#------------------------------------------------------------------------------ #$Date: 2023-12-22 05:01:42 +0200 (Fri, 22 Dec 2023) $ #$Revision: 288500 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312372.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_2312372 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 'C18 H20 N2 O6' _chemical_formula_sum 'C18 H20 N2 O6' _chemical_formula_weight 360.36 _chemical_name_common nitrendipine _chemical_name_systematic ; (rac)-3-ethyl 5-methyl 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 93.615(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8143(5) _cell_length_b 15.3632(8) _cell_length_c 12.9602(7) _cell_measurement_reflns_used 9981 _cell_measurement_temperature 150.00 _cell_measurement_theta_max 66.73 _cell_measurement_theta_min 4.47 _cell_volume 1751.52(16) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection 'Bruker Instrument Service v6.2.6' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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_temperature 150.0 _diffrn_detector 'Bruker Photon II area detector' _diffrn_detector_area_resol_mean 7.3910 _diffrn_detector_type 'Hybrid area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_orient_matrix_type 'Bruker AXS Inc. convention APEX3' _diffrn_radiation_collimation 'focussed source' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21238 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 66.732 _diffrn_reflns_theta_max 66.731 _diffrn_reflns_theta_min 4.468 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_target Cu _diffrn_source_type ; 'Incoatec microfocus 3.0 (cu) X-ray Source' ; _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.6634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1443 before and 0.0747 after correction. The Ratio of minimum to maximum transmission is 0.8812. The \l/2 correction factor is Not present. ; _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 1.367 _exptl_crystal_description plate _exptl_crystal_F_000 760 _exptl_crystal_preparation 'Crystallised from a saturated solution of nitrendipine in DMF.' _exptl_crystal_recrystallization_method 'High-throughput screening via the ENaCt protocol using SPT Labtech mosquito.' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.394 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 243 _refine_ls_number_reflns 3107 _refine_ls_number_restraints 195 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0569 _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^)+(0.0750P)^2^+1.0941P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1517 _refine_ls_wR_factor_ref 0.1557 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2820 _reflns_number_total 3107 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file rm5073sup1.cif _cod_data_source_block nitrendipine _cod_database_code 2312372 _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 0.903 _shelx_estimated_absorpt_t_min 0.642 _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. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Ternary CH refined with riding coordinates: C10(H10) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B) 3.c Aromatic/amide H refined with riding coordinates: C16(H16), C12(H12), C14(H14), C15(H15) 3.d Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C1A(H1AA,H1AB,H1AC), C18A(H18A,H18B,H18C) ; _shelx_res_file ; TITL jpm_010_p1_b7_a.res in P2(1)/c nitrendipine.res created by SHELXL-2018/3 at 14:59:33 on 11-May-2023 REM Old TITL jpm_010_p1_b7 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.199, Rweak 0.008, Alpha 0.023 REM 2.436 for 138 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N3 O4 CELL 1.54178 8.8143 15.3632 12.9602 90 93.615 90 ZERR 4 0.0005 0.0008 0.0007 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 72 80 8 24 RIGU L.S. 12 0 0 PLAN 5 SIZE 0.12 0.43 0.56 TEMP -123.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.075000 1.094100 FVAR 0.54659 O2 4 0.270354 0.356213 0.567007 11.00000 0.07651 0.04623 = 0.03052 0.00156 -0.00011 0.00585 O1 4 0.112976 0.373754 0.693487 11.00000 0.04975 0.04165 = 0.05796 0.00678 0.00416 0.00748 N1 3 0.348164 0.172386 0.856616 11.00000 0.06337 0.03719 = 0.02976 0.00169 -0.00216 -0.00100 O3 4 0.646783 0.130502 0.327605 11.00000 0.10542 0.06024 = 0.04725 0.00419 0.02017 0.01757 O6 4 0.738672 0.210002 0.632971 11.00000 0.04886 0.09890 = 0.05842 -0.02566 0.00544 0.00017 O4 4 0.478936 0.044695 0.252430 11.00000 0.12066 0.07664 = 0.04156 -0.02052 -0.01070 0.03636 N2 3 0.526103 0.089041 0.325551 11.00000 0.09300 0.04753 = 0.03476 0.00065 -0.00049 0.02794 O5 4 0.806090 0.133831 0.774930 11.00000 0.04956 0.07438 = 0.13498 0.01253 -0.01880 0.00260 C4 1 0.303533 0.264855 0.712851 11.00000 0.04409 0.03250 = 0.02963 -0.00450 -0.00292 -0.00225 C3 1 0.229337 0.334460 0.651385 11.00000 0.04591 0.03405 = 0.03377 -0.00612 -0.00509 -0.00253 C5 1 0.257998 0.233772 0.804240 11.00000 0.04793 0.03358 = 0.03088 -0.00484 -0.00397 -0.00427 C11 1 0.395745 0.159552 0.580382 11.00000 0.05246 0.03139 = 0.03271 -0.00130 -0.00602 0.00889 C10 1 0.440837 0.226223 0.664715 11.00000 0.04718 0.03384 = 0.03505 -0.00422 0.00032 -0.00002 AFIX 13 H10 2 0.496495 0.274680 0.632075 11.00000 -1.20000 AFIX 0 C9 1 0.549023 0.184160 0.746669 11.00000 0.04960 0.03765 = 0.04252 -0.00990 -0.00871 0.00167 C13 1 0.435850 0.093748 0.416809 11.00000 0.07116 