#------------------------------------------------------------------------------ #$Date: 2024-04-04 18:30:56 +0300 (Thu, 04 Apr 2024) $ #$Revision: 290787 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/98/7159877.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_7159877 loop_ _publ_author_name 'Shaikh, Aijaz' 'Sahoo, Satyajit' 'Marder, Seth R.' 'Barlow, Stephen' 'Mohapatra, Swagat K.' _publ_section_title ; Reductive dimerization of benzothiazolium salts. ; _journal_issue 10 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 2115 _journal_page_last 2123 _journal_paper_doi 10.1039/d3ob01871g _journal_volume 22 _journal_year 2024 _chemical_formula_sum 'C28 H36 N2 O2 S2' _chemical_formula_weight 496.71 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/1 _audit_update_record ; 2023-09-08 deposited with the CCDC. 2024-01-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 113.816(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 23.932(7) _cell_length_b 9.723(3) _cell_length_c 12.611(4) _cell_measurement_reflns_used 5111 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 26.38 _cell_measurement_theta_min 2.65 _cell_volume 2684.6(14) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.991 _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 0.0455 _diffrn_reflns_av_unetI/netI 0.0310 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 18065 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.600 _diffrn_reflns_theta_min 2.654 _exptl_absorpt_coefficient_mu 0.225 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_correction_T_min 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.229 _exptl_crystal_description Block _exptl_crystal_F_000 1064.0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.244 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.038 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 155 _refine_ls_number_reflns 3098 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0488 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+2.0501P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1243 _refine_ls_wR_factor_ref 0.1584 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2099 _reflns_number_total 3125 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ob01871g2.cif _cod_data_source_block Cy_S2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_cell_volume 2684.4(14) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7159877 _shelx_shelxl_version_number 2019/1 _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_res_file ; TITL Cy_S2_0m_a.res in C2/c Cy_S2_0m_a.res created by SHELXL-2019/1 at 21:12:03 on 27-Feb-2023 CELL 0.71073 23.9319 9.7227 12.6108 90.000 113.816 90.000 ZERR 34.000 0.0069 0.0030 0.0036 0.000 0.010 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N O S UNIT 34 34 34 34 34 REM Old TITL Cy_S2_0m in C2/c REM SHELXT solution in C2/c: R1 0.192, Rweak 0.009, Alpha 0.033 REM 0.325 for 168 systematic absences, Orientation as input REM