#------------------------------------------------------------------------------ #$Date: 2025-02-03 01:06:21 +0200 (Mon, 03 Feb 2025) $ #$Revision: 297568 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573837.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_1573837 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 2024-04-29 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-08-24 deposited with the CCDC. 2025-01-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.751(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.137(3) _cell_length_b 10.6827(16) _cell_length_c 20.015(6) _cell_measurement_reflns_used 2113 _cell_measurement_temperature 423.00 _cell_measurement_theta_max 67.99 _cell_measurement_theta_min 3.96 _cell_volume 2549.5(11) _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 423.00 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.1162 _diffrn_reflns_av_unetI/netI 0.0748 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _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 27069 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 64.997 _diffrn_reflns_theta_max 64.997 _diffrn_reflns_theta_min 3.961 _diffrn_source_current 1.1 _diffrn_source_power 0.05500000000000001 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.675 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.3551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1512 before and 0.0715 after correction. The Ratio of minimum to maximum transmission is 0.4712. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.351 _exptl_crystal_description block _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.559 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 293 _refine_ls_number_reflns 4334 _refine_ls_number_restraints 66 _refine_ls_restrained_S_all 1.296 _refine_ls_R_factor_all 0.2970 _refine_ls_R_factor_gt 0.1446 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+4.1556P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3005 _refine_ls_wR_factor_ref 0.3477 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1365 _reflns_number_total 4334 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06631f2.cif _cod_data_source_block cu_zm_45_423k_0m_a _cod_database_code 1573837 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(F4) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O1) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O2) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C12) = Uanis(C14) 3.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C6(H6A,H6B) 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C8(H8), C9(H9) 3.c Idealised Me refined as rotating group: N1(H1A,H1B,H1C) ; _shelx_res_file ; TITL cu_ZM_45_423K_0m_a.res in P2(1)/n cu_zm_45_423k_0m_a.res created by SHELXL-2018/3 at 19:32:44 on 29-Apr-2024 REM Old TITL Integration of ZM_45_423K REM SHELXT solution in P2(1)/n: R1 0.286, Rweak 0.119, Alpha 0.100 REM 0.410 for 192 systematic absences, Orientation as input REM Formula found by SHELXT: C28 F N2 O6 P CELL 1.54184 12.137 10.6827 20.0148 90 100.751 90 ZERR 4 