#------------------------------------------------------------------------------ #$Date: 2024-10-09 03:51:26 +0300 (Wed, 09 Oct 2024) $ #$Revision: 295374 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160174.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_7160174 loop_ _publ_author_name 'Duari, Surajit' 'Biswas, Subrata' 'Roy, Arnab' 'Maity, Srabani' 'Elsharif, Asma' 'Biswas, Srijit' _publ_section_title ; MeOTf- catalyzed Friedel-Crafts alkylation of benzoxazolones, benzothiazolones, indolinones and benzimidazolones with activated secondary alcohols ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01372G _journal_year 2024 _chemical_formula_moiety 'C21 H17 N O2' _chemical_formula_sum 'C21 H17 N O2' _chemical_formula_weight 315.36 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-04-04 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _audit_update_record ; 2024-06-28 deposited with the CCDC. 2024-10-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.779(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.0708(12) _cell_length_b 12.580(2) _cell_length_c 21.139(4) _cell_measurement_reflns_used 7321 _cell_measurement_temperature 229.24 _cell_measurement_theta_max 26.97 _cell_measurement_theta_min 2.52 _cell_volume 1613.6(5) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 229.24 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_unetI/netI 0.0655 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 16013 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.005 _diffrn_reflns_theta_min 3.239 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.7449 _exptl_absorpt_correction_T_min 0.5025 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1538 before and 0.1135 after correction. The Ratio of minimum to maximum transmission is 0.6746. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 1.298 _exptl_crystal_description block _exptl_crystal_F_000 664 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.230 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef 0.051(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 3487 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0626 _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^)+(0.0927P)^2^+0.5215P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1658 _refine_ls_wR_factor_ref 0.1824 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2781 _reflns_number_total 3487 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01372g2.cif _cod_data_source_block om36 _cod_original_cell_volume 1613.5(5) _cod_database_code 7160174 _shelx_shelxl_version_number 2016/6 _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.a Ternary CH refined with riding coordinates: C9(H9) 1.b Aromatic/amide H refined with riding coordinates: C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 1.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C) ; _shelx_res_file ; TITL om36_a.res in P2(1)/c om36.res created by SHELXL-2016/6 at 10:51:19 on 03-Apr-2024 REM Old TITL OM36 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.203, Rweak 0.011, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C20 N2 O2 CELL 0.71073 6.0708 12.5796 21.1387 90 91.779 90 ZERR 4 0.0012 0.0022 0.0039 0 0.007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 84 68 4 8 L.S. 10 PLAN 5 TEMP -43.91 CONF BOND $H list 4 fmap 2 acta MORE -1 OMIT 0 6 12 OMIT 0 6 18 REM REM REM WGHT 0.092700 0.521500 EXTI 0.051434 FVAR 1.50481 O1 4 0.839258 0.431727 0.459609 11.00000 0.04320 0.04471 = 0.08707 0.02244 -0.02398 -0.01095 O2 4 0.793387 0.277228 0.513807 11.00000 0.06222 0.05543 = 0.09413 0.03182 -0.01626 -0.00067 N1 3 0.515376 0.351959 0.451288 11.00000 0.03559 0.03754 = 0.04227 0.00320 0.00651 -0.00204 C1 1 0.718775 0.344543 0.478985 11.00000 0.04211 0.03914 = 0.05660 0.00510 -0.00559 0.00041 C2 1 0.503663 0.442722 0.413382 11.00000 0.03252 0.03679 = 0.03585 -0.00122 0.00628 -0.00241 C3 1 0.706218 0.491604 0.419202 11.00000 0.03459 0.03408 = 0.04095 -0.00276 -0.00549 0.00053 C4 1 0.758336 0.583420 0.387268 11.00000 0.03186 0.03481 = 0.05420 0.00215 -0.00772 -0.00552 AFIX 43 H4 2 0.897954 0.615167 0.392294 11.00000 -1.20000 AFIX 0 C5 1 0.595386 0.627289 0.347188 11.00000 0.03359 0.03677 = 0.03229 -0.00400 -0.00096 0.00114 C6 1 0.391796 0.578752 0.341472 11.00000 0.03538 0.07085 = 0.06217 0.02487 -0.01427 -0.00907 AFIX 43 H6 2 0.283117 0.609424 0.314599 11.00000 -1.20000 AFIX 0 C7 1 0.341043 0.485567 0.374186 11.00000 0.03642 0.07376 = 0.07497 0.03006 -0.01084 -0.01602 AFIX 43 H7 2 0.201613 0.453489 0.369606 11.00000 -1.20000 AFIX 