#------------------------------------------------------------------------------ #$Date: 2020-04-28 23:24:28 +0300 (Tue, 28 Apr 2020) $ #$Revision: 251239 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557938.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_1557938 loop_ _publ_author_name 'Zhai, Yi-Jie' 'Huo, Guang-Ming' 'Zhang, Qiang' 'Li, Ding' 'Wang, Da-Cheng' 'Qi, Jian-Zhao' 'Han, Wen-Bo' 'Gao, Jin-Ming' _publ_section_title ; Phaeosphaones: Tyrosinase Inhibitory Thiodiketopiperazines from an Endophytic Phaeosphaeria fuckelii ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.0c00046 _journal_year 2020 _chemical_absolute_configuration syn _chemical_formula_moiety 'C17 H19 N3 O3 S2' _chemical_formula_sum 'C17 H19 N3 O3 S2' _chemical_formula_weight 377.47 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2019-04-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 93.931(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.2397(5) _cell_length_b 10.6635(10) _cell_length_c 12.6809(11) _cell_measurement_reflns_used 8943 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 74.802 _cell_measurement_theta_min 3.494 _cell_volume 841.76(13) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 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 ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_unetI/netI 0.0584 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 14366 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.061 _diffrn_reflns_theta_min 3.494 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.068 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.4076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1536 before and 0.1122 after correction. The Ratio of minimum to maximum transmission is 0.5407. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.489 _exptl_crystal_description block _exptl_crystal_F_000 396 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.204 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.103 _refine_ls_abs_structure_details ; Flack x determined using 1214 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.162(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 230 _refine_ls_number_reflns 2979 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0592 _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^)+(0.1076P)^2^+0.6518P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1538 _refine_ls_wR_factor_ref 0.1568 _reflns_Friedel_coverage 0.865 _reflns_Friedel_fraction_full 0.962 _reflns_Friedel_fraction_max 0.971 _reflns_number_gt 2809 _reflns_number_total 2979 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np0c00046_si_002.cif _cod_data_source_block cu_0403_13_0m _cod_database_code 1557938 _shelxl_version_number 2013-4 _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_max 0.862 _shelx_estimated_absorpt_t_min 0.710 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(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: C5(H5), C12(H12) 2.b Aromatic/amide H refined with riding coordinates: N1(H1), N3(H3), C9(H9), C10(H10), C11(H11), C14(H14), C16(H16) 2.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C) 2.d Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; TITL cu_0403_13_0m in P2(1) CELL 1.54184 6.2397 10.6635 12.6809 90 93.9307 90 ZERR 2 0.0005 0.001 0.0011 0 0.0052 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 34 38 6 6 4 L.S. 18 0 0 PLAN 20 SIZE 0.05 0.12 0.08 TEMP -123(2) fmap 2 53 acta SHEL 999 0.837 REM REM REM WGHT 0.107600 0.651800 FVAR 0.36604 S1 5 0.486713 0.608107 0.747725 11.00000 0.01966 0.02571 = 0.02747 -0.00253 0.00357 -0.00195 S3 5 0.393455 0.779720 0.805648 11.00000 0.01928 0.02911 = 0.04039 -0.00684 0.00509 0.00021 O1 4 0.970591 0.686890 0.641064 11.00000 0.02816 0.03242 = 0.02244 0.00040 0.01280 -0.00142 O2 4 0.854280 0.425228 0.878740 11.00000 0.03104 