#------------------------------------------------------------------------------ #$Date: 2023-09-01 10:42:42 +0300 (Fri, 01 Sep 2023) $ #$Revision: 285952 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/04/3000442.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3000442 loop_ _publ_author_name 'Gogoi, Diptajyoti' 'Sasaki, Toshiyuki' 'Nakane, Takanori' 'Kawamoto, Akihiro' 'Hojo, Hironobu' 'Kurisu, Genji' 'Thakuria, Ranjit' _publ_section_title ; Structure Elucidation of Olanzapine Molecular Salts by Combining Mechanochemistry and Micro-Electron Diffraction ; _journal_name_full 'Crystal Growth & Design' _journal_page_first 5821 _journal_page_last 5826 _journal_paper_doi 10.1021/acs.cgd.3c00432 _journal_volume 23 _journal_year 2023 _chemical_formula_moiety '2(C4 H5 O4), C5 H14 N2, H2 O' _chemical_formula_sum 'C13 H26 N2 O9' _chemical_formula_weight 354.36 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-05-11 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 104.04 _cell_angle_beta 97.60 _cell_angle_gamma 97.50 _cell_formula_units_Z 2 _cell_length_a 6.605 _cell_length_b 8.935 _cell_length_c 15.061 _cell_measurement_reflns_used 8948 _cell_measurement_temperature 79 _cell_measurement_theta_max 0.8980291984245176 _cell_measurement_theta_min 0.1560398850479103 _cell_volume 842.398 _computing_cell_refinement 'dials.two_theta_refine (Waterman et al., 2016)' _computing_data_collection 'Verlox (Thermo Fisher Scientific) and SerialEM (Mastronarde, 2005)' _computing_data_reduction 'dials.scale (Beilsten-Edmands et al., 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 79 _diffrn_measured_fraction_theta_full 0.872 _diffrn_measured_fraction_theta_max 0.872 _diffrn_measurement_device_type ; Talos Arctica G2 ; _diffrn_radiation_type electrons _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.3127 _diffrn_reflns_av_unetI/netI 0.5636 _diffrn_reflns_Laue_measured_fraction_full 0.872 _diffrn_reflns_Laue_measured_fraction_max 0.872 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 45547 _diffrn_reflns_point_group_measured_fraction_full 0.872 _diffrn_reflns_point_group_measured_fraction_max 0.872 _diffrn_reflns_theta_full 0.862 _diffrn_reflns_theta_max 0.898 _diffrn_reflns_theta_min 0.128 _diffrn_source electrons _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.397 _exptl_crystal_description plate _exptl_crystal_F_000 132 _refine_diff_density_max 0.221 _refine_diff_density_min -0.136 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef 10953(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 3004 _refine_ls_number_restraints 138 _refine_ls_restrained_S_all 1.172 _refine_ls_R_factor_all 0.2214 _refine_ls_R_factor_gt 0.1475 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4024 _refine_ls_wR_factor_ref 0.4200 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1338 _reflns_number_total 3004 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file SUCA.cif _cod_data_source_block suca _cod_depositor_comments 'Releasing structure 3000442 into public domain as published material.' _cod_original_cell_volume 842.2 _cod_database_code 3000442 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O9-H9C = O9-H9D 0.82 with sigma of 0.02 H9C-O9 \\sim O9-H9D with sigma of 0.02 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Ternary CH refined with riding coordinates: N2(H2) 4.b Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C7(H7A,H7B), C6(H6A,H6B), C9(H9A,H9B), C2(H2A,H2B), C10(H10A, H10B), N1(H1A,H1B), C3(H3A,H3B), C12(H12A,H12B) 4.c Tetrahedral OH refined with riding coordinates: O1(H1), O5(H5) 4.d Idealised Me refined as rotating