#------------------------------------------------------------------------------ #$Date: 2018-06-18 18:53:46 +0300 (Mon, 18 Jun 2018) $ #$Revision: 208483 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/11/2021167.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_2021167 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 H17 I N2 O4' _chemical_formula_moiety 'C19 H17 I N2 O4' _chemical_formula_sum 'C19 H17 I N2 O4' _chemical_formula_weight 464.24 _chemical_name_systematic ; 2-(4-Acetyl-5-methyl-5-phenyl-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 _cell_angle_alpha 90 _cell_angle_beta 110.180(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8370(10) _cell_length_b 20.0560(10) _cell_length_c 11.0150(10) _cell_measurement_reflns_used 9773 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.10 _cell_measurement_theta_min 3.19 _cell_volume 1832.4(3) _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 0.998 _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 0.0285 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 54289 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.506 _diffrn_reflns_theta_min 2.830 _exptl_absorpt_coefficient_mu 1.774 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.683 _exptl_crystal_description block _exptl_crystal_F_000 920 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.974 _refine_diff_density_min -0.587 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 5600 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0217 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.2207P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0500 _reflns_number_gt 4994 _reflns_number_total 5600 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL test2_a.res in P2(1)/c 4h.res created by SHELXL-2016/4 at 15:19:26 on 09-Aug-2017 REM OMIT -4 57 REM SHEL 999 0.74 CELL 0.71073 8.837 20.056 11.015 90 110.18 90 ZERR 4 0.001 0.001 0.001 0 0.01 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N O UNIT 76 68 4 8 16 L.S. 25 PLAN 10 TEMP -173(2) BOND $H LIST 4 HTAB fmap 2 acta CONF MERG 2 SHEL 999 0.7 REM REM REM WGHT 0.021200 1.220700 FVAR 0.32033 I1 3 1.022734 0.443776 0.710434 11.00000 0.02366 0.02116 = 0.02296 0.00274 0.00299 0.00370 O1 5 0.421889 0.510045 0.222996 11.00000 0.01883 0.02013 = 0.01835 0.00029 0.00382 -0.00315 N1 4 0.441049 0.639179 0.324331 11.00000 0.01748 0.01511 = 0.01920 -0.00220 0.00655 0.00002 C1 1 0.819184 0.465195 0.548444 11.00000 0.01844 0.01785 = 0.01924 0.00280 0.00641 0.00054 O2 5 0.572138 0.561728 0.121941 11.00000 0.02565 0.03092 = 0.02384 0.00421 0.00959 -0.00085 N2 4 0.436324 0.705644 0.362216 11.00000 0.01632 0.01588 = 0.01747 -0.00233 0.00407 0.00101 C2 1 0.752168 0.528387 0.536421 11.00000 0.01924 0.01711 = 0.01726 0.00007 0.00703 -0.00095 AFIX 43 H2 2 0.795397 0.560319 0.603141 11.00000 -1.20000 AFIX 0 O3 5 0.638888 0.654917 0.515838 11.00000 0.02409 0.01543 = 0.01479 -0.00071 