#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022899.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_2022899 loop_ _publ_author_name 'Rajendrakumar, Satyasree' 'Surampudi Venkata Sai Durga, Anuja' 'Balasubramanian, Sridhar' _publ_section_title ; Strategic synthon approach in obtaining cocrystals and cocrystal polymorphs of a high-Z′ system deferiprone -- an anti-thalassemia drug ; _journal_coeditor_code LO5093 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials' _journal_page_first 946 _journal_page_last 964 _journal_paper_doi 10.1107/S205252062100980X _journal_volume 77 _journal_year 2021 _chemical_formula_moiety 'C7 H9 N O2, 2(C6 H6 O3)' _chemical_formula_sum 'C19 H21 N O8' _chemical_formula_weight 391.37 _chemical_name_common 'Deferiprone-Pyrogallol (2:4)' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.592(2) _cell_length_b 9.3121(11) _cell_length_c 26.795(4) _cell_measurement_reflns_used 7479 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.50 _cell_measurement_theta_min 2.32 _cell_volume 3641.0(9) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-100' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1197 _diffrn_reflns_av_unetI/netI 0.1854 _diffrn_reflns_Laue_measured_fraction_full 0.967 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 16757 _diffrn_reflns_point_group_measured_fraction_full 0.772 _diffrn_reflns_point_group_measured_fraction_max 0.760 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.493 _diffrn_reflns_theta_min 2.315 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.428 _exptl_crystal_description block _exptl_crystal_F_000 1648 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.447 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.090 _refine_ls_abs_structure_details ; Flack x determined using 732 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.4(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 565 _refine_ls_number_reflns 6362 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.1648 _refine_ls_R_factor_gt 0.0730 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1301 _refine_ls_wR_factor_ref 0.1557 _reflns_Friedel_coverage 0.546 _reflns_Friedel_fraction_full 0.568 _reflns_Friedel_fraction_max 0.549 _reflns_number_gt 3817 _reflns_number_total 6362 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block KA1032_0m_def-pyro_2_4 _cod_original_cell_volume 3640.9(8) _cod_database_code 2022899 _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. ; _shelx_estimated_absorpt_t_min 0.965 _shelx_estimated_absorpt_t_max 0.980 _shelx_res_file ; TITL KA1032_0m_a.res in Pna2(1) KA1032_0m.res created by SHELXL-2018/3 at 13:05:34 on 30-Sep-2020 CELL 0.71073 14.5918 9.3121 26.7948 90.000 90.000 90.000 ZERR 8.00 0.0020 0.0011 0.0037 0.000 0.000 0.000 LATT -1 SYMM -x, -y, z+1/2 SYMM -x+1/2, y+1/2, z+1/2 SYMM x+1/2, -y+1/2, z SFAC C H N O UNIT 152 168 8 64 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173 OMIT -3 55 DFIX 0.82 0.02 O1A H1O O1B H2O O5A H5O O4C H10O O5C H11O ACTA L.S. 10 FMAP 2 PLAN 5 SIZE 0.32 0.28 0.18 BOND $H CONF EQIV $1 x-1/2, -y+3/2, z EQIV $2 x+1/2, -y+3/2, z EQIV $3 x-1/2, -y+5/2, z EQIV $4 x+1/2, -y+5/2, z EQIV $5 x+1/2, -y+1/2, z HTAB O1A O4A_$1 HTAB O1B O4D_$2 HTAB O3A O2A HTAB O4A O3A HTAB O4A O5D HTAB O5A O2A_$2 HTAB O5A O4A HTAB O3B O5B_$3 HTAB O4B O5A HTAB O5B O4B HTAB O3C O4C HTAB O4C O3D HTAB O5C O3C_$4 HTAB O3D O2B_$1 HTAB O3D O4D HTAB O4D O3A HTAB O5D O2B HTAB C13A O4B_$1 HTAB C6B O2A_$5 HTAB C11D O4C_$2 htab WGHT 0.064600 FVAR 0.32140 MOLE 1 C1A 1 0.356171 0.172884 0.440226 11.00000 0.01077 0.02862 = 0.01322 0.00174 -0.00301 -0.00188 C2A 1 0.356200 0.321924 0.445348 11.00000 0.00823 0.01754 = 0.01586 -0.00154 -0.00282 -0.00020 C3A 1 0.438128 0.402265 0.443353 11.00000 0.00804 0.02134 = 0.01100 0.00306 -0.00189 -0.00292 C4A 1 0.519759 0.324604 0.434332 11.00000 0.00370 0.02736 = 0.01913 0.00032 0.00044 -0.00031 AFIX 43 H4A 2 0.576537 0.373994 0.431810 11.00000 -1.20000 AFIX 0 C5A 1 0.517098 0.178245 0.429225 11.00000 0.01042 0.02701 = 0.02160 -0.00134 0.00131 0.00696 AFIX 43 H5A 2 0.572644 0.127773 0.423365 11.00000 -1.20000 AFIX 0 C6A 1 0.441395 -0.054943 0.427686 11.00000 0.01820 0.02103 = 0.03206 0.00277 -0.00102 0.00194 AFIX 137 H6A 2 0.394029 -0.087117 0.404292 11.00000 -1.50000 H6B 2 0.430649 -0.098587 0.460449 11.00000 -1.50000 H6C 2 0.501808 -0.083940 0.415288 11.00000 -1.50000 AFIX 0 C7A 1 0.270688 0.086455 0.442554 11.00000 0.02397 0.01981 = 0.02755 -0.00052 -0.00601 -0.00269 AFIX 137 H7A 2 0.254302 0.053989 0.408928 11.00000 -1.50000 H7B 2 0.220969 0.145466 0.456118 11.00000 -1.50000 H7C 2 0.280410 0.002903 0.464153 11.00000 -1.50000 AFIX 0 O1A 4 0.274810 0.387922 0.453894 11.00000 0.00507 0.02125 = 0.02613 0.00122 0.00131 0.00381 H1O 2 0.280835 0.477025 0.452662 11.00000 0.05605 O2A 4 0.434713 0.541475 0.449462 11.00000 0.00738 0.01895 = 0.01878 -0.00154 0.00103 -0.00249 N1A 3 0.437918 0.103459 0.432267 11.00000 0.01450 0.02195 = 0.01797 -0.00123 -0.00409 0.00339 MOLE 2 C1B 1 0.965663 0.174625 0.563012 11.00000 0.01705 0.01937 = 0.01372 0.00228 -0.00084 -0.00179 C2B 1 0.965921 0.319678 0.558252 11.00000 0.00792 0.02056 = 0.01597 -0.00180 0.00256 -0.00392 C3B 1 0.883528 0.403136 0.559987 11.00000 0.01144 0.02333 = 0.00628 -0.00126 -0.00137 -0.00048 C4B 1 0.803255 0.324177 0.568157 11.00000 0.01413 0.01973 = 0.01743 0.00117 0.00037 -0.00029 AFIX 43 H4B 2 0.746618 0.373940 0.570732 11.00000 -1.20000 AFIX 0 C5B 1 0.803595 0.181040 0.572461 