#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022896.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_2022896 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 '2(C7 H9 N O2), C6 H6 O3' _chemical_formula_sum 'C20 H24 N2 O7' _chemical_formula_weight 404.41 _chemical_name_common 'Bis(Deferiprone) phloroglucinol (2:1)' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _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 6.9983(2) _cell_length_b 18.4416(6) _cell_length_c 28.8960(8) _cell_measurement_reflns_used 4198 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.25 _cell_measurement_theta_min 2.32 _cell_volume 3729.31(19) _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 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.1055 _diffrn_reflns_av_unetI/netI 0.0814 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 18441 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.249 _diffrn_reflns_theta_min 2.620 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.441 _exptl_crystal_description block _exptl_crystal_F_000 1712 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.274 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 3759 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0565 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.1236P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.1150 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2498 _reflns_number_total 3759 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block KA773_0m_def-phg_2_1 _cod_database_code 2022896 _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 0.970 _shelx_estimated_absorpt_t_max 0.987 _shelx_res_file ; TITL KA773_0m_a.res in Pbca KA773_0m.res created by SHELXL-2018/3 at 15:12:19 on 16-Apr-2020 CELL 0.71073 6.9983 18.4416 28.8960 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0006 0.0008 0.000 0.000 0.000 LATT 1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H N O UNIT 160 192 16 56 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! HTAB TEMP -173 ACTA L.S. 20 FMAP 2 PLAN -5 0 0.00 OMIT -3 52.5 SIZE 0.28 0.24 0.12 BOND $H EQIV $1 x+1, y, z EQIV $2 -x+1/2, y-1/2, z EQIV $3 -x+1, y+1/2, -z+3/2 EQIV $4 x-1/2, y, -z+3/2 HTAB O1A O2B HTAB O1B O2A HTAB O1B O2B HTAB O3 O4_$1 HTAB O4 O2B_$2 HTAB O5 O2A HTAB C5B O3_$3 HTAB C6B O1A_$4 CONF WGHT 0.035200 3.123600 FVAR 0.30433 MOLE 1 C1A 1 1.087820 0.945015 0.544030 11.00000 0.01232 0.01377 = 0.01118 0.00292 -0.00169 0.00368 C2A 1 0.919351 0.937000 0.567809 11.00000 0.01325 0.01121 = 0.00697 0.00167 -0.00218 0.00183 C3A 1 0.783267 0.881730 0.557129 11.00000 0.01387 0.00987 = 0.01040 0.00412 -0.00250 0.00116 C4A 1 0.830831 0.837999 0.518654 11.00000 0.01654 0.01144 = 0.01394 0.00150 -0.00536 -0.00192 AFIX 43 H4A 2 0.746161 0.800564 0.509190 11.00000 -1.20000 AFIX 0 C5A 1 0.996444 0.848893 0.495018 11.00000 0.02065 0.01671 = 0.00911 -0.00116 0.00045 0.00445 AFIX 43 H5A 2 1.024005 0.818670 0.469244 11.00000 -1.20000 AFIX 0 C6A 1 1.302693 0.906588 0.480782 11.00000 0.01558 0.02556 = 0.01473 0.00274 0.00604 0.00303 AFIX 137 H6A 2 1.409387 0.892534 0.500833 11.00000 -1.50000 H6B 2 1.320344 0.956772 0.470478 11.00000 -1.50000 H6C 2 1.298486 0.874442 0.453796 11.00000 -1.50000 AFIX 0 C7A 1 1.235058 0.999519 0.557278 11.00000 0.01505 0.01751 = 0.01716 0.00305 0.00224 -0.00154 AFIX 137 H7A 2 1.185485 1.030147 0.582258 11.00000 -1.50000 H7B 2 1.265969 1.029772 0.530420 11.00000 -1.50000 H7C 2 1.350594 0.974499 0.567874 11.00000 -1.50000 AFIX 0 O1A 4 0.885092 0.982859 0.603489 11.00000 0.01357 0.01481 = 0.01490 -0.00461 0.00413 -0.00269 H1O 2 0.765571 0.975010 0.617831 11.00000 0.03136 O2A 4 0.631388 0.874645 0.581511 11.00000 0.01223 0.01767 = 0.01372 -0.00097 0.00132 -0.00465 N1A 3 1.122432 0.900612 0.506647 11.00000 0.01286 0.01591 = 0.00980 0.00157 0.00282 0.00192 MOLE 2 C1B 1 0.677732 0.859597 0.752427 11.00000 0.00587 0.01215 = 0.01777 0.00067 -0.00018 -0.00176 C2B 1 0.656531 0.889156 0.709064 11.00000 0.00728 0.01189 = 0.01365 -0.00282 -0.00054 -0.00398 C3B 1 0.600004 0.962217 0.702175 11.00000 0.00469 0.01351 = 0.01487 -0.00040 0.00060 -0.00290 C4B 1 0.558918 1.001614 0.742589 11.00000 0.00570 0.00940 = 