#------------------------------------------------------------------------------ #$Date: 2018-06-18 18:53:46 +0300 (Mon, 18 Jun 2018) $ #$Revision: 208483 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/11/2021166.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_2021166 loop_ _publ_author_name 'Nguyen Tien, Cong' 'Nguyen Van, Thin' 'Le Duc, Giang' 'Vu Quoc, Manh' 'Vu Quoc, Trung' 'Pham Chien, Thang' 'Nguyen Huy, Hung' 'Dang Thi Tuyet, Anh' 'Nguyen Van, Tuyen' 'Van Meervelt, Luc' _publ_section_title ; Synthesis, structure and in vitro cytotoxicity testing of some 1,3,4-oxadiazoline derivatives from 2-hydroxy-5-iodobenzoic acid ; _journal_coeditor_code SK3693 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229618008719 _journal_volume 74 _journal_year 2018 _chemical_formula_iupac 'C19 H16 Cl I N2 O4' _chemical_formula_moiety 'C19 H16 Cl I N2 O4' _chemical_formula_sum 'C19 H16 Cl I N2 O4' _chemical_formula_weight 498.69 _chemical_name_systematic '2-[4-Acetyl-5-(4-chlorophenyl)-5-methyl-4,5-dihydro-1,3,4-oxadiazol-2-yl]-4-iodophenyl acetate' _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 92.888(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.703(2) _cell_length_b 22.037(4) _cell_length_c 7.4073(12) _cell_measurement_reflns_used 9499 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.10 _cell_measurement_theta_min 2.90 _cell_volume 1907.9(6) _computing_cell_refinement ; SAINT (Bruker, 2013) ; _computing_data_collection ; APEX2 (Bruker, 2014) ; _computing_data_reduction ; SAINT (Bruker, 2013) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 62840 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.496 _diffrn_reflns_theta_min 2.904 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS2014/2 (Bruker, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.736 _exptl_crystal_description block _exptl_crystal_F_000 984 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.398 _refine_diff_density_min -0.659 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 247 _refine_ls_number_reflns 4387 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0213 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.3951P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0514 _reflns_number_gt 3863 _reflns_number_total 4387 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL tp4cl_a.res in P2(1)/c i2-4cl.res created by SHELXL-2016/4 at 14:58:51 on 26-Jan-2018 REM Old TITL tp4Cl in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.183, Rweak 0.013, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C19 N2 O4 Cl I CELL 0.71073 11.7028 22.037 7.4073 90 92.888 90 ZERR 4 0.002 0.0035 0.0012 0 0.008 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl I N O UNIT 76 64 4 4 8 16 L.S. 20 PLAN 20 TEMP -173(2) BOND $H list 4 fmap 2 acta conf OMIT -4 55 REM REM REM WGHT 0.023300 1.395100 FVAR 0.30524 I1 4 0.890064 0.305471 0.884846 11.00000 0.02554 0.03502 = 0.03427 0.02000 -0.01207 -0.00758 CL1 3 0.063741 0.342782 0.419995 11.00000 0.02056 0.03188 = 0.04597 -0.00019 0.01336 0.00113 O1 6 0.773941 0.508233 0.316125 11.00000 