#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:43:31 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225896 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515771.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_4515771 loop_ _publ_author_name 'Zhang, Bo-Sheng' 'Li, Yuke' 'An, Yang' 'Zhang, Zhe' 'Liu, Ce' 'Wang, Xin-Gang' 'Liang, Yong-Min' _publ_section_title ; Carboxylate Ligand-Exchanged Amination/C(sp3)--H Arylation Reaction via Pd/Norbornene Cooperative Catalysis ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11827 _journal_paper_doi 10.1021/acscatal.8b04163 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C18 H26 N2 O3' _chemical_formula_sum 'C18 H26 N2 O3' _chemical_formula_weight 318.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2018-09-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90.00 _cell_angle_beta 99.380(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.2992(11) _cell_length_b 15.1980(11) _cell_length_c 12.6751(8) _cell_measurement_reflns_used 1387 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.9690 _cell_measurement_theta_min 3.8690 _cell_volume 1767.4(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.0733 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -19.00 14.00 1.5000 5.0000 omega____ theta____ kappa____ phi______ frames - -19.5836 -99.0000 120.0000 22 #__ type_ start__ end____ width___ exp.time_ 2 omega -16.00 20.00 1.5000 5.0000 omega____ theta____ kappa____ phi______ frames - -19.5836 -99.0000 -30.0000 24 #__ type_ start__ end____ width___ exp.time_ 3 omega 51.00 78.00 1.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 22.9430 -178.0000 -90.0000 18 #__ type_ start__ end____ width___ exp.time_ 4 omega -7.00 66.50 1.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 22.9430 -99.0000 -120.0000 49 #__ type_ start__ end____ width___ exp.time_ 5 omega 7.00 82.00 1.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 22.9430 38.0000 0.0000 50 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0701751000 _diffrn_orient_matrix_UB_12 -0.0133267000 _diffrn_orient_matrix_UB_13 0.0255998000 _diffrn_orient_matrix_UB_21 -0.0093619000 _diffrn_orient_matrix_UB_22 -0.0410177000 _diffrn_orient_matrix_UB_23 -0.0268862000 _diffrn_orient_matrix_UB_31 0.0310858000 _diffrn_orient_matrix_UB_32 0.0177997000 _diffrn_orient_matrix_UB_33 -0.0428908000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0570 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6801 _diffrn_reflns_theta_full 26.02 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_min 3.48 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.69663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) 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 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.428 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.232 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 3477 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0647 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+0.1545P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1416 _refine_ls_wR_factor_ref 0.1775 _reflns_number_gt 2133 _reflns_number_total 3477 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL zhangbsh_0903 in P21/n #14 REM reset to P21/n #14 CELL 0.71073 9.299248 15.197996 12.675129 90 99.3798 90 ZERR 4 0.001082 0.001092 0.000845 0 0.0089 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 72 104 8 12 L.S. 10 PLAN 20 BOND $H HTAb CONF fmap 2 acta SHEL 999 0.81 REM REM REM WGHT 0.073400 0.154500 FVAR 5.69870 N1 3 0.785151 0.016194 0.003574 11.00000 0.06134 0.03355 = 0.03849 0.00216 0.00992 -0.00108 O2 4 0.804453 -0.099850 -0.106891 11.00000 0.09810 0.04319 = 0.05627 -0.00603 0.02984 -0.00252 O3 4 0.760041 -0.120931 0.060795 11.00000 0.08252 0.03603 = 0.05987 0.00555 0.02388 0.00144 N4 3 0.766420 0.323984 -0.031800 11.00000 0.05218 0.03390 = 0.06230 0.00723 0.00484 0.00233 C5 1 0.775723 0.083507 -0.074265 11.00000 0.04952 0.03840 = 0.03664 0.00456 0.00399 -0.00277 C6 1 0.783586 0.164805 -0.025442 11.00000 0.04732 0.04027 = 0.03823 0.00104 0.00383 -0.00120 C7 1 0.785047 -0.070364 -0.021793 11.00000 0.05511 0.03806 = 0.04689 0.00273 0.01252 -0.00163 C8 1 0.767513 0.055601 0.109741 11.00000 0.05228 0.04085 = 0.03325 -0.00187 0.00580 -0.00296 C9 1 0.766203 0.242051 -0.085317 11.00000 0.05132 0.03698 = 0.04933 0.00660 0.00416 -0.00240 C10 1 0.804832 0.153014 0.093361 11.00000 0.06469 0.03722 = 0.04357 -0.00082 0.00628 -0.00357 AFIX 23 H10A 2 0.740376 0.191487 0.125046 11.00000 -1.20000 H10B 2 0.904762 0.165633 0.125192 11.00000 -1.20000 AFIX 0 C11 1 0.751448 0.075429 -0.184653 11.00000 0.07280 0.05122 = 0.03996 -0.00287 0.00596 -0.00618 AFIX 43 H11 2 0.746189 0.020598 -0.217632 11.00000 -1.20000 AFIX 0 C12 1 0.735388 0.152294 -0.243644 11.00000 0.08819 0.06569 = 0.03771 0.00912 0.00176 -0.00533 