0.01973 0.00118 0.00011 -0.00064 AFIX 43 H4B 2 0.516178 1.050365 0.740205 11.00000 -1.20000 AFIX 0 C5B 1 0.579544 0.970856 0.785084 11.00000 0.00793 0.01543 = 0.01422 -0.00378 0.00277 -0.00133 AFIX 43 H5B 2 0.549349 0.998507 0.811841 11.00000 -1.20000 AFIX 0 C6B 1 0.672580 0.873733 0.837117 11.00000 0.01541 0.02138 = 0.01333 0.00467 0.00011 0.00406 AFIX 137 H6D 2 0.576882 0.836388 0.843823 11.00000 -1.50000 H6E 2 0.660788 0.913218 0.859635 11.00000 -1.50000 H6F 2 0.800729 0.852548 0.839157 11.00000 -1.50000 AFIX 0 C7B 1 0.733712 0.782533 0.760127 11.00000 0.01567 0.01347 = 0.01970 0.00201 -0.00390 0.00182 AFIX 137 H7D 2 0.634968 0.758113 0.778441 11.00000 -1.50000 H7E 2 0.855593 0.780788 0.776789 11.00000 -1.50000 H7F 2 0.747372 0.758041 0.730211 11.00000 -1.50000 AFIX 0 O1B 4 0.694450 0.846203 0.671884 11.00000 0.02321 0.01121 = 0.01175 -0.00256 -0.00097 0.00340 H2O 2 0.667808 0.868391 0.646639 11.00000 0.03555 O2B 4 0.586173 0.987661 0.660699 11.00000 0.01581 0.01425 = 0.00931 0.00266 0.00045 0.00297 N1B 3 0.641568 0.902327 0.790181 11.00000 0.01213 0.01353 = 0.01096 0.00179 -0.00032 -0.00057 MOLE 3 C8 1 0.424262 0.656644 0.654545 11.00000 0.01226 0.01087 = 0.01081 -0.00134 -0.00183 0.00167 C9 1 0.243357 0.627088 0.660089 11.00000 0.01467 0.00939 = 0.01094 0.00263 0.00320 -0.00016 AFIX 43 H9 2 0.221819 0.589960 0.682274 11.00000 -1.20000 AFIX 0 C10 1 0.094464 0.652360 0.632890 11.00000 0.00816 0.00878 = 0.01508 -0.00267 0.00289 0.00010 C11 1 0.122623 0.708055 0.601333 11.00000 0.01367 0.00925 = 0.01169 0.00028 -0.00450 0.00072 AFIX 43 H11 2 0.019877 0.725611 0.583000 11.00000 -1.20000 AFIX 0 C12 1 0.304335 0.737552 0.597155 11.00000 0.01532 0.00603 = 0.01076 -0.00033 -0.00039 -0.00058 C13 1 0.457480 0.712064 0.623231 11.00000 0.00795 0.01193 = 0.01295 -0.00363 0.00324 -0.00184 AFIX 43 H13 2 0.581578 0.732169 0.619639 11.00000 -1.20000 AFIX 0 O3 4 0.567952 0.630343 0.682168 11.00000 0.00873 0.02145 = 0.01769 0.00636 -0.00268 -0.00051 H3O 2 0.685940 0.641959 0.670712 11.00000 0.04355 O4 4 -0.084940 0.622852 0.636391 11.00000 0.01107 0.01260 = 0.02470 0.00427 -0.00018 -0.00286 H4O 2 -0.079940 0.576485 0.645713 11.00000 0.04365 O5 4 0.328244 0.792848 0.566127 11.00000 0.01576 0.01382 = 0.01626 0.00647 -0.00336 -0.00390 H5O 2 0.446817 0.819073 0.572444 11.00000 0.06087 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KA773_0m_a.res in Pbca REM wR2 = 0.1150, GooF = S = 1.041, Restrained GooF = 1.041 for all data REM R1 = 0.0565 for 2498 Fo > 4sig(Fo) and 0.1045 for all 3759 data REM 286 parameters refined using 0 restraints END WGHT 0.0352 3.1236 REM Instructions for potential hydrogen bonds HTAB O1A O2B HTAB C5B O3_$3 HTAB C6B O1A_$4 HTAB O1B O2A HTAB O1B O2B HTAB O3 O4_$1 HTAB O4 O2B_$2 HTAB O5 O2A REM Highest difference peak 0.274, deepest hole -0.303, 1-sigma level 0.067 Q1 1 0.6284 0.9791 0.8223 11.00000 0.05 0.27 Q2 1 0.6365 0.6800 0.6001 11.00000 0.05 0.26 Q3 1 0.5746 0.8814 0.7307 11.00000 0.05 0.25 Q4 1 0.2247 0.7577 0.4746 11.00000 0.05 0.24 Q5 1 0.7269 0.8844 0.7324 11.00000 0.05 0.24 ; _shelx_res_checksum 94584 _shelx_hkl_file ; 1 0 0 0.14 0.60 2 0 0 556.82 27.82 2 0 0 584.24 25.44 3 0 0 0.53 5.46 4 0 0 2568.70 116.98 5 0 0 7.07 10.05 6 0 0 488.96 30.97 7 0 0 -10.46 11.74 8 0 0 99.22 18.76 9 0 0 16.73 22.14 1 -1 0 -2.03 1.51 1 1 0 0.25 1.47 -1 1 0 -1.29 1.29 -1 -1 0 0.93 1.84 -2 1 0 1061.04 45.92 2 1 0 1024.37 47.82 2 1 0 1052.99 45.38 3 1 0 8.35 4.81 3 -1 0 9.42 5.97 4 -1 0 20.03 9.36 5 1 0 12.89 9.69 5 -1 0 -7.75 10.29 6 1 0 304.24 24.39 6 -1 0 348.26 25.14 7 -1 0 10.43 12.24 7 1 0 0.08 11.22 8 1 0 10.86 16.83 8 -1 0 8.84 16.19 9 -1 0 -33.71 21.53 9 1 0 28.88 20.48 -1 2 0 3.98 2.45 1 -2 0 -2.63 2.31 -1 -2 0 -1.24 1.44 1 2 0 -0.23 1.09 2 2 0 933.45 40.69 -2 2 0 847.52 39.91 3 2 0 -0.27 1.26 3 2 0 -6.35 3.74 -3 2 0 -0.17 2.53 4 2 0 460.74 21.64 4 2 0 478.29 25.77 -4 2 0 471.45 21.38 4 -2 0 498.35 28.41 5 -2 0 5.12 10.11 5 2 0 12.45 8.47 6 -2 0 708.70 42.71 6 2 0 777.63 41.32 7 -2 0 -0.08 13.77 7 2 0 -22.13 10.75 8 -2 0 20.55 17.76 8 2 0 30.10 15.72 9 2 0 -0.69 17.09 9 -2 0 -16.34 20.06 0 3 0 1.55 2.52 0 3 0 0.36 1.30 0 -3 0 -0.25 1.33 0 -3 0 -2.42 2.36 1 3 0 2.30 1.03 -1 3 0 4.14 