15 C23 C24 -77.0(3) . . . . ? C14 C15 C23 C25 46.1(3) . . . . ? C27 C26 C31 C30 2.6(3) . . . . ? C27 C26 C31 C34 -176.67(18) . . . . ? C27 C26 B1 N1 -95.2(2) . . . . ? C27 C26 B1 C12 85.1(2) . . . . ? C27 C28 C29 C30 1.6(3) . . . . ? C27 C28 C29 C33 -177.5(2) . . . . ? C21 C22 C23 C15 -170.6(2) . . . . ? C21 C22 C23 C24 72.4(3) . . . . ? C21 C22 C23 C25 -51.0(3) . . . . ? C23 C15 C14 C13 -172.54(18) . . . . ? C23 C22 C21 C20 174.0(2) . . . . ? C31 C26 C27 C28 -2.3(3) . . . . ? C31 C26 C27 C32 -179.59(18) . . . . ? C31 C26 B1 N1 77.4(2) . . . . ? C31 C26 B1 C12 -102.3(3) . . . . ? C31 C30 C29 C28 -1.3(3) . . . . ? C31 C30 C29 C33 177.9(2) . . . . ? C34 C31 C30 C29 178.45(19) . . . . ? C32 C27 C28 C29 177.5(2) . . . . ? B1 N1 C1 C10 11.9(3) . . . . ? B1 N1 C1 C2 -164.97(18) . . . . ? B1 C12 C13 C14 167.95(18) . . . . ? B1 C26 C27 C28 170.76(18) . . . . ? B1 C26 C27 C32 -6.5(3) . . . . ? B1 C26 C31 C30 -169.97(18) . . . . ? B1 C26 C31 C34 10.7(3) . . . . ? _shelx_res_file ; TITL ky463_reprocess_a.res in P2(1)/c ky463_reprocess.res created by SHELXL-2018/3 at 13:23:46 on 30-Apr-2021 REM Old TITL KY463_reprocess in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.185, Rweak 0.127, Alpha 0.034 REM 0.404 for 189 systematic absences, Orientation as input REM Formula found by SHELXT: C35 N CELL 0.71073 12.0461 17.1985 13.07 90 109.463 90 ZERR 4 0.0006 0.0005 0.0006 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B N UNIT 136 120 4 4 L.S. 20 PLAN 2 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.048000 0.804500 FVAR 0.54186 N1 4 0.269318 0.218931 0.862381 11.00000 0.04384 0.03135 = 0.03129 0.00130 0.01172 -0.00535 C10 1 0.412352 0.306555 0.832486 11.00000 0.03853 0.01976 = 0.02470 -0.00369 0.00785 0.00215 C4 1 0.615433 0.298500 0.963400 11.00000 0.04115 0.01966 = 0.02981 -0.00576 0.00502 0.00179 C9 1 0.536023 0.323016 0.860762 11.00000 0.04006 0.01714 = 0.02544 -0.00437 0.00656 0.00355 C8 1 0.586940 0.358014 0.788630 11.00000 0.03707 0.02219 = 0.02934 -0.00574 0.00559 0.00240 AFIX 43 H8 2 0.538194 0.373065 0.720028 11.00000 -1.20000 AFIX 0 C1 1 0.378839 0.254005 0.898525 11.00000 0.03988 0.02372 = 0.02671 -0.00216 0.00825 0.00028 C16 1 0.323178 0.407242 0.684289 11.00000 0.03446 0.02802 = 0.02639 -0.00093 0.01106 0.00307 C11 1 0.321822 0.334061 0.733475 11.00000 0.03363 0.02628 = 0.02579 -0.00301 0.00950 0.00410 C15 1 0.242840 0.423412 0.580591 11.00000 0.03725 0.02951 = 0.02954 0.00146 0.01283 0.00736 C17 1 0.386790 0.480469 0.727034 11.00000 0.03679 0.02286 = 0.03232 0.00228 0.01377 0.00524 C12 1 0.221458 0.285910 0.684985 11.00000 0.03405 0.02746 = 0.03029 -0.00179 0.01036 0.00346 C18 1 0.457347 0.502065 0.831161 11.00000 0.03847 0.02276 = 0.03539 0.00188 0.01399 0.00220 AFIX 43 H18 2 0.478869 0.465644 0.886927 11.00000 -1.20000 AFIX 0 C19 1 0.494937 0.578200 0.850565 11.00000 0.04211 0.02718 = 0.03961 -0.00486 0.01667 -0.00160 AFIX 43 H19 2 0.540967 0.593207 0.920137 11.00000 -1.20000 AFIX 0 C26 1 0.090907 0.158726 0.718040 11.00000 0.03479 0.03409 = 0.02676 0.00387 0.00723 0.00118 C3 1 0.571521 0.255566 1.033910 11.00000 0.04860 0.02509 = 0.02553 -0.00260 0.00259 0.00289 AFIX 43 H3 2 0.621334 0.243174 1.103276 11.00000 -1.20000 AFIX 0 C13 1 0.140312 0.305853 0.583944 11.00000 0.03375 0.03519 = 0.02911 -0.00277 0.00761 0.00145 AFIX 43 H13 2 0.076061 0.273505 0.552642 11.00000 -1.20000 AFIX 0 C2 1 0.457737 0.232332 1.001459 11.00000 0.05328 0.02461 = 0.02607 0.00027 0.01013 -0.00153 AFIX 43 H2 2 0.431151 0.201810 1.047297 11.00000 -1.20000 AFIX 0 C22 1 0.351900 0.536511 0.644557 11.00000 0.04313 0.02854 = 0.03567 0.00463 0.01742 0.00693 C7 1 0.705431 0.370277 0.816903 11.00000 0.04047 0.02858 = 0.03993 -0.00448 0.01198 -0.00015 AFIX 43 H7 2 0.735931 0.392774 0.767243 11.00000 -1.20000 AFIX 0 C5 1 0.736731 0.313550 0.990417 11.00000 0.04349 0.02705 = 0.03315 -0.00357 -0.00057 0.00223 AFIX 43 H5 2 0.787550 0.298629 1.058247 