#------------------------------------------------------------------------------ #$Date: 2024-11-27 01:34:49 +0200 (Wed, 27 Nov 2024) $ #$Revision: 296127 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249640.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7249640 loop_ _publ_author_name 'Kenguva, Gowtham' 'Rekha Rout, Smruti' 'Shaikh, Tabrez R.' 'Baidya, Debjani' 'Shelke, Nikita' 'Sanphui, Palash' 'Dandela, Rambabu' _publ_section_title ; Exploring Novel Cocrystals of Milrinone: A Cardioprotective Drug Combined with Nutraceuticals and NSAID ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00990H _journal_year 2024 _chemical_formula_moiety 'C13 H9 F3 N2 O2, C12 H9 N3 O' _chemical_formula_sum 'C25 H18 F3 N5 O3' _chemical_formula_weight 493.44 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2023-11-27 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-09-21 deposited with the CCDC. 2024-11-25 downloaded from the CCDC. ; _cell_angle_alpha 85.550(2) _cell_angle_beta 65.237(2) _cell_angle_gamma 64.849(2) _cell_formula_units_Z 2 _cell_length_a 10.7282(9) _cell_length_b 10.7734(9) _cell_length_c 11.9845(11) _cell_measurement_reflns_used 2954 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 0.982 _cell_measurement_theta_min 0.977 _cell_volume 1130.01(17) _computing_cell_refinement 'Bruker SHELXL' _computing_data_collection 'Bruker APEX4' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 298.15 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 quest photon detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_unetI/netI 0.0342 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 26687 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 24.942 _diffrn_reflns_theta_max 24.942 _diffrn_reflns_theta_min 2.280 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_correction_T_min 0.977 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.450 _exptl_crystal_description block _exptl_crystal_F_000 508 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.346 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 331 _refine_ls_number_reflns 3938 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0502 _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^)+(0.0533P)^2^+0.6529P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1207 _refine_ls_wR_factor_ref 0.1397 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2954 _reflns_number_total 3938 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00990h2.cif _cod_data_source_block mr_nif _cod_database_code 7249640 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. 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, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: N2(H2A), C5(H5), C9(H9), C11(H11), C15(H15), C17(H17), C19(H19), C23(H23), C4(H4), C7(H7), C14(H14), C20(H20), C22(H22) 2.b Idealised Me refined as rotating group: C24(H24A,H24B,H24C) 2.c Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; TITL mr_nif_a.res in P-1 mr_nif.res created by SHELXL-2018/3 at 10:48:02 on 27-Nov-2023 REM Old TITL MR_NIF in P-1 REM SHELXT solution in P-1: R1 0.193, Rweak 0.008, Alpha 0.049 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C26 F3 N5 O2 CELL 0.71073 10.7282 10.7734 11.9845 85.55 65.237 64.849 ZERR 2 0.0009 0.0009 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H F N O UNIT 50 36 6 10 6 EQIV $1 1-X,2-Y,2-Z L.S. 10 PLAN 5 TEMP 25 CONF HTAB O2 N4 HTAB N2 O3 HTAB N1 O1_$1 list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.053300 0.652900 FVAR 1.43922 F1 3 0.166393 0.095795 -0.095391 11.00000 0.10310 0.13020 = 0.07579 -0.03572 -0.02788 -0.04196 F2 3 0.075783 0.042088 0.080963 11.00000 0.30331 0.12619 = 0.12499 0.05524 -0.14655 -0.14814 F3 3 -0.062869 0.210213 0.020980 11.00000 0.07766 0.11862 = 0.16765 -0.04247 -0.06176 -0.02832 O2 5 0.225851 0.306294 0.658284 11.00000 0.08068 0.07166 = 0.06836 0.01612 -0.04786 -0.05034 AFIX 147 H2 2 0.277644 0.345036 0.657039 11.00000 -1.50000 AFIX 0 O3 5 0.226919 0.412350 0.491229 11.00000 0.06846 0.06461 = 0.05641 0.00674 -0.02925 -0.04462 N2 4 0.116957 0.339079 0.358505 11.00000 0.05785 0.05635 = 0.05077 0.00924 -0.02831 -0.03520 AFIX 43 H2A 2 0.159205 0.386060 0.370101 11.00000 -1.20000 AFIX 0 N5 4 -0.034741 0.225165 0.455653 11.00000 0.05259 0.06427 = 