#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022888.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_2022888 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' _chemical_formula_sum 'C7 H9 N O2' _chemical_formula_weight 139.15 _chemical_name_common 'Deferiprone form IV' _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 16 _cell_length_a 13.70079(19) _cell_length_b 7.16238(10) _cell_length_c 25.8688(4) _cell_measurement_reflns_used 9953 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.56 _cell_measurement_theta_min 2.15 _cell_volume 2538.51(6) _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 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.0329 _diffrn_reflns_av_unetI/netI 0.0350 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 18090 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.568 _diffrn_reflns_theta_min 2.165 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.456 _exptl_crystal_description block _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.160 _refine_diff_density_max 0.467 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 193 _refine_ls_number_reflns 3892 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0415 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+1.1028P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1098 _refine_ls_wR_factor_ref 0.1167 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3243 _reflns_number_total 3892 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block Id _cod_database_code 2022888 _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 0.966 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; TITL KA867_0m_a.res in Pbca KA867_0m.res created by SHELXL-2018/3 at 14:44:19 on 07-Jan-2020 CELL 0.71073 13.70079 7.16238 25.86883 90.000 90.000 90.000 ZERR 16.000 0.00019 0.00010 0.00037 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O UNIT 112 144 16 32 L.S. 10 BOND $H LIST 6 EQIV $1 x-1/2, -y+3/2, -z+1 EQIV $2 -x+1/2, y+1/2, z EQIV $3 x+1/2, y, -z+1/2 EQIV $4 -x+3/2, y-1/2, z HTAB O1A O2B HTAB O1B O2A HTAB C6A O2A_$1 HTAB C7A O2B_$2 HTAB C6B O2B_$3 HTAB C7B O2A_$4 TEMP -173 SIZE 0.32 0.28 0.16 ACTA FMAP 2 PLAN 5 WGHT 0.057200 1.102800 FVAR 0.40948 C1A 1 0.217285 0.626771 0.401353 11.00000 0.01006 0.00933 = 0.00921 -0.00002 0.00030 0.00022 C2A 1 0.316524 0.617785 0.394062 11.00000 0.01042 0.01099 = 0.00825 -0.00041 0.00093 0.00021 C3A 1 0.385159 0.666710 0.433945 11.00000 0.00973 0.01080 = 0.01049 -0.00116 0.00039 -0.00055 C4A 1 0.342094 0.719395 0.481931 11.00000 0.01131 0.01666 = 0.00950 -0.00286 -0.00014 -0.00098 AFIX 43 H4A 2 0.383001 0.748526 0.510465 11.00000 -1.20000 AFIX 0 C5A 1 0.243231 0.728773 0.487652 11.00000 0.01191 0.01471 = 0.00952 -0.00220 0.00153 -0.00116 AFIX 43 H5A 2 0.216874 0.767039 0.519925 11.00000 -1.20000 AFIX 0 C6A 1 0.075953 0.696112 0.457481 11.00000 0.00723 0.01934 = 0.01632 -0.00129 0.00250 0.00053 AFIX 137 H6AA 2 0.046317 0.778195 0.431553 11.00000 -1.50000 H6AB 2 0.063665 0.746489 0.492097 11.00000 -1.50000 H6AC 2 0.047350 0.571088 0.454761 11.00000 -1.50000 AFIX 0 C7A 1 0.145800 0.576424 0.359753 11.00000 0.01147 0.01473 = 0.01151 -0.00065 -0.00282 0.00035 AFIX 137 H7AA 2 0.107538 0.686930 0.350352 11.00000 -1.50000 H7AB 2 0.101953 0.478425 0.372389 11.00000 -1.50000 H7AC 2 0.181177 0.531003 0.329324 11.00000 -1.50000 AFIX 0 O1A 4 0.351655 0.563751 0.346995 11.00000 0.00997 0.02081 = 0.00953 -0.00438 0.00147 0.00182 H1O 2 0.416037 0.541430 0.349731 11.00000 0.03563 O2A 4 0.476351 0.664020 0.425406 11.00000 0.00760 