#------------------------------------------------------------------------------ #$Date: 2024-12-07 19:02:42 +0200 (Sat, 07 Dec 2024) $ #$Revision: 296755 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312704.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_2312704 loop_ _publ_author_name 'Kanagavel, Manimurugan' 'Balasubramanian, Sridhar' 'Nechipadappu, Sunil Kumar' _publ_section_title ; Variable stoichiometry and a salt-cocrystal intermediate in multicomponent systems of flucytosine: structural elucidation and their impact on stability. ; _journal_coeditor_code YH5039 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_page_first 793 _journal_page_last 806 _journal_paper_doi 10.1107/S2052520624010278 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety '3(C4 H4 F N3 O), 2(C6 H6 O2)' _chemical_formula_sum 'C24 H24 F3 N9 O7' _chemical_formula_weight 607.52 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 107.559(16) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.252(4) _cell_length_b 36.579(14) _cell_length_c 10.195(6) _cell_measurement_reflns_used 8594 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.27 _cell_measurement_theta_min 2.39 _cell_volume 2578(2) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.952 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-III' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_unetI/netI 0.0743 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 27167 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.460 _diffrn_reflns_theta_min 2.373 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_density_diffrn 1.565 _exptl_crystal_description block _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.493 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 440 _refine_ls_number_reflns 7480 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0656 _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^)+(0.0851P)^2^+1.2091P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1655 _refine_ls_wR_factor_ref 0.1808 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5135 _reflns_number_total 7480 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yh5039sup1.cif _cod_data_source_block FCY-CAL _cod_depositor_comments 'Adding full bibliography for 2312700--2312704.cif.' _cod_original_cell_volume 2579(2) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2312704 _cod_database_fobs_code 2312704 _shelx_shelxl_version_number 2019/3 _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 0.979 _shelx_estimated_absorpt_t_max 0.984 _shelx_res_file ; TITL FCY-CAL_a.res in P2(1)/c FCY-CAL.res created by SHELXL-2018/3 at 16:26:40 on 21-Jun-2024 CELL 0.71073 7.2521 36.5795 10.1952 90.000 107.559 90.000 ZERR 4.00 0.0037 0.0142 0.0058 0.000 0.016 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O F UNIT 96 96 36 28 12 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 OMIT 0 2 0 OMIT -1 3 6 OMIT -3 2 9 OMIT 0 2 8 OMIT -3 3 8 OMIT 2 6 7 SIZE 0.16 0.14 0.12 DFIX 0.89 0.02 N1A H1N N3A H2N N3A H3N N1B H4N N3B H5N N3B H6N ACTA L.S. 10 FMAP 2 PLAN 5 EQIV $1 -x+1, -y+1, -z+1 EQIV $2 x, y, z-1 EQIV $3 -x+1, -y+1, -z EQIV $4 x, -y+3/2, z+1/2 EQIV $5 x, y, z+1 EQIV $6 x, -y+3/2, z-1/2 EQIV $7 -x+1, y+1/2, -z+1/2 HTAB O1 O1B_$1 HTAB N3A N2B_$2 HTAB N3A O1_$3 HTAB N3C O1C_$4 HTAB N3B N2A_$5 HTAB N1C N2C_$6 HTAB N3C F1A_$7 HTAB N1A O1B HTAB N1B O1A HTAB O2 O1A HTAB O3 O1C HTAB O4 O1 HTAB O4 O3 HTAB BOND $H CONF WGHT 0.085100 1.209100 FVAR 0.47849 MOLE 1 C1A 1 0.223109 0.490835 0.276843 11.00000 0.01729 0.02042 = 0.01488 0.00126 0.00695 -0.00122 C2A 1 0.155114 0.453374 0.082657 11.00000 0.01367 0.01999 = 0.01511 0.00130 0.00697 0.00273 C3A 1 0.107669 0.424261 0.160394 11.00000 0.01728 0.01633 = 0.01495 -0.00051 0.00483 0.00044 C4A 1 0.123159 0.428981 0.294770 11.00000 0.01601 0.01979 = 0.01523 0.00292 0.00584 0.00091 AFIX 43 H4A 2 0.094693 0.409633 0.347746 11.00000 -1.20000 AFIX 0 F1A 5 0.049848 0.391717 0.095592 11.00000 0.03312 0.01764 = 0.02255 -0.00303 0.00999 -0.00353 N1A 3 0.181037 0.462445 0.352130 11.00000 0.02131 0.01955 = 0.01209 0.00068 0.00749 -0.00249 H1N 2 0.188714 0.466463 0.441856 11.00000 0.03071 N2A 3 0.212081 0.485902 0.142495 11.00000 0.01831 0.01950 = 0.01291 0.00040 0.00726 -0.00007 N3A 3 0.144170 0.448886 -0.049235 11.00000 0.02871 0.01902 = 0.01549 -0.00145 0.01141 -0.00119 H2N 2 0.171022 0.467811 -0.098572 11.00000 0.05293 H3N 2 0.110577 0.427595 -0.090797 11.00000 0.02018 O1A 4 0.271286 0.521236 0.335931 11.00000 0.03578 0.02329 = 0.01784 -0.00382 0.01256 -0.01072 MOLE 2 C1B 1 0.238908 0.506116 0.679627 11.00000 0.01592 0.01913 = 0.01320 0.00052 0.00682 0.00089 C2B 1 0.333019 0.543125 0.876262 11.00000 0.01349 0.02122 = 0.01444 0.00155 0.00546 0.00313 C3B 1 0.390039 0.571028 0.797864 11.00000 0.01758 0.01636 = 0.01647 -0.00160 0.00548 -0.00092 C4B 1 0.364060 0.566158 0.662416 11.00000 0.01663 0.01766 = 0.01655 0.00228 0.00666 0.00087 AFIX 43 H4BB 2 0.398170 0.584754 0.608944 11.00000 -1.20000 AFIX 0 