#------------------------------------------------------------------------------ #$Date: 2023-10-10 04:19:25 +0200 (Tue, 10 Oct 2023) $ #$Revision: 286864 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022890.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_2022890 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), 3(C6 H6 O2)' _chemical_formula_sum 'C32 H36 N2 O10' _chemical_formula_weight 608.63 _chemical_name_systematic 'Deferiprone-Catechol (2:3) cocrystal' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90.927(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.9488(17) _cell_length_b 9.982(2) _cell_length_c 20.881(5) _cell_measurement_reflns_used 9899 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.58 _cell_measurement_theta_min 2.83 _cell_volume 1448.2(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 0.995 _diffrn_measured_fraction_theta_max 0.990 _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 0.0490 _diffrn_reflns_av_unetI/netI 0.0435 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 34096 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.604 _diffrn_reflns_theta_min 2.261 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2016' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.396 _exptl_crystal_description block _exptl_crystal_F_000 644 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.409 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.088 _refine_ls_abs_structure_details ; Flack x determined using 3652 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.3(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 458 _refine_ls_number_reflns 8799 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.112 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0616 _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^)+(0.0525P)^2^+2.4574P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1666 _refine_ls_wR_factor_ref 0.1679 _reflns_Friedel_coverage 0.891 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.979 _reflns_number_gt 8447 _reflns_number_total 8799 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lo5093sup1.cif _cod_data_source_block KA1036_0m_Def-cat_2_3 _cod_original_cell_volume 1448.3(6) _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2022890 _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 0.967 _shelx_estimated_absorpt_t_max 0.978 _shelx_res_file ; TITL KA1036_0m_a.res in P2(1) KA1036_0m.res created by SHELXL-2018/3 at 15:50:19 on 09-Dec-2020 CELL 0.71073 6.9488 9.9824 20.8815 90.000 90.927 90.000 ZERR 2.00 0.0017 0.0021 0.0052 0.000 0.007 0.000 LATT -1 SYMM -x, y+1/2, -z SFAC C H N O UNIT 64 72 4 20 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 10 ACTA BOND $H OMIT -1 1 4 OMIT -1 1 3 OMIT -1 -3 7 OMIT -1 3 7 OMIT 1 -1 4 OMIT 2 -2 10 OMIT 2 2 10 FMAP 2 PLAN 5 SIZE 0.32 0.28 0.21 CONF EQIV $1 x-1, y, z EQIV $2 x+1, y, z HTAB O1A O2B HTAB O1B O2A HTAB O3A O4A HTAB O3A O4B HTAB O4A O2B_$1 HTAB O3B O4A HTAB O3B O4B HTAB O4B O2B HTAB O3C O2A HTAB O3' O2A HTAB O4' O3' HTAB C5A O1A_$1 HTAB C4B O4A_$2 HTAB C5B O1B_$2 HTAB C10C O4C_$1 TEMP -173.0 WGHT 0.052500 2.457400 FVAR 0.90650 0.57776 MOLE 1 C1A 1 0.271947 0.649246 0.139907 11.00000 0.01508 0.02077 = 0.01232 -0.00115 -0.00086 0.00046 C2A 1 0.356574 0.541572 0.169572 11.00000 0.01342 0.01904 = 0.01123 -0.00089 -0.00131 -0.00179 C3A 1 0.253963 0.420275 0.181817 11.00000 0.01752 0.02086 = 0.00846 -0.00006 -0.00016 -0.00513 C4A 1 0.057449 0.420205 0.163674 11.00000 0.01642 0.03242 = 0.01858 0.00035 -0.00047 -0.01208 AFIX 43 H4A 2 -0.018600 0.342786 0.170995 11.00000 -1.20000 AFIX 0 C5A 1 -0.023750 0.529610 0.135898 11.00000 0.01142 0.04253 = 0.01949 -0.00039 -0.00138 -0.00358 AFIX 43 H5A 2 -0.157042 0.528008 0.125068 11.00000 -1.20000 AFIX 0 C6A 1 -0.014470 0.756089 0.091668 11.00000 0.02771 0.03946 = 0.02466 0.00514 -0.00634 0.01510 AFIX 137 H6AA 2 0.057348 0.781428 0.053522 11.00000 -1.50000 H6AB 2 -0.017871 0.831972 0.121405 11.00000 -1.50000 H6AC 2 -0.146191 0.731242 0.079099 11.00000 -1.50000 AFIX 0 C7A 1 0.384298 0.772342 0.122925 11.00000 0.02403 0.02033 = 0.01770 0.00341 -0.00205 0.00036 AFIX 137 H7AA 2 0.398524 0.776876 0.076360 11.00000 -1.50000 H7AB 2 0.511831 0.768415 0.143572 11.00000 -1.50000 H7AC 2 0.315875 0.852083 0.137759 11.00000 -1.50000 AFIX 0 N1A 3 0.080303 0.641745 0.123077 11.00000 0.01432 0.03205 = 0.01522 0.00351 -0.00203 0.00591 O1A 4 0.548073 0.548240 0.184411 11.00000 0.01299 0.01996 = 0.01733 0.00625 -0.00529 -0.00449 AFIX 147 H1A 2 0.575399 0.490481 0.212363 11.00000 -1.50000 AFIX 0 O2A 4 0.343429 0.317448 0.205744 11.00000 0.02527 0.01842 = 0.01504 0.00167 -0.00400 -0.00480 MOLE 2 C1B 1 0.709271 0.115105 0.365934 11.00000 0.01159 0.01004 = 0.01110 0.00096 -0.00069 -0.00072 C2B 1 0.645770 0.229822 0.333673 11.00000 0.00969 0.00936 = 0.01347 -0.00019 -0.00046 -0.00095 C3B 1 0.774207 0.337114 0.318830 11.00000 0.00910 0.00995 = 0.01020 -0.00065 -0.00235 -0.00049 C4B 1 0.970857 0.315581 0.335110 11.00000 0.00981 0.01137 = 0.01584 -0.00016 -0.00124 -0.00117 AFIX 43 H4B 2 1.064066 0.381066 0.324301 11.00000 -1.20000 AFIX 0 C5B 1 1.027177 0.201179 0.366263 11.00000 0.00741 0.01315 = 0.01699 0.00034 -0.00095 -0.00004 AFIX 43 H5B 2 1.159657 0.188761 0.376540 11.00000 -1.20000 AFIX 0 C6B 1 0.969454 -0.013447 0.418891 11.00000 0.01658 0.01211 = 0.02088 0.00617 -0.00369 0.00359 AFIX 137 H6BA 2 0.939460 -0.094763 0.394401 11.00000 -1.50000 H6BB 2 0.905816 -0.017344 0.460390 11.00000 -1.50000 H6BC 2 1.108990 -0.006843 0.425731 11.00000 -1.50000 AFIX 0 C7B 1 0.573343 0.005476 0.383716 11.00000 0.01472 0.00891 = 0.01753 0.00294 0.00154 -0.00260 AFIX 137 H7BA 2 0.449223 0.019581 0.361799 11.00000 -1.50000 H7BB 2 0.554977 0.006148 0.430148 11.00000 -1.50000 H7BC 2 0.626807 -0.081103 0.370848 11.00000 -1.50000 AFIX 0 N1B 3 0.900072 0.105369 0.382842 11.00000 0.01067 0.00815 = 0.01496 0.00063 -0.00159 0.00120 O1B 4 0.454405 0.238757 0.320018 11.00000 0.00893 0.01546 = 0.01703 0.00542 -0.00247 -0.00190 AFIX 147 H1B 2 0.437990 0.277578 0.284660 11.00000 -1.50000 AFIX 0 O2B 4 0.710309 0.446818 0.292402 11.00000 0.01021 0.00897 = 0.01412 0.00176 -0.00121 0.00056 MOLE 3 C8A 1 0.134652 0.834846 0.266552 11.00000 0.01262 0.01524 = 0.01061 -0.00093 -0.00286 -0.00320 C9A 1 -0.028710 0.753535 0.271228 11.00000 0.01463 0.00925 = 0.01026 0.00094 -0.00284 -0.00172 C10A 1 -0.210512 0.804299 0.254750 11.00000 0.01272 0.01446 = 0.01619 -0.00302 -0.00139 -0.00117 AFIX 43 H10A 2 -0.321524 0.749479 0.258468 11.00000 -1.20000 AFIX 0 C11A 1 -0.227954 0.935624 0.232866 11.00000 0.01647 0.01736 = 0.01826 -0.00013 -0.00383 0.00425 AFIX 43 H11A 2 -0.350870 0.969958 0.220901 11.00000 -1.20000 AFIX 0 C12A 1 -0.065931 1.016532 0.228497 11.00000 0.02439 0.01120 = 0.01989 0.00256 -0.00319 0.00061 AFIX 43 H12A 2 -0.079036 1.106277 0.213931 11.00000 -1.20000 AFIX 0 C13A 1 0.116749 0.966884 0.245398 11.00000 0.01798 0.01438 = 0.01437 -0.00066 0.00003 -0.00439 AFIX 43 H13A 2 0.227117 1.022576 0.242472 11.00000 -1.20000 AFIX 0 O3A 4 0.315169 0.787968 0.282484 11.00000 0.00957 0.01671 = 0.02563 0.00111 -0.00184 -0.00269 AFIX 147 H3A 2 0.305761 0.712549 0.299998 11.00000 -1.50000 AFIX 0 O4A 4 0.001751 0.626029 0.294081 11.00000 0.01222 0.01019 = 0.01743 0.00314 -0.00399 -0.00311 AFIX 147 H4A1 2 -0.102005 0.582892 0.292445 11.00000 -1.50000 AFIX 0 MOLE 4 C8B 1 0.317818 0.686937 0.441649 11.00000 0.01108 0.01254 = 0.01360 0.00296 0.00020 0.00053 C9B 1 0.466448 0.623977 0.407331 11.00000 0.01163 0.01032 = 0.01285 -0.00011 -0.00170 -0.00076 C10B 1 0.655772 0.636319 0.428834 11.00000 0.01139 0.01447 = 0.01536 0.00209 -0.00120 0.00186 AFIX 43 H10B 2 0.756010 0.593042 0.406365 11.00000 -1.20000 AFIX 0 C11B 1 0.699518 0.712482 0.483627 11.00000 0.01351 0.01559 = 0.01298 0.00371 -0.00219 -0.00114 AFIX 43 H11B 2 0.829099 0.720224 0.498365 11.00000 -1.20000 AFIX 0 C12B 1 0.553616 0.776459 0.516271 11.00000 0.01907 0.01707 = 0.01061 0.00262 -0.00063 0.00069 AFIX 43 H12B 2 0.583573 0.829442 0.552886 11.00000 -1.20000 AFIX 0 C13B 1 0.362633 0.763062 0.495359 11.00000 0.01442 0.01503 = 0.01455 0.00087 0.00173 0.00308 AFIX 43 H13B 2 0.262921 0.806361 0.518072 11.00000 -1.20000 AFIX 0 O3B 4 0.129023 0.672971 0.422499 11.00000 0.00963 0.02490 = 0.01663 -0.00234 -0.00144 0.00270 AFIX 147 H3B 2 0.123517 0.631489 0.387518 11.00000 -1.50000 AFIX 0 O4B 4 0.409982 0.554384 0.353326 11.00000 0.01009 0.01577 = 0.01742 -0.00607 -0.00170 0.00286 AFIX 147 H4B1 2 0.507579 0.524566 0.334864 11.00000 -1.50000 AFIX 66 MOLE 5 PART 1 C8C 1 0.557451 0.139354 0.086283 21.00000 0.01948 0.01544 = 0.01245 0.00295 -0.00212 0.00262 C9C 1 0.363166 0.128749 0.070190 21.00000 0.02067 0.01466 = 0.02251 -0.00291 -0.00134 0.00132 AFIX 43 H9C 2 0.270146 0.175277 0.094530 21.00000 -1.20000 AFIX 65 C10C 1 0.304983 0.050065 0.018482 21.00000 0.02422 0.02632 = 0.01712 -0.00076 -0.00557 -0.00983 AFIX 43 H10C 2 0.172198 0.042817 0.007483 21.00000 -1.20000 AFIX 65 C11C 1 0.441084 -0.018014 -0.017132 21.00000 0.03768 0.01647 = 0.01093 0.00196 -0.00163 -0.00250 AFIX 43 H11C 2 0.401318 -0.071790 -0.052472 21.00000 -1.20000 AFIX 65 C12C 1 0.635369 -0.007409 -0.001039 21.00000 0.03047 0.02329 = 0.01506 0.00373 0.00044 0.00535 AFIX 43 H12C 2 0.728388 -0.053938 -0.025380 21.00000 -1.20000 AFIX 65 C13C 1 0.693555 0.071274 0.050668 21.00000 0.01641 0.02567 = 0.01964 0.00804 -0.00013 0.00647 AFIX 0 O3C 4 0.631259 0.214624 0.137089 21.00000 0.01277 0.02138 = 0.02375 -0.00448 -0.00777 0.00175 AFIX 147 H3C 2 0.567557 0.285703 0.140539 21.00000 -1.50000 AFIX 0 O4C 4 0.882057 0.079166 0.063246 21.00000 0.02651 0.05020 = 0.04835 -0.00490 -0.01075 0.00318 AFIX 147 H4C 2 0.911084 0.026615 0.093299 21.00000 -1.50000 AFIX 66 PART 2 C8' 1 0.420666 0.113830 0.077627 -21.00000 0.02874 0.01199 = 0.01182 -0.00179 0.00201 0.00578 C9' 1 0.389007 0.033200 0.024218 -21.00000 0.01980 0.01628 = 0.01780 0.00743 -0.00301 -0.00347 C10' 1 0.544087 -0.014027 -0.010426 -21.00000 0.02495 0.01884 = 0.01422 -0.00084 -0.00114 -0.00537 AFIX 43 H10' 2 0.522448 -0.069134 -0.046929 -21.00000 -1.20000 AFIX 65 C11' 1 0.730827 0.019376 0.008338 -21.00000 0.02145 0.02929 = 0.02391 0.00695 0.00151 0.00248 AFIX 43 H11' 2 0.836817 -0.012902 -0.015340 -21.00000 -1.20000 AFIX 65 C12' 1 0.762489 0.100006 0.061747 -21.00000 0.00539 0.03560 = 0.02612 0.00116 -0.00201 0.00079 AFIX 43 H12' 2 0.890119 0.122834 0.074571 -21.00000 -1.20000 AFIX 65 C13' 1 0.607411 0.147233 0.096391 -21.00000 0.02209 0.02481 = 0.02032 0.00704 -0.00318 0.00147 AFIX 43 H13' 2 0.629050 0.202340 0.132894 -21.00000 -1.20000 AFIX 0 O3' 4 0.256612 0.151681 0.110685 -21.00000 0.01594 0.02505 = 0.01863 -0.00907 0.00472 -0.00336 AFIX 83 H3' 2 0.288568 0.200047 0.142011 -21.00000 -1.50000 AFIX 0 O4' 4 0.213722 -0.004436 0.004947 -21.00000 0.03173 0.04046 = 0.02588 -0.00414 -0.00094 0.00091 AFIX 83 H4' 2 0.131371 0.046055 0.021380 -21.