3.24 -1 -3 0 -0.98 1.27 -2 3 0 3048.37 133.57 3 3 0 6.26 3.91 -3 3 0 3.60 3.22 -4 3 0 80.72 6.38 4 3 0 75.28 4.80 4 3 0 76.74 9.22 5 3 0 0.07 7.20 5 -3 0 -13.09 10.83 -5 3 0 0.80 2.23 6 3 0 61.26 12.56 6 -3 0 69.44 15.05 7 -3 0 -27.66 15.43 7 3 0 -2.89 9.65 8 -3 0 177.72 27.56 8 3 0 157.18 20.65 9 3 0 -14.05 14.45 9 -3 0 25.36 23.43 0 4 0 4256.15 180.64 0 -4 0 4093.27 179.31 0 4 0 4047.82 179.24 -1 -4 0 0.42 1.19 -1 4 0 0.67 3.90 1 4 0 0.14 1.16 1 4 0 -1.36 1.95 -2 4 0 467.67 23.56 -3 4 0 -6.49 3.74 3 4 0 3.25 3.47 4 4 0 166.31 11.98 -4 4 0 168.63 10.61 5 -4 0 -6.06 10.62 -5 4 0 -3.31 3.83 5 4 0 7.94 7.27 6 4 0 267.64 19.77 6 -4 0 239.19 24.30 7 4 0 -2.15 10.39 7 -4 0 17.84 16.00 8 -4 0 39.41 32.88 8 4 0 5.22 13.96 9 4 0 7.30 16.32 9 -4 0 -25.10 20.56 0 5 0 0.69 3.94 0 5 0 2.40 2.23 1 5 0 -2.59 1.33 1 5 0 -2.97 2.61 -1 5 0 5.51 4.66 -2 5 0 515.05 26.33 -3 5 0 -8.45 4.35 3 5 0 0.56 2.92 4 5 0 638.03 31.37 -4 5 0 652.82 31.18 5 -5 0 -8.27 11.70 -5 5 0 -2.74 4.75 5 5 0 0.91 5.96 6 -5 0 25.10 16.52 6 5 0 46.00 9.82 7 5 0 9.55 9.93 7 -5 0 12.04 16.48 8 -5 0 71.21 21.75 8 5 0 86.66 15.53 9 5 0 11.42 17.86 9 -5 0 -45.99 21.38 0 6 0 2045.59 87.50 0 6 0 1821.09 85.93 1 6 0 1.41 3.86 1 6 0 0.95 2.06 -1 6 0 -1.32 3.80 -1 6 0 -5.39 5.19 -2 6 0 343.00 19.62 2 6 0 326.09 16.23 3 6 0 -0.36 2.66 -3 6 0 2.36 5.37 -4 6 0 3.86 5.84 4 6 0 2.01 4.01 5 6 0 -5.36 5.74 -5 6 0 7.31 5.70 6 -6 0 167.31 21.83 6 6 0 108.12 12.39 7 6 0 21.92 9.07 7 -6 0 -20.82 16.42 8 6 0 7.20 11.64 8 -6 0 9.71 22.56 9 -6 0 -57.09 23.18 0 7 0 4.79 3.34 0 7 0 8.27 5.55 -1 7 0 -6.34 5.20 -1 7 0 3.56 4.25 1 7 0 -0.19 2.50 1 7 0 0.53 4.87 -2 7 0 309.60 19.48 2 7 0 283.99 14.68 2 7 0 327.35 16.01 -3 7 0 -2.92 6.46 3 7 0 -3.87 2.47 -4 7 0 134.16 12.97 4 7 0 148.13 9.45 -5 7 0 6.08 6.81 5 7 0 -0.76 5.24 6 -7 0 172.93 23.83 6 7 0 159.72 15.84 7 -7 0 7.66 20.34 7 7 0 -14.96 7.41 8 -7 0 454.25 39.56 8 7 0 363.25 25.39 9 -7 0 21.33 25.37 0 8 0 7954.63 339.56 0 8 0 7555.77 336.59 -1 8 0 2.64 4.33 1 8 0 1.25 3.28 1 8 0 7.25 5.98 -1 8 0 1.85 7.45 2 8 0 294.30 13.85 -2 8 0 245.79 18.76 2 8 0 272.05 15.90 3 8 0 -0.45 3.61 -3 8 0 1.70 8.04 3 8 0 -0.04 2.51 -4 8 0 52.42 10.37 4 8 0 47.30 5.74 5 8 0 3.53 5.31 -5 8 0 8.38 8.71 6 -8 0 25.17 16.74 7 -8 0 -21.69 20.51 7 8 0 1.55 7.58 8 -8 0 -6.21 21.08 9 -8 0 22.83 26.00 0 9 0 0.99 4.04 0 9 0 -7.41 7.44 1 9 0 -0.42 3.79 1 9 0 6.13 6.55 -1 9 0 -3.30 7.81 -1 9 0 -2.73 4.77 -2 9 0 437.63 27.59 2 9 0 447.31 24.35 2 9 0 485.14 22.05 -3 9 0 12.75 9.10 3 9 0 -0.37 3.02 3 9 0 -4.02 4.79 4 9 0 12.36 4.04 -4 9 0 15.18 10.67 5 9 0 -10.89 4.36 -5 9 0 26.31 12.18 6 9 0 152.87 13.24 6 -9 0 147.73 23.83 7 -9 0 -40.23 19.14 8 -9 0 -6.22 23.93 9 -9 0 -31.67 30.75 0 10 0 133.28 10.23 0 10 0 147.27 15.19 -1 10 0 -3.20 8.45 1 10 0 4.99 7.61 -1 10 0 -7.88 5.18 1 10 0 10.75 4.44 2 10 0 117.67 11.93 -2 10 0 116.39 14.62 2 10 0 107.65 7.96 3 10 0 0.75 3.52 -3 10 0 -11.71 9.03 3 10 0 11.97 6.60 4 10 0 51.92 7.76 4 10 0 48.26 5.80 -4 10 0 62.69 12.25 -5 10 0 3.37 10.49 5 10 0 -0.47 4.67 -6 10 0 -4.96 9.07 6 10 0 9.22 7.07 6 -10 0 -4.20 19.88 8 -10 0 168.38 34.65 9 -10 0 -17.37 27.93 0 11 0 0.90 4.95 0 11 0 12.25 10.26 1 11 0 7.17 8.27 1 11 0 0.55 4.61 -1 11 0 14.57 11.25 2 11 0 185.61 11.25 2 11 0 172.21 15.89 3 11 0 -0.86 4.20 -3 11 0 -10.04 9.59 3 11 0 18.76 8.18 -4 11 0 66.80 13.14 4 11 0 37.28 6.03 4 11 0 49.88 9.11 -5 11 0 6.29 11.16 5 11 0 -3.01 4.92 -6 11 0 98.72 13.84 7 -11 0 -14.90 24.50 8 -11 0 14.41 25.26 9 -11 0 -59.13 26.98 0 12 0 815.39 39.05 0 12 0 787.68 44.41 1 12 0 5.51 10.17 1 12 0 1.64 5.22 -1 12 0 28.10 12.17 2 12 0 7.10 5.43 -2 12 0 3.06 9.93 2 12 0 -5.11 9.21 -3 12 0 -22.60 10.93 3 12 0 3.14 4.70 3 12 0 -2.82 9.85 -4 12 0 58.34 13.52 4 12 0 64.85 11.55 4 12 0 61.26 7.79 -5 12 0 -2.20 11.24 -6 12 0 29.16 11.71 7 -12 0 48.20 24.49 8 -12 0 -25.17 30.44 0 13 0 3.66 10.75 0 13 0 0.79 6.85 -1 13 0 8.96 11.98 1 13 0 -9.26 11.34 1 13 0 3.02 5.79 2 13 0 12.24 12.52 -2 13 0 8.33 10.93 2 13 0 13.78 6.21 3 13 0 5.50 5.88 -3 13 0 24.60 12.44 3 13 0 -0.24 11.31 4 13 0 145.60 17.75 -4 13 0 148.67 20.16 -5 13 0 22.42 13.52 -6 13 0 22.15 13.11 7 -13 0 4.96 25.49 8 -13 0 22.79 29.46 0 14 0 619.99 39.55 0 14 0 675.74 33.84 -1 14 0 -8.06 10.89 1 14 0 2.91 11.61 1 14 0 -0.58 6.29 -2 14 0 21.18 13.99 2 14 0 25.32 12.88 2 14 0 15.26 7.02 3 14 0 9.67 13.50 3 14 0 -5.01 5.92 -3 14 0 2.80 13.61 -4 14 0 122.18 18.65 4 14 0 134.32 18.20 -5 14 0 7.53 14.63 -6 14 0 2.60 15.76 7 -14 0 18.36 26.48 8 -14 0 45.42 34.13 0 15 0 -4.86 11.86 0 15 0 7.35 8.11 -1 15 0 -6.09 13.06 1 15 0 -1.82 7.64 1 15 0 7.65 13.13 2 15 0 12.29 7.50 -2 15 0 -4.46 13.74 2 15 0 7.52 13.57 -3 15 0 19.32 15.66 3 15 0 -5.39 13.85 -4 15 0 18.93 16.45 4 15 0 29.49 14.68 -5 15 0 16.10 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4 -37 -37.63 26.19 1 -4 -37 -5.95 16.28 -2 4 37 -29.90 18.21 2 4 -37 29.27 19.01 2 4 37 20.18 17.24 -2 4 -37 36.39 28.07 2 -4 -37 19.21 16.95 3 4 -37 -12.83 18.40 -3 4 37 44.36 20.58 3 4 37 -1.36 18.93 -3 4 -37 15.46 27.18 3 -4 -37 32.31 20.41 4 4 -37 52.06 20.57 -4 4 37 24.03 23.64 4 -4 -37 27.53 21.39 -4 4 -37 37.30 32.86 0 5 37 -27.98 16.02 0 5 -37 13.81 19.96 0 5 -37 57.42 26.09 1 5 -37 0.94 19.15 1 5 -37 -17.95 21.74 -1 5 37 0.98 16.99 1 5 37 -15.39 17.31 -1 5 -37 4.12 29.93 1 -5 -37 12.09 14.88 -1 5 -37 65.39 25.95 -2 5 37 56.41 18.80 2 5 -37 23.60 21.33 2 -5 -37 22.33 19.48 -2 5 -37 -21.62 23.03 2 5 37 24.06 18.25 3 5 -37 19.60 21.08 3 5 37 -14.74 18.12 3 -5 -37 4.46 17.55 -3 5 -37 24.05 27.78 4 5 -37 32.88 20.75 -4 5 -37 -3.84 34.56 0 6 -37 96.44 22.93 0 6 -37 48.51 27.03 0 6 37 73.51 19.69 -1 6 37 -7.29 17.35 1 6 -37 13.88 23.11 1 6 -37 54.04 22.59 -1 6 -37 46.04 22.11 1 6 37 14.75 17.06 -1 6 -37 17.13 32.25 2 6 -37 28.29 19.29 -2 6 37 36.47 18.54 2 -6 -37 25.29 18.00 -2 6 -37 -6.57 23.51 2 6 37 -20.84 17.65 3 6 -37 5.51 21.33 -3 6 37 -5.49 19.50 -3 6 -37 61.38 31.57 3 6 37 50.85 19.92 3 -6 -37 49.77 21.49 0 7 -37 24.75 24.35 0 7 37 24.42 17.15 0 7 -37 -27.44 25.56 1 7 -37 -3.99 23.36 -1 7 37 10.98 17.24 1 7 -37 -31.60 20.06 1 7 37 -22.73 16.19 -1 7 -37 -41.50 31.02 -1 7 -37 35.20 22.87 2 7 -37 62.70 23.41 -2 7 37 95.65 20.62 2 7 -37 73.19 22.37 -2 7 -37 34.54 28.65 2 7 37 32.85 19.46 -3 7 37 20.05 20.49 3 7 -37 12.34 18.69 -3 7 -37 -29.28 29.83 3 -7 -37 18.58 19.24 3 7 37 -13.90 19.66 0 8 -37 -0.10 20.99 0 8 -37 21.87 28.65 0 8 37 15.04 16.64 -1 8 37 13.47 18.15 1 8 -37 24.79 21.10 1 8 -37 43.35 26.28 -1 8 -37 14.93 22.11 -1 8 -37 14.38 33.29 1 8 37 34.66 17.83 -2 8 37 26.39 18.62 2 8 -37 18.49 20.58 2 8 -37 -17.01 23.15 -2 8 -37 4.50 24.05 2 8 37 14.80 19.00 -2 8 -37 55.93 50.71 3 8 -37 49.78 20.12 -3 8 37 28.23 21.44 3 8 37 -11.96 19.62 -3 8 -37 13.26 27.20 0 9 -37 -27.74 19.80 0 9 37 7.24 17.98 0 9 -37 -30.24 29.31 1 9 -37 -28.55 25.16 1 9 -37 33.80 24.76 -1 9 37 -8.58 17.87 1 9 37 46.75 18.58 -1 9 -37 49.19 36.82 -1 9 -37 -13.67 23.06 2 9 -37 15.52 21.11 2 9 -37 26.90 26.14 -2 9 37 13.90 19.05 2 9 37 26.10 19.02 -2 9 -37 -43.73 24.12 -2 9 -37 -14.20 35.67 0 10 -37 -3.34 23.90 0 10 37 17.50 18.26 0 10 -37 83.56 33.58 1 10 -37 38.92 28.52 -1 10 37 -9.17 17.68 1 10 -37 -25.73 20.17 -1 10 -37 -36.25 26.54 1 10 37 18.99 18.91 -1 10 -37 29.80 37.45 2 10 -37 14.10 27.28 -2 10 37 52.92 20.27 2 10 -37 4.88 22.28 -2 10 -37 26.61 36.44 2 10 37 44.07 20.47 -2 10 -37 8.33 25.87 0 11 -37 1.52 32.49 0 11 37 31.25 19.85 0 11 -37 32.83 27.67 1 11 -37 37.89 22.79 1 11 -37 18.27 31.74 -1 11 37 1.02 19.31 -1 11 -37 -28.00 24.60 1 11 37 7.33 19.89 -1 11 -37 -64.60 36.92 0 0 -38 205.91 30.40 0 0 -38 185.81 27.23 1 0 -38 84.67 21.98 -1 0 -38 15.87 25.58 -2 0 -38 -5.68 23.64 2 0 -38 8.73 21.91 3 0 -38 33.34 21.20 0 1 -38 -5.26 23.93 0 1 -38 37.03 24.85 0 -1 -38 28.11 23.14 -1 -1 -38 61.04 23.54 1 1 -38 49.09 22.64 1 -1 -38 29.49 22.26 -1 1 -38 32.89 24.42 -1 1 -38 -10.40 25.11 2 1 -38 87.50 23.46 -2 1 -38 96.07 29.64 2 -1 -38 45.93 23.54 3 1 -38 -2.22 18.59 3 -1 -38 18.73 20.78 0 2 -38 59.24 23.28 0 2 38 66.14 18.72 0 2 -38 77.35 26.69 0 -2 -38 59.90 23.43 -1 2 38 11.97 18.42 1 2 -38 -1.79 22.79 1 2 38 14.23 18.24 -1 2 -38 17.68 26.02 -1 2 -38 55.63 27.44 1 -2 -38 9.55 19.58 -2 2 38 38.75 20.27 2 2 -38 -30.94 21.62 2 -2 -38 14.84 21.74 -2 2 -38 9.70 25.20 3 2 -38 4.26 19.16 3 -2 -38 5.13 21.00 -3 2 -38 21.05 28.61 0 3 -38 28.70 25.74 0 -3 -38 6.92 20.01 0 3 -38 40.13 22.07 0 3 38 28.04 18.35 -1 3 38 4.28 17.00 1 3 -38 10.85 22.53 1 3 38 -3.37 