0.02238 0.01318 = 0.01529 0.00128 0.00186 0.00016 N1 5 0.643949 0.421522 0.121757 11.00000 0.01624 0.01583 = 0.01428 -0.00087 -0.00035 -0.00121 C1 1 0.843969 0.373582 0.697497 11.00000 0.01451 0.02236 = 0.01561 0.00493 0.00051 -0.00023 O2 6 0.912271 0.470247 0.148806 11.00000 0.02274 0.02419 = 0.01917 0.00134 0.00467 -0.00051 N2 5 0.561467 0.387600 0.022789 11.00000 0.01828 0.01691 = 0.01403 0.00120 -0.00186 -0.00296 C2 1 0.773703 0.359649 0.546516 11.00000 0.01436 0.01510 = 0.01741 0.00047 0.00113 -0.00217 AFIX 43 H2 2 0.742501 0.320035 0.532421 11.00000 -1.20000 AFIX 0 O3 6 0.616268 0.334340 0.270892 11.00000 0.01570 0.01469 = 0.01580 0.00145 -0.00483 -0.00304 C3 1 0.748811 0.404163 0.414700 11.00000 0.01138 0.01562 = 0.01348 -0.00053 0.00182 -0.00042 O4 6 0.442404 0.373698 -0.220085 11.00000 0.02915 0.03428 = 0.01913 0.00054 -0.00881 -0.00405 C4 1 0.797200 0.461795 0.440512 11.00000 0.01517 0.01549 = 0.01370 0.00066 0.00339 0.00104 C5 1 0.864999 0.475629 0.593507 11.00000 0.01895 0.01684 = 0.01726 -0.00320 0.00302 -0.00365 AFIX 43 H5 2 0.895568 0.515324 0.609208 11.00000 -1.20000 AFIX 0 C6 1 0.888355 0.431489 0.724103 11.00000 0.01488 0.02594 = 0.01410 -0.00180 0.00007 -0.00371 AFIX 43 H6 2 0.934058 0.440805 0.830114 11.00000 -1.20000 AFIX 0 C7 1 0.670469 0.389035 0.261012 11.00000 0.01296 0.01314 = 0.01523 -0.00097 0.00265 -0.00044 C8 1 0.532751 0.330510 0.118702 11.00000 0.01501 0.01555 = 0.01253 -0.00036 -0.00226 -0.00126 C9 1 0.413667 0.332271 0.191655 11.00000 0.01646 0.01272 = 0.01307 0.00094 -0.00182 0.00118 C10 1 0.394562 0.367494 0.343626 11.00000 0.01964 0.02060 = 0.01743 -0.00495 -0.00175 -0.00129 AFIX 43 H10 2 0.456042 0.389965 0.399203 11.00000 -1.20000 AFIX 0 C11 1 0.287628 0.370290 0.414891 11.00000 0.02433 0.02049 = 0.01791 -0.00438 0.00227 0.00401 AFIX 43 H11 2 0.275442 0.394248 0.518796 11.00000 -1.20000 AFIX 0 C12 1 0.199109 0.337658 0.332280 11.00000 0.01577 0.01885 = 0.02314 0.00550 0.00473 0.00272 C13 1 0.214827 0.301681 0.182886 11.00000 0.01756 0.02264 = 0.02729 -0.00308 -0.00120 -0.00364 AFIX 43 H13 2 0.152988 0.279055 0.129009 11.00000 -1.20000 AFIX 0 C14 1 0.322848 0.299135 0.112580 11.00000 0.01972 0.02068 = 0.01894 -0.00622 -0.00081 -0.00122 AFIX 43 H14 2 0.334764 0.274592 0.009782 11.00000 -1.20000 AFIX 0 C15 1 0.840638 0.507892 0.168279 11.00000 0.01799 0.01794 = 0.01552 0.00095 -0.00023 -0.00620 C16 1 0.811448 0.560505 0.047525 11.00000 0.03459 0.02732 = 0.02581 0.01212 0.00205 -0.00060 AFIX 137 H16A 2 0.801965 0.596984 0.120947 11.00000 -1.50000 H16B 2 0.740015 0.552037 -0.022698 11.00000 -1.50000 H16C 2 0.873208 0.567020 -0.034917 11.00000 -1.50000 AFIX 0 C17 1 0.558128 0.274283 0.010612 11.00000 0.01905 0.01928 = 0.02078 -0.00536 0.00227 0.00044 AFIX 137 H17A 2 0.548298 0.238187 0.085534 11.00000 -1.50000 H17B 2 0.637073 0.276005 -0.027385 11.00000 -1.50000 H17C 2 0.505453 0.272232 -0.096334 11.00000 -1.50000 AFIX 0 C18 1 0.515253 0.405149 -0.142005 11.00000 0.01960 0.02283 = 0.01460 -0.00020 0.00108 0.00477 C19 1 0.558733 0.463670 -0.217546 11.00000 0.03079 0.02539 = 0.01563 0.00527 0.00223 