#------------------------------------------------------------------------------ #$Date: 2019-10-28 02:15:29 +0200 (Mon, 28 Oct 2019) $ #$Revision: 219587 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/24/1552483.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_1552483 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_name_full 'Journal of agricultural and food chemistry' _journal_paper_doi 10.1021/acs.jafc.9b05349 _journal_year 2019 _chemical_formula_moiety 'C18 H19 N3 O3' _chemical_formula_sum 'C18 H19 N3 O3' _chemical_formula_weight 325.36 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-08-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 103.070(8) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 25.1091(19) _cell_length_b 7.6592(5) _cell_length_c 17.0110(12) _cell_measurement_reflns_used 3397 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 29.0060 _cell_measurement_theta_min 2.6420 _cell_volume 3186.7(4) _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 2018/2 (Sheldrick, 2018)' _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -9.00 79.00 1.00 8.00 -- 11.74 37.00 120.00 88 2 \w -56.00 40.00 1.00 8.00 -- 11.74 -57.00 -60.00 96 ; _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 0.0019981000 _diffrn_orient_matrix_UB_12 0.0490172000 _diffrn_orient_matrix_UB_13 0.0359054000 _diffrn_orient_matrix_UB_21 -0.0147555000 _diffrn_orient_matrix_UB_22 0.0692456000 _diffrn_orient_matrix_UB_23 -0.0227467000 _diffrn_orient_matrix_UB_31 -0.0249032000 _diffrn_orient_matrix_UB_32 -0.0370713000 _diffrn_orient_matrix_UB_33 0.0050396000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6537 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.994 _diffrn_reflns_theta_max 24.994 _diffrn_reflns_theta_min 2.458 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92604 _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 1.356 _exptl_crystal_description block _exptl_crystal_F_000 1376 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.201 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 2796 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.096 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0397 _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^)+(0.0369P)^2^+1.6792P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.0945 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2360 _reflns_number_total 2796 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL b29-1_a.res in C2/c b29-1.res created by SHELXL-2018/3 at 14:33:11 on 14-Aug-2019 REM Old TITL B29-1 in C2/c REM SHELXT solution in C2/c: R1 0.112, Rweak 0.004, Alpha 0.026 REM 0.739 for 254 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N3 O3 CELL 0.71073 25.1091 7.6592 17.011 90 103.07 90 ZERR 8 0.0019 0.0005 0.0012 0 0.008 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O UNIT 144 152 24 24 L.S. 20 0 0 PLAN 20 BOND $H list 4 fmap 2 53 acta OMIT -3 50 REM REM REM WGHT 0.036900 1.679200 FVAR 0.34604 O1 4 0.333657 0.360050 0.592299 11.00000 0.01955 0.01359 = 0.01666 -0.00309 0.00742 -0.00287 O2 4 0.291779 -0.072105 0.444374 11.00000 0.02460 0.01773 = 0.01579 -0.00181 0.00460 -0.00567 O3 4 0.526056 0.258892 0.499475 11.00000 0.01435 0.03684 = 0.01857 -0.00405 0.00288 -0.00732 N2 3 0.357356 0.137495 0.479418 11.00000 0.01546 0.01537 = 0.01412 -0.00489 0.00438 -0.00287 AFIX 43 H2 2 0.370457 0.215728 0.514779 11.00000 -1.20000 AFIX 0 N1 3 0.277326 0.266371 0.673737 11.00000 