16.98 -1 3 -38 17.22 26.70 -1 3 -38 -32.66 26.79 1 -3 -38 13.92 21.66 2 3 -38 -11.38 20.87 -2 3 38 26.44 20.15 2 3 38 -26.40 18.02 -2 3 -38 21.41 30.22 2 -3 -38 10.50 21.92 -3 3 38 23.87 20.50 3 3 -38 -0.27 21.91 3 -3 -38 25.31 19.41 -3 3 -38 -7.25 30.63 0 4 -38 38.92 24.72 0 4 -38 63.59 27.55 0 4 38 35.52 18.90 1 4 -38 19.69 23.69 1 4 -38 35.02 23.31 -1 4 38 44.31 19.16 -1 4 -38 30.15 30.84 1 4 38 31.34 18.73 -1 4 -38 40.13 24.08 1 -4 -38 -0.39 19.98 -2 4 38 8.22 19.79 2 4 -38 -3.99 19.01 -2 4 -38 22.50 28.54 2 4 38 38.58 18.77 2 -4 -38 15.49 21.68 -3 4 38 -0.25 20.42 3 4 -38 -21.74 19.59 3 4 38 -16.84 19.66 -3 4 -38 19.13 28.84 3 -4 -38 16.80 21.53 0 5 -38 34.52 25.39 0 5 -38 3.39 27.19 0 5 38 17.32 18.10 1 5 -38 -29.51 21.92 1 5 -38 16.33 19.95 -1 5 38 -30.69 16.07 -1 5 -38 55.77 33.77 1 5 38 -4.97 18.32 -1 5 -38 46.36 26.43 -2 5 38 -19.01 18.72 2 5 -38 16.17 22.34 2 -5 -38 20.33 20.14 2 5 38 -14.79 17.91 -2 5 -38 -12.20 28.60 -3 5 38 3.56 20.79 3 5 -38 28.63 22.60 -3 5 -38 25.98 32.62 3 5 38 -29.90 19.24 3 -5 -38 16.71 19.18 0 6 -38 63.55 29.72 0 6 38 19.12 17.49 0 6 -38 50.70 25.17 1 6 -38 26.01 20.67 1 6 -38 -11.32 24.30 -1 6 38 18.56 18.46 -1 6 -38 50.55 34.23 1 6 38 -1.23 18.46 -1 6 -38 -17.78 25.85 2 6 -38 81.78 22.39 2 6 -38 84.43 26.24 -2 6 38 100.02 20.93 -2 6 -38 86.43 28.44 2 6 38 92.54 22.08 3 6 -38 46.70 21.03 -3 6 38 19.11 20.43 -3 6 -38 50.39 33.43 3 6 38 52.30 21.37 3 -6 -38 36.11 20.91 0 7 38 -12.89 17.83 0 7 -38 -0.16 28.90 0 7 -38 -7.32 21.52 1 7 -38 -8.11 25.75 1 7 -38 25.95 24.57 -1 7 38 7.70 18.60 -1 7 -38 -16.30 21.82 -1 7 -38 54.96 35.34 1 7 38 -5.68 17.69 -2 7 38 31.77 19.76 2 7 -38 62.10 26.55 2 7 -38 22.05 21.32 -2 7 -38 31.05 29.55 2 7 38 73.54 20.88 0 8 -38 344.54 42.37 0 8 38 282.55 29.63 0 8 -38 254.31 33.09 1 8 -38 19.94 27.38 1 8 -38 53.39 22.72 -1 8 38 -9.55 18.27 -1 8 -38 75.52 37.35 1 8 38 -16.56 17.70 -1 8 -38 29.13 24.14 2 8 -38 -61.10 24.49 -2 8 38 -6.74 19.00 2 8 -38 23.96 21.13 -2 8 -38 -13.63 25.89 2 8 38 -25.85 19.03 0 9 38 -7.91 17.86 0 9 -38 -18.82 31.84 0 9 -38 -31.23 25.35 1 9 -38 7.06 22.90 1 9 -38 17.44 28.65 -1 9 38 1.57 18.92 -1 9 -38 24.44 24.75 -1 9 -38 -35.06 36.74 1 9 38 10.48 19.09 0 10 -38 129.65 37.57 0 10 38 127.68 23.52 1 10 -38 -36.31 24.29 -1 10 -38 22.82 29.04 0 0 -39 -27.34 22.04 0 0 -39 43.84 25.98 -1 0 -39 -53.21 23.98 1 0 -39 0.04 20.59 2 0 -39 11.96 22.92 3 0 -39 23.49 20.24 0 1 -39 4.68 25.39 0 1 -39 68.09 26.35 0 -1 -39 -31.22 23.88 1 1 -39 -34.39 23.08 -1 -1 -39 -21.75 23.44 1 -1 -39 34.81 24.72 -1 1 -39 -16.68 26.72 2 1 -39 93.25 25.03 -2 1 -39 105.93 30.18 2 -1 -39 33.05 22.07 3 1 -39 19.56 20.43 3 -1 -39 -3.00 19.12 0 2 -39 51.59 23.61 0 2 39 -2.15 17.66 0 2 -39 56.32 27.38 1 2 -39 33.43 25.24 -1 2 -39 78.57 29.39 1 -2 -39 107.92 25.81 2 2 -39 24.00 23.27 -2 2 -39 8.42 26.09 2 -2 -39 21.83 23.39 3 2 -39 24.17 23.51 3 -2 -39 41.39 23.71 0 3 39 22.22 19.37 0 3 -39 14.00 25.93 0 3 -39 3.71 27.33 1 3 -39 6.70 22.66 -1 3 39 3.45 18.21 1 3 -39 46.65 22.30 1 -3 -39 49.71 20.73 1 3 39 -1.89 18.75 -1 3 -39 2.35 23.92 -1 3 -39 -14.26 28.12 -2 3 39 5.00 21.08 2 3 -39 -10.35 20.32 2 3 39 -37.85 18.19 2 -3 -39 3.07 19.98 -2 3 -39 46.26 30.12 3 3 -39 18.26 21.20 -3 3 39 -13.18 21.64 -3 3 -39 44.96 30.85 3 -3 -39 22.72 22.40 0 4 -39 100.68 24.62 0 4 39 46.37 20.60 0 4 -39 18.80 29.09 1 4 -39 -20.50 24.37 -1 4 39 -18.20 18.05 1 4 -39 6.52 20.81 1 4 39 21.40 19.26 1 -4 -39 -22.33 19.23 -1 4 -39 28.28 30.73 -1 4 -39 8.60 28.00 -2 4 39 5.68 20.23 2 4 -39 56.78 21.76 -2 4 -39 -19.22 29.30 2 4 39 49.78 20.54 2 -4 -39 30.20 23.07 0 5 39 1.16 18.55 0 5 -39 -15.84 28.38 0 5 -39 26.37 23.14 1 5 -39 -7.90 24.59 -1 5 39 11.26 19.26 1 5 -39 23.41 25.94 -1 5 -39 -6.64 24.85 1 5 39 12.18 19.23 -1 5 -39 32.99 33.36 -2 5 39 -44.49 19.88 2 5 -39 -9.20 22.73 2 -5 -39 -17.19 20.93 -2 5 -39 21.63 30.57 2 5 39 -6.24 19.55 0 6 39 -3.91 18.48 0 6 -39 -6.48 30.81 0 6 -39 17.40 23.56 1 6 -39 -3.46 21.51 1 6 -39 17.35 26.66 -1 6 39 8.30 19.45 1 6 39 31.36 19.86 -1 6 -39 40.03 35.11 -1 6 -39 -17.58 26.90 2 6 -39 -2.35 25.55 -2 6 39 12.85 21.10 2 6 -39 47.84 22.51 -2 6 -39 15.31 26.60 2 6 39 14.98 20.58 0 7 -39 1.07 30.08 0 7 -39 -42.96 21.90 0 7 39 34.76 20.09 