#------------------------------------------------------------------------------ #$Date: 2025-03-28 04:19:37 +0100 (Fri, 28 Mar 2025) $ #$Revision: 298640 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023457.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023457 loop_ _publ_author_name 'Yun-Deng, Wu' 'Hui, Wan' 'Yun, Xia' 'Jie, Ni' 'Jian, Li' 'Hui, Zhang' 'Xiang-Yang, Xu' 'Jun, Xie' _publ_section_title ; Crystal structure of the possible sulindac impurity 2-(5-fluoro-2-methyl-1H-inden-3-yl)acetonitrile ; _journal_coeditor_code WM5750 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 341 _journal_page_last 344 _journal_paper_doi 10.1107/S2056989025002622 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C12 H10 F N' _chemical_formula_moiety 'C12 H10 F N' _chemical_formula_sum 'C12 H10 F N' _chemical_formula_weight 187.21 _chemical_name_systematic ; 2-(5-Fluoro-2-methyl-1H-inden-3-yl)acetonitrile ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 99.176(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.5248(5) _cell_length_b 15.1897(10) _cell_length_c 17.1823(9) _cell_measurement_reflns_used 9932 _cell_measurement_temperature 170.0 _cell_measurement_theta_max 26.74 _cell_measurement_theta_min 2.68 _cell_volume 1938.8(2) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 170.0 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_unetI/netI 0.0188 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 28954 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.774 _diffrn_reflns_theta_min 2.401 _diffrn_source 'sealed tube' _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.283 _exptl_crystal_description block _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.23 _refine_diff_density_max 0.212 _refine_diff_density_min -0.206 _refine_ls_extinction_coef 0.0048(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 256 _refine_ls_number_reflns 4137 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0390 _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^)+(0.0464P)^2^+0.5292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0984 _refine_ls_wR_factor_ref 0.1046 _reflns_number_gt 3530 _reflns_number_total 4137 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mo_201214_gs1_2_0m_a.res in P2(1)/n mo_201214_gs1_2_0m.res created by SHELXL-2018/3 at 22:26:39 on 26-Feb-2025 REM Old TITL mo_201214_GS1_2_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.171, Rweak 0.005, Alpha 0.022 REM 0.688 for 158 systematic absences, Orientation as input REM Formula found by SHELXT: C24 N2 O2 CELL 0.71073 7.5248 15.1897 17.1823 90 99.176 90 ZERR 8 0.0005 0.001 0.0009 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N UNIT 96 80 8 8 L.S. 20 PLAN 1 SIZE 0.23 0.29 0.42 TEMP -103.15 CONF BOND $h htab list 