#------------------------------------------------------------------------------ #$Date: 2021-06-26 08:54:01 +0300 (Sat, 26 Jun 2021) $ #$Revision: 266717 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243857.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243857 loop_ _publ_author_name 'Al-Waleedy, Safiyyah A. H.' 'Mohamed, Shaaban K.' 'Mague, Joel T.' 'Akkurt, Mehmet' 'Abbady, Mohamed S.' 'Bakhite, Etify A.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of ethyl 2-({5-acetyl-3-cyano-6-methyl-4-[(E)-2-phenylethenyl]pyridin-2-yl}sulfanyl)acetate ; _journal_coeditor_code WM5610 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 730 _journal_page_last 733 _journal_paper_doi 10.1107/S2056989021005600 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C21 H20 N2 O3 S' _chemical_formula_moiety 'C21 H20 N2 O3 S' _chemical_formula_sum 'C21 H20 N2 O3 S' _chemical_formula_weight 380.45 _chemical_name_systematic 'Ethyl 2-({5-acetyl-3-cyano-6-methyl-4-[(E)-2-phenylethenyl]pyridin-2-yl}sulfanyl)acetate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90.0660(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.7365(4) _cell_length_b 9.7590(3) _cell_length_c 18.5600(7) _cell_measurement_reflns_used 9951 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 74.6235 _cell_measurement_theta_min 4.7559 _cell_volume 1944.67(12) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 14722 _diffrn_reflns_theta_full 70.000 _diffrn_reflns_theta_max 74.623 _diffrn_reflns_theta_min 4.756 _diffrn_source 'INCOATEC I\mS micro--focus source' _exptl_absorpt_coefficient_mu 1.672 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_description column _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.268 _exptl_crystal_size_mid 0.118 _exptl_crystal_size_min 0.052 _refine_diff_density_max 0.215 _refine_diff_density_min -0.285 _refine_ls_extinction_coef 0.0041(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL 2018/3 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 314 _refine_ls_number_reflns 3912 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.7692P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.0882 _reflns_number_gt 3520 _reflns_number_total 3912 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5610sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2243857 _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_min 0.663 _shelx_estimated_absorpt_t_max 0.918 _shelx_hkl_file ; 0 5 0 11.10 2.50 0 6 0 78.69 4.30 0 7 0 1.20 1.80 0 7 0 0.20 1.80 0 7 0 -1.50 1.90 0 8 0 44.70 4.10 0 8 0 48.50 4.40 0 8 0 42.90 3.90 0 -9 0 0.10 2.00 0 9 0 2.10 1.80 0 9 0 2.80 1.70 0 -10 0 64.69 4.60 0 10 0 75.29 5.10 0 11 0 0.60 1.20 0 11 0 -0.30 1.20 -1 11 0 30.70 2.60 -1 11 0 26.50 2.60 1 -11 0 30.70 3.30 -1 10 0 81.99 4.90 1 -10 0 73.99 4.60 -1 9 0 60.49 4.10 -1 9 0 51.39 5.40 -1 8 0 24.80 3.70 -1 8 0 34.30 3.70 -1 7 0 170.68 7.60 -1 7 0 167.08 7.30 -1 7 0 174.88 7.50 -1 6 0 172.38 7.70 -1 6 0 174.08 8.10 -1 6 0 155.28 7.50 -1 6 0 160.98 7.10 -1 2 0 6.40 0.70 1 -2 0 6.40 0.70 -1 1 0 19.90 1.00 1 -1 0 20.30 1.10 -1 0 0 0.40 0.20 1 0 0 0.20 0.30 -1 -1 0 21.30 1.10 1 1 0 22.10 1.10 -1 -2 0 8.90 0.70 1 2 0 7.00 0.70 1 4 0 2356.06 71.79 1 5 0 79.79 4.10 1 6 0 168.48 8.60 1 7 0 167.78 7.10 1 7 0 171.38 7.40 1 7 0 158.18 7.60 -1 -8 0 21.10 4.40 1 8 0 33.70 3.30 1 8 0 28.30 3.90 1 8 0 31.10 3.70 -1 -9 0 51.19 4.70 1 9 0 52.59 4.20 1 9 0 47.90 4.40 1 9 0 51.89 3.90 -1 -10 0 63.09 5.20 1 10 0 75.09 4.50 1 10 0 77.39 4.20 1 11 0 25.90 2.60 1 11 0 29.60 2.80 -2 12 0 0.80 1.80 -2 11 0 69.29 3.60 -2 11 0 67.79 3.60 2 -11 0 64.79 3.80 -2 10 0 14.20 2.90 -2 10 0 15.70 2.90 -2 9 0 288.37 10.90 -2 9 0 280.07 11.20 -2 8 0 66.99 4.50 -2 8 0 71.29 4.70 -2 7 0 558.94 19.10 -2 7 0 546.05 18.60 -2 7 0 535.05 18.70 -2 6 0 5.40 2.00 -2 6 0 2.10 2.10 -2 6 0 2.30 2.10 2 -4 0 187.58 6.40 -2 3 0 76.59 3.20 2 -3 0 79.59 3.30 -2 2 0 141.99 5.00 2 -2 0 132.89 5.00 -2 1 0 225.98 7.90 2 -1 0 240.28 7.90 -2 0 0 2683.03 79.49 2 0 0 2578.34 79.49 -2 -1 0 236.48 7.80 2 1 0 228.28 7.90 -2 -2 0 135.79 5.00 2 2 0 137.89 5.00 -2 -3 0 86.29 3.40 2 3 0 78.79 3.30 2 4 0 190.38 6.10 2 4 0 176.48 6.90 2 5 0 2629.74 80.29 2 6 0 3.60 1.40 2 6 0 5.30 2.20 -2 -7 0 507.45 18.70 2 7 0 530.75 18.60 2 7 0 574.14 18.70 2 7 0 558.84 18.40 -2 -8 0 63.59 5.60 2 8 0 71.19 5.00 2 8 0 72.59 4.40 2 8 0 72.79 4.50 -2 -9 0 262.77 11.00 2 9 0 275.67 10.70 2 9 0 284.27 10.40 2 9 0 285.87 10.70 2 10 0 15.50 2.60 2 10 0 10.80 1.90 2 10 0 21.20 4.00 2 11 0 61.39 3.30 -3 11 0 254.07 9.20 -3 11 0 251.67 8.90 3 -11 0 249.97 9.00 -3 10 0 77.99 4.30 -3 10 0 70.99 4.40 -3 9 0 61.49 4.30 -3 9 0 71.59 4.60 -3 8 0 8.20 1.90 -3 8 0 4.90 1.60 -3 8 0 4.20 1.80 -3 7 0 549.74 19.40 -3 7 0 561.44 19.00 -3 7 0 556.84 19.10 -3 6 0 208.78 8.20 -3 6 0 194.78 8.40 -3 6 0 187.78 8.30 -3 4 0 8.60 2.60 3 -4 0 4.50 1.30 -3 3 0 16.30 2.90 3 -3 0 13.00 1.90 -3 2 0 4220.58 127.49 3 -2 0 4213.38 127.69 3 -1 0 9999.00 300.17 -3 0 0 -0.20 0.70 3 1 0 9275.57 278.47 -3 -2 0 4118.79 125.59 3 2 0 4196.48 125.69 -3 -3 0 12.40 2.00 3 3 0 12.30 1.90 3 3 0 8.70 2.00 -3 -4 0 4.90 1.40 3 4 0 4.40 1.30 3 4 0 5.00 1.80 3 5 0 61.29 3.60 3 6 0 209.38 8.10 3 6 0 190.58 8.10 3 6 0 190.38 9.30 3 7 0 568.44 18.80 3 7 0 541.05 19.00 3 7 0 556.34 19.10 3 8 0 10.90 2.80 3 8 0 5.80 2.20 3 8 0 10.50 2.90 3 9 0 60.49 4.30 3 9 0 61.39 4.80 3 9 0 68.79 4.10 3 10 0 75.59 5.20 3 10 0 77.29 3.90 3 10 0 72.89 4.60 -4 11 0 1.70 1.10 -4 11 0 2.50 1.30 4 -11 0 2.40 1.90 -4 10 0 24.30 2.70 -4 10 0 20.10 2.60 -4 9 0 2.50 1.60 -4 9 0 -0.80 1.50 -4 8 0 40.60 3.70 -4 8 0 42.70 4.70 -4 8 0 44.70 3.90 -4 7 0 68.79 4.80 -4 7 0 67.29 4.50 -4 7 0 66.59 4.70 -4 6 0 193.78 7.80 -4 6 0 185.18 8.30 -4 6 0 176.08 7.90 -4 5 0 301.17 10.90 -4 5 0 298.77 11.00 -4 5 0 256.17 12.30 -4 5 0 298.17 11.30 -4 4 0 216.58 9.70 4 -4 0 223.18 