#------------------------------------------------------------------------------ #$Date: 2024-02-05 14:04:31 +0200 (Mon, 05 Feb 2024) $ #$Revision: 289678 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312369.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_2312369 loop_ _publ_author_name 'Metherall, Jessica P.' 'Corner, Philip A.' 'McCabe, James F.' 'Hall, Michael J.' 'Probert, Michael R.' _publ_section_title ; High-throughput nanoscale crystallization of dihydropyridine active pharmaceutical ingredients. ; _journal_coeditor_code RM5073SUP1 _journal_issue 1 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_page_first 4 _journal_page_last 12 _journal_paper_doi 10.1107/S2052520623010053 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'C17 H18 N2 O6' _chemical_formula_sum 'C17 H18 N2 O6' _chemical_formula_weight 346.33 _chemical_name_common Nifedipine _chemical_name_systematic 'dimethyl 2,6-dimethyl-4-(2-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-05-11 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _cell_angle_alpha 90 _cell_angle_beta 94.545(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.6713(3) _cell_length_b 10.3971(3) _cell_length_c 14.7824(3) _cell_measurement_reflns_used 5449 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 76.5080 _cell_measurement_theta_min 4.1030 _cell_volume 1634.96(7) _computing_cell_refinement 'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)' _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 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.940 _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 -36.00 11.00 0.50 0.19 -- -45.34 85.00-149.00 94 2 \w -67.00 -41.00 0.50 0.19 -- -45.34 85.00-149.00 52 3 \w 23.00 49.00 0.50 0.19 -- 46.34 -85.00 91.00 52 4 \w -149.00-101.00 0.50 0.19 -- -85.06 -85.00 91.00 96 5 \w -66.00 -32.00 0.50 0.19 -- -85.06 85.00-149.00 68 6 \w 47.00 93.00 0.50 0.19 -- 109.85 -85.00 91.00 92 7 \w 128.00 159.00 0.50 0.19 -- 109.85 85.00-149.00 62 8 \w -14.00 28.00 0.50 0.19 -- -45.34 38.00 30.00 84 9 \w -3.00 29.00 0.50 0.19 -- -45.34 38.00 -60.00 64 10 \w -12.00 34.00 0.50 0.19 -- -45.34 38.00 90.00 92 11 \w -41.00 -11.00 0.50 0.19 -- -85.06 61.00 150.00 60 12 \w -142.00-104.00 0.50 0.19 -- -85.06 -77.00 120.00 76 13 \w -45.00 -18.00 0.50 0.19 -- -85.06 61.00 90.00 54 14 \w -44.00 -19.00 0.50 0.19 -- -85.06 61.00 30.00 50 15 \w -38.00 -12.00 0.50 0.19 -- -85.06 61.00 120.00 52 16 \w -41.00 -15.00 0.50 0.19 -- -85.06 61.00 -30.00 52 17 \w -45.00 -20.00 0.50 0.19 -- -85.06 61.00 0.00 50 18 \w 30.00 56.00 0.50 0.19 -- 100.34 -61.00 150.00 52 19 \w 66.00 133.00 0.50 0.19 -- 100.34 15.00-180.00 134 20 \w 33.00 68.00 0.50 0.19 -- 100.34 -77.00-120.00 70 21 \w 26.00 51.00 0.50 0.19 -- 100.34 -61.00 -60.00 50 22 \w 28.00 53.00 0.50 0.19 -- 100.34 -61.00 120.00 50 23 \w 38.00 63.00 0.50 0.19 -- 100.34 -85.00 91.00 50 24 \w 30.00 55.00 0.50 0.19 -- 100.34 -61.00-120.00 50 25 \w 28.00 53.00 0.50 0.19 -- 100.34 -61.00 30.00 50 26 \w 26.00 51.00 0.50 0.19 -- 100.34 -61.00 0.00 50 27 \w 44.00 71.00 0.50 0.19 -- 109.85 -77.00 150.00 54 28 \w 54.00 79.00 0.50 0.19 -- 109.85 -95.00-180.00 50 29 \w 42.00 80.00 0.50 0.19 -- 109.85 -77.00 -90.00 76 30 \w 46.00 75.00 0.50 0.19 -- 109.85 -77.00-180.00 58 31 \w 44.00 71.00 0.50 0.19 -- 109.85 -77.00 -30.00 54 32 \w 52.00 77.00 0.50 0.19 -- 109.85 -77.00-150.