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KA1036_0m_a.res in P2(1) REM wR2 = 0.1679, GooF = S = 1.112, Restrained GooF = 1.112 for all data REM R1 = 0.0616 for 8447 Fo > 4sig(Fo) and 0.0639 for all 8799 data REM 458 parameters refined using 1 restraints END WGHT 0.0525 2.4574 REM Highest difference peak 0.409, deepest hole -0.406, 1-sigma level 0.088 Q1 1 0.8700 0.3263 0.3250 11.00000 0.05 0.41 Q2 1 -0.4417 0.7853 0.2770 11.00000 0.05 0.40 Q3 1 -0.1498 0.9895 0.2401 11.00000 0.05 0.38 Q4 1 0.1629 0.4179 0.1720 11.00000 0.05 0.36 Q5 1 -0.4361 0.9527 0.2415 11.00000 0.05 0.33 ; _shelx_res_checksum 4079 _shelx_hkl_file ; 1 0 0 409.98 25.58 1 0 0 382.85 25.53 1 0 0 424.47 25.47 1 0 0 384.35 25.48 -1 0 0 397.76 25.58 -1 0 0 421.47 25.50 -1 0 0 378.47 25.45 2 0 0 575.29 34.81 2 0 0 526.21 34.99 -2 0 0 564.35 34.87 -2 0 0 513.30 34.99 -2 0 0 538.29 34.80 2 0 0 544.80 34.95 2 0 0 547.90 34.84 3 0 0 4110.20 245.35 -3 0 0 3625.63 245.73 4 0 0 2.66 1.76 -4 0 0 -0.93 1.16 -4 0 0 0.51 1.45 4 0 0 -0.89 1.52 4 0 0 -0.74 0.85 4 0 0 0.55 1.33 -4 0 0 -0.10 1.02 5 0 0 17.00 2.28 5 0 0 17.26 3.16 -5 0 0 14.87 2.74 -5 0 0 15.50 2.93 -6 0 0 3.56 2.39 6 0 0 1.96 2.73 6 0 0 2.37 1.44 -7 0 0 116.99 9.16 7 0 0 140.39 9.65 7 0 0 139.65 9.96 -7 0 0 102.98 10.19 8 0 0 6.24 2.88 -8 0 0 10.61 4.22 -8 0 0 8.14 2.07 9 0 0 283.79 20.77 9 0 0 317.19 21.05 -9 0 0 288.48 22.10 -1 -1 0 2753.51 200.76 1 -1 0 3278.91 202.47 -1 1 0 3162.64 202.29 1 1 0 3401.93 201.11 -2 -1 0 5.98 0.97 -2 -1 0 5.60 0.96 2 -1 0 5.19 1.29 -2 -1 0 7.04 1.38 2 -1 0 6.12 1.26 2 -1 0 6.91 1.22 2 -1 0 6.29 1.18 2 1 0 6.23 1.27 2 1 0 6.27 0.87 2 1 0 5.71 1.04 -2 1 0 5.36 1.02 -2 1 0 6.03 1.31 3 -1 0 800.21 52.08 -3 -1 0 791.17 51.88 3 -1 0 805.61 52.23 3 -1 0 800.75 52.00 -3 -1 0 805.45 51.96 3 -1 0 755.56 52.21 -3 1 0 847.26 52.04 3 1 0 784.13 52.19 3 1 0 800.08 52.04 3 1 0 841.50 51.93 3 1 0 880.72 51.83 -3 1 0 862.87 52.12 -3 1 0 783.51 52.25 4 -1 0 443.96 32.32 -4 -1 0 502.10 32.18 4 -1 0 472.16 32.47 -4 -1 0 518.56 32.12 4 -1 0 457.64 32.07 4 -1 0 505.49 32.31 4 1 0 540.66 32.34 -4 1 0 499.32 32.28 4 1 0 494.20 32.08 4 1 0 510.23 32.53 -4 1 0 441.20 32.40 4 1 0 539.03 31.95 -4 1 0 502.37 32.19 5 -1 0 552.91 36.38 -5 -1 0 546.18 36.87 -5 -1 0 555.19 36.51 5 -1 0 576.93 37.25 5 1 0 578.64 36.42 5 1 0 514.63 36.48 5 1 0 586.46 36.17 -5 1 0 560.09 36.62 -5 1 0 557.98 36.93 -6 -1 0 77.20 7.49 6 -1 0 83.63 7.38 6 -1 0 85.26 7.01 -6 -1 0 82.78 7.59 -6 1 0 94.25 7.98 6 1 0 89.65 6.73 6 1 0 97.07 7.62 -6 1 0 91.29 7.64 7 -1 0 268.74 19.86 7 -1 0 303.46 19.82 -7 -1 0 288.88 20.71 -7 1 0 261.68 19.50 -7 1 0 272.02 20.52 7 1 0 299.94 20.18 7 1 0 307.15 19.47 7 1 0 290.39 19.63 -8 -1 0 9.23 4.02 8 -1 0 10.72 3.01 -8 -1 0 12.00 2.25 8 -1 0 6.24 3.06 -8 1 0 11.16 2.48 -8 1 0 12.61 3.96 8 1 0 15.00 2.97 8 1 0 9.56 2.78 9 -1 0 13.37 4.15 -9 -1 0 15.75 5.27 9 1 0 12.24 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3.60 1 -1 27 14.95 3.75 -1 -1 -27 9.22 3.39 -1 -1 -27 10.58 2.84 1 1 27 17.46 4.62 -1 1 -27 12.63 3.38 -1 1 -27 13.95 3.16 1 1 27 15.67 3.92 2 -1 27 13.00 3.43 -2 -1 -27 8.79 2.44 -2 -1 -27 9.30 3.28 2 -1 27 10.64 3.33 2 1 27 9.31 4.10 2 1 27 10.75 3.70 -2 1 -27 20.49 3.57 -2 1 -27 8.96 3.55 -3 -1 -27 74.33 6.34 3 -1 27 83.52 7.96 -3 -1 -27 87.42 7.69 3 -1 27 66.50 7.47 -3 1 -27 75.46 6.99 3 1 27 71.91 7.47 -3 1 -27 82.60 7.74 3 1 27 72.14 8.44 -4 -1 -27 17.87 3.52 4 -1 27 30.78 7.47 4 1 27 14.94 4.96 4 1 27 23.12 4.41 4 -2 -27 58.22 7.23 -4 -2 27 54.60 8.30 -4 -2 27 44.99 8.39 -4 2 27 50.70 8.47 -3 -2 27 39.01 7.35 3 -2 -27 36.53 6.75 -3 -2 27 31.52 5.72 -3 -2 27 31.94 5.01 -3 2 27 33.87 5.72 -3 2 27 34.16 6.51 -3 2 27 36.95 7.05 -2 -2 27 15.34 4.73 -2 -2 27 8.01 3.04 2 -2 -27 10.17 3.99 -2 -2 27 11.18 4.37 -2 2 27 8.73 5.07 2 2 -27 18.49 3.80 -2 2 27 12.68 4.04 -2 2 27 15.90 4.77 -1 -2 27 29.70 4.88 -1 -2 27 28.83 5.22 -1 -2 27 33.38 5.78 1 -2 -27 30.16 5.67 -1 2 27 32.46 6.15 1 2 -27 24.37 4.41 -1 2 27 32.12 5.55 -1 2 27 35.21 5.77 0 -2 27 18.87 4.08 0 -2 27 20.82 3.75 0 -2 -27 19.02 3.71 0 2 27 19.49 5.00 0 2 27 19.06 4.65 0 2 27 9.25 3.71 0 2 -27 14.23 3.54 1 -2 27 12.13 3.19 1 -2 27 20.94 4.13 -1 -2 -27 12.13 3.45 1 2 27 23.34 4.97 -1 2 -27 11.65 2.98 -1 2 -27 15.97 3.43 1 2 27 15.92 4.10 2 -2 27 3.87 2.79 2 -2 27 1.82 2.76 -2 -2 -27 0.42 2.89 2 2 27 6.76 4.23 -2 2 -27 9.27 3.10 2 2 27 6.24 3.24 -2 2 -27 3.59 2.87 -3 -2 -27 9.98 3.20 3 -2 27 19.10 3.87 3 -2 27 14.22 3.67 3 2 27 9.26 4.13 -3 2 -27 11.02 3.58 -3 2 -27 13.15 3.47 3 2 27 10.66 3.76 3 -3 -27 62.76 7.62 -3 -3 27 43.03 5.87 -3 -3 27 61.91 7.74 -3 -3 27 58.50 8.54 -3 3 27 43.54 7.92 -3 3 27 73.85 8.93 -3 3 27 48.00 7.83 -2 -3 27 183.31 13.95 -2 -3 27 193.36 13.97 2 -3 -27 180.76 13.33 -2 -3 27 155.85 12.58 -2 3 27 138.37 14.08 2 3 -27 151.68 12.63 -2 3 27 160.59 14.12 -2 3 27 183.99 14.43 1 -3 -27 7.53 3.36 -1 -3 27 7.28 3.64 -1 -3 27 5.04 2.76 -1 -3 27 4.59 4.26 -1 3 27 10.78 4.73 1 3 -27 4.71 3.04 -1 3 27 13.53 4.06 -1 3 27 5.67 4.54 0 -3 27 54.45 6.89 0 -3 27 61.20 6.14 