#------------------------------------------------------------------------------ #$Date: 2024-02-05 14:04:31 +0200 (Mon, 05 Feb 2024) $ #$Revision: 289678 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/23/2312370.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_2312370 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, C2 H4 O' _chemical_formula_sum 'C19 H22 N2 O7' _chemical_formula_weight 390.38 _chemical_name_common 'nifedipine 1,4-dioxane solvate' _chemical_name_systematic ; dimethyl 2,6-dimethyl-4-(2-nitrophenyl) -1,4-dihydropyridine-3,5-dicarboxylate 1,4-dioxane ; _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 97.164(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.0927(5) _cell_length_b 9.2253(4) _cell_length_c 14.5139(5) _cell_measurement_reflns_used 7391 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 74.0180 _cell_measurement_theta_min 3.1530 _cell_volume 1872.21(12) _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 0.952 _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 63.00 103.00 0.50 1.67 -- 38.69 152.00 -22.00 80 2 \w -101.00 -76.00 0.50 1.67 -- -39.38 152.00 -22.00 50 3 \w -83.00 -58.00 0.50 1.67 -- -39.38 122.00 176.00 50 4 \w -110.00 -85.00 0.50 1.67 -- -39.38-152.00 -65.00 50 5 \w -130.00 -27.00 0.50 1.67 -- -95.69 152.00 -22.00 206 6 \w 103.00 128.00 0.50 1.67 -- 102.48 122.00 176.00 50 7 \w 68.00 113.00 0.50 1.67 -- 102.48-152.00 -65.00 90 8 \w 33.00 59.00 0.50 1.67 -- 110.26-152.00 -65.00 52 9 \w 64.00 90.00 0.50 1.67 -- 110.26-122.00 95.00 52 10 \w 63.00 130.00 0.50 1.67 -- 110.26-152.00 -65.00 134 11 \w 6.00 43.00 0.50 1.67 -- 38.69 -38.00 -30.00 74 12 \w -50.00 -3.00 0.50 1.67 -- 38.69 -38.00 -30.00 94 13 \w 42.00 123.00 0.50 1.67 -- 38.69 178.00-180.00 162 14 \w -66.00 44.00 0.50 1.67 -- -39.38 57.00-150.00 220 15 \w 22.00 47.00 0.50 1.67 -- -39.38 19.00 150.00 50 16 \w -35.00 -10.00 0.50 1.67 -- -95.69 30.00 120.00 50 17 \w -35.00 -10.00 0.50 1.67 -- -95.69 30.00 150.00 50 18 \w -34.00 -9.00 0.50 1.67 -- -95.69 30.00-120.00 50 19 \w 18.00 51.00 0.50 1.67 -- 102.48 -45.00 0.00 66 20 \w 16.00 51.00 0.50 1.67 -- 102.48 -45.00 -90.00 70 21 \w 28.00 71.00 0.50 1.67 -- 102.48 -61.00 150.00 86 22 \w 60.00 103.00 0.50 1.67 -- 102.48 152.00 -22.00 86 23 \w 18.00 51.00 0.50 1.67 -- 102.48 -45.00 -30.00 66 24 \w 17.00 43.00 0.50 1.67 -- 102.48 -45.00-120.00 52 25 \w 32.00 104.00 0.50 1.67 -- 102.48 -77.00 90.00 144 26 \w 23.00 48.00 0.50 1.67 -- 110.26 -45.00 120.00 50 27 \w 98.00 177.00 0.50 1.67 -- 110.26 45.00 90.00 158 28 \w 23.00 48.00 0.50 1.67 -- 110.26 -45.00-150.00 50 29 \w 28.00 58.00 0.50 1.67 -- 110.26 -61.00-120.00 60 30 \w 60.00 99.00 0.50 1.67 -- 110.26 -95.00 90.00 78 31 \w 33.00 58.00 0.50 1.67 -- 110.26 -61.00 90.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix-Arc 100' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0774080000 _diffrn_orient_matrix_UB_12 0.1180340000 _diffrn_orient_matrix_UB_13 -0.0011427000 _diffrn_orient_matrix_UB_21 -0.0750481000 _diffrn_orient_matrix_UB_22 -0.1169262000 _diffrn_orient_matrix_UB_23 0.0137270000 _diffrn_orient_matrix_UB_31 0.0227691000 _diffrn_orient_matrix_UB_32 0.0165089000 _diffrn_orient_matrix_UB_33 0.1060980000 _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 0.0239 _diffrn_reflns_av_unetI/netI 0.0262 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 11509 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.634 _diffrn_reflns_theta_min 3.161 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90910 _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 1.385 _exptl_crystal_description block _exptl_crystal_F_000 824 _exptl_crystal_preparation ; 'Crystallised from a saturated solution of nifedipine in 1,4-dioxane.' ; _exptl_crystal_recrystallization_method ; 'High-throughput screening via the ENaCt protocol using an SPT Labtech mosquito.' ; _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.33 _refine_diff_density_max 0.232 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 261 _refine_ls_number_reflns 3659 _refine_ls_number_restraints 198 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0352 _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^)+(0.0449P)^2^+0.5706P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.0946 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3110 _reflns_number_total 3659 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file rm5073sup1.cif _cod_data_source_block nifedipine-dioxane _cod_depositor_comments 'Adding full bibliography for 2312368--2312375.cif.' _cod_database_code 2312370 _cod_database_fobs_code 2312370 _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 0.756 _shelx_estimated_absorpt_t_min 0.653 _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: C9(H9) 3.b Secondary CH2 refined with riding coordinates: C2S(H2SA,H2SB), C1S(H1SA,H1SB) 3.c Aromatic/amide H refined with riding coordinates: C15(H15), C14(H14), C12(H12), C13(H13) 3.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C1(H1A,H1B,H1C) ; _shelx_res_file ; TITL nisoldipine1,4-dioxanesolvate_auto_a.res in P2(1)/c nifedipine1,4-dioxanesolvate.res created by SHELXL-2018/3 at 11:30:07 on 11-May-2023 REM Old TITL nisoldipine 1,4-dioxane solvate_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.128, Rweak 0.011, Alpha 0.017 REM 0.348 for 246 systematic absences, Orientation as input REM Formula found by SHELXT: C20 N2 O6 CELL 1.54184 14.0927 9.2253 14.5139 90 97.164 90 ZERR 4 0.0005 0.0004 0.0005 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 76 88 8 28 RIGU L.S. 4 0 0 PLAN 5 SIZE 0.33 0.47 0.52 TEMP -123 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.044900 0.570600 FVAR 0.59795 O4 4 0.565348 0.872816 0.385910 11.00000 0.02556 0.03340 = 0.01970 -0.00176 0.00546 -0.00774 O1 4 0.222539 0.452769 0.329063 11.00000 0.03159 0.02827 = 0.02615 -0.00402 0.00153 -0.00854 O2 4 0.225122 0.334318 0.463953 11.00000 0.03458 0.02468 = 0.03720 0.00363 0.00613 -0.00289 O5 4 0.242287 0.705789 0.190549 11.00000 0.03735 0.04393 = 0.02029 -0.00286 0.00348 0.00076 O3 4 0.456266 0.790162 0.273913 11.00000 0.03338 0.06220 = 0.01483 0.00230 0.00184 -0.01461 O6 4 0.094958 0.657812 0.208005 11.00000 0.03243 0.04032 = 0.03805 -0.00410 -0.01115 -0.00803 N1 3 0.413576 0.667036 0.579256 11.00000 0.02652 0.02918 = 0.01405 0.00192 0.00233 0.00099 O1S 4 0.026283 0.947214 0.090860 11.00000 0.05791 0.04516 = 0.03023 0.00279 0.00989 0.00668 N2 3 0.172368 0.716701 0.232652 11.00000 0.02870 0.02875 = 0.02067 0.00159 -0.00435 -0.00086 C8 1 0.431823 0.743810 0.428213 11.00000 0.01908 0.02207 = 0.01680 -0.00059 0.00270 0.00152 C6 1 0.464640 0.743132 0.520356 11.00000 0.02152 0.02263 = 0.01839 0.00030 0.00320 0.00327 C10 1 0.254925 0.795473 0.387515 11.00000 0.01996 0.02072 = 0.01844 0.00327 