0.00292 0.00268 C3 1 0.620969 0.545355 0.426300 11.00000 0.01670 0.01576 = 0.01748 0.00026 0.00775 -0.00080 O4 5 0.319863 0.806868 0.325973 11.00000 0.02334 0.01899 = 0.02902 0.00072 0.00829 0.00377 C4 1 0.558998 0.497056 0.330341 11.00000 0.01734 0.01800 = 0.01724 0.00092 0.00600 -0.00262 C5 1 0.626220 0.434044 0.342302 11.00000 0.02568 0.01663 = 0.02297 -0.00288 0.00704 -0.00248 AFIX 43 H5 2 0.582960 0.401921 0.275960 11.00000 -1.20000 AFIX 0 C6 1 0.757325 0.417771 0.451670 11.00000 0.02627 0.01455 = 0.02635 0.00022 0.00821 0.00137 AFIX 43 H6 2 0.804238 0.374628 0.460211 11.00000 -1.20000 AFIX 0 C7 1 0.559007 0.613428 0.416335 11.00000 0.01767 0.01650 = 0.01507 -0.00125 0.00682 -0.00082 C8 1 0.580149 0.721910 0.477730 11.00000 0.01816 0.01653 = 0.01409 -0.00102 0.00464 0.00284 C9 1 0.705619 0.760142 0.439526 11.00000 0.01621 0.01969 = 0.01325 -0.00217 0.00285 0.00081 C10 1 0.823499 0.725499 0.407449 11.00000 0.01985 0.02432 = 0.02353 -0.00333 0.00766 0.00207 AFIX 43 H10 2 0.828901 0.678281 0.414448 11.00000 -1.20000 AFIX 0 C11 1 0.932935 0.759595 0.365373 11.00000 0.01952 0.03877 = 0.03035 -0.00332 0.01107 0.00007 AFIX 43 H11 2 1.012829 0.735524 0.343917 11.00000 -1.20000 AFIX 0 C12 1 0.926623 0.828276 0.354434 11.00000 0.02006 0.03999 = 0.02723 0.00196 0.00712 -0.00648 AFIX 43 H12 2 1.001008 0.851359 0.324678 11.00000 -1.20000 AFIX 0 C13 1 0.810945 0.863211 0.387209 11.00000 0.02765 0.02432 = 0.03612 0.00138 0.00901 -0.00434 AFIX 43 H13 2 0.806516 0.910437 0.380223 11.00000 -1.20000 AFIX 0 C14 1 0.701178 0.829587 0.430301 11.00000 0.02143 0.02076 = 0.02787 -0.00177 0.00800 0.00146 AFIX 43 H14 2 0.623057 0.853966 0.453485 11.00000 -1.20000 AFIX 0 C15 1 0.442345 0.545745 0.123451 11.00000 0.02446 0.01682 = 0.01693 -0.00207 0.00584 0.00034 C16 1 0.282988 0.558917 0.021035 11.00000 0.02641 0.02989 = 0.02065 -0.00033 0.00144 0.00217 AFIX 137 H16A 2 0.245772 0.518532 -0.030777 11.00000 -1.50000 H16B 2 0.294126 0.595176 -0.034930 11.00000 -1.50000 H16C 2 0.204476 0.571687 0.061592 11.00000 -1.50000 AFIX 0 C17 1 0.537859 0.752170 0.587517 11.00000 0.03074 0.02509 = 0.01789 -0.00196 0.01218 0.00416 AFIX 137 H17A 2 0.456948 0.724354 0.605601 11.00000 -1.50000 H17B 2 0.494300 0.797093 0.563247 11.00000 -1.50000 H17C 2 0.634896 0.754692 0.664922 11.00000 -1.50000 AFIX 0 C18 1 0.317884 0.748274 0.293430 11.00000 0.01490 0.02040 = 0.01953 0.00263 0.00849 0.00173 C19 1 0.188625 0.719297 0.177785 11.00000 0.01625 0.02654 = 0.02307 0.00130 0.00396 0.00078 AFIX 137 H19A 2 0.101667 0.751907 0.143604 11.00000 -1.50000 H19B 2 0.145536 0.678758 0.203469 11.00000 -1.50000 H19C 2 0.234431 0.708341 0.110914 11.00000 -1.50000 AFIX 0 HKLF 4 REM test2_a.res in P2(1)/c REM R1 = 0.0217 for 4994 Fo > 4sig(Fo) and 0.0266 for all 5600 data REM 238 parameters refined using 0 restraints END WGHT 0.0212 1.2206 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y-1/2, -z+1/ HTAB C5 O4_$1 EQIV $2 