Formula found by SHELXT: C13 N2 O S L.S. 10 ACTA BOND FMAP 2 PLAN 20 TEMP 0 WGHT 0.063800 2.050100 FVAR 0.76933 S1 5 0.454139 0.333131 0.221724 11.00000 0.06325 0.06710 = 0.07965 -0.01939 0.04018 -0.01132 N1 3 0.335000 0.356121 0.221788 11.00000 0.04834 0.05943 = 0.05670 -0.00806 0.01523 -0.01106 O1 4 0.288215 0.152988 0.206938 11.00000 0.07571 0.08273 = 0.09388 -0.02627 0.02898 -0.03830 C1 1 0.434884 0.465626 0.298354 11.00000 0.04957 0.05033 = 0.05167 -0.00136 0.02241 -0.00577 C6 1 0.374925 0.463224 0.288297 11.00000 0.04636 0.04822 = 0.05054 -0.00139 0.01737 -0.00484 C2 1 0.473459 0.569827 0.361392 11.00000 0.05494 0.06211 = 0.06376 -0.00607 0.02615 -0.01541 AFIX 43 H2 2 0.513755 0.572378 0.369029 11.00000 -1.20000 AFIX 0 C7 1 0.325657 0.236686 0.268644 11.00000 0.04956 0.06216 = 0.07213 -0.01598 0.02825 -0.01452 C3 1 0.451888 0.669766 0.412785 11.00000 0.07895 0.05343 = 0.06418 -0.01257 0.02972 -0.01884 AFIX 43 H3 2 0.478160 0.738324 0.456673 11.00000 -1.20000 AFIX 0 C8 1 0.361333 0.211674 0.395942 11.00000 0.06852 0.05479 = 0.06866 -0.00835 0.03455 -0.01879 AFIX 13 H8 2 0.394294 0.279702 0.424879 11.00000 -1.20000 AFIX 0 C5 1 0.353684 0.566128 0.337846 11.00000 0.05505 0.05779 = 0.06817 0.00031 0.02807 0.00188 AFIX 43 H5 2 0.313200 0.565616 0.329147 11.00000 -1.20000 AFIX 0 C4 1 0.392301 0.669409 0.400060 11.00000 0.07991 0.05155 = 0.06942 -0.00775 0.03724 -0.00130 AFIX 43 H4 2 0.377978 0.738764 0.433367 11.00000 -1.20000 AFIX 0 C14 1 0.298892 0.385350 0.099058 11.00000 0.08248 0.09502 = 0.06494 -0.00119 -0.00111 -0.01596 AFIX 137 H14A 2 0.303101 0.310849 0.052863 11.00000 -1.50000 H14B 2 0.313198 0.468887 0.077925 11.00000 -1.50000 H14C 2 0.256698 0.395483 0.085899 11.00000 -1.50000 AFIX 0 C13 1 0.389920 0.068601 0.418056 11.00000 0.10547 0.07213 = 0.08176 -0.00126 0.04458 0.00653 AFIX 23 H13A 2 0.358124 0.000311 0.383838 11.00000 -1.20000 H13B 2 0.418180 0.061039 0.380760 11.00000 -1.20000 AFIX 0 C9 1 0.320802 0.230497 0.460605 11.00000 0.10697 0.10404 = 0.09479 -0.01112 0.06339 0.00186 AFIX 23 H9A 2 0.305501 0.324110 0.450213 11.00000 -1.20000 H9B 2 0.286043 0.169029 0.428595 11.00000 -1.20000 AFIX 0 C12 1 0.423567 0.039291 0.546342 11.00000 0.11972 0.07359 = 0.08960 0.01027 0.04130 -0.00688 AFIX 23 H12A 2 0.439044 -0.054171 0.556757 11.00000 -1.20000 H12B 2 0.458202 0.101022 0.578860 11.00000 -1.20000 AFIX 0 C11 1 0.383181 0.056984 0.609682 11.00000 0.14191 0.11407 = 0.09110 0.01675 0.05500 -0.03414 AFIX 23 H11A 2 0.406768 0.043464 0.692028 11.00000 -1.20000 H11B 2 0.351004 -0.011565 0.583437 11.00000 -1.20000 AFIX 0 C10 1 0.354816 0.201440 0.588590 11.00000 0.14589 0.16636 = 0.08814 -0.01339 0.07227 0.00084 AFIX 23 H10A 2 0.326884 0.209306 0.626582 11.00000 -1.20000 H10B 2 0.386824 0.269363 0.622397 11.00000 -1.20000 AFIX 0 HKLF 4 REM Cy_S2_0m_a.res in C2/c REM wR2 = 0.1584, GooF = S = 1.081, Restrained GooF = 1.081 for all data REM R1 = 0.0488 for 2099 Fo > 4sig(Fo) and 0.0847 for all 3098 data REM 155 