0.01735 0.01979 = 0.01535 0.00263 0.00599 0.00351 N3 3 0.456353 0.271864 0.563403 11.00000 0.01623 0.02406 = 0.01916 -0.00755 0.00244 -0.00074 C1 1 0.299770 0.237854 0.611253 11.00000 0.01094 0.01512 = 0.01399 0.00404 0.00217 0.00302 C6 1 0.312960 0.045030 0.490206 11.00000 0.01464 0.01065 = 0.01402 0.00287 0.00003 0.00169 C2 1 0.290847 0.085880 0.563180 11.00000 0.01223 0.01614 = 0.01192 0.00273 0.00050 0.00332 C13 1 0.472558 0.229956 0.500328 11.00000 0.01358 0.01262 = 0.01816 0.00278 0.00262 0.00084 C8 1 0.354342 0.052485 0.340089 11.00000 0.01426 0.01594 = 0.01580 0.00104 0.00345 -0.00101 AFIX 43 H8 2 0.317401 0.025883 0.332686 11.00000 -1.20000 AFIX 0 C12 1 0.439245 0.157536 0.424610 11.00000 0.01600 0.01214 = 0.01687 0.00165 0.00448 0.00168 C16 1 0.345323 0.517525 0.642237 11.00000 0.01835 0.01260 = 0.01672 -0.00486 0.00511 0.00118 AFIX 13 H16 2 0.311238 0.564720 0.652436 11.00000 -1.20000 AFIX 0 C3 1 0.256234 -0.038845 0.584311 11.00000 0.01635 0.01618 = 0.01761 0.00205 0.00128 0.00020 AFIX 43 H3 2 0.248675 -0.140820 0.554172 11.00000 -1.20000 AFIX 0 C9 1 0.379981 0.030250 0.277027 11.00000 0.02033 0.01496 = 0.01438 -0.00010 0.00236 0.00075 AFIX 43 H9 2 0.360043 -0.010098 0.227511 11.00000 -1.20000 AFIX 0 C7 1 0.383235 0.114521 0.414969 11.00000 0.01681 0.01107 = 0.01470 0.00132 0.00427 0.00335 C5 1 0.244447 0.141255 0.691898 11.00000 0.01623 0.02346 = 0.01795 0.00399 0.00766 0.00404 AFIX 43 H5 2 0.228549 0.159895 0.735540 11.00000 -1.20000 AFIX 0 C4 1 0.232965 -0.012460 0.649777 11.00000 0.01633 0.02026 = 0.02094 0.00697 0.00663 -0.00134 AFIX 43 H4 2 0.210291 -0.096063 0.664773 11.00000 -1.20000 AFIX 0 C10 1 0.435327 0.067560 0.286761 11.00000 0.02129 0.02078 = 0.01618 0.00122 0.00881 0.00191 AFIX 43 H10 2 0.452618 0.049693 0.244510 11.00000 -1.20000 AFIX 0 C11 1 0.464225 0.131339 0.359802 11.00000 0.01481 0.01904 = 0.02015 0.00188 0.00584 -0.00024 AFIX 43 H11 2 0.501122 0.157545 0.366177 11.00000 -1.20000 AFIX 0 C18 1 0.369222 0.644680 0.591859 11.00000 0.02162 0.01433 = 0.02084 -0.00236 0.00386 -0.00167 AFIX 137 H18A 2 0.402190 0.596881 0.581076 11.00000 -1.50000 H18B 2 0.377346 0.752798 0.620622 11.00000 -1.50000 H18C 2 0.343340 0.665281 0.541821 11.00000 -1.50000 AFIX 0 C15 1 0.551765 0.327347 0.578682 11.00000 0.01675 0.02053 = 0.01868 -0.00125 -0.00201 -0.00307 AFIX 23 H15A 2 0.568415 0.440150 0.574301 11.00000 -1.20000 H15B 2 0.579476 0.247808 0.607463 11.00000 -1.20000 AFIX 0 C17 1 0.384410 0.474399 0.721650 11.00000 0.02454 0.02081 = 0.01865 -0.00039 0.00390 -0.00088 AFIX 137 H17A 2 0.368168 0.388239 0.749911 11.00000 -1.50000 H17B 2 0.391927 0.578138 0.753930 11.00000 -1.50000 H17C 2 0.417891 0.429507 0.711404 11.00000 -1.50000 AFIX 0 C14 1 0.504287 0.343574 0.621146 11.00000 0.01824 0.02115 = 0.01847 -0.00344 -0.00064 0.00047 AFIX 23 H14A 2 0.511712 0.277332 0.671037 11.00000 -1.20000 H14B 2 0.498232 0.464725 0.633276 11.00000 -1.20000 AFIX 0 HKLF 4 REM b29-1_a.res in C2/c REM wR2 = 0.0945, GooF = S = 1.096, Restrained GooF = 1.096 for all data REM R1 = 0.0397 for 2360 Fo > 4sig(Fo) and 0.0487 for all 2796 data REM 219 parameters refined using 0 restraints END WGHT 0.0369 1.6793 REM Highest difference peak 0.201, deepest hole -0.228, 1-sigma level 0.047 Q1 1 0.3838 0.1608 0.5252 11.00000 0.05 0.20 Q2 1 0.4562 0.2061 0.4626 11.00000 0.05 0.16 Q3 1 0.5000 0.1335 0.7500 10.50000 0.05 0.15 Q4 1 0.4034 0.1965 0.4067 11.00000 0.05 0.14 Q5 1 0.2629 0.0578 0.5537 11.00000 0.05 