AFIX 43 H12 2 0.719470 0.148583 -0.317872 11.00000 -1.20000 AFIX 0 C13 1 0.874063 0.017675 0.203196 11.00000 0.06418 0.05757 = 0.04767 0.00717 0.00116 -0.00175 AFIX 137 H13A 2 0.846409 -0.041616 0.216669 11.00000 -1.50000 H13B 2 0.871985 0.052841 0.265846 11.00000 -1.50000 H13C 2 0.970742 0.017972 0.185792 11.00000 -1.50000 AFIX 0 C14 1 0.609935 0.045062 0.127303 11.00000 0.05840 0.05338 = 0.05727 -0.00448 0.01378 -0.00289 AFIX 137 H14A 2 0.545990 0.072511 0.069550 11.00000 -1.50000 H14B 2 0.597956 0.072417 0.193586 11.00000 -1.50000 H14C 2 0.586729 -0.016373 0.129820 11.00000 -1.50000 AFIX 0 O15 4 0.818165 0.501053 0.035478 11.00000 0.07783 0.04172 = 0.14322 -0.01093 0.02358 0.00248 C16 1 0.768062 -0.215734 0.047470 11.00000 0.08673 0.03030 = 0.08985 0.00969 0.03634 0.00954 AFIX 13 H16 2 0.838515 -0.228897 -0.000034 11.00000 -1.20000 AFIX 0 C17 1 0.742067 0.234019 -0.196684 11.00000 0.07448 0.05113 = 0.04988 0.01382 0.00022 -0.00266 AFIX 43 H17 2 0.730478 0.284215 -0.239188 11.00000 -1.20000 AFIX 0 C18 1 0.905067 0.351297 0.030660 11.00000 0.05334 0.04040 = 0.07730 -0.00679 0.01058 -0.00316 AFIX 23 H18A 2 0.973258 0.365744 -0.017044 11.00000 -1.20000 H18B 2 0.945881 0.303319 0.076457 11.00000 -1.20000 AFIX 0 C19 1 0.703482 0.398064 -0.095662 11.00000 0.08434 0.04666 = 0.09740 0.02061 -0.00302 0.00847 AFIX 23 H19A 2 0.609699 0.381396 -0.136008 11.00000 -1.20000 H19B 2 0.766826 0.414844 -0.145962 11.00000 -1.20000 AFIX 0 C20 1 0.883243 0.429768 0.097589 11.00000 0.07657 0.05072 = 0.10574 -0.02005 0.01219 0.00284 AFIX 23 H20A 2 0.821887 0.413356 0.149386 11.00000 -1.20000 H20B 2 0.976783 0.448323 0.136650 11.00000 -1.20000 AFIX 0 C21 1 0.684813 0.473807 -0.024644 11.00000 0.07639 0.04505 = 0.14087 0.01516 0.01790 0.01626 C22 1 0.621785 -0.249385 -0.002146 11.00000 0.10520 0.05175 = 0.20906 -0.02019 0.03789 -0.01624 AFIX 137 H22A 2 0.552420 -0.237376 0.044405 11.00000 -1.50000 H22B 2 0.627215 -0.311715 -0.013140 11.00000 -1.50000 H22C 2 0.591654 -0.220706 -0.069609 11.00000 -1.50000 AFIX 0 C23 1 0.824226 -0.250561 0.155784 11.00000 0.19398 0.07351 = 0.10791 0.04433 0.03847 0.03901 AFIX 137 H23A 2 0.915355 -0.222711 0.183115 11.00000 -1.50000 H23B 2 0.838486 -0.312952 0.151715 11.00000 -1.50000 H23C 2 0.755156 -0.238540 0.202561 11.00000 -1.50000 AFIX 0 H21A 2 0.617366 0.453990 0.026905 11.00000 0.11152 H21B 2 0.651408 0.521611 -0.067872 11.00000 0.11123 HKLF 4 REM zhangbsh_0903 in P21/n #14 REM R1 = 0.0647 for 2133 Fo > 4sig(Fo) and 0.1051 for all 3477 data REM 220 parameters refined using 0 restraints END WGHT 0.0704 0.1508 REM Highest difference peak 0.428, deepest hole -0.489, 1-sigma level 0.232 Q1 1 0.9707 -0.1382 -0.0325 11.00000 0.05 0.43 Q2 1 1.0048 0.4617 0.0042 11.00000 0.05 0.43 Q3 1 0.9971 0.4763 0.0842 11.00000 0.05 0.42 Q4 1 0.9716 0.3573 -0.0883 11.00000 0.05 0.42 Q5 1 1.0021 -0.2175 -0.0053 11.00000 0.05 0.42 Q6 1 0.9800 0.1024 -0.0467 11.00000 0.05 0.41 Q7 1 0.9868 -0.0852 -0.0422 11.00000 0.05 0.41 Q8 1 1.0005 0.2833 0.0197 11.00000 0.05 0.41 Q9 1 0.9969 0.0344 0.0806 11.00000 0.05 0.40 Q10 1 0.9969 0.3557 -0.1336 11.00000 0.05 0.40 Q11 1 0.9804 0.1613 0.0998 11.00000 0.05 0.40 Q12 1 1.0070 -0.2244 0.1218 11.00000 0.05 0.40 Q13 1 1.0030 -0.0779 0.1308 11.00000 0.05 0.40 Q14 1 0.9919 0.4181 -0.0614 11.00000 0.05 0.40 Q15 1 0.9980 -0.0495 -0.0197 11.00000 0.05 0.39 Q16 1 0.9965 -0.1415 0.0951 11.00000 0.05 0.39 Q17 1 1.0035 0.1140 0.0981 11.00000 0.05 0.39 Q18 1 1.0031 0.2737 0.1123 11.00000 0.05 0.39 Q19 1 1.0000 -0.0385 0.0643 11.00000 0.05 0.39 Q20 1 1.0206 -0.1160 0.1571 11.00000 0.05 0.39 REM The information below was added by Olex2. REM REM R1 = 0.0647 for 2133 Fo > 4sig(Fo) and 0.1051 for all 7782 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.43, deepest hole -0.49 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1051 REM R1_gt = 0.0647 REM wR_ref = 0.1775 REM GOOF = 1.053 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 7782 REM Reflections_gt = 2133 REM Parameters = n/a REM Hole = -0.49 REM Peak = 0.43 REM Flack = n/a ; _cod_data_source_file cs8b04163_si_002.cif _cod_data_source_block zhangbsh_0903 _cod_database_code 4515771 _reflns_odcompleteness_completeness 99.63 _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 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: C10(H10a,H10b), C18(H18a,H18b), C19(H19a,H19b), C20(H20a,H20b) 2.c Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C17(H17) 2.d Idealised Me refined as rotating group: C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C22(H22a,H22b,H22c), C23(H23a,H23b, H23c) ; _olex2_date_sample_data_collection 2018-09-04 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 '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_calc_flag _atom_site_refinement_flags_posn N1 N 0.7852(2) 0.01619(12) 0.00357(12) 0.0443(5) Uani 1 d . O2 O 0.8045(2) -0.09985(11) -0.10689(13) 