11.00000 0.00523 0.03003 = 0.01753 -0.00218 -0.00011 -0.00392 AFIX 43 H5B 2 0.747149 0.132030 0.577152 11.00000 -1.20000 AFIX 0 C6B 1 0.879639 -0.054544 0.573588 11.00000 0.03209 0.02304 = 0.02167 0.00616 0.00260 -0.00448 AFIX 137 H6D 2 0.816281 -0.086581 0.578407 11.00000 -1.50000 H6E 2 0.917147 -0.086234 0.601857 11.00000 -1.50000 H6F 2 0.903942 -0.095843 0.542660 11.00000 -1.50000 AFIX 0 C7B 1 1.051258 0.088989 0.560623 11.00000 0.01826 0.01967 = 0.02808 -0.00073 -0.00410 0.00715 AFIX 137 H7D 2 1.042701 0.008030 0.537725 11.00000 -1.50000 H7E 2 1.066167 0.052628 0.593971 11.00000 -1.50000 H7F 2 1.101460 0.149728 0.548595 11.00000 -1.50000 AFIX 0 O1B 4 1.047167 0.388045 0.549753 11.00000 0.00968 0.01943 = 0.02773 0.00343 0.00095 0.00202 H2O 2 1.039644 0.474909 0.542489 11.00000 0.04580 O2B 4 0.887548 0.541615 0.554299 11.00000 0.01064 0.01983 = 0.01902 0.00242 0.00053 0.00012 N1B 3 0.881981 0.104468 0.570315 11.00000 0.01918 0.01441 = 0.01597 -0.00026 0.00280 -0.00305 MOLE 3 C8A 1 0.627424 0.702388 0.413843 11.00000 0.01385 0.01582 = 0.01209 -0.00062 0.00088 0.00688 C9A 1 0.711833 0.770708 0.414310 11.00000 0.01109 0.01576 = 0.01374 -0.00112 -0.00304 0.00523 C10A 1 0.756912 0.799941 0.369771 11.00000 0.01303 0.01609 = 0.01773 -0.00016 0.00129 -0.00024 C11A 1 0.717538 0.765374 0.324913 11.00000 0.01326 0.03021 = 0.01598 -0.00039 0.00176 0.00444 AFIX 43 H11A 2 0.748141 0.787077 0.294542 11.00000 -1.20000 AFIX 0 C12A 1 0.633000 0.698727 0.324236 11.00000 0.02384 0.03172 = 0.01349 -0.00226 -0.00336 -0.00113 AFIX 43 H12A 2 0.605602 0.675173 0.293132 11.00000 -1.20000 AFIX 0 C13A 1 0.586948 0.665251 0.368592 11.00000 0.01439 0.02056 = 0.01644 0.00279 -0.00524 -0.00542 AFIX 43 H13A 2 0.529222 0.618127 0.367821 11.00000 -1.20000 AFIX 0 O3A 4 0.586325 0.672610 0.458763 11.00000 0.00795 0.02825 = 0.01193 0.00024 0.00007 -0.00731 H3O 2 0.527613 0.637155 0.453359 11.00000 0.03388 O4A 4 0.754670 0.812916 0.458115 11.00000 0.02251 0.02157 = 0.01349 0.00300 -0.00158 -0.00926 H4O 2 0.733712 0.757331 0.478774 11.00000 0.00848 O5A 4 0.842328 0.862303 0.369946 11.00000 0.01101 0.02827 = 0.01853 0.00364 -0.00163 -0.00547 H5O 2 0.862025 0.856991 0.398356 11.00000 0.11702 MOLE 4 C8B 1 0.848357 1.264201 0.310595 11.00000 0.01611 0.03474 = 0.01363 0.00161 -0.00049 -0.00326 C9B 1 0.932065 1.193086 0.310822 11.00000 0.00923 0.02160 = 0.01599 0.00289 -0.00234 -0.00292 C10B 1 1.012471 1.273180 0.306223 11.00000 0.01661 0.03298 = 0.01247 0.00246 0.00066 0.00338 C11B 1 1.010739 1.422249 0.300985 11.00000 0.02095 0.03289 = 0.02050 0.00089 0.00252 -0.01162 AFIX 43 H11B 2 1.065798 1.475824 0.297616 11.00000 -1.20000 AFIX 0 C12B 1 0.923963 1.491174 0.300858 11.00000 0.03936 0.02515 = 0.01778 0.00232 -0.00046 0.00359 AFIX 43 H12B 2 0.920408 1.592532 0.297330 11.00000 -1.20000 AFIX 0 C13B 1 0.844845 1.411581 0.305834 11.00000 0.01630 0.03301 = 0.02077 -0.00008 -0.00068 0.00748 AFIX 43 H13B 2 0.787149 1.458846 0.305987 11.00000 -1.20000 AFIX 0 O3B 4 0.772849 1.175760 0.315967 11.00000 0.01007 0.03255 = 0.03325 0.00633 -0.00228 0.00367 H6O 2 0.728017 1.226958 0.311948 11.00000 0.01804 O4B 4 0.942164 1.048291 0.313511 11.00000 0.01343 0.02399 = 0.02737 0.00315 0.00410 -0.00117 H7O 2 0.892521 1.009107 0.325664 11.00000 0.01494 O5B 4 1.095940 1.201789 0.307376 11.00000 0.01130 0.03546 = 0.03257 -0.00031 0.00084 -0.00321 H8O 2 1.085759 1.111156 0.303934 11.00000 0.06941 MOLE 5 C8C 1 0.299507 1.272797 0.694609 11.00000 0.02036 0.02685 = 0.01567 -0.00403 0.00110 0.00238 C9C 1 0.380891 1.197856 0.692039 11.00000 0.02919 0.02620 = 0.01298 -0.00372 0.00186 -0.00020 C10C 1 0.464891 1.271819 0.692144 11.00000 0.01868 0.03222 = 0.01818 -0.00240 0.00149 -0.00265 C11C 1 0.464879 1.421477 0.696104 11.00000 0.04334 0.02965 = 0.01653 -0.00358 0.00396 -0.01281 AFIX 43 H11C 2 0.520792 1.473729 0.696490 11.00000 -1.20000 AFIX 0 C12C 1 0.380952 1.492312 0.699474 11.00000 0.05018 0.02315 = 0.01933 0.00205 0.00216 0.00381 AFIX 43 H12C 2 0.380472 1.593854 0.702884 11.00000 -1.20000 AFIX 0 C13C 1 0.299017 1.420160 0.698026 11.00000 0.02871 0.04353 = 0.01807 -0.00308 0.00471 0.01043 AFIX 43 H13C 2 0.242728 1.471279 0.699365 11.00000 -1.20000 AFIX 0 O3C 4 0.218939 1.195794 0.693584 11.00000 0.01828 0.03951 = 0.03209 -0.00466 0.00134 0.00976 H9O 2 0.226675 1.108158 0.689429 11.00000 0.02973 O4C 4 0.375855 1.051517 0.689979 11.00000 0.01474 0.02852 = 0.02633 -0.00846 -0.00212 -0.00229 H10O 2 0.418996 0.995531 0.686687 11.00000 0.20638 O5C 4 0.540935 1.186994 0.688224 11.00000 0.01033 0.04185 = 0.03935 0.00166 -0.00019 -0.00149 H11O 2 0.591479 1.226330 0.693585 11.00000 0.10420 MOLE 6 C8D 1 0.565208 0.800725 0.634695 11.00000 0.01166 0.01659 = 0.01549 -0.00047 0.00357 -0.00136 C9D 1 0.609999 0.769916 0.589708 11.00000 0.01273 0.01549 = 0.01655 0.00156 -0.00237 -0.00310 C10D 1 0.694963 0.702962 0.590733 11.00000 0.01239 0.01899 = 0.01351 -0.00181 0.00346 -0.00555 C11D 1 0.735640 0.667613 0.636272 11.00000 0.01053 0.02734 = 0.01763 0.00220 0.00358 0.00083 AFIX 43 H11D 2 0.793727 0.621581 0.636940 11.00000 -1.20000 AFIX 0 C12D 1 0.690921 0.699960 0.680493 11.00000 0.01813 0.03630 = 0.01257 0.00115 -0.00129 0.00395 AFIX 43 H12D 2 0.718888 0.676015 0.711409 11.00000 -1.20000 AFIX 0 C13D 1 0.606119 0.766635 0.680309 11.00000 0.02139 0.02999 = 0.01097 -0.00078 0.00414 -0.00207 AFIX 43 H13D 2 0.576139 0.788913 0.710814 11.00000 -1.20000 AFIX 0 O3D 4 0.480389 0.863452 0.634889 11.00000 0.00937 0.03515 = 0.01624 -0.00067 -0.00053 0.00582 H12O 