#------------------------------------------------------------------------------ #$Date: 2025-03-04 21:28:44 +0200 (Tue, 04 Mar 2025) $ #$Revision: 298154 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573836.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_1573836 loop_ _publ_author_name 'Zhu, Ming' 'Huang, Pei-Zhi' 'Li, Lin-Mei' 'Yang, Yi-Xuan' 'Pan, Lei' 'Wang, Zhi-Jie' 'Ni, Hao-Fei' 'Zhang, Feng-Wen' 'Teri, Gele' 'Zhang, Zhi-Xu' 'Liu, Zunqi' 'Fu, Da-Wei' 'Zhang, Yi' _publ_section_title ; Thermal-responsive luminescence/dielectric responses with reversibly shifted light emissions. ; _journal_issue 9 _journal_name_full 'Chemical science' _journal_page_first 4101 _journal_page_last 4108 _journal_paper_doi 10.1039/d4sc06631f _journal_volume 16 _journal_year 2025 _chemical_formula_moiety 'F6 P, C12 H24 O6, C6 H9 N2' _chemical_formula_sum 'C18 H33 F6 N2 O6 P' _chemical_formula_weight 518.43 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2024-08-20 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-08-20 deposited with the CCDC. 2025-01-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.89(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.994(5) _cell_length_b 10.463(3) _cell_length_c 19.815(9) _cell_measurement_reflns_used 3720 _cell_measurement_temperature 403.00 _cell_measurement_theta_max 55.179 _cell_measurement_theta_min 3.965 _cell_volume 2441.9(17) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 403.00 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0902 _diffrn_reflns_av_unetI/netI 0.1082 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18905 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 66.601 _diffrn_reflns_theta_max 66.601 _diffrn_reflns_theta_min 4.003 _diffrn_source_current 1.1 _diffrn_source_power 0.05500000000000001 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.5441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1208 before and 0.0635 after correction. The Ratio of minimum to maximum transmission is 0.7220. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.410 _exptl_crystal_description block _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.127 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.096 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 4250 _refine_ls_number_restraints 42 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.2635 _refine_ls_R_factor_gt 0.1381 _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^)+(0.0100P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2825 _refine_ls_wR_factor_ref 0.3326 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1710 _reflns_number_total 4250 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06631f2.cif _cod_data_source_block cu_zm_45_403k_2_0m_a _cod_depositor_comments 'Adding full bibliography for 1573833--1573838.cif.' _cod_original_cell_volume 2442.0(17) _cod_database_code 1573836 _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_max 0.831 _shelx_estimated_absorpt_t_min 0.805 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(F5) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(P1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 3.