0.00290 AFIX 137 H19A 2 0.516126 0.473014 -0.331441 11.00000 -1.50000 H19B 2 0.640246 0.459579 -0.239569 11.00000 -1.50000 H19C 2 0.548147 0.496532 -0.130830 11.00000 -1.50000 AFIX 0 HKLF 4 REM tp4cl_a.res in P2(1)/c REM R1 = 0.0213 for 3863 Fo > 4sig(Fo) and 0.0274 for all 4387 data REM 247 parameters refined using 0 restraints END WGHT 0.0233 1.3952 REM Highest difference peak 0.398, deepest hole -0.659, 1-sigma level 0.065 Q1 1 0.5448 0.3024 0.0644 11.00000 0.05 0.39 Q2 1 0.7055 0.3984 0.3490 11.00000 0.05 0.39 Q3 1 0.7956 0.3728 0.6328 11.00000 0.05 0.36 Q4 1 0.5471 0.3596 0.0553 11.00000 0.05 0.36 Q5 1 0.4066 0.3491 0.2692 11.00000 0.05 0.35 Q6 1 0.7412 0.5738 0.0647 11.00000 0.05 0.35 Q7 1 0.7487 0.3879 0.4967 11.00000 0.05 0.34 Q8 1 0.7949 0.4298 0.4200 11.00000 0.05 0.34 Q9 1 0.8192 0.4682 0.5297 11.00000 0.05 0.34 Q10 1 0.5567 0.3895 -0.0682 11.00000 0.05 0.33 Q11 1 0.4713 0.3327 0.1598 11.00000 0.05 0.32 Q12 1 0.3426 0.3605 0.3777 11.00000 0.05 0.32 Q13 1 0.9464 0.2885 0.8528 11.00000 0.05 0.31 Q14 1 0.5270 0.4012 -0.0311 11.00000 0.05 0.31 Q15 1 0.9628 0.2999 0.8769 11.00000 0.05 0.30 Q16 1 0.8968 0.3031 0.9701 11.00000 0.05 0.30 Q17 1 0.8820 0.4493 0.6426 11.00000 0.05 0.30 Q18 1 0.2766 0.2922 0.1784 11.00000 0.05 0.29 Q19 1 0.5909 0.4058 0.0575 11.00000 0.05 0.29 Q20 1 0.8275 0.3099 0.8686 11.00000 0.05 0.29 REM The information below was added by Olex2. REM REM R1 = 0.0213 for 3863 Fo > 4sig(Fo) and 0.0274 for all 75844 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.40, deepest hole -0.66 REM Mean Shift 0, Max Shift -0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0274 REM R1_gt = 0.0213 REM wR_ref = 0.0514 REM GOOF = 1.039 REM Shift_max = -0.002 REM Shift_mean = 0 REM Reflections_all = 75844 REM Reflections_gt = 3863 REM Parameters = n/a REM Hole = -0.66 REM Peak = 0.40 REM Flack = n/a ; _cod_data_source_file sk3693sup1.cif _cod_data_source_block 6e _cod_original_cell_volume 1907.9(5) _cod_database_code 2021166 _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. ; 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 I I1 0.89006(2) 0.30547(2) 0.88485(2) 0.03207(5) Uani d 1 Cl Cl1 0.06374(4) 0.34278(2) 0.41999(8) 0.03241(12) Uani d 1 O O1 0.77394(10) 0.50823(5) 0.31612(16) 0.0169(2) Uani d 1 N N1 0.64395(12) 0.42152(6) 0.12176(18) 0.0155(3) Uani d 1 C C1 0.84397(15) 0.37358(8) 0.6975(2) 0.0175(3) Uani d 1 O O2 0.91227(11) 0.47025(6) 0.14881(17) 0.0219(3) Uani d 1 N N2 0.56147(13) 0.38760(6) 0.02279(19) 0.0165(3) Uani d 1 C C2 0.77370(14) 0.35965(7) 0.5465(2) 0.0156(3) Uani d 1 H H2 0.742501 0.320035 0.532421 0.019 Uiso calc 1 O O3 0.61627(10) 0.33434(5) 0.27089(16) 0.0156(2) Uani d 1 C C3 0.74881(14) 0.40416(7) 0.4147(2) 0.0135(3) Uani d 1 O O4 0.44240(12) 0.37370(6) -0.22008(18) 0.0279(3) Uani d 1 C C4 0.79720(14) 0.46180(7) 0.4405(2) 0.0147(3) Uani d 1 C C5 0.86500(15) 0.47563(8) 0.5935(2) 0.0176(3) Uani d 1 H H5 0.895568 0.515324 0.609208 0.021 Uiso calc 1 C C6 0.88836(15) 0.43149(8) 0.7241(2) 0.0183(3) Uani d 1 H H6 0.934058 0.440805 0.830114 0.022 Uiso calc 1 C C7 0.67047(14) 0.38903(7) 0.2610(2) 