9.10 -4 3 0 39.40 4.20 4 -3 0 39.20 3.50 -4 2 0 1587.24 49.00 4 -2 0 1546.05 49.10 -4 1 0 199.08 8.10 4 -1 0 211.18 8.00 -4 0 0 5190.28 152.28 4 0 0 4864.11 152.08 -4 -1 0 207.88 8.20 4 1 0 209.58 8.10 -4 -2 0 1500.85 47.40 4 2 0 1534.75 47.40 -4 -3 0 41.00 3.70 4 3 0 37.30 2.70 4 3 0 38.60 3.30 -4 -4 0 202.88 8.80 4 4 0 213.38 8.60 4 5 0 302.57 11.10 4 5 0 308.27 11.30 4 6 0 189.48 7.90 4 6 0 184.68 7.70 4 7 0 67.69 6.10 4 7 0 64.69 4.30 4 7 0 65.69 4.10 4 8 0 49.70 3.70 4 8 0 46.40 3.60 4 8 0 45.90 5.30 4 9 0 -2.90 1.40 4 10 0 18.40 4.40 -5 11 0 10.00 1.80 -5 11 0 11.50 2.30 5 -11 0 12.40 2.00 -5 10 0 110.69 5.40 -5 10 0 120.89 5.20 -5 9 0 63.09 4.90 -5 8 0 2.70 2.50 -5 8 0 0.60 1.70 -5 8 0 2.30 1.60 5 -8 0 0.40 2.60 -5 7 0 65.89 4.60 -5 7 0 53.29 4.20 -5 7 0 63.19 4.80 -5 6 0 8.60 2.00 -5 6 0 8.30 2.10 -5 5 0 219.38 8.90 -5 5 0 224.28 9.50 -5 5 0 229.18 8.90 -5 5 0 221.58 9.10 -5 4 0 3138.09 95.29 -5 4 0 3174.18 94.69 -5 4 0 2997.00 94.39 -5 4 0 3099.79 94.79 5 -4 0 3092.29 95.99 -5 3 0 829.22 29.50 5 -3 0 805.22 27.50 -5 2 0 76.19 6.40 5 -2 0 74.69 5.10 -5 1 0 0.00 2.20 5 -1 0 1.00 1.70 -5 0 0 2.10 1.80 5 0 0 -1.90 1.40 -5 -1 0 2.50 2.20 5 1 0 1.80 1.50 -5 -2 0 69.09 6.20 5 2 0 77.69 4.90 5 2 0 65.39 3.80 -5 -3 0 669.53 25.40 5 3 0 793.72 25.30 5 3 0 759.12 23.80 5 4 0 3043.70 94.19 5 4 0 3046.10 92.89 5 5 0 225.48 8.80 5 5 0 217.08 8.60 5 6 0 5.90 1.60 5 6 0 10.70 3.10 5 7 0 71.79 4.30 5 7 0 66.79 5.00 5 8 0 0.10 1.50 5 9 0 66.39 4.10 5 10 0 107.99 5.10 -6 10 0 127.39 6.30 -6 10 0 132.09 6.30 -6 9 0 73.19 4.40 -6 9 0 76.29 4.80 -6 8 0 28.50 3.20 -6 8 0 27.60 5.30 -6 8 0 27.50 3.50 -6 7 0 360.16 14.10 -6 7 0 374.16 14.10 -6 7 0 383.86 14.60 -6 6 0 24.30 6.30 -6 6 0 28.40 3.90 -6 6 0 28.20 3.30 -6 5 0 4.80 1.80 -6 5 0 6.00 1.90 -6 5 0 5.60 1.80 -6 5 0 4.90 2.10 -6 4 0 468.85 16.20 -6 4 0 456.25 15.90 -6 4 0 449.26 16.50 -6 4 0 461.45 15.80 -6 3 0 282.37 10.90 -6 3 0 295.47 10.80 -6 3 0 327.87 13.20 -6 3 0 285.97 11.00 6 -3 0 274.87 14.70 6 -2 0 714.93 25.40 6 -1 0 1212.58 40.00 6 0 0 1003.40 33.70 6 1 0 1098.09 35.70 6 1 0 1192.48 38.10 6 2 0 708.73 22.50 6 2 0 685.13 24.70 6 3 0 268.27 10.70 6 3 0 281.77 14.40 6 4 0 453.85 15.60 6 5 0 8.10 2.30 6 6 0 26.00 2.90 6 7 0 345.17 13.10 6 8 0 20.80 4.30 6 9 0 72.99 4.20 -6 -10 0 124.39 5.10 6 10 0 131.09 5.60 -7 10 0 2.40 1.10 -7 10 0 1.30 1.00 -7 9 0 6.60 2.60 -7 9 0 3.50 1.20 -7 8 0 22.60 3.00 -7 8 0 23.10 3.20 -7 8 0 22.20 4.00 -7 7 0 302.27 11.70 -7 7 0 281.07 11.50 -7 6 0 19.10 3.00 -7 6 0 9.50 2.10 -7 6 0 11.40 2.20 -7 5 0 15.80 3.10 -7 5 0 13.40 3.00 -7 5 0 18.40 3.50 -7 5 0 14.50 4.00 -7 4 0 204.58 9.10 -7 4 0 206.68 8.80 -7 4 0 200.78 8.40 -7 4 0 212.48 8.40 -7 3 0 52.69 4.10 -7 3 0 51.09 3.70 -7 3 0 57.79 4.20 -7 3 0 41.00 5.50 -7 2 0 9.70 3.20 -7 2 0 25.20 5.60 -7 2 0 10.90 2.20 -7 1 0 212.28 8.30 -7 1 0 206.38 8.20 -7 1 0 196.48 8.70 -7 0 0 -1.00 2.40 -7 0 0 0.40 1.60 -7 -1 0 202.28 8.10 -7 -2 0 10.70 1.90 7 2 0 8.50 2.50 -7 -3 0 50.19 3.90 7 3 0 50.69 3.60 -7 -4 0 201.78 8.30 7 4 0 211.38 8.40 7 5 0 14.80 2.80 7 6 0 14.30 3.10 7 7 0 253.27 10.70 -7 -8 0 19.50 2.60 7 8 0 22.20 2.60 -7 -9 0 1.50 1.40 7 9 0 4.60 1.50 -8 9 0 14.00 2.00 -8 9 0 11.00 2.10 -8 8 0 0.30 1.30 -8 8 0 0.60 1.40 -8 8 0 -0.10 1.10 8 -8 0 -2.40 1.50 -8 7 0 16.60 4.30 -8 7 0 15.80 3.10 -8 7 0 16.00 4.90 -8 6 0 176.68 7.70 -8 6 0 180.68 8.00 -8 6 0 177.98 8.10 -8 5 0 0.40 2.10 -8 5 0 1.00 1.50 -8 5 0 3.70 1.80 -8 5 0 -1.40 1.60 -8 4 0 411.46 14.90 -8 4 0 416.86 14.90 -8 4 0 420.36 15.40 -8 4 0 429.66 15.30 -8 3 0 69.39 4.60 -8 3 0 72.59 4.70 -8 3 0 68.79 4.30 -8 2 0 73.29 4.80 -8 2 0 72.59 4.30 -8 2 0 66.49 4.70 -8 2 0 56.59 6.60 -8 1 0 26.30 3.10 -8 1 0 19.60 4.30 -8 1 0 24.20 3.50 -8 0 0 406.26 13.80 -8 0 0 368.86 14.00 -8 0 0 400.46 13.90 -8 -1 0 35.50 4.80 -8 -1 0 25.20 3.20 -8 -2 0 62.19 4.10 -8 -3 0 65.69 4.20 8 3 0 72.29 4.60 -8 -4 0 421.16 15.10 8 4 0 443.56 15.40 -8 -5 0 0.90 1.60 8 5 0 0.30 1.70 -8 -6 0 180.58 7.10 8 6 0 151.98 7.20 -8 -7 0 10.60 2.50 8 7 0 17.20 2.70 -8 -8 0 0.80 1.30 8 8 0 0.10 1.60 -8 -9 0 11.90 3.20 8 9 0 12.70 2.70 -9 9 0 3.70 1.10 -9 8 0 4.00 1.10 -9 8 0 6.50 1.90 9 -8 0 3.60 1.50 -9 7 0 2.20 1.30 -9 7 0 0.50 1.50 -9 7 0 1.00 1.30 -9 6 0 80.59 4.60 -9 6 0 79.49 5.00 -9 6 0 83.29 4.80 -9 5 0 123.49 6.20 -9 5 0 122.99 6.00 -9 5 0 134.49 6.50 -9 4 0 225.58 9.90 -9 4 0 249.97 9.80 -9 4 0 244.48 9.50 -9 4 0 235.88 9.80 -9 3 0 2.40 1.80 -9 3 0 -1.90 2.60 -9 3 0 1.20 1.60 -9 3 0 1.40 1.60 -9 2 0 217.68 8.80 -9 2 0 204.58 8.60 -9 2 0 210.68 8.60 -9 1 0 260.87 10.40 -9 1 0 278.67 10.40 -9 1 0 267.87 10.30 -9 0 0 1.40 1.40 -9 0 0 2.10 2.00 -9 0 0 -3.70 2.80 -9 -1 0 263.17 9.90 -9 -1 0 247.98 10.10 -9 -2 0 214.58 8.60 -9 -3 0 -0.20 1.60 -9 -4 0 240.68 9.20 9 4 0 229.68 9.50 -9 -5 0 115.69 5.30 9 5 0 110.19 5.70 -9 -6 0 77.29 4.00 9 6 0 74.09 4.60 -9 -7 0 2.40 1.30 9 7 0 -0.10 1.80 -9 -8 0 1.90 1.50 9 8 0 4.50 1.90 -10 8 0 38.20 2.30 -10 7 0 104.39 4.90 -10 7 0 115.59 4.60 10 -7 0 113.69 4.70 -10 6 0 1.60 1.30 -10 6 0 4.80 1.80 -10 6 0 1.50 1.30 -10 5 0 170.18 6.90 -10 5 0 172.58 7.30 -10 5 0 166.48 7.30 -10 4 0 0.40 1.80 -10 4 0 0.80 2.80 -10 3 0 43.90 3.80 -10 3 0 44.50 3.60 -10 3 0 44.30 3.50 -10 2 0 28.60 3.80 -10 2 0 26.60 3.00 -10 2 0 27.80 3.10 -10 1 0 324.57 12.10 -10 1 0 342.27 12.00 -10 1 0 307.67 12.00 -10 0 0 315.07 11.80 -10 0 0 326.97 11.80 -10 -1 0 305.97 12.00 -10 -1 0 329.47 11.80 -10 -2 0 29.20 2.90 -10 -3 0 45.20 3.30 -10 -4 0 -0.40 1.60 -10 -5 0 151.68 6.20 -10 -6 0 3.60 1.20 -10 -7 0 104.09 4.20 -11 6 0 7.30 2.00 -11 6 0 2.60 1.00 -11 5 0 14.10 2.50 -11 5 0 9.20 2.60 -11 4 0 10.90 2.60 -11 4 0 4.00 1.70 -11 3 0 4.40 1.30 -11 3 0 7.00 1.90 -11 2 0 12.80 3.90 -11 2 0 16.00 4.30 -11 1 0 11.60 2.80 -11 0 0 -0.20 1.60 -11 -2 0 16.40 2.40 -11 -3 0 8.00 2.20 -11 -4 0 4.00 1.20 -11 -5 0 8.60 2.10 -11 -6 0 1.40 1.30 -12 5 0 