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A, H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13B,H13A), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C4(H4B,H4A) 3.b Aromatic/amide H refined with riding coordinates: C6(H6), C8(H8), C14(H14), C15(H15) 3.c Idealised Me refined as rotating group: N1(H1A,H1C,H1B) ; _shelx_res_file ; TITL cu_ZM_45_403K_2_0m_a.res in P2(1)/n cu_zm_45_403k_2_0m_a.res created by SHELXL-2018/3 at 16:02:25 on 20-Aug-2024 REM Old TITL Integration of ZM_45_403K_2 REM SHELXT solution in P2(1)/n: R1 0.329, Rweak 0.247, Alpha 0.111 REM 0.526 for 230 systematic absences, Orientation as input REM Formula found by SHELXT: C25 F5 N2 O2 P CELL 1.54184 11.9942 10.4631 19.8154 90 100.891 90 ZERR 4 0.0052 0.0032 0.0087 0 0.021 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O P UNIT 72 132 24 8 24 4 ISOR 0.01 0.01 F5 F4 F6 F3 F2 F1 P1 L.S. 50 PLAN 4 SIZE 0.11 0.12 0.13 TEMP 129.85 CONF FREE F2 F6 FREE F6 F1 FREE F5 F1 FREE F5 F3 FREE F5 F4 LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 999 0.84 REM REM REM WGHT 0.010000 15.000000 FVAR 0.39051 P1 6 0.180366 0.207198 0.437718 11.00000 0.13020 0.09129 = 0.09325 0.01367 0.02054 0.00181 F1 3 0.209130 0.299624 0.391386 11.00000 0.24260 0.28106 = 0.34280 0.17806 0.08718 -0.00734 F2 3 0.114540 0.302765 0.465704 11.00000 0.30632 0.26721 = 0.23756 -0.04913 0.04582 0.09272 F3 3 0.141927 0.096236 0.470192 11.00000 0.29237 0.24517 = 0.29495 0.09488 0.06338 -0.03846 F4 3 0.261434 0.215725 0.498248 11.00000 0.29005 0.23846 = 0.27427 -0.04088 -0.14721 0.02255 F5 3 0.252566 0.118488 0.413327 11.00000 0.32902 0.30747 = 0.27000 0.01273 0.11406 0.16798 F6 3 0.073327 0.194966 0.383916 11.00000 0.25033 0.22391 = 0.26436 -0.00293 -0.04876 -0.02553 O1 5 0.713409 0.487534 0.332339 11.00000 0.10770 0.09220 = 0.11051 -0.01192 0.00633 -0.01872 O2 5 0.607114 0.069886 0.387788 11.00000 0.14742 0.09754 = 0.11254 0.01718 0.04311 -0.00093 O3 5 0.534024 0.214499 0.158650 11.00000 0.10210 0.15546 = 0.08345 -0.01179 -0.01126 0.00441 O4 5 0.592509 0.458928 0.202039 11.00000 0.11099 0.11302 = 0.09027 0.02595 0.03056 0.01460 O5 5 0.493934 0.037334 0.255156 11.00000 0.13478 0.10185 = 0.14671 -0.03755 0.03776 -0.03718 O6 5 0.688051 0.309883 0.433163 11.00000 0.11056 0.12905 = 0.07487 0.00049 0.00237 0.01227 C2 1 0.457959 0.114244 0.141889 11.00000 0.10171 0.22956 = 0.11662 -0.05488 0.00507 0.00346 AFIX 23 H2A 2 0.455589 0.088800 0.094567 11.00000 -1.20000 H2B 2 0.382455 0.141772 0.146324 11.00000 -1.20000 AFIX 0 C3 1 0.719590 0.195232 0.467183 11.00000 0.14937 0.17958 = 0.06709 0.00803 0.01413 0.04029 AFIX 23 H3A 2 0.742318 0.211051 0.516086 11.00000 -1.20000 H3B 2 0.783887 0.158843 0.450735 11.00000 -1.20000 AFIX 0 C5 1 0.736627 0.510815 0.403152 11.00000 0.13344 0.13924 = 0.12382 -0.03903 0.01201 -0.05479 AFIX 23 H5A 2 0.668406 0.541063 0.417641 11.00000 -1.20000 H5B 2 0.794084 0.576849 0.413480 11.00000 -1.20000 AFIX 0 C7 1 0.519208 -0.061312 0.300700 11.00000 0.15677 0.08761 = 0.23259 -0.01455 0.07547 -0.03257 AFIX 23 H7A 2 0.593125 -0.095720 0.297498 11.00000 -1.20000 H7B 2 0.463614 -0.128799 0.288470 11.00000 -1.20000 AFIX 0 C9 1 0.500689 0.319951 0.117404 11.00000 0.12361 0.20977 = 0.07447 -0.00008 -0.00513 0.02859 AFIX 23 H9A 2 0.427779 0.350771 0.124981 11.00000 -1.20000 H9B 2 0.493043 0.296612 0.069373 11.00000 -1.20000 AFIX 0 C10 1 0.673643 0.592714 0.292832 11.00000 0.11401 0.08575 = 0.16785 0.00807 0.03244 -0.01951 AFIX 23 H10A 2 0.725478 0.663927 0.304511 11.00000 -1.20000 H10B 2 0.599985 0.617755 0.301861 11.00000 -1.20000 AFIX 0 C11 1 0.492195 0.007007 0.186862 11.00000 0.12510 0.17086 = 0.15323 -0.09268 0.02640 -0.04957 AFIX 23 H11A 2 0.440055 -0.063396 0.173564 11.00000 -1.20000 H11B 2 0.567271 -0.020773 0.181673 11.00000 -1.20000 AFIX 0 C12 1 0.623876 0.104333 0.455059 11.00000 0.16406 0.12947 = 0.11301 0.05019 0.04931 0.04943 AFIX 23 H12A 2 0.641496 0.029776 0.484216 11.00000 -1.20000 H12B 2 0.556034 0.144230 0.465366 11.00000 -1.20000 AFIX 0 C13 1 0.587374 0.420952 0.134828 11.00000 0.13925 0.18252 = 0.08189 0.03461 0.03110 0.04538 AFIX 23 H13B 2 0.660808 0.388738 0.129023 11.00000 -1.20000 H13A 2 0.568043 0.493387 0.104308 11.00000 -1.20000 AFIX 0 C16 1 0.664095 0.560430 0.220050 11.00000 0.12248 0.11220 = 0.16206 0.05324 0.04070 0.00667 AFIX 23 H16A 2 0.635774 0.633934 0.192184 11.00000 -1.20000 H16B 2 0.738660 0.539551 0.210960 11.00000 -1.20000 AFIX 0 C17 1 0.520059 -0.020990 0.371831 11.00000 0.17330 0.11616 = 0.19682 0.03681 0.06824 -0.02078 AFIX 23 H17A 2 0.447537 0.016281 0.375818 11.00000 -1.20000 H17B 2 0.534621 -0.093454 0.402776 11.00000 -1.20000 AFIX 0 C18 1 0.775688 0.397074 0.439970 11.00000 0.10252 0.19790 = 0.09470 -0.01007 -0.01302 -0.03110 AFIX 23 H18A 2 0.838635 0.361064 0.421973 11.00000 -1.20000 H18B 2 0.802077 0.416936 0.488157 11.00000 -1.20000 AFIX 0 N1 4 0.543414 0.286676 0.301822 11.00000 0.08964 0.06477 = 0.06940 0.00261 0.01286 -0.00117 AFIX 137 H1A 2 0.562581 0.339089 0.270524 11.00000 -1.20000 H1C 2 0.552151 0.206049 0.289485 11.00000 -1.20000 H1B 2 0.587686 0.301586 0.342422 11.00000 -1.20000 AFIX 0 N2 4 0.357299 0.686191 0.354570 11.00000 0.13257 0.10491 = 0.22037 -0.00655 0.07318 0.00643 C1 1 0.403068 0.438374 0.323971 11.00000 0.06875 0.09143 = 0.09410 0.00684 0.02621 -0.00843 C4 1 0.424370 0.308619 0.306829 11.00000 0.08494 0.09246 = 0.14065 -0.02182 0.03362 -0.01744 AFIX 23 H4B 2 0.376201 0.287164 0.263265 11.00000 -1.20000 H4A 2 0.404397 0.252379 0.341605 11.00000 -1.20000 AFIX 0 C6 1 0.420606 0.482967 0.389327 11.00000 0.11456 0.10146 = 0.10015 0.00082 0.03113 0.00041 AFIX 43 H6 2 0.450942 0.429929 0.425861 11.00000 -1.20000 AFIX 0 C8 1 0.338775 0.648638 0.293540 11.00000 0.08822 0.14111 = 0.18856 0.05561 0.04205 0.02011 AFIX 43 H8 2 0.310255 0.706830 0.259114 11.00000 -1.20000 AFIX 0 C14 1 0.358918 0.523565 0.274758 11.00000 0.09389 0.15881 = 0.11604 0.00559 0.02890 0.00760 AFIX 43 H14 2 0.342178 0.498928 0.228861 11.00000 -1.20000 AFIX 0 C15 1 0.394182 0.602349 0.400523 11.00000 0.16405 0.13633 = 0.14940 -0.03891 0.05471 -0.00979 AFIX 43 H15 2 0.403158 0.628228 0.446131 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_ZM_45_403K_2_0m_a.res in P2(1)/n REM wR2 = 0.3326, GooF = S = 0.998, Restrained GooF = 1.162 for all data REM R1 = 0.1381 for 1710 Fo > 4sig(Fo) and 0.2635 for all 4250 data REM 299 parameters refined using 42 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.127, deepest hole -0.554, 1-sigma level 0.096 Q1 1 0.2042 0.3560 0.4457 11.00000 0.05 1.13 Q2 1 0.3188 0.2035 0.4468 11.00000 0.05 1.02 Q3 1 0.1875 0.1931 0.5131 11.00000 0.05 0.87 Q4 1 0.1745 0.2234 0.3632 11.00000 0.05 0.81 ; _shelx_res_checksum 37846 _shelx_hkl_file ; 1 0 0 0.00 0.17 1 0 0 0.28 0.63 -1 0 0 -0.03 0.67 -1 0 0 0.20 0.18 -1 0 0 0.39 0.13 -2 0 0 10.06 2.08 2 0 0 9.83 2.38 -2 0 0 9.61 1.17 2 0 0 8.57 1.28 -2 0 0 10.30 1.07 3 0 0 0.15 0.51 3 0 0 1.23 2.64 -3 0 0 -0.50 0.22 -3 0 0 1.45 2.31 4 0 0 3.44 0.47 4 0 0 2.74 0.84 -4 0 0 -2.41 5.85 4 0 0 2.64 0.66 -4 0 0 5.73 3.76 5 0 0 -0.07 0.27 -5 0 0 -3.01 5.37 5 0 0 -0.74 0.69 -5 0 0 -4.76 9.16 5 0 0 0.02 0.60 6 0 0 33.25 3.29 -6 0 0 29.64 9.49 -6 0 0 19.80 15.23 6 0 0 25.66 3.81 -7 0 0 -12.42 23.60 7 0 0 0.31 0.58 7 0 0 0.47 0.43 7 0 0 -0.22 2.04 8 0 0 59.26 6.53 8 0 0 -0.96 14.87 -8 0 0 58.69 6.64 8 0 0 59.65 6.30 9 0 0 -0.05 0.53 -9 0 0 -0.92 1.01 9 0 0 -0.40 0.85 9 0 0 -12.19 11.56 10 0 0 10.07 1.86 10 0 0 12.06 1.55 -10 0 0 6.87 1.80 10 0 0 5.40 13.85 11 0 0 -10.20 10.35 11 0 0 -0.49 0.49 -11 0 0 -0.07 0.92 11 0 0 -0.56 0.73 12 0 0 0.06 0.71 -12 0 0 