#------------------------------------------------------------------------------ #$Date: 2021-07-28 00:32:24 +0300 (Wed, 28 Jul 2021) $ #$Revision: 267765 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/89/4518921.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_4518921 loop_ _publ_author_name 'Song, Yulong' 'Fu, Chunling' 'Ma, Shengming' _publ_section_title ; Copper-Catalyzed Syntheses of Multiple Functionalizatized Allenes via Three-Component Reaction of Enynes ; _journal_name_full 'ACS Catalysis' _journal_page_first 10007 _journal_page_last 10013 _journal_paper_doi 10.1021/acscatal.1c02140 _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_moiety 'C25 H23 N3 O' _chemical_formula_sum 'C25 H23 N3 O' _chemical_formula_weight 381.46 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-07-22 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.436(4) _cell_length_b 9.724(3) _cell_length_c 22.389(9) _cell_measurement_reflns_used 9984 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 27.06 _cell_measurement_theta_min 2.28 _cell_volume 2054.3(14) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing.data_collection 'Bruker Instrument Service vV6.2.10' _computing.data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 170.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'zju Bruker D8 Venture Ims3.0' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_unetI/netI 0.0298 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 25642 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.152 _diffrn_reflns_theta_min 2.283 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1521 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.9038. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.233 _exptl_crystal_description plate _exptl_crystal_F_000 808 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.159 _refine_diff_density_min -0.125 _refine_diff_density_rms 0.029 _refine_ls_abs_structure_details ; Flack x determined using 1772 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.2(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4542 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0283 _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^)+(0.0338P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.0714 _reflns_Friedel_coverage 0.748 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.994 _reflns_number_gt 4303 _reflns_number_total 4542 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c02140_si_002.cif _cod_data_source_block 200721_syl_6_110_0m _cod_database_code 4518921 _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. ; _shelx_estimated_absorpt_t_max 0.986 _shelx_estimated_absorpt_t_min 0.969 _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 Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B) 2.b Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19) 2.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C) ; _shelx_res_file ; TITL 200721_syl_6_110_0m_a.res in P2(1)2(1)2(1) 200721_syl_6_110_0m.res created by SHELXL-2018/3 at 14:08:13 on 22-Jul-2020 REM Old TITL 200721_SYL_6_110_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.097, Rweak 0.021, Alpha 0.001 REM 1.768 for 23 systematic absences, Orientation as input REM Flack x = 0.091 ( 0.446 ) from 1680 Parsons' quotients REM Formula found by SHELXT: C25 N3 O CELL 0.71073 9.4361 9.7239 22.3891 90 90 90 ZERR 4 0.0043 0.0034 0.0091 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 100 92 12 4 L.S. 4 0 0 PLAN 20 SIZE 0.19 0.26 0.42 TEMP -103.15 BOND $h htab list 4 fmap 2 53 acta REM REM REM WGHT 0.033800 0.278000 FVAR 0.50804 O1 4 0.748742 0.213984 0.221185 11.00000 0.02696 0.03906 = 0.03716 -0.00983 0.00413 -0.00082 N1 3 0.601638 0.618574 0.381247 11.00000 0.03242 0.03013 = 0.02403 -0.00042 0.00174 -0.00250 N2 3 0.132294 0.641419 0.469234 11.00000 0.03190 0.03951 = 0.04294 -0.00816 -0.00236 0.00521 N3 3 0.778300 -0.150490 0.276424 11.00000 0.04455 0.05063 = 0.03489 -0.01228 -0.00282 0.01162 C1 1 0.814445 0.380308 0.298046 11.00000 0.02105 0.03423 = 0.02765 0.00411 0.00043 -0.00114 AFIX 43 H1 2 0.911987 0.356444 0.296318 11.00000 -1.20000 AFIX 0 C2 1 0.716560 0.317176 0.261282 11.00000 0.02698 0.03079 = 0.02353 0.00163 0.00309 -0.00140 C3 1 0.572312 0.353657 0.262557 11.00000 0.02445 0.03892 = 0.02789 -0.00320 -0.00399 -0.00278 AFIX 43 H3 2 0.507574 0.307781 0.236886 11.00000 -1.20000 AFIX 0 C4 1 0.523350 0.454737 0.300383 11.00000 0.02247 0.03732 = 0.02780 0.00040 -0.00107 0.00098 AFIX 43 H4 2 0.426228 0.480457 0.300739 11.00000 -1.20000 AFIX 0 C5 1 0.621052 0.518050 0.338132 11.00000 0.02724 0.02949 = 0.02139 0.00319 0.00155 -0.00223 C6 1 0.765365 0.480975 0.338114 11.00000 0.02539 0.03172 = 0.02304 0.00437 -0.00084 -0.00517 C7 1 0.831444 0.561027 0.384157 11.00000 0.02922 0.04001 = 0.02784 0.00161 -0.00480 -0.00902 AFIX 43 H7 2 0.928716 0.558801 0.395055 11.00000 -1.20000 AFIX 0 C8 1 0.729745 0.640246 0.409188 11.00000 0.03795 0.03579 = 0.02472 0.00015 -0.00165 -0.00996 AFIX 43 H8 2 0.744548 0.702050 0.441453 11.00000 -1.20000 AFIX 0 C9 1 0.893996 0.179637 0.213208 11.00000 0.02996 0.04931 = 0.04602 -0.00919 0.00925 0.00319 AFIX 137 H9A 2 0.902313 0.106627 0.183239 11.00000 -1.50000 H9B 2 0.933610 0.147584 0.251200 11.00000 -1.50000 H9C 2 0.946170 0.261029 0.199688 11.00000 -1.50000 AFIX 0 C10 1 0.467408 0.673067 0.400191 11.00000 0.03634 0.02622 = 0.02673 0.00291 0.00117 0.00302 AFIX 23 H10A 2 0.407093 0.689323 0.364706 11.00000 -1.20000 H10B 2 0.482789 0.762606 0.420214 11.00000 -1.20000 AFIX 0 C11 1 0.390474 0.576003 0.442998 11.00000 0.02805 0.02434 = 0.02046 -0.00230 -0.00255 0.00212 C12 1 0.448544 0.466833 0.467285 11.00000 0.02619 0.02704 = 0.02205 -0.00408 0.00129 -0.00031 C13 1 0.508840 0.356854 0.489164 11.00000 0.02175 0.02380 = 0.02496 -0.00026 0.00271 0.00032 C14 1 0.585464 0.362108 0.547376 11.00000 0.02247 0.02414 = 0.02290 0.00000 0.00383 0.00149 C15 1 0.639491 0.486057 0.568868 11.00000 0.03297 0.02543 = 0.02885 0.00143 -0.00094 -0.00125 AFIX 43 H15 2 0.632560 0.566833 0.545179 11.00000 -1.20000 AFIX 0 C16 1 0.703438 0.492180 0.624743 11.00000 0.03819 0.03516 = 0.03080 -0.00577 -0.00194 -0.00456 AFIX 43 H16 2 0.739474 0.577206 0.639099 11.00000 -1.20000 AFIX 0 C17 1 0.714947 0.374709 0.659703 11.00000 0.03249 0.04733 = 0.02274 -0.00031 -0.00062 0.00088 AFIX 43 H17 2 0.757651 0.379166 0.698079 11.00000 -1.20000 AFIX 0 C18 1 0.663669 0.251401 0.638088 11.00000 0.03284 0.03584 = 0.02700 0.00812 0.00400 0.00391 AFIX 43 H18 2 0.672160 0.170569 0.661649 11.00000 -1.20000 AFIX 0 C19 1 0.599817 0.244200 0.582292 11.00000 0.02941 0.02488 = 0.02877 0.00121 0.00375 0.00001 AFIX 43 H19 2 0.565743 0.158502 0.567840 11.00000 -1.20000 AFIX 0 C20 1 0.246430 0.610626 0.457534 11.00000 0.03196 0.02500 = 0.02525 -0.00320 -0.00447 0.00116 C21 1 0.500439 0.224100 0.453913 11.00000 0.02512 0.02622 = 0.02963 -0.00393 -0.00247 -0.00031 AFIX 23 H21A 2 0.436635 0.237067 0.419266 11.00000 -1.20000 H21B 2 0.459825 0.150946 0.479463 11.00000 -1.20000 AFIX 0 C22 1 0.646391 0.179361 0.431852 11.00000 0.02737 0.02411 = 0.02759 -0.00225 -0.00002 -0.00032 AFIX 23 H22A 2 0.695375 0.259433 0.413975 11.00000 -1.20000 H22B 2 0.703459 0.147525 0.466284 11.00000 -1.20000 AFIX 0 C23 1 0.637658 0.064580 0.385773 11.00000 0.02882 0.02940 = 0.02857 -0.00507 -0.00171 0.00205 AFIX 23 H23A 2 0.586040 0.097952 0.350110 11.00000 -1.20000 H23B 2 0.584081 -0.013812 0.402689 11.00000 -1.20000 AFIX 0 C24 1 0.785057 0.016534 0.367485 11.00000 0.02929 0.03394 = 0.03306 -0.00831 -0.00207 0.00214 AFIX 23 H24A 2 0.843316 0.097705 0.357019 11.00000 -1.20000 H24B 2 0.830545 -0.029739 0.401891 11.00000 -1.20000 AFIX 0 C25 1 0.782585 -0.078091 0.316665 11.00000 0.02786 0.03648 = 0.03033 -0.00318 -0.00171 0.00683 HKLF 4 REM 200721_syl_6_110_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.0714, GooF = S = 1.030, Restrained GooF = 1.030 for all data REM R1 = 0.0283 for 4303 Fo > 4sig(Fo) and 0.0308 for all 4542 data REM 263 parameters refined using 0 restraints END WGHT 0.0338 0.2780 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB C7 N2_$1 EQIV $2 -x+1, y+1/2, -z+1/2 HTAB C10 O1_$2 REM Highest difference peak 0.159, deepest hole -0.125, 1-sigma level 0.029 Q1 1 0.5476 0.3581 0.5202 11.00000 0.05 0.16 Q2 1 0.6470 0.3524 0.2587 11.00000 0.05 0.14 Q3 1 0.8019 0.5040 0.3597 11.00000 0.05 0.14 Q4 1 0.6425 0.3037 0.2773 11.00000 0.05 0.13 Q5 1 0.6916 0.4855 0.3385 11.00000 0.05 0.13 Q6 1 0.7881 0.4203 0.3223 11.00000 0.05 0.12 Q7 1 0.5782 0.2174 0.4401 11.00000 0.05 0.11 Q8 1 0.7151 0.0286 0.3789 11.00000 0.05 0.10 Q9 1 0.4238 0.6200 0.4187 11.00000 0.05 0.10 Q10 1 0.6037 0.3020 0.5609 11.00000 0.05 0.10 Q11 1 0.7619 0.3586 0.2756 11.00000 0.05 0.10 Q12 1 0.9783 0.0387 0.3078 11.00000 0.05 0.09 Q13 1 0.4895 0.7883 0.4838 11.00000 0.05 0.09 Q14 1 0.7121 0.3117 0.6405 11.00000 0.05 0.09 Q15 1 0.5626 0.4606 0.3337 11.00000 0.05 0.09 Q16 1 