parameters refined using 0 restraints END WGHT 0.0545 2.2160 REM Highest difference peak 0.244, deepest hole -0.286, 1-sigma level 0.038 Q1 1 0.3325 0.1296 0.5576 11.00000 0.05 0.24 Q2 1 0.4424 0.4066 0.1693 11.00000 0.05 0.24 Q3 1 0.4180 0.4496 0.3254 11.00000 0.05 0.17 Q4 1 0.3602 0.3317 0.1598 11.00000 0.05 0.17 Q5 1 0.2611 0.2288 0.2082 11.00000 0.05 0.16 Q6 1 0.2705 0.4976 0.0856 11.00000 0.05 0.15 Q7 1 0.3842 0.1950 0.6053 11.00000 0.05 0.14 Q8 1 0.3689 0.4382 0.4071 11.00000 0.05 0.14 Q9 1 0.3321 0.4299 0.0468 11.00000 0.05 0.14 Q10 1 0.3095 0.3237 0.2555 11.00000 0.05 0.13 Q11 1 0.4182 0.6787 0.3849 11.00000 0.05 0.13 Q12 1 0.2897 0.1462 0.2819 11.00000 0.05 0.13 Q13 1 0.5000 0.4229 0.2500 10.50000 0.05 0.13 Q14 1 0.3722 -0.0215 0.5718 11.00000 0.05 0.12 Q15 1 0.3024 0.0515 0.3728 11.00000 0.05 0.12 Q16 1 0.4189 0.2382 0.3291 11.00000 0.05 0.12 Q17 1 0.5223 0.5159 0.3898 11.00000 0.05 0.11 Q18 1 0.2997 0.4744 0.3255 11.00000 0.05 0.11 Q19 1 0.4666 0.4137 0.3121 11.00000 0.05 0.11 Q20 1 0.3917 -0.0052 0.3283 11.00000 0.05 0.11 ; _shelx_res_checksum 87770 _shelx_hkl_file ; 6 0 0 2286.57 74.39 -6 0 0 2405.26 74.19 6 0 0 2459.15 71.59 6 0 0 2395.46 71.89 -6 0 0 2398.06 71.49 -6 0 0 2329.07 71.59 -8 0 0 3417.76 106.29 -8 0 0 3642.64 110.09 8 0 0 3638.24 106.49 8 0 0 3543.55 106.89 8 0 0 3555.24 110.79 -8 0 0 3634.24 106.49 10 0 0 3005.20 91.19 -10 0 0 2985.60 91.69 -10 0 0 2997.30 95.49 10 0 0 2882.61 91.79 10 0 0 2822.02 96.19 -10 0 0 3022.30 91.49 12 0 0 5000.50 156.08 -12 0 0 5083.39 154.08 12 0 0 4757.42 147.99 -12 0 0 5232.18 149.99 -12 0 0 4973.60 149.09 12 0 0 4732.53 149.39 14 0 0 340.27 21.00 14 0 0 368.56 24.90 -14 0 0 357.36 23.50 14 0 0 378.56 20.40 -14 0 0 358.76 20.50 -14 0 0 392.46 21.30 16 0 0 6.60 4.40 -16 0 0 9.40 6.30 -16 0 0 1.20 3.70 16 0 0 -2.40 3.60 -16 0 0 7.40 5.20 16 0 0 -5.50 4.20 -18 0 0 285.27 20.40 -18 0 0 313.97 21.60 18 0 0 314.57 20.70 -18 0 0 292.87 23.60 18 0 0 330.17 26.90 18 0 0 271.57 20.60 -20 0 0 47.70 12.30 -20 0 0 44.60 10.40 20 0 0 52.09 11.30 20 0 0 28.70 8.60 20 0 0 73.39 14.70 -22 0 0 16.90 8.80 22 0 0 28.30 11.10 -22 0 0 1.20 7.50 -24 0 0 90.29 15.80 -26 0 0 -10.30 8.30 -28 0 0 19.70 11.20 3 -1 0 1546.95 44.90 3 -1 0 1534.25 46.20 -3 -1 0 1517.05 45.90 3 -1 0 1462.85 49.40 -3 -1 0 1513.05 45.80 -3 1 0 1602.84 45.20 -3 1 0 1556.34 46.20 3 1 0 1510.25 45.50 -3 1 0 1414.36 49.20 5 -1 0 3545.85 105.29 -5 -1 0 3589.24 105.49 5 -1 0 3648.44 110.59 5 1 0 3485.45 105.49 -5 1 0 3607.54 104.29 -5 1 0 3584.84 105.39 -5 1 0 3657.63 110.39 5 1 0 3717.63 104.99 7 -1 0 267.57 13.40 7 -1 0 262.97 12.70 -7 -1 0 256.37 13.00 7 -1 0 259.27 16.90 -7 -1 0 269.87 13.70 -7 1 0 273.57 16.80 7 1 0 289.27 14.10 7 1 0 260.77 12.60 7 1 0 274.67 13.80 -7 1 0 252.67 13.30 -7 1 0 269.67 12.90 -9 -1 0 4340.77 118.59 -9 -1 0 3724.73 116.59 9 -1 0 3904.71 116.69 -9 -1 0 3979.00 116.39 9 -1 0 3687.93 123.29 9 -1 0 3782.62 115.69 -9 1 0 3982.10 117.19 -9 1 0 3717.03 122.49 9 1 0 4009.50 115.79 -9 1 0 