11.00000 -1.20000 AFIX 0 C14 1 0.152981 0.372479 0.529160 11.00000 0.03783 0.03821 = 0.02462 0.00113 0.00622 0.00751 AFIX 43 H14 2 0.102136 0.382628 0.459393 11.00000 -1.20000 AFIX 0 C27 1 0.112261 0.090293 0.668302 11.00000 0.03640 0.03478 = 0.03545 -0.00052 0.01148 -0.00079 C21 1 0.393431 0.612044 0.664897 11.00000 0.06041 0.02683 = 0.04239 0.00956 0.02451 0.00523 AFIX 43 H21 2 0.373123 0.648718 0.609439 11.00000 -1.20000 AFIX 0 C23 1 0.264591 0.503539 0.541668 11.00000 0.04662 0.03220 = 0.03146 0.00744 0.01160 0.00595 C31 1 -0.013272 0.163413 0.743290 11.00000 0.03547 0.04310 = 0.02618 0.00283 0.00503 0.00729 C30 1 -0.089535 0.100184 0.723109 11.00000 0.02899 0.05611 = 0.03499 0.00657 0.00974 -0.00093 AFIX 43 H30 2 -0.157840 0.103766 0.741090 11.00000 -1.20000 AFIX 0 C6 1 0.781436 0.349253 0.920090 11.00000 0.03610 0.03306 = 0.04841 -0.00736 0.00601 -0.00106 AFIX 43 H6 2 0.861616 0.359657 0.940135 11.00000 -1.20000 AFIX 0 C28 1 0.033377 0.028837 0.649239 11.00000 0.04738 0.03364 = 0.04575 -0.00175 0.01852 -0.00353 AFIX 43 H28 2 0.048875 -0.015995 0.616563 11.00000 -1.20000 AFIX 0 C29 1 -0.066941 0.032068 0.677082 11.00000 0.04042 0.04443 = 0.03881 0.00396 0.01101 -0.00771 C20 1 0.464723 0.632551 0.767303 11.00000 0.05533 0.02392 = 0.04869 0.00168 0.02397 -0.00237 AFIX 43 H20 2 0.492923 0.683177 0.780926 11.00000 -1.20000 AFIX 0 C34 1 -0.042511 0.237438 0.791005 11.00000 0.05003 0.05695 = 0.04525 -0.00276 0.01568 0.01314 AFIX 137 H34A 2 0.026210 0.255699 0.847482 11.00000 -1.50000 H34B 2 -0.104137 0.227431 0.820596 11.00000 -1.50000 H34C 2 -0.068197 0.276244 0.735271 11.00000 -1.50000 AFIX 0 C24 1 0.319560 0.496112 0.451484 11.00000 0.07044 0.04340 = 0.03706 0.00718 0.02207 -0.00217 AFIX 137 H24A 2 0.387998 0.463465 0.476054 11.00000 -1.50000 H24B 2 0.341757 0.546686 0.433929 11.00000 -1.50000 H24C 2 0.263245 0.473546 0.388164 11.00000 -1.50000 AFIX 0 C32 1 0.222942 0.082116 0.640257 11.00000 0.05134 0.04161 = 0.05885 -0.00719 0.02781 -0.00416 AFIX 137 H32A 2 0.229526 0.125208 0.595945 11.00000 -1.50000 H32B 2 0.220192 0.034475 0.601211 11.00000 -1.50000 H32C 2 0.289827 0.081439 0.705697 11.00000 -1.50000 AFIX 0 C25 1 0.151815 0.552428 0.501407 11.00000 0.05855 0.03815 = 0.04957 0.01082 0.00808 0.01175 AFIX 137 H25A 2 0.096864 0.528055 0.438858 11.00000 -1.50000 H25B 2 0.170484 0.603506 0.482355 11.00000 -1.50000 H25C 2 0.117519 0.556320 0.557812 11.00000 -1.50000 AFIX 0 B1 3 0.193170 0.221125 0.753914 11.00000 0.03700 0.02911 = 0.03262 -0.00136 0.01195 0.00500 C33 1 -0.148874 -0.036828 0.659499 11.00000 0.06126 0.06702 = 0.07455 -0.00566 0.02686 -0.02857 AFIX 137 H33A 2 -0.139985 -0.060970 0.728003 11.00000 -1.50000 H33B 2 -0.130001 -0.073673 0.612612 11.00000 -1.50000 H33C 2 -0.228729 -0.019647 0.626704 11.00000 -1.50000 AFIX 0 H1 2 0.255935 0.188599 0.914568 11.00000 0.05092 HKLF 4 REM ky463_reprocess_a.res in P2(1)/c REM wR2 = 0.1424, GooF = S = 1.017, Restrained GooF = 1.017 for all data REM R1 = 0.0623 for 3743 Fo > 4sig(Fo) and 0.1324 for all 6564 data REM 334 parameters refined using 0 restraints END WGHT 0.0480 0.8024 REM Highest difference peak 0.201, deepest hole -0.204, 1-sigma level 0.044 Q1 1 0.1910 0.2613 0.7197 11.00000 0.05 0.20 Q2 1 -0.0002 0.2959 0.7928 11.00000 0.05 0.20 ; _shelx_res_checksum 57702 _shelx_hkl_file ; 0 0 -3 10.70 4.95 0 0 3 -7.53 5.64 0 0 -3 1.43 5.11 0 0 3 -1.33 2.08 0 0 3 1.83 4.19 0 0 3 5.46 5.30 0 0 3 3.38 5.36 0 0 -3 -2.07 5.47 0 0 -3 4.96 4.71 0 0 4 263.91 18.39 0 0 -4 257.05 17.85 0 0 -4 227.51 18.01 0 0 4 253.81 10.59 0 0 4 234.97 16.03 0 0 4 242.69 19.03 0 0 -4 213.74 17.80 0 0 4 240.45 18.49 0 0 -4 263.36 19.41 0 0 5 -0.25 5.90 0 0 -5 -7.71 5.74 0 0 -5 3.58 6.43 0 0 5 -2.43 2.68 0 0 5 7.27 5.29 0 0 5 1.93 5.91 0 0 -5 -10.22 8.44 0 0 -5 6.67 6.52 0 0 5 -1.36 6.40 0 0 6 744.13 38.12 0 0 -6 785.61 37.97 0 0 -6 772.26 39.23 0 0 6 825.29 22.36 0 0 6 815.73 36.31 0 0 -6 829.68 40.53 0 0 