0.0033 0.0016 0.0055 0 0.015 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 EADP C12 C14 ISOR 0.01 0.02 F4 P1 F1 F2 F3 F5 F6 ISOR 0.01 0.02 O1 C14 ISOR 0.01 0.02 O2 C12 L.S. 100 PLAN 5 TEMP 149.85 CONF FREE F5 F6 FREE F6 F1 FREE F3 F4 FREE F3 F6 LIST 4 MORE -1 BOND $H fmap 2 acta SHEL 999 0.84 OMIT 0 130 REM REM REM WGHT 0.000233 4.155555 FVAR 0.37720 P1 6 0.820382 0.792166 0.561201 11.00000 0.14939 0.10008 = 0.11021 0.01648 0.01553 0.00733 F1 3 0.741207 0.784108 0.499718 11.00000 0.35983 0.26688 = 0.27834 -0.06747 -0.18014 0.05083 F2 3 0.741460 0.873500 0.584433 11.00000 0.41407 0.36531 = 0.28315 0.10790 0.22203 0.25747 F3 3 0.789718 0.703354 0.610341 11.00000 0.21286 0.32117 = 0.40976 0.22144 0.13243 0.04044 F4 3 0.924170 0.801536 0.612266 11.00000 0.25795 0.23510 = 0.33429 -0.00575 -0.10575 -0.03776 F5 3 0.854069 0.906544 0.533404 11.00000 0.32486 0.22183 = 0.35319 0.12952 0.05501 -0.05726 F6 3 0.875600 0.690307 0.535933 11.00000 0.38500 0.29357 = 0.23993 -0.07692 0.00805 0.18518 O1 5 0.311150 0.690642 0.567368 11.00000 0.12045 0.13519 = 0.09221 -0.01209 0.00289 0.00547 O2 5 0.395321 0.929923 0.612778 11.00000 0.15409 0.10755 = 0.14809 0.01667 0.03336 -0.00571 O3 5 0.286759 0.512964 0.668066 11.00000 0.11133 0.08943 = 0.14976 -0.01897 0.00565 -0.02695 O4 5 0.409619 0.542603 0.798455 11.00000 0.11495 0.15277 = 0.09836 0.02545 0.02857 0.00963 O5 5 0.507281 0.962388 0.744753 11.00000 0.15047 0.11696 = 0.18248 -0.05856 0.03549 -0.05627 O6 5 0.468485 0.786663 0.841459 11.00000 0.11686 0.17507 = 0.10824 -0.02435 -0.00805 0.01149 C3 1 0.542911 0.885403 0.857230 11.00000 0.11669 0.22564 = 0.16306 -0.07735 -0.00690 -0.03348 AFIX 23 H3A 2 0.617597 0.858029 0.853206 11.00000 -1.20000 H3B 2 0.544937 0.910848 0.903966 11.00000 -1.20000 AFIX 0 C5 1 0.260570 0.488679 0.598445 11.00000 0.16117 0.17073 = 0.13943 -0.06828 0.02557 -0.05878 AFIX 23 H5A 2 0.201613 0.426259 0.589511 11.00000 -1.20000 H5B 2 0.326067 0.455547 0.583195 11.00000 -1.20000 AFIX 0 C7 1 0.510433 0.993189 0.811857 11.00000 0.15049 0.15807 = 0.18510 -0.10225 0.00980 -0.04129 AFIX 23 H7A 2 0.437113 1.022799 0.817382 11.00000 -1.20000 H7B 2 0.563679 1.060673 0.824599 11.00000 -1.20000 AFIX 0 C10 1 0.500901 0.678458 0.881923 11.00000 0.13268 0.24065 = 0.09397 0.01387 -0.00185 0.04045 AFIX 23 H10A 2 0.510919 0.700190 0.929732 11.00000 -1.20000 H10B 2 0.571708 0.646953 0.873006 11.00000 -1.20000 AFIX 0 C11 1 0.334437 0.444456 0.779821 11.00000 0.13279 0.13869 = 0.21277 0.06507 0.00107 0.02039 AFIX 23 H11A 2 0.261063 0.469306 0.787708 11.00000 -1.20000 H11B 2 0.358606 0.372675 0.808509 11.00000 -1.20000 AFIX 0 C12 1 0.371374 0.892420 0.544247 11.00000 0.15800 0.13951 = 0.11469 0.02134 0.02493 0.02428 AFIX 23 H12A 2 0.437458 0.854320 0.532094 11.00000 -1.20000 H12B 2 0.351738 0.965153 0.515476 11.00000 -1.20000 AFIX 0 C13 1 0.480840 1.062132 0.696616 11.00000 0.18492 0.09802 = 0.29271 -0.01593 0.10357 -0.05000 AFIX 23 H13A 2 0.537007 1.127420 0.706817 11.00000 -1.20000 H13B 2 0.408753 1.097834 0.700347 11.00000 -1.20000 AFIX 0 C14 1 0.279840 0.803999 0.532888 