x-1, y, z- HTAB C16 I1_$2 EQIV $3 x, -y+3/2, z-1/ HTAB C16 O4_$3 HTAB C17 O4 EQIV $4 -x+1, -y+1, -z+ HTAB C19 I1_$4 REM Highest difference peak 0.974, deepest hole -0.587, 1-sigma level 0.070 Q1 1 0.9686 0.4521 0.7494 11.00000 0.05 0.97 Q2 1 0.9828 0.4302 0.6549 11.00000 0.05 0.57 Q3 1 0.7993 0.4418 0.4940 11.00000 0.05 0.46 Q4 1 1.0835 0.4283 0.7414 11.00000 0.05 0.45 Q5 1 0.7579 0.7426 0.4240 11.00000 0.05 0.43 Q6 1 0.5902 0.5191 0.3796 11.00000 0.05 0.42 Q7 1 0.0632 0.5563 0.1203 11.00000 0.05 0.42 Q8 1 0.3563 0.5522 0.0752 11.00000 0.05 0.42 Q9 1 0.6741 0.5333 0.4783 11.00000 0.05 0.42 Q10 1 1.0178 0.8296 0.2083 11.00000 0.05 0.40 REM The information below was added by Olex2. REM REM R1 = 0.0217 for 4994 Fo > 4sig(Fo) and 0.0266 for all 61001 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.97, deepest hole -0.59 REM Mean Shift 0, Max Shift 0.003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0266 REM R1_gt = 0.0217 REM wR_ref = 0.0500 REM GOOF = 1.045 REM Shift_max = 0.003 REM Shift_mean = 0 REM Reflections_all = 61001 REM Reflections_gt = 4994 REM Parameters = n/a REM Hole = -0.59 REM Peak = 0.97 REM Flack = n/a ; _cod_data_source_file sk3693sup1.cif _cod_data_source_block 6c _cod_database_code 2021167 _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 1.02273(2) 0.44378(2) 0.71043(2) 0.02391(4) Uani d 1 O O1 0.42189(12) 0.51004(5) 0.22300(10) 0.0198(2) Uani d 1 N N1 0.44105(14) 0.63918(6) 0.32433(11) 0.0172(2) Uani d 1 C C1 0.81918(17) 0.46520(7) 0.54844(14) 0.0185(3) Uani d 1 O O2 0.57214(14) 0.56173(6) 0.12194(11) 0.0265(2) Uani d 1 N N2 0.43632(14) 0.70564(6) 0.36222(11) 0.0170(2) Uani d 1 C C2 0.75217(17) 0.52839(7) 0.53642(13) 0.0177(3) Uani d 1 H H2 0.795397 0.560319 0.603141 0.021 Uiso calc 1 O O3 0.63889(13) 0.65492(5) 0.51584(9) 0.0191(2) Uani d 1 C C3 0.62097(16) 0.54536(7) 0.42630(13) 0.0162(2) Uani d 1 O O4 0.31986(13) 0.80687(5) 0.32597(11) 0.0240(2) Uani d 1 C C4 0.55900(17) 0.49706(7) 0.33034(13) 0.0175(3) Uani d 1 C C5 0.62622(19) 0.43404(7) 0.34230(15) 0.0221(3) Uani d 1 H H5 0.582960 0.401921 0.275960 0.027 Uiso calc 1 C C6 0.75733(19) 0.41777(7) 0.45167(15) 0.0226(3) Uani d 1 H H6 0.804238 0.374628 0.460211 0.027 Uiso calc 1 C C7 0.55901(16) 0.61343(7) 0.41634(13) 0.0161(2) Uani d 1 C C8 0.58015(17) 0.72191(7) 0.47773(13) 0.0165(2) Uani d 1 C C9 0.70562(16) 0.76014(7) 0.43953(13) 0.0170(2) Uani d 1 C C10 0.82350(18) 0.72550(8) 0.40745(15) 0.0225(3) Uani d 1 H H10 0.828901 0.678281 0.414448 0.027 Uiso calc 1 C C11 0.93294(19) 0.75959(9) 0.36537(16) 0.0289(3) Uani d 1 H H11 1.012829 0.735524 0.343917 0.035 Uiso calc 1 C C12 0.92662(19) 0.82828(9) 0.35443(16) 0.0294(3) Uani d 1 H H12 1.001008 0.851359 0.324678 0.035 Uiso calc 1 C C13 0.8109(2) 0.86321(9) 0.38721(17) 0.0299(3) Uani d 1 H H13 0.806516 0.910437 0.380223 0.036 Uiso calc 1 C C14 0.70118(18) 0.82959(8) 0.43030(15) 0.0235(3) Uani d 1 H H14 0.623057 0.853966 0.453485 0.028 