0.03448 = 0.02083 0.00592 0.00427 0.00102 AFIX 147 H2 2 0.973524 0.411301 0.911472 11.00000 -1.50000 AFIX 0 O3 4 0.785683 0.825489 1.010135 11.00000 0.03225 0.03379 = 0.02015 -0.00303 0.00542 -0.00107 N1 3 0.798367 0.312980 0.532106 11.00000 0.04470 0.03188 = 0.02406 -0.00295 0.01352 0.00228 AFIX 43 H1 2 0.834489 0.290885 0.468857 11.00000 -1.20000 AFIX 0 N2 3 0.790787 0.833751 0.732920 11.00000 0.02440 0.02778 = 0.02421 0.00421 0.00648 0.00125 N3 3 0.817785 0.665897 0.896434 11.00000 0.02416 0.02817 = 0.01413 -0.00011 0.00128 0.00220 AFIX 43 H3 2 0.875694 0.616760 0.946348 11.00000 -1.20000 AFIX 0 C1 1 0.620767 0.329823 0.680569 11.00000 0.02842 0.02491 = 0.02163 -0.00021 0.00680 0.00317 C2 1 0.781922 0.617909 0.790682 11.00000 0.01919 0.03021 = 0.01554 -0.00154 0.00529 -0.00216 C3 1 0.666948 0.856547 0.824462 11.00000 0.01966 0.02585 = 0.01793 -0.00046 0.00738 -0.00481 C4 1 0.860015 0.714977 0.714528 11.00000 0.01732 0.02583 = 0.02335 0.00196 0.00236 -0.00022 C5 1 0.887120 0.488050 0.782341 11.00000 0.02281 0.02567 = 0.02210 0.00312 0.00605 0.00311 AFIX 13 H5 2 1.045102 0.500442 0.777891 11.00000 -1.20000 AFIX 0 C6 1 0.805304 0.410366 0.689255 11.00000 0.02546 0.02384 = 0.02489 0.00132 0.00713 0.00523 C7 1 0.765406 0.782837 0.920475 11.00000 0.02237 0.02783 = 0.02146 0.00414 0.00771 -0.00028 C8 1 0.620726 0.270052 0.581027 11.00000 0.03625 0.02944 = 0.02150 -0.00214 0.00367 0.00399 C9 1 0.908685 0.395617 0.598522 11.00000 0.03587 0.03479 = 0.03018 0.00317 0.01123 0.00272 AFIX 43 H9 2 1.038286 0.436683 0.583599 11.00000 -1.20000 AFIX 0 C10 1 0.465880 0.185218 0.545554 11.00000 0.04716 0.02505 = 0.03301 0.00194 0.00317 0.00229 AFIX 43 H10 2 0.471374 0.145239 0.478845 11.00000 -1.20000 AFIX 0 C11 1 0.452978 0.299943 0.746456 11.00000 0.02978 0.02980 = 0.02449 0.00461 0.00775 0.00453 AFIX 43 H11 2 0.449553 0.336281 0.814720 11.00000 -1.20000 AFIX 0 C12 1 0.633448 0.997046 0.845575 11.00000 0.02920 0.02581 = 0.02487 -0.00497 0.00818 0.00112 AFIX 13 H12 2 0.574078 1.035013 0.777618 11.00000 -1.20000 AFIX 0 C13 1 0.845732 1.061052 0.874226 11.00000 0.03710 0.03176 = 0.03370 -0.00146 0.00133 -0.00785 AFIX 137 H13A 2 0.898225 1.036421 0.945849 11.00000 -1.50000 H13B 2 0.826066 1.152197 0.871350 11.00000 -1.50000 H13C 2 0.950487 1.036022 0.824047 11.00000 -1.50000 AFIX 0 C14 1 0.296494 0.218051 0.710058 11.00000 0.03069 0.02953 = 0.04601 0.00423 0.00317 0.00121 AFIX 43 H14 2 0.181631 0.199914 0.753091 11.00000 -1.20000 AFIX 0 C15 1 0.472782 1.024352 0.927954 11.00000 0.03860 0.03342 = 0.03318 -0.00379 0.01302 0.00773 AFIX 137 H15A 2 0.337487 0.980784 0.908587 11.00000 -1.50000 H15B 2 0.446585 1.114859 0.930892 11.00000 -1.50000 H15C 2 0.531004 0.994963 0.997334 11.00000 -1.50000 AFIX 0 C16 1 0.300642 0.160136 0.611172 11.00000 0.03427 0.03097 = 0.04504 0.00534 -0.00458 -0.00319 AFIX 43 H16 2 0.189795 0.103177 0.588532 11.00000 -1.20000 AFIX 0 C17 1 0.776410 0.921733 0.642833 11.00000 0.06938 0.03118 = 0.02459 0.00896 0.02247 0.00735 AFIX 137 H17A 2 0.625246 0.934654 0.619082 11.00000 -1.50000 H17B 2 0.853378 0.886819 0.584742 11.00000 -1.50000 H17C 2 0.841060 1.002133 0.664869 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_0403_13_0m in P2(1) REM R1 = 0.0592 for 2809 Fo > 4sig(Fo) and 0.0623 for all 2979 data REM 230 parameters refined using 1 restraints END WGHT 0.1104 0.5708 REM Highest difference peak 1.204, deepest hole -0.450, 1-sigma level 0.103 Q1 1 0.6377 0.6090 0.7778 11.00000 0.05 1.20 Q2 1 0.5316 0.7868 0.8428 11.00000 0.05 0.92 Q3 1 0.3461 0.6095 0.7143 11.00000 0.05 0.85 Q4 1 0.2346 0.7808 0.7666 11.00000 0.05 0.65 Q5 1 0.4377 0.6943 0.7779 11.00000 0.05 0.49 Q6 1 0.9262 0.8066 1.0420 11.00000 0.05 0.44 Q7 1 0.9589 0.6788 0.9237 11.00000 0.05 0.41 Q8 1 0.6389 0.8119 0.9811 11.00000 0.05 0.38 Q9 1 0.7112 0.4187 0.8468 11.00000 0.05 0.37 Q10 1 0.4129 0.7876 0.9052 11.00000 