group: C13(H13A,H13B,H13C) ; _shelx_res_file ; TITL suca_a.res in P-1 suca.res created by SHELXL-2018/3 at 10:23:51 on 11-May-2023 REM Old TITL SUCA in P-1 #2 REM SHELXT solution in P-1: R1 0.335, Rweak 0.075, Alpha 0.222 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N O4 CELL 0.02508 6.6045 8.9348 15.0605 104.045 97.604 97.504 ZERR 2 0 0 0 0 0 0 LATT 1 SFAC C 0.731 36.995 1.195 11.297 0.456 2.814 0.125 0.346 0 0 0 0 0.77 12.011 SFAC H 0.375 15.495 0.141 4.126 0.022 0.025 -0.101 46.884 0 0 0 0 0.32 1.008 SFAC N 0.572 28.846 1.042 9.054 0.465 2.421 0.131 0.317 0 0 0 0 0.75 14.007 SFAC O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999 UNIT 26 52 4 18 RIGU SADI H9c O9 O9 H9d DFIX 0.82 O9 H9c O9 H9d L.S. 10 PLAN 10 CONF LIST 6 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.200000 EXTI10953.228516 FVAR 2.60915 O7 4 1.066701 0.773156 0.142929 11.00000 0.03101 0.04160 = 0.05919 0.02291 0.01904 0.01361 C8 1 0.872139 0.771082 0.142189 11.00000 0.02326 0.02598 = 0.05087 0.00957 0.00455 0.00873 O1 4 0.974449 -0.094464 0.386053 11.00000 0.01960 0.03443 = 0.07637 0.02665 0.01408 0.01173 AFIX 83 H1 2 1.022027 -0.012553 0.375223 11.00000 -1.50000 AFIX 0 O6 4 0.552947 1.156877 0.105214 11.00000 0.02397 0.03572 = 0.08088 0.02759 0.00508 0.00639 N2 3 1.165088 0.494106 0.164276 11.00000 0.03339 0.02731 = 0.06617 0.02126 0.01550 0.02220 AFIX 13 H2 2 1.105121 0.588122 0.162095 11.00000 -1.20000 AFIX 0 C5 1 0.453460 1.040546 0.117068 11.00000 0.02875 0.02526 = 0.06016 0.00859 0.00984 0.00759 C1 1 0.777651 -0.092665 0.397191 11.00000 0.02760 0.03538 = 0.05628 0.02399 0.01574 0.02040 O5 4 0.253149 1.035703 0.120034 11.00000 0.02763 0.04340 = 0.07851 0.02751 0.01768 0.01486 AFIX 83 H5 2 0.202901 0.949317 0.124255 11.00000 -1.50000 AFIX 0 O9 4 0.781283 0.526268 0.460148 11.00000 0.02268 0.03314 = 0.10078 0.02583 0.00634 0.01145 C11 1 1.326436 0.531990 0.252013 11.00000 0.03047 0.02627 = 0.06188 0.02055 0.02019 0.01591 AFIX 23 H11A 2 1.432045 0.617797 0.251277 11.00000 -1.20000 H11B 2 1.392834 0.441626 0.252983 11.00000 -1.20000 AFIX 0 O4 4 0.151144 0.150629 0.350273 11.00000 0.02716 0.03013 = 0.07042 0.01832 0.00149 0.00529 C7 1 0.778952 0.916839 0.127801 11.00000 0.02519 0.02514 = 0.05897 0.01252 0.01255 0.01085 AFIX 23 H7A 2 0.842531 1.006931 0.178827 11.00000 -1.20000 H7B 2 0.813207 0.938323 0.070947 11.00000 -1.20000 AFIX 0 O2 4 0.672348 -0.206641 0.411185 11.00000 0.03501 0.04419 = 0.07609 0.02783 0.01021 0.00678 C6 1 0.545484 0.895782 0.122310 11.00000 0.03196 0.03163 = 0.04148 0.01129 0.01482 0.00771 AFIX 23 H6A 2 0.481835 0.811508 0.067954 11.00000 -1.20000 H6B 2 0.510857 0.864385 0.176504 11.00000 -1.20000 AFIX 0 O3 4 0.465263 0.286834 0.360711 11.00000 0.03407 0.02841 = 0.11425 0.02686 0.01403 0.01439 C9 1 0.900149 0.411227 0.255313 11.00000 0.01859 0.03159 = 0.07313 0.02440 0.01109 0.00191 AFIX 23 H9A 2 0.830349 0.499982 0.254348 11.00000 -1.20000 H9B 2 0.797578 0.323216 0.255637 11.00000 -1.20000 AFIX 0 C2 1 0.685054 0.048470 0.386717 11.00000 0.02260 0.04337 = 0.07862 0.03145 0.01921 0.01487 AFIX 23 H2A 2 0.730088 0.080137 0.334277 11.00000 -1.20000 H2B 2 0.738388 0.133845 0.441879 11.00000 -1.20000 AFIX 0 C10 1 0.999511 0.370804 0.170100 11.00000 0.03091 0.02990 = 0.05897 0.01500 0.00402 0.01397 AFIX 23 H10A 2 1.056946 0.275971 0.169000 11.00000 -1.20000 H10B 2 0.893098 0.348786 0.115517 11.00000 -1.20000 AFIX 0 C13 1 1.267103 0.453539 0.085713 11.00000 0.04146 0.03324 = 0.06371 0.01843 0.01239 0.00363 AFIX 137 H13A 2 1.390749 0.528626 0.094053 11.00000 -1.50000 H13B 2 1.176109 0.453541 0.030446 11.00000 -1.50000 H13C 2 1.302819 0.351261 0.079988 