#------------------------------------------------------------------------------ #$Date: 2017-07-12 00:28:33 +0300 (Wed, 12 Jul 2017) $ #$Revision: 198646 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/41/4514161.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_4514161 loop_ _publ_author_name 'Reay, Alan J.' 'Hammarback, L. Anders' 'Bray, Joshua T. W.' 'Sheridan, Thomas' 'Turnbull, David' 'Whitwood, Adrian C.' 'Fairlamb, Ian J. S.' _publ_section_title ; Mild and Regioselective Pd(OAc)2-Catalyzed C--H Arylation of Tryptophans by [ArN2]X, Promoted by Tosic Acid ; _journal_name_full 'ACS Catalysis' _journal_page_first 5174 _journal_paper_doi 10.1021/acscatal.6b03121 _journal_year 2017 _chemical_absolute_configuration syn _chemical_formula_moiety 'C20 H20 N2 O3' _chemical_formula_sum 'C20 H20 N2 O3' _chemical_formula_weight 336.38 _space_group_crystal_system trigonal _space_group_IT_number 146 _space_group_name_Hall 'R 3' _space_group_name_H-M_alt 'R 3' _symmetry_space_group_name_Hall 'R 3' _symmetry_space_group_name_H-M 'R 3 :H' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2017-04-24 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 9 _cell_length_a 21.2602(5) _cell_length_b 21.2602(5) _cell_length_c 10.1814(3) _cell_measurement_reflns_used 3153 _cell_measurement_temperature 110.05(10) _cell_measurement_theta_max 31.9520 _cell_measurement_theta_min 3.5440 _cell_volume 3985.41(18) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _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_environment N~2~ _diffrn_ambient_temperature 110.05(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1450 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.900 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -93.00 -15.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -25.0740 0.0000 150.0000 78 #__ type_ start__ end____ width___ exp.time_ 2 omega 5.00 59.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 26.4802 -99.0000 60.0000 54 #__ type_ start__ end____ width___ exp.time_ 3 omega 35.00 69.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.0201 77.0000 -60.0000 34 #__ type_ start__ end____ width___ exp.time_ 4 omega 37.00 75.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.0201 77.0000 60.0000 38 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0356613000 _diffrn_orient_matrix_UB_12 0.0297314000 _diffrn_orient_matrix_UB_13 0.0084190000 _diffrn_orient_matrix_UB_21 0.0125828000 _diffrn_orient_matrix_UB_22 -0.0134942000 _diffrn_orient_matrix_UB_23 -0.0513138000 _diffrn_orient_matrix_UB_31 -0.0073394000 _diffrn_orient_matrix_UB_32 0.0204228000 _diffrn_orient_matrix_UB_33 -0.0463462000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.900 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6369 _diffrn_reflns_point_group_measured_fraction_full 0.876 _diffrn_reflns_point_group_measured_fraction_max 0.683 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.005 _diffrn_reflns_theta_min 2.983 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_correction_T_min 0.985 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.261 _exptl_crystal_description block _exptl_crystal_F_000 1602 _exptl_crystal_size_max 0.2757 _exptl_crystal_size_mid 0.1814 _exptl_crystal_size_min 0.1572 _refine_diff_density_max 0.265 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.045 _refine_ls_abs_structure_details ; Flack x determined using 1307 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.5(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 4199 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0363 _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^)+(0.0398P)^2^+2.4699P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.0900 _reflns_Friedel_coverage 0.518 _reflns_Friedel_fraction_full 0.752 _reflns_Friedel_fraction_max 0.466 _reflns_number_gt 3948 _reflns_number_total 4199 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; ijsf1413.res created by SHELXL-2014/7 TITL ijsf1413 in R3 CELL 0.71073 21.260206 21.260206 10.181419 90 90 120 ZERR 9 0.000537 0.000537 0.000267 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H N O UNIT 180 180 18 27 EQIV $1 -0.667-Y,-0.333+X-Y,-0.333+Z EQIV $2 -1+Y-X,-1-X,+Z L.S. 8 PLAN 20 HTAB N1 O2_$1 HTAB N2 O3_$2 BOND $H MORE -1 CONF fmap 2 acta REM REM REM WGHT 0.039800 2.469900 FVAR 3.74990 C1 1 -0.464130 -0.338952 -0.380473 11.00000 0.01236 0.01206 = 0.01853 0.00106 0.00255 0.00440 C2 1 -0.460767 -0.357931 -0.523892 11.00000 0.01170 0.01235 = 0.01676 -0.00004 0.00100 0.00554 AFIX 13 H2 2 -0.488844 -0.342561 -0.577891 11.00000 -1.20000 AFIX 0 C3 1 -0.493124 -0.440610 -0.537323 11.00000 0.01313 0.01305 = 0.02046 -0.00145 0.00180 0.00527 AFIX 23 H3A 2 -0.496250 -0.452730 -0.629837 11.00000 -1.20000 H3B 2 -0.460344 -0.454064 -0.496348 11.00000 -1.20000 AFIX 0 C4 1 -0.566969 -0.484634 -0.476839 11.00000 0.01277 0.01206 = 0.01849 -0.00032 0.00104 0.00551 C5 1 -0.579697 -0.515746 -0.346856 11.00000 0.01521 0.01312 = 0.01875 -0.00150 -0.00019 0.00662 C6 1 -0.534405 -0.518538 -0.249160 11.00000 0.01758 0.01605 = 0.02425 -0.00160 -0.00144 0.00801 AFIX 43 H6 2 -0.484267 -0.494080 -0.260165 11.00000 -1.20000 AFIX 0 C7 1 -0.565703 -0.558257 -0.136528 11.00000 0.02749 0.01823 = 0.02206 -0.00201 -0.00553 0.01230 AFIX 43 H7 2 -0.536146 -0.560644 -0.071706 11.00000 -1.20000 AFIX 0 C8 1 -0.641377 -0.595141 -0.118008 11.00000 0.02745 0.01583 = 0.01870 0.00174 0.00157 0.00893 AFIX 43 H8 2 -0.661028 -0.621951 -0.041699 11.00000 -1.20000 AFIX 0 C9 1 -0.687178 -0.592186 -0.211689 11.00000 0.01898 0.01732 = 0.02292 0.00144 0.00398 0.00716 AFIX 43 H9 2 -0.737164 -0.615872 -0.198843 11.00000 -1.20000 AFIX 0 C10 1 -0.655680 -0.552411 -0.326062 11.00000 0.01434 0.01360 = 0.01978 -0.00030 0.00034 0.00595 C11 1 -0.633754 -0.502336 -0.527737 11.00000 0.01390 0.01174 = 0.01880 -0.00080 0.00191 0.00449 C12 1 -0.655057 -0.484424 -0.654071 11.00000 0.01225 0.01178 = 0.01945 0.00061 -0.00032 0.00306 C13 1 -0.705845 -0.460544 -0.653813 11.00000 0.01779 0.02047 = 0.02168 0.00136 0.00205 0.00916 AFIX 43 H13 2 -0.723827 -0.454531 -0.574412 11.00000 -1.20000 AFIX 0 C14 1 -0.729532 -0.445798 -0.770937 11.00000 0.01987 0.02590 = 0.02776 0.00162 -0.00285 0.01248 AFIX 43 H14 2 -0.763566 -0.430496 -0.769925 11.00000 -1.20000 AFIX 0 C15 1 -0.702063 -0.454045 -0.889781 11.00000 0.02561 0.02524 = 0.02085 -0.00007 -0.00649 0.01055 AFIX 43 H15 2 -0.717894 -0.444361 -0.968352 11.00000 -1.20000 AFIX 0 C16 1 -0.651243 -0.476625 -0.891304 11.00000 0.02646 0.02086 = 0.01871 -0.00478 0.00011 0.00881 AFIX 43 H16 2 -0.632592 -0.481402 -0.970920 11.00000 -1.20000 AFIX 0 C17 1 -0.627801 -0.492281 -0.773965 11.00000 0.01926 0.01682 = 0.02312 -0.00301 -0.00001 0.00858 AFIX 43 H17 2 -0.594046 -0.507935 -0.775702 11.00000 -1.20000 AFIX 0 C18 1 -0.531984 -0.314774 -0.226166 11.00000 0.03963 0.05053 = 0.02236 -0.00522 0.00566 0.02989 AFIX 137 H18A 2 -0.547089 -0.357967 -0.175120 11.00000 -1.50000 H18B 2 -0.569055 -0.301583 -0.223506 11.00000 -1.50000 H18C 2 -0.487714 -0.275950 -0.190574 11.00000 -1.50000 AFIX 0 C19 1 -0.343486 -0.249006 -0.559861 11.00000 0.01593 0.01589 = 0.01455 0.00177 0.00184 0.00703 C20 1 -0.266864 -0.218260 -0.609967 11.00000 0.01603 0.01779 = 0.03125 0.00031 0.00678 0.00466 AFIX 137 H20A 2 -0.233263 -0.195000 -0.539140 11.00000 -1.50000 H20B 2 -0.257856 -0.183404 -0.677852 11.00000 -1.50000 H20C 2 -0.260719 -0.256811 -0.644791 11.00000 -1.50000 AFIX 0 N1 3 -0.386178 -0.321919 -0.569541 11.00000 0.01377 0.01396 = 0.02278 0.00087 0.00557 0.00737 H1 2 -0.366636 -0.348135 -0.594407 11.00000 0.02346 N2 3 -0.687358 -0.541956 -0.435662 11.00000 0.01156 0.01787 = 0.02075 0.00237 0.00083 0.00484 H2A 2 -0.731661 -0.564124 -0.453979 11.00000 0.02459 O1 4 -0.520047 -0.328095 -0.360992 11.00000 0.02041 0.02822 = 0.01986 -0.00104 0.00266 0.01653 O2 4 -0.423680 -0.336346 -0.294870 11.00000 0.01615 0.02032 = 0.02046 -0.00068 -0.00243 0.00768 O3 4 -0.366309 -0.210818 -0.512493 11.00000 0.01977 0.01571 = 0.02344 0.00009 0.00271 0.00985 HKLF 4 REM ijsf1413 in R3 REM R1 = 0.0363 for 3948 Fo > 4sig(Fo) and 0.0404 for all 4199 data REM 236 parameters refined using 1 restraints END WGHT 0.0398 2.4699 REM Highest difference peak 0.265, deepest hole -0.227, 1-sigma level 0.045 Q1 1 -0.4635 -0.3490 -0.4512 11.00000 0.05 0.27 Q2 1 -0.4208 -0.3391 -0.5479 11.00000 0.05 0.26 Q3 1 -0.5311 -0.4673 -0.5179 11.00000 0.05 0.25 Q4 1 -0.6169 -0.5304 -0.3311 11.00000 0.05 0.24 Q5 1 -0.7122 -0.4623 -0.7291 11.00000 0.05 0.22 Q6 1 -0.6957 -0.4871 -0.8764 11.00000 0.05 0.22 Q7 1 -0.7002 -0.4304 -0.8239 11.00000 0.05 0.22 Q8 1 -0.6711 -0.5849 -0.2738 11.00000 0.05 0.22 Q9 1 -0.5697 -0.4895 -0.3960 11.00000 0.05 0.21 Q10 1 -0.5557 -0.5195 -0.3079 11.00000 0.05 0.20 Q11 1 -0.6667 -0.3333 -0.3778 10.33333 0.05 0.20 Q12 1 -0.6496 -0.4906 -0.8279 11.00000 0.05 0.20 Q13 1 -0.3059 -0.2283 -0.5911 11.00000 0.05 0.20 Q14 1 -0.6696 -0.4594 -0.6807 11.00000 0.05 0.19 Q15 1 -0.6724 -0.5461 -0.3768 11.00000 0.05 0.19 Q16 1 -0.4791 -0.3993 -0.5217 11.00000 0.05 0.18 Q17 1 -0.6575 -0.5836 -0.1617 11.00000 0.05 0.18 Q18 1 -0.6590 -0.4994 -0.7237 11.00000 0.05 0.18 Q19 1 -0.5939 -0.4781 -0.5092 11.00000 0.05 0.17 Q20 1 -0.5555 -0.5416 -0.2001 11.00000 0.05 0.17 REM The information below was added by Olex2. REM REM R1 = 0.0363 for 3948 Fo > 4sig(Fo) and 0.0404 for all 6369 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.27, deepest hole -0.23 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0404 REM R1_gt = 0.0363 REM wR_ref = 0.0900 REM GOOF = 1.048 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 6369 REM Reflections_gt = 3948 REM Parameters = n/a REM Hole = -0.23 REM Peak = 0.27 REM Flack = -0.5(5) ; _cod_data_source_file cs6b03121_si_002.cif _cod_data_source_block ijsf1413 _cod_original_cell_volume 3985.4(2) _cod_database_code 4514161 _shelx_shelxl_version_number 2014/7 _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. ; _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: C2(H2) 2.