0.0639(5) Uani 1 d . O3 O 0.7600(2) -0.12093(10) 0.06079(12) 0.0581(5) Uani 1 d . N4 N 0.7664(2) 0.32398(12) -0.03180(15) 0.0500(5) Uani 1 d . C5 C 0.7757(2) 0.08351(14) -0.07426(15) 0.0419(5) Uani 1 d . C6 C 0.7836(2) 0.16480(15) -0.02544(16) 0.0423(5) Uani 1 d . C7 C 0.7850(3) -0.07036(15) -0.02179(17) 0.0462(6) Uani 1 d . C8 C 0.7675(3) 0.05560(15) 0.10974(15) 0.0423(5) Uani 1 d . C9 C 0.7662(3) 0.24205(15) -0.08532(17) 0.0463(6) Uani 1 d . C10 C 0.8048(3) 0.15301(14) 0.09336(16) 0.0488(6) Uani 1 d . H10A H 0.7404 0.1915 0.1250 0.059 Uiso 1 calc R H10B H 0.9048 0.1656 0.1252 0.059 Uiso 1 calc R C11 C 0.7514(3) 0.07543(17) -0.18465(16) 0.0550(7) Uani 1 d . H11 H 0.7462 0.0206 -0.2176 0.066 Uiso 1 calc R C12 C 0.7354(3) 0.15229(17) -0.24364(18) 0.0648(8) Uani 1 d . H12 H 0.7195 0.1486 -0.3179 0.078 Uiso 1 calc R C13 C 0.8741(3) 0.01768(17) 0.20320(16) 0.0574(7) Uani 1 d . H13A H 0.8464 -0.0416 0.2167 0.086 Uiso 1 calc GR H13B H 0.8720 0.0528 0.2658 0.086 Uiso 1 calc GR H13C H 0.9707 0.0180 0.1858 0.086 Uiso 1 calc GR C14 C 0.6099(3) 0.04506(17) 0.12730(19) 0.0559(7) Uani 1 d . H14A H 0.5460 0.0725 0.0696 0.084 Uiso 1 calc GR H14B H 0.5980 0.0724 0.1936 0.084 Uiso 1 calc GR H14C H 0.5867 -0.0164 0.1298 0.084 Uiso 1 calc GR O15 O 0.8182(3) 0.50105(12) 0.0355(2) 0.0870(7) Uani 1 d . C16 C 0.7681(3) -0.21573(16) 0.0475(2) 0.0665(8) Uani 1 d . H16 H 0.8385 -0.2289 0.0000 0.080 Uiso 1 calc R C17 C 0.7421(3) 0.23402(17) -0.19668(18) 0.0596(7) Uani 1 d . H17 H 0.7305 0.2842 -0.2392 0.072 Uiso 1 calc R C18 C 0.9051(3) 0.35130(16) 0.0307(2) 0.0570(7) Uani 1 d . H18A H 0.9733 0.3657 -0.0170 0.068 Uiso 1 calc R H18B H 0.9459 0.3033 0.0765 0.068 Uiso 1 calc R C19 C 0.7035(4) 0.39806(17) -0.0957(2) 0.0781(9) Uani 1 d . H19A H 0.6097 0.3814 -0.1360 0.094 Uiso 1 calc R H19B H 0.7668 0.4148 -0.1460 0.094 Uiso 1 calc R C20 C 0.8832(4) 0.42977(19) 0.0976(3) 0.0780(9) Uani 1 d . H20A H 0.8219 0.4134 0.1494 0.094 Uiso 1 calc R H20B H 0.9768 0.4483 0.1366 0.094 Uiso 1 calc R C21 C 0.6848(4) 0.4738(2) -0.0246(4) 0.0874(11) Uani 1 d . C22 C 0.6218(4) -0.2494(2) -0.0021(4) 0.1206(15) Uani 1 d . H22A H 0.5524 -0.2374 0.0444 0.181 Uiso 1 calc GR H22B H 0.6272 -0.3117 -0.0131 0.181 Uiso 1 calc GR H22C H 0.5917 -0.2207 -0.0696 0.181 Uiso 1 calc GR C23 C 0.8242(5) -0.2506(2) 0.1558(3) 0.1236(16) Uani 1 d . H23A H 0.9154 -0.2227 0.1831 0.185 Uiso 1 calc GR H23B H 0.8385 -0.3130 0.1517 0.185 Uiso 1 calc GR H23C H 0.7552 -0.2385 0.2026 0.185 Uiso 1 calc GR H21A H 0.617(4) 0.454(2) 0.027(3) 0.112(12) Uiso 1 d . H21B H 0.651(4) 0.522(2) -0.068(3) 0.111(12) Uiso 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 N1 0.0613(13) 0.0335(10) 0.0385(10) 0.0022(8) 0.0099(9) -0.0011(9) O2 0.0981(15) 0.0432(10) 0.0563(10) -0.0060(8) 0.0298(9) -0.0025(10) O3 0.0825(13) 0.0360(9) 0.0599(10) 0.0056(7) 0.0239(9) 0.0014(9) N4 0.0522(13) 0.0339(11) 0.0623(11) 0.0072(9) 0.0048(10) 0.0023(9) C5 0.0495(14) 0.0384(12) 0.0366(11) 0.0046(9) 0.0040(9) -0.0028(11) C6 0.0473(14) 0.0403(13) 0.0382(11) 0.0010(9) 0.0038(9) -0.0012(11) C7 0.0551(15) 0.0381(13) 0.0469(13) 0.0027(10) 0.0125(10) -0.0016(11) C8 0.0523(14) 0.0409(12) 0.0332(10) -0.0019(9) 0.0058(9) -0.0030(11) C9 0.0513(14) 0.0370(13) 0.0493(12) 0.0066(10) 0.0042(10) -0.0024(11) C10 0.0647(17) 0.0372(13) 0.0436(12) -0.0008(10) 0.0063(11) -0.0036(12) C11 0.0728(18) 0.0512(15) 0.0400(12) -0.0029(11) 0.0060(11) -0.0062(14) C12 0.088(2) 0.0657(18) 0.0377(12) 0.0091(12) 0.0018(12) -0.0053(16) C13 0.0642(17) 0.0576(16) 0.0477(13) 0.0072(11) 0.0012(12) -0.0017(14) C14 0.0584(16) 0.0534(15) 0.0573(14) -0.0045(12) 0.0138(12) -0.0029(13) O15 0.0778(16) 0.0417(12) 0.1432(19) -0.0109(12) 0.0236(14) 0.0025(11) C16 0.087(2) 0.0303(13) 0.0898(19) 0.0097(13) 0.0363(16) 0.0095(14) C17 0.0745(19) 0.0511(15) 0.0499(14) 0.0138(12) 0.0002(12) -0.0027(14) C18 0.0533(16) 0.0404(14) 0.0773(16) -0.0068(12) 0.0106(13) -0.0032(13) C19 0.084(2) 0.0467(17) 0.097(2) 0.0206(15) -0.0030(17) 0.0085(16) C20 0.077(2) 0.0507(17) 0.106(2) -0.0200(16) 0.0122(17) 0.0028(16) C21 0.076(2) 0.0450(18) 0.141(3) 0.015(2) 0.018(2) 0.0163(18) C22 0.105(3) 0.052(2) 0.209(4) -0.020(2) 0.038(3) -0.016(2) C23 0.194(5) 0.074(2) 0.108(3) 0.044(2) 0.038(3) 0.039(3) 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 C5 N1 C8 109.41(17) C7 N1 C5 122.66(17) C7 N1 C8 127.05(17) C7 O3 C16 117.12(18) C9 N4 C18 116.21(19) C9 N4 C19 116.4(2) C19 N4 C18 108.8(2) C6 C5 N1 110.03(17) C6 C5 C11 121.4(2) C11 C5 N1 128.4(2) C5 C6 C9 121.19(19) C5 C6 C10 109.44(18) C9 C6 C10 129.3(2) O2 C7 N1 125.3(2) O2 C7 O3 123.4(2) O3 C7 N1 111.27(18) N1 C8 C10 101.64(16) N1 C8 C13 113.04(18) N1 C8 C14 109.61(17) C13 C8 C10 109.56(19) C14 C8 C10 111.3(2) C14 C8 C13 111.35(19) C6 C9 N4 119.24(19) C6 C9 C17 117.5(2) C17 C9 N4 123.2(2) C6 C10 C8 104.75(17) C6 C10 H10A 110.8 C6 C10 H10B 110.8 C8 C10 H10A 110.8 C8 C10 H10B 110.8 H10A