0.05636 0.00487 -0.02675 -0.03527 C2 1 0.122290 0.335955 0.240078 11.00000 0.04014 0.04925 = 0.04710 0.00358 -0.01963 -0.01714 C3 1 0.072494 0.148783 0.021652 11.00000 0.07275 0.07317 = 0.05267 -0.00044 -0.03309 -0.02768 C5 1 0.165733 0.428911 0.164868 11.00000 0.05634 0.05673 = 0.05914 0.00835 -0.02461 -0.02728 AFIX 43 H5 2 0.184822 0.491981 0.196035 11.00000 -1.20000 AFIX 0 C9 1 -0.068874 0.158533 0.657341 11.00000 0.07300 0.07597 = 0.05069 0.00955 -0.02026 -0.05082 AFIX 43 H9 2 -0.112755 0.116445 0.723206 11.00000 -1.20000 AFIX 0 C11 1 0.180820 0.428804 0.045162 11.00000 0.07742 0.07286 = 0.05960 0.02089 -0.02967 -0.03993 AFIX 43 H11 2 0.209653 0.491987 -0.003449 11.00000 -1.20000 AFIX 0 C13 1 0.185580 0.338991 0.566727 11.00000 0.04880 0.04532 = 0.04832 -0.00397 -0.02240 -0.02125 C15 1 0.024611 0.213616 0.660660 11.00000 0.06326 0.06269 = 0.04661 0.00428 -0.02566 -0.03445 AFIX 43 H15 2 0.045395 0.208029 0.729313 11.00000 -1.20000 AFIX 0 C17 1 0.094441 0.242193 0.191342 11.00000 0.05454 0.05201 = 0.04850 0.00587 -0.02606 -0.02232 AFIX 43 H17 2 0.065978 0.178518 0.239392 11.00000 -1.20000 AFIX 0 C18 1 0.055230 0.279310 0.459036 11.00000 0.04027 0.04193 = 0.04792 0.00089 -0.02053 -0.01779 C19 1 -0.094891 0.167923 0.553748 11.00000 0.05910 0.07119 = 0.06203 0.00361 -0.02521 -0.04240 AFIX 43 H19 2 -0.158931 0.131840 0.551878 11.00000 -1.20000 AFIX 0 C21 1 0.109584 0.244806 0.070622 11.00000 0.05324 0.06053 = 0.05092 0.00402 -0.02604 -0.02189 C23 1 0.153781 0.336286 -0.003796 11.00000 0.07507 0.08367 = 0.04832 0.01309 -0.02884 -0.03493 AFIX 43 H23 2 0.165102 0.335648 -0.085076 11.00000 -1.20000 AFIX 0 C25 1 0.087565 0.277091 0.562422 11.00000 0.04530 0.04353 = 0.04486 -0.00057 -0.02014 -0.02187 O1 5 0.555950 1.061066 0.854158 11.00000 0.09152 0.05500 = 0.04758 0.01355 -0.03969 -0.04997 N1 4 0.486810 0.884388 0.908034 11.00000 0.05997 0.04294 = 0.03439 0.00860 -0.02598 -0.03031 H1 2 0.472386 0.905877 0.986791 11.00000 0.05892 N3 4 0.619105 1.095306 0.539793 11.00000 0.08814 0.07005 = 0.05696 0.02820 -0.04231 -0.05478 N4 4 0.366980 0.444992 0.675096 11.00000 0.05935 0.04943 = 0.05264 0.00501 -0.03019 -0.03145 C1 1 0.432619 0.647184 0.737998 11.00000 0.04278 0.04035 = 0.03233 0.00499 -0.01656 -0.02341 C4 1 0.502179 0.844131 0.682832 11.00000 0.04585 0.03919 = 0.03479 0.00453 -0.02176 -0.02003 AFIX 43 H4 2 0.504714 0.832148 0.605767 11.00000 -1.20000 AFIX 0 C6 1 0.580379 1.029668 0.613968 11.00000 0.05511 0.04357 = 0.04222 0.00799 -0.02799 -0.02816 C7 1 0.463778 0.414066 0.726684 11.00000 0.06396 0.04019 = 0.06305 0.00977 -0.03822 -0.02670 AFIX 43 H7 2 0.508402 0.323624 0.742439 11.00000 -1.20000 AFIX 0 C8 1 0.464439 0.757028 0.771221 11.00000 0.04422 0.03609 = 0.03788 0.00653 -0.02219 -0.02160 C10 1 0.455094 0.781695 0.886316 11.00000 0.04623 0.03614 = 0.03933 0.00735 -0.02316 -0.02182 C12 1 0.535306 0.945933 0.706338 11.00000 0.04566 0.03619 = 0.03513 0.00679 -0.02081 -0.02094 C14 1 0.336478 0.677496 0.680435 11.00000 0.05543 0.04362 = 0.05161 0.01097 -0.03292 -0.02554 AFIX 43 H14 2 0.291855 0.766625 0.662009 11.00000 -1.20000 AFIX 0 C16 1 0.528916 0.970008 0.824835 11.00000 0.05320 0.03923 = 0.03886 0.00739 -0.02562 -0.02437 C20 1 0.500238 0.510470 0.757501 11.00000 0.05649 0.04297 = 0.05552 0.00937 -0.03697 -0.02542 AFIX 43 H20 2 0.570173 0.484097 0.791398 11.00000 -1.20000 AFIX 0 C22 1 0.307500 0.574698 0.650718 11.00000 0.05754 0.05570 = 0.05654 0.00816 -0.03646 -0.02925 AFIX 43 H22 2 0.243205 0.596814 0.611674 11.00000 -1.20000 AFIX 0 C24 1 0.405716 0.708682 0.995548 11.00000 0.07678 0.05438 = 0.04200 0.01525 -0.03130 -0.04111 AFIX 137 H24A 2 0.493766 0.636048 1.000711 11.00000 -1.50000 H24B 2 0.344154 0.670010 0.986586 11.00000 -1.50000 H24C 2 0.347461 0.773017 1.069625 11.00000 -1.50000 AFIX 0 HKLF 4 REM mr_nif_a.res in P-1 REM wR2 = 0.1397, GooF = S = 1.071, Restrained GooF = 1.071 for all data REM R1 = 0.0502 for 2954 Fo > 4sig(Fo) and 0.0718 for all 3938 data REM 331 parameters refined using 0 restraints END WGHT 0.0533 0.6529 REM Highest difference peak 0.346, deepest hole -0.313, 1-sigma level 0.042 Q1 1 -0.0377 0.1266 0.1035 11.00000 0.05 0.35 Q2 1 0.1653 0.0340 -0.0182 11.00000 0.05 0.30 Q3 1 0.0530 0.1812 -0.0803 11.00000 0.05 0.24 Q4 1 0.1071 0.0148 0.0739 11.00000 0.05 0.21 Q5 1 