#------------------------------------------------------------------------------ #$Date: 2023-12-22 05:01:42 +0200 (Fri, 22 Dec 2023) $ #$Revision: 288500 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312374.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_2312374 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_paper_doi 10.1107/S2052520623010053 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'C21 H26 N2 O7' _chemical_formula_sum 'C21 H26 N2 O7' _chemical_formula_weight 418.44 _chemical_name_common nimodipine _chemical_name_systematic ; (rac)-3-isopropyl 5-(2-methoxyethyl) 2,6-dimethyl-4-(3-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 104.604(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8103(2) _cell_length_b 10.7631(2) _cell_length_c 14.8187(3) _cell_measurement_reflns_used 7193 _cell_measurement_temperature 149.99(10) _cell_measurement_theta_max 77.0250 _cell_measurement_theta_min 3.3000 _cell_volume 2131.51(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 149.99(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 0.998 _diffrn_measured_fraction_theta_max 0.929 _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 -75.00 -13.00 0.50 0.44 -- -45.34 125.00-120.00 124 2 \w -46.00 -11.00 0.50 0.44 -- -85.06 61.00 -60.00 70 3 \w -45.00 -16.00 0.50 0.44 -- -85.06 61.00 60.00 58 4 \w -46.00 -15.00 0.50 0.44 -- -85.06 61.00 30.00 62 5 \w -44.00 -18.00 0.50 0.44 -- -85.06 61.00 90.00 52 6 \w -36.00 -9.00 0.50 0.44 -- -85.06 56.00 123.00 54 7 \w -153.00 -83.00 0.50 0.44 -- -85.06 -56.00 -18.00 140 8 \w -146.00-106.00 0.50 0.44 -- -85.06 -77.00 60.00 80 9 \w 57.00 140.00 0.50 0.44 -- 100.34 15.00 90.00 166 10 \w 141.00 170.00 0.50 0.44 -- 109.85 56.00 123.00 58 11 \w 108.00 135.00 0.50 0.44 -- 109.85 56.00 123.00 54 12 \w 116.00 141.00 0.50 0.44 -- 100.34 56.00 123.00 50 13 \w 121.00 166.00 0.50 0.44 -- 109.85 45.00 30.00 90 14 \w 10.00 48.00 0.50 0.44 -- 46.34 -56.00 -18.00 76 15 \w 27.00 53.00 0.50 0.44 -- 100.34 -61.00 -90.00 52 16 \w 26.00 54.00 0.50 0.44 -- 100.34 -61.00-120.00 56 17 \w 29.00 56.00 0.50 0.44 -- 100.34 -61.00 -60.00 54 18 \w 34.00 79.00 0.50 0.44 -- 100.34 -77.00 0.00 90 19 \w 26.00 55.00 0.50 0.44 -- 100.34 -61.00-150.00 58 20 \w 29.00 54.00 0.50 0.44 -- 100.34 -61.00 60.00 50 21 \w 42.00 80.00 0.50 0.44 -- 109.85 -77.00 120.00 76 22 \w 26.00 51.00 0.50 0.44 -- 100.34 -61.00 90.00 50 23 \w 26.00 51.00 0.50 0.44 -- 100.34 -61.00 120.00 50 24 \w 37.00 74.00 0.50 0.44 -- 46.34-125.00 150.00 74 25 \w 48.00 100.00 0.50 0.44 -- 109.85-125.00 -30.00 104 26 \w -37.00 28.00 0.50 0.44 -- -45.34 56.00 123.00 130 27 \w -3.00 24.00 0.50 0.44 -- -45.34 38.00-150.00 54 28 \w -13.00 32.00 0.50 0.44 -- -45.34 38.00-180.00 90 ; _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 -0.1004328000 _diffrn_orient_matrix_UB_12 0.0579634000 _diffrn_orient_matrix_UB_13 0.0053875000 _diffrn_orient_matrix_UB_21 -0.0027200000 _diffrn_orient_matrix_UB_22 0.0761067000 _diffrn_orient_matrix_UB_23 -0.0887034000 _diffrn_orient_matrix_UB_31 -0.0565374000 _diffrn_orient_matrix_UB_32 -0.1064083000 _diffrn_orient_matrix_UB_33 -0.0603711000 _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 0.0302 _diffrn_reflns_av_unetI/netI 0.0285 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.929 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 14528 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.262 _diffrn_reflns_theta_min 3.307 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78820 _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 1.304 _exptl_crystal_description block _exptl_crystal_F_000 888 _exptl_crystal_preparation 'Crystallised from a saturated solution of nimodipine in MeNO2.' _exptl_crystal_recrystallization_method 'High-throughput screening via the ENaCt protocol using SPT Labtech mosquito.' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.289 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 4200 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0416 _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^)+(0.0572P)^2^+0.6851P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.1191 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3488 _reflns_number_total 4200 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file rm5073sup1.cif _cod_data_source_block nimodipine _cod_database_code 2312374 _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. ; _shelx_estimated_absorpt_t_max 0.945 _shelx_estimated_absorpt_t_min 0.661 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C11(H11), C19(H19) 2.