0 C8 1 0.342077 0.274206 0.459632 11.00000 0.04673 0.05635 = 0.07502 0.01883 0.00947 -0.01294 AFIX 137 H8A 2 0.302575 0.242131 0.419121 11.00000 -1.50000 H8B 2 0.213961 0.308981 0.476515 11.00000 -1.50000 H8C 2 0.393865 0.219535 0.488837 11.00000 -1.50000 AFIX 0 C9 1 0.635332 0.729539 0.309838 11.00000 0.03276 0.03760 = 0.03166 -0.00033 -0.00498 0.00153 AFIX 13 H9 2 0.499955 0.741682 0.283509 11.00000 -1.20000 AFIX 0 C10 1 0.824206 0.720637 0.263624 11.00000 0.04084 0.03696 = 0.02691 0.00144 -0.00369 0.00221 C11 1 0.873029 0.625322 0.235366 11.00000 0.07355 0.04177 = 0.05247 -0.01335 0.01867 -0.00982 AFIX 43 H11 2 0.795030 0.563906 0.246515 11.00000 -1.20000 AFIX 0 C12 1 1.035131 0.618123 0.190744 11.00000 0.09708 0.04756 = 0.05413 -0.01146 0.02950 0.00367 AFIX 43 H12 2 1.063540 0.552361 0.171520 11.00000 -1.20000 AFIX 0 C13 1 1.154200 0.705869 0.174416 11.00000 0.06707 0.05833 = 0.03565 0.00579 0.01711 0.01064 AFIX 43 H13 2 1.265335 0.700578 0.144587 11.00000 -1.20000 AFIX 0 C14 1 1.109216 0.800882 0.202028 11.00000 0.07176 0.04641 = 0.05485 0.00900 0.02470 -0.00066 AFIX 43 H14 2 1.189618 0.861624 0.190993 11.00000 -1.20000 AFIX 0 C15 1 0.946135 0.809006 0.246236 11.00000 0.07085 0.03497 = 0.05092 0.00368 0.02072 0.00559 AFIX 43 H15 2 0.917453 0.875304 0.264770 11.00000 -1.20000 AFIX 0 C16 1 0.657134 0.825307 0.354134 11.00000 0.03686 0.03422 = 0.02996 0.00151 0.00508 -0.00242 C17 1 0.844960 0.842827 0.391831 11.00000 0.04956 0.03522 = 0.03826 0.00314 -0.00684 -0.00010 AFIX 43 H17 2 0.965370 0.796203 0.389307 11.00000 -1.20000 AFIX 0 C18 1 0.856819 0.928240 0.433106 11.00000 0.06923 0.04298 = 0.03700 0.00083 -0.00917 -0.00746 AFIX 43 H18 2 0.984189 0.938436 0.458815 11.00000 -1.20000 AFIX 0 C19 1 0.682986 0.998595 0.436810 11.00000 0.07205 0.04185 = 0.03797 -0.00775 0.01825 -0.00994 AFIX 43 H19 2 0.692421 1.057041 0.464469 11.00000 -1.20000 AFIX 0 C20 1 0.497100 0.982463 0.399889 11.00000 0.05214 0.05611 = 0.07071 -0.01955 0.02034 0.00499 AFIX 43 H20 2 0.378173 1.030005 0.402230 11.00000 -1.20000 AFIX 0 C21 1 0.482964 0.895998 0.358838 11.00000 0.03882 0.05471 = 0.06336 -0.01548 0.00364 0.00245 AFIX 43 H21 2 0.353742 0.885380 0.333989 11.00000 -1.20000 AFIX 0 HKLF 4 REM om36_a.res in P2(1)/c REM R1 = 0.0626 for 2781 Fo > 4sig(Fo) and 0.0773 for all 3487 data REM 219 parameters refined using 0 restraints END WGHT 0.0927 0.5215 REM Highest difference peak 0.230, deepest hole -0.215, 1-sigma level 0.048 Q1 1 0.5914 0.9962 0.4179 11.00000 0.05 0.23 Q2 1 0.3900 0.4986 0.4107 11.00000 0.05 0.23 Q3 1 0.4762 0.6209 0.3694 11.00000 0.05 0.20 Q4 1 0.6513 0.7826 0.3315 11.00000 0.05 0.20 Q5 1 1.0294 0.8788 0.2916 11.00000 0.05 0.20 ; _shelx_res_checksum 83859 _shelx_hkl_file ; 2 0 0 1524.75 195.88 2 0 0 1754.12 197.08 2 0 0 1792.62 196.78 -2 0 0 1919.91 197.28 -3 0 0 3380.56 351.96 3 0 0 2791.82 351.36 3 0 0 3252.97 351.36 3 0 0 3057.79 350.06 4 0 0 309.27 41.20 -4 0 0 375.26 39.90 4 0 0 355.36 41.20 -4 0 0 288.87 41.00 5 0 0 292.07 37.30 -5 0 0 281.57 35.20 -6 0 0 1445.76 158.18 6 0 0 1486.85 158.28 6 0 0 1203.38 159.68 7 0 0 110.29 17.70 -7 0 0 125.49 21.00 7 0 0 102.49 22.40 1 -1 0 1935.01 230.68 -1 -1 0 2339.17 231.38 1 -1 0 2006.10 230.78 1 -1 0 1891.31 230.48 1 -1 0 2068.79 230.58 -1 1 0 2131.99 230.88 -1 1 0 2040.40 230.58 2 -1 0 2279.27 280.27 -2 -1 0 2577.94 281.27 2 -1 0 2537.55 281.77 -2 -1 0 2473.45 279.97 -2 1 0 2355.86 280.37 2 1 0 2443.56 281.17 -2 1 0 2699.93 280.17 -2 1 0 2604.74 280.87 3 -1 0 829.12 102.89 3 -1 0 1033.80 102.09 -3 -1 0 740.73 102.99 3 -1 0 882.91 102.59 -3 -1 0 824.82 101.79 -3 1 0 985.70 103.49 3 1 0 891.11 103.09 3 1 0 858.31 103.39 3 1 0 960.20 101.69 -3 1 0 956.20 101.99 -4 -1 0 344.27 44.10 -4 -1 0 274.57 41.10 4 -1 0 359.66 42.80 4 -1 0 334.67 41.30 4 -1 0 381.36 41.90 4 1 0 380.66 41.30 4 1 0 305.07 43.20 4 1 0 366.46 43.40 -4 1 0 430.66 44.10 5 -1 0 607.34 75.59 -5 -1 0 680.63 78.69 5 -1 0 633.24 77.09 -5 -1 0 727.43 75.89 5 1 0 622.44 77.69 -5 1 0 628.94 75.59 -6 -1 0 237.98 32.60 6 -1 0 281.07 35.20 6 -1 0 225.48 32.30 -6 1 0 250.47 32.80 6 1 0 304.47 36.90 6 1 0 261.17 32.50 -7 -1 0 13.20 7.20 7 -1 0 -7.70 7.50 7 -1 0 0.40 5.80 7 1 0 10.10 10.40 7 1 0 2.00 5.50 -7 1 0 -3.50 4.90 0 -2 0 559.94 54.89 0 -2 0 416.06 54.69 0 2 0 520.55 54.89 0 2 0 456.75 54.69 2 -2 0 772.42 86.49 -2 -2 0 760.22 87.59 -2 -2 0 819.22 86.19 2 -2 0 673.83 86.09 2 -2 0 792.92 86.79 2 2 0 637.54 87.19 2 2 0 821.02 85.69 2 2 0 821.82 86.09 -2 2 0 737.93 86.29 -2 2 0 766.02 86.39 3 -2 0 8.60 3.20 3 -2 0 2.90 2.80 3 -2 0 7.80 3.60 3 -2 0 10.00 4.50 -3 -2 0 10.70 