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.046400 0.529200 EXTI 0.004805 FVAR 0.31628 F1 3 0.080055 0.189813 0.052535 11.00000 0.07910 0.06275 = 0.05806 -0.02828 -0.00435 0.00113 N1 4 0.462765 0.134219 0.357640 11.00000 0.04939 0.03351 = 0.04956 0.00274 -0.00034 0.00662 C1 1 0.161712 0.249617 0.179532 11.00000 0.03561 0.03306 = 0.04311 -0.00150 0.00599 0.00308 AFIX 43 H1 2 0.142597 0.194447 0.202895 11.00000 -1.20000 AFIX 0 C2 1 0.135192 0.261003 0.098710 11.00000 0.04054 0.04982 = 0.04147 -0.01470 0.00067 0.00438 C3 1 0.161628 0.339072 0.061894 11.00000 0.04350 0.06687 = 0.02912 0.00151 0.00345 0.00917 AFIX 43 H3 2 0.141755 0.343036 0.006001 11.00000 -1.20000 AFIX 0 C4 1 0.217928 0.412080 0.107878 11.00000 0.03674 0.04890 = 0.03560 0.01142 0.00657 0.00391 AFIX 43 H4 2 0.236765 0.466889 0.083839 11.00000 -1.20000 AFIX 0 C5 1 0.246245 0.404114 0.188994 11.00000 0.02652 0.03431 = 0.03354 0.00642 0.00554 0.00326 C6 1 0.217821 0.323247 0.224684 11.00000 0.02588 0.03093 = 0.03234 0.00257 0.00591 0.00464 C7 1 0.257706 0.335311 0.310243 11.00000 0.03153 0.03138 = 0.03058 0.00471 0.00784 0.00801 C8 1 0.308135 0.418604 0.327414 11.00000 0.03364 0.03416 = 0.03421 0.00103 0.00253 0.00706 C9 1 0.305647 0.470276 0.252502 11.00000 0.03484 0.02999 = 0.04102 0.00501 0.00336 0.00008 AFIX 23 H9A 2 0.219788 0.519996 0.249653 11.00000 -1.20000 H9B 2 0.426803 0.493474 0.248492 11.00000 -1.20000 AFIX 0 C10 1 0.239615 0.262980 0.368172 11.00000 0.05220 0.03652 = 0.03764 0.01018 0.01725 0.01123 AFIX 23 H10A 2 0.262345 0.287413 0.422263 11.00000 -1.20000 H10B 2 0.114754 0.240222 0.358457 11.00000 -1.20000 AFIX 0 C11 1 0.364654 0.190125 0.362652 11.00000 0.04180 0.02984 = 0.02839 0.00463 -0.00010 -0.00044 C12 1 0.361149 0.460696 0.406333 11.00000 0.05862 0.04783 = 0.04113 -0.00911 -0.00230 0.00754 AFIX 137 H12A 2 0.282934 0.511371 0.411000 11.00000 -1.50000 H12B 2 0.486549 0.480414 0.411934 11.00000 -1.50000 H12C 2 0.348725 0.417899 0.447807 11.00000 -1.50000 AFIX 0 F2 3 0.926397 0.553500 0.405920 11.00000 0.09370 0.04825 = 0.05583 -0.02375 -0.01780 0.00700 N2 4 0.529283 0.591110 0.100513 11.00000 0.05275 0.03943 = 0.07578 0.01819 0.01457 0.01197 C13 1 0.839475 0.485669 0.283003 11.00000 0.03691 0.02940 = 0.04102 -0.00253 -0.00106 0.00448 AFIX 43 H13 2 0.857248 0.539097 0.256548 11.00000 -1.20000 AFIX 0 C14 1 0.869290 0.479514 0.364231 11.00000 0.04847 0.03961 = 0.04263 -0.01449 -0.00608 0.00856 C15 1 0.845531 0.403995 0.405599 11.00000 0.05237 0.05587 = 0.02940 -0.00340 0.00124 0.01275 AFIX 43 H15 2 0.868240 0.403684 0.461595 11.00000 -1.20000 AFIX 0 C16 1 0.787623 0.328159 0.363795 11.00000 0.04132 0.04409 = 0.03338 0.00592 0.00795 0.00677 AFIX 43 H16 2 0.769749 0.275137 0.390833 11.00000 -1.20000 AFIX 0 C17 1 0.756459 0.330975 0.282459 11.00000 0.02910 0.03157 = 0.03300 0.00206 0.00668 