11.00000 0.15800 0.13951 = 0.11469 0.02134 0.02493 0.02428 AFIX 23 H14A 2 0.215800 0.839403 0.548796 11.00000 -1.20000 H14B 2 0.257955 0.787785 0.484544 11.00000 -1.20000 AFIX 0 C15 1 0.413182 0.580105 0.865696 11.00000 0.13280 0.22550 = 0.09409 0.04433 0.03735 0.06780 AFIX 23 H15A 2 0.431232 0.509350 0.896145 11.00000 -1.20000 H15B 2 0.340877 0.613097 0.871050 11.00000 -1.20000 AFIX 0 C16 1 0.223578 0.603044 0.560930 11.00000 0.13275 0.22014 = 0.11439 -0.02436 -0.01872 -0.05031 AFIX 23 H16A 2 0.198095 0.583143 0.513265 11.00000 -1.20000 H16B 2 0.161019 0.638928 0.578202 11.00000 -1.20000 AFIX 0 C17 1 0.476983 1.017080 0.627098 11.00000 0.24829 0.10816 = 0.24179 0.03265 0.09225 -0.02351 AFIX 23 H17A 2 0.461568 1.086197 0.595296 11.00000 -1.20000 H17B 2 0.548698 0.980832 0.623001 11.00000 -1.20000 AFIX 0 C18 1 0.325022 0.407428 0.707771 11.00000 0.12751 0.07024 = 0.24028 0.00361 0.04061 -0.01170 AFIX 23 H18A 2 0.397405 0.380836 0.698996 11.00000 -1.20000 H18B 2 0.272482 0.338696 0.697008 11.00000 -1.20000 AFIX 0 N1 4 0.459631 0.712427 0.698080 11.00000 0.08900 0.07388 = 0.08174 -0.00613 0.01433 -0.01351 AFIX 137 H1A 2 0.414847 0.698129 0.658269 11.00000 -1.20000 H1B 2 0.452373 0.791688 0.710257 11.00000 -1.20000 H1C 2 0.440842 0.661810 0.729453 11.00000 -1.20000 AFIX 0 N2 4 0.641856 0.307693 0.646424 11.00000 0.15533 0.08464 = 0.36372 -0.02008 0.13725 0.00024 C1 1 0.598212 0.558762 0.675452 11.00000 0.07323 0.06368 = 0.13630 0.00640 0.02126 -0.00688 C2 1 0.605233 0.393826 0.602433 11.00000 0.21976 0.11998 = 0.22977 -0.06773 0.08255 0.00583 AFIX 43 H2 2 0.595364 0.368266 0.557289 11.00000 -1.20000 AFIX 0 C4 1 0.579612 0.511879 0.611106 11.00000 0.12667 0.13672 = 0.10013 -0.00890 0.03685 -0.00547 AFIX 43 H4 2 0.549561 0.561906 0.574157 11.00000 -1.20000 AFIX 0 C6 1 0.575544 0.688952 0.691962 11.00000 0.08497 0.11752 = 0.15304 -0.00980 0.03911 -0.02344 AFIX 23 H6A 2 0.624040 0.711213 0.734500 11.00000 -1.20000 H6B 2 0.594472 0.743021 0.656837 11.00000 -1.20000 AFIX 0 C8 1 0.639425 0.476516 0.724577 11.00000 0.10300 0.16075 = 0.13482 0.02797 0.02726 0.03731 AFIX 43 H8 2 0.651833 0.499807 0.770138 11.00000 -1.20000 AFIX 0 C9 1 0.662608 0.357970 0.705927 11.00000 0.08846 0.12075 = 0.28380 0.06833 0.03145 0.04014 AFIX 43 H9 2 0.698181 0.306561 0.740887 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_ZM_45_423K_0m_a.res in P2(1)/n REM wR2 = 0.3477, GooF = S = 1.173, Restrained GooF = 1.296 for all data REM R1 = 0.1446 for 1365 Fo > 4sig(Fo) and 0.2970 for all 4334 data REM 293 parameters refined using 66 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.559, deepest hole -0.376, 1-sigma level 0.063 Q1 1 0.6801 0.7847 0.5522 11.00000 0.05 0.56 Q2 1 0.8067 0.8070 0.4880 11.00000 0.05 0.52 Q3 1 0.7839 0.6515 0.5466 11.00000 0.05 0.51 Q4 1 0.8259 0.9249 0.5885 11.00000 0.05 0.50 Q5 1 0.9418 0.7861 0.5533 11.00000 0.05 0.44 ; _shelx_res_checksum 59765 _shelx_hkl_file ; -1 0 0 0.14 0.27 -1 0 0 -0.19 0.38 -1 0 0 -0.52 0.78 -2 0 0 6.95 1.66 -2 0 0 7.68 2.48 -2 0 0 8.13 1.55 2 0 0 5.62 1.64 -3 0 0 -1.77 0.84 -3 0 0 -1.04 