F1B 5 0.467639 0.602532 0.862617 11.00000 0.03003 0.02063 = 0.01966 -0.00349 0.00872 -0.00626 N1B 3 0.287393 0.533778 0.604055 11.00000 0.02455 0.01948 = 0.01204 0.00021 0.00929 -0.00232 H4N 2 0.269068 0.530184 0.511554 11.00000 0.03525 N2B 3 0.261714 0.511400 0.815702 11.00000 0.01845 0.01941 = 0.01306 0.00108 0.00834 -0.00003 N3B 3 0.348775 0.548232 1.009131 11.00000 0.02573 0.02209 = 0.01482 -0.00083 0.00811 -0.00315 H5N 2 0.320026 0.530490 1.060594 11.00000 0.04232 H6N 2 0.395691 0.569731 1.045350 11.00000 0.02623 O1B 4 0.173020 0.476567 0.620167 11.00000 0.02691 0.01886 = 0.01642 -0.00172 0.00988 -0.00357 MOLE 3 C1C 1 0.763820 0.751258 0.106158 11.00000 0.01472 0.01996 = 0.01562 0.00078 0.00533 -0.00334 C2C 1 0.716368 0.803049 0.225610 11.00000 0.01250 0.02167 = 0.01609 -0.00019 0.00482 -0.00310 C3C 1 0.651550 0.822828 0.098605 11.00000 0.01808 0.01591 = 0.02181 0.00150 0.00748 -0.00095 C4C 1 0.643788 0.806297 -0.021124 11.00000 0.01720 0.02012 = 0.01885 0.00590 0.00636 -0.00005 AFIX 43 H4CB 2 0.600976 0.819162 -0.105871 11.00000 -1.20000 AFIX 0 F1C 5 0.602779 0.858560 0.103048 11.00000 0.03192 0.01809 = 0.02649 0.00169 0.01151 0.00421 N1C 3 0.699547 0.770322 -0.017092 11.00000 0.02057 0.01980 = 0.01300 0.00149 0.00764 0.00120 H7N 2 0.710586 0.760187 -0.094283 11.00000 0.02227 N2C 3 0.764190 0.767558 0.226470 11.00000 0.01722 0.01884 = 0.01701 0.00107 0.00677 -0.00144 N3C 3 0.729889 0.819869 0.344046 11.00000 0.02655 0.02011 = 0.01858 -0.00218 0.00735 -0.00112 H8N 2 0.764879 0.806522 0.421010 11.00000 0.04766 H9N 2 0.694660 0.843756 0.340078 11.00000 0.03343 O1C 4 0.818165 0.718683 0.102502 11.00000 0.02698 0.01810 = 0.01813 0.00260 0.00830 0.00274 MOLE 4 C1 1 0.642640 0.612124 0.243780 11.00000 0.01980 0.01803 = 0.01445 -0.00388 0.00590 -0.00333 C2 1 0.621093 0.640243 0.148023 11.00000 0.02535 0.02171 = 0.01568 -0.00110 0.00947 -0.00468 AFIX 43 H2 2 0.725525 0.646495 0.114189 11.00000 -1.20000 AFIX 0 C3 1 0.447034 0.659173 0.101872 11.00000 0.02966 0.02283 = 0.01734 0.00059 0.00412 -0.00096 AFIX 43 H3 2 0.433067 0.678416 0.037016 11.00000 -1.20000 AFIX 0 C4 1 0.292482 0.649895 0.150903 11.00000 0.02131 0.02761 = 0.02415 -0.00062 0.00299 0.00175 AFIX 43 H4 2 0.173322 0.662698 0.118849 11.00000 -1.20000 AFIX 0 C5 1 0.313765 0.621799 0.246976 11.00000 0.01939 0.02992 = 0.02311 -0.00506 0.00855 -0.00471 AFIX 43 H5 2 0.209201 0.615592 0.280734 11.00000 -1.20000 AFIX 0 C6 1 0.488244 0.602810 0.293546 11.00000 0.02205 0.02048 = 0.01607 -0.00245 0.00787 -0.00426 C7 1 1.087187 0.690864 0.452389 11.00000 0.01550 0.02522 = 0.02064 0.00294 0.00794 0.00276 C8 1 1.152234 0.726817 0.479534 11.00000 0.01910 0.02432 = 0.02827 0.00457 0.00837 0.00177 AFIX 43 H8 2 1.131654 0.743985 0.406606 11.00000 -1.20000 AFIX 0 C9 1 1.248122 0.737398 0.615168 11.00000 0.01899 0.02255 = 0.03260 -0.00157 0.00749 0.00039 AFIX 43 H9 2 1.292364 0.761842 0.634190 11.00000 -1.20000 AFIX 0 C10 1 1.278757 0.712292 0.721938 11.00000 0.01798 0.03010 = 0.02693 -0.00344 0.00512 0.00438 AFIX 43 H10 2 1.343679 0.719646 0.813639 11.00000 -1.20000 AFIX 0 C11 1 1.214490 0.676329 0.694897 11.00000 0.02022 0.02749 = 0.02181 0.00299 0.00856 0.00275 AFIX 43 H11 2 1.234692 0.659264 0.768123 11.00000 -1.20000 AFIX 0 C12 1 1.120816 0.665525 0.560542 11.00000 0.01528 0.02057 = 0.02318 0.00183 0.00923 0.00189 O1 4 0.818892 0.594293 0.289911 11.00000 0.01952 0.01901 = 0.02040 0.00118 0.00858 -0.00110 H1O 2 0.805258 0.571265 0.321455 11.00000 0.04117 O2 4 0.519656 0.575645 0.391437 11.00000 0.02558 0.02402 = 0.02259 0.00375 0.01082 -0.00500 H2O 2 0.446063 0.555993 0.360149 11.00000 0.04570 O3 4 0.985960 0.677741 0.324796 11.00000 0.02674 0.02521 = 0.01883 0.00452 0.00315 0.00030 H3O 2 0.946979 0.696287 0.266974 11.00000 0.05776 O4 4 1.056317 0.630093 0.534656 11.00000 0.02813 0.02250 = 0.02309 0.00448 0.00690 -0.00303 H4O 2 1.003278 0.628079 0.450214 11.00000 0.06407 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM FCY-CAL_a.res in P2(1)/c REM wR2 = 0.1808, GooF = S = 1.073, Restrained GooF = 1.072 for all data REM R1 = 0.0656 for 5135 Fo > 4sig(Fo) and 0.0981 for all 7480 data REM 440 parameters refined using 6 restraints END WGHT 0.0851 1.2091 REM Instructions for potential hydrogen bonds HTAB C4A O4_$1 HTAB N1A O1B HTAB N3A N2B_$2 HTAB N3A O1_$3 HTAB C4B F1C_$4 HTAB C4B O2 HTAB N1B O1A HTAB N3B N2A_$5 HTAB N1C N2C_$6 HTAB N3C O1C_$4 HTAB N3C F1A_$7 HTAB N3C F1B_$6 HTAB O1 O1B_$1 HTAB O2 O1A HTAB O3 O1C HTAB O4 O1 HTAB O4 O3 REM Highest difference peak 0.493, deepest hole -0.384, 1-sigma level 0.087 Q1 1 0.3618 0.5712 0.7266 11.00000 0.05 0.49 Q2 1 0.7485 0.7765 0.1301 11.00000 0.05 0.49 Q3 1 0.1075 0.4290 0.2191 11.00000 0.05 0.46 Q4 1 1.0955 0.6771 0.5068 11.00000 0.05 0.44 Q5 1 0.6965 0.8197 0.1797 11.00000 0.05 0.44 ; _shelx_res_checksum 37592 _shelx_hkl_file ; 1 0 0 100.09 8.65 1 0 0 111.26 7.84 -1 0 0 108.09 8.18 -1 0 0 118.22 7.83 1 0 0 102.37 8.11 -3 0 0 56.66 7.79 -3 0 0 54.76 5.73 3 0 0 49.08 7.07 3 0 0 54.11 4.44 3 0 0 