#------------------------------------------------------------------------------ #$Date: 2019-11-04 18:11:02 +0200 (Mon, 04 Nov 2019) $ #$Revision: 223214 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/24/1552485.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1552485 loop_ _publ_author_name 'Wang, Guotong' 'Cui, Pengcheng' 'Bai, Hongjin' 'Wei, Sanyue' 'Li, Shengkun' _publ_section_title ; Late-Stage C-H Functionalization of Nicotinamides for the Expedient Discovery of Novel Antifungal Leads. ; _journal_issue 43 _journal_name_full 'Journal of agricultural and food chemistry' _journal_page_first 11901 _journal_page_last 11910 _journal_paper_doi 10.1021/acs.jafc.9b05349 _journal_volume 67 _journal_year 2019 _chemical_formula_moiety 'C20 H23 N3 O3' _chemical_formula_sum 'C20 H23 N3 O3' _chemical_formula_weight 353.41 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-05-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 93.136(6) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.0408(10) _cell_length_b 15.4293(13) _cell_length_c 16.5882(13) _cell_measurement_reflns_used 2579 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 28.6610 _cell_measurement_theta_min 3.0730 _cell_volume 3588.3(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -84.00 20.00 1.00 5.00 -- -11.59 -77.00-180.00 104 2 \w -45.00 -9.00 1.00 5.00 -- -11.59 107.00 47.00 36 3 \w 43.00 99.00 1.00 5.00 -- 11.74-178.00 60.00 56 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0079439500 _diffrn_orient_matrix_UB_12 -0.0050307500 _diffrn_orient_matrix_UB_13 -0.0417082500 _diffrn_orient_matrix_UB_21 0.0263578000 _diffrn_orient_matrix_UB_22 0.0392703000 _diffrn_orient_matrix_UB_23 0.0009441000 _diffrn_orient_matrix_UB_31 0.0423545500 _diffrn_orient_matrix_UB_32 -0.0234132500 _diffrn_orient_matrix_UB_33 0.0099425500 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7705 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.990 _diffrn_reflns_theta_max 24.990 _diffrn_reflns_theta_min 2.459 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.67053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.308 _exptl_crystal_description block _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.237 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 3164 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0458 _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^)+(0.0476P)^2^+2.3446P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1062 _refine_ls_wR_factor_ref 0.1168 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2515 _reflns_number_total 3164 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL b35-4_a.res in I2/a b35-4.res created by SHELXL-2018/3 at 14:48:41 on 28-May-2019 REM Old TITL B35-4 in I2/a REM SHELXT solution in I2/a: R1 0.173, Rweak 0.150, Alpha 0.026 REM 0.524 for 142 systematic absences, Orientation as input REM Formula found by SHELXT: C20 N4 O2 CELL 0.71073 14.0408 15.4293 16.5882 90 93.136 90 ZERR 8 0.001 0.0013 0.0013 0 0.006 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H N O UNIT 160 184 24 24 L.S. 10 PLAN 20 BOND $H list 4 fmap 2 53 acta OMIT -3 50 REM REM REM WGHT 0.047600 2.344600 EXTI 0.000724 FVAR 0.23926 O1 4 0.391071 0.396252 0.401199 11.00000 0.05106 0.02151 = 0.02668 0.00209 0.00314 0.00523 O2 4 0.364632 0.663735 0.378642 11.00000 0.04424 0.02042 = 0.02752 -0.00191 -0.00279 0.00293 O3 4 0.498121 0.421201 0.103209 11.00000 0.06311 0.04578 = 0.02588 0.00041 0.00748 0.02643 N2 3 0.377931 0.539325 0.306865 11.00000 0.02988 0.01662 = 0.02229 0.00063 -0.00015 0.00271 AFIX 43 H2 2 0.386867 0.484283 0.310391 11.00000 -1.20000 AFIX 0 N1 3 0.380835 0.407651 0.538735 11.00000 0.02543 0.03131 = 0.02614 0.00507 -0.00127 -0.00354 N3 3 0.465037 0.402114 0.233186 11.00000 0.04433 0.02541 = 0.02681 -0.00340 -0.00173 0.00879 C6 1 0.372750 0.584710 0.377277 11.00000 0.02067 0.02041 = 0.02703 -0.00060 -0.00125 0.00080 C12 1 0.410442 0.534183 0.163068 11.00000 0.02271 0.02319 = 0.02476 -0.00103 -0.00338 -0.00217 C7 1 0.369729 0.575946 0.228848 11.00000 0.02390 0.02027 = 0.02251 -0.00011 -0.00178 -0.00353 C2 1 0.375899 0.535956 0.455430 11.00000 0.01920 0.02460 = 0.02464 0.00008 -0.00068 -0.00081 C13 1 0.458779 0.449948 0.171221 11.00000 0.02549 0.02825 = 0.02362 -0.00511 -0.00295 0.00146 C8 1 0.318857 0.652286 0.213577 11.00000 0.03354 0.02381 = 0.02650 -0.00272 -0.00045 0.00309 AFIX 43 H8 2 0.290124 0.679864 0.255784 11.00000 -1.20000 AFIX 0 C1 1 0.382376 0.445986 0.467406 11.00000 0.02316 