3805.92 115.79 9 1 0 3763.82 118.19 9 1 0 3861.31 117.59 -11 -1 0 1520.15 51.99 11 -1 0 1481.45 51.49 11 -1 0 1517.35 52.29 11 -1 0 1437.26 58.69 -11 -1 0 1474.35 52.39 -11 -1 0 1563.94 53.89 11 1 0 1429.66 54.39 11 1 0 1410.56 50.69 -11 1 0 1509.95 51.69 -11 1 0 1637.84 53.29 11 1 0 1486.95 53.09 -11 1 0 1491.95 58.29 -13 -1 0 361.46 19.60 13 -1 0 319.87 18.60 -13 -1 0 343.27 19.30 13 -1 0 332.17 18.90 13 -1 0 304.67 23.10 -13 -1 0 358.56 20.60 -13 1 0 312.57 18.30 13 1 0 288.97 20.20 13 1 0 311.27 17.90 -13 1 0 301.47 22.20 13 1 0 302.67 19.30 -13 1 0 303.17 18.70 -15 -1 0 14.60 5.60 15 -1 0 -2.80 4.50 15 -1 0 11.30 4.40 -15 -1 0 7.40 4.40 15 -1 0 3.10 4.10 15 1 0 14.50 6.90 -15 1 0 7.00 4.10 -15 1 0 4.90 6.30 15 1 0 -1.50 3.90 -15 1 0 7.10 4.50 15 1 0 10.90 5.80 17 -1 0 17.90 6.30 -17 -1 0 21.50 6.70 17 -1 0 39.10 10.60 -17 -1 0 16.00 6.40 17 -1 0 15.70 6.90 -17 1 0 21.10 6.60 -17 1 0 18.10 7.50 17 1 0 17.20 9.10 -17 1 0 15.10 6.60 17 1 0 35.30 7.70 19 -1 0 22.30 7.50 -19 -1 0 23.00 8.30 19 -1 0 12.80 9.60 19 -1 0 -1.20 5.90 19 1 0 12.30 6.50 19 1 0 5.20 6.40 -19 1 0 5.80 5.70 -19 1 0 5.00 6.40 -19 1 0 13.20 8.90 -21 -1 0 23.00 8.90 21 -1 0 1.00 6.60 21 -1 0 13.90 7.70 21 -1 0 4.40 9.90 -21 1 0 4.40 6.50 21 1 0 21.80 7.40 -21 1 0 16.90 9.90 21 1 0 6.90 8.10 -23 -1 0 10.00 7.20 23 -1 0 19.10 8.50 -23 1 0 9.10 10.60 -23 1 0 -6.90 6.20 23 1 0 19.10 10.20 -25 -1 0 4.10 7.30 -25 1 0 5.70 7.70 -25 1 0 -2.40 8.60 -27 -1 0 14.30 10.70 -27 1 0 -6.70 8.80 0 -2 0 1167.68 39.00 0 2 0 1194.38 39.40 0 2 0 1122.49 36.80 0 2 0 1127.39 37.40 2 -2 0 3318.17 104.79 -2 -2 0 3517.85 101.39 2 -2 0 3395.36 100.79 -2 -2 0 3476.75 100.79 -2 2 0 3570.64 101.19 2 2 0 3412.56 100.99 2 2 0 3450.05 100.99 -2 2 0 3430.66 105.49 4 -2 0 690.23 29.90 4 -2 0 703.53 23.50 -4 -2 0 690.33 25.40 4 -2 0 694.63 25.40 -4 2 0 704.73 24.00 -4 2 0 699.73 25.70 -4 2 0 692.83 30.30 4 2 0 638.64 24.50 -6 -2 0 4544.45 130.09 6 -2 0 4351.56 137.39 6 -2 0 4528.95 130.39 -6 2 0 4441.06 130.49 6 2 0 4390.36 128.89 -6 2 0 4406.26 128.29 -6 2 0 4217.28 136.89 8 -2 0 1383.46 47.50 8 -2 0 1456.95 49.99 -8 -2 0 1500.25 49.99 8 -2 0 1443.36 57.19 -8 -2 0 1447.16 49.90 -8 2 0 1499.05 50.49 -8 2 0 1446.56 57.09 8 2 0 1495.65 48.90 8 2 0 1506.55 48.70 -8 2 0 1528.65 48.70 10 -2 0 707.73 27.50 10 -2 0 717.33 36.10 -10 -2 0 653.93 28.60 10 -2 0 669.33 28.70 -10 -2 0 699.83 29.00 10 2 0 686.33 27.50 -10 2 0 721.93 29.70 -10 2 0 674.13 27.60 -10 2 0 698.53 35.90 10 2 0 609.94 27.60 12 -2 0 21.10 5.40 -12 -2 0 33.20 7.20 -12 -2 0 24.00 5.50 12 -2 0 26.80 8.60 12 -2 0 26.60 6.40 12 2 0 21.40 5.90 -12 2 0 19.90 4.90 -12 2 0 39.10 9.80 -12 2 0 31.00 6.80 12 2 0 31.30 6.50 14 -2 0 613.34 37.70 -14 -2 0 653.73 31.00 14 -2 0 694.13 30.30 14 -2 0 649.34 30.60 -14 -2 0 671.43 31.20 -14 2 0 695.63 30.50 -14 2 0 672.73 38.20 14 2 0 656.73 29.50 -14 2 0 651.63 31.30 14 2 0 649.64 32.20 16 -2 0 134.99 13.40 16 -2 0 141.89 14.50 16 -2 0 130.39 19.80 -16 -2 0 131.49 13.80 -16 -2 0 155.38 14.80 