53.19 5.22 4 0 0 188.20 14.60 4 0 0 173.56 13.62 -4 0 0 211.00 17.62 -5 0 0 7.88 6.18 5 0 0 12.89 3.42 -6 0 0 67.02 13.31 6 0 0 74.10 8.06 -7 0 0 20.33 10.27 7 0 0 15.89 4.80 -8 0 0 107.75 18.84 8 0 0 76.67 9.88 -9 0 0 24.43 15.46 -1 -1 0 2091.50 139.93 -1 -1 0 2036.65 139.17 1 -1 0 1896.08 139.53 -1 1 0 2003.10 139.24 1 1 0 1920.05 139.41 1 1 0 1924.87 139.09 -2 -1 0 63.52 4.92 2 -1 0 50.17 4.06 2 -1 0 60.41 5.01 -2 -1 0 35.38 5.90 2 -1 0 53.06 6.31 -2 1 0 49.72 3.96 -2 1 0 41.99 6.07 2 1 0 50.33 4.67 2 1 0 43.76 3.82 -2 1 0 59.49 5.02 2 1 0 38.19 5.55 -3 -1 0 120.61 10.06 -3 -1 0 113.24 11.40 3 -1 0 132.65 9.94 3 -1 0 115.32 11.03 3 -1 0 117.59 9.04 -3 1 0 120.99 11.71 3 1 0 116.30 8.85 3 1 0 118.63 9.70 3 1 0 112.91 11.02 -3 1 0 124.49 10.19 4 -1 0 23.75 2.92 -4 -1 0 32.43 6.67 4 -1 0 19.12 3.82 4 1 0 24.37 3.68 4 1 0 24.46 2.65 -4 1 0 31.80 7.00 -4 1 0 27.93 3.66 -5 -1 0 91.35 12.96 5 -1 0 82.02 8.63 -5 1 0 90.03 13.17 5 1 0 105.31 8.80 6 -1 0 265.53 21.19 -6 -1 0 269.76 26.19 6 1 0 262.86 21.04 -6 1 0 269.26 26.30 7 -1 0 -3.26 3.55 -7 -1 0 -8.76 8.17 -7 1 0 3.31 8.63 7 1 0 2.63 3.57 8 -1 0 14.09 5.15 -8 -1 0 13.43 11.24 -8 1 0 -1.02 10.35 -9 -1 0 6.12 12.43 -9 1 0 24.63 14.21 0 -2 0 -0.03 0.10 0 -2 0 -0.02 0.13 0 2 0 -0.03 0.11 0 2 0 -0.01 0.15 1 -2 0 87.61 6.02 -1 -2 0 69.54 6.55 -1 -2 0 81.44 6.08 1 -2 0 83.64 6.92 -1 2 0 76.75 6.00 1 2 0 81.15 6.00 -1 2 0 87.74 6.40 -1 2 0 72.48 5.91 1 2 0 81.58 6.45 2 -2 0 44.77 3.72 -2 -2 0 48.05 4.42 2 -2 0 43.81 4.30 2 -2 0 47.39 5.95 -2 -2 0 30.46 5.16 -2 2 0 39.59 3.49 2 2 0 36.15 5.13 -2 2 0 45.51 4.77 2 2 0 47.73 4.14 -2 2 0 31.87 3.71 -2 2 0 29.65 5.46 3 -2 0 1164.21 81.73 3 -2 0 1093.72 82.74 -3 -2 0 1145.45 81.93 3 -2 0 1157.42 81.19 -3 -2 0 1133.22 82.98 -3 2 0 1275.68 81.05 -3 2 0 1152.17 82.12 -3 2 0 1150.28 83.27 -3 2 0 1138.78 81.27 3 2 0 1146.37 81.52 3 2 0 1072.99 82.41 3 2 0 1124.56 80.80 4 -2 0 143.03 11.41 4 -2 0 141.39 10.46 -4 -2 0 140.70 13.93 4 2 0 139.82 10.98 4 2 0 127.02 12.34 -4 2 0 118.02 13.47 4 2 0 129.10 9.84 -4 2 0 132.09 10.66 -5 -2 0 10.31 6.03 5 -2 0 13.43 3.62 5 2 0 18.28 3.72 -5 2 0 16.37 7.46 6 -2 0 143.73 12.25 -6 -2 0 142.81 18.44 6 2 0 121.40 11.83 -6 2 0 142.70 19.33 7 -2 0 22.07 5.69 -7 -2 0 41.43 12.67 -7 2 0 29.40 11.25 7 2 0 29.68 5.45 -8 -2 0 -6.23 10.52 8 -2 0 -3.23 4.05 -8 2 0 5.53 10.25 -9 -2 0 11.44 13.82 -9 2 0 5.00 13.96 0 -3 0 -0.32 0.25 0 3 0 -0.03 0.20 0 3 0 -0.01 0.27 1 -3 0 107.91 7.79 -1 -3 0 89.69 8.04 -1 -3 0 113.81 7.72 1 -3 0 100.32 8.71 1 -3 0 106.52 7.80 -1 3 0 110.17 7.77 1 3 0 100.96 7.59 -1 3 0 105.55 7.69 1 3 0 91.38 7.90 -1 3 0 114.20 8.16 2 3 0 9939.54 698.35 -3 -3 0 1149.55 78.98 3 -3 0 1152.07 78.86 -3 -3 0 966.30 79.71 3 -3 0 1082.65 79.90 3 -3 0 1096.10 78.30 -3 3 0 1126.04 79.20 -3 3 0 1046.21 80.20 3 3 0 1069.68 79.42 -3 3 0 1217.78 78.19 -3 3 0 1086.61 78.30 3 3 0 1136.51 78.49 -4 -3 0 618.04 47.78 4 -3 0 611.99 45.29 4 -3 0 689.45 46.13 4 3 0 647.06 45.63 -4 3 0 614.10 45.30 4 3 0 598.81 46.87 -4 3 0 642.21 48.14 -5 -3 0 242.57 23.46 5 -3 0 251.69 20.28 -5 3 0 297.81 24.05 5 3 0 259.00 19.85 -6 -3 0 -7.76 6.06 6 -3 0 1.80 3.59 -6 3 0 -1.02 7.82 6 3 0 -2.65 3.01 7 -3 0 1.04 4.08 -7 -3 0 2.21 8.12 7 3 0 -0.35 3.27 -7 3 0 10.74 10.33 8 -3 0 28.41 6.01 -8 -3 0 25.98 12.17 -8 3 0 34.94 13.16 -9 -3 0 10.18 13.32 -9 3 0 -1.18 13.09 1 -4 0 1429.43 92.55 -1 -4 0 1435.68 92.46 1 -4 0 1226.80 92.61 1 -4 0 1437.08 93.24 -1 -4 0 1291.09 92.65 -1 -4 0 1210.61 92.33 1 4 0 1298.47 92.46 -1 4 0 1226.00 92.58 -1 4 0 1247.50 92.77 1 4 0 1255.69 92.30 -1 4 0 1361.15 92.51 1 4 0 1361.25 92.33 3 -4 0 710.83 50.38 3 -4 0 692.77 49.84 -3 -4 0 702.96 50.39 3 -4 0 686.27 51.52 -3 -4 0 754.76 51.66 -3 4 0 656.25 51.78 3 4 0 713.87 49.90 -3 4 0 665.60 49.75 3 4 0 688.71 50.83 -3 4 0 709.68 49.66 -3 4 0 700.39 50.66 -4 -4 0 1074.33 77.28 4 -4 0 1022.25 74.82 4 -4 0 1153.15 75.60 4 4 0 1006.62 76.16 -4 4 0 1036.11 77.43 -4 4 0 1007.30 74.80 4 4 0 1063.35 74.98 5 -4 0 37.36 5.61 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356.25 26.95 0 -20 0 373.58 26.59 0 -20 0 394.28 27.45 0 20 0 354.70 27.30 1 -20 0 493.46 34.48 1 -20 0 421.36 35.20 -1 -20 0 476.59 34.16 1 -20 0 503.47 34.50 -1 -20 0 477.82 34.86 1 20 0 476.41 34.47 -1 20 0 448.54 34.45 -1 20 0 486.87 34.85 2 -20 0 83.31 7.95 -2 -20 0 74.87 7.64 2 -20 0 91.18 7.78 -2 -20 0 90.69 6.37 2 -20 0 92.26 10.64 -2 -20 0 88.05 6.35 -2 20 0 85.82 8.27 -2 20 0 104.16 10.32 2 20 0 81.75 7.29 -2 20 0 90.15 8.00 3 -20 0 9.78 3.37 -3 -20 0 12.37 3.01 3 -20 0 6.45 2.92 -3 -20 0 11.01 2.68 -3 20 0 13.76 3.30 -3 20 0 4.83 5.47 -3 20 0 12.96 4.40 4 -20 0 1.30 2.62 -4 -20 0 1.85 3.73 4 -20 0 -2.24 2.98 -4 20 0 5.10 2.91 -4 20 0 2.61 6.46 5 -20 0 3.71 4.04 -5 -20 0 2.30 5.08 -5 20 0 -3.35 7.46 -6 -20 0 0.96 6.67 6 -20 0 -0.75 4.04 -6 20 0 1.48 9.46 7 -20 0 19.71 6.21 -7 20 0 9.20 11.78 8 -20 0 -4.58 4.79 -8 20 0 -2.31 12.93 -9 20 0 -1.99 16.69 0 -21 0 3.41 2.88 0 -21 0 1.60 1.39 0 -21 0 -2.45 1.80 0 21 0 -0.33 1.78 -1 -21 0 79.10 6.50 -1 -21 0 75.67 