2 0.460158 0.874478 0.606605 11.00000 0.03543 O4D 4 0.566695 0.810667 0.546491 11.00000 0.01176 0.02431 = 0.01367 -0.00182 -0.00235 0.00725 H13O 2 0.577914 0.772963 0.515858 11.00000 0.07978 O5D 4 0.734180 0.673753 0.545910 11.00000 0.00955 0.02367 = 0.01443 0.00155 0.00274 0.00497 H14O 2 0.777420 0.618265 0.551613 11.00000 0.02149 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KA1032_0m_a.res in Pna2(1) REM wR2 = 0.1557, GooF = S = 1.046, Restrained GooF = 1.045 for all data REM R1 = 0.0730 for 3817 Fo > 4sig(Fo) and 0.1648 for all 6362 data REM 565 parameters refined using 6 restraints END WGHT 0.0647 0.0000 REM Instructions for potential hydrogen bonds EQIV $6 x-1/2, -y+1/2, z HTAB C6A O2B_$6 HTAB O1A O2A HTAB O1A O4A_$1 HTAB C6B O2A_$5 HTAB O1B O2B HTAB O1B O4D_$2 HTAB C13A O4B_$1 HTAB O3A O2A HTAB O4A O3A HTAB O4A O5D HTAB O5A O2A_$2 HTAB O5A O4A HTAB O3B O5B_$3 HTAB O4B O5A HTAB O5B O4B HTAB O3C O4C HTAB O4C O3D HTAB O5C O3C_$4 HTAB C11D O4C_$2 HTAB O3D O2B_$1 HTAB O3D O4D HTAB O4D O3A HTAB O5D O2B REM Highest difference peak 0.447, deepest hole -0.401, 1-sigma level 0.090 Q1 1 0.8857 0.4744 0.5668 11.00000 0.05 0.45 Q2 1 0.9213 0.3658 0.5671 11.00000 0.05 0.39 Q3 1 0.3659 0.2451 0.4471 11.00000 0.05 0.38 Q4 1 0.4419 0.4768 0.4351 11.00000 0.05 0.37 Q5 1 0.3982 0.3646 0.4327 11.00000 0.05 0.36 ; _shelx_res_checksum 28182 _shelx_hkl_file ; 0 -1 0 0.10 0.48 0 2 0 6384.91 375.50 0 2 0 4839.73 376.21 0 3 0 -0.75 1.92 0 3 0 7.21 3.72 0 4 0 172.65 13.44 0 4 0 160.41 12.54 0 5 0 1.58 4.53 0 5 0 2.50 3.19 0 6 0 177.11 14.56 0 6 0 179.14 15.54 0 7 0 21.18 4.26 0 7 0 12.42 13.82 0 8 0 1057.45 66.99 0 8 0 874.26 73.66 0 9 0 5.35 4.65 0 9 0 -3.27 26.41 0 11 0 -71.73 54.77 0 11 0 -5.94 10.87 0 12 0 143.32 76.43 0 13 0 -53.70 73.35 1 -1 0 12.14 1.67 1 -1 0 14.87 1.67 1 1 0 14.58 1.59 -1 -1 0 13.64 1.40 -1 1 0 15.12 1.98 1 1 0 12.89 1.98 -1 2 0 75.24 7.11 1 2 0 71.87 5.90 -1 3 0 7.53 2.31 1 3 0 7.76 2.35 -1 3 0 5.55 3.01 1 3 0 14.37 3.80 -1 4 0 45.77 5.66 -1 4 0 46.63 6.93 1 4 0 47.92 5.76 1 4 0 52.72 6.75 1 5 0 25.63 4.05 1 5 0 17.16 6.99 1 6 0 58.65 8.77 1 6 0 74.59 9.89 -1 6 0 64.11 9.77 -1 6 0 52.90 7.84 1 7 0 5.75 12.09 -1 7 0 2.33 3.33 1 7 0 3.78 3.16 -1 7 0 -1.22 13.36 -1 8 0 63.90 7.90 1 8 0 41.00 19.58 1 8 0 70.46 7.80 1 9 0 14.28 29.19 -1 9 0 45.57 6.61 -1 9 0 27.83 24.13 1 9 0 42.03 6.49 1 10 0 13.99 40.66 -1 10 0 -20.92 35.69 1 10 0 17.14 6.79 1 11 0 -8.04 57.62 1 11 0 7.47 8.55 -1 11 0 21.30 57.34 -1 12 0 -22.20 70.68 1 12 0 -18.35 70.51 -1 13 0 107.30 76.28 1 13 0 255.01 82.01 2 0 0 763.85 48.88 2 0 0 686.12 48.52 -2 1 0 8316.22 555.98 2 2 0 1358.25 93.50 -2 2 0 1415.83 93.66 -2 -2 0 1312.19 93.12 -2 2 0 1519.38 94.58 2 2 0 1359.40 93.90 2 3 0 864.14 59.93 -2 3 0 929.90 60.23 2 3 0 867.31 60.41 2 4 0 16.81 3.60 2 4 0 27.69 5.13 -2 4 0 21.31 4.51 -2 4 0 26.73 4.39 -2 5 0 7.86 4.28 2 5 0 -2.45 2.95 2 5 0 -4.16 4.55 -2 5 0 -2.62 4.40 -2 5 0 -0.38 3.36 -2 6 0 23.20 6.37 2 6 0 34.60 6.87 2 7 0 20.86 3.98 2 7 0 -7.96 16.37 -2 7 0 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-34 39.48 11.32 -4 2 -34 35.11 9.62 4 2 -34 43.78 9.84 -4 -2 -34 21.46 10.58 -4 -2 -34 59.46 12.07 4 -3 -34 -2.01 11.08 -4 3 -34 -2.63 9.08 -4 -3 -34 6.87 10.72 -4 -3 -34 3.62 11.12 4 3 -34 6.73 8.53 -4 4 -34 -1.13 9.58 4 4 -34 -2.15 8.74 -4 -4 -34 -2.86 9.92 -4 -4 -34 10.71 9.74 -4 5 -34 6.52 8.92 4 -5 -34 13.47 13.76 -4 -5 -34 16.28 7.83 4 5 -34 -7.17 8.17 -4 -5 -34 -3.91 10.63 -5 0 -34 10.75 10.55 -5 0 -34 3.36 9.49 -5 1 -34 26.53 10.02 -5 1 -34 6.08 9.39 5 -1 -34 1.15 9.65 -5 -1 -34 32.49 11.98 -5 -1 -34 5.32 9.78 -5 2 -34 47.31 10.25 5 -2 -34 56.78 12.25 -5 2 -34 29.51 10.39 -5 -2 -34 25.62 10.67 -5 -2 -34 61.03 12.87 5 2 -34 46.59 10.23 -5 3 -34 3.66 9.90 -5 -3 -34 -5.59 10.83 5 3 -34 6.80 9.02 -5 -3 -34 2.59 11.74 -5 4 -34 0.85 9.30 5 -4 -34 18.08 12.46 -5 -4 -34 -5.02 9.92 -5 -4 -34 6.10 10.41 5 4 -34 -11.89 8.84 -5 5 -34 -2.34 9.34 -5 -5 -34 7.92 8.96 -5 -5 -34 10.71 11.18 5 5 -34 -7.73 8.28 -6 0 -34 56.41 12.62 -6 0 -34 48.94 10.79 -6 1 -34 -4.07 9.47 -6 1 -34 1.94 12.05 -6 -1 -34 -6.75 12.53 -6 -1 -34 5.12 10.16 -6 2 -34 31.99 11.61 -6 2 -34 16.46 10.26 -6 -2 -34 18.59 12.57 6 2 -34 14.07 9.73 -6 -2 -34 9.84 10.45 -6 3 -34 -16.92 11.44 -6 3 -34 -10.66 10.25 -6 -3 -34 13.14 11.59 6 3 -34 16.42 9.71 -6 -3 -34 15.00 11.29 -6 4 -34 1.22 9.82 6 4 -34 -10.05 8.94 -6 -4 -34 13.50 11.26 -6 -4 -34 9.07 10.54 -7 0 -34 8.97 10.21 -7 0 -34 -7.64 12.91 -7 1 -34 11.11 13.87 -7 1 -34 2.36 10.69 -7 -1 -34 8.26 13.00 -7 -1 -34 8.08 10.97 -7 2 -34 -5.69 10.69 -7 2 -34 15.46 13.59 -7 -2 -34 -12.06 10.19 -7 -2 -34 -7.91 12.48 -7 3 -34 25.37 13.10 -7 3 -34 3.83 10.57 -7 -3 -34 18.41 11.73 -7 -3 -34 20.25 10.65 -7 4 -34 3.03 9.88 -7 4 -34 45.53 14.27 -7 -4 -34 0.76 11.35 -7 -4 -34 27.26 10.41 -8 0 -34 9.79 11.20 -8 0 -34 32.24 13.45 -8 1 -34 38.11 13.82 -8 1 -34 20.46 10.62 -8 -1 -34 -14.49 11.01 -8 -1 -34 8.10 12.92 -8 2 -34 -9.18 10.50 -8 2 -34 0.32 14.36 -8 -2 -34 -6.34 9.82 -8 -2 -34 -16.77 12.26 -8 3 -34 16.22 10.62 -8 3 -34 41.61 13.99 -8 -3 -34 5.48 9.84 -8 -3 -34 -6.62 11.65 -9 0 -34 4.95 13.06 -9 1 -34 31.91 11.39 -9 1 -34 1.85 14.28 -9 -1 -34 38.03 13.18 -9 -1 -34 10.92 10.46 -9 2 -34 0.24 10.75 -9 -2 -34 -1.50 10.49 0 0 -35 -1.59 8.97 0 -1 -35 13.30 9.44 0 1 -35 20.21 8.44 0 2 -35 0.83 8.46 0 -2 -35 11.32 10.07 0 3 -35 30.42 9.17 0 -3 -35 20.18 10.73 0 4 -35 6.33 8.20 0 -4 -35 -10.22 10.69 0 -5 -35 36.75 5.99 0 5 -35 25.66 8.78 -1 0 -35 -3.09 9.21 1 0 -35 0.98 8.94 -1 1 -35 11.22 