#------------------------------------------------------------------------------ #$Date: 2024-12-07 04:41:06 +0200 (Sat, 07 Dec 2024) $ #$Revision: 296733 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312722.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_2312722 loop_ _publ_author_name 'Sukiennik, Jarosław' 'Olczak, Andrzej' 'Gobis, Katarzyna' 'Korona-Głowniak, Izabela' 'Suśniak, Katarzyna' 'Fruziński, Andrzej' 'Szczesio, Małgorzata' _publ_section_title ; Synthesis, structure and biological activity of new picolinohydrazonamide derivatives. ; _journal_coeditor_code WV3017 _journal_issue 1 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S2053229624011549 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C22 H29 N7 S, C3 H7 N O, 0.285H2 O' _chemical_formula_moiety 'C22 H29 N7 S, C3 H7 N O, 0.285(H2 O)' _chemical_formula_sum 'C25 H36.57 N8 O1.29 S' _chemical_formula_weight 501.81 _chemical_name_systematic '4-(4-Phenylpiperazin-1-yl)-N'-(piperidine-1-carbonothioyl)picolinohydrazonamide--dimethylformamide--water (1/1/0.285)' _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 mixed _atom_sites_solution_primary iterative _audit_creation_method ; Olex2 1.5 (compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 98.255(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.1063(3) _cell_length_b 12.8414(2) _cell_length_c 15.6327(3) _cell_measurement_reflns_used 19656 _cell_measurement_temperature 99.9(4) _cell_measurement_theta_max 78.6360 _cell_measurement_theta_min 4.4250 _cell_volume 2603.77(9) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2022) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2019 (Sheldrick, 2015b) ; _computing_structure_solution ; olex2.solve (Bourhis et al., 2015) ; _diffrn_ambient_temperature 99.9(4) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.9986 _diffrn_measured_fraction_theta_max 0.9503 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy Dualflex diffractometer with a Pilatus 300K detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_unetI/netI 0.0235 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 33084 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 78.960 _diffrn_reflns_theta_min 3.407 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.385 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.49758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2022) ; _exptl_crystal_colour 'clear orangish orange' _exptl_crystal_density_diffrn 1.280 _exptl_crystal_description plate _exptl_crystal_F_000 1075 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.261 _refine_diff_density_min -0.261 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 339 _refine_ls_number_reflns 5356 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0350 _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^)+(0.0471P)^2^+1.1183P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0964 _reflns_number_gt 4642 _reflns_number_total 5356 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ka10_auto_a.res in P2(1)/c ka10_auto.res created by SHELXL-2019/3 at 15:52:17 on 16-Apr-2024 REM Old TITL KA10_auto in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.139, Rweak 0.014, Alpha 0.025, Orientation as input REM Formula found by SHELXT: C26 N6 O2 Cl REM LIST 4 REM ##### CELL 1.54184 13.1063 12.8414 15.6327 90 98.255 90 ZERR 4 0.0003 0.0002 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 100 146.28 32 5.14 4 EQIV $1 +X,1.5-Y,0.5+Z EQIV $2 1-X,2-Y,-Z L.S. 30 PLAN 6 SIZE 0.12 0.25 0.43 TEMP -173.2(4) CONF HTAB O1W N3 HTAB O1W S1 HTAB N5 S1 HTAB N4 O1A HTAB N4 S1_$1 HTAB C12 S1_$2 HTAB C18 S1 htab LIST 4 MORE -1 BOND $H fmap -2 acta REM REM REM WGHT 0.047100 1.118300 FVAR 0.35022 0.28525 S1 5 0.748093 0.859899 -0.104603 11.00000 0.02943 0.02436 = 0.01302 0.00313 0.00508 0.00748 O1W 4 0.729838 1.058702 0.034187 21.00000 0.04480 0.03530 = 0.03649 -0.00791 0.01159 -0.00900 H1WA 2 0.670112 1.006884 0.062586 21.00000 0.09983 H1WB 2 0.750068 1.010135 -0.006491 21.00000 0.04113 O1A 4 0.891199 0.546810 0.184485 11.00000 0.04218 0.03344 = 0.02488 0.00177 0.00004 0.01461 N1 3 0.380022 0.898956 0.500994 11.00000 0.02214 0.02724 = 0.01521 0.00221 0.00647 0.00468 C1 1 0.337726 0.895512 0.579059 11.00000 0.01674 0.02980 = 0.01518 -0.00138 0.00299 -0.00256 H5 2 0.679501 0.832249 0.026385 11.00000 -1.50000 N2 3 0.451043 0.896827 0.335903 11.00000 0.02325 0.02338 = 0.01351 0.00238 0.00628 0.00460 C2 1 0.351111 0.809350 0.634135 