3.50 -3 -2 0 12.90 6.10 -3 2 0 4.30 2.90 3 2 0 6.30 5.00 3 2 0 12.20 3.10 4 -2 0 729.83 79.19 -4 -2 0 687.33 80.69 4 -2 0 639.14 78.09 4 -2 0 693.03 78.49 -4 2 0 746.53 78.39 4 2 0 618.64 77.49 4 2 0 618.84 80.09 4 2 0 707.03 80.49 5 -2 0 468.35 61.09 5 -2 0 546.05 60.49 -5 -2 0 520.45 63.19 5 2 0 479.75 62.19 -5 2 0 523.25 59.99 -6 -2 0 7.00 5.40 6 -2 0 -3.80 5.40 6 -2 0 4.10 6.90 6 2 0 -4.60 8.10 -6 2 0 1.80 4.30 -7 -2 0 22.40 8.40 7 -2 0 12.50 9.00 7 -2 0 24.50 8.20 7 2 0 27.20 8.00 7 2 0 4.60 8.80 -7 2 0 30.80 9.00 0 -3 0 2.80 1.90 0 -3 0 1.70 1.80 0 3 0 -0.50 1.30 0 3 0 1.00 1.40 1 -3 0 7.80 1.80 1 -3 0 6.60 1.70 -1 -3 0 11.80 3.60 -1 -3 0 8.50 1.90 1 -3 0 6.90 2.20 1 3 0 5.90 2.80 -1 3 0 10.10 2.60 1 3 0 6.50 1.80 -1 3 0 8.60 1.80 2 -3 0 4725.73 570.54 2 -3 0 5449.65 570.94 -2 -3 0 5307.07 572.04 -2 3 0 4561.64 570.24 2 3 0 5444.66 571.94 3 -3 0 950.80 104.59 3 -3 0 896.51 103.99 -3 -3 0 891.71 106.09 -3 -3 0 1041.30 104.19 3 -3 0 960.90 104.89 3 -3 0 791.82 103.99 -3 3 0 967.80 104.49 3 3 0 835.12 103.09 3 3 0 1091.19 106.69 3 3 0 779.62 103.49 -4 -3 0 95.49 15.80 -4 -3 0 137.09 19.80 4 -3 0 104.99 15.80 4 -3 0 117.29 16.50 4 -3 0 117.69 17.00 4 3 0 146.19 20.80 -4 3 0 147.79 16.80 4 3 0 78.49 18.20 4 3 0 163.68 16.00 -5 -3 0 175.18 24.60 5 -3 0 136.59 20.60 5 -3 0 118.89 21.00 5 -3 0 155.58 21.30 5 3 0 157.38 23.70 -5 3 0 175.08 20.90 -6 -3 0 31.40 8.70 6 -3 0 27.00 8.90 6 -3 0 31.60 8.70 -6 3 0 20.90 8.00 6 3 0 15.80 9.40 7 -3 0 190.58 26.10 -7 -3 0 149.59 23.40 7 3 0 184.48 23.40 7 3 0 141.89 28.60 0 -4 0 38.80 5.10 0 4 0 29.60 5.10 1 -4 0 824.92 90.59 -1 4 0 864.71 89.89 -1 4 0 694.63 90.49 2 -4 0 4418.16 504.25 2 -4 0 4257.57 503.85 2 -4 0 4498.85 504.55 -2 4 0 4825.12 504.75 3 -4 0 1220.38 134.29 3 -4 0 1248.28 134.09 -3 -4 0 1112.49 133.39 3 -4 0 1280.47 133.29 -3 -4 0 1116.69 135.69 -3 4 0 1086.69 133.59 -4 -4 0 83.89 16.60 4 -4 0 89.19 13.10 4 -4 0 84.09 12.10 -4 -4 0 92.19 12.50 4 -4 0 84.29 13.00 4 4 0 82.69 11.00 5 -4 0 0.40 4.60 5 -4 0 0.30 4.80 5 -4 0 0.90 4.60 -5 -4 0 8.30 9.30 -5 -4 0 1.30 4.00 5 4 0 1.20 7.20 5 4 0 -1.00 2.70 6 -4 0 249.97 31.70 6 -4 0 230.98 31.50 -6 -4 0 222.58 31.00 6 4 0 275.37 35.70 -7 -4 0 74.09 13.20 7 -4 0 49.40 11.90 7 -4 0 60.39 12.70 7 4 0 22.10 13.10 0 -5 0 0.40 1.90 0 5 0 -0.30 1.70 1 -5 0 81.29 8.50 1 -5 0 79.09 9.40 1 -5 0 51.39 9.70 -1 -5 0 79.59 10.90 -1 -5 0 66.89 9.30 1 5 0 80.09 10.50 -1 5 0 78.79 9.20 -1 5 0 60.09 10.00 1 5 0 64.19 9.40 2 -5 0 1247.58 123.79 -2 -5 0 1155.08 123.59 -2 -5 0 1068.39 125.79 2 -5 0 1010.30 124.59 2 5 0 1018.20 125.39 -2 5 0 949.80 124.59 2 5 0 1225.18 123.89 -2 5 0 1066.19 123.89 3 -5 0 274.87 30.40 -3 -5 0 186.98 31.80 -3 -5 0 226.28 29.80 3 -5 0 260.27 30.60 3 -5 0 283.57 31.40 3 -5 0 277.27 29.50 3 5 0 266.37 32.60 3 5 0 255.27 29.40 -3 5 0 227.88 30.00 4 -5 0 427.16 48.20 -4 -5 0 428.36 50.99 4 -5 0 367.26 47.40 -4 -5 0 431.76 47.40 -4 5 0 363.16 47.10 -5 -5 0 76.79 18.30 -5 -5 0 116.49 14.70 5 -5 0 90.89 13.40 5 -5 0 83.29 14.40 5 -5 0 86.09 15.20 5 5 0 83.19 18.10 6 -5 0 10.10 6.40 6 -5 0 3.80 5.20 -6 -5 0 5.80 5.50 6 5 0 -3.80 8.10 7 -5 0 -0.80 5.50 7 -5 0 -3.60 5.40 -7 -5 0 -2.30 5.40 7 5 0 -4.30 8.20 0 -6 0 14.80 4.20 0 -6 0 18.10 4.10 0 6 0 18.10 3.70 0 6 0 18.50 4.40 0 6 0 29.10 4.40 1 -6 0 435.76 50.09 -1 6 0 418.66 49.10 1 6 0 438.16 50.09 2 -6 0 0.60 1.40 -2 -6 0 2.90 2.10 2 -6 0 0.20 2.40 2 -6 0 1.30 2.00 -2 -6 0 0.00 4.30 2 6 0 0.70 4.10 2 6 0 0.60 2.00 -2 6 0 2.60 2.30 -2 6 0 1.60 2.40 -3 -6 0 1196.38 151.08 3 -6 0 1280.07 149.29 3 -6 0 1428.66 149.99 3 -6 0 1397.76 148.19 3 6 0 1425.66 151.48 -3 6 0 1164.78 148.59 3 6 0 1315.47 148.29 -4 -6 0 87.79 12.30 4 -6 0 94.29 11.40 4 -6 0 93.29 13.60 4 -6 0 69.29 12.00 -4 -6 0 98.59 18.20 4 6 0 58.29 10.70 -4 6 0 93.39 12.60 -5 -6 0 687.73 85.79 5 -6 0 784.82 87.09 -5 -6 0 687.13 89.89 5 6 0 828.72 84.89 5 6 0 679.53 89.49 -6 -6 0 26.50 8.20 6 -6 0 45.70 8.80 6 6 0 29.40 12.30 -7 -6 0 47.50 12.10 7 -6 0 46.80 12.70 7 -6 0 59.99 11.50 7 6 0 47.70 16.70 0 -7 0 1.10 2.40 0 -7 0 2.90 2.50 0 7 0 2.50 2.20 0 7 0 1.50 1.70 0 7 0 0.40 2.50 -1 -7 0 171.08 19.80 -1 7 0 127.29 19.00 -1 7 0 142.79 18.10 1 7 0 159.58 19.10 2 -7 0 0.70 1.70 -2 -7 0 0.60 2.20 2 -7 0 3.10 3.10 -2 -7 0 0.00 4.20 -2 7 0 2.80 3.80 2 7 0 4.40 3.30 -2 7 0 4.20 2.40 2 7 0 0.80 1.90 -3 -7 0 10.10 2.90 -3 -7 0 6.40 6.90 3 -7 0 8.10 2.90 3 -7 0 7.10 4.80 -3 -7 0 4.90 3.10 3 -7 0 8.90 3.20 -3 7 0 3.60 3.40 3 7 0 5.50 3.00 3 7 0 5.00 4.60 4 -7 0 27.30 5.20 4 -7 0 24.90 5.80 -4 -7 0 16.80 5.90 4 -7 0 10.40 5.60 -4 -7 0 12.60 8.50 -4 7 0 25.00 6.20 4 7 0 20.20 