#------------------------------------------------------------------------------ #$Date: 2019-12-14 02:53:31 +0200 (Sat, 14 Dec 2019) $ #$Revision: 245135 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556575.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_1556575 loop_ _publ_author_name 'Kong, Fan-Dong' 'Zhang, Sheng-Liang' 'Zhou, Shuang-Qing' 'Ma, Qing-Yun' 'Xie, Qing-Yi' 'Chen, Jin-Ping' 'Li, Jiu-Hui' 'Zhou, Li-Man' 'Yuan, Jing-Zhe' 'Hu, Zhong' 'Dai, Hao-Fu' 'Huang, Xiao-Long' 'Zhao, You-Xing' _publ_section_title ; Quinazoline-Containing Indole Alkaloids from the Marine-Derived Fungus Aspergillus sp. HNMF114. ; _journal_name_full 'Journal of natural products' _journal_paper_doi 10.1021/acs.jnatprod.9b00845 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety 'C28 H30 N4 O7 S' _chemical_formula_sum 'C28 H30 N4 O7 S' _chemical_formula_weight 566.62 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-07-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.73600(15) _cell_length_b 16.3578(3) _cell_length_c 18.2142(3) _cell_measurement_reflns_used 5859 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 73.3350 _cell_measurement_theta_min 3.6000 _cell_volume 2602.84(8) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -115.00 -16.00 1.00 1.00 -- -40.98 -38.00 30.00 99 2 \w -115.00 -16.00 1.00 1.00 -- -40.98 -38.00 120.00 99 3 \w 1.00 82.00 1.00 1.00 -- 40.98 -99.00 -90.00 81 4 \w 35.00 136.00 1.00 3.18 -- 106.95 -61.00-180.00 101 5 \w 31.00 135.00 1.00 3.18 -- 106.95 -30.00-120.00 104 6 \w 25.00 109.00 1.00 3.18 -- 106.95 -95.00 60.00 84 7 \w 34.00 66.00 1.00 3.18 -- 106.95 -45.00 -60.00 32 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0013904000 _diffrn_orient_matrix_UB_12 0.0366162000 _diffrn_orient_matrix_UB_13 -0.0779281000 _diffrn_orient_matrix_UB_21 -0.0074107000 _diffrn_orient_matrix_UB_22 -0.0867083000 _diffrn_orient_matrix_UB_23 -0.0330117000 _diffrn_orient_matrix_UB_31 -0.1760306000 _diffrn_orient_matrix_UB_32 0.0038464000 _diffrn_orient_matrix_UB_33 0.0007141000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_unetI/netI 0.0347 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 8966 _diffrn_reflns_point_group_measured_fraction_full 0.918 _diffrn_reflns_point_group_measured_fraction_max 0.876 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.586 _diffrn_reflns_theta_min 3.632 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.587 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77607 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.446 _exptl_crystal_description block _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.194 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Flack x determined using 1619 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.002(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 367 _refine_ls_number_reflns 4597 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0302 _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^)+(0.0403P)^2^+0.4537P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.0767 _reflns_Friedel_coverage 0.602 _reflns_Friedel_fraction_full 0.821 _reflns_Friedel_fraction_max 0.761 _reflns_number_gt 4417 _reflns_number_total 4597 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 22-6_a.res in P2(1)2(1)2(1) 