27.00 2.00 12 -5 0 32.70 2.00 -12 4 0 127.89 5.40 -12 3 0 33.90 2.40 -12 2 0 156.08 6.40 -12 1 0 -0.60 1.20 -12 0 0 6.80 2.00 -12 -1 0 -1.80 1.10 -12 -2 0 151.08 5.90 -12 -3 0 30.90 2.40 -12 -4 0 127.19 4.90 -13 3 0 1.00 1.10 -13 2 0 1.10 1.00 -13 1 0 -1.00 1.10 -13 0 0 -0.80 1.10 -13 -1 0 -0.50 1.10 -13 -2 0 -0.40 1.20 -13 -2 -1 40.00 2.40 -13 -1 -1 28.50 2.10 -13 0 -1 9.90 1.70 -13 1 -1 28.90 2.10 -13 2 -1 44.00 2.50 -13 3 -1 34.50 2.20 -12 -5 -1 10.20 2.30 -12 -4 -1 -0.60 1.10 -12 -3 -1 17.70 2.10 -12 -2 -1 57.19 3.20 -12 -1 -1 1.70 1.00 -12 0 -1 0.90 1.10 -12 1 -1 2.50 1.10 -12 2 -1 55.09 3.20 -12 3 -1 16.80 1.90 -12 4 -1 5.70 1.70 12 -5 1 13.20 1.70 -12 5 -1 11.50 1.70 -11 -6 -1 111.49 4.30 -11 -5 -1 61.79 3.10 -11 -4 -1 4.00 1.20 -11 -3 -1 96.99 4.60 -11 -2 -1 93.29 4.50 -11 0 -1 159.08 7.60 -11 2 -1 104.89 5.30 -11 3 -1 94.59 5.10 -11 3 -1 91.49 5.30 -11 4 -1 3.90 1.20 -11 4 -1 6.00 1.80 -11 5 -1 66.89 3.60 -11 5 -1 67.49 3.90 11 -6 1 117.69 4.80 -11 6 -1 121.99 4.80 -10 -7 -1 70.19 3.30 -10 -6 -1 170.48 6.50 -10 -5 -1 8.60 2.20 -10 -4 -1 112.59 6.10 -10 -3 -1 53.79 3.60 -10 -2 -1 62.19 3.90 -10 -1 -1 100.39 5.20 -10 0 -1 -0.50 1.50 -10 0 -1 -1.60 2.10 -10 1 -1 106.39 5.50 -10 1 -1 111.89 5.60 -10 2 -1 66.99 4.30 -10 2 -1 68.09 4.20 -10 2 -1 72.59 5.00 -10 3 -1 51.99 3.80 -10 3 -1 59.29 6.00 -10 3 -1 50.39 4.20 -10 3 -1 50.49 3.70 -10 4 -1 131.09 6.50 -10 4 -1 113.59 7.20 -10 4 -1 140.59 6.60 -10 5 -1 9.10 2.40 -10 5 -1 5.20 1.60 -10 5 -1 4.70 1.90 -10 6 -1 175.98 7.10 -10 6 -1 182.78 7.20 -10 6 -1 172.78 6.80 10 -7 1 84.69 3.80 -10 7 -1 79.49 3.90 -10 7 -1 79.19 3.60 -10 7 -1 78.59 4.00 10 -8 1 37.80 3.00 -10 8 -1 36.50 2.30 9 8 1 27.80 3.10 -9 -8 -1 27.40 2.30 9 7 1 14.20 3.00 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4 69.29 4.40 4 7 4 71.39 4.30 4 7 4 74.49 4.70 4 6 4 255.77 9.60 4 6 4 262.57 9.90 4 6 4 236.88 9.70 4 5 4 16.30 2.20 4 5 4 14.70 2.80 4 5 4 10.40 2.20 4 4 4 197.88 9.20 4 3 4 459.75 14.40 4 3 4 431.16 15.30 -4 -3 -4 391.26 15.60 4 2 4 422.06 13.60 4 2 4 437.16 14.70 -4 -2 -4 367.36 14.90 4 1 4 405.46 14.60 -4 -1 -4 422.46 15.20 4 0 4 2266.37 70.69 -4 0 -4 2311.47 71.09 4 -1 4 408.46 14.70 -4 1 -4 419.66 15.20 4 -2 4 418.76 14.60 -4 2 -4 398.56 15.10 4 -3 4 441.46 15.70 -4 3 -4 433.26 16.30 4 -4 4 188.98 8.90 -4 5 -4 18.70 4.70 -4 5 -4 15.10 3.60 -4 6 -4 247.28 9.70 -4 6 -4 249.97 10.10 -4 6 -4 246.28 10.20 4 -7 4 67.19 5.10 -4 7 -4 68.29 4.30 -4 7 -4 65.39 5.20 -4 7 -4 71.29 5.00 4 -8 4 103.09 5.90 -4 8 -4 94.09 6.20 -4 8 -4 94.69 5.50 -4 9 -4 298.27 11.50 -4 9 -4 319.67 12.20 4 -10 4 114.29 5.20 -4 10 -4 115.69 5.40 -4 10 -4 113.69 5.70 4 -11 4 98.59 4.60 -4 11 -4 105.89 4.40 3 11 4 20.70 2.50 3 10 4 83.49 4.80 3 10 4 88.59 4.20 3 10 4 85.99 4.30 3 9 4 17.00 2.90 3 9 4 15.40 3.00 3 9 4 14.20 3.10 3 8 4 24.10 3.00 3 8 4 25.60 3.70 3 8 4 25.60 3.30 3 7 4 2.00 1.60 3 7 4 -0.30 1.70 3 7 4 1.60 1.40 3 6 4 184.48 7.60 3 6 4 176.78 7.80 3 6 4 189.38 7.60 3 5 4 3.20 1.20 3 5 4 1.80 2.10 3 5 4 3.80 1.90 3 4 4 30.50 2.20 3 4 4 27.20 3.30 -3 -4 -4 20.90 4.40 3 3 4 82.99 3.90 3 3 4 88.59 4.40 -3 -3 -4 87.49 5.20 3 2 4 64.39 3.70 -3 -2 -4 63.49 4.10 3 1 4 64.29 3.50 -3 -1 -4 70.89 3.90 3 0 4 1.50 0.90 -3 0 -4 -0.20 1.00 3 -1 4 58.79 3.40 -3 1 -4 62.89 3.70 3 -2 4 60.79 3.60 -3 2 -4 68.29 4.10 3 -3 4 90.29 4.50 -3 3 -4 89.79 5.40 3 -4 4 33.10 3.50 -3 4 -4 29.00 4.60 -3 5 -4 2.10 2.00 -3 5 -4 -4.40 2.40 3 -6 4 173.68 7.90 -3 6 -4 168.38 8.20 -3 6 -4 186.18 8.10 -3 6 -4 187.28 7.70 -3 7 -4 0.50 2.20 -3 7 -4 2.60 1.80 3 -8 4 21.40 5.30 -3 8 -4 21.40 4.10 -3 8 -4 21.80 3.80 -3 9 -4 19.80 3.30 -3 9 -4 20.50 4.00 3 -10 4 86.19 4.40 -3 10 -4 77.99 4.50 -3 10 -4 84.09 5.20 3 -11 4 21.40 2.10 -3 11 -4 21.40 2.80 2 11 4 1.10 1.10 2 11 4 2.70 1.00 2 10 4 301.27 10.60 2 10 4 254.67 12.70 2 10 4 310.07 10.50 2 9 4 31.70 3.60 2 9 4 31.70 3.30 2 9 4 29.70 3.10 2 8 4 60.09 4.20 2 8 4 60.99 4.00 2 8 4 60.69 4.20 2 7 4 4.00 1.60 2 7 4 3.50 1.60 2 7 4 2.80 1.60 2 6 4 328.77 12.20 2 6 4 319.07 13.50 2 6 4 353.86 12.10 2 5 4 154.18 6.30 2 4 4 235.48 8.10 2 4 4 219.18 8.20 -2 -4 -4 230.38 8.50 2 3 4 1046.00 32.50 2 3 4 1040.10 32.40 -2 -3 -4 1039.20 32.60 2 2 4 954.60 30.40 -2 -2 -4 988.00 30.50 2 1 4 2.80 0.80 -2 -1 -4 3.30 1.00 2 0 4 9.90 1.40 -2 0 -4 10.30 1.60 2 -1 4 2.60 0.80 -2 1 -4 5.10 1.60 2 -2 4 905.71 26.70 -2 2 -4 778.02 27.30 2 -3 4 1079.99 33.80 -2 3 -4 1083.79 34.00 2 -4 4 238.28 8.60 2 -6 4 304.87 12.40 -2 6 -4 317.87 12.40 -2 6 -4 324.07 12.80 -2 6 -4 351.16 11.90 2 -7 4 -0.90 3.10 -2 7 -4 0.40 2.40 -2 7 -4 1.10 1.90 -2 8 -4 63.39 5.00 -2 8 -4 59.79 4.80 -2 9 -4 36.90 4.30 -2 9 -4 31.70 3.80 2 -10 4 317.37 11.60 -2 10 -4 313.17 11.60 2 -11 4 1.00 1.20 1 11 4 28.10 2.20 1 11 4 23.80 2.20 1 10 4 27.80 2.90 1 10 4 26.80 2.70 1 9 4 268.57 10.80 1 9 4 293.67 11.10 1 9 4 298.37 10.80 1 8 4 1.90 1.70 1 8 4 0.70 2.00 1 8 4 0.10 1.60 1 7 4 127.19 5.90 1 7 4 131.49 6.30 1 7 4 130.89 6.20 1 6 4 2.00 1.80 1 6 4 1.10 1.30 1 6 4 0.30 1.80 1 5 4 5.80 1.20 1 4 4 352.16 12.10 -1 -4 -4 370.46 11.90 1 3 4 334.87 10.90 -1 -3 -4 327.07 11.00 1 2 4 2845.92 88.59 -1 -2 -4 3016.30 88.79 1 1 4 812.32 25.30 1 0 4 0.30 0.40 -1 0 -4 -0.50 0.50 1 -1 4 870.31 27.40 -1 1 -4 894.01 27.50 1 -2 4 2784.02 87.79 -1 2 -4 3019.80 87.99 1 -3 4 326.97 10.90 -1 3 -4 327.57 11.00 1 -4 4 371.26 12.20 -1 4 -4 369.16 12.30 -1 5 -4 4.00 2.00 -1 6 -4 3.40 2.40 -1 6 -4 -2.60 2.20 -1 7 -4 116.99 6.50 -1 7 -4 125.29 7.00 -1 8 -4 1.50 1.90 -1 8 -4 -0.30 2.40 1 -9 4 280.07 10.80 -1 9 -4 269.27 10.70 -1 9 -4 286.27 10.90 1 -10 4 29.30 3.10 -1 10 -4 29.60 3.40 1 -11 4 33.50 2.50 -1 11 -4 32.00 3.70 0 12 4 12.90 1.80 0 12 4 16.90 2.50 0 11 4 29.20 2.30 0 11 4 24.50 2.20 0 10 4 32.60 3.00 0 10 4 29.00 3.00 0 9 4 52.89 3.80 0 9 4 44.60 3.70 0 8 4 7.20 1.80 0 8 4 5.70 1.80 0 8 4 5.90 2.20 0 7 4 265.37 9.90 0 7 4 257.07 10.00 