0.02121 = 0.01585 -0.00489 0.00190 -0.00024 N1A 3 0.181696 0.684964 0.448535 11.00000 0.00768 0.01251 = 0.01029 -0.00107 0.00159 -0.00023 MOLE 2 C1B 1 0.785984 0.461774 0.349633 11.00000 0.01042 0.00940 = 0.00948 -0.00017 -0.00018 0.00084 C2B 1 0.686622 0.470542 0.356682 11.00000 0.01021 0.01049 = 0.00825 -0.00103 0.00067 0.00015 C3B 1 0.618271 0.413063 0.317364 11.00000 0.00980 0.01065 = 0.00973 0.00054 -0.00011 0.00029 C4B 1 0.661770 0.353136 0.270167 11.00000 0.01172 0.01345 = 0.00865 -0.00116 -0.00044 0.00037 AFIX 43 H4B 2 0.621243 0.313886 0.242421 11.00000 -1.20000 AFIX 0 C5B 1 0.760715 0.351230 0.264188 11.00000 0.01280 0.01331 = 0.00919 -0.00006 0.00085 0.00102 AFIX 43 H5B 2 0.787378 0.312561 0.232023 11.00000 -1.20000 AFIX 0 C6B 1 0.927917 0.398287 0.293395 11.00000 0.00815 0.02035 = 0.01632 -0.00011 0.00323 0.00161 AFIX 137 H6BA 2 0.940519 0.364649 0.257286 11.00000 -1.50000 H6BB 2 0.958114 0.305606 0.316218 11.00000 -1.50000 H6BC 2 0.955687 0.521705 0.300548 11.00000 -1.50000 AFIX 0 C7B 1 0.856820 0.511449 0.391610 11.00000 0.00991 0.01532 = 0.01273 -0.00131 -0.00261 0.00048 AFIX 137 H7BA 2 0.898474 0.403569 0.399113 11.00000 -1.50000 H7BB 2 0.820857 0.546837 0.422856 11.00000 -1.50000 H7BC 2 0.897432 0.616411 0.380298 11.00000 -1.50000 AFIX 0 O1B 4 0.651589 0.529545 0.403103 11.00000 0.00920 0.02113 = 0.00972 -0.00448 0.00119 0.00183 H2O 2 0.585783 0.546598 0.401669 11.00000 0.04259 O2B 4 0.527021 0.414367 0.326167 11.00000 0.00777 0.01923 = 0.01422 -0.00286 0.00054 -0.00037 N1B 3 0.822008 0.402642 0.302599 11.00000 0.00802 0.01278 = 0.01032 0.00061 0.00128 0.00031 HKLF 4 REM KA867_0m_a.res in Pbca REM wR2 = 0.1167, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0415 for 3243 Fo > 4sig(Fo) and 0.0519 for all 3892 data REM 193 parameters refined using 0 restraints END WGHT 0.0572 1.1028 REM Highest difference peak 0.467, deepest hole -0.292, 1-sigma level 0.067 Q1 1 0.6417 0.3897 0.2920 11.00000 0.05 0.47 Q2 1 0.3614 0.6874 0.4584 11.00000 0.05 0.42 Q3 1 0.3483 0.6507 0.4135 11.00000 0.05 0.42 Q4 1 0.6556 0.4357 0.3365 11.00000 0.05 0.38 Q5 1 0.2635 0.6602 0.3922 11.00000 0.05 0.36 ; _shelx_res_checksum 2812 _shelx_hkl_file ; 0 1 0 -0.06 0.14 0 -1 0 -0.03 0.10 0 -1 0 0.13 0.15 0 1 0 -0.05 0.10 0 -2 0 1067.57 54.22 0 2 0 1154.18 54.40 0 -2 0 1004.59 54.36 0 -3 0 -0.08 0.26 0 -3 0 -0.25 0.52 0 -4 0 634.81 33.21 0 -4 0 678.38 33.59 0 -5 0 0.47 0.75 0 -6 0 2.31 0.84 0 -7 0 0.86 1.13 0 -8 0 16.49 2.34 0 -9 0 1.28 1.34 0 -10 0 1.17 1.54 -1 -1 0 -0.02 0.21 1 1 0 -0.25 0.20 -1 1 0 0.07 0.07 -1 -3 0 -0.04 0.35 -1 -3 0 0.13 0.41 1 -3 0 0.20 0.41 1 -3 0 -0.06 0.20 1 -4 0 -0.87 0.76 -1 -4 0 -1.12 0.72 1 -4 0 0.08 0.29 1 -5 0 -0.37 0.34 -1 -5 0 0.33 0.73 1 -5 0 -0.09 0.71 -1 -6 0 0.35 0.66 1 -6 0 0.35 0.71 1 -7 0 -0.86 1.17 -1 -7 0 0.93 1.17 -1 -8 0 0.54 1.06 1 -8 0 0.74 1.44 1 -9 0 -0.68 1.77 -1 -9 0 -0.55 1.76 1 -10 0 -1.13 1.97 -1 -10 0 -0.82 1.98 2 -1 0 122.00 6.14 2 1 0 118.64 6.13 -2 1 0 124.67 6.14 -2 -1 0 114.68 6.14 2 -1 0 116.84 6.06 -2 1 0 118.40 6.05 2 -2 0 132.39 7.18 -2 2 0 147.03 7.21 2 -2 0 135.98 6.96 -2 -2 0 137.71 7.19 -2 2 0 137.05 6.96 2 2 0 134.83 7.18 -2 -3 0 32.33 2.20 -2 -3 0 36.36 2.15 2 -3 0 36.35 1.88 -2 3 0 36.62 1.93 2 -3 0 37.90 2.30 2 -4 0 106.81 5.23 2 -4 0 99.51 5.69 -2 -4 0 98.50 5.68 -2 -5 0 8.89 1.16 2 -5 0 10.04 1.39 2 -5 0 11.85 0.76 -2 -6 0 10.87 1.56 2 -6 0 9.48 1.54 -2 -7 0 -0.67 1.11 2 -7 0 0.51 1.26 2 -8 0 82.45 5.88 -2 -8 0 105.51 6.18 -2 -8 0 99.33 5.61 2 -9 0 39.80 3.74 -2 -9 0 38.43 3.73 2 -10 0 36.31 3.76 -2 -10 0 