#------------------------------------------------------------------------------ #$Date: 2025-02-03 01:06:21 +0200 (Mon, 03 Feb 2025) $ #$Revision: 297568 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573835.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_1573835 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_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06631F _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 _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 100.318(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.0220(15) _cell_length_b 10.629(2) _cell_length_c 19.921(4) _cell_measurement_reflns_used 3173 _cell_measurement_temperature 343.00 _cell_measurement_theta_max 63.812 _cell_measurement_theta_min 4.007 _cell_volume 2504.4(8) _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 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 343.00 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _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 0.1761 _diffrn_reflns_av_unetI/netI 0.1057 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _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 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 30653 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 66.838 _diffrn_reflns_theta_max 66.838 _diffrn_reflns_theta_min 4.005 _diffrn_source_current 1.1 _diffrn_source_power 0.05500000000000001 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.5639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1496 before and 0.0850 after correction. The Ratio of minimum to maximum transmission is 0.7491. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.375 _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 0.847 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 4423 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.2332 _refine_ls_R_factor_gt 0.1255 _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^+14.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2452 _refine_ls_wR_factor_ref 0.2979 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1834 _reflns_number_total 4423 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06631f2.cif _cod_data_source_block cu_zm_45_343k_2_0m_a _cod_database_code 1573835 _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 0.835 _shelx_estimated_absorpt_t_min 0.809 _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.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C13(H13A,H13B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C7(H7), C15(H15), C17(H17) 2.c Idealised Me refined as rotating group: N1(H1C,H1D,H1E) ; _shelx_res_file ; TITL cu_ZM_45_343K_2_0m_a.res in P2(1)/n cu_zm_45_343k_2_0m_a.res created by SHELXL-2018/3 at 15:32:39 on 20-Aug-2024 REM Old TITL Integration of ZM_45_343K_2 REM SHELXT solution in P2(1)/n: R1 0.310, Rweak 0.138, Alpha 0.077 REM 0.395 for 259 systematic absences, Orientation as input REM Formula found by SHELXT: C25 F2 N2 O4 P CELL 1.54184 12.022 10.6291 19.9212 90 100.318 90 ZERR 4 0.0015 0.0023 0.004 0 0.013 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 L.S. 50 PLAN 1 SIZE 0.11 0.12 0.13 TEMP 69.85 CONF FREE F6 F5 FREE F2 F1 FREE F3 F1 FREE F4 F6 LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.010000 14.000000 FVAR 0.40033 P1 6 0.180007 0.795053 0.436562 11.00000 0.09168 0.06937 = 0.07699 -0.00782 0.01064 -0.00114 F1 3 0.072311 0.804842 0.387006 11.00000 0.16836 0.15888 = 0.37296 -0.02682 -0.12312 0.02171 F2 3 0.129786 0.685149 0.461959 11.00000 0.52143 0.24519 = 0.16985 0.09658 -0.05334 -0.25757 F3 3 0.208969 0.709740 0.384152 11.00000 0.15365 0.35237 = 