0.04061 = 0.03241 -0.00062 -0.00624 0.02119 C16 1 0.280669 0.099259 0.592488 11.00000 0.05650 0.03452 = 0.03899 -0.00202 -0.00751 0.00403 AFIX 43 H16 2 0.227222 0.099872 0.653887 11.00000 -1.20000 AFIX 0 C7 1 0.496731 0.155508 0.835820 11.00000 0.05661 0.03437 = 0.04336 -0.00858 -0.01215 0.00305 C6 1 0.120158 0.257427 0.859262 11.00000 0.05581 0.04864 = 0.03299 -0.00254 0.00385 -0.00462 AFIX 137 H6A 2 0.089597 0.207847 0.900768 11.00000 -1.50000 H6B 2 0.037170 0.272585 0.808565 11.00000 -1.50000 H6C 2 0.143167 0.307387 0.904594 11.00000 -1.50000 AFIX 0 C12 1 0.475018 0.156413 0.490959 11.00000 0.05762 0.03604 = 0.03399 0.00165 -0.00260 0.01192 AFIX 43 H12 2 0.554724 0.196532 0.480792 11.00000 -1.20000 AFIX 0 C14 1 0.319871 0.035353 0.426350 11.00000 0.07751 0.03702 = 0.04302 -0.00991 -0.01870 0.01620 AFIX 43 H14 2 0.293545 -0.005510 0.373188 11.00000 -1.20000 AFIX 0 C15 1 0.242402 0.037890 0.515978 11.00000 0.06552 0.03580 = 0.05207 -0.00525 -0.01583 0.00360 AFIX 43 H15 2 0.162717 -0.002418 0.525394 11.00000 -1.20000 AFIX 0 C17 1 0.708685 0.172663 0.722534 11.00000 0.04429 0.04450 = 0.07872 -0.02048 -0.01082 -0.00366 C8 1 0.584332 0.106403 0.920338 11.00000 0.08393 0.04952 = 0.04813 -0.00545 -0.02002 0.01545 AFIX 137 H8A 2 0.521761 0.100160 0.979779 11.00000 -1.50000 H8B 2 0.677392 0.138396 0.941349 11.00000 -1.50000 H8C 2 0.610966 0.048633 0.895001 11.00000 -1.50000 AFIX 0 C2 1 0.038381 0.442183 0.630872 11.00000 0.05836 0.04936 = 0.08994 0.01854 -0.00315 0.01062 AFIX 23 H2A 2 0.109734 0.490957 0.621821 11.00000 -1.20000 H2B 2 0.005161 0.419223 0.561729 11.00000 -1.20000 AFIX 0 C1A 1 -0.090866 0.471907 0.683424 11.00000 0.09203 0.11146 = 0.19376 0.05765 0.05373 0.04745 AFIX 137 H1AA 2 -0.138691 0.520836 0.645318 11.00000 -1.50000 H1AB 2 -0.057639 0.490812 0.753456 11.00000 -1.50000 H1AC 2 -0.164345 0.424329 0.687310 11.00000 -1.50000 AFIX 0 C18A 1 0.888898 0.196759 0.595608 11.00000 0.04246 0.11271 = 0.12375 -0.05470 0.01343 -0.01498 AFIX 137 H18A 2 0.886037 0.208960 0.521290 11.00000 -1.50000 H18B 2 0.920533 0.136326 0.608126 11.00000 -1.50000 H18C 2 0.961474 0.236059 0.632200 11.00000 -1.50000 AFIX 0 H1 2 0.315817 0.159876 0.910766 11.00000 0.03880 HKLF 4 REM jpm_010_p1_b7_a.res in P2(1)/c REM wR2 = 0.1557, GooF = S = 1.052, Restrained GooF = 1.022 for all data REM R1 = 0.0569 for 2820 Fo > 4sig(Fo) and 0.0611 for all 3107 data REM 243 parameters refined using 195 restraints END WGHT 0.0749 1.0941 REM Highest difference peak 0.394, deepest hole -0.267, 1-sigma level 0.048 Q1 1 -0.0973 0.4208 0.5964 11.00000 0.05 0.39 Q2 1 0.8868 0.1812 0.5187 11.00000 0.05 0.39 Q3 1 0.7593 0.1386 0.8386 11.00000 0.05 0.31 Q4 1 0.6090 0.2552 0.8355 11.00000 0.05 0.25 Q5 1 0.0829 0.3191 0.8380 11.00000 0.05 0.23 ; _shelx_res_checksum 52999 _shelx_hkl_file ; -1 0 0 5063.09 258.27 -2 0 0 193.28 12.30 -2 0 0 193.98 11.90 -2 0 0 190.28 10.00 2 0 0 189.98 10.00 2 0 0 184.28 9.80 3 0 0 239.78 13.20 3 0 0 255.47 13.40 3 0 0 258.87 13.50 -3 0 0 250.37 16.60 -3 0 0 270.47 13.60 -3 0 0 254.27 18.10 -4 0 0 503.55 35.40 -4 0 0 542.45 28.80 4 0 0 551.64 28.60 4 0 0 559.44 28.50 4 0 0 560.04 28.40 5 0 0 1082.89 54.99 5 0 0 1051.69 55.19 6 0 0 158.08 8.80 -6 0 0 149.88 9.20 6 0 0 143.29 9.00 7 0 0 28.20 3.40 -7 0 0 35.60 2.20 -7 0 0 32.40 3.60 7 0 0 28.80 1.90 -7 0 0 35.00 2.20 7 0 0 34.00 3.20 -7 0 0 31.40 2.50 -8 0 0 25.90 2.30 8 0 0 27.00 1.90 -8 0 0 27.30 2.00 -8 0 0 29.70 2.00 -9 0 0 7.00 1.20 9 0 0 6.80 0.70 -9 0 0 7.40 1.10 -9 0 0 6.40 1.10 -10 0 0 1.10 0.30 -10 0 0 1.80 0.40 -10 0 0 1.20 0.50 0 -1 0 0.50 0.10 0 -1 0 1.60 1.30 0 1 0 -0.70 0.90 1 -1 0 1276.07 61.49 -1 -1 0 1152.78 59.59 1 -1 0 1160.78 59.59 1 -1 0 1111.19 59.49 -1 -1 0 1155.18 60.19 -1 1 0 1154.98 59.59 -1 1 0 1183.38 61.29 1 1 0 1166.18 60.19 -2 -1 0 116.39 6.00 2 -1 0 100.49 5.80 -2 -1 0 105.49 8.10 2 -1 0 113.09 6.00 -2 1 0 108.99 6.00 -2 1 0 99.79 9.20 2 1 0 110.39 5.90 -2 1 0 111.69 9.30 2 1 0 118.99 5.80 3 -1 0 0.20 0.30 -3 -1 0 6.00 3.70 3 -1 0 0.00 0.20 -3 -1 0 0.10 0.30 3 1 0 0.00 0.30 -3 1 0 -6.50 5.60 3 1 0 0.60 0.30 3 1 0 0.00 0.20 -3 1 0 0.40 0.30 -3 1 0 4.00 6.40 4 -1 0 83.79 5.00 4 -1 0 78.99 4.80 4 -1 0 86.69 5.70 -4 -1 0 70.39 9.60 -4 -1 0 92.09 5.40 4 1 0 86.29 4.90 4 1 0 88.19 4.80 4 1 0 82.69 4.70 -4 1 0 78.29 15.00 -4 1 0 75.29 5.10 5 -1 0 27.20 2.20 -5 -1 0 32.10 2.70 5 -1 0 25.90 2.30 5 1 0 30.10 2.30 -5 1 0 23.40 2.40 6 -1 0 28.40 2.70 6 -1 0 36.70 3.00 -6 -1 0 30.60 3.10 6 1 0 28.90 2.80 -6 1 0 36.00 3.80 6 1 0 29.50 2.60 -7 -1 0 11.70 1.10 -7 -1 0 11.50 1.10 -7 -1 0 9.90 1.40 7 -1 0 12.50 1.90 7 -1 0 9.90 0.80 -7 1 0 11.40 1.10 7 1 0 7.70 1.60 -7 1 0 13.40 1.40 -7 1 0 12.30 2.30 7 1 0 9.70 1.90 -7 1 0 12.50 1.20 -8 -1 0 0.20 0.40 8 -1 0 0.60 0.50 -8 -1 0 0.50 0.50 -8 1 0 1.00 0.50 -8 1 0 0.30 0.40 -8 1 0 1.00 0.60 -9 -1 0 5.80 0.90 -9 -1 0 6.50 1.10 -9 -1 0 6.50 0.90 9 -1 0 7.60 0.70 -9 1 0 6.00 1.00 9 1 0 5.90 0.60 -9 1 0 8.20 1.20 -9 1 0 6.60 0.90 -10 -1 0 7.00 0.80 -10 -1 0 6.90 0.80 -10 -1 0 6.40 0.90 10 -1 0 6.70 0.70 -10 1 0 6.40 0.70 -10 1 0 6.90 0.80 10 1 0 7.10 0.60 -10 1 0 6.30 0.90 0 -2 0 2561.04 126.69 0 -2 0 2422.86 124.69 0 2 0 2410.76 126.49 0 2 0 2414.96 124.89 -1 -2 0 165.78 9.60 1 -2 0 146.69 8.20 1 -2 0 155.38 11.10 -1 -2 0 159.68 8.20 1 2 0 161.58 9.90 1 2 0 161.68 8.20 -1 2 0 147.69 10.90 -2 -2 0 830.32 40.20 2 -2 0 726.43 40.20 2 -2 0 748.63 40.20 -2 -2 0 802.42 41.00 2 2 0 840.22 41.20 -2 2 0 751.92 43.80 2 2 0 785.72 40.10 -3 -2 0 0.90 0.40 -3 2 0 4.20 7.20 3 2 0 1.00 0.30 3 2 0 1.10 0.30 3 2 0 0.90 0.30 -3 2 0 -5.00 8.20 -4 -2 0 0.90 0.50 -4 -2 0 0.80 0.80 4 -2 0 0.30 0.30 4 2 0 0.80 0.40 4 2 0 0.20 0.30 -4 2 0 4.50 14.20 -4 2 0 0.90 0.60 5 -2 0 79.99 5.00 5 -2 0 80.49 4.90 -5 -2 0 69.69 5.00 5 2 0 74.99 4.70 -5 2 0 74.69 5.00 5 2 0 75.49 4.50 6 -2 0 48.00 3.80 6 -2 0 41.50 2.50 6 -2 0 47.90 3.60 -6 -2 0 50.99 4.50 6 2 0 46.30 3.40 -6 2 0 46.00 3.80 6 2 0 35.00 4.30 -7 -2 0 57.09 3.30 -7 -2 0 60.29 3.30 7 -2 0 49.10 4.30 -7 -2 0 54.99 3.70 7 2 0 45.00 4.50 7 2 0 55.19 4.10 -7 2 0 53.49 3.70 -7 2 0 49.70 3.30 -7 2 0 52.59 3.30 -8 -2 0 12.60 1.80 8 -2 0 11.10 1.00 -8 -2 0 12.60 1.60 -8 2 0 12.50 1.80 -8 2 0 10.10 1.50 -8 2 0 11.30 1.50 -8 2 0 13.10 2.70 -9 -2 0 1.40 0.60 -9 -2 0 2.70 0.50 -9 -2 0 2.40 0.50 9 -2 0 2.10 0.40 -9 2 0 2.50 0.80 -9 2 0 2.30 0.60 -9 2 0 1.70 0.50 -10 -2 0 -0.10 0.30 -10 -2 0 0.20 0.40 -10 -2 0 0.00 0.30 10 -2 0 0.00 0.20 -10 2 0 0.20 0.30 10 2 0 0.70 0.30 -10 2 0 0.30 0.30 -10 2 0 0.40 0.40 0 -3 0 2.30 3.50 0 3 0 2.40 3.20 1 -3 0 12.60 0.90 1 -3 0 9.80 5.20 1 -3 0 13.60 1.00 -1 -3 0 12.90 0.90 -1 -3 0 17.40 6.50 -1 3 0 13.40 1.10 1 3 0 13.50 1.00 1 3 0 14.20 3.90 -1 3 0 8.10 4.70 -2 -3 0 70.79 6.20 2 -3 0 57.59 3.40 -2 -3 0 57.79 3.30 2 -3 0 61.19 3.40 -2 3 0 62.09 9.20 2 3 0 56.89 3.20 2 3 0 54.29 3.20 2 3 0 55.89 6.60 2 3 0 56.79 3.10 3 -3 0 122.59 6.60 -3 -3 0 119.99 6.50 -3 -3 0 109.89 6.50 3 -3 0 120.79 6.60 3 3 0 113.59 6.40 3 3 0 116.39 6.20 -3 3 0 111.59 6.70 3 3 0 128.69 6.30 -4 -3 0 135.69 7.00 -4 -3 0 130.79 7.40 4 -3 0 114.59 8.10 4 -3 0 126.89 7.30 4 3 0 134.79 7.00 4 3 0 136.09 7.00 -4 3 0 87.79 20.90 -4 3 0 116.09 7.40 4 3 0 124.09 7.10 5 -3 0 130.69 7.20 5 -3 0 97.29 8.20 -5 -3 0 122.49 6.50 -5 -3 0 115.49 7.10 -5 3 0 122.79 7.30 5 3 0 102.49 6.50 5 3 0 113.39 6.70 5 3 0 121.49 6.60 6 -3 0 14.20 2.10 6 -3 0 15.00 2.20 6 -3 0 14.90 1.10 -6 3 0 16.10 2.20 6 3 0 14.00 1.80 6 3 0 14.10 2.10 7 -3 0 8.40 2.00 -7 -3 0 10.00 0.90 -7 -3 0 9.00 0.90 -7 -3 0 7.80 1.30 -7 3 0 9.80 1.40 7 3 0 10.30 1.40 -7 3 0 7.10 1.40 8 -3 0 6.30 0.70 -8 -3 0 5.70 0.80 -8 -3 0 8.10 0.90 -8 -3 0 5.90 1.10 -8 3 0 6.10 1.10 -8 3 0 6.20 0.90 -8 3 0 10.20 2.20 -8 3 0 5.50 0.90 -9 -3 0 9.80 1.00 -9 -3 0 10.10 1.00 9 -3 0 10.10 0.90 -9 -3 0 7.20 1.20 -9 3 0 8.40 1.30 -9 3 0 10.30 1.10 9 3 0 9.40 0.70 -9 3 0 6.80 1.00 -10 -3 0 0.00 0.20 -10 -3 0 0.20 0.30 10 -3 0 0.00 0.20 10 3 0 0.20 0.20 -10 3 0 0.30 0.30 -10 3 0 -0.30 0.20 -10 3 0 0.10 0.30 0 -4 0 1797.02 92.09 0 -4 0 1871.21 96.29 0 4 0 1759.82 95.89 0 4 0 1798.22 92.29 1 -4 0 1232.98 62.49 -1 -4 0 1229.18 62.39 1 -4 0 1215.38 62.59 -1 -4 0 1240.68 66.09 1 -4 0 1294.67 67.99 1 4 0 1220.58 62.59 -1 4 0 1179.18 67.09 -1 4 0 1202.08 62.69 1 4 0 1195.78 65.99 2 -4 0 9.30 0.90 -2 -4 0 9.10 0.80 -2 -4 0 10.50 0.90 -2 -4 0 -4.10 4.80 2 -4 0 9.80 1.20 2 4 0 9.00 0.70 2 4 0 9.20 0.80 -2 4 0 10.00 1.30 -2 4 0 9.40 0.90 2 4 0 10.40 1.00 -2 4 0 8.50 7.90 2 4 0 -0.20 6.10 -3 -4 0 60.99 3.50 -3 -4 0 57.89 3.40 3 -4 0 63.69 3.70 3 -4 0 62.69 3.80 -3 4 0 35.50 12.40 -3 4 0 61.89 3.80 3 4 0 60.79 3.50 3 4 0 54.79 3.30 3 4 0 53.39 3.30 -3 4 0 38.60 15.80 4 -4 0 11.80 1.40 -4 -4 0 11.00 1.00 4 -4 0 11.70 1.40 4 4 0 9.70 1.00 -4 4 0 11.50 1.40 4 4 0 9.20 1.10 4 4 0 8.00 1.00 5 -4 0 55.39 4.00 5 -4 0 56.39 4.10 -5 -4 0 54.79 3.40 5 4 0 47.40 3.40 5 4 0 46.00 3.50 -5 4 0 57.79 4.10 5 4 0 61.19 3.50 5 4 0 54.69 3.40 6 -4 0 14.50 2.40 6 -4 0 18.40 1.20 6 -4 0 16.60 2.40 -6 4 0 20.20 2.40 6 4 0 16.40 1.80 -7 -4 0 32.00 2.00 -7 -4 0 28.60 2.00 7 -4 0 28.50 1.90 -7 4 0 30.30 3.40 -7 4 0 27.00 2.40 -7 4 0 31.30 2.20 -7 4 0 29.00 2.10 8 -4 0 0.70 0.40 -8 -4 0 0.60 0.40 -8 -4 0 0.80 0.40 -8 4 0 -1.30 1.60 -8 4 0 1.10 0.50 -8 4 0 1.20 0.60 -8 4 0 0.90 0.60 -9 -4 0 1.60 0.40 -9 -4 0 1.00 0.50 9 -4 0 2.30 0.40 -9 4 0 3.00 0.60 -9 4 0 2.10 0.50 -9 4 0 2.40 0.70 -10 -4 0 9.20 1.00 10 -4 0 11.10 0.90 -10 4 0 11.50 0.90 -10 4 0 11.80 1.20 -10 4 0 10.50 0.90 0 -5 0 7.70 8.30 0 -5 0 -0.20 0.30 0 5 0 -0.10 0.30 0 5 0 0.00 7.00 1 -5 0 416.26 28.80 -1 -5 0 429.66 26.70 1 -5 0 394.06 21.10 1 -5 0 410.06 21.00 -1 -5 0 410.96 21.00 -1 5 0 400.36 27.60 1 5 0 382.36 26.60 1 5 0 405.46 21.20 -1 5 0 395.46 21.30 -2 -5 0 43.80 2.40 -2 -5 0 48.30 8.40 -2 -5 0 44.30 2.60 2 -5 0 43.90 2.90 2 -5 0 46.00 2.80 2 5 0 42.60 2.70 2 5 0 39.60 2.40 2 5 0 46.90 9.80 -2 5 0 43.20 3.10 -2 5 0 42.70 2.70 2 5 0 38.80 2.50 -2 5 0 18.30 12.30 -3 -5 0 21.90 1.50 3 -5 0 17.20 1.70 -3 -5 0 19.30 1.40 3 -5 0 17.60 1.80 -3 5 0 18.70 19.40 3 5 0 7.40 8.80 -3 5 0 0.00 14.50 3 5 0 19.20 1.40 -3 5 0 19.80 1.70 3 5 0 22.50 1.60 3 5 0 18.70 1.30 4 -5 0 1.50 0.60 -4 -5 0 0.90 0.40 4 -5 0 0.80 0.60 4 5 0 1.30 0.60 4 5 0 0.20 0.50 4 5 0 0.90 0.40 -4 5 0 0.80 0.60 -5 -5 0 9.40 1.20 5 -5 0 9.70 1.70 5 -5 0 10.40 1.80 5 -5 0 10.10 0.80 5 5 0 10.40 1.30 5 5 0 8.50 1.20 -5 5 0 9.80 1.60 6 -5 0 -0.60 1.20 6 -5 0 2.00 0.40 6 -5 0 0.90 1.40 -6 5 0 3.50 1.30 7 -5 0 89.99 5.00 -7 -5 0 97.69 5.10 -7 -5 0 92.19 5.10 7 -5 0 85.19 7.00 -7 5 0 91.09 5.60 -7 5 0 84.39 5.20 -7 5 0 82.39 6.50 -7 5 0 93.09 5.30 -8 -5 0 10.40 1.10 8 -5 0 9.90 1.00 -8 -5 0 9.50 1.00 -8 5 0 8.90 2.20 -8 5 0 8.40 1.30 -8 5 0 9.70 1.20 -8 5 0 9.00 1.10 -9 -5 0 4.00 0.60 9 -5 0 4.50 0.60 -9 -5 0 3.50 0.60 -9 5 0 5.20 0.90 -9 5 0 3.50 0.70 -9 5 0 5.30 0.70 -10 -5 0 1.50 0.40 -10 -5 0 1.50 0.40 10 -5 0 2.20 0.40 -10 