0.14 Q6 1 0.2605 0.0326 0.6926 11.00000 0.05 0.13 Q7 1 0.2995 0.0615 0.5365 11.00000 0.05 0.13 Q8 1 0.5806 0.0991 0.4846 11.00000 0.05 0.13 Q9 1 0.4006 0.1799 0.5938 11.00000 0.05 0.13 Q10 1 0.2219 0.2202 0.7384 11.00000 0.05 0.13 Q11 1 0.2801 0.0244 0.2395 11.00000 0.05 0.13 Q12 1 0.4398 0.1061 0.6364 11.00000 0.05 0.13 Q13 1 0.2982 -0.1527 0.3847 11.00000 0.05 0.13 Q14 1 0.2367 0.1929 0.7589 11.00000 0.05 0.12 Q15 1 0.2575 -0.0225 0.3882 11.00000 0.05 0.12 Q16 1 0.2771 0.1738 0.5672 11.00000 0.05 0.12 Q17 1 0.4851 0.3328 0.3623 11.00000 0.05 0.12 Q18 1 0.3381 0.6369 0.5187 11.00000 0.05 0.12 Q19 1 0.3355 0.4440 0.6162 11.00000 0.05 0.12 Q20 1 0.4219 0.5945 0.8021 11.00000 0.05 0.12 REM The information below was added by Olex2. REM REM R1 = 0.0397 for 2360 Fo > 4sig(Fo) and 0.0487 for all 8117 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.20, deepest hole -0.23 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0487 REM R1_gt = 0.0397 REM wR_ref = 0.0945 REM GOOF = 1.096 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 8117 REM Reflections_gt = 2360 REM Parameters = n/a REM Hole = -0.23 REM Peak = 0.20 REM Flack = n/a ; _cod_data_source_file jf9b05349_si_003.cif _cod_data_source_block b29-1 _cod_database_code 1552483 _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 99.89 _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 Ternary CH refined with riding coordinates: C16(H16) 2.b Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C14(H14A,H14B) 2.c Aromatic/amide H refined with riding coordinates: N2(H2), C8(H8), C3(H3), C9(H9), C5(H5), C4(H4), C10(H10), C11(H11) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C17(H17A,H17B,H17C) ; _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 1.251 _oxdiff_exptl_absorpt_empirical_full_min 0.769 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 0.33366(4) 0.36005(13) 0.59230(6) 0.0161(3) Uani 1 1 d . O2 O 0.29178(5) -0.07211(14) 0.44437(7) 0.0194(3) Uani 1 1 d . O3 O 0.52606(4) 0.25889(16) 0.49947(7) 0.0234(3) Uani 1 1 d . N2 N 0.35736(5) 0.13750(17) 0.47942(8) 0.0148(3) Uani 1 1 d . H2 H 0.370457 0.215728 0.514779 0.018 Uiso 1 1 calc R N1 N 0.27733(5) 0.26637(17) 0.67374(8) 0.0171(3) Uani 1 1 d . N3 N 0.45635(5) 0.27186(18) 0.56340(8) 0.0201(3) Uani 1 1 d . C1 C 0.29977(6) 0.2379(2) 0.61125(9) 0.0135(4) Uani 1 1 d . C6 C 0.31296(6) 0.04503(19) 0.49021(9) 0.0136(4) Uani 1 1 d . C2 C 0.29085(6) 0.0859(2) 0.56318(9) 0.0138(4) Uani 1 1 d . C13 C 0.47256(6) 0.2300(2) 0.50033(10) 0.0149(4) Uani 1 1 d . C8 C 0.35434(6) 0.0525(2) 0.34009(9) 0.0153(4) Uani 1 1 d . H8 H 0.317401 0.025883 0.332686 0.018 Uiso 1 1 calc R C12 C 0.43924(6) 0.1575(2) 0.42461(10) 0.0149(4) Uani 1 1 d . C16 C 0.34532(7) 0.5175(2) 0.64224(10) 0.0157(4) Uani 1 1 d . H16 H 0.311238 0.564720 0.652436 0.019 Uiso 1 1 calc R C3 C 0.25623(6) -0.0388(2) 0.58431(10) 0.0171(4) Uani 1 1 d . H3 H 0.248675 -0.140820 0.554172 0.021 Uiso 1 1 calc R C9 C 0.37998(7) 0.0303(2) 0.27703(10) 0.0168(4) Uani 1 1 d . H9 H 0.360043 -0.010098 0.227511 0.020 Uiso 1 1 calc R C7 C 0.38323(6) 0.11452(19) 0.41497(9) 0.0141(4) Uani 1 1 d . C5 C 0.24445(6) 0.1413(2) 0.69190(10) 0.0186(4) Uani 1 1 d . H5 H 0.228549 0.159895 0.735540 0.022 Uiso 1 1 calc R C4 C 0.23296(6) -0.0125(2) 0.64978(10) 0.0188(4) Uani 1 1 d . H4 H 0.210291 -0.096063 0.664773 0.023 Uiso 1 1 calc R C10 C 0.43533(7) 0.0676(2) 0.28676(10) 0.0187(4) Uani 1 1 d . H10 H 0.452618 0.049693 0.244510 0.022 Uiso 1 1 calc R C11 