16 2 0 112.59 15.60 -16 2 0 147.69 14.20 16 2 0 144.99 13.50 -16 2 0 125.39 13.10 -16 2 0 146.49 20.10 -18 -2 0 179.48 17.10 18 -2 0 181.48 16.40 18 -2 0 153.88 15.30 18 -2 0 127.19 20.40 -18 2 0 170.08 16.10 18 2 0 149.79 14.80 -18 2 0 150.28 22.00 -18 2 0 194.78 17.80 18 2 0 163.48 18.40 20 -2 0 88.39 23.00 20 -2 0 93.29 13.70 -20 -2 0 94.19 15.60 20 -2 0 82.99 13.10 -20 2 0 107.59 15.50 20 2 0 104.49 17.80 -20 2 0 106.39 18.80 20 2 0 68.19 12.50 22 -2 0 304.07 24.30 -22 -2 0 311.47 25.50 -22 2 0 345.17 26.10 -22 2 0 365.66 31.90 22 2 0 239.48 25.80 24 -2 0 44.60 11.40 -24 -2 0 51.49 11.60 24 2 0 53.09 15.80 -24 2 0 66.59 17.50 -24 2 0 43.40 11.00 -26 -2 0 -16.30 6.30 -26 2 0 10.30 11.80 -26 2 0 -1.30 8.30 -28 -2 0 4.70 10.10 -28 2 0 -11.60 9.20 -28 2 0 19.60 13.60 1 -3 0 6810.42 200.18 -1 -3 0 6973.30 197.98 -1 3 0 6633.54 200.58 3 -3 0 4157.58 121.09 3 -3 0 4072.79 118.49 3 -3 0 3954.90 126.89 -3 -3 0 4046.20 121.79 3 3 0 4226.08 121.79 -3 3 0 3942.81 127.39 -3 3 0 4031.20 118.99 -3 3 0 4084.99 121.39 3 3 0 4154.18 121.19 5 -3 0 854.41 38.00 5 -3 0 815.12 28.80 5 -3 0 817.52 31.50 -5 -3 0 868.71 32.40 -5 3 0 832.22 29.80 -5 3 0 867.21 32.50 5 3 0 823.32 31.10 5 3 0 814.22 30.60 -5 3 0 826.02 37.90 -7 -3 0 943.01 35.30 7 -3 0 953.30 43.40 7 -3 0 968.50 32.90 7 -3 0 953.30 35.90 -7 -3 0 930.61 36.00 -7 3 0 892.91 33.60 7 3 0 928.01 34.50 -7 3 0 979.60 36.70 -7 3 0 896.21 42.80 9 -3 0 2695.73 84.79 9 -3 0 2546.55 80.79 -9 -3 0 2702.73 85.19 9 -3 0 2545.25 94.19 -9 -3 0 2615.84 84.19 -9 3 0 2573.34 82.19 9 3 0 2647.73 82.79 -9 3 0 2675.43 85.49 -9 3 0 2603.84 94.59 11 -3 0 42.80 10.70 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14 13.90 7.80 8 -4 -14 15.20 9.30 -8 -4 14 37.30 13.10 -8 4 14 48.60 9.40 -8 4 14 34.40 16.10 6 -4 -14 -24.10 8.90 -6 -4 14 -16.60 5.90 -6 4 14 -3.40 7.10 -6 4 14 0.60 6.70 -4 -4 14 27.40 12.40 -4 4 14 28.80 18.20 -4 4 14 11.20 8.60 -2 -4 14 -10.30 7.20 -2 4 14 -3.40 7.40 0 -4 14 -8.60 9.10 0 4 14 -1.90 9.00 0 4 -14 -3.40 6.10 -19 -5 14 2.80 5.40 -19 -5 14 -5.00 6.40 -19 5 14 -6.20 14.20 -19 5 14 -10.00 4.40 -17 -5 14 -10.00 10.10 -17 -5 14 -19.00 6.00 -17 -5 14 -5.70 6.80 -17 5 14 -22.70 10.20 -15 -5 14 7.50 10.50 -15 -5 14 22.40 11.30 -15 5 14 30.00 8.40 -15 5 14 13.10 2.50 -15 5 14 14.10 11.80 -13 -5 14 -7.30 12.20 -13 -5 14 3.80 9.40 -13 5 14 -17.00 11.40 -13 5 14 4.90 3.70 -11 -5 14 20.70 11.20 -11 5 14 9.70 13.10 -9 -5 14 9.60 10.50 -9 5 14 -0.90 10.30 -9 5 14 -8.20 4.30 7 -5 -14 2.20 8.40 -7 -5 14 13.50 12.30 -7 5 14 9.80 6.30 -7 5 14 -8.70 11.00 5 -5 -14 12.90 11.50 -5 -5 14 4.80 10.00 -5 5 14 10.50 7.50 -5 5 14 18.30 13.40 -3 -5 14 5.20 11.10 -3 5 14 -0.50 10.90 -3 5 14 8.20 8.20 -1 5 14 2.60 11.20 -16 -6 14 11.30 8.30 -16 -6 14 14.70 13.50 -16 6 14 -4.30 12.80 -14 -6 14 5.80 11.90 -12 6 14 7.90 11.70 -10 -6 14 3.60 9.80 -10 6 14 4.20 14.10 -8 -6 14 14.50 13.10 -8 6 14 40.60 16.80 -8 6 14 68.49 9.00 -6 -6 14 -5.30 9.20 -6 6 14 -10.50 4.90 -6 6 14 8.50 14.70 -22 0 15 1.80 