0.02903 = 0.02353 0.00004 -0.00109 -0.00036 C5 1 0.374698 0.457663 0.605017 11.00000 0.01968 0.04266 = 0.02448 0.00371 -0.00268 -0.00715 C4 1 0.370061 0.546262 0.599855 11.00000 0.02840 0.04138 = 0.02335 -0.00442 -0.00128 -0.00242 AFIX 43 H4 2 0.367073 0.579734 0.646273 11.00000 -1.20000 AFIX 0 C11 1 0.400571 0.571856 0.086560 11.00000 0.02871 0.03263 = 0.02350 -0.00270 -0.00024 -0.00017 AFIX 43 H11 2 0.427338 0.544439 0.043290 11.00000 -1.20000 AFIX 0 C3 1 0.369881 0.585151 0.524961 11.00000 0.02713 0.02799 = 0.02871 -0.00279 -0.00452 0.00106 AFIX 43 H3 2 0.365667 0.645170 0.521034 11.00000 -1.20000 AFIX 0 C10 1 0.352240 0.648500 0.073651 11.00000 0.03391 0.03495 = 0.02472 0.00622 -0.00239 -0.00148 AFIX 43 H10 2 0.348002 0.673491 0.022562 11.00000 -1.20000 AFIX 0 C18 1 0.332205 0.248392 0.395187 11.00000 0.03069 0.03307 = 0.02851 -0.00092 0.00426 0.00389 AFIX 23 H18A 2 0.305666 0.258692 0.340813 11.00000 -1.20000 H18B 2 0.283635 0.262471 0.432471 11.00000 -1.20000 AFIX 0 C9 1 0.310169 0.687895 0.137124 11.00000 0.03613 0.02387 = 0.02921 0.00331 -0.00400 0.00383 AFIX 43 H9 2 0.275671 0.738817 0.128476 11.00000 -1.20000 AFIX 0 C17 1 0.416605 0.305902 0.411398 11.00000 0.03810 0.02338 = 0.03215 0.00402 0.00337 0.00283 AFIX 23 H17A 2 0.442456 0.296451 0.466118 11.00000 -1.20000 H17B 2 0.465651 0.291201 0.374757 11.00000 -1.20000 AFIX 0 C19 1 0.358951 0.153105 0.404329 11.00000 0.03772 0.02992 = 0.03220 0.00017 -0.00068 -0.00361 AFIX 23 H19A 2 0.407983 0.139622 0.367296 11.00000 -1.20000 H19B 2 0.385644 0.143311 0.458739 11.00000 -1.20000 AFIX 0 C16 1 0.373295 0.410890 0.683876 11.00000 0.03989 0.05012 = 0.02970 0.00593 -0.00094 -0.01075 AFIX 137 H16A 2 0.316384 0.376517 0.684923 11.00000 -1.50000 H16B 2 0.374433 0.452230 0.727169 11.00000 -1.50000 H16C 2 0.428166 0.373888 0.690171 11.00000 -1.50000 AFIX 0 C14 1 0.515828 0.323291 0.210649 11.00000 0.06210 0.03279 = 0.03343 -0.00604 -0.00151 0.01624 AFIX 23 H14A 2 0.475973 0.272505 0.216103 11.00000 -1.20000 H14B 2 0.573912 0.315950 0.244368 11.00000 -1.20000 AFIX 0 C20 1 0.275978 0.092495 0.388261 11.00000 0.05065 0.04395 = 0.04268 -0.00432 0.00251 -0.01336 AFIX 137 H20A 2 0.249308 0.101507 0.334387 11.00000 -1.50000 H20B 2 0.228228 0.103700 0.426199 11.00000 -1.50000 H20C 2 0.297516 0.033650 0.393957 11.00000 -1.50000 AFIX 0 C15 1 0.538304 0.337019 0.123684 11.00000 0.07031 0.04779 = 0.03456 -0.00460 -0.00271 0.03349 AFIX 23 H15A 2 0.606652 0.336677 0.117770 11.00000 -1.20000 H15B 2 0.509242 0.292212 0.089489 11.00000 -1.20000 AFIX 0 HKLF 4 REM b35-4_a.res in I2/a REM wR2 = 0.1168, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0458 for 2515 Fo > 4sig(Fo) and 0.0625 for all 3164 data REM 238 parameters refined using 0 restraints END WGHT 0.0460 2.3300 REM Highest difference peak 0.237, deepest hole -0.185, 1-sigma level 0.041 Q1 1 0.4693 0.3030 0.1124 11.00000 0.05 0.24 Q2 1 0.4203 0.4017 0.2616 11.00000 0.05 0.20 Q3 1 0.3989 0.5563 0.4211 11.00000 0.05 0.20 Q4 1 0.5611 0.3019 0.0784 11.00000 0.05 0.19 Q5 1 0.4107 0.5650 0.1977 11.00000 0.05 0.19 Q6 1 0.3990 0.3402 0.5432 11.00000 0.05 0.18 Q7 1 0.3933 0.5000 0.4604 11.00000 0.05 0.18 Q8 1 0.3418 0.5460 0.4846 11.00000 0.05 0.17 Q9 1 0.4349 0.4190 0.7178 11.00000 0.05 0.16 Q10 1 0.3158 0.4239 0.7198 11.00000 0.05 0.16 Q11 1 0.4453 0.4989 0.1719 11.00000 0.05 0.16 Q12 1 0.5125 0.2796 0.2443 11.00000 0.05 0.16 Q13 1 0.3986 0.5570 0.4795 11.00000 0.05 0.15 Q14 1 0.3940 0.3880 0.2425 11.00000 0.05 0.15 Q15 1 0.3636 0.3401 0.6760 11.00000 0.05 0.15 Q16 1 0.3376 0.6975 0.4386 11.00000 0.05 0.15 Q17 1 0.4393 0.3999 0.1156 11.00000 0.05 0.15 Q18 1 0.4214 0.4896 0.1646 11.00000 0.05 0.14 Q19 1 0.3981 0.4193 0.5235 11.00000 0.05 0.14 Q20 1 0.4206 0.4979 0.3077 11.00000 0.05 0.14 REM The information below was added by Olex2. REM REM R1 = 0.0458 for 2515 Fo > 4sig(Fo) and 0.0625 for all 9499 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.24, deepest hole -0.18 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0625 REM R1_gt = 0.0458 REM wR_ref = 0.1168 REM GOOF = 1.040 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 9499 REM Reflections_gt = 2515 REM Parameters = n/a REM Hole = -0.18 REM Peak = 0.24 REM Flack = n/a ; _cod_data_source_file jf9b05349_si_004.cif _cod_data_source_block b35-4 _cod_depositor_comments 'Adding full bibliography for 1552483--1552486.cif.' _cod_database_code 1552485 _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. ; _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C18(H18A,H18B), C17(H17A,H17B), C19(H19A,H19B), C14(H14A,H14B), C15(H15A,H15B) 