6 888.04 42.93 0 0 7 10.18 8.31 0 0 7 -5.81 6.21 0 0 7 -0.41 2.82 0 0 -7 -2.38 8.46 0 0 -7 -0.12 7.30 0 0 7 -0.40 8.63 0 0 8 2.95 6.24 0 0 -8 1.89 7.09 0 0 8 -0.38 2.24 0 0 8 10.34 9.76 0 0 -8 5.62 8.01 0 0 9 13.86 11.17 0 0 9 -2.34 3.58 0 0 -9 -7.86 8.76 0 0 9 3.00 9.54 0 0 -9 -11.04 10.99 0 0 10 174.43 25.85 0 0 10 175.80 11.65 0 0 -10 183.23 26.26 0 0 10 175.35 27.68 0 0 -10 172.04 25.23 0 0 11 17.72 11.78 0 0 -11 -3.46 11.65 0 0 -11 10.05 10.63 0 0 11 -2.51 9.04 0 0 12 91.22 20.21 0 0 -12 86.25 21.30 0 0 12 98.69 23.60 0 0 -12 120.78 23.70 0 0 13 4.41 10.24 0 0 -13 0.20 9.77 0 0 13 7.83 17.90 0 0 -13 3.91 11.12 0 0 14 -1.45 9.17 0 0 -14 5.31 9.22 0 0 14 -2.23 11.24 0 0 -14 12.13 15.86 0 0 15 -34.84 15.86 0 0 -15 1.62 10.69 0 0 -15 -5.64 11.95 0 0 15 6.67 13.00 0 0 16 22.70 14.85 0 1 -2 356.45 15.11 0 -1 -2 355.75 15.63 0 1 2 330.26 14.97 0 -1 2 360.83 15.23 0 1 2 370.62 12.48 0 -1 -2 350.03 12.09 0 1 -2 369.07 13.71 0 1 2 359.06 15.74 0 -1 2 371.36 15.96 0 1 2 358.32 15.67 0 -1 -2 381.90 15.94 0 1 -2 370.29 15.69 0 -1 2 334.66 15.55 0 -1 -2 367.29 15.80 0 1 -2 352.70 15.77 0 -1 -3 7128.53 81.78 0 1 3 7121.20 80.71 0 1 -3 7438.35 81.33 0 -1 3 7120.06 80.46 0 -1 -3 7382.85 85.34 0 1 -3 7367.33 72.11 0 -1 -3 7250.90 69.27 0 -1 3 7369.56 79.84 0 -1 3 7286.90 59.26 0 1 3 7248.05 69.09 0 1 3 7289.93 84.42 0 1 3 7241.48 84.52 0 -1 -3 7326.82 83.93 0 -1 -3 7529.07 85.29 0 1 -3 7438.25 85.02 0 1 -3 7185.76 83.63 0 -1 3 7195.22 84.51 0 -1 3 7289.79 84.65 0 -1 -4 20.28 7.29 0 1 4 15.43 7.92 0 1 -4 16.53 6.26 0 -1 4 23.42 7.36 0 1 4 17.42 5.46 0 -1 -4 9.98 4.12 0 -1 -4 15.27 6.77 0 -1 4 11.70 3.94 0 1 -4 13.06 4.62 0 -1 4 18.17 5.94 0 1 4 17.48 8.89 0 -1 -4 12.29 7.97 0 -1 4 13.06 7.82 0 -1 4 17.36 6.66 0 -1 -4 14.46 7.21 0 1 -4 10.73 7.27 0 1 -4 13.55 6.19 0 1 4 11.26 6.28 0 -1 -5 95.68 13.25 0 1 5 98.21 13.65 0 1 -5 94.81 12.69 0 -1 5 73.01 12.56 0 -1 -5 73.61 12.68 0 1 5 96.21 11.27 0 1 -5 86.52 12.96 0 -1 5 102.82 9.18 0 1 5 91.87 5.21 0 -1 5 74.15 10.93 0 1 5 77.50 12.82 0 1 5 71.60 11.63 0 -1 5 79.26 13.05 0 -1 -5 107.89 13.88 0 -1 -5 91.44 13.74 0 1 -5 85.16 12.90 0 -1 5 76.50 12.13 0 1 -5 90.70 13.68 0 1 -6 591.04 33.12 0 1 6 612.12 33.80 0 -1 6 595.44 33.89 0 -1 -6 630.29 34.82 0 1 6 634.47 30.59 0 -1 6 585.31 22.12 0 1 -6 597.79 34.35 0 1 -6 632.12 30.02 0 -1 -6 642.59 35.94 0 -1 6 641.84 33.53 0 1 6 650.55 15.19 0 1 6 617.47 35.72 0 -1 -6 597.26 34.73 0 -1 6 616.67 36.14 0 1 -6 670.76 36.59 0 1 7 108.69 16.25 0 -1 7 101.97 16.17 0 -1 -7 105.92 17.67 0 1 7 110.65 14.53 0 1 7 114.98 6.90 0 -1 7 107.56 10.10 0 1 -7 105.64 16.54 0 1 -7 99.44 16.70 0 1 7 114.96 18.92 0 -1 -7 113.27 17.81 0 -1 7 104.99 17.79 0 1 8 82.02 15.42 0 -1 8 135.24 19.41 0 -1 8 111.35 10.50 0 1 -8 88.97 16.01 0 -1 -8 93.70 16.98 0 1 8 100.37 6.79 0 1 -8 122.74 19.31 0 -1 -8 106.68 18.10 0 1 8 83.74 16.11 0 -1 8 119.57 20.20 0 -1 9 9.88 9.42 0 1 9 4.87 8.05 0 -1 9 6.58 3.65 0 -1 -9 14.63 10.12 0 1 9 5.20 2.08 0 1 -9 12.08 10.69 0 -1 9 10.54 10.02 0 -1 -9 15.69 10.05 0 1 -9 4.55 7.63 0 1 9 4.23 9.27 0 1 10 -7.27 7.33 0 -1 10 -1.51 7.84 0 -1 10 6.45 3.31 0 -1 -10 -4.13 9.64 0 1 -10 -16.08 11.65 0 -1 10 5.35 8.82 0 1 10 -6.35 10.29 0 -1 -10 10.40 10.72 0 1 -10 -2.35 10.38 0 1 11 12.24 8.90 0 -1 11 1.33 8.12 0 -1 -11 1.20 10.40 0 1 -11 14.20 10.43 0 -1 -11 1.76 9.34 0 -1 11 -0.40 10.33 0 1 11 -7.94 9.69 0 1 -11 4.01 8.86 0 1 12 10.46 9.46 0 -1 12 0.25 8.44 0 1 -12 10.52 11.05 0 -1 -12 23.62 13.92 0 -1 -12 2.81 10.54 0 -1 12 8.60 11.02 0 1 -12 1.02 10.10 0 1 12 -13.38 11.43 0 -1 13 12.75 11.06 0 1 13 26.39 12.93 0 -1 -13 27.13 13.61 0 1 -13 19.24 13.06 0 1 -13 19.88 10.75 0 -1 13 27.49 15.03 0 1 13 31.57 16.82 0 -1 -13 41.75 16.94 0 -1 14 20.56 13.55 0 1 14 17.80 13.10 0 1 -14 2.50 9.31 0 -1 -14 13.87 13.46 0 1 14 30.96 18.20 0 -1 14 32.47 17.90 0 1 -14 18.98 14.91 0 -1 -14 5.72 11.53 0 1 15 -5.99 9.99 0 -1 15 -11.61 14.28 0 -1 -15 -20.32 15.81 0 1 -15 9.94 10.92 