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C20(H20A,H20B,H20C) ; _olex2_date_sample_data_collection 2014-02-03 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 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 C1 C -0.46413(10) -0.33895(10) -0.38047(18) 0.0151(3) Uani 1 1 d . C2 C -0.46077(10) -0.35793(10) -0.52389(18) 0.0138(3) Uani 1 1 d . H2 H -0.4888 -0.3426 -0.5779 0.017 Uiso 1 1 calc R C3 C -0.49312(10) -0.44061(10) -0.53732(19) 0.0161(4) Uani 1 1 d . H3A H -0.4963 -0.4527 -0.6298 0.019 Uiso 1 1 calc R H3B H -0.4603 -0.4541 -0.4963 0.019 Uiso 1 1 calc R C4 C -0.56697(10) -0.48463(10) -0.47684(19) 0.0148(3) Uani 1 1 d . C5 C -0.57970(11) -0.51575(10) -0.34686(19) 0.0159(4) Uani 1 1 d . C6 C -0.53441(11) -0.51854(11) -0.2492(2) 0.0195(4) Uani 1 1 d . H6 H -0.4843 -0.4941 -0.2602 0.023 Uiso 1 1 calc R C7 C -0.56570(12) -0.55826(12) -0.1365(2) 0.0222(4) Uani 1 1 d . H7 H -0.5361 -0.5606 -0.0717 0.027 Uiso 1 1 calc R C8 C -0.64138(12) -0.59514(11) -0.1180(2) 0.0215(4) Uani 1 1 d . H8 H -0.6610 -0.6220 -0.0417 0.026 Uiso 1 1 calc R C9 C -0.68718(11) -0.59219(11) -0.2117(2) 0.0206(4) Uani 1 1 d . H9 H -0.7372 -0.6159 -0.1988 0.025 Uiso 1 1 calc R C10 C -0.65568(10) -0.55241(10) -0.32606(19) 0.0164(4) Uani 1 1 d . C11 C -0.63375(10) -0.50234(10) -0.52774(19) 0.0157(3) Uani 1 1 d . C12 C -0.65506(10) -0.48442(10) -0.65407(18) 0.0158(4) Uani 1 1 d . C13 C -0.70585(11) -0.46054(11) -0.6538(2) 0.0202(4) Uani 1 1 d . H13 H -0.7238 -0.4545 -0.5744 0.024 Uiso 1 1 calc R C14 C -0.72953(12) -0.44580(12) -0.7709(2) 0.0241(4) Uani 1 1 d . H14 H -0.7636 -0.4305 -0.7699 0.029 Uiso 1 1 calc R C15 C -0.70206(12) -0.45405(12) -0.8898(2) 0.0249(4) Uani 1 1 d . H15 H -0.7179 -0.4444 -0.9684 0.030 Uiso 1 1 calc R C16 C -0.65124(12) -0.47662(11) -0.8913(2) 0.0234(4) Uani 1 1 d . H16 H -0.6326 -0.4814 -0.9709 0.028 Uiso 1 1 calc R C17 C -0.62780(12) -0.49228(11) -0.7740(2) 0.0199(4) Uani 1 1 d . H17 H -0.5940 -0.5079 -0.7757 0.024 Uiso 1 1 calc R C18 C -0.53198(15) -0.31477(16) -0.2262(2) 0.0342(6) Uani 1 1 d . H18A H -0.5471 -0.3580 -0.1751 0.051 Uiso 1 1 calc GR H18B H -0.5691 -0.3016 -0.2235 0.051 Uiso 1 1 calc GR H18C H -0.4877 -0.2759 -0.1906 0.051 Uiso 1 1 calc GR C19 C -0.34349(10) -0.24901(10) -0.55986(18) 0.0159(4) Uani 1 1 d . C20 C -0.26686(11) -0.21826(11) -0.6100(2) 0.0234(4) Uani 1 1 d . H20A H -0.2333 -0.1950 -0.5391 0.035 Uiso 1 1 calc GR H20B H -0.2579 -0.1834 -0.6779 0.035 Uiso 1 1 calc GR H20C H -0.2607 -0.2568 -0.6448 0.035 Uiso 1 1 calc GR N1 N -0.38618(9) -0.32192(9) -0.56954(17) 0.0166(3) Uani 1 1 d . H1 H -0.3666(14) -0.3481(14) -0.594(3) 0.023(7) Uiso 1 1 d . N2 N -0.68736(9) -0.54196(9) -0.43566(17) 0.0178(3) Uani 1 1 d . H2A H -0.7317(16) -0.5641(15) -0.454(3) 0.025(7) Uiso 1 1 d . O1 O -0.52005(8) -0.32810(8) -0.36099(14) 0.0209(3) Uani 1 1 d . O2 O -0.42368(7) -0.33635(8) -0.29487(14) 0.0196(3) Uani 1 1 d . O3 O -0.36631(8) -0.21082(7) -0.51249(14) 0.0192(3) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0124(8) 0.0121(8) 0.0185(8) 0.0011(7) 0.0026(7) 0.0044(7) C2 0.0117(8) 0.0124(8) 0.0168(8) 0.0000(6) 0.0010(6) 0.0055(7) C3 0.0131(8) 0.0130(8) 0.0205(8) -0.0015(7) 0.0018(7) 0.0053(7) C4 0.0128(8) 0.0121(8) 0.0185(8) -0.0003(7) 0.0010(7) 0.0055(7) C5 0.0152(9) 0.0131(8) 0.0188(8) -0.0015(7) -0.0002(7) 0.0066(7) C6 0.0176(9) 0.0161(9) 0.0242(10) -0.0016(8) -0.0014(8) 0.0080(8) C7 0.0275(11) 0.0182(9) 0.0221(9) -0.0020(8) -0.0055(8) 0.0123(8) C8 0.0275(11) 0.0158(9) 0.0187(9) 0.0017(7) 0.0016(8) 0.0089(8) C9 0.0190(9) 0.0173(9) 0.0229(9) 0.0014(7) 0.0040(8) 0.0072(8) C10 0.0143(9) 0.0136(8) 0.0198(8) -0.0003(7) 0.0003(7) 0.0060(7) C11 0.0139(8) 0.0117(8) 0.0188(8) -0.0008(7) 0.0019(7) 0.0045(7) C12 0.0122(8) 0.0118(8) 0.0195(9) 0.0006(7) -0.0003(7) 0.0031(7) C13 0.0178(9) 0.0205(10) 0.0217(9) 0.0014(8) 0.0020(7) 0.0092(8) C14 0.0199(10) 0.0259(11) 0.0278(10) 0.0016(9) -0.0029(8) 0.0125(9) C15 0.0256(11) 0.0252(11) 0.0209(10) -0.0001(8) -0.0065(8) 0.0105(9) C16 0.0265(11) 0.0209(10) 0.0187(9) -0.0048(8) 0.0001(8) 0.0088(9) C17 0.0193(9) 0.0168(9) 0.0231(9) -0.0030(7) 0.0000(8) 0.0086(8) C18 0.0396(14) 0.0505(16) 0.0224(11) -0.0052(10) 0.0057(10) 0.0299(13) C19 0.0159(9) 0.0159(9) 