22-6.res created by SHELXL-2018/3 at 17:57:26 on 15-Jul-2019 REM Old TITL 22-6 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.075, Rweak 0.024, Alpha 0.004 REM 0.793 for 21 systematic absences, Orientation as input REM Flack x = 0.107 ( 0.010 ) from 1084 Parsons' quotients REM Formula found by SHELXT: C28 N4 O7 Cl CELL 1.54184 8.736002 16.357845 18.214159 90 90 90 ZERR 4 0.000149 0.000277 0.000321 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S UNIT 112 120 16 28 4 L.S. 20 PLAN 20 BOND list 4 fmap 2 acta REM REM REM WGHT 0.040300 0.453700 FVAR 5.59490 S1 5 0.312038 0.620007 0.244625 11.00000 0.01757 0.01899 = 0.02263 0.00452 -0.00066 0.00045 O3 4 0.594657 0.504119 0.374491 11.00000 0.01384 0.01711 = 0.02004 -0.00222 0.00059 -0.00219 O1 4 0.824930 0.364157 0.349794 11.00000 0.02215 0.02304 = 0.01958 0.00044 0.00224 0.00129 O2 4 0.825041 0.553106 0.342573 11.00000 0.02005 0.02400 = 0.02934 -0.00301 0.00351 -0.00626 O6 4 0.329969 0.707071 0.246923 11.00000 0.02431 0.01902 = 0.03518 0.00881 -0.00171 -0.00317 O4 4 0.228423 0.574709 0.515657 11.00000 0.03073 0.02504 = 0.02180 -0.00214 0.00051 0.00313 O7 4 0.954825 0.515367 0.064546 11.00000 0.01852 0.03314 = 0.02829 0.01006 0.00342 -0.00182 AFIX 147 H7 2 1.023680 0.481581 0.068485 11.00000 -1.50000 AFIX 0 O5 4 0.416081 0.571786 0.201701 11.00000 0.02916 0.03401 = 0.02560 0.00477 0.00499 0.00979 N3 3 0.262867 0.491613 0.415555 11.00000 0.01566 0.01609 = 0.02005 0.00277 0.00085 0.00122 N2 3 0.822652 0.420394 0.235625 11.00000 0.01698 0.01845 = 0.01937 0.00169 0.00068 0.00083 N4 3 0.329166 0.586640 0.328917 11.00000 0.02010 0.01337 = 0.02194 0.00079 -0.00098 0.00141 N1 3 1.017935 0.394273 0.149227 11.00000 0.01692 0.02260 = 0.02211 -0.00027 0.00268 0.00002 C1 1 1.026489 0.327293 0.268018 11.00000 0.01509 0.01857 = 0.02349 -0.00166 -0.00119 -0.00209 C17 1 0.317188 0.417469 0.446504 11.00000 0.01296 0.01584 = 0.02297 -0.00006 -0.00227 -0.00176 C8 1 0.886646 0.369267 0.289637 11.00000 0.01830 0.01696 = 0.02288 -0.00021 -0.00166 -0.00130 C12 1 0.715392 0.511781 0.328862 11.00000 0.01654 0.01861 = 0.02124 0.00009 0.00122 0.00093 C7 1 0.895652 0.432733 0.168601 11.00000 0.01603 0.02044 = 0.01984 -0.00143 -0.00047 -0.00293 C13 1 0.325475 0.498341 0.341327 11.00000 0.01540 0.01356 = 0.02090 0.00019 -0.00105 -0.00018 AFIX 13 H13 2 0.255653 0.472510 0.306181 11.00000 -1.20000 AFIX 0 C20 1 0.453573 0.272885 0.483947 11.00000 0.02113 0.01711 = 0.03175 0.00413 -0.00291 0.00028 AFIX 43 H20 2 0.497494 0.223089 0.496725 11.00000 -1.20000 AFIX 0 C15 1 0.279571 0.633972 0.395606 11.00000 0.01647 0.01624 = 0.02217 -0.00145 -0.00112 0.00050 C9 1 0.685349 0.465536 0.257828 11.00000 0.01759 0.01821 = 0.02035 0.00017 0.00004 0.00160 AFIX 13 H9 2 0.661082 0.505366 0.219358 11.00000 -1.20000 AFIX 0 C16 1 0.437850 0.388006 0.404406 11.00000 0.01451 0.01716 = 0.02125 0.00029 -0.00138 -0.00065 C11 1 0.478363 0.449060 0.345112 11.00000 0.01301 0.01445 = 0.02220 -0.00246 -0.00123 -0.00136 C14 1 0.253349 0.565216 0.451051 11.00000 0.01513 0.01884 = 0.02512 -0.00175 -0.00217 0.00109 C18 1 0.264648 0.378072 0.508597 11.00000 0.01503 0.02205 = 0.02606 0.00317 0.00015 -0.00239 AFIX 43 H18 2 0.185644 0.399486 0.536905 11.00000 -1.20000 AFIX 0 C6 1 1.085207 0.339678 0.197324 11.00000 0.01564 0.02220 = 0.02618 -0.00265 -0.00226 -0.00320 C21 1 0.506727 0.314365 0.422333 11.00000 0.01815 0.01886 = 0.02742 -0.00018 0.00024 0.00257 AFIX 43 H21 2 0.586081 0.293304 0.394037 11.00000 -1.20000 AFIX 0 C10 1 0.542483 0.414308 0.272699 11.00000 0.01696 0.01709 = 0.02049 -0.00136 -0.00023 0.00085 AFIX 23 H10A 2 0.568490 0.356960 0.277986 11.00000 -1.20000 H10B 2 0.468782 0.420155 0.233215 11.00000 -1.20000 AFIX 0 C23 1 0.129722 0.681458 0.387034 11.00000 0.01873 0.01960 = 0.03113 0.00018 -0.00069 0.00135 AFIX 137 H23A 2 0.141974 0.722740 0.350036 11.00000 -1.50000 H23B 2 0.103672 0.706813 0.432896 11.00000 -1.50000 H23C 2 0.049509 0.644612 0.372792 11.00000 -1.50000 AFIX 0 C25 1 0.836741 0.496840 0.115105 11.00000 0.01869 0.02073 = 0.02084 0.00160 0.00114 -0.00192 AFIX 13 H25 2 0.813948 0.546567 0.143051 11.00000 -1.20000 AFIX 0 C19 1 0.335967 0.304577 0.526734 11.00000 0.01893 0.02171 = 0.02774 0.00594 -0.00101 -0.00505 AFIX 43 H19 2 0.304243 0.276192 0.568275 11.00000 -1.20000 AFIX 0 C2 1 1.102496 0.275079 0.317272 11.00000 0.02016 0.02174 = 0.02626 0.00039 -0.00294 -0.00155 AFIX 43 H2 2 1.065003 0.267848 0.364616 11.00000 -1.20000 AFIX 0 C26 1 0.690296 0.471200 0.074327 11.00000 0.01727 0.02654 = 0.02176 0.00147 -0.00011 -0.00129 AFIX 13 H26 2 0.610883 0.458924 0.110695 11.00000 -1.20000 AFIX 0 C27 1 0.635986 0.542639 0.026983 11.00000 0.02445 0.02578 = 0.02994 0.00197 -0.00460 0.00654 AFIX 137 H27A 2 0.608720 0.587794 0.058005 11.00000 -1.50000 H27B 2 0.548385 0.526097 -0.001159 11.00000 -1.50000 H27C 2 0.716728 0.558912 -0.005646 11.00000 -1.50000 AFIX 0 C22 1 0.409083 0.688540 0.422674 11.00000 0.02048 0.02041 = 0.03162 -0.00464 -0.00192 -0.00161 AFIX 137 H22A 2 0.502078 0.657401 0.425222 11.00000 -1.50000 H22B 2 0.384360 0.709208 0.470557 11.00000 -1.50000 H22C 2 0.422440 0.733402 0.389303 11.00000 -1.50000 AFIX 0 C5 1 1.217571 0.297659 0.175163 11.00000 0.01732 0.02818 = 0.03061 -0.00413 0.00298 -0.00078 AFIX 43 H5 2 1.256917 0.305074 0.128189 11.00000 -1.20000 AFIX 0 C3 1 1.233143 0.234578 0.294977 11.00000 0.02065 0.02260 = 0.03538 0.00114 -0.00461 0.00036 AFIX 43 H3 2 1.284164 0.200162 0.327426 11.00000 -1.20000 AFIX 0 C24 1 0.125352 0.596703 0.214550 11.00000 0.02518 0.02814 = 0.02692 0.00412 -0.00830 -0.00223 AFIX 137 H24A 2 0.052627 0.627990 0.242330 11.00000 -1.50000 H24B 2 0.105942 0.539463 0.221524 11.00000 -1.50000 H24C 2 0.115784 0.609961 0.163412 11.00000 -1.50000 AFIX 0 C4 1 1.288679 0.245258 0.223773 11.00000 0.01575 0.02856 = 0.03971 -0.00384 -0.00081 0.00265 AFIX 43 H4 2 1.375126 0.216558 0.208821 11.00000 -1.20000 AFIX 0 C28 1 0.716773 0.395366 0.027626 11.00000 0.03166 0.02223 = 0.02961 0.00222 -0.00864 0.00024 AFIX 137 H28A 2 0.790152 0.407460 -0.010075 11.00000 -1.50000 H28B 2 0.621984 0.378844 0.005471 11.00000 -1.50000 H28C 2 0.754887 0.351955 0.058020 11.00000 -1.50000 AFIX 0 HKLF 4 REM 22-6_a.res in P2(1)2(1)2(1) REM wR2 = 0.0767, GooF = S = 1.040, Restrained GooF = 1.040 for all data REM R1 = 0.0302 for 4417 Fo > 4sig(Fo) and 0.0318 for all 4597 data REM 367 parameters refined using 0 restraints END WGHT 0.0412 0.4282 REM Highest difference peak 0.194, deepest hole -0.366, 1-sigma level 0.042 Q1 1 0.4619 0.4156 0.3752 11.00000 0.05 0.19 Q2 1 0.3178 0.6005 0.2958 11.00000 0.05 0.18 Q3 1 0.4025 0.4783 