0 -1 -15 11.07 11.33 0 -1 15 11.33 14.66 0 1 -15 2.25 14.26 0 1 15 -8.05 11.62 0 1 16 5.83 9.77 0 -1 16 -8.49 13.26 0 2 2 32.67 6.27 0 -2 -2 28.74 6.36 0 -2 -2 33.67 3.35 0 -2 2 32.51 5.79 0 -2 -2 29.51 4.16 0 2 2 33.03 6.10 0 -2 -2 25.26 4.68 0 -2 2 44.73 6.69 0 2 -2 33.41 6.06 0 -2 -2 31.26 5.40 0 2 -2 30.44 5.74 0 2 2 28.99 5.91 0 2 2 27.95 5.68 0 -2 2 31.74 5.18 0 -2 -2 35.81 4.35 0 -2 -2 34.22 4.49 0 -2 -2 38.72 6.65 0 -2 -2 34.56 4.23 0 -2 2 34.22 4.17 0 2 2 35.23 4.53 0 2 -2 31.80 5.33 0 2 -2 35.00 4.17 0 -2 2 33.03 5.46 0 -2 3 1079.64 32.28 0 -2 -3 1079.47 32.91 0 2 3 1020.89 32.62 0 2 -3 1084.28 32.29 0 -2 -3 1068.13 32.50 0 -2 3 1074.63 32.70 0 -2 3 1026.99 32.22 0 2 -3 1103.76 32.40 0 2 3 1067.23 32.81 0 2 3 1077.61 32.45 0 -2 -3 1028.93 31.58 0 -2 3 1044.45 29.24 0 2 3 1047.18 32.94 0 2 -3 1110.45 29.47 0 -2 -3 1053.04 23.14 0 -2 3 1065.83 26.83 0 -2 -3 1087.70 25.08 0 2 3 1088.39 24.41 0 -2 -3 1078.19 33.80 0 2 -3 1062.14 19.58 0 2 3 1032.40 19.61 0 -2 3 1058.71 19.47 0 -2 -4 966.66 35.64 0 -2 4 936.97 34.67 0 2 4 988.96 35.53 0 2 -4 1004.62 35.19 0 -2 -4 961.25 35.94 0 2 -4 964.74 35.36 0 -2 -4 971.41 35.71 0 2 -4 974.39 35.55 0 -2 4 922.44 35.21 0 2 4 952.23 35.70 0 2 4 967.47 35.98 0 -2 4 947.85 35.93 0 -2 4 982.29 35.16 0 2 4 922.76 27.29 0 2 4 873.04 34.52 0 -2 4 969.87 27.15 0 -2 -4 933.73 27.86 0 2 -4 958.51 30.93 0 -2 -4 974.53 36.78 0 -2 4 950.17 18.26 0 2 4 925.13 18.41 0 2 -4 909.55 17.84 0 -2 5 304.57 22.28 0 2 5 305.69 22.16 0 2 -5 334.56 23.19 0 -2 -5 299.63 22.54 0 -2 5 347.34 24.65 0 -2 -5 357.50 24.60 0 2 5 369.18 25.53 0 2 5 328.83 24.57 0 2 -5 351.50 24.25 0 2 -5 362.23 24.82 0 -2 5 310.14 23.21 0 -2 -5 323.03 23.39 0 -2 -5 335.49 19.48 0 -2 5 311.57 16.99 0 2 5 318.25 18.51 0 -2 -5 323.53 24.17 0 -2 5 331.12 23.59 0 2 -5 310.55 19.82 0 -2 5 324.69 10.67 0 2 5 333.31 10.91 0 2 6 352.27 26.55 0 -2 6 374.06 27.03 0 -2 -6 349.73 26.74 0 2 -6 341.68 25.57 0 -2 -6 357.01 26.74 0 2 6 400.85 28.95 0 2 -6 336.55 26.44 0 -2 6 384.96 28.77 0 -2 -6 416.91 29.24 0 2 -6 337.70 22.72 0 -2 6 379.86 26.87 0 2 6 402.47 22.97 0 2 -6 380.51 27.34 0 -2 6 329.57 18.34 0 2 6 355.90 10.81 0 -2 6 377.35 10.75 0 -2 7 212.69 22.94 0 2 7 221.03 22.12 0 -2 7 216.64 23.93 0 2 -7 208.33 23.06 0 2 7 243.62 24.73 0 -2 -7 215.80 23.35 0 -2 -7 211.97 23.11 0 -2 7 214.94 15.46 0 2 7 216.43 18.81 0 2 -7 249.17 24.50 0 2 7 196.55 7.17 0 -2 8 134.82 20.16 0 2 8 140.20 20.25 0 2 -8 182.02 22.45 0 -2 8 163.91 14.43 0 -2 -8 157.76 21.58 0 2 8 155.30 17.40 0 -2 8 168.50 23.85 0 2 -8 182.59 24.25 0 -2 -8 154.49 21.37 0 2 8 184.01 23.89 0 2 9 234.87 26.76 0 -2 9 231.77 27.42 0 2 -9 256.70 28.78 0 -2 9 201.97 16.97 0 -2 -9 225.05 27.65 0 -2 9 215.99 27.15 0 2 9 237.87 28.68 0 -2 -9 231.32 27.82 0 2 -9 238.42 27.81 0 2 10 123.04 20.72 0 -2 10 137.75 22.20 0 -2 10 147.16 14.51 0 -2 -10 133.51 23.33 0 2 -10 161.59 24.62 0 -2 10 165.40 26.31 0 2 10 156.28 25.55 0 -2 -10 184.92 26.61 0 2 -10 141.02 23.41 0 -2 11 72.65 18.51 0 2 11 56.52 14.50 0 2 -11 64.40 18.17 0 -2 -11 64.81 17.11 0 -2 -11 101.99 21.58 0 2 -11 65.16 21.62 0 -2 11 83.67 21.13 0 2 11 58.44 19.54 0 2 12 -15.09 12.26 0 -2 12 13.51 10.48 0 -2 -12 -9.53 10.89 0 2 -12 -15.57 12.10 0 2 -12 18.04 13.02 0 2 12 -1.26 10.31 0 -2 12 24.62 15.82 0 -2 -12 -10.19 10.97 0 -2 13 16.44 11.22 0 2 13 31.29 12.67 0 -2 -13 -9.81 11.47 0 2 -13 21.34 13.89 0 2 -13 29.23 15.51 0 2 13 11.38 10.79 0 -2 -13 11.61 9.55 0 -2 13 -3.32 9.72 0 -2 14 -7.97 12.30 0 2 14 40.98 15.73 0 -2 -14 -0.83 10.29 0 2 -14 2.69 8.69 0 -2 14 -5.34 11.30 0 -2 -14 5.95 9.59 0 2 14 3.44 14.12 0 2 -14 7.67 12.05 0 -2 15 -6.48 13.23 0 2 15 9.78 11.45 0 2 -15 0.07 9.83 0 -2 -15 6.66 10.78 0 2 -15 11.18 15.89 0 -2 -15 15.60 17.01 0 2 15 -5.29 14.37 0 -2 15 9.08 14.54 0 2 16 -15.56 15.36 0 -2 16 -8.42 13.41 0 3 0 4.32 3.79 0 -3 0 1.73 3.19 0 -3 0 6.79 2.94 0 3 0 6.10 3.40 0 3 1 1147.80 25.84 0 -3 -1 1105.78 19.49 0 3 1 1121.30 19.72 0 