0.45258 -0.30007 0.12048 -0.04359 F4 3 0.290924 0.787600 0.476330 11.00000 0.25778 0.14752 = 0.53452 -0.06193 -0.27203 0.03615 F5 3 0.157864 0.877483 0.488917 11.00000 0.43646 0.41309 = 0.29806 -0.27485 0.27065 -0.20288 F6 3 0.221632 0.911043 0.410027 11.00000 0.42309 0.20642 = 0.21063 0.05227 -0.02737 -0.20232 O1 5 0.687009 0.692130 0.434772 11.00000 0.07453 0.09924 = 0.05882 0.00218 -0.00123 -0.00177 O2 5 0.608166 0.934218 0.387488 11.00000 0.12098 0.07164 = 0.09493 -0.01299 0.04165 0.00025 O3 5 0.593600 0.537878 0.202881 11.00000 0.07896 0.08656 = 0.07041 -0.01542 0.01540 -0.00301 O4 5 0.495275 0.964159 0.254988 11.00000 0.10574 0.07518 = 0.11430 0.02569 0.03418 0.01959 O5 5 0.714612 0.512392 0.334048 11.00000 0.07775 0.06943 = 0.07915 0.01196 0.00427 0.01054 O6 5 0.536151 0.785603 0.157898 11.00000 0.06727 0.11745 = 0.06934 0.01774 -0.00399 -0.00736 C1 1 0.523788 1.067841 0.299649 11.00000 0.14350 0.06166 = 0.18191 0.00930 0.05801 0.03335 AFIX 23 H1A 2 0.469561 1.135194 0.287239 11.00000 -1.20000 H1B 2 0.598092 1.099176 0.295631 11.00000 -1.20000 AFIX 0 C4 1 0.737515 0.485062 0.405156 11.00000 0.09909 0.11211 = 0.09924 0.03397 0.00917 0.03495 AFIX 23 H4A 2 0.795163 0.420448 0.414686 11.00000 -1.20000 H4B 2 0.669593 0.454675 0.419764 11.00000 -1.20000 AFIX 0 C5 1 0.589418 0.577978 0.133598 11.00000 0.10340 0.12137 = 0.06848 -0.01910 0.02802 -0.02484 AFIX 23 H5A 2 0.571025 0.506991 0.103025 11.00000 -1.20000 H5B 2 0.662763 0.610100 0.128078 11.00000 -1.20000 AFIX 0 C6 1 0.624129 0.896732 0.457212 11.00000 0.12935 0.10910 = 0.09327 -0.03545 0.04558 -0.05000 AFIX 23 H6A 2 0.556208 0.856523 0.466735 11.00000 -1.20000 H6B 2 0.640008 0.969688 0.486618 11.00000 -1.20000 AFIX 0 C8 1 0.497334 0.995411 0.184530 11.00000 0.10091 0.10854 = 0.10986 0.05198 0.01925 0.03092 AFIX 23 H8A 2 0.573487 1.018696 0.179634 11.00000 -1.20000 H8B 2 0.448098 1.066686 0.170834 11.00000 -1.20000 AFIX 0 C9 1 0.667888 0.435017 0.221092 11.00000 0.08406 0.08199 = 0.13743 -0.03999 0.03337 -0.00013 AFIX 23 H9A 2 0.742721 0.456276 0.212803 11.00000 -1.20000 H9B 2 0.641040 0.362410 0.193370 11.00000 -1.20000 AFIX 0 C10 1 0.503349 0.676906 0.116327 11.00000 0.08301 0.16087 = 0.05952 0.00269 -0.00349 -0.03149 AFIX 23 H10A 2 0.496049 0.699029 0.068498 11.00000 -1.20000 H10B 2 0.430709 0.646382 0.124148 11.00000 -1.20000 AFIX 0 C11 1 0.523450 1.027554 0.371924 11.00000 0.15582 0.08602 = 0.15147 -0.02174 0.07316 0.02304 AFIX 23 H11A 2 0.539927 1.098517 0.402715 11.00000 -1.20000 H11B 2 0.450165 0.993588 0.376222 11.00000 -1.20000 AFIX 0 C12 1 0.777266 0.602738 0.442314 11.00000 0.08046 0.15217 = 0.07911 0.01429 -0.00822 0.01357 AFIX 23 H12A 2 0.802815 0.584364 0.490294 11.00000 -1.20000 H12B 2 0.840406 0.637465 0.424194 11.00000 -1.20000 AFIX 0 C14 1 0.673486 0.404670 0.293991 11.00000 0.09445 0.04815 = 0.13461 0.00052 0.01887 0.00881 AFIX 23 H14A 2 0.598952 0.382057 0.302276 11.00000 -1.20000 H14B 2 0.723673 0.333754 0.306580 11.00000 -1.20000 AFIX 0 C16 1 0.720807 0.807229 0.470214 11.00000 0.10614 0.13355 = 0.07105 -0.01725 0.01007 -0.04300 AFIX 23 H16A 2 0.785586 0.842700 0.454117 11.00000 -1.20000 H16B 2 0.741940 0.791272 0.518769 11.00000 -1.20000 AFIX 0 C18 1 0.459485 0.886869 0.140454 11.00000 0.08051 0.16147 = 0.11076 0.05263 -0.00524 0.01646 AFIX 23 H18A 2 0.384312 0.861658 0.146398 11.00000 -1.20000 H18B 2 0.456315 0.909725 0.093009 11.00000 -1.20000 AFIX 0 N1 4 0.545734 0.714572 0.301484 11.00000 0.06604 0.05430 = 0.06238 0.00218 0.01459 0.00727 AFIX 137 H1C 2 0.564240 0.661219 0.270852 11.00000 -1.20000 H1D 2 0.589439 0.700656 0.341810 11.00000 -1.20000 H1E 2 0.555630 0.793181 