0.3409 11.00000 0.05 0.18 Q4 1 0.5511 0.4052 0.1113 11.00000 0.05 0.18 Q5 1 0.3399 0.6626 0.4120 11.00000 0.05 0.18 Q6 1 0.6179 0.4400 0.2635 11.00000 0.05 0.16 Q7 1 0.6955 0.4861 0.2914 11.00000 0.05 0.15 Q8 1 0.2120 0.6016 0.2348 11.00000 0.05 0.15 Q9 1 0.3495 0.3927 0.4161 11.00000 0.05 0.14 Q10 1 0.4661 0.3622 0.4040 11.00000 0.05 0.14 Q11 1 1.0308 0.3163 0.2226 11.00000 0.05 0.14 Q12 1 -0.0019 0.6651 0.3348 11.00000 0.05 0.13 Q13 1 1.1546 0.3167 0.1881 11.00000 0.05 0.13 Q14 1 0.5423 0.5816 0.0777 11.00000 0.05 0.13 Q15 1 0.4350 0.5844 0.2468 11.00000 0.05 0.13 Q16 1 1.0780 0.3545 0.2458 11.00000 0.05 0.12 Q17 1 0.8432 0.4069 0.2536 11.00000 0.05 0.12 Q18 1 1.0616 0.5365 0.0057 11.00000 0.05 0.12 Q19 1 0.5084 0.6612 0.5376 11.00000 0.05 0.12 Q20 1 0.4999 0.4329 0.3070 11.00000 0.05 0.12 REM The information below was added by Olex2. REM REM R1 = 0.0302 for 4417 Fo > 4sig(Fo) and 0.0318 for all 8998 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.19, deepest hole -0.37 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0318 REM R1_gt = 0.0302 REM wR_ref = 0.0767 REM GOOF = 1.040 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 8998 REM Reflections_gt = 4417 REM Parameters = n/a REM Hole = -0.37 REM Peak = 0.19 REM Flack = -0.002(11) ; _cod_data_source_file np9b00845_si_002.cif _cod_data_source_block 22-6 _cod_database_code 1556575 _shelx_shelxl_version_number 2018/3 _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. ; _reflns_odcompleteness_completeness 99.10 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C13(H13), C9(H9), C25(H25), C26(H26) 2.b Secondary CH2 refined with riding coordinates: C10(H10A,H10B) 2.c Aromatic/amide H refined with riding coordinates: C20(H20), C18(H18), C21(H21), C19(H19), C2(H2), C5(H5), C3(H3), C4(H4) 2.d Idealised Me refined as rotating group: C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C24(H24A,H24B, H24C), C28(H28A,H28B,H28C) 2.e Idealised tetrahedral OH refined as rotating group: O7(H7) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.321 _oxdiff_exptl_absorpt_empirical_full_min 0.726 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 S1 S 0.31204(6) 0.62001(3) 0.24463(3) 0.01973(13) Uani 1 1 d . O3 O 0.59466(18) 0.50412(10) 0.37449(9) 0.0170(3) Uani 1 1 d . O1 O 0.8249(2) 0.36416(10) 0.34979(9) 0.0216(3) Uani 1 1 d . O2 O 0.8250(2) 0.55311(11) 0.34257(10) 0.0245(4) Uani 1 1 d . O6 O 0.3300(2) 0.70707(10) 0.24692(10) 0.0262(4) Uani 1 1 d . O4 O 0.2284(2) 0.57471(11) 0.51566(10) 0.0259(4) Uani 1 1 d . O7 O 0.9548(2) 0.51537(12) 0.06455(10) 0.0266(4) Uani 1 1 d . H7 H 1.023680 0.481581 0.068485 0.040 Uiso 1 1 calc GR O5 O 0.4161(2) 0.57179(12) 0.20170(10) 0.0296(4) Uani 1 1 d . N3 N 0.2629(2) 0.49161(12) 0.41555(11) 0.0173(4) Uani 1 1 d . N2 N 0.8227(2) 0.42039(12) 0.23563(10) 0.0183(4) Uani 1 1 d . N4 N 0.3292(2) 0.58664(12) 0.32892(10) 0.0185(4) Uani 1 1 d . N1 N 1.0179(2) 0.39427(13) 0.14923(11) 0.0205(4) Uani 1 1 d . C1 C 1.0265(3) 0.32729(14) 0.26802(13) 0.0190(5) Uani 1 1 d . C17 C 0.3172(3) 0.41747(14) 0.44650(13) 0.0173(4) Uani 1 1 d . C8 C 0.8866(3) 0.36927(14) 0.28964(14) 0.0194(5) Uani 1 1 d . C12 C 0.7154(3) 0.51178(15) 0.32886(13) 0.0188(5) Uani 1 1 d . C7 C 0.8957(3) 0.43273(15) 0.16860(13) 0.0188(5) Uani 1 1 d . C13 C 0.3255(3) 0.49834(13) 