0 -3 -27 60.18 6.37 0 3 -27 60.65 6.21 0 3 27 67.22 7.61 0 3 27 57.10 7.99 1 -3 27 27.15 4.43 -1 -3 -27 24.10 4.17 1 -3 27 21.59 3.97 1 3 27 16.25 4.34 -1 3 -27 25.88 4.20 1 3 27 18.08 5.34 -2 -3 -27 87.53 8.17 2 -3 27 93.83 8.14 2 -3 27 98.65 8.75 2 3 27 87.56 9.36 -2 3 -27 94.96 8.05 2 3 27 96.57 9.03 -3 -3 -27 57.59 6.40 3 -3 27 70.31 6.49 3 -3 27 57.16 6.27 3 3 27 59.84 7.31 3 3 27 41.36 7.41 -3 3 -27 56.97 6.10 -3 -4 27 265.95 19.26 -3 -4 27 232.09 18.64 -3 -4 27 215.94 17.35 3 -4 -27 263.04 18.13 -3 4 27 239.68 20.26 -3 4 27 240.12 18.77 -3 4 27 252.76 18.80 -2 -4 27 179.11 14.19 2 -4 -27 218.34 15.23 -2 -4 27 198.55 15.40 -2 -4 27 200.50 15.71 -2 4 27 198.99 16.14 2 4 -27 187.77 14.50 -2 4 27 209.64 15.79 -2 4 27 179.00 15.64 -1 -4 27 71.18 7.72 -1 -4 27 66.94 6.33 -1 -4 27 60.87 7.34 1 -4 -27 65.62 7.05 -1 4 27 67.00 8.12 -1 4 27 65.26 7.84 -1 4 27 50.77 8.83 1 4 -27 67.67 6.76 0 -4 27 66.02 7.09 0 -4 27 67.68 6.10 0 -4 -27 54.55 6.56 0 4 27 63.40 7.26 0 4 27 62.66 7.96 0 4 -27 61.66 6.50 0 4 27 56.32 8.26 -1 -4 -27 21.27 3.98 1 -4 27 22.57 3.77 1 -4 27 27.48 4.93 1 4 27 15.94 4.35 1 4 27 17.66 4.81 1 4 27 20.89 5.13 -1 4 -27 27.34 4.55 2 -4 27 72.16 7.48 -2 -4 -27 67.53 6.83 2 -4 27 86.10 6.95 -2 4 -27 66.82 6.81 2 4 27 70.23 8.01 -3 -4 -27 71.25 8.44 3 -4 27 76.80 7.80 3 -4 27 94.03 8.08 3 4 27 107.04 9.29 -2 -5 27 64.85 7.48 -2 -5 27 63.89 6.38 2 -5 -27 60.72 7.22 -2 -5 27 69.88 8.41 -2 5 27 49.10 8.49 2 5 -27 77.45 6.84 -2 5 27 61.38 8.94 -1 -5 27 9.04 2.50 -1 -5 27 9.41 3.96 -1 -5 27 7.84 3.65 1 -5 -27 5.89 3.22 1 5 -27 8.47 3.21 -1 5 27 -0.68 4.82 -1 5 27 1.51 4.25 0 -5 27 3.45 3.25 0 -5 -27 2.66 2.83 0 -5 27 7.19 2.36 0 5 27 1.06 5.37 0 5 27 5.39 4.26 0 5 -27 4.74 3.11 1 -5 27 16.24 3.89 -1 -5 -27 20.04 3.98 1 -5 27 24.26 4.03 -1 5 -27 29.29 4.36 1 5 27 23.07 5.00 2 -5 27 42.35 5.89 -2 -5 -27 41.75 5.67 2 -5 27 49.45 5.42 -2 5 -27 49.26 5.23 2 5 27 38.17 6.21 0 -6 27 -0.82 2.98 0 -6 27 3.16 3.76 0 -6 -27 7.47 3.48 0 -6 -27 -2.73 4.19 0 6 27 -3.69 4.39 -3 0 28 -2.53 4.50 -3 0 28 0.88 4.37 -3 0 28 3.31 3.27 -2 0 28 44.98 7.45 -2 0 28 59.22 7.62 -2 0 28 39.87 6.38 1 0 -28 122.95 10.65 -1 0 28 138.74 11.71 -1 0 28 135.37 11.69 1 0 -28 129.31 10.18 -1 0 28 135.98 11.13 0 0 28 1.44 4.26 0 0 28 5.21 3.40 0 0 28 5.71 3.23 0 0 -28 7.47 2.86 0 0 -28 -1.16 3.44 1 0 28 26.44 4.61 1 0 28 20.08 4.26 -1 0 -28 16.65 3.29 -1 0 -28 8.55 3.76 -2 0 -28 302.52 21.42 -2 0 -28 311.83 20.79 2 0 28 314.27 21.86 2 0 28 298.02 21.88 3 0 28 1.16 3.97 3 0 28 9.14 3.24 -3 0 -28 1.51 2.68 -3 0 -28 15.69 3.78 3 -1 -28 2.38 3.93 -3 -1 28 7.41 4.74 -3 -1 28 9.54 3.40 -3 -1 28 16.92 4.66 -3 1 28 4.82 4.59 -3 1 28 3.82 3.70 -3 1 28 17.87 4.89 -2 -1 28 40.11 6.54 2 -1 -28 41.31 6.56 -2 -1 28 31.25 5.58 -2 -1 28 41.06 6.78 -2 1 28 44.52 7.12 -2 1 28 34.30 6.86 -2 1 28 41.06 6.08 -1 -1 28 9.51 3.25 -1 -1 28 6.48 3.41 1 -1 -28 3.89 3.77 1 -1 -28 11.99 3.08 -1 -1 28 9.15 4.40 1 1 -28 4.19 3.32 -1 1 28 13.54 4.02 -1 1 28 7.67 4.37 -1 1 28 10.21 4.17 0 -1 28 11.47 3.53 0 -1 -28 8.68 3.72 0 -1 -28 16.03 3.69 0 -1 28 6.26 3.35 0 1 28 13.24 4.13 0 1 -28 11.41 3.14 0 1 -28 14.42 3.56 0 1 28 2.95 4.20 1 -1 28 6.44 3.27 1 -1 28 9.58 3.48 -1 -1 -28 12.10 3.61 -1 1 -28 7.09 3.25 1 1 28 8.91 3.58 1 1 28 17.97 4.21 -1 1 -28 15.05 3.53 -2 -1 -28 8.34 3.29 2 -1 28 9.54 3.53 2 -1 28 12.01 3.66 2 1 28 10.87 3.48 -2 1 -28 11.23 3.57 2 1 28 11.44 4.23 -2 1 -28 9.77 3.24 -3 -1 -28 117.60 9.53 3 -1 28 108.52 9.72 3 -1 28 100.10 9.62 -3 1 -28 115.35 9.54 3 1 28 108.74 10.29 3 1 28 110.00 10.30 -3 1 -28 112.78 8.93 -3 -2 28 31.06 4.89 3 -2 -28 29.58 5.02 -3 -2 28 34.30 6.12 -3 -2 28 30.54 6.05 -3 2 28 30.36 5.66 -3 2 28 29.29 6.14 -3 2 28 23.46 5.01 2 -2 -28 38.36 6.48 -2 -2 28 31.04 5.86 -2 -2 28 30.94 6.02 -2 -2 28 27.15 5.03 -2 2 28 26.72 5.97 -2 2 28 36.86 5.94 2 2 -28 37.16 5.30 -2 2 28 33.44 6.37 1 -2 -28 6.93 3.75 -1 -2 28 3.20 3.65 -1 -2 28 4.70 2.76 -1 -2 28 3.47 3.54 1 2 -28 4.86 3.29 -1 2 28 3.70 4.61 -1 2 28 3.46 3.96 -1 2 28 3.56 3.91 0 -2 28 13.94 4.07 0 -2 28 15.20 3.20 0 -2 -28 15.38 3.86 0 2 28 13.05 4.62 0 2 28 19.32 5.24 0 2 -28 19.70 3.97 1 -2 28 7.14 2.91 -1 -2 -28 -1.05 2.98 1 2 28 5.13 4.21 -1 2 -28 6.94 3.01 1 2 28 4.47 3.35 -2 -2 -28 7.37 3.16 2 -2 28 5.43 3.02 2 -2 28 13.40 3.37 -2 2 -28 16.00 3.73 -2 2 -28 5.75 3.41 2 2 28 2.67 4.20 3 -2 28 11.54 4.13 3 -2 28 24.25 4.14 3 2 28 15.70 6.27 3 2 28 13.58 4.49 -2 -3 28 70.20 8.47 -2 -3 28 66.44 6.87 2 -3 -28 68.98 7.87 -2 -3 28 73.69 8.42 -2 3 28 73.83 8.90 2 3 -28 75.58 7.16 -2 3 28 51.83 8.20 -1 -3 28 59.89 5.96 1 -3 -28 63.45 7.13 -1 -3 28 54.54 7.56 -1 -3 28 52.21 7.24 -1 3 28 51.14 8.14 1 3 -28 50.02 6.27 -1 3 28 69.32 7.72 -1 3 28 51.21 7.76 0 -3 28 23.10 4.58 0 -3 -28 33.94 5.34 0 -3 28 21.83 3.80 0 3 28 26.33 5.34 0 3 28 11.57 4.45 0 3 28 15.66 5.20 0 3 -28 21.03 4.11 1 -3 28 21.92 3.87 1 -3 28 26.02 4.52 -1 -3 -28 25.96 4.72 -1 3 -28 34.49 4.73 1 3 28 24.22 4.42 1 3 28 22.65 5.55 1 3 28 27.35 5.57 -2 -3 -28 217.95 15.34 2 -3 28 207.95 15.25 2 -3 28 205.38 15.62 2 3 28 209.83 16.00 2 3 28 197.20 15.95 -2 3 -28 213.47 15.10 2 -4 -28 59.47 7.44 -2 -4 28 62.67 8.47 -2 -4 28 74.47 8.83 -2 -4 28 67.12 8.01 -2 4 28 63.75 8.78 -2 4 28 66.46 8.63 1 -4 -28 33.25 5.66 -1 -4 28 35.27 4.98 -1 -4 28 50.67 6.62 -1 -4 28 47.96 6.37 -1 4 28 38.57 7.13 -1 4 28 27.74 6.03 1 4 -28 34.40 5.59 -1 4 28 44.46 6.98 0 -4 -28 7.20 3.12 0 -4 28 11.94 2.75 0 -4 28 8.72 3.79 0 4 -28 8.10 3.17 0 4 28 7.08 4.18 0 4 28 3.74 4.29 -1 -4 -28 9.68 3.12 1 -4 28 16.39 3.80 1 -4 28 11.58 3.17 1 4 28 7.21 4.37 -1 4 -28 17.50 3.65 1 4 28 3.29 4.29 -2 0 29 6.60 4.28 -2 0 29 6.44 3.58 -2 0 29 14.86 4.74 -1 0 29 7.07 3.87 -1 0 29 7.80 4.42 -1 0 29 11.92 3.97 1 0 -29 5.38 3.47 1 0 -29 11.38 3.14 0 0 29 -5.85 4.27 0 0 29 -2.02 3.31 0 0 -29 -1.92 3.33 0 0 -29 2.82 2.79 -1 0 -29 15.48 3.90 -1 0 -29 18.32 3.33 1 0 29 21.85 4.41 2 0 29 -2.67 3.36 2 0 29 5.28 3.49 -2 0 -29 4.20 3.29 -2 0 -29 2.49 3.05 -2 -1 29 47.52 7.22 -2 -1 29 39.56 7.23 2 -1 -29 34.74 6.23 -2 -1 29 40.47 6.15 -2 1 29 50.59 7.36 -2 1 29 52.07 6.68 -2 1 29 39.73 7.28 -1 -1 29 51.06 6.38 -1 -1 29 56.46 7.45 1 -1 -29 59.55 7.12 -1 -1 29 50.25 7.31 -1 1 29 56.90 7.40 -1 1 29 61.95 8.07 -1 1 29 50.90 7.53 1 1 -29 56.67 6.17 0 -1 -29 -3.63 3.18 0 -1 29 -3.24 2.77 0 -1 29 3.25 3.51 0 -1 29 -3.29 3.70 0 1 29 -1.80 3.32 0 1 -29 4.24 3.14 0 1 29 2.49 3.98 0 1 29 -0.04 4.51 -1 -1 -29 12.72 3.88 1 -1 29 14.92 3.82 1 -1 29 9.72 3.53 1 1 29 16.18 4.13 -1 1 -29 14.80 3.47 1 1 29 9.94 4.00 -2 -1 -29 136.54 10.94 2 -1 29 124.36 11.53 2 -1 29 132.75 10.97 2 1 29 135.32 11.60 -2 1 -29 139.43 10.72 -2 -2 29 66.86 8.20 -2 -2 29 59.97 7.82 -2 -2 29 59.35 7.14 -2 2 29 46.99 10.06 -2 2 29 44.43 7.44 -2 2 29 48.41 7.92 -1 -2 29 27.61 4.87 1 -2 -29 25.88 4.73 -1 -2 29 23.21 4.42 -1 -2 29 19.79 4.25 -1 2 29 17.72 5.02 -1 2 29 21.88 5.46 1 2 -29 24.18 4.42 -1 2 29 24.39 5.05 0 -2 29 -5.04 2.90 0 -2 -29 1.03 3.40 0 -2 29 1.23 3.03 0 2 -29 -6.01 3.09 0 2 29 5.82 4.32 0 2 29 5.32 4.00 0 2 29 -4.44 3.30 1 -2 29 17.17 3.98 1 -2 29 19.69 3.79 -1 -2 -29 24.47 4.14 1 2 29 20.13 4.89 1 2 29 21.28 5.05 -1 2 -29 32.72 4.76 -1 -3 29 29.99 5.06 -1 -3 29 28.86 6.69 -1 -3 29 40.66 6.30 -1 3 29 34.33 5.89 -1 3 29 27.14 5.94 0 -3 -29 -0.24 3.15 0 -3 29 4.49 2.97 0 -3 29 -1.34 3.32 0 3 29 -2.25 4.60 0 3 29 6.70 4.02 0 3 29 0.89 4.18 0 3 -29 4.74 3.10 1 -3 29 22.19 4.58 1 -3 29 24.23 4.24 1 3 29 18.34 6.75 1 3 29 12.81 4.60 1 3 29 22.93 5.12 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 0.6487 _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 0.71114 6.953 9.981 20.880 89.984 90.801 89.943 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 41648 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 0.2719(5) 0.6492(4) 0.13991(16) 0.0161(6) Uani 1 1 d . . . . . C2A C 0.3566(5) 0.5416(4) 0.16957(16) 0.0146(6) Uani 1 1 d . . . . . C3A C 0.2540(5) 0.4203(4) 0.18182(16) 0.0156(6) Uani 1 1 d . . . . . C4A C 0.0574(6) 0.4202(5) 0.16367(19) 0.0225(8) Uani 1 1 d . . . . . H4A H -0.018600 0.342786 0.170995 0.027 Uiso 1 1 calc R U . . . C5A C -0.0237(6) 0.5296(5) 0.13590(19) 0.0245(8) Uani 1 1 d . . . . . H5A H -0.157042 0.528008 0.125068 0.029 Uiso 1 1 calc R U . . . C6A C -0.0145(7) 0.7561(5) 0.0917(2) 0.0307(10) Uani 1 1 d . . . . . H6AA H 0.057348 0.781428 0.053522 0.046 Uiso 1 1 calc R U . . . H6AB H -0.017871 0.831972 0.121405 0.046 Uiso 1 1 calc R U . . . H6AC H -0.146191 0.731242 0.079099 0.046 Uiso 1 1 calc R U . . . C7A C 0.3843(6) 0.7723(4) 0.12293(18) 0.0207(7) Uani 1 1 d . . . . . H7AA H 0.398524 0.776876 0.076360 0.031 Uiso 1 1 calc R U . . . H7AB H 0.511831 0.768415 0.143572 0.031 Uiso 1 1 calc R U . . . H7AC H 0.315875 0.852083 0.137759 0.031 Uiso 1 1 calc R U . . . N1A N 0.0803(5) 0.6417(4) 0.12308(15) 0.0206(6) Uani 1 1 d . . . . . O1A O 0.5481(4) 0.5482(3) 0.18441(13) 0.0168(5) Uani 1 1 d . . . . . H1A H 0.575399 0.490481 0.212363 0.025 Uiso 1 1 calc R U . . . O2A O 0.3434(4) 0.3174(3) 0.20574(13) 0.0196(5) Uani 1 1 d . . . . . C1B C 0.7093(5) 0.1151(3) 0.36593(15) 0.0109(5) Uani 1 1 d . . . . . C2B C 0.6458(5) 0.2298(3) 0.33367(16) 0.0108(6) Uani 1 1 d . . . . . C3B C 0.7742(4) 0.3371(3) 0.31883(15) 0.0098(5) Uani 1 1 d . . . . . C4B C 0.9709(5) 0.3156(3) 0.33511(16) 0.0124(6) Uani 1 1 d . . . . . H4B H 1.064066 0.381066 0.324301 0.015 Uiso 1 1 calc R U . . . C5B C 1.0272(5) 0.2012(3) 0.36626(17) 0.0125(6) Uani 1 1 d . . . . . H5B H 1.159657 0.188761 0.376540 0.015 Uiso 1 1 calc R U . . . C6B C 0.9695(5) -0.0134(4) 0.41889(18) 0.0166(7) Uani 1 1 d . . . . . H6BA H 0.939460 -0.094763 0.394401 0.025 Uiso 1 1 calc R U . . . H6BB H 0.905816 -0.017344 0.460390 0.025 Uiso 1 1 calc R U . . . H6BC H 1.108990 -0.006843 0.425731 0.025 Uiso 1 1 calc R U . . . C7B C 0.5733(5) 0.0055(3) 0.38372(17) 0.0137(6) Uani 1 1 d . . . . . H7BA H 0.449223 0.019581 0.361799 0.021 Uiso 1 1 calc R U . . . H7BB H 0.554977 0.006148 0.430148 0.021 Uiso 1 1 calc R U . . . H7BC H 0.626807 -0.081103 0.370848 0.021 Uiso 1 1 calc R U . . . N1B N 0.9001(4) 0.1054(3) 0.38284(14) 0.0113(5) Uani 1 1 d . . . . . O1B O 0.4544(3) 0.2388(3) 0.32002(12) 0.0138(5) Uani 1 1 d . . . . . H1B H 0.437990 0.277578 0.284660 0.021 Uiso 1 1 calc R U . . . O2B O 0.7103(3) 0.4468(2) 0.29240(12) 0.0111(4) Uani 1 1 d . . . . . C8A C 0.1347(5) 0.8348(4) 0.26655(15) 0.0129(6) Uani 1 1 d . . . . . C9A C -0.0287(5) 0.7535(3) 0.27123(15) 0.0114(6) Uani 1 1 d . . . . . C10A C -0.2105(5) 0.8043(4) 0.25475(17) 0.0145(6) Uani 1 1 d . . . . . H10A H -0.321524 0.749479 0.258468 0.017 Uiso 1 1 calc R U . . . C11A C -0.2280(5) 0.9356(4) 0.23287(18) 0.0174(7) Uani 1 1 d . . . . . H11A H -0.350870 0.969958 0.220901 0.021 Uiso 1 1 calc R U . . . C12A C -0.0659(6) 1.0165(4) 0.22850(18) 0.0185(7) Uani 1 1 d . . . . . H12A H -0.079036 1.106277 0.213931 0.022 Uiso 1 1 calc R U . . . C13A C 0.1167(5) 0.9669(4) 0.24540(17) 0.0156(6) Uani 1 1 d . . . . . H13A H 0.227117 1.022576 0.242472 0.019 Uiso 1 1 calc R U . . . O3A O 0.3152(4) 0.7880(3) 0.28248(13) 0.0173(5) Uani 1 1 d . . . . . H3A H 0.305761 0.712549 0.299998 0.026 Uiso 1 1 calc R U . . . O4A O 0.0018(3) 0.6260(2) 0.29408(12) 0.0133(4) Uani 1 1 d . . . . . H4A1 H -0.102005 0.582892 0.292445 0.020 Uiso 1 1 calc R U . . . C8B C 0.3178(5) 0.6869(3) 0.44165(16) 0.0124(6) Uani 1 1 d . . . . . C9B C 0.4664(5) 0.6240(3) 0.40733(15) 0.0116(6) Uani 1 1 d . . . . . C10B C 0.6558(5) 0.6363(4) 0.42883(16) 0.0138(6) Uani 1 1 d . . . . . H10B H 0.756010 0.593042 0.406365 0.017 Uiso 1 1 calc R U . . . C11B C 0.6995(5) 0.7125(4) 0.48363(16) 0.0141(6) Uani 1 1 d . . . . . H11B H 0.829099 0.720224 0.498365 0.017 Uiso 1 1 calc R U . . . C12B C 0.5536(5) 0.7765(4) 0.51627(16) 0.0156(6) Uani 1 1 d . . . . . H12B H 0.583573 0.829442 0.552886 0.019 Uiso 1 1 calc R U . . . C13B C 0.3626(5) 0.7631(4) 0.49536(17) 0.0147(6) Uani 1 1 d . . . . . H13B H 0.262921 0.806361 0.518072 0.018 Uiso 1 1 calc R U . . . O3B O 0.1290(4) 0.6730(3) 0.42250(13) 0.0171(5) Uani 1 1 d . . . . . H3B H 0.123517 0.631489 0.387518 0.026 Uiso 1 1 calc R U . . . O4B O 0.4100(3) 0.5544(3) 0.35333(12) 0.0144(5) Uani 1 1 d . . . . . H4B1 H 0.507579 0.524566 0.334864 0.022 Uiso 1 1 calc R U . . . C8C C 0.5575(8) 0.1394(6) 0.0863(3) 0.0158(17) Uani 0.578(7) 1 d G . P A 1 C9C C 0.3632(8) 0.1287(7) 0.0702(3) 0.0193(19) Uani 0.578(7) 1 d G . P A 1 H9C H 0.270146 0.175277 0.094530 0.023 Uiso 0.578(7) 1 calc R U P A 1 C10C C 0.3050(8) 0.0501(6) 0.0185(2) 0.0226(16) Uani 0.578(7) 1 d G . P A 1 H10C H 0.172198 0.042817 0.007483 0.027 Uiso 0.578(7) 1 calc R U P A 1 C11C C 0.4411(10) -0.0180(5) -0.0171(2) 0.0217(15) Uani 0.578(7) 1 d G . P A 1 H11C H 0.401318 -0.071790 -0.052472 0.026 Uiso 0.578(7) 1 calc R U P A 1 C12C C 0.6354(10) -0.0074(6) -0.0010(2) 0.0229(16) Uani 0.578(7) 1 d G . P A 1 H12C H 0.728388 -0.053938 -0.025380 0.028 Uiso 0.578(7) 1 calc R U P A 1 C13C C 0.6936(7) 0.0713(6) 0.0507(3) 0.0206(15) Uani 0.578(7) 1 d G . P A 1 O3C O 0.6313(7) 0.2146(5) 0.1371(2) 0.0194(11) Uani 0.578(7) 1 d . . P A 1 H3C H 0.567557 0.285703 0.140539 0.029 Uiso 0.578(7) 1 calc R U P A 1 O4C O 0.8821(10) 0.0792(8) 0.0632(4) 0.0418(18) Uani 0.578(7) 1 d . . P A 1 H4C H 0.911084 0.026615 0.093299 0.063 Uiso 0.578(7) 1 calc R U P A 1 C8' C 0.4207(10) 0.1138(10) 0.0776(4) 0.017(3) Uani 0.422(7) 1 d G . P A 2 C9' C 0.3890(10) 0.0332(8) 0.0242(3) 0.018(2) Uani 0.422(7) 1 d G . P A 2 C10' C 0.5441(13) -0.0140(7) -0.0104(3) 0.019(2) Uani 0.422(7) 1 d G . P A 2 H10' H 0.522448 -0.069134 -0.046929 0.023 Uiso 0.422(7) 1 calc R U P A 2 C11' C 0.7308(11) 0.0194(8) 0.0083(3) 0.025(2) Uani 0.422(7) 1 d G . P A 2 H11' H 0.836817 -0.012902 -0.015340 0.030 Uiso 0.422(7) 1 calc R U P A 2 C12' C 0.7625(10) 0.1000(9) 0.0617(4) 0.022(2) Uani 0.422(7) 1 d G . P A 2 H12' H 0.890119 0.122834 0.074571 0.027 Uiso 0.422(7) 1 calc R U P A 2 C13' C 0.6074(12) 0.1472(10) 0.0964(4) 0.022(3) Uani 0.422(7) 1 d G . P A 2 H13' H 0.629050 0.202340 0.132894 0.027 Uiso 0.422(7) 1 calc R U P A 2 O3' O 0.2566(9) 0.1517(7) 0.1107(3) 0.0198(15) Uani 0.422(7) 1 d . . P A 2 H3' H 0.288568 0.200047 0.142011 0.030 Uiso 0.422(7) 1 calc R U P A 2 O4' O 0.2137(13) -0.0044(9) 0.0049(4) 0.033(2) Uani 0.422(7) 1 d . . P A 2 H4' H 0.131371 0.046055 0.021380 0.049 Uiso 0.422(7) 1 calc R U P A 2 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 0.0151(15) 0.0208(17) 0.0123(14) -0.0011(13) -0.0009(11) 0.0005(13) C2A 0.0134(15) 0.0190(16) 0.0112(13) -0.0009(12) -0.0013(11) -0.0018(12) C3A 0.0175(15) 0.0209(17) 0.0085(13) -0.0001(12) -0.0002(11) -0.0051(13) C4A 0.0164(16) 0.032(2) 0.0186(17) 0.0004(15) -0.0005(13) -0.0121(15) C5A 0.0114(15) 0.043(2) 0.0195(17) -0.0004(16) -0.0014(13) -0.0036(15) C6A 0.028(2) 0.039(2) 0.0247(19) 0.0051(18) -0.0063(16) 0.0151(19) C7A 0.0240(18) 0.0203(17) 0.0177(16) 0.0034(14) -0.0020(13) 0.0004(14) N1A 0.0143(14) 0.0321(18) 0.0152(13) 0.0035(13) -0.0020(11) 0.0059(13) O1A 0.0130(11) 0.0200(12) 0.0173(12) 0.0062(10) -0.0053(9) -0.0045(10) O2A 0.0253(13) 0.0184(13) 0.0150(11) 0.0017(10) -0.0040(10) -0.0048(10) C1B 0.0116(13) 0.0100(13) 0.0111(13) 0.0010(11) -0.0007(10) -0.0007(11) C2B 0.0097(13) 0.0094(13) 0.0135(13) -0.0002(11) -0.0005(10) -0.0010(10) C3B 0.0091(13) 0.0100(13) 0.0102(13) -0.0007(11) -0.0023(10) -0.0005(11) C4B 0.0098(13) 0.0114(14) 0.0158(14) -0.0002(11) -0.0012(11) -0.0012(11) C5B 0.0074(13) 0.0132(14) 0.0170(14) 0.0003(11) -0.0010(10) 0.0000(11) C6B 0.0166(16) 0.0121(14) 0.0209(16) 0.0062(12) -0.0037(13) 0.0036(12) C7B 0.0147(15) 0.0089(13) 0.0175(15) 0.0029(11) 0.0015(12) -0.0026(11) N1B 0.0107(12) 0.0082(12) 0.0150(12) 0.0006(10) -0.0016(10) 0.0012(9) O1B 0.0089(10) 0.0155(11) 0.0170(11) 0.0054(9) -0.0025(8) -0.0019(8) O2B 0.0102(10) 0.0090(10) 0.0141(10) 0.0018(8) -0.0012(8) 0.0006(8) C8A 0.0126(14) 0.0152(15) 0.0106(13) -0.0009(11) -0.0029(11) -0.0032(12) C9A 0.0146(14) 0.0093(13) 0.0103(13) 0.0009(10) -0.0028(11) -0.0017(11) C10A 0.0127(14) 0.0145(15) 