7.12 1 -21 0 71.85 8.57 1 -21 0 78.15 6.74 1 -21 0 70.97 6.69 -1 21 0 74.32 6.94 1 21 0 72.77 6.71 -2 -21 0 297.81 22.75 2 -21 0 310.57 22.93 2 -21 0 321.22 22.69 -2 -21 0 303.46 21.33 2 -21 0 256.08 23.92 -2 21 0 303.88 22.97 -2 21 0 277.32 22.82 2 21 0 303.89 22.33 -2 21 0 344.04 24.50 3 -21 0 2.59 2.71 3 -21 0 -1.69 2.32 -3 -21 0 1.47 2.15 -3 21 0 0.79 5.01 -3 21 0 2.54 3.56 -3 21 0 5.37 2.79 4 -21 0 71.92 8.52 4 -21 0 70.76 7.65 -4 -21 0 77.93 8.97 -4 21 0 79.60 12.08 -4 21 0 82.09 7.88 -5 -21 0 6.08 5.64 5 -21 0 1.10 3.82 -5 21 0 3.96 7.75 6 -21 0 133.85 13.02 -6 21 0 109.82 17.77 7 -21 0 2.51 4.62 -7 21 0 0.38 9.68 8 -21 0 -1.54 5.18 -8 21 0 14.32 13.03 0 -22 0 228.16 17.45 0 -22 0 207.12 16.61 0 -22 0 230.38 16.23 0 22 0 211.60 16.94 1 -22 0 63.49 7.87 1 -22 0 66.94 6.24 1 -22 0 60.98 6.24 -1 -22 0 62.79 6.08 -1 22 0 72.33 6.73 1 22 0 74.17 6.48 2 -22 0 104.41 11.61 2 -22 0 114.61 10.02 2 -22 0 112.93 9.81 -2 -22 0 113.13 9.97 -2 22 0 123.01 10.77 -2 22 0 121.20 10.19 -2 22 0 133.58 12.15 2 22 0 112.27 9.42 -3 -22 0 10.08 2.82 3 -22 0 16.06 3.48 3 -22 0 17.77 4.02 -3 22 0 10.46 3.24 -3 22 0 11.39 6.18 -4 -22 0 4.28 4.43 4 -22 0 4.41 3.31 4 -22 0 3.11 3.01 -4 22 0 2.80 6.55 -4 22 0 6.59 3.27 5 -22 0 112.39 11.69 -5 22 0 123.77 17.50 6 -22 0 108.05 11.61 -6 22 0 89.67 17.32 7 -22 0 3.51 5.17 -7 22 0 -14.65 11.64 8 -22 0 7.97 5.60 -8 22 0 -6.92 14.19 0 -23 0 5.02 1.63 0 -23 0 4.51 3.29 0 -23 0 2.23 1.91 0 23 0 3.02 2.17 1 -23 0 525.74 39.25 -1 -23 0 531.26 39.07 1 -23 0 546.56 39.24 1 -23 0 524.81 40.34 -1 23 0 564.02 39.78 1 23 0 549.07 39.37 2 -23 0 239.60 18.51 2 -23 0 214.38 18.12 2 -23 0 247.84 20.95 -2 -23 0 235.59 17.81 -2 -23 0 226.80 18.41 -2 23 0 266.75 19.76 2 23 0 239.24 17.95 -2 23 0 234.66 18.62 3 -23 0 7.34 3.24 3 -23 0 7.48 2.99 -3 23 0 4.54 5.54 -3 23 0 8.62 3.25 4 -23 0 -3.41 2.66 4 -23 0 2.70 3.38 -4 23 0 -1.25 6.80 -4 23 0 3.01 3.12 5 -23 0 34.25 6.32 -5 23 0 19.90 10.04 6 -23 0 53.86 8.23 -6 23 0 24.09 11.32 7 -23 0 7.78 5.34 -7 23 0 8.86 12.83 8 -23 0 79.21 10.90 -8 23 0 39.20 19.54 0 -24 0 1135.52 77.56 0 -24 0 1087.88 78.59 0 -24 0 1090.12 78.01 0 24 0 1058.18 78.33 1 -24 0 201.82 16.01 -1 -24 0 200.45 15.80 1 -24 0 214.84 15.96 1 -24 0 190.79 17.12 -1 24 0 216.45 16.47 1 24 0 211.18 16.18 -2 -24 0 10.28 2.64 2 -24 0 10.33 2.92 2 -24 0 10.20 2.97 -2 24 0 11.28 3.36 2 24 0 9.46 2.55 -2 24 0 8.83 4.94 3 -24 0 7.77 3.30 3 -24 0 12.60 3.79 -3 24 0 13.26 3.71 -3 24 0 9.39 6.06 4 -24 0 11.37 3.84 4 -24 0 10.38 4.30 -4 24 0 13.04 3.84 -4 24 0 3.94 7.10 5 -24 0 2.82 3.77 -5 24 0 -1.25 7.50 6 -24 0 2.76 4.21 -6 24 0 7.52 10.25 7 -24 0 -0.49 4.73 -7 24 0 3.46 10.47 8 -24 0 6.73 5.88 -8 24 0 18.23 19.75 0 -25 0 1.32 1.95 0 -25 0 1.46 1.42 0 25 0 0.24 2.12 -1 -25 0 52.04 5.73 1 -25 0 54.92 5.72 1 -25 0 64.28 6.70 1 -25 0 61.57 7.95 1 25 0 60.81 5.93 -1 25 0 59.43 6.31 2 -25 0 22.63 4.00 -2 -25 0 19.87 3.35 2 -25 0 19.98 3.94 2 25 0 23.25 3.63 -2 25 0 21.85 4.29 3 -25 0 25.24 4.99 3 -25 0 33.96 5.12 -3 25 0 26.21 8.11 -3 25 0 33.97 5.41 4 -25 0 341.80 27.41 4 -25 0 358.66 28.05 -4 25 0 372.81 27.78 -4 25 0 362.23 30.92 5 -25 0 28.52 6.04 -5 25 0 13.62 9.69 6 -25 0 5.58 4.26 -6 25 0 -1.30 8.89 7 -25 0 -2.63 3.92 -7 25 0 4.31 13.43 8 -25 0 5.18 5.89 0 -26 0 22.89 2.94 0 -26 0 21.30 3.75 0 26 0 20.85 3.92 1 -26 0 56.66 6.09 -1 -26 0 56.31 5.65 1 -26 0 51.38 5.45 -1 26 0 51.40 5.89 1 26 0 46.25 5.41 2 -26 0 -0.53 2.61 2 -26 0 -0.17 2.36 -2 -26 0 1.98 1.91 -2 26 0 2.32 2.71 2 26 0 -1.13 1.93 3 -26 0 52.18 6.69 3 -26 0 50.40 6.89 -3 26 0 56.33 6.64 4 -26 0 59.76 7.95 4 -26 0 73.61 8.30 -4 26 0 64.08 7.54 5 -26 0 197.26 16.90 5 -26 0 204.98 17.76 6 -26 0 1.06 4.23 7 -26 0 0.88 4.34 8 -26 0 1.30 5.39 0 -27 0 6.52 2.50 0 -27 0 0.76 1.48 0 27 0 1.43 2.30 1 -27 0 29.74 4.71 1 -27 0 37.99 4.46 -1 -27 0 33.00 4.48 1 27 0 29.90 4.49 -1 27 0 35.16 5.25 -2 -27 0 2.03 2.26 2 -27 0 4.18 2.74 2 -27 0 -1.24 2.53 -2 27 0 -2.00 2.63 3 -27 0 73.28 8.46 3 -27 0 90.58 8.94 -3 27 0 90.49 8.89 4 -27 0 22.45 4.84 4 -27 0 23.00 5.29 -4 27 0 19.12 4.71 5 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5.21 0 -30 0 3.09 2.77 0 30 0 2.09 2.70 1 -30 0 40.73 4.92 1 -30 0 34.92 5.50 -1 -30 0 35.88 5.12 1 30 0 45.32 5.74 -1 30 0 39.10 5.95 2 -30 0 174.76 14.17 -2 -30 0 161.95 13.37 2 -30 0 163.07 13.86 -2 30 0 170.34 14.39 3 -30 0 16.24 4.34 3 -30 0 15.49 4.33 -3 -30 0 17.61 3.72 -3 30 0 16.05 4.59 4 -30 0 -2.42 3.90 4 -30 0 0.73 3.00 -4 30 0 2.81 3.62 5 -30 0 20.61 5.10 5 -30 0 7.38 4.38 6 -30 0 20.44 6.01 7 -30 0 7.68 4.90 0 -31 0 4.72 2.85 0 31 0 4.46 3.17 -1 -31 0 4.44 2.58 1 -31 0 2.84 3.47 1 31 0 2.70 2.66 -1 31 0 0.22 2.76 2 -31 0 13.41 3.99 -2 -31 0 17.30 3.62 2 -31 0 12.61 3.81 -2 31 0 11.06 3.97 3 -31 0 9.92 4.16 -3 -31 0 17.69 3.65 3 -31 0 19.32 4.69 -3 31 0 18.77 4.71 4 -31 0 128.86 13.58 4 -31 0 166.51 14.03 -4 -31 0 147.62 12.38 5 -31 0 11.68 5.05 5 -31 0 4.23 4.37 6 -31 0 7.28 4.99 7 -31 0 2.61 5.07 0 -32 0 547.21 40.73 0 32 0 556.79 41.13 1 -32 0 34.75 5.42 -1 -32 0 29.56 4.58 1 