2.b Aromatic/amide H refined with riding coordinates: N2(H2), C8(H8), C4(H4), C11(H11), C3(H3), C10(H10), C9(H9) 2.c Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C20(H20A,H20B,H20C) ; _olex2_date_sample_data_collection 2019-05-27 _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 1.458 _oxdiff_exptl_absorpt_empirical_full_min 0.724 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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 O1 O 0.39107(9) 0.39625(8) 0.40120(7) 0.0330(3) Uani 1 1 d . O2 O 0.36463(9) 0.66374(8) 0.37864(7) 0.0309(3) Uani 1 1 d . O3 O 0.49812(10) 0.42120(9) 0.10321(8) 0.0447(4) Uani 1 1 d . N2 N 0.37793(10) 0.53933(9) 0.30687(8) 0.0230(4) Uani 1 1 d . H2 H 0.386867 0.484283 0.310391 0.028 Uiso 1 1 calc R N1 N 0.38084(10) 0.40765(10) 0.53874(9) 0.0277(4) Uani 1 1 d . N3 N 0.46504(11) 0.40211(10) 0.23319(9) 0.0323(4) Uani 1 1 d . C6 C 0.37275(11) 0.58471(11) 0.37728(10) 0.0228(4) Uani 1 1 d . C12 C 0.41044(11) 0.53418(12) 0.16307(10) 0.0237(4) Uani 1 1 d . C7 C 0.36973(11) 0.57595(11) 0.22885(10) 0.0223(4) Uani 1 1 d . C2 C 0.37590(11) 0.53596(12) 0.45543(10) 0.0229(4) Uani 1 1 d . C13 C 0.45878(12) 0.44995(12) 0.17122(11) 0.0259(4) Uani 1 1 d . C8 C 0.31886(12) 0.65229(12) 0.21358(11) 0.0280(4) Uani 1 1 d . H8 H 0.290124 0.679864 0.255784 0.034 Uiso 1 1 calc R C1 C 0.38238(11) 0.44599(12) 0.46741(10) 0.0253(4) Uani 1 1 d . C5 C 0.37470(12) 0.45766(14) 0.60502(11) 0.0291(5) Uani 1 1 d . C4 C 0.37006(12) 0.54626(14) 0.59986(11) 0.0311(5) Uani 1 1 d . H4 H 0.367073 0.579734 0.646273 0.037 Uiso 1 1 calc R C11 C 0.40057(12) 0.57186(13) 0.08656(11) 0.0283(4) Uani 1 1 d . H11 H 0.427338 0.544439 0.043290 0.034 Uiso 1 1 calc R C3 C 0.36988(12) 0.58515(13) 0.52496(11) 0.0282(4) Uani 1 1 d . H3 H 0.365667 0.645170 0.521034 0.034 Uiso 1 1 calc R C10 C 0.35224(13) 0.64850(13) 0.07365(11) 0.0313(5) Uani 1 1 d . H10 H 0.348002 0.673491 0.022562 0.038 Uiso 1 1 calc R C18 C 0.33220(12) 0.24839(13) 0.39519(11) 0.0307(5) Uani 1 1 d . H18A H 0.305666 0.258692 0.340813 0.037 Uiso 1 1 calc R H18B H 0.283635 0.262471 0.432471 0.037 Uiso 1 1 calc R C9 C 0.31017(13) 0.68790(13) 0.13712(11) 0.0300(4) Uani 1 1 d . H9 H 0.275671 0.738817 0.128476 0.036 Uiso 1 1 calc R C17 C 0.41660(13) 0.30590(12) 0.41140(12) 0.0312(5) Uani 1 1 d . H17A H 0.442456 0.296451 0.466118 0.037 Uiso 1 1 calc R H17B H 0.465651 0.291201 0.374757 0.037 Uiso 1 1 calc R C19 C 0.35895(14) 0.15310(13) 0.40433(12) 0.0334(5) Uani 1 1 d . H19A H 0.407983 0.139622 0.367296 0.040 Uiso 1 1 calc R H19B H 0.385644 0.143311 0.458739 0.040 Uiso 1 1 calc R C16 C 0.37329(15) 0.41089(15) 0.68388(12) 0.0400(5) Uani 1 1 d . H16A H 0.316384 0.376517 0.684923 0.060 Uiso 1 1 calc GR H16B H 0.374433 0.452230 0.727169 0.060 Uiso 1 1 calc GR H16C H 0.428166 0.373888 0.690171 0.060 Uiso 1 1 calc GR C14 C 0.51583(16) 0.32329(14) 0.21065(12) 0.0429(6) Uani 1 1 d . H14A H 0.475973 0.272505 0.216103 0.052 Uiso 1 1 calc R H14B H 0.573912 0.315950 0.244368 0.052 Uiso 1 1 calc R C20 C 0.27598(15) 0.09250(15) 0.38826(13) 0.0458(6) Uani 1 1 d . H20A H 0.249308 0.101507 0.334387 0.069 Uiso 1 1 calc GR H20B H 0.228228 0.103700 0.426199 0.069 Uiso 1 1 calc GR H20C H 0.297516 0.033650 0.393957 0.069 Uiso 1 1 calc GR C15 C 0.53830(18) 0.33702(15) 0.12368(13) 0.0511(6) Uani 1 1 d . H15A H 0.606652 0.336677 0.117770 0.061 Uiso 1 1 calc R H15B H 0.509242 0.292212 0.089489 0.061 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0511(8) 0.0215(7) 0.0267(7) 0.0021(6) 0.0031(6) 0.0052(6) O2 0.0442(8) 0.0204(7) 0.0275(7) -0.0019(6) -0.0028(6) 0.0029(6) O3 0.0631(10) 0.0458(9) 0.0259(8) 0.0004(7) 0.0075(6) 0.0264(8) N2 0.0299(8) 0.0166(8) 0.0223(8) 0.0006(6) -0.0001(6) 0.0027(7) N1 0.0254(8) 0.0313(9) 0.0261(9) 0.0051(7) -0.0013(6) -0.0035(7) N3 0.0443(9) 0.0254(9) 0.0268(9) -0.0034(7) -0.0017(7) 0.0088(8) C6 0.0207(9) 0.0204(10) 0.0270(10) -0.0006(8) -0.0013(7) 0.0008(8) C12 0.0227(9) 0.0232(10) 0.0248(10) -0.0010(8) -0.0034(7) -0.0022(8) C7 0.0239(9) 0.0203(9) 0.0225(10) -0.0001(8) -0.0018(7) -0.0035(8) C2 0.0192(8) 0.0246(10) 0.0246(10) 0.0001(8) -0.0007(7) -0.0008(8) C13 0.0255(9) 0.0283(11) 0.0236(10) -0.0051(9) -0.0030(7) 0.0015(8) C8 0.0335(10) 0.0238(10) 0.0265(10) -0.0027(8) -0.0005(8) 0.0031(8) C1 0.0232(9) 0.0290(11) 0.0235(10) 0.0000(9) -0.0011(7) -0.0004(8) C5 0.0197(9) 0.0427(13) 0.0245(10) 0.0037(9) -0.0027(7) -0.0071(9) C4 0.0284(10) 0.0414(13) 