0 7 4 265.07 10.30 0 6 4 17.30 3.40 0 6 4 24.20 2.60 0 6 4 17.90 3.50 0 5 4 1638.74 50.49 0 4 4 2.40 1.30 0 -4 -4 2.00 0.80 0 -4 -4 1.30 0.90 0 -3 -4 1185.18 36.40 0 2 4 203.88 7.20 0 -2 -4 213.38 7.30 0 1 4 99.19 4.00 0 -1 -4 110.19 4.10 0 0 4 459.25 15.20 0 0 -4 492.15 15.20 0 -1 4 101.69 4.10 0 1 -4 111.49 4.20 0 -2 4 215.38 7.60 0 2 -4 226.88 7.70 0 3 -4 1155.18 35.60 0 4 -4 2.20 1.50 0 4 -4 1.60 0.90 0 4 -4 1.20 1.00 0 5 -4 1563.14 48.40 0 7 -4 239.38 9.60 0 7 -4 256.47 10.10 0 7 -4 236.38 10.30 0 -8 4 5.30 1.70 0 8 -4 0.90 2.20 0 8 -4 9.20 2.70 0 8 -4 9.00 2.80 0 -9 4 40.70 3.70 0 9 -4 36.70 4.90 0 9 -4 49.40 4.50 0 -10 4 29.50 3.00 0 10 -4 28.40 3.60 0 -11 4 26.50 2.40 -1 11 4 3.40 1.00 -1 11 4 1.50 1.50 -1 10 4 176.88 7.40 -1 10 4 177.18 7.80 -1 9 4 -0.80 1.60 -1 9 4 2.90 1.60 -1 8 4 62.69 4.40 -1 8 4 56.59 4.10 -1 7 4 6.00 2.80 -1 7 4 5.90 1.80 -1 7 4 2.40 1.80 -1 7 4 2.50 2.70 -1 6 4 24.70 3.60 -1 6 4 24.00 3.60 -1 6 4 27.50 3.30 -1 5 4 24.80 2.90 1 -4 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38.20 2.60 -11 0 8 1.40 1.20 -11 0 8 0.70 1.20 -11 -1 8 39.60 2.80 -11 -1 8 38.50 2.80 -11 -2 8 55.89 3.10 -11 -3 8 13.70 2.70 -12 3 8 1.80 1.00 -12 3 8 0.80 0.90 -12 2 8 41.50 2.20 -12 1 8 0.60 1.10 -12 0 8 297.57 9.90 -12 0 8 301.97 10.00 -12 -1 8 -1.70 1.40 -12 -2 -9 19.10 2.00 -12 -1 -9 1.70 1.10 -12 0 -9 1.50 1.20 -12 1 -9 11.60 2.60 -11 -5 -9 -0.40 0.90 -11 -4 -9 41.90 2.30 -11 -3 -9 9.40 1.70 -11 -2 -9 192.48 8.60 -11 -2 -9 208.48 7.50 -11 -1 -9 0.90 1.50 -11 -1 -9 3.10 1.20 -11 0 -9 134.49 5.70 -11 0 -9 134.79 5.50 -11 1 -9 3.30 1.50 -11 1 -9 5.00 1.40 -11 2 -9 228.08 8.20 -11 2 -9 207.88 7.90 11 -3 9 10.00 2.60 -11 3 -9 16.80 3.00 -11 3 -9 12.20 2.30 11 -4 9 42.90 2.50 -11 4 -9 43.00 2.70 11 -5 9 2.50 1.20 -11 5 -9 -1.00 1.10 -10 -6 -9 90.69 3.70 -10 -5 -9 53.99 2.80 -10 -4 -9 6.70 1.60 -10 -4 -9 10.70 2.10 -10 -3 -9 33.60 2.60 -10 -3 -9 34.10 3.00 -10 -2 -9 11.30 2.20 -10 -2 -9 16.80 2.80 -10 -1 -9 14.70 2.40 -10 -1 -9 17.00 2.70 -10 0 -9 0.40 1.40 -10 0 -9 1.90 1.40 -10 1 -9 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1.30 1.40 8 3 9 20.30 4.00 -8 -3 -9 25.80 2.90 -8 -2 -9 17.90 2.90 -8 -1 -9 158.08 6.90 -8 0 -9 12.60 3.10 8 -1 9 150.18 7.00 -8 1 -9 159.68 7.00 -8 1 -9 147.79 7.10 8 -2 9 15.10 3.40 -8 2 -9 18.60 3.70 -8 2 -9 17.00 3.20 8 -3 9 18.80 3.20 -8 3 -9 26.00 3.40 -8 3 -9 20.00 4.30 8 -4 9 2.70 1.70 -8 4 -9 1.80 1.70 -8 4 -9 3.30 2.60 8 -5 9 214.68 9.60 -8 5 -9 236.78 10.60 8 -6 9 4.30 1.30 -8 6 -9 1.80 1.40 -8 7 -9 8.30 2.10 8 -8 9 0.80 1.10 -8 8 -9 0.40 1.10 -7 -9 -9 2.10 0.90 7 8 9 110.09 5.00 -7 -8 -9 114.29 4.70 7 7 9 8.50 2.20 7 7 9 7.30 2.40 -7 -7 -9 11.80 2.10 7 6 9 55.09 3.80 7 6 9 62.79 4.50 7 5 9 -0.40 1.50 7 5 9 0.80 1.60 7 4 9 273.87 10.60 7 4 9 277.97 10.60 -7 -4 -9 268.57 10.30 7 3 9 49.30 4.00 -7 -3 -9 46.90 3.80 7 2 9 534.95 17.40 -7 -2 -9 478.15 17.20 -7 -1 -9 5.00 1.90 7 0 9 4.50 4.10 -7 0 -9 1.70 1.90 7 -1 9 -2.70 2.30 -7 1 -9 1.30 1.60 -7 1 -9 1.00 2.00 7 -2 9 488.15 17.00 -7 2 -9 478.25 17.00 -7 2 -9 496.55 17.40 7 -3 9 44.60 3.90 -7 3 -9 43.60 4.00 -7 3 -9 46.70 5.10 7 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13.10 2.40 5 9 9 8.20 2.00 5 8 9 131.49 7.00 5 8 9 124.29 5.60 5 7 9 118.69 5.70 5 7 9 110.49 5.70 5 6 9 2.80 1.60 5 6 9 6.30 1.70 5 5 9 16.60 3.20 5 5 9 24.70 2.80 5 4 9 61.49 4.20 5 4 9 56.99 3.80 5 3 9 7.40 2.40 5 3 9 4.10 1.70 5 2 9 42.30 3.00 5 2 9 32.90 3.70 5 1 9 2385.66 69.89 5 1 9 2250.77 69.49 -5 -1 -9 2151.28 69.39 5 0 9 14.20 3.30 5 0 9 35.10 7.30 5 -1 9 2001.30 66.39 5 -1 9 2229.08 65.39 5 -2 9 29.10 4.00 -5 2 -9 38.80 4.00 5 -3 9 0.00 1.90 -5 3 -9 0.40 1.90 5 -4 9 56.99 4.00 5 -5 9 23.90 3.40 -5 5 -9 27.40 4.20 5 -6 9 4.50 1.80 -5 6 -9 2.10 2.00 5 -7 9 129.69 6.30 -5 7 -9 128.49 6.80 5 -8 9 136.19 6.00 5 -8 9 128.29 5.90 -5 8 -9 133.39 6.40 5 -9 9 11.40 2.20 5 -9 9 9.20 2.80 -5 9 -9 9.40 2.50 5 -10 9 8.00 1.70 4 10 9 112.29 5.80 4 9 9 23.50 2.40 4 9 9 26.30 2.90 4 8 9 141.59 6.50 4 8 9 140.49 6.40 4 8 9 133.79 6.30 4 7 9 65.79 4.60 4 7 9 65.49 4.00 4 7 9 70.29 4.30 4 6 9 19.60 4.30 4 6 9 18.60 3.40 4 6 9 13.30 2.80 4 5 9 105.19 5.20 4 5 9 95.99 5.10 4 5 9 95.59 5.00 4 4 9 128.89 6.10 4 4 9 137.59 6.30 4 4 9 135.09 6.10 4 3 9 8.00 2.00 4 3 9 4.20 1.30 4 2 9 278.77 10.10 4 2 9 274.57 10.30 4 1 9 17.50 2.30 4 1 9 13.10 3.40 4 0 9 0.50 1.40 4 -1 9 20.80 3.20 4 -2 9 239.98 9.80 4 -2 9 264.87 9.90 -4 2 -9 264.97 10.30 4 -3 9 13.10 3.00 -4 3 -9 5.50 2.20 4 -4 9 137.39 6.30 -4 4 -9 139.19 7.20 4 -5 9 98.19 5.40 -4 5 -9 98.49 6.70 4 -6 9 14.00 3.30 -4 6 -9 18.50 4.20 4 -7 9 71.69 4.60 -4 7 -9 73.79 5.30 4 -8 9 112.69 7.50 4 -9 9 20.10 3.30 4 -9 9 21.50 2.40 -4 9 -9 29.40 3.10 4 -10 9 89.19 3.80 -4 10 -9 86.29 4.90 3 10 9 96.49 4.20 3 9 9 92.29 4.60 3 9 9 104.59 5.00 3 9 9 96.49 4.40 3 8 9 100.89 4.90 3 8 9 99.19 5.30 3 8 9 103.19 5.20 3 7 9 45.90 3.60 3 7 9 41.90 3.40 3 7 9 43.00 3.40 3 6 9 2223.78 69.49 3 6 9 2344.27 70.09 3 6 9 2200.38 69.79 3 5 9 379.36 13.70 3 5 9 406.56 14.20 3 5 9 404.26 14.20 3 4 9 106.49 5.50 3 4 9 103.89 5.50 3 4 9 103.29 4.90 3 3 9 13.00 2.10 3 3 9 11.60 4.00 3 3 9 13.30 2.20 3 2 9 558.14 21.20 3 2 9 621.04 21.00 3 1 9 410.16 13.70 3 1 9 396.46 15.50 3 0 9 17.60 4.70 3 0 9 24.40 2.50 3 -1 9 379.26 15.20 3 -1 9 402.96 13.40 3 -2 9 530.45 19.50 3 -2 9 524.35 17.50 3 -3 9 5.00 4.20 3 -3 9 10.80 3.80 -3 3 -9 14.50 4.80 3 -4 9 98.59 5.30 -3 4 -9 106.59 6.40 3 -5 9 394.26 14.10 -3 5 -9 390.26 14.80 3 -6 9 2275.97 70.99 -3 6 -9 2306.67 71.49 3 -7 9 44.40 3.80 3 -7 9 47.70 3.80 -3 7 -9 39.60 4.60 3 -8 9 104.79 5.50 3 -8 9 103.89 5.40 -3 8 -9 107.89 6.10 3 -9 9 101.39 5.40 3 -9 9 100.59 5.00 -3 9 -9 99.19 5.30 3 -10 9 101.19 5.20 2 11 9 12.40 1.60 2 10 9 3.60 1.00 2 10 9 7.10 1.70 2 9 9 26.20 3.30 2 9 9 26.90 2.50 2 9 9 26.10 2.60 2 8 9 41.60 3.10 2 8 9 34.70 3.10 2 8 9 33.70 3.30 2 