0.93 0.97 -13 0 0 -0.52 0.67 -14 0 0 0.02 0.49 0 -1 0 0.25 0.11 0 -1 0 -0.03 0.14 0 -1 0 2.32 0.95 0 -1 0 0.16 0.12 0 1 0 -0.27 0.85 0 1 0 0.05 0.05 0 1 0 0.05 0.10 -1 -1 0 204.08 20.93 1 -1 0 222.76 21.06 -1 -1 0 196.53 21.06 1 -1 0 191.70 20.94 1 -1 0 196.01 20.99 -1 1 0 202.18 21.55 1 1 0 198.50 20.93 -1 1 0 206.71 21.87 1 1 0 199.36 21.05 -2 -1 0 4316.05 456.59 2 1 0 4351.47 456.63 -2 1 0 4536.59 457.12 -3 -1 0 3911.86 418.42 3 1 0 3951.83 418.54 -3 1 0 4109.54 419.01 -3 1 0 4151.33 419.88 4 -1 0 139.98 15.79 4 -1 0 147.86 15.43 -4 -1 0 150.80 16.93 4 -1 0 154.05 15.58 4 -1 0 154.21 15.61 -4 1 0 188.23 20.89 4 1 0 128.61 15.59 4 1 0 144.53 15.42 4 1 0 150.84 15.53 -4 1 0 158.56 18.00 5 -1 0 232.21 22.43 -5 -1 0 197.96 27.63 5 -1 0 193.23 22.84 5 -1 0 214.70 22.62 -5 -1 0 218.10 24.74 5 -1 0 219.21 22.66 5 1 0 228.45 22.40 -5 1 0 233.57 25.93 -5 1 0 232.25 28.65 5 1 0 210.66 22.42 5 1 0 178.91 22.61 5 1 0 221.46 22.55 5 1 0 224.19 22.59 -6 -1 0 86.59 13.02 6 -1 0 79.00 8.17 6 -1 0 80.01 8.79 -6 -1 0 75.98 16.87 6 -1 0 73.82 8.56 6 1 0 71.61 8.40 6 1 0 80.06 8.13 -6 1 0 82.67 14.51 -6 1 0 72.41 19.14 -7 -1 0 84.11 24.82 7 -1 0 62.71 8.70 7 -1 0 77.19 7.86 -7 1 0 99.46 32.36 -7 1 0 72.40 22.11 7 1 0 76.56 7.81 8 -1 0 19.78 2.39 8 -1 0 19.42 2.71 8 1 0 20.16 2.30 8 1 0 18.76 2.60 -8 1 0 19.90 2.82 8 1 0 2.07 14.38 -9 -1 0 9.04 1.87 9 -1 0 8.09 1.31 9 -1 0 5.74 1.56 9 1 0 9.33 1.67 9 1 0 8.73 1.24 9 1 0 -17.86 11.95 -9 1 0 10.05 1.91 10 -1 0 0.11 0.61 -10 -1 0 0.82 1.06 10 -1 0 -0.53 0.86 10 1 0 -0.35 0.86 10 1 0 -10.64 13.39 -10 1 0 -0.74 1.01 10 1 0 0.23 0.49 11 -1 0 2.32 1.10 -11 -1 0 5.50 1.52 11 -1 0 3.53 0.86 -11 1 0 3.96 1.40 11 1 0 3.93 0.73 11 1 0 2.73 1.08 11 1 0 -6.51 11.32 -12 -1 0 0.59 0.96 12 1 0 -0.23 0.79 -12 1 0 0.46 0.90 12 1 0 -0.99 10.93 -13 -1 0 -0.73 0.66 13 1 0 0.02 0.58 -13 1 0 0.35 0.70 -14 -1 0 0.24 0.51 -14 1 0 -0.05 0.45 0 -2 0 40.27 4.17 0 -2 0 38.28 4.13 0 2 0 38.10 5.36 1 -2 0 1030.04 105.75 -1 -2 0 1020.10 105.67 1 -2 0 988.16 105.76 -1 -2 0 1063.82 106.00 -1 2 0 1053.75 107.00 1 2 0 1005.95 105.88 1 2 0 1076.02 105.67 -1 2 0 907.11 106.89 2 -2 0 513.19 55.63 2 -2 0 524.73 55.61 -2 -2 0 550.73 55.50 -2 -2 0 527.18 55.76 -2 2 0 571.62 57.58 -2 2 0 547.49 56.75 2 2 0 525.09 55.50 2 2 0 533.25 55.71 3 -2 0 4.91 0.96 3 -2 0 6.78 1.31 3 -2 0 5.67 0.96 3 -2 0 6.01 0.77 -3 -2 0 9.41 2.32 -3 2 0 6.28 4.37 -3 2 0 3.91 5.66 3 2 0 6.82 0.70 3 2 0 5.64 0.85 4 -2 0 15.48 2.42 4 -2 0 18.66 2.15 4 -2 0 19.98 2.48 -4 -2 0 21.75 6.15 4 -2 0 18.72 2.64 -4 -2 0 18.03 4.26 4 2 0 20.40 2.22 -4 2 0 22.87 9.93 4 2 0 20.77 2.09 4 2 0 19.42 2.11 -4 2 0 14.26 5.89 4 2 0 21.25 2.31 5 -2 0 18.12 2.53 -5 -2 0 15.99 8.69 -5 -2 0 18.62 5.87 5 -2 0 16.47 2.55 5 -2 0 18.03 2.04 5 -2 0 16.31 2.65 -5 2 0 4.21 11.89 -5 2 0 11.87 7.98 5 2 0 18.94 2.05 5 2 0 19.19 2.38 5 2 0 18.34 2.00 6 -2 0 59.51 6.83 6 -2 0 51.60 6.83 -6 -2 0 50.38 11.08 -6 -2 0 85.12 15.80 6 -2 0 58.02 6.20 6 2 0 56.56 6.43 -6 2 0 56.44 13.83 6 2 0 60.70 6.11 -6 2 0 60.44 24.27 7 -2 0 63.01 7.15 -7 -2 0 91.58 24.36 7 -2 0 46.82 8.12 7 -2 0 65.61 6.93 7 2 0 71.41 6.84 -7 2 0 62.70 21.91 -7 2 0 97.04 36.17 8 -2 0 136.14 14.92 8 -2 0 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-21 -0.75 1.07 2 0 -21 -1.46 1.12 1 0 -21 1.06 1.32 0 0 -21 -0.09 1.13 -1 0 -21 -0.02 1.05 -2 0 -21 -1.03 0.87 -3 0 -21 2.67 1.04 -4 0 -21 -0.20 0.71 -5 0 -21 1.17 0.81 5 -1 -21 -2.78 0.94 4 -1 -21 0.09 1.12 3 -1 -21 4.56 1.51 2 -1 -21 -0.87 1.22 2 1 -21 0.10 0.65 1 -1 -21 -1.20 1.08 1 1 -21 0.27 1.09 0 -1 -21 -1.11 1.12 0 1 -21 -0.14 1.05 -1 -1 -21 -0.85 1.01 -1 