28.59 3.59 -3 0 0 -0.13 0.34 3 -1 0 0.09 0.25 -3 -1 0 -0.03 0.26 3 -1 0 0.27 0.27 3 1 0 -0.21 0.24 -3 1 0 0.11 0.21 -3 1 0 0.08 0.25 3 -2 0 0.04 0.35 3 -2 0 -0.02 0.18 -3 2 0 0.18 0.12 -3 -2 0 0.10 0.37 3 2 0 0.11 0.39 -3 2 0 -0.40 0.34 -3 3 0 0.11 0.18 -3 -3 0 0.01 0.56 3 -3 0 0.19 0.54 3 -3 0 0.25 0.20 3 -4 0 0.00 0.20 -3 -4 0 -0.01 0.78 3 -4 0 -0.59 0.77 3 -5 0 0.17 0.25 3 -5 0 0.24 0.75 -3 -5 0 -0.36 0.72 -3 -6 0 -0.07 0.90 3 -6 0 -0.46 0.90 3 -7 0 -1.37 1.09 -3 -7 0 0.28 0.84 3 -8 0 1.48 1.52 -3 -8 0 3.70 1.27 -3 -8 0 -0.64 1.35 -3 -9 0 -2.30 1.62 3 -9 0 1.72 1.81 3 -10 0 0.43 2.02 -3 -10 0 -1.82 1.40 4 0 0 2155.35 111.50 -4 0 0 2181.05 111.62 4 -1 0 40.98 2.27 -4 1 0 42.67 2.28 -4 1 0 39.41 2.30 4 1 0 40.56 2.27 -4 -1 0 48.18 2.27 4 -2 0 1259.13 65.76 -4 -2 0 1328.29 65.90 4 -2 0 1307.06 65.90 4 2 0 1308.42 65.90 -4 2 0 1319.49 65.90 -4 3 0 226.48 11.81 4 -3 0 229.18 12.14 4 -3 0 229.61 11.84 -4 -3 0 249.10 12.15 -4 -4 0 123.40 6.10 4 -4 0 103.94 5.56 -4 4 0 102.10 5.56 4 -4 0 108.58 6.08 -4 -5 0 7.29 1.25 4 -5 0 10.48 0.69 4 -5 0 6.48 1.24 4 -6 0 9.75 1.57 -4 -6 0 8.41 1.42 -4 -7 0 19.83 2.19 4 -7 0 17.02 1.94 -4 -8 0 66.08 4.22 -4 -8 0 58.19 4.28 4 -8 0 53.20 4.06 4 -9 0 21.13 2.99 -4 -9 0 28.22 3.17 4 -10 0 44.29 4.31 -4 -10 0 52.08 4.36 -5 0 0 2.24 1.95 5 0 0 3.45 1.97 5 1 0 0.01 0.24 -5 1 0 -0.07 0.30 -5 -1 0 0.04 0.24 -5 1 0 0.16 0.24 5 -1 0 -0.09 0.22 -5 -2 0 0.35 0.36 -5 2 0 0.21 0.25 5 -2 0 0.24 0.37 5 -2 0 0.23 0.41 -5 2 0 -0.03 0.37 5 2 0 0.19 0.41 -5 3 0 -0.04 0.16 5 -3 0 -0.16 0.49 5 -3 0 0.25 0.35 -5 -3 0 -0.28 0.48 -5 -4 0 0.36 0.79 -5 4 0 0.04 0.20 5 -4 0 0.48 0.33 5 -4 0 -0.32 0.81 -5 -5 0 -0.27 0.72 5 -5 0 0.36 0.78 -5 -6 0 0.54 0.93 5 -6 0 -0.24 0.97 -5 -7 0 0.87 1.22 -5 -7 0 0.67 1.18 5 -7 0 -1.51 1.14 5 -8 0 0.04 1.44 -5 -8 0 -0.69 1.49 -5 -8 0 0.26 1.45 5 -9 0 -2.52 1.75 -5 -9 0 3.23 1.89 -6 0 0 3881.26 195.65 -6 -1 0 1175.59 60.28 6 1 0 1218.31 60.27 6 -1 0 1184.18 60.26 -6 1 0 1159.89 60.42 -6 1 0 1240.28 60.27 -6 -2 0 1290.95 68.05 6 -2 0 1337.88 68.05 -6 2 0 1451.75 68.08 -6 2 0 1263.22 67.97 6 2 0 1393.96 68.06 -6 -3 0 0.91 0.64 -6 3 0 0.60 0.23 6 -3 0 1.15 0.56 -6 4 0 0.41 0.21 6 -4 0 0.17 0.86 -6 -4 0 1.36 1.05 6 -5 0 3.40 0.96 -6 -5 0 3.70 0.94 6 -6 0 2.68 1.15 -6 -6 0 1.10 0.97 -6 -7 0 2.82 1.38 6 -7 0 0.37 0.98 -6 -7 0 3.04 1.30 -6 -8 0 9.74 2.04 6 -8 0 13.93 2.11 -6 -8 0 8.88 2.03 -6 -9 0 0.27 1.92 -6 -9 0 -3.71 2.57 6 -9 0 0.28 1.90 -7 0 0 9.33 3.34 7 0 0 11.33 3.21 7 1 0 -0.33 0.20 -7 -1 0 0.27 0.22 -7 1 0 -0.35 0.21 -7 1 0 0.09 0.45 -7 -1 0 0.45 0.70 -7 2 0 -0.08 0.47 -7 -2 0 -0.37 0.39 -7 2 0 0.18 0.40 7 2 0 0.21 0.49 7 -2 0 -0.63 0.39 -7 -3 0 -1.18 0.55 7 -3 0 -0.38 0.57 -7 3 0 0.00 0.25 -7 4 0 0.30 0.22 7 -4 0 0.45 0.87 -7 -5 0 -0.01 0.74 7 -5 0 -0.36 0.91 -7 -6 0 -1.14 0.87 -7 -6 0 -0.88 1.22 7 -6 0 -0.25 0.96 -7 -7 0 -0.11 1.12 7 -7 0 -0.32 1.28 -7 -7 0 0.66 1.42 -7 -8 0 4.09 1.75 -7 -8 0 0.72 1.84 7 -8 0 0.57 1.56 7 -9 0 1.49 1.87 -7 -9 0 -1.94 2.15 -7 -9 0 0.87 1.93 -8 0 0 37.42 2.45 -8 1 0 1464.48 78.99 -8 1 0 1601.23 79.34 8 1 0 1642.10 79.00 -8 2 0 2.00 0.52 -8 -2 0 1.61 0.79 -8 -2 0 1.56 0.45 -8 2 0 1.45 0.53 8 -2 0 1.31 0.44 8 2 0 1.55 0.52 8 -3 0 118.45 6.34 -8 -3 0 117.48 6.37 -8 3 0 119.28 6.17 8 -4 0 23.01 2.04 -8 4 0 27.53 1.47 -8 -5 0 23.86 2.45 -8 -5 0 24.72 2.03 8 -5 0 27.34 2.16 8 -6 0 -1.70 0.92 -8 -6 0 1.84 0.98 -8 -6 0 0.63 1.34 8 -7 0 1.25 1.30 -8 -7 0 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1.83 -9 1 28 6.31 1.25 9 1 -28 5.24 1.41 -9 -1 -28 4.96 1.60 -9 2 -28 19.45 2.20 -9 -2 28 17.51 2.17 