C 0.46423(7) 0.1313(2) 0.35980(10) 0.0177(4) Uani 1 1 d . H11 H 0.501122 0.157545 0.366177 0.021 Uiso 1 1 calc R C18 C 0.36922(7) 0.6447(2) 0.59186(10) 0.0191(4) Uani 1 1 d . H18A H 0.402190 0.596881 0.581076 0.029 Uiso 1 1 calc GR H18B H 0.377346 0.752798 0.620622 0.029 Uiso 1 1 calc GR H18C H 0.343340 0.665281 0.541821 0.029 Uiso 1 1 calc GR C15 C 0.55176(7) 0.3273(2) 0.57868(10) 0.0196(4) Uani 1 1 d . H15A H 0.568415 0.440150 0.574301 0.024 Uiso 1 1 calc R H15B H 0.579476 0.247808 0.607463 0.024 Uiso 1 1 calc R C17 C 0.38441(7) 0.4744(2) 0.72165(10) 0.0215(4) Uani 1 1 d . H17A H 0.368168 0.388239 0.749911 0.032 Uiso 1 1 calc GR H17B H 0.391927 0.578138 0.753930 0.032 Uiso 1 1 calc GR H17C H 0.417891 0.429507 0.711404 0.032 Uiso 1 1 calc GR C14 C 0.50429(6) 0.3436(2) 0.62115(10) 0.0200(4) Uani 1 1 d . H14A H 0.511712 0.277332 0.671037 0.024 Uiso 1 1 calc R H14B H 0.498232 0.464725 0.633276 0.024 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 0.0196(6) 0.0136(6) 0.0167(6) -0.0031(5) 0.0074(5) -0.0029(5) O2 0.0246(6) 0.0177(6) 0.0158(6) -0.0018(5) 0.0046(5) -0.0057(5) O3 0.0144(6) 0.0368(7) 0.0186(6) -0.0040(5) 0.0029(5) -0.0073(5) N2 0.0155(7) 0.0154(7) 0.0141(7) -0.0049(6) 0.0044(6) -0.0029(6) N1 0.0174(7) 0.0198(7) 0.0154(7) 0.0026(6) 0.0060(6) 0.0035(6) N3 0.0162(7) 0.0241(8) 0.0192(8) -0.0076(6) 0.0024(6) -0.0007(6) C1 0.0109(8) 0.0151(8) 0.0140(8) 0.0040(7) 0.0022(6) 0.0030(7) C6 0.0146(8) 0.0106(8) 0.0140(8) 0.0029(7) 0.0000(6) 0.0017(7) C2 0.0122(8) 0.0161(8) 0.0119(8) 0.0027(7) 0.0005(6) 0.0033(7) C13 0.0136(8) 0.0126(8) 0.0182(9) 0.0028(7) 0.0026(7) 0.0008(7) C8 0.0143(8) 0.0159(8) 0.0158(9) 0.0010(7) 0.0034(7) -0.0010(7) C12 0.0160(8) 0.0121(8) 0.0169(9) 0.0016(7) 0.0045(7) 0.0017(7) C16 0.0184(9) 0.0126(8) 0.0167(9) -0.0049(7) 0.0051(7) 0.0012(7) C3 0.0163(8) 0.0162(8) 0.0176(9) 0.0020(7) 0.0013(7) 0.0002(7) C9 0.0203(9) 0.0150(8) 0.0144(9) -0.0001(7) 0.0024(7) 0.0008(7) C7 0.0168(8) 0.0111(8) 0.0147(8) 0.0013(6) 0.0043(7) 0.0034(7) C5 0.0162(8) 0.0235(9) 0.0180(9) 0.0040(7) 0.0077(7) 0.0040(7) C4 0.0163(8) 0.0203(9) 0.0209(9) 0.0070(7) 0.0066(7) -0.0013(7) C10 0.0213(9) 0.0208(9) 0.0162(9) 0.0012(7) 0.0088(7) 0.0019(7) C11 0.0148(8) 0.0190(8) 0.0202(9) 0.0019(7) 0.0058(7) -0.0002(7) C18 0.0216(9) 0.0143(8) 0.0208(9) -0.0024(7) 0.0039(7) -0.0017(7) C15 0.0167(9) 0.0205(9) 0.0187(9) -0.0012(7) -0.0020(7) -0.0031(7) C17 0.0245(9) 0.0208(9) 0.0187(9) -0.0004(7) 0.0039(7) -0.0009(8) C14 0.0182(9) 0.0211(9) 0.0185(9) -0.0034(7) -0.0006(7) 0.0005(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 C16 119.03(12) C13 O3 C15 106.29(12) C6 N2 H2 117.5 C6 N2 C7 125.04(13) C7 N2 H2 117.5 C1 N1 C5 117.37(14) C13 N3 C14 106.67(13) O1 C1 C2 117.31(14) N1 C1 O1 118.72(14) N1 C1 C2 123.96(14) O2 C6 N2 122.84(15) O2 C6 C2 119.25(14) N2 C6 C2 117.88(13) C1 C2 C6 127.63(14) C3 C2 C1 116.29(15) C3 C2 C6 116.05(14) O3 C13 C12 114.62(14) N3 C13 O3 118.13(14) N3 C13 C12 127.21(14) C9 C8 H8 119.6 C9 C8 C7 120.83(15) C7 C8 H8 119.6 C7 C12 C13 122.68(14) C11 C12 C13 118.32(14) C11 C12 C7 119.00(14) O1 C16 H16 109.8 O1 C16 C18 104.77(12) O1 C16 C17 109.96(13) C18 C16 H16 109.8 C18 C16 C17 112.73(14) C17 C16 H16 109.8 C2 C3 H3 119.7 C4 C3 C2 120.61(15) C4 C3 H3 119.7 C8 C9 H9 119.6 C8 C9 C10 120.72(15) C10 C9 H9 119.6 N2 C7 C12 120.14(14) C8 C7 N2 121.10(14) C8 C7 C12 118.75(14) N1 C5 H5 118.1 N1 C5 C4 123.89(16) C4 C5 H5 118.1 C3 C4 H4 121.1 C5 C4 C3 117.87(15) C5 C4 H4 121.1 C9 C10 H10 120.4 C11 C10 C9 119.20(16) C11 C10 H10 120.4 C12 C11 H11 119.3 C10 C11 C12 121.46(15) C10 C11 H11 119.3 C16 C18 H18A 109.5 C16 C18 H18B 109.5 C16 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 O3 C15 H15A 111.0 O3 C15 H15B 111.0 O3 C15 C14 103.68(12) H15A C15 H15B 109.0 C14 C15 H15A 111.0 C14 C15 H15B 111.0 C16 C17 H17A 109.5 C16 C17 H17B 109.5 C16 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 N3 C14 C15 105.08(13) N3 C14 H14A 110.7 N3 C14 H14B 110.7 C15 C14 H14A 110.7 C15 C14 H14B 110.7 H14A C14 H14B 108.