1 -21 -0.02 1.02 -2 -1 -21 -0.42 0.90 -2 1 -21 -0.87 0.88 -3 -1 -21 0.05 0.85 -3 1 -21 -0.27 0.80 -4 -1 -21 -1.43 0.65 -4 1 -21 0.06 0.69 -5 -1 -21 -0.29 0.64 -5 1 -21 0.25 0.79 8 2 -21 1.92 6.77 5 -2 -21 2.08 1.13 4 -2 -21 0.69 1.17 3 -2 -21 0.82 1.27 2 -2 -21 1.82 1.37 1 -2 -21 2.48 1.29 0 -2 -21 -1.15 1.02 -1 -2 -21 -0.61 0.99 -1 2 -21 0.47 0.49 -2 -2 -21 -1.17 0.82 -2 2 -21 1.33 0.69 -3 -2 -21 1.59 0.97 -3 2 -21 1.91 1.09 -4 -2 -21 -0.83 0.66 8 3 -21 -4.55 5.40 6 -3 -21 -1.03 0.73 5 -3 -21 0.17 1.04 4 -3 -21 -0.68 1.06 3 -3 -21 0.36 1.22 2 -3 -21 1.30 1.28 1 -3 -21 0.75 1.19 0 -3 -21 -0.27 1.03 -1 -3 -21 -0.04 1.02 -2 -3 -21 -0.67 0.86 -3 -3 -21 -1.03 0.74 -4 -3 -21 0.18 0.71 8 4 -21 0.24 5.94 6 -4 -21 0.17 0.74 5 -4 -21 0.60 0.97 4 -4 -21 -0.41 1.03 3 -4 -21 0.32 1.15 2 -4 -21 0.14 1.11 1 -4 -21 -0.74 1.08 0 -4 -21 -0.48 1.03 -1 -4 -21 -0.35 0.90 -2 -4 -21 -0.63 0.78 -3 -4 -21 0.66 0.79 7 5 -21 2.00 6.24 6 -5 -21 0.39 0.64 5 -5 -21 0.53 0.81 4 -5 -21 0.42 0.98 3 -5 -21 0.52 0.98 2 -5 -21 -0.50 0.96 1 -5 -21 0.65 1.07 0 -5 -21 -0.38 0.92 -1 -5 -21 1.15 0.94 -2 -5 -21 -0.38 0.78 5 -6 -21 0.43 0.65 4 -6 -21 0.74 0.79 3 -6 -21 0.02 0.90 2 -6 -21 1.73 0.99 1 -6 -21 0.04 0.86 0 -6 -21 0.12 0.82 -1 -6 -21 -0.27 0.75 2 0 -22 0.22 0.99 1 0 -22 0.69 1.07 0 0 -22 4.54 1.33 -1 0 -22 -0.24 0.85 -2 0 -22 -0.63 0.75 -3 0 -22 -0.80 0.62 -4 0 -22 0.44 0.59 3 -1 -22 -2.32 0.91 2 -1 -22 2.04 1.18 1 -1 -22 0.34 1.13 0 -1 -22 1.07 1.07 0 1 -22 0.05 0.82 -1 -1 -22 -0.85 0.88 -1 1 -22 -0.63 0.80 -2 -1 -22 0.98 0.83 -2 1 -22 -0.23 0.69 -3 -1 -22 0.27 0.74 -4 -1 -22 0.32 0.66 4 -2 -22 0.12 0.95 3 -2 -22 -0.29 1.03 2 -2 -22 -0.73 1.08 1 -2 -22 0.06 1.09 0 -2 -22 1.19 1.09 -1 -2 -22 0.19 0.94 -2 -2 -22 0.41 0.84 -3 -2 -22 -0.64 0.69 5 -3 -22 0.20 0.74 4 -3 -22 0.70 0.99 3 -3 -22 0.88 1.07 2 -3 -22 -0.20 1.04 1 -3 -22 2.46 1.18 0 -3 -22 -0.44 0.90 -1 -3 -22 0.06 0.88 -2 -3 -22 -0.26 0.78 -3 -3 -22 -0.92 0.64 7 4 -22 3.59 6.47 5 -4 -22 -0.05 0.69 4 -4 -22 0.45 0.90 3 -4 -22 1.02 0.99 2 -4 -22 0.71 1.01 1 -4 -22 -0.47 0.90 0 -4 -22 0.18 0.93 -1 -4 -22 0.45 0.87 -2 -4 -22 -0.51 0.77 5 -5 -22 0.52 0.59 4 -5 -22 0.41 0.75 3 -5 -22 0.33 0.82 2 -5 -22 0.31 0.84 1 -5 -22 1.57 0.91 0 -5 -22 0.51 0.82 -1 -5 -22 -0.79 0.77 0 0 -23 0.02 0.77 -1 0 -23 0.83 0.73 2 -1 -23 0.53 0.82 1 -1 -23 0.22 0.90 0 -1 -23 -0.19 0.85 -1 -1 -23 0.72 0.81 -2 -1 -23 -0.30 0.68 3 -2 -23 -0.73 0.75 2 -2 -23 -0.05 0.88 1 -2 -23 -0.38 0.87 0 -2 -23 0.03 0.85 -1 -2 -23 0.70 0.80 -2 -2 -23 0.14 0.70 4 -3 -23 -1.63 0.66 3 -3 -23 -0.46 0.82 2 -3 -23 1.41 0.93 1 -3 -23 0.40 0.89 0 -3 -23 0.37 0.81 -1 -3 -23 -0.22 0.74 4 -4 -23 -0.67 0.64 3 -4 -23 0.07 0.77 2 -4 -23 -0.15 0.75 1 -4 -23 0.82 0.80 0 -4 -23 -0.08 0.74 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 36589 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 P1 P 0.18037(13) 0.20720(14) 0.43772(7) 0.1050(5) Uani 1 1 d . U . . . F1 F 0.2091(4) 0.2996(5) 0.3914(3) 0.285(2) Uani 1 1 d . U . . . F2 F 0.1145(5) 0.3028(5) 0.4657(3) 0.271(2) Uani 1 1 d . U . . . F3 F 0.1419(5) 0.0962(5) 0.4702(3) 0.276(2) Uani 1 1 d . U . . . F4 F 0.2614(5) 0.2157(5) 0.4982(3) 0.294(2) Uani 1 1 d . U . . . F5 F 0.2526(5) 0.1185(6) 0.4133(3) 0.295(2) Uani 1 1 d . U . . . F6 F 0.0733(5) 0.1950(5) 0.3839(3) 0.259(2) Uani 1 1 d . U . . . O1 O 0.7134(3) 0.4875(3) 0.33234(16) 0.1053(12) Uani 1 1 d . . . . . O2 O 0.6071(3) 0.0699(3) 0.38779(16) 0.1167(13) Uani 1 1 d . . . . . O3 O 0.5340(3) 0.2145(4) 0.15865(15) 0.1174(14) Uani 1 1 d . . . . . O4 O 0.5925(3) 0.4589(3) 0.20204(14) 0.1033(11) Uani 1 1 d . . . . . O5 O 0.4939(3) 0.0373(3) 