0.00280 -0.00172 C16 1 0.483701 0.803156 0.355969 11.00000 0.01926 0.02406 = 0.01835 -0.00068 0.00206 0.00103 C11 1 0.179068 0.808432 0.315935 11.00000 0.02252 0.02427 = 0.02035 0.00199 0.00134 -0.00327 C9 1 0.334316 0.679866 0.393415 11.00000 0.02101 0.02221 = 0.01545 -0.00058 0.00279 0.00044 AFIX 13 H9 2 0.336726 0.638702 0.330011 11.00000 -1.20000 AFIX 0 C3 1 0.311328 0.557753 0.458064 11.00000 0.02069 0.02024 = 0.02195 0.00091 0.00609 0.00287 C15 1 0.251508 0.890441 0.461929 11.00000 0.02611 0.02368 = 0.02147 0.00012 0.00054 0.00226 AFIX 43 H15 2 0.300978 0.886021 0.512695 11.00000 -1.20000 AFIX 0 C2 1 0.249767 0.437661 0.421212 11.00000 0.02070 0.02191 = 0.02783 -0.00017 0.00667 0.00493 C4 1 0.345781 0.563970 0.549441 11.00000 0.02364 0.02245 = 0.02253 0.00209 0.00705 0.00417 C14 1 0.178867 0.990799 0.464653 11.00000 0.03442 0.02505 = 0.02753 -0.00256 0.00419 0.00498 AFIX 43 H14 2 0.179470 1.053819 0.516489 11.00000 -1.20000 AFIX 0 C7 1 0.552766 0.815030 0.568558 11.00000 0.02407 0.03367 = 0.01802 -0.00139 -0.00055 0.00047 AFIX 137 H7A 2 0.553833 0.805326 0.635919 11.00000 -1.50000 H7B 2 0.552282 0.918000 0.551908 11.00000 -1.50000 H7C 2 0.609693 0.768686 0.549306 11.00000 -1.50000 AFIX 0 C12 1 0.105003 0.907103 0.317323 11.00000 0.02329 0.03130 = 0.02976 0.00584 -0.00200 0.00098 AFIX 43 H12 2 0.054629 0.910914 0.267369 11.00000 -1.20000 AFIX 0 C13 1 0.105262 0.999648 0.392010 11.00000 0.02771 0.02783 = 0.03713 0.00396 0.00351 0.00865 AFIX 43 H13 2 0.055509 1.068732 0.393642 11.00000 -1.20000 AFIX 0 C5 1 0.319235 0.467632 0.625723 11.00000 0.03692 0.03174 = 0.02586 0.00849 0.00684 0.00147 AFIX 137 H5A 2 0.349269 0.504034 0.685809 11.00000 -1.50000 H5B 2 0.341537 0.368763 0.616247 11.00000 -1.50000 H5C 2 0.249589 0.467282 0.624851 11.00000 -1.50000 AFIX 0 C17 1 0.617188 0.929628 0.314355 11.00000 0.03212 0.03917 = 0.02706 0.00129 0.01041 -0.01087 AFIX 137 H17A 2 0.629928 0.851303 0.271967 11.00000 -1.50000 H17B 2 0.677897 0.971110 0.342760 11.00000 -1.50000 H17C 2 0.578998 1.005111 0.279672 11.00000 -1.50000 AFIX 0 C1 1 0.162973 0.337879 0.286507 11.00000 0.03618 0.03410 = 0.03730 -0.00987 0.00148 -0.01190 AFIX 137 H1A 2 0.145043 0.359623 0.220541 11.00000 -1.50000 H1B 2 0.105139 0.329798 0.317299 11.00000 -1.50000 H1C 2 0.198262 0.246150 0.292765 11.00000 -1.50000 AFIX 0 C2S 1 0.020821 1.098640 0.071913 11.00000 0.04269 0.04153 = 0.03694 -0.00736 0.01112 0.00060 AFIX 23 H2SA 2 0.084757 1.134794 0.061473 11.00000 -1.20000 H2SB 2 0.001273 1.150274 0.126299 11.00000 -1.20000 AFIX 0 C1S 1 0.049529 0.869564 0.012001 11.00000 0.04198 0.03810 = 0.04025 0.00139 0.01449 0.00618 AFIX 23 H1SA 2 0.049479 0.764281 0.025199 11.00000 -1.20000 H1SB 2 0.114572 0.896960 -0.000686 11.00000 -1.20000 AFIX 0 H1 2 0.432750 0.673096 0.639732 11.00000 0.03064 HKLF 4 REM nisoldipine1,4-dioxanesolvate_auto_a.res in P2(1)/c REM wR2 = 0.0946, GooF = S = 1.054, Restrained GooF = 1.026 for all data REM R1 = 0.0352 for 3110 Fo > 4sig(Fo) and 0.0421 for all 3659 data REM 261 parameters refined using 198 restraints END WGHT 0.0449 0.5706 REM Highest difference peak 0.232, deepest hole -0.204, 1-sigma level 0.040 Q1 1 0.3196 0.6200 0.4261 11.00000 0.05 0.23 Q2 1 0.2947 0.7401 0.3884 11.00000 0.05 0.22 Q3 1 0.2236 0.8079 0.3421 11.00000 0.05 0.21 Q4 1 0.3811 0.4337 0.6583 11.00000 0.05 0.19 Q5 1 0.2805 0.5133 0.4423 11.00000 0.05 0.19 ; _shelx_res_checksum 64887 _shelx_hkl_file ; 0 0 1 -0.10 0.17 0 0 1 0.18 0.18 0 0 1 -0.02 0.20 0 0 1 0.04 0.15 0 0 2 925.14 23.05 0 0 2 923.68 22.99 0 0 2 928.32 22.96 0 0 2 930.08 23.09 0 0 3 0.39 0.54 0 0 3 0.38 0.60 0 0 3 0.29 0.69 0 0 3 0.20 0.46 0 0 4 56.99 2.07 0 0 4 57.02 2.27 0 0 5 -0.06 0.66 0 0 5 -0.13 0.73 0 0 5 -0.27 0.75 0 0 5 0.23 0.82 0 0 6 581.23 14.74 0 0 6 527.29 14.48 0 0 7 0.41 0.96 0 0 7 -0.09 0.79 0 0 7 0.11 1.03 0 0 7 0.50 0.90 0 0 8 920.68 23.91 0 0 8 900.89 24.09 0 0 8 890.92 23.86 0 0 9 -0.14 1.06 0 0 9 0.28 0.96 0 0 9 -0.16 1.12 0 0 9 -0.43 1.07 0 0 10 277.03 8.96 0 0 10 279.63 8.88 0 0 10 271.58 8.85 0 0 10 255.08 8.68 0 0 11 -0.19 1.25 0 0 11 -0.19 1.16 0 0 11 1.15 1.29 0 0 11 0.60 1.45 0 0 11 0.36 1.10 0 0 11 0.55 1.26 0 0 12 103.87 4.89 0 0 12 100.79 4.93 0 0 12 95.82 4.69 0 0 12 101.04 4.82 0 0 13 -0.21 1.41 0 0 13 -0.21 1.43 0 0 13 0.21 1.44 0 0 13 1.80 1.62 0 0 14 126.15 5.46 0 0 14 125.83 5.39 0 0 14 124.13 5.50 0 0 15 -0.34 1.16 0 0 15 0.75 1.34 0 0 15 0.18 1.27 0 0 16 1.21 1.07 0 0 16 1.64 1.15 0 0 17 1.10 0.88 0 -1 0 0.16 0.25 0 1 1 1337.33 32.69 0 -1 1 1327.13 32.69 0 -1 1 1322.80 32.86 0 1 1 1316.92 32.83 0 -1 2 294.43 7.79 0 -1 2 294.39 7.91 0 -1 2 301.74 7.80 0 1 2 304.43 7.80 0 1 2 302.92 7.80 0 1 2 313.64 7.83 0 -1 2 299.93 7.79 0 -1 3 955.17 23.52 0 1 3 914.22 23.52 0 -1 3 932.34 23.35 0 -1 3 939.75 23.58 0 1 3 936.84 23.11 0 1 3 942.42 23.40 0 1 3 921.29 23.49 0 -1 3 932.60 23.48 0 -1 4 24.89 1.44 0 1 4 25.65 1.02 0 1 4 24.15 1.41 0 1 4 24.03 1.29 0 -1 4 21.39 1.30 0 -1 4 28.08 1.46 0 1 4 25.71 1.26 0 1 4 26.00 1.36 0 -1 4 24.47 1.30 0 -1 5 983.96 24.65 0 1 5 933.61 24.11 0 1 5 970.57 24.54 0 1 5 984.22 24.68 0 -1 5 946.68 24.67 0 -1 5 973.71 24.56 0 1 5 941.57 24.33 0 -1 5 980.63 24.55 0 1 5 983.53 24.60 0 -1 6 2745.40 66.50 0 1 6 2656.05 65.88 0 1 6 2634.40 66.03 0 -1 6 2637.49 66.37 0 1 7 15.99 1.61 0 -1 7 19.64 1.53 0 1 7 18.30 1.51 0 -1 7 16.28 1.67 0 -1 7 15.31 1.56 0 1 7 16.13 1.48 0 -1 7 17.25 1.50 0 -1 8 19.08 1.74 0 -1 8 20.18 1.67 0 1 8 15.00 1.57 0 1 8 18.34 1.82 0 -1 8 18.03 1.63 0 1 8 19.18 1.71 0 -1 8 16.40 1.63 0 -1 9 231.94 7.59 0 1 9 243.31 7.75 0 -1 9 243.69 7.72 0 -1 9 227.71 7.59 0 1 9 232.46 7.63 0 -1 9 228.96 7.56 0 1 9 236.87 7.63 0 -1 10 25.37 2.08 0 1 10 22.85 1.98 0 -1 10 20.54 1.95 0 1 10 25.15 2.18 0 -1 10 21.54 2.10 0 1 10 27.27 2.29 0 -1 10 23.63 2.21 0 1 11 20.64 2.17 0 -1 11 18.98 2.14 0 -1 11 20.13 2.11 0 -1 11 19.36 2.15 0 1 11 22.07 2.23 0 -1 11 19.29 2.16 0 1 11 18.55 1.96 0 -1 11 20.55 2.02 0 1 11 22.15 2.30 0 1 11 17.04 2.18 0 -1 11 19.19 2.14 0 -1 11 17.02 2.20 0 -1 11 18.63 1.97 0 -1 12 -0.21 1.72 0 1 12 -1.93 1.75 0 1 12 -2.06 1.71 0 -1 12 -0.41 1.71 0 -1 12 0.40 1.37 0 -1 12 0.42 1.48 0 1 12 0.19 1.22 0 1 12 0.60 1.49 0 -1 12 -0.40 1.57 0 1 13 208.47 7.71 0 -1 13 188.61 7.56 0 -1 13 204.89 7.49 0 1 13 209.00 7.52 0 -1 13 194.15 7.49 0 1 13 186.32 7.13 0 -1 13 196.21 7.31 0 1 13 195.28 7.47 0 -1 13 189.72 7.42 0 1 14 48.66 3.16 0 -1 14 47.88 3.17 0 -1 14 46.64 3.27 0 -1 14 45.33 3.26 0 1 14 49.26 3.30 0 -1 15 1.81 1.28 0 1 15 2.12 1.36 0 -1 15 1.77 1.33 0 1 15 1.45 1.32 0 -1 15 1.10 1.36 0 -1 16 180.50 6.35 0 1 16 185.09 6.37 0 -1 16 182.14 6.36 0 -1 17 8.52 1.18 0 -2 0 925.25 23.08 0 -2 1 2214.89 54.12 0 -2 1 2226.57 54.59 0 -2 -1 2180.39 54.24 0 -2 2 1335.68 33.45 0 -2 2 1371.50 33.22 0 -2 2 1336.61 33.49 0 2 2 1341.62 33.42 0 