0.0137(3) Uani d 1 C C8 0.53275(14) 0.33051(7) 0.1187(2) 0.0145(3) Uani d 1 C C9 0.41367(14) 0.33227(7) 0.1917(2) 0.0142(3) Uani d 1 C C10 0.39456(15) 0.36749(8) 0.3436(2) 0.0193(4) Uani d 1 H H10 0.456042 0.389965 0.399203 0.023 Uiso calc 1 C C11 0.28763(16) 0.37029(8) 0.4149(2) 0.0209(4) Uani d 1 H H11 0.275442 0.394248 0.518796 0.025 Uiso calc 1 C C12 0.19911(15) 0.33766(8) 0.3323(2) 0.0191(4) Uani d 1 C C13 0.21483(16) 0.30168(8) 0.1829(3) 0.0226(4) Uani d 1 H H13 0.152988 0.279055 0.129009 0.027 Uiso calc 1 C C14 0.32285(16) 0.29914(8) 0.1126(2) 0.0198(4) Uani d 1 H H14 0.334764 0.274592 0.009782 0.024 Uiso calc 1 C C15 0.84064(15) 0.50789(8) 0.1683(2) 0.0172(3) Uani d 1 C C16 0.81145(19) 0.56051(9) 0.0475(3) 0.0292(4) Uani d 1 H H16A 0.801965 0.596984 0.120947 0.044 Uiso calc 1 H H16B 0.740015 0.552037 -0.022698 0.044 Uiso calc 1 H H16C 0.873208 0.567020 -0.034917 0.044 Uiso calc 1 C C17 0.55813(15) 0.27428(8) 0.0106(2) 0.0197(4) Uani d 1 H H17A 0.548298 0.238187 0.085534 0.029 Uiso calc 1 H H17B 0.637073 0.276005 -0.027385 0.029 Uiso calc 1 H H17C 0.505453 0.272232 -0.096334 0.029 Uiso calc 1 C C18 0.51525(15) 0.40515(8) -0.1420(2) 0.0190(4) Uani d 1 C C19 0.55873(17) 0.46367(9) -0.2175(2) 0.0239(4) Uani d 1 H H19A 0.516126 0.473014 -0.331441 0.036 Uiso calc 1 H H19B 0.640246 0.459579 -0.239569 0.036 Uiso calc 1 H H19C 0.548147 0.496532 -0.130830 0.036 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 I1 0.02554(8) 0.03502(8) 0.03427(8) -0.00758(5) -0.01207(5) 0.02000(6) Cl1 0.0206(2) 0.0319(3) 0.0460(3) 0.00113(19) 0.0134(2) -0.0002(2) O1 0.0224(6) 0.0132(5) 0.0153(6) 0.0002(5) 0.0019(5) 0.0013(4) N1 0.0162(7) 0.0158(7) 0.0143(7) -0.0012(5) -0.0003(5) -0.0009(5) C1 0.0145(8) 0.0224(9) 0.0156(8) -0.0002(7) 0.0005(6) 0.0049(7) O2 0.0227(7) 0.0242(7) 0.0192(6) -0.0005(5) 0.0047(5) 0.0013(5) N2 0.0183(7) 0.0169(7) 0.0140(7) -0.0030(6) -0.0019(6) 0.0012(5) C2 0.0144(8) 0.0151(8) 0.0174(8) -0.0022(6) 0.0011(6) 0.0005(6) O3 0.0157(6) 0.0147(6) 0.0158(6) -0.0030(5) -0.0048(5) 0.0014(4) C3 0.0114(8) 0.0156(8) 0.0135(7) -0.0004(6) 0.0018(6) -0.0005(6) O4 0.0291(8) 0.0343(8) 0.0191(7) -0.0041(6) -0.0088(6) 0.0005(6) C4 0.0152(8) 0.0155(8) 0.0137(8) 0.0010(6) 0.0034(6) 0.0007(6) C5 0.0190(9) 0.0168(8) 0.0173(8) -0.0037(7) 0.0030(7) -0.0032(6) C6 0.0149(8) 0.0259(9) 0.0141(8) -0.0037(7) 0.0001(6) -0.0018(7) C7 0.0130(8) 0.0131(7) 0.0152(8) -0.0004(6) 0.0026(6) -0.0010(6) C8 0.0150(8) 0.0156(8) 0.0125(8) -0.0013(6) -0.0023(6) -0.0004(6) C9 0.0165(8) 0.0127(7) 0.0131(8) 0.0012(6) -0.0018(6) 0.0009(6) C10 0.0196(9) 0.0206(8) 0.0174(8) -0.0013(7) -0.0018(7) -0.0049(7) C11 0.0243(9) 0.0205(9) 0.0179(9) 0.0040(7) 0.0023(7) -0.0044(7) C12 0.0158(8) 0.0188(8) 0.0231(9) 0.0027(7) 0.0047(7) 0.0055(7) C13 0.0176(9) 0.0226(9) 0.0273(10) -0.0036(7) -0.0012(7) -0.0031(7) C14 0.0197(9) 0.0207(9) 0.0189(8) -0.0012(7) -0.0008(7) -0.0062(7) C15 0.0180(8) 0.0179(8) 0.0155(8) -0.0062(7) -0.0002(7) 0.0010(6) C16 0.0346(11) 0.0273(10) 0.0258(10) -0.0006(8) 0.0021(8) 0.0121(8) C17 0.0191(9) 0.0193(8) 0.0208(9) 0.0004(7) 0.0023(7) -0.0054(7) C18 0.0196(9) 