0.0162(14) -0.0030(12) -0.0014(11) -0.0012(12) C11A 0.0165(15) 0.0174(16) 0.0183(15) -0.0001(13) -0.0038(12) 0.0042(13) C12A 0.0244(18) 0.0112(14) 0.0199(16) 0.0026(12) -0.0032(14) 0.0006(13) C13A 0.0180(15) 0.0144(15) 0.0144(14) -0.0007(12) 0.0000(12) -0.0044(12) O3A 0.0096(11) 0.0167(12) 0.0256(13) 0.0011(10) -0.0018(9) -0.0027(9) O4A 0.0122(10) 0.0102(10) 0.0174(11) 0.0031(9) -0.0040(8) -0.0031(8) C8B 0.0111(14) 0.0125(14) 0.0136(14) 0.0030(11) 0.0002(11) 0.0005(11) C9B 0.0116(13) 0.0103(13) 0.0128(13) -0.0001(11) -0.0017(11) -0.0008(11) C10B 0.0114(14) 0.0145(14) 0.0154(14) 0.0021(12) -0.0012(11) 0.0019(11) C11B 0.0135(14) 0.0156(15) 0.0130(14) 0.0037(12) -0.0022(11) -0.0011(12) C12B 0.0191(16) 0.0171(16) 0.0106(13) 0.0026(12) -0.0006(11) 0.0007(13) C13B 0.0144(15) 0.0150(15) 0.0146(14) 0.0009(12) 0.0017(11) 0.0031(12) O3B 0.0096(11) 0.0249(14) 0.0166(12) -0.0023(10) -0.0014(9) 0.0027(9) O4B 0.0101(10) 0.0158(11) 0.0174(11) -0.0061(9) -0.0017(8) 0.0029(9) C8C 0.019(4) 0.015(3) 0.012(3) 0.003(2) -0.002(3) 0.003(3) C9C 0.021(4) 0.015(4) 0.023(4) -0.003(3) -0.001(3) 0.001(3) C10C 0.024(4) 0.026(4) 0.017(3) -0.001(3) -0.006(3) -0.010(4) C11C 0.038(5) 0.016(3) 0.011(3) 0.002(2) -0.002(3) -0.002(3) C12C 0.030(5) 0.023(4) 0.015(3) 0.004(3) 0.000(4) 0.005(4) C13C 0.016(4) 0.026(4) 0.020(3) 0.008(3) 0.000(3) 0.006(3) O3C 0.013(2) 0.021(2) 0.024(2) -0.0045(19) -0.0078(17) 0.0017(17) O4C 0.027(3) 0.050(4) 0.048(4) -0.005(3) -0.011(3) 0.003(3) C8' 0.029(7) 0.012(4) 0.012(4) -0.002(3) 0.002(4) 0.006(5) C9' 0.020(5) 0.016(4) 0.018(4) 0.007(3) -0.003(4) -0.003(4) C10' 0.025(6) 0.019(4) 0.014(4) -0.001(3) -0.001(5) -0.005(5) C11' 0.021(5) 0.029(5) 0.024(5) 0.007(4) 0.002(4) 0.002(4) C12' 0.005(5) 0.036(6) 0.026(5) 0.001(4) -0.002(4) 0.001(4) C13' 0.022(6) 0.025(5) 0.020(5) 0.007(4) -0.003(4) 0.001(4) O3' 0.016(3) 0.025(3) 0.019(3) -0.009(2) 0.005(2) -0.003(2) O4' 0.032(4) 0.040(5) 0.026(4) -0.004(3) -0.001(3) 0.001(4) 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(3) . . ? C2A C1A C7A 121.9(3) . . ? N1A C1A C7A 119.3(3) . . ? O1A C2A C1A 118.4(3) . . ? O1A C2A C3A 119.2(3) . . ? C1A C2A C3A 122.3(3) . . ? O2A C3A C4A 124.0(3) . . ? O2A C3A C2A 120.1(3) . . ? C4A C3A C2A 115.8(3) . . ? C5A C4A C3A 120.6(4) . . ? C5A C4A H4A 119.7 . . ? C3A C4A H4A 119.7 . . ? C4A C5A N1A 121.9(3) . . ? C4A C5A H5A 119.1 . . ? N1A 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 . . ? C5A N1A C1A 120.7(3) . . ? C5A N1A C6A 119.4(3) . . ? C1A N1A C6A 119.9(4) . . ? C2A O1A H1A 109.5 . . ? N1B C1B C2B 118.6(3) . . ? N1B C1B C7B 119.8(3) . . ? C2B C1B C7B 121.6(3) . . ? O1B C2B C1B 117.1(3) . . ? O1B C2B C3B 121.1(3) . . ? C1B C2B C3B 121.7(3) . . ? O2B C3B C4B 123.3(3) . . ? O2B C3B C2B 120.8(3) . . ? C4B C3B C2B 115.9(3) . . ? C5B C4B C3B 120.5(3) . . ? C5B C4B H4B 119.8 . . ? C3B C4B H4B 119.8 . . ? N1B C5B C4B 122.0(3) . . ? 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 . . ? C5B N1B C1B 121.2(3) . . ? C5B N1B C6B 119.2(3) . . ? C1B N1B C6B 119.6(3) . . ? C2B O1B H1B 109.5 . . ? O3A C8A C13A 118.3(3) . . ? O3A C8A C9A 121.6(3) . . ? C13A C8A C9A 120.1(3) . . ? O4A C9A C10A 123.7(3) . . ? O4A C9A C8A 116.1(3) . . ? C10A C9A C8A 120.2(3) . . ? C11A C10A C9A 119.7(3) . . ? C11A C10A H10A 120.2 . . ? C9A C10A H10A 120.2 . . ? C12A C11A C10A 120.1(3) . . ? C12A C11A H11A 119.9 . . ? C10A C11A H11A 119.9 . . ? C11A C12A C13A 120.6(3) . . ? C11A C12A H12A 119.7 . . ? C13A C12A H12A 119.7 . . ? C8A C13A C12A 119.3(3) . . ? C8A C13A H13A 120.4 . . ? C12A C13A H13A 120.4 . . ? C8A O3A H3A 109.5 . . ? C9A O4A H4A1 109.5 . . ? O3B C8B C13B 119.5(3) . . ? O3B C8B C9B 120.7(3) . . ? C13B C8B C9B 119.8(3) . . ? O4B C9B C10B 124.5(3) . . ? O4B C9B C8B 116.0(3) . . ? C10B C9B C8B 119.5(3) . . ? C9B C10B C11B 120.2(3) . . ? C9B C10B H10B 119.9 . . ? C11B C10B H10B 119.9 . . ? C12B C11B C10B 120.0(3) . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C12B C13B 120.1(3) . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C8B C13B C12B 120.4(3) . . ? C8B C13B H13B 119.8 . . ? C12B C13B H13B 119.8 . . ? C8B O3B H3B 109.5 . . ? C9B O4B H4B1 109.5 . . ? C9C C8C C13C 120.0 . . ? C9C C8C O3C 124.8(4) . . ? C13C C8C O3C 115.2(4) . . ? C10C C9C C8C 120.0 . . ? C10C C9C H9C 120.0 . . ? C8C C9C H9C 120.0 . . ? C9C C10C C11C 120.0 . . ? C9C C10C H10C 120.0 . . ? C11C C10C H10C 120.0 . . ? C12C C11C C10C 120.0 . . ? C12C C11C H11C 120.0 . . ? C10C C11C H11C 120.0 . . ? C13C C12C C11C 120.0 . . ? C13C C12C H12C 120.0 . . ? C11C C12C H12C 120.0 . . ? O4C C13C C12C 117.3(5) . . ? O4C C13C C8C 122.7(5) . . ? C12C C13C C8C 120.0 . . ? C8C O3C H3C 109.5 . . ? C13C O4C H4C 109.5 . . ? C9' C8' C13' 120.0 . . ? C9' C8' O3' 115.7(6) . . ? C13' C8' O3' 124.2(6) . . ? O4' C9' C10' 117.4(6) . . ? O4' C9' C8' 122.6(6) . . ? C10' C9' C8' 120.0 . . ? C9' C10' C11' 120.0 . . ? C9' C10' H10' 120.0 . . ? C11' C10' H10' 120.0 . . ? C10' C11' C12' 120.0 . . ? C10' C11' H11' 120.0 . . ? C12' C11' H11' 120.0 . . ? C13' C12' C11' 120.0 . . ? C13' C12' H12' 120.0 . . ? C11' C12' H12' 120.0 . . ? C12' C13' C8' 120.0 . . ? C12' C13' H13' 120.0 . . ? C8' C13' H13' 120.0 . . ? C8' O3' H3' 109.5 . . ? C9' O4' H4' 109.5 . . ? 