0.05 0.36 Q11 1 1.0355 0.4920 0.8207 11.00000 0.05 0.36 Q12 1 0.6343 0.1734 0.5790 11.00000 0.05 0.36 Q13 1 0.6823 0.6701 0.8650 11.00000 0.05 0.35 Q14 1 0.3145 1.0526 0.8940 11.00000 0.05 0.35 Q15 1 0.3093 0.3156 0.7030 11.00000 0.05 0.34 Q16 1 1.1139 0.7032 0.6796 11.00000 0.05 0.33 Q17 1 0.7837 0.9073 0.8410 11.00000 0.05 0.33 Q18 1 0.7676 0.5165 0.7597 11.00000 0.05 0.32 Q19 1 0.3255 0.1597 0.5008 11.00000 0.05 0.31 Q20 1 0.9888 1.0541 0.9005 11.00000 0.05 0.30 ; _shelx_res_checksum 66656 _shelx_hkl_file ; -1 0 0 281.26 21.10 1 0 0 255.95 21.10 -2 0 0 32.77 2.98 2 0 0 39.94 3.09 2 0 0 35.42 3.59 2 0 0 36.51 3.00 3 0 0 264.99 21.78 3 0 0 271.13 21.99 -3 0 0 285.54 21.68 -4 0 0 1.25 0.80 4 0 0 1.49 0.43 4 0 0 2.04 1.10 4 0 0 2.57 1.77 -4 0 0 -0.62 1.22 -4 0 0 1.23 1.33 4 0 0 0.59 1.33 -4 0 0 0.15 0.69 4 0 0 2.03 1.21 -4 0 0 -0.73 2.31 4 0 0 -0.68 1.36 5 0 0 30.61 3.17 5 0 0 27.48 3.07 5 0 0 26.13 3.60 -5 0 0 27.92 2.63 -5 0 0 33.05 4.68 -5 0 0 31.16 2.77 5 0 0 27.28 3.34 -5 0 0 26.15 3.46 -5 0 0 27.44 3.13 -6 0 0 16.00 1.86 -6 0 0 18.69 2.37 -6 0 0 14.44 1.80 6 0 0 15.26 2.28 6 0 0 13.23 2.27 6 0 0 14.81 2.82 -6 0 0 14.32 2.88 -7 0 0 28.00 3.87 -7 0 0 27.30 2.47 7 0 0 22.62 2.58 -7 0 0 27.52 2.59 7 0 0 28.24 2.71 -7 0 0 29.56 2.41 0 1 0 0.07 0.07 1 -1 0 261.97 21.38 -1 -1 0 277.64 21.37 -1 1 0 268.14 21.38 -1 1 0 279.84 21.35 2 -1 0 231.89 16.63 -2 -1 0 202.82 16.58 -2 1 0 217.82 16.65 2 1 0 194.81 16.58 2 1 0 190.80 16.63 2 1 0 221.15 16.75 -3 -1 0 215.72 18.32 3 -1 0 255.34 18.45 -3 1 0 215.49 18.28 3 1 0 244.53 18.37 -3 1 0 224.15 18.36 3 1 0 230.65 18.49 -4 -1 0 5.41 2.13 -4 -1 0 8.30 1.43 -4 -1 0 8.22 1.49 -4 -1 0 5.71 1.17 4 -1 0 8.10 0.91 4 -1 0 7.74 1.32 4 -1 0 5.35 1.34 4 -1 0 3.95 1.95 -4 1 0 7.77 1.62 4 1 0 8.36 1.53 4 1 0 4.78 1.34 4 1 0 6.98 4.08 -4 1 0 7.72 1.21 -4 1 0 10.78 1.63 4 1 0 5.18 1.34 -4 1 0 6.78 4.27 -5 -1 0 33.78 2.84 -5 -1 0 33.38 3.23 -5 -1 0 29.58 4.05 5 -1 0 31.39 3.07 5 -1 0 27.83 3.58 5 -1 0 31.19 3.16 5 -1 0 24.11 3.67 -5 -1 0 27.30 2.70 -5 1 0 25.60 2.68 5 1 0 25.21 3.37 5 1 0 24.46 3.60 -5 1 0 29.44 3.24 5 1 0 25.97 3.25 -5 1 0 39.77 5.68 -5 1 0 31.26 2.86 5 1 0 25.89 3.14 -6 -1 0 6.76 1.48 -6 -1 0 7.98 2.28 6 -1 0 6.94 1.42 6 -1 0 9.30 1.74 6 -1 0 7.68 1.37 -6 -1 0 7.03 1.30 -6 -1 0 4.85 1.05 -6 1 0 5.20 1.06 -6 1 0 5.84 1.43 6 1 0 4.09 1.36 6 1 0 5.28 1.36 -6 1 0 7.43 1.42 6 1 0 5.05 1.37 6 1 0 7.07 1.65 -7 -1 0 31.70 2.96 -7 -1 0 32.01 2.80 7 -1 0 31.71 2.94 7 -1 0 33.70 3.07 7 1 0 30.22 3.09 -7 1 0 34.58 3.05 -7 1 0 37.43 2.96 7 1 0 26.07 2.97 -7 1 0 36.07 2.83 1 -2 0 171.69 11.98 -1 -2 0 139.63 11.93 -1 2 0 132.68 11.89 1 2 0 161.28 11.94 -2 -2 0 311.49 21.93 2 -2 0 255.64 21.93 -2 2 0 261.79 21.85 2 2 0 299.99 21.93 -2 2 0 272.22 21.87 -2 2 0 264.95 21.95 3 -2 0 55.73 4.59 -3 -2 0 51.92 4.44 3 2 0 57.32 4.80 -3 2 0 48.81 4.32 3 2 0 53.54 4.46 -3 2 0 52.54 4.74 -3 2 0 49.51 4.46 3 2 0 45.77 4.74 4 -2 0 79.30 6.66 4 -2 0 74.16 6.94 -4 -2 0 87.14 6.45 4 -2 0 73.44 6.25 -4 -2 0 71.53 6.33 -4 -2 0 68.66 7.25 4 -2 0 77.32 6.59 4 -2 0 67.97 7.07 -4 -2 0 72.47 6.63 -4 -2 0 69.58 7.02 -4 -2 0 85.44 6.79 4 -2 0 67.65 6.62 4 2 0 81.48 6.64 -4 2 0 77.59 6.39 4 2 0 84.37 6.76 4 2 0 84.90 6.78 4 2 0 79.73 7.18 -4 2 0 91.44 6.86 4 2 0 86.78 6.65 -5 -2 0 133.68 10.61 -5 -2 0 127.27 10.95 -5 -2 0 125.05 10.41 5 -2 0 132.56 10.57 5 -2 0 123.41 10.79 5 -2 0 138.11 10.67 -5 -2 0 128.18 10.40 -5 2 0 135.14 10.69 5 2 0 121.34 10.57 5 2 0 136.12 10.65 5 2 0 121.77 10.65 5 2 0 124.91 10.82 5 2 0 129.58 10.74 -5 2 0 142.99 10.51 -5 2 0 121.21 10.38 6 -2 0 38.04 3.87 6 -2 0 33.41 4.12 -6 -2 0 44.81 4.76 -6 -2 0 38.37 4.78 -6 -2 0 43.55 4.07 6 -2 0 45.13 4.06 -6 -2 0 40.25 3.66 6 2 0 41.07 4.14 6 2 0 41.57 4.27 -6 2 0 47.01 3.77 -6 2 0 43.87 4.21 6 2 0 41.42 4.01 -6 2 0 45.19 3.74 6 2 0 44.45 4.00 -7 -2 0 -0.03 0.48 7 -2 0 1.91 0.68 -7 -2 0 0.96 0.75 7 -2 0 0.51 1.68 