C10 H10B 108.9 C5 C11 H11 121.4 C12 C11 C5 117.2(2) C12 C11 H11 121.4 C11 C12 H12 118.8 C17 C12 C11 122.4(2) C17 C12 H12 118.8 C8 C13 H13A 109.5 C8 C13 H13B 109.5 C8 C13 H13C 109.5 H13A C13 H13B 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C8 C14 H14A 109.5 C8 C14 H14B 109.5 C8 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C21 O15 C20 109.6(2) O3 C16 H16 109.0 O3 C16 C22 109.1(2) O3 C16 C23 105.2(2) C22 C16 H16 109.0 C23 C16 H16 109.0 C23 C16 C22 115.2(3) C9 C17 H17 119.8 C12 C17 C9 120.3(2) C12 C17 H17 119.8 N4 C18 H18A 109.6 N4 C18 H18B 109.6 N4 C18 C20 110.2(2) H18A C18 H18B 108.1 C20 C18 H18A 109.6 C20 C18 H18B 109.6 N4 C19 H19A 109.7 N4 C19 H19B 109.7 N4 C19 C21 109.8(3) H19A C19 H19B 108.2 C21 C19 H19A 109.7 C21 C19 H19B 109.7 O15 C20 C18 112.3(2) O15 C20 H20A 109.1 O15 C20 H20B 109.1 C18 C20 H20A 109.1 C18 C20 H20B 109.1 H20A C20 H20B 107.9 O15 C21 C19 112.1(3) O15 C21 H21A 108.6(19) O15 C21 H21B 106(2) C19 C21 H21A 108(2) C19 C21 H21B 108(2) H21A C21 H21B 115(3) C16 C22 H22A 109.5 C16 C22 H22B 109.5 C16 C22 H22C 109.5 H22A C22 H22B 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C16 C23 H23A 109.5 C16 C23 H23B 109.5 C16 C23 H23C 109.5 H23A C23 H23B 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C5 1.414(3) N1 C7 1.354(3) N1 C8 1.506(3) O2 C7 1.208(2) O3 C7 1.349(3) O3 C16 1.454(3) N4 C9 1.418(3) N4 C18 1.459(3) N4 C19 1.453(3) C5 C6 1.378(3) C5 C11 1.386(3) C6 C9 1.393(3) C6 C10 1.497(3) C8 C10 1.542(3) C8 C13 1.528(3) C8 C14 1.526(3) C9 C17 1.398(3) C10 H10A 0.9700 C10 H10B 0.9700 C11 H11 0.9300 C11 C12 1.382(3) C12 H12 0.9300 C12 C17 1.374(3) C13 H13A 0.9600 C13 H13B 0.9600 C13 H13C 0.9600 C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 O15 C20 1.416(3) O15 C21 1.408(4) C16 H16 0.9800 C16 C22 1.493(4) C16 C23 1.485(4) C17 H17 0.9300 C18 H18A 0.9700 C18 H18B 0.9700 C18 C20 1.496(3) C19 H19A 0.9700 C19 H19B 0.9700 C19 C21 1.489(4) C20 H20A 0.9700 C20 H20B 0.9700 C21 H21A 1.02(4) C21 H21B 0.93(4) C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C23 H23A 0.9600 C23 H23B 0.9600 C23 H23C 0.9600 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 N1 C5 C6 C9 -175.3(2) N1 C5 C6 C10 2.0(3) N1 C5 C11 C12 175.0(2) N1 C8 C10 C6 20.6(2) N4 C9 C17 C12 -176.5(2) N4 C18 C20 O15 -56.8(3) N4 C19 C21 O15 59.7(4) C5 N1 C7 O2 14.6(4) C5 N1 C7 O3 -165.31(19) C5 N1 C8 C10 -20.4(2) C5 N1 C8 C13 -137.7(2) C5 N1 C8 C14 97.4(2) C5 C6 C9 N4 176.2(2) C5 C6 C9 C17 -0.7(4) C5 C6 C10 C8 -14.9(3) C5 C11 C12 C17 -0.3(4) C6 C5 C11 C12 0.0(4) C6 C9 C17 C12 0.3(4) C7 N1 C5 C6 -177.8(2) C7 N1 C5 C11 6.7(4) C7 N1 C8 C10 170.2(2) C7 N1 C8 C13 52.9(3) C7 N1 C8 C14 -71.9(3) C7 O3 C16 C22 -88.6(3) C7 O3 C16 C23 147.2(3) C8 N1 C5 C6 12.3(3) C8 N1 C5 C11 -163.2(2) C8 N1 C7 O2 -177.3(2) C8 N1 C7 O3 2.7(3) C9 N4 C18 C20 -169.9(2) C9 N4 C19 C21 168.8(3) C9 C6 C10 C8 162.2(2) C10 C6 C9 N4 -0.5(4) C10 C6 C9 C17 -177.4(2) C11 C5 C6 C9 0.5(4) C11 C5 C6 C10 177.9(2) C11 C12 C17 C9 0.2(5) C13 C8 C10 C6 140.4(2) C14 C8 C10 C6 -96.0(2) C16 O3 C7 N1 -175.4(2) C16 O3 C7 O2 4.7(3) C18 N4 C9 C6 68.6(3) C18 N4 C9 C17 -114.7(3) C18 N4 C19 C21 -57.6(3) C19 N4 C9 C6 -161.2(2) C19 N4 C9 C17 15.5(4) C19 N4 C18 C20 56.4(3) C20 O15 C21 C19 -58.0(4) C21 O15 C20 C18 56.6(4) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 3 20.6712 15.5959 4 0 0 -3 18.3928 12.8117 4 0 0 -3 18.9961 17.591 3 0 0 -3 55.2808 24.5281 5 0 0 4 19302.9 444.568 4 0 0 -4 19041.8 433.651 5 0 0 -4 18494.5 526.467 4 0 0 4 18292.8 433.061 5 0 0 -4 18306.1 619.378 3 0 0 5 141.029 51.0612 5 0 0 -5 266.933 78.6499 4 0 0 -5 181.823 95.02 3 0 0 5 200.636 57.5695 4 0 0 6 3660.66 233.727 5 0 0 -6 3988.49 321.247 4 0 0 7 621.404 110.626 5 0 0 -7 1347.32 264.34 3 0 0 -7 1213.91 204.912 4 0 0 8 445.855 91.3019 5 0 0 8 1052.94 296.129 1 0 0 -8 835.689 217.268 3 0 0 -8 716.809 162.244 4 0 0 -9 8.39897 52.6978 4 0 0 -9 -59.5112 115.778 3 0 0 9 -3.59374 122.762 1 0 0 10 14668.1 1216.46 1 0 0 -10 15150.7 838.157 4 0 0 -11 -26.3924 93.2457 4 0 0 11 -145.512 203.944 1 0 0 12 -165.481 150.386 1 0 0 13 12.1547 107.549 1 0 0 14 1379.87 464.248 1 0 0 15 -282.239 241.849 1 0 0 16 166.068 214.619 1 0 1 -2 79344 823.468 4 0 -1 -2 76597.1 1231.46 1 0 -1 -2 76823.7 783.473 5 0 -1 -2 79428.4 857.834 3 0 -1 -3 91398 1509.63 1 0 1 3 93085.9 735.049 4 0 -1 -3 88581.4 1162.02 3 0 1 -3 88351.9 1183.33 3 0 -1 -3 91082.9 866.202 4 0 -1 -3 89477 883.321 5 0 1 -3 88958.1 1057.99 4 0 -1 -4 595.455 84.5779 4 0 -1 -4 697.942 87.1698 5 0 1 -4 716.755 106.838 4 0 -1 4 726.02 96.7411 5 0 1 -4 639.9 120.172 3 0 1 4 721.31 73.5406 4 0 -1 4 769.221 101.984 4 0 -1 -4 665.028 119.474 3 0 -1 5 -14.0177 16.3601 5 0 1 -5 -4.15063 24.5189 4 0 1 -5 -5.93891 28.453 3 0 -1 -5 -29.8961 59.7331 3 0 1 5 79.7562 29.107 4 0 -1 -5 9.87296 12.6602 4 0 -1 -5 -2.20404 16.8988 5 0 -1 -6 93646.4 1418.3 4 0 1 6 89437.4 1078.49 4 0 -1 -6 93409.6 1171.27 5 0 1 -6 90771.9 1516.83 