1.29 -3 0 0 -0.08 3.17 3 0 0 -1.90 1.33 4 0 0 3.88 2.10 -4 0 0 0.39 3.20 -4 0 0 3.75 1.24 -4 0 0 0.08 1.60 -5 0 0 -0.04 2.47 5 0 0 -1.94 2.62 -5 0 0 -2.44 3.31 -5 0 0 2.04 1.11 -6 0 0 24.68 7.31 -6 0 0 25.77 5.37 -6 0 0 24.34 6.32 7 0 0 -8.63 7.07 -7 0 0 -0.32 5.68 -7 0 0 0.31 4.68 8 0 0 48.48 9.45 -8 0 0 48.94 12.08 -8 0 0 33.17 12.16 -8 0 0 87.10 20.26 -9 0 0 -16.72 9.66 -9 0 0 -2.89 6.93 -9 0 0 -0.11 6.14 -10 0 0 2.73 7.01 -10 0 0 2.60 8.10 -10 0 0 12.46 13.43 -11 0 0 -3.36 5.73 -11 0 0 -0.67 7.81 -11 0 0 -3.85 10.17 -12 0 0 0.04 7.07 -12 0 0 -5.14 9.33 -13 0 0 -7.04 5.62 -13 0 0 -10.76 7.08 -14 0 0 -3.28 3.67 -14 0 0 -1.51 5.46 0 -1 0 0.04 0.58 0 -1 0 -0.18 0.20 0 -1 0 -0.10 0.28 0 1 0 -0.05 0.31 0 1 0 0.13 1.05 0 1 0 0.12 0.60 -1 -1 0 192.97 35.92 1 -1 0 215.59 35.88 1 -1 0 212.81 35.87 -1 -1 0 199.99 35.96 -1 -1 0 191.42 36.06 -1 1 0 199.79 35.91 1 1 0 159.93 36.30 -1 1 0 175.41 35.88 1 1 0 194.47 35.97 -2 -1 0 4566.34 809.98 2 -1 0 4316.68 809.90 2 1 0 4423.64 809.99 -2 1 0 4285.41 809.89 3 -1 0 3827.87 703.50 -3 -1 0 3903.67 703.57 3 1 0 3775.66 703.59 -3 1 0 3770.75 703.48 -4 -1 0 153.64 26.79 4 -1 0 144.18 26.91 4 -1 0 138.81 26.73 -4 -1 0 134.84 27.28 -4 -1 0 151.78 26.96 4 1 0 139.21 27.05 -4 1 0 143.57 27.12 -4 1 0 144.17 26.85 5 -1 0 190.72 35.33 -5 -1 0 196.77 35.76 5 -1 0 180.21 35.05 -5 -1 0 179.81 35.35 -5 -1 0 199.05 35.08 -5 1 0 189.21 35.24 -5 1 0 186.16 35.53 5 1 0 188.22 35.53 -6 -1 0 56.68 12.89 -6 -1 0 55.11 12.46 -6 -1 0 62.64 11.48 -6 1 0 58.11 12.50 -6 1 0 62.75 12.33 -7 -1 0 50.38 12.23 -7 -1 0 58.00 13.10 -7 -1 0 55.33 10.74 -7 1 0 50.39 11.99 -7 1 0 60.51 12.89 -8 -1 0 14.97 12.76 8 -1 0 15.71 4.31 -8 -1 0 13.57 7.35 -8 -1 0 12.26 8.60 -8 1 0 16.21 7.02 8 1 0 22.17 4.83 -9 -1 0 5.06 8.03 -9 -1 0 -0.74 11.66 -9 -1 0 5.51 7.06 -9 1 0 -2.21 10.07 -9 1 0 10.84 7.78 -9 1 0 3.62 6.31 9 1 0 3.41 10.85 -10 -1 0 -2.72 6.62 -10 -1 0 -11.12 7.53 -10 -1 0 -14.24 10.18 -10 1 0 0.23 6.12 -10 1 0 3.54 11.99 -10 1 0 -0.36 7.17 -11 -1 0 -0.82 6.47 -11 -1 0 12.96 12.62 -11 -1 0 -2.46 7.38 -11 1 0 -1.71 7.38 -11 1 0 2.13 5.82 -11 1 0 14.94 12.35 -12 -1 0 9.50 11.49 -12 -1 0 -9.80 6.49 -12 1 0 8.71 10.54 -12 1 0 -7.43 6.60 -13 -1 0 0.60 5.85 -13 -1 0 -3.87 8.08 -13 1 0 -4.27 6.75 -13 1 0 -0.79 5.74 -14 -1 0 -8.07 5.17 -14 -1 0 -4.33 3.23 -14 1 0 -1.84 3.87 -14 1 0 -5.88 4.33 0 -2 0 47.81 8.98 0 -2 0 50.51 8.94 0 -2 0 45.91 9.13 0 2 0 45.67 9.76 0 2 0 48.81 9.04 -1 -2 0 995.36 181.16 -1 -2 0 966.22 181.00 -1 2 0 1011.32 180.90 1 2 0 970.00 181.05 -1 2 0 967.76 180.90 -2 -2 0 505.22 93.95 -2 -2 0 506.59 94.19 -2 -2 0 506.64 93.87 2 2 0 518.58 94.02 -2 2 0 525.80 93.93 -2 2 0 491.66 93.80 3 -2 0 5.40 1.50 3 -2 0 7.34 1.29 -3 -2 0 4.51 1.97 -3 -2 0 4.35 1.53 -3 -2 0 5.99 3.74 -3 2 0 4.49 1.60 3 2 0 3.27 2.16 -3 2 0 6.29 2.68 4 -2 0 21.95 4.26 -4 -2 0 15.93 4.37 -4 -2 0 19.88 4.02 4 -2 0 16.05 3.68 -4 -2 0 22.38 5.90 -4 2 0 20.44 4.08 -4 2 0 23.07 5.07 4 2 0 18.27 4.95 -5 -2 0 19.08 5.13 -5 -2 0 17.89 4.10 -5 -2 0 15.53 6.16 5 -2 0 18.28 4.56 5 -2 0 17.90 3.84 -5 2 0 21.57 4.62 -5 2 0 24.51 5.68 5 2 0 