7 2 0 -0.79 0.72 -7 2 0 1.02 0.65 7 2 0 2.05 0.67 -7 2 0 0.91 0.81 7 2 0 -0.51 0.81 0 3 0 0.22 0.45 0 3 0 -0.10 0.19 1 -3 0 115.82 10.25 -1 -3 0 118.67 10.19 1 3 0 133.92 10.22 -1 3 0 139.40 10.16 1 3 0 136.57 10.21 -2 -3 0 299.62 22.84 2 3 0 309.58 22.85 -2 3 0 292.09 22.78 -2 3 0 255.84 22.75 3 -3 0 36.48 3.90 3 -3 0 37.94 3.83 -3 -3 0 37.23 3.66 -3 -3 0 43.09 4.49 3 3 0 46.50 3.74 -3 3 0 36.96 4.07 -3 3 0 45.85 3.69 3 3 0 32.65 4.08 -3 3 0 41.64 3.48 3 3 0 40.66 4.32 3 3 0 43.26 4.30 -4 -3 0 6.35 1.67 4 -3 0 2.35 1.17 -4 -3 0 3.22 1.75 4 -3 0 4.30 1.09 -4 -3 0 3.95 1.98 4 -3 0 4.61 1.07 4 -3 0 1.63 1.60 -4 3 0 5.42 1.56 4 3 0 3.96 1.45 4 3 0 3.92 1.17 4 3 0 2.45 1.17 -5 -3 0 18.41 2.95 5 -3 0 11.33 2.16 5 -3 0 8.12 1.81 5 -3 0 13.49 2.04 5 -3 0 10.73 2.16 5 3 0 17.78 2.51 -5 3 0 9.87 2.35 -5 3 0 16.91 2.68 5 3 0 6.96 4.09 5 3 0 13.88 2.02 5 3 0 12.35 2.11 6 -3 0 70.02 7.34 -6 -3 0 91.16 7.10 6 -3 0 79.22 7.26 6 3 0 100.62 7.97 -6 3 0 79.55 7.10 -6 3 0 95.03 7.35 7 -3 0 24.49 2.38 -7 -3 0 28.07 2.30 -7 -3 0 26.83 2.75 7 -3 0 25.34 2.53 -7 3 0 23.44 2.31 7 3 0 20.80 2.57 -7 3 0 31.18 2.57 -7 3 0 30.94 2.51 0 -4 0 75.25 6.04 0 4 0 82.01 6.22 0 4 0 71.17 6.03 -1 -4 0 305.24 23.92 -1 4 0 294.42 23.88 1 4 0 311.27 23.95 1 4 0 314.38 23.93 -1 4 0 295.06 24.03 2 -4 0 9.04 1.49 -2 -4 0 7.01 1.05 -2 4 0 7.50 0.97 2 4 0 7.83 1.84 -2 4 0 5.92 0.83 2 4 0 6.49 1.07 -2 4 0 10.03 1.62 -3 -4 0 76.49 7.30 -3 -4 0 80.63 7.26 -3 -4 0 82.62 7.07 -3 -4 0 78.79 7.21 3 -4 0 92.46 6.96 3 -4 0 88.22 7.06 3 -4 0 87.15 7.44 3 -4 0 89.23 6.70 -3 -4 0 82.11 6.82 -3 -4 0 77.27 7.09 -3 4 0 75.07 6.81 3 4 0 76.53 7.19 -3 4 0 95.58 7.61 3 4 0 88.56 7.20 4 -4 0 74.81 7.86 -4 -4 0 91.05 7.47 4 -4 0 89.79 7.28 4 -4 0 95.91 6.89 4 -4 0 85.37 7.18 -4 -4 0 87.27 7.80 -4 -4 0 72.16 7.33 -4 -4 0 81.45 7.54 -4 4 0 77.02 7.31 4 4 0 79.78 7.64 4 4 0 84.43 7.37 -4 4 0 102.33 7.54 -4 4 0 96.34 7.56 4 4 0 87.63 7.31 -4 4 0 98.35 7.23 4 4 0 84.15 7.26 4 4 0 70.90 7.67 5 -4 0 37.13 3.68 5 -4 0 32.37 3.94 -5 -4 0 32.44 3.70 -5 -4 0 34.75 3.93 -5 -4 0 32.56 3.14 5 -4 0 33.93 3.37 5 -4 0 31.41 3.43 5 4 0 35.03 5.78 5 4 0 35.31 3.52 5 4 0 38.61 3.84 -5 4 0 42.45 3.87 -5 4 0 38.46 3.51 5 4 0 39.76 3.64 5 4 0 37.96 4.00 6 -4 0 30.67 3.33 -6 -4 0 39.33 3.66 -6 -4 0 37.59 2.96 -6 -4 0 30.70 3.29 6 -4 0 28.68 3.11 6 -4 0 27.96 3.45 -6 4 0 33.11 3.39 6 4 0 33.34 3.29 6 4 0 29.67 3.46 6 4 0 36.73 3.49 6 4 0 31.89 3.26 -6 4 0 37.78 3.25 6 4 0 29.75 3.50 -7 -4 0 32.28 2.73 -7 -4 0 32.88 2.94 7 4 0 34.47 3.06 7 4 0 31.21 3.24 7 4 0 29.45 2.92 -7 4 0 34.16 2.92 -7 4 0 30.74 2.75 -7 4 0 35.60 2.93 0 5 0 0.60 0.37 0 5 0 0.92 0.79 0 5 0 0.31 0.66 -1 -5 0 185.60 14.43 1 5 0 178.12 14.47 1 5 0 202.66 14.49 -1 5 0 173.90 14.41 -1 5 0 173.26 14.63 2 -5 0 45.92 4.40 -2 -5 0 45.16 4.11 -2 -5 0 49.76 4.96 -2 -5 0 42.70 4.59 2 -5 0 43.58 4.17 -2 -5 0 44.63 4.40 -2 5 0 57.78 4.02 -2 5 0 45.99 3.94 2 5 0 55.19 4.22 3 -5 0 50.61 5.00 3 -5 0 59.66 5.14 -3 -5 0 56.70 5.31 -3 -5 0 53.82 5.31 3 -5 0 61.01 5.01 3 -5 0 64.17 4.76 -3 -5 0 58.40 4.97 -3 -5 0 58.06 5.35 3 -5 0 59.40 5.58 -3 -5 0 52.56 5.20 3 5 0 56.51 5.34 3 5 0 68.17 5.51 -4 -5 0 6.77 1.78 4 -5 0 8.58 1.91 4 -5 0 8.86 1.56 -4 -5 0 9.48 1.72 -4 -5 0 10.20 1.46 -4 -5 0 12.71 2.41 4 -5 0 7.40 1.25 4 -5 0 10.88 1.72 -4 5 0 8.33 1.95 -4 5 0 5.77 1.86 4 5 0 6.18 2.39 -4 5 0 8.95 1.55 4 5 0 8.60 1.59 4 5 0 9.34 1.78 -5 -5 0 3.73 1.84 -5 -5 0 6.94 1.06 5 -5 0 7.44 1.67 5 -5 0 6.91 1.59 5 -5 0 6.94 1.20 -5 -5 0 8.64 1.75 5 -5 0 7.70 1.33 5 5 0 5.20 1.46 -5 5 0 8.91 1.32 5 5 0 3.87 1.86 5 5 0 7.04 1.51 5 5 0 8.52 3.40 -5 5 0 4.42 1.86 -5 5 0 8.40 1.78 5 5 0 5.29 1.21 6 -5 0 11.13 1.96 -6 -5 0 10.84 1.35 6 -5 0 12.29 1.90 6 -5 0 10.52 1.62 6 -5 0 10.40 1.75 6 -5 0 10.13 1.66 -6 -5 0 13.15 2.09 6 5 0 6.89 1.71 6 5 0 10.01 1.75 6 5 0 9.82 1.90 6 5 0 10.88 1.73 -6 5 0 12.40 2.00 -6 5 0 12.55 1.52 7 -5 0 1.01 