0.288331 11.00000 -1.20000 AFIX 0 N2 4 0.357715 0.314621 0.356490 11.00000 0.10146 0.08000 = 0.18176 0.00246 0.05010 -0.00744 C2 1 0.397364 0.398564 0.403725 11.00000 0.13967 0.08990 = 0.11590 0.02664 0.05301 -0.00478 AFIX 43 H2 2 0.409867 0.373032 0.449107 11.00000 -1.20000 AFIX 0 C3 1 0.402142 0.561958 0.323619 11.00000 0.05712 0.06391 = 0.08018 -0.00369 0.01964 0.00254 C7 1 0.421044 0.520378 0.389908 11.00000 0.09062 0.08065 = 0.08548 0.00012 0.03257 -0.00265 AFIX 43 H7 2 0.449858 0.574976 0.425242 11.00000 -1.20000 AFIX 0 C13 1 0.426238 0.695779 0.307216 11.00000 0.06226 0.07778 = 0.10973 0.02018 0.02978 0.01412 AFIX 23 H13A 2 0.378460 0.719372 0.264531 11.00000 -1.20000 H13B 2 0.407743 0.750265 0.342703 11.00000 -1.20000 AFIX 0 C15 1 0.359016 0.476972 0.274759 11.00000 0.06722 0.12481 = 0.07711 -0.00618 0.01086 -0.00099 AFIX 43 H15 2 0.344741 0.499975 0.228979 11.00000 -1.20000 AFIX 0 C17 1 0.336466 0.354677 0.294286 11.00000 0.06473 0.10355 = 0.14687 -0.03715 0.02037 -0.01382 AFIX 43 H17 2 0.304202 0.298723 0.260448 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_ZM_45_343K_2_0m_a.res in P2(1)/n REM wR2 = 0.2979, GooF = S = 1.043, Restrained GooF = 1.043 for all data REM R1 = 0.1255 for 1834 Fo > 4sig(Fo) and 0.2332 for all 4423 data REM 299 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.847, deepest hole -0.637, 1-sigma level 0.082 Q1 1 0.1559 0.9335 0.4496 11.00000 0.05 0.85 ; _shelx_res_checksum 57667 _shelx_hkl_file ; 1 0 0 0.82 1.84 -1 0 0 -0.32 0.87 -1 0 0 0.91 0.25 2 0 0 10.59 4.67 2 0 0 8.22 3.22 -2 0 0 12.43 1.70 -2 0 0 13.37 1.57 -2 0 0 12.20 3.34 -3 0 0 -0.73 0.83 3 0 0 0.16 4.36 -3 0 0 0.41 0.70 -3 0 0 -1.70 2.87 3 0 0 5.43 6.21 4 0 0 13.21 7.14 -4 0 0 1.44 1.24 -4 0 0 -1.61 3.44 4 0 0 4.95 8.64 -5 0 0 -1.94 4.00 5 0 0 8.26 11.00 6 0 0 10.35 17.78 -6 0 0 44.59 6.09 -6 0 0 41.76 6.68 6 0 0 26.63 19.50 -6 0 0 81.01 13.83 7 0 0 8.45 29.56 -7 0 0 -2.02 3.28 -7 0 0 3.65 5.53 -7 0 0 -4.00 5.71 -8 0 0 100.38 14.63 -8 0 0 78.40 18.89 8 0 0 98.23 12.85 -9 0 0 -5.89 8.03 -9 0 0 4.57 6.02 -9 0 0 -22.72 8.54 9 0 0 1.54 5.08 -9 0 0 0.89 8.20 10 0 0 32.47 8.33 -10 0 0 15.93 14.71 -10 0 0 11.46 8.41 -10 0 0 5.39 10.33 -10 0 0 26.91 11.49 -11 0 0 10.39 21.96 -11 0 0 6.61 10.19 11 0 0 2.51 1.75 -11 0 0 -11.72 8.51 -11 0 0 -0.85 7.98 11 0 0 12.36 7.02 12 0 0 8.66 6.24 -12 0 0 12.06 10.09 -12 0 0 3.88 7.37 -12 0 0 -9.85 7.78 -13 0 0 0.68 5.91 -13 0 0 6.53 7.98 13 0 0 7.88 5.26 -14 0 0 2.68 7.09 14 0 0 -5.07 2.54 -14 0 0 3.70 4.11 0 -1 0 0.06 0.32 0 -1 0 0.19 1.15 0 -1 0 0.01 0.22 0 1 0 0.10 0.29 0 1 0 -0.52 1.83 0 1 0 0.44 1.33 -1 -1 0 198.58 23.26 1 -1 0 190.24 21.61 1 -1 0 203.24 22.18 -1 -1 0 219.76 21.66 -1 -1 0 210.68 21.72 1 -1 0 196.58 21.64 1 1 0 219.50 23.31 -1 1 0 199.46 22.11 1 1 0 227.62 22.89 -1 1 0 190.76 22.23 1 1 0 230.59 21.72 -1 1 0 201.88 21.64 2 -1 0 4337.31 453.32 -2 -1 0 4089.58 454.78 -2 1 0 4193.90 453.14 -2 1 0 4229.51 452.59 2 1 0 4899.88 454.88 -3 -1 0 4446.31 463.80 3 -1 0 4577.53 465.26 3 -1 0 4321.59 464.86 -3 1 0 4037.69 463.69 -3 1 0 4580.73 463.63 3 1 0 4777.93 466.60 4 -1 0 203.72 22.98 -4 -1 0 174.53 21.74 -4 -1 0 164.80 18.32 4 -1 0 168.99 22.08 -4 -1 0 167.52 18.16 -4 -1 0 171.49 17.96 -4 1 0 173.09 20.42 -4 1 0 171.38 17.90 4 1 0 112.53 26.32 4 1 0 218.40 25.95 -4 1 0 161.76 18.03 -5 -1 0 271.30 33.85 -5 -1 0 280.78 29.83 -5 -1 0 266.15 30.00 5 -1 0 320.66 35.28 5 -1 0 280.68 35.50 -5 1 0 269.82 32.73 5 1 0 361.42 39.78 -5 1 0 290.60 29.56 5 1 0 264.47 38.17 -5 1 0 271.06 29.72 -6 -1 0 96.89 11.34 -6 -1 0 91.10 13.36 -6 -1 0 89.35 11.76 6 -1 0 115.16 21.70 -6 -1 0 107.35 17.00 6 -1 0 108.54 20.29 -6 1 0 