9 2 28 24.57 3.07 9 -2 -28 21.44 2.82 9 2 -28 20.50 2.56 -9 2 28 24.71 2.25 -9 -2 -28 24.78 2.77 9 3 28 11.03 2.36 -9 3 -28 19.86 2.09 9 -3 -28 16.45 2.63 -9 -3 28 18.27 2.31 9 3 -28 18.53 2.12 -9 -3 -28 17.38 2.54 -9 3 28 13.23 2.00 9 4 28 6.03 1.98 9 -4 -28 6.46 2.40 -9 -4 28 6.14 1.61 -9 4 28 4.92 1.40 -9 -4 -28 6.72 2.14 10 0 -28 124.53 7.40 -10 0 -28 120.13 7.29 10 0 28 128.57 7.73 -10 0 28 130.08 7.22 10 1 28 31.16 3.51 10 -1 -28 34.14 3.22 -10 1 -28 31.65 2.75 -10 -1 28 29.81 2.65 10 1 -28 30.42 2.95 -10 1 28 31.09 2.64 10 -1 28 28.49 3.40 -10 -1 -28 34.44 3.03 10 2 28 36.98 3.82 -10 -2 28 29.03 2.75 -10 2 -28 33.87 2.85 10 -2 -28 30.52 3.58 -10 2 28 32.06 2.68 10 2 -28 30.33 2.98 -10 -2 -28 37.69 3.28 -10 3 -28 5.73 1.45 10 -3 -28 11.30 2.25 -10 -3 28 7.87 1.59 10 3 28 5.42 2.10 -10 -3 -28 4.18 2.10 10 3 -28 7.74 1.74 -10 3 28 6.45 1.40 -10 -4 28 3.43 1.63 -10 4 -28 3.78 1.37 10 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47.30 3.68 2 -3 29 41.72 3.00 -2 3 29 43.09 3.21 -2 -3 -29 42.35 3.61 2 -4 -29 1.42 1.74 2 4 29 0.02 1.26 -2 -4 -29 1.36 1.69 -2 4 29 0.52 1.20 2 -5 -29 29.94 3.13 2 5 29 34.13 3.19 -2 -5 -29 32.27 3.20 -2 5 29 36.02 3.11 2 6 29 27.43 3.33 2 -6 -29 40.63 3.91 -2 6 29 29.21 3.23 -2 -6 -29 34.39 3.80 -3 0 -29 4.76 1.23 3 0 -29 1.56 1.05 -3 0 29 1.11 0.91 3 0 29 0.55 0.96 -3 -1 29 31.07 2.44 3 -1 -29 32.16 2.77 3 1 29 34.57 2.73 -3 1 -29 31.63 2.58 3 -1 29 35.13 2.61 3 1 -29 33.57 2.62 -3 -1 -29 33.89 2.79 -3 1 29 35.83 2.59 -3 2 -29 10.63 1.55 3 -2 -29 11.12 1.88 3 2 29 15.46 2.05 -3 -2 29 11.20 1.54 3 -2 29 12.64 1.69 -3 2 29 13.71 1.74 -3 -2 -29 13.91 2.01 3 2 -29 12.73 1.68 3 3 29 0.29 1.18 -3 -3 29 1.65 0.95 3 -3 -29 -0.66 1.10 -3 -3 -29 1.94 1.54 -3 3 29 0.43 1.10 3 -3 29 0.54 1.09 -3 -4 29 0.68 1.02 3 4 29 1.70 1.29 3 -4 -29 -0.17 1.30 -3 4 29 1.73 1.29 -3 -4 -29 1.17 1.65 3 5 29 29.17 3.00 3 -5 -29 22.29 3.35 -3 -5 29 27.81 2.39 -3 5 29 29.08 2.77 -3 -5 -29 23.93 2.87 3 -6 -29 9.64 2.61 3 6 29 10.32 2.15 -3 -6 -29 4.60 2.29 -3 6 29 10.77 1.93 4 0 -29 0.65 1.05 -4 0 29 0.42 0.87 4 0 29 -1.02 1.19 -4 0 -29 2.63 1.17 -4 -1 29 28.68 2.35 4 -1 -29 30.23 2.64 -4 1 -29 29.52 2.48 4 1 29 29.89 2.73 -4 -1 -29 34.19 2.71 4 1 -29 31.16 2.51 -4 1 29 30.21 2.42 4 -1 29 28.01 2.63 4 -2 -29 5.76 1.59 4 2 29 7.24 1.58 -4 2 -29 6.89 1.28 -4 -2 29 6.47 1.23 -4 -2 -29 6.29 1.58 4 2 -29 6.17 1.28 -4 2 29 5.43 1.25 4 -2 29 6.60 1.33 4 -3 -29 2.22 1.57 -4 -3 29 3.28 1.05 4 3 29 1.13 1.39 -4 3 29 1.67 1.07 -4 -3 -29 1.25 1.53 4 -3 29 1.45 1.12 4 -4 -29 29.55 3.01 4 4 29 33.06 3.14 -4 -4 29 31.19 2.58 -4 4 29 35.74 2.87 -4 -4 -29 32.61 3.38 -4 -5 29 7.20 1.54 4 5 29 4.65 1.75 4 -5 -29 6.17 2.20 -4 -5 -29 7.15 2.22 -4 5 29 6.25 1.46 4 6 29 -0.63 1.95 4 -6 -29 4.96 1.84 -4 -6 -29 -0.99 2.17 -4 6 29 -1.60 1.63 5 0 -29 -0.55 1.01 -5 0 29 -1.73 0.87 -5 -1 29 123.06 7.16 5 -1 -29 130.18 7.46 5 1 29 127.13 7.49 -5 1 -29 128.11 7.32 -5 -1 -29 132.43 7.48 -5 1 29 124.09 7.22 5 1 -29 135.96 7.35 5 -1 29 127.27 7.33 -5 2 -29 160.51 8.59 5 -2 -29 139.69 8.72 -5 -2 29 160.99 8.50 5 2 29 170.14 8.96 -5 2 29 166.08 8.62 -5 -2 -29 140.90 8.75 5 2 -29 141.60 8.46 5 -2 29 157.93 8.61 5 -3 -29 2.75 1.67 -5 -3 29 1.32 1.11 5 3 29 2.94 1.57 5 -3 29 3.30 1.25 -5 3 29 2.62 1.11 -5 -3 -29 4.33 1.63 5 -4 -29 0.26 1.77 5 4 29 1.50 1.61 -5 -4 29 -0.69 1.11 -5 4 29 0.55 1.18 -5 -4 -29 2.51 1.82 5 5 29 6.49 2.01 -5 -5 29 7.23 1.60 5 -5 -29 10.52 2.43 -5 -5 -29 10.04 2.38 -5 5 29 8.17 1.74 6 0 -29 0.02 1.07 -6 0 29 -1.79 0.77 -6 0 -29 0.34 1.17 6 0 29 -0.26 1.16 6 1 29 0.33 1.31 -6 1 -29 -1.12 1.06 6 -1 -29 -1.03 1.16 -6 -1 -29 1.82 1.34 6 -1 29 0.37 1.29 6 1 -29 -0.36 1.05 -6 1 29 -0.48 0.97 6 2 29 42.30 3.52 -6 -2 29 42.97 3.01 -6 2 -29 46.74 3.09 6 -2 -29 41.15 3.36 6 2 -29 41.09 3.00 6 -2 29 35.91 3.23 -6 2 29 40.73 2.99 -6 -2 -29 41.01 3.39 6 -3 -29 71.71 4.94 -6 -3 29 65.01 4.29 -6 3 -29 66.93 4.29 6 3 29 70.23 4.88 -6 -3 -29 63.02 4.85 -6 3 29 72.76 4.43 6 3 -29 70.26 4.31 -6 -4 29 17.32 2.14 6 -4 -29 17.88 2.73 6 4 29 16.67 2.49 -6 -4 -29 18.66 2.70 -6 4 29 17.85 2.16 -6 -5 29 37.25 3.07 6 -5 -29 39.98 4.13 6 5 29 36.70 3.77 -6 5 29 34.90 3.20 -6 -5 -29 42.51 3.98 7 0 29 0.49 1.33 -7 0 -29 0.04 1.20 -7 0 29 2.09 1.02 7 0 -29 0.45 1.14 -7 -1 29 25.57 2.39 7 1 29 28.57 3.11 7 -1 -29 28.35 2.75 -7 1 -29 28.84 2.56 7 1 -29 30.28 2.75 -7 -1 -29 26.77 2.71 7 -1 29 30.93 3.36 -7 1 29 29.35 2.43 7 -2 -29 1.06 1.53 -7 -2 29 1.54 1.16 -7 2 -29 0.64 1.20 7 2 29 -0.41 1.55 -7 2 29 1.44 1.07 -7 -2 -29 3.75 1.50 7 -2 29 2.54 1.45 7 2 -29 4.16 1.31 7 3 29 50.89 4.14 -7 -3 29 47.14 3.40 7 -3 -29 48.31 4.06 -7 3 -29 47.91 3.35 7 3 -29 47.88 3.47 -7 3 29 49.05 3.42 -7 -3 -29 43.40 3.92 -7 -4 29 115.50 6.86 7 4 29 120.62 7.51 7 -4 -29 116.59 7.59 -7 4 29 116.83 6.90 -7 -4 -29 124.84 7.63 7 -5 -29 19.63 3.22 -7 -5 29 20.55 2.68 7 5 29 22.39 3.24 -7 5 29 21.51 2.72 -7 -5 -29 23.44 3.23 -8 0 29 0.78 1.04 8 0 -29 -1.73 1.28 8 0 29 -1.36 1.54 -8 0 -29 -1.50 1.23 8 1 29 32.84 3.25 -8 1 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1.15 9 -4 -29 19.65 2.95 9 4 29 19.23 2.71 -9 -4 29 13.36 2.04 -9 4 -29 13.75 2.01 9 4 -29 12.99 2.01 -9 -4 -29 18.13 3.00 -9 4 29 13.24 1.90 10 0 29 -2.19 2.02 -10 0 29 -0.49 1.08 10 0 -29 -0.67 1.76 -10 0 -29 1.26 1.46 -10 1 -29 27.84 2.67 10 1 29 25.15 3.47 10 -1 -29 27.28 2.84 -10 -1 29 26.32 2.47 10 1 -29 26.45 2.92 -10 1 29 23.09 2.28 10 -1 29 21.96 2.79 -10 -1 -29 29.67 2.90 -10 2 -29 78.29 5.02 10 -2 -29 82.54 5.60 -10 -2 29 66.35 4.87 10 2 29 78.12 5.64 10 2 -29 80.79 4.99 -10 -2 -29 89.53 5.70 -10 2 29 79.23 4.90 -10 -3 29 3.82 1.46 10 -3 -29 8.32 2.21 10 3 29 5.04 2.24 -10 3 -29 5.56 1.56 -10 -3 -29 6.21 2.16 -10 3 29 2.27 1.36 10 3 -29 4.98 1.48 11 0 29 0.86 2.19 -11 0 29 1.55 1.24 -11 0 -29 -2.11 1.49 -11 -1 29 92.01 5.61 11 1 29 83.99 6.46 -11 -1 -29 97.59 6.03 -11 1 29 92.35 5.58 -11 2 -29 55.45 4.21 -11 -2 29 66.40 4.34 -11 -2 -29 64.80 4.66 -11 2 29 66.67 4.29 -12 0 29 0.97 1.33 -12 -1 29 128.20 7.53 -12 1 29 130.82 7.53 0 0 -30 9.53 1.59 0 0 30 9.89 1.40 0 1 -30 0.33 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2.09 -4 -5 -30 8.37 2.04 -4 5 30 15.04 2.01 5 0 30 4.84 1.42 -5 0 30 1.76 1.02 -5 0 -30 0.95 1.23 5 0 -30 2.71 1.31 -5 1 -30 28.74 2.56 5 -1 -30 29.15 2.78 5 1 30 27.26 2.78 -5 -1 30 31.83 2.45 5 1 -30 27.10 2.56 -5 1 30 29.26 2.43 -5 -1 -30 28.03 2.71 -5 2 -30 41.08 3.02 5 2 30 38.20 3.43 5 -2 -30 42.20 3.44 -5 -2 30 41.88 2.95 -5 2 30 39.09 3.02 5 -2 30 40.48 3.25 5 2 -30 40.77 3.02 -5 -2 -30 39.66 3.41 -5 3 -30 11.99 1.74 5 -3 -30 10.04 2.21 -5 -3 30 11.91 1.68 5 3 30 13.59 2.13 -5 3 30 16.55 2.01 -5 -3 -30 18.63 2.67 5 3 -30 14.52 1.85 5 4 30 165.91 9.54 5 -4 -30 177.53 9.82 -5 -4 30 165.82 9.05 -5 -4 -30 138.27 9.41 -5 4 30 168.13 9.21 5 -5 -30 93.43 6.48 5 5 30 91.41 6.18 -5 -5 30 87.76 5.52 -5 -5 -30 85.69 6.29 -5 5 30 93.96 5.82 6 0 30 1.68 1.34 6 0 -30 0.67 1.21 -6 0 30 0.42 1.11 -6 0 -30 -0.58 1.26 6 1 30 3.16 1.55 -6 -1 30 2.03 1.08 6 -1 -30 2.79 1.47 -6 1 -30 1.37 1.26 6 -1 30 1.10 1.44 -6 -1 -30 2.54 1.44 6 1 -30 2.17 1.30 -6 1 30 4.51 1.26 6 -2 -30 37.99 3.25 6 2 30 38.15 