0.3254 0.3810 0.6617 11.00000 0.05 0.20 ; _shelx_res_checksum 45950 _shelx_hkl_file ; -1 0 0 182.48 8.30 -1 0 0 192.68 10.60 1 0 0 180.88 8.70 -4 0 0 58.59 4.60 -4 0 0 68.79 4.70 -4 0 0 63.99 7.20 -4 0 0 53.99 4.70 4 0 0 60.89 5.10 -5 0 0 681.63 32.20 -5 0 0 694.53 32.40 -5 0 0 721.13 31.70 -5 0 0 690.73 35.00 5 0 0 752.52 33.00 -6 0 0 51.09 5.60 -6 0 0 55.79 5.10 -6 0 0 33.00 5.30 6 0 0 38.70 6.90 -7 0 0 319.67 19.70 -7 0 0 330.17 18.30 -7 0 0 289.27 16.50 -7 0 0 329.97 18.90 7 0 0 303.87 18.00 7 0 0 378.66 20.50 -8 0 0 47.90 7.00 -8 0 0 67.89 5.70 -8 0 0 61.99 9.00 -8 0 0 60.89 13.60 8 0 0 50.89 7.20 8 0 0 66.49 7.60 -9 0 0 8.30 6.10 -9 0 0 11.30 8.70 -9 0 0 13.40 4.90 9 0 0 22.10 4.50 9 0 0 13.20 3.80 -10 0 0 -2.40 8.90 -10 0 0 -0.40 6.30 -10 0 0 -5.90 4.20 -9 1 0 -1.50 3.40 -9 1 0 -2.00 6.70 -9 1 0 8.40 5.50 8 -1 0 14.90 2.60 8 -1 0 16.30 2.60 -8 1 0 19.70 8.90 -8 1 0 22.60 5.30 -8 1 0 22.60 6.30 7 -1 0 136.19 9.40 7 -1 0 122.99 8.90 -7 1 0 136.09 10.20 -7 1 0 129.29 11.80 6 -1 0 41.50 6.30 6 -1 0 42.50 4.90 -6 1 0 39.10 3.40 -6 1 0 36.20 3.00 -6 1 0 53.99 7.00 -6 1 0 37.90 5.20 5 -1 0 938.61 48.90 5 -1 0 1051.29 45.20 -5 1 0 1029.20 42.90 -5 1 0 1010.60 44.40 -5 1 0 1016.50 45.30 -5 1 0 1037.90 44.50 4 -1 0 6.50 3.80 4 -1 0 4.20 2.30 -4 1 0 3.70 1.70 -4 1 0 4.30 1.60 3 -1 0 461.95 21.30 3 -1 0 458.45 23.60 -3 1 0 458.35 20.00 -3 1 0 454.85 19.70 -3 1 0 459.65 19.60 -2 -1 0 1093.79 46.60 -2 -1 0 989.80 51.09 -2 -1 0 1148.09 46.40 -2 -1 0 1029.40 46.20 2 1 0 1096.09 46.40 2 1 0 1173.78 50.39 2 1 0 1124.79 46.20 2 1 0 1087.89 46.10 -3 -1 0 936.71 40.70 -3 -1 0 942.51 41.00 -3 -1 0 943.41 40.80 3 1 0 936.21 40.00 3 1 0 920.21 40.10 3 1 0 967.10 40.90 3 1 0 940.71 45.50 -4 -1 0 293.77 15.70 -4 -1 0 311.17 15.80 -4 -1 0 288.07 22.50 -4 -1 0 338.37 16.30 4 1 0 310.87 20.50 4 1 0 312.07 15.90 4 1 0 321.37 13.80 4 1 0 315.17 13.80 -5 -1 0 157.68 10.20 -5 -1 0 171.48 10.30 -5 -1 0 135.49 15.20 -5 -1 0 167.38 10.50 5 1 0 154.58 10.20 5 1 0 173.88 14.30 -6 -1 0 197.88 13.30 -6 -1 0 217.48 13.20 -6 -1 0 205.28 17.60 -6 -1 0 201.98 12.90 6 1 0 204.98 12.90 6 1 0 233.98 16.90 -7 -1 0 206.88 14.20 -7 -1 0 184.58 16.80 -7 -1 0 186.78 13.00 -7 -1 0 180.48 12.80 7 1 0 194.48 13.00 -8 -1 0 -4.60 2.70 -8 -1 0 -5.50 4.80 -8 -1 0 -1.10 2.80 -8 -1 0 7.20 5.00 -8 -1 0 4.40 3.90 8 1 0 1.50 3.00 -9 -1 0 5.60 4.10 -9 -1 0 4.10 3.60 -9 -1 0 6.90 7.50 -9 -1 0 5.40 5.10 9 1 0 9.30 4.50 9 1 0 13.60 4.80 -10 -1 0 -0.10 6.50 -10 -1 0 -5.70 1.90 -10 -1 0 -5.20 3.30 -10 -1 0 -10.00 7.20 10 1 0 -2.60 4.00 10 1 0 -0.30 4.00 -9 2 0 32.70 6.20 -9 2 0 42.70 9.40 -9 2 0 22.40 11.30 -8 2 0 41.40 11.50 -8 2 0 41.50 8.60 -8 2 0 33.90 5.90 -7 2 0 94.29 10.40 -7 2 0 102.09 8.90 6 -2 0 153.48 8.80 6 -2 0 161.88 10.70 -6 2 0 147.79 11.70 -6 2 0 161.18 10.50 5 -2 0 131.09 11.90 5 -2 0 142.09 9.10 -5 2 0 146.99 10.10 -5 2 0 148.79 9.20 4 -2 0 563.54 26.00 4 -2 0 593.14 28.80 -4 2 0 545.45 24.80 -4 2 0 536.65 26.00 -4 2 0 551.44 24.70 -4 2 0 537.65 23.90 3 -2 0 1873.01 78.69 3 -2 0 1805.52 79.69 -3 2 0 1879.01 77.89 -3 2 0 1809.82 77.89 -3 2 0 1836.62 76.79 -3 2 0 1909.11 77.69 0 -2 0 4031.10 166.08 -1 -2 0 1881.01 85.59 -1 -2 0 1939.01 83.19 -1 -2 0 1997.80 83.49 1 2 0 2123.29 85.79 -2 -2 0 413.56 20.30 -2 -2 0 389.16 19.70 -2 -2 0 451.15 24.40 -2 -2 0 379.16 19.40 2 2 0 413.06 19.60 2 2 0 418.56 22.60 2 2 0 385.96 19.60 -3 -2 0 39.50 9.00 -3 -2 0 41.30 4.40 -3 -2 0 39.80 5.30 3 2 0 41.00 7.00 3 2 0 36.10 4.20 3 2 0 40.50 4.00 3 2 0 35.10 4.10 -4 -2 0 305.67 16.00 -4 -2 0 235.58 22.70 -4 -2 0 308.27 16.80 -4 -2 0 322.17 16.30 4 2 0 285.67 15.80 4 2 0 300.37 20.40 4 2 0 292.07 15.40 4 2 0 292.87 15.50 -5 -2 0 863.41 40.40 -5 -2 0 726.43 50.09 -5 -2 0 840.12 40.70 -5 -2 0 857.61 41.20 5 2 0 905.51 39.20 5 2 0 961.30 46.70 5 2 0 909.41 39.10 5 2 0 933.61 40.70 -6 -2 0 1256.07 58.19 -6 -2 0 1243.48 57.39 -6 -2 0 1146.79 68.59 -6 -2 0 1318.67 58.69 6 2 0 1398.56 63.99 6 2 0 1288.07 53.49 6 2 0 1278.57 57.39 6 2 0 1290.37 53.49 -7 -2 0 -0.30 2.60 -7 -2 0 14.90 8.40 -7 -2 0 2.90 4.90 -7 -2 0 0.40 2.70 -7 -2 0 -0.80 2.70 7 2 0 0.10 2.60 7 2 0 7.10 3.70 -8 -2 0 17.20 8.40 -8 -2 0 3.00 4.20 -8 -2 0 6.80 4.20 -8 -2 0 3.20 5.60 -8 -2 0 8.80 4.10 8 2 0 13.70 5.10 8 2 0 11.00 4.30 -9 -2 0 7.90 6.80 -9 -2 0 4.90 4.60 -9 -2 0 -4.30 3.00 -9 -2 0 1.20 