8.37 1 -1 -35 0.10 9.07 -1 -1 -35 9.49 9.07 1 1 -35 8.55 8.03 -1 2 -35 -13.17 8.65 1 -2 -35 18.02 10.17 -1 -2 -35 -20.78 9.70 1 2 -35 -2.80 8.49 -1 3 -35 4.75 8.97 1 -3 -35 13.30 10.50 -1 -3 -35 35.25 11.19 1 3 -35 9.08 9.03 -1 4 -35 3.33 8.10 1 -4 -35 7.64 10.95 1 4 -35 -3.64 8.14 -1 -4 -35 7.51 10.55 -1 -4 -35 -9.57 6.51 1 -5 -35 9.21 11.50 -1 5 -35 -18.17 8.44 -1 -5 -35 25.35 11.47 -1 -5 -35 -7.28 5.63 1 5 -35 -17.17 8.26 -2 0 -35 -19.70 8.79 2 0 -35 -11.25 8.95 -2 1 -35 -11.48 8.39 2 -1 -35 5.72 9.13 2 1 -35 -4.87 8.11 -2 -1 -35 6.40 9.00 -2 2 -35 6.40 9.03 2 -2 -35 25.30 10.60 -2 -2 -35 -2.10 9.95 2 2 -35 8.41 8.47 2 -3 -35 -7.13 10.21 -2 3 -35 3.50 8.83 2 3 -35 -3.19 8.91 -2 -3 -35 15.85 10.27 -2 -3 -35 6.33 8.72 -2 4 -35 -6.24 8.24 2 -4 -35 6.71 11.19 -2 -4 -35 4.53 8.66 -2 -4 -35 28.62 9.85 2 4 -35 10.72 8.37 2 -5 -35 -21.74 11.62 -2 5 -35 12.93 8.67 -2 -5 -35 0.14 11.09 -2 -5 -35 9.14 6.74 2 5 -35 -8.00 8.57 3 0 -35 1.40 9.17 -3 0 -35 8.64 9.44 3 -1 -35 30.04 9.67 -3 1 -35 3.09 9.02 3 1 -35 -0.99 8.65 -3 -1 -35 10.73 8.53 -3 -1 -35 -9.84 9.13 3 -2 -35 -7.23 10.43 -3 2 -35 5.91 8.74 -3 -2 -35 -8.22 9.48 -3 -2 -35 -18.53 9.76 -3 3 -35 -8.09 8.88 3 -3 -35 12.44 10.71 -3 -3 -35 -18.85 9.88 -3 -3 -35 -4.05 10.02 3 3 -35 4.87 8.98 3 -4 -35 14.72 12.08 -3 4 -35 0.75 8.68 -3 -4 -35 -7.85 9.51 3 4 -35 -6.61 8.14 -3 -4 -35 -5.49 9.48 3 -5 -35 10.44 12.25 -3 5 -35 17.41 9.48 -3 -5 -35 4.91 11.65 3 5 -35 -10.67 8.55 -3 -5 -35 -10.66 7.43 4 0 -35 48.14 10.90 -4 0 -35 44.47 10.55 -4 0 -35 36.18 9.55 -4 1 -35 -10.38 9.51 4 -1 -35 0.91 9.74 4 1 -35 13.43 8.64 -4 -1 -35 9.28 10.13 -4 -1 -35 16.43 9.77 -4 2 -35 29.20 9.92 4 -2 -35 23.84 11.46 -4 -2 -35 21.82 11.39 4 2 -35 20.04 9.28 -4 -2 -35 25.89 9.95 4 -3 -35 7.79 10.91 -4 3 -35 -10.86 8.86 -4 -3 -35 -15.93 10.01 4 3 -35 -6.72 8.85 -4 -3 -35 -11.56 11.64 -4 4 -35 -8.90 9.06 4 4 -35 -16.53 8.32 -4 -4 -35 -12.74 9.79 -4 -4 -35 -13.44 10.64 -5 0 -35 -0.16 10.23 -5 0 -35 9.92 10.04 -5 1 -35 -1.37 9.64 -5 1 -35 9.33 10.17 -5 -1 -35 -9.52 10.14 5 1 -35 22.71 9.42 -5 -1 -35 0.38 11.82 -5 2 -35 16.23 9.91 5 2 -35 30.42 9.61 -5 -2 -35 19.18 9.86 -5 -2 -35 19.27 12.83 -5 3 -35 -11.37 9.58 -5 -3 -35 -1.87 11.80 5 3 -35 10.08 9.07 -5 -3 -35 2.49 10.13 -5 4 -35 33.52 9.69 5 4 -35 28.01 9.17 -5 -4 -35 7.63 11.64 -5 -4 -35 45.43 10.97 -6 0 -35 20.67 12.87 -6 0 -35 5.85 9.80 -6 1 -35 2.90 11.59 -6 1 -35 6.58 9.85 -6 -1 -35 10.37 10.37 6 1 -35 -1.82 9.51 -6 -1 -35 9.32 12.65 -6 2 -35 -0.73 11.70 -6 2 -35 -13.30 9.44 -6 -2 -35 -7.63 9.62 6 2 -35 -7.30 9.35 -6 -2 -35 -9.26 12.79 6 3 -35 18.12 9.46 -6 -3 -35 2.57 10.59 -6 -3 -35 25.60 12.12 -7 0 -35 -8.05 9.75 -7 0 -35 3.74 13.16 -7 1 -35 -1.75 10.19 -7 1 -35 9.40 13.17 -7 -1 -35 11.27 13.23 -7 -1 -35 8.11 10.22 -7 2 -35 18.26 12.77 -7 2 -35 -1.70 9.50 -7 -2 -35 21.89 13.37 -7 -2 -35 0.26 9.38 -7 3 -35 0.11 9.82 -7 -3 -35 -8.15 10.35 7 3 -35 24.35 9.63 -8 0 -35 5.68 13.35 -8 1 -35 -1.25 13.62 -8 1 -35 -13.06 9.77 -8 -1 -35 -15.53 10.25 -8 -1 -35 7.11 13.16 0 0 -36 22.85 9.61 0 -1 -36 8.56 9.55 0 1 -36 5.81 8.91 0 2 -36 -17.47 8.41 0 -2 -36 1.01 10.18 0 3 -36 -2.94 8.04 0 -3 -36 24.46 10.10 0 -4 -36 2.76 10.19 0 4 -36 3.70 8.45 -1 0 -36 -10.25 9.25 1 0 -36 -18.34 9.29 -1 1 -36 26.97 9.04 1 -1 -36 37.19 9.96 1 1 -36 34.96 9.15 -1 -1 -36 18.05 9.67 -1 2 -36 -6.89 8.54 1 -2 -36 -4.09 10.33 1 2 -36 -8.69 8.41 -1 -2 -36 -13.31 10.02 -1 3 -36 0.81 8.23 1 -3 -36 3.06 10.13 1 3 -36 2.49 8.36 -1 -3 -36 19.55 10.01 1 -4 -36 -8.60 10.29 -1 4 -36 3.07 8.60 1 4 -36 4.02 8.30 -1 -4 -36 0.49 10.00 -2 0 -36 14.05 9.87 2 0 -36 22.34 10.00 -2 1 -36 -13.91 8.46 2 -1 -36 6.46 9.43 -2 -1 -36 -10.84 8.97 2 1 -36 -5.53 8.45 -2 2 -36 -12.61 8.23 2 -2 -36 -20.32 10.54 -2 -2 -36 -15.07 9.41 2 2 -36 13.25 8.98 2 -3 -36 -20.01 10.30 -2 3 -36 4.69 8.35 -2 -3 -36 -3.93 11.77 -2 -3 -36 4.68 9.97 2 -4 -36 -9.99 10.35 -2 4 -36 -7.50 8.63 2 4 -36 11.59 8.51 -2 -4 -36 -13.33 8.99 -3 0 -36 -10.51 9.17 3 0 -36 -1.84 9.20 -3 1 -36 -8.29 8.58 3 -1 -36 20.91 9.73 3 1 -36 -2.38 8.77 -3 -1 -36 12.36 8.94 3 -2 -36 12.44 10.81 -3 2 -36 1.29 8.42 -3 -2 -36 -11.52 10.03 -3 -2 -36 7.37 9.06 3 2 -36 2.35 8.50 -3 3 -36 -5.18 8.49 3 -3 -36 4.67 10.58 -3 -3 -36 -10.26 9.75 -3 -3 -36 4.99 10.00 3 3 -36 -0.97 8.42 -3 4 -36 22.38 9.66 3 -4 -36 29.04 11.07 -3 -4 -36 20.90 10.96 -3 -4 -36 10.21 9.99 3 4 -36 9.83 8.88 -4 0 -36 -1.01 9.25 4 0 -36 1.93 9.84 4 -1 -36 -6.15 9.72 -4 -1 -36 9.25 9.08 4 1 -36 12.01 9.15 -4 -1 -36 12.79 9.81 -4 2 -36 12.51 9.08 4 -2 -36 -8.93 10.91 -4 -2 -36 5.71 10.78 -4 -2 -36 -5.86 9.02 -4 3 -36 -14.17 8.96 4 3 -36 -7.00 8.04 -4 -3 -36 9.07 11.02 -4 -3 -36 3.94 10.41 -5 0 -36 3.34 8.79 5 0 -36 8.97 10.23 -5 0 -36 20.36 10.56 -5 1 -36 -3.33 9.06 5 1 -36 1.03 9.46 -5 -1 -36 -4.81 11.48 -5 2 -36 -9.12 8.89 5 -2 -36 -8.95 11.09 -5 -2 -36 5.54 12.23 -5 -2 -36 -18.97 9.35 -5 3 -36 -2.29 9.67 -5 -3 -36 25.62 11.95 5 3 -36 5.93 8.78 -5 -3 -36 -6.89 10.91 -6 0 -36 17.39 11.60 -6 0 -36 -17.26 9.00 -6 1 -36 -4.96 9.31 -6 1 -36 -10.87 11.74 -6 -1 -36 -7.63 12.14 -6 -1 -36 -3.45 9.84 -6 2 -36 -13.13 9.34 -6 -2 -36 -6.00 12.94 -6 -2 -36 3.96 10.07 -7 0 -36 -5.95 9.72 -7 1 -36 20.43 9.81 -7 -1 -36 -7.81 10.39 0 0 -37 2.02 8.90 0 -1 -37 44.40 9.21 0 1 -37 24.81 8.78 0 2 -37 -13.19 7.94 0 -2 -37 -5.86 9.19 0 3 -37 46.29 9.23 0 -3 -37 10.63 10.64 -1 0 -37 -15.13 8.65 1 0 -37 -11.77 8.69 -1 1 -37 12.13 8.44 1 -1 -37 13.56 8.78 -1 -1 -37 -13.44 8.46 1 1 -37 6.99 8.31 1 -2 -37 -6.88 9.30 1 2 -37 2.36 8.16 -1 -2 -37 -3.11 9.24 -1 3 -37 8.03 