10.60 -22 0 15 4.50 9.50 -20 0 15 -11.90 8.40 -20 0 15 -8.50 9.40 -18 0 15 5.70 11.00 -18 0 15 -1.20 2.90 -16 0 15 -3.50 8.40 -16 0 15 -10.50 5.90 -16 0 15 -11.70 3.50 -14 0 15 2.10 4.70 -14 0 15 -17.90 9.00 -14 0 15 -5.20 7.40 -12 0 15 -12.40 4.30 -12 0 15 -11.10 5.50 -12 0 15 -6.80 9.30 -10 0 15 -8.70 5.70 -8 0 15 0.20 7.30 -6 0 15 -6.00 6.90 -4 0 15 4.90 8.90 -2 0 15 -2.80 7.70 0 0 15 -5.30 8.90 -21 -1 15 8.90 10.90 -21 -1 15 26.00 12.00 -21 1 15 0.40 11.90 -21 1 15 19.50 10.40 -19 -1 15 54.99 13.90 -19 -1 15 53.99 15.80 -19 1 15 30.70 9.90 -19 1 15 51.59 16.90 -17 -1 15 87.99 16.10 -17 -1 15 49.60 14.50 -17 1 15 56.49 13.10 -17 1 15 61.99 16.00 -17 1 15 47.00 6.30 -15 -1 15 18.10 11.90 -15 -1 15 -19.80 7.80 -15 1 15 6.90 10.00 -15 1 15 2.80 8.10 -13 -1 15 5.00 5.30 -13 -1 15 -7.50 7.20 -13 -1 15 -16.40 8.90 -13 1 15 -14.60 6.10 -13 1 15 -2.30 5.60 -13 1 15 0.90 9.70 -11 -1 15 22.10 6.30 -11 -1 15 23.00 11.20 -11 1 15 5.10 10.10 -11 1 15 11.40 8.40 -11 1 15 1.00 6.00 -9 -1 15 4.00 7.30 -9 -1 15 8.60 8.20 -9 1 15 -11.30 6.30 -9 1 15 -0.50 6.50 -7 -1 15 7.70 8.80 -7 1 15 4.50 7.30 -5 -1 15 18.80 9.90 -5 1 15 24.40 10.20 -3 -1 15 -12.40 7.20 -3 1 15 -11.50 6.90 -1 -1 15 3.80 8.40 -1 1 15 -15.90 7.40 -22 -2 15 -18.50 10.50 -22 -2 15 12.20 8.10 -22 2 15 28.30 15.60 -22 2 15 -3.00 7.40 -20 -2 15 -1.40 8.70 -20 -2 15 14.00 9.80 -20 2 15 -3.60 12.40 -20 2 15 8.80 8.50 -18 -2 15 19.00 9.90 -18 -2 15 18.30 9.50 -18 2 15 35.70 16.10 -18 2 15 15.70 8.50 -16 -2 15 -3.80 7.60 -16 -2 15 12.70 11.80 -16 -2 15 -1.30 4.90 -16 2 15 -0.70 11.40 -16 2 15 19.70 9.90 -14 -2 15 -11.60 8.40 -14 -2 15 9.80 5.50 -14 -2 15 -0.20 6.40 -14 2 15 5.90 5.30 -14 2 15 15.20 8.90 -14 2 15 -8.00 10.50 -12 -2 15 7.00 5.30 -12 -2 15 -8.00 6.90 -12 2 15 -0.10 9.50 -12 2 15 -12.50 4.50 -12 2 15 -4.20 5.80 -10 -2 15 32.20 10.10 -10 -2 15 28.80 12.40 -10 2 15 20.00 14.00 -10 2 15 28.80 10.20 -10 2 15 8.70 7.30 -8 -2 15 -9.90 7.70 -6 -2 15 -0.50 9.00 -6 2 15 -5.70 6.90 -4 -2 15 -2.00 9.30 -4 2 15 7.90 9.70 -2 -2 15 16.50 9.00 -2 2 15 23.90 9.40 -19 -3 15 10.10 9.50 -19 -3 15 -6.20 8.80 -19 3 15 -16.50 5.70 -19 3 15 -8.10 10.00 -17 -3 15 -10.70 7.90 -17 -3 15 -10.70 9.20 -17 -3 15 4.50 11.00 -17 3 15 3.50 13.70 -15 -3 15 -10.10 9.10 -15 -3 15 -9.20 7.90 -15 3 15 -7.50 5.40 -15 3 15 -0.50 5.30 -15 3 15 -2.10 10.10 -13 -3 15 -11.20 7.80 -13 -3 15 -4.50 5.90 -13 3 15 18.00 14.30 -13 3 15 -3.80 6.10 -13 3 15 -7.00 5.30 -11 -3 15 -17.10 8.80 -11 3 15 14.70 12.70 -11 3 15 14.90 7.90 -11 3 15 7.80 7.00 -9 -3 15 13.90 10.50 -9 3 15 0.50 7.50 -9 3 15 19.40 12.60 -7 -3 15 -15.40 8.90 -7 3 15 -14.30 10.80 -7 3 15 -1.90 6.60 -5 3 15 8.00 8.60 -3 -3 15 5.70 9.90 -3 3 15 -3.20 7.60 -18 -4 15 18.20 7.70 -18 -4 15 29.90 11.90 -18 4 15 16.10 5.80 -18 4 15 16.00 15.70 -16 -4 15 15.20 10.30 -16 -4 15 -10.50 7.90 -16 4 15 -12.90 4.40 -16 4 15 -14.10 12.20 -14 -4 15 0.20 7.70 -14 4 15 -19.40 11.50 -14 4 15 -7.20 4.90 -12 -4 15 16.80 11.50 -12 4 15 -11.40 11.50 -12 4 15 15.00 6.60 -10 -4 15 20.20 12.00 -10 4 15 27.00 8.80 -10 4 15 55.99 19.50 -8 -4 15 1.70 9.70 -8 4 15 5.00 14.30 -8 4 15 10.10 8.00 -6 4 15 -12.50 6.30 -6 4 15 8.40 15.50 -13 -5 15 15.00 11.30 -13 5 15 -25.40 10.90 -13 5 15 14.20 6.00 -11 -5 15 1.60 12.10 -11 5 15 12.00 6.20 -11 5 15 -7.80 15.40 -9 -5 15 41.30 13.90 -9 5 15 31.90 8.60 -9 5 15 53.79 15.50 -18 0 16 9.20 11.10 -18 0 16 -9.20 8.70 -16 0 16 4.80 9.30 -16 0 16 -3.50 8.50 -14 0 16 2.20 7.90 -14 0 16 -6.00 11.10 -12 0 16 19.70 11.40 -12 0 16 29.50 16.40 -10 0 16 49.20 13.10 -8 0 16 -2.70 8.40 -6 0 16 -2.40 7.80 -17 -1 16 -9.20 10.40 -17 1 16 -10.40 7.60 -17 1 16 13.60 12.40 -15 -1 16 -22.90 10.20 -15 -1 16 -6.70 8.30 -15 1 16 -6.30 8.40 -15 1 16 -15.80 9.50 -13 -1 16 -7.00 9.50 -13 1 16 -14.30 8.90 -13 1 16 0.40 7.90 -11 -1 16 1.80 9.30 -11 1 16 -5.90 8.10 -9 -1 16 -10.10 8.70 -9 1 16 -8.40 7.50 -7 -1 16 -9.70 8.40 -7 1 16 4.80 9.50 -16 -2 16 -14.40 8.10 -16 -2 16 6.70 11.90 -16 2 16 -3.60 6.60 -16 2 16 -7.70 11.80 -14 -2 16 -2.80 11.20 -14 -2 16 -19.90 8.00 -14 2 16 12.10 14.30 -14 2 16 -7.40 7.10 -12 -2 16 -12.20 10.30 -12 2 16 -10.80 13.00 -10 -2 16 -9.30 8.10 -10 2 16 13.00 8.20 -10 2 16 1.90 11.10 -8 -2 16 -0.60 8.70 -8 2 16 -10.70 13.00 -8 2 16 -3.00 8.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 43601 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 S1 S 0.45414(3) 0.33313(7) 0.22172(6) 0.0664(2) Uani 1 1 d . . . . . N1 N 0.33500(8) 0.35612(19) 0.22179(16) 0.0567(5) Uani 1 1 d . . . . . O1 O 0.28821(9) 0.1530(2) 0.20694(18) 0.0858(6) Uani 1 1 d . . . . . C1 C 0.43488(9) 0.4656(2) 0.29835(18) 0.0499(5) Uani 1 1 d . . . . . C6 C 0.37493(9) 0.4632(2) 0.28830(18) 0.0491(5) Uani 1 1 d . . . . . C2 C 0.47346(10) 0.5698(2) 0.3614(2) 0.0596(6) Uani 1 1 d . . . . . H2 H 0.513755 0.572378 0.369029 0.071 Uiso 1 1 calc R U . . . C7 C 0.32566(10) 0.2367(2) 0.2686(2) 0.0601(6) Uani 1 1 d . . . . . C3 C 0.45189(12) 0.6698(2) 0.4128(2) 0.0653(6) Uani 1 1 d . . . . . H3 H 0.478160 0.738324 0.456673 0.078 Uiso 1 1 calc R U . . . C8 C 0.36133(11) 0.2117(2) 0.3959(2) 0.0618(6) Uani 1 1 d . . . . . H8 H 0.394294 0.279702 0.424879 0.074 Uiso 1 1 calc R U . . . C5 C 0.35368(10) 0.5661(2) 0.3378(2) 0.0593(6) Uani 1 1 d . . . . . H5 H 0.313200 0.565616 0.329147 0.071 Uiso 1 1 calc R U . . . C4 C 0.39230(12) 0.6694(2) 0.4001(2) 0.0647(6) Uani 1 1 d . . . . . H4 H 0.377978 0.738764 0.433367 0.078 Uiso 1 1 calc R U . . . C14 C 0.29889(14) 0.3854(3) 0.0991(2) 0.0907(9) Uani 1 1 d . . . . . H14A H 0.303101 0.310849 0.052863 0.136 Uiso 1 1 calc R U . . . H14B H 0.313198 0.468887 0.077925 0.136 Uiso 1 1 calc R U . . . H14C H 0.256698 0.395483 0.085899 0.136 Uiso 1 1 calc R U . . . C13 C 0.38992(15) 0.0686(3) 0.4181(3) 0.0843(8) Uani 1 1 d . . . . . H13A H 0.358124 0.000311 0.383838 0.101 Uiso 1 1 calc R U . . . H13B H 0.418180 0.061039 0.380760 0.101 Uiso 1 1 calc R U . . . C9 C 0.32080(16) 0.2305(4) 0.4606(3) 0.0946(10) Uani 1 1 d . . . . . H9A H 0.305501 0.324110 0.450213 