4 0 1 -6 95294.6 1832.54 3 0 -1 6 91131.7 1269.31 5 0 -1 -6 87947.6 1749.6 3 0 -1 -7 3292.97 360.349 3 0 1 -7 3078.14 315.619 4 0 -1 -7 3296.55 226.084 5 0 1 -7 3222 375.737 3 0 -1 -7 3727.28 318.207 4 0 -1 7 2857.43 238.132 5 0 1 8 5278.25 637.567 1 0 1 -8 5066 433.759 4 0 -1 8 5696.88 623.172 1 0 1 -8 5546.5 525.847 3 0 -1 -8 5495.98 415.044 4 0 -1 8 4585.48 307.377 5 0 -1 -8 5296.12 496.147 3 0 1 9 12667.4 1062.33 1 0 -1 -9 10419.1 614.416 4 0 -1 9 9888.23 893.305 1 0 1 -9 10731.6 685.321 4 0 1 -9 10721.4 783.909 3 0 -1 -10 2461.4 319.717 4 0 -1 10 1509.46 356.432 1 0 1 -10 2168.58 325.647 4 0 1 10 1841.89 444.091 1 0 1 -10 1714.74 323.779 3 0 -1 11 3471.81 620.786 1 0 1 -11 2850.66 400.187 4 0 1 11 3406.94 637.068 1 0 1 12 1442.99 447.406 1 0 -1 12 1155.12 380.926 1 0 -1 13 215.76 203.832 1 0 1 13 62.5437 128.058 1 0 -1 14 232.542 251.124 1 0 1 14 -252.197 229.83 1 0 -1 15 1107.36 443.101 1 0 -1 16 165.217 155.931 1 0 2 -2 9757.4 332.631 4 0 2 -2 9443.76 327.372 3 0 2 2 9265.51 261.438 3 0 2 -3 44374.8 799.525 4 0 2 -3 43869.6 860.643 3 0 2 3 45974.5 700.791 3 0 -2 -3 43671.7 806.28 3 0 2 -4 1848.05 189.095 4 0 2 -4 1810.69 207.658 3 0 -2 -4 1961.98 173.936 5 0 2 4 1957.99 169.352 3 0 -2 -4 1860.55 199.015 3 0 2 4 1911.4 100.938 4 0 -2 5 61181.7 1050.79 5 0 2 5 62348.1 647.266 4 0 2 -5 60451.3 1316.12 3 0 2 -5 60746 1172.39 4 0 -2 -5 57320.2 869.634 4 0 -2 -5 61788.8 975.937 5 0 -2 -5 58735.2 1250.92 3 0 2 -6 1275.45 216.88 3 0 2 -6 1360.46 197.425 4 0 -2 -6 1205.66 196.127 3 0 -2 -6 1381.61 150.615 5 0 -2 6 1299.74 163.106 5 0 2 6 1281.98 109.419 4 0 -2 -6 1567.61 166.02 4 0 -2 -7 35173.2 869.719 4 0 2 -7 36018.2 1095.53 4 0 2 -7 36810.7 1279.67 3 0 -2 7 35455.8 903.529 5 0 -2 -7 37430.1 829.421 5 0 -2 8 8462.85 747.526 1 0 -2 -8 7080.1 437.785 4 0 -2 -8 7638.85 385.705 5 0 2 -8 7065.32 595.045 3 0 2 -8 7766.91 556.712 4 0 2 8 7008.57 779.02 1 0 -2 8 7228.18 427.751 5 0 2 -9 -114.371 163.91 3 0 2 -9 203.831 99.6302 4 0 -2 -9 233.699 69.467 5 0 -2 -9 174.4 71.7242 4 0 2 9 186.555 93.8613 1 0 -2 9 67.1747 118.998 1 0 2 -10 7107.12 701.529 3 0 2 -10 6856.74 604.923 4 0 -2 10 8387.35 859.343 1 0 2 10 7945.59 938.721 1 0 2 11 11681.5 1215.08 1 0 -2 11 10966.4 1057.37 1 0 2 -11 12453.9 870.264 4 0 -2 12 -145.312 155.184 1 0 2 -12 15.1376 40.3736 4 0 -2 13 448.514 245.472 1 0 -2 14 372.429 227.886 1 0 -2 15 190.72 201.581 1 0 3 0 0.06919 9.96131 4 0 3 -1 16064 413.735 2 0 3 -1 16456.9 443.149 4 0 3 -1 15794.6 360.51 3 0 3 -2 185744 1642.13 4 0 3 -2 189474 1548.13 3 0 -3 2 186732 1496.05 2 0 3 3 19050.4 436.07 3 0 3 -3 19151.3 591.584 3 0 3 -3 19337.4 588.369 4 0 3 -4 2.61918 40.1983 4 0 3 4 1.21479 10.0897 3 0 3 -4 70.1612 46.8732 3 0 -3 -5 30506.9 816.657 5 0 3 -5 31696.8 982.344 3 0 3 -5 30999.4 911.346 4 0 3 -6 13495.5 713.001 3 0 -3 -6 13634.9 535.935 5 0 3 6 11865 262.306 4 0 3 -6 12956.1 628.427 4 0 3 -7 17638.8 796.812 4 0 -3 -7 19406.6 651.522 5 0 3 -7 18651.8 916.44 3 0 3 -8 909.529 220.649 3 0 3 -8 989.825 199.667 4 0 -3 -8 736.434 129.12 5 0 -3 -9 4107.98 311.166 5 0 3 -9 4356.46 512.811 3 0 3 -9 4910.33 487.588 4 0 -3 9 4450.44 573.617 1 0 3 -10 9859.94 743.549 4 0 3 -10 9858.23 832.003 3 0 -3 10 9639.69 917.338 1 0 3 -11 246.992 73.3226 3 0 3 -11 107.924 72.7059 4 0 -3 11 70.9187 118.867 1 0 -3 12 5693.41 801.69 1 0 3 -12 5281.82 616.425 4 0 -3 13 42.2512 101.041 1 0 -3 14 360.176 250.187 1 0 -3 15 1023.46 402.069 1 0 4 0 43328.1 747.107 4 0 4 -1 24038.5 485.357 3 0 4 -1 23351.2 598.949 2 0 4 -1 24773.7 610.141 4 0 4 -2 77.9355 46.9547 4 0 4 -2 90.5501 44.795 3 0 -4 2 26.319 22.1184 2 0 4 -2 9.27278 13.3913 2 0 4 3 1927.08 127.953 3 0 4 -3 1743.59 184.496 3 0 -4 3 2046.25 188.622 2 0 4 -3 1819.52 192.906 4 0 4 4 46345.4 752.619 3 0 4 -4 45855.7 1079.71 3 0 4 -4 46235.2 1069.07 4 0 4 -5 5260.39 407.68 3 0 4 -5 5349.45 392.662 4 0 4 -6 71366.1 1678.54 3 0 4 -6 75149.9 1580.75 4 0 -4 -6 71403.5 1426.41 5 0 4 -7 682.205 160.832 4 0 -4 -7 368.574 98.8441 5 0 4 -7 493.025 149.561 3 0 -4 -8 152.916 72.0228 5 0 4 -8 59.7921 96.9167 3 0 4 -9 11102.1 754.875 4 0 4 -9 10289.4 807.759 3 0 -4 -9 10572.3 548.835 5 0 4 -10 3056.32 427.619 4 0 -4 10 2839.36 499.906 1 0 4 -10 2694.06 432.073 3 0 4 -11 7864.94 738.156 4 0 -4 11 6795.68 832.092 1 0 4 -11 6697.5 729.192 3 0 4 -12 136.66 112.755 4 0 -4 12 263.106 164.783 1 0 -4 13 332.727 219.275 1 0 4 -13 -116.912 146.456 4 0 -4 14 3078.51 672.557 1 0 -4 15 -474.158 287.67 1 0 5 0 43.6165 33.6475 4 0 5 -1 36159.2 823.861 4 0 5 -1 36949.8 856.027 2 0 5 1 38227.3 722.001 4 0 5 -1 37006.1 648.229 3 0 5 -2 1113.17 133.924 3 0 5 2 959.271 105.492 4 0 5 -2 852.218 122.674 2 0 5 -2 998.099 143.416 4 0 5 -3 27526 808.478 4 0 5 -3 25578 744.099 3 0 5 3 27239 429.915 3 0 -5 3 26548.4 715.149 2 0 -5 4 14816 577.06 2 0 5 -4 15037.8 643.468 4 0 5 4 15259 404.755 3 0 5 -4 14582 627.183 3 0 5 -5 10079.7 569.689 4 0 5 -5 9835.43 575.146 3 