21.14 5.90 -6 -2 0 50.05 9.82 -6 -2 0 57.90 12.21 -6 -2 0 43.14 10.87 -6 2 0 45.18 11.02 -6 2 0 60.23 10.87 -7 -2 0 61.17 13.46 -7 -2 0 54.44 10.79 -7 -2 0 66.74 13.55 -7 2 0 43.94 12.01 -7 2 0 56.95 12.38 -8 -2 0 95.55 20.67 -8 -2 0 57.72 23.28 8 -2 0 96.06 16.75 -8 -2 0 80.10 18.75 -8 2 0 88.67 18.44 8 2 0 41.54 20.94 -9 -2 0 -3.13 4.47 -9 -2 0 -4.09 11.27 -9 -2 0 -1.88 6.29 -9 -2 0 -0.49 8.10 -9 2 0 -0.47 5.57 9 2 0 1.59 10.53 -9 2 0 13.72 12.34 -9 2 0 -0.41 6.69 -10 -2 0 -2.09 4.73 -10 -2 0 -3.81 11.42 -10 -2 0 3.95 8.25 -10 -2 0 1.06 7.26 10 2 0 -8.08 7.53 -10 2 0 4.35 6.23 -10 2 0 -1.11 7.06 -10 2 0 17.57 12.88 -11 -2 0 -1.17 6.01 -11 -2 0 -6.01 4.22 -11 -2 0 -4.84 9.66 -11 -2 0 -2.27 7.16 -11 2 0 3.56 5.84 -11 2 0 1.92 7.13 -11 2 0 8.28 10.29 -12 -2 0 -3.49 10.12 -12 -2 0 0.17 6.98 -12 2 0 -9.72 7.56 -12 2 0 -0.30 6.41 -13 -2 0 -3.76 4.55 -13 -2 0 -6.09 7.97 -13 2 0 -3.17 5.42 -13 2 0 -2.00 6.53 14 -2 0 -2.05 5.29 -14 -2 0 0.69 3.31 -14 2 0 -4.03 3.43 -14 2 0 5.09 4.59 0 -3 0 -0.12 0.62 0 -3 0 1.26 0.85 0 3 0 -7.08 3.47 0 3 0 -0.75 1.15 -1 -3 0 680.84 116.80 1 -3 0 662.73 116.44 -1 -3 0 643.57 116.56 1 3 0 664.29 116.68 -1 3 0 580.84 116.81 -1 3 0 650.51 116.48 1 3 0 523.55 117.26 -2 -3 0 66.94 11.65 -2 -3 0 66.11 11.88 -2 -3 0 63.71 12.32 2 3 0 61.20 12.09 -2 3 0 57.32 11.49 -2 3 0 64.45 12.02 2 3 0 55.10 14.05 -2 3 0 61.42 11.50 -3 -3 0 266.74 50.93 -3 -3 0 271.96 50.40 -3 -3 0 275.22 50.57 -3 3 0 285.23 50.58 -3 3 0 263.95 50.26 -3 3 0 273.90 50.23 3 3 0 269.78 50.76 -4 -3 0 11.91 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1.94 2.66 0 2 22 4.51 5.14 1 -2 22 4.01 6.63 1 -2 22 -1.10 2.55 1 -2 22 -2.36 1.91 1 2 22 8.76 10.21 -1 2 -22 -3.29 2.36 1 2 22 -0.06 4.50 1 2 22 -4.70 4.20 2 -2 22 -2.12 1.69 2 -2 22 -2.43 2.13 2 -2 22 -3.13 5.39 2 2 22 -7.78 7.32 -2 2 -22 -1.62 2.41 3 -2 22 -1.57 1.51 3 -2 22 3.00 2.00 -3 2 -22 3.29 3.01 3 2 22 -3.42 6.10 8 -3 -22 -3.34 2.85 -8 3 22 -3.19 3.38 -7 -3 22 0.88 1.82 -7 3 22 -2.95 4.58 -6 -3 22 1.27 1.92 -6 -3 22 0.66 2.14 -6 3 22 -1.34 2.55 -6 3 22 -2.37 5.25 -5 -3 22 1.22 2.13 -5 -3 22 -2.11 2.27 -5 3 22 -0.06 2.70 -5 3 22 -0.60 5.62 -4 -3 22 2.58 2.32 -4 -3 22 -2.01 2.28 -4 3 22 0.28 5.76 -4 3 22 1.98 2.69 -3 -3 22 0.30 2.15 -3 -3 22 -1.17 2.53 -3 3 22 -2.12 2.47 -3 3 22 -2.19 5.53 -2 -3 22 5.00 2.98 -2 -3 22 0.38 2.20 2 -3 -22 -5.31 3.92 -2 3 22 -3.34 4.35 2 3 -22 0.34 2.20 -2 3 22 4.71 5.79 -1 -3 22 4.63 2.99 -1 -3 22 0.51 2.33 1 -3 -22 6.24 3.83 1 3 -22 -1.98 2.52 -1 3 22 -1.35 5.35 0 -3 22 1.15 2.70 0 -3 22 -1.34 1.91 0 3 22 5.33 5.25 0 3 -22 4.72 3.26 1 -3 22 -0.30 1.98 1 -3 22 2.54 2.57 -1 3 -22 0.93 2.93 1 3 22 -1.15 8.72 1 3 22 3.49 4.24 2 -3 22 -2.00 1.56 2 -3 22 -1.00 2.00 -2 3 -22 2.29 2.65 2 3 22 -0.42 7.97 3 -3 22 -2.74 1.20 3 3 22 0.68 6.49 -3 3 -22 -2.42 1.80 7 -4 -22 -3.90 3.34 -7 4 22 -2.93 3.82 -6 -4 22 0.55 1.35 -6 -4 22 1.46 1.91 -6 4 22 -2.22 4.57 -5 -4 22 -0.55 2.05 -5 -4 22 2.37 1.78 -5 4 22 -2.56 5.25 -4 -4 22 0.05 1.70 -4 -4 22 0.61 2.25 -4 4 22 2.85 5.53 -3 -4 22 -0.59 1.87 -3 -4 22 1.52 2.34 3 -4 -22 -6.10 3.80 -3 4 22 -5.68 5.08 3 