11.00000 -1.50000 AFIX 0 C4 1 0.355044 0.165177 0.362189 11.00000 0.02161 0.03761 = 0.07130 0.02638 0.00972 0.01366 O8 4 0.749398 0.656327 0.150269 11.00000 0.03684 0.04171 = 0.09482 0.04398 0.01976 0.01518 N1 3 1.061886 0.450415 0.341268 11.00000 0.04158 0.02765 = 0.05133 0.01697 0.01439 0.01780 AFIX 23 H1A 2 1.002819 0.479888 0.391052 11.00000 -1.20000 H1B 2 1.115595 0.365404 0.345063 11.00000 -1.20000 AFIX 0 C3 1 0.451812 0.022607 0.372342 11.00000 0.02535 0.02625 = 0.07152 0.02357 0.01692 0.00988 AFIX 23 H3A 2 0.407158 -0.009983 0.424581 11.00000 -1.20000 H3B 2 0.398884 -0.062513 0.317009 11.00000 -1.20000 AFIX 0 C12 1 1.230003 0.577414 0.340872 11.00000 0.02875 0.03343 = 0.05367 0.00804 0.00626 0.01758 AFIX 23 H12A 2 1.335935 0.595564 0.395258 11.00000 -1.20000 H12B 2 1.174744 0.673437 0.343241 11.00000 -1.20000 AFIX 0 H9C 2 0.667693 0.465717 0.440858 11.00000 0.04513 H9D 2 0.744710 0.609333 0.453957 11.00000 0.15739 HKLF 4 REM suca_a.res in P-1 REM wR2 = 0.4200, GooF = S = 1.195, Restrained GooF = 1.172 for all data REM R1 = 0.1475 for 1338 Fo > 4sig(Fo) and 0.2214 for all 3004 data REM 227 parameters refined using 138 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.221, deepest hole -0.136, 1-sigma level 0.048 Q1 1 1.1907 0.5235 0.2583 11.00000 0.05 0.22 Q2 1 1.2955 0.5138 0.1655 11.00000 0.05 0.19 Q3 1 1.3264 0.4216 0.0143 11.00000 0.05 0.18 Q4 1 1.2093 0.4534 0.1822 11.00000 0.05 0.17 Q5 1 0.3705 1.0568 0.1192 11.00000 0.05 0.17 Q6 1 0.9296 0.4211 0.3632 11.00000 0.05 0.16 Q7 1 0.9601 0.4513 0.4008 11.00000 0.05 0.15 Q8 1 1.1404 0.5518 0.3359 11.00000 0.05 0.14 Q9 1 1.1379 0.5207 0.3878 11.00000 0.05 0.14 Q10 1 1.2585 0.5348 0.3326 11.00000 0.05 0.14 ; _shelx_res_checksum 80338 _shelx_hkl_file ; -2 -7 -1 9.68 18.80 -7 -4 3 0.55 8.02 7 -4 -6 3.04 9.40 -6 1 4 1.11 5.81 -5 3 4 12.44 13.27 -3 -9 -1 1.11 5.53 -4 -8 0 0.00 6.36 -5 -7 1 0.83 5.25 2 -9 -4 7.47 9.13 1 -8 -3 7.47 9.95 -3 -6 0 2.77 6.36 4 -8 -5 1.11 7.74 -4 -5 1 118.07 13.27 3 -7 -4 6.91 9.68 -3 -3 1 389.34 29.59 8 -2 -6 0.00 2.49 -6 5 5 2.21 6.08 -3 4 3 11.06 7.47 -4 6 4 299.47 25.99 -1 5 2 16.87 8.85 -5 7 5 21.85 7.19 2 5 0 5.53 8.30 6 4 -3 1.11 4.42 -2 7 3 7.47 10.23 1 6 1 15.21 8.57 5 5 -2 1.66 4.98 -3 8 4 3.04 8.30 0 8 2 2.21 9.95 -1 9 3 2.49 7.19 3 8 0 19.91 9.40 -1 10 3 6.64 8.57 2 9 1 0.55 6.91 -1 -9 -2 3.32 8.57 -2 -8 -1 1.66 8.30 -6 -6 2 0.55 4.98 -3 -7 0 4.70 9.13 4 -9 -5 3.87 7.74 -1 -6 -1 24.06 10.78 -5 -4 2 8.85 6.08 -2 -5 0 4.70 9.68 2 -6 -3 6.64 9.95 6 -7 -6 1.38 6.36 1 -5 -2 15.21 9.95 5 -6 -5 13.83 8.57 4 -5 -4 5.53 8.57 -7 -1 4 0.55 1.66 -4 -2 2 1.38 4.42 3 -4 -3 30.69 9.68 7 -5 -6 3.59 4.98 -2 -1 1 220.94 16.04 -7 3 5 3.04 3.87 -4 2 3 1.66 4.42 7 -1 -5 2.49 1.94 -5 4 4 137.15 14.10 -2 3 2 38.99 9.40 -3 5 3 31.25 10.51 0 4 1 0.28 8.57 3 4 -1 3.87 7.47 7 3 -4 0.00 2.77 -1 6 2 9.68 11.61 -5 8 5 6.91 7.74 2 6 0 22.40 10.51 -2 8 3 8.02 11.06 1 7 1 70.24 13.55 5 6 -2 1.94 6.36 -3 9 4 0.55 8.30 4 7 -1 0.55 7.19 0 9 2 1.66 8.85 3 9 0 2.21 7.74 -2 -9 -1 0.55 8.57 1 -10 -3 4.98 7.74 -3 -8 0 20.19 8.30 1 -9 -3 1.94 9.68 -4 -6 1 44.52 9.95 -1 -7 -1 63.60 12.72 3 -8 -4 1.11 9.13 2 -7 -3 5.81 10.51 1 -6 -2 10.23 10.78 5 -7 -5 18.53 8.85 -6 -3 3 0.55 4.15 -3 -4 1 3.59 8.57 4 -6 -4 271.82 23.50 2 -3 -2 37.61 9.68 6 -4 -5 1.38 5.81 5 -3 -4 88.49 10.23 1 3 0 114.48 13.00 -6 6 5 2.21 6.64 4 3 -2 8.02 5.81 -6 7 5 0.55 6.64 0 5 1 25.72 11.06 -4 7 4 33.46 10.51 3 5 -1 20.19 9.40 -4 8 4 11.61 8.30 -1 7 2 0.83 10.23 6 5 -3 0.55 5.25 2 7 0 4.70 9.13 -2 9 3 1.38 7.74 1 8 1 2.77 10.23 5 7 -2 0.83 6.64 1 9 1 0.55 8.30 4 8 -1 6.36 7.47 0 10 2 0.28 8.57 -3 -9 0 2.21 6.91 -4 -7 1 0.00 7.47 -1 -8 -1 4.98 9.13 3 -9 -4 2.21 7.74 2 -8 -3 8.30 8.30 -5 -5 2 4.15 6.64 -2 -6 0 20.19 10.78 5 -8 -5 5.25 7.47 4 -7 -4 29.86 9.13 3 -5 -3 29.86 10.51 -1 -3 0 107.01 12.44 6 -5 -5 1.11 6.64 -8 1 5 11.06 2.21 4 -2 -3 18.53 6.08 -7 4 5 1.94 4.98 -4 3 3 5.53 6.91 -1 2 1 265.46 21.02 -5 5 4 60.28 9.95 -2 4 2 297.54 25.16 -3 6 3 6.36 9.68 -3 7 3 5.53 9.40 0 6 1 6.91 10.51 7 4 -4 0.00 3.59 3 6 -1 30.69 9.13 -4 9 4 1.11 8.02 -1 8 2 6.91 10.23 6 6 -3 0.55 5.81 -1 9 2 1.38 8.85 2 8 0 24.06 9.40 -2 10 3 5.25 8.02 1 10 1 0.83 7.47 -4 -8 1 4.98 7.47 -1 -9 -1 0.55 8.57 2 -9 -3 1.38 8.30 -5 -6 2 5.81 6.36 -2 -7 0 8.30 10.51 1 -7 -2 1.38 10.23 4 -8 -4 7.74 8.02 -6 -4 3 1.94 5.25 -3 -5 1 18.80 9.40 3 -6 -3 11.61 9.68 -4 -3 2 7.74 7.19 6 -6 -5 1.94 6.64 2 -4 -2 279.84 24.06 5 -4 -4 141.86 13.83 1 -2 -1 257.99 20.19 -6 2 4 5.53 4.42 -7 5 5 0.55 5.53 2 2 -1 859.43 58.90 5 2 -3 17.97 4.70 -5 6 4 8.57 8.30 -2 5 2 84.06 14.38 1 4 0 73.83 11.89 -5 7 4 0.00 7.19 4 4 -2 23.78 7.74 -3 8 3 6.08 9.95 0 7 1 166.74 18.80 -3 9 3 3.87 8.57 0 8 1 102.59 14.93 3 7 -1 5.81 9.13 -1 10 2 4.70 8.02 2 9 0 11.34 8.02 -1 -10 -1 1.38 7.74 2 -10 -3 4.15 8.02 -5 -7 2 1.94 6.91 -2 -8 0 27.38 11.06 1 -9 -2 2.77 9.95 1 -8 -2 6.08 9.95 4 -9 -4 2.21 8.02 -3 -6 1 58.07 11.89 3 -7 -3 8.85 9.95 6 -7 -5 2.77 7.19 -1 -4 0 67.47 11.61 2 -5 -2 87.66 13.83 5 -5 -4 42.86 9.40 -2 -2 1 846.71 58.07 -3 1 2 573.78 39.27 7 -2 -5 40.65 5.25 -4 4 3 3.59 8.30 -1 3 1 63.05 10.51 -7 6 5 0.00 5.53 -2 6 2 6.36 10.51 1 5 0 5.25 9.68 -5 8 4 2.21 8.02 -2 7 2 11.06 11.06 1 6 0 55.30 12.44 4 5 -2 13.00 8.57 4 6 -2 6.36 8.30 -3 10 3 6.08 7.74 0 9 1 15.49 10.23 3 8 -1 2.49 7.74 0 10 1 1.11 8.85 3 9 -1 1.38 8.30 -2 -9 0 21.02 9.40 1 -10 -2 6.64 8.85 -3 -7 1 12.44 10.51 3 -9 -3 0.28 9.95 -6 -5 3 1.94 6.36 3 -8 -3 4.98 9.95 -4 -4 2 21.85 8.85 -1 -5 0 6.91 10.23 2 -6 -2 11.61 11.61 -7 -2 4 0.28 3.32 5 -6 -4 3.87 8.57 1 -3 -1 37.88 9.40 4 -3 -3 2.21 7.19 -8 2 5 0.55 3.59 7 -3 -5 2.77 4.98 -6 3 4 18.53 6.36 -6 4 4 2.77 6.91 -4 5 3 56.69 11.61 -1 4 1 1436.53 99.27 2 3 -1 29.86 8.57 -4 6 3 212.64 20.74 5 3 -3 12.44 6.36 -4 7 3 3.32 9.68 -2 8 2 26.55 11.61 1 7 0 92.63 14.93 -2 9 2 74.38 13.55 1 8 0 71.34 13.83 4 7 -2 5.81 8.85 -2 10 2 55.30 12.17 1 9 0 2.21 10.51 4 8 -2 3.32 8.57 1 10 0 1.38 9.40 -3 -9 1 5.81 9.40 -3 -8 1 1.94 8.85 3 -10 -3 3.87 9.40 -6 -6 3 1.11 6.64 -1 -7 0 115.03 16.87 2 -8 -2 24.33 12.72 -4 -5 2 19.63 9.13 -1 -6 0 85.17 14.66 2 -7 -2 2.49 11.34 5 -8 -4 0.83 9.13 -7 -3 4 1.38 4.70 5 -7 -4 1.11 9.68 -2 -3 1 76.32 10.78 1 -4 -1 1394.22 96.78 4 -5 -3 35.95 10.51 4 -4 -3 19.08 9.40 7 -4 -5 1.38 6.36 -8 3 5 0.28 4.98 -3 2 2 352.84 26.55 -6 5 4 16.04 8.02 -6 6 4 1.38 8.30 -6 7 4 1.11 8.57 -1 5 1 728.36 54.20 2 4 -1 41.20 10.78 -1 6 1 199.37 21.02 2 5 -1 48.11 12.44 5 4 -3 39.54 8.85 -4 8 3 53.92 12.17 -1 7 1 53.65 14.38 2 6 -1 4.15 10.51 5 5 -3 1.38 8.30 -4 9 3 0.55 9.13 -1 8 1 21.57 13.00 5 6 -3 1.66 8.30 -1 9 1 6.08 11.89 5 7 -3 0.55 8.85 -1 -9 0 3.87 11.89 2 -10 -2 60.28 13.83 -4 -7 2 2.49 9.95 -1 -8 0 59.18 14.10 2 -9 -2 70.79 14.66 -4 -6 2 8.57 9.95 -7 -4 4 0.83 5.53 1 -6 -1 185.82 21.02 4 -7 -3 11.61 11.34 -2 -4 1 17.14 10.23 1 -5 -1 778.13 57.52 4 -6 -3 208.22 21.57 7 -6 -5 0.55 8.30 -5 -1 3 16.04 3.32 7 -5 -5 1.66 7.74 3 -1 -2 623.00 42.58 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1 10.23 33.46 -1 9 2 0.00 17.42 0 9 2 1.38 22.12 1 9 2 4.42 24.33 3 8 2 0.83 30.42 -5 -7 -1 3.59 30.97 -4 -8 -1 4.70 34.01 -4 -7 -1 3.32 35.95 -3 -7 -1 86.83 38.99 -2 -7 -1 6.91 37.05 -2 -6 -1 15.49 33.74 -1 -6 -1 31.52 29.03 0 -6 -1 6.91 22.95 1 -6 -1 199.37 24.61 6 -7 -1 9.40 21.29 7 -7 -1 0.00 22.67 -7 -2 0 6.08 40.10 -7 -1 0 0.83 36.50 -6 -2 0 4.70 41.48 -6 -1 0 0.83 35.39 -5 -1 0 10.23 41.75 -4 -1 0 61.39 38.16 -2 0 0 253.57 31.80 2 0 0 361.97 39.82 3 0 0 93.74 31.25 4 0 0 177.25 39.82 5 0 0 0.00 35.95 6 -1 0 2.21 32.63 7 -1 0 13.83 38.44 8 -2 0 1.94 29.59 8 -1 0 6.36 36.22 -8 3 1 3.32 33.46 -7 4 1 11.61 30.14 -6 4 1 2.21 32.35 -1 5 1 618.85 47.29 0 5 1 26.27 22.40 1 5 1 19.63 27.38 2 5 1 48.67 34.57 3 5 1 10.78 36.78 4 5 1 7.19 37.05 5 5 1 -0.55 38.44 -5 9 2 0.28 13.83 2 9 2 9.68 29.31 -3 -9 -1 3.04 38.99 -3 -8 -1 10.23 39.82 -2 -8 -1 0.83 35.12 -1 -7 -1 39.27 33.18 0 -7 -1 227.30 39.54 3 -6 -1 3.87 9.40 4 -6 -1 26.27 18.80 5 -6 -1 19.91 23.78 6 -6 -1 11.89 30.42 7 -6 -1 0.83 34.57 -7 -3 0 1.66 41.48 -6 -3 0 70.24 54.47 -5 -2 0 59.18 44.24 -4 -2 0 133.56 46.18 -3 -1 0 1.66 29.86 4 1 0 66.37 43.69 5 1 0 5.81 44.80 6 0 0 0.55 38.44 6 1 0 0.28 46.73 7 0 0 1.11 37.33 7 1 0 -3.87 50.33 8 0 0 1.94 44.80 -8 2 1 1.66 44.24 -7 3 1 22.40 41.48 -6 3 1 25.72 39.82 -5 4 1 372.75 48.67 2 6 1 12.72 36.50 3 6 1 2.21 39.54 4 6 1 3.04 43.97 5 6 1 -1.11 46.46 -1 10 2 6.64 25.44 0 10 2 -0.28 25.72 -2 -9 -1 -1.11 43.41 -1 -9 -1 47.84 49.77 -1 -8 -1 13.55 38.99 0 -8 -1 101.21 43.14 1 -7 -1 48.39 28.48 5 -5 -1 189.69 41.48 6 -5 -1 19.63 34.29 7 -5 -1 -0.28 39.82 7 -4 -1 0.00 61.11 -6 -5 0 21.57 71.34 -6 -4 0 12.17 50.88 -5 -4 0 120.56 68.85 -5 -3 0 129.41 56.41 -4 -3 0 267.95 61.11 -3 -2 0 38.44 42.86 5 2 0 71.07 56.41 6 2 0 5.53 62.77 7 2 0 0.83 65.26 -8 0 1 19.63 68.58 -8 1 1 -2.77 45.90 -7 1 1 110.61 66.64 -7 2 1 19.91 44.80 -6 2 1 97.89 53.92 -5 3 1 660.89 72.73 -4 4 1 163.98 32.63 0 6 1 8.85 30.97 1 6 1 12.44 35.95 3 7 1 78.53 54.75 4 7 1 4.15 57.24 5 7 1 4.70 58.07 -6 8 2 46.18 33.18 -2 10 2 33.46 22.95 -1 -10 -1 2.21 70.51 0 -9 -1 20.74 58.07 4 -5 -1 155.96 28.76 5 -4 -1 400.13 64.98 6 -4 -1 8.85 53.92 6 -3 -1 68.85 69.96 7 -3 -1 23.78 70.79 8 -3 -1 3.59 87.66 8 -2 -1 14.93 97.34 -5 -7 0 1.11 100.10 -5 -6 0 3.04 88.76 -5 -5 0 106.18 76.32 -4 -5 0 9.68 68.02 -4 -4 0 36.50 58.35 -3 -3 0 150.43 53.65 -2 -2 0 941.00 81.57 6 3 0 88.21 78.53 7 3 0 0.28 75.21 -7 -1 1 17.42 90.42 -7 0 1 36.50 86.55 -6 1 1 113.37 71.62 -5 2 1 38.71 50.05 -4 3 1 49.50 38.44 -3 4 1 36.78 24.06 1 7 1 40.37 52.26 2 7 1 9.13 54.75 3 8 1 5.53 74.66 4 8 1 14.66 95.95 -7 6 2 11.61 75.21 0 -10 -1 9.68 71.62 1 -8 -1 25.16 38.99 3 -5 -1 61.66 22.95 4 -4 -1 329.89 47.84 5 -3 -1 513.22 73.55 6 -2 -1 119.18 76.87 7 -2 -1 24.06 95.40 7 -1 -1 191.35 106.74 8 -1 -1 33.46 129.96 8 0 -1 -1.94 132.45 -4 -7 0 4.15 102.31 -4 -6 0 3.87 89.04 -3 -5 0 18.80 57.79 -3 -4 0 7.74 48.94 -2 -3 0 6.64 32.91 5 5 0 97.06 93.74 -7 -3 1 17.97 126.92 -7 -2 1 14.10 97.06 -6 -1 1 30.69 80.47 -6 0 1 21.02 72.45 -5 1 1 4.15 56.96 -1 6 1 207.39 33.46 0 7 1 158.17 51.99 1 8 1 25.16 67.19 2 8 1 12.72 75.49 3 9 1 17.14 114.20 -8 3 2 68.85 115.59 -7 5 2 3.32 91.80 -6 7 2 19.63 58.35 -5 8 2 2.77 44.24 -4 9 2 2.21 4.42 -3 10 2 8.57 11.34 1 -9 -1 17.97 54.20 4 -3 -1 36.50 38.71 5 -2 -1 27.93 55.03 6 -1 -1 149.04 86.27 6 0 -1 23.78 77.98 7 0 -1 47.01 102.87 7 1 -1 5.81 113.10 -4 -8 0 6.08 113.10 -3 -7 0 -2.49 86.55 -3 -6 0 3.87 73.83 -2 -4 0 14.93 41.75 -1 -2 0 606.41 51.71 2 3 0 0.55 35.39 3 4 0 8.02 56.96 4 5 0 1.11 86.55 5 6 0 16.59 131.07 -7 -4 1 5.81 138.26 -6 -4 1 1.38 113.93 -6 -3 1 -5.53 102.04 -6 -2 1 9.40 88.49 -5 -1 1 4.70 62.49 -5 0 1 9.13 57.24 -4 2 1 37.05 42.31 2 9 1 2.49 104.80 -8 1 2 -15.49 130.24 -8 2 2 45.90 142.13 -7 4 2 9.13 90.70 -6 6 2 56.96 73.55 1 -10 -1 4.15 71.07 2 -7 -1 19.08 14.66 3 -4 -1 11.34 22.95 4 -2 -1 26.82 38.44 5 -1 -1 1.11 53.37 5 0 -1 8.57 64.15 6 1 -1 7.74 94.29 6 2 -1 11.61 95.12 7 2 -1 5.81 124.99 7 3 -1 7.19 138.26 -3 -9 0 -3.04 