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15 19.57 2.01 0 -3 16 5.52 1.09 0 -3 16 5.25 1.32 0 -3 17 65.62 2.87 0 -4 0 0.66 0.70 0 -4 1 325.61 9.16 0 -4 2 71.95 3.11 0 -4 2 76.13 3.04 0 -4 3 8.23 0.90 0 -4 3 9.67 1.34 0 -4 3 8.61 1.37 0 -4 4 18.02 1.70 0 -4 4 16.49 1.29 0 -4 -4 15.37 1.35 0 -4 4 16.73 1.61 0 -4 5 1.30 1.19 0 4 5 2.49 1.04 0 -4 5 2.24 1.04 0 -4 6 6.59 1.45 0 -4 7 84.97 4.12 0 -4 8 19.33 2.20 0 -4 8 26.35 2.43 0 -4 9 547.79 16.19 0 -4 9 523.18 16.09 0 4 9 554.55 16.07 0 -4 9 548.53 16.42 0 -4 10 20.97 2.56 0 -4 10 23.55 2.36 0 -4 10 26.29 2.69 0 -4 10 22.54 2.52 0 -4 11 41.10 3.10 0 -4 11 45.61 3.38 0 -4 11 36.19 3.11 0 -4 12 12.16 1.95 0 -4 12 12.66 2.15 0 -4 12 9.85 1.92 0 -4 13 63.88 3.78 0 -4 13 63.32 3.85 0 -4 13 73.79 4.08 0 -4 14 2.45 1.34 0 -4 15 30.15 2.18 0 -4 15 23.31 2.07 0 -4 16 1.35 0.95 0 -4 16 0.63 0.92 0 -5 0 0.53 1.06 0 5 1 184.04 6.42 0 -5 1 185.27 6.35 0 -5 -1 188.39 6.28 0 5 2 21.88 1.90 0 -5 -2 21.09 1.75 0 -5 2 19.25 1.69 0 -5 2 22.90 1.95 0 5 3 79.79 3.61 0 -5 3 71.18 3.49 0 -5 -3 70.88 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21.38 2.44 2 -3 12 22.71 2.53 2 3 12 25.34 2.38 2 -3 12 26.72 2.44 2 -3 13 96.66 4.48 2 3 13 92.58 4.40 2 -3 13 94.12 4.60 2 3 13 90.45 4.28 2 -3 13 95.54 4.38 2 -3 13 86.11 4.52 2 -3 14 0.19 1.24 2 -3 14 0.18 1.32 2 -3 15 163.88 5.93 2 -3 15 163.49 5.97 2 -3 16 5.32 1.06 -2 -4 17 -0.13 1.26 -2 -4 16 91.67 3.71 -2 -4 16 101.07 3.84 -2 -4 15 95.26 4.17 -2 -4 15 91.81 4.12 -2 -4 14 3.12 1.49 -2 -4 13 29.13 2.70 -2 -4 13 37.70 2.91 -2 -4 13 31.29 2.76 -2 -4 12 41.54 3.26 -2 -4 12 43.16 3.24 -2 -4 12 47.98 3.39 -2 -4 11 27.71 2.92 -2 -4 11 27.03 2.67 -2 -4 10 145.18 5.76 -2 -4 10 137.10 6.19 -2 -4 9 185.36 7.10 -2 -4 9 199.93 7.00 -2 -4 9 193.38 7.40 -2 4 8 103.96 4.84 -2 -4 8 110.27 4.49 -2 -4 8 94.41 4.56 -2 -4 8 103.15 4.75 -2 -4 7 38.72 2.41 -2 -4 6 1.04 0.91 -2 4 6 1.25 1.11 -2 -4 5 348.27 10.13 -2 4 5 349.46 10.54 -2 -4 4 262.89 7.94 -2 4 4 275.11 8.45 -2 4 3 529.87 14.76 -2 -4 2 259.32 8.12 -2 4 2 283.42 8.34 -2 -4 1 699.11 18.50 2 -4 -1 692.59 17.82 -2 4 1 678.54 18.53 2 -4 0 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2 -5 11 55.80 3.62 2 -5 12 119.17 5.05 2 -5 13 151.45 5.72 2 -5 13 153.19 6.00 2 -5 14 13.31 1.53 2 -5 14 15.12 1.74 2 -5 15 7.70 1.26 -2 -6 15 1.86 1.25 -2 -6 14 0.10 0.90 -2 -6 14 0.13 1.02 -2 -6 13 30.11 2.13 -2 -6 13 30.05 2.49 -2 -6 13 28.96 2.39 -2 -6 12 36.28 2.95 -2 -6 12 37.35 2.86 -2 -6 11 14.06 2.22 -2 -6 10 21.90 2.72 -2 -6 10 18.45 2.31 -2 -6 9 23.08 2.51 -2 -6 9 18.44 2.33 -2 -6 9 21.49 2.64 -2 -6 8 7.13 1.88 -2 6 8 4.61 1.83 -2 -6 7 3.99 1.51 -2 6 7 6.72 1.97 -2 6 7 2.32 1.79 -2 6 6 1.58 1.37 -2 -6 6 1.35 1.34 -2 6 6 2.74 1.87 -2 6 6 -0.24 1.57 -2 6 5 396.89 12.66 -2 6 5 398.07 12.77 -2 6 4 370.83 12.08 -2 6 4 384.08 12.15 -2 6 3 -1.04 1.30 -2 6 3 1.20 1.52 -2 6 2 138.58 5.79 -2 6 1 191.30 7.19 -2 6 0 86.55 4.30 2 -6 0 83.94 4.13 2 -6 1 -1.12 1.29 2 6 1 0.92 1.17 -2 6 -1 0.20 1.23 2 -6 2 3.43 1.31 2 6 2 3.44 1.29 -2 6 -2 4.37 1.56 2 -6 3 232.27 7.98 2 -6 3 232.17 8.16 2 6 3 228.75 7.98 -2 6 -3 239.34 8.32 2 6 3 227.68 8.21 2 -6 4 82.25 4.25 2 -6 4 86.62 4.30 -2 6 -4 91.72 4.47 2 6 4 91.04 4.59 2 -6 5 0.82 1.22 2 -6 5 -0.22 1.34 2 6 5 1.83 1.65 -2 6 -5 -0.42 1.17 2 6 6 13.07 2.15 2 -6 6 14.26 2.09 2 -6 6 13.07 1.92 2 -6 6 13.57 2.04 2 6 6 12.35 2.14 2 6 6 12.89 2.16 2 -6 7 4.03 1.37 2 6 7 4.73 1.83 2 -6 7 4.53 1.72 2 6 7 5.12 1.80 2 -6 8 11.59 1.90 2 -6 8 8.31 1.87 2 6 8 10.79 2.19 2 -6 9 218.98 7.93 2 6 9 213.17 8.23 2 -6 9 212.52 8.30 2 -6 10 2.91 1.53 2 -6 10 3.45 1.70 2 -6 10 5.47 1.82 2 -6 11 1.43 1.42 2 -6 11 -1.18 1.40 2 -6 12 4.53 1.43 2 -6 13 19.32 1.85 2 -6 14 59.69 2.80 -2 -7 13 62.62 2.97 -2 -7 12 7.09 1.44 -2 -7 12 8.00 1.61 -2 -7 11 11.18 1.73 -2 -7 10 24.33 2.60 -2 -7 10 24.67 2.34 -2 -7 10 26.43 2.46 -2 -7 9 2.37 1.68 -2 -7 9 3.15 1.64 -2 -7 9 5.35 1.60 -2 -7 8 209.31 7.90 -2 -7 8 202.93 7.48 -2 7 7 31.13 3.16 -2 7 7 34.04 3.29 -2 7 6 107.24 5.47 -2 7 6 97.11 5.46 -2 7 5 48.44 3.61 2 7 -5 45.63 3.39 -2 7 5 43.39 3.70 2 -7 -4 48.24 3.21 -2 7 4 49.10 3.66 -2 7 4 44.03 3.48 -2 7 4 45.20 3.60 2 7 -4 53.66 3.64 2 -7 -3 183.42 7.08 -2 7 3 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2 2.66 0.84 5 -1 2 4.17 0.90 5 1 2 3.75 1.05 5 1 3 192.46 5.97 5 -1 4 655.48 16.95 5 1 4 627.35 16.89 5 -1 4 614.30 17.09 5 -1 5 260.57 8.04 5 1 5 266.26 8.05 5 -1 5 262.62 8.16 5 -1 6 33.51 2.26 5 -1 7 0.16 0.97 5 -1 7 1.28 1.04 5 1 7 -0.14 1.11 5 -1 8 12.51 1.80 5 -1 8 11.87 1.76 5 1 8 13.83 1.77 5 1 8 13.54 1.83 5 -1 8 13.99 1.82 5 -1 8 11.96 1.55 5 -1 8 11.88 1.92 5 1 8 12.51 1.88 5 1 9 1.59 1.37 5 -1 9 0.20 1.35 5 1 9 0.59 1.30 5 -1 9 -0.40 1.33 5 1 9 2.40 1.31 5 -1 9 0.76 1.37 5 -1 9 -0.87 1.34 5 1 9 -0.43 1.37 5 -1 9 2.06 1.41 5 1 9 1.34 1.43 5 1 9 3.04 1.46 5 -1 9 1.43 1.43 5 -1 9 0.19 1.40 5 -1 10 132.89 5.80 5 -1 10 137.64 5.89 5 1 10 145.05 5.99 5 -1 10 132.72 5.71 5 1 10 130.52 5.72 5 -1 10 136.13 5.91 5 -1 10 147.61 5.86 5 1 10 139.46 5.81 5 1 10 132.76 5.90 5 -1 10 135.59 5.92 5 1 11 101.09 5.03 5 -1 11 98.40 4.92 5 -1 11 96.24 4.80 5 -1 11 91.26 4.68 5 -1 11 103.01 4.90 5 1 11 95.46 4.85 5 -1 11 104.43 4.99 5 -1 12 64.40 3.84 5 1 12 63.94 3.91 5 -1 12 68.65 4.00 5 -1 12 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452.29 14.79 5 8 2 2.45 1.81 5 -8 2 2.31 1.66 5 8 3 -0.80 1.91 5 8 3 1.06 1.66 5 -8 3 -0.95 1.61 5 -8 4 32.02 3.06 5 8 4 31.43 3.03 5 -8 5 5.65 1.85 5 8 5 5.36 1.64 5 8 6 7.44 1.80 5 -8 6 8.60 1.91 5 8 7 -0.21 1.40 5 8 8 -0.88 1.30 5 -8 8 1.50 1.63 5 8 9 1.76 1.01 5 -8 9 2.69 1.39 5 -8 9 1.38 1.23 5 -8 10 119.82 4.44 -5 -9 10 5.53 1.33 -5 9 9 36.65 2.26 -5 -9 9 40.62 2.28 -5 9 8 10.06 1.57 -5 -9 8 10.00 1.45 -5 -9 8 10.00 1.69 -5 9 7 62.03 3.58 5 9 -7 46.62 2.93 -5 -9 7 63.46 3.52 -5 -9 7 51.35 2.89 -5 -9 6 14.80 2.04 5 9 -6 11.24 1.87 -5 -9 5 4.76 1.63 5 9 -5 2.95 1.52 -5 -9 4 40.99 3.19 -5 -9 3 0.22 1.40 5 9 -2 123.92 5.77 5 9 -2 112.07 5.23 -5 -9 2 119.19 5.37 5 9 -1 1.97 1.58 5 9 -1 0.76 1.71 5 9 0 37.68 3.07 5 9 0 29.82 2.97 5 9 1 9.24 1.94 5 9 1 7.46 1.95 5 9 2 24.42 2.60 5 9 3 0.23 1.51 5 -9 3 0.19 1.34 5 9 4 0.43 1.52 5 -9 4 1.14 1.42 5 9 4 0.42 1.40 5 9 5 98.14 4.62 5 -9 5 90.81 4.37 5 9 5 83.29 4.21 5 -9 6 18.52 2.09 5 9 6 25.16 2.31 5 -9 7 4.76 1.50 5 9 7 8.22 1.45 5 -9 8 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7.53 1.82 -10 2 5 9.20 1.88 -10 -2 5 8.54 1.55 -10 2 5 5.38 1.74 10 -2 -5 5.67 1.61 -10 -2 5 10.79 2.08 -10 2 5 9.87 2.07 -10 2 4 524.94 16.15 10 -2 -4 541.06 15.99 -10 2 4 569.90 16.58 -10 -2 4 527.02 16.06 -10 -2 4 544.66 16.09 -10 -2 3 1.34 1.12 -10 2 3 1.10 1.46 10 -2 -3 4.17 1.45 -10 2 3 5.26 1.59 -10 -2 3 2.59 1.50 10 -2 -2 12.94 1.91 10 2 -2 11.99 1.97 -10 2 2 12.08 1.85 -10 -2 2 15.65 1.70 -10 -2 2 11.21 1.77 10 -2 -1 168.70 6.03 10 2 -1 160.58 