0.0234(10) -0.0044(9) -0.0013(7) -0.0024(9) C11 0.0287(9) 0.0326(11) 0.0235(10) -0.0027(9) -0.0002(7) -0.0002(9) C3 0.0271(9) 0.0280(11) 0.0287(11) -0.0028(9) -0.0045(7) 0.0011(8) C10 0.0339(10) 0.0350(12) 0.0247(10) 0.0062(9) -0.0024(8) -0.0015(9) C18 0.0307(10) 0.0331(12) 0.0285(11) -0.0009(9) 0.0043(8) 0.0039(9) C9 0.0361(10) 0.0239(10) 0.0292(11) 0.0033(8) -0.0040(8) 0.0038(8) C17 0.0381(11) 0.0234(10) 0.0321(11) 0.0040(9) 0.0034(8) 0.0028(9) C19 0.0377(10) 0.0299(11) 0.0322(11) 0.0002(9) -0.0007(8) -0.0036(9) C16 0.0399(11) 0.0501(14) 0.0297(11) 0.0059(10) -0.0009(8) -0.0107(10) C14 0.0621(14) 0.0328(12) 0.0334(12) -0.0060(10) -0.0015(10) 0.0162(11) C20 0.0507(13) 0.0439(14) 0.0427(13) -0.0043(11) 0.0025(10) -0.0134(11) C15 0.0703(15) 0.0478(15) 0.0346(12) -0.0046(11) -0.0027(10) 0.0335(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1 O1 C17 119.02(14) C13 O3 C15 105.60(15) C6 N2 H2 117.5 C6 N2 C7 124.96(15) C7 N2 H2 117.5 C1 N1 C5 118.52(17) C13 N3 C14 106.83(15) O2 C6 N2 122.34(16) O2 C6 C2 118.84(16) N2 C6 C2 118.81(15) C7 C12 C13 122.42(16) C11 C12 C7 119.17(16) C11 C12 C13 118.33(16) N2 C7 C12 120.59(16) C8 C7 N2 121.36(15) C8 C7 C12 118.01(16) C1 C2 C6 128.14(16) C3 C2 C6 116.41(16) C3 C2 C1 115.44(16) O3 C13 C12 114.80(16) N3 C13 O3 118.13(17) N3 C13 C12 127.04(16) C7 C8 H8 119.3 C9 C8 C7 121.45(17) C9 C8 H8 119.3 O1 C1 C2 117.03(15) N1 C1 O1 118.65(17) N1 C1 C2 124.32(17) N1 C5 C4 121.60(17) N1 C5 C16 116.18(18) C4 C5 C16 122.21(18) C5 C4 H4 120.4 C5 C4 C3 119.19(18) C3 C4 H4 120.4 C12 C11 H11 119.2 C10 C11 C12 121.57(17) C10 C11 H11 119.2 C2 C3 H3 119.5 C4 C3 C2 120.90(19) C4 C3 H3 119.5 C11 C10 H10 120.3 C11 C10 C9 119.32(17) C9 C10 H10 120.3 H18A C18 H18B 108.0 C17 C18 H18A 109.3 C17 C18 H18B 109.3 C17 C18 C19 111.52(15) C19 C18 H18A 109.3 C19 C18 H18B 109.3 C8 C9 H9 119.8 C10 C9 C8 120.43(18) C10 C9 H9 119.8 O1 C17 C18 111.25(15) O1 C17 H17A 109.4 O1 C17 H17B 109.4 C18 C17 H17A 109.4 C18 C17 H17B 109.4 H17A C17 H17B 108.0 C18 C19 H19A 108.9 C18 C19 H19B 108.9 H19A C19 H19B 107.7 C20 C19 C18 113.43(17) C20 C19 H19A 108.9 C20 C19 H19B 108.9 C5 C16 H16A 109.5 C5 C16 H16B 109.5 C5 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 N3 C14 H14A 110.8 N3 C14 H14B 110.8 N3 C14 C15 104.90(16) H14A C14 H14B 108.8 C15 C14 H14A 110.8 C15 C14 H14B 110.8 C19 C20 H20A 109.5 C19 C20 H20B 109.5 C19 C20 H20C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 O3 C15 C14 104.53(16) O3 C15 H15A 110.8 O3 C15 H15B 110.8 C14 C15 H15A 110.8 C14 C15 H15B 110.8 H15A C15 H15B 108.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.351(2) O1 C17 1.447(2) O2 C6 1.225(2) O3 C13 1.358(2) O3 C15 1.449(2) N2 H2 0.8600 N2 C6 1.367(2) N2 C7 1.411(2) N1 C1 1.324(2) N1 C5 1.350(2) N3 C13 1.265(2) N3 C14 1.469(2) C6 C2 1.497(2) C12 C7 1.415(2) C12 C13 1.469(3) C12 C11 1.396(2) C7 C8 1.394(3) C2 C1 1.405(3) C2 C3 1.387(2) C8 H8 0.9300 C8 C9 1.381(3) C5 C4 1.371(3) C5 C16 1.495(3) C4 H4 0.9300 C4 C3 1.380(3) C11 H11 0.9300 C11 C10 1.374(3) C3 H3 0.9300 C10 H10 0.9300 C10 C9 1.377(3) C18 H18A 0.9700 C18 H18B 0.9700 C18 C17 1.493(3) C18 C19 1.523(3) C9 H9 0.9300 C17 H17A 0.9700 C17 H17B 0.9700 C19 H19A 0.9700 C19 H19B 0.9700 C19 C20 1.506(3) C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C14 H14A 0.9700 C14 H14B 0.9700 C14 C15 1.508(3) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C15 H15A 0.9700 C15 H15B 0.9700 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 2 80.95 2.44 0 0 4 4431.09 53.12 0 0 6 1869.65 27.52 0 0 -6 1853.77 27.64 0 0 -8 226.34 8.23 0 0 8 222.12 8.03 0 0 10 879.02 19.54 0 0 -10 870.29 19.62 0 0 -12 136.15 7.78 0 0 12 117.96 7.24 0 0 -14 511.82 17.25 0 0 -16 162.35 10.16 0 0 -18 11.21 2.83 0 0 -20 6.63 2.48 0 -1 3 1104.86 15.97 0 1 3 1125.55 15.96 0 -1 5 54.93 3.05 0 1 -5 55.93 3.15 0 1 5 56.23 3.11 0 1 -7 72.48 4.2 0 -1 -7 65.23 3.99 0 -1 7 65.57 3.93 0 1 7 69.44 4.07 0 -1 9 29.34 3.05 0 1 9 32.74 3.2 0 -1 -11 1.83 1.08 0 -1 11 4.35 1.28 0 1 -11 2.72 1.06 0 1 11 1.68 0.79 0 -1 -13 724.45 20.07 0 1 -13 718.25 19.92 0 1 -15 0.53 0.83 0 -1 -15 -0.16 1.05 0 1 -17 23.85 4.11 0 -1 -17 30.49 4.68 0 -1 -19 6.29 2.44 0 1 -19 8.22 2.79 0 1 -21 30.62 5.75 0 -1 -21 31.17 5.6 0 -2 0 2621.9 30.41 0 2 0 2677.53 30.28 0 -2 2 24.48 1.42 0 2 2 23.58 1.68 0 -2 4 87.68 3.62 0 2 4 84.79 3.65 0 2 -4 89.15 3.72 0 2 -6 82.13 4.28 0 2 6 81.28 4.18 0 -2 6 80.13 4.19 0 2 8 192.33 7.65 0 -2 8 214.51 7.88 0 -2 10 2.57 1.15 0 2 10 2.07 0.94 0 2 -10 1.4 0.91 0 -2 -10 1.24 0.86 0 -2 12 7.33 1.75 0 2 -12 8.58 1.95 0 -2 -12 10.84 