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.3520(18) O1 C16 1.4662(18) O2 C6 1.2280(18) O3 C13 1.3647(19) O3 C15 1.4539(19) N2 H2 0.8600 N2 C6 1.368(2) N2 C7 1.406(2) N1 C1 1.329(2) N1 C5 1.346(2) N3 C13 1.272(2) N3 C14 1.477(2) C1 C2 1.411(2) C6 C2 1.503(2) C2 C3 1.392(2) C13 C12 1.476(2) C8 H8 0.9300 C8 C9 1.381(2) C8 C7 1.399(2) C12 C7 1.417(2) C12 C11 1.401(2) C16 H16 0.9800 C16 C18 1.509(2) C16 C17 1.516(2) C3 H3 0.9300 C3 C4 1.384(2) C9 H9 0.9300 C9 C10 1.391(2) C5 H5 0.9300 C5 C4 1.374(2) C4 H4 0.9300 C10 H10 0.9300 C10 C11 1.379(2) C11 H11 0.9300 C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C15 H15A 0.9700 C15 H15B 0.9700 C15 C14 1.532(2) C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C14 H14A 0.9700 C14 H14B 0.9700 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 2 4093.01 23.01 0 0 -3 0.39 0.52 0 0 3 0.71 0.68 0 0 -4 679.77 13.07 0 0 4 686.53 13.64 0 0 -5 3.66 1.33 0 0 5 5.14 1.55 0 0 6 444.61 13.49 0 0 -6 417.59 12.74 0 0 -7 29 3.93 0 0 7 46.82 5.27 0 0 -8 22.74 3.54 0 0 8 38.75 4.86 0 0 9 4.08 1.93 0 0 10 348.07 15.81 0 0 -11 5.45 2.61 0 0 11 4.07 2.22 0 0 -12 1074.63 28.62 0 0 12 1091.62 31.53 0 0 13 9.23 3.4 0 0 -13 3.68 2.06 0 0 14 1286.23 37.17 0 0 15 3.73 2.68 0 0 16 1.41 2.09 0 0 17 0.06 1.42 0 0 18 59.82 9.69 0 0 19 -1.35 2.95 0 0 20 10.25 4.62 0 0 21 6.25 4.87 0 -2 0 70.93 4.38 0 2 0 76.24 4.43 0 2 -1 2659.89 27.35 0 -2 1 2580.05 26.59 0 -2 -1 2630.98 26.78 0 2 -2 3364.92 32.52 0 -2 2 3408.09 31.01 0 -2 3 1091.19 18.41 0 -2 3 1022.98 17.42 0 2 -3 1071.21 19.42 0 -2 -3 1084.05 15.92 0 2 4 3.42 1.13 0 -2 -4 3.74 1.23 0 -2 4 4.59 1.52 0 2 -4 2.06 1.12 0 -2 4 3.44 1.25 0 2 5 12.2 2.16 0 2 -5 8.88 2.09 0 -2 5 11.3 2.16 0 -2 5 12.68 2.55 0 -2 -5 11.74 1.9 0 -2 6 112.97 7.68 0 -2 -6 108.71 6.36 0 2 -6 119.68 7.73 0 2 6 113.77 6.75 0 -2 -7 320.67 11.66 0 2 -7 346.88 13.84 0 -2 7 353.02 14.45 0 2 7 339.61 12.34 0 -2 -8 48.63 4.8 0 2 8 50.44 5.18 0 2 -8 40.7 5.17 0 -2 8 54.03 6.03 0 2 9 -0.39 0.86 0 -2 -9 0.34 1 0 -2 9 0.89 1.91 0 2 -9 0.67 0.88 0 -2 10 811.75 26.16 0 2 -10 869.53 25.93 0 2 10 857.22 23.92 0 2 -10 838.06 24.98 0 2 -11 8.67 2.83 0 2 -11 12.63 3.12 0 2 11 11.64 2.89 0 -2 11 12.61 3.46 0 -2 12 186.14 13.71 0 -2 -12 197.26 12.17 0 2 12 192.41 12.64 0 -2 -13 129.45 10.15 0 -2 13 118.95 11.47 0 2 13 114.6 10.23 0 2 14 232.46 15.35 0 -2 14 227.79 16.77 0 -2 -14 221.74 13.88 0 -2 15 784.02 32.28 0 2 15 777.71 29.21 0 -2 16 532.68 27.68 0 2 16 513.9 24.83 0 2 17 18.4 4.97 0 -2 17 34.25 7.55 0 -2 18 14.39 5.37 0 2 18 9.51 3.9 0 2 19 24.52 6.61 0 -2 19 23.2 6.99 0 -2 20 2.71 3.32 0 2 20 2.28 2.94 0 2 21 96.27 13.28 0 2 22 -1.87 3.47 0 -4 0 34.5 4.45 0 4 -1 80.31 6.58 0 -4 1 68.07 6.03 0 -4 -1 87.46 7.05 0 4 -2 184.27 10.48 0 -4 2 181.61 9.82 0 -4 -2 174.26 10.04 0 -4 3 1572.62 28.99 0 -4 -3 1608.03 30.82 0 4 -3 1604.28 31.79 0 4 -4 327.73 14.93 0 -4 4 356.22 13.91 0 -4 -4 338.03 12.14 0 -4 4 329.22 13.25 0 -4 5 140.07 9.3 0 -4 5 132.12 