4.70 5 -7 0 0.30 3.30 -5 -7 0 -5.20 3.50 -5 -7 0 -5.00 6.90 5 -7 0 6.10 4.60 5 -7 0 3.60 5.60 5 7 0 0.10 3.30 6 -7 0 39.10 8.00 6 -7 0 43.00 10.70 -6 -7 0 36.90 8.90 6 7 0 25.30 11.80 0 -8 0 20.40 5.10 0 -8 0 37.20 6.50 0 8 0 26.00 5.40 0 8 0 24.20 5.90 -1 -8 0 1373.96 165.08 -1 -8 0 1339.77 164.28 -1 8 0 1499.25 164.08 -1 8 0 1634.54 165.68 1 8 0 1442.16 164.78 -2 -8 0 3.20 5.00 2 -8 0 4.40 4.40 -2 -8 0 6.90 2.80 -2 8 0 5.00 2.90 2 8 0 5.70 4.50 2 8 0 8.70 3.30 3 -8 0 574.74 69.89 -3 -8 0 546.15 71.49 3 -8 0 616.34 68.19 -3 -8 0 692.63 68.29 3 -8 0 620.64 67.39 3 8 0 520.05 68.29 -3 8 0 571.74 68.69 4 -8 0 34.50 9.00 -4 -8 0 26.80 7.40 4 -8 0 45.20 6.90 4 -8 0 39.40 6.50 -4 -8 0 47.30 12.90 -4 8 0 20.70 6.70 5 -8 0 32.50 6.80 5 -8 0 26.50 5.90 -5 -8 0 1.50 9.30 -5 -8 0 26.30 7.70 5 -8 0 22.80 8.20 5 8 0 22.20 6.00 6 -8 0 -9.80 4.80 6 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-2 2 22 196.18 26.50 1 -2 -22 26.60 4.90 -1 -2 22 20.00 8.30 -1 2 22 37.10 9.10 0 -2 22 26.00 10.00 0 -2 -22 26.60 5.80 0 2 22 27.30 9.10 -1 -2 -22 86.89 14.60 -1 2 -22 126.79 14.60 2 -2 22 12.30 8.10 -2 -2 -22 2.10 4.60 2 2 22 15.10 8.40 -2 2 -22 -1.50 3.80 -3 -2 -22 -5.60 5.80 3 -2 22 29.40 10.10 -3 2 -22 0.80 5.10 3 2 22 -1.30 8.90 4 -2 22 32.40 11.80 -4 -2 -22 14.30 7.50 4 2 22 7.50 9.40 -4 2 -22 20.20 7.70 4 -3 -22 21.20 5.40 -4 -3 22 26.70 11.80 -4 3 22 14.40 9.10 -3 -3 22 1.40 6.80 3 -3 -22 -0.10 1.70 3 -3 -22 2.00 3.40 -3 -3 22 -1.80 3.80 -3 3 22 -1.00 8.10 2 -3 -22 56.19 7.80 -2 -3 22 65.89 15.50 -2 -3 22 46.90 8.90 -2 3 22 81.19 15.40 -2 3 22 60.19 10.60 -1 -3 22 -3.10 6.00 -1 -3 22 -4.70 5.00 1 -3 -22 0.20 2.50 -1 -3 22 -0.30 3.70 -1 3 22 -6.80 4.50 0 -3 -22 44.60 8.50 0 -3 22 47.10 12.00 0 3 22 75.19 13.00 -1 -3 -22 261.57 35.70 1 -3 22 286.97 38.50 1 3 22 370.66 39.80 -2 -3 -22 1.80 5.00 2 -3 22 0.00 6.90 2 3 22 9.00 7.20 -3 -3 -22 4.80 5.60 3 -3 22 -0.70 8.10 -3 3 -22 4.30 5.60 3 3 22 -2.20 7.60 -4 -3 -22 63.99 14.30 4 -3 22 112.29 19.60 4 3 22 74.99 18.80 -4 3 -22 81.69 14.90 4 -4 -22 20.50 5.80 -4 -4 22 31.20 13.30 -4 4 22 29.60 12.20 -3 -4 22 -3.20 8.00 3 -4 -22 1.90 3.80 3 -4 -22 -5.60 2.90 2 -4 -22 49.80 8.80 -2 -4 22 46.50 7.60 2 -4 -22 26.90 9.10 -2 -4 22 41.50 13.00 2 -4 -22 48.00 6.90 -2 4 22 58.29 13.20 -2 4 22 53.19 9.10 -1 -4 22 -2.30 4.10 -1 -4 22 -0.80 7.20 1 -4 -22 2.70 2.80 -1 4 22 3.30 4.90 0 -4 -22 21.80 5.60 0 -4 22 19.80 8.60 0 4 22 20.90 7.40 -1 -4 -22 0.10 4.10 1 -4 22 3.40 5.90 1 4 22 3.30 6.00 2 -4 22 25.60 10.20 -2 -4 -22 37.30 8.90 2 4 22 38.90 10.90 -3 -4 -22 4.70 7.10 3 -4 22 3.40 7.50 3 4 22 9.40 8.20 3 -5 -22 179.78 22.50 -3 -5 22 160.58 28.80 2 -5 -22 61.59 10.50 -2 -5 22 61.59 16.30 2 -5 -22 43.90 10.70 -2 -5 22 61.99 9.00 -2 -5 22 48.60 8.30 -2 5 22 57.99 9.30 -2 5 22 75.79 14.30 1 -5 -22 7.60 5.10 -1 -5 22 -1.90 7.00 -1 -5 22 -5.20 3.60 -1 -5 22 2.40 7.30 -1 5 22 2.20 4.80 0 -5 -22 139.69 21.00 0 -5 22 188.18 25.60 0 5 22 196.88 24.00 1 -5 22 6.20 7.40 -1 -5 -22 4.70 4.10 1 5 22 3.00 6.00 -2 -5 -22 72.39 12.30 2 -5 22 45.40 12.80 2 5 22 69.19 15.20 3 -5 22 9.00 8.00 -3 -5 -22 16.80 7.20 3 5 22 12.70 9.70 -3 -6 22 8.40 9.80 3 -6 -22 -1.00 5.10 -3 6 22 7.80 7.80 2 -6 -22 2.40 4.90 -2 -6 22 10.30 9.90 2 -6 -22 -8.10 5.20 -2 -6 22 -5.80 2.90 -2 -6 22 2.20 3.10 -2 6 22 5.90 3.40 -2 6 22 4.10 6.90 -1 -6 22 3.80 6.90 1 -6 -22 2.20 4.40 -1 -6 22 -1.70 4.40 1 -6 -22 0.80 3.40 -1 -6 22 5.00 9.10 -1 6 22 3.50 4.80 0 -6 22 23.30 8.80 0 -6 -22 19.30 6.30 0 6 22 41.40 9.20 -1 -6 -22 16.30 5.30 1 -6 22 20.30 8.50 1 -6 22 7.80 4.20 1 6 22 22.20 8.30 -2 -6 -22 6.20 5.80 2 -6 22 7.80 7.80 2 6 22 11.00 8.00 3 -6 22 -3.30 6.30 -3 -6 -22 1.70 4.80 3 6 22 -0.90 8.70 -3 -7 22 11.60 11.40 3 -7 -22 4.00 5.40 -3 7 22 4.20 8.00 2 -7 -22 0.30 4.00 -2 -7 22 5.60 9.30 -2 -7 22 0.10 2.40 -2 7 22 -2.20 5.70 1 -7 -22 -3.80 3.70 1 -7 -22 -1.70 3.70 -1 -7 22 -4.30 5.90 -1 -7 22 2.60 8.20 -1 -7 22 -1.00 4.70 -1 7 22 -6.10 3.70 0 -7 -22 19.60 6.80 0 -7 -22 25.90 6.60 0 -7 22 20.30 7.60 0 -7 22 33.40 10.20 0 -7 22 23.20 11.20 0 7 22 26.50 8.00 -1 -7 -22 27.60 7.80 1 -7 22 14.50 8.40 1 -7 22 44.40 11.60 1 7 22 29.20 9.60 -2 -7 -22 24.20 7.80 2 -7 22 26.10 9.20 2 7 22 6.50 7.70 2 -8 -22 0.60 4.60 -2 -8 22 8.20 10.10 -2 8 22 -8.60 6.00 1 -8 -22 74.89 13.50 -1 -8 22 94.69 20.20 -1 -8 22 71.79 15.10 0 -8 -22 23.00 7.80 0 -8 22 48.20 9.90 0 -8 -22 46.40 9.60 0 -8 22 42.00 13.60 0 -8 22 33.70 10.80 0 8 22 62.79 11.60 -1 -8 -22 37.40 8.90 1 -8 22 32.90 10.30 1 -8 22 36.50 11.50 1 8 22 38.70 10.90 2 -8 22 21.50 9.30 2 -8 22 -8.60 7.80 -2 -8 -22 -4.20 5.90 2 8 22 -6.60 7.70 -1 -9 22 15.00 