11.00000 0.02431 0.03352 = 0.02029 0.00284 0.00714 0.00517 AFIX 43 H2 2 0.383534 0.748410 0.616512 11.00000 -1.20000 AFIX 0 N3 3 0.568149 0.911586 0.098215 11.00000 0.03227 0.03372 = 0.01513 0.00579 0.00691 0.01058 C3 1 0.317319 0.811989 0.714715 11.00000 0.02890 0.03998 = 0.02084 0.00816 0.00751 0.00493 AFIX 43 H3 2 0.328472 0.753230 0.751801 11.00000 -1.20000 AFIX 0 N4 3 0.739330 0.707948 0.190637 11.00000 0.02432 0.02374 = 0.01360 0.00194 0.00612 0.00492 AFIX 93 H4A 2 0.788172 0.669564 0.173442 11.00000 -1.20000 H4B 2 0.725273 0.702003 0.243799 11.00000 -1.20000 AFIX 0 C4 1 0.267825 0.898673 0.741637 11.00000 0.02734 0.04258 = 0.01670 -0.00037 0.00772 -0.00026 AFIX 43 H4 2 0.245498 0.900201 0.796814 11.00000 -1.20000 AFIX 0 N5 3 0.707897 0.783586 0.057181 11.00000 0.02182 0.02236 = 0.01308 0.00080 0.00423 0.00326 C5 1 0.251592 0.983200 0.686225 11.00000 0.02340 0.03086 = 0.02292 -0.00627 0.00759 -0.00241 AFIX 43 H5A 2 0.216650 1.042807 0.703350 11.00000 -1.20000 AFIX 0 N6 3 0.786476 0.726338 0.030684 11.00000 0.02294 0.02102 = 0.01509 -0.00005 0.00548 0.00313 C6 1 0.285529 0.982184 0.606180 11.00000 0.02200 0.02633 = 0.02045 -0.00114 0.00550 -0.00324 AFIX 43 H6 2 0.273277 1.040945 0.569213 11.00000 -1.20000 AFIX 0 N7 3 0.884719 0.700826 -0.076484 11.00000 0.02437 0.02229 = 0.01502 0.00170 0.00616 0.00429 C7 1 0.324852 0.955748 0.427817 11.00000 0.02301 0.03095 = 0.01829 0.00344 0.00675 0.00573 AFIX 23 H7A 2 0.292966 1.018819 0.449007 11.00000 -1.20000 H7B 2 0.268996 0.911407 0.397939 11.00000 -1.20000 AFIX 0 N8 3 0.969029 0.449154 0.297086 11.00000 0.02920 0.02786 = 0.02481 0.00343 0.00277 0.00561 C8 1 0.396662 0.987154 0.364626 11.00000 0.02729 0.02348 = 0.01776 0.00137 0.00799 0.00464 AFIX 23 H8A 2 0.356404 1.021276 0.313854 11.00000 -1.20000 H8B 2 0.447580 1.038099 0.392536 11.00000 -1.20000 AFIX 0 C9 1 0.500865 0.833137 0.407785 11.00000 0.02761 0.03134 = 0.01675 0.00648 0.00862 0.00958 AFIX 23 H9A 2 0.560477 0.871614 0.438736 11.00000 -1.20000 H9B 2 0.527099 0.768205 0.384641 11.00000 -1.20000 AFIX 0 C10 1 0.426987 0.805776 0.470914 11.00000 0.03115 0.02688 = 0.02011 0.00430 0.01059 0.00646 AFIX 23 H10A 2 0.372398 0.759074 0.442265 11.00000 -1.20000 H10B 2 0.464814 0.768180 0.520984 11.00000 -1.20000 AFIX 0 C11 1 0.492933 0.903749 0.260018 11.00000 0.02175 0.02439 = 0.01354 -0.00058 0.00439 -0.00059 C12 1 0.457106 0.976846 0.195952 11.00000 0.03317 0.03493 = 0.01999 0.00572 0.00953 0.01537 AFIX 43 H12 2 0.406553 1.026609 0.206074 11.00000 -1.20000 AFIX 0 C13 1 0.495532 0.976300 0.118054 11.00000 0.03982 0.03945 = 0.02024 0.01096 0.01096 0.02004 AFIX 43 H13 2 0.468185 1.025644 0.075581 11.00000 -1.20000 AFIX 0 C14 1 0.604476 0.843035 0.160509 11.00000 0.02006 0.02221 = 0.01368 -0.00029 0.00232 0.00016 C15 1 0.570532 0.835364 0.240205 11.00000 0.02102 0.02045 = 0.01326 0.00057 0.00273 0.00001 AFIX 43 H15 2 0.599137 0.784691 0.281025 11.00000 -1.20000 AFIX 0 C16 1 0.687018 0.774612 0.136549 11.00000 0.01963 0.01936 = 0.01278 -0.00098 0.00243 -0.00259 C17 1 0.809192 0.757411 -0.045403 11.00000 0.02143 0.01837 = 0.01387 -0.00215 0.00269 -0.00097 C18 1 0.945726 0.746220 -0.138713 11.00000 0.02823 0.03021 = 0.01769 0.00234 0.01040 0.00447 AFIX 23 H18A 2 0.903308 0.797497 -0.175406 11.00000 -1.20000 H18B 2 0.966442 0.690744 -0.176697 11.00000 -1.20000 AFIX 0 C19 1 1.041683 0.799748 -0.091770 11.00000 0.02759 0.03757 = 0.03377 0.00808 0.00906 0.00030 AFIX 23 H19A 2 1.020869 0.860523 -0.059349 11.00000 -1.20000 H19B 2 1.084542 0.825333 -0.134615 11.00000 -1.20000 AFIX 0 C20 1 1.104999 0.724897 -0.029252 11.00000 0.02506 0.04497 = 0.03929 0.00633 0.00209 0.00494 AFIX 23 H20A 2 1.135905 0.670685 -0.062543 11.00000 -1.20000 H20B 2 1.161812 0.763591 0.005483 11.00000 -1.20000 AFIX 0 C21 1 1.038593 0.673246 0.030888 11.00000 0.03203 0.03151 = 0.02357 0.00232 0.00071 0.00905 AFIX 23 H21A 2 1.079464 0.619445 0.065932 11.00000 -1.20000 H21B 2 1.016790 0.725933 0.070809 11.00000 -1.20000 AFIX 0 C22 1 0.944235 0.623482 -0.020350 11.00000 0.02961 0.02136 = 0.02092 0.00157 0.00705 0.00769 AFIX 23 H22A 2 0.965867 0.566230 -0.056173 11.00000 -1.20000 H22B 2 0.900250 0.593476 0.019865 11.00000 -1.20000 AFIX 0 C23 1 0.967286 0.520749 0.234984 11.00000 0.03663 0.02518 = 0.02100 -0.00177 0.00555 0.00740 AFIX 43 H23 2 1.030522 0.554458 0.229425 11.00000 -1.20000 AFIX 0 C24 1 1.063738 0.421981 0.353136 11.00000 0.03444 0.03540 = 0.02895 0.00655 -0.00038 0.00372 AFIX 137 H24A 2 1.054698 0.433529 