0.0145(8) 0.0018(7) 0.0018(7) 0.0070(7) C20 0.0160(9) 0.0178(9) 0.0313(11) 0.0003(8) 0.0068(8) 0.0047(8) N1 0.0138(7) 0.0140(8) 0.0228(8) 0.0009(6) 0.0056(6) 0.0074(6) N2 0.0116(8) 0.0179(8) 0.0208(8) 0.0024(6) 0.0008(6) 0.0048(7) O1 0.0204(7) 0.0282(8) 0.0199(7) -0.0010(6) 0.0027(5) 0.0165(6) O2 0.0161(7) 0.0203(7) 0.0205(7) -0.0007(6) -0.0024(6) 0.0077(6) O3 0.0198(7) 0.0157(7) 0.0234(7) 0.0001(6) 0.0027(6) 0.0098(6) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1 2 0 0.0846 -1.0001 2.0001 -0.0000 0.0238 -0.0396 0.0482 5 0 3 0.1106 5.0001 0.0001 3.0001 0.2036 -0.0910 -0.1757 5 -1 0 0.0631 5.0000 -0.9998 0.0000 0.1486 0.0764 -0.0571 1 1 0 0.0807 0.9999 1.0001 -0.0000 0.0654 -0.0009 0.0131 0 5 1 0.0946 -0.0003 5.0002 0.9999 0.1571 -0.1188 0.0558 0 1 -1 0.0984 -0.0001 1.0001 -1.0000 0.0213 0.0378 0.0668 -1 1 1 0.0874 -1.0000 1.0000 1.0000 0.0025 -0.0774 -0.0186 0 0 -1 0.1285 -0.0000 0.0001 -1.0000 -0.0084 0.0513 0.0463 -2 -1 -1 0.1177 -2.0000 -1.0001 -1.0000 -0.1095 0.0396 0.0406 3 -2 0 0.0709 3.0001 -2.0000 0.0000 0.0475 0.0647 -0.0629 1 0 0 0.0689 1.0000 0.0001 -0.0000 0.0357 0.0126 -0.0073 -1 -1 0 0.0806 -0.9999 -1.0001 0.0000 -0.0654 0.0009 -0.0131 1 -2 0 0.0968 1.0001 -2.0001 0.0000 -0.0238 0.0396 -0.0482 -1 0 0 0.0883 -1.0000 -0.0001 0.0000 -0.0357 -0.0126 0.0073 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 C1 C2 110.58(16) O2 C1 C2 125.24(17) O2 C1 O1 124.13(17) C1 C2 H2 109.4 C1 C2 C3 109.48(15) C3 C2 H2 109.4 N1 C2 C1 110.52(15) N1 C2 H2 109.4 N1 C2 C3 108.70(15) C2 C3 H3A 108.8 C2 C3 H3B 108.8 H3A C3 H3B 107.7 C4 C3 C2 113.98(15) C4 C3 H3A 108.8 C4 C3 H3B 108.8 C5 C4 C3 124.07(17) C11 C4 C3 129.14(18) C11 C4 C5 106.78(17) C6 C5 C4 133.83(19) C6 C5 C10 119.22(18) C10 C5 C4 106.88(17) C5 C6 H6 120.6 C7 C6 C5 118.83(19) C7 C6 H6 120.6 C6 C7 H7 119.4 C6 C7 C8 121.3(2) C8 C7 H7 119.4 C7 C8 H8 119.5 C9 C8 C7 121.07(19) C9 C8 H8 119.5 C8 C9 H9 121.1 C8 C9 C10 117.75(19) C10 C9 H9 121.1 C9 C10 C5 121.84(18) N2 C10 C5 107.78(16) N2 C10 C9 130.36(18) C4 C11 C12 131.75(18) C4 C11 N2 109.48(17) N2 C11 C12 118.72(17) C13 C12 C11 118.84(17) C17 C12 C11 122.13(18) C17 C12 C13 119.01(18) C12 C13 H13 119.6 C14 C13 C12 120.7(2) C14 C13 H13 119.6 C13 C14 H14 120.2 C13 C14 C15 119.7(2) C15 C14 H14 120.2 C14 C15 H15 119.9 C16 C15 C14 120.2(2) C16 C15 H15 119.9 C15 C16 H16 119.8 C15 C16 C17 120.4(2) C17 C16 H16 119.8 C12 C17 C16 120.00(19) C12 C17 H17 120.0 C16 C17 H17 120.0 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 O1 C18 H18A 109.5 O1 C18 H18B 109.5 O1 C18 H18C 109.5 N1 C19 C20 115.62(17) O3 C19 C20 122.82(18) O3 C19 N1 121.57(18) 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 C2 N1 H1 119.6(17) C19 N1 C2 120.78(16) C19 N1 H1 119.1(17) C10 N2 C11 109.01(16) C10 N2 H2A 126.4(19) C11 N2 H2A 122.9(19) C1 O1 C18 115.64(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.526(3) C1 O1 1.334(2) C1 O2 1.206(2) C2 H2 0.9800 C2 C3 1.540(3) C2 N1 1.450(2) C3 H3A 0.9700 C3 H3B 0.9700 C3 C4 1.500(3) C4 C5 1.443(3) C4 C11 1.375(3) C5 C6 1.406(3) C5 C10 1.415(3) C6 H6 0.9300 C6 C7 1.382(3) C7 H7 0.9300 C7 C8 1.406(3) C8 H8 0.9300 C8 C9 1.387(3) C9 H9 0.9300 C9 C10 1.398(3) C10 N2 1.378(3) C11 C12 1.475(3) C11 N2 1.388(2) C12 C13 1.404(3) C12 C17 1.397(3) C13 H13 0.9300 C13 C14 1.390(3) C14 H14 0.9300 C14 C15 1.392(3) C15 H15 0.9300 C15 C16 1.384(3) C16 H16 0.9300 C16 C17 1.397(3) C17 H17 0.9300 C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C18 O1 1.449(3) C19 C20 1.509(3) C19 N1 1.353(2) C19 O3 1.233(2) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 N1 H1 0.88(3) N2 H2A 0.84(3) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.88(3) 2.07(3) 2.944(2) 171(2) 8_444 N2 H2A O3 0.84(3) 2.18(3) 3.010(2) 172(3) 3_445 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 C1 C2 C3 C4 51.5(2) C1 C2 N1 C19 -55.2(2) C2 C1 O1 C18 175.74(18) C2 C3 C4 C5 -96.7(2) C2 C3 C4 C11 81.9(2) C3 C2 N1 C19 -175.40(17) C3 C4 C5 C6 -3.6(3) C3 C4 C5 C10 179.60(17) C3 C4 C11 C12 -0.5(3) C3 C4 C11 N2 -177.94(18) C4 C5 C6 C7 -175.3(2) C4 C5 C10 C9 176.50(18) C4 C5 C10 N2 -2.1(2) C4 C11 C12 C13 -134.0(2) C4 C11 C12 C17 47.7(3) C4 C11 N2 C10 -2.2(2) C5 C4 C11 C12 178.27(19) C5 C4 C11 N2 0.8(2) C5 C6 C7 C8 -0.4(3) C5 C10 N2 C11 2.6(2) C6 C5 C10 C9 -0.8(3) C6 C5 C10 N2 -179.38(17) C6 C7 C8 C9 -0.8(3) C7 C8 C9 C10 1.1(3) C8 C9 C10 C5 -0.3(3) C8 C9 C10 N2 177.9(2) C9 C10 N2 C11 -175.8(2) C10 C5 C6 C7 1.2(3) C11 C4 C5 C6 177.5(2) C11 C4 C5 C10 0.7(2) C11 C12 C13 C14 -177.49(18) C11 C12 C17 C16 178.12(18) C12 C11 N2 C10 -179.99(17) C12 C13 C14 C15 -0.7(3) C13 C12 C17 C16 -0.2(3) C13 C14 C15 C16 -0.2(3) C14 C15 C16 C17 0.9(3) C15 C16 C17 C12 -0.7(3) C17 C12 C13 C14 0.8(3) C20 C19 N1 C2 179.59(17) N1 C2 C3 C4 172.32(16) N2 C11 C12 C13 43.2(3) N2 