1.18 -7 -5 0 0.21 0.37 -7 -5 0 0.56 0.91 7 5 0 -0.87 0.69 -7 5 0 0.73 0.74 7 5 0 0.42 0.79 -7 5 0 0.38 0.50 7 5 0 -0.66 0.74 -7 5 0 1.35 0.60 0 -6 0 98.34 8.12 0 -6 0 90.57 8.36 0 -6 0 111.26 8.62 0 6 0 110.38 8.66 1 -6 0 91.91 8.62 -1 -6 0 101.96 8.22 1 -6 0 100.18 8.22 -1 -6 0 115.91 8.03 -1 -6 0 99.32 8.58 1 -6 0 89.48 8.08 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6 0 20.16 5.02 5 6 0 18.18 2.40 -6 -6 0 4.18 1.03 6 -6 0 1.94 1.54 -6 -6 0 5.67 1.02 6 -6 0 3.31 0.98 6 6 0 4.37 1.13 6 6 0 2.12 1.06 6 6 0 2.76 0.92 -6 6 0 3.29 0.72 -6 6 0 5.00 1.13 -6 6 0 2.61 1.05 6 6 0 1.24 0.88 0 -7 0 1.11 0.95 0 -7 0 0.25 0.81 0 -7 0 -0.72 0.90 0 -7 0 0.26 1.39 0 -7 0 -0.01 1.45 0 -7 0 1.10 1.35 0 7 0 -0.14 0.74 -1 -7 0 54.40 4.66 1 -7 0 51.88 4.47 1 -7 0 49.30 4.56 -1 -7 0 51.15 4.69 -1 -7 0 53.47 4.53 1 -7 0 53.04 5.41 -1 -7 0 50.91 5.03 1 -7 0 53.90 4.63 -2 -7 0 22.64 3.08 2 -7 0 22.93 2.86 2 -7 0 24.12 3.66 2 -7 0 30.66 3.03 -2 -7 0 33.03 3.35 2 -7 0 26.82 4.35 -2 -7 0 19.44 4.59 2 7 0 30.14 3.59 2 7 0 24.87 3.49 2 7 0 21.99 3.79 3 -7 0 37.91 3.51 3 -7 0 33.89 4.06 -3 -7 0 34.51 3.62 -3 -7 0 30.91 3.67 3 -7 0 38.58 3.38 3 -7 0 42.95 4.02 3 -7 0 38.09 3.13 -3 -7 0 33.27 3.69 -3 -7 0 33.37 3.48 -3 -7 0 35.50 4.13 3 7 0 33.80 3.91 3 7 0 33.21 4.24 4 -7 0 8.94 1.82 -4 -7 0 10.48 1.74 4 -7 0 9.38 1.61 -4 -7 0 6.20 1.56 -4 -7 0 9.25 1.74 4 -7 0 6.66 1.36 -4 -7 0 8.60 1.88 4 -7 0 9.70 2.44 4 7 0 7.25 1.52 -4 7 0 6.21 1.48 -4 7 0 11.84 2.49 4 7 0 5.63 1.51 4 7 0 5.59 1.34 5 -7 0 21.33 3.05 5 -7 0 23.33 2.48 -5 -7 0 24.87 2.87 5 -7 0 21.30 2.77 5 -7 0 25.09 2.79 -5 -7 0 26.69 2.45 -5 7 0 26.80 2.62 5 7 0 28.92 3.01 5 7 0 23.29 2.54 -5 7 0 20.93 3.23 5 7 0 23.12 2.64 6 -7 0 5.29 1.11 -6 7 0 6.80 1.43 -6 7 0 6.10 0.93 0 -8 0 24.99 3.36 0 -8 0 28.10 2.79 0 -8 0 23.21 2.85 0 -8 0 25.71 3.17 0 -8 0 28.38 2.67 0 8 0 25.07 2.56 -1 -8 0 31.65 2.96 1 -8 0 30.02 4.58 1 -8 0 30.82 3.06 1 -8 0 28.81 2.88 1 -8 0 29.49 2.89 -1 -8 0 30.74 3.06 -1 -8 0 30.57 4.58 1 -8 0 30.49 3.41 -1 -8 0 25.49 3.41 -1 -8 0 30.04 3.14 -2 -8 0 15.32 2.00 2 -8 0 12.68 2.04 -2 -8 0 17.01 2.23 2 -8 0 15.67 2.70 2 -8 0 13.60 2.10 -2 -8 0 16.00 2.30 2 -8 0 15.64 1.92 -2 -8 0 13.11 2.49 -2 -8 0 13.43 2.30 2 -8 0 11.39 2.42 2 8 0 14.19 2.48 2 8 0 11.92 2.81 2 8 0 15.02 3.17 3 -8 0 11.40 1.97 3 -8 0 6.82 1.67 3 -8 0 11.49 2.62 3 -8 0 13.87 1.76 -3 -8 0 10.68 1.66 -3 -8 0 9.43 1.94 -3 -8 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19.90 1.78 0 0 1 23.68 1.79 0 0 -1 21.25 1.78 0 0 -1 25.28 1.79 -2 0 -1 1000.00 73.43 2 0 1 947.42 73.41 2 0 1 859.15 73.42 -3 0 -1 5.45 1.17 3 0 1 15.25 6.64 -4 0 -1 3.31 0.95 4 0 1 4.67 1.67 -4 0 -1 2.83 1.29 4 0 1 4.56 1.20 -4 0 -1 6.86 3.04 4 0 1 3.33 0.58 4 0 1 5.16 2.04 -4 0 -1 5.24 1.42 4 0 1 4.61 1.20 5 0 1 60.15 6.10 5 0 1 71.60 5.77 5 0 1 69.95 5.69 -5 0 -1 65.71 5.52 -5 0 -1 54.52 7.09 5 0 1 58.90 5.86 -5 0 -1 65.38 5.42 -5 0 -1 70.48 5.80 -6 0 -1 15.12 2.32 6 0 1 24.08 3.84 6 0 1 16.41 2.33 -6 0 -1 16.69 3.86 -6 0 -1 13.97 1.90 -6 0 -1 17.39 1.89 6 0 1 16.40 2.23 6 0 1 14.01 2.73 7 0 1 0.53 0.69 7 0 1 0.54 0.66 -7 0 -1 1.99 0.81 -7 0 -1 0.72 0.51 7 0 1 0.82 1.52 7 -1 -1 7.44 1.40 -7 -1 1 10.64 1.50 -7 -1 1 14.20 2.47 7 -1 -1 8.96 1.51 -7 -1 1 10.73 1.18 -7 1 1 11.47 1.49 -7 1 1 10.02 1.26 7 1 -1 10.11 1.65 7 1 -1 6.75 1.50 7 1 -1 7.85 1.56 -7 1 1 9.19 1.20 -6 -1 1 15.98 2.00 6 -1 -1 19.23 2.59 -6 -1 1 18.70 2.48 6 -1 -1 19.05 2.40 -6 -1 1 18.44 2.19 6 -1 -1 19.04 2.44 -6 -1 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13 7.44 0.93 2 -7 -13 13.80 2.09 -2 -7 13 15.88 1.32 2 -7 -13 16.38 2.17 1 -7 -13 14.17 1.62 1 -7 -13 10.42 1.77 1 -7 -13 10.70 1.96 -1 -7 13 14.77 1.15 -1 7 13 14.91 1.28 0 -7 13 6.27 0.59 0 -7 -13 6.48 1.22 0 7 13 4.83 1.01 0 7 13 5.36 0.86 1 -7 13 8.54 0.77 -1 -7 -13 10.01 1.12 1 7 13 9.06 1.26 4 0 -14 0.62 1.37 -4 0 14 0.15 0.41 4 0 -14 0.03 0.90 -4 0 14 0.31 