0.114 Uiso 1 1 calc R U . . . H9B H 0.286043 0.169029 0.428595 0.114 Uiso 1 1 calc R U . . . C12 C 0.42357(17) 0.0393(3) 0.5463(3) 0.0946(9) Uani 1 1 d . . . . . H12A H 0.439044 -0.054171 0.556757 0.114 Uiso 1 1 calc R U . . . H12B H 0.458202 0.101022 0.578860 0.114 Uiso 1 1 calc R U . . . C11 C 0.3832(2) 0.0570(4) 0.6097(3) 0.1131(13) Uani 1 1 d . . . . . H11A H 0.406768 0.043464 0.692028 0.136 Uiso 1 1 calc R U . . . H11B H 0.351004 -0.011565 0.583437 0.136 Uiso 1 1 calc R U . . . C10 C 0.3548(2) 0.2014(5) 0.5886(3) 0.1254(14) Uani 1 1 d . . . . . H10A H 0.326884 0.209306 0.626582 0.151 Uiso 1 1 calc R U . . . H10B H 0.386824 0.269363 0.622397 0.151 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 S1 0.0632(4) 0.0671(4) 0.0797(4) -0.0194(3) 0.0402(3) -0.0113(3) N1 0.0483(10) 0.0594(11) 0.0567(10) -0.0081(8) 0.0152(8) -0.0111(8) O1 0.0757(12) 0.0827(13) 0.0939(14) -0.0263(10) 0.0290(10) -0.0383(10) C1 0.0496(11) 0.0503(11) 0.0517(11) -0.0014(9) 0.0224(9) -0.0058(9) C6 0.0464(10) 0.0482(11) 0.0505(11) -0.0014(9) 0.0174(9) -0.0048(8) C2 0.0549(12) 0.0621(13) 0.0638(14) -0.0061(11) 0.0262(11) -0.0154(10) C7 0.0496(12) 0.0622(14) 0.0721(15) -0.0160(11) 0.0282(11) -0.0145(10) C3 0.0789(16) 0.0534(13) 0.0642(14) -0.0126(11) 0.0297(12) -0.0188(12) C8 0.0685(14) 0.0548(12) 0.0687(15) -0.0083(11) 0.0346(12) -0.0188(11) C5 0.0550(12) 0.0578(13) 0.0682(14) 0.0003(11) 0.0281(11) 0.0019(10) C4 0.0799(16) 0.0515(13) 0.0694(15) -0.0078(11) 0.0372(13) -0.0013(11) C14 0.0825(19) 0.095(2) 0.0649(16) -0.0012(15) -0.0011(14) -0.0160(16) C13 0.105(2) 0.0721(17) 0.0818(19) -0.0013(14) 0.0446(17) 0.0065(16) C9 0.107(2) 0.104(2) 0.095(2) -0.0111(19) 0.063(2) 0.002(2) C12 0.120(3) 0.0736(19) 0.090(2) 0.0103(16) 0.0413(19) -0.0069(17) C11 0.142(3) 0.114(3) 0.091(2) 0.017(2) 0.055(2) -0.034(3) C10 0.146(3) 0.166(4) 0.088(2) -0.013(3) 0.072(2) 0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 S1 S1 106.96(7) . 2_655 ? C7 N1 C6 123.59(18) . . ? C7 N1 C14 119.6(2) . . ? C6 N1 C14 116.56(19) . . ? C2 C1 C6 119.3(2) . . ? C2 C1 S1 125.64(17) . . ? C6 C1 S1 115.02(15) . . ? C5 C6 C1 120.14(19) . . ? C5 C6 N1 120.74(19) . . ? C1 C6 N1 119.07(18) . . ? C3 C2 C1 119.7(2) . . ? O1 C7 N1 119.7(2) . . ? O1 C7 C8 121.6(2) . . ? N1 C7 C8 118.65(18) . . ? C4 C3 C2 120.9(2) . . ? C7 C8 C9 110.2(2) . . ? C7 C8 C13 111.2(2) . . ? C9 C8 C13 110.5(2) . . ? C4 C5 C6 120.1(2) . . ? C3 C4 C5 119.8(2) . . ? C12 C13 C8 111.9(2) . . ? C10 C9 C8 111.6(3) . . ? C11 C12 C13 111.7(3) . . ? C12 C11 C10 110.4(3) . . ? C9 C10 C11 111.4(3) . . ? 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 S1 C1 1.779(2) . ? S1 S1 2.0156(14) 2_655 ? N1 C7 1.362(3) . ? N1 C6 1.433(3) . ? N1 C14 1.464(3) . ? O1 C7 1.228(3) . ? C1 C2 1.385(3) . ? C1 C6 1.389(3) . ? C6 C5 1.381(3) . ? C2 C3 1.379(3) . ? C7 C8 1.503(3) . ? C3 C4 1.369(4) . ? C8 C9 1.509(4) . ? C8 C13 1.525(4) . ? C5 C4 1.376(3) . ? C13 C12 1.515(4) . ? C9 C10 1.512(5) . ? C12 C11 1.492(5) . ? C11 C10 1.536(6) . ?