8.49 0 4 -5 156.03 10.64 0 -4 -5 144.08 7.93 0 -4 6 1304.12 29.52 0 -4 6 1325.51 27.45 0 -4 -6 1292.71 24.22 0 4 -6 1287.85 31.79 0 -4 -7 36.47 4.21 0 -4 7 33.07 4.46 0 4 -7 29.55 4.93 0 -4 7 39.01 5.57 0 -4 8 381.95 17.69 0 4 -8 367.3 18.19 0 -4 -8 332.84 13.14 0 -4 -9 3.18 1.92 0 4 -9 2.44 1.92 0 -4 9 -1.08 1.14 0 4 -10 24.34 5.09 0 4 10 24.91 4.51 0 -4 -10 19.21 3.55 0 -4 10 21.92 4.83 0 -4 11 242.53 16.41 0 4 11 251.42 14.25 0 -4 12 13 4.27 0 4 12 7.45 2.97 0 -4 -12 11.52 3.43 0 4 13 102.72 9.9 0 -4 13 105.5 11.65 0 -4 -13 90.92 8.48 0 -4 14 97.42 11.66 0 4 14 76.69 8.95 0 -4 -14 82.54 8.25 0 -4 15 300.66 21.36 0 4 15 264.81 17.54 0 4 16 10.51 3.77 0 -4 16 17.35 5.53 0 -4 17 144.89 16.02 0 4 17 109.61 12.2 0 4 18 639.9 30.29 0 -4 18 565.85 32.6 0 4 19 8.47 4 0 -6 0 1.5 1.5 0 -6 1 144.93 10.61 0 -6 -1 133.72 10.61 0 -6 -2 147.17 11.24 0 6 -2 128.68 10.34 0 -6 2 124.88 9.89 0 -6 -3 336.81 17.35 0 -6 3 335.06 15.75 0 6 -3 326.42 17.06 0 -6 3 319.47 15.11 0 -6 4 264.23 14.04 0 -6 -4 244.78 15.04 0 6 -4 260.69 15.9 0 -6 -4 245.38 12.87 0 -6 4 268.5 14.39 0 -6 5 6.02 2.43 0 6 -5 11.65 3.68 0 -6 5 5.26 2.23 0 -6 -5 4.89 1.77 0 -6 -5 5.87 2.34 0 6 -6 108.08 10.92 0 -6 -6 97.45 7.79 0 -6 6 84.95 8.77 0 -6 -6 124.07 11.31 0 -6 6 97.36 8.74 0 -6 7 73.75 7.55 0 6 -7 79.29 9.68 0 -6 7 69.18 8.44 0 -6 -7 79.06 6.93 0 -6 8 30.26 5.77 0 -6 -8 31.06 4.42 0 6 -8 37.4 6.91 0 -6 8 30.34 5.04 0 -6 9 83.22 10 0 -6 10 0.93 1.33 0 -6 11 8.72 3.59 0 -6 12 5.7 2.78 0 -6 13 -0.28 1.78 0 -6 14 3.52 2.99 0 -6 15 15.2 5.58 0 -6 16 212.98 20.12 0 -8 0 246.53 14.12 0 -8 0 251.05 15.89 0 -8 -1 91.75 9.85 0 -8 1 91.4 9.46 0 -8 1 102.97 9.41 0 -8 -2 1.59 1.71 0 -8 2 4.79 2.66 0 -8 2 4.66 2.44 0 -8 3 116.83 10.62 0 -8 -3 123.48 11.84 0 -8 3 114.97 10.35 0 -8 -4 81.09 10.18 0 -8 4 81.68 8.72 0 -8 4 73.31 8.77 0 -8 5 101.92 9.61 0 -8 -5 99.48 11.23 0 -8 5 98.62 10.59 0 -8 6 32.34 5.4 0 -8 -6 26.09 5.67 0 -8 6 36.53 6.85 0 -8 7 41.53 6.28 0 -8 -7 41.54 7.72 0 -8 7 30.71 6.51 0 -8 -8 96.23 11.77 0 -8 8 118.3 10.74 0 -8 8 105.23 12.06 0 -8 -9 2.53 2.4 0 -8 9 3.63 2.57 0 -8 -10 77.83 11.38 0 -8 10 54.07 9.14 0 -8 -11 -4.71 3.96 0 -8 11 2.62 1.94 0 -8 12 20.87 6.41 0 -8 -12 31.48 7.79 -1 1 22 0.97 2.08 -1 1 21 7.31 4.67 -1 -1 21 3.84 4.24 -1 -1 20 5.86 4.12 -1 1 20 10.82 4.56 -1 1 19 22.69 6.66 -1 -1 19 22.64 6.48 -1 -1 18 -1.62 1.74 -1 1 18 0.65 1.99 -1 -1 17 2.29 1.74 -1 1 17 0.81 1.88 -1 1 16 0.61 1.98 -1 -1 16 6.6 3.7 -1 1 15 301.93 18.54 -1 -1 15 309.4 19.6 -1 1 14 409.84 20.58 -1 -1 14 417.16 21.98 1 -1 -13 28.89 4.96 -1 1 13 28.93 5.4 -1 -1 13 34.82 6.12 -1 -1 12 -0.95 1.05 -1 1 12 0.88 1.21 1 -1 -12 -0.32 1.3 1 1 -12 2.89 2.34 1 -1 -11 106.84 8.7 1 1 -11 126.26 9.78 -1 -1 11 109.32 9.67 1 1 -11 118.85 9.36 -1 1 11 119.4 9.6 -1 1 10 162.61 10.48 1 1 -10 166.04 10.65 -1 -1 10 176.14 11.62 1 1 -10 191.02 11.11 -1 1 9 24.99 3.85 1 -1 -9 27.17 4.16 -1 -1 9 26.5 4.23 -1 1 8 29.51 4.05 -1 -1 8 26.38 4.16 1 -1 -8 25.13 3.66 -1 1 7 64.55 5.43 1 -1 -7 69.52 5.56 -1 -1 7 59.75 5.61 -1 -1 6 735.4 18.41 1 -1 -6 743.97 17.07 -1 1 6 758.8 17.43 1 -1 -5 523.76 13.06 -1 -1 5 511.84 13.97 -1 1 5 527.14 13.29 -1 -1 4 806.36 16.06 1 1 -4 830.89 14.49 1 -1 -4 830.71 14.75 -1 1 4 846.98 15.28 1 1 -3 53.23 3.24 -1 1 3 56.39 3.54 -1 -1 3 46.15 3.35 1 -1 -3 50.11 3.36 1 1 -2 1107.83 12.71 1 1 -2 1148.47 13.83 -1 -1 2 1173.76 12.31 -1 1 2 1137.22 14.46 1 -1 -2 1131.4 14.17 -1 -1 2 1149.24 14.4 1 1 -1 2032.46 14.44 -1 -1 1 1983.79 15.03 -1 -1 1 1979.58 