0.413559 11.00000 -1.50000 H24B 2 1.120288 0.465589 0.338843 11.00000 -1.50000 H24C 2 1.080003 0.348526 0.344748 11.00000 -1.50000 AFIX 0 C25 1 0.875544 0.394711 0.309891 11.00000 0.03498 0.04440 = 0.05043 0.01481 0.00571 0.00121 AFIX 137 H25A 2 0.883424 0.320253 0.298750 11.00000 -1.50000 H25B 2 0.817343 0.422409 0.270016 11.00000 -1.50000 H25C 2 0.862651 0.404660 0.369566 11.00000 -1.50000 AFIX 0 HKLF 4 REM ka10_auto_a.res in P2(1)/c REM wR2 = 0.0964, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0350 for 4642 Fo > 4sig(Fo) and 0.0417 for all 5356 data REM 339 parameters refined using 0 restraints END WGHT 0.0471 1.1183 REM Instructions for potential hydrogen bonds HTAB O1W N3 HTAB O1W S1 HTAB N5 S1 HTAB N4 O1A HTAB N4 S1_$1 HTAB C12 S1_$2 HTAB C18 S1 REM Highest difference peak 0.261, deepest hole -0.261, 1-sigma level 0.044 Q1 1 0.7248 0.8237 -0.1068 11.00000 0.05 -0.26 Q2 1 0.4615 0.8285 0.4359 11.00000 0.05 0.26 Q3 1 0.7809 0.8577 -0.0736 11.00000 0.05 -0.26 Q4 1 0.7808 0.8350 -0.1011 11.00000 0.05 -0.23 Q5 1 0.6406 0.8053 0.1462 11.00000 0.05 0.23 Q6 1 0.3572 0.9741 0.3981 11.00000 0.05 0.22 REM The information below was added by Olex2. REM REM R1 = 0.0350 for 4642 Fo > 4sig(Fo) and 0.0417 for all 34083 data REM 339 parameters refined using n/a restraints REM Highest difference peak 0.26, deepest hole -0.26 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0417 REM R1_gt = 0.0350 REM wR_ref = 0.0964 REM GOOF = 1.050 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 34083 REM Reflections_gt = 4642 REM Parameters = 339 REM Hole = -0.26 REM Peak = 0.26 REM Flack = n/a ; _cod_data_source_file wv3017sup1.cif _cod_data_source_block 2 _cod_database_code 2312722 _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 0.587 _shelx_estimated_absorpt_t_max 0.851 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_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 0.74809(3) 0.85990(3) -0.10460(2) 0.02207(10) Uani d 1 . . O O1W 0.7298(4) 1.0587(3) 0.0342(3) 0.0383(16) Uani d 0.285(5) . . H H1WA 0.670(8) 1.007(9) 0.063(7) 0.10(3) Uiso d 0.285(5) . . H H1WB 0.750(5) 1.010(6) -0.006(5) 0.041(19) Uiso d 0.285(5) . . O O1A 0.89120(9) 0.54681(9) 0.18448(7) 0.0340(3) Uani d 1 . . N N1 0.38002(9) 0.89896(9) 0.50099(7) 0.0212(2) Uani d 1 . . C C1 0.33773(10) 0.89551(11) 0.57906(8) 0.0205(3) Uani d 1 . . H H5 0.6795(14) 0.8322(15) 0.0264(12) 0.031 Uiso d 1 . . N N2 0.45104(9) 0.89683(9) 0.33590(7) 0.0197(2) Uani d 1 . . C C2 0.35111(11) 0.80935(12) 0.63413(9) 0.0257(3) Uani d 1 . . H H2 0.383534 0.748410 0.616512 0.031 Uiso calc 1 . . N N3 0.56815(10) 0.91159(10) 0.09821(7) 0.0267(3) Uani d 1 . . C C3 0.31732(12) 0.81199(13) 0.71471(9) 0.0295(3) Uani d 1 . . H H3 0.328472 0.753230 0.751801 0.035 Uiso calc 1 . . N N4 0.73933(9) 0.70795(9) 0.19064(7) 0.0202(2) Uani d 1 . . H H4A 0.788172 0.669564 0.173442 0.024 Uiso calc 1 . . H H4B 0.725273 0.702003 0.243799 0.024 Uiso calc 1 . . C C4 0.26782(12) 0.89867(13) 0.74164(9) 0.0284(3) Uani d 1 . . H H4 0.245498 0.900201 0.796814 0.034 Uiso calc 1 . . N N5 0.70790(9) 0.78359(9) 0.05718(7) 0.0189(2) Uani d 1 . . C C5 0.25159(11) 0.98320(12) 0.68623(9) 0.0253(3) Uani d 1 . . H H5A 0.216650 1.042807 0.703350 0.030 Uiso calc 1 . . N N6 0.78648(9) 0.72634(9) 0.03068(7) 0.0194(2) Uani d 1 . . C C6 0.28553(11) 0.98218(11) 0.60618(9) 0.0227(3) Uani d 1 . . H H6 0.273277 1.040945 0.569213 0.027 Uiso calc 1 . . N N7 0.88472(9) 0.70083(9) -0.07648(7) 0.0202(2) Uani d 1 . . C C7 0.32485(11) 0.95575(12) 0.42782(9) 0.0237(3) Uani d 1 . . H H7A 0.292966 1.018819 0.449007 0.028 Uiso calc 1 . . H H7B 0.268996 0.911407 0.397939 0.028 Uiso calc 1 . . N N8 0.96903(10) 0.44915(10) 0.29709(8) 0.0274(3) Uani d 1 . . C C8 0.39666(11) 0.98715(11) 0.36463(9) 0.0224(3) Uani d 1 . . H H8A 0.356404 1.021276 0.313854 0.027 Uiso calc 1 . . H H8B 0.447580 1.038099 0.392536 0.027 Uiso calc 1 . . C C9 0.50086(12) 0.83314(12) 0.40779(9) 0.0247(3) Uani d 1 . . H H9A 0.560477 0.871614 0.438736 0.030 Uiso calc 1 . . H H9B 0.527099 0.768205 0.384641 0.030 Uiso calc 1 . . C C10 0.42699(12) 0.80578(12) 0.47091(9) 0.0254(3) Uani d 1 . . H H10A 0.372398 0.759074 0.442265 0.030 Uiso calc 1 . . H H10B 0.464814 0.768180 0.520984 0.030 Uiso calc 1 . . C C11 0.49293(11) 0.90375(11) 0.26002(8) 0.0197(3) Uani d 1 . . C C12 0.45711(12) 0.97685(12) 0.19595(9) 0.0288(3) Uani d 1 . . H H12 0.406553 1.026609 0.206074 0.035 Uiso calc 1 . . C C13 0.49553(13) 0.97630(13) 0.11805(10) 