3 1 1126.18 23.51 0 -3 -1 1140.30 23.37 0 -3 -1 1102.37 25.33 0 3 1 1144.97 19.35 0 -3 -1 1096.61 18.38 0 3 -1 1124.58 18.33 0 -3 1 1088.38 19.17 0 -3 1 1077.13 18.76 0 3 -1 1115.71 18.37 0 3 1 1151.31 19.41 0 -3 -1 1111.07 18.63 0 -3 -1 1116.83 21.57 0 -3 1 1179.89 26.21 0 3 1 1107.88 22.68 0 3 -1 1140.47 25.48 0 -3 -1 1070.00 21.75 0 3 1 1119.43 22.03 0 3 1 1110.28 24.16 0 -3 1 1162.45 22.94 0 -3 1 1125.24 24.21 0 -3 -1 1106.11 24.65 0 3 -1 1091.26 24.11 0 3 -1 1109.83 22.79 0 -3 -1 1161.63 25.15 0 3 2 2362.68 37.89 0 3 2 2380.84 28.04 0 -3 -2 2405.28 27.21 0 -3 -2 2417.01 36.80 0 -3 -2 2292.14 41.56 0 -3 -2 2349.56 44.08 0 -3 2 2354.95 39.88 0 -3 -2 2422.60 39.03 0 3 2 2361.88 39.42 0 3 2 2375.32 39.76 0 3 -2 2372.79 38.60 0 -3 2 2388.97 40.06 0 3 -2 2415.96 38.79 0 -3 -2 2385.63 38.85 0 3 2 2345.09 42.84 0 -3 -2 2353.75 41.93 0 3 -2 2445.60 41.60 0 -3 -2 2443.62 33.88 0 -3 2 2384.44 41.68 0 3 2 2351.56 35.17 0 -3 2 2455.92 42.77 0 -3 -2 2432.21 36.31 0 3 2 2373.90 35.31 0 -3 2 2407.62 35.71 0 3 -2 2507.93 36.73 0 3 -2 2395.79 35.52 0 -3 -3 826.04 16.70 0 -3 -3 783.18 29.87 0 3 3 889.74 31.77 0 -3 -3 859.13 24.77 0 -3 -3 796.67 27.81 0 -3 3 819.87 28.91 0 -3 3 778.47 28.81 0 3 -3 794.57 28.31 0 -3 -3 850.63 28.72 0 3 3 821.92 28.94 0 3 3 836.24 28.75 0 3 -3 814.51 28.13 0 3 3 812.52 29.93 0 -3 -3 857.29 30.70 0 -3 -3 823.50 20.71 0 3 -3 835.26 27.09 0 -3 3 833.77 27.46 0 -3 -3 852.97 22.20 0 -3 3 844.51 26.39 0 3 -3 812.87 21.31 0 -3 -3 875.11 22.12 0 -3 3 841.61 21.11 0 3 3 831.91 21.09 0 3 4 505.79 26.55 0 -3 -4 490.88 20.88 0 -3 4 524.86 26.76 0 -3 -4 530.35 27.62 0 3 4 471.52 25.31 0 -3 -4 490.28 25.64 0 3 4 495.21 25.86 0 3 -4 516.57 25.93 0 3 -4 515.06 26.30 0 -3 -4 488.65 25.71 0 -3 4 485.92 26.06 0 -3 4 464.24 25.48 0 -3 -4 506.66 19.70 0 -3 4 509.43 22.19 0 3 -4 501.61 23.50 0 -3 4 536.39 27.58 0 3 4 495.22 26.94 0 -3 -4 492.52 26.95 0 -3 -4 522.10 18.91 0 -3 4 480.23 23.42 0 3 4 496.20 16.41 0 3 -4 488.02 16.40 0 -3 4 518.00 16.50 0 -3 -5 256.45 21.83 0 3 5 252.52 20.78 0 -3 5 254.43 20.71 0 -3 -5 220.43 19.76 0 3 -5 241.26 20.88 0 3 5 253.94 21.37 0 -3 5 229.67 19.89 0 -3 -5 245.07 20.14 0 -3 5 209.43 19.76 0 3 -5 228.45 19.98 0 3 5 207.66 20.34 0 -3 -5 216.51 15.24 0 3 5 253.45 15.21 0 3 -5 234.46 18.32 0 -3 -5 238.02 21.24 0 -3 5 268.51 17.36 0 -3 5 243.02 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130.92 22.80 0 14 -7 127.13 19.38 0 14 7 100.69 17.23 0 14 8 33.10 11.15 0 -14 8 62.63 15.11 0 -14 -8 73.31 18.26 0 14 8 51.35 13.78 0 14 -8 50.54 13.51 0 -14 8 20.54 9.93 0 -14 -8 45.55 13.88 0 -14 9 39.84 16.10 0 -14 -9 55.50 16.73 0 -14 9 24.98 11.03 0 -14 9 29.34 12.03 0 -14 -9 37.56 11.91 0 14 9 28.99 10.15 0 14 -9 31.08 10.98 0 -14 -10 -13.87 12.40 0 -14 10 -0.13 10.12 0 -14 10 5.86 9.00 0 14 10 -0.01 6.37 0 14 -10 2.63 6.51 0 -14 -10 13.38 7.79 0 -14 -11 -6.03 9.47 0 -14 11 -5.67 13.62 0 -14 -11 6.78 9.09 0 -14 12 -3.57 12.47 0 -14 -12 20.30 12.04 0 -14 -13 6.35 9.11 0 15 0 -5.59 7.58 0 15 0 -1.58 7.04 0 15 0 -0.90 7.65 0 -15 0 -4.26 7.86 0 -15 0 2.29 6.58 0 15 1 6.25 7.41 0 15 -1 -9.00 8.10 0 15 -1 0.79 7.70 0 15 1 0.92 8.21 0 -15 -1 9.27 7.58 0 15 1 10.09 8.95 0 -15 1 18.94 11.47 0 -15 -1 13.65 7.88 0 15 -1 -0.50 8.50 0 -15 1 8.33 7.66 0 15 -2 197.05 24.75 0 15 2 193.97 23.97 0 15 2 200.04 23.59 0 15 -2 221.90 25.29 0 15 2 227.59 26.77 0 -15 2 201.99 25.65 0 15 -2 210.76 26.12 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6.27 2 11 0 92.52 5.95 -2 -11 0 103.15 6.17 -2 11 0 107.12 15.60 -2 -11 0 106.04 13.18 2 11 0 100.14 11.71 2 11 0 85.78 14.47 -2 -11 0 108.86 15.18 2 -11 0 121.69 16.76 -2 11 0 95.73 15.74 -2 -11 0 121.26 16.75 2 -11 0 104.64 15.24 -2 -11 -1 -2.41 6.12 -2 11 -1 7.25 7.07 2 11 1 2.15 4.98 2 -11 1 5.53 2.63 -2 -11 -1 5.19 2.33 2 11 1 4.26 3.28 2 11 1 3.96 2.42 -2 11 -1 7.86 2.97 2 -11 1 4.72 2.66 -2 -11 -1 -0.66 3.30 -2 11 -1 6.58 6.03 2 11 1 -0.62 5.46 -2 -11 -1 11.71 8.09 -2 