0.7214 -0.1481 0.2355 11.00000 0.05 0.09 Q17 1 0.2079 0.6875 0.4581 11.00000 0.05 0.09 Q18 1 0.5982 0.4212 0.5623 11.00000 0.05 0.09 Q19 1 0.2461 0.7809 0.4428 11.00000 0.05 0.09 Q20 1 0.9623 -0.1254 0.4110 11.00000 0.05 0.08 ; _shelx_res_checksum 63749 _shelx_hkl_file ; -2 0 0 2393.46 183.98 3 0 0 0.10 0.20 -3 0 0 0.20 0.30 3 0 0 -0.20 0.20 -3 0 0 0.10 0.20 4 0 0 91.39 2.90 -4 0 0 89.59 3.00 -4 0 0 92.09 3.40 -5 0 0 0.70 0.50 5 0 0 0.90 0.40 -5 0 0 1.00 0.40 6 0 0 274.07 7.60 -6 0 0 257.77 8.40 -6 0 0 270.97 7.80 -7 0 0 2.00 0.70 7 0 0 1.40 0.50 -7 0 0 2.50 0.60 -8 0 0 255.77 7.70 8 0 0 253.67 7.30 -8 0 0 249.78 8.60 9 0 0 -0.40 0.30 -9 0 0 -0.60 0.50 -9 0 0 0.50 0.60 -10 0 0 10.00 1.30 -10 0 0 8.90 1.70 -11 0 0 1.40 0.60 -11 0 0 -0.10 0.70 -12 0 0 -1.10 0.80 -12 0 0 0.70 0.50 -1 1 0 165.18 4.40 1 1 0 159.48 4.40 1 -1 0 169.78 4.40 -2 1 0 990.70 135.29 2 -1 0 1232.98 142.89 -2 -1 0 948.21 101.49 2 1 0 952.90 105.99 -3 -1 0 3.10 0.50 3 -1 0 4.80 0.70 3 -1 0 4.60 0.50 -3 1 0 3.70 0.40 -3 -1 0 4.40 0.60 -4 1 0 39.50 1.50 4 1 0 38.50 1.10 4 -1 0 38.20 2.00 -4 1 0 39.10 1.90 -4 -1 0 37.50 1.90 -4 -1 0 38.30 1.70 4 -1 0 37.60 1.60 -5 1 0 1.40 0.50 5 1 0 1.80 0.20 -5 -1 0 1.30 0.50 5 1 0 1.40 0.50 -5 1 0 1.60 0.40 5 -1 0 1.40 0.50 5 -1 0 0.50 0.30 -5 -1 0 1.40 0.60 6 -1 0 153.18 5.10 6 1 0 149.69 4.10 6 -1 0 146.29 4.70 -6 1 0 151.18 5.40 -6 -1 0 152.68 5.00 -6 -1 0 150.18 5.40 -6 1 0 148.19 4.70 -7 -1 0 21.20 1.80 7 1 0 21.80 0.80 -7 1 0 22.00 1.80 -7 -1 0 21.20 1.50 -7 1 0 23.20 1.40 7 -1 0 21.90 1.60 8 -1 0 1.20 0.60 -8 -1 0 -0.10 0.60 -8 1 0 0.80 0.70 -8 -1 0 -0.30 0.40 -8 1 0 0.30 0.40 -9 1 0 22.20 2.10 9 -1 0 25.70 1.70 -9 -1 0 19.50 1.70 -9 1 0 21.60 1.50 -9 -1 0 23.50 2.10 -10 -1 0 1.20 0.80 -10 1 0 1.40 0.80 -10 1 0 1.00 0.50 10 -1 0 0.70 0.60 -10 -1 0 0.80 0.70 -11 -1 0 2.00 0.80 -11 1 0 1.10 1.00 11 -1 0 0.70 0.60 -11 -1 0 1.20 0.90 -11 1 0 1.70 0.60 12 -1 0 5.50 0.80 -12 -1 0 12.50 2.10 -12 1 0 6.00 0.90 -12 -1 0 5.70 1.10 -12 1 0 6.30 1.60 0 2 0 91.19 2.50 0 -2 0 93.49 2.50 -1 -2 0 62.99 1.90 2 -2 0 219.28 6.00 2 2 0 211.28 6.10 2 -2 0 221.98 6.80 -2 -2 0 226.68 5.90 3 -2 0 336.57 9.50 3 2 0 311.77 8.90 3 -2 0 322.77 8.60 -3 2 0 316.87 8.50 -3 -2 0 307.47 8.80 4 -2 0 109.59 4.20 -4 -2 0 115.09 3.80 4 -2 0 111.79 3.50 4 2 0 104.79 3.90 -4 2 0 99.99 3.60 -5 2 0 6.40 0.70 -5 -2 0 6.70 0.90 5 2 0 7.30 1.10 5 -2 0 7.10 1.10 5 -2 0 5.90 0.70 -5 -2 0 6.90 0.90 -6 -2 0 4.00 0.80 -6 2 0 4.50 0.70 6 -2 0 4.40 0.90 6 -2 0 3.20 0.60 6 2 0 2.90 0.80 -6 2 0 3.80 0.90 -6 -2 0 3.60 0.90 7 -2 0 0.10 0.50 -7 2 0 1.10 0.60 -7 2 0 0.20 0.40 -7 -2 0 0.40 0.50 -7 -2 0 0.30 0.50 -8 2 0 9.40 1.00 -8 -2 0 9.60 1.30 8 -2 0 12.00 1.20 -8 2 0 9.20 1.60 8 -2 0 12.40 1.60 -8 -2 0 11.10 1.60 -9 -2 0 8.70 1.30 -9 -2 0 6.60 1.30 -9 2 0 9.80 1.60 9 -2 0 7.60 1.30 -9 2 0 7.70 1.00 -10 -2 0 2.40 0.90 -10 -2 0 2.40 1.00 -10 2 0 3.00 1.00 10 -2 0 1.40 0.70 -10 2 0 2.30 0.60 -11 2 0 4.90 1.40 -11 -2 0 4.10 1.20 11 -2 0 6.30 1.10 -11 2 0 5.80 0.90 -11 -2 0 8.90 1.40 0 3 0 0.10 0.10 0 -3 0 0.10 0.10 0 -3 0 0.20 0.40 -1 -3 0 425.16 11.70 1 -3 0 428.16 12.20 2 3 0 14.30 0.90 2 -3 0 14.60 1.40 -2 -3 0 15.30 1.00 3 3 0 7.00 0.80 -3 -3 0 9.30 0.60 3 -3 0 7.30 0.70 3 -3 0 9.50 1.40 -4 -3 0 1.00 0.10 4 -3 0 1.30 0.70 -4 3 0 0.40 0.30 -4 -3 0 0.90 0.40 4 3 0 0.90 0.50 4 -3 0 1.20 0.40 -5 -3 0 164.78 5.50 5 -3 0 167.28 6.30 5 3 0 162.48 5.70 5 -3 0 172.98 5.20 -5 3 0 174.98 5.10 6 -3 0 17.40 1.70 6 -3 0 18.60 1.30 -6 -3 0 17.30 1.50 -6 -3 0 18.00 1.50 -6 3 0 18.20 1.20 6 3 0 16.80 1.60 -7 -3 0 32.10 2.20 -7 -3 0 33.30 2.20 -7 3 0 31.00 1.60 7 -3 0 27.30 2.30 7 -3 0 32.30 1.80 -7 3 0 28.00 2.20 8 -3 0 1.60 0.90 -8 -3 0 2.10 1.50 -8 -3 0 0.00 0.60 8 -3 0 0.60 0.50 -8 3 0 -0.40 0.50 -8 3 0 0.40 0.40 -9 3 0 237.08 8.70 -9 -3 0 238.88 8.20 -9 3 0 236.28 7.10 9 -3 0 241.48 8.60 9 -3 0 239.58 7.40 -9 -3 0 244.88 8.50 -10 -3 0 3.80 1.10 10 -3 0 4.30 1.10 -10 -3 0 4.80 1.20 -10 3 0 3.50 0.70 -10 3 0 2.00 1.10 -11 -3 0 0.20 0.90 -11 -3 0 0.20 0.70 11 -3 0 -1.00 0.60 -11 3 0 0.10 0.70 0 -4 0 198.78 6.60 0 -4 0 194.08 5.40 0 4 0 205.08 5.40 1 -4 0 17.00 1.60 -1 4 0 15.30 0.80 1 4 0 16.30 0.90 -1 -4 0 15.70 0.80 -1 -4 0 14.40 1.30 2 -4 0 5.70 1.10 -2 -4 0 7.30 0.60 2 -4 0 7.80 1.00 2 4 0 7.70 0.70 -2 -4 0 6.10 0.80 -3 -4 0 177.48 5.30 3 4 0 172.38 5.50 -3 -4 0 182.78 5.30 3 -4 0 183.28 6.60 3 -4 0 165.08 6.80 4 -4 0 1.10 0.70 -4 -4 0 1.20 0.40 4 4 0 0.90 0.50 -4 -4 0 1.10 0.30 4 -4 0 0.90 0.40 5 4 0 193.88 6.60 5 -4 0 