0.25516(18) 0.1263(14) Uani 1 1 d . . . . . O6 O 0.6881(3) 0.3099(3) 0.43316(14) 0.1068(12) Uani 1 1 d . . . . . C2 C 0.4580(5) 0.1142(7) 0.1419(3) 0.151(3) Uani 1 1 d . . . . . H2A H 0.455589 0.088800 0.094567 0.182 Uiso 1 1 calc R U . . . H2B H 0.382455 0.141772 0.146324 0.182 Uiso 1 1 calc R U . . . C3 C 0.7196(5) 0.1952(6) 0.4672(2) 0.133(2) Uani 1 1 d . . . . . H3A H 0.742318 0.211051 0.516086 0.159 Uiso 1 1 calc R U . . . H3B H 0.783887 0.158843 0.450735 0.159 Uiso 1 1 calc R U . . . C5 C 0.7366(5) 0.5108(6) 0.4032(3) 0.134(2) Uani 1 1 d . . . . . H5A H 0.668406 0.541063 0.417641 0.161 Uiso 1 1 calc R U . . . H5B H 0.794084 0.576849 0.413480 0.161 Uiso 1 1 calc R U . . . C7 C 0.5192(5) -0.0613(5) 0.3007(3) 0.154(3) Uani 1 1 d . . . . . H7A H 0.593125 -0.095720 0.297498 0.185 Uiso 1 1 calc R U . . . H7B H 0.463614 -0.128799 0.288470 0.185 Uiso 1 1 calc R U . . . C9 C 0.5007(5) 0.3200(6) 0.1174(2) 0.139(3) Uani 1 1 d . . . . . H9A H 0.427779 0.350771 0.124981 0.167 Uiso 1 1 calc R U . . . H9B H 0.493043 0.296612 0.069373 0.167 Uiso 1 1 calc R U . . . C10 C 0.6736(5) 0.5927(5) 0.2928(3) 0.122(2) Uani 1 1 d . . . . . H10A H 0.725478 0.663927 0.304511 0.146 Uiso 1 1 calc R U . . . H10B H 0.599985 0.617755 0.301861 0.146 Uiso 1 1 calc R U . . . C11 C 0.4922(5) 0.0070(6) 0.1869(3) 0.150(2) Uani 1 1 d . . . . . H11A H 0.440055 -0.063396 0.173564 0.180 Uiso 1 1 calc R U . . . H11B H 0.567271 -0.020773 0.181673 0.180 Uiso 1 1 calc R U . . . C12 C 0.6239(5) 0.1043(5) 0.4551(2) 0.132(2) Uani 1 1 d . . . . . H12A H 0.641496 0.029776 0.484216 0.159 Uiso 1 1 calc R U . . . H12B H 0.556034 0.144230 0.465366 0.159 Uiso 1 1 calc R U . . . C13 C 0.5874(5) 0.4210(6) 0.1348(2) 0.133(2) Uani 1 1 d . . . . . H13B H 0.660808 0.388738 0.129023 0.160 Uiso 1 1 calc R U . . . H13A H 0.568043 0.493387 0.104308 0.160 Uiso 1 1 calc R U . . . C16 C 0.6641(5) 0.5604(5) 0.2200(3) 0.130(2) Uani 1 1 d . . . . . H16A H 0.635774 0.633934 0.192184 0.157 Uiso 1 1 calc R U . . . H16B H 0.738660 0.539551 0.210960 0.157 Uiso 1 1 calc R U . . . C17 C 0.5201(5) -0.0210(6) 0.3718(3) 0.158(3) Uani 1 1 d . . . . . H17A H 0.447537 0.016281 0.375818 0.189 Uiso 1 1 calc R U . . . H17B H 0.534621 -0.093454 0.402776 0.189 Uiso 1 1 calc R U . . . C18 C 0.7757(4) 0.3971(6) 0.4400(3) 0.136(3) Uani 1 1 d . . . . . H18A H 0.838635 0.361064 0.421973 0.163 Uiso 1 1 calc R U . . . H18B H 0.802077 0.416936 0.488157 0.163 Uiso 1 1 calc R U . . . N1 N 0.5434(3) 0.2867(3) 0.30182(15) 0.0749(11) Uani 1 1 d . . . . . H1A H 0.562581 0.339089 0.270524 0.090 Uiso 1 1 calc R U . . . H1C H 0.552151 0.206049 0.289485 0.090 Uiso 1 1 calc R U . . . H1B H 0.587686 0.301586 0.342422 0.090 Uiso 1 1 calc R U . . . N2 N 0.3573(4) 0.6862(5) 0.3546(3) 0.147(2) Uani 1 1 d . . . . . C1 C 0.4031(3) 0.4384(4) 0.3240(2) 0.0833(14) Uani 1 1 d . . . . . C4 C 0.4244(4) 0.3086(4) 0.3068(3) 0.1044(18) Uani 1 1 d . . . . . H4B H 0.376201 0.287164 0.263265 0.125 Uiso 1 1 calc R U . . . H4A H 0.404397 0.252379 0.341605 0.125 Uiso 1 1 calc R U . . . C6 C 0.4206(4) 0.4830(5) 0.3893(2) 0.1040(18) Uani 1 1 d . . . . . H6 H 0.450942 0.429929 0.425861 0.125 Uiso 1 1 calc R U . . . C8 C 0.3388(4) 0.6486(6) 0.2935(3) 0.137(2) Uani 1 1 d . . . . . H8 H 0.310255 0.706830 0.259114 0.165 Uiso 1 1 calc R U . . . C14 C 0.3589(4) 0.5236(6) 0.2748(3) 0.122(2) Uani 1 1 d . . . . . H14 H 0.342178 0.498928 0.228861 0.146 Uiso 1 1 calc R U . . . C15 C 0.3942(5) 0.6023(6) 0.4005(3) 0.147(3) Uani 1 1 d . . . . . H15 H 0.403158 0.628228 0.446131 0.176 Uiso 1 1 calc R U . . . 