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix-Arc 100' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0868982000 _diffrn_orient_matrix_UB_12 -0.1149612000 _diffrn_orient_matrix_UB_13 -0.0154861000 _diffrn_orient_matrix_UB_21 0.1056629000 _diffrn_orient_matrix_UB_22 0.0635908000 _diffrn_orient_matrix_UB_23 0.0616148000 _diffrn_orient_matrix_UB_31 -0.0477910000 _diffrn_orient_matrix_UB_32 -0.0685980000 _diffrn_orient_matrix_UB_33 0.0829130000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10751 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.098 _diffrn_reflns_theta_min 4.156 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.407 _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_preparation 'Crystallised from a saturated solution of nifedipine in 2,2,2-TFE.' _exptl_crystal_recrystallization_method 'High-throughput screening via the ENaCt protocol using SPT Labtech mosquito.' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.407 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 234 _refine_ls_number_reflns 3255 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0409 _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^)+(0.0646P)^2^+0.4924P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1146 _refine_ls_wR_factor_ref 0.1191 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2857 _reflns_number_total 3255 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file rm5073sup1.cif _cod_data_source_block nifedipine _cod_depositor_comments 'Adding full bibliography for 2312368--2312375.cif.' _cod_database_code 2312369 _cod_database_fobs_code 2312369 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H N O' _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_max 0.825 _shelx_estimated_absorpt_t_min 0.655 _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 Ternary CH refined with riding coordinates: C9(H9) 2.b Aromatic/amide H refined with riding coordinates: C15(H15), C13(H13), C14(H14), C12(H12) 2.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C) ; _shelx_res_file ; TITL nifedipine4degknown_auto_a.res in P2(1)/c nifedipine.res created by SHELXL-2018/3 at 10:47:36 on 11-May-2023 REM Old TITL nifedipine 4 deg known_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.137, Rweak 0.053, Alpha 0.015 REM 0.450 for 194 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N2 O5 CELL 1.54184 10.6713 10.3971 14.7824 90 94.545 90 ZERR 4 0.0003 0.0003 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 68 72 8 24 L.S. 4 PLAN 5 SIZE 0.22 0.45 0.51 TEMP -123 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.064600 0.492400 FVAR 0.72097 O1 4 0.859539 0.631082 0.475017 11.00000 0.04128 0.02602 = 0.03240 0.00035 0.01030 -0.01033 O6 4 0.457917 0.217948 0.534391 11.00000 0.03402 0.03010 = 0.03795 -0.00602 0.00640 -0.00907 O5 4 0.368568 0.266420 0.662243 11.00000 0.03060 0.03418 = 0.03625 0.00609 0.00768 -0.00368 O3 4 0.656134 0.197541 0.397513 11.00000 0.04943 0.03635 = 0.03292 -0.00448 -0.00245 -0.00328 O2 4 0.824137 0.428789 0.430968 11.00000 0.06581 0.02689 = 0.03451 -0.00355 0.02252 -0.00646 O4 4 0.847880 0.138280 0.385131 11.00000 0.06650 0.05008 = 0.03507 -0.00261 0.01946 0.01617 N2 3 0.761527 0.170681 0.430541 11.00000 0.04416 0.02152 = 0.02850 -0.00410 0.00748 -0.00211 N1 3 0.642302 0.565791 0.694976 11.00000 0.03343 0.02903 = 0.02847 -0.00853 0.00695 -0.00304 C3 1 0.733527 0.498972 0.562285 11.00000 0.02648 0.02029 = 0.02592 0.00120 0.00257 -0.00061 C16 1 0.448576 0.288832 0.609491 11.00000 0.02498 0.02406 = 0.02942 0.00458 0.00137 0.00246 C4 1 0.730957 0.581708 0.632694 11.00000 