8.69 1 -3 -37 5.28 10.10 1 3 -37 -9.06 8.49 -1 -3 -37 0.36 10.53 2 0 -37 49.64 9.96 -2 0 -37 44.92 9.72 -2 1 -37 -9.57 8.18 2 -1 -37 0.00 8.83 -2 -1 -37 -14.39 8.65 2 1 -37 -13.75 8.22 2 -2 -37 -16.67 9.62 -2 2 -37 12.19 8.46 2 2 -37 -3.39 8.10 -2 -2 -37 2.08 8.98 2 -3 -37 -0.45 10.15 -2 3 -37 -5.11 9.23 -2 -3 -37 17.32 10.90 -3 0 -37 -19.32 8.80 3 0 -37 4.54 9.07 3 -1 -37 17.44 9.11 -3 1 -37 21.65 8.62 3 1 -37 -1.39 8.31 -3 -1 -37 -4.18 8.90 3 -2 -37 -9.10 9.97 -3 2 -37 6.09 9.01 3 2 -37 -15.88 8.11 -3 -2 -37 -6.95 9.24 4 0 -37 9.05 9.24 -4 1 -37 8.11 9.20 4 -1 -37 11.63 9.26 4 1 -37 9.11 8.48 -4 -1 -37 5.86 9.58 -4 2 -37 7.30 9.71 4 -2 -37 -7.09 9.90 -4 -2 -37 20.93 11.41 5 0 -37 -8.03 8.99 -5 0 -37 -21.09 9.23 -5 1 -37 -2.83 9.79 -5 -1 -37 -20.80 10.31 -5 -1 -37 7.44 11.94 5 1 -37 13.60 8.50 0 0 -38 4.77 9.12 0 -1 -38 -20.14 8.88 0 1 -38 -13.43 8.85 1 0 -38 -1.54 8.84 -1 0 -38 -6.88 9.12 1 -1 -38 -5.32 8.84 -1 1 -38 16.23 9.05 1 1 -38 -0.85 8.69 -1 -1 -38 4.49 9.40 2 0 -38 11.44 9.05 -2 0 -38 6.67 9.40 2 -1 -38 2.20 8.79 -2 1 -38 -5.82 9.70 2 1 -38 15.34 8.52 -2 -1 -38 5.62 10.02 0 0 0 0.00 0.00 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5447 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71074 9.285 14.594 26.847 89.880 89.977 89.901 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 63829 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.3562(4) 0.1729(7) 0.4402(2) 0.0175(14) Uani 1 1 d . . . . . C2A C 0.3562(4) 0.3219(7) 0.4453(2) 0.0139(13) Uani 1 1 d . . . . . C3A C 0.4381(4) 0.4023(6) 0.44335(18) 0.0135(12) Uani 1 1 d . . . . . C4A C 0.5198(4) 0.3246(6) 0.43433(19) 0.0167(13) Uani 1 1 d . . . . . H4A H 0.576537 0.373994 0.431810 0.020 Uiso 1 1 calc R U . . . C5A C 0.5171(4) 0.1782(7) 0.4292(2) 0.0197(13) Uani 1 1 d . . . . . H5A H 0.572644 0.127773 0.423365 0.024 Uiso 1 1 calc R U . . . C6A C 0.4414(4) -0.0549(6) 0.4277(2) 0.0238(14) Uani 1 1 d . . . . . H6A H 0.394029 -0.087117 0.404292 0.036 Uiso 1 1 calc R U . . . H6B H 0.430649 -0.098587 0.460449 0.036 Uiso 1 1 calc R U . . . H6C H 0.501808 -0.083940 0.415288 0.036 Uiso 1 1 calc R U . . . C7A C 0.2707(4) 0.0865(7) 0.4426(2) 0.0238(16) Uani 1 1 d . . . . . H7A H 0.254302 0.053989 0.408928 0.036 Uiso 1 1 calc R U . . . H7B H 0.220969 0.145466 0.456118 0.036 Uiso 1 1 calc R U . . . H7C H 0.280410 0.002903 0.464153 0.036 Uiso 1 1 calc R U . . . O1A O 0.2748(3) 0.3879(5) 0.45389(15) 0.0175(9) Uani 1 1 d D . . . . H1O H 0.281(5) 0.477(3) 0.453(3) 0.06(3) Uiso 1 1 d D . . . . O2A O 0.4347(2) 0.5415(4) 0.44946(13) 0.0150(9) Uani 1 1 d . . . . . N1A N 0.4379(3) 0.1035(5) 0.43227(16) 0.0181(11) Uani 1 1 d . . . . . C1B C 0.9657(4) 0.1746(6) 0.5630(2) 0.0167(13) Uani 1 1 d . . . . . C2B C 0.9659(4) 0.3197(6) 0.55825(19) 0.0148(12) Uani 1 1 d . . . . . C3B C 0.8835(4) 0.4031(7) 0.55999(19) 0.0137(13) Uani 1 1 d . . . . . C4B C 0.8033(4) 0.3242(6) 0.5682(2) 0.0171(14) Uani 1 1 d . . . . . H4B H 0.746618 0.373940 0.570732 0.021 Uiso 1 1 calc R U . . . C5B C 0.8036(4) 0.1810(6) 0.5725(2) 0.0176(14) Uani 1 1 d . . . . . H5B H 0.747149 0.132030 0.577152 0.021 Uiso 1 1 calc R U . . . C6B C 0.8796(5) -0.0545(6) 0.5736(2) 0.0256(15) Uani 1 1 d . . . . . H6D H 0.816281 -0.086581 0.578407 0.038 Uiso 1 1 calc R U . . . H6E H 0.917147 -0.086234 0.601857 0.038 Uiso 1 1 calc R U . . . H6F H 0.903942 -0.095843 0.542660 0.038 Uiso 1 1 calc R U . . . C7B C 1.0513(4) 0.0890(6) 0.5606(2) 0.0220(14) Uani 1 1 d . . . . . H7D H 1.042701 0.008030 0.537725 0.033 Uiso 1 1 calc R U . . . H7E H 1.066167 0.052628 0.593971 0.033 Uiso 1 1 calc R U . . . H7F H 1.101460 0.149728 0.548595 0.033 Uiso 1 1 calc R U . . . O1B O 1.0472(3) 0.3880(4) 0.54975(14) 0.0189(9) Uani 1 1 d D . . . . H2O H 1.040(5) 0.475(3) 0.542(3) 0.05(2) Uiso 1 1 d D . . . . O2B O 0.8875(2) 0.5416(4) 0.55430(14) 0.0165(9) Uani 1 1 d . . . . . N1B N 0.8820(3) 0.1045(5) 0.57032(16) 0.0165(11) Uani 1 1 d . . . . . C8A C 0.6274(4) 0.7024(6) 0.41384(19) 0.0139(12) Uani 1 1 d . . . . . C9A C 0.7118(4) 0.7707(6) 0.41431(19) 0.0135(12) Uani 1 1 d . . . . . C10A C 0.7569(4) 0.7999(6) 0.3698(2) 0.0156(12) Uani 1 1 d . . . . . C11A C 0.7175(4) 0.7654(6) 0.3249(2) 0.0198(13) Uani 1 1 d . . . . . H11A H 0.748141 0.787077 0.294542 0.024 Uiso 1 1 calc R U . . . C12A C 0.6330(5) 0.6987(7) 0.3242(2) 0.0230(14) Uani 1 1 d . . . . . H12A H 0.605602 0.675173 0.293132 0.028 Uiso 1 1 calc R U . . . C13A C 0.5869(4) 0.6653(6) 0.3686(2) 0.0171(14) Uani 1 1 d . . . . . H13A H 0.529222 0.618127 0.367821 0.021 Uiso 1 1 calc R U . . . O3A O 0.5863(3) 0.6726(4) 0.45876(13) 0.0160(10) Uani 1 1 d . . . . . H3O H 0.528(5) 0.637(6) 0.453(2) 0.034(19) Uiso 1 1 d . . . . . O4A O 0.7547(3) 0.8129(4) 0.45811(14) 0.0192(9) Uani 1 1 d . . . . . H4O H 0.734(4) 0.757(6) 0.479(2) 0.008(14) Uiso 1 1 d . . . . . O5A O 0.8423(3) 0.8623(4) 0.36995(15) 0.0193(9) Uani 1 1 d D . . . . H5O H 0.862(8) 0.857(11) 0.3984(18) 0.12(4) Uiso 1 1 d D . . . . C8B C 0.8484(4) 1.2642(7) 0.3106(2) 0.0215(15) Uani 1 1 d . . . . . C9B C 0.9321(4) 1.1931(6) 0.3108(2) 0.0156(13) Uani 1 1 d . . . . . C10B C 1.0125(4) 1.2732(7) 0.30622(19) 0.0207(14) Uani 1 1 d . . . . . C11B C 1.0107(4) 1.4222(7) 0.3010(2) 0.0248(14) Uani 1 1 d . . . . . H11B H 1.065798 1.475824 0.297616 0.030 Uiso 1 1 calc R U . . . C12B C 0.9240(5) 1.4912(7) 0.3009(2) 0.0274(15) Uani 1 1 d . . . . . H12B H 0.920408 1.592532 0.297330 0.033 Uiso 1 1 calc R U . . . C13B C 0.8448(4) 1.4116(7) 0.3058(2) 0.0234(14) Uani 1 1 d . . . . . H13B H 0.787149 1.458846 