#------------------------------------------------------------------------------ #$Date: 2023-04-20 11:36:01 +0300 (Thu, 20 Apr 2023) $ #$Revision: 282767 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/70/8107099.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_8107099 loop_ _publ_author_name 'El-Hiti, Gamal A.' 'Smith, Keith' 'Hegazy, Amany S.' 'Alanazi, Saud A.' 'Kariuki, Benson M.' _publ_section_title ; Crystal structure of 2-(4-methoxyphenyl)-1,3-thiazolo[4,5-b]pyridine, C13H10N2OS ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 1067 _journal_page_last 1068 _journal_paper_doi 10.1515/ncrs-2016-0053 _journal_volume 231 _journal_year 2016 _chemical_formula_moiety 'C13 H10 N2 O S' _chemical_formula_sum 'C13 H10 N2 O S' _chemical_formula_weight 242.29 _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 _cell_angle_alpha 90 _cell_angle_beta 101.162(17) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.182(3) _cell_length_b 5.9674(6) _cell_length_c 26.683(4) _cell_measurement_reflns_used 987 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.3400 _cell_measurement_theta_min 3.8390 _cell_volume 2215.5(6) _computing_cell_refinement 'CrysAlis PRO [6]' _computing_data_collection 'CrysAlis PRO [6]' _computing_data_reduction 'CrysAlis PRO [6]' _computing_molecular_graphics 'ORTEP-3 for Windows [7]' _computing_publication_material 'WinGX [7] and CHEMDRAW Ultra [8]' _computing_structure_refinement 'SHELXL-2013 [5]' _computing_structure_solution 'SHELXS2013 [5]' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.898 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.1195 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.898 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 6077 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.898 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.689 _diffrn_reflns_theta_min 3.502 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET) (compiled Dec 9 2014,15:38:47) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.453 _exptl_crystal_description plate _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.416 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.028 _refine_diff_density_max 0.540 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.086 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 309 _refine_ls_number_reflns 6077 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.928 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0634 _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^)+(0.0776P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1330 _refine_ls_wR_factor_ref 0.1514 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3490 _reflns_number_total 6077 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_ncrs-2016-0053_suppl.cif _cod_data_source_block bmk1547c _cod_original_cell_volume 2215.4(6) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 8107099 _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 0.894 _shelx_estimated_absorpt_t_max 0.992 _shelxl_version_number 2013-4 _shelx_res_file ; TITL bmk1547c_twin in