10.20 1 -9 -22 34.00 8.60 -1 -9 22 16.90 6.70 -1 9 22 23.50 6.30 0 -9 -22 -0.50 4.10 0 -9 22 -13.40 4.50 0 -9 -22 4.50 5.40 0 -9 22 -8.40 7.30 0 -9 22 -1.60 6.20 0 9 22 5.20 6.30 -4 0 23 -11.00 7.60 -3 0 23 -0.20 7.10 -3 0 23 -9.80 4.90 -2 0 23 0.00 6.20 -2 0 23 -3.90 4.40 -1 0 23 -1.20 5.50 0 0 -23 3.40 2.60 0 0 23 5.40 6.80 -1 0 -23 2.60 3.60 -2 0 -23 10.50 5.60 2 0 23 3.40 7.70 -3 0 -23 -2.60 5.00 3 0 23 2.50 8.00 -4 -1 23 0.40 9.80 -4 1 23 5.90 8.80 -3 -1 23 -9.50 4.50 -3 -1 23 4.80 8.30 -3 1 23 17.10 10.70 -2 -1 23 12.00 8.80 -2 -1 23 13.20 6.60 -2 1 23 5.50 8.50 -2 1 23 11.50 6.20 -1 -1 23 14.90 8.50 -1 1 23 21.60 7.50 0 -1 -23 232.08 27.60 0 -1 23 206.48 30.90 0 1 23 262.17 31.90 -1 -1 -23 10.00 4.70 1 -1 23 13.80 7.80 -1 1 -23 15.70 4.70 1 1 23 17.30 8.00 -2 -1 -23 0.40 4.60 2 -1 23 0.90 7.20 -2 1 -23 2.30 4.30 2 1 23 11.10 11.40 -3 -1 -23 125.29 18.80 3 -1 23 143.69 22.60 3 1 23 108.29 22.20 -4 -2 23 25.80 13.30 -4 2 23 29.80 11.70 -3 -2 23 -0.10 5.60 -3 -2 23 -3.10 7.50 -3 2 23 8.70 9.20 -2 -2 23 56.39 10.30 -2 -2 23 91.89 18.60 -2 2 23 80.29 16.80 -2 2 23 60.69 11.60 -1 -2 23 63.89 14.60 1 -2 -23 69.49 9.50 -1 2 23 79.99 13.00 0 -2 -23 1.90 3.70 0 2 23 6.40 6.30 1 -2 23 393.06 50.69 -1 -2 -23 412.36 47.90 2 -2 23 45.60 12.20 -2 -2 -23 33.50 8.20 -2 2 -23 33.90 7.60 2 2 23 38.30 11.10 3 -2 23 -1.30 6.80 -3 -2 -23 -4.70 4.50 -3 2 -23 -0.10 5.00 3 2 23 -1.80 7.30 4 -3 -23 -0.80 3.40 -4 -3 23 -8.00 8.60 -4 3 23 4.50 7.60 -3 -3 23 17.50 10.90 -3 3 23 18.20 9.80 2 -3 -23 27.20 5.40 2 -3 -23 42.40 5.50 -2 -3 23 56.29 14.50 -2 -3 23 17.30 6.20 -2 3 23 46.50 12.10 -2 3 23 35.30 7.90 -1 -3 23 29.00 11.00 1 -3 -23 22.00 4.90 -1 3 23 30.90 8.70 0 -3 23 163.38 26.80 0 -3 -23 185.48 24.20 0 3 23 231.58 26.90 1 -3 23 6.70 7.00 -1 -3 -23 4.90 4.10 1 3 23 18.00 8.20 -2 -3 -23 4.50 5.50 2 -3 23 24.70 9.20 2 3 23 17.00 9.20 3 -3 23 16.30 9.20 3 3 23 7.40 8.80 -3 3 -23 8.60 6.10 -3 -4 23 -5.00 8.20 3 -4 -23 6.70 4.10 3 -4 -23 0.20 2.20 -3 4 23 5.40 7.70 2 -4 -23 5.60 4.80 -2 -4 23 5.90 8.70 -2 4 23 11.40 8.00 -2 4 23 0.00 4.00 1 -4 -23 9.10 3.40 -1 -4 23 -4.30 5.80 -1 -4 23 10.70 6.80 -1 -4 23 -8.90 5.90 -1 4 23 0.30 5.20 0 -4 23 47.10 12.00 0 -4 -23 42.70 8.40 0 4 23 75.59 12.80 -1 -4 -23 37.20 8.90 1 -4 23 65.89 13.70 1 4 23 66.29 13.00 -2 -4 -23 2.10 5.30 2 -4 23 5.60 8.10 2 4 23 4.10 8.30 -3 -4 -23 8.90 5.90 3 -4 23 16.40 9.00 3 4 23 25.80 12.00 -3 -5 23 235.58 33.00 3 -5 -23 195.98 25.10 -3 5 23 177.38 28.90 -2 -5 23 6.10 4.10 2 -5 -23 6.60 8.40 2 -5 -23 4.30 4.80 -2 -5 23 7.40 10.60 -2 5 23 12.20 4.60 -1 -5 23 370.56 48.40 1 -5 -23 338.57 42.40 -1 -5 23 316.77 45.60 -1 5 23 428.06 44.70 0 -5 -23 17.60 5.30 0 -5 23 17.10 8.30 0 5 23 23.40 7.80 -1 -5 -23 116.49 19.20 1 -5 23 159.98 22.90 1 5 23 184.28 22.90 -2 -5 -23 8.90 5.30 2 -5 23 26.80 10.30 2 5 23 15.20 9.50 -3 -5 -23 168.88 23.00 3 -5 23 136.79 24.30 3 5 23 176.28 27.10 3 -6 -23 41.10 9.00 -3 -6 23 46.10 15.30 2 -6 -23 -2.30 3.70 -2 -6 23 7.00 9.20 -2 -6 23 2.10 3.30 -2 6 23 6.80 11.20 -1 -6 23 -1.90 6.50 -1 -6 23 2.40 4.30 1 -6 -23 -5.80 3.00 1 -6 -23 7.30 4.80 -1 -6 23 -5.00 7.20 -1 6 23 9.60 5.30 0 -6 -23 50.69 9.70 0 -6 23 50.79 13.50 0 6 23 75.29 12.90 1 -6 23 0.30 6.20 -1 -6 -23 -8.30 4.50 1 6 23 8.00 7.80 2 -6 23 20.50 9.20 -2 -6 -23 15.90 7.40 2 6 23 18.40 9.10 2 -7 -23 1.70 4.50 -2 -7 23 -5.10 6.40 -2 7 23 3.30 6.80 -1 -7 23 -3.80 4.50 1 -7 -23 -2.50 3.60 1 -7 -23 4.40 4.90 -1 -7 23 5.80 9.00 -1 7 23 -2.90 4.70 0 -7 -23 134.39 21.20 0 -7 23 168.68 25.30 0 -7 23 187.98 27.30 0 7 23 194.28 24.20 1 -7 23 34.50 11.40 1 -7 23 38.90 11.90 -1 -7 -23 39.80 9.10 1 7 23 54.89 12.90 -2 -7 -23 157.28 23.60 2 -7 23 181.68 26.50 2 7 23 188.98 27.90 1 -8 -23 10.10 6.00 -1 -8 23 0.10 4.90 1 -8 -23 -0.10 4.10 -1 -8 23 34.60 12.40 -1 8 23 7.50 5.30 0 -8 23 60.79 15.60 0 -8 -23 57.19 11.80 0 -8 23 47.00 11.30 0 -8 -23 58.49 10.60 0 -8 23 68.09 15.30 0 8 23 67.99 12.50 1 -8 23 130.49 20.70 1 8 23 99.19 21.00 -3 0 24 35.30 13.50 -2 0 24 72.79 14.60 -2 0 24 109.19 20.30 -1 0 24 129.59 20.00 0 0 24 159.88 24.50 0 0 -24 158.08 19.00 1 0 24 163.18 21.70 -1 0 -24 116.89 16.80 -2 0 -24 62.69 11.40 3 0 24 0.70 7.80 -3 0 -24 3.80 6.30 -3 -1 24 109.99 23.30 -3 1 24 138.29 22.90 -2 -1 24 18.30 10.20 -2 -1 24 17.00 6.80 -2 1 24 4.90 5.60 -2 1 24 17.50 8.90 -1 -1 24 309.27 38.60 -1 1 24 281.57 37.70 0 -1 -24 144.79 18.60 0 -1 24 161.88 23.30 0 1 24 157.48 23.20 1 -1 24 75.09 15.00 -1 -1 -24 54.79 9.90 -1 1 -24 51.39 9.30 1 1 24 77.19 14.60 2 -1 24 8.80 8.50 -2 -1 -24 5.60 5.10 -2 1 -24 -1.00 4.80 2 1 24 7.60 7.70 3 -1 24 11.70 8.70 -3 -1 -24 -3.40 5.20 -3 1 -24 -8.10 4.80 3 1 24 5.20 9.30 -3 -2 24 18.50 10.50 -3 2 24 11.50 8.90 -2 -2 24 0.80 6.30 -2 -2 24 11.60 8.40 -2 2 24 11.50 8.60 -2 2 24 12.20 6.10 1 -2 -24 36.80 6.10 -1 -2 24 32.70 10.30 -1 -2 24 45.90 14.20 -1 2 24 55.59 11.40 0 -2 24 53.29 12.40 0 -2 -24 37.40 7.00 0 2 24 23.40 9.30 1 -2 24 55.39 14.10 1 2 24 73.59 14.90 -2 -2 -24 18.90 6.60 2 -2 24 30.10 10.10 -2 2 -24 17.70 6.00 2 2 24 46.00 12.80 3 -2 24 3.50 8.30 -3 2 -24 -4.60 4.70 3 2 24 5.20 9.00 -3 -3 24 5.40 9.90 -3 3 24 4.20 9.80 2 -3 -24 -1.40 1.90 -2 -3 24 -4.60 6.50 -2 3 24 2.40 4.80 -2 3 24 -2.70 7.30 -1 -3 24 42.40 13.40 1 -3 -24 32.70 5.90 -1 -3 24 24.60 10.00 -1 3 24 28.90 8.70 0 -3 24 3.00 6.50 0 3 24 6.90 6.80 -1 -3 -24 10.60 5.40 1 -3 24 1.30 7.30 1 3 24 0.70 8.30 -2 -3 -24 25.60 8.00 2 -3 24 12.50 10.10 2 3 24 24.50 10.90 3 -3 24 12.40 9.50 -3 -3 -24 -0.30 5.80 3 3 24 5.30 8.60 3 -4 -24 5.20 2.50 3 -4 -24 5.10 4.20 -3 -4 24 5.20 9.10 -3 4 24 12.10 8.00 -2 -4 24 -0.30 8.20 2 -4 -24 8.40 3.10 -2 4 24 2.40 4.50 -2 4 24 4.40 7.70 1 -4 -24 5.10 3.30 -1 -4 24 -3.90 6.70 -1 -4 24 -9.80 6.50 -1 4 24 0.30 5.30 0 -4 24 69.49 14.60 0 -4 -24 47.10 9.40 0 4 24 84.59 14.40 -1 -4 -24 32.50 8.00 1 -4 24 38.80 11.50 1 4 24 37.70 13.80 -2 -4 -24 -4.60 4.50 2 -4 24 -6.70 6.60 2 4 24 -3.90 6.70 -2 -5 24 12.90 4.90 2 -5 -24 19.60 5.60 -2 -5 24 16.40 9.40 -2 5 24 16.20 5.50 -2 5 24 17.10 8.60 -1 -5 24 15.20 9.90 1 -5 -24 3.50 3.80 -1 -5 24 9.50 7.40 -1 5 24 0.90 5.30 0 -5 24 7.20 6.40 0 -5 -24 -4.80 3.40 0 5 24 3.20 6.40 -1 -5 -24 21.60 6.70 1 -5 24 28.90 10.30 1 5 24 56.09 16.70 -2 -5 -24 9.30 7.00 2 -5 24 4.70 8.00 2 5 24 -7.10 7.50 2 -6 -24 22.70 6.40 -2 -6 24 14.80 4.60 2 -6 -24 23.20 5.30 -2 -6 24 20.90 12.20 -2 6 24 9.80 8.90 1 -6 -24 33.00 8.50 -1 -6 24 61.69 15.80 -1 -6 24 42.60 12.30 -1 -6 24 26.80 7.70 1 -6 -24 46.10 8.00 -1 6 24 48.00 9.70 0 -6 24 5.00 7.20 0 -6 24 3.40 9.00 0 -6 -24 5.30 4.80 0 6 24 6.80 6.60 1 -6 24 4.50 7.00 -1 -6 -24 -3.50 4.30 1 6 24 -3.30 7.20 1 -7 -24 -0.20 4.40 -1 -7 24 -5.40 4.50 -1 -7 24 4.30 9.60 -1 7 24 10.40 6.20 0 -7 24 -7.50 5.80 0 -7 24 -14.60 6.20 0 -7 24 13.70 8.50 0 -7 -24 -1.50 4.10 0 7 24 -2.70 6.20 -3 0 25 10.20 8.00 -2 0 25 5.80 9.90 -1 0 25 2.30 7.10 0 0 25 3.30 7.30 -1 0 -25 2.40 4.80 1 0 25 19.80 8.90 -2 0 -25 -2.80 4.70 2 0 25 -1.20 7.30 -3 -1 25 1.00 8.10 -3 1 25 3.30 8.00 -2 -1 25 3.40 8.10 -2 1 25 6.10 8.80 -2 1 25 0.60 5.90 -1 -1 25 59.99 13.70 -1 1 25 74.19 13.90 0 -1 25 367.26 44.70 0 -1 -25 313.27 40.20 0 1 25 397.06 45.20 -1 -1 -25 47.70 9.20 1 -1 25 70.19 14.70 -1 1 -25 50.39 8.60 1 1 25 49.10 13.90 2 -1 25 38.30 12.60 -2 -1 -25 20.40 7.00 -2 1 -25 16.90 6.20 2 1 25 22.00 11.40 -2 -2 25 70.49 17.50 -2 2 25 37.50 9.40 -2 2 25 38.80 13.00 -1 -2 25 13.50 7.30 -1 -2 25 -1.90 9.30 -1 2 25 -5.40 5.70 0 -2 25 86.79 17.60 0 2 25 91.79 17.30 1 -2 25 115.19 22.30 -1 -2 -25 132.59 17.80 1 2 25 137.69 21.40 2 -2 25 110.19 19.40 2 2 25 96.79 18.30 -2 2 -25 74.79 13.60 -2 -3 25 0.10 8.50 -2 3 25 11.80 8.60 -2 3 25 -0.90 5.40 1 -3 -25 4.80 3.30 -1 -3 25 9.20 8.00 -1 -3 25 10.00 10.10 -1 3 25 -5.50 5.40 0 -3 25 0.00 6.40 0 3 25 1.80 6.90 1 -3 25 25.60 9.90 -1 -3 -25 19.90 6.80 1 3 25 15.30 8.70 -2 -3 -25 19.50 7.20 2 -3 25 23.80 11.70 2 3 25 34.80 11.90 -2 -4 25 12.00 10.60 2 -4 -25 2.60 2.70 -2 4 25 -11.90 5.30 -2 4 25 0.00 4.60 -1 -4 25 60.69 14.80 -1 -4 25 88.39 19.20 1 -4 -25 64.69 10.10 -1 4 25 71.39 13.40 0 -4 25 13.20 8.30 0 -4 -25 4.60 4.30 0 4 25 16.90 8.40 1 -4 25 2.00 7.90 -1 -4 -25 3.60 4.80 1 4 25 -15.20 6.00 1 -5 -25 7.60 4.00 -1 -5 25 0.90 7.80 -1 -5 25 9.00 9.70 -1 5 25 10.80 6.80 0 -5 -25 78.19 13.80 0 -5 25 133.49 19.90 0 5 25 125.69 18.10 1 -5 25 24.10 10.60 -1 -5 -25 21.40 6.50 1 5 25 19.70 9.70 0 -6 25 -1.00 7.50 0 -6 -25 0.00 4.70 0 -6 25 24.80 9.50 0 6 25 5.00 7.30 -2 0 26 -6.20 8.70 -1 0 26 163.78 24.80 0 0 26 92.09 18.20 1 0 26 86.69 16.30 -1 0 -26 44.80 13.30 -2 -1 26 4.50 10.50 -2 1 26 7.90 6.90 -2 1 26 9.40 10.00 -1 -1 26 87.79 19.70 -1 -1 26 59.79 13.70 -1 1 26 70.29 18.70 0 -1 -26 121.89 16.70 0 -1 26 162.38 23.50 0 1 26 153.38 22.40 1 -1 26 316.47 42.50 1 1 26 329.67 42.50 -2 -2 26 -1.90 10.00 -2 2 26 8.70 6.50 -2 2 26 5.10 8.80 -1 -2 26 11.70 7.70 -1 -2 26 -1.10 8.50 -1 2 26 13.80 7.60 0 -2 -26 5.70 4.10 0 -2 26 28.50 11.00 0 2 26 18.90 9.50 1 -2 26 51.19 13.10 -1 -2 -26 34.20 8.30 1 2 26 64.19 13.50 -1 -3 26 33.50 11.70 1 -3 -26 28.30 5.30 -1 -3 26 18.50 11.10 -1 3 26 31.80 10.10 0 -3 26 89.09 17.90 0 3 26 96.69 17.40 1 -3 26 38.80 12.10 -1 -3 -26 30.90 7.70 1 3 26 27.20 10.10 -1 -4 26 -2.20 7.10 -1 4 26 12.50 7.50 0 -4 26 24.60 10.10 0 -4 -26 18.90 5.50 0 4 26 5.70 9.