0.00458 C18 1 0.781969 0.409197 0.242190 11.00000 0.02569 0.02891 = 0.03250 0.00015 0.00332 0.00481 C19 1 0.738094 0.392335 0.157416 11.00000 0.02673 0.02676 = 0.03055 0.00154 0.00511 0.00351 C20 1 0.687861 0.307975 0.145005 11.00000 0.03024 0.02818 = 0.03279 -0.00002 0.00663 0.00216 C21 1 0.695550 0.260847 0.222616 11.00000 0.03555 0.02734 = 0.03626 0.00320 0.00833 -0.00032 AFIX 23 H21A 2 0.575673 0.237782 0.229008 11.00000 -1.20000 H21B 2 0.782483 0.211482 0.227027 11.00000 -1.20000 AFIX 0 C22 1 0.752930 0.461310 0.095892 11.00000 0.03686 0.02950 = 0.03494 0.00427 0.00686 0.00141 AFIX 23 H22A 2 0.877380 0.484612 0.103829 11.00000 -1.20000 H22B 2 0.729198 0.433713 0.043056 11.00000 -1.20000 AFIX 0 C23 1 0.627114 0.534414 0.098545 11.00000 0.03742 0.03120 = 0.04161 0.01002 0.00400 -0.00182 C24 1 0.630872 0.261472 0.068646 11.00000 0.05361 0.03277 = 0.03779 -0.00492 0.00521 0.00058 AFIX 137 H24A 2 0.626613 0.303465 0.025088 11.00000 -1.50000 H24B 2 0.511239 0.235723 0.068025 11.00000 -1.50000 H24C 2 0.717319 0.214674 0.062657 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_201214_gs1_2_0m_a.res in P2(1)/n REM wR2 = 0.1046, GooF = S = 1.028, Restrained GooF = 1.028 for all data REM R1 = 0.0390 for 3530 Fo > 4sig(Fo) and 0.0466 for all 4137 data REM 256 parameters refined using 0 restraints END WGHT 0.0464 0.5292 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y-1/2, -z+1/2 HTAB C10 N2_$1 EQIV $2 -x+2, -y+1, -z+1 HTAB C15 F2_$2 EQIV $3 -x+3/2, y+1/2, -z+1/2 HTAB C22 N1_$3 REM Highest difference peak 0.212, deepest hole -0.206, 1-sigma level 0.036 Q1 1 0.6591 0.3599 0.1444 11.00000 0.05 0.21 REM The information below was added by Olex2. REM REM R1 = 0.0390 for 3530 Fo > 4sig(Fo) and 0.0466 for all 29464 data REM 256 parameters refined using n/a restraints REM Highest difference peak 0.21, deepest hole -0.21 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0466 REM R1_gt = 0.0390 REM wR_ref = 0.1046 REM GOOF = 1.028 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 29464 REM Reflections_gt = 3530 REM Parameters = 256 REM Hole = -0.21 REM Peak = 0.21 REM Flack = n/a ; _cod_data_source_file wm5750.cif _cod_data_source_block I _cod_database_code 2023457 _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. ; _shelx_estimated_absorpt_t_min 0.964 _shelx_estimated_absorpt_t_max 0.980 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group F F1 0.08006(14) 0.18981(6) 0.05253(6) 0.0683(3) Uani d 1 . . N N1 0.46276(16) 0.13422(7) 0.35764(7) 0.0451(3) Uani d 1 . . C C1 0.16171(16) 0.24962(8) 0.17953(8) 0.0373(3) Uani d 1 . . H H1 0.142597 0.194447 0.202895 0.045 Uiso calc 1 . . C C2 0.13519(18) 0.26100(9) 0.09871(8) 0.0446(3) Uani d 1 . . C C3 0.16163(18) 0.33907(10) 0.06189(8) 0.0468(3) Uani d 1 . . H H3 0.141755 0.343036 0.006001 0.056 Uiso