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-0.32 1.30 -1 -2 -35 -0.34 1.67 1 3 35 2.94 1.57 -1 3 -35 -2.47 1.25 -1 -3 35 1.15 1.47 1 -3 -35 2.97 2.04 -1 -3 -35 0.77 2.00 -1 3 35 2.36 1.44 1 3 -35 0.24 1.38 1 -3 35 -1.73 1.38 2 0 -35 -0.17 1.49 2 0 35 -1.89 1.44 -2 0 35 0.58 1.24 -2 0 -35 2.27 1.45 2 1 35 4.94 1.65 -2 -1 35 3.98 1.36 2 -1 -35 6.01 1.75 -2 1 -35 6.16 1.66 2 -1 35 3.23 1.74 2 1 -35 5.98 1.65 -2 1 35 3.35 1.45 -2 -1 -35 5.17 1.77 2 2 35 5.78 1.69 2 -2 -35 0.90 1.78 -2 2 -35 3.75 1.13 -2 -2 35 4.92 1.46 -2 -2 -35 6.87 1.85 2 2 -35 5.90 1.55 -2 2 35 3.18 1.41 2 -2 35 6.48 1.73 2 -3 -35 12.76 2.60 2 3 35 10.97 2.02 -2 -3 35 12.89 1.96 -2 3 -35 12.18 1.93 2 3 -35 14.88 2.15 -2 -3 -35 11.33 2.09 -2 3 35 11.76 1.87 3 0 -35 0.39 1.49 -3 0 35 0.29 1.20 -3 0 -35 1.55 1.48 3 0 35 0.02 1.53 -3 -1 35 64.38 4.16 -3 1 -35 52.77 4.16 3 -1 -35 69.21 4.60 3 1 35 56.26 4.34 -3 -1 -35 54.12 4.36 -3 1 35 58.56 4.06 3 1 -35 63.06 4.32 3 -1 35 54.07 4.43 -3 2 -35 1.95 1.11 3 2 35 -1.55 1.56 -3 -2 35 1.77 1.34 3 -2 -35 -1.93 1.65 3 -2 35 -1.13 1.65 -3 2 35 0.45 1.27 -3 -2 -35 0.69 1.66 3 2 -35 2.10 1.50 -4 0 35 2.79 1.34 -4 0 -35 1.67 1.48 4 0 -35 -0.20 1.54 4 0 35 -1.24 1.60 -4 -1 35 6.10 1.40 -4 1 -35 3.91 1.61 4 1 35 2.88 1.69 4 -1 -35 6.58 1.87 4 1 -35 5.26 1.62 4 -1 35 5.28 1.88 -4 -1 -35 8.85 1.66 -4 1 35 5.34 1.45 -4 -2 35 25.11 2.73 -4 2 -35 28.39 2.74 4 -2 -35 29.03 3.08 4 2 35 20.87 3.04 -4 -2 -35 33.14 3.18 4 2 -35 24.35 2.38 -4 2 35 25.12 2.70 4 -2 35 29.30 3.03 5 0 -35 -1.81 1.55 5 0 35 -0.33 1.78 -5 0 -35 2.21 1.57 -5 0 35 -0.87 1.22 5 1 35 41.06 3.64 -5 1 -35 31.38 3.21 5 -1 -35 36.92 3.63 -5 -1 35 38.79 3.14 -5 1 35 35.75 3.10 5 1 -35 38.03 3.37 5 -1 35 40.47 3.68 -5 -1 -35 40.51 3.51 -5 -2 35 44.79 3.44 5 2 35 42.80 3.94 5 -2 -35 41.47 4.08 -5 2 -35 46.89 3.67 -5 -2 -35 53.09 4.07 5 2 -35 47.89 3.70 -5 2 35 44.22 3.51 5 -2 35 45.55 5.32 -6 0 35 0.96 1.32 6 0 35 0.93 2.13 6 0 -35 -0.69 1.68 -6 0 -35 -1.64 1.54 6 1 35 -1.51 1.82 6 -1 -35 1.00 1.83 -6 -1 35 0.19 1.33 -6 1 -35 2.38 1.59 -6 -1 -35 0.29 1.81 6 1 -35 2.00 1.65 -6 1 35 0.97 1.27 6 -1 35 4.78 2.01 0 0 36 450.91 21.61 0 0 -36 364.92 21.57 0 -1 36 0.30 1.43 0 -1 -36 2.60 1.75 0 1 36 0.65 1.45 0 1 -36 -0.96 1.04 0 -2 36 8.04 1.81 0 2 -36 11.62 1.87 0 2 36 8.35 1.90 0 -2 -36 8.37 1.79 -1 0 36 193.38 10.92 1 0 -36 207.95 11.19 1 0 36 197.04 11.01 -1 0 -36 188.40 11.09 -1 -1 36 11.28 2.01 -1 1 -36 16.70 2.25 1 1 36 16.20 2.18 1 -1 -36 16.24 2.43 -1 -1 -36 14.09 2.24 1 1 -36 11.57 2.07 1 -1 36 14.73 2.12 -1 1 36 13.96 2.04 1 2 36 1.59 1.72 1 -2 -36 -4.32 1.72 -1 -2 36 0.27 1.43 -1 2 -36 0.46 1.40 -1 2 36 5.22 1.62 -1 -2 -36 -1.25 1.25 1 2 -36 2.84 1.62 1 -2 36 2.60 1.70 -2 0 -36 12.81 2.14 2 0 -36 13.69 2.19 2 0 36 14.76 2.17 -2 0 36 13.01 1.86 2 -1 -36 23.21 2.94 2 1 36 23.68 2.97 -2 1 -36 18.51 2.53 -2 -1 36 24.67 2.51 -2 -1 -36 28.23 2.99 -2 1 36 21.42 2.58 2 -1 36 28.03 3.07 2 1 -36 17.74 2.51 -2 -2 36 1.77 1.56 2 -2 -36 2.05 1.96 -2 2 -36 2.59 1.26 2 2 36 -2.56 1.50 2 -2 36 3.09 1.78 2 2 -36 -0.29 1.53 -2 -2 -36 2.22 1.91 -2 2 36 2.04 1.45 -3 0 36 10.10 1.71 3 0 -36 12.22 2.14 3 0 36 10.50 2.03 -3 0 -36 12.13 2.13 -3 1 -36 0.21 1.43 -3 -1 36 1.00 1.31 3 -1 -36 0.88 1.77 3 1 36 0.58 1.69 3 1 -36 1.62 1.58 -3 1 36 1.14 1.39 -3 -1 -36 0.67 1.68 3 -1 36 1.70 1.79 4 0 36 6.96 2.04 4 0 -36 4.04 1.78 -4 0 36 4.51 1.52 -4 0 -36 6.60 1.83 4 1 36 8.59 2.19 -4 1 -36 11.05 1.96 -4 -1 36 9.32 1.73 4 -1 -36 14.44 2.37 4 -1 36 13.37 2.32 -4 -1 -36 7.88 2.12 -4 1 36 9.46 1.69 4 1 -36 16.94 2.39 