4.50 9 2 0 2.90 4.20 9 2 0 -2.60 3.40 -10 -2 0 9.60 5.30 -10 -2 0 18.80 7.80 -10 -2 0 1.40 8.60 -10 -2 0 13.50 7.30 10 2 0 10.10 5.50 -11 -2 0 6.50 8.90 -11 -2 0 7.10 5.70 11 2 0 -7.40 6.10 -8 3 0 20.40 5.10 -8 3 0 21.70 6.60 -8 3 0 11.50 9.90 -7 3 0 663.23 40.60 -7 3 0 634.64 31.20 -7 3 0 560.54 32.10 -6 3 0 112.59 9.60 -6 3 0 141.59 11.30 5 -3 0 118.49 10.80 5 -3 0 115.19 8.20 -5 3 0 122.39 8.60 -5 3 0 128.19 10.10 4 -3 0 1989.80 87.29 4 -3 0 2059.09 85.39 -4 3 0 2017.20 86.09 -4 3 0 1968.50 83.39 -4 3 0 1931.91 84.19 -4 3 0 1992.60 83.19 3 -3 0 425.06 22.50 -3 3 0 461.15 21.50 -3 3 0 412.66 22.20 -3 3 0 456.35 22.40 -3 3 0 435.66 21.00 2 -3 0 679.33 35.50 2 -3 0 784.22 35.40 -2 3 0 761.02 34.10 -2 3 0 730.23 35.30 -2 3 0 734.83 34.70 -2 3 0 743.03 33.10 1 -3 0 116.09 7.90 1 -3 0 144.79 8.90 1 -3 0 138.09 10.40 1 -3 0 148.29 10.50 -1 3 0 140.09 8.40 -1 3 0 128.19 10.30 -1 3 0 133.49 9.20 -1 3 0 115.19 11.20 -1 3 0 138.09 9.80 0 -3 0 540.65 25.80 0 -3 0 535.05 26.70 0 -3 0 553.14 28.30 0 -3 0 549.05 27.80 0 -3 0 544.35 26.90 0 3 0 555.44 27.00 0 3 0 542.25 25.00 0 3 0 543.85 28.20 0 3 0 567.54 26.90 0 3 0 567.54 26.00 -1 -3 0 2603.14 110.09 -1 -3 0 2596.24 110.79 -1 -3 0 2660.53 111.59 -1 -3 0 2512.85 109.59 -1 -3 0 2610.84 113.49 1 3 0 2747.93 108.99 1 3 0 2517.95 109.69 1 3 0 2419.96 110.19 1 3 0 2629.74 110.59 1 3 0 2827.12 113.39 -2 -3 0 5664.03 239.38 -3 -3 0 364.66 20.00 -3 -3 0 316.77 18.30 -3 -3 0 344.57 23.90 -3 -3 0 314.07 17.40 -3 -3 0 301.67 17.50 3 3 0 310.97 17.40 3 3 0 290.07 20.20 3 3 0 308.17 17.10 -4 -3 0 93.69 9.80 -4 -3 0 100.39 8.80 -4 -3 0 91.59 7.80 -4 -3 0 58.59 12.10 -4 -3 0 84.09 7.80 4 3 0 81.79 11.80 4 3 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347.77 26.70 4 6 0 363.96 22.40 -5 -6 0 8.90 5.00 -5 -6 0 11.90 5.00 -5 -6 0 9.20 6.90 -5 -6 0 15.70 6.10 -5 -6 0 19.50 6.20 5 6 0 18.30 5.90 5 6 0 4.90 5.80 5 6 0 12.70 4.50 -6 -6 0 98.89 20.70 -6 -6 0 139.69 13.70 -6 -6 0 152.48 15.40 -6 -6 0 139.89 16.00 -6 -6 0 136.09 13.80 6 6 0 140.09 16.50 6 6 0 157.88 13.90 6 6 0 135.59 12.60 6 6 0 132.89 12.90 -7 -6 0 2.40 6.20 -7 -6 0 17.90 11.80 -7 -6 0 2.20 4.10 -7 -6 0 2.70 4.00 -7 -6 0 -5.10 2.90 7 6 0 2.40 4.10 7 6 0 6.90 4.90 7 6 0 -5.30 2.80 7 6 0 6.70 4.50 -8 -6 0 65.79 15.50 -8 -6 0 45.90 18.50 -8 -6 0 69.59 11.60 -8 -6 0 75.69 12.60 -8 -6 0 69.59 13.40 8 6 0 59.89 14.30 8 6 0 74.29 11.30 8 6 0 63.29 10.00 8 6 0 63.49 10.90 -9 -6 0 40.40 10.60 -9 -6 0 43.80 14.80 -9 -6 0 26.40 14.00 -9 -6 0 38.90 9.70 -9 -6 0 23.50 9.40 9 6 0 35.00 7.40 9 6 0 33.60 8.00 9 6 0 33.80 10.80 -10 -6 0 57.69 11.90 -10 -6 0 53.29 20.70 -10 -6 0 42.90 14.00 -10 -6 0 36.60 12.10 10 6 0 42.10 8.60 10 6 0 60.89 14.40 10 6 0 61.99 9.80 -11 -6 0 270.77 32.20 -11 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29.70 1 -1 13 108.69 23.10 1 -1 13 136.99 25.10 1 -1 13 110.19 31.60 -2 1 -13 86.19 14.30 -2 1 -13 86.19 17.80 2 -1 13 89.59 17.90 2 -1 13 83.59 19.40 2 -1 13 63.69 24.10 2 -1 13 75.89 21.80 -3 1 -13 43.80 11.90 -3 1 -13 41.50 12.40 3 -1 13 23.70 12.30 3 -1 13 56.29 30.10 3 -1 13 67.29 17.40 -4 1 -13 7.30 8.40 -4 1 -13 5.70 8.00 4 -1 13 7.60 12.20 4 -1 13 10.00 7.30 4 -1 13 9.10 18.30 -5 1 -13 7.50 7.80 -5 1 -13 5.30 8.20 5 -1 13 29.60 24.60 5 -1 13 12.50 8.90 5 -1 13 27.40 13.70 -6 1 -13 200.18 28.90 -6 1 -13 148.49 21.40 6 -1 13 165.08 33.30 6 -1 13 176.28 47.20 6 -1 13 266.17 29.40 -7 1 -13 8.20 9.10 -7 1 -13 -8.60 6.10 7 -1 13 23.30 19.30 7 -1 13 -7.40 14.10 7 -1 13 1.10 10.70 -8 1 -13 10.70 6.90 -8 1 -13 -3.80 8.40 8 -1 13 -0.70 11.00 8 -1 13 -17.50 21.70 -1 0 -13 11.00 8.90 -1 0 -13 27.30 9.40 -1 0 -13 6.30 5.60 1 0 13 -17.70 10.20 1 0 13 17.40 11.10 1 0 13 -4.20 17.30 1 0 13 11.20 9.90 -2 0 -13 7.10 7.00 -2 0 -13 -13.00 8.20 -2 0 -13 8.00 9.40 2 0 13 -13.30 8.70 2 0 13 -16.40 10.50 2 0 13 29.00 11.80 2 0 13 4.70 17.60 -3 0 -13 2.50 6.60 -3 0 -13 15.50 9.10 3 0 13 4.90 9.50 3 0 13 20.70 27.80 3 0 13 8.60 15.40 3 0 13 3.00 10.50 -4 0 -13 71.29 16.70 -4 0 -13 84.69 15.00 4 0 13 106.59 20.90 4 0 13 88.69 23.20 -5 0 -13 19.50 11.30 -5 0 -13 14.30 9.00 5 0 13 -6.30 21.50 5 0 13 19.20 11.30 5 0 13 5.00 13.40 -6 0 -13 2.30 7.00 -6 0 -13 -1.20 6.20 6 0 13 12.50 10.20 6 0 13 4.00 14.80 -7 0 -13 -0.80 8.80 -7 0 -13 12.70 8.60 7 0 13 -11.60 7.80 7 0 13 14.20 18.90 7 0 13 23.60 16.80 -8 0 -13 8.30 8.80 -8 0 -13 30.50 10.10 8 0 13 38.00 14.50 8 0 13 6.70 19.00 8 0 13 21.00 27.90 -1 -1 -13 -10.10 5.50 -1 -1 -13 -11.70 9.10 -1 -1 -13 -8.60 4.60 1 1 13 22.70 10.20 1 1 13 7.60 18.00 1 1 13 5.00 16.40 1 1 13 4.10 9.30 -2 -1 -13 -5.60 5.10 -2 -1 -13 43.10 15.00 -2 -1 -13 0.10 5.80 2 1 13 -20.80 16.70 2 1 13 -17.10 6.80 2 1 13 1.80 10.90 2 1 13 -22.80 8.10 3 1 13 15.50 13.60 3 1 13 9.80 9.70 -4 -1 -13 63.29 12.60 -4 -1 -13 29.90 9.30 4 1 13 42.70 18.80 4 1 13 8.20 20.00 4 1 13 6.50 8.00 4 1 13 34.00 12.60 -5 -1 -13 137.69 22.00 -5 -1 -13 153.88 19.90 5 1 13 72.29 31.10 5 1 13 109.89 22.60 5 1 13 114.39 29.00 -6 -1 -13 7.70 7.70 -6 -1 -13 7.10 5.60 6 1 13 10.20 9.80 6 1 13 38.40 21.20 6 1 13 -34.30 15.30 -7 -1 -13 49.50 12.30 -7 -1 -13 76.99 16.50 7 1 13 47.90 24.50 7 1 13 87.99 18.80 7 1 13 82.09 33.40 -8 -1 -13 30.40 11.90 -8 -1 -13 31.70 11.10 8 1 13 -2.40 15.90 8 1 13 6.90 13.00 8 1 13 18.70 13.10 -9 -1 -13 30.70 11.40 -9 -1 -13 33.80 12.90 9 1 13 36.90 26.40 9 1 13 21.30 14.80 -2 -2 -13 1.80 10.00 -2 -2 -13 14.90 8.20 2 2 13 18.60 10.80 2 2 13 22.30 22.50 2 2 13 44.90 19.40 2 2 13 31.40 13.00 -3 -2 -13 10.20 6.80 -3 -2 -13 28.50 10.80 -3 -2 -13 23.10 12.30 3 2 13 -11.80 17.50 3 2 13 -8.30 9.20 3 2 13 24.70 14.40 3 2 13 25.10 11.70 -4 -2 -13 3.10 7.70 -4 -2 -13 2.50 6.20 4 2 13 18.30 10.00 4 2 13 -6.90 12.90 4 2 13 5.10 10.50 4 2 13 21.30 11.90 -5 -2 -13 32.30 10.20 -5 -2 -13 47.90 10.70 5 2 13 36.60 14.10 5 2 13 41.00 21.30 5 2 13 31.10 15.10 5 2 13 29.50 25.50 -6 -2 -13 75.79 15.80 -6 -2 -13 57.69 12.90 6 2 13 41.20 11.70 6 2 13 120.59 30.10 -7 -2 -13 36.70 11.00 -7 -2 -13 46.30 12.10 7 2 13 16.20 10.50 7 2 13 -2.50 17.80 7 2 13 11.70 17.50 -8 -2 -13 -4.30 5.60 -8 -2 -13 2.80 4.90 8 2 13 -28.80 14.70 8 2 13 1.00 8.50 -9 -2 -13 29.00 10.70 -9 -2 -13 36.60 11.90 9 2 13 7.60 16.00 9 2 13 22.90 15.00 -2 -3 -13 19.90 8.30 -2 -3 -13 8.00 10.60 2 3 13 -6.10 10.50 2 3 13 30.70 19.90 2 3 13 38.60 12.60 2 3 13 -17.80 14.60 -3 -3 -13 54.59 12.50 -3 -3 -13 47.80 9.40 -3 -3 -13 66.59 15.10 3 3 13 52.09 15.40 3 3 13 82.59 18.80 3 3 13 61.29 22.30 3 3 13 14.70 21.40 -4 -3 -13 385.36 29.80 -4 -3 -13 331.17 24.60 -4 -3 -13 379.86 32.80 4 3 13 252.77 44.50 4 3 13 304.77 54.99 4 3 13 327.67 32.20 4 3 13 341.67 33.70 -5 -3 -13 17.10 7.70 -5 -3 -13 32.50 10.90 5 3 13 27.70 12.20 5 3 13 20.30 19.30 5 3 13 -1.80 19.30 5 3 13 4.10 9.80 -6 -3 -13 18.40 7.40 -6 -3 -13 27.90 9.80 6 3 13 26.30 15.70 6 3 13 27.20 19.10 6 3 13 16.50 12.70 -7 -3 -13 39.50 11.70 -7 -3 -13 46.10 12.00 7 3 13 26.00 17.60 7 3 13 38.90 27.30 7 3 13 28.20 12.50 -8 -3 -13 72.29 15.00 -8 -3 -13 56.09 13.80 8 3 13 30.00 22.00 8 3 13 68.59 19.70 -9 -3 -13 3.80 6.80 -9 -3 -13 -1.00 5.30 9 3 13 55.19 28.30 9 3 13 -10.30 9.00 -3 -4 -13 41.70 10.80 -3 -4 -13 48.70 13.70 3 4 13 27.40 19.20 3 4 13 28.10 13.60 3 4 13 47.90 14.60 3 4 13 30.30 20.70 -4 -4 -13 2.70 10.40 -4 -4 -13 -6.70 6.30 -4 -4 -13 1.00 6.70 4 4 13 8.60 14.90 4 4 13 1.50 10.10 4 4 13 23.60 12.70 4 4 13 1.80 18.10 -5 -4 -13 -13.40 4.50 -5 -4 -13 -12.60 5.10 5 4 13 6.10 6.40 5 4 13 13.70 17.50 5 4 13 -2.20 9.10 5 4 13 -4.40 21.90 6 4 13 19.50 17.30 6 4 13 -0.60 8.40 6 4 13 21.70 15.70 -7 -4 -13 12.80 7.10 -7 -4 -13 12.20 7.80 7 4 13 -12.90 21.10 7 4 13 20.40 11.10 7 4 13 52.79 22.00 -8 -4 -13 7.70 7.90 -8 -4 -13 11.00 9.10 8 4 13 28.10 11.00 8 4 13 28.90 19.30 -9 -4 -13 87.29 15.90 -9 -4 -13 51.29 13.30 9 4 13 62.89 17.70 9 4 13 132.69 37.10 -4 -5 -13 -9.20 10.10 -4 -5 -13 -11.80 5.30 -4 -5 -13 -12.60 5.30 4 5 13 -0.70 9.60 4 5 13 20.30 19.20 4 5 13 -11.20 10.30 4 5 13 8.60 18.40 5 5 13 13.90 17.70 5 5 13 32.60 13.00 5 5 13 35.80 14.90 5 5 13 67.79 25.70 -6 -5 -13 2.90 6.30 -6 -5 -13 25.40 9.10 6 5 13 4.00 10.20 6 5 13 4.30 16.80 6 5 13 20.20 19.40 -7 -5 -13 57.39 14.70 -7 -5 -13 88.39 14.80 7 5 13 104.49 23.00 7 5 13 128.59 35.90 -8 -5 -13 24.20 9.50 -8 -5 -13 49.10 13.50 8 5 13 60.99 16.20 8 5 13 32.60 20.10 -9 -5 -13 1.80 7.70 -9 -5 -13 15.80 9.90 9 5 13 0.70 19.60 9 5 13 19.00 10.70 -7 -6 -13 13.50 7.70 -7 -6 -13 6.60 6.90 7 6 13 48.10 22.50 7 6 13 -16.00 8.20 -4 1 -14 19.30 9.10 -4 1 -14 26.50 13.40 4 -1 14 26.90 17.80 4 -1 14 12.30 12.70 -5 1 -14 16.20 9.70 -5 1 -14 4.30 8.80 5 -1 14 22.70 14.30 5 -1 14 20.70 23.90 -4 0 -14 -3.80 6.70 -4 0 -14 12.50 9.90 4 0 14 -3.90 13.40 4 0 14 2.10 6.50 4 0 14 -0.90 19.40 -5 0 -14 20.50 10.10 -5 0 -14 30.90 11.40 5 0 14 17.80 11.80 5 0 14 4.50 19.60 5 0 14 -10.80 14.00 -6 0 -14 36.40 12.60 -6 0 -14 18.00 9.70 6 0 14 -7.80 14.50 6 0 14 37.30 27.20 6 0 14 60.59 18.50 -4 -1 -14 51.69 14.30 -4 -1 -14 22.20 8.80 4 1 14 54.89 31.60 4 1 14 14.60 15.60 4 1 14 7.60 10.50 -5 -1 -14 -2.00 5.30 -5 -1 -14 13.40 7.00 5 1 14 0.10 6.50 5 1 14 -8.90 9.60 5 1 14 -2.80 15.80 -6 -1 -14 17.00 10.30 -6 -1 -14 12.80 9.80 6 1 14 -21.00 19.70 6 1 14 2.80 17.70 6 1 14 29.30 14.00 -7 -1 -14 3.40 9.40 -7 -1 -14 16.30 11.40 7 1 14 -17.10 25.40 -5 -2 -14 -10.40 5.50 -5 -2 -14 3.90 7.90 5 2 14 -22.10 14.20 5 2 14 -3.50 8.90 5 2 14 -39.20 20.50 -6 -2 -14 -4.40 6.00 -6 -2 -14 -0.60 5.40 6 2 14 0.80 7.90 6 2 14 -5.30 14.10 6 2 14 -13.20 15.10 -7 -2 -14 19.30 10.40 -7 -2 -14 2.20 7.60 7 2 14 4.60 14.40 7 2 14 -38.00 18.80 7 2 14 22.60 12.60 -6 -3 -14 -10.70 4.80 -6 -3 -14 0.10 7.10 6 3 14 -26.40 23.00 6 3 14 -12.20 10.10 6 3 14 -21.60 9.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 28851 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 F1 F 0.1664(2) 0.0958(2) -0.09539(19) 0.1072(7) Uani 1 1 d . . . . . F2 F 0.0758(4) 0.0421(3) 0.0810(2) 0.1453(12) Uani 1 1 d . . . . . F3 F -0.0629(2) 0.2102(2) 0.0210(3) 0.1194(9) Uani 1 1 d . . . . . O2 O 0.2259(2) 0.3063(2) 0.65828(18) 0.0613(5) Uani 1 1 d . . . . . H2 H 0.277644 0.345036 0.657039 0.092 Uiso 1 1 calc R U . . . O3 O 0.2269(2) 0.41235(19) 0.49123(16) 0.0561(5) Uani 1 1 d . . . . . N2 N 0.1170(2) 0.3391(2) 0.35851(19) 0.0492(5) Uani 1 1 d . . . . . H2A H 0.159205 0.386060 0.370101 0.059 Uiso 1 1 calc R U . . . N5 N -0.0347(2) 0.2252(2) 0.4557(2) 0.0524(5) Uani 1 1 d . . . . . C2 C 0.1223(3) 0.3360(2) 0.2401(2) 0.0458(6) Uani 1 1 d . . . . . C3 C 0.0725(4) 0.1488(3) 0.0217(3) 0.0648(8) Uani 1 1 d . . . . . C5 C 0.1657(3) 0.4289(3) 0.1649(3) 0.0564(7) Uani 1 1 d . . . . . H5 H 0.184822 0.491981 0.196035 0.068 Uiso 1 1 calc R U . . . C9 C -0.0689(3) 0.1585(3) 0.6573(3) 0.0619(7) Uani 1 1 d . . . . . H9 H -0.112755 0.116445 0.723206 0.074 Uiso 1 1 calc R U . . . C11 C 0.1808(4) 0.4288(3) 0.0452(3) 0.0678(8) Uani 1 1 d . . . . . H11 H 0.209653 0.491987 -0.003449 0.081 Uiso 1 1 calc R U . . . C13 C 0.1856(3) 0.3390(2) 0.5667(2) 0.0459(6) Uani 1 1 d . . . . . C15 C 0.0246(3) 0.2136(3) 0.6607(2) 0.0538(6) Uani 1 1 d . . . . . H15 H 0.045395 0.208029 0.729313 0.065 Uiso 1 1 calc R U . . . C17 C 0.0944(3) 0.2422(3) 0.1913(2) 0.0504(6) Uani 1 1 d . . . . . H17 H 0.065978 0.178518 0.239392 0.061 Uiso 1 1 calc R U . . . C18 C 0.0552(3) 0.2793(2) 0.4590(2) 0.0425(5) Uani 1 1 d . . . . . C19 C -0.0949(3) 0.1679(3) 0.5537(3) 0.0586(7) Uani 1 1 d . . . . . H19 H -0.158931 0.131840 0.551878 0.070 Uiso 1 1 calc R U . . . C21 C 0.1096(3) 0.2448(3) 0.0706(2) 0.0544(6) Uani 1 1 d . . . . . C23 C 0.1538(3) 0.3363(3) -0.0038(3) 0.0682(8) Uani 1 1 d . . . . . H23 H 0.165102 0.335648 -0.085076 0.082 Uiso 1 1 calc R U . . . C25 C 0.0876(3) 0.2771(2) 0.5624(2) 0.0428(5) Uani 1 1 d . . . . . O1 O 0.5559(2) 1.06107(17) 0.85416(15) 0.0544(5) Uani 1 1 d . . . . . N1 N 0.4868(2) 0.88439(19) 0.90803(18) 0.0407(4) Uani 1 1 d . . . . . H1 H 0.472(3) 0.906(3) 0.987(3) 0.059(8) Uiso 1 1 d . . . . . N3 N 0.6191(3) 1.0953(2) 0.5398(2) 0.0609(6) Uani 1 1 d . . . . . N4 N 0.3670(2) 0.4450(2) 0.67510(19) 0.0483(5) Uani 1 1 d . . . . . C1 C 0.4326(2) 0.6472(2) 0.73800(19) 0.0363(5) Uani 1 1 d . . . . . C4 C 0.5022(2) 0.8441(2) 0.6828(2) 0.0376(5) Uani 1 1 d . . . . . H4 H 0.504714 0.832148 0.605767 0.045 Uiso 1 1 calc R U . . . C6 C 0.5804(3) 1.0297(2) 0.6140(2) 0.0418(5) Uani 1 1 d . . . . . C7 C 0.4638(3) 0.4141(2) 0.7267(2) 0.0502(6) Uani 1 1 d . . . . . H7 H 0.508402 0.323624 0.742439 0.060 Uiso 1 1 calc R U . . . C8 C 0.4644(2) 0.7570(2) 0.77122(19) 0.0362(5) Uani 1 1 d . . . . . C10 C 0.4551(2) 0.7817(2) 0.8863(2) 0.0374(5) Uani 1 1 d . . . . . C12 C 0.5353(2) 0.9459(2) 0.70634(19) 0.0366(5) Uani 1 1 d . . . . . C14 C 0.3365(3) 0.6775(2) 0.6804(2) 0.0452(6) Uani 1 1 d . . . . . H14 H 0.291855 0.766625 0.662009 0.054 Uiso 1 1 calc R U . . . C16 C 0.5289(3) 0.9700(2) 0.8248(2) 0.0400(5) Uani 1 1 d . . . . . C20 C 0.5002(3) 0.5105(2) 0.7575(2) 0.0455(6) Uani 1 1 d . . . . . H20 H 0.570173 0.484097 0.791398 0.055 Uiso 1 1 calc