calc 1 . . C C4 0.21793(17) 0.41208(9) 0.10788(7) 0.0403(3) Uani d 1 . . H H4 0.236765 0.466889 0.083839 0.048 Uiso calc 1 . . C C5 0.24625(15) 0.40411(8) 0.18899(7) 0.0314(3) Uani d 1 . . C C6 0.21782(14) 0.32325(7) 0.22468(7) 0.0296(2) Uani d 1 . . C C7 0.25771(15) 0.33531(8) 0.31024(7) 0.0308(3) Uani d 1 . . C C8 0.30813(16) 0.41860(8) 0.32741(7) 0.0343(3) Uani d 1 . . C C9 0.30565(16) 0.47028(8) 0.25250(7) 0.0356(3) Uani d 1 . . H H9A 0.219788 0.519996 0.249653 0.043 Uiso calc 1 . . H H9B 0.426803 0.493474 0.248492 0.043 Uiso calc 1 . . C C10 0.23961(19) 0.26298(8) 0.36817(8) 0.0410(3) Uani d 1 . . H H10A 0.262345 0.287413 0.422263 0.049 Uiso calc 1 . . H H10B 0.114754 0.240222 0.358457 0.049 Uiso calc 1 . . C C11 0.36465(16) 0.19013(8) 0.36265(7) 0.0340(3) Uani d 1 . . C C12 0.3611(2) 0.46070(10) 0.40633(8) 0.0503(4) Uani d 1 . . H H12A 0.282934 0.511371 0.411000 0.075 Uiso calc 1 . . H H12B 0.486549 0.480414 0.411934 0.075 Uiso calc 1 . . H H12C 0.348725 0.417899 0.447807 0.075 Uiso calc 1 . . F F2 0.92640(14) 0.55350(6) 0.40592(5) 0.0692(3) Uani d 1 . . N N2 0.52928(17) 0.59111(8) 0.10051(8) 0.0555(3) Uani d 1 . . C C13 0.83947(16) 0.48567(8) 0.28300(7) 0.0366(3) Uani d 1 . . H H13 0.857248 0.539097 0.256548 0.044 Uiso calc 1 . . C C14 0.86929(19) 0.47951(9) 0.36423(8) 0.0450(3) Uani d 1 . . C C15 0.84553(19) 0.40399(10) 0.40560(8) 0.0465(3) Uani d 1 . . H H15 0.868240 0.403684 0.461595 0.056 Uiso calc 1 . . C C16 0.78762(17) 0.32816(9) 0.36380(7) 0.0394(3) Uani d 1 . . H H16 0.769749 0.275137 0.390833 0.047 Uiso calc 1 . . C C17 0.75646(15) 0.33098(7) 0.28246(7) 0.0310(3) Uani d 1 . . C C18 0.78197(14) 0.40920(7) 0.24219(7) 0.0292(2) Uani d 1 . . C C19 0.73809(14) 0.39234(7) 0.15742(6) 0.0280(2) Uani d 1 . . C C20 0.68786(15) 0.30797(7) 0.14500(7) 0.0302(2) Uani d 1 . . C C21 0.69555(16) 0.26085(7) 0.22262(7) 0.0328(3) Uani d 1 . . H H21A 0.575673 0.237782 0.229008 0.039 Uiso calc 1 . . H H21B 0.782483 0.211482 0.227027 0.039 Uiso calc 1 . . C C22 0.75293(16) 0.46131(7) 0.09589(7) 0.0336(3) Uani d 1 . . H H22A 0.877380 0.484612 0.103829 0.040 Uiso calc 1 . . H H22B 0.729198 0.433713 0.043056 0.040 Uiso calc 1 . . C C23 0.62711(17) 0.53441(8) 0.09855(7) 0.0370(3) Uani d 1 . . C C24 0.63087(19) 0.26147(8) 0.06865(8) 0.0416(3) Uani d 1 . . H H24A 0.626613 0.303465 0.025088 0.062 Uiso calc 1 . . H H24B 0.511239 0.235723 0.068025 0.062 Uiso calc 1 . . H H24C 0.717319 0.214674 0.062657 0.062 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F1 0.0791(7) 0.0627(6) 0.0581(6) 0.0011(5) -0.0044(5) -0.0283(5) N1 0.0494(6) 0.0335(6) 0.0496(7) 0.0066(5) -0.0003(5) 0.0027(5) C1 0.0356(6) 0.0331(6) 0.0431(7) 0.0031(5) 0.0060(5) -0.0015(5) C2 0.0405(7) 0.0498(8) 0.0415(7) 0.0044(6) 0.0007(5) -0.0147(6) C3 0.0435(7) 0.0669(9) 0.0291(6) 0.0092(6) 0.0035(5) 