P2(1)/c CELL 0.71073 14.1821 5.9674 26.6826 90.000 101.162 90.000 ZERR 8.00 0.0029 0.0006 0.0037 0.000 0.017 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 104 80 16 8 8 MERG 2 FMAP 2 PLAN 5 SIZE 0.028 0.108 0.416 ACTA BOND $H L.S. 10 TEMP -123.00 WGHT 0.077600 FVAR 0.90965 C1 1 0.623640 0.440588 0.013605 11.00000 0.01317 0.02034 = 0.03451 -0.00083 0.00374 -0.00157 C2 1 0.672930 0.646775 0.093149 11.00000 0.01905 0.02973 = 0.02846 -0.00283 0.00785 0.00259 C3 1 0.636371 0.428244 0.097121 11.00000 0.01560 0.01957 = 0.02639 -0.00220 0.00498 0.00058 C4 1 0.703544 0.772503 0.136886 11.00000 0.02822 0.02580 = 0.03990 -0.00183 0.00875 0.00031 AFIX 43 H4 2 0.727109 0.921016 0.135643 11.00000 -1.20000 AFIX 0 C5 1 0.697712 0.668906 0.182290 11.00000 0.02977 0.04190 = 0.02886 -0.00750 0.00075 0.00212 AFIX 43 H5 2 0.719165 0.746778 0.213466 11.00000 -1.20000 AFIX 0 C6 1 0.661380 0.454136 0.183672 11.00000 0.03447 0.03563 = 0.02374 0.00334 0.00961 0.00150 AFIX 43 H6 2 0.658526 0.390709 0.216000 11.00000 -1.20000 AFIX 0 C7 1 0.605951 0.370807 -0.040201 11.00000 0.01791 0.01111 = 0.02338 -0.00242 0.00117 0.00216 C8 1 0.559777 0.168964 -0.054844 11.00000 0.02195 0.01996 = 0.02738 0.00633 0.00731 0.00060 AFIX 43 H8 2 0.539600 0.078580 -0.029564 11.00000 -1.20000 AFIX 0 C9 1 0.542263 0.095461 -0.104731 11.00000 0.01773 0.02293 = 0.02609 -0.00268 0.00709 -0.00121 AFIX 43 H9 2 0.508711 -0.040779 -0.113940 11.00000 -1.20000 AFIX 0 C10 1 0.574605 0.224384 -0.141259 11.00000 0.01994 0.03147 = 0.02019 0.00241 -0.00026 0.00586 C11 1 0.621603 0.427272 -0.127768 11.00000 0.01537 0.02716 = 0.03004 0.00771 0.00247 0.00380 AFIX 43 H11 2 0.643096 0.515381 -0.153010 11.00000 -1.20000 AFIX 0 C12 1 0.636752 0.499419 -0.078085 11.00000 0.01539 0.02511 = 0.03107 0.00201 -0.00067 -0.00129 AFIX 43 H12 2 0.668473 0.638107 -0.069166 11.00000 -1.20000 AFIX 0 C13 1 0.512539 -0.030764 -0.208081 11.00000 0.04892 0.03133 = 0.02626 -0.00627 0.00425 -0.00558 AFIX 137 H13A 2 0.544896 -0.159309 -0.189332 11.00000 -1.50000 H13B 2 0.509485 -0.052256 -0.244773 11.00000 -1.50000 H13C 2 0.447248 -0.017871 -0.201329 11.00000 -1.50000 AFIX 0 C14 1 0.882838 -0.057305 0.007934 11.00000 0.01145 0.02519 = 0.02788 0.00409 0.00791 0.00555 C15 1 0.886525 0.164707 0.085350 11.00000 0.02175 0.02540 = 0.02626 -0.00091 0.00847 -0.00690 C16 1 0.926364 -0.049719 0.091639 11.00000 0.01506 0.03595 = 0.02747 -0.00033 0.00715 -0.00030 C17 1 0.885738 0.299566 0.127145 11.00000 0.01982 0.03179 = 0.03325 0.00183 0.00432 -0.00288 AFIX 43 H17 2 0.858358 0.445356 0.123500 11.00000 -1.20000 AFIX 0 C18 1 0.926267 0.214683 0.174523 11.00000 0.02928 0.03840 = 0.02898 -0.00524 0.00915 0.00118 AFIX 43 H18 2 0.928849 0.301638 0.204582 11.00000 -1.20000 AFIX 0 C19 1 0.963087 -0.000907 0.177020 11.00000 0.03858 0.04344 = 0.02767 0.00833 -0.00045 0.00836 AFIX 43 H19 2 0.988978 -0.057802 0.210072 11.00000 -1.20000 AFIX 0 C20 1 0.863150 -0.135079 -0.044395 11.00000 0.01296 0.02441 = 0.02742 -0.00187 0.00383 0.00010 C21 1 0.903369 -0.335262 -0.057397 11.00000 0.01222 0.03246 = 0.02453 0.00465 0.00549 -0.00036 AFIX 