125.26 -3 -8 0 17.97 107.57 -2 -6 0 8.30 57.52 -2 -5 0 9.40 47.29 2 4 0 6.91 40.65 3 5 0 6.91 65.54 4 6 0 2.49 88.21 4 7 0 7.47 103.97 5 7 0 12.44 134.94 -6 -6 1 -3.87 174.48 -6 -5 1 4.42 129.96 -5 -3 1 1.94 78.81 -5 -2 1 2.49 69.13 -4 0 1 14.38 42.31 -4 1 1 9.40 37.61 -3 3 1 14.10 25.44 0 8 1 161.21 61.94 1 9 1 12.44 85.17 -8 -1 2 -12.72 153.75 -8 0 2 -1.66 159.28 -7 2 2 -4.15 101.21 -7 3 2 9.95 99.82 -6 5 2 -6.64 74.94 -5 7 2 3.87 53.92 7 -6 -2 11.89 108.40 7 -5 -2 0.00 100.93 8 -3 -2 30.69 137.15 8 -2 -2 17.97 127.48 4 -1 -1 8.85 41.48 5 1 -1 -4.70 62.49 5 2 -1 8.30 69.41 6 3 -1 0.00 104.52 7 4 -1 -14.10 155.40 -2 -9 0 6.64 97.06 -2 -8 0 20.46 80.74 -2 -7 0 8.85 67.19 -1 -3 0 86.00 26.82 2 5 0 6.08 47.84 3 6 0 -4.70 67.19 3 7 0 6.64 88.76 4 8 0 -1.66 139.37 -5 -7 1 -2.21 130.24 -5 -6 1 1.11 126.65 -5 -5 1 12.72 111.99 -5 -4 1 9.40 91.25 -4 -2 1 11.06 52.54 -4 -1 1 1.38 51.71 -3 2 1 4.42 25.99 -1 7 1 36.78 34.84 0 9 1 15.76 68.58 1 10 1 -0.28 103.70 -7 -1 2 22.12 109.50 -7 0 2 15.76 117.24 -7 1 2 37.33 100.38 -6 3 2 28.21 71.62 -6 4 2 9.68 73.83 -5 6 2 15.76 52.54 6 -8 -2 47.01 78.26 6 -7 -2 -1.11 78.81 7 -4 -2 10.51 104.52 7 -3 -2 0.00 98.16 7 -2 -2 2.49 103.14 8 -1 -2 13.55 151.26 8 0 -2 3.04 159.83 8 1 -2 4.98 150.15 2 -8 -1 17.14 23.50 3 -3 -1 16.87 25.72 4 0 -1 9.40 41.48 4 1 -1 2.21 48.67 6 6 -1 8.57 146.28 -1 -5 0 -1.11 38.16 -1 -4 0 57.52 33.46 1 3 0 80.47 27.10 2 6 0 14.66 57.79 3 8 0 8.57 106.18 -4 -5 1 27.65 77.70 -4 -4 1 6.36 69.41 -4 -3 1 94.85 64.71 -3 1 1 451.28 51.43 0 10 1 -0.83 91.80 -7 -4 2 -19.91 167.02 -7 -3 2 2.77 133.01 -7 -2 2 14.38 120.29 -6 1 2 44.80 83.51 -6 2 2 27.65 76.32 -5 5 2 11.34 55.03 6 -6 -2 34.84 77.98 6 -5 -2 -9.95 79.91 6 -4 -2 -2.21 77.43 7 -1 -2 28.48 117.24 7 0 -2 -2.49 120.01 7 1 -2 -13.83 119.73 2 -10 -1 -0.83 55.58 2 -9 -1 14.93 42.58 3 -2 -1 8.02 27.65 3 -1 -1 472.85 54.75 5 6 -1 -7.74 126.92 -1 -10 0 1.38 110.61 -1 -9 0 6.36 93.74 -1 -8 0 50.33 77.15 -1 -7 0 97.89 60.01 -1 -6 0 58.90 50.33 1 4 0 58.62 32.35 2 7 0 -1.11 70.24 2 8 0 4.98 95.40 3 9 0 5.53 136.88 -4 -8 1 -8.57 133.28 -4 -7 1 3.32 113.10 -4 -6 1 22.95 86.55 -3 0 1 17.14 35.12 -1 8 1 14.38 45.35 -6 -4 2 17.14 120.01 -6 -3 2 -6.36 106.74 -6 -2 2 87.93 101.48 -6 -1 2 -1.94 98.16 -6 0 2 11.61 78.81 -5 4 2 33.74 59.73 -4 8 2 7.74 21.57 -8 1 3 5.81 137.71 -8 2 3 -23.78 144.34 -8 3 3 0.83 134.94 6 -3 -2 4.15 86.83 6 -2 -2 8.57 89.87 6 -1 -2 39.82 104.25 7 2 -2 10.78 126.92 7 3 -2 2.77 139.92 3 0 -1 20.46 42.58 3 1 -1 29.03 52.26 4 5 -1 19.36 100.93 5 7 -1 4.70 133.01 1 5 0 1.38 41.48 2 9 0 20.46 113.37 -3 -3 1 403.17 81.85 -3 -2 1 92.91 58.62 -3 -1 1 23.78 39.54 -6 -6 2 6.91 153.47 -6 -5 2 19.91 134.39 -5 2 2 3.32 66.64 -5 3 2 165.91 68.58 -8 -1 3 -2.49 156.51 -8 0 3 13.55 144.07 -7 5 3 6.36 124.43 -7 6 3 -4.42 119.73 -3 -5 1 22.95 82.68 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 17302 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 O7 O 1.0667(9) 0.7732(7) 0.1429(7) 0.040(3) Uani 1 1 d . . . . . C8 C 0.8721(9) 0.7711(7) 0.1422(8) 0.033(3) Uani 1 1 d . . . . . O1 O 0.9744(8) -0.0945(7) 0.3861(7) 0.040(3) Uani 1 1 d . . . . . H1 H 1.022027 -0.012553 0.375223 0.060 Uiso 1 1 calc R U . . . O6 O 0.5529(8) 1.1569(7) 0.1052(7) 0.045(3) Uani 1 1 d . . . . . N2 N 1.1651(9) 0.4941(7) 0.1643(7) 0.038(2) Uani 1 1 d . . . . . H2 H 1.105121 0.588122 0.162095 0.046 Uiso 1 1 calc R U . . . C5 C 0.4535(10) 1.0405(7) 0.1171(8) 0.038(3) Uani 1 1 d . . . . . C1 C 0.7777(10) -0.0927(8) 0.3972(8) 0.035(3) Uani 1 1 d . . . . . O5 O 0.2531(9) 1.0357(7) 0.1200(7) 0.046(3) Uani 1 1 d . . . . . H5 H 0.202901 0.949317 0.124255 0.069 Uiso 1 1 calc R U . . . O9 O 