0.02815 0.02260 = 0.02774 -0.00011 0.00243 -0.00010 C8 1 0.546233 0.387556 0.618626 11.00000 0.02437 0.02488 = 0.02525 0.00262 0.00265 0.00015 C9 1 0.654464 0.376563 0.557519 11.00000 0.02727 0.02076 = 0.02322 -0.00018 0.00392 -0.00283 AFIX 13 H9 2 0.619027 0.363525 0.493509 11.00000 -1.20000 AFIX 0 C11 1 0.787607 0.169162 0.529871 11.00000 0.02980 0.02210 = 0.02704 -0.00001 0.00517 -0.00564 C15 1 0.773658 0.246272 0.679081 11.00000 0.02842 0.02697 = 0.02693 0.00026 0.00573 -0.00274 AFIX 43 H15 2 0.744527 0.307489 0.720271 11.00000 -1.20000 AFIX 0 C2 1 0.810636 0.514026 0.484861 11.00000 0.02927 0.02220 = 0.02500 0.00215 0.00124 -0.00128 C10 1 0.737708 0.260349 0.586464 11.00000 0.02419 0.02064 = 0.02684 0.00080 0.00557 -0.00540 C6 1 0.545151 0.478273 0.684183 11.00000 0.02765 0.02893 = 0.02740 -0.00058 0.00372 0.00141 C13 1 0.895477 0.056998 0.654742 11.00000 0.02785 0.02425 = 0.04221 0.00657 0.00421 -0.00121 AFIX 43 H13 2 0.946863 -0.012048 0.677787 11.00000 -1.20000 AFIX 0 C14 1 0.849859 0.146947 0.713228 11.00000 0.02958 0.03230 = 0.02881 0.00671 0.00408 -0.00424 AFIX 43 H14 2 0.870916 0.140379 0.776715 11.00000 -1.20000 AFIX 0 C12 1 0.865160 0.069230 0.562610 11.00000 0.03079 0.02094 = 0.03823 -0.00313 0.00777 -0.00340 AFIX 43 H12 2 0.897210 0.009494 0.521631 11.00000 -1.20000 AFIX 0 C5 1 0.817332 0.693397 0.656283 11.00000 0.04330 0.02826 = 0.03569 -0.00717 0.00543 -0.00852 AFIX 137 H5A 2 0.772323 0.774210 0.642974 11.00000 -1.50000 H5B 2 0.890413 0.688560 0.620244 11.00000 -1.50000 H5C 2 0.845456 0.690088 0.720979 11.00000 -1.50000 AFIX 0 C7 1 0.445871 0.495850 0.749685 11.00000 0.03342 0.04377 = 0.03804 -0.00948 0.01191 -0.00103 AFIX 137 H7A 2 0.454225 0.428285 0.795995 11.00000 -1.50000 H7B 2 0.362529 0.490500 0.716918 11.00000 -1.50000 H7C 2 0.456080 0.580234 0.778879 11.00000 -1.50000 AFIX 0 C1 1 0.926556 0.647298 0.394804 11.00000 0.03757 0.03841 = 0.03651 0.00516 0.01067 -0.01118 AFIX 137 H1A 2 0.868971 0.633156 0.340728 11.00000 -1.50000 H1B 2 0.995572 0.585019 0.395653 11.00000 -1.50000 H1C 2 0.960662 0.734738 0.393530 11.00000 -1.50000 AFIX 0 C17 1 0.367947 0.115993 0.520018 11.00000 0.03689 0.03184 = 0.05059 -0.00638 0.00213 -0.01066 AFIX 137 H17A 2 0.377694 0.075332 0.461178 11.00000 -1.50000 H17B 2 0.282802 0.151111 0.520683 11.00000 -1.50000 H17C 2 0.381888 0.051891 0.568372 11.00000 -1.50000 AFIX 0 H1 2 0.640445 0.621985 0.740837 11.00000 0.03613 HKLF 4 REM nifedipine4degknown_auto_a.res in P2(1)/c REM wR2 = 0.1191, GooF = S = 1.063, Restrained GooF = 1.063 for all data REM R1 = 0.0409 for 2857 Fo > 4sig(Fo) and 0.0459 for all 3255 data REM 234 parameters refined using 0 restraints END WGHT 0.0646 0.4924 REM Highest difference peak 0.407, deepest hole -0.182, 1-sigma level 0.047 Q1 1 0.6098 0.3767 0.4619 11.00000 0.05 0.41 Q2 1 0.7633 0.5136 0.5272 11.00000 0.05 0.25 Q3 1 0.7791 0.1793 0.4894 11.00000 0.05 0.23 Q4 1 0.6010 0.3785 0.5943 11.00000 0.05 0.23 Q5 1 0.4985 0.4853 0.7186 11.00000 0.05 0.22 ; _shelx_res_checksum 19895 _shelx_hkl_file ; 0 0 1 0.02 0.18 0 0 2 5239.51 140.71 0 0 3 0.64 0.58 0 0 4 1243.58 34.26 0 0 5 0.16 0.43 0 0 6 25.15 1.72 0 0 7 0.12 0.56 0 0 7 0.69 0.84 0 0 7 0.49 0.71 0 0 8 184.94 7.52 0 0 8 182.00 7.66 0 0 8 184.41 7.62 0 0 8 167.24 6.67 0 0 9 -1.03 0.92 0 0 9 -0.74 1.13 0 0 9 -0.23 0.94 0 0 9 -0.25 0.89 0 0 10 -0.27 1.88 0 0 10 2.46 1.24 0 0 10 3.45 1.44 0 0 10 2.02 1.20 0 0 11 0.62 1.04 0 0 11 -0.31 1.07 0 0 11 0.31 1.05 0 0 11 0.33 1.22 0 0 12 0.34 2.43 0 0 12 1.03 