0.48 3 0 -14 24.73 3.29 -3 0 14 21.69 1.85 3 0 -14 17.45 2.12 -2 0 14 56.08 4.60 -2 0 14 49.58 4.75 -2 0 14 56.26 4.55 2 0 -14 63.48 4.99 -1 0 14 12.64 1.30 -1 0 14 13.20 1.50 -1 0 14 13.60 1.36 0 0 -14 6.01 1.11 0 0 -14 4.11 0.76 0 0 14 3.94 0.97 0 0 -14 -0.84 3.02 0 0 14 3.18 0.56 1 0 14 18.65 2.05 1 0 14 22.42 1.95 -1 0 -14 25.96 2.12 1 0 14 22.98 2.06 2 0 14 1.03 0.48 -2 0 -14 0.98 0.42 -2 0 -14 2.14 0.69 -3 0 -14 -0.05 0.39 3 0 14 -0.20 0.31 -3 0 -14 0.43 0.74 4 -1 -14 0.19 1.15 -4 1 14 -0.34 0.55 4 1 -14 0.07 0.80 3 -1 -14 7.11 1.87 3 -1 -14 2.35 0.95 3 -1 -14 3.40 1.03 3 1 -14 6.45 2.13 2 -1 -14 5.53 3.55 2 -1 -14 2.84 0.88 -2 -1 14 5.13 0.75 -2 -1 14 3.46 0.79 2 -1 -14 4.82 1.19 -2 1 14 4.18 0.76 -2 1 14 4.75 0.84 2 1 -14 -1.40 4.73 2 1 -14 3.61 0.91 -2 1 14 4.89 1.10 -1 -1 14 3.64 0.47 -1 -1 14 4.21 0.92 -1 -1 14 4.07 0.75 1 -1 -14 4.26 0.98 1 -1 -14 5.98 1.16 -1 -1 14 4.84 0.87 1 1 -14 2.19 3.62 -1 1 14 2.54 0.70 -1 1 14 3.94 0.78 1 1 -14 5.60 1.23 -1 1 14 3.20 0.57 0 -1 14 3.79 0.54 0 -1 -14 4.45 3.63 0 -1 14 2.78 0.70 0 -1 14 2.83 0.45 0 -1 -14 3.93 0.88 0 1 14 3.66 0.72 0 1 -14 -0.57 2.87 0 1 -14 4.39 1.07 0 1 14 5.01 0.83 -1 -1 -14 21.20 1.86 1 -1 14 21.04 1.87 1 1 14 17.08 1.73 2 -1 14 4.14 0.66 -2 -1 -14 4.32 0.94 -2 1 -14 4.76 1.66 3 -1 14 0.85 0.39 -3 -1 -14 -0.13 0.43 -3 -1 -14 0.83 0.62 3 1 14 0.07 0.25 -3 1 -14 0.00 0.41 3 -2 -14 20.04 2.95 3 -2 -14 16.78 1.98 -3 2 14 20.32 1.92 3 2 -14 15.98 1.90 -3 2 14 17.46 1.68 2 -2 -14 0.59 2.59 -2 -2 14 0.84 0.46 -2 -2 14 0.01 0.27 2 -2 -14 0.67 0.79 -2 2 14 0.74 0.53 2 2 -14 2.25 5.04 -2 2 14 0.79 0.55 2 2 -14 1.76 0.82 1 -2 -14 13.18 1.88 1 2 -14 15.77 1.79 -1 2 14 14.60 1.46 -1 2 14 13.46 1.40 0 -2 -14 0.35 0.72 0 -2 14 -1.01 0.80 0 -2 14 0.86 0.30 0 -2 -14 0.03 0.49 0 2 14 0.10 0.47 0 2 -14 1.23 0.66 0 2 -14 2.39 0.92 0 2 -14 -1.35 2.56 0 2 14 0.49 0.39 1 -2 14 3.03 0.44 1 -2 14 2.59 0.92 -1 -2 -14 2.34 0.84 -1 -2 -14 3.82 0.84 -1 2 -14 -1.77 2.88 -2 -2 -14 4.82 1.13 2 -2 14 5.05 0.83 2 2 14 8.18 0.75 -2 2 -14 11.63 2.02 2 2 14 6.64 0.79 2 2 14 6.74 1.05 -2 2 -14 9.23 1.09 3 -2 14 7.52 0.90 -3 -2 -14 9.50 1.06 3 -3 -14 0.28 0.89 -3 -3 14 0.28 0.27 3 -3 -14 0.21 1.20 -3 3 14 0.27 0.58 -3 3 14 0.25 0.67 3 3 -14 -0.82 0.93 -3 3 14 -0.11 0.62 2 -3 -14 0.62 1.58 2 3 -14 -3.58 7.18 -2 3 14 0.34 0.39 2 3 -14 1.59 0.67 -2 3 14 0.99 0.39 1 -3 -14 -0.17 1.11 1 -3 -14 0.68 0.73 -1 -3 14 1.19 0.30 1 3 -14 1.73 0.72 -1 3 14 1.67 0.53 -1 3 14 1.20 0.47 1 3 -14 1.61 3.01 0 -3 14 1.73 0.28 0 -3 -14 3.57 0.90 0 3 -14 1.14 2.77 0 3 -14 2.95 1.47 0 3 14 2.43 0.55 0 3 14 1.79 0.45 1 -3 14 1.62 0.85 -1 -3 -14 1.75 0.79 -1 -3 -14 0.69 0.69 1 -3 14 1.92 0.29 -1 3 -14 2.59 0.63 1 3 14 1.07 0.44 1 3 14 3.12 0.60 2 -3 14 3.10 0.46 2 -3 14 4.64 0.92 -2 -3 -14 3.45 1.38 -2 -3 -14 4.41 0.77 -2 3 -14 3.56 0.71 2 3 14 5.06 0.71 2 3 14 4.72 0.87 3 -4 -14 5.09 1.30 3 4 -14 5.94 1.13 -3 4 14 6.22 1.00 -3 4 14 5.50 0.93 2 -4 -14 23.40 4.97 2 -4 -14 22.99 2.36 2 -4 -14 19.15 3.01 2 4 -14 23.09 2.42 -2 4 14 25.71 2.05 1 -4 -14 4.12 2.61 -1 -4 14 1.76 0.25 -1 4 14 1.09 0.36 1 4 -14 0.73 0.72 -1 4 14 2.46 0.56 1 4 -14 1.35 1.25 0 4 14 28.15 2.35 0 4 -14 27.67 2.62 0 4 14 26.43 2.36 1 -4 14 13.03 0.99 -1 -4 -14 11.23 1.42 1 4 14 10.23 1.08 2 -4 14 2.37 0.34 2 4 14 2.07 0.48 -2 4 -14 2.57 0.77 2 -5 -14 3.31 0.93 2 -5 -14 1.93 1.98 2 -5 -14 1.13 1.55 -2 5 14 3.26 0.67 2 5 -14 3.20 0.84 -2 5 14 4.14 0.59 1 -5 -14 1.08 0.64 -1 -5 14 0.74 0.21 1 -5 -14 1.19 1.48 -1 5 14 0.44 0.38 1 5 -14 -0.07 1.67 -1 5 14 1.46 0.62 1 5 -14 0.85 0.81 0 -5 -14 3.49 0.78 0 -5 14 3.11 0.36 0 5 14 4.18 0.77 -1 -5 -14 3.60 0.71 -1 -5 -14 3.47 0.79 1 -5 14 2.77 0.36 1 5 14 3.46 0.69 1 5 14 3.24 0.67 1 -6 -14 5.71 1.99 1 -6 -14 5.60 1.05 -1 -6 14 4.63 0.51 -1 6 14 5.64 1.01 -1 6 14 6.82 0.78 0 -6 14 1.78 0.28 0 -6 -14 1.74 0.60 -3 0 15 0.27 0.56 3 0 -15 -0.29 0.81 2 0 -15 1.82 0.91 