0.34133(12) 0.0166(4) Uani 1 1 d . H13 H 0.255653 0.472510 0.306181 0.020 Uiso 1 1 calc R C20 C 0.4536(3) 0.27289(15) 0.48395(15) 0.0233(5) Uani 1 1 d . H20 H 0.497494 0.223089 0.496725 0.028 Uiso 1 1 calc R C15 C 0.2796(3) 0.63397(14) 0.39561(13) 0.0183(5) Uani 1 1 d . C9 C 0.6853(3) 0.46554(14) 0.25783(13) 0.0187(4) Uani 1 1 d . H9 H 0.661082 0.505366 0.219358 0.022 Uiso 1 1 calc R C16 C 0.4379(3) 0.38801(15) 0.40441(13) 0.0176(5) Uani 1 1 d . C11 C 0.4784(3) 0.44906(14) 0.34511(13) 0.0166(4) Uani 1 1 d . C14 C 0.2533(3) 0.56522(15) 0.45105(13) 0.0197(5) Uani 1 1 d . C18 C 0.2646(3) 0.37807(15) 0.50860(14) 0.0210(5) Uani 1 1 d . H18 H 0.185644 0.399486 0.536905 0.025 Uiso 1 1 calc R C6 C 1.0852(3) 0.33968(16) 0.19732(14) 0.0213(5) Uani 1 1 d . C21 C 0.5067(3) 0.31437(14) 0.42233(14) 0.0215(5) Uani 1 1 d . H21 H 0.586081 0.293304 0.394037 0.026 Uiso 1 1 calc R C10 C 0.5425(3) 0.41431(14) 0.27270(13) 0.0182(5) Uani 1 1 d . H10A H 0.568490 0.356960 0.277986 0.022 Uiso 1 1 calc R H10B H 0.468782 0.420155 0.233215 0.022 Uiso 1 1 calc R C23 C 0.1297(3) 0.68146(15) 0.38703(15) 0.0232(5) Uani 1 1 d . H23A H 0.141974 0.722740 0.350036 0.035 Uiso 1 1 calc GR H23B H 0.103672 0.706813 0.432896 0.035 Uiso 1 1 calc GR H23C H 0.049509 0.644612 0.372792 0.035 Uiso 1 1 calc GR C25 C 0.8367(3) 0.49684(15) 0.11510(13) 0.0201(5) Uani 1 1 d . H25 H 0.813948 0.546567 0.143051 0.024 Uiso 1 1 calc R C19 C 0.3360(3) 0.30458(15) 0.52673(14) 0.0228(5) Uani 1 1 d . H19 H 0.304243 0.276192 0.568275 0.027 Uiso 1 1 calc R C2 C 1.1025(3) 0.27508(15) 0.31727(15) 0.0227(5) Uani 1 1 d . H2 H 1.065003 0.267848 0.364616 0.027 Uiso 1 1 calc R C26 C 0.6903(3) 0.47120(15) 0.07433(13) 0.0219(5) Uani 1 1 d . H26 H 0.610883 0.458924 0.110695 0.026 Uiso 1 1 calc R C27 C 0.6360(3) 0.54264(16) 0.02698(15) 0.0267(6) Uani 1 1 d . H27A H 0.608720 0.587794 0.058005 0.040 Uiso 1 1 calc GR H27B H 0.548385 0.526097 -0.001159 0.040 Uiso 1 1 calc GR H27C H 0.716728 0.558912 -0.005646 0.040 Uiso 1 1 calc GR C22 C 0.4091(3) 0.68854(15) 0.42267(15) 0.0242(5) Uani 1 1 d . H22A H 0.502078 0.657401 0.425222 0.036 Uiso 1 1 calc GR H22B H 0.384360 0.709208 0.470557 0.036 Uiso 1 1 calc GR H22C H 0.422440 0.733402 0.389303 0.036 Uiso 1 1 calc GR C5 C 1.2176(3) 0.29766(16) 0.17516(15) 0.0254(5) Uani 1 1 d . H5 H 1.256917 0.305074 0.128189 0.030 Uiso 1 1 calc R C3 C 1.2331(3) 0.23458(16) 0.29498(16) 0.0262(5) Uani 1 1 d . H3 H 1.284164 0.200162 0.327426 0.031 Uiso 1 1 calc R C24 C 0.1254(3) 0.59670(16) 0.21455(15) 0.0267(6) Uani 1 1 d . H24A H 0.052627 0.627990 0.242330 0.040 Uiso 1 1 calc GR H24B H 0.105942 0.539463 0.221524 0.040 Uiso 1 1 calc GR H24C H 0.115784 0.609961 0.163412 0.040 Uiso 1 1 calc GR C4 C 1.2887(3) 0.24526(17) 0.22377(16) 0.0280(6) Uani 1 1 d . H4 H 1.375126 0.216558 0.208821 0.034 Uiso 1 1 calc R C28 C 0.7168(3) 0.39537(16) 0.02763(15) 0.0278(6) Uani 1 1 d . H28A H 0.790152 0.407460 -0.010075 0.042 Uiso 1 1 calc GR H28B H 0.621984 0.378844 0.005471 0.042 Uiso 1 1 calc GR H28C H 0.754887 0.351955 0.058020 0.042 Uiso 1 1 calc GR 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 0.0176(3) 0.0190(3) 0.0226(3) 0.0045(2) -0.0007(2) 0.0005(2) O3 0.0138(8) 0.0171(8) 0.0200(8) -0.0022(7) 0.0006(6) -0.0022(6) O1 0.0221(8) 0.0230(8) 0.0196(8) 0.0004(7) 0.0022(7) 