1.86 0 0 12 5.12 1.83 0 0 13 -1.10 1.52 0 0 13 -0.36 1.47 0 0 14 135.99 8.57 0 0 14 155.85 9.10 0 0 15 -0.68 1.22 0 0 15 -0.34 1.28 0 0 16 14.85 2.57 0 0 16 16.53 2.53 0 0 17 0.67 1.02 0 0 18 0.89 1.62 0 -1 0 0.09 0.23 0 -1 1 1928.42 51.56 0 -1 1 1897.87 51.38 0 -1 2 1862.46 51.26 0 -1 2 1913.27 51.40 0 -1 2 1927.93 51.42 0 -1 3 235.85 6.95 0 -1 3 223.34 6.68 0 -1 4 146.25 4.97 0 -1 4 150.83 4.61 0 -1 5 33.37 1.85 0 -1 5 31.32 1.39 0 -1 6 1742.70 40.63 0 -1 6 1763.51 41.31 0 1 6 1801.03 41.34 0 -1 7 31.81 2.63 0 1 7 29.73 2.52 0 -1 7 34.92 2.64 0 1 7 35.03 2.72 0 -1 7 38.19 2.35 0 -1 7 36.26 2.69 0 1 7 34.45 2.30 0 1 8 989.43 29.24 0 -1 8 973.57 29.26 0 -1 8 981.09 29.43 0 -1 8 953.83 28.34 0 1 8 968.08 28.48 0 1 8 1006.85 29.68 0 1 9 6.91 1.59 0 -1 9 10.41 1.84 0 -1 9 7.81 1.54 0 -1 9 8.46 1.63 0 -1 9 2.57 1.56 0 1 9 4.86 1.67 0 1 10 145.04 7.25 0 -1 10 142.10 7.25 0 -1 10 135.72 6.90 0 1 10 149.48 7.59 0 1 10 138.92 7.32 0 -1 10 139.87 7.24 0 1 10 148.83 7.32 0 -1 10 136.48 7.20 0 -1 10 154.56 7.51 0 1 11 23.74 3.04 0 -1 11 25.75 3.10 0 -1 11 27.09 3.10 0 1 11 21.09 2.77 0 -1 11 19.42 2.76 0 -1 11 25.63 2.90 0 1 11 24.07 2.89 0 1 11 22.85 3.04 0 1 12 218.47 10.72 0 -1 12 232.73 10.72 0 1 12 250.59 10.93 0 1 12 249.26 11.37 0 1 12 239.28 10.75 0 -1 12 235.56 10.89 0 -1 12 222.11 10.23 0 -1 13 11.56 2.89 0 1 13 10.41 2.95 0 -1 13 15.67 2.79 0 1 13 17.37 3.08 0 -1 13 10.27 3.14 0 1 13 14.42 3.22 0 -1 14 81.70 5.87 0 1 14 87.98 6.08 0 -1 14 81.12 5.91 0 1 14 82.87 5.97 0 1 14 85.54 6.23 0 -1 15 95.38 6.33 0 1 15 108.23 6.59 0 1 15 103.38 6.49 0 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12 1.36 1.30 0 -2 12 4.31 1.48 0 2 12 -1.56 1.53 0 2 13 129.59 7.60 0 -2 13 123.11 7.52 0 -2 13 116.91 7.40 0 2 13 117.84 7.26 0 2 13 119.94 7.64 0 2 14 163.24 8.98 0 -2 14 153.65 8.62 0 2 14 174.25 8.96 0 2 14 172.56 9.01 0 -2 14 179.07 9.12 0 2 15 143.04 8.18 0 2 15 162.22 8.35 0 -2 15 176.02 8.56 0 2 15 165.94 7.88 0 2 15 161.31 8.26 0 -2 15 165.20 8.38 0 -2 16 402.82 14.39 0 2 16 417.75 14.48 0 -2 17 19.96 2.28 0 2 17 22.97 2.39 0 2 18 10.63 1.34 0 -2 18 10.80 1.44 0 -3 0 0.99 0.66 0 -3 -1 1467.71 39.57 0 -3 1 1369.83 39.46 0 3 2 634.65 16.90 0 -3 2 644.13 18.03 0 -3 3 561.67 16.54 0 3 3 631.70 16.64 0 -3 3 619.22 17.36 0 -3 3 560.52 16.17 0 3 4 269.47 8.40 0 -3 4 256.36 8.35 0 -3 4 264.95 8.72 0 3 5 140.73 5.24 0 -3 5 132.23 5.18 0 -3 5 129.38 5.13 0 -3 6 0.98 0.68 0 3 6 0.70 0.68 0 -3 6 2.13 0.86 0 -3 6 0.34 0.51 0 -3 7 587.51 18.67 0 -3 7 568.23 18.13 0 -3 8 24.21 2.63 0 -3 8 20.33 2.37 0 3 8 30.56 2.94 0 -3 8 24.01 2.26 0 -3 8 28.03 2.68 0 3 8 22.74 2.46 0 3 9 15.52 2.25 0 -3 9 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-11 -3 -1 3.50 1.44 -11 -3 -1 3.77 1.31 -11 3 -2 11.47 2.07 -11 -3 -2 10.33 1.90 -11 -3 -2 15.33 2.06 -11 3 -3 111.86 5.96 -11 -3 -3 118.12 5.97 -11 3 -4 -0.91 1.07 -11 -3 -4 -0.22 1.05 -11 3 -5 92.08 4.93 -11 -3 -5 86.44 4.75 -11 -3 -6 13.41 1.48 11 3 7 1.67 0.76 -11 4 10 5.19 0.89 -11 4 9 0.29 0.67 -11 4 8 5.00 1.12 -11 -4 8 6.54 1.48 -11 -4 8 3.60 0.98 -11 4 7 23.80 2.27 -11 -4 7 27.89 2.77 -11 -4 7 25.78 2.40 -11 4 6 11.13 1.62 -11 -4 6 10.62 1.75 -11 -4 6 12.24 2.01 -11 -4 5 88.12 5.20 -11 -4 5 88.30 4.94 -11 -4 5 89.73 5.34 -11 -4 4 96.88 5.56 -11 -4 4 90.98 5.25 -11 -4 4 85.02 5.30 -11 -4 3 6.96 1.73 -11 -4 3 7.29 1.73 -11 -4 3 6.79 1.60 -11 -4 2 42.13 3.72 -11 -4 2 40.43 3.60 -11 -4 2 39.54 3.36 -11 -4 1 80.69 5.10 -11 -4 1 69.18 4.42 -11 -4 1 85.50 5.35 -11 4 0 157.81 7.14 -11 -4 