2.34 0 -2 -14 268.45 12.23 0 2 -14 281.99 12.5 0 2 -16 28.17 4.3 0 -2 -16 34.93 4.9 0 -2 -18 6.8 2.48 0 2 -18 4.42 2.19 0 -2 -20 2.56 2.12 0 2 -20 2.5 1.74 0 3 -1 644.84 9.66 0 -3 1 665.5 9.75 0 3 3 54.41 3.15 0 -3 3 54.55 2.63 0 3 -3 55.99 2.84 0 3 5 50.75 3.19 0 3 -5 47.64 3.11 0 -3 5 45.68 2.91 0 3 7 420.08 11.16 0 3 -7 391.3 10.98 0 -3 7 400.12 10.89 0 3 9 138 6.83 0 -3 9 147.98 7.01 0 3 11 61.81 4.96 0 3 -11 56.01 4.77 0 -3 11 58.25 4.8 0 3 11 45.56 1.65 0 -3 -11 61.86 5.22 0 -3 -13 22.22 3.37 0 3 -13 14.67 2.56 0 -3 -15 20 3.6 0 3 -15 30.47 4.34 0 -3 -17 23.61 4.26 0 3 -17 21.99 4.06 0 3 -19 -0.42 1.16 0 -3 -19 3.83 2.39 0 3 -21 8.49 3.15 0 -4 0 2685.92 32.91 0 -4 2 2.06 0.55 0 4 -2 0.5 0.27 0 4 -4 14.2 1.69 0 4 4 11.53 1.71 0 4 -4 12.1 1.32 0 4 -6 432.25 11.23 0 -4 6 433.71 10.8 0 4 8 179.33 7.51 0 -4 8 159.54 6.95 0 -4 10 55.43 4.46 0 4 10 52.69 4.47 0 4 -10 54.65 4.73 0 -4 -10 60.94 5.23 0 -4 -12 28.39 3.94 0 4 -12 24.89 3.56 0 4 12 25.55 1.55 0 4 -14 -1.21 1.59 0 -4 -14 0.77 0.98 0 4 -16 -0.72 1.39 0 -4 -16 0.51 1.57 0 -4 -18 3.01 2.28 0 4 -18 3.42 1.96 0 4 -20 44.11 6.31 0 -4 -20 37.83 6.64 0 5 -1 74.86 3.05 0 -5 1 80.72 3.27 0 -5 -1 78.79 3.28 0 5 -3 0.47 0.42 0 5 -3 0.73 0.44 0 5 5 229.44 8.33 0 5 -5 220.93 6.41 0 5 -5 222.11 7.54 0 5 7 296.19 9.87 0 -5 7 291.7 9.16 0 -5 9 116 6.24 0 5 -9 114.97 6.56 0 5 9 113.19 6.47 0 -5 -9 100.75 7 0 -5 11 8.09 1.83 0 5 -11 9.2 1.98 0 -5 -11 6.09 1.93 0 -5 -13 53.03 6.15 0 5 -13 53.93 5.43 0 5 13 53.44 2.61 0 5 -15 15.12 3.18 0 -5 -15 14.53 3.43 0 -5 -17 19.46 4.13 0 5 -17 27.98 4.59 0 5 -19 1.85 1.68 0 -5 -19 3.79 2.65 0 -6 0 908.8 15.17 0 -6 2 105.27 4.11 0 6 -2 102.26 3.92 0 6 -4 17.76 1.7 0 6 -4 18.1 2.06 0 6 4 20.66 2.65 0 6 6 104.66 5.95 0 6 -6 102.29 4.59 0 6 8 12.7 2.16 0 6 -8 11.09 2.11 0 -6 8 14.32 2.08 0 -6 10 18.58 2.67 0 6 10 16.36 2.68 0 6 -10 17.61 2.7 0 -6 -10 22.79 3.57 0 6 -12 28.96 3.82 0 -6 -12 33.31 4.69 0 6 -14 279.45 13.09 0 6 14 292.6 7.29 0 -6 -14 273.59 14.72 0 -6 -16 54.55 7.02 0 6 -16 42.5 5.5 0 -6 -18 1.22 2.38 0 6 -18 3.06 1.95 0 6 -20 2.42 2.22 0 -7 -1 299.76 8.22 0 7 -1 310.92 7.65 0 7 -3 107.55 4.38 0 -7 3 107.58 4.53 0 7 -5 22.27 2.1 0 7 5 24.08 3.03 0 7 -7 8.94 1.52 0 7 7 10.77 2.05 0 7 -7 9.77 1.88 0 7 -9 36.28 3.2 0 7 -9 31.57 3.66 0 7 9 39.45 4.09 0 7 -11 1.03 1.09 0 7 -13 29.97 4.13 0 -7 -15 8.65 2.84 0 7 -15 4.92 1.85 0 7 -17 39.96 5.63 0 -7 -17 40.08 6.32 0 -7 -19 8.35 3.6 0 7 -19 3.24 1.97 0 -8 0 1764.57 26.86 0 -8 2 0.12 0.54 0 -8 -2 -0.22 0.7 0 8 -2 0.17 0.42 0 8 -4 44.26 3.02 0 8 -6 1.96 1.03 0 8 -6 -0.13 0.6 0 8 6 0.62 0.93 0 8 -8 9.36 1.97 0 8 -8 10.34 1.78 0 8 8 9.67 2.06 0 8 -10 8.44 2.22 0 8 -10 5.76 1.52 0 8 -12 9.51 2.34 0 8 -12 12.02 2.17 0 8 -14 4.05 1.76 0 8 -16 14.05 4.04 0 8 -18 8.72 2.77 0 -9 1 33.3 2.87 0 -9 -1 34.43 2.93 0 -9 -3 63.23 4.21 0 9 -3 66.73 3.93 0 -9 3 67.82 4.09 0 9 -5 1.31 0.83 0 9 -5 -0.95 0.56 0 9 5 0.3 1.07 0 9 7 23.49 3.46 0 9 -7 22.22 2.5 0 9 -7 26 3.31 0 9 -9 4.39 1.26 0 9 -9 1.7 1.25 0 9 -11 28.9 3.18 0 9 -11 24.38 3.67 0 9 -13 29.4 4.28 0 9 -15 -2.42 1.67 0 9 -17 25.65 5.05 0 9 -19 1.14 1.32 0 -10 0 130.21 6.13 0 -10 2 0.1 0.55 0 -10 -2 0.6 0.7 0 -10 -4 44.94 3.79 0 -10 4 43.83 3.52 0 10 -4 49.45 3.57 0 10 -6 8 1.65 0 10 -6 6.44 1.84 0 10 -8 48.14 3.87 0 10 -8 39.97 4.35 0 10 -10 23.73 2.89 0 10 -10 15.37 2.75 0 10 -12 0.22 1.05 0 10 -14 2.68 1.68 0 10 -16 -0.93 1.57 0 10 -18 22.96 4.7 0 -11 -1 5.68 1.52 0 -11 1 4.32 1.39 0 11 -3 5.09 1.29 0 -11 -3 5.46 1.56 0 -11 3 9.16 1.78 0 11 -5 0.05 0.89 0 -11 -5 0.95 1.02 0 11 -5 1.12 0.71 0 11 -7 26.42 2.98 0 11 -7 24.89 3.57 0 11 -9 97.94 7.31 0 11 -9 111.45 6.24 0 11 -11 21.31 2.87 0 11 -11 28.16 4.16 0 11 -13 5.64 2.28 0 11 -15 0.12 1.31 0 11 -17 -0.05 1.57 0 -12 0 294.95 10.51 0 -12 -2 0.39 0.79 0 -12 2 0.72 1.04 0 12 -4 19.97 2.48 0 -12 4 24.97 3 0 -12 -4 25.75 3.25 0 12 -6 95.14 5.71 0 -12 -6 108.42 6.78 0 12 -6 103.59 7.2 0 12 -8 168.64 9.8 0 12 -8 166.4 7.79 0 12 -10 27.05 4.22 0 12 -10 27.05 3.32 0 12 -12 62.26 6.59 0 12 -14 -0.2 1.1 0 12 -16 1.44 1.8 0 -13 1 111.68 6.47 0 -13 -1 112.39 6.63 0 -13 -3 -0.49 0.96 0 -13 3 -0.11 0.83 0 -13 -5 96.17 6.54 0 13 -5 98.47 7.02 0 13 -5 84.95 5.43 0 -13 -7 360.23 13.41 0 13 -7 355.99 11.93 0 13 -7 357.76 14.39 0 13 -9 99.68 8.02 0 13 -11 82.7 7.61 0 13 -13 -0.96 1.24 0 13 -15 28.62 5.08 0 -14 0 139.81 7.71 0 -14 -2 12.55 2.39 0 -14 2 9.64 2.27 0 -14 -4 28.29 3.71 0 -14 4 29.74 3.5 0 -14 -6 18.63 3.18 0 14 -6 18.82 3.32 0 14 -8 2.53 1.72 0 -14 -8 -0.51 1 0 14 -10 1.71 1.99 0 14 -12 