0.0015(6) C4 0.0367(6) 0.0489(7) 0.0356(6) 0.0039(5) 0.0066(5) 0.0114(5) C5 0.0265(5) 0.0343(6) 0.0335(6) 0.0033(4) 0.0055(4) 0.0064(5) C6 0.0259(5) 0.0309(6) 0.0323(6) 0.0046(4) 0.0059(4) 0.0026(4) C7 0.0315(6) 0.0314(6) 0.0306(6) 0.0080(4) 0.0078(4) 0.0047(4) C8 0.0336(6) 0.0342(6) 0.0342(6) 0.0071(5) 0.0025(5) 0.0010(5) C9 0.0348(6) 0.0300(6) 0.0410(7) 0.0001(5) 0.0034(5) 0.0050(5) C10 0.0522(8) 0.0365(7) 0.0376(7) 0.0112(6) 0.0172(6) 0.0102(5) C11 0.0418(6) 0.0298(6) 0.0284(6) -0.0004(5) -0.0001(5) 0.0046(4) C12 0.0586(9) 0.0478(8) 0.0411(7) 0.0075(7) -0.0023(6) -0.0091(6) F2 0.0937(7) 0.0482(5) 0.0558(5) 0.0070(5) -0.0178(5) -0.0238(4) N2 0.0527(7) 0.0394(6) 0.0758(9) 0.0120(6) 0.0146(6) 0.0182(6) C13 0.0369(6) 0.0294(6) 0.0410(7) 0.0045(5) -0.0011(5) -0.0025(5) C14 0.0485(8) 0.0396(7) 0.0426(7) 0.0086(6) -0.0061(6) -0.0145(6) C15 0.0524(8) 0.0559(8) 0.0294(6) 0.0127(6) 0.0012(6) -0.0034(6) C16 0.0413(7) 0.0441(7) 0.0334(6) 0.0068(5) 0.0079(5) 0.0059(5) C17 0.0291(5) 0.0316(6) 0.0330(6) 0.0046(4) 0.0067(4) 0.0021(5) C18 0.0257(5) 0.0289(6) 0.0325(6) 0.0048(4) 0.0033(4) 0.0001(4) C19 0.0267(5) 0.0268(5) 0.0305(6) 0.0035(4) 0.0051(4) 0.0015(4) C20 0.0302(5) 0.0282(6) 0.0328(6) 0.0022(4) 0.0066(4) 0.0000(4) C21 0.0356(6) 0.0273(6) 0.0363(6) -0.0003(4) 0.0083(5) 0.0032(5) C22 0.0369(6) 0.0295(6) 0.0349(6) 0.0014(5) 0.0069(5) 0.0043(5) C23 0.0374(6) 0.0312(6) 0.0416(7) -0.0018(5) 0.0040(5) 0.0100(5) C24 0.0536(8) 0.0328(6) 0.0378(7) 0.0006(5) 0.0052(6) -0.0049(5) 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' F F 0.0171 0.0103 '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' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 1 0 0 1 0 0 -1 0 0 -1 0 0 2 0 0 2 0 0 3 0 0 -3 0 0 3 0 0 3 0 0 4 0 0 4 0 0 -4 0 0 4 0 0 5 0 0 5 0 0 5 0 0 -5 0 0 6 0 0 6 0 0 6 0 0 -6 0 0 7 0 0 7 0 0 7 0 0 8 0 0 8 0 0 8 0 0 9 0 0 9 0 0 9 0 0 -1 -1 0 -1 -1 0 1 -1 0 1 -1 0 1 -1 0 1 1 0 1 1 0 -1 1 0 -1 1 0 -1 1 0 -2 1 0 2 1 0 3 -1 0 -3 -1 0 3 -1 0 3 -1 0 3 1 0 -3 1 0 3 1 0 -3 1 0 4 -1 0 4 -1 0 -4 -1 0 4 -1 0 4 1 0 -4 1 0 4 1 0 5 -1 0 -5 -1 0 5 -1 0 5 -1 0 -5 1 0 5 1 0 5 1 0 5 1 0 6 -1 0 -6 -1 0 6 -1 0 6 -1 0 -6 1 0 6 1 0 6 1 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-1 -4 19 -1 4 19 1 4 -19 1 4 -19 0 -4 -19 0 -4 19 0 4 -19 1 -4 19 -1 -4 -19 1 4 19 -1 4 -19 -2 -4 -19 2 -4 19 2 4 19 -2 4 -19 5 -5 -19 5 -5 -19 5 5 -19 4 -5 -19 4 -5 -19 4 -5 -19 4 5 -19 4 5 -19 3 -5 -19 3 -5 -19 -3 5 19 3 5 -19 3 5 -19 -2 -5 19 2 -5 -19 2 -5 -19 -2 5 19 2 5 -19 2 5 -19 -1 -5 19 1 -5 -19 1 -5 -19 1 5 -19 1 5 -19 -1 5 19 0 -5 -19 0 -5 19 0 5 19 0 5 -19 -1 -5 -19 1 -5 19 1 5 19 -1 5 -19 -2 -5 -19 2 -5 19 -2 5 -19 2 5 19 4 -6 -19 4 -6 -19 4 -6 -19 -4 6 19 4 6 -19 4 6 -19 4 6 -19 3 -6 -19 3 -6 -19 3 6 -19 -3 6 19 3 6 -19 2 -6 -19 2 -6 -19 -2 -6 19 2 6 -19 -2 6 19 2 6 -19 -1 -6 