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C2(H2A,H2B) 2.c Aromatic/amide H refined with riding coordinates: C17(H17), C13(H13), C15(H15), C16(H16) 2.d Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C) ; _shelx_res_file ; TITL nimodipine_auto_a.res in P2(1)/c nimodipine.res created by SHELXL-2018/3 at 11:32:20 on 11-May-2023 REM Old TITL nimodipine_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.159, Rweak 0.027, Alpha 0.021 REM 0.362 for 240 systematic absences, Orientation as input REM Formula found by SHELXT: C22 N2 O6 CELL 1.54184 13.8103 10.7631 14.8187 90 104.604 90 ZERR 4 0.0002 0.0002 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 84 104 8 28 L.S. 4 PLAN 1 SIZE 0.07 0.55 0.52 TEMP -123 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.057200 0.685100 FVAR 0.42827 O2 4 0.733654 0.775024 0.365841 11.00000 0.03631 0.02659 = 0.03629 -0.00005 0.01181 -0.00054 O7 4 0.826099 0.360197 0.429200 11.00000 0.03053 0.02733 = 0.05078 0.00425 0.00497 0.00291 O1 4 0.720785 0.894924 0.189326 11.00000 0.03190 0.05715 = 0.02820 0.00280 0.00825 0.00406 O6 4 0.720990 0.200914 0.426894 11.00000 0.04026 0.02854 = 0.06922 0.01202 0.00208 -0.00132 O3 4 0.581917 0.851522 0.363924 11.00000 0.03714 0.02865 = 0.07894 -0.00609 0.00942 0.00451 N1 3 0.487439 0.471318 0.351034 11.00000 0.02754 0.03281 = 0.03257 0.00021 0.00610 -0.00113 O5 4 0.948262 0.533206 0.085217 11.00000 0.06848 0.06121 = 0.06134 -0.01033 0.04480 -0.01024 N2 3 0.929449 0.551858 0.160486 11.00000 0.04271 0.05086 = 0.04894 -0.00029 0.02207 0.00126 C12 1 0.711278 0.527836 0.264530 11.00000 0.03255 0.02090 = 0.02478 0.00078 0.00725 0.00231 O4 4 0.992826 0.586951 0.229280 11.00000 0.03603 0.13913 = 0.05649 -0.00611 0.01572 -0.00462 C11 1 0.687547 0.534176 0.359835 11.00000 0.02803 0.02524 = 0.02284 -0.00043 0.00441 0.00148 AFIX 13 H11 2 0.749808 0.558961 0.407283 11.00000 -1.20000 AFIX 0 C10 1 0.655723 0.405976 0.385871 11.00000 0.03222 0.02647 = 0.02254 0.00063 0.00446 0.00074 C5 1 0.606874 0.630790 0.360271 11.00000 0.03192 0.02739 = 0.02050 0.00029 0.00485 0.00212 C8 1 0.558179 0.378559 0.375483 11.00000 0.03423 0.02927 = 0.02203 0.00068 0.00518 -0.00063 C6 1 0.510198 0.595637 0.350184 11.00000 0.03295 0.03030 = 0.02361 -0.00038 0.00554 0.00295 C17 1 0.636004 0.500655 0.184782 11.00000 0.03482 0.02617 = 0.02899 -0.00107 0.00655 -0.00168 AFIX 43 H17 2 0.569317 0.489564 0.189801 11.00000 -1.20000 AFIX 0 C13 1 0.807938 0.545811 0.256000 11.00000 0.03138 0.02944 = 0.02947 0.00074 0.00651 0.00191 AFIX 43 H13 2 0.860407 0.566069 0.309002 11.00000 -1.20000 AFIX 0 C3 1 0.771160 0.897916 0.355351 11.00000 0.04126 0.02880 = 0.03288 -0.00273 0.00673 -0.00507 AFIX 23 H3A 2 0.827931 0.917329 0.409227 11.00000 -1.20000 H3B 2 0.717868 0.960161 0.353287 11.00000 -1.20000 AFIX 0 C18 1 0.733779 0.310537 0.415618 11.00000 0.03470 0.02915 = 0.02830 0.00255 0.00314 -0.00115 C14 1 0.826864 0.533724 0.168675 11.00000 0.03865 0.03190 = 0.03783 -0.00003 0.01635 0.00198 C4 1 0.635190 0.762639 0.363507 11.00000 0.03188 0.03050 = 0.02453 -0.00127 0.00343 0.00372 C9 1 0.513191 0.255119 0.388971 11.00000 0.03822 0.03392 = 0.03725 0.00275 0.00784 -0.00615 AFIX 137 H9A 2 0.506691 0.248754 0.453154 11.00000 -1.50000 H9B 2 0.556547 0.188294 0.377047 11.00000 -1.50000 H9C 2 0.446968 0.247728 0.345519 11.00000 -1.50000 AFIX 0 C15 1 0.753408 0.504709 0.089575 11.00000 0.05514 0.03449 = 0.02973 -0.00369 0.01763 -0.00268 AFIX 43 H15 2 0.768775 0.495451 0.030956 11.00000 -1.20000 AFIX 0 C2 1 0.804936 0.903335 0.266835 11.00000 0.02942 0.03948 = 0.03704 0.00253 0.00647 -0.00405 AFIX 23 H2A 2 0.840774 0.982355 0.264093 11.00000 -1.20000 H2B 2 0.851524 0.833922 0.265282 11.00000 -1.20000 AFIX 0 C16 1 0.656639 0.489480 0.098134 11.00000 0.04713 0.03476 = 0.02639 -0.00295 0.00594 -0.00511 AFIX 43 H16 2 0.604177 0.471332 0.044604 11.00000 -1.20000 AFIX 0 C7 1 0.419931 0.678062 0.337353 11.00000 0.03209 0.03822 = 0.04285 -0.00048 0.00959 0.00546 AFIX 137 H7A 2 0.362055 0.637071 0.296133 11.00000 -1.50000 H7B 2 0.432729 0.757019 0.309514 11.00000 -1.50000 H7C 2 0.406135 0.693854 0.398042 11.00000 -1.50000 AFIX 0 C19 1 0.911151 0.277242 0.463636 11.00000 0.03372 0.02696 = 0.07979 0.00414 0.00363 0.00561 AFIX 13 H19 2 0.894395 0.191977 0.437557 11.00000 -1.20000 AFIX 0 C1 1 0.748297 0.889218 0.103383 11.00000 0.05434 0.08634 = 0.03412 0.00580 0.01901 0.00853 AFIX 137 H1A 2 0.687857 0.886017 