208.58 6.20 -5 -4 0 197.68 6.30 5 -4 0 199.48 7.50 -6 -4 0 70.19 3.20 6 4 0 72.59 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40.80 2.40 7 -6 0 33.40 3.20 7 6 0 32.10 3.10 7 -6 0 39.90 2.40 8 6 0 -0.80 0.40 -8 -6 0 -0.10 0.70 8 -6 0 -0.20 0.50 -8 -6 0 0.00 0.60 9 -6 0 20.50 1.80 -9 -6 0 19.90 1.90 -9 6 0 21.70 2.30 9 -6 0 21.00 2.80 -9 -6 0 22.80 2.50 9 6 0 20.80 2.30 10 6 0 0.70 1.00 -10 -6 0 4.40 1.30 10 -6 0 2.60 1.50 -10 6 0 3.20 1.20 10 -6 0 2.60 0.80 0 -7 0 1.90 1.00 0 7 0 0.30 0.30 -1 -7 0 338.17 11.00 1 7 0 318.37 9.30 -1 -7 0 328.97 9.10 -1 7 0 325.67 9.00 1 -7 0 336.67 11.40 2 -7 0 5.70 1.50 2 -7 0 2.50 0.80 -2 -7 0 3.80 1.10 2 7 0 2.80 0.70 -2 7 0 2.40 0.50 -2 -7 0 2.40 0.50 3 7 0 7.80 1.10 -3 -7 0 9.50 1.40 -3 -7 0 10.00 0.90 3 -7 0 9.50 1.90 -3 7 0 7.70 0.80 3 -7 0 9.50 1.30 -4 -7 0 15.30 1.10 4 7 0 13.80 1.40 4 -7 0 15.10 2.30 -4 -7 0 10.60 1.40 4 -7 0 14.10 1.40 5 -7 0 19.00 2.80 -5 -7 0 22.40 1.50 -5 -7 0 21.60 1.50 5 -7 0 21.30 1.80 5 7 0 24.50 2.00 -6 -7 0 3.60 0.90 6 7 0 1.30 0.80 6 -7 0 1.40 1.20 6 -7 0 3.10 0.90 -6 -7 0 2.90 0.70 -7 -7 0 87.19 3.70 7 -7 0 80.89 3.80 8 -7 0 39.00 2.50 -8 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1.20 -1 -4 -25 4.40 1.50 1 -4 25 5.70 1.60 -1 4 25 4.80 0.90 1 -4 25 5.60 1.60 -1 -4 -25 1.90 1.30 -1 4 25 3.70 1.40 1 4 -25 6.70 1.50 -1 4 -25 6.20 1.70 1 4 25 7.80 1.90 -1 -4 25 6.80 1.60 1 4 25 6.20 1.10 -1 -4 25 7.20 1.70 1 -4 -25 6.50 1.60 2 -4 25 3.60 1.30 -2 -4 -25 7.10 2.90 -2 4 25 5.30 1.00 -2 -4 -25 6.00 1.80 2 -4 -25 8.50 1.90 2 4 25 5.40 1.10 -2 -4 25 5.50 0.60 -2 4 -25 5.00 1.50 -2 -4 25 5.50 0.40 2 4 25 2.90 1.40 2 -4 -25 5.60 1.30 -2 -4 25 5.90 1.60 -2 -4 25 5.60 1.50 -3 4 25 8.30 2.20 -3 -4 -25 8.10 1.90 3 -4 25 7.80 2.00 3 -4 25 3.70 1.80 3 4 25 8.70 1.40 3 4 25 10.50 2.20 -3 4 -25 10.90 2.00 3 -4 -25 13.30 1.70 -3 -4 25 10.40 0.70 3 -4 -25 11.80 2.20 -3 -4 25 10.80 1.00 -3 -4 25 11.60 1.90 4 -4 25 -0.30 1.00 -4 -4 -25 4.80 1.70 -4 4 25 1.10 1.30 -4 4 25 1.30 0.80 4 -4 25 0.30 1.10 -4 -4 25 2.50 1.20 4 4 25 0.70 0.80 4 -4 -25 2.30 0.70 4 4 25 2.10 1.30 -4 -4 25 1.20 0.90 -4 -4 25 1.60 0.60 0 -5 -25 -0.20 0.90 0 5 -25 0.30 1.00 0 -5 25 2.30 1.30 0 -5 -25 3.20 1.40 0 5 25 1.40 1.60 -1 5 25 7.50 2.10 -1 -5 -25 14.80 2.30 -1 5 25 11.50 1.40 1 -5 25 10.20 2.10 1 -5 25 14.50 2.40 -1 -5 -25 12.00 2.40 -1 5 -25 9.90 1.90 1 -5 -25 14.80 2.50 -1 -5 25 15.90 2.30 1 -5 -25 9.70 1.80 -2 -5 -25 31.00 3.20 2 -5 25 32.70 3.30 -2 5 25 28.80 2.00 2 -5 25 30.70 3.10 -2 5 25 32.90 3.60 -2 -5 -25 28.60 3.00 -2 -5 25 40.50 3.50 2 5 25 27.10 2.60 -2 -5 25 35.70 3.00 -2 5 -25 36.20 3.20 2 5 25 28.80 4.20 -3 -5 -25 15.40 2.40 -3 -5 -25 17.30 2.60 -3 5 25 15.50 1.50 3 -5 25 11.50 2.50 3 -5 25 15.00 2.60 -3 5 25 15.20 2.80 3 -5 -25 13.10 1.80 3 5 25 14.10 1.80 -3 -5 25 16.90 2.50 -3 -5 25 16.80 2.50 -3 -5 25 14.50 0.80 0 -6 -25 1.80 1.10 0 6 25 -0.50 1.00 0 -6 25 1.20 1.00 0 -6 25 1.00 1.10 -1 -6 -25 18.10 2.60 1 -6 25 17.70 2.70 -1 6 25 22.50 3.30 -1 6 25 20.70 1.80 1 -6 25 16.90 2.80 1 6 25 16.60 2.90 1 6 25 18.40 1.70 -1 -6 25 19.80 2.90 1 -6 -25 13.30 2.10 -1 -6 25 17.60 3.70 0 0 26 32.10 3.20 0 0 26 29.50 1.70 0 0 -26 32.10 2.70 0 0 26 32.50 3.00 1 0 26 17.90 2.60 1 0 -26 20.10 2.40 -1 0 26 19.20 2.80 -1 0 26 24.60 2.50 1 0 26 15.30 2.50 1 0 26 19.20 1.40 -1 0 -26 18.80 2.50 -2 0 26 0.20 0.80 2 0 26 0.90 1.10 -2 0 26 1.40 1.20 -2 0 26 -0.20 0.40 -2 0 -26 0.20 0.90 2 0 26 0.10 0.50 2 0 26 0.00 1.00 -3 0 26 8.20 2.00 -3 0 -26 7.50 1.80 3 0 26 6.10 1.70 3 0 26 6.90 1.10 -3 0 26 8.10 1.00 -3 0 26 9.40 1.70 3 0 26 5.40 1.70 3 0 -26 6.60 1.40 4 0 26 1.70 1.10 -4 0 26 0.60 0.60 -4 0 -26 -0.50 1.00 4 0 -26 -0.80 0.60 4 0 26 0.20 1.10 -4 0 26 1.90 0.80 -4 0 26 2.90 1.30 5 0 26 5.30 1.00 5 0 26 1.10 1.30 5 0 26 0.70 1.30 -5 0 26 5.60 1.10 0 -1 26 65.59 4.20 0 -1 26 67.69 4.60 0 1 26 58.89 4.50 0 -1 26 66.99 2.60 0 1 26 62.89 4.10 0 -1 -26 67.69 4.00 0 1 26 69.29 2.80 0 1 -26 64.59 3.90 -1 1 26 7.90 1.00 1 1 -26 10.00 1.70 -1 -1 -26 7.50 1.70 -1 1 26 7.40 1.90 1 -1 26 8.60 1.70 1 -1 26 6.00 1.70 -1 1 26 10.40 1.90 1 -1 26 7.40 0.90 1 1 26 7.90 1.10 -1 1 -26 8.90 1.70 1 1 26 9.00 1.80 -1 -1 26 5.90 1.50 1 1 26 8.30 1.90 -1 -1 26 7.30 0.80 -1 -1 26 6.50 1.80 -2 1 26 8.90 1.10 -2 1 26 7.40 1.80 2 -1 26 3.90 1.60 2 -1 26 8.40 1.00 -2 1 26 7.30 1.50 -2 -1 -26 10.20 1.90 2 -1 26 8.90 1.90 -2 1 -26 9.50 2.80 2 1 26 9.90 1.30 -2 -1 26 4.10 1.50 2 -1 -26 8.30 1.40 -2 -1 26 9.50 0.90 -2 -1 26 9.70 1.70 2 1 26 9.70 2.00 2 