8.72 2.95 0 14 -14 35.22 5.74 0 14 -16 3.33 2.46 0 -15 -1 42.62 4.45 0 -15 1 39.2 4.14 0 -15 -3 -0.92 0.9 0 -15 3 1.32 1.34 0 15 -5 15.35 2.88 0 -15 -5 15.19 2.83 0 15 -7 -1.56 1.64 0 -15 -7 0 1.09 0 -15 -9 5.51 2.22 0 15 -9 2.71 1.66 0 15 -11 1.33 1.33 0 -15 -11 1.08 1.8 0 15 -13 41.21 6.03 0 -16 0 192.34 9.73 0 -16 -2 2.38 1.4 0 -16 2 1.7 1.49 0 -16 4 1.09 0.99 0 -16 -4 -0.55 0.93 0 16 -6 1.52 1.32 0 -16 -6 0.12 1.09 0 -16 -8 2.62 1.69 0 16 -8 0.71 1.06 0 16 -10 3.62 2.03 0 -16 -10 4.24 2.42 0 16 -12 9.74 2.97 0 -16 -12 21.85 4.07 0 -17 -1 0.91 1.47 0 -17 1 1.83 1.82 0 -17 -3 -1.41 1.06 0 -17 3 0.18 1.04 0 -17 -5 18.41 3.52 0 17 -5 21.59 3.83 0 -17 -7 5.68 2.42 0 17 -7 5.21 2.21 0 -17 -9 4.33 1.93 0 17 -9 11.87 3.37 0 17 -11 2.09 2.29 0 -17 -11 0.87 1.31 0 -18 0 51.86 5.46 0 -18 -2 0.13 1.62 0 -18 2 1.5 1.56 0 18 -4 1.91 1.63 0 -18 -4 -1.4 2.02 0 18 -6 4.02 2.28 0 -18 -6 -1.02 1.49 0 -18 -8 0.76 1.52 0 18 -8 -1.26 1.35 0 18 -10 -2.47 1.93 0 -19 1 4.54 2.29 0 -19 -1 7.57 2.44 0 -19 -3 1.63 1.68 0 -19 3 1.25 1.88 0 19 -5 17.73 3.71 0 -19 -5 14.41 3.32 0 19 -7 0.77 1.83 0 -19 -7 2.55 2.16 0 -20 0 70.77 6.84 0 -20 -2 5.4 2.43 0 -20 -4 8.8 2.83 0 -20 -6 12.59 3.26 0 -21 -3 6.03 2.71 1 0 -21 -0.31 1.78 1 0 -19 -0.6 1.51 1 0 -17 0.46 1.37 1 0 -15 0.68 1.28 1 0 -13 3.32 1.95 1 0 -11 0.63 0.87 -1 0 11 1.16 0.78 -1 0 9 0.12 0.61 1 0 -7 0.32 0.45 -1 0 7 -0.05 0.59 -1 0 5 0.06 0.31 1 0 -5 -0.04 0.26 1 0 -3 0.08 0.19 1 0 -3 0.02 0.16 1 0 1 0.06 0.09 1 0 3 -0.18 0.22 1 0 5 0.5 0.51 1 0 7 0.02 0.59 1 0 9 0.52 0.88 -1 0 -11 -0.2 0.58 1 0 11 0.29 0.47 -1 0 -13 2.17 1.4 -1 0 -15 1.76 1.29 -1 0 -17 -0.3 1.29 -1 0 -19 0.23 1.45 1 1 -20 60.86 7.33 1 -1 -20 62.13 7.52 1 1 -18 36.51 5.27 1 -1 -18 38.36 5.39 1 -1 -16 101.03 7.96 1 1 -16 104.13 8.04 1 1 -14 461.7 16.1 1 -1 -14 512.91 16.94 1 1 -12 44.66 4.32 -1 -1 12 47.97 4.54 -1 1 12 48.18 4.52 1 -1 -12 55.46 4.87 -1 -1 10 356.91 11.53 -1 1 10 346.75 11.38 1 -1 -10 355.26 11.61 -1 -1 8 40.55 3.28 1 1 -8 35.3 3.14 -1 1 8 37.77 3.18 1 -1 -8 38.92 3.31 1 1 -6 31.34 2.52 1 -1 -6 30.26 2.5 -1 1 6 36.67 2.75 -1 -1 6 34.05 2.55 -1 1 6 30.14 1.35 1 -1 -4 1222.61 17.74 -1 1 4 1167.14 17.49 -1 -1 4 1166.58 17.24 1 1 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28.99 3.28 -4 2 8 22.27 2.47 -4 2 6 38.76 2.81 -4 2 6 41.93 2.91 4 2 -6 36.51 2.43 -4 -2 6 38.23 2.46 4 -2 -4 10.76 1.38 -4 2 4 11.46 1.49 4 2 -4 11.47 0.99 4 2 -4 9.87 0.76 4 -2 -4 10.53 1.3 -4 2 4 11.29 1.49 -4 -2 4 11.09 0.96 -4 2 2 330.11 8.43 -4 2 2 346.06 7.65 4 -2 -2 340.21 8.34 -4 -2 2 323.95 5.09 4 -2 -2 339.74 7.63 -4 2 0 2005.02 27.79 4 2 0 1912.15 22.71 -4 2 0 1961.69 26.2 -4 -2 0 1865.39 23.21 4 -2 0 1989.09 26.44 -4 2 -2 258.27 7.29 4 -2 2 254.3 7.1 -4 -2 -2 252.26 6.08 -4 2 -2 258.49 6.86 4 2 2 263.96 6.15 4 2 4 333.16 8.5 -4 -2 -4 314.14 8.33 4 -2 4 315.19 8.52 -4 2 -4 318.16 8.86 -4 2 -4 306.55 8.24 4 2 6 28.71 2.69 -4 2 -6 26.02 2.26 -4 2 -6 30.54 2.97 -4 -2 -6 25.93 2.63 4 -2 6 25.82 2.64 4 2 8 150.9 7.1 -4 2 -8 157.43 7.55 -4 2 -8 151.32 5.61 4 -2 8 139.69 7 -4 -2 -8 162.26 7.46 -4 -2 -10 4.55 1.6 4 -2 10 4.08 1.42 4 2 10 3.82 0.81 -4 2 -10 3.34 1.17 4 2 10 3.95 1.32 4 2 12 11.23 1.28 -4 2 -12 8.52 2.19 -4 -2 -12 8.87 2.35 -4 2 -14 68.22 6.46 -4 -2 -14 58.58 6.03 -4 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5.33 -4 4 -2 679 13.71 4 4 2 665.24 12.14 4 -4 2 649.46 13.49 -4 4 -2 644.62 13.11 -4 -4 -4 38.75 3.16 -4 4 -4 40.5 2.99 4 4 4 39.21 2.86 -4 4 -4 40.45 3.21 -4 4 -6 3.88 1.09 4 4 6 6.16 1.45 4 -4 6 3.02 1.14 -4 4 -6 3.18 0.86 -4 -4 -6 4.44 1.24 4 4 8 1.19 0.8 -4 4 -8 0.6 0.76 -4 4 -8 0.8 0.58 -4 -4 -8 1.82 1 4 -4 8 0.17 0.66 -4 4 -10 10.69 1.53 -4 -4 -10 11.55 2.35 -4 4 -10 7.33 1.95 4 4 10 12.42 2.37 -4 4 -12 1.56 0.7 -4 -4 -12 1.54 0.99 -4 4 -12 3.49 1.71 -4 -4 -14 5.8 2.24 4 4 14 4.04 0.82 -4 4 -14 4.8 1.84 -4 4 -16 3.41 2.1 -4 -4 -16 3.03 1.96 -4 -4 -18 18.4 4.14 -4 4 -18 22.46 4.45 4 5 -21 -2.51 2.5 4 5 -19 0.88 1.51 4 5 -17 0.55 1.4 4 5 -15 55.04 3.53 4 5 -15 43.56 4.96 -4 -5 13 28.86 3.43 -4 5 13 29.95 2.84 4 5 -13 23.52 3.29 -4 -5 11 -0.94 0.91 -4 5 11 0.48 0.75 4 5 -11 -0.27 0.59 -4 5 9 4.64 1.32 -4 -5 9 3.72 1.08 -4 5 9 5.47 1.31 4 5 -7 285.06 8.53 -4 5 7 284.79 8.71 -4 5 7 286.29 10.39 -4 -5 7 285.42 7.92 -4 5 5 27.22 2.48 4 -5 -5 25.55 2.5 4 5 -5 26.61 2.13 4 -5 -3 7.21 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28.81 2.84 4 -7 3 29.47 2.96 4 7 3 31.46 3.03 4 7 5 10.89 1.83 -4 7 -5 7.64 1.66 -4 7 -5 6.25 1.54 -4 7 -7 31.48 3.47 4 7 7 25.67 3.2 -4 7 -7 28.88 3.52 -4 -7 -9 23.52 3.9 -4 7 -9 14.6 2.5 -4 7 -9 21.54 3.29 -4 7 -11 64.62 4.57 -4 -7 -11 70.01 6.92 -4 7 -11 57.91 5.81 -4 7 -13 39.46 3.62 -4 -7 -13 42.84 5.8 -4 7 -13 34.26 4.83 -4 -7 -15 13.95 3.81 -4 7 -15 18.49 3.97 -4 7 -17 15.84 3.76 -4 -7 -17 12.79 3.82 4 8 -20 1.57 2.09 4 8 -18 2.28 1.63 4 8 -16 4.19 1.91 4 8 -14 6.64 2.05 4 8 -12 4.12 1.12 -4 8 12 2.04 1.14 4 8 -12 3.38 1.39 4 8 -10 67.33 5.16 4 8 -10 64.46 3.41 4 -8 -8 11.1 2.19 4 8 -8 9.33 1.13 4 -8 -6 13.05 2.22 4 8 -6 11.3 1.77 4 8 -6 8.36 0.88 4 -8 -4 5.11 1.29 4 8 -4 6.03 1.19 4 -8 -2 5.72 1.53 -4 -8 2 4.85 0.75 -4 8 0 108.52 5.62 4 -8 0 118.54 6.01 4 -8 2 93.29 5.45 -4 8 -2 87.46 5.11 4 8 2 89.69 5.51 4 8 4 46.78 3.98 -4 8 -4 48.83 4.01 -4 8 -4 49.87 4.31 -4 8 -6 19.32 2.62 -4 8 -6 18.12 2.77 4 8 6 13.99 2.27 -4 8 -8 0.62 0.89 4 8 8 0.39 0.9 -4 8 -8 3.26 1.64 -4 8 -10 4.47 1.71 -4 8 -12 2.04 1.4 -4 -8 -12 5.16 2.42 -4 8 -12 1.82 1.09 -4 8 -14 10.03 2.85 -4 -8 -14 3.67 2.45 -4 -8 -16 0.26 2.17 -4 8 -16 0.67 2.09 -4 8 -18 23.36 4.9 -4 -8 -18 23.85 5.68 4 9 -19 10 3.05 4 9 -17 0.58 1.46 4 9 -15 7.29 2.42 4 9 -13 173.56 9.66 -4 9 13 183.04 8.59 4 9 -11 4.81 1.17 4 9 -11 3.26 1.31 4 9 -9 11.55 1.4 4 9 -9 11.14 2.11 4 -9 -9 9.17 1.97 4 9 -7 17.6 1.44 4 -9 -7 19.79 2.9 4 -9 -5 18.72 2.63 4 -9 -3 24.05 2.91 -4 -9 3 32.09 1.99 4 -9 -1 152.26 7.19 -4 9 1 154.83 6.83 -4 -9 1 147.21 5.04 -4 9 -1 16.11 2.26 4 -9 1 14.97 2.31 -4 9 -3 10.54 1.87 4 9 3 11.82 2.12 4 -9 3 11.91 2.16 4 9 5 0.3 0.69 -4 9 -5 -0.34 0.69 -4 9 -5 0.9 0.98 4 9 7 212.42 9.64 -4 9 -7 213.72 9.3 -4 9 -7 212.23 10.39 -4 9 -9 0.14 1.47 -4 9 -11 68.61 6.71 -4 9 -13 12.36 3.12 -4 9 -13 14.5 2.46 -4 9 -15 8.62 3.06 -4 9 -17 -0.43 1.62 4 10 -20 3.98 1.95 4 10 -18 1.42 1.48 4 10 -16 0.78 1.27 4 10 -14 4.38 1.92 4 10 -12 5.97 1.87 4 -10 -10 6.27 1.85 4 10 -10 4.66 1.7 4 10 -10 4.57 0.94 4 10 -8 28.85 3.34 4 -10 -8 21.83 3.25 4 10 -8 25.78 2 4 -10 -6 287.81 11.47 4 10 -6 264.94 9.66 4 -10 -4 1.36 1.12 -4 -10 2 49.61 2.95 4 -10 -2 41.09 3.94 -4 -10 0 255.76 7.66 4 -10 0 265.02 10.1 -4 10 0 259.82 9.48 4 10 2 54.24 4.8 4 -10 2 52.08 4.4 -4 10 -2 51.96 4.26 -4 10 -4 40.92 3.83 4 10 4 39.62 4.09 -4 10 -4 43.87 4.64 4 10 6 -1 1.06 -4 10 -6 -0.8 0.85 -4 10 -8 1.41 1.23 -4 10 -10 113.13 8.57 -4 10 -12 30.93 4.79 -4 10 -14 22.73 4.41 -4 10 -16 2.56 1.88 4 11 -19 2.56 1.6 4 11 -17 0.1 1.06 4 11 -15 -0.94 1.37 4 11 -13 3.94 1.9 4 11 -11 8.73 2.28 4 -11 -11 8.22 2.3 4 11 -9 69.25 3.59 4 11 -9 76.6 5.96 4 -11 -9 73.58 6.46 4 11 -7 63.71 5.08 4 -11 -7 72.79 6.01 4 -11 -5 155.84 8.56 4 11 -5 160.29 7.53 -4 -11 3 26.95 2.23 4 -11 -3 22.22 3.01 -4 -11 1 102.05 4.77 4 -11 -1 103.27 6.5 4 -11 1 71.62 5.45 -4 -11 -1 69.41 4.17 4 -11 3 9.2 2.23 4 11 3 9.11 2.61 -4 11 -5 1.33 0.98 -4 11 -7 23.4 3.78 -4 11 -9 -1.74 1.66 -4 11 -11 -0.87 1.44 -4 11 -13 -0.72 1.47 -4 11 -15 7.62 2.75 4 12 -18 8.15 3.03 4 12 -16 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5 90.98 5.66 -5 8 -7 3.54 1.48 5 8 7 2.02 1.05 -5 8 -9 14.56 2.79 -5 8 -9 17.29 2.62 -5 -8 -11 1.96 1.67 -5 8 -11 0.59 1.2 -5 8 -11 3.82 1.28 -5 -8 -13 2.07 1.38 -5 8 -13 5.79 1.6 -5 8 -13 4.6 2.08 -5 -8 -15 32.2 5.57 -5 8 -15 31.19 5.05 -5 8 -17 5.62 2.56 -5 -8 -17 13.13 4.18 5 9 -20 4.69 2.28 5 9 -18 1.99 1.69 5 9 -16 7.32 2.26 5 9 -14 9.37 2.35 5 -9 -12 24.33 3.76 5 9 -12 15.92 2.82 -5 9 12 23.12 3.19 5 -9 -10 12.2 2.45 5 9 -10 14.42 2.43 -5 9 10 18.25 2.71 5 9 -10 13.47 1.33 5 -9 -8 0.51 1.18 5 -9 -6 1.31 1.23 5 -9 -4 -0.47 0.78 5 9 -4 0.49 0.51 -5 -9 2 42.59 2.28 5 -9 -2 42.93 3.95 5 -9 0 57.2 4.56 -5 9 0 61.54 4.56 5 9 2 42.08 3.94 5 -9 2 43.32 4.06 -5 9 -2 39.36 3.67 5 9 4 148.16 7.34 -5 9 -4 155.15 8.15 -5 9 -4 146.2 7.48 -5 9 -6 138.65 8.21 5 9 6 134.04 7.37 -5 9 -8 954.86 24.84 -5 9 -10 0.14 0.98 -5 9 -10 2.66 1.24 -5 9 -12 9.48 2.65 -5 9 -12 12.78 2.38 -5 9 -14 51.07 6.4 -5 9 -16 11.4 3.28 5 10 -19 1.44 2.25 5 10 -17 4.1 1.71 5 10 -15 4.6 2.03 5 -10 -13 8.22 2.58 5 10 -13 5.77 2.01 5 10 -11 13.02 2.58 5 -10 -11 14.65 3.02 5 10 -9 93.82 6.12 5 -10 -9 96.18 7.09 5 10 -7 238.57 9.23 5 -10 -7 257.4 11.38 5 -10 -5 103.11 6.73 5 -10 -3 16.9 2.63 -5 -10 3 20.28 1.57 5 -10 -1 3.86 1.45 -5 -10 1 3.74 0.86 5 -10 1 50.79 4.61 5 10 1 61.26 4.9 5 10 3 3.59 1.33 5 -10 3 3.13 1.17 5 10 5 37.71 3.84 -5 10 -5 48.01 4.92 -5 10 -7 25.92 3.94 -5 10 -9 3.86 1.94 -5 10 -11 18.13 3.66 -5 10 -13 5.44 2.48 -5 10 -15 6.28 2.62 5 11 -18 3.99 2.14 5 -11 -16 4.57 2.45 5 11 -16 5.13 2.18 5 11 -14 3.56 1.34 5 -11 -14 11.21 3.2 5 -11 -12 0.74 1.43 5 11 -12 -1.45 1.37 5 -11 -10 -0.88 