43 H21 2 0.943853 -0.418366 -0.031401 11.00000 -1.20000 AFIX 0 C22 1 0.886281 -0.416293 -0.106693 11.00000 0.02159 0.02719 = 0.02838 -0.00497 0.00876 -0.00060 AFIX 43 H22 2 0.914495 -0.553020 -0.114567 11.00000 -1.20000 AFIX 0 C23 1 0.827027 -0.294459 -0.144707 11.00000 0.01944 0.03164 = 0.02324 0.00111 0.00316 -0.00702 C24 1 0.786786 -0.092498 -0.132652 11.00000 0.02006 0.03050 = 0.02674 0.00495 0.00465 0.00874 AFIX 43 H24 2 0.746459 -0.008679 -0.158573 11.00000 -1.20000 AFIX 0 C25 1 0.805704 -0.015666 -0.083264 11.00000 0.02245 0.02256 = 0.02972 0.00016 0.00718 0.00277 AFIX 43 H25 2 0.778753 0.122839 -0.075520 11.00000 -1.20000 AFIX 0 C26 1 0.839505 -0.567495 -0.208213 11.00000 0.04043 0.04191 = 0.03181 -0.01193 0.00800 0.00448 AFIX 137 H26A 2 0.909929 -0.564741 -0.201008 11.00000 -1.50000 H26B 2 0.816159 -0.596403 -0.244658 11.00000 -1.50000 H26C 2 0.816926 -0.686278 -0.188072 11.00000 -1.50000 AFIX 0 N1 3 0.608618 0.317428 0.050987 11.00000 0.02353 0.02700 = 0.02129 -0.00206 0.00699 -0.00508 N2 3 0.629891 0.330600 0.141543 11.00000 0.02758 0.03202 = 0.02737 0.00412 0.00620 -0.00375 N3 3 0.924525 -0.173222 0.047617 11.00000 0.01896 0.02976 = 0.02340 0.00038 0.00512 0.00021 N4 3 0.965749 -0.136152 0.137661 11.00000 0.03514 0.03674 = 0.02758 -0.00362 0.00333 0.00793 O1 4 0.565125 0.169627 -0.191731 11.00000 0.03436 0.02971 = 0.02803 0.00507 0.00454 -0.00472 O2 4 0.803765 -0.356049 -0.194937 11.00000 0.03216 0.03454 = 0.02074 -0.00194 0.00047 0.00860 S1 5 0.670548 0.709253 0.030032 11.00000 0.02758 0.02335 = 0.03274 0.00038 0.00578 -0.00374 S2 5 0.844800 0.214357 0.021554 11.00000 0.02684 0.02451 = 0.02957 0.00218 0.00492 0.00335 HKLF 5 REM bmk1547c_twin in P2(1)/c REM R1 = 0.0634 for 3490 Fo > 4sig(Fo) and 0.1173 for all 6077 data REM 309 parameters refined using 0 restraints END WGHT 0.0776 0.0000 REM Highest difference peak 0.540, deepest hole -0.465, 1-sigma level 0.086 Q1 1 0.8280 0.2154 0.0300 11.00000 0.05 0.54 Q2 1 0.8623 0.2176 0.0120 11.00000 0.05 0.39 Q3 1 0.6001 0.3196 0.0638 11.00000 0.05 0.37 Q4 1 0.5847 0.3147 -0.1295 11.00000 0.05 0.35 Q5 1 0.6067 0.1077 0.0631 11.00000 0.05 0.34 ; _shelx_res_checksum 67226 _shelx_hkl_file ; 0 0 -6 4592.42 96.9277 -2 0 0 6 4592.42 96.9277 1 0 0 -8 2319.96 57.3443 -2 0 0 8 2319.96 57.3443 1 0 0 10 464.106 29.1310 -2 0 0 -10 464.106 29.1310 1 0 0 12 8607.77 64.5224 -2 0 0 -12 8607.77 64.5224 1 0 0 14 782.594 33.3444 -2 0 0 -14 782.594 33.3444 1 0 0 -16 82.0053 29.1054 -2 0 0 16 82.0053 29.1054 1 0 0 18 8787.88 79.4258 -2 0 0 -18 8787.88 79.4258 1 0 0 20 65.1567 28.5922 -2 0 0 -20 65.1567 28.5922 1 0 0 22 1258.71 45.2605 -2 0 0 -22 1258.71 45.2605 1 0 0 24 408.389 67.0825 -2 0 0 -24 408.389 67.0825 1 0 0 26 1484.74 77.1196 -2 0 0 -26 1484.74 77.1196 1 0 0 28 2.36623 47.9372 -2 0 0 -28 2.36623 47.9372 1 0 0 30 84.9437 48.7820 -2 0 0 -30 84.9437 48.7820 1 0 0 32 146.380 75.7286 -2 0 0 -32 146.380 75.7286 1 0 1 1 17.9493 9.48728 -2 0 -1 -1 17.9493 9.48728 1 0 1 2 46.2549 22.6771 -2 0 -1 -2 46.2549 22.6771 1 0 -1 3 68.7824 13.1197 -2 0 1 -3 68.7824 13.1197 1 0 -1 -4 7.04636 14.6680 -2 0 1 