1 26 10.70 2.10 -3 1 26 54.89 4.40 3 -1 26 52.39 2.50 3 -1 26 56.99 4.20 -3 1 26 53.59 2.50 3 -1 26 52.89 4.10 -3 -1 -26 50.59 3.80 -3 1 26 54.69 3.30 3 1 -26 57.59 3.20 -3 1 -26 52.79 4.00 3 1 26 56.79 2.90 -3 -1 26 54.69 2.30 3 -1 -26 55.19 3.10 3 1 26 53.69 4.10 -3 -1 26 53.79 3.40 -3 -1 26 53.99 4.10 3 1 26 52.79 4.10 -4 -1 -26 2.90 1.30 -4 1 26 1.40 0.70 4 -1 26 2.10 0.70 4 -1 26 0.20 1.00 -4 -1 26 2.00 0.90 -4 -1 26 0.90 0.60 4 1 26 0.20 1.00 4 -1 -26 0.50 0.70 4 1 26 1.30 0.80 4 1 26 2.70 1.40 -4 -1 26 -0.40 1.00 -4 1 -26 2.20 1.30 5 -1 26 13.40 1.30 5 -1 26 12.00 2.30 -5 1 26 15.30 2.70 5 -1 26 18.40 2.80 5 1 26 16.50 2.70 -5 -1 26 17.70 3.10 5 1 26 12.80 1.70 -5 -1 26 16.20 1.70 0 -2 -26 17.70 2.30 0 -2 26 13.80 0.90 0 2 -26 11.00 1.90 0 -2 26 10.70 1.90 0 2 26 10.90 2.10 0 2 26 10.70 1.90 0 2 26 13.10 1.20 0 -2 26 11.40 2.20 1 -2 26 1.00 0.40 -1 -2 -26 0.30 0.80 1 2 -26 2.00 1.00 1 -2 26 0.40 1.10 -1 2 26 -0.20 1.00 -1 2 26 1.50 0.60 1 -2 26 1.70 1.10 -1 -2 26 1.50 1.00 1 2 26 1.10 1.10 -1 -2 26 1.40 0.40 -1 -2 26 0.60 1.10 -1 2 -26 0.50 1.00 1 2 26 1.00 0.60 1 2 26 0.80 1.20 2 -2 26 1.00 1.10 -2 2 26 0.80 0.60 2 -2 26 0.20 0.30 2 -2 26 2.70 1.20 -2 -2 -26 1.40 1.20 -2 2 26 -0.80 1.20 2 2 -26 2.10 0.90 2 2 26 -0.10 0.90 -2 -2 26 -0.40 0.70 2 -2 -26 1.30 1.00 2 2 26 1.60 0.70 -2 2 -26 1.40 1.00 -2 -2 26 1.60 1.20 -2 -2 26 0.30 0.30 2 2 26 0.00 0.90 2 -2 -26 2.80 1.00 3 -2 26 27.90 1.50 -3 2 26 29.70 1.80 3 -2 26 29.90 3.60 -3 -2 -26 31.50 3.10 3 -2 -26 21.90 3.00 3 2 26 27.70 3.40 -3 -2 26 26.80 2.50 -3 -2 26 29.60 3.00 -3 -2 26 28.30 1.50 3 -2 -26 23.70 2.10 3 2 26 29.00 3.10 3 2 26 29.60 2.10 -3 2 -26 29.90 3.00 -4 2 26 0.30 0.60 4 -2 26 2.20 1.30 -4 -2 -26 -0.70 1.10 -4 2 26 0.60 1.20 4 -2 26 0.10 0.40 4 -2 26 1.30 1.20 4 -2 -26 -0.40 0.90 -4 -2 26 0.50 0.80 4 2 26 0.60 0.70 4 2 26 2.20 1.10 -4 -2 26 0.90 0.50 -4 2 -26 0.30 1.20 4 2 26 -0.70 0.90 -4 -2 26 0.20 0.60 -4 -2 26 -2.30 0.80 4 -2 -26 0.40 0.60 0 -3 26 5.90 1.40 0 -3 26 1.40 0.30 0 -3 26 1.30 0.30 0 3 -26 1.40 1.10 0 -3 -26 0.90 1.10 0 3 26 1.10 0.60 0 -3 26 0.60 1.00 0 -3 -26 3.40 1.30 0 3 26 1.20 1.10 -1 -3 -26 8.30 1.80 1 3 -26 9.50 1.60 -1 3 26 7.80 1.10 1 -3 26 8.50 2.30 -1 3 26 10.10 3.10 1 -3 26 7.60 1.80 -1 -3 26 4.80 1.60 -1 -3 26 9.00 0.60 -1 -3 26 8.80 1.80 1 -3 -26 8.40 1.60 1 3 26 7.60 2.00 -1 3 -26 6.90 1.80 1 3 26 10.00 1.30 1 -3 -26 6.90 1.80 2 -3 26 11.10 2.10 2 3 -26 7.70 1.60 -2 -3 -26 7.10 2.00 -2 3 26 7.60 1.10 -2 3 26 4.60 2.10 2 3 26 5.30 1.80 2 -3 -26 7.30 1.50 -2 -3 26 7.90 1.80 -2 -3 26 10.10 1.10 -2 3 -26 8.90 1.80 2 -3 -26 9.00 1.90 -2 -3 26 8.60 1.70 2 3 26 7.60 1.20 -2 -3 26 8.30 0.70 -3 3 26 39.60 2.20 3 -3 26 35.70 3.50 3 -3 26 39.50 3.60 -3 3 26 38.50 3.80 -3 -3 -26 40.10 3.40 -3 3 -26 37.00 3.30 3 3 26 37.30 2.40 -3 -3 26 37.90 2.20 3 3 26 39.60 3.70 3 -3 -26 42.20 3.60 -3 -3 26 37.40 1.60 3 -3 -26 35.80 2.60 -3 -3 26 41.20 3.60 -3 -3 26 35.30 2.90 -4 3 26 36.10 3.80 4 -3 26 34.30 3.60 4 -3 26 35.00 3.30 -4 3 26 35.70 2.30 -4 -3 26 33.70 2.70 4 -3 -26 33.70 2.30 -4 -3 26 31.40 1.70 -4 -3 26 36.70 2.30 4 3 26 37.00 2.60 0 4 -26 4.50 1.40 0 4 26 3.30 1.60 0 -4 -26 2.40 1.20 0 -4 26 1.50 1.20 0 -4 -26 3.80 1.40 0 -4 26 0.20 1.00 0 4 26 3.50 0.90 1 -4 26 13.70 2.40 -1 -4 -26 15.90 2.50 -1 4 26 13.50 1.40 -1 4 26 14.70 2.60 1 4 -26 12.50 2.20 1 -4 26 12.80 2.20 -1 -4 -26 13.80 2.20 1 4 26 13.40 1.40 1 -4 -26 15.00 2.50 -1 -4 26 10.90 3.30 -1 -4 26 16.10 2.40 -1 4 -26 15.40 2.30 1 4 26 13.90 3.00 1 -4 -26 15.40 2.20 -2 -4 -26 13.40 2.30 2 -4 26 18.00 2.80 -2 4 26 15.50 2.90 2 -4 26 15.60 2.60 -2 4 -26 15.60 2.40 2 4 26 14.60 3.20 2 4 26 14.80 1.60 -2 -4 26 14.70 2.20 -2 -4 26 16.10 0.90 -3 -4 -26 8.40 2.00 -3 4 26 8.80 1.30 3 -4 26 10.40 2.10 3 -4 26 9.00 2.10 -3 4 26 4.40 1.80 3 4 26 6.00 2.20 -3 -4 26 6.90 0.90 3 -4 -26 7.90 1.40 3 4 26 6.20 1.30 -3 -4 26 9.10 1.80 -3 -4 26 7.80 0.60 0 -5 -26 1.10 1.10 0 5 -26 2.00 1.10 0 5 26 0.90 0.70 0 -5 26 1.00 1.00 0 5 26 -2.30 1.00 1 -5 26 3.30 1.60 1 -5 26 2.80 1.40 -1 -5 -26 2.20 1.30 -1 5 26 2.30 1.50 -1 5 26 3.90 0.90 1 -5 -26 2.00 1.30 1 5 26 1.40 1.40 -1 -5 26 1.20 1.10 -1 -5 26 1.40 1.00 -1 5 -26 0.50 1.10 1 5 26 1.30 0.80 0 0 27 -1.10 0.80 0 0 27 1.10 1.30 0 0 -27 -0.40 0.90 1 0 27 7.30 1.00 1 0 -27 10.10 1.70 -1 0 27 9.00 1.80 -1 0 27 8.40 1.00 -1 0 -27 5.00 1.60 1 0 27 7.30 1.70 -1 0 27 7.60 2.20 -2 0 -27 1.20 1.10 2 0 27 -0.70 0.40 -2 0 27 0.70 0.40 2 0 27 1.40 1.30 -2 0 27 0.80 0.90 2 0 -27 0.10 0.80 2 0 27 -0.10 0.90 -3 0 27 1.00 0.80 -3 0 -27 1.80 1.20 3 0 27 1.50 1.20 3 0 -27 1.40 0.80 -3 0 27 2.80 1.20 -3 0 27 0.90 0.50 3 0 27 1.90 1.10 -4 0 27 -0.50 0.50 4 0 -27 0.20 0.70 -4 0 27 4.00 1.70 -4 0 27 -0.20 0.70 4 0 27 -1.20 0.80 4 0 27 0.40 0.60 4 0 27 -0.30 0.90 0 -1 27 26.10 2.70 0 -1 -27 30.10 2.70 0 1 27 25.80 1.70 0 1 -27 29.60 2.70 0 -1 27 27.00 1.50 0 1 27 27.30 2.80 -1 1 27 25.40 2.60 -1 1 27 22.80 1.60 1 1 -27 23.70 2.40 1 -1 27 25.90 3.10 -1 -1 -27 24.60 2.60 1 -1 27 22.00 1.40 -1 -1 27 18.90 2.50 -1 -1 27 24.70 1.40 1 -1 -27 26.10 2.40 1 1 27 24.80 1.70 1 1 27 25.30 2.80 2 -1 27 21.60 3.00 2 -1 27 19.50 1.40 2 -1 27 16.70 2.60 -2 1 27 19.00 1.40 2 1 -27 16.90 2.20 -2 1 27 17.20 2.20 -2 1 27 17.10 3.30 -2 -1 -27 18.30 2.60 2 1 27 17.60 2.60 -2 1 -27 20.60 2.70 -2 -1 27 16.40 2.30 2 1 27 20.50 1.60 3 -1 27 21.00 3.20 -3 1 27 23.30 2.30 -3 1 27 24.70 1.60 3 -1 27 20.80 1.50 3 -1 27 15.90 2.80 -3 1 27 21.60 3.20 -3 -1 -27 23.90 3.00 3 1 27 19.90 1.80 -3 -1 27 27.00 2.40 3 -1 -27 27.20 2.20 -3 -1 27 23.00 1.40 -3 1 -27 26.70 3.20 -3 -1 27 24.30 3.80 3 1 27 21.40 3.00 0 2 27 0.50 0.50 0 2 27 -2.30 1.00 0 -2 27 0.60 0.30 0 2 -27 0.60 1.00 0 -2 -27 0.50 0.80 0 -2 27 0.70 1.00 0 -2 27 0.30 1.00 -1 -2 -27 0.10 1.00 1 -2 27 4.80 1.50 -1 2 27 2.10 0.70 -1 2 27 1.10 1.30 1 2 -27 2.30 1.00 1 -2 27 2.30 1.30 1 -2 27 1.80 0.40 -1 -2 27 1.90 0.40 -1 -2 27 2.50 1.40 1 -2 -27 2.40 1.00 1 2 27 1.90 1.20 -1 2 -27 1.00 1.00 1 2 27 1.50 0.60 -1 -2 27 2.80 1.30 1 2 27 2.70 1.50 2 -2 27 13.10 2.20 2 2 -27 11.10 1.80 -2 2 27 12.00 2.50 2 -2 27 11.00 0.90 -2 2 27 13.30 1.30 -2 -2 -27 13.10 2.20 2 -2 27 12.30 2.20 -2 -2 27 12.40 0.90 2 2 27 12.60 1.40 2 2 27 12.30 2.40 -2 -2 27 12.50 2.00 2 2 27 14.10 2.30 -2 2 -27 12.20 2.10 -2 -2 27 6.20 2.20 -3 2 27 35.70 2.00 3 -2 27 32.60 3.40 3 2 -27 39.70 2.80 -3 2 27 39.60 3.90 3 -2 27 34.60 1.70 -3 -2 -27 39.60 3.40 3 -2 27 36.70 3.50 -3 -2 27 38.90 3.00 3 2 27 35.40 3.40 -3 -2 27 29.10 3.30 3 -2 -27 32.00 2.40 -3 -2 27 35.60 1.70 -3 2 -27 36.00 3.50 3 2 27 34.80 2.40 3 2 27 28.80 3.20 0 -3 27 4.70 0.40 0 -3 27 4.10 1.40 0 3 27 5.40 1.00 0 3 -27 6.40 1.50 0 -3 -27 5.30 1.50 0 3 27 5.80 1.80 0 -3 27 5.90 0.40 0 -3 27 11.90 2.10 1 -3 27 7.30 1.70 -1 3 27 5.40 0.90 1 3 -27 4.20 1.30 1 -3 27 2.60 1.40 -1 3 27 4.00 1.60 1 -3 -27 1.70 1.00 -1 3 -27 2.40 1.30 1 3 27 2.80 0.80 -1 -3 27 4.00 0.50 1 3 27 3.00 1.40 -1 -3 27 2.90 1.40 -1 -3 27 3.60 1.40 2 3 -27 1.40 1.10 -2 3 27 3.90 1.50 -2 3 27 3.10 0.80 2 -3 27 0.60 1.20 -2 -3 -27 2.90 1.40 2 -3 27 3.20 1.50 -2 -3 27 2.70 0.50 -2 -3 27 2.10 0.60 -2 -3 27 2.50 1.10 -2 3 -27 1.40 1.10 -2 -3 27 3.10 1.20 2 3 27 4.90 1.70 2 3 27 3.00 0.90 0 -4 -27 22.60 2.70 0 -4 27 21.30 3.00 0 -4 27 27.70 2.90 0 4 -27 26.40 2.60 0 4 27 20.30 3.20 1 4 -27 5.60 1.50 1 -4 27 1.80 1.30 -1 4 27 3.20 1.00 1 -4 27 2.80 1.30 -1 -4 -27 3.30 1.30 -1 4 27 2.80 1.60 -1 4 -27 5.60 1.60 -1 -4 27 3.40 1.60 1 -4 -27 3.10 1.20 -1 -4 27 2.00 1.30 1 4 27 3.70 1.20 1 4 27 2.40 1.40 0 0 28 36.30 3.10 0 0 -28 33.00 3.00 0 0 28 36.20 3.50 0 0 28 37.90 2.00 1 0 28 2.70 0.80 1 0 28 1.40 1.20 -1 0 28 2.40 1.20 -1 0 28 -1.10 1.10 1 0 -28 2.70 1.10 -1 0 28 2.40 0.60 -1 0 -28 1.20 1.00 1 0 28 2.60 1.30 -2 0 28 3.80 0.70 2 0 28 3.00 1.40 -2 0 28 2.10 1.10 -2 0 -28 6.20 1.70 -2 0 28 4.50 1.80 2 0 -28 4.90 1.30 0 1 28 20.00 2.90 0 1 28 12.10 2.20 0 -1 28 12.40 1.10 0 -1 -28 12.00 2.10 0 1 28 12.10 1.20 0 -1 28 11.20 2.10 0 -1 28 13.50 2.50 1 -1 28 57.49 2.50 -1 -1 -28 63.49 4.10 1 -1 28 54.49 4.00 -1 1 28 62.79 4.00 1 -1 28 62.19 4.60 -1 1 28 67.49 4.80 1 1 -28 57.39 3.70 -1 1 28 59.19 2.60 -1 1 -28 60.39 4.10 -1 -1 28 62.69 2.40 -1 -1 28 56.19 4.40 1 1 28 58.59 4.20 1 -1 -28 63.69 3.80 -1 -1 28 56.59 4.00 1 1 28 56.59 4.50 1 1 28 55.19 2.70 2 1 -28 1.50 1.00 2 -1 28 1.60 0.60 -2 1 28 1.80 0.60 2 -1 28 2.00 1.10 -2 1 28 2.00 1.00 -2 1 28 1.40 1.50 -2 -1 -28 1.40 1.30 2 -1 28 3.40 1.50 2 1 28 4.60 0.90 -2 -1 28 1.30 1.00 -2 1 -28 3.40 1.50 2 1 28 5.80 1.70 2 -1 -28 2.00 1.10 -2 -1 28 2.30 0.60 -2 -1 28 1.20 1.10 0 -2 28 16.30 1.10 0 2 28 17.20 1.40 0 -2 28 18.70 2.50 0 -2 28 20.10 3.10 0 2 28 17.10 2.80 0 -2 -28 19.30 2.50 0 2 -28 18.90 2.40 -1 2 28 10.40 2.30 -1 -2 -28 9.20 1.80 1 2 -28 7.40 1.90 1 -2 28 8.90 1.90 1 -2 28 8.60 2.00 1 -2 28 7.40 0.70 -1 2 28 8.30 1.10 1 2 28 6.80 1.80 1 2 28 7.60 1.10 1 -2 -28 6.60 1.60 -1 -2 28 4.60 1.70 -1 -2 28 7.30 0.80 -1 2 -28 7.20 1.60 -1 -2 28 10.40 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 20951 