Uiso calc 1 C C15 0.44235(18) 0.54575(7) 0.12345(14) 0.0197(3) Uani d 1 C C16 0.2830(2) 0.55892(8) 0.02103(15) 0.0274(3) Uani d 1 H H16A 0.245772 0.518532 -0.030777 0.041 Uiso calc 1 H H16B 0.294126 0.595176 -0.034930 0.041 Uiso calc 1 H H16C 0.204476 0.571687 0.061592 0.041 Uiso calc 1 C C17 0.5379(2) 0.75217(8) 0.58752(14) 0.0236(3) Uani d 1 H H17A 0.456948 0.724354 0.605601 0.035 Uiso calc 1 H H17B 0.494300 0.797093 0.563247 0.035 Uiso calc 1 H H17C 0.634896 0.754692 0.664922 0.035 Uiso calc 1 C C18 0.31788(16) 0.74827(7) 0.29343(13) 0.0176(3) Uani d 1 C C19 0.18862(18) 0.71930(8) 0.17778(15) 0.0227(3) Uani d 1 H H19A 0.101667 0.751907 0.143604 0.034 Uiso calc 1 H H19B 0.145536 0.678758 0.203469 0.034 Uiso calc 1 H H19C 0.234431 0.708341 0.110914 0.034 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 0.02366(5) 0.02116(5) 0.02296(5) 0.00370(3) 0.00299(4) 0.00274(3) O1 0.0188(5) 0.0201(5) 0.0183(5) -0.0032(4) 0.0038(4) 0.0003(4) N1 0.0175(5) 0.0151(5) 0.0192(5) 0.0000(4) 0.0065(4) -0.0022(4) C1 0.0184(6) 0.0178(6) 0.0192(6) 0.0005(5) 0.0064(5) 0.0028(5) O2 0.0257(6) 0.0309(6) 0.0238(5) -0.0008(4) 0.0096(4) 0.0042(4) N2 0.0163(5) 0.0159(5) 0.0175(5) 0.0010(4) 0.0041(4) -0.0023(4) C2 0.0192(6) 0.0171(6) 0.0173(6) -0.0010(5) 0.0070(5) 0.0001(5) O3 0.0241(5) 0.0154(5) 0.0148(4) 0.0027(4) 0.0029(4) -0.0007(4) C3 0.0167(6) 0.0158(6) 0.0175(6) -0.0008(5) 0.0078(5) 0.0003(5) O4 0.0233(5) 0.0190(5) 0.0290(5) 0.0038(4) 0.0083(4) 0.0007(4) C4 0.0173(6) 0.0180(6) 0.0172(6) -0.0026(5) 0.0060(5) 0.0009(5) C5 0.0257(7) 0.0166(7) 0.0230(7) -0.0025(5) 0.0070(6) -0.0029(5) C6 0.0263(7) 0.0145(6) 0.0264(7) 0.0014(5) 0.0082(6) 0.0002(5) C7 0.0177(6) 0.0165(6) 0.0151(6) -0.0008(5) 0.0068(5) -0.0013(5) C8 0.0182(6) 0.0165(6) 0.0141(6) 0.0028(5) 0.0046(5) -0.0010(5) C9 0.0162(6) 0.0197(6) 0.0133(6) 0.0008(5) 0.0028(5) -0.0022(5) C10 0.0198(7) 0.0243(7) 0.0235(7) 0.0021(5) 0.0077(5) -0.0033(6) C11 0.0195(7) 0.0388(9) 0.0304(8) 0.0001(6) 0.0111(6) -0.0033(7) C12 0.0201(7) 0.0400(9) 0.0272(8) -0.0065(6) 0.0071(6) 0.0020(7) C13 0.0276(8) 0.0243(8) 0.0361(9) -0.0043(6) 0.0090(7) 0.0014(7) C14 0.0214(7) 0.0208(7) 0.0279(7) 0.0015(5) 0.0080(6) -0.0018(6) C15 0.0245(7) 0.0168(6) 0.0169(6) 0.0003(5) 0.0058(5) -0.0021(5) C16 0.0264(8) 0.0299(8) 0.0206(7) 0.0022(6) 0.0014(6) -0.0003(6) C17 0.0307(8) 0.0251(7) 0.0179(6) 0.0042(6) 0.0122(6) -0.0020(5) C18 0.0149(6) 0.0204(6) 0.0195(6) 0.0017(5) 0.0085(5) 0.0026(5) C19 0.0162(6) 0.0265(7) 0.0231(7) 0.0008(5) 0.0040(5) 0.0013(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 117.34(11) C7 N1 N2 104.29(11) C2 C1 I1 118.81(10) C2 C1 C6 120.65(13) C6 C1 I1 120.47(11) N1 N2 C8 110.97(11) C18 N2 N1 121.85(12) C18 N2 C8 127.06(12) C1 C2 H2 119.9 C1 C2 C3 120.26(13) C3 C2 H2 119.9 C7 O3 C8 107.38(10) C2 C3 C7 117.97(12) C4 C3 C2 118.53(13) C4 C3 C7 123.48(13) O1 C4 C3 120.69(12) C5 C4 O1 118.05(12) C5 C4 C3 121.16(13) C4 C5 H5 120.0 C4 C5 C6 119.91(14) C6 