0.0228(9) 0.0146(8) 0.0048(7) 0.0011(7) -0.0002(7) C19 0.0308(10) 0.0254(9) 0.0156(9) 0.0029(8) 0.0022(7) 0.0053(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C15 O1 C4 114.96(13) C7 N1 N2 104.84(14) C2 C1 I1 119.80(13) C6 C1 I1 118.83(13) C6 C1 C2 121.32(16) N1 N2 C8 111.55(13) C18 N2 N1 123.28(14) C18 N2 C8 125.17(14) C1 C2 H2 120.0 C1 C2 C3 119.95(15) C3 C2 H2 120.0 C7 O3 C8 107.76(12) C2 C3 C7 118.79(15) C4 C3 C2 118.07(15) C4 C3 C7 123.10(15) O1 C4 C3 120.76(15) C5 C4 O1 117.65(15) C5 C4 C3 121.53(15) C4 C5 H5 120.0 C4 C5 C6 120.03(16) C6 C5 H5 120.0 C1 C6 C5 119.06(16) C1 C6 H6 120.5 C5 C6 H6 120.5 N1 C7 O3 116.24(15) N1 C7 C3 128.02(15) O3 C7 C3 115.71(14) N2 C8 C9 112.35(14) N2 C8 C17 112.57(14) O3 C8 N2 99.28(12) O3 C8 C9 108.34(13) O3 C8 C17 108.37(13) C17 C8 C9 114.64(14) C10 C9 C8 119.22(15) C14 C9 C8 122.03(15) C14 C9 C10 118.74(16) C9 C10 H10 119.4 C11 C10 C9 121.16(16) C11 C10 H10 119.4 C10 C11 H11 120.6 C12 C11 C10 118.76(16) C12 C11 H11 120.6 C11 C12 Cl1 118.47(14) C11 C12 C13 121.84(16) C13 C12 Cl1 119.69(14) C12 C13 H13 120.6 C12 C13 C14 118.87(17) C14 C13 H13 120.6 C9 C14 H14 119.7 C13 C14 C9 120.60(16) C13 C14 H14 119.7 O1 C15 C16 110.52(15) O2 C15 O1 122.00(15) O2 C15 C16 127.46(17) C15 C16 H16A 109.5 C15 C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16B 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C8 C17 H17A 109.5 C8 C17 H17B 109.5 C8 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 N2 C18 C19 116.68(16) O4 C18 N2 119.87(16) O4 C18 C19 123.46(16) C18 C19 H19A 109.5 C18 C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C1 2.0963(17) Cl1 C12 1.7459(18) O1 C4 1.395(2) O1 C15 1.377(2) N1 N2 1.399(2) N1 C7 1.281(2) C1 C2 1.389(2) C1 C6 1.388(2) O2 C15 1.193(2) N2 C8 1.491(2) N2 C18 1.366(2) C2 H2 0.9500 C2 C3 1.404(2) O3 C7 1.366(2) O3 C8 1.4568(19) C3 C4 1.400(2) C3 C7 1.464(2) O4 C18 1.221(2) C4 C5 1.384(2) C5 H5 0.9500 C5 C6 1.389(2) C6 H6 0.9500 C8 C9 1.520(2) C8 C17 1.513(2) C9 C10 1.395(2) C9 C14 1.394(2) C10 H10 0.9500 C10 C11 1.384(3) C11 H11 0.9500 C11 C12 1.379(3) C12 C13 1.381(3) C13 H13 0.9500 C13 C14 1.392(3) C14 H14 0.9500 C15 C16 1.493(2) C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 C19 1.505(3) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 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 C6 H6 O2 1_556 0.95 2.47 3.258(2) 140 yes C11 H11 O1 3_666 0.95 2.55 3.435(2) 155 yes C19 H19B Cg2 1_554 0.98 2.75 3.649(2) 153 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 I1 C1 C2 C3 -175.79(12) I1 C1 C6 C5 175.24(13) Cl1 C12 C13 C14 178.69(14) O1 C4 C5 C6 178.30(15) N1 N2 C8 O3 -5.26(16) N1 N2 C8 C9 109.07(15) N1 N2 C8 C17 -119.69(15) N1 N2 C18 O4 -179.05(16) N1 N2 C18 C19 0.9(2) C1 C2 C3 C4 0.4(2) C1 C2 C3 C7 -177.32(15) N2 N1 C7 O3 0.98(19) N2 N1 C7 C3 -176.59(16) N2 C8 C9 C10 -74.07(19) N2 C8 C9 C14 106.70(18) C2 C1 C6 C5 -2.3(3) C2 C3 C4 O1 -178.77(14) C2 C3 C4 C5 -1.9(2) C2 C3 C7 N1 -174.43(16) C2 C3 C7 O3 8.0(2) O3 C8 C9 C10 34.6(2) O3 C8 C9 C14 -144.63(15) C3 C4 C5 C6 1.3(3) C4 O1 C15 O2 0.4(2) C4 O1 C15 C16 -178.08(15) C4 C3 C7 N1 8.0(3) C4 C3 C7 