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.74874(12) 0.21398(12) 0.22119(5) 0.0344(3) Uani 1 1 d . . . . . N1 N 0.60164(15) 0.61857(14) 0.38125(6) 0.0289(3) Uani 1 1 d . . . . . N2 N 0.13229(16) 0.64142(16) 0.46923(7) 0.0381(3) Uani 1 1 d . . . . . N3 N 0.77830(18) -0.15049(18) 0.27642(7) 0.0434(4) Uani 1 1 d . . . . . C1 C 0.81445(16) 0.38031(17) 0.29805(7) 0.0276(3) Uani 1 1 d . . . . . H1 H 0.911987 0.356444 0.296318 0.033 Uiso 1 1 calc R . . . . C2 C 0.71656(16) 0.31718(16) 0.26128(7) 0.0271(3) Uani 1 1 d . . . . . C3 C 0.57231(16) 0.35366(18) 0.26256(7) 0.0304(3) Uani 1 1 d . . . . . H3 H 0.507574 0.307781 0.236886 0.037 Uiso 1 1 calc R . . . . C4 C 0.52335(16) 0.45474(17) 0.30038(7) 0.0292(3) Uani 1 1 d . . . . . H4 H 0.426228 0.480457 0.300739 0.035 Uiso 1 1 calc R . . . . C5 C 0.62105(16) 0.51805(16) 0.33813(6) 0.0260(3) Uani 1 1 d . . . . . C6 C 0.76537(17) 0.48098(16) 0.33811(6) 0.0267(3) Uani 1 1 d . . . . . C7 C 0.83144(18) 0.56103(18) 0.38416(7) 0.0324(4) Uani 1 1 d . . . . . H7 H 0.928716 0.558801 0.395055 0.039 Uiso 1 1 calc R . . . . C8 C 0.72975(19) 0.64025(18) 0.40919(7) 0.0328(4) Uani 1 1 d . . . . . H8 H 0.744548 0.702050 0.441453 0.039 Uiso 1 1 calc R . . . . C9 C 0.89400(19) 0.1796(2) 0.21321(9) 0.0418(4) Uani 1 1 d . . . . . H9A H 0.902313 0.106627 0.183239 0.063 Uiso 1 1 calc GR . . . . H9B H 0.933610 0.147584 0.251200 0.063 Uiso 1 1 calc GR . . . . H9C H 0.946170 0.261029 0.199688 0.063 Uiso 1 1 calc GR . . . . C10 C 0.46741(18) 0.67307(16) 0.40019(7) 0.0298(3) Uani 1 1 d . . . . . H10A H 0.407093 0.689323 0.364706 0.036 Uiso 1 1 calc R . . . . H10B H 0.482789 0.762606 0.420214 0.036 Uiso 1 1 calc R . . . . C11 C 0.39047(16) 0.57600(15) 0.44300(6) 0.0243(3) Uani 1 1 d . . . . . C12 C 0.44854(16) 0.46683(16) 0.46729(6) 0.0251(3) Uani 1 1 d . . . . . C13 C 0.50884(15) 0.35685(15) 0.48916(6) 0.0235(3) Uani 1 1 d . . . . . C14 C 0.58546(15) 0.36211(15) 0.54738(6) 0.0232(3) Uani 1 1 d . . . . . C15 C 0.63949(18) 0.48606(16) 0.56887(7) 0.0291(3) Uani 1 1 d . . . . . H15 H 0.632560 0.566833 0.545179 0.035 Uiso 1 1 calc R . . . . C16 C 0.70344(19) 0.49218(18) 0.62474(7) 0.0347(4) Uani 1 1 d . . . . . H16 H 0.739474 0.577206 0.639099 0.042 Uiso 1 1 calc R . . . . C17 C 0.71495(18) 0.3747(2) 0.65970(7) 0.0342(4) Uani 1 1 d . . . . . H17 H 0.757651 0.379166 0.698079 0.041 Uiso 1 1 calc R . . . . C18 C 0.66367(18) 0.25140(18) 0.63809(7) 0.0319(3) Uani 1 1 d . . . . . H18 H 0.672160 0.170569 0.661649 0.038 Uiso 1 1 calc R . . . . C19 C 0.59982(17) 0.24420(16) 0.58229(7) 0.0277(3) Uani 1 1 d . . . . . H19 H 0.565743 0.158502 0.567840 0.033 Uiso 1 1 calc R . . . . C20 C 0.24643(17) 0.61063(16) 0.45753(6) 0.0274(3) Uani 1 1 d . . . . . C21 C 0.50044(16) 0.22410(16) 0.45391(7) 0.0270(3) Uani 1 1 d . . . . . H21A H 0.436635 0.237067 0.419266 0.032 Uiso 1 1 calc R . . . . H21B H 0.459825 0.150946 0.479463 0.032 Uiso 1 1 calc R . . . . C22 C 0.64639(16) 0.17936(16) 0.43185(7) 0.0264(3) Uani 1 1 d . . . . . H22A H 0.695375 0.259433 0.413975 0.032 Uiso 1 1 calc R . . . . H22B H 0.703459 0.147525 0.466284 0.032 Uiso 1 1 calc R . . . . C23 C 0.63766(17) 0.06458(17) 0.38577(7) 0.0289(3) Uani 1 1 d . . . . . H23A H 0.586040 0.097952 0.350110 0.035 Uiso 1 1 calc R . . . . H23B H 0.584081 -0.013812 0.402689 0.035 Uiso 1 1 calc R . . . . C24 C 0.78506(17) 0.01653(18) 0.36748(7) 0.0321(3) Uani 1 1 d . . . . . H24A H 0.843316 0.097705 0.357019 0.039 Uiso 1 1 calc R . . . . H24B H 0.830545 -0.029739 0.401891 0.039 Uiso 1 1 calc R . . . . C25 C 0.78258(17) -0.07809(18) 0.31667(7) 0.0316(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 O1 0.0270(6) 0.0391(6) 0.0372(6) -0.0098(5) 0.0041(5) -0.0008(5) N1 0.0324(7) 0.0301(6) 0.0240(6) -0.0004(5) 0.0017(5) -0.0025(6) N2 0.0319(8) 0.0395(8) 0.0429(8) -0.0082(7) -0.0024(6) 0.0052(7) N3 0.0445(9) 0.0506(9) 0.0349(7) -0.0123(7) -0.0028(7) 0.0116(7) C1 0.0210(7) 0.0342(8) 0.0276(7) 0.0041(6) 0.0004(6) -0.0011(6) C2 0.0270(8) 0.0308(8) 0.0235(7) 0.0016(6) 0.0031(6) -0.0014(6) C3 0.0245(8) 0.0389(9) 0.0279(7) -0.0032(7) -0.0040(6) -0.0028(7) C4 0.0225(7) 0.0373(9) 0.0278(7) 0.0004(6) -0.0011(6) 0.0010(6) C5 0.0272(7) 0.0295(7) 0.0214(6) 0.0032(6) 0.0015(6) -0.0022(6) C6 0.0254(7) 0.0317(8) 0.0230(6) 0.0044(6) -0.0008(6) -0.0052(6) C7 0.0292(8) 0.0400(9) 0.0278(7) 0.0016(7) -0.0048(6) -0.0090(7) C8 0.0379(9) 0.0358(8) 0.0247(7) 0.0002(7) -0.0016(6) -0.0100(7) C9 0.0300(9) 0.0493(11) 0.0460(10) -0.0092(8) 0.0093(7) 