0.305987 0.028 Uiso 1 1 calc R U . . . O3B O 0.7728(3) 1.1758(5) 0.31597(16) 0.0253(10) Uani 1 1 d . . . . . H6O H 0.728(5) 1.227(7) 0.312(2) 0.018(19) Uiso 1 1 d . . . . . O4B O 0.9422(3) 1.0483(5) 0.31351(15) 0.0216(9) Uani 1 1 d . . . . . H7O H 0.893(4) 1.009(6) 0.326(2) 0.015(15) Uiso 1 1 d . . . . . O5B O 1.0959(3) 1.2018(6) 0.30738(16) 0.0264(11) Uani 1 1 d . . . . . H8O H 1.086(6) 1.111(9) 0.304(3) 0.07(3) Uiso 1 1 d . . . . . C8C C 0.2995(4) 1.2728(7) 0.6946(2) 0.0210(14) Uani 1 1 d . . . . . C9C C 0.3809(5) 1.1979(7) 0.6920(2) 0.0228(14) Uani 1 1 d . . . . . C10C C 0.4649(4) 1.2718(7) 0.6921(2) 0.0230(15) Uani 1 1 d . . . . . C11C C 0.4649(5) 1.4215(7) 0.6961(2) 0.0298(16) Uani 1 1 d . . . . . H11C H 0.520792 1.473729 0.696490 0.036 Uiso 1 1 calc R U . . . C12C C 0.3810(5) 1.4923(7) 0.6995(2) 0.0309(17) Uani 1 1 d . . . . . H12C H 0.380472 1.593854 0.702884 0.037 Uiso 1 1 calc R U . . . C13C C 0.2990(5) 1.4202(7) 0.6980(2) 0.0301(16) Uani 1 1 d . . . . . H13C H 0.242728 1.471279 0.699365 0.036 Uiso 1 1 calc R U . . . O3C O 0.2189(3) 1.1958(6) 0.69358(16) 0.0300(11) Uani 1 1 d . . . . . H9O H 0.227(5) 1.108(7) 0.689(2) 0.03(2) Uiso 1 1 d . . . . . O4C O 0.3759(3) 1.0515(5) 0.68998(15) 0.0232(10) Uani 1 1 d D . . . . H10O H 0.419(7) 0.996(13) 0.687(6) 0.21(7) Uiso 1 1 d D . . . . O5C O 0.5409(3) 1.1870(6) 0.68822(18) 0.0305(11) Uani 1 1 d D . . . . H11O H 0.591(4) 1.226(10) 0.694(5) 0.10(5) Uiso 1 1 d D . . . . C8D C 0.5652(4) 0.8007(6) 0.6347(2) 0.0146(12) Uani 1 1 d . . . . . C9D C 0.6100(4) 0.7699(6) 0.58971(19) 0.0149(12) Uani 1 1 d . . . . . C10D C 0.6950(4) 0.7030(6) 0.59073(18) 0.0150(12) Uani 1 1 d . . . . . C11D C 0.7356(4) 0.6676(6) 0.6363(2) 0.0185(13) Uani 1 1 d . . . . . H11D H 0.793727 0.621581 0.636940 0.022 Uiso 1 1 calc R U . . . C12D C 0.6909(4) 0.7000(7) 0.6805(2) 0.0223(14) Uani 1 1 d . . . . . H12D H 0.718888 0.676015 0.711409 0.027 Uiso 1 1 calc R U . . . C13D C 0.6061(4) 0.7666(6) 0.6803(2) 0.0208(14) Uani 1 1 d . . . . . H13D H 0.576139 0.788913 0.710814 0.025 Uiso 1 1 calc R U . . . O3D O 0.4804(3) 0.8635(4) 0.63489(15) 0.0203(9) Uani 1 1 d . . . . . H12O H 0.460(5) 0.874(7) 0.607(3) 0.04(2) Uiso 1 1 d . . . . . O4D O 0.5667(3) 0.8107(4) 0.54649(14) 0.0166(10) Uani 1 1 d . . . . . H13O H 0.578(6) 0.773(9) 0.516(4) 0.08(3) Uiso 1 1 d . . . . . O5D O 0.7342(3) 0.6738(4) 0.54591(13) 0.0159(9) Uani 1 1 d . . . . . H14O H 0.777(4) 0.618(6) 0.552(2) 0.021(17) Uiso 1 1 d . . . . . 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 C1A 0.011(3) 0.029(4) 0.013(3) 0.002(2) -0.003(2) -0.002(3) C2A 0.008(3) 0.018(3) 0.016(3) -0.002(2) -0.003(2) 0.000(2) C3A 0.008(3) 0.021(4) 0.011(3) 0.003(2) -0.002(2) -0.003(2) C4A 0.004(3) 0.027(4) 0.019(3) 0.000(2) 0.000(2) 0.000(2) C5A 0.010(3) 0.027(4) 0.022(3) -0.001(2) 0.001(2) 0.007(3) C6A 0.018(3) 0.021(4) 0.032(3) 0.003(3) -0.001(3) 0.002(3) C7A 0.024(4) 0.020(4) 0.028(3) -0.001(2) -0.006(3) -0.003(3) O1A 0.005(2) 0.021(3) 0.026(2) 0.0012(18) 0.0013(17) 0.0038(17) O2A 0.007(2) 0.019(2) 0.0188(19) -0.0015(16) 0.0010(16) -0.0025(16) N1A 0.014(3) 0.022(3) 0.018(2) -0.001(2) -0.004(2) 0.003(2) C1B 0.017(3) 0.019(3) 0.014(2) 0.002(2) -0.001(2) -0.002(3) C2B 0.008(3) 0.021(3) 0.016(3) -0.002(2) 0.003(2) -0.004(2) C3B 0.011(3) 0.023(4) 0.006(2) -0.001(2) -0.001(2) 0.000(2) C4B 0.014(3) 0.020(3) 0.017(3) 0.001(2) 0.000(2) 0.000(3) C5B 0.005(3) 0.030(4) 0.018(3) -0.002(2) 0.000(2) -0.004(3) C6B 0.032(4) 0.023(4) 0.022(3) 0.006(2) 0.003(3) -0.004(3) C7B 0.018(3) 0.020(3) 0.028(3) -0.001(2) -0.004(3) 0.007(3) O1B 0.010(2) 0.019(3) 0.028(2) 0.0034(18) 0.0010(18) 0.0020(18) O2B 0.011(2) 0.020(2) 0.0190(19) 0.0024(16) 0.0005(16) 0.0001(16) N1B 0.019(3) 0.014(3) 0.016(2) -0.0003(19) 0.003(2) -0.003(2) C8A 0.014(3) 0.016(3) 0.012(2) -0.001(2) 0.001(2) 0.007(2) C9A 0.011(3) 0.016(3) 0.014(2) -0.001(2) -0.003(2) 0.005(2) C10A 0.013(3) 0.016(3) 0.018(2) 0.000(2) 0.001(2) 0.000(2) C11A 0.013(3) 0.030(4) 0.016(3) 0.000(2) 0.002(2) 0.004(3) C12A 0.024(4) 0.032(4) 0.013(2) -0.002(2) -0.003(3) -0.001(3) C13A 0.014(3) 0.021(4) 0.016(3) 0.003(2) -0.005(2) -0.005(2) O3A 0.008(2) 0.028(3) 0.0119(19) 0.0002(16) 0.0001(16) -0.0073(18) O4A 0.023(2) 0.022(2) 0.0135(18) 0.0030(16) -0.0016(17) -0.0093(19) O5A 0.011(2) 0.028(3) 0.0185(19) 0.0036(17) -0.0016(18) -0.0055(17) C8B 0.016(4) 0.035(4) 0.014(3) 0.002(3) 0.000(3) -0.003(3) C9B 0.009(3) 0.022(4) 0.016(3) 0.003(2) -0.002(2) -0.003(2) C10B 0.017(3) 0.033(4) 0.012(3) 0.002(2) 0.001(2) 0.003(3) C11B 0.021(4) 0.033(4) 0.021(3) 0.001(2) 0.003(3) -0.012(3) C12B 0.039(4) 0.025(4) 0.018(3) 0.002(2) 0.000(3) 0.004(3) C13B 0.016(4) 0.033(4) 0.021(3) 0.000(3) -0.001(3) 0.007(3) O3B 0.010(2) 0.033(3) 0.033(2) 0.0063(19) -0.002(2) 0.004(2) O4B 0.013(2) 0.024(3) 0.027(2) 0.0032(19) 0.0041(19) -0.0012(19) O5B 0.011(3) 0.035(3) 0.033(3) 0.000(2) 0.001(2) -0.003(2) C8C 0.020(4) 0.027(4) 0.016(3) -0.004(2) 0.001(3) 0.002(3) C9C 0.029(4) 0.026(4) 0.013(3) -0.004(2) 0.002(3) 0.000(3) C10C 0.019(4) 0.032(4) 0.018(3) -0.002(3) 0.001(3) -0.003(3) C11C 0.043(5) 0.030(4) 0.017(3) -0.004(3) 0.004(3) -0.013(3) C12C 0.050(5) 0.023(4) 0.019(3) 0.002(2) 0.002(3) 0.004(3) C13C 0.029(4) 0.044(5) 0.018(3) -0.003(3) 0.005(3) 0.010(3) O3C 0.018(3) 0.040(3) 0.032(2) -0.005(2) 0.001(2) 0.010(2) O4C 0.015(2) 0.029(3) 0.026(2) -0.0085(19) -0.0021(19) -0.002(2) O5C 0.010(3) 0.042(3) 0.039(3) 0.002(2) 0.000(2) -0.001(2) C8D 0.012(3) 0.017(3) 0.015(2) 0.000(2) 0.004(2) -0.001(3) C9D 0.013(3) 0.015(3) 0.017(3) 