0.0013(7) O2 0.0201(9) 0.0240(9) 0.0293(9) -0.0030(7) 0.0035(7) -0.0063(7) O6 0.0243(8) 0.0190(8) 0.0352(9) 0.0088(8) -0.0017(8) -0.0032(7) O4 0.0307(10) 0.0250(9) 0.0218(9) -0.0021(7) 0.0005(7) 0.0031(7) O7 0.0185(9) 0.0331(10) 0.0283(9) 0.0101(8) 0.0034(7) -0.0018(7) O5 0.0292(10) 0.0340(10) 0.0256(9) 0.0048(8) 0.0050(8) 0.0098(8) N3 0.0157(9) 0.0161(9) 0.0200(9) 0.0028(8) 0.0008(8) 0.0012(7) N2 0.0170(9) 0.0184(9) 0.0194(9) 0.0017(8) 0.0007(8) 0.0008(8) N4 0.0201(10) 0.0134(9) 0.0219(10) 0.0008(8) -0.0010(8) 0.0014(8) N1 0.0169(10) 0.0226(10) 0.0221(10) -0.0003(8) 0.0027(8) 0.0000(8) C1 0.0151(10) 0.0186(10) 0.0235(12) -0.0017(10) -0.0012(9) -0.0021(9) C17 0.0130(10) 0.0158(10) 0.0230(11) -0.0001(9) -0.0023(9) -0.0018(9) C8 0.0183(11) 0.0170(11) 0.0229(11) -0.0002(9) -0.0017(9) -0.0013(9) C12 0.0165(12) 0.0186(11) 0.0212(11) 0.0001(9) 0.0012(8) 0.0009(9) C7 0.0160(11) 0.0204(11) 0.0198(12) -0.0014(9) -0.0005(9) -0.0029(9) C13 0.0154(10) 0.0136(10) 0.0209(11) 0.0002(9) -0.0010(9) -0.0002(9) C20 0.0211(12) 0.0171(11) 0.0317(13) 0.0041(10) -0.0029(10) 0.0003(9) C15 0.0165(11) 0.0162(11) 0.0222(11) -0.0015(9) -0.0011(8) 0.0005(8) C9 0.0176(11) 0.0182(10) 0.0203(11) 0.0002(9) 0.0000(10) 0.0016(9) C16 0.0145(11) 0.0172(11) 0.0213(11) 0.0003(10) -0.0014(9) -0.0007(8) C11 0.0130(10) 0.0145(10) 0.0222(11) -0.0025(9) -0.0012(9) -0.0014(8) C14 0.0151(11) 0.0188(11) 0.0251(12) -0.0018(10) -0.0022(9) 0.0011(9) C18 0.0150(11) 0.0221(12) 0.0261(12) 0.0032(10) 0.0002(9) -0.0024(9) C6 0.0156(11) 0.0222(12) 0.0262(13) -0.0026(10) -0.0023(9) -0.0032(9) C21 0.0182(12) 0.0189(11) 0.0274(12) -0.0002(10) 0.0002(9) 0.0026(9) C10 0.0170(11) 0.0171(10) 0.0205(11) -0.0014(9) -0.0002(9) 0.0009(9) C23 0.0187(12) 0.0196(11) 0.0311(13) 0.0002(10) -0.0007(10) 0.0013(9) C25 0.0187(12) 0.0207(11) 0.0208(11) 0.0016(10) 0.0011(9) -0.0019(9) C19 0.0189(12) 0.0217(12) 0.0277(12) 0.0059(10) -0.0010(10) -0.0050(9) C2 0.0202(12) 0.0217(12) 0.0263(12) 0.0004(10) -0.0029(10) -0.0015(9) C26 0.0173(11) 0.0265(12) 0.0218(11) 0.0015(10) -0.0001(10) -0.0013(10) C27 0.0245(13) 0.0258(13) 0.0299(13) 0.0020(11) -0.0046(10) 0.0065(10) C22 0.0205(12) 0.0204(12) 0.0316(13) -0.0046(10) -0.0019(10) -0.0016(9) C5 0.0173(12) 0.0282(13) 0.0306(13) -0.0041(11) 0.0030(10) -0.0008(10) C3 0.0207(13) 0.0226(12) 0.0354(14) 0.0011(11) -0.0046(10) 0.0004(10) C24 0.0252(13) 0.0281(13) 0.0269(13) 0.0041(11) -0.0083(10) -0.0022(10) C4 0.0158(12) 0.0286(13) 0.0397(15) -0.0038(12) -0.0008(10) 0.0027(10) C28 0.0317(14) 0.0222(12) 0.0296(13) 0.0022(11) -0.0086(10) 0.0002(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O6 S1 O5 119.52(12) O6 S1 N4 107.10(11) O6 S1 C24 108.97(12) O5 S1 N4 105.66(11) O5 S1 C24 107.33(13) N4 S1 C24 107.71(12) C12 O3 C11 112.08(18) C17 N3 C13 107.85(18) C14 N3 C17 125.8(2) C14 N3 C13 113.14(19) C8 N2 C9 115.58(19) C7 N2 C8 121.2(2) C7 N2 C9 122.95(19) C13 N4 S1 118.20(15) C13 N4 C15 112.16(18) C15 N4 S1 124.03(15) C7 N1 C6 119.6(2) C6 C1 C8 119.2(2) C6 C1 C2 120.1(2) C2 C1 C8 120.7(2) C16 C17 N3 109.3(2) C18 C17 N3 127.8(2) C18 C17 C16 122.8(2) O1 C8 N2 119.4(2) O1 C8 C1 125.4(2) N2 C8 C1 115.1(2) O3 C12 C9 110.05(19) O2 C12 O3 123.3(2) O2 C12 C9 126.5(2) N2 C7 C25 120.4(2) N1 C7 N2 123.3(2) N1 C7 C25 116.2(2) N3 C13 C11 103.90(18) N4 C13 N3 103.03(18) N4 C13 C11 