0.0325(4) Uani d 1 . . H H13 0.468185 1.025644 0.075581 0.039 Uiso calc 1 . . C C14 0.60448(10) 0.84303(11) 0.16051(8) 0.0187(3) Uani d 1 . . C C15 0.57053(10) 0.83536(10) 0.24021(8) 0.0182(3) Uani d 1 . . H H15 0.599137 0.784691 0.281025 0.022 Uiso calc 1 . . C C16 0.68702(10) 0.77461(10) 0.13655(8) 0.0172(3) Uani d 1 . . C C17 0.80919(10) 0.75741(10) -0.04540(8) 0.0179(3) Uani d 1 . . C C18 0.94573(11) 0.74622(12) -0.13871(9) 0.0247(3) Uani d 1 . . H H18A 0.903308 0.797497 -0.175406 0.030 Uiso calc 1 . . H H18B 0.966442 0.690744 -0.176697 0.030 Uiso calc 1 . . C C19 1.04168(12) 0.79975(13) -0.09177(11) 0.0325(4) Uani d 1 . . H H19A 1.020869 0.860523 -0.059349 0.039 Uiso calc 1 . . H H19B 1.084542 0.825333 -0.134615 0.039 Uiso calc 1 . . C C20 1.10500(13) 0.72490(15) -0.02925(11) 0.0367(4) Uani d 1 . . H H20A 1.135905 0.670685 -0.062543 0.044 Uiso calc 1 . . H H20B 1.161812 0.763591 0.005483 0.044 Uiso calc 1 . . C C21 1.03859(12) 0.67325(13) 0.03089(10) 0.0294(3) Uani d 1 . . H H21A 1.079464 0.619445 0.065932 0.035 Uiso calc 1 . . H H21B 1.016790 0.725933 0.070809 0.035 Uiso calc 1 . . C C22 0.94424(11) 0.62348(11) -0.02035(9) 0.0236(3) Uani d 1 . . H H22A 0.965867 0.566230 -0.056173 0.028 Uiso calc 1 . . H H22B 0.900250 0.593476 0.019865 0.028 Uiso calc 1 . . C C23 0.96729(13) 0.52075(12) 0.23498(9) 0.0275(3) Uani d 1 . . H H23 1.030522 0.554458 0.229425 0.033 Uiso calc 1 . . C C24 1.06374(13) 0.42198(14) 0.35314(10) 0.0334(4) Uani d 1 . . H H24A 1.054698 0.433529 0.413559 0.050 Uiso calc 1 . . H H24B 1.120288 0.465589 0.338843 0.050 Uiso calc 1 . . H H24C 1.080003 0.348526 0.344748 0.050 Uiso calc 1 . . C C25 0.87554(14) 0.39471(15) 0.30989(13) 0.0433(4) Uani d 1 . . H H25A 0.883424 0.320253 0.298750 0.065 Uiso calc 1 . . H H25B 0.817343 0.422409 0.270016 0.065 Uiso calc 1 . . H H25C 0.862651 0.404660 0.369566 0.065 Uiso calc 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 0.02943(19) 0.02436(18) 0.01302(15) 0.00748(13) 0.00508(13) 0.00313(12) O1W 0.045(3) 0.035(3) 0.036(3) -0.0090(19) 0.0116(19) -0.0079(18) O1A 0.0422(7) 0.0334(6) 0.0249(5) 0.0146(5) 0.0000(5) 0.0018(4) N1 0.0221(6) 0.0272(6) 0.0152(5) 0.0047(5) 0.0065(4) 0.0022(4) C1 0.0167(6) 0.0298(7) 0.0152(6) -0.0026(5) 0.0030(5) -0.0014(5) N2 0.0232(6) 0.0234(6) 0.0135(5) 0.0046(5) 0.0063(4) 0.0024(4) C2 0.0243(7) 0.0335(8) 0.0203(7) 0.0052(6) 0.0071(6) 0.0028(6) N3 0.0323(7) 0.0337(7) 0.0151(5) 0.0106(5) 0.0069(5) 0.0058(5) C3 0.0289(8) 0.0400(9) 0.0208(7) 0.0049(7) 0.0075(6) 0.0082(6) N4 0.0243(6) 0.0237(6) 0.0136(5) 0.0049(5) 0.0061(4) 0.0019(4) C4 0.0273(8) 0.0426(9) 0.0167(6) -0.0003(7) 0.0077(6) -0.0004(6) N5 0.0218(6) 0.0224(6) 0.0131(5) 0.0033(5) 0.0042(4) 0.0008(4) C5 0.0234(7) 0.0309(8) 0.0229(7) -0.0024(6) 0.0076(6) -0.0063(6) N6 0.0229(6) 0.0210(6) 0.0151(5) 0.0031(4) 0.0055(4) -0.0001(4) C6 0.0220(7) 0.0263(7) 0.0204(7) -0.0032(6) 0.0055(5) -0.0011(5) N7 0.0244(6) 0.0223(6) 0.0150(5) 0.0043(5) 0.0062(4) 0.0017(4) C7 0.0230(7) 0.0310(8) 0.0183(6) 0.0057(6) 0.0067(5) 0.0034(6) N8 0.0292(7) 0.0279(6) 0.0248(6) 0.0056(5) 0.0028(5) 0.0034(5) C8 0.0273(7) 0.0235(7) 0.0178(6) 0.0046(6) 0.0080(6) 0.0014(5) C9 0.0276(7) 0.0313(8) 0.0167(6) 0.0096(6) 0.0086(6) 0.0065(6) C10 0.0312(8) 0.0269(7) 0.0201(7) 0.0065(6) 0.0106(6) 0.0043(6) C11 0.0218(7) 0.0244(7) 0.0135(6) -0.0006(5) 0.0044(5) -0.0006(5) C12 0.0332(8) 0.0349(8) 0.0200(7) 0.0154(6) 0.0095(6) 0.0057(6) C13 0.0398(9) 0.0394(9) 0.0202(7) 0.0200(7) 0.0110(6) 0.0110(6) C14 0.0201(6) 0.0222(7) 0.0137(6) 0.0002(5) 0.0023(5) -0.0003(5) C15 0.0210(6) 0.0204(6) 0.0133(6) 0.0000(5) 0.0027(5) 0.0006(5) C16 0.0196(6) 0.0194(6) 0.0128(6) -0.0026(5) 0.0024(5) -0.0010(5) C17 0.0214(7) 0.0184(6) 0.0139(6) -0.0010(5) 0.0027(5) -0.0021(5) C18 0.0282(7) 0.0302(8) 0.0177(6) 0.0045(6) 0.0104(6) 0.0023(6) C19 0.0276(8) 0.0376(9) 0.0338(8) 0.0003(7) 0.0091(7) 0.0081(7) C20 0.0251(8) 0.0450(10) 0.0393(9) 0.0049(7) 0.0021(7) 0.0063(8) C21 0.0320(8) 0.0315(8) 0.0236(7) 0.0091(6) 0.0007(6) 0.0023(6) C22 0.0296(7) 0.0214(7) 0.0209(6) 0.0077(6) 0.0071(6) 0.0016(5) C23 0.0366(8) 0.0252(7) 0.0210(7) 0.0074(6) 0.0055(6) -0.0018(6) C24 0.0344(9) 0.0354(9) 0.0289(8) 0.0037(7) -0.0004(7) 0.0065(7) C25 0.0350(9) 0.0444(10) 0.0504(11) 0.0012(8) 0.0057(8) 0.0148(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 0 -2 0 0 -2 0 0 3 0 0 3 0 0 3 0 0 3 0 0 -3 0 0 3 0 0 -3 0 0 4 0 0 -4 0 0 -4 0 0 5 0 0 5 0 0 5 0 0 -5 0 0 -5 0 0 6 0 0 6 0 0 6 0 0 -6 0 0 -6 0 0 -6 0 0 7 0 0 -7 0 0 7 0 0 -7 0 0 -7 0 0 -8 0 0 -8 0 0 -8 0 0 -9 0 0 -9 0 0 -9 0 0 10 0 0 10 0 0 -10 0 0 -10 0 0 -11 0 0 -11 0 0 11 0 0 11 0 0 11 0 0 -11 0 0 -12 0 0 -12 0 0 12 0 0 12 0 0 12 0 0 -12 0 0 -13 0 0 13 0 0 -13 0 0 13 0 0 -13 0 0 -14 0 0 14 0 0 -14 0 0 -14 0 0 -15 0 0 15 0 0 -15 0 0 16 0 0 17 0 0 18 0 0 18 0 0 19 0 -1 0 0 -1 0 0 -1 0 0 -1 1 0 -1 1 0 -1 -1 0 -1 -1 0 -1 -1 0 -1 2 0 -1 2 0 1 -2 0 -1 -2 0 -1 -2 0 -1 3 0 -1 3 0 -1 -3 0 1 -3 0 -1 -3 0 1 -3 0 1 3 0 -1 -3 0 -1 4 0 -1 4 0 -1 -4 0 -1 -4 0 1 -4 0 -1 -4 0 1 -4 0 1 5 0 1 5 0 1 5 0 1 5 0 1 -5 0 -1 -5 0 -1 -5 0 1 5 0 1 6 0 1 -6 0 -1 -6 0 1 6 0 -1 6 0 1 6 0 -1 6 0 1 -6 0 -1 -6 0 -1 -6 0 1 -6 0 -1 7 0 1 -7 0 1 -7 0 -1 -7 0 -1 -7 0 -1 -7 0 1 -7 0 1 -8 0 -1 8 0 1 -8 0 1 -8 0 -1 -8 0 -1 -8 0 1 8 0 -1 9 0 1 9 0 1 -9 0 -1 -9 0 1 -9 0 -1 -9 0 -1 -10 0 -1 10 0 -1 10 0 -1 -10 0 -1 -10 0 1 -10 0 -1 -11 0 1 -11 0 -1 -11 0 1 11 0 -1 11 0 -1 11 0 -1 11 0 1 11 0 -1 -11 0 1 -11 0 1 -12 0 -1 -12 0 -1 12 0 1 12 0 -1 12 0 -1 -12 0 -1 12 0 1 12 0 -1 -12 0 -1 -12 0 1 -12 0 -1 -13 0 1 -13 0 1 13 0 -1 13 0 -1 -13 0 -1 13 0 1 13 0 -1 13 0 -1 -13 0 -1 -13 0 1 -13 0 1 -14 0 -1 -14 0 1 14 0 -1 14 0 -1 -14 0 1 14 0 -1 14 0 -1 -14 0 1 -14 0 1 -15 0 1 -15 0 1 15 0 -1 15 0 -1 16 0 1 16 0 1 17 0 -1 17 0 -1 18 0 -1 18 0 -1 19 0 1 19 0 1 19 0 -1 19 0 -2 0 0 -2 0 0 -2 0 0 -2 -1 0 -2 1 0 -2 -1 0 -2 -1 0 -2 1 0 -2 1 0 -2 1 0 -2 2 0 -2 2 0 -2 -2 0 -2 -2 0 -2 2 0 -2 -2 0 -2 -3 0 -2 -3 0 -2 3 0 -2 3 0 -2 -3 0 2 4 0 -2 -4 0 -2 -4 0 2 4 0 -2 4 0 -2 4 0 -2 -4 0 -2 -4 0 2 5 0 -2 -5 0 2 5 0 -2 5 0 -2 5 0 -2 -5 0 2 -5 0 -2 -5 0 2 -5 0 -2 -5 0 2 6 0 -2 -6 0 2 6 0 2 6 0 2 6 0 2 -6 0 2 -6 0 -2 -6 0 -2 -6 0 -2 -6 0 2 7 0 -2 7 0 2 7 0 2 -7 0 -2 -7 0 -2 7 0 2 -7 0 -2 -7 0 2 -7 0 -2 -7 0 2 -7 0 2 8 0 -2 8 0 2 -8 0 -2 -8 0 2 8 0 2 -8 0 -2 -8 0 -2 -8 0 -2 -8 0 2 -9 0 -2 -9 0 -2 9 0 2 9 0 2 -9 0 -2 -9 0 2 10 0 2 -10 0 -2 -10 0 -2 10 0 -2 -10 0 2 10 0 -2 10 0 -2 10 0 -2 -10 0 2 11 0 -2 -11 0 2 11 0 -2 11 0 -2 11 0 -2 -11 0 2 11 0 -2 11 0 -2 -11 0 -2 -11 0 2 -11 0 -2 -11 0 -2 -12 0 2 12 0 -2 12 0 -2 12 0 -2 -12 0 2 12 0 -2 12 0 -2 -12 0 -2 -12 0 2 -12 0 -2 -13 0 2 -13 0 2 -13 0 2 13 0 -2 13 0 -2 -13 0 -2 13 0 2 13 0 -2 13 0 -2 -13 0 2 -14 0 2 14 0 -2 14 0 -2 14 0 2 14 0 -2 15 0 2 15 0 -2 -15 0 2 15 0 -2 15 0 -2 15 0 -2 15 0 2 16 0 -2 16 0 -2 16 0 2 17 0 2 17 0 2 17 0 -2 17 0 2 18 0 -2 18 0 -2 18 0 -2 19 0 2 19 0 -3 0 0 -3 0 0 -3 -1 0 -3 1 0 -3 1 0 -3 1 0 -3 1 0 -3 -1 0 -3 -2 0 -3 2 0 -3 2 0 -3 -2 0 -3 2 0 -3 -3 0 -3 3 0 -3 3 0 -3 -3 0 -3 -3 0 3 3 0 3 4 0 -3 -4 0 -3 4 0 -3 4 0 -3 -4 0 -3 -4 0 3 4 0 -3 -5 0 -3 5 0 -3 -5 0 -3 -5 0 -3 -5 0 3 5 0 -3 -6 0 3 6 0 3 6 0 3 6 0 3 -6 0 -3 -6 0 -3 -6 0 -3 -6 0 3 -7 0 3 7 0 -3 -7 0 3 7 0 -3 -7 0 3 7 0 -3 7 0 3 -7 0 -3 -7 0 -3 -7 0 -3 -8 0 3 -8 0 3 8 0 -3 -8 0 3 8 0 -3 -8 0 -3 -8 0 -3 -9 0 -3 -9 0 3 -9 0 3 9 0 -3 -9 0 3 10 0 3 -10 0 -3 10 0 -3 -10 0 3 10 0 3 -10 0 -3 -10 0 -3 -10 0 -3 -11 0 -3 11 0 3 11 0 -3 11 0 3 -11 0 -3 -11 0 3 -12 0 -3 -12 0 -3 -12 0 -3 -12 0 -3 12 0 3 12 0 -3 12 0 -3 -12 0 -3 12 0 -3 -12 0 -3 -13 0 3 -13 0 -3 13 0 3 -13 0 -3 13 0 3 13 0 -3 13 0 -3 13 0 -3 -13 0 -3 14 0 -3 -14 0 3 -14 0 3 -14 0 -3 14 0 3 14 0 -3 14 0 -3 -14 0 3 15 0 -3 15 0 3 15 0 3 16 0 -3 16 0 -3 16 0 3 17 0 3 17 0 -3 17 0 3 17 0 3 18 0 3 18 0 -3 18 0 -3 19 0 3 19 0 4 0 0 -4 0 0 -4 0 0 4 1 0 -4 1 0 -4 -1 0 -4 -1 0 4 2 0 -4 2 0 -4 -2 0 -4 2 0 4 3 0 -4 -3 0 -4 3 0 -4 -3 0 4 4 0 -4 4 0 -4 -4 0 -4 -4 0 -4 -4 0 4 5 0 -4 -5 0 -4 5 0 -4 -5 0 -4 -5 0 -4 -5 0 4 6 0 4 6 0 -4 6 0 -4 -6 0 -4 6 0 -4 -6 0 -4 -6 0 -4 -6 0 4 7 0 4 7 0 4 -7 0 -4 7 0 -4 -7 0 4 7 0 -4 -7 0 -4 -7 0 -4 -7 0 4 8 0 4 -8 0 4 8 0 -4 8 0 -4 8 0 -4 -8 0 -4 -8 0 -4 -8 0 4 8 0 4 9 0 4 9 0 4 -9 0 -4 9 0 -4 9 0 -4 -9 0 -4 9 0 4 9 0 -4 -9 0 -4 9 0 4 10 0 4 -10 0 -4 -10 0 -4 10 0 -4 10 0 -4 -10 0 -4 10 0 -4 -10 0 -4 10 0 -4 10 0 4 10 0 -4 -10 0 -4 -10 0 4 -10 0 4 11 0 -4 -11 0 -4 11 0 -4 11 0 -4 11 0 -4 -11 0 -4 11 0 4 11 0 -4 11 0 -4 -11 0 4 -11 0 -4 -11 0 4 12 0 -4 -12 0 -4 12 0 -4 12 0 4 12 0 -4 12 0 4 12 0 4 -12 0 -4 -12 0 -4 -12 0 4 -13 0 -4 13 0 -4 -13 0 4 -13 0 -4 -13 0 -4 13 0 4 13 0 -4 13 0 4 13 0 -4 -13 0 4 -14 0 -4 14 0 4 14 0 -4 -14 0 -4 -14 0 4 -14 0 -4 15 0 -4 15 0 4 15 0 -4 -15 0 4 16 0 -4 16 0 4 16 0 -4 16 0 4 16 0 -4 16 0 -4 17 0 -4 17 0 4 17 0 -4 18 0 4 18 0 -4 19 0 -5 0 0 5 0 0 -5 -1 0 -5 1 0 -5 1 0 -5 -1 0 5 1 0 -5 -2 0 -5 2 0 -5 -2 0 -5 -2 0 5 2 0 -5 -3 0 -5 -3 0 -5 -3 0 5 3 0 -5 -4 0 -5 -4 0 5 4 0 -5 -4 0 -5 -4 0 5 5 0 -5 -5 0 5 5 0 -5 -5 0 -5 -5 0 -5 -5 0 -5 -6 0 -5 -6 0 5 6 0 -5 -6 0 -5 -6 0 -5 -7 0 5 7 0 5 -7 0 -5 7 0 -5 -7 0 5 7 0 -5 -7 0 -5 -7 0 5 8 0 5 8 0 5 8 0 -5 -8 0 5 -8 0 -5 8 0 -5 -8 0 -5 8 0 5 8 0 -5 -8 0 -5 -8 0 5 9 0 5 9 0 5 -9 0 -5 -9 0 -5 -9 0 -5 9 0 5 9 0 -5 9 0 -5 -9 0 -5 -10 0 5 10 0 5 -10 0 -5 -10 0 -5 10 0 -5 -10 0 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-2 -13 6 -2 -13 -6 -2 -13 -6 -3 -13 -6 -3 -13 -6 -3 -13 6 -3 -13 -6 -4 -13 -6 -5 -13 -6 -5 13 -6 7 -13 -7 10 -13 -7 9 13 -7 -8 -13 -7 8 13 -7 -7 -13 -7 7 13 -7 -6 -13 -7 6 -13 -7 6 13 -7 -5 -13 -7 5 -13 -7 5 13 -7 -4 -13 -7 4 -13 -7 4 -13 -7 4 -13 -7 3 -13 -7 3 -13 -7 3 13 -7 -3 -13 -7 2 -13 -7 2 -13 -7 1 -13 -7 1 -13 7 1 -13 -7 0 -13 7 0 -13 -7 -1 -13 7 -1 -13 -7 -1 -13 -7 -2 -13 -7 -2 -13 -7 -2 -13 -7 -3 -13 -7 -4 -13 -7 -4 13 -7 5 13 -7 6 -13 -8 9 -13 -8 7 13 -8 -7 -13 -8 6 -13 -8 6 13 -8 -6 -13 -8 5 -13 -8 5 13 -8 -5 -13 -8 4 -13 -8 4 13 -8 -4 -13 -8 3 -13 -8 3 -13 -8 2 -13 -8 2 -13 -8 1 -13 -8 1 -13 -8 0 -13 -8 -1 -13 -8 -1 -13 -8 -2 -13 -8 -3 -13 -8 -4 13 -8 4 -13 -9 7 -13 -9 6 -13 -9 6 -13 -9 5 -13 -9 5 -13 -9 4 -13 -9 4 -13 -9 3 -13 -9 3 -13 -9 2 -13 -9 2 -13 -9 2 -13 -9 1 -13 -9 1 -13 -9 1 -13 -9 0 -13 -9 0 -13 -9 -1 -13 -9 -2 -13 -9 -3 -13 -10 4 -13 -10 4 -13 -10 3 -13 -10 3 -13 -10 2 -13 -10 2 -13 -10 1 -13 -10 0 -14 0 10 -14 0 9 -14 0 8 -14 0 7 -14 0 6 14 0 -6 14 0 -5 14 0 -4 -14 0 4 14 0 -3 -14 0 3 14 0 -2 -14 0 2 14 0 -1 -14 0 1 14 0 0 -14 0 0 14 0 1 -14 0 -1 14 0 2 -14 0 -2 14 0 3 -14 0 -3 14 0 4 -14 0 -4 14 0 5 -14 0 -5 14 0 6 -14 0 -6 14 0 7 14 0 8 -14 1 10 -14 -1 10 14 1 -10 -14 1 9 -14 -1 9 14 1 -9 -14 -1 8 -14 1 8 14 -1 -8 -14 -1 7 -14 1 7 14 -1 -7 -14 -1 6 -14 1 6 14 -1 -6 14 -1 -5 -14 1 5 -14 -1 5 -14 -1 4 14 -1 -4 -14 1 4 14 -1 -3 -14 1 3 14 -1 -2 14 1 -2 -14 1 2 14 1 -1 14 -1 -1 -14 1 1 14 1 0 14 -1 0 -14 -1 0 -14 1 0 14 -1 1 -14 -1 -1 -14 1 -1 14 1 1 -14 -1 -2 -14 1 -2 14 1 2 14 -1 2 -14 -1 -3 -14 1 -3 14 -1 3 14 1 3 14 1 4 14 -1 4 -14 -1 -5 -14 1 -5 14 1 5 14 -1 5 -14 1 -6 14 1 6 14 -1 6 14 -1 7 14 1 7 14 -2 -11 -14 -2 10 14 -2 -10 -14 2 10 -14 -2 9 -14 2 9 14 -2 -9 -14 2 8 14 2 -8 14 -2 -8 -14 -2 7 -14 2 7 14 2 -7 14 -2 -7 -14 -2 6 -14 2 6 14 2 -6 14 -2 -6 14 -2 -5 -14 2 5 -14 2 4 14 -2 -4 -14 2 3 14 -2 -3 -14 -2 2 -14 2 2 14 -2 -2 -14 2 1 14 -2 -1 -14 2 0 14 -2 0 -14 2 -1 14 -2 1 -14 2 -2 14 -2 2 14 2 2 -14 2 -3 14 2 3 14 -2 3 -14 2 -4 14 2 4 14 -2 4 -14 2 -5 14 2 5 14 -2 5 14 2 6 14 -2 6 14 2 7 14 -3 -12 14 -3 -11 -14 -3 10 14 -3 -10 -14 -3 9 -14 3 9 14 -3 -9 14 -3 -8 -14 -3 8 -14 3 8 14 -3 -7 -14 -3 7 -14 3 7 -14 3 6 14 -3 -6 14 3 -6 -14 3 5 14 -3 -5 14 3 -5 -14 3 5 -14 3 4 14 3 -4 14 -3 -4 -14 -3 3 -14 3 3 14 -3 -3 14 3 -3 -14 3 2 -14 -3 2 14 -3 -2 -14 -3 1 14 -3 -1 -14 3 1 14 -3 0 -14 3 0 14 -3 1 -14 3 -1 14 -3 2 -14 3 -2 14 -3 3 -14 3 -3 14 -3 4 -14 3 -4 -14 -3 -5 -14 3 -5 14 -3 7 14 -4 -11 -14 -4 10 14 -4 -10 -14 -4 9 14 -4 -9 -14 -4 8 14 -4 -8 -14 -4 7 14 -4 -7 14 -4 -6 -14 -4 6 14 -4 -5 -14 -4 4 -14 4 4 14 -4 -4 -14 -4 3 14 -4 -3 14 4 -3 -14 4 3 -14 -4 2 -14 4 2 14 -4 -2 14 4 -2 -14 -4 1 14 -4 -1 -14 4 1 14 4 -1 -14 -4 0 14 -4 0 14 4 0 -14 4 0 -14 -4 -1 14 -4 1 14 4 1 -14 4 -1 -14 -4 -2 -14 -4 -2 -14 4 -2 -14 -4 -3 -14 -4 -4 -14 -4 -6 14 -5 -11 14 -5 -10 -14 -5 9 14 -5 -9 -14 -5 8 -14 -5 8 14 -5 -8 -14 -5 7 14 -5 -7 -14 -5 6 14 -5 -6 -14 -5 5 -14 5 5 14 -5 -5 14 -5 -4 -14 -5 4 -14 5 4 -14 5 3 -14 -5 3 -14 5 3 14 -5 -3 -14 5 2 -14 -5 2 -14 5 2 -14 -5 1 -14 5 1 -14 -5 0 -14 -5 -1 -14 -5 -1 -14 -5 -2 -14 -5 -2 -14 -5 -3 -14 -5 -4 14 -5 6 14 -6 -9 -14 -6 8 -14 -6 8 -14 -6 7 -14 -6 7 14 -6 -7 -14 -6 6 -14 -6 6 -14 -6 5 -14 -6 5 -14 -6 5 -14 -6 4 -14 -6 4 -14 -6 3 -14 -6 3 -14 -6 2 -14 -6 2 -14 -6 1 -14 -6 1 -14 6 0 -14 -6 0 -14 -6 -1 -14 -6 -1 -14 -6 -2 -14 -6 -3 14 -6 5 -14 -7 7 -14 -7 6 -14 -7 5 -14 -7 5 -14 -7 4 -14 -7 4 -14 -7 3 -14 -7 3 -14 -7 2 -14 -7 2 -14 -7 1 -14 -7 1 -14 -7 0 -14 -7 0 -14 -7 -1 -14 -7 -1 -14 -7 -2 -14 -7 -4 14 -7 4 -14 -8 6 -14 -8 5 -14 -8 5 -14 -8 4 -14 -8 4 -14 -8 3 -14 -8 3 -14 -8 2 -14 -8 2 -14 -8 1 -14 -8 1 -14 -8 0 -14 -8 0 -14 -8 -1 -14 -8 -1 -14 -8 -2 -15 0 8 -15 0 7 -15 0 6 -15 0 5 15 0 -4 15 0 -3 15 0 -2 15 0 -1 -15 0 1 15 0 0 -15 0 0 15 0 1 -15 0 -1 15 0 2 -15 0 -2 15 0 3 15 0 4 15 0 5 15 0 6 -15 1 8 15 1 -8 -15 -1 7 -15 1 7 15 -1 -7 -15 -1 6 -15 1 6 15 -1 -6 -15 -1 5 -15 1 5 15 -1 -5 15 -1 -4 -15 1 4 15 -1 -3 15 -1 -2 -15 1 1 15 1 -1 15 -1 -1 -15 1 0 15 1 0 15 -1 0 -15 1 -1 15 -1 1 15 1 1 -15 1 -2 15 1 2 15 -1 2 15 1 3 15 -1 3 15 1 4 15 -1 4 15 1 5 15 -1 5 -15 -1 -5 15 -2 -9 15 -2 -8 -15 2 7 15 -2 -7 -15 2 6 