5.96 10 -2 -1 150.34 6.46 10 2 -1 152.45 6.45 10 2 -1 163.73 6.08 10 -2 -1 165.63 6.09 -10 -2 1 162.35 6.28 10 2 0 366.12 11.26 10 -2 0 378.96 11.33 10 2 0 357.24 11.24 10 -2 0 372.48 11.28 10 -2 0 365.65 11.89 10 2 0 352.29 11.74 10 -2 1 2.98 1.24 10 2 1 1.76 1.17 10 -2 1 1.38 1.44 10 -2 1 2.61 1.31 10 2 1 1.93 1.28 10 2 1 2.80 1.34 10 -2 2 4.47 1.33 10 2 2 5.72 1.49 10 -2 2 3.78 1.43 10 2 2 3.16 1.35 10 -2 2 5.37 1.39 10 2 2 5.22 1.46 10 -2 2 2.72 1.33 10 2 2 4.38 1.47 10 -2 2 2.71 1.46 10 -2 3 54.35 3.46 10 2 3 55.19 3.31 10 -2 3 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5.36 1.74 -10 4 9 29.81 3.16 -10 4 9 25.47 3.05 -10 -4 9 30.33 3.02 -10 4 8 173.45 7.58 -10 4 7 30.78 3.29 -10 -4 7 28.43 3.04 -10 4 6 11.30 2.39 -10 -4 6 7.20 2.07 -10 4 5 46.28 3.78 -10 -4 5 47.07 3.58 -10 4 4 74.68 4.65 -10 -4 4 82.65 4.72 -10 4 3 1645.08 44.05 -10 -4 3 1694.52 43.92 10 -4 -3 1615.54 43.21 10 -4 -2 15.84 2.05 10 -4 -2 12.02 1.90 -10 -4 2 13.90 2.11 -10 4 2 18.05 2.49 -10 -4 1 27.27 2.54 10 -4 -1 27.76 2.61 10 4 -1 20.84 2.38 10 4 -1 27.37 2.67 10 4 -1 24.64 2.73 10 -4 0 -0.46 1.55 10 4 0 0.79 1.76 10 -4 1 26.12 2.73 10 4 1 22.67 2.90 10 -4 2 108.74 5.15 10 -4 2 106.72 5.42 10 4 2 117.59 5.93 10 -4 3 9.26 1.98 10 -4 3 9.29 1.92 10 4 3 7.65 2.40 10 -4 4 1.41 1.65 10 -4 4 1.01 1.42 10 4 4 -0.57 2.17 10 4 5 89.64 5.04 10 -4 5 79.63 4.58 10 4 6 1.60 1.87 10 4 6 0.76 1.65 10 4 6 1.44 1.55 10 -4 6 -0.47 1.51 10 4 7 2.37 1.66 10 4 7 -0.25 1.65 10 -4 8 0.84 1.44 10 4 9 5.60 1.53 10 -4 9 2.21 1.51 10 4 10 20.14 1.86 10 -4 10 23.26 2.11 10 -4 11 13.05 1.44 -10 -5 13 3.57 1.14 10 5 -12 0.77 1.01 -10 -5 12 0.89 1.17 10 5 -11 13.09 1.80 -10 -5 11 11.23 1.71 -10 5 11 12.80 1.94 -10 5 11 10.97 1.79 -10 -5 11 11.04 1.86 -10 5 10 -0.23 1.50 -10 -5 10 -0.62 1.34 -10 5 10 0.87 1.51 10 5 -10 -1.04 1.59 -10 5 9 2.85 1.75 10 5 -9 2.33 1.62 -10 -5 9 1.63 1.46 -10 -5 8 51.53 3.71 -10 5 7 323.77 11.63 -10 -5 7 331.25 11.46 -10 5 6 4.05 2.06 -10 5 5 43.13 3.68 -10 -5 5 48.53 3.61 -10 5 4 19.13 2.70 10 5 -4 20.34 2.58 -10 -5 4 14.85 2.30 -10 5 3 67.99 4.39 -10 -5 3 73.27 4.39 10 5 -3 73.65 4.43 10 -5 -2 349.68 11.41 -10 -5 2 355.78 11.80 10 5 -2 350.18 11.90 10 5 -1 11.94 2.22 10 -5 -1 16.47 2.19 10 5 0 2.31 1.95 10 -5 0 0.95 1.34 10 5 0 -0.94 1.55 10 5 1 25.52 3.00 10 -5 1 35.66 3.03 10 5 2 6.25 2.12 10 -5 2 9.79 1.97 10 5 3 1.09 1.97 10 -5 3 -0.22 1.47 10 5 4 24.21 2.75 10 5 4 28.67 3.11 10 5 4 24.50 2.82 10 -5 4 24.93 2.70 10 5 5 2.49 1.59 10 5 5 3.99 1.91 10 5 5 5.24 1.96 10 -5 5 6.15 1.76 10 5 6 56.87 3.74 10 5 6 56.89 3.84 10 -5 7 11.04 1.94 10 5 7 7.45 1.65 10 5 8 41.07 2.70 10 5 8 43.63 3.05 10 -5 8 37.06 2.80 10 5 9 10.47 1.62 10 -5 9 10.02 1.62 10 -5 10 4.45 1.10 -10 -6 12 -0.38 1.09 -10 -6 12 0.10 1.28 10 6 -11 21.35 1.81 -10 -6 11 21.42 1.86 10 6 -10 20.51 2.07 -10 -6 10 20.75 2.10 -10 6 10 19.27 2.21 -10 6 10 19.58 2.04 -10 -6 10 22.36 2.14 -10 6 9 5.48 1.68 -10 -6 9 2.96 1.43 -10 6 9 3.06 1.59 10 6 -9 4.14 1.55 -10 -6 8 15.21 2.11 -10 6 8 13.85 2.31 10 6 -7 120.10 5.70 -10 6 7 118.02 5.88 -10 -6 7 121.68 5.68 -10 -6 6 2.48 1.71 10 6 -6 1.00 1.63 -10 -6 5 7.33 1.98 10 6 -5 7.73 2.02 -10 6 4 15.12 2.48 -10 -6 4 21.45 2.54 10 6 -4 22.08 2.67 -10 6 3 20.45 2.65 10 6 -3 20.74 2.69 -10 6 2 113.64 5.71 10 6 -2 119.88 5.75 10 6 -1 1.00 1.56 10 6 0 41.84 3.27 10 6 0 42.56 3.14 10 6 1 50.48 3.74 10 6 1 46.50 3.45 10 6 2 -1.29 1.58 10 6 2 -0.70 1.62 10 6 3 0.47 1.47 10 -6 4 15.94 2.05 10 6 4 14.49 2.25 10 6 5 18.43 2.38 10 -6 5 12.60 1.94 10 6 6 61.47 3.67 10 -6 6 58.52 3.47 10 6 6 62.04 3.72 10 6 7 3.81 1.59 10 -6 7 4.54 1.47 10 6 7 3.76 1.33 10 -6 8 8.74 1.51 10 6 8 9.34 1.56 10 -6 9 -0.11 1.01 -10 -7 11 2.62 1.55 -10 7 10 22.62 1.94 -10 -7 10 17.12 1.62 10 7 -10 22.98 1.71 10 7 -9 103.82 4.36 -10 7 9 101.74 4.50 -10 -7 9 106.30 4.40 -10 7 9 101.96 4.23 -10 -7 9 98.50 4.09 10 7 -8 36.32 2.72 -10 -7 8 39.52 2.73 -10 7 8 36.92 2.84 -10 -7 8 33.23 2.39 -10 -7 7 8.38 1.74 -10 7 7 7.45 1.79 10 7 -7 4.56 1.59 -10 -7 6 32.01 2.70 -10 7 6 31.03 2.87 10 7 -6 36.02 2.97 -10 -7 5 73.66 4.20 -10 7 5 78.00 4.42 -10 -7 4 46.65 3.34 -10 7 4 52.12 3.57 -10 -7 3 1.09 1.42 -10 7 3 0.48 1.54 10 7 -3 1.19 1.55 -10 -7 2 45.73 3.16 -10 7 2 44.37 3.31 10 7 -2 47.66 3.18 10 7 -2 48.28 3.47 10 7 -1 2.36 1.48 10 7 -1 0.23 1.46 10 7 0 2.66 1.44 10 7 1 2.24 1.59 10 7 2 1.14 1.33 10 7 2 2.88 1.58 10 7 3 6.81 1.69 10 7 3 8.12 1.95 10 -7 3 6.08 1.43 10 7 4 14.45 1.91 10 7 4 12.44 1.99 10 -7 4 12.68 1.74 10 7 5 0.17 1.30 10 7 5 0.18 1.28 10 7 5 -1.28 1.16 10 -7 5 1.55 1.20 10 7 6 89.67 3.99 10 -7 6 82.79 3.77 10 -7 7 0.12 0.95 10 -7 8 2.16 1.36 -10 -8 9 6.07 1.59 -10 8 8 0.12 1.44 10 8 -8 0.11 1.29 -10 8 7 0.74 1.11 10 8 -7 -0.14 1.18 -10 -8 7 0.55 1.03 10 8 -6 58.42 3.21 -10 8 6 57.88 3.23 -10 -8 6 56.15 3.08 -10 -8 5 20.74 2.03 -10 8 5 22.24 2.21 10 8 -5 19.37 2.10 -10 -8 4 21.83 2.09 -10 8 4 20.76 2.17 10 8 -4 19.34 2.20 -10 -8 3 21.34 2.05 -10 8 3 22.50 2.20 10 8 -3 20.25 2.30 -10 -8 2 1.43 1.13 -10 8 2 1.57 1.28 10 8 -2 0.57 1.37 10 8 -1 16.19 1.79 10 8 -1 19.16 2.12 10 8 0 4.22 1.31 10 8 0 3.46 1.42 10 8 1 4.64 1.44 10 8 1 3.42 1.25 10 8 2 1.47 1.22 10 8 3 57.96 3.16 10 8 4 22.27 1.90 10 -8 4 17.24 1.55 10 9 -5 0.72 1.79 10 9 -4 6.42 1.80 10 9 -3 22.30 2.01 10 9 -2 24.46 1.89 10 9 -2 28.25 2.09 10 9 -1 1.15 1.09 10 9 -1 -0.47 1.11 10 9 0 6.35 1.10 10 9 0 7.28 1.53 10 9 1 7.57 1.62 -11 0 15 -1.09 1.42 -11 0 14 31.53 2.23 -11 0 14 31.60 2.07 -11 0 13 -1.59 1.35 -11 0 12 2.67 1.42 -11 0 11 0.87 1.42 -11 0 10 11.29 2.02 -11 0 10 16.46 2.44 -11 0 10 11.06 2.33 -11 0 9 3.73 1.99 -11 0 9 0.88 1.94 -11 0 8 153.14 6.62 -11 0 8 157.53 6.92 -11 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14 41.04 2.44 -11 -1 13 63.01 3.33 -11 1 13 66.39 3.33 -11 1 12 21.81 2.18 -11 -1 12 26.02 2.39 -11 1 12 21.28 2.47 -11 -1 11 -1.49 1.61 -11 1 11 -0.42 1.55 -11 1 11 1.04 1.73 -11 -1 10 27.71 2.74 -11 -1 10 26.30 2.84 -11 1 10 29.73 2.94 -11 1 10 33.75 2.87 -11 1 10 31.27 3.23 -11 -1 10 27.88 3.07 -11 -1 9 85.10 4.92 -11 1 9 81.45 4.78 -11 -1 9 85.75 5.07 -11 1 9 84.47 5.09 -11 -1 8 63.70 4.09 -11 1 8 56.26 3.84 -11 1 8 59.27 4.11 -11 -1 8 58.53 4.11 -11 -1 8 66.82 4.46 -11 1 8 61.54 4.42 -11 -1 7 264.51 9.49 -11 1 7 263.60 9.39 -11 -1 7 258.19 9.62 -11 1 7 253.77 9.53 -11 -1 7 251.84 9.77 -11 1 7 249.14 9.84 -11 -1 6 95.31 5.03 -11 1 6 97.26 4.97 -11 -1 6 89.17 5.19 -11 1 6 101.88 5.50 -11 -1 5 99.49 5.04 -11 1 5 102.96 5.08 -11 -1 5 95.70 5.18 -11 1 5 94.13 5.24 11 -1 -4 10.15 1.94 11 1 -4 7.30 1.89 -11 -1 4 8.65 2.08 11 1 -3 122.09 5.69 11 -1 -3 114.08 5.57 11 -1 -2 12.56 1.90 11 1 -2 10.99 1.84 11 1 -2 9.85 1.99 11 -1 -2 12.99 2.17 11 1 -1 218.67 8.44 11 -1 -1 228.33 8.53 11 -1 -1 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2 5 217.80 8.20 -11 -2 5 223.83 8.59 -11 2 4 160.53 6.93 -11 -2 4 177.50 6.95 -11 2 4 164.45 6.74 -11 2 4 164.22 7.20 -11 -2 4 160.24 6.92 -11 2 3 43.28 3.43 11 -2 -3 48.05 3.48 11 2 -3 52.27 3.60 -11 -2 3 49.57 3.50 -11 -2 2 75.26 4.20 11 2 -2 73.74 3.87 11 -2 -2 68.50 3.72 11 -2 -2 69.90 3.65 11 2 -2 76.03 3.86 11 -2 -2 68.04 4.10 11 2 -2 67.76 4.17 11 -2 -1 17.15 1.98 11 2 -1 22.80 2.27 11 2 -1 20.08 2.47 11 -2 -1 16.97 2.29 11 2 -1 22.95 2.19 11 -2 -1 14.01 1.86 11 -2 0 142.73 5.82 11 2 0 144.37 5.83 11 -2 0 142.86 5.77 11 2 0 150.22 5.91 11 -2 0 142.39 6.37 11 2 0 145.12 6.34 11 -2 1 24.62 2.30 11 2 1 23.33 2.30 11 -2 1 21.33 2.17 11 -2 1 23.58 2.34 11 2 1 22.11 2.32 11 2 2 199.65 7.45 11 -2 2 209.87 7.53 11 -2 2 208.56 7.56 11 2 2 209.84 7.62 11 -2 3 -0.20 1.30 11 -2 3 1.08 1.51 11 2 3 -0.21 1.33 11 -2 3 0.79 1.39 11 2 3 -0.79 1.41 11 -2 4 4.13 1.62 11 -2 4 5.88 1.68 11 2 4 4.65 1.50 11 -2 4 4.98 1.77 11 -2 4 7.11 1.76 11 2 4 3.45 1.60 11 -2 5 2.09 1.66 11 2 5 1.72 1.95 11 -2 5 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16.60 2.33 11 5 -2 48.90 3.53 11 5 -1 18.35 2.32 11 5 -1 9.02 2.05 11 5 0 8.23 2.10 11 5 1 73.07 4.55 11 -5 2 39.48 3.10 11 5 2 37.94 3.32 11 -5 3 21.45 2.67 11 5 3 28.07 2.94 11 -5 4 115.61 5.16 11 5 4 123.74 5.61 11 -5 5 0.20 1.38 11 5 5 1.14 1.65 11 5 5 3.58 1.58 11 -5 6 2.23 1.46 11 5 6 5.55 1.60 11 -5 7 11.74 1.74 11 5 7 12.35 1.64 11 -5 8 76.48 3.57 11 5 8 73.12 3.58 11 -5 9 61.49 2.91 11 5 9 60.23 2.93 11 6 -11 0.98 0.99 -11 -6 11 1.79 1.30 -11 -6 10 22.90 1.99 -11 -6 10 28.63 2.07 -11 6 10 31.19 2.31 -11 6 10 24.72 2.00 11 6 -10 29.62 2.17 -11 -6 9 18.69 2.03 -11 6 9 26.41 2.29 -11 6 9 19.17 2.18 11 6 -9 23.19 2.21 -11 6 8 9.99 1.81 11 6 -8 11.87 1.90 -11 -6 8 11.21 1.87 -11 -6 7 33.14 2.76 11 6 -7 33.40 2.87 -11 6 6 -0.24 1.47 -11 -6 6 1.78 1.63 -11 6 5 34.55 3.08 -11 -6 5 37.34 3.08 11 6 -5 42.67 3.33 -11 6 4 50.50 3.62 11 6 -4 51.69 3.63 -11 -6 4 47.98 3.35 -11 6 3 30.72 2.83 -11 -6 3 31.65 2.77 11 6 -3 30.05 2.91 -11 -6 2 82.58 4.38 11 6 -2 90.83 4.70 11 6 -1 5.86 1.79 11 6 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3.79 1.22 11 7 5 9.00 1.51 11 7 5 6.44 1.39 11 -7 5 4.96 1.12 11 7 6 48.64 2.66 11 -7 6 46.36 2.29 11 8 -7 20.95 2.09 -11 8 6 95.85 3.95 11 8 -6 96.26 4.06 -11 8 5 0.77 1.00 11 8 -5 4.69 1.38 -11 8 4 -0.13 0.96 11 8 -4 0.15 1.16 -11 8 3 0.63 0.95 11 8 -3 1.64 1.19 11 8 -2 1.03 1.23 11 8 -1 13.02 1.44 11 8 -1 12.22 1.60 11 8 0 24.51 1.92 11 8 1 40.88 2.41 11 8 2 97.52 4.03 11 8 3 0.68 0.93 -12 0 14 -0.30 1.28 -12 0 13 -0.52 1.05 -12 0 12 199.46 6.99 -12 0 11 -0.19 1.38 -12 0 11 -0.24 1.64 -12 0 10 78.53 4.49 -12 0 10 69.15 4.07 -12 0 10 77.57 4.61 -12 0 9 0.76 1.64 -12 0 9 0.47 1.49 -12 0 9 -0.28 1.78 -12 0 8 -0.52 1.55 -12 0 8 1.70 1.92 -12 0 7 -0.53 1.70 -12 0 7 0.25 1.65 -12 0 7 1.70 1.93 -12 0 6 158.94 6.86 -12 0 6 159.33 7.18 -12 0 5 -2.42 1.73 -12 0 5 0.97 1.64 -12 0 4 26.79 2.87 12 0 -3 -0.20 1.46 12 0 -2 1.81 1.47 12 0 -1 0.20 1.47 12 0 0 407.07 12.73 12 0 1 -1.46 1.60 12 0 1 -1.03 1.52 12 0 2 12.09 1.90 12 0 2 11.00 1.97 12 0 3 0.86 1.44 12 0 3 -0.21 1.46 12 0 4 129.95 5.67 12 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0.80 1.54 12 1 -1 92.96 4.63 12 -1 -1 96.25 4.63 12 -1 0 22.75 2.48 12 1 0 25.98 2.57 12 -1 0 29.24 2.61 12 -1 1 69.90 3.98 12 1 1 78.01 4.15 12 -1 1 72.41 4.04 12 1 1 77.01 4.10 12 -1 2 90.38 4.63 12 1 2 91.52 4.59 12 -1 2 94.12 4.70 12 1 2 99.93 4.79 12 -1 3 102.29 4.86 12 -1 3 106.87 5.00 12 1 3 101.06 4.85 12 -1 3 103.08 4.97 12 1 3 102.53 4.96 12 -1 4 65.77 3.80 12 -1 4 60.35 3.70 12 1 4 56.82 3.62 12 -1 4 56.36 3.59 12 1 4 57.40 3.62 12 -1 5 209.78 7.82 12 -1 5 200.74 7.73 12 -1 6 80.57 4.35 12 1 6 85.26 4.44 12 1 6 74.58 4.55 12 -1 6 81.71 4.21 12 -1 7 328.15 10.59 12 -1 7 312.91 10.48 12 1 7 323.86 10.54 12 -1 7 315.95 10.44 12 1 7 311.78 10.45 12 -1 8 287.51 9.39 12 1 8 278.68 9.31 12 -1 8 299.33 9.49 12 1 8 271.21 9.28 12 -1 9 18.53 1.88 12 1 9 15.89 1.79 12 -1 9 10.33 1.64 12 1 9 12.52 1.68 12 -1 10 -0.62 0.96 12 1 10 0.25 1.00 12 -1 10 0.74 1.04 12 1 10 0.37 1.02 12 -1 11 14.64 1.61 12 1 11 15.45 1.65 -12 2 14 20.90 1.58 -12 -2 14 24.90 1.67 -12 -2 13 4.59 1.08 -12 2 13 5.16 1.12 -12 2 12 5.36 1.56 -12 -2 12 5.17 1.15 -12 -2 12 6.46 1.33 -12 2 12 5.62 1.22 -12 2 11 -0.43 1.55 -12 -2 11 -0.51 1.20 -12 2 11 -0.82 1.17 -12 -2 10 353.25 11.44 -12 2 10 349.75 11.38 -12 -2 10 359.56 11.21 -12 2 10 327.01 10.91 -12 2 10 349.85 11.76 -12 -2 9 8.02 1.78 -12 2 9 8.36 1.78 -12 -2 8 2.46 1.64 -12 2 8 1.95 1.58 -12 2 8 1.70 1.97 -12 -2 8 0.46 1.51 -12 2 8 2.00 1.52 -12 2 7 24.82 2.74 -12 -2 7 24.81 2.82 -12 2 7 26.31 3.15 -12 -2 6 68.31 4.17 -12 2 6 62.63 3.94 -12 -2 6 60.39 3.99 -12 -2 6 66.39 4.15 -12 2 6 65.43 4.47 -12 -2 5 256.96 9.10 -12 2 5 232.13 8.79 -12 -2 4 224.54 8.59 -12 2 4 229.57 8.58 12 -2 -4 237.57 8.21 -12 -2 4 228.32 8.75 12 -2 -3 141.20 5.84 12 2 -3 141.33 5.89 12 2 -2 228.95 8.17 12 -2 -2 231.48 8.15 12 2 -1 56.24 3.49 12 -2 -1 52.70 3.36 12 -2 0 39.84 2.97 12 2 0 39.49 2.95 12 2 0 36.73 2.83 12 -2 0 33.89 2.78 12 -2 1 3.18 1.37 12 2 1 2.99 1.46 12 -2 1 5.44 1.61 12 2 1 4.49 1.57 12 -2 2 63.44 3.63 12 2 2 58.20 3.55 12 -2 2 60.23 3.63 12 2 2 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-1.10 1.30 15 0 -7 0.44 1.11 15 0 -6 109.45 4.49 -15 0 6 103.86 4.83 -15 0 5 -0.38 1.50 -15 0 5 -0.41 1.41 15 0 -5 1.48 1.17 15 0 -4 345.84 10.82 -15 0 4 350.10 11.22 15 0 -3 -2.44 1.52 -15 0 3 -1.00 1.60 15 0 -2 181.22 6.57 -15 0 2 165.53 6.72 15 0 -1 -0.70 1.43 15 0 0 248.82 8.36 15 0 1 0.66 1.25 15 0 1 0.17 1.23 15 0 2 3.65 1.33 15 0 2 6.75 1.45 15 0 3 -0.65 1.16 15 0 4 227.58 6.52 15 0 4 218.05 6.31 15 0 5 -0.78 1.05 15 0 5 0.66 0.98 15 0 5 0.85 1.26 15 0 6 55.51 2.44 15 0 6 58.04 2.45 15 0 7 1.09 1.41 15 -1 -10 4.79 1.00 15 1 -10 4.63 1.09 -15 -1 9 4.26 1.14 -15 1 9 4.62 1.10 -15 -1 9 5.04 1.27 -15 1 9 7.26 1.31 15 -1 -9 5.30 1.09 15 1 -9 7.65 1.17 -15 -1 8 64.17 3.32 -15 1 8 61.47 3.24 -15 -1 8 45.18 2.86 -15 1 8 47.38 2.83 15 -1 -8 54.99 2.82 15 1 -8 58.79 2.93 -15 1 8 64.50 3.31 -15 -1 7 0.89 1.29 -15 1 7 -0.88 1.27 15 -1 -7 0.56 1.04 15 1 -7 1.14 1.14 -15 1 7 0.69 1.25 -15 -1 7 1.15 1.25 -15 1 7 1.61 1.22 -15 -1 6 11.19 1.86 -15 1 6 10.80 1.76 15 -1 -6 10.43 1.57 15 1 -6 10.58 1.52 -15 1 6 8.21 1.62 -15 -1 6 8.34 1.61 -15 1 6 10.12 1.73 -15 -1 5 1.50 1.43 -15 1 5 3.32 1.46 15 -1 -5 2.55 1.25 15 1 -5 2.58 1.29 -15 -1 5 3.59 1.48 -15 1 5 1.19 1.45 -15 -1 4 201.56 7.62 -15 1 4 206.48 7.65 15 -1 -4 214.02 7.37 15 1 -4 225.01 7.47 -15 -1 3 0.59 1.48 -15 1 3 -1.36 1.49 15 -1 -3 -1.69 1.32 15 1 -3 -0.34 1.32 -15 -1 2 20.20 2.29 -15 1 2 14.85 2.07 15 -1 -2 16.04 1.88 15 1 -2 16.59 1.95 15 -1 -1 1.02 1.24 15 1 -1 1.21 1.18 15 -1 0 30.40 2.36 15 1 0 24.11 2.23 15 -1 1 25.15 2.18 15 1 1 23.79 2.15 15 -1 1 24.55 2.35 15 -1 1 24.19 2.15 15 1 1 20.94 2.05 15 -1 2 2.76 1.17 15 1 2 4.01 