O3 -169.58(15) C4 C5 C6 C1 0.8(3) C6 C1 C2 C3 1.7(3) C7 N1 N2 C8 2.98(18) C7 N1 N2 C18 -176.27(16) C7 O3 C8 N2 5.51(15) C7 O3 C8 C9 -111.89(14) C7 O3 C8 C17 123.16(14) C7 C3 C4 O1 -1.2(2) C7 C3 C4 C5 175.70(15) C8 N2 C18 O4 1.8(3) C8 N2 C18 C19 -178.20(15) C8 O3 C7 N1 -4.56(19) C8 O3 C7 C3 173.32(13) C8 C9 C10 C11 -179.82(16) C8 C9 C14 C13 179.91(16) C9 C10 C11 C12 -0.3(3) C10 C9 C14 C13 0.7(3) C10 C11 C12 Cl1 -178.58(14) C10 C11 C12 C13 1.1(3) C11 C12 C13 C14 -1.0(3) C12 C13 C14 C9 0.1(3) C14 C9 C10 C11 -0.6(3) C15 O1 C4 C3 -83.54(19) C15 O1 C4 C5 99.47(17) C17 C8 C9 C10 155.75(16) C17 C8 C9 C14 -23.5(2) C18 N2 C8 O3 173.97(15) C18 N2 C8 C9 -71.7(2) C18 N2 C8 C17 59.5(2) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas 0 0 2 40.9 0 0 2 42.4 0 0 -2 37.6 0 0 -2 34.2 0 0 -2 40.3 0 0 2 30.7 0 0 2 39.2 0 0 2 36.7 0 0 -2 38.5 0 0 3 1 0 0 3 0.4 0 0 3 0.9 0 0 3 0.6 0 0 -3 0.3 0 0 -3 -0.9 0 0 3 2 0 0 -3 0.5 0 0 -3 -0.9 0 0 -3 0.1 0 0 4 2126.69 0 0 4 2222.98 0 0 -4 1951.4 0 0 4 2008.3 0 0 -4 2032.1 0 0 4 2015.3 0 0 -4 2054.99 0 0 -4 2018.1 0 0 -5 -4.3 0 0 5 3.6 0 0 -5 -1 0 0 -5 -3 0 0 5 -1.6 0 0 5 3.1 0 0 5 3 0 0 -5 2.5 0 0 -6 156.88 0 0 6 155.28 0 0 -6 159.38 0 0 -6 220.88 0 0 6 164.18 0 0 -6 156.68 0 0 -6 155.08 0 0 6 163.38 0 0 6 143.79 0 0 -7 0.2 0 0 -7 -2.9 0 0 7 -6.4 0 0 7 2.5 0 0 -7 -3 0 0 7 5.8 0 0 -7 1 0 0 7 2.5 0 0 -7 2.3 0 0 -7 -8.7 0 0 -8 100.59 0 0 8 111.59 0 0 -8 100.89 0 0 -8 79.59 0 0 -8 92.59 0 0 -8 73.79 0 0 -8 90.59 0 0 8 86.99 0 0 8 88.29 0 0 8 57.09 0 0 -9 5.1 0 0 9 6.1 0 0 -9 -0.6 0 0 9 -0.7 0 0 -10 21.9 0 0 -10 31.4 0 0 10 27.6 0 0 10 35.2 0 1 1 99.59 0 -1 1 93.49 0 1 2 3343.67 0 1 -2 2962.8 0 1 2 3057.29 0 1 -2 3190.68 0 1 2 3142.59 0 1 -2 3071.79 0 1 2 3125.09 0 1 2 3112.79 0 1 -2 3136.29 0 1 -2 3129.79 0 -1 2 3200.78 0 -1 -2 2972.7 0 -1 -2 3173.48 0 -1 2 3240.98 0 -1 2 3090.79 0 -1 2 3104.19 0 -1 -2 3105.59 0 -1 -2 3065.19 0 -1 2 3266.57 0 1 -3 190.08 0 1 -3 173.48 0 1 3 177.78 0 1 -3 181.98 0 1 -3 172.28 0 1 3 172.48 0 1 3 169.78 0 1 -3 184.58 0 1 -3 188.78 0 1 3 168.48 0 -1 3 169.88 0 -1 -3 168.68 0 -1 -3 177.38 0 -1 3 188.98 0 -1 3 177.98 0 -1 3 179.38 0 -1 -3 175.28 0 -1 -3 175.18 0 -1 3 180.98 0 1 4 173.48 0 1 -4 184.28 0 1 4 173.88 0 1 4 165.98 0 1 4 165.28 0 1 -4 161.48 0 1 -4 166.28 0 1 -4 173.68 0 -1 4 170.58 0 -1 -4 170.68 0 -1 -4 166.78 0 -1 -4 168.28 0 -1 4 159.28 0 -1 -4 192.08 0 -1 4 155.68 0 1 5 15.1 0 1 -5 24.8 0 1 -5 21.1 0 1 5 27.8 0 1 -5 15.9 0 1 5 18.3 0 1 5 23.7 0 1 -5 21.3 0 1 -5 21.8 0 -1 -5 18.4 0 -1 5 26 0 -1 5 21 0 -1 5 17.6 0 -1 -5 18.9 0 -1 -5 18 0 -1 -5 13.6 0 -1 -5 9 0 -1 5 22.9 0 1 -6 406.16 0 1 6 421.96 0 1 6 408.86 0 1 -6 402.26 0 1 6 380.86 0 1 6 417.46 0 1 -6 393.26 0 1 -6 396.36 0 1 -6 411.26 0 1 6 393.16 0 1 -6 363.96 0 -1 -6 392.36 0 -1 6 428.06 0 -1 -6 393.96 0 -1 -6 410.06 0 -1 -6 417.96 0 -1 6 422.36 0 -1 6 402.16 0 -1 -6 402.86 0 1 -7 201.18 0 1 7 185.08 0 1 -7 211.68 0 1 -7 212.48 0 1 7 193.28 0 1 7 185.88 0 1 7 202.58 0 1 -7 205.18 0 1 -7 171.38 0 1 7 190.38 0 1 -7 181.38 0 -1 -7 194.88 0 -1 -7 202.68 0 -1 -7 208.08 0 -1 7 213.78 0 -1 7 213.98 0 -1 -7 202.28 0 -1 7 