5 0 2.30 0.50 -10 5 0 2.10 0.50 -10 5 0 2.70 0.40 0 -6 0 270.97 13.90 0 -6 0 282.07 23.60 0 -6 0 259.97 13.90 0 6 0 257.47 14.20 1 -6 0 53.99 3.50 1 -6 0 67.79 15.20 -1 -6 0 29.80 11.60 -1 -6 0 56.69 3.20 1 -6 0 55.99 3.40 1 6 0 54.89 3.50 -1 6 0 51.09 3.70 -1 6 0 53.49 3.60 -1 6 0 54.69 12.50 1 6 0 58.19 12.30 2 -6 0 181.58 9.90 -2 -6 0 169.68 19.40 2 -6 0 188.38 9.80 -2 -6 0 175.28 9.50 -2 6 0 124.89 20.20 -2 6 0 184.38 9.70 2 6 0 162.68 9.70 -2 6 0 180.68 10.10 3 -6 0 11.60 1.50 -3 -6 0 12.80 1.20 3 -6 0 9.20 1.30 -3 6 0 14.40 23.70 3 6 0 12.00 1.30 3 6 0 13.70 1.30 -3 6 0 10.50 1.30 4 -6 0 2.80 1.00 -4 -6 0 2.50 0.60 4 -6 0 4.30 1.00 4 6 0 1.90 0.70 -4 6 0 2.70 0.90 5 -6 0 0.60 0.30 -5 -6 0 1.00 0.60 5 -6 0 -0.10 1.00 5 -6 0 0.70 1.10 5 6 0 0.90 0.60 -5 6 0 1.00 0.80 5 6 0 -0.50 0.60 -6 -6 0 7.00 1.30 6 -6 0 10.20 2.10 6 6 0 7.60 1.30 7 -6 0 90.09 5.00 -7 -6 0 83.89 5.00 -7 -6 0 82.29 5.00 -7 6 0 100.99 5.30 -7 6 0 88.79 5.50 -7 6 0 88.49 6.60 -7 6 0 84.79 5.10 8 -6 0 3.50 0.50 -8 -6 0 1.00 0.40 -8 -6 0 1.90 0.50 -8 6 0 1.50 1.80 -8 6 0 2.40 0.60 -8 6 0 2.20 0.60 -8 6 0 2.30 0.80 9 -6 0 -0.10 0.30 -9 -6 0 0.00 0.30 -9 -6 0 0.80 0.40 -9 6 0 -0.10 0.40 -9 6 0 0.20 0.30 -9 6 0 0.10 0.30 0 -7 0 0.30 0.30 0 -7 0 0.00 0.50 0 -7 0 12.80 15.30 0 7 0 0.00 0.30 0 7 0 -1.70 12.90 0 7 0 0.60 0.60 -1 -7 0 17.50 15.10 -1 -7 0 0.60 0.30 1 -7 0 -0.80 0.80 1 -7 0 -29.50 17.50 1 -7 0 -0.40 0.50 -1 7 0 1.70 14.60 1 7 0 0.10 0.50 -1 7 0 0.20 0.60 1 7 0 0.50 0.40 1 7 0 -1.30 13.50 -1 7 0 -0.20 0.30 -2 -7 0 438.66 35.30 2 -7 0 474.85 23.70 -2 -7 0 456.35 23.40 2 -7 0 468.25 23.30 2 -7 0 455.65 23.90 2 7 0 428.76 23.60 -2 7 0 426.96 44.80 -2 7 0 428.16 23.20 2 7 0 345.07 36.10 -2 7 0 451.45 24.00 3 -7 0 2.00 1.40 -3 -7 0 0.00 0.30 3 -7 0 -0.50 0.60 3 7 0 0.50 0.50 -3 7 0 0.30 0.50 3 7 0 -15.10 20.90 -4 -7 0 74.99 4.80 4 -7 0 77.69 5.70 4 -7 0 84.79 5.50 4 7 0 76.49 4.90 4 7 0 74.59 4.80 -4 7 0 84.39 5.80 5 -7 0 8.40 2.20 -5 -7 0 6.80 1.20 5 -7 0 7.30 1.70 -5 7 0 6.90 1.40 5 7 0 10.40 1.40 5 7 0 7.40 1.20 6 -7 0 380.36 21.80 6 -7 0 383.16 19.60 -6 -7 0 365.06 19.60 -6 7 0 373.06 19.70 -6 7 0 380.86 20.10 -6 7 0 366.36 20.40 -6 7 0 383.86 21.20 7 -7 0 24.70 1.70 -7 7 0 25.40 3.20 -7 7 0 21.40 2.20 -8 -7 0 11.40 1.00 -8 -7 0 9.30 1.20 8 -7 0 9.00 1.10 -8 7 0 9.70 1.20 -8 7 0 7.50 2.10 -8 7 0 12.20 1.10 -8 7 0 10.30 1.80 9 -7 0 5.40 0.60 -9 -7 0 5.30 0.60 -9 7 0 6.00 0.70 -9 7 0 6.40 1.00 -9 7 0 4.00 0.80 0 -8 0 126.79 6.90 0 -8 0 126.09 6.90 0 8 0 116.49 6.80 0 8 0 121.09 7.50 0 8 0 129.19 7.00 -1 -8 0 106.69 5.70 1 -8 0 90.29 5.60 1 -8 0 104.29 5.90 1 8 0 99.19 6.10 -1 8 0 47.00 24.60 -1 8 0 100.99 5.70 -1 8 0 99.19 6.30 -1 8 0 99.39 5.60 1 8 0 90.19 5.40 2 -8 0 224.08 13.50 -2 -8 0 270.27 13.70 2 -8 0 266.87 14.10 2 8 0 272.97 14.10 -2 8 0 240.28 13.50 -2 8 0 257.77 13.80 -2 8 0 306.87 47.30 -2 8 0 250.57 14.50 -3 -8 0 3.40 0.70 3 -8 0 3.00 1.50 3 -8 0 1.50 0.90 -3 8 0 3.00 0.80 3 8 0 3.00 0.90 4 -8 0 116.59 6.40 -4 -8 0 116.49 6.90 4 -8 0 127.59 7.70 4 -8 0 105.39 10.00 4 8 0 119.09 7.00 -4 8 0 116.29 7.40 4 8 0 120.19 7.10 5 -8 0 0.70 1.50 5 -8 0 -4.00 2.00 5 -8 0 0.30 0.30 -5 -8 0 0.40 0.60 5 8 0 1.40 0.70 -5 8 0 -0.50 0.70 5 8 0 0.40 0.80 6 -8 0 10.20 1.00 6 -8 0 10.50 3.30 -6 8 0 8.40 1.10 -6 8 0 9.90 2.00 -6 8 0 7.30 1.20 -6 8 0 8.00 0.90 -7 -8 0 7.90 0.90 7 -8 0 7.50 0.90 -7 8 0 8.10 1.10 -7 8 0 6.00 1.80 -7 8 0 7.10 0.90 -7 8 0 8.70 1.20 -8 -8 0 -0.20 0.30 8 -8 0 0.30 0.30 -8 8 0 0.30 0.50 -8 8 0 0.70 0.40 -8 8 0 0.10 0.40 9 -8 0 0.60 0.40 -9 -8 0 -0.10 0.30 -9 8 0 0.00 0.30 -9 8 0 0.60 0.40 -9 8 0 0.40 0.30 0 -9 0 2.10 0.60 0 9 0 2.00 1.00 0 9 0 2.70 0.70 -1 -9 0 402.26 20.20 1 -9 0 396.56 20.80 1 -9 0 371.46 20.10 1 9 0 389.86 20.80 -1 9 0 378.76 20.20 1 9 0 402.96 20.30 1 9 0 350.16 19.90 -1 9 0 377.66 20.20 -1 9 0 364.46 20.90 2 -9 0 -0.80 1.00 -2 -9 0 1.40 0.60 2 9 0 1.00 0.60 2 9 0 1.40 0.80 -2 9 0 0.60 0.60 3 -9 0 1.70 1.10 -3 -9 0 0.00 0.40 3 9 0 0.40 0.50 3 9 0 -0.10 0.70 -3 9 0 0.10 0.70 4 -9 0 1.00 0.50 -4 -9 0 0.10 0.50 4 -9 0 1.00 1.40 4 9 0 2.40 0.90 -4 9 0 1.30 0.80 4 9 0 0.00 0.60 -5 -9 0 95.69 6.00 -5 -9 0 106.29 6.70 -5 -9 0 102.59 6.70 5 -9 0 116.09 6.20 -5 9 0 117.59 6.50 -5 9 0 114.19 6.30 -5 9 0 123.69 7.70 5 9 0 109.59 6.80 5 9 0 107.39 6.60 -6 -9 0 234.48 12.80 -6 -9 0 247.68 12.80 6 -9 0 236.48 12.80 -6 -9 0 244.18 13.70 -6 9 0 240.28 13.30 -6 9 0 247.78 13.20 -6 9 0 259.57 14.70 6 9 0 252.87 13.90 -6 9 0 228.28 12.90 -7 -9 0 7.80 0.90 7 -9 0 9.20 1.00 -7 9 0 11.10 1.10 -7 9 0 8.00 2.10 -7 9 0 9.20 1.20 -7 9 0 11.20 1.40 8 -9 0 1.30 0.40 -8 -9 0 2.30 0.50 -8 9 0 1.80 0.50 -8 9 0 2.40 0.60 -8 9 0 2.10 0.60 9 -9 0 10.90 0.90 -9 9 0 11.00 1.00 -9 9 0 8.00 0.90 -9 9 0 9.30 0.80 0 -10 0 493.45 25.20 0 10 0 463.95 25.00 0 10 0 456.25 24.50 0 10 0 495.65 25.30 0 10 0 475.25 26.70 -1 -10 0 2.10 0.70 1 -10 0 2.40 0.80 1 10 0 1.50 1.00 -1 10 0 2.30 0.80 -1 10 0 1.60 0.70 1 10 0 2.00 0.30 -1 10 0 1.60 1.30 1 10 0 1.60 0.60 1 10 0 2.30 0.90 -2 -10 0 35.60 2.70 2 10 0 35.60 2.70 2 10 0 36.60 3.30 2 10 0 33.70 2.00 -2 10 0 35.80 2.90 3 -10 0 3.00 2.80 -3 -10 0 1.40 0.60 3 10 0 1.00 0.20 -3 10 0 1.80 0.90 3 10 0 1.10 0.70 -4 -10 0 24.20 1.60 -4 -10 0 24.90 2.60 4 10 0 20.40 1.40 -4 10 0 29.80 3.00 4 10 0 26.50 2.60 4 10 0 20.30 2.50 5 -10 0 12.90 1.50 -5 -10 0 17.60 2.00 -5 -10 0 18.00 1.30 -5 10 0 14.80 2.50 5 10 0 17.50 2.10 5 10 0 17.50 1.10 5 10 0 18.60 2.40 -5 10 0 13.30 