0 5 -6 596.318 150.795 4 0 -5 -6 655.974 147.05 5 0 5 -6 943.385 201.518 3 0 -5 -7 2467.01 290.097 5 0 5 -7 2103.12 306.308 3 0 5 -7 2280.91 305.812 4 0 5 -8 2507.52 344.005 4 0 -5 -8 1931.98 252.032 5 0 5 -8 1757.59 299.713 3 0 -5 -9 6004.81 443.112 5 0 5 -9 6084 574.729 4 0 5 -9 5739 623.336 3 0 5 -10 15006.2 1063.31 3 0 5 -10 16203.8 1007.35 4 0 -5 11 -12.4055 115.216 1 0 5 -11 43.784 72.8119 4 0 -5 12 156.2 136.829 1 0 5 -12 -35.0426 88.2957 4 0 5 -13 225.669 143.29 4 0 -5 13 160.266 182.96 1 0 -5 14 -15.2709 120.38 1 0 -5 15 -23.1251 82.2794 1 0 6 0 20126.1 413.293 3 0 6 0 21153.6 641.789 4 0 6 -1 1230.11 128.798 3 0 6 1 1332.93 151.641 4 0 6 -1 1374.45 172.733 4 0 6 -1 1096.57 159.745 2 0 6 -2 22857.8 636.752 3 0 6 2 23230.9 586.361 4 0 6 -2 23195.8 757.035 4 0 6 -2 22967.3 682.434 2 0 -6 3 12.6678 36.853 2 0 6 -3 18.7633 30.7786 3 0 6 3 6.48282 11.9411 4 0 6 -3 37.4787 47.7928 4 0 6 3 10.1051 10.2881 3 0 6 4 161158 1266.94 4 0 6 -4 166277 2228.55 3 0 -6 4 164856 2011.42 2 0 6 -4 165036 2280.68 4 0 6 -5 7126.62 504.154 4 0 -6 5 7288.81 452.327 2 0 6 -5 6994.95 504.56 3 0 6 5 7469.48 217.26 4 0 6 -6 12853.4 739.896 3 0 6 -6 15051.2 785.615 4 0 -6 6 13142.9 648.028 2 0 6 -7 3424.04 415.437 3 0 6 -7 3583.64 404.018 4 0 -6 -7 3195.81 364.268 5 0 6 -8 6543.73 621.406 3 0 -6 -8 6538.87 507.699 5 0 6 -8 6667.77 588.487 4 0 6 -9 10454.7 847.841 3 0 6 -9 10851.6 799.049 4 0 -6 -9 10931.2 650.923 5 0 6 -10 2771.36 430.944 4 0 6 -10 2259.3 406.793 3 0 6 -11 49.465 114.246 4 0 6 -11 -267.745 234.765 3 0 6 -12 263.675 165.694 4 0 -6 12 -22.0575 94.8528 1 0 6 -13 471.051 215.297 4 0 -6 13 525.329 265.612 1 0 -6 14 313.772 276.704 1 0 -6 15 124.354 213.958 1 0 7 0 279.131 91.9012 4 0 7 0 276.813 59.1708 3 0 7 1 51496.2 1022.79 4 0 7 1 51703.6 527.788 3 0 7 -1 53127.9 1154.11 4 0 7 -2 80980.2 1272.72 3 0 7 2 79765.2 1205.73 4 0 7 -2 82092.6 1528.96 4 0 7 3 3133.79 230.011 4 0 7 -3 3058.77 318.816 4 0 7 -3 3086.89 281.185 3 0 7 -4 0.46358 35.2542 3 0 7 4 2.8256 16.1074 4 0 -7 4 34.4239 33.2504 2 0 7 -4 42.3476 54.5189 4 0 -7 5 4194.93 352.289 2 0 7 -5 4338.58 419.649 4 0 7 -5 4021.54 391.966 3 0 7 5 4307.35 205.791 4 0 7 -6 1089.89 224.693 3 0 -7 6 1228.85 207.221 2 0 7 6 870.219 72.5181 4 0 7 -6 1046.67 202.286 4 0 7 -7 62.259 77.2282 3 0 -7 7 -25.7061 39.9641 2 0 -7 -8 7138.95 581.485 5 0 7 -8 7785.62 662.332 4 0 7 -8 5834.33 605.898 3 0 7 -9 919.583 229.784 3 0 7 -9 1288.88 287.861 4 0 -7 -9 1124.05 231.905 5 0 7 -10 6387.83 717.065 3 0 7 -10 6654.93 675.906 4 0 7 -11 -36.8075 102.436 4 0 7 -11 -96.0264 183.493 3 0 7 -12 274.15 167.995 4 0 7 -13 1573.24 394.875 4 0 -7 13 1855.76 483.26 1 0 7 -14 337.536 173.467 4 0 -7 14 390.768 250.849 1 0 8 0 28782.5 875.565 4 0 8 0 27167.2 587.407 3 0 8 -1 7846.76 370.32 3 0 8 1 7927.7 245.123 3 0 8 1 7864.35 435.954 4 0 8 -1 7874.71 481.931 4 0 8 -2 6621.09 393.277 3 0 8 -2 7103.9 480.71 4 0 8 2 6782.85 381.131 4 0 8 -3 6330.22 422.668 3 0 8 -3 6066.68 465.893 4 0 8 3 6075.91 342.526 4 0 8 -4 8069.42 525.61 3 0 8 4 7871.89 362.691 4 0 8 -4 8335.84 575.912 4 0 8 5 -9.42257 16.7285 4 0 -8 5 -29.0856 46.6738 2 0 8 -5 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5138.17 506.378 3 0 10 -6 51.8767 90.4946 3 0 10 -6 122.229 66.237 4 0 -10 7 1182.4 226.102 2 0 10 -7 933.564 247.184 3 0 10 -7 833.853 251.274 4 0 10 -8 1041.8 260.273 3 0 10 -8 1731.79 357.371 4 0 10 -9 -64.0562 143.277 3 0 10 -9 151.58 128.478 4 0 -10 -9 284.199 123.203 5 0 10 -10 -206.952 196.377 3 0 10 -10 250.003 180.209 4 0 10 -11 127.569 138.105 4 0 10 -12 37.0272 52.3794 4 0 10 -13 64.4013 62.9104 4 0 10 -14 317.494 217.261 4 0 11 0 98.8673 72.688 4 0 11 0 14.9155 40.3069 3 0 11 1 10476.4 627.351 4 0 11 -1 9538.91 647.079 4 0 11 -1 9984.27 524.256 3 0 11 2 490.849 139.77 4 0 11 -2 615.33 134.265 3 0 11 -2 466.219 148.133 4 0 11 3 19.1973 48.5147 4 0 11 -3 -61.2177 78.9573 3 0 11 -4 19282.4 1032.71 4 0 11 -4 18047.1 912.275 3 0 11 4 19151.2 761.425 4 0 11 5 589.62 125.595 4 0 11 -5 567.959 162.604 3 0 11 -5 530.853 172.139 4 0 11 -6 -47.4102 95.7157 3 0 11 -6 127.143 70.086 4 0 11 -7 1269.21 289.875 4 0 11 -7 522.778 184.243 3 0 11 -8 190.752 135.622 4 0 11 -8 -8.31423 142.778 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753.676 197.002 4 0 13 2 4707.07 471.824 4 0 13 -2 4335.26 512.475 4 0 13 -3 -9.59137 78.5524 3 0 13 -3 147.898 147.781 4 0 13 3 291.915 114.867 4 0 13 -4 2498.59 367.011 3 0 13 -4 3151.92 467.631 4 0 13 4 2400.12 314.597 4 0 13 -5 2466.27 415.306 4 0 13 -5 2410.82 385.364 3 0 13 -6 -162.152 151.588 3 0 13 -6 -95.2901 135.155 4 0 13 -7 960.949 308.589 4 0 13 -7 199.268 77.3221 3 0 13 -8 360.647 188.876 4 0 13 -9 118.125 108.857 4 0 13 -10 311.523 180.896 4 0 13 -11 2270.49 531.523 4 0 13 -12 194.915 108.14 4 0 14 0 231.216 141.3 4 0 14 1 304.103 118.059 4 0 14 -1 422.831 160.111 4 0 14 -2 92.2658 70.9485 4 0 14 2 -63.9412 99.2826 4 0 14 -3 