1 7 -39 -4.60 22.10 -1 7 39 19.19 19.06 1 7 -39 24.04 27.86 -1 7 -39 78.42 36.69 1 7 39 4.85 19.20 -1 7 -39 83.16 30.24 0 8 -39 416.22 48.08 0 8 39 374.44 34.41 0 8 -39 350.27 41.90 -1 8 39 29.50 19.91 1 8 -39 -3.32 26.02 1 8 -39 16.41 28.64 1 8 39 -0.22 19.57 -1 8 -39 0.85 24.69 -1 8 -39 -27.64 35.83 0 0 -40 4.15 26.66 0 0 -40 30.96 24.47 -1 0 -40 -17.57 25.95 1 0 -40 12.02 22.57 2 0 -40 23.05 23.35 0 -1 -40 -9.70 24.14 0 1 -40 1.99 24.29 0 1 -40 -1.77 27.36 0 -1 -40 -0.02 25.44 1 1 -40 -3.83 25.27 1 -1 -40 5.87 24.90 -1 1 -40 -27.56 28.11 2 1 -40 5.47 21.32 2 -1 -40 7.57 24.21 0 2 -40 119.82 30.30 0 -2 -40 105.92 28.12 0 2 -40 75.33 29.98 1 2 -40 28.33 21.91 1 -2 -40 7.50 25.15 -1 2 -40 -16.20 28.99 2 2 -40 -19.01 21.04 2 -2 -40 -8.46 20.38 -2 2 -40 40.52 30.54 0 3 -40 -49.36 27.46 0 3 40 -8.38 19.95 0 3 -40 -2.16 24.36 1 3 -40 102.90 26.92 -1 3 40 53.99 22.20 1 3 -40 64.67 25.01 1 -3 -40 15.83 23.39 1 3 40 63.45 22.53 -1 3 -40 -20.75 29.71 2 3 -40 25.78 21.23 -2 3 40 17.48 22.53 -2 3 -40 41.31 28.82 2 -3 -40 8.44 24.57 0 4 40 28.32 19.32 0 4 -40 65.51 26.02 0 4 -40 50.49 29.95 1 4 -40 26.63 22.77 1 4 -40 17.72 25.23 -1 4 40 -1.04 19.55 -1 4 -40 28.64 40.25 -1 4 -40 -7.17 27.91 1 4 40 42.52 20.65 -2 4 -40 24.55 31.47 0 5 -40 -43.95 25.93 0 5 -40 27.38 31.59 0 5 40 12.62 20.66 -1 5 40 -11.34 19.87 1 5 -40 -22.85 23.01 1 5 -40 -32.37 26.14 -1 5 -40 5.99 25.49 -1 5 -40 59.14 32.61 1 5 40 -15.09 20.41 0 6 -40 71.25 27.70 0 6 -40 -55.72 30.93 0 6 40 19.48 20.91 1 6 -40 -15.95 26.20 -1 6 -40 5.50 26.27 0 0 -41 60.82 28.88 0 0 -41 29.79 26.32 1 0 -41 11.86 24.18 0 -1 -41 27.55 25.84 0 -1 -41 -28.08 23.78 0 1 -41 25.23 25.19 0 1 -41 5.29 27.31 1 1 -41 -1.45 27.85 1 -1 -41 -25.44 22.63 -1 1 -41 44.03 27.39 0 2 -41 33.20 29.55 0 2 -41 53.03 30.19 0 3 41 26.37 21.62 0 3 -41 33.29 30.31 0 3 -41 -44.94 24.89 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 0.6560 _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 0.71072 6.988 18.461 28.914 90.047 89.985 89.976 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 23809 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' 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 1.0878(4) 0.94502(14) 0.54403(8) 0.0124(6) Uani 1 1 d . . . . . C2A C 0.9194(4) 0.93700(13) 0.56781(7) 0.0105(6) Uani 1 1 d . . . . . C3A C 0.7833(4) 0.88173(14) 0.55713(7) 0.0114(6) Uani 1 1 d . . . . . C4A C 0.8308(4) 0.83800(14) 0.51865(8) 0.0140(6) Uani 1 1 d . . . . . H4A H 0.746161 0.800564 0.509190 0.017 Uiso 1 1 calc R U . . . C5A C 0.9964(4) 0.84889(14) 0.49502(8) 0.0155(6) Uani 1 1 d . . . . . H5A H 1.024005 0.818670 0.469244 0.019 Uiso 1 1 calc R U . . . C6A C 1.3027(4) 0.90659(15) 0.48078(8) 0.0186(6) Uani 1 1 d . . . . . H6A H 1.409387 0.892534 0.500833 0.028 Uiso 1 1 calc R U . . . H6B H 1.320344 0.956772 0.470478 0.028 Uiso 1 1 calc R U . . . H6C H 1.298486 0.874442 0.453796 0.028 Uiso 1 1 calc R U . . . C7A C 1.2351(4) 0.99952(14) 0.55728(8) 0.0166(6) Uani 1 1 d . . . . . H7A H 1.185485 1.030147 0.582258 0.025 Uiso 1 1 calc R U . . . H7B H 1.265969 1.029772 0.530420 0.025 Uiso 1 1 calc R U . . . H7C H 1.350594 0.974499 0.567874 0.025 Uiso 1 1 calc R U . . . O1A O 0.8851(3) 0.98286(9) 0.60349(6) 0.0144(4) Uani 1 1 d . . . . . H1O H 0.766(5) 0.9750(16) 0.6178(9) 0.031(9) Uiso 1 1 d . . . . . O2A O 0.6314(2) 0.87464(9) 0.58151(5) 0.0145(4) Uani 1 1 d . . . . . N1A N 1.1224(3) 0.90061(11) 0.50665(6) 0.0129(5) Uani 1 1 d . . . . . C1B C 0.6777(4) 0.85960(13) 0.75243(8) 0.0119(6) Uani 1 1 d . . . . . C2B C 0.6565(3) 0.88916(14) 0.70906(8) 0.0109(6) Uani 1 1 d . . . . . C3B C 0.6000(4) 0.96222(13) 0.70218(8) 0.0110(6) Uani 1 1 d . . . . . C4B C 0.5589(3) 1.00161(14) 0.74259(8) 0.0116(5) Uani 1 1 d . . . . . H4B H 0.516178 1.050365 0.740205 0.014 Uiso 1 1 calc R U . . . C5B C 0.5795(4) 0.97086(14) 0.78508(8) 0.0125(6) Uani 1 1 d . . . . . H5B H 0.549349 0.998507 0.811841 0.015 Uiso 1 1 calc R U . . . C6B C 0.6726(4) 0.87373(15) 0.83712(8) 0.0167(6) Uani 1 1 d . . . . . H6D H 0.576882 0.836388 0.843823 0.025 Uiso 1 1 calc R U . . . H6E H 0.660788 0.913218 0.859635 0.025 Uiso 1 1 calc R U . . . H6F H 0.800729 0.852548 0.839157 0.025 Uiso 1 1 calc R U . . . C7B C 