0 149.09 7.27 -11 4 -1 0.22 1.01 -11 -4 -1 -0.71 0.93 -11 -4 -2 1.01 1.12 -11 4 -2 0.21 0.95 -11 -4 -2 0.62 0.85 -11 -4 -3 2.27 1.08 -11 4 -3 2.12 1.06 -11 -4 -3 1.84 0.81 -11 -4 -4 1.36 0.81 -11 -4 -5 0.76 0.64 11 -4 5 0.28 0.56 11 4 6 -0.09 0.45 -11 5 8 8.25 1.12 -11 5 7 9.65 1.25 -11 -5 7 12.41 1.59 -11 5 6 0.27 0.60 -11 -5 6 0.20 0.80 -11 -5 5 37.95 2.84 -11 -5 5 30.78 2.96 -11 -5 4 5.86 1.25 -11 -5 4 9.94 1.68 -11 -5 4 10.13 1.76 -11 -5 4 10.29 1.77 -11 -5 3 14.86 2.04 -11 -5 3 13.47 2.00 -11 -5 2 36.29 3.19 -11 -5 2 38.52 3.24 -11 -5 1 17.46 2.29 -11 -5 1 16.79 2.14 -11 -5 0 1.71 1.13 -11 -5 0 1.71 0.95 -11 -5 -1 33.74 2.94 -11 -5 -1 27.14 2.43 -11 -5 -2 14.34 1.86 -11 -5 -2 12.34 1.49 -11 -5 -3 2.02 0.97 -11 -5 -4 0.59 0.70 -11 -6 5 0.69 0.77 -11 -6 4 3.59 1.02 -11 -6 4 2.95 0.89 -11 -6 4 2.60 0.98 -11 -6 3 12.79 1.81 -11 -6 3 13.42 1.68 -11 -6 3 13.15 1.80 -11 -6 2 31.40 2.67 -11 -6 2 31.74 2.58 -11 -6 2 29.02 2.53 -11 -6 1 0.61 0.84 -11 -6 1 1.06 0.85 -11 -6 0 16.46 1.93 -11 -6 0 15.00 1.65 -11 -6 -1 0.36 0.75 -11 -6 -1 0.13 0.57 -11 -6 -2 4.00 0.97 -11 -6 -3 0.13 0.52 -11 -7 3 61.70 3.10 -11 -7 2 0.13 0.62 -11 -7 1 30.20 2.26 -11 -7 0 19.11 1.75 -11 -7 -1 3.63 0.89 -11 -7 -2 5.30 0.89 -12 0 9 1.05 0.66 -12 0 8 18.66 1.98 -12 0 7 -0.61 0.93 -12 0 6 47.40 3.14 -12 0 6 54.99 3.71 -12 0 5 -0.41 0.81 -12 0 5 2.29 1.17 -12 0 4 87.42 5.16 -12 0 3 -0.50 1.34 -12 0 2 72.14 4.78 -12 0 1 -2.03 1.93 -12 0 0 119.92 6.36 -12 0 -1 -0.25 1.14 -12 0 -2 37.97 3.28 -12 0 -3 -0.87 1.11 -12 0 -4 3.35 1.23 12 0 7 -0.10 0.44 -12 -1 9 -0.38 0.56 -12 1 9 0.12 0.55 -12 -1 8 42.61 2.94 -12 1 8 39.29 2.77 -12 1 7 40.60 2.83 -12 -1 7 48.88 3.34 -12 -1 6 59.40 3.59 -12 -1 6 58.79 3.87 -12 1 6 63.71 3.94 -12 1 6 55.02 3.46 -12 -1 6 60.62 3.98 -12 -1 5 11.88 1.72 -12 -1 5 12.52 1.87 -12 1 5 9.70 1.71 -12 -1 5 14.28 2.03 -12 -1 4 2.53 1.09 -12 -1 4 2.82 1.24 -12 1 4 2.31 1.29 -12 -1 4 0.95 0.99 -12 -1 3 7.51 1.63 -12 1 3 7.39 1.70 -12 -1 3 5.57 1.42 -12 -1 2 7.37 1.48 -12 -1 1 2.10 0.99 -12 1 1 0.74 1.33 -12 -1 1 2.47 1.59 -12 1 0 36.50 3.28 -12 -1 0 33.97 3.18 -12 1 -1 38.29 3.40 -12 -1 -1 44.18 3.53 -12 1 -2 179.64 7.99 -12 -1 -2 191.42 8.12 -12 1 -3 110.90 5.58 -12 -1 -3 102.04 5.45 -12 -1 -4 3.10 0.81 12 -1 6 16.81 1.63 12 1 6 19.77 1.75 12 1 7 1.06 0.52 -12 2 9 2.59 0.67 -12 -2 9 3.96 0.80 -12 -2 8 2.02 0.85 -12 2 8 0.84 0.62 -12 -2 7 14.17 1.50 -12 -2 7 14.13 1.76 -12 2 7 10.94 1.36 -12 2 6 19.75 1.78 -12 -2 6 20.31 2.18 -12 -2 6 21.59 2.05 -12 -2 5 30.41 2.72 -12 2 5 33.57 2.80 -12 -2 5 37.72 3.11 -12 -2 5 34.58 2.80 -12 -2 4 54.92 3.49 -12 -2 4 54.89 3.77 -12 -2 4 55.56 3.78 -12 2 4 58.31 3.75 -12 -2 4 46.40 3.55 -12 -2 3 148.79 6.84 -12 -2 3 135.74 6.59 -12 2 3 144.80 6.67 -12 -2 3 132.90 6.41 -12 -2 2 7.17 1.53 -12 -2 2 8.13 1.44 -12 2 2 4.18 1.55 -12 2 1 29.85 2.88 -12 -2 1 33.47 2.98 -12 -2 1 28.79 2.81 -12 2 0 1.11 1.24 -12 -2 0 0.22 1.15 -12 -2 0 -0.23 0.89 -12 2 -1 33.87 2.99 -12 -2 -1 34.04 3.01 -12 -2 -1 33.21 2.79 -12 2 -2 82.72 4.73 -12 -2 -2 76.38 4.26 -12 -2 -3 6.75 1.16 12 -2 6 8.32 1.04 12 2 6 6.81 0.98 -12 -3 8 1.04 0.69 -12 -3 7 0.48 0.79 -12 -3 6 31.29 2.39 -12 -3 6 30.29 2.57 -12 -3 5 12.07 1.69 -12 -3 5 10.40 1.68 -12 -3 4 31.23 2.72 -12 -3 4 30.80 2.48 -12 -3 4 33.83 2.73 -12 -3 3 19.95 2.24 -12 -3 3 19.40 2.16 -12 -3 3 25.74 2.31 -12 -3 2 -0.22 0.88 -12 -3 2 -0.43 0.84 -12 -3 2 0.17 0.68 -12 -3 1 4.25 1.25 -12 -3 1 3.74 1.26 -12 -3 0 3.19 1.08 -12 -3 -1 27.92 2.39 -12 -3 -2 0.30 0.68 -12 -3 -2 0.95 0.90 -12 -3 -3 3.48 0.99 -12 -3 -4 0.53 0.53 -12 -4 6 11.79 1.38 -12 -4 5 61.65 3.44 -12 -4 5 55.11 3.31 -12 -4 4 0.70 0.78 -12 -4 4 1.47 0.70 -12 -4 4 1.41 0.80 -12 -4 3 2.94 1.08 -12 -4 3 2.56 0.98 -12 -4 2 109.90 5.25 -12 -4 2 109.89 5.26 -12 -4 1 9.95 1.51 -12 -4 1 9.49 1.55 -12 -4 0 13.96 1.64 -12 -4 0 18.83 2.02 -12 -4 -1 1.10 0.73 -12 -4 -1 0.53 0.75 -12 -4 -2 0.31 0.70 -12 -4 -3 18.84 1.67 -12 -5 4 1.48 0.73 -12 -5 3 7.79 1.18 -12 -5 3 5.58 1.02 -12 -5 2 18.21 1.73 -12 -5 2 14.15 1.40 -12 -5 2 16.97 1.70 -12 -5 1 5.98 0.99 -12 -5 1 6.01 1.19 -12 -5 0 8.59 1.25 -12 -5 -1 13.14 1.42 -13 0 6 53.87 2.73 -13 0 5 -0.47 0.60 -13 0 4 3.20 0.81 -13 0 3 -0.11 0.55 -13 0 3 -0.42 0.64 -13 0 2 36.65 2.52 -13 0 1 -0.30 0.74 -13 0 0 2.58 0.86 -13 0 -1 -0.13 0.57 -13 1 6 0.39 0.47 -13 -1 5 51.71 2.71 -13 1 5 55.14 2.82 -13 -1 4 38.09 2.25 -13 1 4 34.34 2.23 -13 1 3 20.19 1.61 -13 -1 3 22.96 1.93 -13 1 3 23.12 1.84 -13 -1 2 58.34 3.28 -13 -1 1 20.38 1.85 -13 -1 0 28.91 2.17 -13 2 5 28.78 1.83 -13 2 4 4.13 0.76 -13 -2 3 30.04 2.13 -13 -2 2 3.86 0.93 -13 -2 1 39.56 2.47 -13 -2 0 56.89 3.06 0 0 0 0.00 0.00 TITL nifedipine 4 deg known_auto in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 10.671251 10.397115 14.782356 90.0000 94.5450 90.0000 ZERR 31.00 0.000264 0.000254 0.000335 0.0000 0.0021 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 31.00 31.00 31.00 31.00 REM CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0 TEMP -123 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 57855 _olex2_exptl_crystal_mounting_method ; 'Crystal mounted using inert oil from the encapsulation crystallisation technique onto a MiTeGen Kapton micromount.' ; _olex2_submission_original_sample_id Nifedipine _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 1.158 _oxdiff_exptl_absorpt_empirical_full_min 0.831 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' 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 O1 O 0.85954(10) 0.63108(10) 0.47502(7) 0.0328(3) Uani 1 1 d . . . . . O6 O 0.45792(10) 0.21795(10) 0.53439(7) 0.0338(3) Uani 1 1 d . . . . . O5 O 0.36857(10) 0.26642(11) 0.66224(7) 0.0334(3) Uani 1 1 d . . . . . O3 O 0.65613(12) 0.19754(11) 0.39751(7) 0.0399(3) Uani 1 1 d . . . . . O2 O 0.82414(12) 0.42879(11) 0.43097(7) 0.0414(3) Uani 1 1 d . . . . . O4 O 0.84788(14) 0.13828(13) 0.38513(8) 0.0497(3) Uani 1 1 d . . . . . N2 N 0.76153(13) 0.17068(12) 0.43054(8) 0.0312(3) Uani 1 1 d . . . . . N1 N 0.64230(12) 0.56579(12) 0.69498(9) 0.0301(3) Uani 1 1 d . . . . . C3 C 0.73353(13) 0.49897(13) 0.56229(9) 0.0242(3) Uani 1 1 d . . . . . C16 C 0.44858(13) 0.28883(14) 0.60949(10) 0.0262(3) Uani 1 1 d . . . . . C4 C 0.73096(13) 0.58171(13) 0.63269(9) 0.0262(3) Uani 1 1 d . . . . . C8 C 0.54623(13) 0.38756(14) 0.61863(9) 0.0248(3) Uani 1 1 d . . . . . C9 C 0.65446(13) 0.37656(13) 0.55752(9) 0.0236(3) Uani 1 1 d . . . . . H9 H 0.619027 0.363525 0.493509 0.028 Uiso 1 1 calc R U . . . C11 C 0.78761(13) 0.16916(14) 0.52987(9) 0.0262(3) Uani 1 1 d . . . . . C15 C 0.77366(13) 0.24627(14) 0.67908(9) 0.0272(3) Uani 1 1 d . . . . . H15 H 0.744527 0.307489 0.720271 0.033 Uiso 1 1 calc R U . . . C2 C 0.81064(13) 0.51403(13) 0.48486(9) 0.0255(3) Uani 1 1 d . . . . . C10 C 0.73771(13) 0.26035(13) 0.58646(9) 0.0237(3) Uani 1 1 d . . . . . C6 C 0.54515(13) 0.47827(14) 0.68418(9) 0.0279(3) Uani 1 1 d . . . . . C13 C 0.89548(14) 0.05700(14) 0.65474(11) 0.0314(3) Uani 1 1 d . . . . . H13 H 0.946863 -0.012048 0.677787 0.038 Uiso 1 1 calc R U . . . C14 