13.42 -1 1 0 456.68 9.16 1 -1 0 478.01 9.42 -1 1 -1 1634.53 18.3 1 -1 1 1654.58 17.94 1 1 2 865.24 9.42 -1 1 -2 839.8 14.11 1 -1 2 845.42 13.53 -1 -1 -2 858.04 9.04 -1 -1 -3 1744.68 16.52 1 -1 3 1747.04 20.83 1 -1 3 1788.66 20.95 1 1 3 1810.36 16.98 -1 1 -3 1761.56 21.83 1 -1 4 305.66 9.75 1 1 4 315.63 8.48 -1 1 -4 303.68 9.9 -1 -1 -4 317.54 8.33 1 -1 4 313.16 9.57 -1 -1 -5 50.72 3.74 -1 1 -5 55.81 4.66 1 -1 5 50.91 4.45 1 1 5 52.4 3.88 1 1 6 9.25 1.88 -1 -1 -6 9.12 1.87 1 -1 6 6.42 2 -1 1 -6 9.02 2.06 -1 1 -6 6 1.56 1 -1 7 0.21 0.78 -1 1 -7 0.74 0.86 1 1 7 1.65 0.99 -1 1 -7 0.75 0.65 -1 -1 -7 0.92 0.99 1 -1 8 12.73 2.87 1 1 8 18.06 3.09 -1 -1 -8 15.82 2.75 1 1 9 198.65 10.82 -1 -1 -9 188.75 10.07 1 -1 9 204.55 11.7 -1 1 -10 320.64 14.68 -1 1 -10 309.06 14.91 1 -1 10 323 15.77 1 1 10 292.95 13.93 -1 -1 -11 313.61 14.4 1 1 11 332.51 15.58 -1 1 -11 360.01 16.94 -1 1 -11 309.48 15.22 1 -1 11 324.19 16.63 1 -1 12 14.78 4.13 -1 1 -12 8.87 2.87 1 1 12 13.85 3.28 -1 -1 -12 5.77 2.19 1 -1 13 3.82 2.81 -1 -1 -13 2.38 1.53 1 1 13 0.48 1.32 1 1 14 26.59 5.35 1 -1 14 24.32 5.43 1 1 15 67.5 8.67 1 -1 15 72.1 9.6 1 -1 16 0.52 2.12 1 1 16 7.54 3.25 1 -1 17 25.89 6.51 1 1 17 32.38 6.89 1 -1 18 22.23 6.2 1 1 18 25.67 6.09 1 -1 19 80.79 11.57 1 1 19 68.55 10.4 1 -1 20 46.64 9.16 1 1 20 46.77 9.11 1 -1 21 74.91 12.09 1 1 21 73.07 11.81 1 1 22 12.97 5.51 -1 3 21 -1.61 2.42 -1 3 20 47.46 9.21 -1 3 19 14.98 5.46 -1 -3 19 14.82 6.12 -1 3 18 138.37 14.65 -1 -3 18 176 17.86 -1 3 17 64.75 9.46 -1 -3 17 78.99 11.78 -1 -3 16 23.7 6.73 -1 3 16 20.72 5.14 -1 -3 15 53.42 9.05 -1 3 15 51.69 7.64 1 -3 -14 365.91 18.13 -1 -3 14 384.16 22.2 -1 3 14 380.08 20.1 1 -3 -13 98.62 9.12 -1 -3 13 96.65 10.8 -1 3 13 89.52 9.3 1 -3 -12 29.14 4.69 -1 3 12 38.19 5.64 -1 -3 12 31.28 6.15 -1 3 11 35 5.31 -1 -3 11 28.58 5.38 1 3 -11 26.62 5.05 1 3 -10 460.2 19.79 -1 -3 10 479.32 20.69 -1 3 10 457.86 18.28 -1 -3 9 286.89 15.52 -1 3 9 294.89 13.93 1 -3 -9 282.42 12.92 1 3 -9 289.54 14.98 -1 3 8 -1.36 1.23 1 -3 -8 0.42 0.87 -1 -3 8 -0.22 1.06 1 3 -8 1.15 1.97 1 3 -7 21.51 3.71 -1 -3 7 19.48 3.62 1 -3 -7 21.56 3.17 -1 3 7 15.19 2.85 1 -3 -6 10.38 2.23 -1 -3 6 11.44 2.27 1 3 -6 11.21 2.54 -1 -3 6 10.86 2.53 1 3 -5 307.85 12.83 -1 -3 5 273.29 11.94 -1 -3 5 301.1 11.12 1 -3 -5 285.23 10.73 -1 -3 4 1365.04 22.55 1 -3 -4 1305.39 22.53 -1 -3 4 1343.8 24.41 1 3 -4 1309.89 25.25 1 3 -3 2.21 1.17 -1 -3 3 1.79 1.2 -1 -3 3 4.96 1.66 1 -3 -2 258.13 11.13 -1 -3 2 252.36 9.51 1 3 -2 229.55 9.61 -1 -3 1 837.16 17.16 1 3 -1 852.49 17.39 1 -3 -1 845.01 19.89 1 -3 0 96.37 6.69 -1 -3 0 106.92 6.14 -1 3 0 107.08 6.86 -1 -3 -1 675.88 15.72 -1 3 -1 697.28 18.21 1 -3 1 672.47 17.64 -1 3 -2 162.43 9.15 1 -3 2 149.9 8.32 -1 3 -3 372.86 14.31 1 -3 3 359.73 12.91 -1 -3 -3 351.15 9.91 1 -3 4 826.14 20.01 -1 3 -4 773.4 21.25 -1 -3 -4 794.38 14.9 1 -3 4 831.23 19.85 -1 3 -5 394.58 15.84 -1 -3 -5 393.92 11.06 1 -3 5 397.06 14.45 1 -3 5 383.32 13.83 1 3 6 850.99 18.42 1 -3 6 859.52 22.45 -1 -3 -6 867.13 17.28 1 -3 6 866.41 21.46 -1 3 -6 866.48 24.39 -1 3 -7 -0.43 1.57 1 -3 7 1.17 1.3 1 3 7 -0.27 0.76 -1 -3 -7 0.32 0.98 1 -3 7 0.95 1.27 1 3 8 127.92 8.2 -1 3 -8 125.48 10.08 -1 -3 -8 117.49 7.3 1 -3 8 122.45 9.69 -1 3 -9 203.77 13.35 1 -3 9 189.25 12.61 1 3 9 192.27 10.59 -1 -3 -9 190.63 9.9 -1 3 -10 12.48 3.55 1 -3 10 11.56 3.48 -1 -3 -10 11.74 2.77 1 3 10 10.83 2.75 1 -3 11 1.81 2.27 1 3 11 0.75 1 1 3 12 113.88 9.77 -1 -3 -12 107.39 8.68 1 -3 12 101.46 10.76 1 -3 13 103.23 