0.7813(9) 0.5263(7) 0.4601(8) 0.051(3) Uani 1 1 d D . . . . C11 C 1.3264(10) 0.5320(7) 0.2520(8) 0.036(2) Uani 1 1 d . . . . . H11A H 1.432045 0.617797 0.251277 0.043 Uiso 1 1 calc R U . . . H11B H 1.392834 0.441626 0.252983 0.043 Uiso 1 1 calc R U . . . O4 O 0.1511(8) 0.1506(6) 0.3503(7) 0.042(3) Uani 1 1 d . . . . . C7 C 0.7790(9) 0.9168(7) 0.1278(8) 0.035(3) Uani 1 1 d . . . . . H7A H 0.842531 1.006931 0.178827 0.042 Uiso 1 1 calc R U . . . H7B H 0.813207 0.938323 0.070947 0.042 Uiso 1 1 calc R U . . . O2 O 0.6723(9) -0.2066(7) 0.4112(8) 0.050(3) Uani 1 1 d . . . . . C6 C 0.5455(10) 0.8958(8) 0.1223(7) 0.034(3) Uani 1 1 d . . . . . H6A H 0.481835 0.811508 0.067954 0.040 Uiso 1 1 calc R U . . . H6B H 0.510857 0.864385 0.176504 0.040 Uiso 1 1 calc R U . . . O3 O 0.4653(9) 0.2868(7) 0.3607(8) 0.057(3) Uani 1 1 d . . . . . C9 C 0.9001(10) 0.4112(8) 0.2553(8) 0.039(2) Uani 1 1 d . . . . . H9A H 0.830349 0.499982 0.254348 0.047 Uiso 1 1 calc R U . . . H9B H 0.797578 0.323216 0.255637 0.047 Uiso 1 1 calc R U . . . C2 C 0.6851(9) 0.0485(8) 0.3867(8) 0.044(3) Uani 1 1 d . . . . . H2A H 0.730088 0.080137 0.334277 0.052 Uiso 1 1 calc R U . . . H2B H 0.738388 0.133845 0.441879 0.052 Uiso 1 1 calc R U . . . C10 C 0.9995(10) 0.3708(7) 0.1701(8) 0.039(2) Uani 1 1 d . . . . . H10A H 1.056946 0.275971 0.169000 0.047 Uiso 1 1 calc R U . . . H10B H 0.893098 0.348786 0.115517 0.047 Uiso 1 1 calc R U . . . C13 C 1.2671(12) 0.4535(8) 0.0857(9) 0.045(2) Uani 1 1 d . . . . . H13A H 1.390749 0.528626 0.094053 0.068 Uiso 1 1 calc R U . . . H13B H 1.176109 0.453541 0.030446 0.068 Uiso 1 1 calc R U . . . H13C H 1.302819 0.351261 0.079988 0.068 Uiso 1 1 calc R U . . . C4 C 0.3550(10) 0.1652(8) 0.3622(8) 0.040(3) Uani 1 1 d . . . . . O8 O 0.7494(9) 0.6563(7) 0.1503(8) 0.052(3) Uani 1 1 d . . . . . N1 N 1.0619(9) 0.4504(7) 0.3413(7) 0.037(2) Uani 1 1 d . . . . . H1A H 1.002819 0.479888 0.391052 0.045 Uiso 1 1 calc R U . . . H1B H 1.115595 0.365404 0.345063 0.045 Uiso 1 1 calc R U . . . C3 C 0.4518(9) 0.0226(7) 0.3723(8) 0.038(3) Uani 1 1 d . . . . . H3A H 0.407158 -0.009983 0.424581 0.045 Uiso 1 1 calc R U . . . H3B H 0.398884 -0.062513 0.317009 0.045 Uiso 1 1 calc R U . . . C12 C 1.2300(11) 0.5774(8) 0.3409(8) 0.038(2) Uani 1 1 d . . . . . H12A H 1.335935 0.595564 0.395258 0.046 Uiso 1 1 calc R U . . . H12B H 1.174744 0.673437 0.343241 0.046 Uiso 1 1 calc R U . . . H9C H 0.668(4) 0.466(4) 0.441(4) 0.045(11) Uiso 1 1 d D . . . . H9D H 0.745(13) 0.609(7) 0.454(9) 0.16(3) Uiso 1 1 d 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 O7 0.031(3) 0.042(3) 0.059(8) 0.023(4) 0.019(4) 0.014(2) C8 0.023(3) 0.026(3) 0.051(9) 0.010(4) 0.005(4) 0.009(2) O1 0.020(2) 0.034(3) 0.076(8) 0.027(4) 0.014(3) 0.012(2) O6 0.024(3) 0.036(3) 0.081(9) 0.028(4) 0.005(4) 0.006(2) N2 0.033(3) 0.027(3) 0.066(6) 0.021(4) 0.015(3) 0.022(2) C5 0.029(3) 0.025(3) 0.060(10) 0.009(4) 0.010(4) 0.008(3) C1 0.028(3) 0.035(4) 0.056(9) 0.024(5) 0.016(4) 0.020(3) O5 0.028(3) 0.043(3) 0.079(9) 0.028(4) 0.018(4) 0.015(2) O9 0.023(3) 0.033(3) 0.101(10) 0.026(5) 0.006(4) 0.011(2) C11 0.030(3) 0.026(3) 0.062(7) 0.021(4) 0.020(4) 0.016(3) O4 0.027(3) 0.030(3) 0.070(8) 0.018(4) 0.001(3) 0.005(2) C7 0.025(3) 0.025(3) 0.059(9) 0.013(4) 0.013(4) 0.011(3) O2 0.035(3) 0.044(3) 0.076(10) 0.028(5) 0.010(4) 0.007(3) C6 0.032(3) 0.032(3) 0.041(9) 0.011(4) 0.015(4) 0.008(3) O3 0.034(3) 0.028(3) 0.114(11) 0.027(4) 0.014(4) 0.014(2) C9 0.019(3) 0.032(3) 0.073(8) 0.024(4) 0.011(4) 0.002(3) C2 0.023(3) 0.043(4) 0.079(11) 0.031(5) 0.019(4) 0.015(3) C10 0.031(3) 0.030(3) 0.059(7) 0.015(4) 0.004(4) 0.014(3) C13 0.041(4) 0.033(4) 0.064(8) 0.018(5) 