11 -1 6.38 8.66 2 11 1 -0.50 6.86 2 11 1 13.13 4.42 2 -11 1 -0.41 7.29 2 -11 1 11.04 7.33 -2 11 -2 222.94 22.52 -2 -11 -2 234.21 23.88 2 11 2 238.54 20.27 2 11 2 227.84 17.40 2 11 2 225.12 15.22 2 -11 2 193.38 14.22 -2 11 -2 217.16 13.23 2 11 2 224.09 15.29 2 -11 2 219.62 15.05 -2 -11 -2 235.24 13.38 2 -11 2 245.61 23.90 -2 11 -2 188.73 19.26 -2 -11 -2 211.00 13.93 2 11 2 227.95 20.17 -2 11 -2 246.98 23.84 -2 -11 -2 242.62 23.07 2 -11 2 200.62 20.65 2 11 2 200.37 20.68 2 11 2 246.14 14.77 -2 -11 -3 33.44 11.56 2 11 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3.81 4 -11 1 1.61 3.54 -4 -11 -1 2.30 3.59 -4 11 -1 3.66 4.50 4 11 1 0.18 3.80 4 -11 1 -0.34 3.92 4 11 1 7.17 8.06 -4 11 -1 1.77 6.52 4 -11 1 9.91 8.05 -4 11 -1 5.41 8.31 -4 -11 -1 11.53 8.16 4 11 1 9.02 7.72 4 -11 1 8.91 8.68 4 11 2 6.54 3.63 -4 -11 -2 14.21 8.27 4 11 2 9.35 6.01 -4 11 -2 -3.27 7.97 4 11 2 8.13 5.67 4 -11 2 11.24 6.29 4 11 2 9.93 6.04 4 -11 2 15.79 7.22 -4 -11 -2 7.17 5.00 -4 11 -2 13.05 6.43 -4 11 -2 14.59 8.28 4 11 2 10.11 5.23 4 11 2 12.92 6.43 -4 -11 -2 3.94 5.54 4 11 2 9.27 6.97 -4 11 -2 10.04 8.32 4 -11 2 3.64 7.21 -4 -11 -2 30.43 10.21 4 11 3 34.30 8.13 -4 -11 -3 53.73 14.19 4 11 3 52.33 8.52 4 11 3 45.67 7.32 -4 11 -3 54.86 12.07 -4 -11 -3 36.68 9.21 -4 11 -3 61.86 10.68 4 11 3 67.38 12.71 4 -11 3 61.13 12.14 -4 11 -3 51.92 11.73 4 11 3 32.44 8.12 4 11 3 53.16 12.13 -4 -11 -3 40.47 8.39 4 -11 3 49.77 12.98 -4 11 -3 55.35 13.10 -4 -11 -4 136.36 20.22 -4 11 -4 125.21 18.29 4 11 4 147.77 15.48 4 11 4 152.33 19.09 4 -11 4 126.67 17.85 4 11 4 128.66 14.71 4 -11 4 152.70 22.09 -4 11 -4 128.68 17.75 -4 11 -4 119.13 18.79 4 11 4 125.30 17.94 -4 -11 -4 97.01 12.10 4 11 4 113.59 11.85 -4 11 -5 -7.03 6.69 -4 -11 -5 -11.59 9.73 4 -11 5 5.17 9.90 4 11 5 10.34 6.81 4 11 5 16.77 10.28 4 11 5 3.93 4.56 -4 11 -5 -6.29 8.14 4 -11 5 1.79 7.96 -4 11 -5 -3.84 7.67 4 11 5 4.55 7.83 -4 -11 -5 4.78 4.83 -4 -11 -6 16.34 9.25 4 11 6 10.47 9.17 4 -11 6 9.03 9.01 4 11 6 8.96 5.32 4 -11 6 11.03 8.33 -4 11 -6 -7.44 6.97 -4 -11 -6 14.99 5.78 4 11 6 21.91 10.23 4 -11 7 20.78 8.72 -4 -11 -7 16.00 8.08 4 11 7 23.42 11.76 4 -11 7 19.27 9.39 -4 11 -7 14.38 7.33 4 11 7 29.53 10.21 -4 -11 -8 90.47 19.67 4 -11 8 91.35 18.66 4 11 8 118.48 22.13 4 -11 8 93.53 19.05 -4 11 -8 97.91 16.64 4 11 8 107.18 17.78 4 -11 9 54.38 16.32 -4 -11 -9 56.54 16.48 4 11 9 40.44 17.53 4 -11 9 82.10 20.24 -4 11 -9 53.83 13.02 4 11 9 53.79 13.08 -4 -11 -10 16.18 12.04 4 -11 10 4.41 8.68 -4 11 -10 -0.14 6.23 4 11 10 0.89 13.37 4 -11 10 22.01 16.73 4 -11 11 9.27 10.39 -4 -11 -11 20.83 12.80 4 11 11 27.13 14.88 4 -11 11 7.18 12.85 4 -11 12 7.29 9.96 4 11 12 19.76 13.94 4 -12 -15 13.76 13.88 4 12 -15 18.20 13.60 -4 -12 15 9.90 11.16 -4 12 15 -8.22 12.94 4 -12 -14 31.30 15.81 4 -12 -14 17.85 12.23 4 -12 -14 18.88 11.04 -4 12 14 1.73 11.50 4 12 -14 43.74 15.67 -4 -12 14 26.95 15.44 -4 -12 13 43.72 18.92 4 -12 -13 0.30 8.47 4 -12 -13 16.75 12.73 4 -12 -13 12.13 11.49 4 12 -13 9.59 13.09 -4 12 13 27.13 15.89 -4 -12 13 21.07 13.28 -4 -12 12 38.69 19.27 4 -12 -12 39.70 14.92 -4 -12 12 58.14 17.92 4 -12 -12 62.55 16.83 4 12 -12 72.67 18.21 -4 12 12 67.33 20.72 4 -12 -12 67.84 17.42 -4 -12 12 58.43 15.96 4 -12 -11 -4.31 5.94 -4 -12 11 -22.71 15.12 4 -12 -11 5.19 8.06 4 12 -11 23.75 13.62 4 -12 -11 4.65 8.10 -4 12 11 11.05 10.29 -4 -12 11 2.39 10.05 -4 -12 11 13.84 10.28 4 -12 -11 2.32 6.90 -4 12 11 7.97 7.53 4 -12 -11 1.05 5.22 4 12 -11 1.92 5.92 4 -12 -10 80.19 14.10 4 -12 -10 66.36 17.05 -4 -12 10 65.28 21.48 4 -12 -10 93.16 18.57 4 12 -10 72.79 17.31 4 -12 -10 44.00 12.47 4 -12 -10 51.01 13.72 -4 12 10 57.85 14.10 -4 -12 10 64.02 16.55 4 -12 -10 64.53 13.07 4 12 -10 80.74 14.38 4 -12 -9 30.41 9.18 4 -12 -9 12.09 9.18 -4 -12 9 0.77 9.49 4 -12 -9 24.31 10.73 4 12 -9 20.20 9.91 4 -12 -9 24.63 9.57 4 -12 -9 27.07 10.99 4 -12 -9 17.51 12.76 4 -12 -9 21.41 8.33 -4 -12 9 15.22 8.89 -4 12 9 31.32 9.33 4 12 -9 10.86 7.30 