119.86(19) C19 C20 C21 121.1(2) N4 C15 C14 101.42(18) N4 C15 C23 115.2(2) N4 C15 C22 110.43(19) C14 C15 C23 108.22(19) C22 C15 C14 109.2(2) C22 C15 C23 111.78(19) N2 C9 C12 110.12(18) N2 C9 C10 116.19(18) C12 C9 C10 105.24(19) C17 C16 C11 110.0(2) C21 C16 C17 120.1(2) C21 C16 C11 129.8(2) O3 C11 C13 107.04(17) O3 C11 C16 107.97(18) O3 C11 C10 106.76(18) C16 C11 C13 99.92(18) C16 C11 C10 116.89(19) C10 C11 C13 117.60(19) O4 C14 N3 125.8(2) O4 C14 C15 125.2(2) N3 C14 C15 109.0(2) C17 C18 C19 116.6(2) N1 C6 C1 121.4(2) N1 C6 C5 119.0(2) C1 C6 C5 119.7(2) C16 C21 C20 118.0(2) C9 C10 C11 104.26(18) O7 C25 C7 108.5(2) O7 C25 C26 110.52(19) C7 C25 C26 113.76(19) C20 C19 C18 121.3(2) C3 C2 C1 119.6(2) C27 C26 C25 108.8(2) C28 C26 C25 111.5(2) C28 C26 C27 110.8(2) C4 C5 C6 119.4(2) C2 C3 C4 120.0(2) C5 C4 C3 121.2(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O6 1.4334(17) S1 O5 1.4351(19) S1 N4 1.6363(19) S1 C24 1.762(3) O3 C12 1.349(3) O3 C11 1.459(3) O1 C8 1.224(3) O2 C12 1.199(3) O4 C14 1.207(3) O7 C25 1.416(3) N3 C17 1.419(3) N3 C13 1.463(3) N3 C14 1.369(3) N2 C8 1.407(3) N2 C7 1.392(3) N2 C9 1.465(3) N4 C13 1.462(3) N4 C15 1.504(3) N1 C7 1.289(3) N1 C6 1.382(3) C1 C8 1.456(3) C1 C6 1.401(4) C1 C2 1.405(4) C17 C16 1.390(3) C17 C18 1.380(3) C12 C9 1.522(3) C7 C25 1.521(3) C13 C11 1.562(3) C20 C21 1.391(4) C20 C19 1.390(4) C15 C14 1.529(3) C15 C23 1.530(3) C15 C22 1.523(3) C9 C10 1.528(3) C16 C11 1.513(3) C16 C21 1.386(3) C11 C10 1.542(3) C18 C19 1.394(3) C6 C5 1.404(3) C25 C26 1.538(3) C2 C3 1.381(4) C26 C27 1.528(3) C26 C28 1.522(4) C5 C4 1.380(4) C3 C4 1.396(4) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 1 73.2911 36.8687 1 0 0 2 615837 11549.5 1 0 0 3 21.0474 117.007 1 0 0 4 237875 5085.67 1 0 0 5 91.3394 248.638 1 0 0 6 8521.18 681.956 1 0 0 7 10.1872 187.736 1 0 0 8 52244 2104.13 1 0 0 9 -58.4587 220.53 1 0 0 10 85680.1 3147.8 1 0 0 11 1223.04 535.3 1 0 0 12 186826 5654.73 1 0 0 -13 75.7659 150.141 5 0 0 -13 154.504 240.799 2 0 0 -14 4047.34 795.269 2 0 0 14 5537.26 939.195 1 0 0 -14 4381.03 416.391 5 0 0 -15 -47.1093 162.641 5 0 0 15 170.719 404.046 1 0 0 -16 584.028 231.53 5 0 0 -17 -211.671 188.203 5 0 0 -18 1323.05 285.317 5 0 0 -19 -116.921 176.945 5 0 1 0 -1.70443 40.071 2 0 1 -1 10376.2 375.426 2 0 1 1 9857.23 359.285 1 0 1 2 273193 5408.75 1 0 1 -2 282081 5407.89 2 0 -1 2 276266 5433.98 1 0 1 3 30936.2 1000.15 1 0 -1 3 31227.4 1029.16 1 0 -1 4 38901.4 1321.14 1 0 1 4 38437.7 1316.12 1 0 -1 5 169539 4016.77 1 0 1 5 169858 4023.14 1 0 1 6 355922 7606.58 1 0 -1 6 352437 7647.65 1 0 1 7 43126.9 1739.8 1 0 -1 7 43290.2 1764.07 1 0 1 8 7692.53 744.734 1 0 -1 8 6573.62 730.277 1 0 1 9 40584.6 1894.91 1 0 -1 9 41395.4 1958.05 1 0 1 10 81859.3 3095.12 1 0 -1 10 90454.8 3250.73 1 0 1 -10 90410.7 3126.64 2 0 1 11 11991.9 1129.01 1 0 1 -11 12983.2 1115.07 2 0 -1 11 13283.5 1256.1 1 0 -1 12 20189.2 1590.96 1 0 1 12 21466.3 1598.15 1 0 1 -12 20707.2 1517.89 2 0 1 -13 13001.3 691.365 5 0 -1 -13 13394.2 707.123 5 0 1 13 15248.3 1413.99 1 0 1 -13 14972.1 1345.42 2 0 -1 13 14325.4 1407.55 1 0 -1 14 2504.05 705.465 1 0 -1 -14 2943.08 636.145 2 0 1 -14 2531.42 615.102 2 0 1 -14 2852.42 342.332 5 0 -1 -14 2263.01 320.974 5 0 1 14 2417.17 666.327 1 0 -1 -15 817.745 242.634 5 0 1 -15 1293.37 257.831 5 0 -1 -16 25610.3 1077.54 