4 7.04636 14.6680 1 0 -1 -5-5.83297 23.0324 -2 0 1 5-5.83297 23.0324 1 0 -1 -6 110.511 17.8056 -2 0 1 6 110.511 17.8056 1 0 -1 -7 60.5310 16.4246 -2 0 1 7 60.5310 16.4246 1 0 -1 -8 0.93682 11.2697 -2 0 1 8 0.93682 11.2697 1 0 -1 9 12.5746 10.4611 -2 0 1 -9 12.5746 10.4611 1 0 1 10 116.891 12.0772 -2 0 -1 -10 116.891 12.0772 1 0 -1 -11 34.0166 12.8197 -2 0 1 11 34.0166 12.8197 1 0 1 12 11.6994 12.8108 -2 0 -1 -12 11.6994 12.8108 1 0 1 13 523.834 19.9251 -2 0 -1 -13 523.834 19.9251 1 0 -1 -14 296.356 20.4305 -2 0 1 14 296.356 20.4305 1 0 -1 15 2.71191 15.6192 -2 0 1 -15 2.71191 15.6192 1 0 -1 16 264.822 19.0009 -2 0 1 -16 264.822 19.0009 1 0 -1 17 5.63907 17.8768 -2 0 1 -17 5.63907 17.8768 1 0 -1 -18 639.283 29.7629 -2 0 1 18 639.283 29.7629 1 0 -1 19 8.03442 18.3532 -2 0 1 -19 8.03442 18.3532 1 0 -1 20 1073.40 32.3870 -2 0 1 -20 1073.40 32.3870 1 0 -1 -21 16.5388 18.3388 -2 0 1 21 16.5388 18.3388 1 0 1 22 230.879 25.5332 -2 0 -1 -22 230.879 25.5332 1 0 -1 -23 248.757 26.2198 -2 0 1 23 248.757 26.2198 1 0 -1 -24 122.940 25.3425 -2 0 1 24 122.940 25.3425 1 0 1 25 24.4828 24.7112 -2 0 -1 -25 24.4828 24.7112 1 0 -1 -26 174.891 33.1050 -2 0 1 26 174.891 33.1050 1 0 -1 -27 56.5092 28.8177 -2 0 1 27 56.5092 28.8177 1 0 -1 28 24.3675 32.7941 -2 0 1 -28 24.3675 32.7941 1 0 -1 29 11.6814 30.8511 -2 0 1 -29 11.6814 30.8511 1 0 -1 30 26.3602 35.5176 -2 0 1 -30 26.3602 35.5176 1 0 -1 31 127.776 43.7069 -2 0 1 -31 127.776 43.7069 1 0 -1 32 161.357 60.0761 -2 0 1 -32 161.357 60.0761 1 0 -1 33 120.846 57.7896 -2 0 1 -33 120.846 57.7896 1 0 -1 34 193.879 67.4608 -2 0 1 -34 193.879 67.4608 1 0 -1 35 84.2684 61.3116 -2 0 1 -35 84.2684 61.3116 1 0 -1 36-13.6453 75.1351 -2 0 1 -36-13.6453 75.1351 1 0 -2 0 4054.14 47.8747 -2 0 2 0 4054.14 47.8747 1 0 2 1 2609.49 29.8871 -2 0 -2 -1 2609.49 29.8871 1 0 -2 2 3443.10 32.6401 -2 0 2 -2 3443.10 32.6401 1 0 -2 -3 1140.30 19.3321 -2 0 2 3 1140.30 19.3321 1 0 -2 -4 923.986 16.7904 -2 0 2 4 923.986 16.7904 1 0 -2 5 1343.31 27.7330 -2 0 2 -5 1343.31 27.7330 1 0 -2 6 4959.39 45.8483 -2 0 2 -6 4959.39 45.8483 1 0 -2 7 181.582 21.5074 -2 0 2 -7 181.582 21.5074 1 0 -2 8 7.10841 20.0082 -2 0 2 -8 7.10841 20.0082 1 0 -2 9 306.148 28.2285 -2 0 2 -9 306.148 28.2285 1 0 -2 10 8092.34 97.3833 -2 0 2 -10 8092.34 97.3833 1 0 -2 11 228.784 28.5046 -2 0 2 -11 228.784 28.5046 1 0 -2 12 3788.76 73.9307 -2 0 2 -12 3788.76 73.9307 1 0 2 13 1639.30 26.3966 -2 0 -2 -13 1639.30 26.3966 1 0 -2 14 326.994 15.3198 -2 0 2 -14 326.994 15.3198 1 0 -2 -15 622.352 20.4115 -2 0 2 15 622.352 20.4115 1 0 -2 16 180.246 16.7735 -2 0 2 -16 180.246 16.7735 1 0 2 17 51.9901 16.2017 -2 0 -2 -17 51.9901 16.2017 1 0 -2 18 1545.46 29.4389 -2 0 2 -18 1545.46 29.4389 1 0 2 19 75.8032 17.9051 -2 0 -2 -19 75.8032 17.9051 1 0 -2 20 151.659 20.4440 -2 0 2 -20 151.659 20.4440 1 0 2 21 1606.21 36.9528 -2 0 -2 -21 1606.21 36.9528 1 0 2 22 22.1753 21.2529 -2 0 -2 -22 22.1753 21.2529 1 0 2 23 2064.06 46.0218 -2 0 -2 -23 2064.06 46.0218 1 0 2 24 1074.28 39.8933 -2 0 -2 -24 1074.28 39.8933 1 0 -2 -25 12.2341 24.5214 -2 0 2 25 12.2341 24.5214 1 0 -2 -26 126.917 27.7747 -2 0 2 26 126.917 27.7747 1 0 -2 -27 26.1536 27.4479 -2 0 2 27 26.1536 27.4479 1 0 -2 -28 65.1726 50.3261 -2 0 2 28 65.1726 50.3261 1 0 -2 -29 19.2573 38.5038 -2 0 2 29 19.2573 38.5038 1 0 -2 -30 1.22814 41.0101 -2 0 2 30 1.22814 41.0101 1 0 -2 31 68.3325 45.3775 -2 0 2 -31 68.3325 45.3775 1 0 -2 32 9.65577 47.8017 -2 0 2 -32 9.65577 47.8017 1 0 -2 33-35.4899 78.3554 -2 0 2 -33-35.4899 78.3554 1 0 -2 34 217.681 68.3364 -2 0 2 -34 217.681 68.3364 1 0 -3 -1 56.8318 16.4373 -2 0 3 1 56.8318 16.4373 1 0 3 2 3.36997 15.4546 -2 0 -3 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29.2387 2 -10 0 2 331.839 29.1679 2 -10 0 0 57.5083 18.9230 2 -10 0 -2 72.5427 19.2063 2 -10 0 -4 251.262 21.4372 2 10 0 6 92.9658 19.5634 2 10 0 8 57.8704 19.6414 2 10 0 10 9.20437 34.1108 2 10 0 12 2.35696 23.7836 2 10 0 14 150.761 27.7811 2 10 0 16 583.107 75.1755 2 10 0 18 57.6504 62.8847 2 10 0 20 0.35336 52.9841 2 10 0 22 48.6284 63.6540 2 10 0 24 1.17541 64.8397 2 10 0 26 45.5634 65.6106 2 10 3 2 47.8056 16.8182 2 12 0 -28 17.3290 98.7061 2 12 0 -26 128.040 100.533 2 12 0 -24 84.4520 99.8453 2 12 0 -22-2.62248 91.3263 2 12 0 -20-7.22398 91.4174 2 12 0 -18 1.52375 85.1166 2 12 0 -16 475.729 90.9878 2 12 0 -14 173.200 82.0704 2 12 0 -12 6.16054 77.5626 2 12 0 -10 327.114 78.7058 2 12 0 -8-4.18666 71.8826 2 12 0 -6 1962.68 96.4801 2 12 0 -4 2489.33 88.5384 2 12 0 -2 652.581 58.7298 2 12 0 0 151.092 45.8842 2 12 0 2 92.8215 24.9053 2 12 0 4 246.768 29.9443 2 12 0 6 168.533 27.0458 2 12 0 8 394.894 27.8830 2 12 0 10 7.05524 18.9146 2 12 0 12 123.672 60.6504 2 12 0 14 220.914 64.4620 2 12 0 16 517.806 72.7564 2 12 0 18 100.125 65.2986 2 12 0 20 24.8900 59.2653 2 12 0 22 159.440 79.5219 2 12 0 24-44.1358 67.4445 2 12 1 4-4.57336 13.5529 2 12 2 1 22.8375 21.0366 2 13 0 -26 210.914 106.871 2 13 0 -24 55.9744 96.9259 2 13 0 -22 99.7676 92.1455 2 13 0 -20 22.3639 88.2298 2 13 0 -18-0.63946 85.4502 2 13 0 -16 14.1803 85.5576 2 13 0 -14 127.919 84.9192 2 13 0 -12 658.530 92.4576 2 13 0 -10 274.511 83.3101 2 13 0 -8 82.4509 77.1588 2 13 0 -6 475.655 80.4170 2 13 0 -4-16.8133 61.8316 2 13 0 -2 96.9419 41.6387 2 13 0 0 228.741 49.4972 2 13 0 2 619.857 43.4142 2 13 0 4 736.658 38.4498 2 13 0 6 249.248 31.1448 2 13 0 8 39.5582 23.7252 2 13 0 10 15.1048 42.2257 2 13 0 12 5.53422 63.5242 2 13 0 14 100.444 68.4897 2 13 0 16 0.16354 70.0182 2 13 0 18 77.5281 67.3923 2 13 0 20 69.9172 72.8468 2 13 0 22-19.7653 73.7529 2 13 1 4-6.16402 13.5282 2 13 2 0 115.101 28.6210 2 13 2 1 24.7272 18.0203 2 15 0 -24 201.984 105.437 2 15 0 -22-3.72970 91.1312 2 15 0 -20 5.51938 82.1742 2 15 0 -18 0.02088 79.1060 2 15 0 -16 85.5911 82.5113 2 15 0 -14 946.232 100.127 2 15 0 -12 191.275 78.9635 2 15 0 -10-8.45298 73.0997 2 15 0 -8 206.913 80.3136 2 15 0 -6 19.0515 64.6116 2 15 0 -4 95.0722 43.3837 2 15 0 -2 101.240 51.4788 2 15 0 0 62.3064 38.6545 2 15 0 2 154.116 35.5952 2 15 0 4 159.395 59.9472 2 15 0 6 2.10111 57.6173 2 15 0 8 41.6008 42.3380 2 15 0 10-6.26680 39.1776 2 15 0 12 3.36810 62.5398 2 15 0 14 138.673 70.6099 2 15 0 16 37.4852 79.5918 2 16 -1 12-3.70880 49.0219 2 16 2 -8 