1.31 15 -1 2 1.11 1.08 15 1 2 0.96 1.11 15 -1 2 3.97 1.36 15 1 3 45.20 2.69 15 -1 3 55.49 3.01 15 -1 4 1.26 1.10 15 1 4 -0.14 1.06 15 1 4 2.29 0.97 15 -1 4 2.14 1.02 15 1 4 0.17 1.44 15 1 5 5.85 1.44 15 -1 5 5.53 1.36 15 -1 5 16.11 1.58 15 1 5 20.25 1.72 15 -1 5 17.52 1.66 15 1 5 13.01 1.57 15 -1 6 36.08 1.96 15 1 6 40.75 2.07 15 -1 6 38.36 2.08 15 1 6 36.69 2.07 15 -1 7 3.07 1.40 15 1 7 5.05 1.43 15 -2 -9 1.46 0.86 15 2 -9 1.93 0.89 -15 2 9 2.16 1.17 -15 -2 8 -0.56 1.15 -15 2 8 0.28 1.14 -15 -2 8 -0.13 0.97 -15 2 8 0.61 0.92 15 -2 -8 0.87 0.93 15 2 -8 1.37 0.94 -15 2 8 -1.24 1.19 15 -2 -7 44.41 2.51 15 2 -7 52.30 2.68 -15 -2 7 42.90 2.74 -15 2 7 46.54 2.83 -15 -2 7 39.24 2.58 -15 2 7 45.27 2.64 -15 2 7 52.11 3.06 -15 -2 6 11.95 1.75 -15 2 6 10.39 1.70 -15 -2 6 9.82 1.60 -15 2 6 10.81 1.62 15 -2 -6 13.74 1.57 15 2 -6 11.96 1.55 -15 2 6 11.23 1.75 15 -2 -5 99.02 4.07 15 2 -5 93.60 4.01 -15 2 5 98.96 4.42 -15 2 5 87.44 4.17 -15 -2 5 91.61 4.35 -15 2 5 92.58 4.33 15 -2 -5 96.78 4.05 15 2 -4 135.10 5.03 15 -2 -4 126.60 4.89 15 -2 -4 123.68 4.85 15 2 -4 119.03 4.86 15 -2 -4 128.61 5.03 -15 -2 4 106.88 4.99 -15 2 4 115.91 5.02 15 -2 -3 1.38 1.15 15 2 -3 1.42 1.15 15 -2 -3 3.36 1.27 -15 -2 3 4.54 1.56 -15 2 3 1.58 1.36 15 -2 -3 2.28 1.29 15 2 -3 3.40 1.35 15 -2 -2 12.10 1.65 15 2 -2 19.16 1.90 15 -2 -2 16.50 1.94 -15 -2 2 14.43 1.94 -15 2 2 12.94 1.88 15 -2 -2 14.70 1.76 15 2 -2 15.23 1.77 15 -2 -1 15.84 1.76 15 2 -1 9.41 1.54 15 -2 -1 10.61 1.76 -15 -2 1 10.17 1.82 -15 2 1 11.45 1.83 15 -2 -1 14.32 1.73 15 2 -1 13.29 1.66 15 -2 0 2.77 1.24 15 2 0 4.74 1.31 15 -2 0 1.65 1.13 15 2 0 3.34 1.31 15 2 0 1.43 1.55 15 -2 0 6.42 1.44 15 -2 1 8.52 1.42 15 2 1 10.45 1.54 15 -2 1 6.38 1.29 15 2 1 7.50 1.45 15 -2 1 8.43 1.58 15 2 2 16.53 1.70 15 -2 2 20.25 2.01 15 -2 3 24.84 2.10 15 -2 3 23.68 1.92 15 2 3 22.89 1.92 15 -2 4 11.15 1.47 15 2 4 13.78 1.55 15 -2 4 14.33 1.53 15 2 4 14.92 1.56 15 -2 4 10.58 1.38 15 2 5 1.53 1.18 15 -2 5 2.98 1.13 15 2 5 2.23 1.11 15 -2 5 5.60 1.06 15 2 5 3.66 0.99 15 -2 5 5.65 1.06 15 2 5 6.70 1.17 15 -2 6 27.13 1.58 15 2 6 27.83 1.75 15 2 6 26.32 1.59 15 3 -10 5.26 1.74 -15 3 9 6.72 1.65 15 3 -9 6.27 1.45 15 3 -8 7.47 1.00 15 3 -8 8.06 1.33 15 3 -8 6.86 1.01 -15 3 8 10.55 1.55 15 3 -7 19.52 1.55 15 3 -7 23.15 1.93 15 3 -7 20.89 1.53 -15 3 7 21.17 1.95 -15 -3 7 20.29 1.74 -15 3 7 20.42 1.72 -15 3 6 16.82 1.89 15 -3 -6 17.47 1.49 15 3 -6 16.06 1.47 15 3 -6 15.15 1.43 15 3 -6 18.52 1.80 15 -3 -6 19.31 1.51 -15 -3 6 11.64 1.46 -15 3 6 12.95 1.41 -15 -3 6 14.13 1.58 -15 3 6 16.29 1.67 -15 -3 5 45.88 2.82 -15 -3 5 63.07 3.17 -15 3 5 69.48 3.29 -15 3 5 52.17 2.88 15 3 -5 70.01 3.28 15 -3 -5 60.39 2.83 15 3 -5 63.86 2.97 15 -3 -5 61.62 2.85 15 3 -5 59.33 2.87 -15 3 5 60.85 3.34 15 -3 -4 -0.48 0.98 15 3 -4 0.64 0.96 15 -3 -4 0.72 0.91 15 3 -4 0.12 0.96 -15 -3 4 0.74 1.09 -15 3 4 0.28 1.03 -15 -3 4 0.15 1.08 -15 3 4 0.15 1.09 15 -3 -3 26.37 1.98 15 3 -3 30.76 2.12 15 -3 -3 27.84 1.96 15 3 -3 28.71 2.03 15 -3 -3 31.14 2.23 -15 -3 3 23.60 2.14 -15 3 3 21.34 1.95 -15 -3 3 29.40 2.26 15 3 -2 44.10 2.55 15 -3 -2 42.95 2.51 15 -3 -2 47.15 2.83 15 -3 -2 46.59 2.54 15 3 -2 50.42 2.65 -15 -3 2 35.91 2.56 -15 3 2 36.06 2.53 15 3 -1 0.67 1.36 -15 -3 1 -1.07 1.31 -15 3 1 -1.29 1.18 15 -3 -1 -1.13 1.11 15 3 -1 -2.32 1.18 15 -3 -1 -0.51 1.15 15 -3 -1 -1.41 1.18 15 3 -1 -1.62 1.18 15 3 0 1.55 1.42 -15 -3 0 4.89 1.34 -15 3 0 5.42 1.28 15 -3 0 5.52 1.14 15 3 0 5.42 1.19 15 -3 0 7.16 1.21 15 3 0 5.05 1.17 15 -3 0 8.19 1.49 -15 -3 -1 4.93 1.31 -15 3 -1 5.41 1.28 15 -3 1 9.16 1.54 15 3 1 6.63 1.29 15 -3 2 1.64 1.00 15 3 2 1.57 1.06 15 3 2 -0.16 1.34 15 -3 3 25.88 1.79 15 3 3 29.43 1.88 15 -3 3 32.78 2.18 15 -3 3 28.26 1.81 15 3 3 29.56 1.90 15 3 4 20.80 1.50 15 3 4 22.53 1.66 15 3 4 24.39 1.55 15 3 4 22.40 1.90 15 3 5 42.15 1.94 15 3 5 50.37 2.53 15 4 -8 4.00 1.37 -15 4 7 0.38 1.15 15 4 -7 0.56 0.90 -15 4 6 13.44 1.64 15 4 -6 14.12 1.48 -15 4 5 49.43 2.84 15 4 -5 50.14 2.62 -15 4 4 4.80 1.30 15 -4 -3 8.00 1.23 15 -4 -2 15.07 1.56 15 -4 -1 35.12 2.16 15 4 -1 -0.12 1.11 15 -4 0 9.88 1.44 15 4 0 -0.79 1.18 15 -4 1 3.92 1.16 15 4 1 -0.40 1.17 15 4 2 -0.69 1.20 15 4 2 0.94 1.13 15 4 2 0.38 1.17 15 4 3 93.16 3.81 15 4 3 87.37 3.67 15 4 4 4.03 1.55 15 4 5 8.17 1.77 15 5 -6 56.01 2.51 15 5 -3 22.64 1.74 15 5 -2 -0.12 0.92 15 5 -1 5.58 1.27 15 5 -1 4.81 1.05 15 5 0 3.30 1.20 15 5 0 3.50 0.99 15 5 1 41.61 2.37 15 5 1 39.28 2.48 15 5 2 21.42 1.95 15 5 2 23.74 2.00 15 5 3 28.17 2.12 16 0 -8 64.23 2.77 -16 0 8 62.04 3.07 -16 0 7 0.41 0.99 -16 0 7 0.12 0.94 16 0 -7 0.33 0.87 16 0 -6 0.36 0.96 -16 0 6 0.68 1.05 -16 0 6 3.56 1.29 16 0 -6 2.60 1.08 16 0 -5 -0.39 1.03 -16 0 5 -0.64 1.22 16 0 -5 -0.13 1.03 -16 0 5 -0.88 1.11 16 0 -4 62.12 3.03 16 0 -4 64.06 3.09 -16 0 4 63.61 3.43 16 0 -3 -0.14 1.08 16 0 -3 0.27 1.12 -16 0 3 1.43 1.33 16 0 -2 67.50 3.25 16 0 -2 72.10 3.32 16 0 -1 -1.35 1.20 -16 0 1 -0.32 1.35 16 0 -1 -0.28 1.26 16 0 0 8.59 1.44 -16 0 0 4.62 1.42 16 0 0 7.13 1.38 16 0 1 -0.73 1.07 16 0 1 -0.53 1.07 16 0 1 -0.51 1.11 16 0 2 -0.40 0.90 16 0 2 1.08 1.41 16 0 3 0.54 1.17 16 0 3 0.34 0.99 16 0 4 -0.65 1.46 16 0 4 0.30 1.18 16 0 4 0.91 1.06 16 0 5 0.40 1.36 16 -1 -9 8.29 1.34 16 1 -9 10.10 1.45 16 -1 -8 89.21 3.42 16 1 -8 86.95 3.42 16 -1 -8 93.43 3.41 16 1 -8 89.80 3.44 -16 -1 8 91.91 3.69 -16 1 8 88.70 3.66 16 -1 -7 1.02 0.83 16 1 -7 2.19 0.97 16 -1 -7 2.12 0.90 16 1 -7 1.43 0.91 -16 -1 7 0.90 1.02 -16 1 7 1.92 1.13 16 -1 -6 6.60 1.18 16 1 -6 8.11 1.27 16 -1 -6 7.41 1.20 16 1 -6 6.13 1.21 -16 -1 6 3.56 1.15 -16 1 6 4.24 1.14 -16 -1 6 9.50 1.50 -16 1 6 7.10 1.37 -16 -1 5 1.98 1.22 -16 1 5 1.98 1.17 16 -1 -5 0.94 0.84 16 -1 -5 1.10 0.99 16 1 -5 2.75 1.11 16 -1 -5 2.17 1.05 -16 1 5 0.98 1.08 -16 -1 5 1.28 1.10 -16 -1 4 17.43 1.86 -16 1 4 18.24 1.91 -16 -1 4 20.75 2.07 -16 1 4 27.02 2.22 16 -1 -4 19.06 1.77 16 1 -4 21.49 1.87 16 -1 -4 24.95 1.92 16 1 -4 22.63 1.85 16 -1 -4 21.90 1.81 16 -1 -3 1.18 1.08 -16 1 3 -1.97 1.37 16 -1 -3 -0.40 1.16 16 1 -3 -0.67 1.19 16 1 -3 0.55 1.13 16 -1 -3 -0.78 1.23 16 1 -3 -0.79 1.18 -16 -1 2 66.46 3.29 -16 1 2 65.51 3.23 16 -1 -2 82.40 3.27 16 1 -2 87.33 3.36 16 -1 -2 88.38 3.55 16 -1 -2 80.43 3.21 16 1 -2 84.96 3.29 -16 -1 1 33.46 2.42 16 -1 -1 38.11 2.34 16 1 -1 42.85 2.46 16 -1 -1 40.81 2.52 16 -1 -1 38.32 2.30 16 1 -1 40.87 2.35 -16 -1 0 23.85 2.12 -16 1 0 24.49 2.09 16 -1 0 33.13 2.17 16 1 0 32.52 2.17 16 -1 0 37.55 2.40 16 -1 0 37.99 2.26 16 1 0 32.28 2.13 16 -1 1 20.63 1.75 16 1 1 21.90 1.78 16 -1 1 21.06 1.89 16 1 2 31.02 1.99 16 -1 2 37.97 2.21 16 -1 3 0.76 0.90 16 1 3 3.93 1.16 16 1 3 1.29 1.38 16 -1 3 0.88 0.92 16 -1 4 5.26 1.21 16 1 4 5.23 1.22 16 -1 4 6.66 1.33 16 1 4 5.05 1.28 16 1 4 1.05 1.57 16 -1 4 -0.20 1.32 16 -1 5 9.91 1.56 16 1 5 9.39 1.60 16 -2 -8 4.98 1.00 16 2 -8 5.24 1.18 16 2 -8 5.77 1.11 16 -2 -7 22.35 1.48 16 2 -7 23.85 1.56 16 -2 -7 20.03 1.39 16 2 -7 20.15 1.52 -16 -2 7 20.16 1.61 -16 2 7 20.24 1.62 -16 -2 6 0.36 0.90 -16 2 6 0.61 0.95 16 -2 -6 0.75 0.82 16 2 -6 1.26 0.86 16 -2 -6 0.67 0.75 16 2 -6 -0.10 0.84 16 -2 -5 63.80 2.72 16 2 -5 62.32 2.74 -16 -2 5 35.55 2.47 -16 -2 5 62.24 2.97 -16 2 5 68.33 3.11 -16 2 5 39.02 2.47 16 -2 -5 61.28 2.70 16 2 -5 63.75 2.76 -16 -2 4 21.84 1.98 -16 2 4 25.85 2.01 -16 -2 4 38.26 2.37 -16 2 4 32.02 2.25 16 -2 -4 36.26 2.10 16 2 -4 35.77 2.12 16 -2 -4 36.14 2.11 16 -2 -4 37.43 2.11 16 2 -4 38.86 2.17 -16 -2 3 32.20 2.42 -16 2 3 30.43 2.33 -16 -2 3 50.64 2.84 -16 2 3 55.86 2.88 16 -2 -3 55.57 2.63 16 2 -3 53.09 2.64 16 -2 -3 50.13 2.56 16 2 -3 52.96 2.60 16 -2 -3 49.86 2.64 -16 -2 2 69.42 3.07 -16 2 2 69.90 3.06 16 -2 -2 98.94 3.24 16 2 -2 109.84 3.45 16 -2 -2 107.96 3.63 16 -2 -2 99.86 3.23 16 2 -2 105.52 3.32 16 -2 -1 -0.11 1.11 16 2 -1 -0.58 1.06 16 -2 -1 -1.64 1.06 16 2 -1 -1.34 1.17 16 -2 -1 0.14 0.99 16 2 -1 0.41 1.15 -16 -2 1 -1.64 1.28 -16 2 1 -1.18 1.14 16 -2 0 0.22 0.97 16 2 0 -0.45 1.00 16 -2 0 -0.34 0.93 16 2 0 -0.71 0.99 -16 -2 0 -1.18 1.04 -16 2 0 -0.38 1.10 16 2 0 1.27 1.26 16 -2 0 -0.57 1.00 -16 -2 -1 3.58 1.15 16 2 1 0.69 1.31 16 -2 2 6.20 1.17 16 -2 2 8.14 1.18 16 2 2 7.49 1.18 16 -2 3 35.55 1.82 16 2 3 29.90 1.85 16 -2 3 34.32 1.81 16 2 3 32.45 1.92 16 2 4 24.38 1.86 16 -2 4 24.65 1.58 16 2 4 29.35 1.79 16 3 -6 0.84 0.63 16 3 -5 150.48 4.74 16 3 -4 17.45 1.34 16 3 -4 16.30 1.35 16 3 -3 -0.74 0.77 16 3 -3 0.35 0.70 -16 -3 3 -0.84 0.94 16 3 -2 1.32 0.84 16 3 -2 1.76 0.83 -16 -3 2 0.21 0.90 16 3 -1 32.37 1.70 16 -3 -1 37.05 2.05 -16 -3 1 34.17 1.85 16 3 0 0.87 1.02 16 -3 0 1.47 0.93 16 3 1 99.71 2.61 16 3 1 0.54 1.38 16 3 2 12.23 1.41 16 3 2 10.74 1.05 16 3 3 3.91 1.58 16 4 -2 3.00 0.93 16 4 -1 0.72 1.10 16 4 -1 0.54 1.37 16 4 0 1.73 1.40 16 4 0 0.63 1.39 16 4 1 42.68 2.42 16 4 2 28.44 2.12 17 0 -7 0.50 1.35 17 0 -6 5.49 1.46 -17 0 5 1.05 1.42 17 0 -5 -0.17 1.20 17 0 -5 0.34 1.12 -17 0 4 2.03 1.33 17 0 -4 0.98 1.16 17 0 -4 0.18 1.10 -17 0 3 -0.12 1.26 17 0 -3 -0.93 1.15 17 0 -3 0.38 1.02 17 0 -2 7.22 1.23 17 0 -2 6.37 1.23 -17 0 2 5.19 1.37 17 0 -1 -1.57 1.14 17 0 -1 0.42 1.38 17 0 -1 -0.29 1.01 17 0 0 0.74 1.68 17 0 1 -1.05 1.28 17 0 1 1.37 1.76 17 0 2 3.21 1.48 17 0 2 1.59 1.82 17 -1 -6 1.68 1.20 17 1 -6 0.14 1.23 17 -1 -5 2.91 1.22 17 1 -5 2.49 1.28 17 1 -4 71.39 2.90 17 -1 -4 68.81 2.86 -17 -1 4 68.86 3.12 -17 1 4 68.74 3.10 17 -1 -4 63.04 2.78 17 1 -4 68.18 2.93 17 -1 -3 5.09 1.10 17 1 -3 6.71 1.27 -17 -1 3 6.02 1.44 -17 1 3 6.50 1.37 17 -1 -3 4.50 1.16 17 1 -3 5.35 1.23 17 -1 -2 6.79 1.15 17 1 -2 10.25 1.38 -17 -1 2 4.64 1.33 -17 1 2 9.01 1.45 17 -1 -2 8.49 1.29 17 1 -2 8.35 1.29 17 1 -1 0.46 1.20 17 -1 -1 0.36 0.96 17 1 -1 0.92 1.10 17 -1 -1 1.54 1.04 17 1 -1 1.31 1.16 17 1 0 0.28 1.48 17 -1 1 0.08 1.24 17 1 1 -0.81 1.33 17 1 1 1.77 1.85 17 -1 1 0.67 1.82 17 -1 2 57.81 2.60 17 1 2 57.41 2.61 17 -2 -4 20.80 1.48 17 2 -4 22.02 1.60 17 -2 -3 43.30 2.00 17 2 -3 41.71 2.12 17 2 -2 43.86 2.12 17 2 0 9.73 1.39 0 0 0 0.00 0.00 TITL nisoldipine 1,4-dioxane solvate_auto in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 14.092718 9.225294 14.513936 90.0000 97.1641 90.0000 ZERR 35.00 0.000452 0.000368 0.000468 0.0000 0.0030 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 35.00 35.00 35.00 35.00 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 95778 _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 1,4-dioxane solvate' _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 1.293 _oxdiff_exptl_absorpt_empirical_full_min 0.806 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 O4 O 0.56535(6) 0.87282(11) 0.38591(6) 0.0260(2) Uani 1 1 d . . . . . O1 O 0.22254(7) 0.45277(11) 0.32906(6) 0.0288(2) Uani 1 1 d . . . . . O2 O 0.22512(7) 0.33432(11) 0.46395(7) 0.0320(2) Uani 1 1 d . . . . . O5 O 0.24229(7) 0.70579(12) 0.19055(6) 0.0339(2) Uani 1 1 d . . . . . O3 O 0.45627(7) 0.79016(13) 0.27391(6) 0.0369(3) Uani 1 1 d . . . . . O6 O 0.09496(7) 0.65781(13) 0.20801(7) 0.0382(3) Uani 1 1 d . . . . . N1 N 0.41358(8) 0.66704(13) 0.57926(7) 0.0233(2) Uani 1 1 d . . . . . O1S O 0.02628(9) 0.94721(14) 0.09086(7) 0.0441(3) Uani 1 1 d . . . . . N2 N 0.17237(8) 0.71670(13) 0.23265(7) 0.0267(3) Uani 1 1 d . . . . . C8 C 0.43182(8) 0.74381(14) 0.42821(8) 0.0193(3) Uani 1 1 d . . . . . C6 C 0.46464(9) 0.74313(14) 0.52036(8) 0.0208(3) Uani 1 1 d . . . . . C10 C 0.25493(8) 0.79547(14) 0.38752(8) 0.0197(3) Uani 1 1 d . . . . . C16 C 0.48370(8) 0.80316(15) 0.35597(8) 0.0206(3) Uani 1 1 d . . . . . C11 C 0.17907(9) 0.80843(15) 0.31593(8) 0.0225(3) Uani 1 1 d . . . . . C9 C 0.33432(9) 0.67987(14) 0.39342(8) 0.0195(3) Uani 1 1 d . . . . . H9 H 0.336726 0.638702 0.330011 0.023 Uiso 1 1 calc R U . . . C3 C 0.31133(9) 0.55775(14) 0.45806(8) 0.0207(3) Uani 1 1 d . . . . . C15 C 0.25151(9) 0.89044(15) 0.46193(9) 0.0240(3) Uani 1 1 d . . . . . H15 H 0.300978 0.886021 0.512695 0.029 Uiso 1 1 calc R U . . . C2 C 0.24977(9) 0.43766(15) 0.42121(9) 0.0232(3) Uani 1 1 d . . . . . C4 C 0.34578(9) 0.56397(15) 0.54944(9) 0.0225(3) Uani 1 1 d . . . . . C14 C 0.17887(10) 0.99080(16) 0.46465(10) 0.0290(3) Uani 1 1 d . . . . . H14 H 0.179470 1.053819 0.516489 0.035 Uiso 1 1 calc R U . . . C7 C 0.55277(9) 0.81503(16) 0.56856(8) 0.0255(3) Uani 1 1 d . . . . . H7A H 0.553833 0.805326 0.635919 0.038 Uiso 1 1 calc R U . . . H7B H 0.552282 0.918000 0.551908 0.038 Uiso 1 1 calc R U . . . H7C H 0.609693 0.768686 0.549306 0.038 Uiso 1 1 calc R U . . . C12 C 0.10500(9) 0.90710(16) 0.31732(10) 0.0286(3) Uani 1 1 d . . . . . H12 H 0.054629 0.910914 0.267369 0.034 Uiso 1 1 calc R U . . . C13 C 0.10526(10) 0.99965(16) 0.39201(10) 0.0309(3) Uani 1 1 d . . . . . H13 H 0.055509 1.068732 0.393642 0.037 Uiso 1 1 calc R U . . . C5 C 0.31923(11) 0.46763(17) 0.62572(9) 0.0313(3) Uani 1 1 d . . . . . H5A H 0.349269 0.504034 0.685809 0.047 Uiso 1 1 calc R U . . . H5B H 0.341537 0.368763 0.616247 0.047 Uiso 1 1 calc R U . . . H5C H 0.249589 0.467282 0.624851 0.047 Uiso 1 1 calc R U . . . C17 C 0.61719(10) 0.92963(18) 0.31435(10) 0.0322(3) Uani 1 1 d . . . . . H17A H 0.629928 0.851303 0.271967 0.048 Uiso 1 1 calc R U . . . H17B H 0.677897 0.971110 0.342760 0.048 Uiso 1 1 calc R U . . . H17C H 0.578998 1.005111 0.279672 0.048 Uiso 1 1 calc R U . . . C1 C 0.16297(11) 0.33788(18) 0.28651(11) 0.0361(3) Uani 1 1 d . . . . . H1A H 0.145043 0.359623 0.220541 0.054 Uiso 1 1 calc R U . . . H1B H 0.105139 0.329798 0.317299 0.054 Uiso 1 1 calc R U . . . H1C H 0.198262 0.246150 0.292765 0.054 Uiso 1 1 calc R U . . . C2S C 0.02082(12) 1.09864(19) 0.07191(11) 0.0399(4) Uani 1 1 d . . . . . H2SA H 0.084757 1.134794 0.061473 0.048 Uiso 1 1 calc R U . . . H2SB H 0.001273 1.150274 0.126299 0.048 Uiso 1 1 calc R U . . . C1S C 0.04953(12) 