C5 H5 120.0 C1 C6 H6 120.3 C5 C6 C1 119.49(14) C5 C6 H6 120.3 N1 C7 O3 116.29(12) N1 C7 C3 128.01(13) O3 C7 C3 115.68(12) N2 C8 C9 111.22(11) N2 C8 C17 113.42(12) O3 C8 N2 99.15(10) O3 C8 C9 108.96(11) O3 C8 C17 107.66(11) C17 C8 C9 115.08(12) C10 C9 C8 119.86(13) C10 C9 C14 118.89(14) C14 C9 C8 121.19(13) C9 C10 H10 119.8 C11 C10 C9 120.41(15) C11 C10 H10 119.8 C10 C11 H11 119.7 C12 C11 C10 120.55(15) C12 C11 H11 119.7 C11 C12 H12 120.3 C11 C12 C13 119.49(15) C13 C12 H12 120.3 C12 C13 H13 119.8 C12 C13 C14 120.47(16) C14 C13 H13 119.8 C9 C14 H14 119.9 C13 C14 C9 120.17(15) C13 C14 H14 119.9 O1 C15 C16 110.24(13) O2 C15 O1 122.81(13) O2 C15 C16 126.93(14) 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 116.25(13) O4 C18 N2 120.54(13) O4 C18 C19 123.21(13) 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 2.0951(14) O1 C4 1.3948(17) O1 C15 1.3727(17) N1 N2 1.4017(16) N1 C7 1.2851(18) C1 C2 1.386(2) C1 C6 1.392(2) O2 C15 1.1966(19) N2 C8 1.4917(18) N2 C18 1.3614(18) C2 H2 0.9500 C2 C3 1.4004(19) O3 C7 1.3631(16) O3 C8 1.4493(16) C3 C4 1.3986(19) C3 C7 1.4610(19) O4 C18 1.2270(18) C4 C5 1.383(2) C5 H5 0.9500 C5 C6 1.392(2) C6 H6 0.9500 C8 C9 1.522(2) C8 C17 1.5107(19) C9 C10 1.395(2) C9 C14 1.396(2) C10 H10 0.9500 C10 C11 1.388(2) C11 H11 0.9500 C11 C12 1.382(3) C12 H12 0.9500 C12 C13 1.386(2) C13 H13 0.9500 C13 C14 1.392(2) 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 1.504(2) 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 C5 H5 O4 2_645 0.95 2.51 3.2828(19) 139 yes C16 H16B O4 4_575 0.98 2.55 3.529(2) 177 yes C17 H17C Cg3 4_576 0.98 2.70 3.5766(17) 150 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 176.86(10) I1 C1 C6 C5 -177.27(11) O1 C4 C5 C6 -176.23(13) N1 N2 C8 O3 -13.43(13) N1 N2 C8 C9 101.12(13) N1 N2 C8 C17 -127.29(12) N1 N2 C18 O4 -177.27(12) N1 N2 C18 C19 2.50(19) C1 C2 C3 C4 0.6(2) C1 C2 C3 C7 -177.68(13) N2 N1 C7 O3 -0.09(16) N2 N1 C7 C3 -178.50(13) N2 C8 C9 C10 -88.99(15) N2 C8 C9 C14 88.16(15) C2 C1 C6 C5 -0.4(2) C2 C3 C4 O1 175.70(12) C2 C3 C4 C5 -0.8(2) C2 C3 C7 N1 179.85(14) C2 C3 C7 O3 1.42(18) O3 C8 C9 C10 19.29(17) O3 C8 C9 C14 -163.56(12) C3 C4 C5 C6 0.3(2) C4 O1 C15 O2 5.2(2) C4 O1 C15 C16 -176.26(12) C4 C3 C7 N1 1.6(2) C4 C3 C7 O3 -176.80(12) C4 C5 C6 C1 0.3(2) C6 C1 C2 C3 0.0(2) C7 N1 N2 C8 9.02(14) C7 N1 N2 C18 -174.80(12) C7 O3 C8 N2 12.66(13) C7 O3 C8 C9 -103.64(12) C7 O3 C8 C17 130.93(12) C7 C3 C4 O1 -6.1(2) C7 C3 C4 C5 177.43(13) C8 N2 C18 O4 -1.7(2) C8 N2 C18 C19 178.03(12) C8 O3 C7 N1 -8.94(16) C8 O3 C7 C3 169.68(11) C8 C9 C10 C11 176.32(14) C8 C9 C14 C13 -175.89(14) C9 C10 C11 C12 -0.1(2) C10 C9 C14 C13 1.3(2) C10 C11 C12 C13 0.7(3) C11 C12 C13 C14 -0.3(3) C12 C13 C14 C9 -0.7(3) C14 C9 C10 C11 -0.9(2) C15 O1 C4 C3 81.18(16) C15 O1 C4 C5 -102.23(15) C17 C8 C9 C10 140.28(14) C17 C8 C9 C14 -42.57(18) C18 N2 C8 O3 170.64(12) C18 N2 C8 C9 -74.81(16) C18 N2 C8 C17 56.77(18) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas -2 0 0 2545.05 -2 0 0 2552.64 2 0 0 2570.34 2 0 0 2776.52 2 0 0 2550.44 3 0 0 2144.29 3 0 0 2232.48 3 0 0 2111.99 -3 0 0 2151.48 -3 0 0 2182.38 4 0 0 1126.89 -4 0 0 1083.39 4 0 0 1052.49 4 0 0 1103.59 -4 0 0 1129.09 -5 0 0 1916.71 -5 0 0 1929.31 5 0 0 1913.11 5 0 0 1885.31 5 0 0 1962.9 6 0 0 110.89 -6 0 0 113.29 6 0 0 122.29 6 0 0 124.79 -7 0 0 647.14 7 0 0 653.93 7 0 0 651.33 8 0 0 90.29 -8 0 0 98.29 8 0 0 99.49 9 0 0 71.19 -9 0 0 69.59 9 0 0 64.09 10 0 0 -5.3 -10 0 0 -1.1 11 0 0 21.2 -11 0 0 29.8 -12 0 0 -8.7 12 0 0 3.4 -2 -1 0 131.99 -2 -1 0 136.69 2 -1 0 141.79 -2 -1 0 135.79 -2 -1 0 128.79 2 -1 0 130.19 2 -1 0 134.39 2 1 0 148.79 2 1 0 129.99 -2 1 0 140.59 -2 1 0 136.89 2 1 0 129.39 -2 1 0 133.59 -3 -1 0 412.16 3 -1 0 414.26 -3 -1 0 408.66 -3 -1 0 412.76 3 -1 0 456.35 3 -1 0 388.06 -3 -1 0 410.76 -3 1 0 414.56 3 1 0 419.86 3 1 0 424.26 3 1 0 404.56 -3 1 0 388.16 4 -1 0 115.39 4 -1 0 108.79 4 -1 0 106.79 4 1 0 111.69 4 1 0 108.49 -4 1 0 116.59 4 1 0 113.59 -4 1 0 117.39 5 -1 0 117.89 -5 -1 0 113.69 5 -1 0 113.59 -5 -1 0 116.19 5 -1 0 116.09 5 1 0 108.19 -5 1 0 116.59 5 1 0 119.89 -5 1 0 111.99 5 1 0 121.09 6 -1 0 158.98 6 -1 0 149.79 -6 -1 0 154.48 6 1 0 180.58 -6 1 0 155.88 6 1 0 153.08 6 1 0 149.09 -7 -1 0 34.6 7 -1 0 33.9 7 -1 0 35.9 7 1 0 35 7 1 0 31.5 -8 -1 0 90.89 8 -1 0 89.09 8 1 0 88.39 8 1 0 59.99 -8 1 0 86.59 -9 -1 0 27.2 9 -1 0 36.8 9 -1 0 26.8 -9 1 0 32.9 9 1 0 26.3 9 1 0 28.3 -10 -1 0 -0.2 10 -1 0 -1.7 -10 1 0 0.5 10 1 0 -3.4 -11 -1 0 24.6 11 -1 0 19.7 11 1 0 18.4 -11 1 0 27.6 -12 -1 0 2.3 12 -1 0 7.6 12 1 0 8.4 -12 1 0 2.5 -1 -2 0 860.01 1 -2 0 956.8 -1 -2 0 870.11 1 -2 0 989.4 1 -2 0 975.6 -1 -2 0 975.6 1 -2 0 901.21 -1 -2 0 935.21 1 2 0 997.8 -1 2 0 1066.59 1 2 0 978.8 -1 2 0 922.41 -1 2 0 1007.4 1 2 0 1002.1 -1 2 0 882.61 2 -2 0 2126.99 -2 -2 0 2051.39 2 -2 0 2040 -2 -2 0 2107.39 2 -2 0 2039.8 -2 -2 0 1997.7 2 -2 0 2084.49 -2 -2 0 1974.4 -2 2 0 2035.5 2 2 0 1990.9 -2 2 0 2035.9 2 2 0 1947.41 -2 2 0 2053.19 -2 2 0 1935.31 -3 -2 0 782.92 -3 -2 0 746.23 3 -2 0 762.02 3 -2 0 746.53 -3 -2 0 776.02 3 -2 0 772.72 -3 -2 0 783.92 3 -2 0 756.72 3 -2 0 779.82 3 2 0 785.32 -3 2 0 791.22 -3 2 0 734.23 -3 2 0 755.82 -3 2 0 812.02 3 2 0 798.12 -4 -2 0 889.81 -4 -2 0 889.21 4 -2 0 918.31 4 -2 0 883.91 -4 -2 0 885.41 -4 -2 0 885.41 -4 -2 0 815.22 -4 -2 0 828.92 4 -2 0 849.72 -4 2 0 875.71 4 2 0 912.91 4 2 0 857.91 4 2 0 880.01 -5 -2 0 1471.05 5 -2 0 1452.45 5 -2 0 1482.65 -5 -2 0 1484.45 5 -2 0 1463.55 5 2 0 1422.46 5 2 0 1479.25 5 2 0 1497.65 6 -2 0 11.6 -6 -2 0 10 6 -2 0 12.9 -6 -2 0 9.7 6 -2 0 12.3 -6 2 0 11.8 6 2 0 15 6 2 0 10.2 6 2 0 8 7 -2 0 228.38 7 -2 0 223.48 -7 -2 0 215.08 -7 2 0 217.88 7 2 0 234.88 7 2 0 225.88 -8 -2 0 287.07 8 -2 0 272.47 8 -2 0 263.97 8 2 0 280.07 8 2 0 295.27 -8 2 0 271.07 9 -2 0 21.7 9 -2 0 18.9 -9 -2 0 17.6 -9 2 0 25.1 9 2 0 24.4 9 2 0 23 -10 -2 0 10.7 10 -2 0 6.1 -10 2 0 3.1 10 2 0 1.9 11 -2 0 -4.7 -11 -2 0 4.6 