0.051803 11.00000 -1.50000 H1B 2 0.788617 0.814592 0.102205 11.00000 -1.50000 H1C 2 0.787415 0.963104 0.096793 11.00000 -1.50000 AFIX 0 C20 1 0.933314 0.273111 0.568782 11.00000 0.05904 0.05320 = 0.07506 0.01057 -0.02251 0.00288 AFIX 137 H20A 2 0.950181 0.356742 0.594017 11.00000 -1.50000 H20B 2 0.989841 0.217151 0.593140 11.00000 -1.50000 H20C 2 0.874293 0.242763 0.587387 11.00000 -1.50000 AFIX 0 C21 1 0.995912 0.329974 0.428927 11.00000 0.04239 0.04425 = 0.14409 0.00780 0.03042 0.00692 AFIX 137 H21A 2 0.977982 0.328895 0.360593 11.00000 -1.50000 H21B 2 1.056150 0.279719 0.452565 11.00000 -1.50000 H21C 2 1.008851 0.415681 0.451000 11.00000 -1.50000 AFIX 0 H1 2 0.423152 0.449366 0.338351 11.00000 0.04276 HKLF 4 REM nimodipine_auto_a.res in P2(1)/c REM wR2 = 0.1191, GooF = S = 1.051, Restrained GooF = 1.051 for all data REM R1 = 0.0416 for 3488 Fo > 4sig(Fo) and 0.0496 for all 4200 data REM 280 parameters refined using 0 restraints END WGHT 0.0572 0.6851 REM Highest difference peak 0.289, deepest hole -0.242, 1-sigma level 0.040 Q1 1 0.4366 0.7602 0.3727 11.00000 0.05 0.29 ; _shelx_res_checksum 45576 _shelx_hkl_file ; 0 0 -1 0.88 0.13 0 0 -2 552.47 16.35 0 0 -3 -0.03 0.31 0 0 -4 9999.00 291.26 0 0 -5 0.06 0.39 0 0 -6 493.87 15.32 0 0 -7 -0.29 0.47 0 0 -8 185.96 6.81 0 0 -8 188.47 6.82 0 0 -9 -0.13 0.53 0 0 -9 0.41 0.56 0 0 -10 218.55 8.10 0 0 -10 206.38 8.07 0 0 10 217.96 7.66 0 0 -11 -0.18 0.57 0 0 -11 0.36 0.69 0 0 -12 61.18 3.59 0 0 -12 64.06 3.65 0 0 -12 60.37 3.43 0 0 -13 -0.17 0.56 0 0 -13 -0.21 0.72 0 0 -13 -0.18 0.70 0 0 -13 -0.84 0.73 0 0 -14 24.09 2.22 0 0 -15 -0.63 0.69 0 0 -15 0.33 0.76 0 0 -16 -0.14 0.59 0 0 -16 -0.13 0.54 0 0 -16 0.14 0.51 0 0 -17 -0.39 0.39 0 -1 0 0.11 0.11 0 -1 -1 37.43 1.22 0 -1 -1 37.68 1.23 0 1 -1 37.83 1.23 0 -1 -1 38.35 1.23 0 -1 -1 35.86 1.27 0 1 -2 97.15 3.17 0 -1 -2 101.57 3.17 0 -1 -2 98.64 3.13 0 1 -3 15.74 0.83 0 -1 -3 14.50 0.81 0 1 -4 1964.34 56.94 0 -1 -4 1911.04 56.92 0 -1 -5 37.46 1.77 0 1 -5 38.64 1.78 0 1 -6 683.69 20.71 0 -1 -6 673.15 20.70 0 1 -7 169.07 6.03 0 -1 -7 165.69 6.00 0 -1 -8 493.51 15.63 0 1 -8 478.02 15.60 0 -1 -8 485.68 15.59 0 1 -8 496.73 15.64 0 1 -9 1.08 0.63 0 -1 -9 -0.40 0.56 0 -1 -9 0.41 0.50 0 1 -9 0.27 0.53 0 -1 9 -0.34 0.47 0 -1 10 160.33 6.19 0 1 -10 169.31 6.52 0 -1 -10 164.94 6.46 0 -1 -10 164.48 6.50 0 1 -10 160.09 6.48 0 -1 -10 155.94 6.30 0 -1 11 103.85 4.52 0 -1 -11 100.01 4.58 0 -1 -11 101.39 4.80 0 1 -11 96.50 4.69 0 -1 -11 97.32 4.74 0 1 -11 97.44 4.72 0 -1 -11 108.66 4.71 0 -1 12 185.39 7.11 0 -1 -12 182.65 7.25 0 -1 -12 179.76 7.43 0 1 -12 192.51 7.55 0 1 -12 182.99 7.47 0 -1 -12 168.58 7.35 0 -1 -12 186.72 7.33 0 -1 -13 5.96 1.10 0 1 -13 6.34 1.22 0 -1 -13 6.17 1.24 0 1 -13 5.18 1.13 0 -1 -13 6.46 1.26 0 -1 -13 6.24 1.26 0 1 -13 5.50 1.12 0 1 -14 -0.20 0.74 0 -1 -14 0.40 0.70 0 -1 -14 0.50 0.60 0 1 -15 31.47 2.27 0 -1 -15 29.90 2.14 0 -1 -15 29.56 2.27 0 1 -15 30.51 2.20 0 -1 -15 33.45 2.31 0 1 -16 24.33 1.83 0 -1 -16 24.39 1.73 0 1 -16 26.17 1.87 0 -1 -16 28.82 1.95 0 1 -16 26.45 1.89 0 1 -17 0.86 0.46 0 -1 -17 0.74 0.42 0 -2 0 830.95 24.47 0 -2 -1 288.07 8.54 0 -2 -1 287.02 8.52 0 -2 -1 286.17 8.45 0 2 -1 279.61 8.45 0 -2 -1 298.90 8.70 0 -2 1 284.18 8.63 0 -2 -1 287.97 8.65 0 -2 -2 2701.49 78.14 0 -2 -2 2693.47 78.15 0 2 -2 2622.95 78.14 0 -2 -2 2719.06 78.29 0 -2 -2 2666.81 78.24 0 2 -3 1392.18 40.64 0 -2 -3 1407.16 40.64 0 -2 -3 1361.09 40.71 0 -2 -3 1368.44 40.59 0 2 -4 92.89 3.27 0 -2 -4 94.69 3.28 0 -2 -4 89.53 3.26 0 2 -5 6.13 0.71 0 -2 -5 6.93 0.72 0 -2 -5 5.60 0.62 0 -2 -6 23.15 1.44 0 2 -6 23.77 1.48 0 -2 -6 26.89 1.45 0 2 -7 67.42 3.04 0 -2 -7 70.17 3.04 0 -2 -8 7.82 0.93 0 -2 -8 7.17 0.93 0 2 -8 6.34 0.95 0 2 -8 6.40 0.94 0 -2 -8 8.14 0.99 0 -2 -8 7.22 0.91 0 -2 -9 26.71 1.79 0 -2 9 24.60 1.77 0 -2 -9 23.16 1.75 0 -2 -9 22.57 1.78 0 2 -9 22.49 1.75 0 -2 -9 23.42 1.81 0 2 -9 23.64 1.83 0 -2 -10 1.87 0.65 0 -2 -10 1.27 0.65 0 2 -10 0.95 0.64 0 2 -10 1.26 0.73 0 -2 -10 1.41 0.64 0 -2 10 1.44 0.69 0 -2 -10 2.11 0.78 0 2 -11 137.03 5.92 0 -2 -11 133.71 5.91 0 -2 11 137.04 5.76 0 -2 -11 151.40 5.93 0 -2 -11 127.83 5.84 0 2 -11 143.33 5.97 0 -2 -11 140.60 5.90 0 2 -12 125.56 5.73 0 -2 -12 132.03 5.79 0 -2 12 128.75 5.52 0 -2 -12 119.31 5.61 0 -2 -12 127.46 5.71 0 2 -12 126.37 5.76 0 -2 -12 130.40 5.62 0 -2 -13 5.25 1.08 0 2 -13 5.23 1.07 0 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1 -3 1.54 0.71 14 -1 4 1.17 0.45 -14 1 -4 1.78 0.65 -14 -1 -4 2.24 0.68 -14 1 -4 1.28 0.55 -14 1 -5 7.63 0.87 -14 -1 -5 10.92 1.13 -14 -1 -6 4.10 0.65 -14 -2 14 0.17 0.28 -14 2 13 3.42 0.64 -14 -2 13 3.28 0.65 -14 2 12 1.57 0.68 -14 -2 12 1.49 0.63 -14 -2 11 11.17 1.03 -14 -2 11 11.71 1.29 -14 2 11 12.74 1.35 14 -2 -11 14.43 1.32 14 2 -11 11.68 1.23 -14 2 10 0.16 0.66 -14 -2 10 -0.15 0.64 14 -2 -10 0.15 0.54 14 2 -10 -0.44 0.65 -14 -2 10 0.11 0.44 -14 2 9 15.49 1.62 -14 -2 9 13.28 1.51 14 -2 -9 10.96 1.37 14 2 -9 12.54 1.49 -14 -2 9 13.01 1.31 -14 -2 8 3.34 0.83 14 -2 -8 2.77 0.84 14 2 -8 3.66 0.97 -14 2 8 1.63 0.84 -14 -2 8 4.84 1.07 14 -2 -7 1.27 0.73 14 2 -7 1.47 0.81 -14 -2 7 0.74 0.61 14 -2 -6 17.27 1.81 14 2 -6 18.04 1.82 -14 -2 6 16.25 1.60 14 -2 -5 38.51 2.81 14 2 -5 47.42 3.04 -14 -2 5 40.56 2.62 -14 2 5 41.40 2.90 -14 -2 5 43.36 2.97 14 -2 -4 25.93 2.30 14 2 -4 28.99 2.41 -14 -2 4 28.88 2.16 -14 2 4 25.03 2.30 -14 -2 4 29.38 2.46 14 -2 -3 -0.19 1.00 14 2 -3 -0.59 0.94 -14 -2 3 0.81 0.61 -14 2 3 1.39 0.65 -14 2 3 0.20 0.98 -14 -2 3 -1.62 1.29 14 -2 -2 -0.96 1.03 14 2 -2 0.59 0.86 -14 2 2 1.62 0.67 -14 2 1 0.27 0.57 -14 -2 0 0.89 0.73 -14 2 0 0.78 0.55 -14 -2 -1 2.22 0.80 -14 2 -1 2.18 0.79 -14 2 -1 2.40 0.69 14 -2 1 2.85 0.86 -14 -2 -2 48.53 2.94 -14 2 -2 51.07 2.85 14 -2 2 46.47 2.79 14 -2 3 0.37 0.48 -14 -2 -3 0.29 0.62 -14 2 -3 -0.12 0.50 -14 2 -3 0.54 0.52 14 -2 4 1.18 0.54 -14 2 -4 3.09 0.60 -14 -2 -4 3.26 0.80 -14 2 -4 3.39 0.66 -14 -2 -5 7.88 0.97 -14 -2 -6 24.87 1.45 -14 3 13 4.16 0.53 -14 3 12 19.85 1.33 -14 -3 12 22.06 1.43 -14 -3 12 18.35 1.19 -14 3 11 3.65 0.76 -14 -3 11 3.09 0.73 -14 -3 11 3.22 0.61 -14 3 10 3.27 0.80 -14 -3 10 2.81 0.77 -14 -3 10 1.78 0.59 14 -3 -10 2.25 0.67 14 3 -10 3.32 0.75 -14 3 9 2.35 0.77 -14 -3 9 3.12 0.83 -14 -3 9 2.66 0.70 14 -3 -9 2.67 0.70 14 3 -9 2.08 0.67 -14 3 8 4.91 1.02 -14 -3 8 5.62 1.07 -14 -3 8 6.51 0.99 14 -3 -8 7.65 1.08 14 3 -8 6.20 1.01 -14 3 7 2.17 0.78 -14 -3 7 1.86 0.80 -14 -3 7 2.21 0.73 14 -3 -7 1.62 0.71 14 3 -7 1.29 0.66 -14 3 6 5.33 1.10 -14 -3 6 5.79 1.10 14 -3 -6 3.89 0.96 14 3 -6 6.07 1.08 -14 -3 6 7.04 1.12 14 -3 -5 40.24 2.67 14 3 -5 37.70 2.62 -14 -3 5 39.60 2.54 14 3 -4 13.29 1.60 -14 -3 4 12.50 1.45 14 -3 -3 0.88 0.83 14 3 -3 1.07 0.93 14 -3 -2 13.71 1.64 14 3 -2 15.71 1.71 -14 3 2 13.84 1.29 14 -3 -1 0.17 0.64 14 3 -1 0.35 0.71 -14 3 1 0.72 0.61 -14 -3 1 0.34 0.70 -14 3 0 16.04 1.37 14 -3 0 14.15 1.55 14 3 0 14.39 1.58 -14 3 0 12.29 1.36 -14 -3 0 14.81 1.59 -14 -3 -1 9.45 1.26 -14 3 -1 9.15 1.14 -14 3 -1 11.84 1.16 14 -3 1 10.77 1.26 14 -3 2 -0.27 0.54 -14 -3 -2 0.29 0.60 -14 3 -2 0.44 0.44 -14 3 -2 -0.32 0.44 14 -3 3 3.57 0.76 -14 -3 -3 4.75 0.91 -14 3 -3 5.75 0.81 -14 -3 -4 10.09 1.09 14 -3 4 8.35 0.93 -14 -3 -5 -0.09 0.40 -14 4 11 0.15 0.34 -14 -4 11 0.09 0.38 -14 -4 10 0.89 0.46 -14 4 10 0.59 0.44 -14 -4 10 1.24 0.57 -14 -4 9 1.21 0.53 -14 4 9 -0.12 0.47 -14 -4 9 0.12 0.50 -14 -4 9 0.83 0.58 -14 -4 8 -0.26 0.58 -14 4 8 0.39 0.56 -14 -4 8 -0.25 0.45 -14 -4 8 0.52 0.53 14 4 -8 0.59 0.48 14 4 -7 3.89 0.77 -14 -4 7 3.59 0.89 -14 4 7 3.17 0.80 -14 -4 7 3.82 0.85 14 -4 -6 3.52 0.76 14 4 -6 3.17 0.76 -14 -4 6 3.75 0.84 -14 4 6 3.59 0.85 -14 -4 6 1.48 0.68 14 -4 -5 3.78 0.81 14 4 -5 4.03 0.85 -14 -4 5 3.40 0.85 -14 4 5 2.49 0.79 -14 -4 5 4.13 0.93 14 -4 -4 -0.59 0.81 14 4 -4 -1.33 0.93 -14 -4 4 1.20 0.72 -14 4 4 0.30 0.60 -14 -4 4 -0.93 0.76 -14 -4 3 50.35 2.81 14 -4 -3 41.83 2.63 14 4 -3 45.10 2.73 -14 -4 2 0.89 0.63 14 -4 -2 0.15 0.61 14 4 -2 0.90 0.70 -14 4 1 -0.10 0.44 14 -4 -1 0.14 0.54 14 4 -1 0.44 0.56 -14 -4 1 0.15 0.58 14 -4 0 2.15 0.75 -14 4 0 1.72 0.55 14 4 0 2.39 0.71 -14 -4 0 2.38 0.75 14 -4 1 0.93 0.59 -14 4 -1 1.07 0.49 14 4 1 2.60 0.72 -14 -4 -1 1.18 0.63 -14 -4 -2 1.08 0.59 -14 4 -2 1.84 0.55 14 -4 2 0.96 0.60 14 -4 3 3.44 0.69 -14 -4 -3 4.69 0.79 14 -4 4 0.17 0.38 -14 -4 -4 0.17 0.42 14 -4 5 0.25 0.33 -14 -5 11 7.36 0.75 -14 -5 10 1.60 0.53 -14 -5 9 27.60 1.74 -14 -5 8 4.91 0.82 -14 -5 7 8.95 1.12 -14 -5 6 1.16 0.65 -14 -5 5 49.92 2.75 -14 -5 4 11.34 1.27 -14 -5 3 12.75 1.35 14 -5 -2 4.71 0.92 14 -5 -1 4.81 0.91 14 -5 0 0.88 0.60 14 -5 1 1.26 0.59 -14 -5 -1 1.26 0.55 14 -5 2 0.20 0.46 14 -5 3 2.88 0.57 14 -5 4 11.55 0.92 -14 -6 10 9.03 0.81 -14 -6 9 0.33 0.39 -14 -6 8 7.33 0.87 -14 -6 7 0.20 0.47 -14 -6 6 7.34 0.93 -14 -6 5 3.28 0.71 14 -6 -5 1.95 0.55 -14 -6 4 3.08 0.72 14 -6 -4 2.44 0.62 14 -6 -3 1.92 0.57 14 -6 -2 4.23 0.75 14 -6 -1 -0.11 0.43 14 -6 0 4.11 0.73 14 -6 1 7.67 0.85 14 -6 2 4.77 0.67 14 -6 2 5.66 0.70 14 -6 3 4.84 0.59 -14 -7 7 4.58 0.62 -14 -7 6 0.15 0.36 -14 -7 5 5.56 0.72 -15 0 13 0.47 