C11 C12 C17 -135.1(2) O1 C1 C2 C3 -100.79(18) O1 C1 C2 N1 139.51(16) O2 C1 C2 C3 76.9(2) O2 C1 C2 N1 -42.8(2) O2 C1 O1 C18 -2.0(3) O3 C19 N1 C2 -0.1(3) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 -12 17558 1238.34 2 0 0 -9 169104 4081.44 2 0 0 -6 40589.7 1360.52 2 0 0 -3 706976 11818.2 2 0 0 6 37988 1221.46 4 0 0 9 163469 3766.6 4 0 0 12 17566 1120.82 4 1 -1 -13 7438.62 835.905 2 0 1 -13 6630.45 821.409 2 0 1 -10 4191.95 554.423 2 -1 0 -10 3693.45 519.728 2 1 -1 -10 3496.18 481.249 2 1 -1 -7 89200.8 2356.33 2 -1 0 -7 87407.7 2348.51 2 0 1 -7 85800.5 2389.9 2 -1 0 -4 996.296 177.607 2 0 1 -4 1071.84 191.095 2 1 -1 -4 835.818 147.673 2 1 -1 2 159442 2954.81 2 0 1 2 163851 2881.97 2 0 1 2 163120 2854.51 4 0 1 5 42805.6 1195.39 4 0 1 5 42288.7 1121.35 3 -1 0 5 44250.6 1028.97 3 -1 0 5 39502.1 1199.42 4 0 1 8 49477 1603.46 4 1 -1 8 49336.8 1597.39 4 -1 0 8 53085.4 1364.29 3 -1 0 8 51959.5 1669.98 4 1 -1 11 211.155 178.987 4 0 1 11 325.784 192.412 4 -1 0 11 538.194 234.464 4 1 0 -14 2485.89 548.675 2 -1 1 -11 623.263 248.42 2 0 -1 -11 619.126 327.088 2 1 0 -11 88.3565 214.631 2 1 0 -8 51698.1 1795.83 2 0 -1 -8 48434.5 1700.07 2 -1 1 -8 51510.5 1796.58 2 1 0 -5 44210.2 1320.42 2 0 -1 -5 42977.6 1301.77 2 -1 1 -5 44167.7 1356.73 2 0 -1 -2 160825 2854.7 2 0 -1 -2 160155 2824.58 4 -1 1 -2 162545 2934.95 2 1 0 -2 157300 2875.14 2 -1 1 4 873.201 112.916 3 1 0 4 779.248 130.583 4 -1 1 4 801.061 148.491 4 0 -1 7 84591.3 2181.47 4 -1 1 7 86901 1951.59 3 1 0 7 86589.9 2142.92 4 -1 1 7 83849 2181.36 4 1 0 10 4810.96 515.903 4 0 -1 10 4219.5 492.551 4 -1 1 10 3620.37 457.277 4 0 -1 13 8047.88 795.058 4 -1 1 13 7139.79 746.262 4 1 0 13 7432.56 748.805 4 1 1 -15 5566.61 818.676 2 1 1 -12 3284.94 582.668 2 -2 1 -12 2430.51 496.821 2 1 -2 -12 3259.57 532.534 2 -2 1 -9 37596.9 1584.69 2 1 1 -9 42299.8 1693.8 2 1 -2 -9 35964 1503.96 2 1 -2 -6 24901 986.091 2 1 1 -6 24628.2 1035.95 2 -2 1 -6 25179.9 1050.39 2 1 -2 -3 525457 8603.45 4 -2 1 -3 511840 8712.53 2 1 -2 -3 510090 8570 2 -2 1 3 102600 1871.8 3 1 1 3 105060 1992.44 4 -2 1 3 103733 2105.99 4 -2 1 6 31634.4 877.06 3 1 1 6 30930.5 1031.5 4 -2 1 6 30392 1092.49 4 1 -2 9 21468.5 1046.69 4 -2 1 9 21496 1072.32 4 1 1 9 20409.1 994.849 4 -2 1 12 238.551 205.302 4 1 -2 12 -161.738 198.036 4 1 1 12 -188.625 170.299 4 2 -3 -13 7585.77 818.728 2 1 2 -13 7720.49 901.343 2 1 2 -10 15681.1 1076.81 2 -3 1 -10 14434.2 1012.86 2 2 -3 -10 16321.4 1021.22 2 1 2 -7 39111.5 1491.19 2 -3 1 -7 40718 1481.61 2 2 -3 -7 41191.7 1400.57 2 2 -3 -4 59824.7 1435.32 4 1 2 -4 54953.2 1487.89 2 2 -3 -4 56559.2 1364.04 2 -3 1 -4 58243.2 1509.35 2 1 2 -1 581467 9576.89 1 -3 1 -1 587063 9560.72 1 1 2 2 59437.1 1345.82 3 -3 1 2 64766 1345.43 4 -3 1 5 18077.3 527.452 3 1 2 5 19818.5 746.652 3 -3 1 5 16525.3 741.435 4 1 2 5 18441.6 694.275 4 -3 1 8 2785.91 233.387 3 1 2 8 2795.19 351.1 4 -3 1 8 2275.43 337.235 4 1 2 11 11281 818.152 4 -3 1 11 12443.6 927.868 4 2 -3 11 14051.8 931.74 4 0 2 -14 7300.24 909.375 2 2 -2 -14 6361.95 803.448 2 0 2 -11 859.845 340.72 2 -2 0 -11 52.4798 221.657 2 2 -2 -11 808.39 271.254 2 2 -2 -8 6543.33 562.157 2 0 2 -8 6600.63 627.448 2 -2 0 -8 6903.63 610.741 2 -2 0 -5 100476 2335.61 2 2 -2 -5 99859.4 2258.81 2 0 2 -5 100034 2386.77 2 2 -2 -2 179722 3106.76 3 0 2 -2 180083 3269.2 2 2 -2 -2 180291 3220.96 4 2 -2 -2 179586 3129.05 2 2 -2 1 146780 2651.19 2 0 2 1 151359 2639.81 3 -2 0 4 98368 1813.2 3 0 2 4 101037 2077.97 4 0 2 4 100581 2077.46 3 -2 0 7 7755.83 376.655 3 0 2 7 7125.28 511.01 4 -2 0 7 6863.05 526.31 4 2 -2 7 7361.63 506.553 4 2 -2 10 30566.6 1334.49 4 -2 0 10 30568.8 1398.31 4 0 2 10 33816.2 1407.36 4 0 2 13 2322.92 433.007 4 -2 0 13 2437.71 466.841 4 2 -2 13 2158.75 412.459 4 2 -1 -12 -3.57979 234.234 2 -1 2 -12 -136.131 277.055 2 2 -1 -9 23140.7 1192.22 2 -1 -1 -9 19882.6 1086.94 2 -1 2 -9 20670.5 1168.71 2 -1 -1 -6 32331.3 1167.06 2 2 -1 -6 32218.6 1158.19 2 -1 2 -6 31817.9 1234.26 2 -1 2 -3 101843 2149.26 2 2 -1 -3 100654 2041 2 -1 -1 -3 102175 2063.95 2 -1 2 3 505870 8602.74 3 -1 2 3 510088 8674.73 4 -1 2 3 527551 8624.15 2 -1 2 6 24200.7 934.114 4 2 -1 6 24432.6 888.646 4 -1 2 6 25959.2 850.329 3 -1 -1 6 25388.2 728.27 3 -1 2 9 37277 1438.24 4 -1 -1 9 38350.3 1483.45 4 2 -1 9 39629.6 1424.53 4 -1 2 12 2559.81 443.357 4 -1 -1 12 2479.69 455.072 4 2 -1 12 2773.36 443.779 4 -2 2 -13 2084.82 510.964 2 2 0 -13 2192.7 499.772 2 -2 2 -10 31870.9 1544.67 2 2 0 -10 33580.9 1579.82 2 0 -2 -10 32132.4 1474.45 2 -2 2 -7 7018.17 594.117 2 0 -2 -7 7621.19 557.448 2 2 0 -7 6707.9 557.463 2 -2 2 -4 102776 2289.72 2 2 0 -4 98928.7 2186.09 2 0 -2 -4 99127.4 2119.2 2 0 -2 -1 155504 2727.93 3 -2 2 -1 155037 2743.65 2 -2 2 2 177475 3192.84 4 2 0 2 184973 3244.75 2 2 0 2 176303 3042.51 4 2 0 5 