19 1 -6 -19 1 6 -19 -1 6 19 1 6 -19 0 -6 -19 0 -6 19 0 6 -19 0 6 19 -1 -6 -19 1 -6 19 1 6 19 1 6 19 -1 6 -19 1 6 19 2 -6 19 -2 -6 -19 -2 6 -19 2 6 19 2 6 19 4 -7 -19 4 -7 -19 4 -7 -19 4 7 -19 4 7 -19 4 7 -19 -4 7 19 4 7 -19 4 7 -19 3 -7 -19 3 -7 -19 3 7 -19 3 7 -19 2 -7 -19 2 -7 -19 -2 -7 19 -2 7 19 -2 7 19 2 7 -19 2 7 -19 1 -7 -19 -1 -7 19 1 7 -19 -1 7 19 1 7 -19 -1 7 19 0 -7 19 0 -7 -19 0 7 -19 0 7 19 0 7 19 1 -7 19 -1 -7 -19 1 7 19 -1 7 -19 1 7 19 3 -8 -19 3 -8 -19 -3 8 19 -3 8 19 3 8 -19 3 8 -19 -2 -8 19 2 -8 -19 2 8 -19 -2 8 19 2 8 -19 -2 8 19 -1 -8 19 1 -8 -19 -1 8 19 1 8 -19 0 -8 19 0 -8 -19 0 8 -19 0 8 19 0 8 19 1 -8 19 -1 -8 -19 -1 8 -19 2 -9 -19 -2 9 19 -2 9 19 2 9 -19 2 9 -19 1 -9 -19 -1 -9 19 -1 9 19 1 9 -19 0 9 19 5 0 -20 4 0 -20 4 0 -20 3 0 -20 3 0 -20 -3 0 20 2 0 -20 -2 0 20 2 0 -20 1 0 -20 -1 0 20 1 0 -20 0 0 20 0 0 -20 1 0 20 -1 0 -20 -2 0 -20 2 0 20 5 -1 -20 5 1 -20 5 1 -20 4 -1 -20 4 1 -20 4 1 -20 3 -1 -20 -3 -1 20 3 -1 -20 -3 1 20 3 1 -20 3 1 -20 2 -1 -20 2 -1 -20 -2 -1 20 2 1 -20 2 1 -20 1 -1 -20 -1 -1 20 1 -1 -20 -1 1 20 1 1 -20 1 1 -20 0 -1 -20 0 -1 20 0 1 20 1 -1 20 -1 -1 -20 -1 1 -20 1 1 20 2 -1 20 -2 -1 -20 -2 1 -20 2 1 20 4 -2 -20 4 -2 -20 4 2 -20 3 -2 -20 3 -2 -20 -3 2 20 3 2 -20 3 2 -20 -2 -2 20 2 -2 -20 2 -2 -20 2 2 -20 -2 2 20 2 2 -20 -1 -2 20 1 -2 -20 1 -2 -20 -1 2 20 1 2 -20 1 2 -20 0 -2 20 0 -2 -20 1 -2 20 -1 -2 -20 -1 2 -20 1 2 20 -2 -2 -20 2 -2 20 2 2 20 -2 2 -20 4 -3 -20 4 -3 -20 4 3 -20 4 3 -20 3 -3 -20 3 3 -20 3 3 -20 -3 3 20 2 -3 -20 -2 -3 20 2 -3 -20 2 3 -20 2 3 -20 -2 3 20 1 -3 -20 -1 -3 20 1 -3 -20 1 3 -20 -1 3 20 1 3 -20 0 -3 -20 0 -3 20 0 3 20 -1 -3 -20 1 -3 20 -1 3 -20 1 3 20 2 -3 20 -2 3 -20 2 3 20 4 -4 -20 4 -4 -20 4 -4 -20 4 4 -20 3 -4 -20 3 -4 -20 3 4 -20 3 4 -20 -3 4 20 2 -4 -20 2 -4 -20 -2 -4 20 2 4 -20 -2 4 20 2 4 -20 1 -4 -20 -1 -4 20 1 4 -20 -1 4 20 1 4 -20 0 -4 20 0 -4 -20 -1 -4 -20 1 -4 20 1 4 20 -1 4 -20 4 -5 -20 4 -5 -20 4 -5 -20 4 5 -20 4 5 -20 3 -5 -20 3 -5 -20 3 5 -20 3 5 -20 -3 5 20 -2 -5 20 2 -5 -20 2 -5 -20 -2 5 20 2 5 -20 2 5 -20 -1 -5 20 1 -5 -20 1 5 -20 -1 5 20 1 5 -20 0 -5 -20 0 -5 20 -1 -5 -20 1 -5 20 -1 5 -20 1 5 20 3 -6 -20 3 -6 -20 -3 6 20 3 6 -20 3 6 -20 2 -6 -20 -2 -6 20 2 6 -20 -2 6 20 -1 -6 20 1 -6 -20 -1 6 20 1 6 -20 0 -6 20 0 -6 -20 0 6 -20 0 6 20 -2 -7 20 2 -7 -20 -2 7 20 2 7 -20 2 7 -20 1 -7 -20 -1 -7 20 1 7 -20 -1 7 20 0 -7 20 0 -7 -20 0 7 20 0 7 -20 3 0 -21 3 0 -21 2 0 -21 -2 0 21 -1 0 21 1 0 -21 1 0 -21 0 0 21 0 0 -21 1 0 21 -1 0 -21 3 -1 -21 3 -1 -21 -3 -1 21 3 1 -21 3 1 -21 -2 -1 21 2 -1 -21 -2 1 21 2 1 -21 2 1 -21 1 -1 -21 -1 -1 21 1 1 -21 -1 1 21 1 1 -21 0 -1 21 0 -1 -21 0 1 21 3 -2 -21 3 -2 -21 -3 2 21 3 2 -21 3 2 -21 2 -2 -21 2 -2 -21 -2 -2 21 -2 2 21 2 2 -21 -1 -2 21 1 -2 -21 1 2 -21 1 2 -21 -1 2 21 0 -2 -21 0 -2 21 0 2 21 0 2 -21 3 -3 -21 3 -3 -21 3 3 -21 -3 3 21 3 3 -21 -2 -3 21 2 -3 -21 2 -3 -21 2 3 -21 -1 -3 21 1 -3 -21 1 3 -21 -1 3 21 0 -3 -21 0 -3 21 0 3 -21 0 3 21 -2 -4 21 2 -4 -21 2 -4 -21 -2 4 21 2 4 -21 2 4 -21 -1 -4 21 1 -4 -21 -1 4 21 1 4 -21 0 -4 -21 0 -4 21 0 4 21 0 4 -21 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 H1 . . 