R U . . . C22 C 0.3075(3) 0.5747(3) 0.6507(2) 0.0503(6) Uani 1 1 d . . . . . H22 H 0.243205 0.596814 0.611674 0.060 Uiso 1 1 calc R U . . . C24 C 0.4057(3) 0.7087(3) 0.9955(2) 0.0512(6) Uani 1 1 d . . . . . H24A H 0.493766 0.636048 1.000711 0.077 Uiso 1 1 calc R U . . . H24B H 0.344154 0.670010 0.986586 0.077 Uiso 1 1 calc R U . . . H24C H 0.347461 0.773017 1.069625 0.077 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.1031(15) 0.1302(17) 0.0758(13) -0.0357(12) -0.0279(11) -0.0420(14) F2 0.303(4) 0.1262(19) 0.125(2) 0.0552(16) -0.147(3) -0.148(2) F3 0.0777(14) 0.1186(17) 0.168(2) -0.0425(16) -0.0618(15) -0.0283(13) O2 0.0807(13) 0.0717(12) 0.0684(12) 0.0161(10) -0.0479(11) -0.0503(11) O3 0.0685(11) 0.0646(11) 0.0564(11) 0.0067(9) -0.0292(9) -0.0446(10) N2 0.0579(12) 0.0563(12) 0.0508(12) 0.0092(10) -0.0283(10) -0.0352(10) N5 0.0526(12) 0.0643(13) 0.0564(13) 0.0049(10) -0.0268(10) -0.0353(11) C2 0.0401(12) 0.0492(13) 0.0471(13) 0.0036(11) -0.0196(11) -0.0171(11) C3 0.0728(19) 0.0732(19) 0.0527(16) -0.0004(14) -0.0331(15) -0.0277(16) C5 0.0563(15) 0.0567(15) 0.0591(16) 0.0084(13) -0.0246(13) -0.0273(13) C9 0.0730(18) 0.0760(18) 0.0507(15) 0.0096(13) -0.0203(14) -0.0508(16) C11 0.077(2) 0.0729(19) 0.0596(18) 0.0209(15) -0.0297(15) -0.0399(16) C13 0.0488(13) 0.0453(13) 0.0483(14) -0.0040(11) -0.0224(11) -0.0212(11) C15 0.0633(16) 0.0627(16) 0.0466(14) 0.0043(12) -0.0257(13) -0.0344(14) C17 0.0545(14) 0.0520(14) 0.0485(14) 0.0059(11) -0.0261(12) -0.0223(12) C18 0.0403(12) 0.0419(12) 0.0479(13) 0.0009(10) -0.0205(11) -0.0178(10) C19 0.0591(16) 0.0712(18) 0.0620(17) 0.0036(14) -0.0252(13) -0.0424(14) C21 0.0532(15) 0.0605(16) 0.0509(15) 0.0040(12) -0.0260(12) -0.0219(13) C23 0.075(2) 0.084(2) 0.0483(16) 0.0131(15) -0.0288(15) -0.0349(17) C25 0.0453(13) 0.0435(12) 0.0449(13) -0.0006(10) -0.0201(11) -0.0219(10) O1 0.0915(13) 0.0550(10) 0.0476(10) 0.0135(8) -0.0397(9) -0.0500(10) N1 0.0600(12) 0.0429(10) 0.0344(10) 0.0086(8) -0.0260(9) -0.0303(9) N3 0.0881(17) 0.0701(15) 0.0570(14) 0.0282(12) -0.0423(13) -0.0548(14) N4 0.0594(12) 0.0494(11) 0.0526(12) 0.0050(9) -0.0302(10) -0.0314(10) C1 0.0428(12) 0.0403(11) 0.0323(11) 0.0050(9) -0.0166(9) -0.0234(10) C4 0.0459(12) 0.0392(11) 0.0348(11) 0.0045(9) -0.0218(10) -0.0200(10) C6 0.0551(14) 0.0436(12) 0.0422(13) 0.0080(11) -0.0280(11) -0.0282(11) C7 0.0640(15) 0.0402(12) 0.0630(16) 0.0098(11) -0.0382(13) -0.0267(12) C8 0.0442(12) 0.0361(11) 0.0379(11) 0.0065(9) -0.0222(10) -0.0216(10) C10 0.0462(12) 0.0361(11) 0.0393(12) 0.0074(9) -0.0232(10) -0.0218(10) C12 0.0457(12) 0.0362(11) 0.0351(11) 0.0068(9) -0.0208(10) -0.0209(10) C14 0.0554(14) 0.0436(12) 0.0516(14) 0.0110(11) -0.0329(12) -0.0255(11) C16 0.0532(13) 0.0392(12) 0.0389(12) 0.0074(9) -0.0256(11) -0.0244(10) C20 0.0565(14) 0.0430(13) 0.0555(14) 0.0094(11) -0.0370(12) -0.0254(11) C22 0.0575(15) 0.0557(15) 0.0565(15) 0.0082(12) -0.0365(13) -0.0292(12) C24 0.0768(17) 0.0544(14) 0.0420(13) 0.0153(11) -0.0313(13) -0.0411(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 O2 H2 109.5 . . ? C2 N2 H2A 114.8 . . ? C18 N2 H2A 114.8 . . ? C18 N2 C2 130.4(2) . . ? C19 N5 C18 117.9(2) . . ? C5 C2 N2 117.0(2) . . ? C5 C2 C17 118.5(2) . . ? C17 C2 N2 124.4(2) . . ? F1 C3 C21 113.6(3) . . ? F2 C3 F1 104.6(3) . . ? F2 C3 F3 106.7(3) . . ? F2 C3 C21 114.6(2) . . ? F3 C3 F1 103.7(2) . . ? F3 C3 C21 112.6(2) . . ? C2 C5 H5 119.5 . . ? C11 C5 C2 120.9(3) . . ? C11 C5 H5 119.5 . . ? C15 C9 H9 121.1 . . ? C19 C9 H9 121.1 . . ? C19 C9 C15 117.7(2) . . ? C5 C11 H11 119.6 . . ? C5 C11 C23 120.9(3) . . ? C23 C11 H11 119.6 . . ? O2 C13 C25 113.9(2) . . ? O3 C13 O2 122.8(2) . . ? O3 C13 C25 123.3(2) . . ? C9 C15 H15 119.8 . . ? C9 C15 C25 120.3(2) . . ? C25 C15 H15 119.8 . . ? C2 C17 H17 120.3 . . ? C21 C17 C2 119.4(2) . . ? C21 C17 H17 120.3 . . ? N2 C18 C25 119.6(2) . . ? N5 C18 N2 118.2(2) . . ? N5 C18 C25 122.2(2) . . ? N5 C19 C9 124.4(2) . . ? N5 C19 H19 117.8 . . ? C9 C19 H19 117.8 . . ? C17 C21 C3 118.9(2) . . ? C23 C21 C3 119.2(2) . . ? C23 C21 C17 121.9(3) . . ? C11 C23 H23 120.8 . . ? C21 C23 C11 118.4(3) . . ? C21 C23 H23 120.8 . . ? C15 C25 C13 120.5(2) . . ? C15 C25 C18 117.4(2) . . ? C18 C25 C13 122.2(2) . . ? C10 N1 H1 119.3(16) . . ? C10 N1 C16 126.18(19) . . ? C16 N1 H1 114.3(16) . . ? C22 N4 C7 