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 P1 0.1302(11) 0.0913(8) 0.0933(8) 0.0137(7) 0.0205(7) 0.0018(9) F1 0.243(4) 0.281(4) 0.343(4) 0.178(3) 0.087(3) -0.007(3) F2 0.306(4) 0.267(4) 0.238(4) -0.049(3) 0.046(3) 0.093(3) F3 0.292(4) 0.245(4) 0.295(4) 0.095(3) 0.063(3) -0.038(3) F4 0.290(4) 0.238(4) 0.274(4) -0.041(3) -0.147(3) 0.023(3) F5 0.329(4) 0.307(4) 0.270(4) 0.013(3) 0.114(3) 0.168(3) F6 0.250(4) 0.224(4) 0.264(4) -0.003(3) -0.049(3) -0.026(3) O1 0.108(2) 0.092(2) 0.111(2) -0.0119(19) 0.0063(19) -0.019(2) O2 0.147(3) 0.098(2) 0.113(2) 0.0172(19) 0.0431(19) -0.001(2) O3 0.102(2) 0.155(3) 0.0835(19) -0.012(2) -0.0113(18) 0.004(2) O4 0.111(2) 0.113(2) 0.0903(17) 0.0259(17) 0.0306(16) 0.015(2) O5 0.135(3) 0.102(2) 0.147(3) -0.038(2) 0.038(2) -0.037(2) O6 0.111(2) 0.129(3) 0.0749(17) 0.0005(19) 0.0024(17) 0.012(2) C2 0.102(4) 0.230(7) 0.117(4) -0.055(4) 0.005(3) 0.003(5) C3 0.149(5) 0.180(6) 0.067(3) 0.008(3) 0.014(3) 0.040(4) C5 0.133(4) 0.139(4) 0.124(4) -0.039(3) 0.012(3) -0.055(4) C7 0.157(5) 0.088(4) 0.233(6) -0.015(4) 0.075(4) -0.033(4) C9 0.124(4) 0.210(6) 0.074(3) 0.000(4) -0.005(3) 0.029(5) C10 0.114(4) 0.086(3) 0.168(5) 0.008(3) 0.032(3) -0.020(3) C11 0.125(4) 0.171(5) 0.153(4) -0.093(3) 0.026(4) -0.050(4) C12 0.164(5) 0.129(4) 0.113(3) 0.050(3) 0.049(3) 0.049(4) C13 0.139(4) 0.183(5) 0.082(3) 0.035(3) 0.031(3) 0.045(4) C16 0.122(4) 0.112(4) 0.162(4) 0.053(3) 0.041(3) 0.007(3) C17 0.173(5) 0.116(4) 0.197(5) 0.037(4) 0.068(4) -0.021(4) C18 0.103(4) 0.198(6) 0.095(3) -0.010(4) -0.013(3) -0.031(4) N1 0.090(2) 0.0648(18) 0.0694(18) 0.0026(16) 0.0129(16) -0.0012(19) N2 0.133(3) 0.105(3) 0.220(4) -0.007(3) 0.073(3) 0.006(3) C1 0.069(2) 0.091(3) 0.094(3) 0.007(2) 0.026(2) -0.008(2) C4 0.085(3) 0.092(3) 0.141(4) -0.022(3) 0.034(3) -0.017(3) C6 0.115(3) 0.101(3) 0.100(3) 0.001(3) 0.031(3) 0.000(3) C8 0.088(3) 0.141(5) 0.189(5) 0.056(4) 0.042(3) 0.020(3) C14 0.094(3) 0.159(5) 0.116(4) 0.006(4) 0.029(3) 0.008(4) C15 0.164(5) 0.136(5) 0.149(4) -0.039(4) 0.055(4) -0.010(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 F1 P1 F2 89.7(3) . . ? F1 P1 F3 166.5(3) . . ? F1 P1 F6 83.1(3) . . ? F2 P1 F6 82.9(3) . . ? F3 P1 F2 98.1(3) . . ? F3 P1 F6 86.9(3) . . ? F4 P1 F1 107.3(3) . . ? F4 P1 F2 88.2(3) . . ? F4 P1 F3 84.1(3) . . ? F4 P1 F5 87.9(3) . . ? F4 P1 F6 166.4(4) . . ? F5 P1 F1 89.2(3) . . ? F5 P1 F2 175.4(3) . . ? F5 P1 F3 83.8(3) . . ? F5 P1 F6 101.3(3) . . ? C10 O1 C5 114.3(4) . . ? C12 O2 C17 111.5(4) . . ? C9 O3 C2 110.9(4) . . ? C16 O4 C13 112.7(4) . . ? C7 O5 C11 115.6(4) . . ? C18 O6 C3 113.0(4) . . ? O3 C2 H2A 109.7 . . ? O3 C2 H2B 109.7 . . ? O3 C2 C11 110.0(4) . . ? H2A C2 H2B 108.2 . . ? C11 C2 H2A 109.7 . . ? C11 C2 H2B 109.7 . . ? O6 C3 H3A 109.6 . . ? O6 C3 H3B 109.6 . . ? O6 C3 C12 110.2(4) . . ? H3A C3 H3B 108.1 . . ? C12 C3 H3A 109.6 . . ? C12 C3 H3B 109.6 . . ? O1 C5 H5A 109.5 . . ? O1 C5 H5B 109.5 . . ? O1 C5 C18 110.6(5) . . ? H5A C5 H5B 108.1 . . ? C18 C5 H5A 109.5 . . ? C18 C5 H5B 109.5 . . ? O5 C7 H7A 109.2 . . ? O5 C7 H7B 109.2 . . ? O5 C7 C17 112.1(5) . . ? H7A C7 H7B 107.9 . . ? C17 C7 H7A 109.2 . . ? C17 C7 H7B 109.2 . . ? O3 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? O3 C9 C13 108.7(4) . . ? H9A C9 H9B 108.3 . . ? C13 C9 H9A 110.0 . . ? C13 C9 H9B 110.0 . . ? O1 C10 H10A 109.8 . . ? O1 C10 H10B 109.8 . . ? O1 C10 C16 109.2(4) . . ? H10A C10 H10B 108.3 . . ? C16 C10 H10A 109.8 . . ? C16 C10 H10B 109.8 . . ? O5 C11 C2 112.0(5) . . ? O5 C11 H11A 109.2 . . ? O5 C11 H11B 109.2 . . ? C2 C11 H11A 109.2 . . ? C2 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? O2 C12 C3 107.3(4) . . ? O2 