1.40 -5 10 0 13.30 1.50 -6 -10 0 22.40 1.90 -6 -10 0 24.50 2.60 -6 -10 0 25.70 1.70 6 10 0 23.30 1.40 6 10 0 20.40 2.50 -6 10 0 21.60 3.00 -6 10 0 20.50 2.00 -6 10 0 23.50 2.00 -6 10 0 22.00 2.10 -7 -10 0 32.90 2.10 7 -10 0 34.10 2.30 -7 10 0 29.40 2.30 -7 10 0 35.10 3.60 -7 10 0 33.50 2.50 -7 10 0 33.40 2.20 8 -10 0 13.10 1.10 8 10 0 10.50 0.80 -8 10 0 10.30 1.10 -8 10 0 11.00 1.00 -8 10 0 11.40 1.10 0 -11 0 -0.20 0.50 0 11 0 0.60 0.20 0 11 0 1.80 1.40 0 11 0 0.20 0.60 1 -11 0 161.78 9.20 -1 -11 0 164.78 9.30 1 11 0 157.58 10.00 -1 11 0 161.08 9.30 1 11 0 167.58 9.40 -1 11 0 156.18 10.40 -1 11 0 152.78 9.20 1 11 0 164.88 8.40 -1 11 0 151.28 8.40 -2 -11 0 34.00 2.70 2 11 0 36.30 3.50 2 11 0 35.80 2.90 -2 11 0 30.30 2.90 2 11 0 33.30 2.00 -3 -11 0 23.20 1.70 3 -11 0 25.70 2.20 -3 -11 0 24.00 2.30 -3 11 0 26.60 2.00 3 11 0 26.50 3.00 3 11 0 24.30 2.50 3 11 0 24.00 1.50 4 -11 0 7.40 1.00 -4 -11 0 5.40 0.70 -4 -11 0 4.60 1.10 -4 11 0 7.70 1.80 4 11 0 3.60 1.10 -4 11 0 6.90 1.00 4 11 0 5.40 0.50 4 11 0 3.80 1.50 -4 11 0 7.50 1.10 5 -11 0 16.40 2.00 -5 -11 0 15.10 1.70 -5 11 0 15.20 2.00 5 11 0 13.90 1.30 -5 11 0 16.60 2.00 5 11 0 14.60 2.40 6 -11 0 16.00 1.50 -6 -11 0 17.90 1.40 -6 -11 0 17.40 2.30 -6 11 0 14.50 1.70 6 11 0 18.80 1.20 6 11 0 15.30 2.30 -6 11 0 16.40 2.80 7 -11 0 8.40 1.00 -7 -11 0 10.00 1.00 -7 11 0 7.40 1.00 7 11 0 9.10 0.70 8 -11 0 0.10 0.30 8 11 0 0.10 0.30 -8 11 0 -0.40 0.30 0 -12 0 9.90 1.50 0 12 0 10.60 0.90 0 12 0 11.50 2.40 0 12 0 11.60 1.70 0 12 0 9.70 1.60 1 -12 0 124.49 6.50 -1 -12 0 113.89 7.00 1 -12 0 107.69 6.70 -1 12 0 108.99 6.30 -1 12 0 101.59 6.70 -1 12 0 103.29 5.90 1 12 0 105.69 7.70 -1 12 0 105.99 6.90 1 12 0 119.19 7.30 1 12 0 105.59 6.20 -2 -12 0 15.90 1.80 2 -12 0 9.80 1.90 -2 -12 0 15.20 1.20 -2 -12 0 18.00 1.50 2 -12 0 13.60 1.60 -2 12 0 12.30 2.00 2 12 0 16.90 2.50 2 12 0 16.60 1.10 2 12 0 15.10 1.90 -2 12 0 12.30 1.40 3 -12 0 0.60 0.60 -3 -12 0 -0.20 0.50 -3 -12 0 0.20 0.70 -3 -12 0 1.00 0.40 3 -12 0 1.40 0.60 -3 12 0 0.00 1.00 3 12 0 -0.30 1.40 3 12 0 0.70 0.30 -3 12 0 0.20 0.60 3 12 0 -0.10 0.70 4 -12 0 24.10 2.00 -4 -12 0 24.50 1.70 -4 -12 0 23.60 2.40 -4 12 0 20.20 3.20 4 12 0 21.70 2.50 4 12 0 24.70 1.50 -4 12 0 24.30 2.00 -5 -12 0 1.20 0.90 5 -12 0 1.30 0.50 -5 -12 0 1.00 0.40 -5 12 0 0.60 0.60 -5 12 0 1.20 0.60 5 12 0 0.50 0.20 5 12 0 0.90 0.90 -5 12 0 1.00 1.30 -6 -12 0 1.20 0.50 6 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4 35.10 2.50 4 9 -4 34.30 2.90 -4 9 4 32.40 2.50 -4 9 4 34.60 3.50 4 9 -4 36.50 2.80 -3 -9 4 0.40 0.50 -3 -9 4 1.10 0.90 3 9 -4 0.90 1.30 3 9 -4 0.70 0.60 -3 9 4 -0.20 0.90 3 9 -4 -0.10 0.30 -2 -9 4 9.50 1.30 2 9 -4 9.80 1.30 2 9 -4 6.50 1.40 2 9 -4 6.90 0.60 -2 9 4 10.00 1.50 -1 -9 4 99.19 7.00 -1 -9 4 106.49 6.20 1 9 -4 102.29 6.00 1 9 -4 100.09 6.70 -1 9 4 109.99 6.70 1 9 -4 92.59 5.30 0 -9 4 41.20 2.90 0 -9 4 34.30 3.80 0 9 4 40.30 3.90 0 9 -4 43.70 3.70 0 9 -4 38.00 2.80 0 9 -4 41.40 2.20 0 9 4 37.00 3.10 1 -9 4 22.30 1.80 1 -9 4 19.10 3.00 1 9 4 24.40 2.30 -1 9 -4 23.00 2.00 1 9 4 25.90 3.10 -1 9 -4 21.20 1.40 1 9 4 24.30 1.50 2 -9 4 395.66 22.50 2 9 4 401.86 21.90 -2 9 -4 426.06 21.50 2 9 4 398.46 20.80 2 9 4 386.46 22.50 3 -9 4 1.60 1.60 3 9 4 2.40 1.40 -3 9 -4 -0.30 0.50 3 9 4 1.40 0.80 3 9 4 0.80 0.30 -4 -9 -4 24.90 1.90 -4 -9 -4 25.10 1.90 -4 -9 -4 26.40 1.90 -4 9 -4 25.60 2.00 4 9 4 29.20 2.80 4 9 4 28.20 1.70 -4 9 -4 24.70 2.60 4 9 4 28.50 3.40 -5 -9 -4 184.48 10.00 -5 -9 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-5 6 13 0.50 0.30 -4 -6 13 30.00 1.70 -4 -6 13 28.90 1.60 4 -6 -13 27.40 1.70 4 -6 -13 26.00 1.70 4 6 -13 26.70 1.60 -4 6 13 24.70 1.80 -4 6 13 25.60 1.70 4 6 -13 22.20 1.70 -3 -6 13 20.50 1.30 -3 -6 13 17.00 1.40 3 -6 -13 19.50 1.40 3 -6 -13 19.00 1.80 3 6 -13 18.40 1.50 -3 6 13 18.80 1.60 3 6 -13 20.90 1.20 -3 6 13 17.00 1.40 -3 6 13 20.10 1.40 -2 -6 13 11.70 0.90 -2 -6 13 9.10 1.00 -2 -6 13 10.00 0.90 2 -6 -13 10.50 1.00 -2 6 13 10.30 1.00 2 6 -13 9.50 1.00 2 6 -13 9.80 0.90 -1 -6 13 2.80 0.50 -1 -6 13 2.80 0.60 1 -6 -13 3.60 0.60 -1 6 13 3.80 0.60 1 6 -13 2.80 0.60 0 -6 13 1.30 0.30 0 -6 -13 1.00 0.40 0 6 -13 1.80 0.50 0 6 13 1.20 0.40 -1 -6 -13 2.30 0.40 1 -6 13 2.20 0.40 -1 6 -13 2.50 0.50 1 6 13 2.40 0.50 -2 -6 -13 0.80 0.40 -2 6 -13 0.20 0.40 -3 -6 -13 18.70 1.30 -3 6 -13 18.50 1.40 3 6 13 18.40 1.30 4 -7 -13 3.50 0.50 -4 -7 13 3.40 0.50 -4 -7 13 3.90 0.50 -4 7 13 4.10 0.60 4 7 -13 3.20 0.40 -4 7 13 4.40 0.60 3 -7 -13 0.30 0.30 -3 -7 13 0.30 0.30 -3 -7 13 0.50 0.30 -3 -7 13 0.50 0.30 -3 7 13 -0.10 0.20 3 7 -13 0.10 0.20 3 7 -13 0.30 0.20 -2 -7 13 2.50 0.50 2 -7 -13 4.00 0.70 -2 -7 13 3.50 0.50 2 7 -13 3.30 0.50 -2 7 13 3.90 0.70 2 7 -13 2.80 0.40 1 -7 -13 0.40 0.30 -1 7 13 -0.10 0.30 1 7 -13 0.40 0.40 0 -7 -13 14.00 1.20 0 -7 13 13.00 1.00 0 7 -13 11.70 1.30 0 7 13 14.60 1.20 -1 -7 -13 0.50 0.40 -1 7 -13 0.70 0.30 -2 -7 -13 6.90 0.70 2 7 13 7.50 0.80 -2 7 -13 5.90 0.70 -3 -7 -13 0.60 0.30 3 7 13 0.50 0.30 -3 7 -13 1.00 0.30 3 -8 -13 14.90 1.10 -3 -8 13 15.70 1.20 -3 -8 13 16.10 1.00 3 8 -13 14.40 1.00 -3 8 13 15.80 1.10 -2 -8 13 1.50 0.30 2 -8 -13 1.00 0.40 2 8 -13 1.50 0.40 -2 8 13 1.30 0.40 2 8 -13 1.40 0.30 -1 -8 13 16.90 1.10 1 -8 -13 19.00 1.30 -1 8 13 16.90 1.30 1 8 -13 14.50 1.20 0 -8 -13 0.00 0.30 0 -8 13 0.20 0.20 0 8 -13 -0.10 0.20 0 8 13 0.10 0.30 -1 -8 -13 17.90 1.30 -1 8 -13 18.40 1.30 1 8 13 18.90 1.40 -2 -8 -13 0.00 0.20 2 8 13 -0.20 0.20 -2 