99.16 11.18 -6 1 0 97.49 10.81 -6 1 0 92.09 15.48 6 1 0 101.55 27.14 -7 -1 0 109.87 13.25 -7 -1 0 105.34 14.89 -7 -1 0 105.12 18.72 7 -1 0 -6.22 30.38 -7 1 0 100.68 11.99 -7 1 0 126.43 13.91 7 1 0 -12.87 34.72 -7 1 0 81.11 16.91 8 -1 0 24.17 53.45 -8 -1 0 39.66 10.53 -8 -1 0 19.57 11.40 8 -1 0 22.77 6.30 -8 -1 0 10.17 11.88 -8 1 0 34.48 7.98 -8 1 0 20.63 10.57 8 1 0 31.18 7.46 9 -1 0 25.74 7.03 -9 -1 0 6.44 7.80 -9 -1 0 4.73 10.66 -9 -1 0 11.37 10.21 -9 -1 0 27.43 10.81 9 1 0 30.33 8.00 -9 1 0 17.36 12.22 -9 1 0 29.77 9.23 -10 -1 0 12.94 11.02 -10 -1 0 -4.04 9.60 10 -1 0 3.93 5.87 -10 -1 0 -7.50 10.13 -10 -1 0 -1.25 7.94 10 -1 0 2.68 2.37 -10 1 0 1.42 15.68 -10 1 0 6.13 9.06 10 1 0 11.90 7.36 -10 1 0 0.67 6.27 -11 -1 0 13.28 11.50 -11 -1 0 -29.31 19.22 -11 -1 0 0.50 9.56 11 -1 0 19.55 7.38 -11 -1 0 15.38 8.70 -11 1 0 7.45 10.30 11 1 0 11.95 7.28 -11 1 0 -2.30 7.28 -12 -1 0 -1.87 8.04 -12 -1 0 11.20 10.91 12 -1 0 16.83 6.85 -12 -1 0 5.00 7.66 12 1 0 3.97 6.14 -12 1 0 0.99 9.04 12 1 0 1.56 1.54 -12 1 0 -1.23 6.67 -13 -1 0 3.45 6.10 -13 -1 0 10.96 8.33 13 -1 0 5.50 4.89 -13 1 0 1.17 5.72 13 1 0 0.94 4.65 -13 1 0 2.36 7.37 14 -1 0 3.07 3.04 -14 -1 0 3.63 9.03 -14 -1 0 4.13 4.29 14 1 0 -0.28 2.80 -14 1 0 -1.71 3.56 -14 1 0 4.96 6.01 0 -2 0 64.30 8.41 0 -2 0 68.89 6.74 0 -2 0 62.89 6.86 0 2 0 68.37 9.87 0 2 0 59.32 6.79 0 2 0 55.07 8.70 1 -2 0 1080.85 109.70 -1 -2 0 992.52 111.30 1 -2 0 1038.83 110.07 -1 -2 0 1003.92 109.16 1 -2 0 1004.95 109.08 -1 2 0 930.52 110.04 -1 2 0 1041.74 109.05 1 2 0 1128.31 111.54 -1 2 0 1031.03 110.30 1 2 0 1093.70 110.79 1 2 0 1165.09 109.15 -2 -2 0 626.61 61.88 -2 -2 0 532.13 59.26 2 -2 0 551.35 59.09 -2 -2 0 560.24 59.13 2 -2 0 539.70 59.99 -2 -2 0 523.73 62.47 2 2 0 664.95 61.65 -2 2 0 521.92 60.11 -2 2 0 535.29 59.06 2 2 0 614.01 59.23 -2 2 0 515.29 60.08 2 2 0 652.63 63.01 -3 -2 0 3.15 4.87 -3 -2 0 7.21 1.84 3 -2 0 10.54 1.54 -3 -2 0 8.55 1.48 3 -2 0 11.97 4.95 -3 -2 0 9.96 11.90 3 -2 0 7.66 1.13 -3 2 0 10.54 3.43 -3 2 0 6.35 4.19 3 2 0 3.50 10.09 3 2 0 9.07 1.64 -3 2 0 8.06 1.30 -4 -2 0 19.69 2.65 -4 -2 0 16.47 7.16 -4 -2 0 16.12 2.88 4 -2 0 24.15 7.91 4 -2 0 19.54 7.64 -4 2 0 19.21 2.74 4 2 0 17.57 14.49 -4 2 0 18.43 4.94 -4 2 0 20.99 2.36 5 -2 0 11.77 10.65 -5 -2 0 6.67 6.81 -5 -2 0 11.62 2.16 -5 -2 0 10.11 2.82 -5 -2 0 12.13 2.89 -5 2 0 10.33 1.60 -5 2 0 9.67 5.06 -5 2 0 11.13 2.01 5 2 0 16.47 13.56 5 2 0 35.36 19.28 -6 -2 0 69.32 9.09 -6 -2 0 55.98 9.34 6 -2 0 71.29 14.80 -6 -2 0 76.45 12.23 -6 -2 0 45.70 8.44 6 -2 0 80.36 17.65 -6 -2 0 62.95 14.43 6 2 0 -0.20 24.05 6 2 0 119.55 33.26 -6 2 0 62.90 7.22 -6 2 0 70.93 7.67 -6 2 0 60.13 12.05 -7 -2 0 87.70 13.95 -7 -2 0 107.79 19.68 -7 -2 0 102.32 14.98 7 -2 0 102.95 12.42 7 -2 0 121.44 23.99 -7 2 0 78.14 15.83 -7 2 0 92.33 10.55 -8 -2 0 212.26 35.43 8 -2 0 294.89 29.10 -8 -2 0 227.28 30.52 -8 -2 0 235.55 32.57 -8 -2 0 225.78 29.56 8 2 0 300.99 29.75 -8 2 0 211.26 33.03 -8 2 0 284.67 28.83 -9 -2 0 -9.53 8.21 -9 -2 0 12.77 10.75 -9 -2 0 -5.77 9.56 9 -2 0 -8.87 4.34 -9 -2 0 2.83 7.68 -9 2 0 9.94 6.67 -9 2 0 -2.41 9.80 9 2 0 -0.02 6.11 -10 -2 0 15.09 11.57 -10 -2 0 29.04 12.35 -10 -2 0 30.96 9.62 -10 -2 0 -0.29 11.72 10 -2 0 14.19 6.76 10 2 0 28.55 8.28 -10 2 0 24.14 9.72 -10 2 0 3.04 17.31 11 -2 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-0.80 9.85 -1 3 -21 4.47 9.82 -2 -3 -21 1.20 1.63 -2 3 -21 2.55 9.44 -3 3 -21 0.48 8.61 7 -4 -21 1.09 1.27 7 -4 -21 4.10 2.12 -7 4 21 -2.48 4.43 6 -4 -21 2.53 1.43 6 -4 -21 2.41 2.34 -6 4 21 -1.00 5.17 5 -4 -21 1.78 1.55 5 -4 -21 4.56 2.64 -5 4 21 -0.89 6.23 4 -4 -21 5.58 2.78 4 -4 -21 1.42 1.52 -4 4 21 -6.91 6.35 -4 4 21 -11.27 3.21 3 -4 -21 2.59 2.71 -3 4 21 -3.72 3.49 -3 4 21 -6.25 7.51 2 -4 -21 8.37 3.15 -2 4 21 -3.96 3.48 -2 4 21 -17.77 8.79 1 -4 -21 0.16 2.54 1 4 -21 -5.05 8.28 -1 4 21 -9.24 3.06 0 -4 -21 4.62 2.32 0 4 -21 4.67 9.50 0 4 21 -7.57 2.83 0 4 21 -15.11 10.97 -1 4 -21 -12.24 8.82 -2 -4 -21 -2.24 1.30 -2 4 -21 3.77 8.46 5 -5 -21 -0.31 1.20 5 -5 -21 1.03 2.16 -5 5 21 -5.16 4.72 -5 5 21 -2.17 2.90 4 -5 -21 -0.08 1.34 4 -5 -21 1.94 2.23 -4 5 21 -9.60 6.25 -4 5 21 -7.93 2.88 3 -5 -21 -0.12 2.27 -3 5 21 -13.97 6.77 -3 5 21 -2.36 3.32 2 -5 -21 2.47 2.40 -2 5 21 -4.79 2.44 -2 5 21 -21.67 8.86 1 -5 -21 0.64 2.04 -1 5 21 -6.08 2.50 1 5 -21 -4.47 7.61 -1 5 21 -22.20 9.99 0 -5 -21 1.74 1.75 0 5 21 -8.88 10.06 0 5 -21 6.79 7.65 0 5 21 -4.84 2.88 -1 -5 -21 0.24 1.34 1 5 21 1.43 2.56 1 5 21 -12.46 4.39 -1 5 -21 -2.66 7.60 -7 0 22 -1.56 9.12 7 0 -22 0.07 1.66 6 0 -22 2.06 2.29 -6 0 22 -12.67 10.29 -5 0 22 -19.28 11.39 -4 0 22 -11.05 12.46 -3 0 22 -15.95 14.29 -2 0 22 -8.78 2.98 -2 0 22 17.56 13.80 0 0 22 12.79 2.85 -7 -1 22 -6.95 11.37 7 -1 -22 2.17 1.72 -7 1 22 -2.97 8.37 7 1 -22 -3.33 1.39 -6 -1 22 -13.06 12.53 6 -1 -22 -1.98 1.96 -6 1 22 1.72 9.35 -5 -1 22 -8.97 13.70 -5 1 22 -5.19 10.54 -4 -1 22 -14.65 12.81 -4 1 22 0.26 11.89 -3 -1 22 -2.72 13.97 -3 1 22 -18.57 12.64 -2 1 22 -30.07 13.14 -1 -1 22 1.23 2.52 -1 1 22 30.88 10.32 0 1 22 -1.10 2.76 -7 -2 22 5.44 12.78 7 -2 -22 1.73 1.66 -7 2 22 1.93 7.71 -6 -2 22 -14.01 13.63 6 -2 -22 3.30 2.30 -6 2 22 2.01 7.91 5 -2 -22 5.22 2.53 -5 -2 22 -1.70 14.13 -5 2 22 -0.43 9.39 4 -2 -22 3.34 2.45 -4 -2 22 3.69 12.95 -4 2 22 -7.77 9.89 -3 2 22 -8.44 3.17 -3 2 22 -10.90 11.41 -2 2 22 -7.09 3.00 -2 2 22 -24.87 10.96 -1 2 22 -13.85 11.54 -2 -2 -22 -1.18 1.31 6 -3 -22 1.06 1.87 -6 3 22 -1.44 6.97 5 -3 -22 5.27 2.46 -5 3 22 -7.92 7.46 4 -3 -22 3.43 2.38 -4 3 22 -4.67 9.06 -4 3 22 -7.04 3.15 3 -3 -22 2.81 2.61 -3 3 22 -8.02 3.06 -3 3 22 -19.65 10.08 2 -3 -22 4.74 2.59 -2 3 22 -14.36 11.32 -2 3 22 -4.99 3.28 1 -3 -22 11.34 2.82 -1 3 22 -2.08 3.19 -1 3 22 10.60 12.11 -1 -3 -22 1.16 1.78 -1 3 -22 -22.95 10.54 5 -4 -22 2.83 2.01 -5 4 22 -7.57 6.44 -5 4 22 -3.28 2.89 4 -4 -22 1.96 2.01 -4 4 22 -7.12 8.08 -4 4 22 -5.00 2.87 3 -4 -22 2.52 2.09 -3 4 22 -5.74 2.93 -3 4 22 -17.17 8.67 2 -4 -22 4.90 2.33 -2 4 22 -3.58 3.11 -2 4 22 -17.26 9.91 1 -4 -22 2.83 2.05 -1 4 22 0.17 10.45 -1 4 22 -5.97 2.52 0 -4 -22 -1.91 1.54 0 4 22 -3.73 2.56 -5 0 23 -6.93 11.90 -4 0 23 7.91 12.03 -3 0 23 49.66 11.68 -2 0 23 -6.35 2.61 -1 0 23 15.36 5.00 -5 -1 23 16.06 11.77 5 -1 -23 3.38 2.17 -5 1 23 1.62 11.76 -4 -1 23 47.51 12.29 -4 1 23 -7.33 12.32 -3 -1 23 -4.66 2.41 -3 1 23 -8.51 2.82 -3 1 23 -2.76 10.96 -2 -1 23 3.45 1.84 -2 1 23 -7.72 2.65 -1 1 23 -4.85 2.38 5 -2 -23 2.80 1.76 -5 2 23 -3.37 10.13 4 -2 -23 1.13 1.82 -4 -2 23 -2.91 2.12 -4 2 23 -7.94 2.54 -4 2 23 -11.74 9.96 3 -2 -23 4.20 2.27 -3 2 23 -8.11 2.55 -3 2 23 -10.59 10.52 -2 2 23 24.33 9.52 -1 2 23 -6.02 2.45 0 -2 -23 1.00 1.53 3 -3 -23 1.31 1.81 -3 3 23 0.86 2.90 -3 3 23 -2.08 9.46 2 -3 -23 1.86 1.76 -2 3 23 -2.63 2.52 -2 3 23 11.18 8.32 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 49119 _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 0.18001(11) 0.79505(11) 0.43656(6) 0.0799(4) Uani 1 1 d . . . . . F1 F 0.0723(4) 0.8048(4) 0.3870(3) 0.255(3) Uani 1 1 d . . . . . F2 F 0.1298(5) 0.6851(4) 0.4620(2) 0.326(3) Uani 1 1 d . . . . . F3 F 0.2090(3) 0.7097(5) 0.3842(3) 0.311(2) Uani 1 1 d . . . . . F4 F 0.2909(4) 0.7876(4) 0.4763(3) 0.356(3) Uani 1 1 d . . . . . F5 F 0.1579(5) 0.8775(5) 0.4889(2) 0.357(2) Uani 1 1 d . . . . . F6 F 0.2216(5) 0.9110(4) 0.4100(3) 0.290(3) Uani 1 1 d . . . . . O1 O 0.6870(2) 