2 0 -15 0.24 0.86 -2 0 15 1.04 0.43 -1 0 15 -0.24 0.46 1 0 -15 2.13 0.76 1 0 -15 -0.57 0.60 -1 0 15 0.26 0.73 0 0 -15 5.43 0.78 0 0 -15 7.92 1.57 -1 0 -15 7.36 0.94 1 0 15 8.14 1.04 -1 0 -15 6.06 1.08 2 0 15 1.08 0.41 -2 0 -15 1.48 0.81 3 -1 -15 7.37 1.31 3 1 -15 5.01 1.09 2 -1 -15 1.50 0.81 2 -1 -15 2.78 0.95 2 1 -15 2.16 1.05 -2 1 15 2.34 0.54 -2 1 15 3.48 1.31 1 1 -15 26.26 2.48 -1 1 15 22.69 2.36 0 -1 -15 3.45 0.59 0 -1 15 3.08 0.78 0 -1 -15 2.43 0.84 0 1 -15 1.21 0.90 0 1 -15 3.17 0.67 0 1 15 2.73 0.58 0 1 15 2.52 0.76 0 1 15 2.26 0.52 -1 -1 -15 11.23 1.43 1 -1 15 9.76 1.37 -1 -1 -15 11.12 1.60 -1 1 -15 9.27 1.59 -2 -1 -15 3.77 0.58 2 -2 -15 1.34 0.87 -2 -2 15 1.56 0.60 -2 2 15 1.62 0.66 -2 2 15 1.91 0.49 2 2 -15 2.09 0.91 1 -2 -15 1.08 0.73 -1 -2 15 0.50 0.29 1 -2 -15 -0.58 1.06 1 2 -15 1.34 1.01 -1 2 15 0.42 0.74 1 2 -15 0.54 0.66 -1 2 15 0.41 0.35 0 2 15 4.06 0.77 0 2 -15 4.32 0.92 0 2 -15 3.03 1.35 0 2 15 4.81 0.80 -1 -2 -15 12.51 1.69 1 2 15 13.23 1.31 1 2 15 16.62 1.54 -1 2 -15 15.55 1.43 2 -3 -15 7.73 1.35 2 3 -15 6.50 1.13 -2 3 15 6.05 0.86 -2 3 15 5.94 1.00 1 -3 -15 1.83 1.40 -1 -3 15 1.32 0.26 1 3 -15 2.51 1.02 -1 3 15 1.34 0.40 1 3 -15 2.70 0.71 -1 3 15 1.57 0.42 0 -3 15 0.09 0.22 0 -3 -15 1.48 0.79 0 3 15 0.22 0.37 0 3 -15 0.68 0.57 0 3 15 -0.36 0.57 -1 -3 -15 2.68 0.68 -1 -3 -15 3.28 0.83 1 3 15 2.79 0.40 1 3 15 2.26 0.42 1 3 15 3.11 0.50 -1 3 -15 1.63 0.58 -1 -4 15 0.96 0.21 1 -4 -15 1.07 0.54 1 4 -15 1.90 0.68 -1 4 15 1.28 0.44 -1 4 15 0.80 0.28 0 -4 15 12.70 1.00 0 -4 -15 11.63 1.16 0 4 15 10.88 1.10 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14915 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.4867(2) 0.60811(16) 0.74772(11) 0.0242(4) Uani 1 1 d . . . . . S3 S 0.3935(2) 0.77972(15) 0.80565(13) 0.0295(4) Uani 1 1 d . . . . . O1 O 0.9706(7) 0.6869(4) 0.6411(3) 0.0272(10) Uani 1 1 d . . . . . O2 O 0.8543(7) 0.4252(5) 0.8787(3) 0.0287(10) Uani 1 1 d . . . . . H2 H 0.9735 0.4113 0.9115 0.043 Uiso 1 1 calc GR . . . . O3 O 0.7857(7) 0.8255(4) 1.0101(3) 0.0286(10) Uani 1 1 d . . . . . N1 N 0.7984(10) 0.3130(6) 0.5321(4) 0.0330(13) Uani 1 1 d . . . . . H1 H 0.8345 0.2909 0.4689 0.040 Uiso 1 1 calc R . . . . N2 N 0.7908(9) 0.8338(5) 0.7329(4) 0.0252(12) Uani 1 1 d . . . . . N3 N 0.8178(8) 0.6659(5) 0.8964(4) 0.0222(10) Uani 1 1 d . . . . . H3 H 0.8757 0.6168 0.9463 0.027 Uiso 1 1 calc R . . . . C1 C 0.6208(10) 0.3298(6) 0.6806(5) 0.0248(13) Uani 1 1 d . . . . . C2 C 0.7819(9) 0.6179(7) 0.7907(4) 0.0215(12) Uani 1 1 d . . . . . C3 C 0.6669(9) 0.8565(6) 0.8245(4) 0.0209(12) Uani 1 1 d . . . . . C4 C 0.8600(9) 0.7150(6) 0.7145(5) 0.0221(12) Uani 1 1 d . . . . . C5 C 0.8871(9) 0.4880(6) 0.7823(5) 0.0233(13) Uani 1 1 d . . . . . H5 H 1.0451 0.5004 0.7779 0.028 Uiso 1 1 calc R . . . . C6 C 0.8053(10) 0.4104(6) 0.6893(5) 0.0245(13) Uani 1 1 d . . . . . C7 C 0.7654(9) 0.7828(7) 0.9205(4) 0.0236(12) Uani 1 1 d . . . . . C8 C 0.6207(11) 0.2701(7) 0.5810(5) 0.0290(14) Uani 1 1 d . . . . . C9 C 0.9087(12) 0.3956(7) 0.5985(5) 0.0332(15) Uani 1 1 d . . . . . H9 H 1.0383 0.4367 0.5836 0.040 Uiso 1 1 calc R . . . . C10 C 0.4659(12) 0.1852(7) 0.5456(6) 0.0351(15) Uani 1 1 d . . . . . H10 H 0.4714 0.1452 0.4788 0.042 Uiso 1 1 calc R . . . . C11 C 0.4530(10) 0.2999(7) 0.7465(5) 0.0278(14) Uani 1 1 d . . . . . H11 H 0.4496 0.3363 0.8147 0.033 Uiso 1 1 calc R . . . . C12 C 0.6334(10) 0.9970(7) 0.8456(5) 0.0263(13) Uani 1 1 d . . . . . H12 H 0.5741 1.0350 0.7776 0.032 Uiso 1 1 calc R . . . . C13 C 0.8457(12) 1.0611(7) 0.8742(6) 0.0342(15) Uani 1 1 d . . . . . H13A H 0.8982 1.0364 0.9458 0.051 Uiso 1 1 calc GR . . . . H13B H 0.8261 1.1522 0.8714 0.051 Uiso 1 1 calc GR . . . . H13C H 0.9505 1.0360 0.8240 0.051 Uiso 1 1 calc GR . . . . C14 C 0.2965(11) 0.2181(7) 0.7101(6) 0.0354(16) Uani 1 1 d . . . . . H14 H 0.1816 0.1999 0.7531 0.042 Uiso 1 1 calc R . . . . C15 C 0.4728(12) 