7 9 11.20 2.80 2 7 9 13.40 2.80 2 6 9 947.91 29.80 2 6 9 916.51 29.70 2 6 9 877.61 29.30 2 5 9 44.10 3.30 2 5 9 54.49 3.90 2 5 9 46.90 3.80 2 4 9 103.89 6.00 2 4 9 107.89 5.00 2 4 9 111.99 5.60 2 3 9 24.10 2.30 2 3 9 22.20 5.80 2 2 9 72.89 3.70 2 2 9 80.39 5.70 2 1 9 238.98 10.20 2 1 9 247.48 8.80 2 0 9 1.40 1.20 2 0 9 0.70 1.70 2 -1 9 243.98 10.20 2 -1 9 240.08 8.80 2 -2 9 75.49 4.10 2 -2 9 79.49 5.60 2 -3 9 19.80 5.80 2 -3 9 24.00 3.20 2 -3 9 25.10 4.10 2 -4 9 99.49 5.20 2 -4 9 109.89 11.00 -2 4 -9 98.49 7.60 2 -5 9 43.80 3.70 -2 5 -9 32.70 5.10 2 -6 9 885.51 28.40 2 -6 9 848.12 28.40 -2 6 -9 880.71 29.00 2 -7 9 6.90 2.00 2 -7 9 13.70 3.00 -2 7 -9 6.90 2.50 2 -8 9 42.70 3.60 2 -8 9 41.20 4.00 -2 8 -9 45.40 4.80 2 -9 9 29.40 2.80 -2 9 -9 33.00 5.00 2 -10 9 3.70 1.00 2 -11 9 15.20 1.60 1 11 9 55.49 2.70 1 10 9 64.09 3.20 1 10 9 65.89 3.40 1 9 9 5.50 2.30 1 9 9 5.90 1.40 1 9 9 7.30 2.20 1 8 9 63.99 3.90 1 8 9 59.89 3.90 1 8 9 54.39 4.00 1 7 9 234.78 9.30 1 7 9 242.88 9.60 1 7 9 243.98 9.50 1 6 9 149.39 6.70 1 6 9 140.99 6.40 1 5 9 106.89 4.90 1 5 9 97.79 5.20 1 5 9 91.79 5.40 1 4 9 108.69 5.70 1 4 9 107.69 5.00 1 3 9 361.26 12.50 1 2 9 99.09 4.50 1 2 9 99.29 5.90 1 1 9 1741.63 52.29 1 1 9 1590.44 50.89 -1 -1 -9 1636.24 53.39 1 0 9 107.19 5.90 1 0 9 113.69 4.80 -1 0 -9 111.09 7.30 1 -1 9 1587.54 50.39 1 -1 9 1685.03 51.69 1 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106.39 5.10 -8 -4 9 98.59 6.40 8 4 -9 101.39 5.60 8 5 -9 664.03 22.40 -8 -6 9 70.09 3.70 8 6 -9 64.29 4.20 -8 -7 9 116.49 4.80 8 7 -9 119.79 5.40 -9 7 9 0.00 1.70 -9 7 9 0.80 1.00 -9 6 9 9.40 2.10 -9 6 9 13.80 3.50 -9 6 9 9.40 2.10 -9 5 9 1.00 1.80 -9 5 9 1.20 1.10 -9 5 9 -0.50 1.10 -9 4 9 105.49 4.90 -9 4 9 102.49 5.10 -9 4 9 105.19 5.60 -9 3 9 26.80 3.00 -9 3 9 30.90 3.30 -9 3 9 32.20 5.10 -9 2 9 7.90 2.50 -9 2 9 5.10 1.40 -9 1 9 276.07 10.50 -9 1 9 286.67 11.10 -9 0 9 260.67 10.10 -9 0 9 270.67 10.10 -9 -1 9 274.87 10.20 -9 -1 9 264.67 10.10 -9 -2 9 7.60 2.40 -9 -3 9 31.70 3.80 -9 -3 9 33.60 3.20 -9 -4 9 108.29 5.00 9 4 -9 111.79 6.30 -9 -5 9 -0.20 1.30 9 5 -9 -1.30 2.30 -9 -6 9 6.00 1.40 9 6 -9 3.10 2.30 -10 6 9 66.69 3.00 -10 5 9 38.70 2.50 -10 5 9 43.30 2.60 -10 4 9 2.20 1.00 -10 4 9 2.60 1.00 -10 3 9 7.40 2.00 -10 3 9 8.70 1.90 -10 2 9 13.10 2.20 -10 2 9 8.50 2.20 -10 1 9 175.78 7.20 -10 1 9 173.88 7.10 -10 0 9 0.50 1.40 -10 0 9 0.10 1.30 -10 -1 9 173.28 6.90 -10 -1 9 176.08 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8 10 39.10 3.40 3 8 10 40.20 3.30 3 7 10 223.58 8.50 3 7 10 209.88 8.70 3 7 10 213.08 8.80 3 6 10 25.40 3.10 3 6 10 22.50 3.20 3 6 10 28.70 3.10 3 5 10 100.29 5.20 3 5 10 106.09 5.50 3 4 10 -0.40 1.50 3 4 10 -1.20 2.10 3 4 10 -0.90 1.30 3 3 10 30.80 2.60 3 3 10 30.30 3.60 3 3 10 33.70 5.50 3 2 10 737.43 23.50 3 2 10 706.13 23.60 3 1 10 42.70 4.70 3 1 10 41.80 2.90 3 0 10 -0.60 1.30 3 -1 10 45.70 3.20 3 -2 10 687.23 22.80 3 -2 10 733.03 23.10 -3 2 -10 676.23 23.40 3 -3 10 26.60 4.20 3 -3 10 30.30 3.60 -3 3 -10 28.10 4.70 3 -4 10 1.30 1.70 3 -4 10 4.60 2.50 -3 4 -10 1.10 2.40 3 -5 10 99.29 5.50 3 -5 10 107.29 8.20 -3 5 -10 104.89 6.50 3 -6 10 20.20 3.30 3 -6 10 27.60 3.50 -3 6 -10 34.10 4.80 3 -7 10 217.88 9.00 3 -7 10 231.68 9.20 -3 7 -10 220.58 9.50 3 -8 10 42.10 3.80 3 -8 10 42.70 5.10 -3 8 -10 47.50 4.50 3 -9 10 127.59 5.60 3 -9 10 120.29 6.20 -3 9 -10 117.49 6.20 3 -10 10 6.70 1.60 2 10 10 69.59 3.30 2 10 10 72.69 3.80 2 9 10 8.80 3.20 2 9 10 13.60 2.10 2 9 10 9.40 2.10 2 8 10 18.00 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650.43 21.90 -5 -5 10 197.58 8.10 -5 -5 10 195.18 8.20 5 5 -10 200.58 9.20 -5 -6 10 280.57 10.30 5 6 -10 260.77 10.80 -5 -7 10 219.68 8.40 5 7 -10 199.98 8.80 -5 -8 10 47.70 3.00 5 8 -10 46.30 3.60 -5 -9 10 31.00 2.20 5 9 -10 34.80 3.20 -6 9 10 130.59 5.00 -6 8 10 248.98 8.90 -6 8 10 248.88 8.90 -6 7 10 13.70 3.00 -6 7 10 15.90 2.90 -6 6 10 2.50 2.30 -6 6 10 11.00 3.10 -6 6 10 2.70 2.00 -6 5 10 541.45 18.30 -6 5 10 542.85 18.60 -6 5 10 538.85 18.60 -6 4 10 6.10 1.90 -6 4 10 5.80 2.80 -6 4 10 6.10 1.90 -6 3 10 489.25 16.90 -6 3 10 483.85 16.70 -6 2 10 293.17 10.80 -6 2 10 283.57 10.80 -6 1 10 392.36 15.70 -6 0 10 175.08 8.50 -6 0 10 153.58 7.90 6 0 -10 184.68 7.70 -6 -1 10 428.56 16.60 6 1 -10 420.76 15.10 -6 -2 10 266.87 10.20 -6 -2 10 273.67 10.30 6 2 -10 280.37 10.80 -6 -3 10 505.85 17.00 -6 -3 10 477.15 16.80 6 3 -10 504.15 17.60 -6 -4 10 8.80 2.10 -6 -4 10 5.20 1.60 6 4 -10 9.60 3.30 -6 -5 10 478.65 16.70 -6 -5 10 482.35 16.30 6 5 -10 467.95 17.20 -6 -6 10 5.00 1.50 6 6 -10 1.40 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-6 -4 19 6.40 1.80 -7 2 19 -1.90 1.10 -7 1 19 34.60 2.20 -7 0 19 17.40 1.60 -7 -1 19 32.60 2.00 -7 -1 19 29.80 2.70 -7 -2 19 7.50 2.10 -6 -1 -20 83.89 5.10 -5 -3 -20 80.69 3.90 -5 -2 -20 45.30 3.20 -5 -1 -20 8.20 1.90 5 -3 20 80.69 3.40 4 3 20 11.90 3.00 -4 -3 -20 12.30 3.10 4 2 20 350.26 12.20 -4 -2 -20 340.27 13.00 4 1 20 11.20 3.40 4 0 20 144.79 6.70 4 -3 20 11.40 2.00 4 -4 20 55.59 2.60 3 4 20 -1.30 1.60 3 3 20 0.20 1.50 3 2 20 122.89 5.60 3 1 20 19.90 3.00 3 0 20 -2.10 1.90 3 -1 20 19.60 2.60 3 -2 20 119.09 4.90 3 -3 20 0.20 1.00 3 -4 20 1.10 0.90 2 4 20 9.60 2.50 2 3 20 8.20 2.60 2 2 20 154.48 6.80 2 1 20 29.80 3.00 2 0 20 4.80 1.80 2 0 20 3.40 1.70 2 -1 20 23.70 2.50 2 -2 20 164.38 6.30 2 -3 20 9.90 1.80 -2 3 -20 -0.70 2.90 2 -4 20 8.20 1.70 2 -5 20 142.69 6.00 1 4 20 0.30 1.60 1 3 20 8.90 2.50 1 2 20 3.80 1.50 1 1 20 86.59 4.70 1 0 20 -2.60 1.60 1 0 20 -0.50 1.60 1 -1 20 87.39 4.20 1 -2 20 2.80 1.10 1 -3 20 10.40 1.80 -1 3 -20 13.70 3.40 1 -4 20 1.40 0.90 1 -5 20 3.00 0.80 1 -6 20 22.80 1.70 0 4 20 151.48 6.40 0 3 20 1.50 1.60 0 2 20 378.66 13.60 0 1 20 17.40 2.80 0 1 20 15.30 3.40 0 0 20 53.39 3.30 0 0 20 50.79 3.70 0 -1 20 23.20 2.40 0 -2 20 383.66 13.00 0 -3 20 -0.10 0.90 0 3 -20 -0.10 1.80 0 -4 20 138.69 5.70 