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 1.369(5) . ? C1A N1A 1.374(4) . ? C1A C7A 1.501(5) . ? C2A O1A 1.363(4) . ? C2A C3A 1.430(5) . ? C3A O2A 1.296(5) . ? C3A C4A 1.411(5) . ? C4A C5A 1.355(6) . ? C4A H4A 0.9500 . ? C5A N1A 1.362(6) . ? C5A H5A 0.9500 . ? C6A N1A 1.467(6) . ? 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 H1A 0.8400 . ? C1B N1B 1.370(4) . ? C1B C2B 1.397(4) . ? C1B C7B 1.496(5) . ? C2B O1B 1.358(4) . ? C2B C3B 1.431(4) . ? C3B O2B 1.301(4) . ? C3B C4B 1.419(4) . ? C4B C5B 1.368(5) . ? C4B H4B 0.9500 . ? C5B N1B 1.351(4) . ? C5B H5B 0.9500 . ? C6B N1B 1.481(4) . ? 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 H1B 0.8400 . ? C8A O3A 1.375(4) . ? C8A C13A 1.395(5) . ? C8A C9A 1.400(4) . ? C9A O4A 1.375(4) . ? C9A C10A 1.399(5) . ? C10A C11A 1.393(5) . ? C10A H10A 0.9500 . ? C11A C12A 1.390(5) . ? C11A H11A 0.9500 . ? C12A C13A 1.403(5) . ? C12A H12A 0.9500 . ? C13A H13A 0.9500 . ? O3A H3A 0.8400 . ? O4A H4A1 0.8400 . ? C8B O3B 1.372(4) . ? C8B C13B 1.386(5) . ? C8B C9B 1.414(5) . ? C9B O4B 1.376(4) . ? C9B C10B 1.389(4) . ? C10B C11B 1.403(5) . ? C10B H10B 0.9500 . ? C11B C12B 1.387(5) . ? C11B H11B 0.9500 . ? C12B C13B 1.397(5) . ? C12B H12B 0.9500 . ? C13B H13B 0.9500 . ? O3B H3B 0.8400 . ? O4B H4B1 0.8400 . ? C8C C9C 1.3900 . ? C8C C13C 1.3900 . ? C8C O3C 1.391(6) . ? C9C C10C 1.3900 . ? C9C H9C 0.9500 . ? C10C C11C 1.3900 . ? C10C H10C 0.9500 . ? C11C C12C 1.3900 . ? C11C H11C 0.9500 . ? C12C C13C 1.3900 . ? C12C H12C 0.9500 . ? C13C O4C 1.334(8) . ? O3C H3C 0.8400 . ? O4C H4C 0.8400 . ? C8' C9' 1.3900 . ? C8' C13' 1.3900 . ? C8' O3' 1.394(8) . ? C9' O4' 1.331(11) . ? C9' C10' 1.3900 . ? C10' C11' 1.3900 . ? C10' H10' 0.9500 . ? C11' C12' 1.3900 . ? C11' H11' 0.9500 . ? C12' C13' 1.3900 . ? C12' H12' 0.9500 . ? C13' H13' 0.9500 . ? O3' H3' 0.8400 . ? O4' H4' 0.8400 . ? 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 H1A O2B 0.84 1.95 2.702(3) 148.0 . yes O1B H1B O2A 0.84 1.81 2.617(4) 160.8 . yes O3A H3A O4A 0.84 2.28 2.726(3) 113.2 . yes O3A H3A O4B 0.84 2.06 2.833(4) 153.4 . yes O4A H4A1 O2B 0.84 1.88 2.702(3) 164.5 1_455 yes O3B H3B O4A 0.84 2.11 2.849(4) 145.8 . yes O3B H3B O4B 0.84 2.26 2.719(4) 114.5 . yes O4B H4B1 O2B 0.84 1.85 2.686(3) 175.3 . yes O3C^a^ H3C^a^ O2A 0.84 2.11 2.684(6) 125.3 . yes O3'^b^ H3'^b^ O2A 0.84 1.81 2.646(7) 174.3 . yes O4'^b^ H4'^b^ O3'^b^ 0.84 2.30 2.715(11) 110.8 . yes C5A H5A O1A 0.95 2.42 3.164(5) 135.0 1_455 yes C4B H4B O4A 0.95 2.56 3.223(4) 127.0 1_655 yes C5B H5B O1B 0.95 2.43 3.159(4) 133.2 1_655 yes C10C^a^ H10C^a^ O4C^a^ 0.95 2.37 3.112(9) 134.4 1_455 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 178.1(3) . . . . ? C7A C1A C2A O1A 0.7(5) . . . . ? N1A C1A C2A C3A 2.0(5) . . . . ? C7A C1A C2A C3A -175.4(3) . . . . ? O1A C2A C3A O2A -1.2(5) . . . . ? C1A C2A C3A O2A 174.9(3) . . . . ? O1A C2A C3A C4A -178.5(3) . . . . ? C1A C2A C3A C4A -2.4(5) . . . . ? O2A C3A C4A C5A -176.6(4) . . . . ? C2A C3A C4A C5A 0.6(5) . . . . ? C3A C4A C5A N1A 1.6(6) . . . . ? C4A C5A N1A C1A -2.1(6) . . . . ? C4A C5A N1A C6A 178.7(4) . . . . ? C2A C1A N1A C5A 0.3(5) . . . . ? C7A C1A N1A C5A 177.8(4) . . . . ? C2A C1A N1A C6A 179.5(4) . . . . ? C7A C1A N1A C6A -3.0(5) . . . . ? N1B C1B C2B O1B -177.3(3) . . . . ? C7B C1B C2B O1B 1.1(5) . . . . ? N1B C1B C2B C3B -0.8(5) . . . . ? C7B C1B C2B C3B 177.5(3) . . . . ? O1B C2B C3B O2B 0.7(5) . . . . ? C1B C2B C3B O2B -175.6(3) . . . . ? O1B C2B C3B C4B -179.7(3) . . . . ? C1B C2B C3B C4B 4.0(5) . . . . ? O2B C3B C4B C5B 176.1(3) . . . . ? C2B C3B C4B C5B -3.5(5) . . . . ? C3B C4B C5B N1B -0.2(5) . . . . ? C4B C5B N1B C1B 3.7(5) . . . . ? C4B C5B N1B C6B -177.5(3) . . . . ? C2B C1B N1B C5B -3.1(5) . . . . ? C7B C1B N1B C5B 178.5(3) . . . . ? C2B C1B N1B C6B 178.1(3) . . . . ? C7B C1B N1B C6B -0.3(5) . . . . ? O3A C8A C9A O4A 1.6(5) . . . . ? C13A C8A C9A O4A -178.4(3) . . . . ? O3A C8A C9A C10A 179.9(3) . . . . ? C13A C8A C9A C10A 0.0(5) . . . . ? O4A C9A C10A C11A 179.0(3) . . . . ? C8A C9A C10A C11A 0.8(5) . . . . ? C9A C10A C11A C12A -1.1(5) . . . . ? C10A C11A C12A C13A 0.6(6) . . . . ? O3A C8A C13A C12A 179.6(3) . . . . ? C9A C8A C13A C12A -0.5(5) . . . . ? C11A C12A C13A C8A 0.2(5) . . . . ? O3B C8B C9B O4B 2.6(5) . . . . ? C13B C8B C9B O4B -177.7(3) . . . . ? O3B C8B C9B C10B -178.0(3) . . . . ? C13B C8B C9B C10B 1.6(5) . . . . ? O4B C9B C10B C11B 178.3(3) . . . . ? C8B C9B C10B C11B -1.0(5) . . . . ? C9B C10B C11B C12B -0.4(5) . . . . ? C10B C11B C12B C13B 1.2(5) . . . . ? O3B C8B C13B C12B 178.8(3) . . . . ? C9B C8B C13B C12B -0.9(5) . . . . ? C11B C12B C13B C8B -0.6(5) . . . . ? C13C C8C C9C C10C 0.0 . . . . ? O3C C8C C9C C10C -179.7(7) . . . . ? C8C C9C C10C C11C 0.0 . . . . ? C9C C10C C11C C12C 0.0 . . . . ? C10C C11C C12C C13C 0.0 . . . . ? C11C C12C C13C O4C -179.1(6) . . . . ? C11C C12C C13C C8C 0.0 . . . . ? C9C C8C C13C O4C 179.0(7) . . . . ? O3C C8C C13C O4C -1.3(7) . . . . ? C9C C8C C13C C12C 0.0 . . . . ? O3C C8C C13C C12C 179.7(6) . . . . ? C13' C8' C9' O4' 178.4(8) . . . . ? O3' C8' C9' O4' 0.9(9) . . . . ? C13' C8' C9' C10' 0.0 . . . . ? O3' C8' C9' C10' -177.5(8) . . . . ? O4' C9' C10' C11' -178.5(8) . . . . ? C8' C9' C10' C11' 0.0 . . . . ? C9' C10' C11' C12' 0.0 . . . . ? C10' C11' C12' C13' 0.0 . . . . ? C11' C12' C13' C8' 0.0 . . . . ? C9' C8' C13' C12' 0.0 . . . . ? O3' C8' C13' C12' 177.3(9) . . . . ? _cod_database_fobs_code 2022890