0.7337(4) 0.78253(14) 0.76013(8) 0.0163(6) Uani 1 1 d . . . . . H7D H 0.634968 0.758113 0.778441 0.024 Uiso 1 1 calc R U . . . H7E H 0.855593 0.780788 0.776789 0.024 Uiso 1 1 calc R U . . . H7F H 0.747372 0.758041 0.730211 0.024 Uiso 1 1 calc R U . . . O1B O 0.6944(3) 0.84620(10) 0.67188(6) 0.0154(4) Uani 1 1 d . . . . . H2O H 0.668(4) 0.8684(17) 0.6466(10) 0.036(10) Uiso 1 1 d . . . . . O2B O 0.5862(2) 0.98766(9) 0.66070(5) 0.0131(4) Uani 1 1 d . . . . . N1B N 0.6416(3) 0.90233(11) 0.79018(6) 0.0122(5) Uani 1 1 d . . . . . C8 C 0.4243(4) 0.65664(14) 0.65454(8) 0.0113(5) Uani 1 1 d . . . . . C9 C 0.2434(4) 0.62709(14) 0.66009(7) 0.0117(5) Uani 1 1 d . . . . . H9 H 0.221819 0.589960 0.682274 0.014 Uiso 1 1 calc R U . . . C10 C 0.0945(4) 0.65236(13) 0.63289(8) 0.0107(5) Uani 1 1 d . . . . . C11 C 0.1226(4) 0.70806(13) 0.60133(8) 0.0115(6) Uani 1 1 d . . . . . H11 H 0.019877 0.725611 0.583000 0.014 Uiso 1 1 calc R U . . . C12 C 0.3043(4) 0.73755(13) 0.59715(8) 0.0107(6) Uani 1 1 d . . . . . C13 C 0.4575(4) 0.71206(14) 0.62323(7) 0.0109(6) Uani 1 1 d . . . . . H13 H 0.581578 0.732169 0.619639 0.013 Uiso 1 1 calc R U . . . O3 O 0.5680(3) 0.63034(10) 0.68217(6) 0.0160(4) Uani 1 1 d . . . . . H3O H 0.686(5) 0.6420(18) 0.6707(10) 0.044(10) Uiso 1 1 d . . . . . O4 O -0.0849(3) 0.62285(11) 0.63639(6) 0.0161(4) Uani 1 1 d . . . . . H4O H -0.080(5) 0.5765(18) 0.6457(10) 0.044(10) Uiso 1 1 d . . . . . O5 O 0.3282(3) 0.79285(10) 0.56613(6) 0.0153(4) Uani 1 1 d . . . . . H5O H 0.447(5) 0.8191(19) 0.5724(11) 0.061(12) 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 0.0123(14) 0.0138(14) 0.0112(12) 0.0029(10) -0.0017(11) 0.0037(12) C2A 0.0132(15) 0.0112(14) 0.0070(11) 0.0017(10) -0.0022(10) 0.0018(11) C3A 0.0139(15) 0.0099(14) 0.0104(11) 0.0041(10) -0.0025(10) 0.0012(11) C4A 0.0165(16) 0.0114(14) 0.0139(12) 0.0015(10) -0.0054(11) -0.0019(12) C5A 0.0207(15) 0.0167(15) 0.0091(11) -0.0012(11) 0.0004(11) 0.0044(13) C6A 0.0156(15) 0.0256(16) 0.0147(13) 0.0027(11) 0.0060(11) 0.0030(13) C7A 0.0151(15) 0.0175(15) 0.0172(13) 0.0031(11) 0.0022(11) -0.0015(12) O1A 0.0136(11) 0.0148(10) 0.0149(9) -0.0046(7) 0.0041(8) -0.0027(8) O2A 0.0122(10) 0.0177(10) 0.0137(8) -0.0010(7) 0.0013(7) -0.0046(8) N1A 0.0129(12) 0.0159(12) 0.0098(10) 0.0016(9) 0.0028(9) 0.0019(10) C1B 0.0059(13) 0.0122(14) 0.0178(12) 0.0007(11) -0.0002(10) -0.0018(11) C2B 0.0073(14) 0.0119(15) 0.0136(12) -0.0028(10) -0.0005(10) -0.0040(11) C3B 0.0047(14) 0.0135(14) 0.0149(12) -0.0004(10) 0.0006(10) -0.0029(11) C4B 0.0057(13) 0.0094(13) 0.0197(13) 0.0012(10) 0.0001(10) -0.0006(11) C5B 0.0079(14) 0.0154(15) 0.0142(12) -0.0038(10) 0.0028(10) -0.0013(12) C6B 0.0154(15) 0.0214(16) 0.0133(12) 0.0047(11) 0.0001(11) 0.0041(12) C7B 0.0157(15) 0.0135(14) 0.0197(13) 0.0020(11) -0.0039(11) 0.0018(12) O1B 0.0232(12) 0.0112(10) 0.0118(9) -0.0026(8) -0.0010(8) 0.0034(8) O2B 0.0158(10) 0.0142(10) 0.0093(8) 0.0027(7) 0.0004(7) 0.0030(8) N1B 0.0121(12) 0.0135(12) 0.0110(10) 0.0018(9) -0.0003(9) -0.0006(10) C8 0.0123(14) 0.0109(13) 0.0108(11) -0.0013(10) -0.0018(10) 0.0017(12) C9 0.0147(14) 0.0094(13) 0.0109(11) 0.0026(10) 0.0032(11) -0.0002(12) C10 0.0082(14) 0.0088(13) 0.0151(12) -0.0027(10) 0.0029(10) 0.0001(11) C11 0.0137(15) 0.0093(13) 0.0117(11) 0.0003(10) -0.0045(10) 0.0007(11) C12 0.0153(15) 0.0060(13) 0.0108(11) -0.0003(10) -0.0004(10) -0.0006(11) C13 0.0079(14) 0.0119(14) 0.0129(12) -0.0036(10) 0.0032(10) -0.0018(11) O3 0.0087(11) 0.0214(11) 0.0177(9) 0.0064(8) -0.0027(8) -0.0005(9) O4 0.0111(10) 0.0126(11) 0.0247(9) 0.0043(8) -0.0002(8) -0.0029(9) O5 0.0158(11) 0.0138(10) 0.0163(9) 0.0065(8) -0.0034(8) -0.0039(9) 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 C2A C1A N1A 118.7(2) . . ? C2A C1A C7A 122.6(2) . . ? N1A C1A C7A 118.8(2) . . ? O1A C2A C1A 117.8(2) . . ? O1A C2A C3A 119.5(2) . . ? C1A C2A C3A 122.8(2) . . ? O2A C3A C4A 124.7(2) . . ? O2A C3A C2A 120.4(2) . . ? C4A C3A C2A 114.8(2) . . ? C5A C4A C3A 120.8(2) . . ? C5A C4A H4A 119.6 . . ? C3A C4A H4A 119.6 . . ? N1A C5A C4A 122.6(2) . . ? N1A C5A H5A 118.7 . . ? C4A C5A H5A 118.7 . . ? 