0 4 -20 153.98 6.60 0 -5 20 22.60 1.70 0 -6 20 1.90 0.90 -1 4 20 26.80 3.30 -1 3 20 41.00 3.40 -1 1 20 -0.20 1.60 -1 1 20 -1.50 1.60 -1 0 20 1.20 1.40 -1 -1 20 3.60 1.20 -1 -2 20 2.70 1.10 -1 -3 20 44.00 2.70 1 3 -20 47.20 3.60 -1 -4 20 24.90 2.00 1 4 -20 25.20 3.50 -1 -5 20 118.19 4.50 -1 -6 20 61.59 2.70 -2 3 20 201.38 8.00 -2 1 20 39.80 3.00 -2 0 20 24.60 2.40 -2 -1 20 32.80 2.50 -2 -2 20 16.70 2.10 -2 -3 20 197.28 7.40 2 3 -20 212.98 8.30 -2 -4 20 13.20 1.60 2 4 -20 10.80 3.00 -2 -5 20 128.29 4.80 -3 2 20 53.59 3.50 -3 1 20 1.50 1.40 -3 0 20 0.80 1.20 -3 -1 20 -0.10 1.10 -3 -2 20 50.39 2.80 3 2 -20 50.19 3.70 -3 -3 20 20.20 1.90 3 3 -20 23.30 2.90 -3 -4 20 43.40 2.40 3 4 -20 42.00 3.50 -3 -5 20 0.20 0.90 -4 2 20 108.69 4.90 -4 1 20 1.80 1.30 -4 0 20 100.69 4.30 4 0 -20 99.39 5.20 -4 -1 20 1.60 1.00 4 1 -20 -0.60 1.90 -4 -2 20 107.49 4.40 4 2 -20 105.59 5.10 -4 -3 20 0.70 0.90 4 3 -20 2.20 1.80 -4 -4 20 80.69 3.30 -4 -5 20 13.60 2.20 -5 2 20 75.39 3.60 -5 1 20 11.70 2.00 -5 0 20 -0.90 1.00 -5 -1 20 10.40 2.10 -5 -2 20 71.99 3.20 -5 -3 20 0.80 0.80 -5 -4 20 28.50 1.90 -6 1 20 151.48 5.40 -6 0 20 3.30 1.00 -6 -1 20 137.69 5.00 -6 -2 20 15.30 1.50 3 2 21 128.89 5.70 3 1 21 50.19 3.60 3 -2 21 127.99 4.80 3 -3 21 0.10 1.00 3 -4 21 41.40 2.20 2 3 21 55.79 3.60 2 2 21 6.70 1.70 2 1 21 3.70 1.70 2 -2 21 7.30 1.90 2 -3 21 52.09 3.50 2 -4 21 11.60 1.50 1 3 21 3.00 1.70 1 2 21 270.07 10.00 1 1 21 136.39 6.10 1 -1 21 145.39 5.60 1 -2 21 265.07 9.10 1 -3 21 2.40 0.90 1 -4 21 43.00 2.50 0 3 21 35.40 3.10 0 2 21 13.60 2.70 0 1 21 -1.80 1.50 0 0 21 -2.70 1.50 0 -1 21 0.40 1.20 0 -2 21 19.10 1.90 0 -3 21 34.10 2.30 0 3 -21 44.20 3.90 0 -4 21 3.50 1.20 0 -5 21 25.20 1.70 -1 3 21 -0.20 1.90 -1 1 21 -0.30 1.90 -1 0 21 23.40 2.50 -1 -1 21 0.60 1.10 -1 -2 21 140.29 5.40 -1 -3 21 3.30 0.90 1 3 -21 2.60 1.90 -1 -5 21 69.49 2.90 -2 1 21 70.69 5.00 -2 0 21 0.60 1.20 -2 -1 21 75.59 3.50 -2 -2 21 0.20 1.00 2 2 -21 -0.30 1.70 -2 -3 21 0.90 0.90 2 3 -21 1.60 1.80 -2 -4 21 0.40 0.80 -3 1 21 186.68 6.70 -3 0 21 7.40 2.00 -3 -1 21 179.48 6.80 3 1 -21 183.48 7.30 -3 -2 21 120.99 4.80 3 2 -21 132.19 5.80 -3 -4 21 140.49 5.00 -4 1 21 0.90 1.30 -4 0 21 -2.10 1.10 -4 -1 21 0.50 1.00 -4 -2 21 4.50 1.00 -4 -3 21 79.59 3.20 -5 1 21 65.69 3.10 -5 0 21 100.59 3.90 -5 -1 21 57.59 2.60 -5 -2 21 34.70 2.00 2 -2 22 28.90 2.50 2 -3 22 1.10 1.10 1 -1 22 31.50 2.70 1 -2 22 6.50 1.90 1 -3 22 69.89 3.00 0 -1 22 7.60 2.10 0 -2 22 132.49 4.90 0 -3 22 91.59 3.60 -1 0 22 0.10 1.50 -1 -1 22 17.80 2.00 -1 -2 22 1.60 0.90 -1 -3 22 10.30 1.40 -2 0 22 19.60 2.40 -2 -1 22 260.57 8.70 -2 -2 22 179.68 6.30 -2 -3 22 21.50 1.70 -3 0 22 2.00 1.20 -3 -1 22 23.90 1.90 -3 -2 22 18.40 1.60 -4 -1 22 17.50 1.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 67839 _shelx_res_file ; TITL SKM284_0ma_a.res in P2(1)/n SKM284_0ma_a.res created by SHELXL-2018/3 at 14:36:55 on 13-Aug-2020 REM Old TITL SKM284_0ma in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.099, Rweak 0.003, Alpha 0.019, Orientation as input REM Formula found by SHELXT: C21 N2 O3 S CELL 1.54178 10.7365 9.7590 18.5600 90.000 90.066 90.000 ZERR 4.000 0.0004 0.0003 0.0007 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 84 80 8 12 4 TEMP -123 SIZE 0.052 0.118 0.268 L.S. 5 BOND $H LIST 4 CONF EQIV $1 -x+2, -y+1, -z+1 HTAB C15 O2_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C18 O1_$2 ACTA 140 MPLA N1 C1 > C5 MPLA C8 > C13 FMAP 2 PLAN 5 WGHT 0.042600 0.769200 EXTI 0.004081 FVAR 0.65310 S1 5 0.629636 0.762401 0.453269 11.00000 0.03027 0.01732 = 0.02199 -0.00091 -0.00303 0.00121 O1 4 0.651334 0.076060 0.479949 11.00000 0.03159 0.02020 = 0.03666 0.00465 0.00425 -0.00004 O2 4 0.855130 0.829819 0.549096 11.00000 0.02485 0.04642 = 0.03894 -0.01211 -0.00246 0.00599 O3 4 0.736410 0.930318 0.633732 11.00000 0.02891 0.03561 = 0.02662 -0.00922 -0.00588 0.00204 N1 3 0.672705 0.517027 0.514224 11.00000 0.02568 0.02016 = 0.02075 -0.00044 -0.00333 -0.00205 N2 3 0.581376 0.652977 0.272608 11.00000 0.04734 0.02948 = 0.02850 0.00230 -0.00966 -0.00068 C1 1 0.663298 0.374250 0.382298 11.00000 0.01995 0.01995 = 0.02086 -0.00086 -0.00093 -0.00301 C2 1 0.690192 0.306036 0.446982 11.00000 0.02035 0.01797 = 0.02236 0.00067 -0.00179 -0.00212 C3 1 0.691027 0.380439 0.511674 11.00000 0.02243 0.02007 = 0.02197 0.00076 -0.00320 -0.00248 C4 1 0.650424 0.583709 0.453051 11.00000 0.01987 0.01919 = 0.02114 -0.00022 -0.00230 -0.00212 C5 1 0.642807 0.516096 0.386469 11.00000 0.02226 0.02030 = 0.01990 0.00122 -0.00328 -0.00223 C6 1 0.649715 0.307250 0.311651 11.00000 0.02834 0.02215 = 0.01946 -0.00098 -0.00119 -0.00098 H6 2 0.675102 0.362914 0.271101 11.00000 0.03779 C7 1 0.598463 0.184690 0.300864 11.00000 0.02811 0.02448 = 0.01925 -0.00097 -0.00003 -0.00242 H7 2 0.571695 0.132692 0.342003 11.00000 0.03269 C8 1 0.572378 0.121141 0.230828 11.00000 0.02334 0.02304 = 0.02012 -0.00284 -0.00098 -0.00014 C9 1 0.584804 0.190749 0.165176 11.00000 0.02711 0.02327 = 0.02325 0.00030 -0.00122 -0.00207 H9 2 0.613579 0.283914 0.164847 11.00000 0.03444 C10 1 0.555748 0.126546 0.100765 11.00000 0.02901 0.03294 = 0.02089 0.00065 -0.00224 0.00104 H10 2 0.562877 0.178160 0.056654 11.00000 0.04079 C11 1 0.513802 -0.008110 0.100779 11.00000 0.03366 0.03228 = 0.02260 -0.00643 -0.00568 0.00085 H11 2 0.491287 -0.052866 0.055505 11.00000 0.03984 C12 1 0.502150 -0.078403 0.165006 11.00000 0.04183 0.02304 = 0.02872 -0.00463 -0.00445 -0.00479 H12 2 0.471583 -0.170410 0.165241 11.00000 0.03697 C13 1 0.531136 -0.014476 0.229669 11.00000 0.03680 0.02402 = 0.02282 -0.00063 -0.00177 -0.00352 H13 2 0.524007 -0.065875 0.276264 11.00000 0.03630 C14 1 0.720867 0.154790 0.449550 11.00000 0.02439 0.02016 = 0.02136 -0.00048 -0.00419 -0.00023 C15 1 0.841029 0.109137 0.416810 11.00000 0.03113 0.02942 = 0.04485 0.00293 0.00684 0.00524 H15A 2 0.906852 