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 0.6863 _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 0.71073 7.167 13.712 25.875 89.967 90.024 90.012 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 82770 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -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 0.21728(7) 0.62677(14) 0.40135(3) 0.00954(18) Uani 1 1 d . . . . . C2A C 0.31652(7) 0.61778(14) 0.39406(3) 0.00989(19) Uani 1 1 d . . . . . C3A C 0.38516(7) 0.66671(14) 0.43395(4) 0.01034(19) Uani 1 1 d . . . . . C4A C 0.34209(8) 0.71939(16) 0.48193(4) 0.0125(2) Uani 1 1 d . . . . . H4A H 0.383001 0.748526 0.510465 0.015 Uiso 1 1 calc R U . . . C5A C 0.24323(8) 0.72877(15) 0.48765(4) 0.0120(2) Uani 1 1 d . . . . . H5A H 0.216874 0.767039 0.519925 0.014 Uiso 1 1 calc R U . . . C6A C 0.07595(7) 0.69611(16) 0.45748(4) 0.0143(2) Uani 1 1 d . . . . . H6AA H 0.046317 0.778195 0.431553 0.021 Uiso 1 1 calc R U . . . H6AB H 0.063665 0.746489 0.492097 0.021 Uiso 1 1 calc R U . . . H6AC H 0.047350 0.571088 0.454761 0.021 Uiso 1 1 calc R U . . . C7A C 0.14580(8) 0.57642(15) 0.35975(4) 0.0126(2) Uani 1 1 d . . . . . H7AA H 0.107538 0.686930 0.350352 0.019 Uiso 1 1 calc R U . . . H7AB H 0.101953 0.478425 0.372389 0.019 Uiso 1 1 calc R U . . . H7AC H 0.181177 0.531003 0.329324 0.019 Uiso 1 1 calc R U . . . O1A O 0.35166(6) 0.56375(11) 0.34700(3) 0.01343(17) Uani 1 1 d . . . . . H1O H 0.4160(13) 0.541(3) 0.3497(7) 0.036(5) Uiso 1 1 d . . . . . O2A O 0.47635(5) 0.66402(12) 0.42541(3) 0.01489(17) Uani 1 1 d . . . . . N1A N 0.18170(6) 0.68496(12) 0.44853(3) 0.01016(17) Uani 1 1 d . . . . . C1B C 0.78598(7) 0.46177(14) 0.34963(4) 0.00977(19) Uani 1 1 d . . . . . C2B C 0.68662(7) 0.47054(14) 0.35668(3) 0.00965(19) Uani 1 1 d . . . . . C3B C 0.61827(7) 0.41306(14) 0.31736(4) 0.01006(19) Uani 1 1 d . . . . . C4B C 0.66177(8) 0.35314(15) 0.27017(4) 0.01127(19) Uani 1 1 d . . . . . H4B H 0.621243 0.313886 0.242421 0.014 Uiso 1 1 calc R U . . . C5B C 0.76071(8) 0.35123(15) 0.26419(4) 0.01177(19) Uani 1 1 d . . . . . H5B H 0.787378 0.312561 0.232023 0.014 Uiso 1 1 calc R U . . . C6B C 0.92792(8) 0.39829(16) 0.29339(4) 0.0149(2) Uani 1 1 d . . . . . H6BA H 0.940519 0.364649 0.257286 0.022 Uiso 1 1 calc R U . . . H6BB H 0.958114 0.305606 0.316218 0.022 Uiso 1 1 calc R U . . . H6BC H 0.955687 0.521705 0.300548 0.022 Uiso 1 1 calc R U . . . C7B C 0.85682(8) 0.51145(15) 0.39161(4) 0.0127(2) Uani 1 1 d . . . . . H7BA H 0.898474 0.403569 0.399113 0.019 Uiso 1 1 calc R U . . . H7BB H 0.820857 0.546837 0.422856 0.019 Uiso 1 1 calc R U . . . H7BC H 0.897432 0.616411 0.380298 0.019 Uiso 1 1 calc R U . . . O1B O 0.65159(6) 0.52954(12) 0.40310(3) 0.01335(16) Uani 1 1 d . . . . . H2O H 0.5858(14) 0.547(3) 0.4017(7) 0.043(5) Uiso 1 1 d . . . . . O2B O 0.52702(5) 0.41437(11) 0.32617(3) 0.01374(17) Uani 1 1 d . . . . . N1B N 0.82201(6) 0.40264(12) 0.30260(3) 0.01037(18) Uani 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 0.0101(4) 0.0093(4) 0.0092(4) 0.0000(3) 0.0003(3) 0.0002(4) C2A 0.0104(4) 0.0110(4) 0.0083(4) -0.0004(3) 0.0009(3) 0.0002(4) C3A 0.0097(5) 0.0108(4) 0.0105(4) -0.0012(3) 0.0004(3) -0.0005(3) C4A 0.0113(5) 0.0167(5) 0.0095(4) -0.0029(3) -0.0001(3) -0.0010(4) C5A 0.0119(5) 0.0147(5) 0.0095(4) -0.0022(3) 0.0015(3) -0.0012(4) C6A 0.0072(4) 0.0193(5) 0.0163(4) -0.0013(4) 0.0025(3) 0.0005(4) C7A 0.0115(5) 0.0147(5) 0.0115(4) -0.0007(3) -0.0028(3) 0.0003(4) O1A 0.0100(4) 0.0208(4) 0.0095(3) -0.0044(3) 0.0015(2) 0.0018(3) O2A 0.0076(4) 0.0212(4) 0.0159(3) -0.0049(3) 0.0019(3) -0.0002(3) N1A 