121.8 ? C2 C1 C6 . . 116.30(12) ? C6 C1 H1 . . 121.8 ? F1 C2 C1 . . 117.80(13) ? F1 C2 C3 . . 117.96(12) ? C3 C2 C1 . . 124.24(12) ? C2 C3 H3 . . 120.6 ? C2 C3 C4 . . 118.76(12) ? C4 C3 H3 . . 120.6 ? C3 C4 H4 . . 120.4 ? C5 C4 C3 . . 119.23(12) ? C5 C4 H4 . . 120.4 ? C4 C5 C6 . . 120.50(12) ? C4 C5 C9 . . 131.01(11) ? C6 C5 C9 . . 108.49(10) ? C1 C6 C5 . . 120.97(11) ? C1 C6 C7 . . 131.10(11) ? C5 C6 C7 . . 107.93(10) ? C6 C7 C10 . . 123.20(11) ? C8 C7 C6 . . 110.16(10) ? C8 C7 C10 . . 126.63(11) ? C7 C8 C9 . . 109.85(10) ? C7 C8 C12 . . 128.96(12) ? C12 C8 C9 . . 121.19(11) ? C5 C9 C8 . . 103.57(9) ? C5 C9 H9A . . 111.0 ? C5 C9 H9B . . 111.0 ? C8 C9 H9A . . 111.0 ? C8 C9 H9B . . 111.0 ? H9A C9 H9B . . 109.0 ? C7 C10 H10A . . 109.1 ? C7 C10 H10B . . 109.1 ? H10A C10 H10B . . 107.8 ? C11 C10 C7 . . 112.47(10) ? C11 C10 H10A . . 109.1 ? C11 C10 H10B . . 109.1 ? N1 C11 C10 . . 179.06(14) ? C8 C12 H12A . . 109.5 ? C8 C12 H12B . . 109.5 ? C8 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C14 C13 H13 . . 121.9 ? C14 C13 C18 . . 116.15(12) ? C18 C13 H13 . . 121.9 ? F2 C14 C13 . . 117.48(13) ? F2 C14 C15 . . 118.12(12) ? C15 C14 C13 . . 124.40(12) ? C14 C15 H15 . . 120.7 ? C14 C15 C16 . . 118.66(12) ? C16 C15 H15 . . 120.7 ? C15 C16 H16 . . 120.5 ? C17 C16 C15 . . 119.08(12) ? C17 C16 H16 . . 120.5 ? C16 C17 C18 . . 120.72(11) ? C16 C17 C21 . . 130.98(11) ? C18 C17 C21 . . 108.30(10) ? C13 C18 C17 . . 120.99(11) ? C13 C18 C19 . . 130.62(11) ? C17 C18 C19 . . 108.40(10) ? C18 C19 C22 . . 123.15(10) ? C20 C19 C18 . . 109.75(10) ? C20 C19 C22 . . 127.09(10) ? C19 C20 C21 . . 110.04(10) ? C19 C20 C24 . . 128.72(11) ? C24 C20 C21 . . 121.24(10) ? C17 C21 C20 . . 103.51(9) ? C17 C21 H21A . . 111.1 ? C17 C21 H21B . . 111.1 ? C20 C21 H21A . . 111.1 ? C20 C21 H21B . . 111.1 ? H21A C21 H21B . . 109.0 ? C19 C22 H22A . . 109.1 ? C19 C22 H22B . . 109.1 ? H22A C22 H22B . . 107.8 ? C23 C22 C19 . . 112.65(10) ? C23 C22 H22A . . 109.1 ? C23 C22 H22B . . 109.1 ? N2 C23 C22 . . 179.90(19) ? C20 C24 H24A . . 109.5 ? C20 C24 H24B . . 109.5 ? C20 C24 H24C . . 109.5 ? H24A C24 H24B . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 C2 . 1.3660(15) ? N1 C11 . 1.1375(16) ? C1 H1 . 0.9500 ? C1 C2 . 1.3820(19) ? C1 C6 . 1.3880(17) ? C2 C3 . 1.373(2) ? C3 H3 . 0.9500 ? C3 C4 . 1.388(2) ? C4 H4 . 0.9500 ? C4 C5 . 1.3813(17) ? C5 C6 . 1.4044(16) ? C5 C9 . 1.4983(17) ? C6 C7 . 1.4643(16) ? C7 C8 . 1.3402(17) ? C7 C10 . 1.5032(16) ? C8 C9 . 1.5051(16) ? C8 C12 . 