0.149011 0.446963 11.00000 0.05573 H15B 2 0.846108 0.007993 0.417343 11.00000 0.05811 H14C 2 0.851610 0.146813 0.365811 11.00000 0.05088 C16 1 0.714901 0.313933 0.583308 11.00000 0.03928 0.02387 = 0.02141 0.00217 -0.00653 -0.00157 AFIX 137 H16A 2 0.723453 0.384753 0.620421 11.00000 -1.50000 H16B 2 0.791792 0.260036 0.580824 11.00000 -1.50000 H16C 2 0.645041 0.253596 0.595442 11.00000 -1.50000 AFIX 0 C17 1 0.609672 0.592147 0.322926 11.00000 0.02926 0.02105 = 0.02307 -0.00156 -0.00441 -0.00217 C18 1 0.631093 0.801404 0.547602 11.00000 0.02571 0.02068 = 0.02298 -0.00273 0.00067 0.00041 H18A 2 0.609967 0.716680 0.574035 11.00000 0.03731 H18B 2 0.567242 0.869379 0.555384 11.00000 0.02706 C19 1 0.754569 0.853658 0.574665 11.00000 0.02770 0.02232 = 0.02308 -0.00079 -0.00377 0.00378 C20 1 0.848249 0.987173 0.666822 11.00000 0.03289 0.04294 = 0.03826 -0.01188 -0.01405 0.00258 H20A 2 0.904442 0.910296 0.680710 11.00000 0.05291 H20B 2 0.895784 1.047374 0.629844 11.00000 0.05568 C21 1 0.807752 1.070118 0.730708 11.00000 0.04580 0.04464 = 0.03244 -0.00955 -0.01002 -0.00110 H21A 2 0.883039 1.109084 0.755016 11.00000 0.06451 H21B 2 0.762388 1.014409 0.763904 11.00000 0.05130 H21C 2 0.751277 1.143573 0.716725 11.00000 0.04918 HKLF 4 REM SKM284_0ma_a.res in P2(1)/n REM wR2 = 0.088200, GooF = S = 1.04052, Restrained GooF = 1.04052 for all data REM R1 = 0.033440 for 3520 Fo > 4sig(Fo) and 0.037943 for all 3912 data REM 314 parameters refined using 0 restraints END WGHT 0.0426 0.7692 REM Highest difference peak 0.215, deepest hole -0.285, 1-sigma level 0.043 Q1 1 0.7026 0.2004 0.5829 11.00000 0.05 0.22 Q2 1 0.6491 0.3443 0.6191 11.00000 0.05 0.21 Q3 1 0.7855 0.3516 0.6100 11.00000 0.05 0.21 Q4 1 0.7008 0.2360 0.4490 11.00000 0.05 0.20 Q5 1 0.6527 0.5553 0.4184 11.00000 0.05 0.19 ; _shelx_res_checksum 41469 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.62964(3) 0.76240(3) 0.45327(2) 0.02319(11) Uani d 1 . . O O1 0.65133(9) 0.07606(9) 0.47995(6) 0.0295(2) Uani d 1 . . O O2 0.85513(10) 0.82982(12) 0.54910(6) 0.0367(3) Uani d 1 . . O O3 0.73641(9) 0.93032(11) 0.63373(5) 0.0304(2) Uani d 1 . . N N1 0.67271(10) 0.51703(11) 0.51422(6) 0.0222(2) Uani d 1 . . N N2 0.58138(13) 0.65298(13) 0.27261(7) 0.0351(3) Uani d 1 . . C C1 0.66330(11) 0.37425(13) 0.38230(7) 0.0203(3) Uani d 1 . . C C2 0.69019(12) 0.30604(13) 0.44698(7) 0.0202(3) Uani d 1 . . C C3 0.69103(12) 0.38044(13) 0.51167(7) 0.0215(3) Uani d 1 . . C C4 0.65042(12) 0.58371(13) 0.45305(7) 0.0201(3) Uani d 1 . . C C5 0.64281(12) 0.51610(13) 0.38647(7) 0.0208(3) Uani d 1 . . C C6 0.64972(13) 0.30725(14) 0.31165(7) 0.0233(3) Uani d 1 . . H H6 0.6751(17) 0.363(2) 0.2711(10) 0.038(5) Uiso d 1 . . C C7 0.59846(13) 0.18469(14) 0.30086(7) 0.0239(3) Uani d 1 . . H H7 0.5717(16) 0.1327(18) 0.3420(10) 0.033(4) Uiso d 1 . . C C8 0.57238(12) 0.12114(13) 0.23083(7) 0.0222(3) Uani d 1 . . C C9 0.58480(13) 0.19075(14) 0.16518(7) 0.0245(3) Uani d 1 . . H H9 0.6136(17) 0.284(2) 0.1648(9) 0.034(5) Uiso d 1 . . C C10 0.55575(13) 0.12655(16) 0.10077(8) 0.0276(3) Uani d 1 . . H H10 0.5629(17) 0.178(2) 0.0567(10) 0.041(5) Uiso d 1 . . C C11 0.51380(14) -0.00811(16) 0.10078(8) 0.0295(3) Uani d 1 . . H H11 0.4913(18) -0.0529(19) 0.0555(10) 0.040(5) Uiso d 1 . . C C12 0.50215(15) -0.07840(15) 0.16501(8) 0.0312(3) Uani d 1 . . H H12 0.4716(17) -0.170(2) 0.1652(10) 0.037(5) Uiso d 1 . . C C13 0.53114(14) -0.01448(15) 0.22967(8) 0.0279(3) Uani d 1 . . H H13 0.5240(17) -0.0659(18) 0.2763(10) 0.036(5) Uiso d 1 . . C C14 0.72087(12) 0.15479(13) 0.44955(7) 0.0220(3) Uani d 1 . . C C15 0.84103(15) 0.10914(17) 0.41681(10) 0.0351(3) Uani d 1 . . H H15A 0.907(2) 0.149(2) 0.4470(12) 0.056(6) Uiso d 1 . . H H15B 0.846(2) 0.008(2) 0.4173(12) 0.058(6) Uiso d 1 . . H H14C 0.8516(19) 0.147(2) 0.3658(12) 0.051(6) Uiso d 1 . . C C16 0.71490(14) 0.31393(14) 0.58331(7) 0.0282(3) Uani d 1 . . H H16A 0.723453 0.384753 0.620421 0.042 Uiso calc 1 . . H H16B 0.791792 0.260036 0.580824 0.042 Uiso calc 1 . . H H16C 0.645041 0.253596 0.595442 0.042 Uiso calc 1 . . C C17 0.60967(13) 0.59215(14) 0.32293(7) 0.0245(3) Uani d 1 . . C C18 0.63109(13) 0.80140(14) 0.54760(7) 0.0231(3) Uani d 1 . . H H18A 0.6100(17) 0.717(2) 0.5740(10) 0.037(5) Uiso d 1 . . H H18B 0.5672(16) 0.8694(18) 0.5554(9) 0.027(4) Uiso d 1 . . C C19 0.75457(13) 0.85366(14) 0.57467(7) 0.0244(3) Uani d 1 . . C C20 0.84825(15) 0.98717(19) 0.66682(9) 0.0380(4) Uani d 1 . . H H20A 0.904(2) 0.910(2) 0.6807(12) 0.053(6) Uiso d 1 . . H H20B 0.896(2) 1.047(2) 0.6298(12) 0.056(6) Uiso d 1 . . C C21 0.80775(18) 1.0701(2) 0.73071(10) 0.0410(4) Uani d 1 . . H H21A 0.883(2) 1.109(2) 0.7550(13) 0.065(7) Uiso d 1 . . H H21B 0.762(2) 1.014(2) 0.7639(12) 0.051(6) Uiso d 1 . . H H21C 0.751(2) 1.144(2) 0.7167(11) 0.049(6) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.03027(19) 0.01732(17) 0.02199(18) 0.00121(12) -0.00303(12) -0.00091(11) O1 0.0316(5) 0.0202(5) 0.0367(6) 0.0000(4) 0.0043(4) 0.0046(4) O2 0.0248(5) 0.0464(7) 0.0389(6) 0.0060(4) -0.0025(4) -0.0121(5) O3 0.0289(5) 0.0356(6) 0.0266(5) 0.0020(4) -0.0059(4) -0.0092(4) N1 0.0257(6) 0.0202(5) 0.0208(6) -0.0021(4) -0.0033(4) -0.0004(4) N2 0.0473(8) 0.0295(6) 0.0285(7) -0.0007(6) -0.0097(6) 0.0023(5) C1 0.0199(6) 0.0200(6) 0.0209(6) -0.0030(5) -0.0009(5) -0.0009(5) C2 0.0203(6) 0.0180(6) 0.0224(6) -0.0021(5) -0.0018(5) 0.0007(5) C3 0.0224(6) 0.0201(6) 0.0220(7) -0.0025(5) -0.0032(5) 0.0008(5) C4 0.0199(6) 0.0192(6) 0.0211(6) -0.0021(5) -0.0023(5) -0.0002(5) C5 0.0223(6) 0.0203(6) 0.0199(6) -0.0022(5) -0.0033(5) 0.0012(5) C6 0.0283(7) 0.0222(6) 0.0195(6) -0.0010(5) -0.0012(5) -0.0010(5) C7 0.0281(7) 0.0245(7) 0.0193(6) -0.0024(5) 0.0000(5) -0.0010(5) C8 0.0233(6) 0.0230(6) 0.0201(6) -0.0001(5) -0.0010(5) -0.0028(5) C9 0.0271(7) 0.0233(7) 0.0232(7) -0.0021(5) -0.0012(5) 0.0003(5) C10 0.0290(7) 0.0329(7) 0.0209(7) 0.0010(6) -0.0022(5) 0.0007(6) C11 0.0337(7) 0.0323(7) 0.0226(7) 0.0009(6) -0.0057(6) -0.0064(6) C12 0.0418(8) 0.0230(7) 0.0287(8) -0.0048(6) -0.0045(6) -0.0046(6) C13 0.0368(8) 0.0240(7) 0.0228(7) -0.0035(6) -0.0018(6) -0.0006(5) C14 0.0244(6) 0.0202(6) 0.0214(6) -0.0002(5) -0.0042(5) -0.0005(5) C15 0.0311(8) 0.0294(8) 0.0448(10) 0.0052(6) 0.0068(7) 0.0029(7) C16 0.0393(8) 0.0239(7) 0.0214(7) -0.0016(6) -0.0065(6) 0.0022(5) C17 0.0293(7) 0.0211(6) 0.0231(7) -0.0022(5) -0.0044(5) -0.0016(5) C18 0.0257(7) 0.0207(6) 0.0230(7) 0.0004(5) 0.0007(5) -0.0027(5) C19 0.0277(7) 0.0223(6) 0.0231(6) 0.0038(5) -0.0038(5) -0.0008(5) C20 0.0329(8) 0.0429(9) 0.0383(9) 0.0026(7) -0.0140(7) -0.0119(7) C21 0.0458(10) 0.0446(10) 0.0324(9) -0.0011(8) -0.0100(7) -0.0095(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 S1 C18 . . 