0.86956(19) 0.01200(11) 0.0393(4) Uani 1 1 d . . . . . H1SA H 0.049479 0.764281 0.025199 0.047 Uiso 1 1 calc R U . . . H1SB H 0.114572 0.896960 -0.000686 0.047 Uiso 1 1 calc R U . . . H1 H 0.4327(12) 0.6731(18) 0.6397(12) 0.031(4) 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 O4 0.0256(5) 0.0334(5) 0.0197(4) -0.0018(4) 0.0055(3) -0.0077(4) O1 0.0316(5) 0.0283(5) 0.0261(5) -0.0040(4) 0.0015(4) -0.0085(4) O2 0.0346(5) 0.0247(5) 0.0372(5) 0.0036(4) 0.0061(4) -0.0029(4) O5 0.0374(5) 0.0439(6) 0.0203(5) -0.0029(4) 0.0035(4) 0.0008(5) O3 0.0334(5) 0.0622(8) 0.0148(4) 0.0023(5) 0.0018(4) -0.0146(5) O6 0.0324(5) 0.0403(6) 0.0381(6) -0.0041(5) -0.0112(4) -0.0080(5) N1 0.0265(5) 0.0292(6) 0.0140(5) 0.0019(4) 0.0023(4) 0.0010(5) O1S 0.0579(7) 0.0452(7) 0.0302(5) 0.0028(5) 0.0099(5) 0.0067(6) N2 0.0287(6) 0.0288(6) 0.0207(5) 0.0016(5) -0.0044(4) -0.0009(5) C8 0.0191(6) 0.0221(6) 0.0168(6) -0.0006(5) 0.0027(4) 0.0015(5) C6 0.0215(6) 0.0226(6) 0.0184(6) 0.0003(5) 0.0032(4) 0.0033(5) C10 0.0200(6) 0.0207(6) 0.0184(6) 0.0033(5) 0.0028(4) -0.0017(5) C16 0.0193(6) 0.0241(7) 0.0184(6) -0.0007(5) 0.0021(4) 0.0010(5) C11 0.0225(6) 0.0243(7) 0.0203(6) 0.0020(5) 0.0013(5) -0.0033(5) C9 0.0210(6) 0.0222(6) 0.0154(5) -0.0006(5) 0.0028(4) 0.0004(5) C3 0.0207(6) 0.0202(6) 0.0219(6) 0.0009(5) 0.0061(5) 0.0029(5) C15 0.0261(6) 0.0237(7) 0.0215(6) 0.0001(5) 0.0005(5) 0.0023(5) C2 0.0207(6) 0.0219(7) 0.0278(6) -0.0002(5) 0.0067(5) 0.0049(5) C4 0.0236(6) 0.0225(6) 0.0225(6) 0.0021(5) 0.0070(5) 0.0042(5) C14 0.0344(7) 0.0251(7) 0.0275(7) -0.0026(6) 0.0042(5) 0.0050(6) C7 0.0241(6) 0.0337(8) 0.0180(6) -0.0014(5) -0.0005(5) 0.0005(6) C12 0.0233(6) 0.0313(8) 0.0298(7) 0.0058(6) -0.0020(5) 0.0010(6) C13 0.0277(7) 0.0278(7) 0.0371(7) 0.0040(6) 0.0035(6) 0.0086(6) C5 0.0369(7) 0.0317(8) 0.0259(7) 0.0085(6) 0.0068(6) 0.0015(6) C17 0.0321(7) 0.0392(8) 0.0271(7) 0.0013(6) 0.0104(5) -0.0109(6) C1 0.0362(8) 0.0341(8) 0.0373(8) -0.0099(7) 0.0015(6) -0.0119(7) C2S 0.0427(8) 0.0415(9) 0.0369(8) -0.0074(7) 0.0111(7) 0.0006(7) C1S 0.0420(8) 0.0381(9) 0.0403(8) 0.0014(7) 0.0145(7) 0.0062(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 C16 O4 C17 115.60(10) . . ? C2 O1 C1 115.22(11) . . ? C6 N1 C4 123.52(11) . . ? C6 N1 H1 117.6(11) . . ? C4 N1 H1 117.9(11) . . ? C1S O1S C2S 110.54(12) . . ? O5 N2 O6 123.83(12) . . ? O5 N2 C11 118.95(11) . . ? O6 N2 C11 117.19(11) . . ? C6 C8 C16 124.73(11) . . ? C6 C8 C9 120.45(11) . . ? C16 C8 C9 114.82(10) . . ? N1 C6 C7 113.70(11) . . ? C8 C6 N1 118.24(12) . . ? C8 C6 C7 128.05(12) . . ? C11 C10 C9 125.63(11) . . ? C15 C10 C11 115.07(12) . . ? C15 C10 C9 119.10(11) . . ? O4 C16 C8 115.70(10) . . ? O3 C16 O4 121.42(11) . . ? O3 C16 C8 122.88(11) . . ? C10 C11 N2 121.76(12) . . ? C12 C11 N2 114.76(11) . . ? C12 C11 C10 123.49(12) . . ? C8 C9 C10 111.68(10) . . ? C8 C9 H9 108.6 . . ? C8 C9 C3 109.51(10) . . ? C10 C9 H9 108.6 . . ? C3 C9 C10 109.68(9) . . ? C3 C9 H9 108.6 . . ? C2 C3 C9 119.64(11) . . ? C4 C3 C9 119.51(12) . . ? C4 C3 C2 120.82(12) . . ? C10 C15 H15 118.7 . . ? C14 C15 C10 122.59(12) . . ? C14 C15 H15 118.7 . . ? O1 C2 C3 111.41(11) . . ? O2 C2 O1 121.57(12) . . ? O2 C2 C3 127.02(12) . . ? N1 C4 C5 113.77(11) . . ? C3 C4 N1 119.07(12) . . ? C3 C4 C5 127.16(13) . . ? C15 C14 H14 119.9 . . ? C15 C14 C13 120.23(13) . . ? C13 C14 H14 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 . . ? C11 C12 H12 120.4 . . ? C13 C12 C11 119.30(12) . . ? C13 C12 H12 120.4 . . ? C14 C13 H13 120.3 . . ? C12 C13 C14 119.32(13) . . ? C12 C13 H13 120.3 . . ? 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 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 . . ? O1S C2S H2SA 109.4 . . ? O1S C2S H2SB 109.4 . . ? O1S C2S C1S 111.28(14) . 3_575 ? H2SA C2S H2SB 108.0 . . ? C1S C2S H2SA 109.4 3_575 . ? C1S C2S H2SB 109.4 3_575 . ? O1S C1S C2S 111.07(13) . 3_575 ? O1S C1S H1SA 109.4 . . ? O1S C1S H1SB 109.4 . . ? C2S C1S H1SA 109.4 3_575 . ? C2S C1S H1SB 109.4 3_575 . ? H1SA C1S H1SB 108.0 . . ? 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 O4 C16 1.3420(15) . ? O4 C17 1.4409(15) . ? O1 C2 1.3518(16) . ? O1 C1 1.4423(17) . ? O2 C2 1.2117(17) . ? O5 N2 1.2266(15) . ? O3 C16 1.2114(15) . ? O6 N2 1.2312(15) . ? N1 C6 1.3766(16) . ? N1 C4 1.3788(18) . ? N1 H1 0.887(17) . ? O1S C2S 1.424(2) . ? O1S C1S 1.4227(19) . ? N2 C11 1.4689(17) . ? C8 C6 1.3595(17) . ? C8 C16 1.4577(17) . ? C8 C9 1.5226(17) . ? C6 C7 1.5017(18) . ? C10 C11 1.3998(17) . ? C10 C9 1.5403(17) . ? C10 C15 1.3962(18) . ? C11 C12 1.3870(19) . ? C9 H9 1.0000 . ? C9 C3 1.5265(17) . ? C3 C2 1.4664(19) . ? C3 C4 1.3555(18) . ? C15 H15 0.9500 . ? C15 C14 1.3845(19) . ? C4 C5 1.5030(18) . ? C14 H14 0.9500 . ? C14 C13 1.386(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C12 H12 0.9500 . ? C12 C13 1.379(2) . ? C13 H13 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C2S C1S 1.500(2) 3_575 ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? 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 O5 N2 C11 C10 -49.97(18) . . . . ? O5 N2 C11 C12 130.03(13) . . . . ? O6 N2 C11 C10 131.83(13) . . . . ? O6 N2 C11 C12 -48.17(17) . . . . ? N2 C11 C12 C13 -179.18(13) . . . . ? C8 C9 C3 C2 -151.06(11) . . . . ? C8 C9 C3 C4 30.91(15) . . . . ? C6 N1 C4 C3 -15.20(19) . . . . ? C6 N1 C4 C5 164.13(12) . . . . ? C6 C8 C16 O4 -6.28(19) . . . . ? C6 C8 C16 O3 173.06(14) . . . . ? C6 C8 C9 C10 91.88(14) . . . . ? C6 C8 C9 C3 -29.81(16) . . . . ? C10 C11 C12 C13 0.8(2) . . . . ? C10 C9 C3 C2 86.05(13) . . . . ? C10 C9 C3 C4 -91.98(13) . . . . ? C10 C15 C14 C13 0.4(2) . . . . ? C16 C8 C6 N1 -171.79(12) . . . . ? C16 C8 C6 C7 7.4(2) . . . . ? C16 C8 C9 C10 -88.02(13) . . . . ? C16 C8 C9 C3 150.29(11) . . . . ? C11 C10 C9 C8 139.23(12) . . . . ? C11 C10 C9 C3 -99.18(14) . . . . ? C11 C10 C15 C14 -0.40(19) . . . . ? C11 C12 C13 C14 -0.8(2) . . . . ? C9 C8 C6 N1 8.32(18) . . . . ? C9 C8 C6 C7 -172.51(12) . . . . ? C9 C8 C16 O4 173.62(11) . . . . ? C9 C8 C16 O3 -7.04(19) . . . . ? C9 C10 C11 N2 -5.37(19) . . . . ? C9 C10 C11 C12 174.63(12) . . . . ? C9 C10 C15 C14 -175.58(12) . . . . ? C9 C3 C2 O1 1.38(16) . . . . ? C9 C3 C2 O2 -179.62(12) . . . . ? C9 C3 C4 N1 -10.77(18) . . . . ? C9 C3 C4 C5 170.00(12) . . . . ? C15 C10 C11 N2 179.80(12) . . . . ? C15 C10 C11 C12 -0.19(19) . . . . ? C15 C10 C9 C8 -46.14(15) . . . . ? C15 C10 C9 C3 75.45(14) . . . . ? C15 C14 C13 C12 0.3(2) . . . . ? C2 C3 C4 N1 171.23(11) . . . . ? C2 C3 C4 C5 -8.0(2) . . . . ? C4 N1 C6 C8 16.47(19) . . . . ? C4 N1 C6 C7 -162.81(12) . . . . ? C4 C3 C2 O1 179.38(11) . . . . ? C4 C3 C2 O2 -1.6(2) . . . . ? C17 O4 C16 O3 -0.18(19) . . . . ? C17 O4 C16 C8 179.17(12) . . . . ? C1 O1 C2 O2 -0.08(18) . . . . ? C1 O1 C2 C3 178.98(11) . . . . ? C2S O1S C1S C2S -55.97(19) . . . 3_575 ? C1S O1S C2S C1S 56.09(18) . . . 3_575 ?