442.308 57.4539 2 18 0 -18 89.5510 78.8591 2 18 0 -16-56.9510 81.5964 2 18 0 -14 111.867 77.8342 2 18 0 -12 0.30054 67.5736 2 18 0 -10 81.7699 69.6754 2 18 0 -4 259.351 81.0310 2 18 0 -2-4.38365 73.4368 2 18 0 0 78.2539 65.4909 2 18 0 2 12.0880 67.3357 2 18 0 4 6.13957 57.1950 2 ; _shelx_hkl_checksum 38134 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 C1 C 0.6236(3) 0.4406(7) 0.01361(17) 0.0228(10) Uani 1 1 d . . . . . C2 C 0.6729(3) 0.6468(7) 0.09315(16) 0.0253(10) Uani 1 1 d . . . . . C3 C 0.6364(3) 0.4282(7) 0.09712(16) 0.0204(10) Uani 1 1 d . . . . . C4 C 0.7035(3) 0.7725(7) 0.13689(16) 0.0310(10) Uani 1 1 d . . . . . H4 H 0.7271 0.9210 0.1356 0.037 Uiso 1 1 calc R U . . . C5 C 0.6977(3) 0.6689(8) 0.18229(17) 0.0342(11) Uani 1 1 d . . . . . H5 H 0.7192 0.7468 0.2135 0.041 Uiso 1 1 calc R U . . . C6 C 0.6614(3) 0.4541(8) 0.18367(16) 0.0307(11) Uani 1 1 d . . . . . H6 H 0.6585 0.3907 0.2160 0.037 Uiso 1 1 calc R U . . . C7 C 0.6060(3) 0.3708(6) -0.04020(16) 0.0178(9) Uani 1 1 d . . . . . C8 C 0.5598(3) 0.1690(7) -0.05484(15) 0.0228(10) Uani 1 1 d . . . . . H8 H 0.5396 0.0786 -0.0296 0.027 Uiso 1 1 calc R U . . . C9 C 0.5423(3) 0.0955(7) -0.10473(15) 0.0219(10) Uani 1 1 d . . . . . H9 H 0.5087 -0.0408 -0.1139 0.026 Uiso 1 1 calc R U . . . C10 C 0.5746(3) 0.2244(7) -0.14126(15) 0.0244(10) Uani 1 1 d . . . . . C11 C 0.6216(3) 0.4273(7) -0.12777(16) 0.0244(10) Uani 1 1 d . . . . . H11 H 0.6431 0.5154 -0.1530 0.029 Uiso 1 1 calc R U . . . C12 C 0.6368(3) 0.4994(7) -0.07809(15) 0.0245(10) Uani 1 1 d . . . . . H12 H 0.6685 0.6381 -0.0692 0.029 Uiso 1 1 calc R U . . . C13 C 0.5125(4) -0.0308(7) -0.20808(16) 0.0359(12) Uani 1 1 d . . . . . H13A H 0.5449 -0.1593 -0.1893 0.054 Uiso 1 1 calc R U . . . H13B H 0.5095 -0.0523 -0.2448 0.054 Uiso 1 1 calc R U . . . H13C H 0.4472 -0.0179 -0.2013 0.054 Uiso 1 1 calc R U . . . C14 C 0.8828(3) -0.0573(7) 0.00793(16) 0.0210(9) Uani 1 1 d . . . . . C15 C 0.8865(3) 0.1647(7) 0.08535(15) 0.0240(10) Uani 1 1 d . . . . . C16 C 0.9264(3) -0.0497(8) 0.09164(17) 0.0258(10) Uani 1 1 d . . . . . C17 C 0.8857(3) 0.2996(8) 0.12715(15) 0.0284(10) Uani 1 1 d . . . . . H17 H 0.8584 0.4454 0.1235 0.034 Uiso 1 1 calc R U . . . C18 C 0.9263(3) 0.2147(8) 0.17452(16) 0.0317(10) Uani 1 1 d . . . . . H18 H 0.9288 0.3016 0.2046 0.038 Uiso 1 1 calc R U . . . C19 C 0.9631(3) -0.0009(8) 0.17702(18) 0.0375(12) Uani 1 1 d . . . . . H19 H 0.9890 -0.0578 0.2101 0.045 Uiso 1 1 calc R U . . . C20 C 0.8632(3) -0.1351(7) -0.04439(16) 0.0216(10) Uani 1 1 d . . . . . C21 C 0.9034(3) -0.3353(7) -0.05740(15) 0.0228(10) Uani 1 1 d . . . . . H21 H 0.9439 -0.4184 -0.0314 0.027 Uiso 1 1 calc R U . . . C22 C 0.8863(3) -0.4163(7) -0.10669(16) 0.0252(10) Uani 1 1 d . . . . . H22 H 0.9145 -0.5530 -0.1146 0.030 Uiso 1 1 calc R U . . . C23 C 0.8270(3) -0.2945(8) -0.14471(16) 0.0249(10) Uani 1 1 d . . . . . C24 C 0.7868(3) -0.0925(7) -0.13265(16) 0.0258(10) Uani 1 1 d . . . . . H24 H 0.7465 -0.0087 -0.1586 0.031 Uiso 1 1 calc R U . . . C25 C 0.8057(3) -0.0157(7) -0.08326(15) 0.0246(10) Uani 1 1 d . . . . . H25 H 0.7788 0.1228 -0.0755 0.030 Uiso 