15 2 -6 15 -2 -6 -15 2 5 15 -2 -5 15 2 -5 -15 -2 4 -15 2 4 15 -2 -4 -15 2 4 -15 2 3 15 -2 -3 -15 2 2 15 -2 -2 -15 -2 2 -15 2 1 -15 -2 1 -15 2 0 15 -2 0 -15 -2 0 -15 2 -1 15 -2 1 -15 -2 -1 -15 2 -2 15 -2 2 -15 -2 -2 15 -2 3 -15 -2 -3 15 -2 4 -15 -2 -4 -15 -2 -5 15 -3 -10 15 -3 -9 15 -3 -8 15 -3 -7 15 -3 -6 15 -3 -5 15 3 -4 15 -3 -4 15 -3 -3 -15 3 3 15 3 -3 -15 -3 3 15 -3 -2 -15 3 2 15 3 -2 -15 -3 2 15 -3 -1 -15 3 1 15 3 -1 -15 -3 1 -15 3 0 15 -3 0 -15 -3 0 -15 3 -1 15 -3 1 -15 -3 -1 15 -3 2 -15 -3 -2 15 -3 3 -15 -3 -3 -15 -3 -4 15 -4 -9 15 -4 -8 -15 -4 8 15 -4 -7 15 -4 -6 15 -4 -5 15 -4 -4 -15 4 3 15 -4 -3 -15 4 2 15 -4 -2 -15 -4 2 -15 4 1 15 -4 -1 -15 -4 1 -15 4 0 15 -4 0 -15 -4 0 -15 -4 0 -15 -4 -1 -15 -4 -2 -15 -4 -3 -15 -4 -4 -15 -5 8 -15 -5 7 -15 -5 6 15 -5 -6 -15 -5 5 15 -5 -5 -15 -5 4 -15 -5 4 15 -5 -4 -15 -5 3 15 -5 -3 -15 -5 3 -15 -5 2 -15 -5 2 -15 -5 1 -15 -5 0 -15 -5 0 -15 -5 -1 -15 -5 -2 -15 -5 -3 -15 -6 6 -15 -6 5 -15 -6 4 -15 -6 4 -15 -6 3 -15 -6 3 -15 -6 2 -15 -6 2 -15 -6 1 -15 -6 1 -15 -6 0 -15 -6 -1 -15 -7 4 -15 -7 3 -15 -7 2 -15 -7 1 16 0 -2 16 0 -1 16 0 0 16 0 1 -16 0 -1 16 0 2 -16 0 -2 16 -1 -5 16 -1 -4 16 -1 -3 16 -1 -2 16 -1 -1 16 -1 0 -16 -1 0 16 -1 1 -16 -1 -1 16 -1 2 -16 -1 -2 -16 1 -2 16 -2 -7 16 -2 -6 16 -2 -5 16 -2 -4 16 -2 -3 16 -2 -2 16 -2 -1 -16 -2 1 16 -2 0 -16 -2 0 16 -2 1 -16 -2 -1 16 -2 2 -16 -2 -2 16 -3 -6 16 -3 -5 16 -3 -4 16 -3 -3 16 -3 -2 -16 -3 1 16 -3 -1 -16 -3 0 -16 -3 -1 -16 -4 5 16 -4 -5 16 -4 -4 -16 -4 4 -16 -4 3 16 -4 -3 16 -4 -2 -16 -4 1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.1593 0 5 1 0.2642 -1 1 5 0.1084 1 0 -5 0.1056 1 2 -5 0.1320 -1 -5 4 0.1737 5 0 1 0.0457 -5 -1 0 0.0421 -5 2 -3 0.1194 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 H1WA O1W H1WB . . 98(6) ? C1 N1 C7 . . 118.81(11) ? C1 N1 C10 . . 119.39(11) ? C10 N1 C7 . . 110.07(11) ? C2 C1 N1 . . 121.82(13) ? C2 C1 C6 . . 117.73(12) ? C6 C1 N1 . . 120.35(13) ? C8 N2 C9 . . 112.93(10) ? C11 N2 C8 . . 118.92(11) ? C11 N2 C9 . . 120.45(11) ? C1 C2 H2 . . 119.7 ? C3 C2 C1 . . 120.62(14) ? C3 C2 H2 . . 119.7 ? C13 N3 C14 . . 115.40(12) ? C2 C3 H3 . . 119.4 ? C4 C3 C2 . . 121.19(14) ? C4 C3 H3 . . 119.4 ? H4A N4 H4B . . 120.0 ? C16 N4 H4A . . 120.0 ? C16 N4 H4B . . 120.0 ? C3 C4 H4 . . 120.8 ? C3 C4 C5 . . 118.45(13) ? C5 C4 H4 . . 120.8 ? N6 N5 H5 . . 120.8(12) ? C16 N5 H5 . . 118.0(12) ? C16 N5 N6 . . 120.25(12) ? C4 C5 H5A . . 119.5 ? C4 C5 C6 . . 121.08(14) ? C6 C5 H5A . . 119.5 ? C17 N6 N5 . . 112.49(11) ? C1 C6 H6 . . 119.6 ? C5 C6 C1 . . 120.89(14) ? C5 C6 H6 . . 119.6 ? C17 N7 C18 . . 120.96(11) ? C17 N7 C22 . . 119.58(11) ? C18 N7 C22 . . 111.77(11) ? N1 C7 H7A . . 109.4 ? N1 C7 H7B . . 109.4 ? N1 C7 C8 . . 111.13(11) ? H7A C7 H7B . . 108.0 ? C8 C7 H7A . . 109.4 ? C8 C7 H7B . . 109.4 ? C23 N8 C24 . . 121.81(14) ? C23 N8 C25 . . 120.41(14) ? C25 N8 C24 . . 117.78(13) ? N2 C8 C7 . . 111.37(11) ? N2 C8 H8A . . 109.4 ? N2 C8 H8B . . 109.4 ? C7 C8 H8A . . 109.4 ? C7 C8 H8B . . 109.4 ? H8A C8 H8B . . 108.0 ? N2 C9 H9A . . 109.3 ? N2 C9 H9B . . 109.3 ? N2 C9 C10 . . 111.82(12) ? H9A C9 H9B . . 107.9 ? C10 C9 H9A . . 109.3 ? C10 C9 H9B . . 109.3 ? N1 C10 C9 . . 111.01(12) ? N1 C10 H10A . . 109.4 ? N1 C10 H10B . . 109.4 ? C9 C10 H10A . . 109.4 ? C9 C10 H10B . . 109.4 ? H10A C10 H10B . . 108.0 ? N2 C11 C12 . . 121.53(12) ? N2 C11 C15 . . 122.47(12) ? C12 C11 C15 . . 115.93(12) ? C11 C12 H12 . . 120.1 ? C13 C12 C11 . . 119.88(13) ? C13 C12 H12 . . 120.1 ? N3 C13 C12 . . 124.78(13) ? N3 C13 H13 . . 117.6 ? C12 C13 H13 . . 117.6 ? N3 C14 C15 . . 124.78(13) ? N3 C14 C16 . . 113.53(11) ? C15 C14 C16 . . 121.68(12) ? C11 C15 H15 . . 120.4 ? C14 C15 C11 . . 119.19(12) ? C14 C15 H15 . . 120.4 ? N4 C16 C14 . . 123.48(11) ? N5 C16 N4 . . 120.08(12) ? N5 C16 C14 . . 116.43(12) ? N6 C17 S1 . . 124.01(10) ? N6 C17 N7 . . 115.08(12) ? N7 C17 S1 . . 120.90(9) ? N7 C18 H18A . . 109.5 ? N7 C18 H18B . . 109.5 ? N7 C18 C19 . . 110.52(12) ? H18A C18 H18B . . 108.1 ? C19 C18 H18A . . 109.5 ? C19 C18 H18B . . 109.5 ? C18 C19 H19A . . 109.4 ? C18 C19 H19B . . 109.4 ? C18 C19 C20 . . 111.02(14) ? H19A C19 H19B . . 108.0 ? C20 C19 H19A . . 109.4 ? C20 C19 H19B . . 109.4 ? C19 C20 H20A . . 109.4 ? C19 C20 H20B . . 109.4 ? H20A C20 H20B . . 108.0 ? C21 C20 C19 . . 111.29(13) ? C21 C20 H20A . . 109.4 ? C21 C20 H20B . . 109.4 ? C20 C21 H21A . . 109.5 ? C20 C21 H21B . . 109.5 ? H21A C21 H21B . . 108.1 ? C22 C21 C20 . . 110.67(13) ? C22 C21 H21A . . 109.5 ? C22 C21 H21B . . 