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 113.3(17) . . ? C5A N1A C1A 120.2(2) . . ? C5A N1A C6A 119.3(2) . . ? C1A N1A C6A 120.3(2) . . ? N1B C1B C2B 118.6(2) . . ? N1B C1B C7B 118.6(2) . . ? C2B C1B C7B 122.9(2) . . ? O1B C2B C1B 117.9(2) . . ? O1B C2B C3B 119.8(2) . . ? C1B C2B C3B 122.3(2) . . ? O2B C3B C4B 124.6(2) . . ? O2B C3B C2B 119.8(2) . . ? C4B C3B C2B 115.6(2) . . ? C5B C4B C3B 120.9(2) . . ? C5B C4B H4B 119.6 . . ? C3B C4B H4B 119.6 . . ? N1B C5B C4B 121.7(2) . . ? N1B C5B H5B 119.2 . . ? C4B C5B H5B 119.2 . . ? 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 111(2) . . ? C5B N1B C1B 120.9(2) . . ? C5B N1B C6B 119.0(2) . . ? C1B N1B C6B 120.1(2) . . ? O3 C8 C13 121.2(2) . . ? O3 C8 C9 117.5(2) . . ? C13 C8 C9 121.2(2) . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? O4 C10 C9 120.8(2) . . ? O4 C10 C11 118.2(2) . . ? C9 C10 C11 121.0(2) . . ? C10 C11 C12 118.5(2) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? O5 C12 C11 117.5(2) . . ? O5 C12 C13 120.8(2) . . ? C11 C12 C13 121.7(2) . . ? C8 C13 C12 118.3(2) . . ? C8 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C8 O3 H3O 112(2) . . ? C10 O4 H4O 111(2) . . ? C12 O5 H5O 110(2) . . ? 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 C2A 1.373(3) . ? C1A N1A 1.377(3) . ? C1A C7A 1.490(4) . ? C2A O1A 1.355(3) . ? C2A C3A 1.429(4) . ? C3A O2A 1.282(3) . ? C3A C4A 1.413(3) . ? C4A C5A 1.360(4) . ? C4A H4A 0.9500 . ? C5A N1A 1.342(3) . ? C5A H5A 0.9500 . ? C6A N1A 1.470(3) . ? 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 0.94(3) . ? C1B N1B 1.369(3) . ? C1B C2B 1.375(3) . ? C1B C7B 1.491(3) . ? C2B O1B 1.361(3) . ? C2B C3B 1.418(4) . ? C3B O2B 1.291(3) . ? C3B C4B 1.405(3) . ? C4B C5B 1.360(3) . ? C4B H4B 0.9500 . ? C5B N1B 1.344(3) . ? C5B H5B 0.9500 . ? C6B N1B 1.471(3) . ? 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 0.86(3) . ? C8 O3 1.372(3) . ? C8 C13 1.385(3) . ? C8 C9 1.388(4) . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 O4 1.372(3) . ? C10 C11 1.388(3) . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 O5 1.368(3) . ? C12 C13 1.392(3) . ? C13 H13 0.9500 . ? O3 H3O 0.92(3) . ? O4 H4O 0.90(3) . ? O5 H5O 0.98(4) . ? 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 O2B 0.94(3) 1.78(3) 2.668(2) 156(3) . yes O1B H2O O2A 0.86(3) 1.90(3) 2.700(2) 154(3) . yes O1B H2O O2B 0.86(3) 2.31(3) 2.736(2) 111(2) . yes O3 H3O O4 0.92(3) 1.92(3) 2.769(3) 154(3) 1_655 yes O4 H4O O2B 0.90(3) 1.69(3) 2.590(2) 175(3) 6_655 yes O5 H5O O2A 0.98(4) 1.67(4) 2.641(3) 172(3) . yes C5B H5B O3 0.95 2.57 3.258(3) 129.3 3_656 yes C6B H6E O1A 0.98 2.55 3.323(3) 135.7 8_557 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 -177.8(2) . . . . ? C7A C1A C2A O1A 2.6(3) . . . . ? N1A C1A C2A C3A 3.8(4) . . . . ? C7A C1A C2A C3A -175.8(2) . . . . ? O1A C2A C3A O2A -1.2(3) . . . . ? C1A C2A C3A O2A 177.2(2) . . . . ? O1A C2A C3A C4A 178.6(2) . . . . ? C1A C2A C3A C4A -3.0(3) . . . . ? O2A C3A C4A C5A -179.3(2) . . . . ? C2A C3A C4A C5A 0.9(3) . . . . ? C3A C4A C5A N1A 0.2(4) . . . . ? C4A C5A N1A C1A 0.5(4) . . . . ? C4A C5A N1A C6A 177.0(2) . . . . ? C2A C1A N1A C5A -2.5(3) . . . . ? C7A C1A N1A C5A 177.1(2) . . . . ? C2A C1A N1A C6A -178.9(2) . . . . ? C7A C1A N1A C6A 0.7(3) . . . . ? N1B C1B C2B O1B 179.5(2) . . . . ? C7B C1B C2B O1B -2.1(4) . . . . ? N1B C1B C2B C3B 0.4(4) . . . . ? C7B C1B C2B C3B 178.9(2) . . . . ? O1B C2B C3B O2B -0.5(4) . . . . ? C1B C2B C3B O2B 178.5(2) . . . . ? O1B C2B C3B C4B 178.3(2) . . . . ? C1B C2B C3B C4B -2.7(4) . . . . ? O2B C3B C4B C5B -179.2(2) . . . . ? C2B C3B C4B C5B 2.1(4) . . . . ? C3B C4B C5B N1B 0.7(4) . . . . ? C4B C5B N1B C1B -3.2(4) . . . . ? C4B C5B N1B C6B 176.1(2) . . . . ? C2B C1B N1B C5B 2.5(4) . . . . ? C7B C1B N1B C5B -176.0(2) . . . . ? C2B C1B N1B C6B -176.8(2) . . . . ? C7B C1B N1B C6B 4.7(3) . . . . ? O3 C8 C9 C10 179.9(2) . . . . ? C13 C8 C9 C10 1.7(4) . . . . ? C8 C9 C10 O4 177.9(2) . . . . ? C8 C9 C10 C11 -1.9(4) . . . . ? O4 C10 C11 C12 -179.2(2) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C10 C11 C12 O5 -179.4(2) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? O3 C8 C13 C12 -178.3(2) . . . . ? C9 C8 C13 C12 -0.2(4) . . . . ? O5 C12 C13 C8 179.1(2) . . . . ? C11 C12 C13 C8 -1.1(4) . . . . ? _cod_database_fobs_code 2022896