8 -13 0.10 0.20 -2 -9 13 28.40 1.60 -2 -9 13 27.70 1.60 2 -9 -13 25.10 1.70 1 -9 -13 22.00 1.50 -1 9 13 24.20 1.60 0 -9 -13 6.00 0.60 0 -9 13 5.80 0.50 0 9 13 6.30 0.70 0 9 -13 4.80 0.50 -1 -9 -13 3.50 0.50 1 9 13 4.10 0.60 -5 0 14 1.60 0.30 4 0 -14 2.50 0.50 -4 0 14 2.90 0.60 -4 0 14 2.20 0.40 4 0 -14 1.80 0.40 -4 0 14 2.40 0.40 -3 0 14 0.80 0.40 -3 0 14 1.00 0.40 3 0 -14 0.30 0.40 -3 0 14 0.40 0.40 -2 0 14 127.29 7.30 -2 0 14 131.99 7.20 2 0 -14 134.49 7.40 1 0 -14 38.70 2.50 -1 0 14 38.70 2.40 -1 0 14 34.80 2.50 0 0 -14 56.19 3.40 0 0 14 56.29 3.50 0 0 14 56.69 3.40 -1 0 -14 24.70 1.80 1 0 14 25.40 2.00 2 0 14 41.70 2.50 -2 0 -14 44.60 2.60 -3 0 -14 122.99 6.60 -4 -1 14 0.80 0.30 4 -1 -14 1.00 0.40 -4 -1 14 1.00 0.30 -4 -1 14 1.20 0.40 4 1 -14 0.80 0.30 -4 1 14 0.90 0.30 -4 1 14 0.90 0.40 4 1 -14 1.50 0.40 -4 1 14 1.10 0.30 -3 -1 14 1.60 0.40 -3 -1 14 2.00 0.60 3 -1 -14 1.20 0.50 -3 -1 14 1.10 0.50 -3 1 14 1.40 0.40 3 1 -14 1.40 0.50 -3 1 14 0.90 0.50 2 -1 -14 0.00 0.30 -2 -1 14 1.20 0.40 -2 -1 14 1.90 0.50 -2 1 14 0.60 0.30 -2 1 14 0.20 0.30 2 1 -14 0.70 0.40 -1 -1 14 39.20 2.40 -1 -1 14 37.70 2.50 1 -1 -14 38.10 2.50 -1 1 14 37.80 2.50 -1 1 14 38.20 2.40 1 1 -14 34.60 2.50 0 -1 -14 0.20 0.30 0 -1 14 0.40 0.30 0 -1 14 -0.10 0.30 0 1 -14 0.00 0.30 0 1 14 0.10 0.30 0 1 14 -0.40 0.20 -1 -1 -14 81.89 4.70 1 -1 14 77.39 5.00 -1 1 -14 79.69 4.60 1 1 14 82.29 4.80 -2 -1 -14 56.49 3.30 2 -1 14 54.79 3.20 -2 1 -14 59.29 3.40 2 1 14 59.69 3.30 -3 -1 -14 10.00 0.90 -3 1 -14 9.00 0.90 -4 -2 14 0.30 0.30 -4 -2 14 0.30 0.30 -4 -2 14 0.20 0.20 4 -2 -14 0.40 0.30 -4 2 14 0.40 0.30 4 2 -14 0.20 0.30 -4 2 14 0.00 0.30 -4 2 14 0.00 0.20 4 2 -14 0.10 0.30 -3 -2 14 0.00 0.30 -3 -2 14 0.20 0.40 3 -2 -14 0.30 0.30 -3 -2 14 0.40 0.50 -3 2 14 -0.20 0.30 3 2 -14 0.00 0.30 3 2 -14 0.20 0.30 -2 -2 14 8.20 0.80 2 -2 -14 8.00 1.00 -2 -2 14 7.90 1.00 -2 2 14 7.30 0.80 -2 2 14 8.20 0.90 2 2 -14 6.50 0.90 -1 -2 14 1.70 0.50 -1 -2 14 1.50 0.40 1 -2 -14 1.50 0.40 1 2 -14 1.90 0.50 -1 2 14 1.00 0.40 -1 2 14 1.90 0.50 0 -2 -14 42.70 2.50 0 -2 14 38.90 2.40 0 -2 14 34.40 2.50 0 2 -14 36.70 2.50 0 2 14 40.80 2.50 0 2 14 41.30 2.50 -1 -2 -14 10.70 0.90 1 -2 14 10.00 0.90 -1 2 -14 9.00 1.00 -2 -2 -14 0.20 0.30 -2 2 -14 0.10 0.20 2 2 14 0.40 0.30 -3 -2 -14 1.20 0.30 -3 2 -14 1.20 0.30 -4 -3 14 5.30 0.50 -4 -3 14 6.10 0.70 4 -3 -14 5.60 0.70 -4 -3 14 4.40 0.70 -4 3 14 6.30 0.70 -4 3 14 4.80 0.60 -4 3 14 6.50 0.80 4 3 -14 4.40 0.50 4 3 -14 5.60 0.70 -3 -3 14 8.30 0.70 -3 -3 14 7.50 0.90 -3 -3 14 7.00 0.70 3 -3 -14 8.30 0.90 -3 3 14 9.30 0.90 -3 3 14 9.30 0.90 3 3 -14 8.50 0.90 2 -3 -14 0.80 0.40 2 -3 -14 0.60 0.40 -2 -3 14 1.70 0.50 2 3 -14 1.80 0.50 -2 3 14 0.80 0.30 -2 3 14 1.30 0.40 1 -3 -14 6.20 0.80 -1 -3 14 8.10 0.80 1 -3 -14 7.10 0.80 -1 -3 14 7.80 0.90 -1 3 14 7.40 0.80 -1 3 14 7.00 0.80 1 3 -14 9.40 1.00 0 -3 -14 42.40 2.50 0 -3 -14 43.00 2.60 0 3 -14 36.70 2.60 0 3 14 44.30 2.60 -1 -3 -14 11.30 0.90 1 -3 14 9.90 0.80 -1 -3 -14 9.10 0.80 -1 3 -14 9.80 1.00 -2 -3 -14 39.60 2.50 -2 -3 -14 40.80 2.50 -2 3 -14 42.30 2.60 2 3 14 45.60 2.50 -3 -3 -14 2.00 0.30 -4 -4 14 11.90 0.90 4 -4 -14 11.70 1.00 -4 -4 14 13.60 0.90 -4 -4 14 10.00 1.00 -4 4 14 13.40 0.90 -4 4 14 11.40 1.00 -4 4 14 13.30 0.90 3 -4 -14 0.20 0.30 3 -4 -14 0.50 0.30 -3 -4 14 0.10 0.30 -3 -4 14 0.10 0.30 -3 -4 14 0.50 0.30 3 4 -14 0.00 0.30 -3 4 14 0.40 0.30 -3 4 14 0.90 0.30 3 4 -14 0.00 0.30 -2 -4 14 0.30 0.30 2 -4 -14 0.50 0.30 2 -4 -14 0.40 0.30 -2 -4 14 0.50 0.40 -2 4 14 0.50 0.30 -2 4 14 0.40 0.30 2 4 -14 0.40 0.30 1 -4 -14 17.50 1.30 1 -4 -14 17.10 1.30 -1 -4 14 16.80 1.40 1 4 -14 17.30 1.40 -1 4 14 18.00 1.30 -1 4 14 18.40 1.40 0 -4 -14 0.20 0.30 0 -4 14 0.50 0.30 0 -4 -14 0.00 0.30 0 4 14 -0.20 0.40 0 4 -14 0.10 0.30 -1 -4 -14 0.40 0.30 1 -4 14 0.50 0.30 1 4 14 0.30 0.30 -1 4 -14 0.40 0.30 -2 -4 -14 5.70 0.60 -2 4 -14 4.60 0.70 2 4 14 6.30 0.70 -3 -4 -14 3.10 0.40 3 4 14 3.70 0.60 -3 4 -14 3.30 0.50 -3 -5 14 6.80 0.80 -3 -5 14 7.90 0.70 3 -5 -14 9.40 0.80 3 -5 -14 8.00 0.70 -3 -5 14 8.90 0.70 -3 5 14 8.60 0.70 3 5 -14 7.30 0.80 -3 5 14 9.90 0.80 2 -5 -14 10.80 0.90 -2 -5 14 10.80 1.10 2 -5 -14 10.60 1.00 -2 5 14 13.40 1.00 2 5 -14 12.70 1.10 -2 5 14 12.60 0.90 1 -5 -14 -0.10 0.30 -1 -5 14 0.40 0.30 1 5 -14 0.20 0.30 -1 5 14 0.40 0.30 0 -5 -14 18.10 1.30 0 -5 14 17.00 1.20 0 5 14 19.90 1.40 0 5 -14 18.90 1.40 -1 -5 -14 12.10 0.90 1 -5 14 10.60 0.80 1 5 14 12.60 1.00 -1 5 -14 11.50 1.00 -2 -5 -14 19.90 1.50 -2 5 -14 19.50 1.40 2 5 14 20.70 1.40 -3 -6 14 5.80 0.50 -3 -6 14 6.00 0.50 -3 -6 14 3.70 0.60 3 -6 -14 4.10 0.50 -3 6 14 4.50 0.50 3 6 -14 5.30 0.60 -2 -6 14 0.40 0.20 2 -6 -14 -0.20 0.20 -2 6 14 0.10 0.20 2 6 -14 0.30 0.20 -1 -6 14 26.20 1.60 1 -6 -14 29.30 1.80 1 6 -14 23.50 1.80 -1 6 14 29.90 1.80 0 -6 14 13.80 1.10 0 -6 -14 14.70 1.10 0 6 14 14.60 1.10 0 6 -14 12.40 1.10 -1 -6 -14 2.20 0.40 1 6 14 2.50 0.50 -1 6 -14 1.30 0.40 -2 -6 -14 4.60 0.50 -2 6 -14 6.10 0.70 2 6 14 5.10 0.60 2 -7 -14 1.60 0.40 -2 -7 14 2.20 0.40 2 7 -14 1.60 0.30 -2 7 14 1.80 0.50 1 -7 -14 0.90 0.30 -1 -7 14 0.70 0.30 1 7 -14 0.80 0.40 -1 7 14 1.60 0.40 0 -7 -14 0.30 0.30 0 7 -14 0.80 0.30 0 7 14 1.60 0.40 -1 -7 -14 2.30 0.40 -1 7 -14 2.20 0.40 1 7 14 3.30 0.50 -3 0 15 0.00 0.20 -3 0 15 0.30 0.30 3 0 -15 0.10 0.30 2 0 -15 0.10 0.20 -2 0 15 0.10 0.20 -2 0 15 -0.10 0.20 -1 0 15 -0.10 0.20 1 0 -15 0.00 0.20 -1 0 15 0.50 0.30 0 0 15 -0.10 0.20 0 0 -15 0.10 0.20 