C 0.84986(14) 0.14695(15) 0.71323(10) 0.0301(3) Uani 1 1 d . . . . . H14 H 0.870916 0.140379 0.776715 0.036 Uiso 1 1 calc R U . . . C12 C 0.86516(14) 0.06923(14) 0.56261(10) 0.0297(3) Uani 1 1 d . . . . . H12 H 0.897210 0.009494 0.521631 0.036 Uiso 1 1 calc R U . . . C5 C 0.81733(16) 0.69340(15) 0.65628(11) 0.0356(4) Uani 1 1 d . . . . . H5A H 0.772323 0.774210 0.642974 0.053 Uiso 1 1 calc R U . . . H5B H 0.890413 0.688560 0.620244 0.053 Uiso 1 1 calc R U . . . H5C H 0.845456 0.690088 0.720979 0.053 Uiso 1 1 calc R U . . . C7 C 0.44587(15) 0.49585(18) 0.74968(11) 0.0379(4) Uani 1 1 d . . . . . H7A H 0.454225 0.428285 0.795995 0.057 Uiso 1 1 calc R U . . . H7B H 0.362529 0.490500 0.716918 0.057 Uiso 1 1 calc R U . . . H7C H 0.456080 0.580234 0.778879 0.057 Uiso 1 1 calc R U . . . C1 C 0.92656(16) 0.64730(17) 0.39480(11) 0.0371(4) Uani 1 1 d . . . . . H1A H 0.868971 0.633156 0.340728 0.056 Uiso 1 1 calc R U . . . H1B H 0.995572 0.585019 0.395653 0.056 Uiso 1 1 calc R U . . . H1C H 0.960662 0.734738 0.393530 0.056 Uiso 1 1 calc R U . . . C17 C 0.36795(16) 0.11599(17) 0.52002(13) 0.0398(4) Uani 1 1 d . . . . . H17A H 0.377694 0.075332 0.461178 0.060 Uiso 1 1 calc R U . . . H17B H 0.282802 0.151111 0.520683 0.060 Uiso 1 1 calc R U . . . H17C H 0.381888 0.051891 0.568372 0.060 Uiso 1 1 calc R U . . . H1 H 0.6404(17) 0.6220(19) 0.7408(12) 0.036(5) 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 O1 0.0413(6) 0.0260(5) 0.0324(6) 0.0003(4) 0.0103(5) -0.0103(4) O6 0.0340(6) 0.0301(6) 0.0379(6) -0.0060(4) 0.0064(4) -0.0091(4) O5 0.0306(6) 0.0342(6) 0.0362(6) 0.0061(5) 0.0077(4) -0.0037(4) O3 0.0494(7) 0.0364(6) 0.0329(6) -0.0045(5) -0.0024(5) -0.0033(5) O2 0.0658(8) 0.0269(6) 0.0345(6) -0.0036(5) 0.0225(5) -0.0065(5) O4 0.0665(8) 0.0501(8) 0.0351(6) -0.0026(5) 0.0195(6) 0.0162(6) N2 0.0442(8) 0.0215(6) 0.0285(6) -0.0041(5) 0.0075(5) -0.0021(5) N1 0.0334(7) 0.0290(6) 0.0285(6) -0.0085(5) 0.0069(5) -0.0030(5) C3 0.0265(7) 0.0203(6) 0.0259(7) 0.0012(5) 0.0026(5) -0.0006(5) C16 0.0250(7) 0.0241(7) 0.0294(7) 0.0046(6) 0.0014(5) 0.0025(5) C4 0.0281(7) 0.0226(7) 0.0277(7) -0.0001(5) 0.0024(5) -0.0001(5) C8 0.0244(7) 0.0249(7) 0.0252(7) 0.0026(5) 0.0027(5) 0.0001(5) C9 0.0273(7) 0.0208(6) 0.0232(6) -0.0002(5) 0.0039(5) -0.0028(5) C11 0.0298(7) 0.0221(7) 0.0270(7) 0.0000(5) 0.0052(5) -0.0056(5) C15 0.0284(7) 0.0270(7) 0.0269(7) 0.0003(6) 0.0057(5) -0.0027(6) C2 0.0293(7) 0.0222(7) 0.0250(6) 0.0022(5) 0.0012(5) -0.0013(5) C10 0.0242(6) 0.0206(6) 0.0268(7) 0.0008(5) 0.0056(5) -0.0054(5) C6 0.0277(7) 0.0289(7) 0.0274(7) -0.0006(6) 0.0037(5) 0.0014(6) C13 0.0279(7) 0.0243(7) 0.0422(8) 0.0066(6) 0.0042(6) -0.0012(6) C14 0.0296(7) 0.0323(8) 0.0288(7) 0.0067(6) 0.0041(6) -0.0042(6) C12 0.0308(7) 0.0209(7) 0.0382(8) -0.0031(6) 0.0078(6) -0.0034(6) C5 0.0433(9) 0.0283(8) 0.0357(8) -0.0072(6) 0.0054(7) -0.0085(7) C7 0.0334(8) 0.0438(9) 0.0380(8) -0.0095(7) 0.0119(6) -0.0010(7) C1 0.0376(8) 0.0384(9) 0.0365(8) 0.0052(7) 0.0107(7) -0.0112(7) C17 0.0369(9) 0.0318(8) 0.0506(10) -0.0064(7) 0.0021(7) -0.0107(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 O1 C1 114.79(11) . . ? C16 O6 C17 115.81(12) . . ? O3 N2 O4 123.38(13) . . ? O3 N2 C11 119.73(12) . . ? O4 N2 C11 116.80(13) . . ? C4 N1 H1 118.9(12) . . ? C6 N1 C4 123.38(12) . . ? C6 N1 H1 117.1(12) . . ? C4 C3 C9 121.43(12) . . ? C4 C3 C2 125.33(13) . . ? C2 C3 C9 113.24(11) . . ? O6 C16 C8 111.27(12) . . ? O5 C16 O6 121.58(13) . . ? O5 C16 C8 127.12(14) . . ? N1 C4 C5 112.14(12) . . ? C3 