109.5 ? N7 C22 C21 . . 110.67(12) ? N7 C22 H22A . . 109.5 ? N7 C22 H22B . . 109.5 ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 108.1 ? O1A C23 N8 . . 125.70(16) ? O1A C23 H23 . . 117.1 ? N8 C23 H23 . . 117.1 ? N8 C24 H24A . . 109.5 ? N8 C24 H24B . . 109.5 ? N8 C24 H24C . . 109.5 ? H24A C24 H24B . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? N8 C25 H25A . . 109.5 ? N8 C25 H25B . . 109.5 ? N8 C25 H25C . . 109.5 ? H25A C25 H25B . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? 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 C17 . 1.7369(14) ? O1W H1WA . 1.16(12) ? O1W H1WB . 0.96(8) ? O1A C23 . 1.2262(19) ? N1 C1 . 1.4117(16) ? N1 C7 . 1.4580(17) ? N1 C10 . 1.4543(18) ? C1 C2 . 1.397(2) ? C1 C6 . 1.403(2) ? N2 C8 . 1.4652(17) ? N2 C9 . 1.4654(17) ? N2 C11 . 1.3797(16) ? C2 H2 . 0.9500 ? C2 C3 . 1.3944(19) ? N3 C13 . 1.3332(19) ? N3 C14 . 1.3479(18) ? C3 H3 . 0.9500 ? C3 C4 . 1.384(2) ? N4 H4A . 0.8800 ? N4 H4B . 0.8800 ? N4 C16 . 1.3234(17) ? C4 H4 . 0.9500 ? C4 C5 . 1.386(2) ? N5 H5 . 0.84(2) ? N5 N6 . 1.3767(16) ? N5 C16 . 1.3134(16) ? C5 H5A . 0.9500 ? C5 C6 . 1.3870(19) ? N6 C17 . 1.3283(16) ? C6 H6 . 0.9500 ? N7 C17 . 1.3719(17) ? N7 C18 . 1.4659(17) ? N7 C22 . 1.4725(17) ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C7 C8 . 1.5137(19) ? N8 C23 . 1.3349(19) ? N8 C24 . 1.455(2) ? N8 C25 . 1.449(2) ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C9 C10 . 1.5196(19) ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C11 C12 . 1.4034(19) ? C11 C15 . 1.4113(19) ? C12 H12 . 0.9500 ? C12 C13 . 1.3830(19) ? C13 H13 . 0.9500 ? C14 C15 . 1.3853(17) ? C14 C16 . 1.4829(18) ? C15 H15 . 0.9500 ? C18 H18A . 0.9900 ? C18 H18B . 0.9900 ? C18 C19 . 1.526(2) ? C19 H19A . 0.9900 ? C19 H19B . 0.9900 ? C19 C20 . 1.528(2) ? C20 H20A . 0.9900 ? C20 H20B . 0.9900 ? C20 C21 . 1.522(2) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C21 C22 . 1.515(2) ? C22 H22A . 0.9900 ? C22 H22B . 0.9900 ? C23 H23 . 0.9500 ? C24 H24A . 0.9800 ? C24 H24B . 0.9800 ? C24 H24C . 0.9800 ? C25 H25A . 0.9800 ? C25 H25B . 0.9800 ? C25 H25C . 0.9800 ? 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 O1W H1WA N3 . 1.16(12) 1.95(12) 3.110(4) 174(8) yes O1W H1WB S1 . 0.96(8) 2.46(8) 3.381(4) 161(6) yes N5 H5 S1 . 0.84(2) 2.378(18) 2.8314(12) 114.4(15) yes N4 H4A O1A . 0.88 2.07 2.8823(16) 153.8 yes N4 H4B S1 4_576 0.88 2.48 3.3034(11) 156.7 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 N1 C1 C2 C3 . . . . 173.65(13) ? N1 C1 C6 C5 . . . . -174.27(13) ? N1 C7 C8 N2 . . . . 55.24(16) ? C1 N1 C7 C8 . . . . 157.84(12) ? C1 N1 C10 C9 . . . . -158.86(12) ? C1 C2 C3 C4 . . . . 1.4(2) ? N2 C9 C10 N1 . . . . -54.18(17) ? N2 C11 C12 C13 . . . . -175.12(15) ? N2 C11 C15 C14 . . . . 176.13(12) ? C2 C1 C6 C5 . . . . 2.1(2) ? C2 C3 C4 C5 . . . . 0.5(2) ? N3 C14 C15 C11 . . . . -0.6(2) ? N3 C14 C16 N4 . . . . 174.11(13) ? N3 C14 C16 N5 . . . . -5.17(18) ? C3 C4 C5 C6 . . . . -1.1(2) ? C4 C5 C6 C1 . . . . -0.2(2) ? N5 N6 C17 S1 . . . . 0.80(16) ? N5 N6 C17 N7 . . . . -177.91(11) ? N6 N5 C16 N4 . . . . -2.17(19) ? N6 N5 C16 C14 . . . . 177.14(11) ? C6 C1 C2 C3 . . . . -2.7(2) ? N7 C18 C19 C20 . . . . 54.92(17) ? C7 N1 C1 C2 . . . . 147.74(14) ? C7 N1 C1 C6 . . . . -36.04(19) ? C7 N1 C10 C9 . . . . 58.53(16) ? C8 N2 C9 C10 . . . . 50.47(17) ? C8 N2 C11 C12 . . . . -22.1(2) ? C8 N2 C11 C15 . . . . 160.89(13) ? C9 N2 C8 C7 . . . . -50.91(16) ? C9 N2 C11 C12 . . . . -169.34(14) ? C9 N2 C11 C15 . . . . 13.6(2) ? C10 N1 C1 C2 . . . . 8.3(2) ? C10 N1 C1 C6 . . . . -175.43(13) ? C10 N1 C7 C8 . . . . -59.31(16) ? C11 N2 C8 C7 . . . . 159.50(12) ? C11 N2 C9 C10 . . . . -160.45(13) ? C11 C12 C13 N3 . . . . -1.7(3) ? C12 C11 C15 C14 . . . . -1.1(2) ? C13 N3 C14 C15 . . . . 1.1(2) ? C13 N3 C14 C16 . . . . -178.43(14) ? C14 N3 C13 C12 . . . . 0.0(3) ? C15 C11 C12 C13 . . . . 2.1(2) ? C15 C14 C16 N4 . . . . -5.5(2) ? C15 C14 C16 N5 . . . . 175.27(12) ? C16 N5 N6 C17 . . . . -168.99(12) ? C16 C14 C15 C11 . . . . 178.93(12) ? C17 N7 C18 C19 . . . . 89.83(16) ? C17 N7 C22 C21 . . . . -89.36(15) ? C18 N7 C17 S1 . . . . 25.27(17) ? C18 N7 C17 N6 . . . . -155.98(12) ? C18 N7 C22 C21 . . . . 60.38(15) ? C18 C19 C20 C21 . . . . -52.08(19) ? C19 C20 C21 C22 . . . . 52.71(18) ? C20 C21 C22 N7 . . . . -56.30(16) ? C22 N7 C17 S1 . . . . 172.19(10) ? C22 N7 C17 N6 . . . . -9.06(18) ? C22 N7 C18 C19 . . . . -59.43(15) ? C24 N8 C23 O1A . . . . 178.88(14) ? C25 N8 C23 O1A . . . . -0.3(2) ? _cod_database_fobs_code 2312722