525.766 202.26 4 0 14 3 509.749 167.963 4 0 14 -4 2774.11 448.898 4 0 14 -5 71.9317 76.1062 4 0 14 -6 -56.9427 114.403 4 0 14 -7 -56.6767 117.052 4 0 14 -8 127.537 175.007 4 0 14 -9 189.691 160.963 4 0 14 -10 197.494 177.06 4 0 15 0 -17.0701 121.361 4 0 15 1 262.513 137.31 4 0 15 -1 342.332 118.65 4 0 15 -2 152.305 97.7557 4 0 15 2 461.912 169.136 4 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9 3645.37 539.307 1 -1 1 9 3415.75 550.82 1 1 1 -8 255.564 126.947 4 1 -1 -8 267.753 96.7572 4 1 1 -7 15893.9 810.579 4 1 -1 -7 15471.6 745.693 4 1 1 -6 5644.61 452.561 4 1 -1 -6 5695.79 421.788 4 -1 -1 6 5890.35 209.908 5 1 1 -5 643.071 133.917 4 -1 1 5 574.717 109.131 4 1 -1 -5 657.826 127.835 4 1 -1 -4 6025.96 366.753 4 1 1 -4 6703.95 415.36 4 -1 1 4 5793.54 335.807 4 1 1 -3 -12.4712 20.3767 4 -1 1 3 29.606 31.7434 4 1 1 -2 20819.3 623.735 4 1 -1 -2 21468.9 646.238 1 -1 -1 -2 30.6837 16.5573 5 -1 -1 -2 109.213 55.4749 1 -1 1 -2 129.414 52.8386 5 -1 1 -3 19692.6 604.298 5 -1 -1 -3 18345.7 578.654 5 1 -1 3 17754.7 605.391 5 1 1 3 17883.7 573.992 5 -1 -1 -3 18764.9 674.527 1 1 -1 4 8618.98 448.67 5 1 1 4 8009.44 417.696 5 1 1 4 9089.07 597.546 1 -1 -1 -4 8450.27 251.428 4 -1 -1 -4 8528.29 419.209 5 -1 -1 -5 1732.95 202.999 5 -1 -1 -5 1770.11 134.407 4 -1 -1 -5 1680.26 194.077 3 1 1 5 1696.68 202.219 5 -1 1 -5 1994.11 181.931 4 1 1 5 2091.79 311.701 1 1 -1 5 2146.2 282.974 1 -1 1 -5 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181.388 4 -1 15 -9 76.6732 100.891 3 1 16 -8 52.3785 111.999 4 1 16 -7 653.079 271.91 4 1 16 -6 285.007 227.547 4 1 16 -5 315.207 186.424 4 1 16 -4 94.9769 90.163 4 1 16 -3 1063.06 316.858 4 -1 16 3 1208.97 278.218 4 1 16 -2 -110.553 129.573 4 -1 16 2 68.1257 80.7125 4 1 16 -1 964.635 292.035 4 -1 16 1 1078.36 271.574 4 1 16 0 526.738 199.868 4 -1 16 0 230.054 123.275 4 1 16 1 420.175 181.256 4 -1 16 -1 721.28 235.236 4 -1 16 -2 22.861 59.8563 4 1 16 2 61.4431 84.0387 4 -1 16 -3 81.8271 82.3411 4 -1 16 -4 859.233 281.688 4 -1 16 -5 95.5175 120.216 4 -1 16 -6 142.482 95.1934 4 -1 16 -7 312.323 173.867 4 -1 16 -8 594.771 280.267 4 -1 -16 -8 239.874 174.451 5 1 17 -7 297.753 212.884 4 1 17 -6 683.846 302.808 4 1 17 -5 285.183 195.11 4 1 17 -4 151.642 151.512 4 1 17 -3 149.764 171.493 4 -1 17 2 172.557 118.941 4 1 17 -2 398.232 192.939 4 1 17 -1 -97.8928 98.4313 4 -1 17 1 -65.5506 109.576 4 -1 17 0 128.248 96.771 4 1 17 0 67.0486 83.0889 4 1 17 1 125.067 124.051 4 -1 17 -1 80.5994 105.739 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454.44 1 -2 0 11 93.8881 163.454 1 2 0 -11 -55.9218 130.535 4 -2 0 10 2808.68 532.424 1 2 0 -10 3140.95 454.427 4 -2 0 9 -15.0053 67.241 1 2 0 -9 46.1125 60.5501 4 2 0 -8 639.224 182.214 4 2 0 -7 -100.485 74.051 4 2 0 -6 2043.62 292.384 4 2 0 -5 -13.9075 52.2482 4 2 0 -4 33272.8 554.6 5 -2 0 4 33000.5 545.965 5 2 0 -4 33289.1 1082.75 4 -2 0 3 1.55119 25.6597 5 2 0 -3 7.31911 11.5786 5 -2 0 2 447559 2732.86 1 -2 0 2 449094 2621.92 5 -2 0 1 141.784 65.9185 5 -2 0 1 85.4816 44.2651 1 -2 0 0 999999 4474.62 5 -2 0 -1 26.0449 44.4556 5 2 0 2 69909.7 1039.99 1 -2 0 -2 69046.8 1330.42 5 -2 0 -3 -21.5308 73.3119 5 2 0 3 -28.2735 46.9911 1 2 0 4 9218.32 555.114 1 -2 0 -4 9633.1 541.742 5 -2 0 -5 -12.1786 51.9563 5 2 0 5 -23.5757 49.4031 1 2 0 6 39136.5 1439.83 1 -2 0 -6 38720 1179.49 5 -2 0 -7 7.03609 39.5915 4 -2 0 -7 -3.43529 41.7507 5 -2 0 -8 -18.4048 26.2775 4 2 0 8 -23.0293 75.0061 1 -2 0 -8 51.3681 83.1477 3 -2 0 -8 -24.2158 83.5791 5 2 0 9 22.625 70.3908 1 -2 0 -9 39.9072 98.4292 3 -2 0 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1947.02 1 -2 -1 3 152825 1453.83 5 2 1 -3 149985 2235.66 4 2 -1 -3 149789 1399.1 5 2 1 -2 327529 2347.15 5 2 -1 -2 323094 2259.56 5 2 -1 -2 337136 2484.34 1 -2 -1 2 322666 2292.16 5 -2 1 2 332076 2717.74 1 2 1 -2 331744 3176.55 4 -2 1 1 74716.7 1155.02 5 2 -1 -1 75415.2 983.13 1 -2 -1 1 74682.9 1160.6 5 2 1 -1 73356.1 1202.29 2 -2 1 0 13907.6 402.062 2 -2 1 0 14576.9 552.117 5 -2 -1 0 13468.3 523.168 5 2 1 0 13100.3 494.436 2 2 -1 1 211212 1565.47 2 -2 -1 -1 211642 2200.24 5 -2 1 -1 209969 2201.37 5 -2 1 -2 8412.19 466.521 5 -2 -1 -2 8493.27 468.026 5 -2 -1 -2 8130.74 379.167 1 -2 -1 -3 133423 1943.17 5 -2 1 -3 136720 1967.97 5 -2 -1 -3 131237 1716.79 1 -2 1 -4 758.569 154.118 5 2 -1 4 665.162 138.842 1 -2 -1 -4 728.381 143.984 5 2 1 4 767.742 178.132 1 -2 1 -5 180.86 86.7683 5 -2 -1 -5 278.539 101.021 5 2 -1 5 185.213 86.18 1 2 1 5 457.193 156.734 1 -2 1 -6 67144.6 1537.61 5 2 -1 6 68334 1802.99 1 -2 -1 -6 64421.2 1538.13 5 2 1 6 63617.4 1926.24 1 -2 -1 -7 2077.38 286.619 5 -2 1 -7 1945.45 265.724 3 -2 -1 -7 1781.15 249.551 3 -2 -1 -7 1890.38 177.27 4 -2 1 -7 1860.35 208.569 4 2 1 8 2617.51 459.487 1 2 -1 8 3171.29 466.242 1 -2 -1 -8 2742.36 338.634 5 -2 1 -8 2903.68 349.639 3 -2 -1 -8 2686.7 232.721 4 -2 1 -8 2973.44 275.203 4 -2 -1 -8 3037.52 344.907 3 2 -1 9 11866.3 997.119 