11 2 0 -0.9 -11 2 0 6.7 -12 -2 0 2.4 12 -2 0 -0.8 12 2 0 7.2 -12 2 0 0.9 0 -3 0 -1.5 0 -3 0 -1.7 0 -3 0 -1.9 0 3 0 -1 0 3 0 -1.9 0 3 0 -1.4 1 -3 0 4.5 1 -3 0 4.8 -1 -3 0 4.1 1 -3 0 4.1 1 -3 0 3.2 1 -3 0 4.8 -1 -3 0 4 -1 -3 0 3.2 -1 -3 0 3.1 1 3 0 4.1 1 3 0 3.8 1 3 0 3.7 1 3 0 5.7 -1 3 0 5.1 1 3 0 3.8 -1 3 0 4.5 -1 3 0 4.8 -1 3 0 3.1 -2 -3 0 57.69 2 -3 0 58.79 2 -3 0 58.59 2 -3 0 58.69 -2 -3 0 60.09 2 -3 0 56.39 -2 -3 0 59.29 -2 -3 0 56.99 -2 3 0 57.39 2 3 0 69.69 -2 3 0 58.19 -2 3 0 60.09 2 3 0 61.19 2 3 0 56.99 2 3 0 53.49 3 -3 0 374.16 -3 -3 0 382.36 3 -3 0 367.16 3 -3 0 384.86 -3 -3 0 379.26 -3 -3 0 379.76 3 -3 0 376.66 -3 -3 0 366.46 3 -3 0 350.36 -3 3 0 374.66 3 3 0 370.56 -3 3 0 366.26 -3 3 0 381.36 3 3 0 386.06 3 3 0 344.77 -4 -3 0 298.07 4 -3 0 317.77 4 -3 0 340.67 -4 -3 0 321.27 -4 -3 0 336.37 4 -3 0 329.57 4 -3 0 322.87 -4 -3 0 323.27 -4 -3 0 331.97 -4 3 0 325.77 4 3 0 339.67 -4 3 0 321.67 4 3 0 334.97 -5 -3 0 208.28 -5 -3 0 205.88 5 -3 0 209.08 -5 -3 0 209.58 -5 -3 0 208.98 -5 -3 0 205.48 5 -3 0 196.68 -5 -3 0 209.98 5 -3 0 208.78 -5 3 0 204.98 5 3 0 206.88 5 3 0 217.98 5 3 0 211.98 -6 -3 0 513.45 -6 -3 0 522.15 6 -3 0 548.85 6 -3 0 528.75 6 -3 0 511.35 6 3 0 522.55 -6 3 0 518.05 6 3 0 544.55 6 3 0 525.25 7 -3 0 486.95 7 -3 0 456.25 -7 -3 0 440.76 7 3 0 455.55 7 3 0 431.96 -7 3 0 443.66 8 -3 0 223.38 8 -3 0 234.68 -8 -3 0 234.18 8 3 0 238.58 -8 3 0 236.18 8 3 0 229.68 9 -3 0 209.18 -9 -3 0 214.28 9 -3 0 240.78 9 3 0 216.58 9 3 0 219.28 -9 3 0 234.88 10 -3 0 324.87 -10 -3 0 323.97 10 3 0 344.57 -10 3 0 349.77 11 -3 0 115.39 -11 -3 0 120.19 11 3 0 120.59 -11 3 0 128.79 12 -3 0 84.09 -12 -3 0 94.59 12 3 0 110.39 -12 3 0 83.89 0 -4 0 2439.56 0 -4 0 2476.75 0 -4 0 2581.14 0 -4 0 2503.75 0 4 0 2549.54 0 4 0 2504.25 0 4 0 2513.25 1 -4 0 4.4 -1 -4 0 3.9 -1 -4 0 4.6 1 -4 0 5.1 1 -4 0 5.4 -1 -4 0 4.8 1 -4 0 5.3 -1 -4 0 5.7 -1 4 0 5.3 1 4 0 7.1 -1 4 0 4.4 -1 4 0 4.3 -1 4 0 5.4 1 4 0 4 -1 4 0 5.8 1 4 0 4.1 1 4 0 4 1 4 0 5.1 2 -4 0 93.49 -2 -4 0 103.29 -2 -4 0 105.29 2 -4 0 103.59 2 -4 0 103.59 2 -4 0 106.69 2 -4 0 106.29 -2 -4 0 104.19 2 4 0 104.39 -2 4 0 98.09 -2 4 0 108.29 2 4 0 107.19 2 4 0 101.49 -2 4 0 117.29 -2 4 0 106.89 -3 -4 0 8.4 3 -4 0 12.5 3 -4 0 11.9 -3 -4 0 9.6 -3 -4 0 8.9 -3 -4 0 10.4 3 -4 0 7.8 -3 4 0 9.7 3 4 0 10.9 -3 4 0 10.4 3 4 0 8.3 -3 4 0 10.7 -3 4 0 8.2 3 4 0 10.2 4 -4 0 54.19 -4 -4 0 55.79 4 -4 0 49.99 4 -4 0 51.79 4 -4 0 52.59 -4 -4 0 51.89 4 -4 0 49.5 -4 -4 0 47.2 -4 -4 0 46.9 -4 4 0 49 4 4 0 50.99 -4 4 0 49.99 4 4 0 51.19 4 4 0 43.6 -4 4 0 52.29 -4 4 0 49.8 4 4 0 52.69 -5 -4 0 16 -5 -4 0 19.4 5 -4 0 18.8 5 -4 0 18.9 5 -4 0 18.5 -5 -4 0 18.9 -5 -4 0 17.7 -5 -4 0 15.7 5 -4 0 18.3 5 -4 0 17.9 5 4 0 17.5 5 4 0 17 5 4 0 19.7 -6 -4 0 0.8 -6 -4 0 0.7 -6 -4 0 1.5 -6 -4 0 1.8 -6 -4 0 0.9 -6 -4 0 0.6 6 -4 0 -1 6 -4 0 -1.7 6 -4 0 -0.3 6 4 0 2.7 -6 4 0 1.4 6 4 0 -0.2 6 4 0 -0.5 7 -4 0 49.3 7 -4 0 53.29 -7 -4 0 54.29 7 4 0 54.99 7 4 0 52.89 -7 4 0 59.99 -8 -4 0 42.6 8 -4 0 37.8 8 -4 0 40.3 8 4 0 33.8 8 4 0 43.5 -8 4 0 36.6 9 -4 0 -1 -9 -4 0 1.1 9 -4 0 2.6 9 4 0 -1.8 -9 4 0 2.7 9 4 0 1 -10 -4 0 3.6 10 -4 0 6 -10 4 0 4.4 10 4 0 5.2 -11 -4 0 3.1 11 -4 0 -2.5 11 4 0 11.2 -11 4 0 11.5 12 -4 0 -6.8 -12 -4 0 0.3 12 4 0 0.5 -12 4 0 6.3 0 -5 0 -4.4 0 -5 0 -4.9 0 -5 0 -5.2 0 -5 0 -4.8 0 5 0 -4 0 5 0 -5.1 0 5 0 -4 -1 -5 0 87.49 1 -5 0 84.09 -1 -5 0 88.39 1 -5 0 81.79 1 -5 0 88.29 -1 -5 0 88.89 1 -5 0 85.29 1 -5 0 85.99 -1 -5 0 86.79 -1 -5 0 88.39 1 5 0 86.89 1 5 0 88.09 1 5 0 83.69 -1 5 0 88.49 -1 5 0 86.29 -1 5 0 85.09 -1 5 0 84.99 1 5 0 86.99 -1 5 0 81.39 2 -5 0 173.78 -2 -5 0 176.58 2 -5 0 172.88 2 -5 0 175.08 -2 -5 0 170.28 -2 -5 0 172.78 2 -5 0 177.48 2 -5 0 172.28 -2 -5 0 170.28 2 5 0 169.18 -2 5 0 186.48 2 5 0 178.18 -2 5 0 176.78 -2 5 0 173.08 -2 5 0 172.08 2 5 0 170.48 -3 -5 0 851.41 -3 -5 0 857.01 3 -5 0 864.51 -3 -5 0 851.71 3 -5 0 846.12 3 -5 0 868.51 3 -5 0 858.01 3 -5 0 869.11 -3 -5 0 861.81 -3 5 0 813.62 3 5 0 857.81 -3 5 0 870.71 3 5 0 853.51 -3 5 0 856.31 3 5 0 850.11 3 5 0 894.51 4 -5 0 253.17 4 -5 0 257.47 -4 -5 0 263.47 4 -5 0 257.27 -4 -5 0 262.37 -4 -5 0 256.87 4 -5 0 254.37 -4 -5 0 236.88 4 -5 0 255.57 -4 5 0 259.47 4 5 0 250.07 -4 5 0 255.97 4 5 0 260.77 -4 5 0 262.87 -4 5 0 250.07 4 5 0 260.27 4 5 0 259.87 5 -5 0 1120.79 5 -5 0 1148.99 -5 -5 0 1171.88 -5 -5 0 1129.79 5 -5 0 1089.49 5 -5 0 1141.89 -5 -5 0 1120.09 -5 -5 0 1130.19 5 -5 0 1149.08 -5 5 0 1203.58 5 5 0 1057.59 -5 5 0 1146.09 5 5 0 1152.88 5 5 0 1149.48 -6 -5 0 414.16 6 -5 0 357.06 -6 -5 0 352.86 6 -5 0 348.67 -6 -5 0 352.16 -6 -5 0 360.66 6 -5 0 347.67 -6 -5 0 358.66 6 5 0 358.46 -6 5 0 362.96 6 5 0 377.86 6 5 0 366.56 -7 -5 0 364.96 7 -5 0 344.47 7 -5 0 358.86 7 5 0 363.36 -7 5 0 366.46 7 5 0 365.06 8 -5 0 509.25 8 -5 0 471.75 -8 -5 0 477.75 8 5 0 455.45 8 5 0 475.15 -8 5 0 473.85 9 -5 0 355.26 9 -5 0 377.86 -9 -5 0 363.56 9 5 0 374.46 9 5 0 378.46 -9 5 0 358.86 10 -5 0 267.47 -10 -5 0 255.97 -10 5 0 263.87 10 5 0 270.67 11 -5 0 121.99 -11 -5 0 116.09 -11 5 0 138.89 11 5 0 119.89 -12 -5 0 63.09 12 -5 0 63.19 -12 5 0 57.09 12 5 0 59.89 0 -6 0 1417.06 0 -6 0 1369.66 0 -6 0 1434.16 0 -6 0 1386.56 0 6 0 1454.75 0 6 0 1413.56 0 6 0 1369.16 1 -6 0 870.31 1 -6 0 856.41 1 -6 0 901.11 -1 -6 0 872.61 -1 -6 0 868.01 -1 -6 0 858.41 -1 -6 0 875.11 1 -6 0 919.21 -1 6 0 880.51 -1 6 0 912.41 -1 6 0 855.81 -1 6 0 882.71 1 6 0 854.71 1 6 0 838.82 1 6 0 903.71 -1 6 0 866.41 1 6 0 850.61 -2 -6 0 444.66 2 -6 0 437.56 2 -6 0 463.35 -2 -6 0 430.46 2 -6 0 433.46 2 -6 0 450.55 -2 -6 0 438.16 2 -6 0 443.46 -2 -6 0 431.96 2 6 0 425.26 -2 6 0 433.46 2 6 0 425.26 -2 6 0 465.95 2 6 0 427.06 -2 6 0 450.55 -2 6 0 423.06 -2 6 0 415.96 2 6 0 401.26 -3 -6 0 378.56 -3 -6 0 370.76 3 -6 0 371.26 3 -6 0 375.16 3 -6 0 382.16 3 -6 0 369.86 -3 -6 0 364.26 3 -6 0 372.86 -3 -6 0 389.46 -3 6 0 379.56 3 6 0 365.96 -3 6 0 383.46 3 6 0 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