4 -12 -8 -0.50 6.43 4 -12 -8 4.79 5.92 4 -12 -8 1.55 6.60 4 12 -8 -1.76 7.07 4 -12 -8 -2.52 7.74 4 -12 -8 12.02 10.91 -4 -12 8 13.00 8.28 -4 12 8 3.20 7.21 4 -12 -8 8.01 7.00 4 12 -8 2.83 5.91 4 -12 -7 35.07 10.42 4 -12 -7 35.14 13.06 4 -12 -7 44.78 11.56 4 12 -7 33.97 9.48 4 -12 -7 32.75 8.91 4 12 -7 39.26 11.61 4 -12 -7 34.23 11.01 -4 -12 7 45.60 12.59 -4 12 7 36.46 12.26 4 -12 -7 49.75 12.24 4 -12 -6 210.58 23.73 -4 12 6 219.64 27.89 4 -12 -6 221.02 22.75 4 -12 -6 251.11 23.27 4 12 -6 217.66 22.33 4 -12 -6 236.92 21.31 -4 -12 6 296.16 28.46 4 -12 -6 217.96 22.13 -4 12 6 238.77 25.47 4 -12 -6 238.64 27.23 4 12 -6 257.74 26.55 4 -12 -5 390.94 31.04 -4 12 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16.63 4 -13 -4 64.04 13.36 -4 13 4 85.42 16.96 -4 -13 4 59.09 13.79 -4 -13 4 71.51 10.97 4 -13 -4 63.14 14.31 4 -13 -3 13.12 8.92 -4 13 3 1.42 3.08 -4 13 3 -0.17 8.31 4 -13 -3 3.16 3.60 4 13 -3 4.21 3.73 -4 13 3 -0.85 3.91 -4 13 3 -1.13 8.01 4 13 -3 -8.46 9.89 4 -13 -3 4.33 6.21 -4 13 3 6.40 7.24 -4 -13 3 5.42 8.22 -4 -13 3 -1.75 4.29 4 -13 -3 -2.87 7.45 4 -13 -2 3.10 6.36 -4 13 2 -0.45 4.03 -4 13 2 -2.57 7.02 4 13 -2 1.79 2.93 -4 13 2 -0.20 3.95 4 -13 -2 6.21 3.74 -4 -13 2 -0.87 4.06 -4 13 2 -9.28 8.18 4 13 -2 2.88 7.08 -4 -13 2 1.13 6.62 4 -13 -2 -2.90 7.00 4 -13 -2 -0.84 5.75 -4 13 2 0.31 8.36 -4 -13 2 1.66 5.05 -4 13 1 293.24 29.00 4 -13 -1 281.04 17.33 4 13 -1 270.26 17.21 -4 -13 1 279.95 17.60 -4 13 1 283.20 17.34 -4 -13 1 228.50 21.97 -4 13 1 289.57 28.54 4 -13 -1 312.96 28.56 -4 13 1 266.68 28.32 -4 -13 1 332.69 30.30 4 13 -1 294.98 28.76 4 -13 -1 307.96 28.50 -4 -13 1 287.55 25.18 -4 13 0 39.63 12.65 4 13 0 23.01 5.84 4 -13 0 16.53 4.85 -4 -13 0 17.97 5.05 -4 13 0 28.59 6.00 4 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-12 5 21.97 15.81 -14 12 5 -10.36 12.99 -14 12 5 2.65 7.62 -14 -12 4 -9.89 12.11 -14 12 4 -25.84 15.31 -14 12 4 8.95 10.23 -14 -12 3 17.46 11.43 -14 12 3 53.71 20.28 -14 -12 2 -7.15 10.57 -15 0 9 -9.57 11.94 15 0 -8 -12.11 12.48 -15 0 8 4.43 12.43 -15 0 7 -19.29 17.27 15 0 -7 -21.42 15.49 15 0 -7 14.34 14.90 -15 0 7 -8.82 12.91 15 0 -6 2.46 8.61 -15 0 6 10.09 15.03 15 0 -6 -11.71 10.92 15 0 -5 3.73 8.20 -15 0 5 -2.52 12.16 15 0 -5 -16.16 14.45 -15 0 5 0.05 9.07 15 0 -4 26.24 12.08 -15 0 4 15.91 12.48 15 0 -4 14.31 11.84 -15 0 4 36.71 16.71 15 0 -3 -1.38 9.03 15 0 -3 -6.84 12.61 15 0 -2 -17.29 10.64 15 0 -2 -4.05 9.89 15 0 -1 6.79 10.83 15 0 0 44.46 18.87 15 0 1 4.06 12.08 -15 1 10 12.73 12.92 15 1 -9 9.15 10.16 -15 1 9 5.60 10.06 15 1 -8 -12.34 11.42 15 -1 -8 -3.46 13.48 -15 -1 8 34.07 19.99 -15 1 8 6.91 11.46 15 -1 -7 0.63 9.73 -15 -1 7 -10.62 11.33 -15 1 7 4.75 14.19 15 1 -7 5.16 10.77 15 1 -7 21.61 15.32 15 -1 -7 3.71 11.20 -15 1 7 32.68 15.31 -15 -1 7 -0.64 9.25 15 -1 -6 -2.89 8.87 -15 -1 6 17.65 16.21 -15 1 6 23.59 18.43 15 1 -6 15.03 13.57 15 1 -6 -4.87 11.43 15 -1 -6 8.45 12.77 -15 -1 6 43.98 17.72 -15 1 6 31.22 16.29 15 1 -5 4.67 7.85 15 -1 -5 0.77 8.18 -15 -1 5 9.39 12.54 -15 1 5 7.90 13.87 15 1 -5 13.35 12.08 15 -1 -5 -3.62 10.76 -15 1 5 12.08 9.91 -15 -1 5 -7.22 8.89 15 1 -4 25.49 12.91 15 -1 -4 11.50 10.97 -15 -1 4 21.69 18.29 -15 1 4 -2.46 15.85 15 1 -4 -4.71 10.02 15 -1 -4 20.20 13.71 -15 -1 4 16.57 13.14 -15 1 4 24.41 15.32 15 1 -3 5.92 9.28 15 -1 -3 -16.93 13.19 15 1 -3 -0.72 10.13 15 -1 -3 1.26 10.53 15 1 -2 11.43 10.42 15 -1 -2 26.31 12.81 15 1 -2 47.47 19.50 15 -1 -2 27.66 12.96 15 1 -1 20.47 14.01 15 -1 -1 -18.94 17.14 15 1 0 3.59 8.41 15 -1 0 13.27 11.35 15 1 1 16.47 9.05 -15 2 10 12.80 10.66 15 2 -9 -1.14 9.77 -15 2 9 3.64 12.59 15 2 -8 6.54 11.30 -15 2 8 -0.94 8.89 15 -2 -7 -7.28 10.01 -15 -2 7 2.13 15.55 -15 2 7 18.67 15.86 15 2 -7 -2.91 11.29 15 2 -7 -0.82 10.01 -15 2 7 10.43 12.04 -15 -2 7 -3.66 9.42 15 -2 -6 1.21 7.61 -15 -2 6 -16.67 13.68 -15 2 6 6.38 11.97 15 2 -6 -6.97 10.88 15 2 -6 -6.81 14.56 15 -2 -6 -4.02 10.80 -15 -2 6 16.92 13.80 -15 2 6 -0.88 9.34 15 -2 -5 -7.06 11.73 -15 -2 5 21.76 15.76 -15 2 5 -3.28 10.67 15 2 -5 2.40 10.08 15 2 -5 -1.82 10.31 15 -2 -5 -14.93 14.08 -15 2 5 8.34 8.79 -15 -2 5 23.96 13.01 15 2 -4 5.48 8.85 15 -2 -4 0.09 9.24 -15 -2 4 -6.83 11.36 -15 2 4 4.32 10.01 15 2 -4 -0.54 12.12 15 -2 -4 8.32 10.49 -15 2 4 26.01 15.03 -15 -2 4 30.72 15.38 15 2 -3 -2.12 7.40 15 -2 -3 -6.18 8.89 15 2 -3 -2.50 8.74 15 -2 -3 -22.56 14.37 15 -2 -2 -7.93 10.48 15 2 -2 -5.63 13.15 15 -2 -2 -15.52 14.51 15 -2 -1 -4.01 8.34 15 2 -1 3.58 11.95 15 -2 -1 -6.59 9.69 15 2 0 34.98 17.37 15 2 1 3.04 8.26 -15 3 11 -12.81 12.26 -15 3 10 -8.31 11.75 15 3 -9 21.36 14.09 -15 3 9 -8.41 10.97 15 3 -8 -6.35 15.72 -15 3 8 -12.68 14.61 15 -3 -7 22.32 13.16 -15 -3 7 7.14 11.59 15 3 -7 -2.70 10.84 -15 3 7 29.99 14.09 15 -3 -6 10.78 8.80 -15 -3 6 32.76 18.00 -15 3 6 -18.44 16.19 15 3 -6 15.70 12.90 15 3 -6 18.18 17.00 -15 3 6 2.74 9.47 15 -3 -5 4.08 8.68 -15 -3 5 10.30 13.63 -15 3 5 11.23 12.00 15 3 -5 18.56 17.07 15 3 -5 15.67 11.82 15 -3 -5 -5.37 11.24 -15 3 5 18.20 13.16 15 -3 -4 -5.84 7.49 15 3 -4 -2.88 7.74 -15 -3 4 8.24 9.86 -15 3 4 -21.89 17.91 15 3 -4 14.45 13.15 15 3 -4 -4.78 11.10 15 -3 -4 1.72 10.92 -15 3 4 -1.87 9.98 15 3 -3 -5.06 10.08 15 -3 -3 17.07 10.65 15 3 -3 -13.29 11.51 15 -3 -3 12.47 12.20 15 -3 -2 16.77 11.37 15 3 -2 50.10 19.91 15 -3 -1 0.50 7.42 15 3 -1 -2.69 10.45 15 3 0 34.34 15.93 15 3 1 8.49 9.16 -15 4 11 -0.88 9.20 -15 4 10 3.82 9.96 15 4 -9 19.02 13.24 -15 4 9 7.94 9.53 15 4 -8 2.55 9.11 -15 4 8 -0.45 10.04 15 4 -7 13.94 11.75 -15 4 7 -38.53 15.96 15 -4 -6 11.96 9.83 -15 -4 6 5.25 11.03 -15 4 6 12.48 10.93 15 4 -6 21.72 13.62 -15 4 6 -20.22 12.13 15 -4 -5 -7.87 8.54 -15 -4 5 37.15 18.12 -15 4 5 13.60 14.08 15 4 -5 23.34 12.92 15 4 -5 -3.65 13.05 -15 4 5 22.10 12.30 15 -4 -4 -7.95 8.73 15 4 -4 -1.67 10.58 15 4 -4 -2.43 10.47 -15 4 4 -4.58 12.34 15 4 -3 1.40 7.84 15 -4 -3 -8.81 8.27 15 4 -3 9.82 9.91 15 4 -3 2.02 10.04 15 -4 -2 0.30 11.96 15 4 -2 -5.54 8.86 15 -4 -1 1.79 7.28 15 4 -1 0.16 9.35 15 4 0 -12.85 13.39 15 4 1 -22.83 15.10 -15 5 11 31.57 15.93 -15 5 10 -18.71 17.88 15 5 -9 36.45 16.47 -15 5 9 11.10 10.48 15 5 -8 10.87 12.54 -15 5 8 7.00 10.11 15 5 -7 9.30 10.68 -15 5 7 4.13 11.32 15 5 -6 13.98 14.77 -15 5 6 11.02 12.47 15 -5 -5 53.47 16.96 15 5 -5 30.29 15.65 -15 5 5 0.02 9.33 15 -5 -4 -10.18 13.09 15 5 -4 18.89 11.18 15 5 -4 -4.66 9.70 -15 5 4 23.44 11.36 15 -5 -3 58.77 17.50 15 5 -3 52.47 19.80 15 -5 -2 9.53 9.17 15 5 -2 -13.11 12.66 15 -5 -1 1.74 8.37 15 5 -1 3.88 9.64 15 -5 0 6.89 7.40 15 5 0 31.71 16.14 -15 6 10 34.24 17.27 15 6 -9 22.15 14.87 -15 6 9 6.10 11.48 15 6 -8 -2.30 11.44 -15 6 8 -1.26 8.74 15 6 -7 0.74 10.25 -15 6 7 -2.75 8.45 15 6 -6 10.08 13.11 -15 6 6 17.52 13.41 15 6 -5 1.04 9.16 -15 6 5 0.75 10.39 15 6 -1 25.49 14.95 15 6 0 24.30 12.90 -15 7 9 24.61 16.11 15 7 -8 33.67 15.82 -15 7 8 10.23 12.62 15 7 -7 20.74 15.45 -15 7 7 8.87 8.93 15 7 -6 -16.55 12.14 -15 7 6 3.58 9.78 -15 7 5 -0.60 9.11 -15 8 9 -3.66 10.27 15 8 -8 -1.53 9.73 -15 8 8 29.79 14.36 15 8 -7 7.42 10.60 -15 8 7 10.92 13.68 -15 8 6 -16.38 13.75 15 9 -8 -9.53 13.23 -15 9 7 20.23 12.04 -15 9 6 -9.43 10.29 16 0 -4 29.07 14.04 16 0 -3 -21.07 12.46 16 1 -4 -7.51 8.94 16 1 -3 51.97 16.99 16 -1 -3 20.14 12.16 16 2 -6 6.95 10.03 16 2 -5 9.07 10.60 16 2 -5 4.09 10.88 16 2 -4 4.91 10.11 16 2 -4 -14.55 14.04 16 3 -6 7.07 10.83 16 3 -5 11.01 10.88 16 3 -5 -6.20 12.13 16 3 -4 -5.55 9.80 16 3 -4 6.80 10.32 16 4 -6 2.78 11.17 16 4 -5 -10.86 11.26 16 5 -6 0.18 10.64 0 0 0 0.00 0.00 TITL KY463_reprocess in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 12.046074 17.198544 13.069988 90.0000 109.4628 90.0000 ZERR 4.00 0.000602 0.000548 0.000596 0.0000 0.0052 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H B N UNIT 136.00 120.00 4.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 42714 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.276 _oxdiff_exptl_absorpt_empirical_full_min 0.738