32 0 37.78 5.53 -1 32 0 23.41 5.13 2 -32 0 6.97 3.15 -2 -32 0 6.29 3.02 2 -32 0 4.65 3.75 -2 32 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11.16 9 -11 -4 15.56 6.58 -9 11 4 7.67 11.82 8 -11 -4 51.20 9.07 -8 -11 4 35.78 12.04 -8 11 4 42.79 13.34 -7 -11 4 88.83 14.48 7 -11 -4 81.10 11.29 -7 11 4 100.74 17.12 -6 -11 4 1.05 5.30 6 -11 -4 -0.34 4.50 6 11 -4 1.54 3.39 -6 11 4 2.38 3.45 -6 11 4 -6.81 7.23 -5 -11 4 12.58 2.86 -5 -11 4 10.06 5.42 5 -11 -4 11.28 4.88 -5 11 4 13.23 3.80 -5 11 4 16.59 7.07 5 11 -4 10.59 3.82 4 -11 -4 426.56 28.12 -4 -11 4 325.04 27.02 4 11 -4 363.49 26.64 -4 11 4 332.67 28.14 -4 11 4 317.43 26.37 4 11 -4 333.23 25.60 -3 -11 4 17.63 5.45 3 -11 -4 26.20 5.53 -3 -11 4 23.60 4.46 -3 11 4 15.73 5.42 -3 11 4 25.75 4.61 3 11 -4 18.95 3.15 3 11 -4 18.13 4.11 -3 11 4 24.22 5.68 2 -11 -4 1654.95 127.04 -2 -11 4 1646.09 127.41 -2 -11 4 1990.17 126.16 2 -11 -4 1891.83 126.94 -2 11 4 1523.33 125.40 -2 11 4 1834.51 127.33 2 11 -4 1840.76 126.88 2 11 -4 1637.85 125.34 -2 11 4 1892.04 126.68 -2 11 4 1878.06 126.90 -1 -11 4 383.34 28.75 -1 -11 4 335.18 30.88 1 -11 -4 399.02 29.25 1 -11 -4 429.94 30.81 1 -11 -4 407.66 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-0.77 6.99 2 17 -13 7.05 15.72 1 -17 -13 -7.80 14.81 -1 -17 13 3.39 9.23 1 17 -13 13.93 17.07 -1 17 13 5.24 7.30 0 -17 -13 -25.43 14.80 0 17 -13 -5.14 17.25 0 17 13 1.15 7.33 -5 -18 13 -3.70 8.75 4 -18 -13 1.40 14.24 -4 -18 13 -5.54 10.74 -4 18 13 12.47 8.78 -3 -18 13 -0.37 8.64 3 -18 -13 2.23 13.86 -3 18 13 12.89 8.30 -2 -18 13 11.38 9.57 2 -18 -13 11.65 15.61 -2 18 13 12.27 8.39 -1 -18 13 52.95 15.81 1 -18 -13 80.16 20.03 -1 18 13 65.03 12.18 1 18 -13 48.14 19.12 0 18 13 16.33 9.08 -5 -19 13 8.67 9.92 -4 -19 13 -2.42 10.31 4 -19 -13 -4.53 13.55 -4 19 13 5.20 8.44 -3 -19 13 73.26 16.67 3 -19 -13 81.25 20.77 -3 19 13 65.94 12.82 -2 -19 13 11.82 10.99 2 -19 -13 3.96 15.24 -2 19 13 17.98 8.57 1 -19 -13 3.99 15.72 -1 19 13 42.76 10.28 -5 -20 13 10.80 8.93 4 -20 -13 5.63 14.15 -3 -20 13 38.50 13.62 3 -20 -13 37.80 16.78 -3 20 13 74.94 13.13 2 -20 -13 -5.09 14.45 -2 -20 13 3.56 13.40 -2 20 13 6.54 7.96 1 -20 -13 37.72 18.19 -1 20 13 28.41 9.48 4 -21 -13 85.46 25.10 3 -21 -13 126.12 24.56 -3 21 13 96.01 15.64 2 -21 -13 10.09 15.65 -2 21 13 9.64 8.60 -1 21 13 36.92 10.33 3 -22 -13 24.53 16.40 2 -22 -13 3.89 15.58 -2 22 13 4.34 10.09 -5 0 14 11.19 10.02 -5 0 14 4.69 17.90 -4 0 14 23.16 18.97 4 0 -14 75.18 19.73 -4 0 14 74.65 13.40 -3 0 14 -14.40 12.56 3 0 -14 28.73 16.25 -3 0 14 4.00 12.37 2 0 -14 20.74 16.09 -2 0 14 54.21 11.85 -5 -1 14 25.06 20.02 -5 -1 14 18.52 10.61 -5 1 14 28.42 11.56 -5 1 14 -9.93 16.27 -4 -1 14 4.45 8.20 -4 -1 14 9.81 17.72 4 -1 -14 -3.39 12.86 -4 1 14 23.32 9.16 4 1 -14 9.11 14.83 -4 1 14 -0.06 16.24 -3 -1 14 5.20 8.05 3 -1 -14 6.34 15.08 -3 -1 14 -6.51 9.70 -3 1 14 -11.41 14.59 -3 1 14 7.67 11.38 3 1 -14 -2.80 14.10 2 -1 -14 10.93 14.93 -2 -1 14 1.96 12.98 -2 -1 14 34.73 10.73 -2 1 14 14.72 8.95 2 1 -14 4.81 16.81 -1 -1 14 40.22 12.13 -5 -2 14 -0.68 11.85 -5 -2 14 28.32 11.71 -5 2 14 24.00 10.98 -5 2 14 13.28 13.65 5 2 -14 15.34 22.17 -4 -2 14 33.82 10.97 -4 -2 14 17.42 15.49 4 -2 -14 41.40 16.35 -4 2 14 30.31 13.75 -4 2 14 65.16 12.41 4 2 -14 34.82 17.15 -3 -2 14 -2.43 10.11 -3 -2 14 22.66 9.36 3 -2 -14 14.48 15.69 -3 2 14 1.55 8.00 3 2 -14 9.33 15.39 -2 -2 14 8.06 12.49 2 -2 -14 5.62 14.78 -2 -2 14 21.24 13.10 -2 2 14 32.86 9.72 2 2 -14 4.68 16.00 -1 -2 14 42.52 12.47 -1 2 14 65.71 14.70 -5 -3 14 5.58 9.72 -5 -3 14 -3.50 12.01 -5 3 14 6.56 12.46 4 -3 -14 1.03 13.28 -4 -3 14 11.29 17.20 -4 -3 14 3.97 8.58 4 3 -14 25.32 15.82 -4 3 14 11.64 8.73 -3 -3 14 -1.92 9.64 3 -3 -14 -8.23 13.84 -3 -3 14 3.59 7.67 -3 3 14 8.59 8.49 3 3 -14 -3.26 12.99 -2 -3 14 14.33 13.49 2 -3 -14 4.89 16.01 -2 -3 14 15.13 12.65 2 3 -14 9.12 16.33 -2 3 14 40.47 10.52 -1 3 14 65.80 14.57 -5 -4 14 14.19 13.42 -5 -4 14 20.44 11.05 5 4 -14 11.38 14.95 4 -4 -14 5.73 14.86 -4 -4 14 -2.88 10.78 -4 -4 14 1.06 8.15 -4 4 14 21.82 9.48 4 4 -14 5.85 13.45 -3 -4 14 42.52 13.61 3 -4 -14 42.67 17.81 -3 -4 14 64.97 12.36 3 4 -14 53.81 17.35 -3 4 14 46.02 11.37 2 -4 -14 1.60 15.24 -2 -4 14 8.95 12.23 -2 -4 14 -1.86 11.59 2 4 -14 3.64 15.79 -2 4 14 16.92 8.97 -1 -4 14 -0.25 12.36 -1 4 14 30.18 11.64 -5 -5 14 43.10 13.17 5 5 -14 45.05 19.19 -4 -5 14 13.08 8.83 -4 -5 14 8.61 11.34 4 -5 -14 -8.33 13.61 -4 5 14 8.79 8.49 4 5 -14 13.28 15.12 3 -5 -14 1.73 15.87 -3 -5 14 -0.38 11.62 -3 -5 14 2.01 8.15 3 5 -14 8.89 15.55 -3 5 14 9.47 8.50 -2 -5 14 -4.74 11.86 -2 5 14 4.54 7.96 2 5 -14 13.15 15.10 -1 -5 14 -4.12 11.10 -1 5 14 2.49 9.90 5 6 -14 42.78 18.55 -4 -6 14 12.82 8.25 -4 -6 14 -0.58 12.63 -4 6 14 -0.33 7.85 4 6 -14 11.97 15.57 3 -6 -14 68.21 20.99 -3 -6 14 52.66 16.61 -3 -6 14 21.66 13.55 -3 6 14 45.28 11.34 3 6 -14 63.32 19.31 -2 -6 14 16.99 13.65 2 6 -14 10.64 17.21 -2 6 14 19.53 9.10 -1 -6 14 22.49 16.39 -1 6 14 26.96 11.84 5 7 -14 45.25 15.75 -4 -7 14 10.42 12.96 -4 -7 14 39.86 10.70 4 7 -14 60.05 18.74 -3 -7 14 4.14 12.29 3 -7 -14 4.05 22.32 -3 7 14 9.28 8.07 3 7 -14 14.32 14.54 -2 -7 14 -1.42 9.27 2 7 -14 -3.16 16.15 5 8 -14 100.73 21.35 -4 -8 14 12.35 9.66 -4 -8 14 4.74 13.31 4 8 -14 24.72 16.01 -3 -8 14 65.84 16.53 -3 -8 14 53.43 17.90 3 -8 -14 88.68 31.30 -3 8 14 71.32 13.36 3 8 -14 65.33 20.23 -2 -8 14 41.17 15.69 -2 8 14 65.03 15.34 2 8 -14 74.19 19.89 4 9 -14 2.11 14.73 3 9 -14 64.99 19.22 -2 -9 14 4.58 11.52 2 9 -14 34.63 19.35 -2 9 14 24.37 14.02 4 10 -14 54.51 17.89 -3 -10 14 10.77 11.61 3 10 -14 19.32 14.54 -2 -10 14 -4.03 11.56 2 10 -14 -2.95 17.25 4 11 -14 14.42 15.92 3 11 -14 387.19 41.96 2 11 -14 2.11 16.35 3 12 -14 27.99 17.20 3 13 -14 359.45 40.10 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.5573 _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 0.71112 7.200 36.634 10.135 89.816 107.578 90.114 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 56943 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.2231(3) 0.49084(6) 0.2768(2) 0.0171(4) Uani 1 1 d . . . . . C2A C 0.1551(3) 0.45337(6) 0.0827(2) 0.0157(4) Uani 1 1 d . . . . . C3A C 0.1077(3) 0.42426(5) 0.1604(2) 0.0162(4) Uani 1 1 d . . . . . C4A C 0.1232(3) 0.42898(6) 0.2948(2) 0.0168(4) Uani 1 1 d . . . . . H4A H 0.094693 0.409633 0.347746 0.020 Uiso 1 1 calc R U . . . F1A F 0.0498(2) 0.39172(3) 0.09559(14) 0.0241(3) Uani 1 1 d . . . . . N1A N 0.1810(3) 0.46244(5) 0.35213(19) 0.0171(4) Uani 1 1 d D . . . . H1N H 0.189(4) 0.4665(7) 0.4419(19) 0.031(8) Uiso 1 1 d D . . . . N2A N 0.2121(3) 0.48590(5) 0.14250(19) 0.0163(4) Uani 1 1 d . . . . . N3A N 0.1442(3) 0.44889(5) -0.0492(2) 0.0200(4) Uani 1 1 d D . . . . H2N H 0.171(5) 0.4678(7) -0.099(3) 0.053(10) Uiso 1 1 d D . . . . H3N H 0.111(4) 0.4276(5) -0.091(3) 0.020(7) Uiso 1 1 d D . . . . O1A O 0.2713(3) 0.52124(4) 0.33593(17) 0.0246(4) Uani 1 1 d . . . . . C1B C 0.2389(3) 0.50612(5) 0.6796(2) 0.0155(4) Uani 1 1 d . . . . . C2B C 0.3330(3) 0.54312(6) 0.8763(2) 0.0161(4) Uani 1 1 d . . . . . C3B C 0.3900(3) 0.57103(5) 0.7979(2) 0.0167(4) Uani 1 1 d . . . . . C4B C 0.3641(3) 0.56616(5) 0.6624(2) 0.0166(4) Uani 1 1 d . . . . . H4BB H 0.398170 0.584754 0.608944 0.020 Uiso 1 1 calc R U . . . F1B F 0.4676(2) 0.60253(3) 0.86262(14) 0.0232(3) Uani 1 1 d . . . . . N1B N 0.2874(3) 0.53378(5) 0.60406(19) 0.0179(4) Uani 1 1 d D . . . . H4N H 0.269(4) 0.5302(7) 0.5116(19) 0.035(8) Uiso 1 1 d D . . . . N2B N 0.2617(3) 0.51140(5) 0.81570(19) 0.0162(4) Uani 1 1 d . . . . . N3B N 0.3488(3) 0.54823(5) 1.0091(2) 0.0204(4) Uani 1 1 d D . . . . H5N H 0.320(5) 0.5305(7) 1.061(3) 0.042(9) Uiso 1 1 d D . . . . H6N H 0.396(4) 0.5697(5) 1.045(3) 0.026(7) Uiso 1 1 d D . . . . O1B O 0.1730(2) 0.47657(4) 0.62017(16) 0.0200(3) Uani 1 1 d . . . . . C1C C 0.7638(3) 0.75126(6) 0.1062(2) 0.0166(4) Uani 1 1 d . . . . . C2C C 0.7164(3) 0.80305(6) 0.2256(2) 0.0166(4) Uani 1 1 d . . . . . C3C C 0.6516(3) 0.82283(5) 0.0986(2) 0.0183(4) Uani 1 1 d . . . . . C4C C 0.6438(3) 0.80630(6) -0.0211(2) 0.0185(4) Uani 1 1 d . . . . . H4CB H 0.600976 0.819162 -0.105871 0.022 Uiso 1 1 calc R U . . . F1C F 0.6028(2) 0.85856(3) 0.10305(15) 0.0249(3) Uani 1 1 d . . . . . N1C N 0.6995(3) 0.77032(5) -0.0171(2) 0.0172(4) Uani 1 1 d . . . . . H7N H 0.711(4) 0.7602(7) -0.094(3) 0.022(7) Uiso 1 1 d . . . . . N2C N 0.7642(3) 0.76756(5) 0.22647(19) 0.0173(4) Uani 1 1 d . . . . . N3C N 0.7299(3) 0.81987(6) 0.3440(2) 0.0216(4) Uani 1 1 d . . . . . H8N H 0.765(5) 0.8065(9) 0.421(4) 0.048(9) Uiso 1 1 d . . . . . H9N H 0.695(4) 0.8438(8) 0.340(3) 0.033(8) Uiso 1 1 d . . . . . O1C O 0.8182(2) 0.71868(4) 0.10250(17) 0.0207(3) Uani 1 1 d . . . . . C1 C 0.6426(3) 0.61212(6) 0.2438(2) 0.0173(4) Uani 1 1 d . . . . . C2 C 0.6211(3) 0.64024(6) 0.1480(2) 0.0202(5) Uani 1 1 d . . . . . H2 H 0.725525 0.646495 0.114189 0.024 Uiso 1 1 calc R U . . . C3 C 0.4470(4) 0.65917(6) 0.1019(2) 0.0239(5) Uani 1 1 d . . . . . H3 H 0.433067 0.678416 0.037016 0.029 Uiso 1 1 calc R U . . . C4 C 0.2925(4) 0.64990(6) 0.1509(3) 0.0252(5) Uani 1 1 d . . . . . H4 H 0.173322 0.662698 0.118849 0.030 Uiso 1 1 calc R U . . . C5 C 0.3138(3) 0.62180(6) 0.2470(3) 0.0237(5) Uani 1 1 d . . . . . H5 H 0.209201 0.615592 0.280734 0.028 Uiso 1 1 calc R U . . . C6 C 0.4882(3) 0.60281(6) 0.2935(2) 0.0191(4) Uani 1 1 d . . . . . C7 C 1.0872(3) 0.69086(6) 0.4524(2) 0.0199(4) Uani 1 1 d . . . . . C8 C 1.1522(3) 0.72682(6) 0.4795(3) 0.0236(5) Uani 1 1 d . . . . . H8 H 1.131654 0.743985 0.406606 0.028 Uiso 1 1 calc R U . . . C9 C 1.2481(3) 0.73740(6) 0.6152(3) 0.0248(5) Uani 1 1 d . . . . . H9 H 1.292364 0.761842 0.634190 0.030 Uiso 1 1 calc R U . . . C10 C 1.2788(3) 0.71229(6) 0.7219(3) 0.0254(5) Uani 1 1 d . . . . . H10 H 1.343679 0.719646 0.813639 0.030 Uiso 1 1 calc R U . . . C11 C 1.2145(3) 0.67633(6) 0.6949(3) 0.0227(5) Uani 1 1 d . . . . . H11 H 1.234692 0.659264 0.768123 0.027 Uiso 1 1 calc R U . . . C12 C 1.1208(3) 0.66553(6) 0.5605(2) 0.0189(4) Uani 1 1 d . . . . . O1 O 0.8189(2) 0.59429(4) 0.28991(17) 0.0191(3) Uani 1 1 d . . . . . H1O H 0.805(4) 0.5713(8) 0.321(3) 0.041(9) Uiso 