1.4947(17) ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C10 C11 . 1.4654(17) ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? F2 C14 . 1.3648(15) ? N2 C23 . 1.1370(17) ? C13 H13 . 0.9500 ? C13 C14 . 1.3810(18) ? C13 C18 . 1.3898(16) ? C14 C15 . 1.376(2) ? C15 H15 . 0.9500 ? C15 C16 . 1.3903(19) ? C16 H16 . 0.9500 ? C16 C17 . 1.3804(17) ? C17 C18 . 1.4035(16) ? C17 C21 . 1.5006(16) ? C18 C19 . 1.4639(15) ? C19 C20 . 1.3434(16) ? C19 C22 . 1.5051(15) ? C20 C21 . 1.5065(16) ? C20 C24 . 1.4916(17) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C22 H22A . 0.9900 ? C22 H22B . 0.9900 ? C22 C23 . 1.4646(17) ? C24 H24A . 0.9800 ? C24 H24B . 0.9800 ? C24 H24C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C10 H10B N2 2_545 0.99 2.65 3.3978(18) 132.1 yes C22 H22A N1 2_655 0.99 2.61 3.4010(16) 137.3 yes C24 H24C F2 2_645 0.98 2.76 3.227(2) 109.5 yes C24 H24B F2 2_645 0.98 2.83 3.227(2) 105.1 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag F1 C2 C3 C4 . . . . -179.90(11) ? C1 C2 C3 C4 . . . . -0.3(2) ? C1 C6 C7 C8 . . . . 179.91(12) ? C1 C6 C7 C10 . . . . -1.04(19) ? C2 C1 C6 C5 . . . . -0.34(17) ? C2 C1 C6 C7 . . . . 179.76(11) ? C2 C3 C4 C5 . . . . 0.22(19) ? C3 C4 C5 C6 . . . . -0.25(18) ? C3 C4 C5 C9 . . . . -179.87(12) ? C4 C5 C6 C1 . . . . 0.32(17) ? C4 C5 C6 C7 . . . . -179.76(10) ? C4 C5 C9 C8 . . . . 179.75(12) ? C5 C6 C7 C8 . . . . 0.00(13) ? C5 C6 C7 C10 . . . . 179.05(10) ? C6 C1 C2 F1 . . . . 179.96(11) ? C6 C1 C2 C3 . . . . 0.3(2) ? C6 C5 C9 C8 . . . . 0.10(12) ? C6 C7 C8 C9 . . . . 0.06(13) ? C6 C7 C8 C12 . . . . 179.99(12) ? C6 C7 C10 C11 . . . . 64.09(16) ? C7 C8 C9 C5 . . . . -0.10(13) ? C8 C7 C10 C11 . . . . -117.02(13) ? C9 C5 C6 C1 . . . . -179.98(10) ? C9 C5 C6 C7 . . . . -0.06(12) ? C10 C7 C8 C9 . . . . -178.95(11) ? C10 C7 C8 C12 . . . . 1.0(2) ? C12 C8 C9 C5 . . . . 179.97(11) ? F2 C14 C15 C16 . . . . -179.92(12) ? C13 C14 C15 C16 . . . . 0.0(2) ? C13 C18 C19 C20 . . . . -179.93(12) ? C13 C18 C19 C22 . . . . 1.14(18) ? C14 C13 C18 C17 . . . . 0.04(17) ? C14 C13 C18 C19 . . . . 179.88(11) ? C14 C15 C16 C17 . . . . 0.2(2) ? C15 C16 C17 C18 . . . . -0.24(18) ? C15 C16 C17 C21 . . . . 179.58(12) ? C16 C17 C18 C13 . . . . 0.13(17) ? C16 C17 C18 C19 . . . . -179.75(10) ? C16 C17 C21 C20 . . . . 179.62(12) ? C17 C18 C19 C20 . . . . -0.07(13) ? C17 C18 C19 C22 . . . . -179.00(10) ? C18 C13 C14 F2 . . . . 179.80(11) ? C18 C13 C14 C15 . . . . -0.1(2) ? C18 C17 C21 C20 . . . . -0.54(12) ? C18 C19 C20 C21 . . . . -0.29(13) ? C18 C19 C20 C24 . . . . 179.74(11) ? C18 C19 C22 C23 . . . . -64.72(14) ? C19 C20 C21 C17 . . . . 0.51(12) ? C20 C19 C22 C23 . . . . 116.54(13) ? C21 C17 C18 C13 . . . . -179.73(10) ? C21 C17 C18 C19 . . . . 0.40(12) ? C22 C19 C20 C21 . . . . 178.59(11) ? C22 C19 C20 C24 . . . . -1.4(2) ? C24 C20 C21 C17 . . . . -179.52(10) ?