1 1 calc R U . . . C26 C 0.8395(4) -0.5675(8) -0.20821(17) 0.0379(12) Uani 1 1 d . . . . . H26A H 0.9099 -0.5647 -0.2010 0.057 Uiso 1 1 calc R U . . . H26B H 0.8162 -0.5964 -0.2447 0.057 Uiso 1 1 calc R U . . . H26C H 0.8169 -0.6863 -0.1881 0.057 Uiso 1 1 calc R U . . . N1 N 0.6086(2) 0.3174(6) 0.05099(13) 0.0236(8) Uani 1 1 d . . . . . N2 N 0.6299(3) 0.3306(6) 0.14154(13) 0.0289(9) Uani 1 1 d . . . . . N3 N 0.9245(2) -0.1732(6) 0.04762(13) 0.0239(8) Uani 1 1 d . . . . . N4 N 0.9657(3) -0.1362(6) 0.13766(14) 0.0335(10) Uani 1 1 d . . . . . O1 O 0.5651(2) 0.1696(5) -0.19173(10) 0.0309(7) Uani 1 1 d . . . . . O2 O 0.8038(2) -0.3560(5) -0.19494(10) 0.0298(7) Uani 1 1 d . . . . . S1 S 0.67055(8) 0.7093(2) 0.03003(4) 0.0279(3) Uani 1 1 d . . . . . S2 S 0.84480(8) 0.2144(2) 0.02155(4) 0.0270(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.013(2) 0.020(2) 0.035(3) -0.001(2) 0.0037(18) -0.0016(18) C2 0.019(2) 0.030(3) 0.028(2) -0.0028(19) 0.0078(18) 0.003(2) C3 0.016(2) 0.020(2) 0.026(2) -0.0022(19) 0.0050(18) 0.0006(18) C4 0.028(2) 0.026(2) 0.040(3) -0.002(2) 0.009(2) 0.000(2) C5 0.030(3) 0.042(3) 0.029(3) -0.007(2) 0.0008(19) 0.002(2) C6 0.034(3) 0.036(3) 0.024(2) 0.003(2) 0.010(2) 0.002(2) C7 0.018(2) 0.0111(19) 0.023(2) -0.0024(18) 0.0012(17) 0.0022(17) C8 0.022(2) 0.020(2) 0.027(2) 0.0063(19) 0.0073(18) 0.0006(19) C9 0.018(2) 0.023(2) 0.026(2) -0.0027(19) 0.0071(18) -0.0012(19) C10 0.020(2) 0.031(2) 0.020(2) 0.002(2) -0.0003(17) 0.006(2) C11 0.015(2) 0.027(2) 0.030(2) 0.008(2) 0.0025(19) 0.004(2) C12 0.015(2) 0.025(2) 0.031(2) 0.0020(19) -0.0007(18) -0.0013(19) C13 0.049(3) 0.031(3) 0.026(3) -0.006(2) 0.004(2) -0.006(2) C14 0.011(2) 0.025(2) 0.028(2) 0.004(2) 0.0079(17) 0.0055(18) C15 0.022(2) 0.025(3) 0.026(2) -0.0009(19) 0.0085(18) -0.007(2) C16 0.015(2) 0.036(3) 0.027(3) 0.000(2) 0.0071(18) 0.000(2) C17 0.020(2) 0.032(2) 0.033(2) 0.002(2) 0.0043(19) -0.003(2) C18 0.029(2) 0.038(3) 0.029(2) -0.005(2) 0.0091(19) 0.001(2) C19 0.039(3) 0.043(3) 0.028(3) 0.008(2) 0.000(2) 0.008(2) C20 0.013(2) 0.024(2) 0.027(2) -0.002(2) 0.0038(17) 0.0001(18) C21 0.012(2) 0.032(3) 0.025(2) 0.005(2) 0.0055(17) -0.0004(19) C22 0.022(2) 0.027(2) 0.028(3) -0.005(2) 0.0088(19) -0.001(2) C23 0.019(2) 0.032(2) 0.023(2) 0.001(2) 0.0032(17) -0.007(2) C24 0.020(2) 0.031(2) 0.027(2) 0.0049(19) 0.0046(19) 0.009(2) C25 0.022(2) 0.023(2) 0.030(2) 0.0002(19) 0.007(2) 0.003(2) C26 0.040(3) 0.042(3) 0.032(3) -0.012(2) 0.008(2) 0.004(2) N1 0.0235(19) 0.027(2) 0.0213(18) -0.0021(17) 0.0070(15) -0.0051(17) N2 0.028(2) 0.032(2) 0.027(2) 0.0041(18) 0.0062(16) -0.0037(17) N3 0.0190(18) 0.030(2) 0.023(2) 0.0004(17) 0.0051(15) 0.0002(17) N4 0.035(2) 0.037(2) 0.028(2) -0.0036(18) 0.0033(18) 0.0079(19) O1 0.0344(17) 0.0297(18) 0.0280(17) 0.0051(14) 0.0045(13) -0.0047(14) O2 0.0322(17) 0.0345(18) 0.0207(16) -0.0019(13) 0.0005(13) 0.0086(14) S1 0.0276(6) 0.0234(6) 0.0327(6) 0.0004(5) 0.0058(5) -0.0037(6) S2 0.0268(6) 0.0245(6) 0.0296(6) 0.0022(5) 0.0049(5) 0.0034(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 C1 C7 124.9(4) . . N1 C1 S1 116.0(3) . . C7 C1 S1 