0.012(5) 0.004(3) C4 0.022(3) 0.038(4) 0.071(10) 0.026(5) 0.010(4) 0.014(3) O8 0.037(3) 0.042(3) 0.095(10) 0.044(5) 0.020(4) 0.015(3) N1 0.042(3) 0.028(3) 0.051(7) 0.017(4) 0.014(4) 0.018(3) C3 0.025(3) 0.026(3) 0.072(10) 0.024(5) 0.017(4) 0.010(3) C12 0.029(3) 0.033(3) 0.054(7) 0.008(4) 0.006(4) 0.018(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0000 0.0000 '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 O7 C8 C7 118.4(6) . . O8 C8 O7 123.9(6) . . O8 C8 C7 117.6(5) . . C1 O1 H1 109.5 . . C11 N2 H2 108.5 . . C10 N2 H2 108.5 . . C10 N2 C11 108.1(8) . . C13 N2 H2 108.5 . . C13 N2 C11 108.3(6) . . C13 N2 C10 114.7(7) . . O6 C5 O5 119.2(6) . . O6 C5 C6 122.8(6) . . O5 C5 C6 117.9(6) . . O1 C1 C2 117.9(6) . . O2 C1 O1 120.8(6) . . O2 C1 C2 121.1(6) . . C5 O5 H5 109.5 . . H9C O9 H9D 100(7) . . N2 C11 H11A 109.2 . . N2 C11 H11B 109.2 . . N2 C11 C12 112.0(6) . . H11A C11 H11B 107.9 . . C12 C11 H11A 109.2 . . C12 C11 H11B 109.2 . . C8 C7 H7A 108.9 . . C8 C7 H7B 108.9 . . H7A C7 H7B 107.7 . . C6 C7 C8 113.3(5) . . C6 C7 H7A 108.9 . . C6 C7 H7B 108.9 . . C5 C6 C7 114.3(5) . . C5 C6 H6A 108.7 . . C5 C6 H6B 108.7 . . C7 C6 H6A 108.7 . . C7 C6 H6B 108.7 . . H6A C6 H6B 107.6 . . H9A C9 H9B 108.2 . . C10 C9 H9A 109.7 . . C10 C9 H9B 109.7 . . N1 C9 H9A 109.7 . . N1 C9 H9B 109.7 . . N1 C9 C10 110.0(6) . . C1 C2 H2A 108.7 . . C1 C2 H2B 108.7 . . C1 C2 C3 114.2(5) . . H2A C2 H2B 107.6 . . C3 C2 H2A 108.7 . . C3 C2 H2B 108.7 . . N2 C10 C9 114.4(8) . . N2 C10 H10A 108.7 . . N2 C10 H10B 108.7 . . C9 C10 H10A 108.7 . . C9 C10 H10B 108.7 . . H10A C10 H10B 107.6 . . N2 C13 H13A 109.5 . . N2 C13 H13B 109.5 . . N2 C13 H13C 109.5 . . H13A C13 H13B 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . O4 C4 C3 117.9(6) . . O3 C4 O4 121.7(6) . . O3 C4 C3 120.4(6) . . C9 N1 H1A 109.3 . . C9 N1 H1B 109.3 . . H1A N1 H1B 108.0 . . C12 N1 C9 111.7(7) . . C12 N1 H1A 109.3 . . C12 N1 H1B 109.3 . . C2 C3 C4 114.9(5) . . C2 C3 H3A 108.5 . . C2 C3 H3B 108.5 . . C4 C3 H3A 108.5 . . C4 C3 H3B 108.5 . . H3A C3 H3B 107.5 . . C11 C12 H12A 109.7 . . C11 C12 H12B 109.7 . . N1 C12 C11 110.0(7) . . N1 C12 H12A 109.7 . . N1 C12 H12B 109.7 . . H12A C12 H12B 108.2 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O7 C8 1.281(8) . C8 C7 1.560(8) . C8 O8 1.262(9) . O1 H1 0.8200 . O1 C1 1.334(8) . O6 C5 1.219(9) . N2 H2 0.9800 . N2 C11 1.521(13) . N2 C10 1.475(9) . N2 C13 1.432(14) . C5 O5 1.325(8) . C5 C6 1.514(8) . C1 O2 1.234(8) . C1 C2 1.504(8) . O5 H5 0.8200 . O9 H9C 0.837(16) . O9 H9D 0.832(16) . C11 H11A 0.9700 . C11 H11B 0.9700 . C11 C12 1.546(14) . O4 C4 1.320(8) . C7 H7A 0.9700 . C7 H7B 0.9700 . C7 C6 1.517(9) . C6 H6A 0.9700 . C6 H6B 0.9700 . O3 C4 1.233(9) . C9 H9A 0.9700 . C9 H9B 0.9700 . C9 C10 1.506(14) . C9 N1 1.502(13) . C2 H2A 0.9700 . C2 H2B 0.9700 . C2 C3 1.506(8) . C10 H10A 0.9700 . C10 H10B 0.9700 . C13 H13A 0.9600 . C13 H13B 0.9600 . C13 H13C 0.9600 . C4 C3 1.528(8) . N1 H1A 0.8900 . N1 H1B 0.8900 . N1 C12 1.482(8) . C3 H3A 0.9700 . C3 H3B 0.9700 . C12 H12A 0.9700 . C12 H12B 0.9700 . 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 O7 C8 C7 C6 176.4(10) . . . . C8 C7 C6 C5 174.8(9) . . . . O1 C1 C2 C3 162.9(10) . . . . O6 C5 C6 C7 9.7(16) . . . . N2 C11 C12 N1 56.5(7) . . . . C1 C2 C3 C4 179.6(9) . . . . O5 C5 C6 C7 -174.4(10) . . . . C11 N2 C10 C9 56.2(7) . . . . O4 C4 C3 C2 -179.4(10) . . . . O2 C1 C2 C3 -13.6(15) . . . . O3 C4 C3 C2 4.1(16) . . . . C9 N1 C12 C11 -55.8(8) . . . . C10 N2 C11 C12 -55.1(7) . . . . C10 C9 N1 C12 55.4(7) . . . . C13 N2 C11 C12 180.0(5) . . . . C13 N2 C10 C9 177.1(8) . . . . O8 C8 C7 C6 -2.0(14) . . . . N1 C9 C10 N2 -56.8(8) . . . .