1 2 1 9 11755.6 1043.28 1 -2 -1 -9 11623.6 718.19 5 -2 -1 -9 11755.6 747.923 3 -2 -1 -9 11715.3 544.033 4 -2 1 -9 12393.9 775.237 3 -2 1 -9 12091.7 611.256 4 2 1 10 949.036 318.025 1 -2 1 -10 1136.14 205.582 4 -2 -1 -10 869.814 190.137 5 2 -1 10 614.92 251.405 1 -2 -1 -10 1147.81 254.411 3 -2 1 -10 1318.84 282.577 3 -2 1 -11 3412.47 488.189 3 -2 -1 -11 3291.66 471.36 3 2 1 11 3727.56 667.364 1 2 -1 11 3872.47 671.171 1 2 -1 12 183.753 154.85 1 -2 1 -12 173.347 150.151 3 -2 -1 -12 -96.1868 134.36 3 2 1 12 -20.4521 100.987 1 -2 -1 -13 51.8153 73.6869 3 2 -1 13 316.72 224.328 1 -2 1 -13 216.333 172.669 3 2 -1 14 44.4045 136.553 1 -2 -1 -14 51.1182 77.5852 3 -2 1 -14 -234.626 218.14 3 2 -1 15 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12665.8 814.483 5 -4 -1 -4 12773 824.103 5 4 -1 4 12255.9 612.041 1 -4 1 -5 1851.67 324.094 5 -4 -1 -5 1509.12 289.091 5 4 -1 5 1710 265.961 1 -4 1 -6 22735.4 1141.7 5 -4 -1 -6 22142.7 1138.64 5 4 -1 6 22601.7 1075.04 1 -4 1 -7 306.565 143.665 5 -4 -1 -7 180.596 93.7821 5 -4 1 -8 637.54 210.491 5 -4 -1 -8 492.028 188.933 5 4 -1 8 339.701 158.078 1 -4 -1 -9 -86.1916 102.793 5 4 -1 9 -0.4298 103.389 1 -4 1 -9 -17.4081 45.0041 4 -4 -1 -10 239.995 125.423 5 4 -1 10 200.44 149.982 1 -4 -1 -10 267.68 121.526 3 -4 1 -10 327.294 163.577 3 4 -1 11 1432.02 400.252 1 -4 -1 -11 1959.5 353.947 3 -4 1 -11 1954.91 353.028 3 4 -1 12 -91.0901 129.713 1 -4 -1 -12 78.8475 79.4236 3 -4 1 -12 -26.0281 68.834 3 4 -1 13 -245.74 203.277 1 -4 -1 -13 -86.9858 152.668 3 -4 1 -13 94.0063 139.209 3 -4 -1 -14 10.6768 74.0897 3 -4 1 -14 -15.5757 81.7456 3 -4 -1 -15 -91.8607 126.259 3 -4 -2 15 403.494 285.124 1 -4 -2 14 -149.69 221.08 1 -4 -2 13 482.125 254.306 1 -4 2 13 269.055 194.784 1 -4 -2 12 4074.4 700.755 1 -4 2 12 3423.14 705.233 1 -4 -2 11 2005.25 475.664 1 -4 2 11 1934 509.267 1 4 2 -11 2000.63 449.148 4 4 2 -10 2700.21 491.637 4 -4 2 10 2726.35 556.872 1 -4 -2 10 2914.62 531.421 1 -4 2 9 1698.08 423.52 1 -4 -2 9 1815.77 401.24 1 4 2 -9 1351.69 345.686 4 -4 -2 8 9407.71 436.21 5 -4 -2 8 11094.9 879.848 1 -4 2 8 10894.3 982.701 1 4 2 -8 10188.3 907.867 4 -4 -2 7 586.842 120.633 5 -4 -2 7 728.719 212.129 1 4 -2 -7 528.273 104.965 5 4 2 -7 769.349 260.657 4 -4 2 7 629.637 194.479 1 -4 -2 6 22539.8 800.257 5 -4 2 6 22536.9 1223.6 1 4 2 -6 23320.1 1296.11 4 -4 -2 5 2260.09 262.25 5 -4 -2 4 15450.9 717.823 5 -4 -2 3 1553.32 234.425 5 -4 2 3 1854.99 248.458 5 -4 2 2 18629.3 825.896 5 -4 -2 2 16945.7 801.75 5 4 -2 -2 16916.2 602.215 1 -4 2 1 42527.1 1068 2 -4 -2 1 43930.9 1331.3 5 4 -2 -1 42127.8 827.846 1 -4 2 1 44030.2 1315.09 5 -4 2 0 18816.2 664.616 2 -4 -2 0 20583.4 938.579 5 -4 2 0 18698.6 884.914 5 4 -2 1 -5.50908 43.9736 2 -4 2 -1 1.82926 103.217 5 -4 -2 -1 -22.9119 62.7098 5 4 -2 2 1392.63 178.933 2 -4 2 -2 1526.89 270.314 5 -4 -2 -2 1485.96 270.819 5 -4 -2 -2 1983.7 212.631 1 -4 2 -3 9194.72 686.029 5 -4 -2 -3 9855.74 708.189 5 -4 -2 -3 8899.84 469.382 1 4 -2 3 10142.2 442.383 1 -4 2 -4 5028.43 513.173 5 -4 -2 -4 5090.87 519.747 5 4 -2 4 5788.32 399.226 1 -4 2 -5 4423.64 489.221 5 4 -2 5 3975.69 383.475 1 -4 -2 -5 4179.68 486.839 5 -4 -2 -6 91.1583 78.5931 5 4 -2 6 170.924 69.2712 1 -4 -2 -7 1454.21 312.508 5 -4 -2 -8 93.2641 95.2548 5 4 -2 8 204.679 138.401 1 -4 -2 -9 828.969 262.576 5 -4 2 -9 947.639 197.093 4 4 -2 9 1214.67 303.182 1 -4 -2 -10 323.634 166.09 5 -4 2 -10 604.856 161.549 4 4 -2 10 152.727 130.54 1 -4 -2 -10 56.8124 56.9829 3 -4 2 -10 383.567 148.09 3 4 -2 11 4405.18 697.85 1 -4 -2 -11 4170.66 509.718 3 -4 2 -11 4050.72 523.419 3 4 -2 12 369.128 198.652 1 -4 -2 -12 551.434 219.334 3 -4 2 -12 183.688 152.282 3 4 -2 13 605.749 294.749 1 -4 -2 -13 57.1259 64.4881 3 -4 2 -13 503.993 219.824 3 -4 -2 -14 120.052 125.82 3 -4 2 -14 -87.7992 118.582 3 -4 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741.19 5 4 -3 6 421.411 121.456 1 -4 -3 -6 678.194 216.077 5 -4 -3 -7 8076.7 733.25 5 -4 -3 -8 509.226 197.535 5 4 -3 8 235.741 138.043 1 4 -3 9 81.7193 61.0202 1 -4 -3 -9 -84.0655 100.339 5 -4 3 -9 130.507 87.9529 4 -4 -3 -9 233.579 113.025 3 -4 -3 -10 492.003 206.087 5 4 -3 10 170.666 112.619 1 -4 3 -10 355.847 140.032 4 -4 3 -10 449.763 188.522 3 4 -3 11 101.099 84.9438 1 -4 -3 -11 134.336 125.522 3 -4 3 -11 301.069 142.798 3 -4 -3 -12 652.934 217.489 3 -4 3 -12 532.827 227.394 3 4 -3 12 1168.16 392.401 1 -4 -3 -13 330.466 181.429 3 -4 3 -13 108.156 141.824 3 -4 -3 -14 406.655 211.691 3 -4 3 -14 110.476 90.2353 3 -4 -4 15 712.938 335.285 1 -4 -4 14 484.374 302.009 1 4 4 -14 -72.8729 115.964 4 4 4 -13 473.87 258.186 4 -4 -4 13 282.995 160.178 1 -4 -4 12 793.825 315.651 1 4 4 -12 982.964 340.602 4 -4 -4 11 602.39 259.169 1 4 4 -11 1077.04 351.988 4 -4 -4 10 11950.9 1045.75 1 4 4 -10 10879.1 1044.06 4 4 4 -9 1905.68 429.616 4 -4 -4 8 10469.3 580.152 5 4 4 -8 10668.1 974.091 4 -4 -4 7 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