97501.8 2128.87 4 -2 2 5 99961.4 2041.12 3 -2 2 5 102687 2270.98 4 -2 2 8 5815.52 518.285 4 2 0 8 5801.11 477.24 4 0 -2 8 7111.69 406.846 3 0 -2 8 6316.47 530.864 4 -2 2 11 934.406 292.04 4 2 0 11 610.887 205.557 4 0 -2 11 741.729 272.056 4 2 1 -14 2938.18 580.944 2 -3 2 -11 11359.4 957.86 2 2 1 -11 11494.8 985.317 2 1 -3 -11 10196.5 838.962 2 2 1 -8 1496.61 315.154 2 -3 2 -8 1533.08 327.027 2 1 -3 -8 1627.13 280.693 2 1 -3 -5 139270 2855.98 2 2 1 -5 134171 2971.09 2 -3 2 -5 136565 3030.94 2 1 -3 -2 324938 5468.67 3 1 -3 -2 325200 5445.85 4 -3 2 -2 322358 5287.72 1 1 -3 -2 306262 5301.85 2 -3 2 -2 323615 5562.81 2 2 1 1 270688 4670.38 1 -3 2 1 279398 4646.53 4 1 -3 1 271862 4675.14 2 2 1 4 97493.3 1978.29 4 -3 2 4 98599.2 2153.93 4 -3 2 7 9420.07 629.263 4 2 1 7 8725 547.613 4 -3 2 7 11218.9 489.113 3 1 -3 10 10801 790.445 4 2 1 10 11760.8 779.399 4 -3 2 10 10662.7 811.763 4 -3 2 13 2694.65 475.808 4 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2 21 -10 -5 96104.1 3098.02 1 -11 21 -5 90810.6 2860 2 21 -10 -2 2656.32 427.675 1 21 -10 1 13725.3 904.435 1 21 -10 4 26832.3 1236.1 1 21 -9 -9 10290.7 1063.02 1 21 -9 -6 -39.7384 289.294 1 21 -9 -3 29723.8 1508.32 1 21 -9 0 7022.87 666.519 1 21 -9 3 21984.4 1159.93 1 21 -8 -10 762.184 379.325 1 21 -8 -7 4667.02 682.893 1 21 -8 -4 7659.99 796.146 1 21 -8 -1 2539.8 443.746 1 21 -8 2 5014.09 566.546 1 21 -8 5 10424.6 768.271 1 21 -7 -8 3725.26 618.788 1 21 -7 -5 18247.6 1243.5 1 21 -7 -2 6297.69 671.411 1 21 -7 1 12510.3 906.848 1 21 -7 4 11425.5 850.701 1 21 -6 -9 47756.2 2357.68 1 21 -6 -6 26772.7 1579.51 1 21 -6 -3 6794.94 720.797 1 21 -6 0 78614.1 2610.01 1 21 -6 3 2983.08 477.723 1 21 -6 6 4591.65 549.402 1 21 -5 -10 2497.02 545.004 1 21 -5 -10 2010.19 499.843 2 21 -5 -7 1959.57 501.819 1 21 -5 -4 10439.1 934.041 1 21 -5 -1 11122.4 925.249 1 21 -5 2 10854.5 895.667 1 21 -5 5 4799.05 581.062 1 21 -4 -8 736.487 380.09 1 21 -4 -5 2851.78 542.18 1 21 -4 -2 1427.19 411.767 1 21 -4 1 4547.2 594.768 1 21 -4 4 6652.68 697.337 1 21 -3 -9 11047.8 1118.25 1 21 -3 -6 1691.59 430.008 1 21 -3 -3 16287.9 1175.36 1 21 -3 0 5226.26 662.727 1 21 -3 3 6675.11 724.086 1 21 -3 6 2050.02 424.375 1 21 -2 -7 2332.64 552.067 1 21 -2 -4 3794.03 615.759 1 21 -2 -1 32334.2 1668.16 1 21 -2 2 14525.1 1086.58 1 -2 -19 2 14746.3 1008.05 3 21 -2 5 3050.68 521.502 1 21 -1 -8 6300.14 880.231 1 21 -1 -5 10636.4 1030.53 1 21 -1 -2 4623.47 654.824 1 21 -1 1 8555.18 853.395 1 -1 -20 1 8477.51 800.069 3 -1 -20 4 9156.72 764.578 3 21 -1 4 9176.36 882.386 1 21 0 -6 3014.19 599.688 1 21 0 -3 8719.08 908.993 1 21 0 0 7899.83 853.448 1 0 -21 0 6445.1 734.141 3 0 -21 3 8987.36 805.983 3 21 0 3 9354.55 914.253 1 21 1 -7 1206.89 477.548 1 21 1 -4 4616.64 700.203 1 21 1 -1 11099.3 1024.9 1 1 -22 -1 11312.2 1006.43 3 21 1 2 18802 1310.41 1 1 -22 2 18646.3 1228.74 3 21 1 5 4301.24 649.909 1 21 2 -8 2497.72 585.411 1 21 2 -5 2663.99 563.956 1 21 2 -2 5503.66 761.554 1 2 -23 -2 7043.94 818.582 3 2 -23 1 9023.84 873.104 3 21 2 1 6880.18 830.671 1 2 -23 4 7868.74 771.726 3 21 2 4 8545.32 920.757 1 21 3 -6 18897.2 1461.24 1 21 3 -3 1206 405.609 1 3 -24 0 6956.57 811.724 3 21 3 0 7873.54 906.927 1 3 -24 3 782.418 326.131 3 21 3 3 658.89 329.048 1 21 4 -4 31271.8 1885.51 1 21 4 -1 7738.64 923.45 1 4 -25 -1 5011.5 721.041 3 4 -25 2 8622.39 885.404 3 21 4 2 8724.59 951.191 1 21 5 -5 6730.33 909.284 1 21 5 -2 2740.91 584.326 1 5 -26 1 15191.3 1224.38 3 21 5 1 15685.3 1301.26 1 5 -26 4 7743.68 841.958 3 21 5 4 7777.86 945.731 1 21 6 -3 6366.78 880.818 1 21 6 0 1098.31 483.443 1 21 6 3 10248.2 1088.37 1 21 7 -1 3674.69 683.305 1 21 7 2 7860.05 973.052 1 5 22 -5 8827.22 954.722 2 4 22 -6 292.266 270.117 2 3 22 -7 3405.48 663.232 2 3 22 -4 1592.52 411.173 2 2 22 -5 497.638 278.936 2 1 22 -6 2825.93 547.439 2 22 -23 -6 2244.54 503.255 3 0 22 -7 1295.14 390.83 2 0 22 -4 25114.3 1445.08 2 -1 22 -8 2282.74 520.068 2 -1 22 -5 5733.57 707.796 2 -21 -1 7 614.12 301.275 4 -2 22 -9 3512.16 658.088 2 -2 22 -6 23293.8 1488.33 2 -20 -2 6 5319.5 634.375 4 -3 22 -7 8810.43 948.402 2 -3 22 -4 4949.4 613.076 2 22 -19 -1 32317 1468.07 1 -19 -3 5 1470.12 336.74 4 -4 22 -8 790.574 411.341 2 -4 22 -5 11378.7 964.299 2 22 -18 -2 14021.2 984.789 1 -18 -4 4 21830.4 1167.3 4 -18 -4 7 4476.24 619.522 4 -5 22 -9 4245.3 717.214 2 -5 22 -6 225.85 264.038 2 22 -17 -3 4685.44 607.714 1 -5 22 -3 5495.89 579.431 2 22 -17 0 8632.29 708.633 1 -17 -5 3 2554.36 378.4 4 -17 -5 6 8287.64 783.376 4 -6 22 -7 256.36 202.356 2 -6 22 -4 9228.17 804.572 2 22 -16 -4 8744.77 840.19 1 22 -16 -1 12523.3 894.957 1 -16 -6 5 2877.15 448.446 4 -7 22 -8 664.006 291.952 2 -7 22 -5 14231.6 1059.06 2 22 -15 -5 14806.2 1117.51 1 22 -15 -2 10144.3 842.564 1 22 -15 1 11974.6 809.593 1 -15 -7 7 40.6607 