190.28 0 -1 -7 199.58 0 -1 -7 191.28 0 -1 7 220.98 0 1 8 105.99 0 1 -8 102.09 0 1 -8 125.99 0 1 -8 124.49 0 1 8 152.38 0 1 8 124.09 0 1 8 113.89 0 -1 -8 84.59 0 -1 -8 79.69 0 -1 -8 122.89 0 -1 8 136.29 0 -1 8 119.09 0 -1 -8 127.29 0 -1 8 132.89 0 -1 8 122.59 0 -1 -8 122.19 0 1 9 34.7 0 1 -9 41.4 0 1 9 24.2 0 1 -9 41 0 -1 -9 33.5 0 -1 -9 35 0 -1 9 26.5 0 -1 9 26.9 0 1 -10 2.4 0 1 10 6 0 1 10 10.5 0 1 -10 5.8 0 -1 -10 11.3 0 -1 10 2.8 0 -1 -10 6.3 0 -1 10 12.6 0 2 1 16.8 0 2 1 18.3 0 2 1 13.3 0 2 -1 15.8 0 2 -1 21 0 2 1 19.8 0 2 1 19.1 0 -2 -1 19.4 0 -2 -1 16.6 0 -2 -1 16.8 0 -2 1 20 0 -2 1 15.8 0 -2 -1 18.7 0 -2 1 14.1 0 -2 1 19.4 0 2 -2 230.88 0 2 2 232.98 0 2 2 244.98 0 2 2 219.18 0 2 2 253.97 0 2 -2 226.98 0 2 2 228.58 0 -2 -2 241.68 0 -2 2 246.08 0 -2 -2 240.28 0 -2 2 232.38 0 -2 -2 246.68 0 -2 2 248.18 0 -2 2 244.38 0 -2 -2 236.18 0 -2 -2 232.58 0 2 3 4 0 2 -3 1.6 0 2 -3 2.5 0 2 -3 0.2 0 2 3 3.5 0 2 -3 3.2 0 2 3 5.4 0 2 3 0.5 0 2 3 3.2 0 2 3 3.3 0 2 -3 3.1 0 2 -3 3.9 0 -2 3 3.3 0 -2 -3 2.3 0 -2 3 4.4 0 -2 3 0.9 0 -2 -3 3.3 0 -2 -3 4 0 -2 3 2.9 0 2 4 518.85 0 2 4 526.05 0 2 -4 523.25 0 2 -4 519.65 0 2 4 517.35 0 2 -4 584.74 0 2 4 509.05 0 2 -4 532.95 0 2 -4 523.15 0 2 -4 515.45 0 2 4 535.65 0 -2 4 539.55 0 -2 -4 542.75 0 -2 -4 547.05 0 -2 4 490.05 0 -2 -4 491.25 0 -2 -4 516.45 0 -2 4 507.35 0 -2 4 514.05 0 2 -5 43.2 0 2 5 48.2 0 2 -5 47.4 0 2 5 83.59 0 2 -5 36.7 0 2 5 50.79 0 2 5 54.09 0 2 -5 54.79 0 2 -5 51.39 0 2 5 58.29 0 2 -5 50.19 0 -2 -5 50.19 0 -2 -5 55.89 0 -2 -5 61.29 0 -2 5 54.49 0 -2 5 43.8 0 -2 -5 49 0 -2 5 57.49 0 -2 5 49.99 0 2 -6 51.19 0 2 -6 52.09 0 2 6 64.69 0 2 -6 58.19 0 2 6 61.79 0 2 6 56.09 0 2 6 52.49 0 2 6 62.69 0 2 -6 62.79 0 2 -6 47.6 0 -2 -6 50.69 0 -2 6 59.19 0 -2 -6 51.59 0 -2 6 62.49 0 -2 -6 78.59 0 -2 -6 67.09 0 -2 -6 63.19 0 -2 6 59.09 0 -2 6 57.19 0 2 7 51.19 0 2 -7 51.69 0 2 -7 36.3 0 2 7 41.2 0 2 7 24.1 0 2 7 49.4 0 2 -7 53.99 0 2 7 47.5 0 2 -7 30.4 0 -2 -7 59.89 0 -2 -7 32.7 0 -2 7 56.89 0 -2 -7 51.69 0 -2 -7 43.4 0 -2 7 42.6 0 -2 7 41.1 0 -2 -7 47 0 2 8 146.09 0 2 -8 157.58 0 2 8 144.99 0 2 -8 198.98 0 2 8 181.28 0 2 -8 165.78 0 2 -8 161.58 0 2 8 175.18 0 -2 -8 163.08 0 -2 -8 175.78 0 -2 8 176.68 0 -2 -8 159.28 0 -2 -8 181.18 0 -2 -8 188.48 0 -2 8 149.88 0 2 9 -3.8 0 2 -9 10.8 0 2 9 3.1 0 2 -9 9.9 0 2 9 8.6 0 -2 9 6.8 0 -2 9 -3.9 0 -2 -9 -0.2 0 -2 9 2 0 -2 -9 -5.8 0 2 10 26.8 0 2 -10 47 0 2 10 19.7 0 2 -10 34.3 0 -2 -10 50.89 0 -2 10 36.9 0 -2 -10 46.5 0 -2 10 9.6 0 3 1 586.24 0 3 1 603.34 0 3 -1 652.73 0 3 -1 616.04 0 3 -1 596.34 0 3 1 623.14 0 3 1 586.24 0 3 1 594.44 0 3 -1 617.64 0 -3 1 622.04 0 -3 1 637.64 0 -3 -1 588.64 0 -3 -1 600.04 0 -3 -1 603.84 0 -3 -1 596.84 0 -3 -1 611.54 0 -3 1 621.14 0 -3 1 646.44 0 -3 1 609.14 0 3 2 113.99 0 3 -2 105.19 0 3 2 111.09 0 3 -2 111.89 0 3 2 112.39 0 3 -2 112.29 0 3 2 108.69 0 3 2 113.39 0 -3 2 111.79 0 -3 2 116.99 0 -3 2 111.39 0 -3 -2 108.09 0 -3 -2 116.39 0 -3 2 113.29 0 -3 -2 112.99 0 -3 -2 112.89 0 3 -3 307.47 0 3 3 301.07 0 3 -3 307.27 0 3 -3 308.87 0 3 3 308.97 0 3 -3 300.37 0 3 3 319.57 0 3 3 316.87 0 3 3 324.07 0 3 -3 316.27 0 -3 -3 286.57 0 -3 -3 315.67 0 -3 3 317.47 0 -3 3 316.27 0 -3 -3 303.37 0 -3 -3 295.47 0 -3 3 319.67 0 -3 -3 303.87 0 -3 3 297.07 0 3 4 -1.9 0 3 -4 0 0 3 4 1 0 3 4 -1.1 0 3 4 0.5 0 3 -4 1.5 0 3 4 -0.3 0 3 -4 1.2 0 3 -4 1.1 0 3 -4 -1.8 0 3 4 -1.7 0 -3 -4 0.1 0 -3 -4 2.9 0 -3 4 5.6 0 -3 -4 2.3 0 -3 4 6.1 0 -3 -4 3.9 0 -3 4 1.6 0 -3 -4 0.3 0 -3 4 -0.6 0 3 -5 342.77 0 3 5 376.26 0 3 -5 380.36 0 3 -5 376.56 0 3 -5 382.06 0 3 5 357.46 0 3 5 391.66 0 3 5 371.16 0 3 5 360.66 0 -3 -5 379.86 0 -3 -5 361.56 0 -3 5 388.56 0 -3 5 384.76 0 -3 5 391.76 0 -3 5 381.66 0 -3 -5 368.96 0 -3 -5 383.66 0 -3 -5 374.06 0 3 6 175.88 0 3 -6 187.98 0 3 6 177.88 0 3 6 182.68 0 3 6 196.58 0 3 -6 172.18 0 3 -6 189.98 0 3 6 198.68 0 3 -6 173.48 0 -3 6 202.48 0 -3 6 196.18 0 -3 -6 187.78 0 -3 -6 187.88 0 -3 -6 191.18 0 -3 -6 192.38 0 -3 6 194.68 0 -3 6 194.18 0 -3 -6 208.28 0 3 -7 75.29 0 3 7 54.89 0 3 -7 78.39 0 3 7 64.79 0 3 7 56.69 0 3 -7 62.79 0 3 7 66.79 0 3 -7 45.4 0 -3 -7 59.79 0 -3 -7 68.39 0 -3 -7 55.49 0 -3 -7 61.39 0 -3 7 61.49 0 -3 7 71.69 0 -3 7 65.89 0 -3 -7 64.19 0 -3 7 53.59 0 3 -8 -3.6 0 3 8 4.3 0 3 -8 -6.2 0 3 8 -4.5 0 3 -8 -0.6 0 3 -8 0.1 0 3 8 -1.6 0 3 8 -1.5 0 -3 -8 -2.9 0 -3 -8 -4 0 -3 -8 8.4 0 -3 -8 -2.6 0 -3 -8 -8.6 0 -3 -8 -4.6 0 -3 8 -6 0 3 -9 176.48 0 3 9 190.78 0 3 -9 203.78 0 3 9 180.58 0 3 9 166.58 0 -3 9 164.88 0 -3 9 237.98 0 -3 -9 157.88 0 -3 -9 160.98 0 -3 -9 196.68 0 3 -10 45.7 0 3 10 55.69 0 3 -10 45.6 0 3 10 44 0 -3 -10 58.19 0 -3 -10 25.3 0 -3 10 29 0 -3 10 35.3 0 4 0 766.22 0 4 0 862.01 0 4 0 822.92 0 4 0 856.91 0 -4 0 831.02 0 -4 0 874.21 0 -4 0 868.21 0 -4 0 877.01 0 4 1 21.1 0 4 1 24.2 0 4 -1 21.4 0 4 -1 21.9 0 4 -1 20.8 0 4 -1 22.4 0 4 1 22.7 0 4 1 21.4 0 -4 -1 21.7 0 -4 1 20.2 0 -4 -1 22.9 0 -4 -1 21.6 0 -4 1 20 0 -4 1 20.2 0 -4 1 21.1 0 -4 -1 21.3 0 -4 -1 23.3 0 -4 1 20.3 0 4 -2 0.1 0 4 -2 0.2 0 4 -2 -1.4 0 4 2 -2.9 0 4 2 1.1 0 4 -2 0.8 0 4 2 -0.8 0 4 2 -0.4 0 4 2 0.2 0 -4 -2 -2.5 0 -4 2 0.3 0 -4 2 1.5 0 -4 -2 -0.1 0 -4 2 -0.4 0 -4 -2 1.9 0 -4 -2 3.2 0 -4 -2 0.3 0 4 3 1575.04 0 4 -3 1617.14 0 4 3 1539.45 0 4 3 1555.84 0 4 -3 1554.24 0 4 3 1633.64 0 4 -3 1576.04 0 4 -3 1804.12 0 4 3 1628.04 0 4 3 1674.03 0 -4 3 1516.45 0 -4 -3 1533.55 0 -4 -3 1595.14 0 -4 -3 1645.04 0 -4 3 1589.14 0 -4 -3 1540.65 0 -4 3 1717.63 0 -4 3 1624.44 0 -4 -3 1581.04 0 4 -4 144.39 0 4 -4 129.39 0 4 4 124.59 0 4 -4 130.79 0 4 4 124.39 0 4 4 136.29 0 4 4 133.79 0 4 4 133.19 0 4 -4 133.79 0 4 -4 137.39 0 -4 4 143.19 0 -4 4 134.89 0 -4 -4 122.49 0 -4 -4 122.19 0 -4 -4 132.39 0 -4 4 133.89 0 -4 4 123.19 0 -4 -4 127.29 0 4 5 204.68 0 4 5 220.18 0 4 -5 212.18 0 4 5 204.78 0 4 -5 198.38 0 4 5 207.38 0 4 -5 200.58 0 4 -5 210.58 0 4 -5 205.08 0 -4 -5 194.48 0 -4 5 212.88 0 -4 -5 189.68 0 -4 -5 201.98 0 -4 5 204.68 0 -4 -5 202.68 0 -4 5 187.68 0 -4 5 195.58 0 4 -6 126.19 0 4 6 112.39 0 4 6 112.49 0 4 -6 118.39 0 4 -6 120.59 0 4 6 107.09 0 4 6 105.39 0 4 6 119.29 0 4 -6 116.19 0 -4 6 105.49 0 -4 -6 125.79 0 -4 -6 116.49 0 -4 6 120.09 0 -4 -6 90.39 0 -4 6 111.79 0 -4 -6 118.29 0 -4 6 123.89 0 -4 -6 129.89 0 4 -7 292.07 0 4 -7 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