0.35 -15 0 12 15.78 1.26 -15 0 11 -0.46 0.61 15 0 -10 1.29 0.58 -15 0 10 0.67 0.64 15 0 -9 0.14 0.52 -15 0 9 -0.15 0.67 15 0 -8 5.51 1.00 -15 0 8 4.35 0.97 15 0 -7 -0.17 0.71 -15 0 7 0.68 0.72 15 0 -6 80.81 4.12 -15 0 6 84.64 4.21 15 0 -5 -0.36 0.86 -15 0 5 -1.26 1.01 15 0 -4 101.91 4.86 -15 0 4 102.51 4.87 15 0 -3 -0.89 1.01 15 0 -2 0.17 0.84 15 0 -1 -0.17 0.62 -15 0 0 2.09 0.78 15 0 0 2.54 0.81 15 0 0 2.63 0.70 15 0 1 0.30 0.38 -15 0 -1 0.27 0.57 -15 0 -2 1.09 0.60 -15 0 -3 -0.41 0.51 -15 0 -4 3.99 0.62 -15 1 13 4.67 0.57 -15 -1 13 5.92 0.64 -15 1 12 1.77 0.56 -15 -1 12 0.18 0.40 -15 1 11 58.62 2.86 -15 -1 11 57.59 2.84 15 -1 -10 9.66 1.17 15 1 -10 8.75 1.11 -15 1 10 11.85 1.30 -15 -1 10 10.56 1.21 15 -1 -9 2.09 0.69 15 1 -9 1.83 0.68 -15 1 9 1.46 0.75 -15 -1 9 1.15 0.73 15 -1 -8 0.91 0.66 15 1 -8 0.62 0.59 -15 1 8 1.74 0.72 -15 -1 8 0.16 0.70 15 -1 -7 8.10 1.17 15 1 -7 6.07 1.08 -15 -1 7 6.14 0.89 -15 1 7 7.52 1.20 -15 -1 7 5.28 1.06 15 -1 -6 6.58 1.20 15 1 -6 6.85 1.17 -15 1 6 5.19 1.09 -15 -1 6 6.19 1.14 -15 -1 6 5.17 0.84 -15 1 5 26.13 2.09 -15 -1 5 23.32 2.03 15 -1 -5 19.71 1.91 15 1 -5 21.47 1.99 15 -1 -4 -0.70 0.93 15 1 -4 -0.71 0.83 -15 -1 4 -0.54 0.85 15 -1 -3 11.41 1.51 15 1 -3 13.11 1.59 -15 1 3 11.75 1.50 -15 -1 3 13.47 1.64 15 -1 -2 0.67 0.69 15 1 -2 2.08 0.87 15 -1 -1 12.65 1.50 15 1 -1 11.47 1.43 -15 -1 0 3.12 0.90 -15 1 0 2.97 0.79 -15 1 0 4.50 0.87 15 -1 0 3.98 0.87 15 1 0 1.71 0.72 15 -1 0 3.33 0.78 -15 -1 -1 7.29 1.07 -15 1 -1 6.81 0.97 -15 1 -1 5.85 0.89 15 -1 1 7.87 0.99 -15 1 -2 7.83 0.98 -15 -1 -2 7.00 0.98 -15 1 -2 10.10 1.05 15 -1 2 7.49 0.86 -15 1 -3 5.44 0.76 -15 -1 -3 3.85 0.74 -15 -1 -4 0.90 0.44 -15 2 12 0.21 0.36 -15 -2 12 0.30 0.39 -15 2 11 16.35 1.27 -15 -2 11 14.02 1.19 -15 -2 10 8.64 0.81 -15 2 10 9.69 1.10 -15 -2 10 9.28 1.06 -15 -2 9 19.33 1.35 15 -2 -9 19.21 1.56 15 2 -9 23.27 1.69 -15 2 9 22.34 1.72 -15 -2 9 21.38 1.69 -15 2 8 -0.29 0.62 -15 -2 8 0.14 0.61 -15 -2 8 -0.21 0.45 15 -2 -8 -0.28 0.55 15 2 -8 0.14 0.49 -15 -2 7 13.27 1.26 -15 -2 7 14.41 1.49 -15 2 7 13.43 1.46 15 -2 -7 16.08 1.52 15 2 -7 14.77 1.48 -15 2 6 0.64 0.64 -15 -2 6 -0.16 0.65 -15 -2 6 0.86 0.58 15 -2 -6 0.31 0.61 15 2 -6 0.16 0.57 -15 2 5 4.11 0.98 -15 -2 5 4.46 1.02 15 -2 -5 4.65 0.95 15 2 -5 2.62 0.88 -15 2 4 5.80 1.11 -15 -2 4 7.87 1.24 15 -2 -4 6.79 1.12 15 2 -4 5.16 1.05 -15 2 3 0.66 0.69 -15 -2 3 -0.33 0.71 15 -2 -3 -0.64 0.72 15 2 -3 -0.17 0.72 15 -2 -2 16.91 1.62 15 2 -2 15.39 1.63 -15 2 2 15.71 1.39 -15 -2 1 2.06 0.74 -15 2 1 1.63 0.66 15 -2 -1 1.95 0.71 15 2 -1 1.39 0.64 -15 -2 0 3.90 0.86 -15 2 0 2.88 0.75 15 -2 0 2.96 0.79 15 2 0 2.84 0.79 -15 2 0 4.87 0.81 15 -2 0 5.50 0.92 -15 -2 -1 -0.13 0.57 -15 2 -1 0.11 0.50 15 -2 1 0.39 0.54 15 2 1 0.63 0.60 15 -2 1 1.05 0.56 -15 2 -1 0.42 0.51 -15 2 -2 5.60 0.77 -15 -2 -2 5.16 0.87 15 -2 2 5.68 0.77 -15 -2 -3 4.74 0.75 -15 -2 -4 7.43 0.77 -15 3 11 1.47 0.45 -15 -3 11 1.52 0.52 -15 -3 10 -0.09 0.50 -15 3 10 0.09 0.46 -15 -3 10 0.73 0.40 -15 3 9 0.64 0.50 -15 -3 9 0.44 0.53 -15 -3 9 0.18 0.41 15 -3 -8 -0.23 0.49 15 3 -8 -0.12 0.43 -15 3 8 -0.36 0.54 -15 -3 8 0.74 0.60 -15 -3 8 -0.21 0.47 15 -3 -7 0.13 0.51 15 3 -7 -0.13 0.53 -15 3 7 -0.26 0.58 -15 -3 7 0.13 0.54 -15 -3 7 0.23 0.52 15 -3 -6 4.58 0.85 15 3 -6 2.72 0.72 -15 3 6 3.97 0.86 -15 -3 6 4.48 0.92 -15 -3 6 3.37 0.74 15 -3 -5 2.23 0.71 15 3 -5 1.13 0.61 -15 3 5 -0.14 0.56 -15 -3 5 1.88 0.72 -15 -3 5 1.87 0.66 15 -3 -4 2.40 0.73 15 3 -4 1.59 0.73 -15 -3 4 2.33 0.73 15 -3 -3 -0.56 0.63 15 3 -3 -0.14 0.55 15 -3 -2 2.33 0.76 15 3 -2 1.69 0.73 -15 -3 2 1.74 0.66 15 -3 -1 1.53 0.65 -15 -3 1 1.81 0.69 -15 3 1 0.22 0.48 -15 3 1 2.10 0.60 15 -3 -1 1.04 0.63 15 3 -1 0.53 0.56 15 -3 0 21.60 1.59 15 -3 0 17.65 1.52 15 3 0 13.41 1.34 -15 3 0 18.74 1.35 -15 -3 0 18.55 1.50 -15 3 0 16.48 1.30 15 -3 1 4.73 0.81 -15 -3 -1 5.58 0.84 -15 3 -1 4.91 0.67 15 -3 2 1.57 0.52 -15 -3 -2 2.05 0.60 -15 -3 -3 0.08 0.39 -15 -4 10 2.14 0.48 -15 -4 9 5.12 0.71 -15 4 9 4.88 0.62 -15 4 8 8.35 0.87 -15 -4 8 10.23 1.02 -15 -4 7 5.19 0.79 -15 4 7 5.29 0.76 -15 4 6 9.11 1.02 -15 -4 6 10.58 1.12 -15 -4 5 3.20 0.77 -15 -4 4 -0.43 0.54 -15 -4 3 7.88 0.98 15 -4 -2 12.79 1.23 -15 -4 2 9.41 1.04 15 -4 -1 1.01 0.57 -15 -4 1 1.14 0.52 15 -4 0 5.96 0.82 -15 -4 0 3.95 0.71 15 -4 1 2.01 0.56 -15 -4 -1 2.31 0.55 15 -4 2 5.52 0.70 -15 -5 9 0.54 0.37 -15 -5 8 -0.24 0.37 -15 -5 7 3.16 0.63 -15 -5 6 1.78 0.56 15 -5 -5 7.92 0.89 -15 -5 5 8.78 0.98 15 -5 -4 1.10 0.50 15 -5 -3 3.13 0.67 15 -5 -2 0.79 0.47 15 -5 -1 2.86 0.60 15 -5 0 12.33 1.05 15 -5 1 3.13 0.54 15 -5 2 4.30 0.53 -15 -6 7 1.57 0.41 -16 0 11 0.29 0.38 -16 0 10 38.81 2.05 -16 0 9 -1.17 0.58 -16 0 8 15.69 1.40 -16 0 7 0.26 0.62 16 0 -7 -0.25 0.48 -16 0 6 4.17 0.92 16 0 -6 3.72 0.81 -16 0 5 0.41 0.62 16 0 -5 0.27 0.53 -16 0 4 5.00 0.95 16 0 -4 3.43 0.81 16 0 -3 0.27 0.57 -16 0 2 0.48 0.53 16 0 -2 -0.13 0.49 -16 0 1 0.11 0.48 16 0 -1 0.25 0.36 16 0 -1 0.24 0.55 -16 0 0 14.17 1.21 -16 0 -1 -0.09 0.40 -16 1 11 5.21 0.61 -16 -1 11 5.32 0.64 -16 1 10 -0.09 0.44 -16 -1 10 -0.26 0.44 -16 1 9 21.92 1.54 -16 -1 9 21.13 1.52 -16 1 8 -0.58 0.73 -16 -1 8 -0.11 0.66 -16 1 7 10.99 1.23 -16 -1 7 11.59 1.23 16 -1 -7 11.45 1.17 16 1 -7 10.66 1.17 -16 1 6 5.12 0.97 -16 -1 6 5.58 0.99 16 1 -6 4.80 0.90 -16 1 5 62.70 3.20 -16 -1 5 62.56 3.20 16 -1 -5 62.72 3.19 16 1 -5 66.42 3.25 16 -1 -4 -1.05 0.77 16 -1 -3 0.13 0.63 16 1 -3 1.19 0.68 -16 1 2 4.32 0.79 -16 -1 2 6.48 0.95 16 -1 -2 4.70 0.85 16 1 -2 4.29 0.79 -16 -1 1 2.55 0.68 -16 1 1 2.10 0.63 16 -1 -1 2.15 0.56 -16 -1 0 -0.10 0.45 -16 1 0 0.28 0.40 16 -1 0 0.39 0.36 -16 1 -1 1.30 0.46 -16 -1 -1 0.35 0.42 -16 2 10 15.64 1.08 -16 -2 10 18.13 1.16 -16 2 9 8.64 0.89 -16 -2 9 9.73 0.95 -16 2 8 -0.50 0.57 -16 -2 8 -0.40 0.52 -16 2 7 -0.22 0.54 -16 -2 7 -0.33 0.49 -16 2 6 -0.23 0.55 -16 -2 6 0.12 0.55 -16 2 5 2.05 0.70 -16 -2 5 1.09 0.63 16 -2 -5 1.41 0.58 16 -2 -4 0.47 0.52 -16 -2 3 0.22 0.51 -16 -2 2 -0.11 0.53 -16 2 2 -0.39 0.48 16 -2 -2 0.32 0.51 -16 -2 1 0.40 0.49 -16 2 1 0.62 0.43 16 -2 -1 0.77 0.46 -16 -2 0 10.91 1.02 -16 2 0 9.53 0.88 16 -2 0 11.33 0.98 -16 -2 -1 10.75 0.92 -16 3 8 2.56 0.51 -16 -3 8 1.22 0.44 -16 3 7 4.14 0.67 -16 -3 7 4.25 0.68 -16 -3 5 12.84 1.09 -16 -3 4 47.96 2.34 -16 3 3 0.90 0.42 -16 -3 3 0.46 0.44 16 -3 -3 1.55 0.54 -16 -3 2 2.58 0.57 16 -3 -2 3.67 0.66 -16 -3 1 18.75 1.30 16 -3 -1 22.33 1.41 16 -3 0 0.37 0.34 16 -4 -5 0.08 0.37 16 -4 -4 12.07 1.01 16 -4 -3 1.60 0.49 16 -4 -2 3.31 0.56 16 -4 -1 15.93 1.08 -17 0 8 17.20 1.14 -17 0 4 0.08 0.36 -17 0 3 -0.15 0.34 -17 -1 5 -0.07 0.35 -17 -1 4 0.22 0.36 0 0 0 0.00 0.00 TITL nimodipine_auto in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 13.810295 10.763123 14.818743 90.0000 104.6035 90.0000 ZERR 9.00 0.000236 0.000171 0.000252 0.0000 0.0018 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 99.00 90.00 9.00 9.00 REM CrysAlisPro recorded range (K): Min=149.9; max=150.0; aver:150.0 TEMP -123 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 84206 _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 Nimodipine _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 1.291 _oxdiff_exptl_absorpt_empirical_full_min 0.642 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 O2 O 0.73365(8) 0.77502(9) 0.36584(7) 0.0326(2) Uani 1 1 d . . . . . O7 O 0.82610(8) 0.36020(10) 0.42920(8) 0.0372(3) Uani 1 1 d . . . . . O1 O 0.72079(8) 0.89492(11) 0.18933(7) 0.0390(3) Uani 1 1 d . . . . . O6 O 0.72099(9) 0.20091(11) 0.42689(9) 0.0481(3) Uani 1 1 d . . . . . O3 O 0.58192(9) 0.85152(10) 0.36392(10) 0.0492(3) Uani 1 1 d . . . . . N1 N 0.48744(9) 0.47132(12) 0.35103(9) 0.0312(3) Uani 1 1 d . . . . . O5 O 0.94826(11) 0.53321(13) 0.08522(10) 0.0586(4) Uani 1 1 d . . . . . N2 N 0.92945(11) 0.55186(14) 0.16049(11) 0.0456(4) Uani 1 1 d . . . . . C12 C 0.71128(10) 0.52784(12) 0.26453(9) 0.0261(3) Uani 1 1 d . . . . . O4 O 0.99283(10) 0.58695(19) 0.22928(10) 0.0765(5) Uani 1 1 d . . . . . C11 C 0.68755(10) 0.53418(13) 0.35984(9) 0.0257(3) Uani 1 1 d . . . . . H11 H 0.749808 0.558961 0.407283 0.031 Uiso 1 1 calc R U . . . C10 C 0.65572(10) 0.40598(13) 0.38587(9) 0.0275(3) Uani 1 1 d . . . . . C5 C 0.60687(10) 0.63079(13) 0.36027(9) 0.0269(3) Uani 1 1 d . . . . . C8 C 0.55818(11) 0.37856(13) 0.37548(9) 0.0289(3) Uani 1 1 d . . . . . C6 C 0.51020(11) 0.59564(13) 0.35018(9) 0.0292(3) Uani 1 1 d . . . . . C17 C 0.63600(11) 0.50066(13) 0.18478(10) 0.0303(3) Uani 1 1 d . . . . . H17 H 0.569317 0.489564 0.189801 0.036 Uiso 1 1 calc R U . . . C13 C 0.80794(11) 0.54581(13) 0.25600(10) 0.0303(3) Uani 1 1 d . . . . . H13 H 0.860407 0.566069 0.309002 0.036 Uiso 1 1 calc R U . . . C3 C 0.77116(12) 0.89792(14) 0.35535(11) 0.0348(3) Uani 1 1 d . . . . . H3A H 0.827931 0.917329 0.409227 0.042 Uiso 1 1 calc R U . . . H3B H 0.717868 0.960161 0.353287 0.042 Uiso 1 1 calc R U . . . C18 C 0.73378(11) 0.31054(14) 0.41562(10) 0.0316(3) Uani 1 1 d . . . . . C14 C 0.82686(12) 0.53372(14) 0.16868(11) 0.0349(3) Uani 1 1 d . . . . . C4 C 0.63519(11) 0.76264(14) 0.36351(10) 0.0296(3) Uani 1 1 