0.0032(8) C10 0.0363(9) 0.0262(7) 0.0267(7) 0.0029(6) 0.0012(6) 0.0030(7) C11 0.0281(7) 0.0243(7) 0.0205(6) -0.0023(6) -0.0025(5) 0.0021(6) C12 0.0262(7) 0.0270(7) 0.0220(6) -0.0041(6) 0.0013(5) -0.0003(6) C13 0.0218(7) 0.0238(7) 0.0250(7) -0.0003(6) 0.0027(5) 0.0003(6) C14 0.0225(7) 0.0241(7) 0.0229(6) 0.0000(6) 0.0038(5) 0.0015(6) C15 0.0330(8) 0.0254(7) 0.0288(7) 0.0014(6) -0.0009(6) -0.0013(6) C16 0.0382(9) 0.0352(9) 0.0308(8) -0.0058(7) -0.0019(7) -0.0046(7) C17 0.0325(8) 0.0473(10) 0.0227(7) -0.0003(7) -0.0006(6) 0.0009(8) C18 0.0328(8) 0.0358(9) 0.0270(7) 0.0081(7) 0.0040(6) 0.0039(7) C19 0.0294(8) 0.0249(7) 0.0288(7) 0.0012(6) 0.0038(6) 0.0000(6) C20 0.0320(8) 0.0250(7) 0.0253(7) -0.0032(6) -0.0045(6) 0.0012(6) C21 0.0251(7) 0.0262(7) 0.0296(7) -0.0039(6) -0.0025(6) -0.0003(6) C22 0.0274(7) 0.0241(7) 0.0276(7) -0.0023(6) 0.0000(6) -0.0003(6) C23 0.0288(8) 0.0294(8) 0.0286(7) -0.0051(6) -0.0017(6) 0.0020(6) C24 0.0293(8) 0.0339(8) 0.0331(8) -0.0083(7) -0.0021(6) 0.0021(7) C25 0.0279(8) 0.0365(9) 0.0303(7) -0.0032(7) -0.0017(6) 0.0068(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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C9 117.68(13) . . ? C5 N1 C10 125.60(13) . . ? C8 N1 C5 107.95(13) . . ? C8 N1 C10 125.67(14) . . ? C2 C1 H1 121.0 . . ? C2 C1 C6 117.99(15) . . ? C6 C1 H1 121.0 . . ? O1 C2 C1 124.31(14) . . ? O1 C2 C3 114.17(14) . . ? C1 C2 C3 121.52(15) . . ? C2 C3 H3 119.4 . . ? C4 C3 C2 121.13(14) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4 121.1 . . ? C3 C4 C5 117.78(14) . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 130.27(15) . . ? N1 C5 C6 107.97(13) . . ? C4 C5 C6 121.74(14) . . ? C1 C6 C5 119.78(14) . . ? C1 C6 C7 133.88(15) . . ? C5 C6 C7 106.33(14) . . ? C6 C7 H7 126.3 . . ? C8 C7 C6 107.37(15) . . ? C8 C7 H7 126.3 . . ? N1 C8 H8 124.8 . . ? C7 C8 N1 110.33(14) . . ? C7 C8 H8 124.8 . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 H10A 109.2 . . ? N1 C10 H10B 109.2 . . ? N1 C10 C11 112.09(13) . . ? H10A C10 H10B 107.9 . . ? C11 C10 H10A 109.2 . . ? C11 C10 H10B 109.2 . . ? C12 C11 C10 124.12(15) . . ? C12 C11 C20 119.36(14) . . ? C20 C11 C10 116.51(13) . . ? C13 C12 C11 177.46(15) . . ? C12 C13 C14 120.71(14) . . ? C12 C13 C21 118.64(13) . . ? C14 C13 C21 120.65(13) . . ? C15 C14 C13 120.56(13) . . ? C19 C14 C13 120.59(14) . . ? C19 C14 C15 118.80(14) . . ? C14 C15 H15 119.8 . . ? C16 C15 C14 120.42(15) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 119.8 . . ? C17 C16 C15 120.39(15) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 120.4 . . ? C18 C17 C16 119.30(14) . . ? C18 C17 H17 120.4 . . ? C17 C18 H18 119.6 . . ? C17 C18 C19 120.74(15) . . ? C19 C18 H18 119.6 . . ? C14 C19 H19 119.8 . . ? C18 C19 C14 120.33(15) . . ? C18 C19 H19 119.8 . . ? N2 C20 C11 178.41(18) . . ? C13 C21 H21A 109.4 . . ? C13 C21 H21B 109.4 . . ? C13 C21 C22 111.36(13) . . ? H21A C21 H21B 108.0 . . ? C22 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C21 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C23 C22 C21 112.30(13) . . ? C23 C22 H22A 109.1 . . ? C23 C22 H22B 109.1 . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? C22 C23 C24 110.96(13) . . ? H23A C23 H23B 108.0 . . ? C24 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C23 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C25 C24 C23 112.78(13) . . ? C25 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? N3 C25 C24 178.53(18) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.3802(19) . ? O1 C9 1.422(2) . ? N1 C5 1.386(2) . ? N1 C8 1.377(2) . ? N1 C10 1.437(2) . ? N2 C20 1.148(2) . ? N3 C25 1.144(2) . ? C1 H1 0.9500 . ? C1 C2 1.381(2) . ? C1 C6 1.406(2) . ? C2 C3 1.407(2) . ? C3 H3 0.9500 . ? C3 C4 1.377(2) . ? C4 H4 0.9500 . ? C4 C5 1.394(2) . ? C5 C6 1.409(2) . ? C6 C7 1.434(2) . ? C7 H7 0.9500 . ? C7 C8 1.352(3) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.529(2) . ? C11 C12 1.313(2) . ? C11 C20 1.438(2) . ? C12 C13 1.307(2) . ? C13 C14 1.491(2) . ? C13 C21 1.515(2) . ? C14 C15 1.394(2) . ? C14 C19 1.394(2) . ? C15 H15 0.9500 . ? C15 C16 1.390(2) . ? C16 H16 0.9500 . ? C16 C17 1.389(2) . ? C17 H17 0.9500 . ? C17 C18 1.381(3) . ? C18 H18 0.9500 . ? C18 C19 1.389(2) . ? C19 H19 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.526(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.522(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.523(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C25 1.463(2) . ?