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 29929 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.8393(2) 0.43173(11) 0.45961(8) 0.0589(5) Uani 1 1 d . . . . . O2 O 0.7934(3) 0.27723(13) 0.51381(9) 0.0710(5) Uani 1 1 d . . . . . N1 N 0.5154(2) 0.35196(12) 0.45129(7) 0.0384(4) Uani 1 1 d . . . . . C1 C 0.7188(3) 0.34454(15) 0.47898(10) 0.0461(5) Uani 1 1 d . . . . . C2 C 0.5037(3) 0.44272(14) 0.41338(8) 0.0349(4) Uani 1 1 d . . . . . C3 C 0.7062(3) 0.49160(14) 0.41920(8) 0.0367(4) Uani 1 1 d . . . . . C4 C 0.7583(3) 0.58342(14) 0.38727(9) 0.0405(4) Uani 1 1 d . . . . . H4 H 0.897954 0.615167 0.392294 0.049 Uiso 1 1 calc R U . . . C5 C 0.5954(3) 0.62729(14) 0.34719(8) 0.0343(4) Uani 1 1 d . . . . . C6 C 0.3918(3) 0.57875(19) 0.34147(11) 0.0565(6) Uani 1 1 d . . . . . H6 H 0.283117 0.609424 0.314599 0.068 Uiso 1 1 calc R U . . . C7 C 0.3410(3) 0.4856(2) 0.37419(12) 0.0620(7) Uani 1 1 d . . . . . H7 H 0.201613 0.453489 0.369606 0.074 Uiso 1 1 calc R U . . . C8 C 0.3421(4) 0.27421(18) 0.45963(12) 0.0592(6) Uani 1 1 d . . . . . H8A H 0.302575 0.242131 0.419121 0.089 Uiso 1 1 calc R U . . . H8B H 0.213961 0.308981 0.476515 0.089 Uiso 1 1 calc R U . . . H8C H 0.393865 0.219535 0.488837 0.089 Uiso 1 1 calc R U . . . C9 C 0.6353(3) 0.72954(13) 0.30984(8) 0.0341(4) Uani 1 1 d . . . . . H9 H 0.499955 0.741682 0.283509 0.041 Uiso 1 1 calc R U . . . C10 C 0.8242(3) 0.72064(13) 0.26362(7) 0.0350(4) Uani 1 1 d . . . . . C11 C 0.8730(4) 0.62532(17) 0.23537(10) 0.0556(6) Uani 1 1 d . . . . . H11 H 0.795030 0.563906 0.246515 0.067 Uiso 1 1 calc R U . . . C12 C 1.0351(5) 0.61812(19) 0.19074(11) 0.0657(7) Uani 1 1 d . . . . . H12 H 1.063540 0.552361 0.171520 0.079 Uiso 1 1 calc R U . . . C13 C 1.1542(4) 0.70587(18) 0.17442(9) 0.0534(6) Uani 1 1 d . . . . . H13 H 1.265335 0.700578 0.144587 0.064 Uiso 1 1 calc R U . . . C14 C 1.1092(4) 0.80088(18) 0.20203(10) 0.0572(6) Uani 1 1 d . . . . . H14 H 1.189618 0.861624 0.190993 0.069 Uiso 1 1 calc R U . . . C15 C 0.9461(4) 0.80901(16) 0.24624(10) 0.0519(5) Uani 1 1 d . . . . . H15 H 0.917453 0.875304 0.264770 0.062 Uiso 1 1 calc R U . . . C16 C 0.6571(3) 0.82531(13) 0.35413(7) 0.0336(4) Uani 1 1 d . . . . . C17 C 0.8450(3) 0.84283(14) 0.39183(8) 0.0412(4) Uani 1 1 d . . . . . H17 H 0.965370 0.796203 0.389307 0.049 Uiso 1 1 calc R U . . . C18 C 0.8568(4) 0.92824(16) 0.43311(9) 0.0500(5) Uani 1 1 d . . . . . H18 H 0.984189 0.938436 0.458815 0.060 Uiso 1 1 calc R U . . . C19 C 0.6830(4) 0.99859(16) 0.43681(9) 0.0503(5) Uani 1 1 d . . . . . H19 H 0.692421 1.057041 0.464469 0.060 Uiso 1 1 calc R U . . . C20 C 0.4971(4) 0.98246(19) 0.39989(12) 0.0593(6) Uani 1 1 d . . . . . H20 H 0.378173 1.030005 0.402230 0.071 Uiso 1 1 calc R U . . . C21 C 0.4830(3) 0.89600(17) 0.35884(10) 0.0523(5) Uani 1 1 d . . . . . H21 H 0.353742 0.885380 0.333989 0.063 Uiso 1 1 calc R U . . . 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 0.0432(8) 0.0447(8) 0.0871(11) 0.0224(7) -0.0240(7) -0.0110(6) O2 0.0622(10) 0.0554(10) 0.0941(13) 0.0318(9) -0.0163(9) -0.0007(8) N1 0.0356(8) 0.0375(8) 0.0423(8) 0.0032(6) 0.0065(6) -0.0020(6) C1 0.0421(10) 0.0391(10) 0.0566(11) 0.0051(8) -0.0056(8) 0.0004(8) C2 0.0325(8) 0.0368(9) 0.0359(8) -0.0012(7) 0.0063(7) -0.0024(6) C3 0.0346(9) 0.0341(9) 0.0410(9) -0.0028(7) -0.0055(7) 0.0005(7) C4 0.0319(9) 0.0348(9) 0.0542(11) 0.0022(8) -0.0077(7) -0.0055(7) C5 0.0336(8) 0.0368(9) 0.0323(8) -0.0040(6) -0.0010(6) 0.0011(7) C6 0.0354(10) 0.0708(14) 0.0622(12) 0.0249(11) -0.0143(9) -0.0091(9) C7 0.0364(10) 0.0738(15) 0.0750(15) 0.0301(12) -0.0108(9) -0.0160(10) C8 0.0467(11) 0.0564(13) 0.0750(15) 0.0188(11) 0.0095(10) -0.0129(9) C9 0.0328(8) 0.0376(9) 0.0317(8) -0.0003(6) -0.0050(6) 0.0015(7) C10 0.0408(9) 0.0370(9) 0.0269(8) 0.0014(6) -0.0037(6) 0.0022(7) C11 0.0736(14) 0.0418(11) 0.0525(12) -0.0134(9) 0.0187(10) -0.0098(10) C12 0.0971(19) 0.0476(12) 0.0541(12) -0.0115(10) 0.0295(12) 0.0037(12) C13 0.0671(13) 0.0583(13) 0.0357(10) 0.0058(8) 0.0171(9) 0.0106(10) C14 0.0718(14) 0.0464(11) 0.0549(12) 0.0090(9) 0.0247(11) -0.0007(10) C15 0.0708(13) 0.0350(10) 0.0509(11) 0.0037(8) 0.0207(10) 0.0056(9) C16 0.0369(8) 0.0342(9) 0.0300(8) 0.0015(6) 0.0051(6) -0.0024(6) C17 0.0496(10) 0.0352(9) 0.0383(9) 0.0031(7) -0.0068(8) -0.0001(8) C18 0.0692(13) 0.0430(11) 0.0370(9) 0.0008(8) -0.0092(9) -0.0075(9) C19 0.0720(14) 0.0419(10) 0.0380(9) -0.0077(8) 0.0182(9) -0.0099(9) C20 0.0521(12) 0.0561(13) 0.0707(14) -0.0196(11) 0.0203(11) 0.0050(10) C21 0.0388(10) 0.0547(12) 0.0634(13) -0.0155(10) 