0.6921(3) 0.43477(13) 0.0792(10) Uani 1 1 d . . . . . O2 O 0.6082(3) 0.9342(3) 0.38749(15) 0.0931(11) Uani 1 1 d . . . . . O3 O 0.5936(2) 0.5379(3) 0.20288(14) 0.0784(10) Uani 1 1 d . . . . . O4 O 0.4953(3) 0.9642(3) 0.25499(16) 0.0966(11) Uani 1 1 d . . . . . O5 O 0.7146(2) 0.5124(3) 0.33405(14) 0.0766(9) Uani 1 1 d . . . . . O6 O 0.5362(2) 0.7856(3) 0.15790(14) 0.0867(11) Uani 1 1 d . . . . . C1 C 0.5238(5) 1.0678(4) 0.2996(3) 0.125(2) Uani 1 1 d . . . . . H1A H 0.469561 1.135194 0.287239 0.151 Uiso 1 1 calc R U . . . H1B H 0.598092 1.099176 0.295631 0.151 Uiso 1 1 calc R U . . . C4 C 0.7375(4) 0.4851(5) 0.4052(2) 0.1045(19) Uani 1 1 d . . . . . H4A H 0.795163 0.420448 0.414686 0.125 Uiso 1 1 calc R U . . . H4B H 0.669593 0.454675 0.419764 0.125 Uiso 1 1 calc R U . . . C5 C 0.5894(4) 0.5780(5) 0.1336(2) 0.0962(18) Uani 1 1 d . . . . . H5A H 0.571025 0.506991 0.103025 0.115 Uiso 1 1 calc R U . . . H5B H 0.662763 0.610100 0.128078 0.115 Uiso 1 1 calc R U . . . C6 C 0.6241(4) 0.8967(5) 0.4572(2) 0.1074(19) Uani 1 1 d . . . . . H6A H 0.556208 0.856523 0.466735 0.129 Uiso 1 1 calc R U . . . H6B H 0.640008 0.969688 0.486618 0.129 Uiso 1 1 calc R U . . . C8 C 0.4973(4) 0.9954(5) 0.1845(2) 0.1064(18) Uani 1 1 d . . . . . H8A H 0.573487 1.018696 0.179634 0.128 Uiso 1 1 calc R U . . . H8B H 0.448098 1.066686 0.170834 0.128 Uiso 1 1 calc R U . . . C9 C 0.6679(4) 0.4350(4) 0.2211(2) 0.0995(18) Uani 1 1 d . . . . . H9A H 0.742721 0.456276 0.212803 0.119 Uiso 1 1 calc R U . . . H9B H 0.641040 0.362410 0.193370 0.119 Uiso 1 1 calc R U . . . C10 C 0.5033(4) 0.6769(5) 0.1163(2) 0.103(2) Uani 1 1 d . . . . . H10A H 0.496049 0.699029 0.068498 0.124 Uiso 1 1 calc R U . . . H10B H 0.430709 0.646382 0.124148 0.124 Uiso 1 1 calc R U . . . C11 C 0.5234(5) 1.0276(5) 0.3719(3) 0.125(2) Uani 1 1 d . . . . . H11A H 0.539927 1.098517 0.402715 0.151 Uiso 1 1 calc R U . . . H11B H 0.450165 0.993588 0.376222 0.151 Uiso 1 1 calc R U . . . C12 C 0.7773(4) 0.6027(5) 0.4423(2) 0.107(2) Uani 1 1 d . . . . . H12A H 0.802815 0.584364 0.490294 0.128 Uiso 1 1 calc R U . . . H12B H 0.840406 0.637465 0.424194 0.128 Uiso 1 1 calc R U . . . C14 C 0.6735(4) 0.4047(4) 0.2940(2) 0.0926(18) Uani 1 1 d . . . . . H14A H 0.598952 0.382057 0.302276 0.111 Uiso 1 1 calc R U . . . H14B H 0.723673 0.333754 0.306580 0.111 Uiso 1 1 calc R U . . . C16 C 0.7208(4) 0.8072(5) 0.4702(2) 0.1043(19) Uani 1 1 d . . . . . H16A H 0.785586 0.842700 0.454117 0.125 Uiso 1 1 calc R U . . . H16B H 0.741940 0.791272 0.518769 0.125 Uiso 1 1 calc R U . . . C18 C 0.4595(4) 0.8869(5) 0.1405(3) 0.120(2) Uani 1 1 d . . . . . H18A H 0.384312 0.861658 0.146398 0.144 Uiso 1 1 calc R U . . . H18B H 0.456315 0.909725 0.093009 0.144 Uiso 1 1 calc R U . . . N1 N 0.5457(2) 0.7146(3) 0.30148(15) 0.0605(10) Uani 1 1 d . . . . . H1C H 0.564240 0.661219 0.270852 0.073 Uiso 1 1 calc R U . . . H1D H 0.589439 0.700656 0.341810 0.073 Uiso 1 1 calc R U . . . H1E H 0.555630 0.793181 0.288331 0.073 Uiso 1 1 calc R U . . . N2 N 0.3577(3) 0.3146(4) 0.3565(2) 0.1180(18) Uani 1 1 d . . . . . C2 C 0.3974(5) 0.3986(5) 0.4037(3) 0.111(2) Uani 1 1 d . . . . . H2 H 0.409867 0.373032 0.449107 0.134 Uiso 1 1 calc R U . . . C3 C 0.4021(3) 0.5620(4) 0.3236(2) 0.0662(13) Uani 1 1 d . . . . . C7 C 0.4210(4) 0.5204(4) 0.3899(2) 0.0835(16) Uani 1 1 d . . . . . H7 H 0.449858 0.574976 0.425242 0.100 Uiso 1 1 calc R U . . . C13 C 0.4262(3) 0.6958(4) 0.3072(2) 0.0815(15) Uani 1 1 d . . . . . H13A H 0.378460 0.719372 0.264531 0.098 Uiso 1 1 calc R U . . . H13B H 0.407743 0.750265 0.342703 0.098 Uiso 1 1 calc R U . . . C15 C 0.3590(4) 0.4770(5) 0.2748(2) 0.0900(17) Uani 1 1 d . . . . . H15 H 0.344741 0.499975 0.228979 0.108 Uiso 1 1 calc R U . . . C17 C 0.3365(4) 0.3547(5) 0.2943(3) 0.105(2) Uani 1 1 d . . . . . H17 H 0.304202 0.298723 0.260448 0.126 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 0.0917(8) 0.0694(6) 0.0770(7) -0.0078(6) 0.0106(6) -0.0011(7) F1 0.168(3) 0.159(4) 0.373(6) -0.027(4) -0.123(3) 0.022(3) F2 0.521(6) 0.245(3) 0.170(3) 0.097(2) -0.053(4) -0.258(3) F3 0.154(3) 0.352(4) 0.453(4) -0.300(3) 0.120(3) -0.044(3) F4 0.258(3) 0.148(4) 0.535(6) -0.062(4) -0.272(3) 0.036(3) F5 0.436(5) 0.413(5) 0.298(3) -0.275(2) 0.271(2) -0.203(4) F6 0.423(6) 0.206(3) 0.211(4) 0.052(3) -0.027(4) -0.202(3) O1 0.0745(17) 0.099(2) 0.0588(16) 0.0022(16) -0.0012(14) -0.0018(17) O2 0.121(2) 0.0716(18) 0.095(2) -0.0130(16) 0.0417(17) 0.0003(18) O3 0.0790(17) 0.0866(18) 0.0704(17) -0.0154(15) 0.0154(14) -0.0030(16) O4 0.106(2) 0.0752(18) 0.114(2) 0.0257(17) 0.0342(18) 0.0196(18) O5 0.0778(17) 0.0694(16) 0.0791(18) 0.0120(15) 0.0043(15) 0.0105(15) O6 0.0673(17) 0.117(2) 0.0693(17) 0.0177(17) -0.0040(15) -0.0074(18) C1 0.144(4) 0.062(3) 0.182(5) 0.009(3) 0.058(4) 0.033(3) C4 0.099(3) 0.112(3) 0.099(3) 0.034(3) 0.009(3) 0.035(3) C5 0.103(3) 0.121(4) 0.068(3) -0.019(3) 0.028(2) -0.025(3) C6 0.129(4) 0.109(3) 0.093(3) -0.035(3) 0.046(3) -0.050(3) C8 0.101(3) 0.109(3) 0.110(3) 0.052(3) 0.019(3) 0.031(3) C9 0.084(3) 0.082(3) 0.137(4) -0.040(3) 0.033(3) 0.000(3) C10 0.083(3) 0.161(5) 0.060(3) 0.003(3) -0.003(2) -0.031(3) C11 0.156(4) 0.086(3) 0.151(4) -0.022(3) 0.073(3) 0.023(3) C12 0.080(3) 0.152(5) 0.079(3) 0.014(3) -0.008(3) 0.014(3) C14 0.094(3) 0.048(2) 0.135(4) 0.001(3) 0.019(3) 0.009(2) C16 0.106(3) 0.134(4) 0.071(3) -0.017(3) 0.010(3) -0.043(3) C18 0.081(3) 0.161(5) 0.111(4) 0.053(3) -0.005(3) 0.016(3) N1 0.0660(18) 0.0543(17) 0.0624(18) 0.0022(15) 0.0146(15) 0.0073(16) N2 0.101(3) 0.080(3) 0.182(4) 0.002(3) 0.050(3) -0.007(2) C2 0.140(4) 0.090(3) 0.116(4) 0.027(3) 0.053(3) -0.005(3) C3 0.057(2) 0.064(2) 0.080(3) -0.004(2) 0.0196(19) 0.003(2) C7 0.091(3) 0.081(3) 0.085(3) 0.000(2) 0.033(2) -0.003(3) C13 0.062(2) 0.078(3) 0.110(3) 0.020(3) 0.030(2) 0.014(2) C15 0.067(3) 0.125(4) 0.077(3) -0.006(3) 0.011(2) -0.001(3) C17 0.065(3) 0.104(3) 0.147(4) -0.037(3) 0.020(3) -0.014(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 F2 P1 F1 85.4(3) . . ? F2 P1 F3 85.2(3) . . ? F2 P1 F6 175.3(3) . . ? F3 P1 F1 82.0(3) . . ? F4 P1 F1 172.2(4) . . ? F4 P1 F2 99.7(3) . . ? F4 P1 F3 92.5(3) . . ? F4 P1 F6 84.3(3) . . ? F5 P1 F1 100.9(3) . . ? F5 P1 F2 95.5(3) . . ? F5 P1 F3 177.1(3) . . ? F5 P1 F4 84.6(3) . . ? F5 P1 F6 82.4(3) . . ? F6 P1 F1 90.8(3) . . ? F6 P1 F3 97.1(3) . . ? C12 O1 C16 111.9(3) . . ? C11 O2 C6 112.1(4) . . ? C9 O3 C5 112.8(3) . . ? C1 O4 C8 112.7(4) . . ? C4 O5 C14 112.2(3) . . ? C18 O6 C10 111.7(3) . . ? O4 C1 H1A 109.7 . . ? O4 C1 H1B 109.7 . . ? O4 C1 C11 109.7(4) . . ? H1A C1 H1B 108.2 . . ? C11 C1 H1A 109.7 . . ? C11 C1 H1B 109.7 . . ? O5 C4 H4A 110.1 . . ? O5 C4 H4B 110.1 . . ? O5 C4 C12 108.1(4) . . ? H4A C4 H4B 108.4 . . ? C12 C4 H4A 110.1 . . ? C12 C4 H4B 110.1 . . ? O3 C5 H5A 109.7 . . ? O3 C5 H5B 109.7 . . ? O3 C5 C10 109.8(4) . . ? H5A C5 H5B 108.2 . . ? C10 C5 H5A 109.7 . . ? C10 C5 H5B 109.7 . . ? O2 C6 H6A 110.0 . . ? O2 C6 H6B 110.0 . . ? O2 C6 C16 108.2(4) . . ? H6A C6 H6B 108.4 . . ? C16 C6 H6A 110.0 . . ? C16 C6 H6B 110.0 . . ? O4 C8 H8A 109.7 . . ? O4 C8 H8B 109.7 . . ? O4 C8 C18 110.0(4) . . ? H8A C8 H8B 108.2 . . ? C18 C8 H8A 109.7 . . ? C18 C8 H8B 109.7 . . ? O3 C9 H9A 109.7 . . ? O3 C9 H9B 109.7 . . ? O3 C9 C14 109.6(4) . . ? H9A C9 H9B 108.2 . . ? C14 C9 H9A 109.7 . . ? C14 C9 H9B 109.7 . . ? O6 