1 0 15 0.50 0.30 3 -1 -15 3.30 0.50 3 1 -15 3.10 0.50 -2 -1 15 3.50 0.60 2 -1 -15 3.70 0.50 -2 -1 15 4.50 0.60 2 1 -15 3.50 0.50 -2 1 15 4.90 0.60 -2 1 15 4.30 0.50 1 -1 -15 0.20 0.20 -1 -1 15 0.00 0.20 -1 -1 15 0.10 0.20 -1 1 15 0.20 0.30 1 1 -15 -0.10 0.20 -1 1 15 0.40 0.30 0 -1 -15 13.80 1.00 0 -1 15 13.00 1.00 0 1 -15 13.50 1.10 0 1 15 13.60 1.10 1 -1 15 0.40 0.30 -1 -1 -15 0.50 0.20 -1 1 -15 0.10 0.20 1 1 15 1.00 0.30 -2 -2 15 1.90 0.30 -2 -2 15 2.00 0.40 2 -2 -15 2.90 0.50 -2 2 15 2.80 0.40 -2 2 15 2.80 0.50 2 2 -15 2.10 0.40 1 -2 -15 1.10 0.40 -1 -2 15 1.60 0.30 1 2 -15 1.00 0.30 -1 2 15 0.60 0.30 0 -2 -15 11.30 0.90 0 -2 15 13.30 1.00 0 2 15 12.40 1.00 0 2 -15 12.70 1.00 1 -2 15 15.30 1.00 -1 -2 -15 15.90 1.10 -1 2 -15 17.50 1.20 1 2 15 16.20 1.10 2 -3 -15 5.50 0.60 -2 -3 15 4.70 0.50 -2 -3 15 4.60 0.60 -2 3 15 6.20 0.60 2 3 -15 4.10 0.60 -2 3 15 5.20 0.60 1 -3 -15 0.90 0.30 -1 -3 15 0.80 0.30 1 3 -15 0.70 0.30 -1 3 15 1.50 0.40 0 -3 15 10.70 0.80 0 -3 -15 9.30 0.80 0 3 -15 10.80 0.90 0 3 15 12.00 0.90 1 -3 15 1.10 0.30 1 3 15 1.00 0.30 -1 -4 15 8.30 0.70 1 4 -15 10.60 0.90 -1 4 15 7.80 0.80 0 -4 15 7.20 0.60 0 4 -15 6.90 0.70 0 4 15 9.00 1.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 80907 _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 Nitrendipine _olex2_submission_special_instructions 'No special instructions were received' 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 0.2704(2) 0.35621(10) 0.56701(11) 0.0512(4) Uani 1 1 d . . . . . O1 O 0.11298(18) 0.37375(10) 0.69349(13) 0.0498(4) Uani 1 1 d . . . . . N1 N 0.3482(2) 0.17239(11) 0.85662(14) 0.0437(4) Uani 1 1 d . . . . . O3 O 0.6468(3) 0.13050(13) 0.32761(14) 0.0703(6) Uani 1 1 d . . . . . O6 O 0.7387(2) 0.21000(15) 0.63297(15) 0.0686(6) Uani 1 1 d . . . . . O4 O 0.4789(3) 0.04469(14) 0.25243(14) 0.0803(7) Uani 1 1 d . . . . . N2 N 0.5261(3) 0.08904(14) 0.32555(14) 0.0586(6) Uani 1 1 d . . . . . O5 O 0.8061(2) 0.13383(15) 0.7749(2) 0.0873(7) Uani 1 1 d . . . . . C4 C 0.3035(2) 0.26486(12) 0.71285(14) 0.0356(4) Uani 1 1 d . . . . . C3 C 0.2293(2) 0.33446(13) 0.65138(15) 0.0382(4) Uani 1 1 d . . . . . C5 C 0.2580(2) 0.23377(13) 0.80424(15) 0.0377(4) Uani 1 1 d . . . . . C11 C 0.3957(2) 0.15955(13) 0.58038(15) 0.0392(5) Uani 1 1 d . . . . . C10 C 0.4408(2) 0.22622(13) 0.66471(15) 0.0388(5) Uani 1 1 d . . . . . H10 H 0.496495 0.274680 0.632075 0.047 Uiso 1 1 calc R U . . . C9 C 0.5490(2) 0.18416(14) 0.74667(16) 0.0437(5) Uani 1 1 d . . . . . C13 C 0.4358(3) 0.09375(14) 0.41681(16) 0.0485(5) Uani 1 1 d . . . . . C16 C 0.2807(3) 0.09926(13) 0.59249(16) 0.0438(5) Uani 1 1 d . . . . . H16 H 0.227222 0.099872 0.653887 0.053 Uiso 1 1 calc R U . . . C7 C 0.4967(3) 0.15551(14) 0.83582(17) 0.0454(5) Uani 1 1 d . . . . . C6 C 0.1202(3) 0.25743(15) 0.85926(16) 0.0458(5) Uani 1 1 d . . . . . H6A H 0.089597 0.207847 0.900768 0.069 Uiso 1 1 calc R U . . . H6B H 0.037170 0.272585 0.808565 0.069 Uiso 1 1 calc R U . . . H6C H 0.143167 0.307387 0.904594 0.069 Uiso 1 1 calc R U . . . C12 C 0.4750(3) 0.15641(14) 0.49096(15) 0.0428(5) Uani 1 1 d . . . . . H12 H 0.554724 0.196532 0.480792 0.051 Uiso 1 1 calc R U . . . C14 C 0.3199(3) 0.03535(14) 0.42635(18) 0.0535(6) Uani 1 1 d . . . . . H14 H 0.293545 -0.005510 0.373188 0.064 Uiso 1 1 calc R U . . . C15 C 0.2424(3) 0.03789(15) 0.51598(18) 0.0520(6) Uani 1 1 d . . . . . H15 H 0.162717 -0.002418 0.525394 0.062 Uiso 1 1 calc R U . . . C17 C 0.7087(3) 0.17266(16) 0.7225(2) 0.0565(6) Uani 1 1 d . . . . . C8 C 0.5843(3) 0.10640(17) 0.9203(2) 0.0615(7) Uani 1 1 d . . . . . H8A H 0.521761 0.100160 0.979779 0.092 Uiso 1 1 calc R U . . . H8B H 0.677392 0.138396 0.941349 0.092 Uiso 1 1 calc R U . . . H8C H 0.610966 0.048633 0.895001 0.092 Uiso 1 1 calc R U . . . C2 C 0.0384(3) 0.44218(18) 0.6309(3) 0.0662(7) Uani 1 1 d . . . . . H2A H 0.109734 0.490957 0.621821 0.079 Uiso 1 1 calc R U . . . H2B H 0.005161 0.419223 0.561729 0.079 Uiso 1 1 calc R U . . . C1A C -0.0909(5) 0.4719(3) 0.6834(4) 0.131(2) Uani 1 1 d . . . . . H1AA H -0.138691 0.520836 0.645318 0.196 Uiso 1 1 calc R U . . . H1AB H -0.057639 0.490812 0.753456 0.196 Uiso 1 1 calc R U . . . H1AC H -0.164345 0.424329 0.687310 0.196 Uiso 1 1 calc R U . . . C18A C 0.8889(3) 0.1968(3) 0.5956(3) 0.0926(12) Uani 1 1 d . . . . . H18A H 0.886037 0.208960 0.521290 0.139 Uiso 1 1 calc R U . . . H18B H 0.920533 0.136326 0.608126 0.139 Uiso 1 1 calc R U . . . H18C H 0.961474 0.236059 0.632200 0.139 Uiso 1 1 calc R U . . . H1 H 0.316(3) 0.1599(15) 0.911(2) 0.039(6) 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 0.0765(11) 0.0462(9) 0.0305(7) 0.0016(6) -0.0001(7) 0.0058(8) O1 0.0498(9) 0.0417(8) 0.0580(9) 0.0068(7) 0.0042(7) 0.0075(7) N1 0.0634(11) 0.0372(9) 0.0298(9) 0.0017(7) -0.0022(8) -0.0010(8) O3 0.1054(16) 0.0602(11) 0.0473(10) 0.0042(8) 0.0202(10) 0.0176(11) O6 0.0489(10) 0.0989(15) 0.0584(11) -0.0257(10) 0.0054(8) 0.0002(9) O4 0.1207(18) 0.0766(13) 0.0416(10) -0.0205(9) -0.0107(10) 0.0364(12) N2 0.0930(16) 0.0475(11) 0.0348(10) 0.0006(8) -0.0005(10) 0.0279(11) O5 0.0496(11) 0.0744(14) 0.135(2) 0.0125(13) -0.0188(12) 0.0026(10) C4 0.0441(10) 0.0325(10) 0.0296(9) -0.0045(7) -0.0029(7) -0.0022(8) C3 0.0459(11) 0.0340(10) 0.0338(10) -0.0061(8) -0.0051(8) -0.0025(8) C5 0.0479(11) 0.0336(10) 0.0309(9) -0.0048(7) -0.0040(8) -0.0043(8) C11 0.0525(11) 0.0314(10) 0.0327(10) -0.0013(8) -0.0060(8) 0.0089(8) C10 0.0472(11) 