d . . . . . C9 C 0.51319(12) 0.25512(15) 0.38897(11) 0.0368(4) Uani 1 1 d . . . . . H9A H 0.506691 0.248754 0.453154 0.055 Uiso 1 1 calc R U . . . H9B H 0.556547 0.188294 0.377047 0.055 Uiso 1 1 calc R U . . . H9C H 0.446968 0.247728 0.345519 0.055 Uiso 1 1 calc R U . . . C15 C 0.75341(13) 0.50471(15) 0.08958(11) 0.0385(4) Uani 1 1 d . . . . . H15 H 0.768775 0.495451 0.030956 0.046 Uiso 1 1 calc R U . . . C2 C 0.80494(11) 0.90333(16) 0.26684(11) 0.0357(3) Uani 1 1 d . . . . . H2A H 0.840774 0.982355 0.264093 0.043 Uiso 1 1 calc R U . . . H2B H 0.851524 0.833922 0.265282 0.043 Uiso 1 1 calc R U . . . C16 C 0.65664(12) 0.48948(15) 0.09813(10) 0.0367(4) Uani 1 1 d . . . . . H16 H 0.604177 0.471332 0.044604 0.044 Uiso 1 1 calc R U . . . C7 C 0.41993(11) 0.67806(15) 0.33735(12) 0.0377(4) Uani 1 1 d . . . . . H7A H 0.362055 0.637071 0.296133 0.057 Uiso 1 1 calc R U . . . H7B H 0.432729 0.757019 0.309514 0.057 Uiso 1 1 calc R U . . . H7C H 0.406135 0.693854 0.398042 0.057 Uiso 1 1 calc R U . . . C19 C 0.91115(12) 0.27724(16) 0.46364(15) 0.0487(5) Uani 1 1 d . . . . . H19 H 0.894395 0.191977 0.437557 0.058 Uiso 1 1 calc R U . . . C1 C 0.74830(15) 0.8892(2) 0.10338(12) 0.0569(5) Uani 1 1 d . . . . . H1A H 0.687857 0.886017 0.051803 0.085 Uiso 1 1 calc R U . . . H1B H 0.788617 0.814592 0.102205 0.085 Uiso 1 1 calc R U . . . H1C H 0.787415 0.963104 0.096793 0.085 Uiso 1 1 calc R U . . . C20 C 0.93331(17) 0.2731(2) 0.56878(17) 0.0695(7) Uani 1 1 d . . . . . H20A H 0.950181 0.356742 0.594017 0.104 Uiso 1 1 calc R U . . . H20B H 0.989841 0.217151 0.593140 0.104 Uiso 1 1 calc R U . . . H20C H 0.874293 0.242763 0.587387 0.104 Uiso 1 1 calc R U . . . C21 C 0.99591(15) 0.3300(2) 0.4289(2) 0.0757(8) Uani 1 1 d . . . . . H21A H 0.977982 0.328895 0.360593 0.114 Uiso 1 1 calc R U . . . H21B H 1.056150 0.279719 0.452565 0.114 Uiso 1 1 calc R U . . . H21C H 1.008851 0.415681 0.451000 0.114 Uiso 1 1 calc R U . . . H1 H 0.4232(15) 0.4494(18) 0.3384(13) 0.043(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 O2 0.0363(6) 0.0266(5) 0.0363(6) -0.0001(4) 0.0118(4) -0.0005(4) O7 0.0305(5) 0.0273(5) 0.0508(7) 0.0042(5) 0.0050(5) 0.0029(4) O1 0.0319(6) 0.0572(7) 0.0282(5) 0.0028(5) 0.0083(4) 0.0041(5) O6 0.0403(6) 0.0285(6) 0.0692(8) 0.0120(6) 0.0021(6) -0.0013(5) O3 0.0371(6) 0.0287(6) 0.0789(9) -0.0061(6) 0.0094(6) 0.0045(5) N1 0.0275(6) 0.0328(7) 0.0326(6) 0.0002(5) 0.0061(5) -0.0011(5) O5 0.0685(9) 0.0612(8) 0.0613(8) -0.0103(7) 0.0448(7) -0.0102(7) N2 0.0427(8) 0.0509(9) 0.0489(8) -0.0003(7) 0.0221(7) 0.0013(7) C12 0.0326(7) 0.0209(7) 0.0248(7) 0.0008(5) 0.0073(5) 0.0023(5) O4 0.0360(7) 0.1391(16) 0.0565(9) -0.0061(9) 0.0157(7) -0.0046(8) C11 0.0280(7) 0.0252(7) 0.0228(6) -0.0004(5) 0.0044(5) 0.0015(5) C10 0.0322(7) 0.0265(7) 0.0225(6) 0.0006(5) 0.0045(5) 0.0007(6) C5 0.0319(7) 0.0274(7) 0.0205(6) 0.0003(5) 0.0048(5) 0.0021(6) C8 0.0342(7) 0.0293(7) 0.0220(6) 0.0007(5) 0.0052(6) -0.0006(6) C6 0.0330(7) 0.0303(7) 0.0236(7) -0.0004(6) 0.0055(6) 0.0029(6) C17 0.0348(7) 0.0262(7) 0.0290(7) -0.0011(6) 0.0066(6) -0.0017(6) C13 0.0314(7) 0.0294(7) 0.0295(7) 0.0007(6) 0.0065(6) 0.0019(6) C3 0.0413(8) 0.0288(8) 0.0329(8) -0.0027(6) 0.0067(6) -0.0051(6) C18 0.0347(8) 0.0291(8) 0.0283(7) 0.0026(6) 0.0031(6) -0.0012(6) C14 0.0387(8) 0.0319(8) 0.0378(8) 0.0000(6) 0.0163(7) 0.0020(6) C4 0.0319(7) 0.0305(8) 0.0245(7) -0.0013(6) 0.0034(6) 0.0037(6) C9 0.0382(8) 0.0339(8) 0.0372(8) 0.0027(6) 0.0078(7) -0.0062(6) C15 0.0551(10) 0.0345(8) 0.0297(8) -0.0037(6) 0.0176(7) -0.0027(7) C2 0.0294(7) 0.0395(8) 0.0370(8) 0.0025(7) 0.0065(6) -0.0040(6) C16 0.0471(9) 0.0348(8) 0.0264(7) -0.0029(6) 0.0059(6) -0.0051(7) C7 0.0321(8) 0.0382(9) 0.0429(9) -0.0005(7) 0.0096(7) 0.0055(6) C19 0.0337(8) 0.0270(8) 0.0798(14) 0.0041(8) 0.0036(8) 0.0056(7) C1 0.0543(11) 0.0863(15) 0.0341(9) 0.0058(9) 0.0190(8) 0.0085(10) C20 0.0590(13) 0.0532(12) 0.0751(15) 0.0106(11) -0.0225(11) 0.0029(10) C21 0.0424(11) 0.0442(11) 0.144(2) 0.0078(13) 0.0304(13) 0.0069(9) 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 C4 O2 C3 118.13(11) . . ? C18 O7 C19 117.13(12) . . ? C2 O1 C1 112.34(13) . . ? C8 N1 H1 117.7(12) . . ? C6 N1 C8 123.92(13) . . ? C6 N1 H1 118.3(12) . . ? O5 N2 C14 119.05(15) . . ? O4 N2 O5 122.56(15) . . ? O4 N2 C14 118.39(14) . . ? C17 C12 C11 120.29(12) . . ? C13 C12 C11 120.90(12) . . ? C13 C12 C17 118.79(13) . . ? C12 C11 H11 108.3 . . ? C10 C11 C12 109.59(11) . . ? C10 C11 H11 108.3 . . ? C5 C11 C12 111.17(11) . . ? C5 C11 H11 108.3 . . ? C5 