1.58 5 11 -10 0.65 0.94 5 -11 -8 9.15 2.35 5 11 -8 8.36 1.81 5 -11 -6 34.3 4.07 5 11 -6 33.61 3.43 5 -11 -4 14.78 2.5 -5 -11 2 10.14 1.33 5 -11 -2 9.6 2.24 5 -11 0 0.62 0.94 -5 -11 0 0.66 0.64 5 11 2 1.98 1.57 5 -11 2 0.77 1.18 5 11 4 5.98 1.76 -5 11 -4 4.66 1.94 -5 11 -6 10.95 2.51 -5 11 -8 5.03 1.88 -5 11 -10 6.76 2.37 -5 11 -12 0.76 1.97 -5 11 -14 11.74 3.36 5 12 -17 0.18 1.27 5 -12 -15 16.1 3.64 5 12 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4.37 1.09 10 -3 3 2.42 1.43 10 3 5 6.48 1.48 -10 -3 -5 3.66 1.16 10 3 5 3.87 1.77 -10 3 -5 4.82 1.64 10 -3 5 5.22 1.8 10 3 7 19.4 2.68 10 3 7 15.89 2.76 -10 3 -7 21.62 3.22 -10 -3 -7 24.49 3.21 -10 -3 -9 5.7 1.78 10 3 9 3.91 1.48 -10 3 -9 0.53 1.25 -10 3 -11 69.58 6.76 10 3 11 59.33 5.26 -10 -3 -11 69.44 6.29 -10 3 -13 -0.07 1.46 -10 -3 -13 -0.74 1.1 10 3 13 0.74 0.86 -10 3 -15 1.74 1.18 -10 -3 -15 7.2 2.7 -10 -3 -17 0.12 1.64 10 -4 -18 1.22 1.62 10 -4 -16 10.92 2.53 10 -4 -14 13.08 2.76 10 4 -14 13.1 2.68 10 4 -12 10.04 1.31 10 -4 -12 10.47 2.28 10 4 -12 12.12 2.71 10 4 -10 38.8 4.65 -10 4 10 42.97 4.17 10 4 -10 38.52 2.07 10 -4 -10 33.19 3.68 -10 4 8 129.74 6.87 10 -4 -8 124.56 7.01 -10 4 6 261.36 10.2 10 -4 -6 244.09 9.67 -10 4 4 1.72 0.87 10 -4 -4 1.51 0.84 10 -4 -2 68.14 5.04 -10 -4 2 57.74 3.02 -10 4 2 62.54 4.66 -10 4 0 9.36 1.91 -10 4 0 12.46 1.91 -10 -4 0 10.88 1.49 10 4 2 27.62 2.13 -10 4 -2 26.58 2.93 -10 -4 -2 25.61 2.5 -10 -4 -4 7.4 1.54 10 4 4 6.33 1.37 -10 4 -4 5.06 1.54 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-5 -11 6.6 2.17 -10 -5 -13 2.41 1.84 10 5 13 2.77 1.31 -10 -5 -15 23.21 4.7 -10 5 -15 18.86 4 10 -6 -18 -0.82 1.58 10 -6 -16 6.15 2.46 10 -6 -14 23.66 3.88 10 6 -14 19.85 3.49 10 -6 -12 2.07 1.43 10 -6 -10 1.93 1.6 10 6 -10 4.84 1.05 10 -6 -8 2.15 1.19 -10 6 8 3.02 1.49 10 -6 -6 263.37 10.74 10 -6 -4 13.93 2.52 -10 -6 2 0.53 0.43 10 -6 -2 1.01 1.15 -10 6 0 33.53 3.27 -10 -6 0 35.26 2.49 10 -6 0 35.25 3.97 10 6 0 28.47 1.51 -10 6 -2 308.97 11.09 10 6 2 340.27 8.71 -10 6 -4 164.7 8.56 10 6 4 172.64 7.21 -10 6 -6 1.82 1.12 10 6 6 1.57 1 -10 -6 -6 0.8 1.1 -10 6 -8 -0.17 0.92 -10 -6 -8 1.3 1.24 -10 6 -10 121.9 9.01 -10 -6 -10 124.02 9.08 10 6 12 2.06 1.31 -10 -6 -12 1.25 1.08 -10 6 -12 4.69 2.3 -10 -6 -14 -3.05 2.29 -10 6 -14 0.99 2.02 -10 -6 -16 9.46 3.72 10 -7 -17 0.84 1.77 10 -7 -15 5.39 2.21 10 7 -15 1.26 1.11 10 -7 -13 9.75 2.61 10 -7 -11 13.92 2.67 10 -7 -9 0.26 1.04 10 7 -9 1.27 0.48 10 -7 -7 -1.98 1.5 10 -7 -5 105.05 6.89 10 -7 -3 49.85 4.73 10 -7 -1 5 1.85 -10 -7 1 4.85 0.83 10 7 1 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3.28 10 9 1 -0.08 0.44 -10 9 -1 -0.61 1.01 10 -9 1 0.34 1.04 10 9 3 15.57 2.3 -10 9 -3 10.2 2.29 10 9 5 6.16 1.72 -10 9 -5 2.79 1.52 -10 9 -7 73.59 6.86 -10 9 -9 91.36 8.07 -10 9 -11 1.92 1.83 -10 9 -13 5.81 2.85 10 -10 -14 0.86 1.42 10 -10 -12 9.48 3.01 10 -10 -10 2.38 1.66 10 -10 -8 11.48 3.02 10 -10 -6 347.7 14.23 10 10 -4 60.72 2.82 10 -10 -4 62.28 5.94 10 10 -2 7.56 1.13 10 -10 -2 8.94 2.54 10 10 0 66.73 3.91 10 -10 0 59.42 5.81 10 10 2 18.36 2.33 -10 10 -2 19.34 3.12 -10 10 -4 90.01 7.23 -10 10 -6 94.7 7.79 -10 10 -8 22.09 4.03 -10 10 -10 29.38 4.98 -10 10 -12 -0.52 1.94 10 -11 -13 5.61 3.5 10 -11 -11 5.1 2.07 10 -11 -9 -0.45 1.7 10 -11 -7 220.15 11.84 10 -11 -5 6.49 2.35 10 -11 -3 0.57 1.6 10 11 -3 -0.25 0.45 10 -11 -1 11.77 2.94 -10 11 -1 4.3 1.63 10 -11 1 1.58 1.44 -10 11 -3 5.81 1.85 -10 11 -5 7.23 2.38 -10 11 -7 145.63 10.25 -10 11 -9 1.43 1.83 -10 11 -11 2.12 1.62 10 -12 -12 3.5 2.01 10 -12 -10 2.34 1.4 10 -12 -8 74.06 7.29 10 -12 -6 177.5 10.74 10 -12 -4 3.96 1.96 10 -12 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10.27 3.07 17 -1 -2 10.96 3.09 17 1 0 19.85 4.29 17 -1 0 18.18 3.9 17 1 2 1.16 1.47 17 -1 2 2.81 1.88 17 1 4 1.08 1.72 17 -1 4 4.44 2.11 17 1 6 -0.32 0.96 17 -1 6 3.83 1.95 17 1 8 7.38 2.99 17 -1 8 13.58 3.47 17 2 -7 4.51 2.45 17 -2 -7 1.27 1.9 17 2 -5 31.21 5.39 17 -2 -5 24.17 4.51 17 2 -3 31.11 5.57 17 -2 -3 24.21 4.71 17 2 -1 0.88 1.17 17 -2 -1 1.62 1.7 17 2 1 30.75 5.3 17 -2 1 28.64 4.89 17 2 3 -0.57 1.22 17 -2 3 0.52 1.31 17 2 5 14.01 3.57 17 -2 5 16.64 3.76 17 2 7 9.19 3.12 17 3 -6 2.72 1.89 17 3 -4 0.3 1.57 17 -3 -4 2.2 1.51 17 3 -2 26.52 5.12 17 -3 -2 30.31 5.15 17 3 0 17.54 4.4 17 -3 0 21.56 4.24 17 3 2 6.81 3.05 17 3 4 8.43 2.93 17 3 6 -0.68 1.39 17 4 -5 11.81 3.64 17 4 -3 6.21 2.71 17 4 -1 0.6 1.54 17 4 1 10.16 3.42 17 4 3 8.85 2.81 17 4 5 3.93 2.44 17 5 -2 -5.15 2.62 17 5 0 25.21 5.16 17 5 2 3.79 2.42 17 -6 -9 9.14 2.98 17 -7 -8 -2.62 1.62