117.38(19) . . ? C14 C1 C8 120.20(19) . . ? C14 C1 C20 116.85(19) . . ? C20 C1 C8 122.89(19) . . ? C8 C4 H4 118.9 . . ? C12 C4 H4 118.9 . . ? C12 C4 C8 122.23(19) . . ? N3 C6 C12 178.8(3) . . ? N4 C7 H7 118.6 . . ? N4 C7 C20 122.7(2) . . ? C20 C7 H7 118.6 . . ? C4 C8 C1 119.07(18) . . ? C10 C8 C1 123.58(19) . . ? C10 C8 C4 117.32(18) . . ? N1 C10 C8 119.39(19) . . ? N1 C10 C24 114.70(19) . . ? C8 C10 C24 125.85(19) . . ? C4 C12 C6 121.77(19) . . ? C4 C12 C16 120.61(19) . . ? C6 C12 C16 117.61(19) . . ? C1 C14 H14 120.2 . . ? C22 C14 C1 119.5(2) . . ? C22 C14 H14 120.2 . . ? O1 C16 N1 121.08(19) . . ? O1 C16 C12 124.7(2) . . ? N1 C16 C12 114.22(19) . . ? C1 C20 H20 120.0 . . ? C7 C20 C1 120.0(2) . . ? C7 C20 H20 120.0 . . ? N4 C22 C14 123.3(2) . . ? N4 C22 H22 118.3 . . ? C14 C22 H22 118.3 . . ? C10 C24 H24A 109.5 . . ? C10 C24 H24B 109.5 . . ? C10 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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 C3 1.327(3) . ? F2 C3 1.299(4) . ? F3 C3 1.319(3) . ? O2 H2 0.8200 . ? O2 C13 1.312(3) . ? O3 C13 1.221(3) . ? N2 H2A 0.8600 . ? N2 C2 1.399(3) . ? N2 C18 1.371(3) . ? N5 C18 1.337(3) . ? N5 C19 1.330(3) . ? C2 C5 1.392(3) . ? C2 C17 1.395(3) . ? C3 C21 1.488(4) . ? C5 H5 0.9300 . ? C5 C11 1.375(4) . ? C9 H9 0.9300 . ? C9 C15 1.379(4) . ? C9 C19 1.370(4) . ? C11 H11 0.9300 . ? C11 C23 1.379(4) . ? C13 C25 1.483(3) . ? C15 H15 0.9300 . ? C15 C25 1.383(3) . ? C17 H17 0.9300 . ? C17 C21 1.386(4) . ? C18 C25 1.416(3) . ? C19 H19 0.9300 . ? C21 C23 1.378(4) . ? C23 H23 0.9300 . ? O1 C16 1.245(3) . ? N1 H1 0.92(3) . ? N1 C10 1.359(3) . ? N1 C16 1.372(3) . ? N3 C6 1.143(3) . ? N4 C7 1.335(3) . ? N4 C22 1.334(3) . ? C1 C8 1.485(3) . ? C1 C14 1.386(3) . ? C1 C20 1.389(3) . ? C4 H4 0.9300 . ? C4 C8 1.406(3) . ? C4 C12 1.368(3) . ? C6 C12 1.428(3) . ? C7 H7 0.9300 . ? C7 C20 1.376(3) . ? C8 C10 1.379(3) . ? C10 C24 1.492(3) . ? C12 C16 1.432(3) . ? C14 H14 0.9300 . ? C14 C22 1.377(3) . ? C20 H20 0.9300 . ? C22 H22 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2 H2 N4 0.82 1.79 2.606(2) 171.4 . yes N2 H2A O3 0.86 1.96 2.665(2) 138.6 . yes N1 H1 O1 0.92(3) 1.84(3) 2.759(2) 177(2) 2_677 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 C3 C21 C17 -141.1(3) . . . . ? F1 C3 C21 C23 40.7(4) . . . . ? F2 C3 C21 C17 -21.0(4) . . . . ? F2 C3 C21 C23 160.8(3) . . . . ? F3 C3 C21 C17 101.3(3) . . . . ? F3 C3 C21 C23 -76.9(3) . . . . ? O2 C13 C25 C15 11.3(3) . . . . ? O2 C13 C25 C18 -168.3(2) . . . . ? O3 C13 C25 C15 -169.6(2) . . . . ? O3 C13 C25 C18 10.8(4) . . . . ? N2 C2 C5 C11 177.0(2) . . . . ? N2 C2 C17 C21 -177.1(2) . . . . ? N2 C18 C25 C13 0.7(3) . . . . ? N2 C18 C25 C15 -179.0(2) . . . . ? N5 C18 C25 C13 -179.1(2) . . . . ? N5 C18 C25 C15 1.3(3) . . . . ? C2 N2 C18 N5 -11.4(4) . . . . ? C2 N2 C18 C25 168.9(2) . . . . ? C2 C5 C11 C23 -0.2(4) . . . . ? C2 C17 C21 C3 -177.1(2) . . . . ? C2 C17 C21 C23 1.0(4) . . . . ? C3 C21 C23 C11 177.0(3) . . . . ? C5 C2 C17 C21 -0.5(4) . . . . ? C5 C11 C23 C21 0.7(4) . . . . ? C9 C15 C25 C13 178.7(2) . . . . ? C9 C15 C25 C18 -1.6(4) . . . . ? C15 C9 C19 N5 0.8(4) . . . . ? C17 C2 C5 C11 0.1(4) . . . . ? C17 C21 C23 C11 -1.1(4) . . . . ? C18 N2 C2 C5 167.5(2) . . . . ? C18 N2 C2 C17 -15.8(4) . . . . ? C18 N5 C19 C9 -1.2(4) . . . . ? C19 N5 C18 N2 -179.7(2) . . . . ? C19 N5 C18 C25 0.1(4) . . . . ? C19 C9 C15 C25 0.7(4) . . . . ? N4 C7 C20 C1 1.6(4) . . . . ? C1 C8 C10 N1 179.8(2) . . . . ? C1 C8 C10 C24 -3.0(4) . . . . ? C1 C14 C22 N4 0.4(4) . . . . ? C4 C8 C10 N1 -2.0(3) . . . . ? C4 C8 C10 C24 175.2(2) . . . . ? C4 C12 C16 O1 -179.3(2) . . . . ? C4 C12 C16 N1 -0.5(3) . . . . ? C6 C12 C16 O1 2.0(3) . . . . ? C6 C12 C16 N1 -179.14(19) . . . . ? C7 N4 C22 C14 -2.6(4) . . . . ? C8 C1 C14 C22 -179.7(2) . . . . ? C8 C1 C20 C7 178.8(2) . . . . ? C8 C4 C12 C6 177.0(2) . . . . ? C8 C4 C12 C16 -1.6(3) . . . . ? C10 N1 C16 O1 -179.8(2) . . . . ? C10 N1 C16 C12 1.3(3) . . . . ? C12 C4 C8 C1 -178.9(2) . . . . ? C12 C4 C8 C10 2.8(3) . . . . ? C14 C1 C8 C4 -47.0(3) . . . . ? C14 C1 C8 C10 131.2(2) . . . . ? C14 C1 C20 C7 -3.7(3) . . . . ? C16 N1 C10 C8 0.0(3) . . . . ? C16 N1 C10 C24 -177.5(2) . . . . ? C20 C1 C8 C4 130.4(2) . . . . ? C20 C1 C8 C10 -51.5(3) . . . . ? C20 C1 C14 C22 2.8(3) . . . . ? C22 N4 C7 C20 1.6(4) . . . . ?