0.002(2) -0.002(2) -0.003(2) C10D 0.012(3) 0.019(3) 0.014(2) -0.002(2) 0.003(2) -0.006(2) C11D 0.011(3) 0.027(4) 0.018(3) 0.002(2) 0.004(2) 0.001(2) C12D 0.018(3) 0.036(4) 0.013(2) 0.001(2) -0.001(2) 0.004(3) C13D 0.021(4) 0.030(4) 0.011(2) -0.001(2) 0.004(2) -0.002(3) O3D 0.009(2) 0.035(3) 0.0162(18) -0.0007(17) -0.0005(18) 0.0058(18) O4D 0.012(2) 0.024(2) 0.0137(19) -0.0018(16) -0.0024(17) 0.0073(18) O5D 0.010(2) 0.024(3) 0.0144(18) 0.0015(16) 0.0027(17) 0.0050(18) 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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A C1A C2A 118.9(6) . . ? N1A C1A C7A 118.7(6) . . ? C2A C1A C7A 122.4(6) . . ? O1A C2A C1A 117.8(5) . . ? O1A C2A C3A 120.5(5) . . ? C1A C2A C3A 121.6(6) . . ? O2A C3A C2A 119.2(5) . . ? O2A C3A C4A 124.1(5) . . ? C2A C3A C4A 116.7(6) . . ? C5A C4A C3A 120.1(5) . . ? C5A C4A H4A 119.9 . . ? C3A C4A H4A 119.9 . . ? N1A C5A C4A 122.1(6) . . ? N1A C5A H5A 119.0 . . ? C4A C5A H5A 119.0 . . ? N1A C6A H6A 109.5 . . ? N1A C6A H6B 109.5 . . ? H6A C6A H6B 109.5 . . ? N1A C6A H6C 109.5 . . ? H6A C6A H6C 109.5 . . ? H6B C6A H6C 109.5 . . ? C1A C7A H7A 109.5 . . ? C1A C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? C1A C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C2A O1A H1O 111(6) . . ? C5A N1A C1A 120.6(5) . . ? C5A N1A C6A 118.6(5) . . ? C1A N1A C6A 120.8(5) . . ? C2B C1B N1B 118.7(5) . . ? C2B C1B C7B 121.9(6) . . ? N1B C1B C7B 119.3(5) . . ? C1B C2B O1B 118.8(5) . . ? C1B C2B C3B 122.3(6) . . ? O1B C2B C3B 118.8(5) . . ? O2B C3B C4B 125.2(6) . . ? O2B C3B C2B 119.8(5) . . ? C4B C3B C2B 115.0(6) . . ? C5B C4B C3B 122.2(6) . . ? C5B C4B H4B 118.9 . . ? C3B C4B H4B 118.9 . . ? C4B C5B N1B 121.7(6) . . ? C4B C5B H5B 119.1 . . ? N1B C5B H5B 119.1 . . ? N1B C6B H6D 109.5 . . ? N1B C6B H6E 109.5 . . ? H6D C6B H6E 109.5 . . ? N1B C6B H6F 109.5 . . ? H6D C6B H6F 109.5 . . ? H6E C6B H6F 109.5 . . ? C1B C7B H7D 109.5 . . ? C1B C7B H7E 109.5 . . ? H7D C7B H7E 109.5 . . ? C1B C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? H7E C7B H7F 109.5 . . ? C2B O1B H2O 112(5) . . ? C5B N1B C1B 120.0(5) . . ? C5B N1B C6B 120.4(5) . . ? C1B N1B C6B 119.6(5) . . ? O3A C8A C9A 118.2(5) . . ? O3A C8A C13A 121.9(5) . . ? C9A C8A C13A 119.9(5) . . ? C8A C9A O4A 122.6(5) . . ? C8A C9A C10A 120.2(5) . . ? O4A C9A C10A 117.3(5) . . ? C11A C10A O5A 118.8(5) . . ? C11A C10A C9A 120.6(5) . . ? O5A C10A C9A 120.6(5) . . ? C10A C11A C12A 119.4(5) . . ? C10A C11A H11A 120.3 . . ? C12A C11A H11A 120.3 . . ? C11A C12A C13A 121.2(5) . . ? C11A C12A H12A 119.4 . . ? C13A C12A H12A 119.4 . . ? C8A C13A C12A 118.7(5) . . ? C8A C13A H13A 120.7 . . ? C12A C13A H13A 120.7 . . ? C8A O3A H3O 110(4) . . ? C9A O4A H4O 103(4) . . ? C10A O5A H5O 107(8) . . ? C13B C8B O3B 124.9(6) . . ? C13B C8B C9B 120.5(6) . . ? O3B C8B C9B 114.6(6) . . ? O4B C9B C8B 124.7(6) . . ? O4B C9B C10B 116.4(5) . . ? C8B C9B C10B 118.9(6) . . ? O5B C10B C9B 118.7(6) . . ? O5B C10B C11B 119.6(6) . . ? C9B C10B C11B 121.7(6) . . ? C10B C11B C12B 117.8(6) . . ? C10B C11B H11B 121.1 . . ? C12B C11B H11B 121.1 . . ? C13B C12B C11B 120.2(6) . . ? C13B C12B H12B 119.9 . . ? C11B C12B H12B 119.9 . . ? C12B C13B C8B 120.9(6) . . ? C12B C13B H13B 119.6 . . ? C8B C13B H13B 119.6 . . ? C8B O3B H6O 106(5) . . ? C9B O4B H7O 110(4) . . ? C10B O5B H8O 108(6) . . ? C13C C8C O3C 121.1(6) . . ? C13C C8C C9C 120.8(6) . . ? O3C C8C C9C 118.1(6) . . ? O4C C9C C8C 117.4(6) . . ? O4C C9C C10C 122.4(6) . . ? C8C C9C C10C 120.2(6) . . ? O5C C10C C11C 125.6(6) . . ? O5C C10C C9C 115.1(6) . . ? C11C C10C C9C 119.2(6) . . ? C12C C11C C10C 118.5(6) . . ? C12C C11C H11C 120.8 . . ? C10C C11C H11C 120.8 . . ? C13C C12C C11C 122.1(6) . . ? C13C C12C H12C 118.9 . . ? C11C C12C H12C 118.9 . . ? C12C C13C C8C 119.1(6) . . ? C12C C13C H13C 120.5 . . ? C8C C13C H13C 120.5 . . ? C8C O3C H9O 113(5) . . ? C9C O4C H10O 127(10) . . ? C10C O5C H11O 117(7) . . ? O3D C8D C13D 118.7(5) . . ? O3D C8D C9D 120.8(5) . . ? C13D C8D C9D 120.5(5) . . ? O4D C9D C10D 123.5(5) . . ? O4D C9D C8D 117.0(5) . . ? C10D C9D C8D 119.5(5) . . ? O5D C10D C9D 116.7(5) . . ? O5D C10D C11D 123.1(5) . . ? C9D C10D C11D 120.2(5) . . ? C12D C11D C10D 119.7(5) . . ? C12D C11D H11D 120.1 . . ? C10D C11D H11D 120.1 . . ? C13D C12D C11D 121.0(5) . . ? C13D C12D H12D 119.5 . . ? C11D C12D H12D 119.5 . . ? C12D C13D C8D 119.1(5) . . ? C12D C13D H13D 120.4 . . ? C8D C13D H13D 120.4 . . ? C8D O3D H12O 112(5) . . ? C9D O4D H13O 125(6) . . ? C10D O5D H14O 106(4) . . ? 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 C1A N1A 1.373(8) . ? C1A C2A 1.395(9) . ? C1A C7A 1.486(8) . ? C2A O1A 1.357(7) . ? C2A C3A 1.411(8) . ? C3A O2A 1.308(7) . ? C3A C4A 1.414(8) . ? C4A C5A 1.370(9) . ? C4A H4A 0.9500 . ? C5A N1A 1.352(8) . ? C5A H5A 0.9500 . ? C6A N1A 1.481(8) . ? C6A H6A 0.9800 . ? C6A H6B 0.9800 . ? C6A H6C 0.9800 . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 0.9800 . ? O1A H1O 0.84(3) . ? C1B C2B 1.357(8) . ? C1B N1B 1.399(8) . ? C1B C7B 1.483(8) . ? C2B O1B 1.365(7) . ? C2B C3B 1.432(8) . ? C3B O2B 1.300(7) . ? C3B C4B 1.400(9) . ? C4B C5B 1.338(8) . ? C4B H4B 0.9500 . ? C5B N1B 1.349(8) . ? C5B H5B 0.9500 . ? C6B N1B 1.484(8) . ? C6B H6D 0.9800 . ? C6B H6E 0.9800 . ? C6B H6F 0.9800 . ? C7B H7D 0.9800 . ? C7B H7E 0.9800 . ? C7B H7F 0.9800 . ? O1B H2O 0.84(3) . ? C8A O3A 1.373(6) . ? C8A C9A 1.386(8) . ? C8A C13A 1.392(8) . ? C9A O4A 1.387(6) . ? C9A C10A 1.390(8) . ? C10A C11A 1.371(8) . ? C10A O5A 1.375(7) . ? C11A C12A 1.381(9) . ? C11A H11A 0.9500 . ? C12A C13A 1.400(8) . ? C12A H12A 0.9500 . ? C13A H13A 0.9500 . ? O3A H3O 0.93(7) . ? O4A H4O 0.82(5) . ? O5A H5O 0.82(3) . ? C8B C13B 1.379(9) . ? C8B O3B 1.383(7) . ? C8B C9B 1.389(9) . ? C9B O4B 1.358(7) . ? C9B C10B 1.396(9) . ? C10B O5B 1.388(8) . ? C10B C11B 1.395(8) . ? C11B C12B 1.420(9) . ? C11B H11B 0.9500 . ? C12B C13B 1.378(9) . ? C12B H12B 0.9500 . ? C13B H13B 0.9500 . ? O3B H6O 0.82(7) . ? O4B H7O 0.87(6) . ? O5B H8O 0.86(9) . ? C8C C13C 1.375(9) . ? C8C O3C 1.377(8) . ? C8C C9C 1.379(10) . ? C9C O4C 1.366(8) . ? C9C C10C 1.406(9) . ? C10C O5C 1.366(8) . ? C10C C11C 1.398(9) . ? C11C C12C 1.394(10) . ? C11C H11C 0.9500 . ? C12C C13C 1.372(10) . ? C12C H12C 0.9500 . ? C13C H13C 0.9500 . ? O3C H9O 0.83(7) . ? O4C H10O 0.82(3) . ? O5C H11O 0.84(3) . ? C8D O3D 1.369(7) . ? C8D C13D 1.397(8) . ? C8D C9D 1.401(8) . ? C9D O4D 1.373(6) . ? C9D C10D 1.388(8) . ? C10D O5D 1.358(6) . ? C10D C11D 1.396(8) . ? C11D C12D 1.386(8) . ? C11D H11D 0.9500 . ? C12D C13D 1.384(9) . ? C12D H12D 0.9500 . ? C13D H13D 0.9500 . ? O3D H12O 0.82(7) . ? O4D H13O 0.91(9) . ? O5D H14O 0.83(6) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1A H1O O4A 0.84(3) 2.00(4) 2.804(6) 162(8) 4_465 yes O1B H2O O4D 0.84(3) 2.04(4) 2.821(6) 155(7) 4_565 yes O3A H3O O2A 0.93(7) 1.63(7) 2.539(5) 167(6) . yes O4A H4O O3A 0.82(5) 2.35(6) 2.782(6) 114(4) . yes O4A H4O O5D 0.82(5) 1.96(5) 2.702(5) 151(5) . yes O5A H5O O2A 0.82(3) 1.97(7) 2.676(5) 144(10) 4_565 yes O5A H5O O4A 0.82(3) 2.28(11) 2.726(6) 115(10) . yes O3B H6O O5B 0.82(7) 2.04(7) 2.831(7) 163(6) 4_475 yes O4B H7O O5A 0.87(6) 1.95(6) 2.722(6) 146(5) . yes O5B H8O O4B 0.86(9) 2.19(9) 2.666(6) 114(7) . yes O3C H9O O4C 0.83(7) 2.24(7) 2.657(7) 111(6) . yes O4C H10O O3D 0.82(3) 2.06(11) 2.752(6) 142(15) . yes O5C H11O O3C 0.84(3) 2.00(4) 2.821(7) 169(12) 4_575 yes O3D H12O O2B 0.82(7) 1.92(7) 2.698(6) 157(7) 4_465 yes O3D H12O O4D 0.82(7) 2.32(7) 2.727(6) 112(6) . yes O4D H13O O3A 0.91(9) 1.80(9) 2.695(5) 170(9) . yes O5D H14O O2B 0.83(6) 1.76(6) 2.564(5) 163(6) . yes C13A H13A O4B 0.95 2.48 3.255(7) 139 4_465 yes C6B H6F O2A 0.98 2.59 3.424(7) 143 4 yes C11D H11D O4C 0.95 2.46 3.228(7) 138 4_565 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A C1A C2A O1A -179.1(5) . . . . ? C7A C1A C2A O1A 1.6(8) . . . . ? N1A C1A C2A C3A -1.0(8) . . . . ? C7A C1A C2A C3A 179.6(5) . . . . ? O1A C2A C3A O2A -0.5(8) . . . . ? C1A C2A C3A O2A -178.5(5) . . . . ? O1A C2A C3A C4A 179.9(5) . . . . ? C1A C2A C3A C4A 1.9(7) . . . . ? O2A C3A C4A C5A 178.9(5) . . . . ? C2A C3A C4A C5A -1.6(7) . . . . ? C3A C4A C5A N1A 0.3(8) . . . . ? C4A C5A N1A C1A 0.6(8) . . . . ? C4A C5A N1A C6A -178.4(5) . . . . ? C2A C1A N1A C5A -0.3(8) . . . . ? C7A C1A N1A C5A 179.1(5) . . . . ? C2A C1A N1A C6A 178.7(5) . . . . ? C7A C1A N1A C6A -1.9(7) . . . . ? N1B C1B C2B O1B -178.2(4) . . . . ? C7B C1B C2B O1B 1.7(8) . . . . ? N1B C1B C2B C3B -0.6(8) . . . . ? C7B C1B C2B C3B 179.3(5) . . . . ? C1B C2B C3B O2B -178.7(5) . . . . ? O1B C2B C3B O2B -1.1(7) . . . . ? C1B C2B C3B C4B 1.5(8) . . . . ? O1B C2B C3B C4B 179.1(4) . . . . ? O2B C3B C4B C5B 178.3(5) . . . . ? C2B C3B C4B C5B -2.0(8) . . . . ? C3B C4B C5B N1B 1.6(9) . . . . ? C4B C5B N1B C1B -0.5(8) . . . . ? C4B C5B N1B C6B -178.0(5) . . . . ? C2B C1B N1B C5B 0.1(8) . . . . ? C7B C1B N1B C5B -179.9(5) . . . . ? C2B C1B N1B C6B 177.6(5) . . . . ? C7B C1B N1B C6B -2.4(7) . . . . ? O3A C8A C9A O4A -1.7(8) . . . . ? C13A C8A C9A O4A 178.7(5) . . . . ? O3A C8A C9A C10A 178.5(5) . . . . ? C13A C8A C9A C10A -1.1(9) . . . . ? C8A C9A C10A C11A 1.8(8) . . . . ? O4A C9A C10A C11A -178.0(5) . . . . ? C8A C9A C10A O5A -177.3(5) . . . . ? O4A C9A C10A O5A 2.9(8) . . . . ? O5A C10A C11A C12A 178.0(5) . . . . ? C9A C10A C11A C12A -1.1(9) . . . . ? C10A C11A C12A C13A -0.3(9) . . . . ? O3A C8A C13A C12A -179.8(5) . . . . ? C9A C8A C13A C12A -0.2(8) . . . . ? C11A C12A C13A C8A 0.9(9) . . . . ? C13B C8B C9B O4B -177.5(5) . . . . ? O3B C8B C9B O4B 3.2(8) . . . . ? C13B C8B C9B C10B 0.1(9) . . . . ? O3B C8B C9B C10B -179.2(5) . . . . ? O4B C9B C10B O5B -3.4(7) . . . . ? C8B C9B C10B O5B 178.9(5) . . . . ? O4B C9B C10B C11B 177.2(5) . . . . ? C8B C9B C10B C11B -0.6(9) . . . . ? O5B C10B C11B C12B -178.9(5) . . . . ? C9B C10B C11B C12B 0.5(8) . . . . ? C10B C11B C12B C13B 0.1(9) . . . . ? C11B C12B C13B C8B -0.5(9) . . . . ? O3B C8B C13B C12B 179.7(5) . . . . ? C9B C8B C13B C12B 0.5(9) . . . . ? C13C C8C C9C O4C 178.4(5) . . . . ? O3C C8C C9C O4C -1.7(8) . . . . ? C13C C8C C9C C10C -0.9(9) . . . . ? O3C C8C C9C C10C 179.0(5) . . . . ? O4C C9C C10C O5C 2.3(9) . . . . ? C8C C9C C10C O5C -178.5(5) . . . . ? O4C C9C C10C C11C -177.7(5) . . . . ? C8C C9C C10C C11C 1.5(9) . . . . ? O5C C10C C11C C12C 179.6(6) . . . . ? C9C C10C C11C C12C -0.4(9) . . . . ? C10C C11C C12C C13C -1.3(9) . . . . ? C11C C12C C13C C8C 1.9(9) . . . . ? O3C C8C C13C C12C 179.3(5) . . . . ? C9C C8C C13C C12C -0.8(9) . . . . ? O3D C8D C9D O4D 2.6(8) . . . . ? C13D C8D C9D O4D -178.0(5) . . . . ? O3D C8D C9D C10D -178.4(5) . . . . ? C13D C8D C9D C10D 1.0(8) . . . . ? O4D C9D C10D O5D -2.1(8) . . . . ? C8D C9D C10D O5D 178.9(5) . . . . ? O4D C9D C10D C11D 178.5(5) . . . . ? C8D C9D C10D C11D -0.5(8) . . . . ? O5D C10D C11D C12D -179.5(6) . . . . ? C9D C10D C11D C12D -0.2(8) . . . . ? C10D C11D C12D C13D 0.2(9) . . . . ? C11D C12D C13D C8D 0.4(10) . . . . ? O3D C8D C13D C12D 178.4(6) . . . . ? C9D C8D C13D C12D -1.0(9) . . . . ? _cod_database_fobs_code 2022899