102.24(6) ? C19 O3 C20 . . 115.85(11) ? C4 N1 C3 . . 118.68(11) ? C2 C1 C5 . . 116.93(11) ? C2 C1 C6 . . 124.86(12) ? C5 C1 C6 . . 118.14(11) ? C1 C2 C3 . . 119.21(12) ? C1 C2 C14 . . 122.32(11) ? C3 C2 C14 . . 118.47(11) ? N1 C3 C2 . . 122.74(12) ? N1 C3 C16 . . 114.90(11) ? C2 C3 C16 . . 122.34(12) ? N1 C4 C5 . . 122.14(12) ? N1 C4 S1 . . 120.40(10) ? C5 C4 S1 . . 117.46(10) ? C4 C5 C1 . . 120.22(12) ? C4 C5 C17 . . 119.59(12) ? C1 C5 C17 . . 120.16(12) ? C7 C6 C1 . . 124.98(12) ? C7 C6 H6 . . 120.3(11) ? C1 C6 H6 . . 114.6(11) ? C6 C7 C8 . . 126.26(13) ? C6 C7 H7 . . 118.6(11) ? C8 C7 H7 . . 115.1(11) ? C13 C8 C9 . . 118.47(12) ? C13 C8 C7 . . 118.34(12) ? C9 C8 C7 . . 123.18(12) ? C10 C9 C8 . . 120.64(13) ? C10 C9 H9 . . 119.7(11) ? C8 C9 H9 . . 119.7(11) ? C9 C10 C11 . . 120.03(13) ? C9 C10 H10 . . 118.6(12) ? C11 C10 H10 . . 121.4(12) ? C12 C11 C10 . . 119.98(13) ? C12 C11 H11 . . 119.8(11) ? C10 C11 H11 . . 120.2(11) ? C11 C12 C13 . . 120.18(13) ? C11 C12 H12 . . 120.1(11) ? C13 C12 H12 . . 119.7(11) ? C12 C13 C8 . . 120.69(13) ? C12 C13 H13 . . 120.2(10) ? C8 C13 H13 . . 119.0(10) ? O1 C14 C15 . . 122.21(12) ? O1 C14 C2 . . 119.95(12) ? C15 C14 C2 . . 117.77(12) ? C14 C15 H15A . . 105.7(13) ? C14 C15 H15B . . 109.9(13) ? H15A C15 H15B . . 110.5(18) ? C14 C15 H14C . . 111.5(12) ? H15A C15 H14C . . 107.7(17) ? H15B C15 H14C . . 111.2(17) ? C3 C16 H16A . . 109.5 ? C3 C16 H16B . . 109.5 ? H16A C16 H16B . . 109.5 ? C3 C16 H16C . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? N2 C17 C5 . . 178.94(16) ? C19 C18 S1 . . 113.86(10) ? C19 C18 H18A . . 108.7(11) ? S1 C18 H18A . . 107.8(11) ? C19 C18 H18B . . 110.0(10) ? S1 C18 H18B . . 106.7(10) ? H18A C18 H18B . . 109.7(14) ? O2 C19 O3 . . 124.17(13) ? O2 C19 C18 . . 126.38(13) ? O3 C19 C18 . . 109.43(11) ? O3 C20 C21 . . 107.39(14) ? O3 C20 H20A . . 108.7(13) ? C21 C20 H20A . . 112.2(13) ? O3 C20 H20B . . 110.0(12) ? C21 C20 H20B . . 111.1(12) ? H20A C20 H20B . . 107.4(17) ? C20 C21 H21A . . 109.1(13) ? C20 C21 H21B . . 110.5(13) ? H21A C21 H21B . . 109.7(18) ? C20 C21 H21C . . 111.6(12) ? H21A C21 H21C . . 110.1(18) ? H21B C21 H21C . . 105.8(18) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C4 . 1.7581(13) ? S1 C18 . 1.7918(14) ? O1 C14 . 1.2112(16) ? O2 C19 . 1.2026(17) ? O3 C19 . 1.3417(17) ? O3 C20 . 1.4578(18) ? N1 C4 . 1.3301(17) ? N1 C3 . 1.3482(17) ? N2 C17 . 1.1473(19) ? C1 C2 . 1.4025(18) ? C1 C5 . 1.4038(18) ? C1 C6 . 1.4723(18) ? C2 C3 . 1.4032(18) ? C2 C14 . 1.5130(17) ? C3 C16 . 1.5013(18) ? C4 C5 . 1.4032(18) ? C5 C17 . 1.4378(18) ? C6 C7 . 1.332(2) ? C6 H6 . 0.968(19) ? C7 C8 . 1.4669(18) ? C7 H7 . 0.961(18) ? C8 C13 . 1.3958(19) ? C8 C9 . 1.4016(19) ? C9 C10 . 1.385(2) ? C9 H9 . 0.960(19) ? C10 C11 . 1.389(2) ? C10 H10 . 0.96(2) ? C11 C12 . 1.381(2) ? C11 H11 . 0.98(2) ? C12 C13 . 1.388(2) ? C12 H12 . 0.956(19) ? C13 H13 . 1.003(19) ? C14 C15 . 1.4946(19) ? C15 H15A . 0.98(2) ? C15 H15B . 0.99(2) ? C15 H14C . 1.02(2) ? C16 H16A . 0.9800 ? C16 H16B . 0.9800 ? C16 H16C . 0.9800 ? C18 C19 . 1.5061(19) ? C18 H18A . 0.988(19) ? C18 H18B . 0.965(17) ? C20 C21 . 1.500(2) ? C20 H20A . 1.00(2) ? C20 H20B . 1.04(2) ? C21 H21A . 1.00(2) ? C21 H21B . 0.96(2) ? C21 H21C . 0.97(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C15 H15A O2 3_766 0.98(2) 2.56(2) 3.375(2) 139.9(17) yes C18 H18B O1 3_666 0.965(17) 2.493(17) 3.2989(17) 140.9(13) yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C5 C1 C2 C3 . . . . 2.15(18) ? C6 C1 C2 C3 . . . . -175.01(12) ? C5 C1 C2 C14 . . . . -176.70(11) ? C6 C1 C2 C14 . . . . 6.15(19) ? C4 N1 C3 C2 . . . . 1.39(19) ? C4 N1 C3 C16 . . . . -179.73(12) ? C1 C2 C3 N1 . . . . -3.20(19) ? C14 C2 C3 N1 . . . . 175.69(12) ? C1 C2 C3 C16 . . . . 177.99(12) ? C14 C2 C3 C16 . . . . -3.12(19) ? C3 N1 C4 C5 . . . . 1.39(19) ? C3 N1 C4 S1 . . . . -178.47(10) ? C18 S1 C4 N1 . . . . -5.66(12) ? C18 S1 C4 C5 . . . . 174.48(10) ? N1 C4 C5 C1 . . . . -2.31(19) ? S1 C4 C5 C1 . . . . 177.55(10) ? N1 C4 C5 C17 . . . . 175.55(12) ? S1 C4 C5 C17 . . . . -4.59(17) ? C2 C1 C5 C4 . . . . 0.44(18) ? C6 C1 C5 C4 . . . . 177.79(12) ? C2 C1 C5 C17 . . . . -177.42(12) ? C6 C1 C5 C17 . . . . -0.06(18) ? C2 C1 C6 C7 . . . . 36.5(2) ? C5 C1 C6 C7 . . . . -140.67(14) ? C1 C6 C7 C8 . . . . 173.53(13) ? C6 C7 C8 C13 . . . . 172.91(14) ? C6 C7 C8 C9 . . . . -8.2(2) ? C13 C8 C9 C10 . . . . 0.5(2) ? C7 C8 C9 C10 . . . . -178.32(13) ? C8 C9 C10 C11 . . . . 0.0(2) ? C9 C10 C11 C12 . . . . -0.6(2) ? C10 C11 C12 C13 . . . . 0.6(2) ? C11 C12 C13 C8 . . . . 0.0(2) ? C9 C8 C13 C12 . . . . -0.5(2) ? C7 C8 C13 C12 . . . . 178.38(14) ? C1 C2 C14 O1 . . . . -114.75(15) ? C3 C2 C14 O1 . . . . 66.40(17) ? C1 C2 C14 C15 . . . . 68.12(17) ? C3 C2 C14 C15 . . . . -110.73(15) ? C4 S1 C18 C19 . . . . 98.96(10) ? C20 O3 C19 O2 . . . . 0.6(2) ? C20 O3 C19 C18 . . . . 179.32(12) ? S1 C18 C19 O2 . . . . -26.34(19) ? S1 C18 C19 O3 . . . . 154.93(10) ? C19 O3 C20 C21 . . . . 179.23(14) ? _cod_database_fobs_code 2243857