210.538 4 -8 22 -9 -91.5246 314.054 2 22 -14 -9 491.143 337.114 1 22 -14 -6 8178.69 858.548 1 -8 22 -6 8698.63 852.768 2 22 -14 -3 14516.2 1050.09 1 -8 22 -3 15869.5 955.814 2 22 -14 0 9733.94 767.119 1 -9 22 -10 769.963 355.863 2 22 -13 -7 883.003 380.077 1 -9 22 -7 701.253 342.274 2 22 -13 -4 19271 1245.97 1 -9 22 -4 17339.9 1072.37 2 22 -13 -1 28885 1417.13 1 22 -13 2 2034.46 356.643 1 22 -12 -8 1482.12 450.856 1 -10 22 -8 1648.92 463.624 2 22 -12 -5 28941.4 1602.8 1 -10 22 -5 28621.8 1471.65 2 22 -12 -2 965.227 297.554 1 22 -12 1 4489.22 531.098 1 22 -11 -9 2399.37 569.866 1 -11 22 -9 3487.87 640.697 2 22 -11 -6 3872.44 616.622 1 -11 22 -6 5368.53 664.261 2 22 -11 -3 5538.1 652.021 1 22 -11 0 16428.6 1048.36 1 22 -11 3 5718.12 574.087 1 22 -10 -7 18880.8 1387.34 1 22 -10 -4 16185.3 1149.4 1 22 -10 -1 1593.56 369.244 1 22 -10 2 24634.9 1262.66 1 22 -9 -8 3565.02 640.032 1 22 -9 -5 1738 447.215 1 22 -9 -2 706.535 296.022 1 22 -9 1 10405.4 833.833 1 22 -9 4 9135.11 742.396 1 22 -8 -9 1736.2 521.523 1 22 -8 -6 11016.8 1021.69 1 22 -8 -3 7205.16 759.726 1 22 -8 0 1163.87 339.974 1 22 -8 3 12292.4 899.042 1 22 -7 -7 17080.7 1327.23 1 22 -7 -4 7153.07 801.247 1 22 -7 -1 5312.46 641.998 1 22 -7 2 2046.38 417.406 1 22 -7 5 2335.85 401.683 1 22 -6 -8 13781.5 1238.81 1 22 -6 -5 8803.15 917.164 1 22 -6 -2 4540.48 611.618 1 22 -6 1 9534.01 841.143 1 22 -6 4 564.264 255.751 1 22 -5 -9 12477.8 1196.6 1 22 -5 -6 2242.75 537.5 1 22 -5 -3 609.819 327.573 1 22 -5 0 17970.2 1193.5 1 22 -5 3 1966.33 404.08 1 22 -5 6 2177.99 420.469 1 22 -4 -10 338.611 313.805 2 22 -4 -7 10474.1 1064.26 1 22 -4 -4 6392.26 794.965 1 22 -4 -1 3684.21 581.453 1 22 -4 2 6977.99 753.07 1 22 -4 5 11568.3 957.979 1 22 -3 -8 3469.6 657.113 1 22 -3 -5 9120.72 945.888 1 22 -3 -2 10161.2 950.333 1 22 -3 1 29379.4 1605.71 1 22 -3 4 8868.12 853.53 1 22 -2 -6 3643.03 633.661 1 22 -2 -3 8440.72 891.051 1 22 -2 0 2380.79 507.262 1 22 -2 3 7836.97 821.76 1 22 -1 -7 4028.26 692.747 1 22 -1 -4 4077.52 648.221 1 22 -1 -1 6258.99 787.119 1 -1 -21 2 4236.74 582.878 3 22 -1 2 4823.91 668.065 1 22 -1 5 2544.29 534.745 1 22 0 -5 13602.8 1227.5 1 22 0 -2 317.776 342.034 1 22 0 1 4082.56 660.553 1 0 -22 1 4498.32 614.906 3 22 0 4 24676 1542.64 1 22 1 -6 2954.66 616.841 1 22 1 -3 18632.3 1399.96 1 22 1 0 1030.84 416.432 1 1 -23 0 816.3 329.168 3 1 -23 3 17014.4 1182.05 3 22 1 3 17352.6 1305.81 1 22 2 -7 18480.1 1503.9 1 22 2 -4 18923.1 1446.96 1 22 2 -1 1008.83 384.262 1 2 -24 -1 1875.16 486.222 3 22 2 2 337.208 333.292 1 2 -24 2 345.628 274.634 3 22 2 5 14039.6 1217.98 1 22 3 -5 19890 1524.08 1 22 3 -2 3488.34 671.981 1 22 3 1 12668.9 1158.92 1 3 -25 1 15182.5 1196.03 3 22 3 4 45287.3 2267.56 1 22 4 -3 694.137 453.521 1 22 4 0 14452.5 1264.1 1 22 4 3 -418.169 332.812 1 4 -26 3 -161.821 248.053 3 22 5 -4 671.461 376.938 1 22 5 -1 -197.597 338.176 1 22 5 2 1398.23 458.624 1 22 6 -2 5803.31 855.489 1 22 6 1 17404 1445.41 1 2 23 -6 95.157 259.752 2 1 23 -7 955.325 379.53 2 0 23 -8 4944.15 800.174 2 0 23 -5 3375.61 557.27 2 -1 23 -6 240.661 197.427 2 -2 23 -7 2355.39 511.532 2 23 -21 -1 7909.45 723.861 1 -3 23 -8 1202.65 438.775 2 -3 23 -5 9524.08 901.996 2 23 -20 -2 2553.61 447.904 1 -20 -3 7 11351.5 978.614 4 -4 23 -9 5129.79 811.909 2 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490.26 1 -10 23 -6 1779.23 401.473 2 23 -13 -3 10969.8 929.351 1 23 -13 0 -13.7445 195.765 1 23 -12 -7 10616.1 1065.6 1 -11 23 -7 10936.1 1013.3 2 23 -12 -4 20698 1337.61 1 -11 23 -4 20399.3 1162.84 2 23 -12 -1 7844.92 747.255 1 23 -12 2 5480.95 574.84 1 23 -11 -8 9126.19 1019.99 1 23 -11 -5 10484.5 987.714 1 23 -11 -2 872.907 299.843 1 23 -11 1 367.506 256.693 1 23 -10 -9 9812.87 1076.17 1 23 -10 -6 1317.62 432.102 1 23 -10 -3 11058.6 948.372 1 23 -10 0 24238.9 1331.96 1 23 -10 3 426.024 235.042 1 23 -9 -7 6993.7 868.051 1 23 -9 -4 4429.33 631.892 1 23 -9 -1 6414.4 702.559 1 23 -9 2 6277.87 669.497 1 23 -8 -8 6921.95 892.119 1 23 -8 -5 1845.37 478.068 1 23 -8 -2 314.941 312.964 1 23 -8 1 12548.8 966.835 1 23 -8 4 5868.37 636.095 1 23 -7 -6 12329.5 1107.16 1 23 -7 -3 6483.56 766.234 1 23 -7 0 2683.28 501.129 1 23 -7 3 22201 1308.49 1 23 -6 -10 6157.11 856.447 2 23 -6 -7 2375.53 519.473 1 23 -6 -4 26071.2 1580.84 1 23 -6 -1 20809.1 1341.21 1 23 -6 2 15665.5 1131.95 1 23 -6 5 471.337 240.254 1 23 -5 -8 4360.09 728.294 1 23 -5 -5 11251.2 1060.1 1 23 -5 -2 4149.44 628.508 1 23 -5 1 3623.7 591.867 1 23 -5 4 953.027 339.827 1 23 -4 -6 8782.89 981.632 1 23 -4 -3 6113.45 792.989 1 23 -4 0 1489.78 422.705 1 23 -4 3 8065.3 834.322 1 23 -4 6 4147.24 599.175 1 23 -3 -7 14380.1 1296.38 1 23 -3 -4 2607.46 557.577 1 23 -3 -1 986.964 370.051 1 23 -3 2 5485.95 726.855 1 23 -3 5 2805.26 522.744 1 23 -2 -5 6197.88 824.799 1 23 -2 -2 7953.25 901.768 1 23 -2 1 14370 1174.11 1 23 -2 4 814.82 354.4 1 23 -1 -6 3772.22 697.426 1 23 -1 -3 8322.5 938.582 1 23 -1 0 8271.5 920.536 1 23 -1 3 3070.34 588.199 1 -1 -22 3 2795 475.794 3 23 0 -4 8364.72 950.786 1 23 0 -1 2667.42 558.04 1 23 0 2 -117.181 266.839 1 0 -23 2 -224.56 244.998 3 23 0 5 3776.37 634.312 1 23 1 -5 6032.61 843.792 1 23 1 -2 2751.74 565.772 1 1 -24 1 5589.46 727.743 3 23 1 1 6101.12 827.945 1 23 1 4 3284.24 622.612 1 23 2 -3 8320.24 1011.67 1 23 2 0 -6.09679 326.833 1 2 -25 3 16760.9 1213.46 3 23 2 3 15272.8 1302.92 1 23 3 -4 4074.35 736.11 1 23 3 -1 18408.7 1470.97 1 23 3 2 5165.85 781.712 1 23 4 -2 17977.5 1506.57 1 23 4 1 28232.2 1818.78 1 23 4 4 3694.2 705.879 1 23 5 0 3305.75 688.147 1 -1 24 -7 -301.796 288.107 2 -2 24 -8 1845.12 499.75 2 24 -22 -2 354.57 180.856 1 -3 24 -6 -425.75 276.661 2 24 -21 -3 852.015 327.709 1 -4 24 -7 1208.35 444.294 2 24 -20 -4 16603.1 1214.23 1 24 -20 -1 11969.7 908.511 1 -5 24 -8 1926.59 512.235 2 24 -19 -5 5034.71 717.34 1 24 -19 -2 2196.02 429.271 1 -6 24 -9 81.7938 259.707 2 -6 24 -6 3514.14 590.817 2 24 -18 -6 2811.84 543.297 1 24 -18 -3 10308.1 916.14 1 24 -18 0 8481.56 733.465 1 -18 -6 6 13819 1060.5 4 24 -17 -7 108.306 298.288 1 -7 24 -7 -968.899 363.509 2 24 -17 -4 13331.4 1082.56 1 24 -17 -1 10574.5 862.713 1 -17 -7 5 202.957 174.935 4 24 -16 -8 5318.51 797.938 1 -8 24 -8 4186.92 687.787 2 24 -16 -5 691.689 342.34 1 24 -16 -2 5169.9 644.556 1 24 -16 1 4580.36 543.34 1 -9 24 -9 2119.29 527.857 2 24 -15 -6 6241.37 803.117 1 -9 24 -6 6611.73 772.985 2 24 -15 -3 3510.86 558.402 1 24 -15 0 5075.5 584.217 1 -10 24 -7 6821.22 805.211 2 24 -14 -7 7962.17 934.531 1 24 -14 -4 29964.8 1660.3 1 24 -14 -1 17848.1 1144.33 1 24 -14 2 30264.6 1405.6 1 24 -13 -8 294.998 298.668 1 -11 24 -8 633.065 288.676 2 24 -13 -5 2542.57 521.802 1 -11 24 -5 2209.33 427.529 2 24 -13 -2 35597.6 1728.59 1 24 -13 1 14645.6 1004.47 1 24 -12 -6 3109.97 611.247 1 24 -12 -3 298.709 229.666 1 24 -12 0 3404.17 530.21 1 24 -12 3 1089.72 277.383 1 24 -11 -7 11071 1106.25 1 24 -11 -4 44597.9 2081.92 1 24 -11 -1 9583.66 870.944 1 24 -11 2 5548.04 620.081 1 24 -10 -8 3452.31 670.955 1 24 -10 -5 5651.54 758.793 1 24 -10 -2 4715.32 650.333 1 24 -10 1 6183.24 690.578 1 24 -9 -6 13248.1 1174.09 1 24 -9 -3 14447.6 1139.47 1 24 -9 0 15449.7 1125.32 1 24 -9 3 2430.93 449.722 1 24 -8 -7 17898.3 1420.38 1 24 -8 -4 8422.11 917.435 1 24 -8 -1 13813.4 1082.26 1 24 -8 2 9399.17 864.953 1 24 -7 -8 4382.59 745.358 1 24 -7 -5 5054.66 734.915 1 24 -7 -2 2647.79 527.01 1 24 -7 1 10780.6 961.289 1 24 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956.919 1 24 3 3 9623.91 1084.42 1 25 -23 -3 17073.1 1199.71 1 25 -22 -4 39759.8 1958.32 1 -4 25 -8 18.7559 257.059 2 25 -21 -5 3890.31 656.705 1 25 -21 -2 8943.64 839.789 1 25 -20 -6 5688.89 796.531 1 25 -20 -3 13978.1 1088.58 1 -6 25 -7 1519.71 429.265 2 25 -19 -7 1507.53 464.928 1 25 -19 -4 4432.18 655.067 1 25 -19 -1 13284.8 989.516 1 -7 25 -8 1021.49 392.33 2 25 -18 -5 2773.14 533.406 1 25 -18 -2 5415.01 667.249 1 25 -17 -6 6334.77 833.395 1 25 -17 -3 4865.62 662.786 1 25 -17 0 4276.15 546.099 1 -17 -8 6 6733.53 743.337 4 25 -16 -7 4825.11 746.72 1 -9 25 -7 4298.77 653.116 2 25 -16 -4 1765.46 455.945 1 25 -16 -1 963.579 292.145 1 -10 25 -8 446.333 282.764 2 25 -15 -5 670.779 343.902 1 25 -15 -2 5720.74 690.97 1 25 -15 1 1245.91 348.177 1 -11 25 -9 4133.01 709.8 2 25 -14 -6 941.529 417.155 1 25 -14 -3 589.666 302.873 1 25 -14 0 10106.8 867.902 1 25 -13 -7 2497.29 591.771 1 25 -13 -4 6092.8 774.778 1 25 -13 -1 377.608 237.491 1 25 -13 2 7278.19 711.805 1 25 -12 -5 1708.87 508.804 1 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850.781 1 26 -2 1 11377.5 1136.69 1 26 -2 4 8236.24 952.406 1 26 -1 0 16613.9 1410.81 1 26 -1 3 307.857 345.598 1 26 0 -1 1976.64 572.718 1 26 0 2 13257.8 1241.47 1 27 -23 -4 2922.23 564.459 1 27 -22 -5 -256.898 260.598 1 27 -21 -3 9307.54 926.586 1 27 -20 -4 8742.85 932.297 1 27 -19 -5 9145.73 981.971 1 27 -19 -2 2289.79 459.399 1 27 -18 -6 452.925 324.252 1 27 -18 -3 2026.7 448.787 1 27 -17 -4 4651.03 706.155 1 27 -17 -1 9606.41 883.728 1 27 -16 -5 1572.49 465.058 1 27 -16 -2 -338.149 244.162 1 27 -15 -6 1385.16 488.863 1 27 -15 -3 7117.69 840.606 1 27 -15 0 771.83 298.998 1 27 -14 -4 5376.92 751.606 1 27 -14 -1 -158.534 277.632 1 27 -13 -5 4032.61 677.72 1 27 -13 -2 11182.4 1030.61 1 27 -13 1 4650.13 626.835 1 27 -12 -6 5129.94 788.324 1 27 -12 -3 10918.5 1056.58 1 27 -12 0 -91.874 252.732 1 27 -11 -4 15067.6 1282.73 1 27 -11 -1 1093.18 406.087 1 27 -11 2 6830.25 766.285 1 27 -10 -5 768.268 390.249 1 27 -10 -2 2069.9 475.114 1 27 -10 1 9947.27 944.788 1 27 -9 -3 6346.75 826.03 1 27 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