0.0338(10) 0.0350(10) -0.0042(8) 0.0003(8) 0.0000(8) C9 0.0496(12) 0.0377(11) 0.0425(11) -0.0099(9) -0.0087(9) 0.0017(9) C13 0.0712(14) 0.0406(11) 0.0324(10) -0.0006(8) -0.0062(9) 0.0212(10) C16 0.0565(12) 0.0345(10) 0.0390(11) -0.0020(8) -0.0075(9) 0.0040(9) C7 0.0566(12) 0.0344(10) 0.0434(11) -0.0086(8) -0.0121(9) 0.0031(9) C6 0.0558(12) 0.0486(12) 0.0330(10) -0.0025(9) 0.0039(9) -0.0046(10) C12 0.0576(13) 0.0360(10) 0.0340(10) 0.0017(8) -0.0026(9) 0.0119(9) C14 0.0775(16) 0.0370(11) 0.0430(12) -0.0099(9) -0.0187(11) 0.0162(11) C15 0.0655(14) 0.0358(11) 0.0521(13) -0.0052(9) -0.0158(10) 0.0036(10) C17 0.0443(12) 0.0445(12) 0.0787(17) -0.0205(11) -0.0108(11) -0.0037(10) C8 0.0839(18) 0.0495(13) 0.0481(13) -0.0054(10) -0.0200(12) 0.0154(13) C2 0.0584(15) 0.0494(14) 0.090(2) 0.0185(13) -0.0032(13) 0.0106(11) C1A 0.092(3) 0.111(3) 0.194(5) 0.058(3) 0.054(3) 0.047(3) C18A 0.0425(14) 0.113(3) 0.124(3) -0.055(2) 0.0134(16) -0.0150(15) 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 C3 O1 C2 115.41(19) . . ? C5 N1 H1 111.7(17) . . ? C7 N1 C5 123.77(19) . . ? C7 N1 H1 121.6(17) . . ? C17 O6 C18A 117.6(3) . . ? O3 N2 C13 117.7(2) . . ? O4 N2 O3 123.7(2) . . ? O4 N2 C13 118.6(3) . . ? C3 C4 C10 113.76(17) . . ? C5 C4 C3 125.75(19) . . ? C5 C4 C10 120.49(18) . . ? O2 C3 O1 121.39(19) . . ? O2 C3 C4 122.74(19) . . ? O1 C3 C4 115.87(17) . . ? N1 C5 C6 113.05(18) . . ? C4 C5 N1 118.32(19) . . ? C4 C5 C6 128.63(19) . . ? C16 C11 C10 121.56(18) . . ? C16 C11 C12 118.64(19) . . ? C12 C11 C10 119.74(19) . . ? C4 C10 C11 112.16(16) . . ? C4 C10 H10 107.9 . . ? C4 C10 C9 111.05(16) . . ? C11 C10 H10 107.9 . . ? C9 C10 C11 109.64(16) . . ? C9 C10 H10 107.9 . . ? C7 C9 C10 120.3(2) . . ? C7 C9 C17 121.8(2) . . ? C17 C9 C10 117.8(2) . . ? C12 C13 N2 117.9(2) . . ? C14 C13 N2 119.0(2) . . ? C14 C13 C12 123.1(2) . . ? C11 C16 H16 119.5 . . ? C11 C16 C15 121.1(2) . . ? C15 C16 H16 119.5 . . ? N1 C7 C8 113.8(2) . . ? C9 C7 N1 119.20(19) . . ? C9 C7 C8 127.0(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 C12 H12 120.5 . . ? C13 C12 C11 119.0(2) . . ? C13 C12 H12 120.5 . . ? C13 C14 H14 121.1 . . ? C13 C14 C15 117.8(2) . . ? C15 C14 H14 121.1 . . ? C16 C15 H15 119.8 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.8 . . ? O6 C17 C9 112.2(2) . . ? O5 C17 O6 121.6(3) . . ? O5 C17 C9 126.2(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C2 H2A 110.1 . . ? O1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C1A C2 O1 107.9(3) . . ? C1A C2 H2A 110.1 . . ? C1A C2 H2B 110.1 . . ? C2 C1A H1AA 109.5 . . ? C2 C1A H1AB 109.5 . . ? C2 C1A H1AC 109.5 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O6 C18A H18A 109.5 . . ? O6 C18A H18B 109.5 . . ? O6 C18A H18C 109.5 . . ? H18A C18A H18B 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 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 1.220(3) . ? O1 C3 1.336(3) . ? O1 C2 1.459(3) . ? N1 C5 1.383(3) . ? N1 C7 1.378(3) . ? N1 H1 0.80(3) . ? O3 N2 1.239(3) . ? O6 C17 1.336(4) . ? O6 C18A 1.453(3) . ? O4 N2 1.219(3) . ? N2 C13 1.468(3) . ? O5 C17 1.217(3) . ? C4 C3 1.463(3) . ? C4 C5 1.361(3) . ? C4 C10 1.517(3) . ? C5 C6 1.492(3) . ? C11 C10 1.532(3) . ? C11 C16 1.390(3) . ? C11 C12 1.391(3) . ? C10 H10 1.0000 . ? C10 C9 1.526(3) . ? C9 C7 1.345(3) . ? C9 C17 1.471(3) . ? C13 C12 1.388(3) . ? C13 C14 1.372(4) . ? C16 H16 0.9500 . ? C16 C15 1.394(3) . ? C7 C8 1.503(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C12 H12 0.9500 . ? C14 H14 0.9500 . ? C14 C15 1.385(4) . ? C15 H15 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C1A 1.438(5) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 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 O3 N2 C13 C12 12.0(3) . . . . ? O3 N2 C13 C14 -166.5(2) . . . . ? O4 N2 C13 C12 -168.2(2) . . . . ? O4 N2 C13 C14 13.3(3) . . . . ? N2 C13 C12 C11 -177.05(18) . . . . ? N2 C13 C14 C15 176.26(19) . . . . ? C4 C10 C9 C7 24.8(3) . . . . ? C4 C10 C9 C17 -158.00(18) . . . . ? C3 O1 C2 C1A 175.2(3) . . . . ? C3 C4 C5 N1 -174.89(17) . . . . ? C3 C4 C5 C6 4.6(3) . . . . ? C3 C4 C10 C11 -80.6(2) . . . . ? C3 C4 C10 C9 156.34(17) . . . . ? C5 N1 C7 C9 -15.7(3) . . . . ? C5 N1 C7 C8 163.32(19) . . . . ? C5 C4 C3 O2 -175.69(19) . . . . ? C5 C4 C3 O1 4.6(3) . . . . ? C5 C4 C10 C11 98.5(2) . . . . ? C5 C4 C10 C9 -24.6(3) . . . . ? C11 C10 C9 C7 -99.7(2) . . . . ? C11 C10 C9 C17 77.5(2) . . . . ? C11 C16 C15 C14 0.6(3) . . . . ? C10 C4 C3 O2 3.3(3) . . . . ? C10 C4 C3 O1 -176.40(16) . . . . ? C10 C4 C5 N1 6.2(3) . . . . ? C10 C4 C5 C6 -174.36(18) . . . . ? C10 C11 C16 C15 -178.86(19) . . . . ? C10 C11 C12 C13 177.94(18) . . . . ? C10 C9 C7 N1 -6.5(3) . . . . ? C10 C9 C7 C8 174.6(2) . . . . ? C10 C9 C17 O6 6.3(3) . . . . ? C10 C9 C17 O5 -173.2(2) . . . . ? C13 C14 C15 C16 1.1(3) . . . . ? C16 C11 C10 C4 -41.6(3) . . . . ? C16 C11 C10 C9 82.2(2) . . . . ? C16 C11 C12 C13 0.4(3) . . . . ? C7 N1 C5 C4 15.8(3) . . . . ? C7 N1 C5 C6 -163.70(18) . . . . ? C7 C9 C17 O6 -176.5(2) . . . . ? C7 C9 C17 O5 4.0(4) . . . . ? C12 C11 C10 C4 140.96(18) . . . . ? C12 C11 C10 C9 -95.2(2) . . . . ? C12 C11 C16 C15 -1.4(3) . . . . ? C12 C13 C14 C15 -2.2(3) . . . . ? C14 C13 C12 C11 1.4(3) . . . . ? C17 C9 C7 N1 176.45(19) . . . . ? C17 C9 C7 C8 -2.4(3) . . . . ? C2 O1 C3 O2 1.2(3) . . . . ? C2 O1 C3 C4 -179.13(19) . . . . ? C18A O6 C17 O5 4.9(4) . . . . ? C18A O6 C17 C9 -174.6(2) . . . . ? _cod_database_fobs_code 2312372