0.0077(4) 0.0125(4) 0.0103(3) -0.0011(3) 0.0016(3) -0.0002(3) C1B 0.0104(4) 0.0094(4) 0.0095(4) -0.0002(3) -0.0002(3) 0.0008(4) C2B 0.0102(4) 0.0105(4) 0.0082(4) -0.0010(3) 0.0007(3) 0.0002(3) C3B 0.0098(4) 0.0107(4) 0.0097(4) 0.0005(3) -0.0001(3) 0.0003(3) C4B 0.0117(5) 0.0134(5) 0.0087(4) -0.0012(3) -0.0004(3) 0.0004(4) C5B 0.0128(5) 0.0133(5) 0.0092(4) -0.0001(3) 0.0009(3) 0.0010(4) C6B 0.0082(4) 0.0203(5) 0.0163(4) -0.0001(4) 0.0032(3) 0.0016(4) C7B 0.0099(4) 0.0153(5) 0.0127(4) -0.0013(4) -0.0026(3) 0.0005(4) O1B 0.0092(3) 0.0211(4) 0.0097(3) -0.0045(3) 0.0012(2) 0.0018(3) O2B 0.0078(3) 0.0192(4) 0.0142(3) -0.0029(3) 0.0005(3) -0.0004(3) N1B 0.0080(4) 0.0128(4) 0.0103(3) 0.0006(3) 0.0013(3) 0.0003(3) 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 119.05(9) . . ? C2A C1A C7A 122.45(9) . . ? N1A C1A C7A 118.50(9) . . ? O1A C2A C1A 118.98(9) . . ? O1A C2A C3A 118.55(9) . . ? C1A C2A C3A 122.46(9) . . ? O2A C3A C4A 124.28(9) . . ? O2A C3A C2A 120.99(9) . . ? C4A C3A C2A 114.73(9) . . ? C5A C4A C3A 121.23(9) . . ? C5A C4A H4A 119.4 . . ? C3A C4A H4A 119.4 . . ? N1A C5A C4A 121.72(9) . . ? N1A C5A H5A 119.1 . . ? C4A C5A H5A 119.1 . . ? N1A C6A H6AA 109.5 . . ? N1A C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? N1A C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? C1A C7A H7AA 109.5 . . ? C1A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C1A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C2A O1A H1O 109.0(11) . . ? C5A N1A C1A 120.76(9) . . ? C5A N1A C6A 118.92(8) . . ? C1A N1A C6A 120.30(8) . . ? C2B C1B N1B 119.02(9) . . ? C2B C1B C7B 122.28(9) . . ? N1B C1B C7B 118.69(9) . . ? O1B C2B C1B 118.72(9) . . ? O1B C2B C3B 118.81(9) . . ? C1B C2B C3B 122.43(9) . . ? O2B C3B C4B 124.56(9) . . ? O2B C3B C2B 120.68(9) . . ? C4B C3B C2B 114.75(9) . . ? C5B C4B C3B 121.04(9) . . ? C5B C4B H4B 119.5 . . ? C3B C4B H4B 119.5 . . ? N1B C5B C4B 122.08(9) . . ? N1B C5B H5B 119.0 . . ? C4B C5B H5B 119.0 . . ? N1B C6B H6BA 109.5 . . ? N1B C6B H6BB 109.5 . . ? H6BA C6B H6BB 109.5 . . ? N1B C6B H6BC 109.5 . . ? H6BA C6B H6BC 109.5 . . ? H6BB C6B H6BC 109.5 . . ? C1B C7B H7BA 109.5 . . ? C1B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C1B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? C2B O1B H2O 110.8(11) . . ? C5B N1B C1B 120.63(9) . . ? C5B N1B C6B 119.21(8) . . ? C1B N1B C6B 120.15(8) . . ? 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 1.3742(14) . ? C1A N1A 1.3788(12) . ? C1A C7A 1.4991(13) . ? C2A O1A 1.3652(11) . ? C2A C3A 1.4393(13) . ? C3A O2A 1.2689(12) . ? C3A C4A 1.4253(13) . ? C4A C5A 1.3642(15) . ? C4A H4A 0.9500 . ? C5A N1A 1.3540(13) . ? C5A H5A 0.9500 . ? C6A N1A 1.4693(13) . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? O1A H1O 0.899(18) . ? C1B C2B 1.3749(14) . ? C1B N1B 1.3796(12) . ? C1B C7B 1.4992(13) . ? C2B O1B 1.3605(11) . ? C2B C3B 1.4425(13) . ? C3B O2B 1.2708(12) . ? C3B C4B 1.4248(13) . ? C4B C5B 1.3645(15) . ? C4B H4B 0.9500 . ? C5B N1B 1.3521(13) . ? C5B H5B 0.9500 . ? C6B N1B 1.4708(13) . ? C6B H6BA 0.9800 . ? C6B H6BB 0.9800 . ? C6B H6BC 0.9800 . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? O1B H2O 0.911(19) . ? 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 0.899(18) 1.874(18) 2.6847(11) 149(2) . yes O1B H2O O2A 0.911(19) 1.825(19) 2.6504(11) 150(2) . yes C6A H6AB O2A 0.98 2.53 3.4705(12) 161 4_466 yes C7A H7AA O2B 0.98 2.54 3.4957(13) 165 8_665 yes C6B H6BA O2B 0.98 2.49 3.3798(12) 151 6_656 yes C7B H7BA O2A 0.98 2.52 3.4901(13) 171 8_755 yes _cod_database_fobs_code 2022888