1 1 d . . . . . O2 O 0.5197(2) 0.57564(4) 0.39144(18) 0.0233(4) Uani 1 1 d . . . . . H2O H 0.446(5) 0.5560(8) 0.360(4) 0.046(9) Uiso 1 1 d . . . . . O3 O 0.9860(2) 0.67774(5) 0.32480(18) 0.0244(4) Uani 1 1 d . . . . . H3O H 0.947(5) 0.6963(9) 0.267(4) 0.058(11) Uiso 1 1 d . . . . . O4 O 1.0563(3) 0.63009(4) 0.5347(2) 0.0248(4) Uani 1 1 d . . . . . H4O H 1.003(6) 0.6281(9) 0.450(4) 0.064(12) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0173(10) 0.0204(10) 0.0149(10) 0.0013(8) 0.0070(8) -0.0012(8) C2A 0.0137(10) 0.0200(10) 0.0151(10) 0.0013(8) 0.0070(8) 0.0027(8) C3A 0.0173(10) 0.0163(9) 0.0149(10) -0.0005(8) 0.0048(8) 0.0004(8) C4A 0.0160(10) 0.0198(10) 0.0152(10) 0.0029(8) 0.0058(8) 0.0009(8) F1A 0.0331(8) 0.0176(6) 0.0225(7) -0.0030(5) 0.0100(6) -0.0035(5) N1A 0.0213(10) 0.0195(9) 0.0121(9) 0.0007(7) 0.0075(8) -0.0025(7) N2A 0.0183(9) 0.0195(8) 0.0129(9) 0.0004(7) 0.0073(7) -0.0001(7) N3A 0.0287(11) 0.0190(9) 0.0155(9) -0.0015(7) 0.0114(8) -0.0012(8) O1A 0.0358(10) 0.0233(8) 0.0178(8) -0.0038(6) 0.0126(7) -0.0107(7) C1B 0.0159(10) 0.0191(10) 0.0132(10) 0.0005(8) 0.0068(8) 0.0009(8) C2B 0.0135(10) 0.0212(10) 0.0144(10) 0.0016(8) 0.0055(8) 0.0031(8) C3B 0.0176(10) 0.0164(9) 0.0165(10) -0.0016(8) 0.0055(8) -0.0009(8) C4B 0.0166(10) 0.0177(10) 0.0165(10) 0.0023(8) 0.0067(8) 0.0009(8) F1B 0.0300(8) 0.0206(6) 0.0197(7) -0.0035(5) 0.0087(6) -0.0063(5) N1B 0.0245(10) 0.0195(9) 0.0120(9) 0.0002(7) 0.0093(8) -0.0023(7) N2B 0.0185(9) 0.0194(8) 0.0131(9) 0.0011(7) 0.0083(7) 0.0000(7) N3B 0.0257(10) 0.0221(9) 0.0148(9) -0.0008(7) 0.0081(8) -0.0032(8) O1B 0.0269(9) 0.0189(7) 0.0164(8) -0.0017(6) 0.0099(7) -0.0036(6) C1C 0.0147(10) 0.0200(10) 0.0156(11) 0.0008(8) 0.0053(8) -0.0033(8) C2C 0.0125(10) 0.0217(10) 0.0161(11) -0.0002(8) 0.0048(8) -0.0031(8) C3C 0.0181(11) 0.0159(9) 0.0218(12) 0.0015(8) 0.0075(9) -0.0010(8) C4C 0.0172(11) 0.0201(10) 0.0189(11) 0.0059(8) 0.0064(9) -0.0001(8) F1C 0.0319(8) 0.0181(6) 0.0265(8) 0.0017(5) 0.0115(6) 0.0042(5) N1C 0.0206(10) 0.0198(9) 0.0130(9) 0.0015(7) 0.0076(8) 0.0012(7) N2C 0.0172(9) 0.0188(9) 0.0170(9) 0.0011(7) 0.0068(8) -0.0014(7) N3C 0.0265(11) 0.0201(9) 0.0186(10) -0.0022(8) 0.0073(8) -0.0011(8) O1C 0.0270(9) 0.0181(7) 0.0181(8) 0.0026(6) 0.0083(7) 0.0027(6) C1 0.0198(11) 0.0180(10) 0.0145(10) -0.0039(8) 0.0059(8) -0.0033(8) C2 0.0253(12) 0.0217(10) 0.0157(11) -0.0011(8) 0.0095(9) -0.0047(9) C3 0.0297(13) 0.0228(11) 0.0173(11) 0.0006(9) 0.0041(10) -0.0010(9) C4 0.0213(12) 0.0276(12) 0.0241(13) -0.0006(9) 0.0030(10) 0.0018(9) C5 0.0194(11) 0.0299(12) 0.0231(12) -0.0051(9) 0.0086(10) -0.0047(9) C6 0.0220(11) 0.0205(10) 0.0161(11) -0.0025(8) 0.0079(9) -0.0043(8) C7 0.0155(10) 0.0252(11) 0.0206(11) 0.0029(9) 0.0079(9) 0.0028(8) C8 0.0191(11) 0.0243(11) 0.0283(13) 0.0046(9) 0.0084(10) 0.0018(9) C9 0.0190(11) 0.0226(11) 0.0326(14) -0.0016(9) 0.0075(10) 0.0004(9) C10 0.0180(11) 0.0301(12) 0.0269(13) -0.0034(10) 0.0051(10) 0.0044(9) C11 0.0202(11) 0.0275(11) 0.0218(12) 0.0030(9) 0.0086(9) 0.0027(9) C12 0.0153(10) 0.0206(10) 0.0232(12) 0.0018(8) 0.0092(9) 0.0019(8) O1 0.0195(8) 0.0190(7) 0.0204(8) 0.0012(6) 0.0086(7) -0.0011(6) O2 0.0256(9) 0.0240(8) 0.0226(9) 0.0037(7) 0.0108(7) -0.0050(7) O3 0.0267(9) 0.0252(8) 0.0188(9) 0.0045(7) 0.0031(7) 0.0003(7) O4 0.0281(10) 0.0225(8) 0.0231(10) 0.0045(7) 0.0069(8) -0.0030(7) 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' F F 0.0171 0.0103 '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 O1A C1A N2A 121.41(19) . . ? O1A C1A N1A 118.3(2) . . ? N2A C1A N1A 120.33(19) . . ? N3A C2A N2A 118.91(19) . . ? N3A C2A C3A 121.08(19) . . ? N2A C2A C3A 120.00(19) . . ? C4A C3A F1A 121.44(18) . . ? C4A C3A C2A 120.42(19) . . ? F1A C3A C2A 118.13(19) . . ? C3A C4A N1A 117.97(19) . . ? C3A C4A H4A 121.0 . . ? N1A C4A H4A 121.0 . . ? C4A N1A C1A 121.81(19) . . ? C4A N1A H1N 119.5(17) . . ? C1A N1A H1N 118.7(17) . . ? C2A N2A C1A 119.43(18) . . ? C2A N3A H2N 120(2) . . ? C2A N3A H3N 121.0(17) . . ? H2N N3A H3N 119(3) . . ? O1B C1B N2B 121.60(18) . . ? O1B C1B N1B 118.92(19) . . ? N2B C1B N1B 119.48(18) . . ? N3B C2B N2B 119.33(19) . . ? N3B C2B C3B 121.0(2) . . ? N2B C2B C3B 119.69(19) . . ? C4B C3B F1B 121.18(19) . . ? C4B C3B C2B 120.19(19) . . ? F1B C3B C2B 118.62(19) . . ? C3B C4B N1B 118.26(19) . . ? C3B C4B H4BB 120.9 . . ? N1B C4B H4BB 120.9 . . ? C4B N1B C1B 122.09(19) . . ? C4B N1B H4N 118.9(17) . . ? C1B N1B H4N 119.0(17) . . ? C2B N2B C1B 120.21(17) . . ? C2B N3B H5N 122(2) . . ? C2B N3B H6N 116.6(19) . . ? H5N N3B H6N 122(3) . . ? O1C C1C N2C 121.7(2) . . ? O1C C1C N1C 118.10(19) . . ? N2C C1C N1C 120.23(19) . . ? N3C C2C N2C 119.5(2) . . ? N3C C2C C3C 120.0(2) . . ? N2C C2C C3C 120.5(2) . . ? C4C C3C F1C 121.4(2) . . ? C4C C3C C2C 120.3(2) . . ? F1C C3C C2C 118.25(19) . . ? C3C C4C N1C 118.1(2) . . ? C3C C4C H4CB 120.9 . . ? N1C C4C H4CB 120.9 . . ? C4C N1C C1C 121.57(19) . . ? C4C N1C H7N 118.3(17) . . ? C1C N1C H7N 119.5(17) . . ? C2C N2C C1C 119.11(19) . . ? C2C N3C H8N 118(2) . . ? C2C N3C H9N 