0.0036(9) 0.0024(9) 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 C3 O1 C1 108.08(14) . . ? C1 N1 C2 109.54(15) . . ? C1 N1 C8 123.79(17) . . ? C2 N1 C8 126.66(16) . . ? O2 C1 O1 123.09(19) . . ? O2 C1 N1 129.44(19) . . ? N1 C1 O1 107.47(16) . . ? C3 C2 N1 106.54(15) . . ? C3 C2 C7 120.00(17) . . ? C7 C2 N1 133.45(16) . . ? C2 C3 O1 108.38(15) . . ? C2 C3 C4 123.23(16) . . ? C4 C3 O1 128.38(16) . . ? C3 C4 H4 121.3 . . ? C3 C4 C5 117.32(15) . . ? C5 C4 H4 121.3 . . ? C4 C5 C9 121.60(15) . . ? C6 C5 C4 119.60(17) . . ? C6 C5 C9 118.80(16) . . ? C5 C6 H6 118.8 . . ? C5 C6 C7 122.49(18) . . ? C7 C6 H6 118.8 . . ? C2 C7 C6 117.36(18) . . ? C2 C7 H7 121.3 . . ? C6 C7 H7 121.3 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9 106.1 . . ? C5 C9 C10 113.60(14) . . ? C10 C9 H9 106.1 . . ? C16 C9 C5 110.97(13) . . ? C16 C9 H9 106.1 . . ? C16 C9 C10 113.29(14) . . ? C11 C10 C9 121.04(16) . . ? C11 C10 C15 117.26(17) . . ? C15 C10 C9 121.63(15) . . ? C10 C11 H11 119.4 . . ? C10 C11 C12 121.27(19) . . ? C12 C11 H11 119.4 . . ? C11 C12 H12 119.7 . . ? C13 C12 C11 120.7(2) . . ? C13 C12 H12 119.7 . . ? C12 C13 H13 120.5 . . ? C14 C13 C12 119.01(18) . . ? C14 C13 H13 120.5 . . ? C13 C14 H14 119.6 . . ? C13 C14 C15 120.7(2) . . ? C15 C14 H14 119.6 . . ? C10 C15 H15 119.5 . . ? C14 C15 C10 121.08(19) . . ? C14 C15 H15 119.5 . . ? C17 C16 C9 122.04(15) . . ? C21 C16 C9 119.81(16) . . ? C21 C16 C17 118.12(17) . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.71(19) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.7 . . ? C19 C18 C17 120.5(2) . . ? C19 C18 H18 119.7 . . ? C18 C19 H19 120.3 . . ? C20 C19 C18 119.41(19) . . ? C20 C19 H19 120.3 . . ? C19 C20 H20 119.8 . . ? C19 C20 C21 120.4(2) . . ? C21 C20 H20 119.8 . . ? C16 C21 C20 120.9(2) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? 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 C1 1.387(2) . ? O1 C3 1.381(2) . ? O2 C1 1.201(2) . ? N1 C1 1.353(2) . ? N1 C2 1.395(2) . ? N1 C8 1.451(2) . ? C2 C3 1.377(2) . ? C2 C7 1.379(3) . ? C3 C4 1.380(2) . ? C4 H4 0.9400 . ? C4 C5 1.396(2) . ? C5 C6 1.380(3) . ? C5 C9 1.532(2) . ? C6 H6 0.9400 . ? C6 C7 1.400(3) . ? C7 H7 0.9400 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9 0.9900 . ? C9 C10 1.533(2) . ? C9 C16 1.529(2) . ? C10 C11 1.376(3) . ? C10 C15 1.391(3) . ? C11 H11 0.9400 . ? C11 C12 1.387(3) . ? C12 H12 0.9400 . ? C12 C13 1.370(3) . ? C13 H13 0.9400 . ? C13 C14 1.362(3) . ? C14 H14 0.9400 . ? C14 C15 1.386(3) . ? C15 H15 0.9400 . ? C16 C17 1.388(3) . ? C16 C21 1.388(3) . ? C17 H17 0.9400 . ? C17 C18 1.385(3) . ? C18 H18 0.9400 . ? C18 C19 1.381(3) . ? C19 H19 0.9400 . ? C19 C20 1.367(3) . ? C20 H20 0.9400 . ? C20 C21 1.392(3) . ? C21 H21 0.9400 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C3 C4 C5 177.86(18) . . . . ? N1 C2 C3 O1 0.25(19) . . . . ? N1 C2 C3 C4 178.66(16) . . . . ? N1 C2 C7 C6 -178.25(19) . . . . ? C1 O1 C3 C2 0.2(2) . . . . ? C1 O1 C3 C4 -178.11(18) . . . . ? C1 N1 C2 C3 -0.62(19) . . . . ? C1 N1 C2 C7 177.9(2) . . . . ? C2 N1 C1 O1 0.7(2) . . . . ? C2 N1 C1 O2 -178.7(2) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C3 O1 C1 O2 178.9(2) . . . . ? C3 O1 C1 N1 -0.6(2) . . . . ? C3 C2 C7 C6 0.1(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C3 C4 C5 C9 179.57(15) . . . . ? C4 C5 C6 C7 -0.5(3) . . . . ? C4 C5 C9 C10 60.7(2) . . . . ? C4 C5 C9 C16 -68.3(2) . . . . ? C5 C6 C7 C2 0.2(4) . . . . ? C5 C9 C10 C11 30.8(2) . . . . ? C5 C9 C10 C15 -152.29(18) . . . . ? C5 C9 C16 C17 74.46(19) . . . . ? C5 C9 C16 C21 -103.56(18) . . . . ? C6 C5 C9 C10 -120.23(19) . . . . ? C6 C5 C9 C16 110.75(19) . . . . ? C7 C2 C3 O1 -178.50(19) . . . . ? C7 C2 C3 C4 -0.1(3) . . . . ? C8 N1 C1 O1 179.28(18) . . . . ? C8 N1 C1 O2 -0.1(4) . . . . ? C8 N1 C2 C3 -179.10(18) . . . . ? C8 N1 C2 C7 -0.6(3) . . . . ? C9 C5 C6 C7 -179.6(2) . . . . ? C9 C10 C11 C12 176.2(2) . . . . ? C9 C10 C15 C14 -176.76(19) . . . . ? C9 C16 C17 C18 -177.73(16) . . . . ? C9 C16 C21 C20 178.56(18) . . . . ? C10 C9 C16 C17 -54.7(2) . . . . ? C10 C9 C16 C21 127.26(17) . . . . ? C10 C11 C12 C13 1.2(4) . . . . ? C11 C10 C15 C14 0.3(3) . . . . ? C11 C12 C13 C14 -0.9(4) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? C13 C14 C15 C10 0.0(4) . . . . ? C15 C10 C11 C12 -0.9(3) . . . . ? C16 C9 C10 C11 158.62(17) . . . . ? C16 C9 C10 C15 -24.5(2) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C17 C16 C21 C20 0.5(3) . . . . ? C17 C18 C19 C20 0.9(3) . . . . ? C18 C19 C20 C21 -0.1(3) . . . . ? C19 C20 C21 C16 -0.6(3) . . . . ? C21 C16 C17 C18 0.3(3) . . . . ?