C4 N1 119.57(13) . . ? C3 C4 C5 128.26(13) . . ? C16 C8 C9 117.41(12) . . ? C6 C8 C16 120.62(12) . . ? C6 C8 C9 121.74(12) . . ? C3 C9 C8 110.61(11) . . ? C3 C9 H9 108.8 . . ? C3 C9 C10 109.69(11) . . ? C8 C9 H9 108.8 . . ? C8 C9 C10 109.95(11) . . ? C10 C9 H9 108.8 . . ? C10 C11 N2 122.60(13) . . ? C12 C11 N2 114.52(13) . . ? C12 C11 C10 122.88(13) . . ? C10 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C14 C15 C10 122.82(13) . . ? O1 C2 C3 115.41(12) . . ? O2 C2 O1 121.89(13) . . ? O2 C2 C3 122.60(13) . . ? C11 C10 C9 127.21(12) . . ? C11 C10 C15 115.26(13) . . ? C15 C10 C9 117.46(12) . . ? N1 C6 C7 114.04(13) . . ? C8 C6 N1 119.59(12) . . ? C8 C6 C7 126.37(14) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C12 C13 C14 119.09(14) . . ? C15 C14 C13 120.02(14) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C11 C12 H12 120.1 . . ? C13 C12 C11 119.90(14) . . ? C13 C12 H12 120.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O6 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? O6 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 O1 C2 1.3367(17) . ? O1 C1 1.4423(18) . ? O6 C16 1.3428(18) . ? O6 C17 1.4347(19) . ? O5 C16 1.2235(17) . ? O3 N2 1.2224(18) . ? O2 C2 1.2079(18) . ? O4 N2 1.2293(17) . ? N2 C11 1.4727(18) . ? N1 C4 1.3813(18) . ? N1 C6 1.3791(19) . ? N1 H1 0.90(2) . ? C3 C4 1.3522(19) . ? C3 C9 1.5255(19) . ? C3 C2 1.4700(19) . ? C16 C8 1.461(2) . ? C4 C5 1.506(2) . ? C8 C9 1.5259(18) . ? C8 C6 1.353(2) . ? C9 H9 1.0000 . ? C9 C10 1.5401(19) . ? C11 C10 1.397(2) . ? C11 C12 1.391(2) . ? C15 H15 0.9500 . ? C15 C10 1.3999(19) . ? C15 C14 1.385(2) . ? C6 C7 1.502(2) . ? C13 H13 0.9500 . ? C13 C14 1.388(2) . ? C13 C12 1.381(2) . ? C14 H14 0.9500 . ? C12 H12 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 O6 C16 C8 C9 -12.76(17) . . . . ? O6 C16 C8 C6 172.67(13) . . . . ? O5 C16 C8 C9 165.21(13) . . . . ? O5 C16 C8 C6 -9.4(2) . . . . ? O3 N2 C11 C10 -39.42(19) . . . . ? O3 N2 C11 C12 140.19(14) . . . . ? O4 N2 C11 C10 143.90(14) . . . . ? O4 N2 C11 C12 -36.49(18) . . . . ? N2 C11 C10 C9 -2.3(2) . . . . ? N2 C11 C10 C15 -178.94(12) . . . . ? N2 C11 C12 C13 -179.43(13) . . . . ? C3 C9 C10 C11 -101.87(15) . . . . ? C3 C9 C10 C15 74.66(15) . . . . ? C16 C8 C9 C3 169.12(11) . . . . ? C16 C8 C9 C10 -69.58(15) . . . . ? C16 C8 C6 N1 176.15(13) . . . . ? C16 C8 C6 C7 -3.9(2) . . . . ? C4 N1 C6 C8 11.8(2) . . . . ? C4 N1 C6 C7 -168.13(14) . . . . ? C4 C3 C9 C8 20.26(18) . . . . ? C4 C3 C9 C10 -101.19(15) . . . . ? C4 C3 C2 O1 -15.0(2) . . . . ? C4 C3 C2 O2 168.53(15) . . . . ? C8 C9 C10 C11 136.28(14) . . . . ? C8 C9 C10 C15 -47.19(16) . . . . ? C9 C3 C4 N1 -9.5(2) . . . . ? C9 C3 C4 C5 168.72(14) . . . . ? C9 C3 C2 O1 165.78(12) . . . . ? C9 C3 C2 O2 -10.7(2) . . . . ? C9 C8 C6 N1 1.8(2) . . . . ? C9 C8 C6 C7 -178.24(14) . . . . ? C2 C3 C4 N1 171.37(13) . . . . ? C2 C3 C4 C5 -10.4(2) . . . . ? C2 C3 C9 C8 -160.50(11) . . . . ? C2 C3 C9 C10 78.04(14) . . . . ? C10 C11 C12 C13 0.2(2) . . . . ? C10 C15 C14 C13 0.9(2) . . . . ? C6 N1 C4 C3 -7.9(2) . . . . ? C6 N1 C4 C5 173.64(14) . . . . ? C6 C8 C9 C3 -16.38(18) . . . . ? C6 C8 C9 C10 104.92(15) . . . . ? C14 C15 C10 C9 -178.99(13) . . . . ? C14 C15 C10 C11 -2.0(2) . . . . ? C14 C13 C12 C11 -1.4(2) . . . . ? C12 C11 C10 C9 178.08(13) . . . . ? C12 C11 C10 C15 1.5(2) . . . . ? C12 C13 C14 C15 0.9(2) . . . . ? C1 O1 C2 O2 1.2(2) . . . . ? C1 O1 C2 C3 -175.29(12) . . . . ? C17 O6 C16 O5 0.5(2) . . . . ? C17 O6 C16 C8 178.62(12) . . . . ?