117.5(19) . . ? H8N N3C H9N 125(3) . . ? O1 C1 C2 118.84(19) . . ? O1 C1 C6 121.2(2) . . ? C2 C1 C6 119.9(2) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.1(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C6 C5 C4 120.2(2) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? O2 C6 C5 122.7(2) . . ? O2 C6 C1 117.5(2) . . ? C5 C6 C1 119.8(2) . . ? O3 C7 C8 124.7(2) . . ? O3 C7 C12 115.4(2) . . ? C8 C7 C12 119.8(2) . . ? C7 C8 C9 119.5(2) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.3(2) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.8(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? O4 C12 C11 119.6(2) . . ? O4 C12 C7 120.2(2) . . ? C11 C12 C7 120.2(2) . . ? C1 O1 H1O 111(2) . . ? C6 O2 H2O 112(2) . . ? C7 O3 H3O 110(2) . . ? C12 O4 H4O 108(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A O1A 1.263(3) . ? C1A N2A 1.360(3) . ? C1A N1A 1.379(3) . ? C2A N3A 1.333(3) . ? C2A N2A 1.344(3) . ? C2A C3A 1.430(3) . ? C3A C4A 1.351(3) . ? C3A F1A 1.365(2) . ? C4A N1A 1.367(3) . ? C4A H4A 0.9500 . ? N1A H1N 0.911(17) . ? N3A H2N 0.911(18) . ? N3A H3N 0.885(16) . ? C1B O1B 1.261(3) . ? C1B N2B 1.360(3) . ? C1B N1B 1.380(3) . ? C2B N3B 1.338(3) . ? C2B N2B 1.343(3) . ? C2B C3B 1.432(3) . ? C3B C4B 1.348(3) . ? C3B F1B 1.362(2) . ? C4B N1B 1.366(3) . ? C4B H4BB 0.9500 . ? N1B H4N 0.921(17) . ? N3B H5N 0.898(18) . ? N3B H6N 0.891(16) . ? C1C O1C 1.259(3) . ? C1C N2C 1.363(3) . ? C1C N1C 1.389(3) . ? C2C N3C 1.332(3) . ? C2C N2C 1.343(3) . ? C2C C3C 1.433(3) . ? C3C C4C 1.348(3) . ? C3C F1C 1.358(2) . ? C4C N1C 1.374(3) . ? C4C H4CB 0.9500 . ? N1C H7N 0.90(3) . ? N3C H8N 0.89(3) . ? N3C H9N 0.91(3) . ? C1 O1 1.385(3) . ? C1 C2 1.394(3) . ? C1 C6 1.404(3) . ? C2 C3 1.391(3) . ? C2 H2 0.9500 . ? C3 C4 1.400(4) . ? C3 H3 0.9500 . ? C4 C5 1.396(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 O2 1.378(3) . ? C7 O3 1.373(3) . ? C7 C8 1.396(3) . ? C7 C12 1.404(3) . ? C8 C9 1.402(4) . ? C8 H8 0.9500 . ? C9 C10 1.390(4) . ? C9 H9 0.9500 . ? C10 C11 1.395(3) . ? C10 H10 0.9500 . ? C11 C12 1.390(3) . ? C11 H11 0.9500 . ? C12 O4 1.376(3) . ? O1 H1O 0.92(3) . ? O2 H2O 0.89(3) . ? O3 H3O 0.89(4) . ? O4 H4O 0.83(4) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H1O O1B 0.92(3) 1.84(3) 2.744(2) 168(3) 3_666 yes N3A H2N N2B 0.911(18) 2.021(19) 2.926(3) 172(3) 1_554 yes N3A H3N O1 0.885(16) 2.38(2) 2.997(3) 127(2) 3_665 yes N3C H8N O1C 0.89(3) 2.00(4) 2.885(3) 172(3) 4_576 yes N3B H5N N2A 0.898(18) 2.089(18) 2.974(3) 168(3) 1_556 yes N1C H7N N2C 0.90(3) 2.22(3) 3.117(3) 174(2) 4_575 yes N3C H9N F1B 0.91(3) 2.62(3) 3.454(3) 153(2) 4_575 yes N3C H9N F1A 0.91(3) 2.49(3) 3.040(3) 119(2) 2_655 yes N1A H1N O1B 0.911(17) 1.892(18) 2.799(3) 173(3) . yes N1B H4N O1A 0.921(17) 1.825(18) 2.739(3) 171(3) . yes O2 H2O O1A 0.89(3) 1.76(3) 2.629(2) 163(3) . yes O3 H3O O1C 0.89(4) 1.85(4) 2.683(3) 156(3) . yes O4 H4O O1 0.83(4) 2.16(4) 2.883(3) 145(3) . yes O4 H4O O3 0.83(4) 2.20(4) 2.686(3) 117(3) . 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 N3A C2A C3A C4A 178.7(2) . . . . ? N2A C2A C3A C4A -1.2(3) . . . . ? N3A C2A C3A F1A -0.3(3) . . . . ? N2A C2A C3A F1A 179.78(18) . . . . ? F1A C3A C4A N1A -179.67(18) . . . . ? C2A C3A C4A N1A 1.4(3) . . . . ? C3A C4A N1A C1A -0.1(3) . . . . ? O1A C1A N1A C4A 178.3(2) . . . . ? N2A C1A N1A C4A -1.5(3) . . . . ? N3A C2A N2A C1A 179.8(2) . . . . ? C3A C2A N2A C1A -0.3(3) . . . . ? O1A C1A N2A C2A -178.2(2) . . . . ? N1A C1A N2A C2A 1.7(3) . . . . ? N3B C2B C3B C4B -176.6(2) . . . . ? N2B C2B C3B C4B 3.0(3) . . . . ? N3B C2B C3B F1B 2.4(3) . . . . ? N2B C2B C3B F1B -177.96(18) . . . . ? F1B C3B C4B N1B 179.33(18) . . . . ? C2B C3B C4B N1B -1.7(3) . . . . ? C3B C4B N1B C1B -0.9(3) . . . . ? O1B C1B N1B C4B -178.33(19) . . . . ? N2B C1B N1B C4B 2.2(3) . . . . ? N3B C2B N2B C1B 177.95(19) . . . . ? C3B C2B N2B C1B -1.7(3) . . . . ? O1B C1B N2B C2B 179.72(19) . . . . ? N1B C1B N2B C2B -0.8(3) . . . . ? N3C C2C C3C C4C 177.8(2) . . . . ? N2C C2C C3C C4C -2.1(3) . . . . ? N3C C2C C3C F1C -0.9(3) . . . . ? N2C C2C C3C F1C 179.26(18) . . . . ? F1C C3C C4C N1C 178.54(18) . . . . ? C2C C3C C4C N1C 0.0(3) . . . . ? C3C C4C N1C C1C -0.5(3) . . . . ? O1C C1C N1C C4C -177.88(19) . . . . ? N2C C1C N1C C4C 3.2(3) . . . . ? N3C C2C N2C C1C -175.1(2) . . . . ? C3C C2C N2C C1C 4.7(3) . . . . ? O1C C1C N2C C2C 175.83(19) . . . . ? N1C C1C N2C C2C -5.2(3) . . . . ? O1 C1 C2 C3 -178.67(19) . . . . ? C6 C1 C2 C3 0.2(3) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C4 C5 C6 O2 177.9(2) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? O1 C1 C6 O2 0.9(3) . . . . ? C2 C1 C6 O2 -177.87(19) . . . . ? O1 C1 C6 C5 178.73(19) . . . . ? C2 C1 C6 C5 -0.1(3) . . . . ? O3 C7 C8 C9 177.6(2) . . . . ? C12 C7 C8 C9 -1.0(3) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C10 C11 C12 O4 -179.5(2) . . . . ? C10 C11 C12 C7 -1.3(3) . . . . ? O3 C7 C12 O4 1.0(3) . . . . ? C8 C7 C12 O4 179.7(2) . . . . ? O3 C7 C12 C11 -177.2(2) . . . . ? C8 C7 C12 C11 1.5(3) . . . . ?