119.1(3) . . C4 C2 C3 119.7(4) . . C4 C2 S1 130.7(3) . . C3 C2 S1 109.6(3) . . N2 C3 N1 121.5(4) . . N2 C3 C2 123.8(4) . . N1 C3 C2 114.7(4) . . C5 C4 C2 115.8(4) . . C5 C4 H4 122.1 . . C2 C4 H4 122.1 . . C4 C5 C6 121.7(4) . . C4 C5 H5 119.2 . . C6 C5 H5 119.2 . . N2 C6 C5 123.3(4) . . N2 C6 H6 118.3 . . C5 C6 H6 118.3 . . C8 C7 C12 117.8(4) . . C8 C7 C1 120.1(4) . . C12 C7 C1 122.0(4) . . C9 C8 C7 122.3(4) . . C9 C8 H8 118.9 . . C7 C8 H8 118.9 . . C8 C9 C10 118.7(4) . . C8 C9 H9 120.7 . . C10 C9 H9 120.7 . . O1 C10 C9 125.2(4) . . O1 C10 C11 114.4(4) . . C9 C10 C11 120.4(4) . . C12 C11 C10 120.0(4) . . C12 C11 H11 120.0 . . C10 C11 H11 120.0 . . C11 C12 C7 120.8(4) . . C11 C12 H12 119.6 . . C7 C12 H12 119.6 . . O1 C13 H13A 109.5 . . O1 C13 H13B 109.5 . . H13A C13 H13B 109.5 . . O1 C13 H13C 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . N3 C14 C20 125.8(4) . . N3 C14 S2 115.3(3) . . C20 C14 S2 118.9(3) . . C17 C15 C16 120.3(4) . . C17 C15 S2 130.3(3) . . C16 C15 S2 109.4(3) . . N4 C16 N3 120.4(4) . . N4 C16 C15 123.1(4) . . N3 C16 C15 116.5(4) . . C15 C17 C18 117.4(4) . . C15 C17 H17 121.3 . . C18 C17 H17 121.3 . . C17 C18 C19 118.1(4) . . C17 C18 H18 120.9 . . C19 C18 H18 120.9 . . N4 C19 C18 126.4(4) . . N4 C19 H19 116.8 . . C18 C19 H19 116.8 . . C25 C20 C21 117.6(4) . . C25 C20 C14 122.2(4) . . C21 C20 C14 120.2(4) . . C22 C21 C20 122.2(4) . . C22 C21 H21 118.9 . . C20 C21 H21 118.9 . . C21 C22 C23 118.9(4) . . C21 C22 H22 120.6 . . C23 C22 H22 120.6 . . O2 C23 C22 124.9(4) . . O2 C23 C24 115.2(4) . . C22 C23 C24 119.9(4) . . C25 C24 C23 119.8(4) . . C25 C24 H24 120.1 . . C23 C24 H24 120.1 . . C24 C25 C20 121.6(4) . . C24 C25 H25 119.2 . . C20 C25 H25 119.2 . . O2 C26 H26A 109.5 . . O2 C26 H26B 109.5 . . H26A C26 H26B 109.5 . . O2 C26 H26C 109.5 . . H26A C26 H26C 109.5 . . H26B C26 H26C 109.5 . . C1 N1 C3 110.7(4) . . C3 N2 C6 115.6(4) . . C14 N3 C16 109.7(4) . . C19 N4 C16 114.6(4) . . C10 O1 C13 116.5(3) . . C23 O2 C26 116.8(3) . . C2 S1 C1 88.9(2) . . C15 S2 C14 89.2(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N1 1.289(5) . C1 C7 1.469(6) . C1 S1 1.758(4) . C2 C4 1.385(6) . C2 C3 1.415(6) . C2 S1 1.719(4) . C3 N2 1.340(5) . C3 N1 1.386(5) . C4 C5 1.377(6) . C4 H4 0.9500 . C5 C6 1.384(6) . C5 H5 0.9500 . C6 N2 1.346(5) . C6 H6 0.9500 . C7 C8 1.390(5) . C7 C12 1.404(5) . C8 C9 1.378(5) . C8 H8 0.9500 . C9 C10 1.388(5) . C9 H9 0.9500 . C10 O1 1.367(5) . C10 C11 1.395(6) . C11 C12 1.371(5) . C11 H11 0.9500 . C12 H12 0.9500 . C13 O1 1.432(5) . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 0.9800 . C14 N3 1.306(5) . C14 C20 1.446(5) . C14 S2 1.768(4) . C15 C17 1.377(6) . C15 C16 1.396(6) . C15 S2 1.716(4) . C16 N4 1.349(5) . C16 N3 1.383(5) . C17 C18 1.380(6) . C17 H17 0.9500 . C18 C19 1.385(6) . C18 H18 0.9500 . C19 N4 1.331(6) . C19 H19 0.9500 . C20 C25 1.386(6) . C20 C21 1.396(6) . C21 C22 1.378(5) . C21 H21 0.9500 . C22 C23 1.391(6) . C22 H22 0.9500 . C23 O2 1.367(5) . C23 C24 1.397(6) . C24 C25 1.372(5) . C24 H24 0.9500 . C25 H25 0.9500 . C26 O2 1.430(5) . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 .