5 0 1 -16 20848.4 985.555 5 0 1 -17 2240.73 340.071 5 0 -1 -17 2933.97 364.509 5 0 1 -18 33808.5 1268.64 5 0 -1 -18 30685.5 1236.97 5 0 -1 -19 2305.18 327.058 5 0 1 -19 2484.1 334.778 5 0 1 -20 -68.9524 130.875 5 0 2 0 842671 15713.6 2 0 2 -1 9981.01 323.472 3 0 2 -1 10423.9 481.376 2 0 2 1 10205.4 487.148 2 0 2 2 40047.4 1149.52 1 0 2 -2 42602.6 1207.17 2 0 2 3 19058.6 769.931 1 0 -2 3 18301 773.943 1 0 2 -3 19418.6 787.258 2 0 -2 4 179737 4017.16 1 0 2 4 172233 3921.55 1 0 2 -4 173239 3946.01 2 0 -2 5 60445.1 1949.14 1 0 2 5 59387.3 1877.72 1 0 2 -5 62848.2 1913.58 2 0 -2 6 14869.2 934.615 1 0 2 6 14764.7 887.219 1 0 2 -6 12611.3 826.158 2 0 -2 7 50730 1985.52 1 0 2 -7 48152 1855.61 2 0 2 7 48946.9 1895.4 1 0 2 8 3411.56 502.364 1 0 -2 8 2953.7 526.252 1 0 2 -8 3039.47 486.729 2 0 2 9 963.444 309.445 1 0 -2 9 1827.69 442.065 1 0 2 -9 1277.98 358.115 2 0 2 10 87795.5 3157.31 1 0 -2 10 87016.7 3274.55 1 0 2 -10 87042.5 3112.09 2 0 -2 11 -221.018 263.13 1 0 2 11 112.35 232.386 1 0 2 -11 238.339 286.232 2 0 2 12 7901.07 961.702 1 0 -2 12 8532.95 1066.5 1 0 2 -12 6596.93 881.123 2 0 2 13 16820.5 1513.46 1 0 2 -13 19509.4 1557.25 2 0 -2 -13 16572.3 804.863 5 0 2 -13 16904.2 790.265 5 0 2 14 2085.42 620.728 1 0 2 -14 2870.13 344.88 5 0 2 -14 1931.86 610.463 2 0 -2 -14 2786.67 357.542 5 0 -2 -15 67668.8 2007.91 5 0 2 -15 67420.7 1972.16 5 0 2 15 68605.7 3455.23 1 0 -2 -16 811.35 225.962 5 0 2 -16 1144.07 256.035 5 0 2 -17 7618.37 575.131 5 0 -2 -17 7551.73 593.547 5 0 2 -18 9394.04 625.148 5 0 -2 -18 9391.44 639.036 5 0 2 -19 1943.48 284.503 5 0 2 -20 -44.8952 140.406 5 0 3 0 -16.604 125.604 2 0 3 -1 73088.3 1969.91 2 0 3 1 72772.4 1964.51 2 0 3 -1 74816.1 1625.06 3 0 3 2 29547.7 1026.67 1 0 3 -2 29235.6 738.592 3 0 3 2 30196.2 1106.57 2 0 3 -2 30244.5 1084.48 2 0 3 3 15278.8 735.791 1 0 3 -3 15168.1 768.211 2 0 3 -4 341876 7167.31 2 0 3 4 344422 7095.76 1 0 3 -5 5702.52 537.178 2 0 3 5 4280.62 455.931 1 0 3 -6 157.897 185.975 2 0 3 6 48.2778 180.8 1 0 3 7 266473 6160.62 1 0 3 -7 259251 6174.15 2 0 -3 8 170418 4736.81 1 0 3 -8 167209 4597.07 2 0 3 8 173765 4590.37 1 0 3 -9 78651.5 2868.53 2 0 3 9 78911.1 2852.65 1 0 3 -10 488.425 316.967 2 0 3 10 744.961 303.873 1 0 3 11 42958.2 2230.75 1 0 3 -11 44972.3 2255.42 2 0 3 12 157.475 263.076 1 0 3 -12 2.30198 268.907 2 0 -3 -13 3673.64 385.015 5 0 3 13 4033.73 782.665 1 0 3 -13 3165.98 342.651 5 0 3 -13 4120.86 771.343 2 0 3 14 3788.36 808.74 1 0 -3 -14 5454.87 478.734 5 0 3 -14 4668.66 429.966 5 0 3 -14 3892.63 778.213 2 0 -3 -15 4446.8 456.802 5 0 3 -15 4700.52 440.046 5 0 -3 -16 4324.49 457.859 5 0 3 -16 4335.47 430.652 5 0 -3 -17 381.197 216.33 5 0 3 -17 310.499 201.68 5 0 3 -18 3.56409 156.768 5 0 3 -19 2549.7 315.958 5 0 3 -20 8159.09 506.932 5 0 3 -21 6916.59 408.49 5 0 4 0 5483.27 514.255 2 0 4 -1 -76.5213 206.988 2 0 4 -1 63.7116 112.854 3 0 4 1 9.44004 210.574 2 0 4 -2 82974.9 2268.26 2 0 4 2 80897.7 2277.72 2 0 4 2 77909.9 2123 1 0 4 -3 19157.5 963.138 2 0 4 3 19440.4 928.962 1 0 4 -4 213817 4956.49 2 0 4 4 213963 4841.44 1 0 4 -5 149920 3880.5 2 0 4 5 147438 3737.83 1 0 4 -6 2751.46 449.912 2 0 4 6 3021.54 413.901 1 0 4 7 196659 4999.75 1 0 4 -7 202033 5170.1 2 0 4 -8 83493.9 2953.41 2 0 4 8 82486.8 2870.31 1 0 4 -9 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