11.2 1 3 13 97.98 9.41 -1 -3 -13 95.5 8.52 -1 -3 -14 41.71 5.93 1 -3 14 35.17 6.87 1 3 14 34.27 5.98 1 3 15 183.04 14.25 1 -3 15 145.9 14.58 1 3 16 25.77 5.83 1 -3 16 24.59 6.76 1 3 17 20.78 5.32 1 -3 17 16.48 5.31 1 3 18 4.91 3.11 1 -3 18 5.37 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6 73.6 8.05 10 6 -6 59.49 4.29 -10 -6 5 132.91 10.05 10 -6 -5 149.85 15.13 10 -6 -4 1.82 2.89 -10 -6 4 0.85 0.82 10 -6 -3 84.01 10.98 -10 -6 3 102.38 7.49 10 -6 -2 15.74 4.19 -10 -6 2 24.59 3.31 -10 -6 1 89.5 5.46 10 -6 -1 93.88 11.6 -10 -6 0 453.43 9.31 10 -6 0 435.94 25.02 10 -6 1 372.33 22.95 10 -6 2 312.69 20.77 10 -6 3 11.26 4.03 -10 -6 -3 12.21 1.67 -10 -6 -3 11.66 1.4 10 -6 4 281.36 19.75 -10 -6 -4 268.12 10.06 -10 -6 -4 269.97 8.57 -10 -6 -5 91.26 5.71 -10 -6 -5 100.76 7.05 10 -6 5 72.69 10.17 10 -6 6 56.93 9.04 10 -6 7 58.9 8.76 10 -6 8 6.63 3.1 10 -6 8 6.22 2.6 10 -6 9 134.64 13.66 10 -6 9 132.17 13.63 10 -6 10 0.36 3 10 -6 10 2.12 2.37 10 -6 11 6.37 3.48 10 -6 11 6.65 3.73 10 -6 12 11.13 4.39 10 -6 12 10.63 4.8 10 -6 13 -1.21 2.72 -10 -8 14 -0.77 2.45 -10 -8 13 86.42 12.84 10 -8 -13 33.87 8.91 10 -8 -12 2.53 3.28 -10 -8 12 -2.22 3.67 10 -8 -11 85.69 13.83 -10 -8 11 111.19 13.09 10 -8 -10 65.87 11.94 -10 -8 10 71.68 10.41 10 -8 -9 64.91 11.8 -10 -8 9 57.6 8.79 -10 -8 8 13.95 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473.29 6.91 11 -3 1 474.52 21.86 11 -3 2 33.31 5.51 -11 -3 -2 27.85 3 -11 3 -2 20.36 5 -11 -3 -3 0.54 0.78 11 -3 3 0.47 1.28 -11 3 -3 0.34 1.75 -11 -3 -4 254 10.85 11 -3 4 251.91 15.93 -11 3 -4 260.27 17.56 -11 3 -5 7.06 3.39 -11 -3 -5 4.24 1.6 11 -3 5 2.78 2 11 3 6 78.21 3.57 -11 -3 -6 80.01 7.04 11 -3 6 72.04 8.61 11 3 7 3.42 1.18 11 -3 7 4.31 2.57 11 3 8 856.67 16.59 11 -3 8 895.78 30.69 -11 -3 -8 884.84 25.75 -11 -3 -9 80.97 8.36 11 3 9 84.12 5.86 11 -3 9 76.13 9.07 11 -3 9 78.15 8.86 11 3 10 37.86 4.43 11 -3 10 37.44 6.54 -11 -3 -10 33.44 5.61 11 -3 10 32.11 5.94 11 -3 11 18.61 4.55 11 3 11 22.82 3.64 11 -3 11 19.53 4.97 11 3 12 13.9 3.13 11 -3 12 19.9 5.15 11 3 13 86.76 8.03 11 -3 13 72.31 10.01 11 3 14 24.1 4.65 11 -3 14 18.66 5.69 11 -3 15 1.37 2.36 11 -3 16 30.77 7.57 11 -3 17 4.34 2.06 -11 -5 18 1.7 2.68 -11 -5 17 117.2 15.02 -11 -5 16 9.07 4.46 -11 -5 15 16.52 5.69 -11 -5 14 123.89 13.86 -11 -5 13 12.96 4.36 -11 -5 12 6.05 3.47 11 5 -12 6.52 2.61 -11 -5 11 33.87 6.35 11 5 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129.73 13.61 11 -5 12 28.78 6.72 11 -5 12 24.45 6.3 11 -5 13 22.65 6.31 11 -5 14 2.01 3.16 -11 -7 15 27.29 7.22 11 -7 -15 24.35 7.56 11 -7 -14 -2.27 2.82 -11 -7 14 3.94 3.03 -11 -7 13 11.76 4.75 11 -7 -13 17.68 6.26 -11 -7 12 1.72 2.32 11 -7 -12 -0.44 2.47 -11 -7 11 86.68 11.16 11 -7 -11 78.35 12.73 -11 -7 10 3.47 2.35 11 -7 -10 5.3 4.4 11 -7 -9 20.66 6.58 -11 -7 9 16.13 4.65 11 -7 -8 58.06 10.81 -11 -7 8 83.6 9.74 -11 -7 7 2.6 2.59 11 -7 -7 1.15 2.12 -11 -7 6 5.45 2.1 11 -7 -6 4.51 2.7 -11 -7 5 56.9 6.82 11 -7 -5 44.97 9.31 -11 -7 4 217.2 12.17 11 -7 -4 231.04 20.31 11 -7 -3 0.66 2.92 -11 -7 3 0.77 0.74 -11 -7 2 34.98 4.02 11 -7 -2 38.4 8.36 11 -7 -1 11.52 4.36 11 -7 0 20.81 5.84 11 -7 1 28.1 6.61 11 -7 2 23.86 6.64 11 -7 3 10.23 4.06 11 -7 4 88.83 11.91 11 -7 5 91.56 12.06 11 -7 6 10.29 4.55 11 -7 7 0.55 1.44 11 -7 8 -0.08 2.4 11 -7 8 -1.48 3.02 11 -7 9 67.17 10.32 11 -7 9 53.02 9.26 11 -7 10 23.79 6.41 11 -7 10 26 6.84 11 -7 11 5.94 3.55 11 -9 -10 107.32 16.39 11 -9 -9 1.96 3.79 11 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