C11 C10 110.97(11) . . ? C8 C10 C11 120.76(13) . . ? C8 C10 C18 121.04(13) . . ? C18 C10 C11 118.04(12) . . ? C6 C5 C11 120.54(13) . . ? C6 C5 C4 121.22(13) . . ? C4 C5 C11 118.03(12) . . ? N1 C8 C9 112.70(13) . . ? C10 C8 N1 119.48(13) . . ? C10 C8 C9 127.81(14) . . ? N1 C6 C7 113.04(13) . . ? C5 C6 N1 119.36(13) . . ? C5 C6 C7 127.60(14) . . ? C12 C17 H17 119.4 . . ? C16 C17 C12 121.26(14) . . ? C16 C17 H17 119.4 . . ? C12 C13 H13 120.5 . . ? C12 C13 C14 118.92(14) . . ? C14 C13 H13 120.5 . . ? O2 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? O2 C3 C2 109.21(12) . . ? H3A C3 H3B 108.3 . . ? C2 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? O7 C18 C10 111.14(12) . . ? O6 C18 O7 122.03(14) . . ? O6 C18 C10 126.82(14) . . ? C13 C14 N2 118.53(14) . . ? C15 C14 N2 118.64(14) . . ? C15 C14 C13 122.83(14) . . ? O2 C4 C5 110.62(12) . . ? O3 C4 O2 121.97(14) . . ? O3 C4 C5 127.42(14) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C15 H15 121.0 . . ? C14 C15 C16 118.00(14) . . ? C16 C15 H15 121.0 . . ? O1 C2 C3 109.53(12) . . ? O1 C2 H2A 109.8 . . ? O1 C2 H2B 109.8 . . ? C3 C2 H2A 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C17 C16 H16 119.9 . . ? C15 C16 C17 120.17(14) . . ? C15 C16 H16 119.9 . . ? 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 . . ? O7 C19 H19 109.8 . . ? O7 C19 C20 108.31(16) . . ? O7 C19 C21 106.05(15) . . ? C20 C19 H19 109.8 . . ? C21 C19 H19 109.8 . . ? C21 C19 C20 113.03(19) . . ? 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 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 O2 C3 1.4431(18) . ? O2 C4 1.3581(18) . ? O7 C18 1.3499(18) . ? O7 C19 1.4612(18) . ? O1 C2 1.4160(18) . ? O1 C1 1.4192(19) . ? O6 C18 1.2108(19) . ? O3 C4 1.2078(18) . ? N1 C8 1.3798(19) . ? N1 C6 1.3753(19) . ? N1 H1 0.892(19) . ? O5 N2 1.2239(19) . ? N2 O4 1.224(2) . ? N2 C14 1.465(2) . ? C12 C11 1.5297(18) . ? C12 C17 1.394(2) . ? C12 C13 1.386(2) . ? C11 H11 1.0000 . ? C11 C10 1.5269(19) . ? C11 C5 1.5252(19) . ? C10 C8 1.349(2) . ? C10 C18 1.474(2) . ? C5 C6 1.359(2) . ? C5 C4 1.470(2) . ? C8 C9 1.501(2) . ? C6 C7 1.503(2) . ? C17 H17 0.9500 . ? C17 C16 1.389(2) . ? C13 H13 0.9500 . ? C13 C14 1.389(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C2 1.500(2) . ? C14 C15 1.379(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C15 H15 0.9500 . ? C15 C16 1.384(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C16 H16 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C19 H19 1.0000 . ? C19 C20 1.511(3) . ? C19 C21 1.503(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 O2 C3 C2 O1 68.61(16) . . . . ? O5 N2 C14 C13 175.10(15) . . . . ? O5 N2 C14 C15 -4.5(2) . . . . ? N2 C14 C15 C16 -179.16(14) . . . . ? C12 C11 C10 C8 -100.93(15) . . . . ? C12 C11 C10 C18 74.42(15) . . . . ? C12 C11 C5 C6 99.73(15) . . . . ? C12 C11 C5 C4 -74.96(15) . . . . ? C12 C17 C16 C15 0.3(2) . . . . ? C12 C13 C14 N2 -179.49(13) . . . . ? C12 C13 C14 C15 0.1(2) . . . . ? O4 N2 C14 C13 -5.9(2) . . . . ? O4 N2 C14 C15 174.44(17) . . . . ? C11 C12 C17 C16 -177.37(13) . . . . ? C11 C12 C13 C14 177.15(13) . . . . ? C11 C10 C8 N1 -7.3(2) . . . . ? C11 C10 C8 C9 173.86(13) . . . . ? C11 C10 C18 O7 9.94(17) . . . . ? C11 C10 C18 O6 -169.64(15) . . . . ? C11 C5 C6 N1 7.9(2) . . . . ? C11 C5 C6 C7 -171.92(13) . . . . ? C11 C5 C4 O2 -0.13(17) . . . . ? C11 C5 C4 O3 179.67(15) . . . . ? C10 C11 C5 C6 -22.51(17) . . . . ? C10 C11 C5 C4 162.80(12) . . . . ? C5 C11 C10 C8 22.22(17) . . . . ? C5 C11 C10 C18 -162.43(12) . . . . ? C8 N1 C6 C5 10.2(2) . . . . ? C8 N1 C6 C7 -169.96(13) . . . . ? C8 C10 C18 O7 -174.73(13) . . . . ? C8 C10 C18 O6 5.7(2) . . . . ? C6 N1 C8 C10 -10.5(2) . . . . ? C6 N1 C8 C9 168.49(13) . . . . ? C6 C5 C4 O2 -174.78(12) . . . . ? C6 C5 C4 O3 5.0(2) . . . . ? C17 C12 C11 C10 64.89(16) . . . . ? C17 C12 C11 C5 -58.15(17) . . . . ? C17 C12 C13 C14 -1.3(2) . . . . ? C13 C12 C11 C10 -113.49(14) . . . . ? C13 C12 C11 C5 123.47(14) . . . . ? C13 C12 C17 C16 1.0(2) . . . . ? C13 C14 C15 C16 1.2(2) . . . . ? C3 O2 C4 O3 -8.8(2) . . . . ? C3 O2 C4 C5 171.05(11) . . . . ? C18 O7 C19 C20 -85.72(18) . . . . ? C18 O7 C19 C21 152.68(17) . . . . ? C18 C10 C8 N1 177.50(12) . . . . ? C18 C10 C8 C9 -1.4(2) . . . . ? C14 C15 C16 C17 -1.4(2) . . . . ? C4 O2 C3 C2 -115.35(14) . . . . ? C4 C5 C6 N1 -177.55(12) . . . . ? C4 C5 C6 C7 2.6(2) . . . . ? C19 O7 C18 O6 -3.5(2) . . . . ? C19 O7 C18 C10 176.90(13) . . . . ? C1 O1 C2 C3 -175.15(15) . . . . ? _cod_database_fobs_code 2312374