C10 C5 109.3(3) . . ? O6 C10 H10A 109.8 . . ? O6 C10 H10B 109.8 . . ? C5 C10 H10A 109.8 . . ? C5 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? O2 C11 C1 106.5(4) . . ? O2 C11 H11A 110.4 . . ? O2 C11 H11B 110.4 . . ? C1 C11 H11A 110.4 . . ? C1 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? O1 C12 C4 109.6(4) . . ? O1 C12 H12A 109.7 . . ? O1 C12 H12B 109.7 . . ? C4 C12 H12A 109.7 . . ? C4 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O5 C14 C9 108.9(4) . . ? O5 C14 H14A 109.9 . . ? O5 C14 H14B 109.9 . . ? C9 C14 H14A 109.9 . . ? C9 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? O1 C16 C6 108.4(4) . . ? O1 C16 H16A 110.0 . . ? O1 C16 H16B 110.0 . . ? C6 C16 H16A 110.0 . . ? C6 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O6 C18 C8 109.3(4) . . ? O6 C18 H18A 109.8 . . ? O6 C18 H18B 109.8 . . ? C8 C18 H18A 109.8 . . ? C8 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? H1C N1 H1D 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C13 N1 H1C 109.5 . . ? C13 N1 H1D 109.5 . . ? C13 N1 H1E 109.5 . . ? C17 N2 C2 116.4(5) . . ? N2 C2 H2 118.0 . . ? N2 C2 C7 124.0(5) . . ? C7 C2 H2 118.0 . . ? C7 C3 C13 120.7(4) . . ? C15 C3 C7 116.8(4) . . ? C15 C3 C13 122.5(4) . . ? C2 C7 C3 119.7(4) . . ? C2 C7 H7 120.2 . . ? C3 C7 H7 120.2 . . ? N1 C13 C3 112.0(3) . . ? N1 C13 H13A 109.2 . . ? N1 C13 H13B 109.2 . . ? C3 C13 H13A 109.2 . . ? C3 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C3 C15 H15 120.4 . . ? C3 C15 C17 119.1(4) . . ? C17 C15 H15 120.4 . . ? N2 C17 C15 124.0(5) . . ? N2 C17 H17 118.0 . . ? C15 C17 H17 118.0 . . ? 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 1.485(4) . ? P1 F2 1.447(5) . ? P1 F3 1.471(5) . ? P1 F4 1.426(4) . ? P1 F5 1.423(5) . ? P1 F6 1.464(5) . ? O1 C12 1.430(6) . ? O1 C16 1.434(6) . ? O2 C6 1.425(5) . ? O2 C11 1.416(6) . ? O3 C5 1.437(5) . ? O3 C9 1.417(5) . ? O4 C1 1.419(6) . ? O4 C8 1.447(6) . ? O5 C4 1.424(5) . ? O5 C14 1.432(5) . ? O6 C10 1.435(6) . ? O6 C18 1.419(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C11 1.503(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C12 1.488(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C10 1.472(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C16 1.488(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C18 1.472(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C14 1.477(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N1 C13 1.475(5) . ? N2 C2 1.322(7) . ? N2 C17 1.292(7) . ? C2 H2 0.9300 . ? C2 C7 1.364(7) . ? C3 C7 1.372(6) . ? C3 C13 1.499(6) . ? C3 C15 1.361(6) . ? C7 H7 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 H15 0.9300 . ? C15 C17 1.397(7) . ? C17 H17 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 O2 C6 C16 O1 -69.4(5) . . . . ? O3 C5 C10 O6 64.2(5) . . . . ? O3 C9 C14 O5 -60.1(5) . . . . ? O4 C1 C11 O2 62.3(5) . . . . ? O4 C8 C18 O6 -63.1(5) . . . . ? O5 C4 C12 O1 66.8(5) . . . . ? C1 O4 C8 C18 -176.1(4) . . . . ? C4 O5 C14 C9 -171.7(4) . . . . ? C5 O3 C9 C14 176.3(4) . . . . ? C6 O2 C11 C1 174.2(4) . . . . ? C8 O4 C1 C11 -178.2(4) . . . . ? C9 O3 C5 C10 174.9(4) . . . . ? C10 O6 C18 C8 -179.9(4) . . . . ? C11 O2 C6 C16 -175.2(4) . . . . ? C12 O1 C16 C6 177.5(4) . . . . ? C14 O5 C4 C12 -178.8(4) . . . . ? C16 O1 C12 C4 179.5(4) . . . . ? C18 O6 C10 C5 176.4(4) . . . . ? N2 C2 C7 C3 0.9(8) . . . . ? C2 N2 C17 C15 3.8(8) . . . . ? C3 C15 C17 N2 -2.5(7) . . . . ? C7 C3 C13 N1 85.1(5) . . . . ? C7 C3 C15 C17 0.2(6) . . . . ? C13 C3 C7 C2 179.3(4) . . . . ? C13 C3 C15 C17 -178.6(4) . . . . ? C15 C3 C7 C2 0.5(7) . . . . ? C15 C3 C13 N1 -96.2(5) . . . . ? C17 N2 C2 C7 -3.1(8) . . . . ?