1.0244(7) 0.9280(5) 0.0346(16) Uani 1 1 d . . . . . H15A H 0.3375 0.9808 0.9086 0.052 Uiso 1 1 calc GR . . . . H15B H 0.4466 1.1149 0.9309 0.052 Uiso 1 1 calc GR . . . . H15C H 0.5310 0.9950 0.9973 0.052 Uiso 1 1 calc GR . . . . C16 C 0.3006(12) 0.1601(7) 0.6112(6) 0.0371(16) Uani 1 1 d . . . . . H16 H 0.1898 0.1032 0.5885 0.045 Uiso 1 1 calc R . . . . C17 C 0.7764(15) 0.9217(7) 0.6428(5) 0.0408(18) Uani 1 1 d . . . . . H17A H 0.6252 0.9347 0.6191 0.061 Uiso 1 1 calc GR . . . . H17B H 0.8534 0.8868 0.5847 0.061 Uiso 1 1 calc GR . . . . H17C H 0.8411 1.0021 0.6649 0.061 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 0.0197(7) 0.0257(7) 0.0275(7) -0.0025(6) 0.0036(5) -0.0020(6) S3 0.0193(7) 0.0291(8) 0.0404(9) -0.0068(7) 0.0051(6) 0.0002(6) O1 0.028(2) 0.032(3) 0.022(2) 0.0004(18) 0.0128(17) -0.0014(19) O2 0.031(2) 0.034(3) 0.021(2) 0.0059(18) 0.0043(17) 0.001(2) O3 0.032(2) 0.034(3) 0.020(2) -0.0030(18) 0.0054(17) -0.0011(19) N1 0.045(3) 0.032(3) 0.024(3) -0.003(2) 0.014(2) 0.002(2) N2 0.024(3) 0.028(3) 0.024(3) 0.004(2) 0.006(2) 0.001(2) N3 0.024(2) 0.028(3) 0.014(2) 0.000(2) 0.0013(18) 0.002(2) C1 0.028(3) 0.025(3) 0.022(3) 0.000(2) 0.007(2) 0.003(2) C2 0.019(2) 0.030(3) 0.016(3) -0.002(2) 0.005(2) -0.002(3) C3 0.020(3) 0.026(3) 0.018(3) 0.000(2) 0.007(2) -0.005(2) C4 0.017(3) 0.026(3) 0.023(3) 0.002(2) 0.002(2) 0.000(2) C5 0.023(3) 0.026(3) 0.022(3) 0.003(2) 0.006(2) 0.003(2) C6 0.025(3) 0.024(3) 0.025(3) 0.001(2) 0.007(2) 0.005(2) C7 0.022(3) 0.028(3) 0.021(3) 0.004(3) 0.008(2) 0.000(3) C8 0.036(3) 0.029(3) 0.022(3) -0.002(3) 0.004(2) 0.004(3) C9 0.036(4) 0.035(4) 0.030(3) 0.003(3) 0.011(3) 0.003(3) C10 0.047(4) 0.025(3) 0.033(3) 0.002(3) 0.003(3) 0.002(3) C11 0.030(3) 0.030(4) 0.024(3) 0.005(3) 0.008(2) 0.005(3) C12 0.029(3) 0.026(3) 0.025(3) -0.005(3) 0.008(2) 0.001(3) C13 0.037(4) 0.032(4) 0.034(3) -0.001(3) 0.001(3) -0.008(3) C14 0.031(3) 0.030(4) 0.046(4) 0.004(3) 0.003(3) 0.001(3) C15 0.039(4) 0.033(4) 0.033(3) -0.004(3) 0.013(3) 0.008(3) C16 0.034(4) 0.031(4) 0.045(4) 0.005(3) -0.005(3) -0.003(3) C17 0.069(5) 0.031(4) 0.025(3) 0.009(3) 0.022(3) 0.007(4) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 S1 S3 98.1(2) . . ? C3 S3 S1 98.9(2) . . ? C9 N1 C8 108.7(5) . . ? C3 N2 C17 120.2(5) . . ? C4 N2 C3 118.8(5) . . ? C4 N2 C17 117.5(5) . . ? C7 N3 C2 121.5(5) . . ? C8 C1 C6 106.8(5) . . ? C8 C1 C11 118.0(6) . . ? C11 C1 C6 135.2(6) . . ? N3 C2 S1 112.0(4) . . ? N3 C2 C4 108.3(5) . . ? N3 C2 C5 110.1(5) . . ? C4 C2 S1 101.7(4) . . ? C4 C2 C5 114.4(5) . . ? C5 C2 S1 110.0(4) . . ? N2 C3 S3 110.5(4) . . ? N2 C3 C7 109.9(5) . . ? N2 C3 C12 112.7(5) . . ? C7 C3 S3 100.7(4) . . ? C12 C3 S3 108.1(4) . . ? C12 C3 C7 114.2(5) . . ? O1 C4 N2 123.7(6) . . ? O1 C4 C2 122.4(6) . . ? N2 C4 C2 113.9(5) . . ? O2 C5 C2 106.1(4) . . ? O2 C5 C6 110.8(5) . . ? C6 C5 C2 115.2(5) . . ? C1 C6 C5 128.2(5) . . ? C9 C6 C1 106.8(6) . . ? C9 C6 C5 124.8(6) . . ? O3 C7 N3 123.4(6) . . ? O3 C7 C3 123.7(6) . . ? N3 C7 C3 112.8(5) . . ? N1 C8 C1 107.4(6) . . ? C10 C8 N1 129.5(6) . . ? C10 C8 C1 123.0(6) . . ? C6 C9 N1 110.2(6) . . ? C8 C10 C16 117.5(7) . . ? C14 C11 C1 118.9(6) . . ? C13 C12 C3 110.7(5) . . ? C13 C12 C15 110.8(6) . . ? C15 C12 C3 114.1(6) . . ? C11 C14 C16 121.9(7) . . ? C10 C16 C14 120.7(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 S3 2.070(2) . ? S1 C2 1.888(6) . ? S3 C3 1.893(6) . ? O1 C4 1.234(8) . ? O2 C5 1.421(7) . ? O3 C7 1.223(8) . ? N1 C8 1.385(9) . ? N1 C9 1.371(10) . ? N2 C3 1.458(7) . ? N2 C4 1.363(8) . ? N2 C17 1.476(9) . ? N3 C2 1.438(7) . ? N3 C7 1.330(9) . ? C1 C6 1.435(9) . ? C1 C8 1.414(9) . ? C1 C11 1.420(9) . ? C2 C4 1.519(9) . ? C2 C5 1.539(9) . ? C3 C7 1.541(8) . ? C3 C12 1.539(9) . ? C5 C6 1.503(9) . ? C6 C9 1.366(9) . ? C8 C10 1.376(10) . ? C10 C16 1.394(11) . ? C11 C14 1.366(11) . ? C12 C13 1.512(10) . ? C12 C15 1.525(8) . ? C14 C16 1.400(11) . ?