C12 H12A 110.3 . . ? O2 C12 H12B 110.3 . . ? C3 C12 H12A 110.3 . . ? C3 C12 H12B 110.3 . . ? H12A C12 H12B 108.5 . . ? O4 C13 C9 109.4(4) . . ? O4 C13 H13B 109.8 . . ? O4 C13 H13A 109.8 . . ? C9 C13 H13B 109.8 . . ? C9 C13 H13A 109.8 . . ? H13B C13 H13A 108.2 . . ? O4 C16 C10 111.3(4) . . ? O4 C16 H16A 109.4 . . ? O4 C16 H16B 109.4 . . ? C10 C16 H16A 109.4 . . ? C10 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? O2 C17 C7 106.3(5) . . ? O2 C17 H17A 110.5 . . ? O2 C17 H17B 110.5 . . ? C7 C17 H17A 110.5 . . ? C7 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? O6 C18 C5 109.3(4) . . ? O6 C18 H18A 109.8 . . ? O6 C18 H18B 109.8 . . ? C5 C18 H18A 109.8 . . ? C5 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? H1A N1 H1C 109.5 . . ? H1A N1 H1B 109.5 . . ? H1C N1 H1B 109.5 . . ? C4 N1 H1A 109.5 . . ? C4 N1 H1C 109.5 . . ? C4 N1 H1B 109.5 . . ? C8 N2 C15 116.5(6) . . ? C6 C1 C4 123.4(4) . . ? C14 C1 C4 121.1(4) . . ? C14 C1 C6 115.5(5) . . ? N1 C4 H4B 109.1 . . ? N1 C4 H4A 109.1 . . ? C1 C4 N1 112.5(4) . . ? C1 C4 H4B 109.1 . . ? C1 C4 H4A 109.1 . . ? H4B C4 H4A 107.8 . . ? C1 C6 H6 120.4 . . ? C15 C6 C1 119.2(5) . . ? C15 C6 H6 120.4 . . ? N2 C8 H8 118.5 . . ? N2 C8 C14 123.0(6) . . ? C14 C8 H8 118.5 . . ? C1 C14 C8 119.3(5) . . ? C1 C14 H14 120.3 . . ? C8 C14 H14 120.3 . . ? N2 C15 C6 126.2(6) . . ? N2 C15 H15 116.9 . . ? C6 C15 H15 116.9 . . ? 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 P1 F1 1.420(5) . ? P1 F2 1.448(6) . ? P1 F3 1.445(6) . ? P1 F4 1.397(5) . ? P1 F5 1.415(6) . ? P1 F6 1.511(5) . ? O1 C5 1.399(6) . ? O1 C10 1.382(6) . ? O2 C12 1.359(6) . ? O2 C17 1.403(7) . ? O3 C2 1.389(7) . ? O3 C9 1.386(7) . ? O4 C13 1.380(5) . ? O4 C16 1.370(6) . ? O5 C7 1.367(7) . ? O5 C11 1.386(6) . ? O6 C3 1.393(6) . ? O6 C18 1.379(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C11 1.443(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C12 1.475(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C18 1.428(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C17 1.469(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C13 1.477(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C16 1.465(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13B 0.9700 . ? C13 H13A 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N1 H1A 0.8900 . ? N1 H1C 0.8900 . ? N1 H1B 0.8900 . ? N1 C4 1.468(5) . ? N2 C8 1.251(8) . ? N2 C15 1.281(8) . ? C1 C4 1.434(6) . ? C1 C6 1.355(6) . ? C1 C14 1.353(7) . ? C4 H4B 0.9700 . ? C4 H4A 0.9700 . ? C6 H6 0.9300 . ? C6 C15 1.318(8) . ? C8 H8 0.9300 . ? C8 C14 1.394(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? 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 O1 C5 C18 O6 -67.9(6) . . . . ? O1 C10 C16 O4 58.7(6) . . . . ? O3 C2 C11 O5 61.0(6) . . . . ? O3 C9 C13 O4 -63.3(6) . . . . ? O5 C7 C17 O2 -62.8(6) . . . . ? O6 C3 C12 O2 68.7(6) . . . . ? C2 O3 C9 C13 -177.0(5) . . . . ? C3 O6 C18 C5 179.4(4) . . . . ? C5 O1 C10 C16 174.0(4) . . . . ? C7 O5 C11 C2 176.4(5) . . . . ? C9 O3 C2 C11 -178.1(5) . . . . ? C10 O1 C5 C18 179.2(5) . . . . ? C11 O5 C7 C17 179.6(5) . . . . ? C12 O2 C17 C7 -173.5(4) . . . . ? C13 O4 C16 C10 -176.1(4) . . . . ? C16 O4 C13 C9 -174.6(4) . . . . ? C17 O2 C12 C3 177.6(4) . . . . ? C18 O6 C3 C12 -177.3(4) . . . . ? N2 C8 C14 C1 -1.6(8) . . . . ? C1 C6 C15 N2 -3.7(10) . . . . ? C4 C1 C6 C15 -177.2(5) . . . . ? C4 C1 C14 C8 179.6(5) . . . . ? C6 C1 C4 N1 -84.8(6) . . . . ? C6 C1 C14 C8 2.2(7) . . . . ? C8 N2 C15 C6 4.3(10) . . . . ? C14 C1 C4 N1 98.0(5) . . . . ? C14 C1 C6 C15 0.2(7) . . . . ? C15 N2 C8 C14 -1.5(9) . . . . ?