4 -22 1.92 2.17 2 -4 -22 -0.96 3.50 -2 -4 22 -1.35 2.29 -2 -4 22 -0.43 1.79 2 4 -22 -2.71 2.29 -2 4 22 -6.25 5.09 -1 -4 22 -1.11 1.70 1 -4 -22 6.05 3.39 -1 -4 22 -4.12 1.89 -1 4 22 1.50 5.10 1 4 -22 -2.50 2.27 0 -4 22 1.92 1.92 0 -4 22 1.85 2.36 0 4 22 3.05 4.75 0 4 -22 -2.12 2.55 0 4 22 -4.75 7.40 1 -4 22 0.04 1.59 1 -4 22 -1.01 1.88 -1 4 -22 -1.96 2.10 1 4 22 -0.02 7.44 1 4 22 2.10 4.29 2 -4 22 -0.80 1.69 2 -4 22 -1.11 1.21 2 4 22 12.02 7.10 -2 4 -22 -0.83 2.22 6 -5 -22 -1.76 3.05 -6 -5 22 -0.88 1.06 -6 5 22 -1.88 3.65 -5 -5 22 -0.07 1.31 5 -5 -22 -4.83 3.35 -5 5 22 -4.06 3.94 4 -5 -22 -5.65 3.47 -4 -5 22 -0.39 1.91 -4 -5 22 -0.52 1.44 -4 5 22 -0.78 4.84 -4 5 22 -0.96 6.42 -3 -5 22 -0.23 1.61 -3 -5 22 -4.32 1.80 3 -5 -22 -1.26 3.45 -3 5 22 2.26 5.41 -3 5 22 9.10 7.95 3 5 -22 1.84 2.21 -2 -5 22 1.22 1.85 -2 -5 22 -0.11 1.56 2 -5 -22 -3.36 2.53 -2 5 22 0.07 4.90 -2 5 22 -4.07 6.89 2 5 -22 -2.18 1.78 1 -5 -22 2.18 3.74 -1 -5 22 -1.11 1.61 -1 -5 22 -0.42 1.54 1 5 -22 -0.79 2.40 -1 5 22 2.21 7.46 -1 5 22 3.34 4.73 0 -5 22 -0.07 1.38 0 -5 22 0.48 1.54 0 5 22 0.26 4.13 0 5 -22 -3.77 1.64 0 5 22 2.96 6.99 1 -5 22 -0.81 1.02 1 5 22 1.07 3.58 1 5 22 3.52 6.52 -1 5 -22 1.11 2.04 -3 -6 22 0.91 1.07 3 -6 -22 -0.44 2.86 -2 -6 22 0.33 1.08 8 0 -23 -2.83 2.98 -7 0 23 1.55 1.88 -7 0 23 1.29 3.03 -6 0 23 2.70 2.29 -6 0 23 -1.40 3.40 -5 0 23 -0.21 3.66 -5 0 23 -0.11 2.19 -4 0 23 0.22 2.49 -4 0 23 2.04 3.92 -3 0 23 -0.28 2.52 -3 0 23 5.11 3.89 -2 0 23 -0.71 2.57 -2 0 23 -8.62 7.96 2 0 -23 0.45 2.84 -1 0 23 -1.03 2.41 -1 0 23 1.69 2.58 0 0 23 -2.54 2.02 0 0 23 1.59 2.29 1 0 23 -2.89 1.84 1 0 23 4.47 2.28 1 0 23 3.56 6.97 2 0 23 1.70 4.72 2 0 23 1.63 1.88 8 -1 -23 -4.24 2.94 8 1 -23 -3.98 3.09 -7 -1 23 1.02 1.91 -7 1 23 -2.06 3.22 -7 1 23 -1.18 1.77 -6 -1 23 5.35 4.96 -6 -1 23 -2.81 1.70 -6 1 23 -0.63 3.87 -6 1 23 -1.69 1.82 -5 -1 23 -0.65 2.22 -5 -1 23 3.25 4.42 -5 1 23 1.71 2.36 -5 1 23 -2.55 3.92 -4 -1 23 -1.60 2.25 -4 1 23 2.09 2.52 -4 1 23 -5.08 4.07 -3 -1 23 -0.22 2.59 -3 -1 23 4.12 2.58 -3 1 23 -2.11 4.11 -3 1 23 0.84 2.47 2 -1 -23 -1.39 3.21 -2 -1 23 2.60 2.45 -2 -1 23 -0.77 2.22 -2 1 23 -1.01 2.39 -2 1 23 1.29 4.28 -1 -1 23 0.59 2.40 -1 -1 23 -0.78 2.13 -1 1 23 -1.77 2.08 -1 1 23 -2.15 3.68 0 -1 23 -2.53 2.01 0 -1 23 -2.23 1.81 0 1 23 5.51 2.41 1 -1 23 0.94 2.15 1 -1 23 -2.60 4.85 1 -1 23 0.16 1.79 1 1 23 -2.49 6.66 2 -1 23 2.00 3.06 2 -1 23 0.65 1.49 2 1 23 -2.68 5.19 -7 -2 23 0.02 1.52 -7 2 23 -1.60 3.47 -6 -2 23 1.59 2.07 -6 2 23 -0.21 2.04 -6 2 23 0.70 4.27 -5 -2 23 -0.19 2.08 -5 2 23 1.61 2.28 -5 2 23 -4.16 4.00 -4 -2 23 0.96 2.17 -4 -2 23 2.54 2.43 -4 2 23 1.11 4.49 -4 2 23 3.34 2.53 3 -2 -23 -4.75 3.52 -3 -2 23 1.17 2.31 -3 -2 23 -1.14 2.13 -3 2 23 -1.64 4.27 -3 2 23 -0.37 2.43 2 -2 -23 0.67 3.13 -2 -2 23 -3.30 2.21 -2 -2 23 0.85 1.95 -2 2 23 -4.61 2.25 -2 2 23 0.82 4.52 -1 -2 23 -1.65 1.77 -1 -2 23 2.39 2.44 -1 2 23 -2.48 3.87 0 -2 23 -2.24 2.21 0 -2 23 -1.32 1.76 0 2 23 -9.63 6.51 1 -2 23 0.75 2.15 1 -2 23 -0.48 1.54 1 2 23 0.38 6.97 2 -2 23 -1.90 1.17 2 -2 23 0.79 1.77 2 2 23 1.93 5.78 -6 -3 23 0.46 1.77 -6 3 23 -2.27 3.82 -5 -3 23 1.23 1.48 -5 -3 23 -0.85 1.85 -5 3 23 -3.29 4.02 -4 -3 23 1.35 1.68 -4 -3 23 -0.52 2.15 -4 3 23 -1.66 4.20 -3 -3 23 -1.38 1.66 -3 -3 23 1.21 2.24 -3 3 23 -0.15 4.51 -2 -3 23 -1.42 1.56 -2 -3 23 -0.02 2.03 2 -3 -23 0.15 2.96 -2 3 23 1.13 4.23 -1 -3 23 -0.61 1.70 -1 -3 23 -0.10 2.07 -1 3 23 2.76 3.95 0 -3 23 -0.89 1.78 0 -3 23 -1.30 1.43 0 3 23 0.63 3.75 0 3 23 -1.07 6.59 1 -3 23 -0.06 1.51 1 -3 23 -0.25 1.57 1 3 23 -2.08 5.37 -5 -4 23 0.57 1.24 5 -4 -23 -2.10 2.96 -5 4 23 -2.28 3.90 4 -4 -23 -2.93 3.05 -4 -4 23 1.28 1.41 -4 -4 23 -2.75 1.52 -4 4 23 -4.55 4.03 3 -4 -23 0.08 2.92 -3 -4 23 0.04 1.43 -3 -4 23 -1.91 1.79 -3 4 23 -1.27 4.19 2 -4 -23 2.68 2.53 -2 -4 23 0.26 2.07 -2 -4 23 -0.71 1.49 -2 4 23 -2.48 4.03 -2 4 23 0.99 7.38 -1 -4 23 0.70 1.82 -1 -4 23 -0.65 1.43 -1 4 23 13.31 8.88 -1 4 23 -1.27 3.78 0 -4 23 -1.21 1.13 0 -4 23 2.81 1.70 0 4 23 -2.06 3.47 0 4 23 -3.58 5.16 -5 0 24 -0.08 1.71 -4 0 24 -2.07 2.01 3 0 -24 -1.00 2.37 -3 0 24 -0.46 2.24 -2 0 24 -2.44 1.90 -1 0 24 1.43 2.26 0 0 24 -2.80 5.15 -6 -1 24 0.83 1.94 -6 1 24 -1.55 2.97 -5 -1 24 0.04 1.77 -5 1 24 -2.49 2.88 -4 -1 24 -1.68 1.91 -4 1 24 -0.97 2.95 -4 1 24 -2.97 1.77 3 -1 -24 -0.57 2.57 -3 -1 24 -1.40 1.87 -3 1 24 2.00 4.68 3 1 -24 1.07 2.19 -3 1 24 -1.24 1.81 2 -1 -24 12.07 3.09 -1 -1 24 0.16 1.83 -1 -1 24 -0.07 1.72 0 -1 24 0.46 1.80 0 -1 24 1.65 1.63 0 -1 24 3.29 4.94 0 1 24 -0.96 5.15 -5 -2 24 -2.31 1.75 -5 2 24 -0.64 3.11 -4 -2 24 1.92 1.88 4 -2 -24 -4.32 2.73 -4 2 24 0.04 3.30 -3 -2 24 0.90 1.77 3 -2 -24 -0.70 2.44 -3 2 24 -3.40 2.95 -2 -2 24 2.21 2.17 -2 -2 24 3.86 1.75 -2 2 24 0.95 4.64 -1 -2 24 1.50 4.27 -1 -2 24 1.02 1.61 -1 -2 24 0.56 1.47 -1 2 24 -5.23 6.60 0 -2 24 0.71 1.24 4 -3 -24 -0.54 2.35 3 -3 -24 0.42 2.24 -3 -3 24 0.65 1.16 -3 3 24 0.78 3.31 -2 -3 24 0.46 1.29 -2 3 24 -6.44 4.94 -2 3 24 -1.31 2.94 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 40421 _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 0.82038(15) 0.79217(15) 0.56120(7) 0.1210(6) Uani 1 1 d . U . . . F1 F 0.7412(5) 0.7841(5) 0.4997(3) 0.333(3) Uani 1 1 d . U . . . F2 F 0.7415(4) 0.8735(5) 0.5844(2) 0.334(2) Uani 1 1 d . U . . . F3 F 0.7897(4) 0.7034(5) 0.6103(3) 0.305(2) Uani 1 1 d . U . . . F4 F 0.9242(4) 0.8015(5) 0.6123(3) 0.297(3) Uani 1 1 d . U . . . F5 F 0.8541(5) 0.9065(5) 0.5334(3) 0.301(3) Uani 1 1 d . U . . . F6 F 0.8756(5) 0.6903(5) 0.5359(2) 0.313(3) Uani 1 1 d . U . . . O1 O 0.3112(3) 0.6906(3) 0.56737(15) 0.1181(13) Uani 1 1 d . U . . . O2 O 0.3953(3) 0.9299(3) 0.61278(18) 0.1359(14) Uani 1 1 d . U . . . O3 O 0.2868(3) 0.5130(3) 0.66807(17) 0.1192(13) Uani 1 1 d . . . . . O4 O 0.4096(3) 0.5426(3) 0.79846(15) 0.1209(13) Uani 1 1 d . . . . . O5 O 0.5073(3) 0.9624(3) 0.7448(2) 0.1494(16) Uani 1 1 d . . . . . O6 O 0.4685(3) 0.7867(4) 0.84146(16) 0.1371(15) Uani 1 1 d . . . . . C3 C 0.5429(5) 0.8854(6) 0.8572(3) 0.173(3) Uani 1 1 d . . . . . H3A H 0.617597 0.858029 0.853206 0.207 Uiso 1 1 calc R U . . . H3B H 0.544937 0.910848 0.903966 0.207 Uiso 1 1 calc R U . . . C5 C 0.2606(5) 0.4887(6) 0.5984(3) 0.157(3) Uani 1 1 d . . . . . H5A H 0.201613 0.426259 0.589511 0.189 Uiso 1 1 calc R U . . . H5B H 0.326067 0.455547 0.583195 0.189 Uiso 1 1 calc R U . . . C7 C 0.5104(5) 0.9932(6) 0.8119(3) 0.167(3) Uani 1 1 d . . . . . H7A H 0.437113 1.022799 0.817382 0.201 Uiso 1 1 calc R U . . . H7B H 0.563679 1.060673 0.824599 0.201 Uiso 1 1 calc R U . . . C10 C 0.5009(5) 0.6785(6) 0.8819(3) 0.159(3) Uani 1 1 d . . . . . H10A H 0.510919 0.700190 0.929732 0.190 Uiso 1 1 calc R U . . . H10B H 0.571708 0.646953 0.873006 0.190 Uiso 1 1 calc R U . . . C11 C 0.3344(5) 0.4445(6) 0.7798(3) 0.165(3) Uani 1 1 d . . . . . H11A H 0.261063 0.469306 0.787708 0.199 Uiso 1 1 calc R U . . . H11B H 0.358606 0.372675 0.808509 0.199 Uiso 1 1 calc R U . . . C12 C 0.3714(5) 0.8924(5) 0.5442(2) 0.1375(16) Uani 1 1 d . U . . . H12A H 0.437458 0.854320 0.532094 0.165 Uiso 1 1 calc R U . . . H12B H 0.351738 0.965153 0.515476 0.165 Uiso 1 1 calc R U . . . C13 C 0.4808(5) 1.0621(6) 0.6966(3) 0.184(3) Uani 1 1 d . . . . . H13A H 0.537007 1.127420 0.706817 0.221 Uiso 1 1 calc R U . . . H13B H 0.408753 1.097834 0.700347 0.221 Uiso 1 1 calc R U . . . C14 C 0.2798(5) 0.8040(5) 0.5329(3) 0.1375(16) Uani 1 1 d . U . . . H14A H 0.215800 0.839403 0.548796 0.165 Uiso 1 1 calc R U . . . H14B H 0.257955 0.787785 0.484544 0.165 Uiso 1 1 calc R U . . . C15 C 0.4132(4) 0.5801(6) 0.8657(2) 0.149(3) Uani 1 1 d . . . . . H15A H 0.431232 0.509350 0.896145 0.178 Uiso 1 1 calc R U . . . H15B H 0.340877 0.613097 0.871050 0.178 Uiso 1 1 calc R U . . . C16 C 0.2236(5) 0.6030(6) 0.5609(3) 0.161(3) Uani 1 1 d . . . . . H16A H 0.198095 0.583143 0.513265 0.193 Uiso 1 1 calc R U . . . H16B H 0.161019 0.638928 0.578202 0.193 Uiso 1 1 calc R U . . . C17 C 0.4770(6) 1.0171(6) 0.6271(3) 0.193(3) Uani 1 1 d . . . . . H17A H 0.461568 1.086197 0.595296 0.232 Uiso 1 1 calc R U . . . H17B H 0.548698 0.980832 0.623001 0.232 Uiso 1 1 calc R U . . . C18 C 0.3250(5) 0.4074(5) 0.7078(3) 0.145(3) Uani 1 1 d . . . . . H18A H 0.397405 0.380836 0.698996 0.174 Uiso 1 1 calc R U . . . H18B H 0.272482 0.338696 0.697008 0.174 Uiso 1 1 calc R U . . . N1 N 0.4596(3) 0.7124(3) 0.69808(15) 0.0817(12) Uani 1 1 d . . . . . H1A H 0.414847 0.698129 0.658269 0.098 Uiso 1 1 calc R U . . . H1B H 0.452373 0.791688 0.710257 0.098 Uiso 1 1 calc R U . . . H1C H 0.440842 0.661810 0.729453 0.098 Uiso 1 1 calc R U . . . N2 N 0.6419(4) 0.3077(4) 0.6464(3) 0.190(2) Uani 1 1 d . . . . . C1 C 0.5982(4) 0.5588(4) 0.6755(2) 0.0908(16) Uani 1 1 d . . . . . C2 C 0.6052(6) 0.3938(6) 0.6024(3) 0.185(3) Uani 1 1 d . . . . . H2 H 0.595364 0.368266 0.557289 0.222 Uiso 1 1 calc R U . . . C4 C 0.5796(4) 0.5119(5) 0.6111(2) 0.119(2) Uani 1 1 d . . . . . H4 H 0.549561 0.561906 0.574157 0.143 Uiso 1 1 calc R U . . . C6 C 0.5755(4) 0.6890(5) 0.6920(3) 0.116(2) Uani 1 1 d . . . . . H6A H 0.624040 0.711213 0.734500 0.140 Uiso 1 1 calc R U . . . H6B H 0.594472 0.743021 0.656837 0.140 Uiso 1 1 calc R U . . . C8 C 0.6394(4) 0.4765(5) 0.7246(3) 0.132(2) Uani 1 1 d . . . . . H8 H 0.651833 0.499807 0.770138 0.159 Uiso 1 1 calc R U . . . C9 C 0.6626(4) 0.3580(5) 0.7059(4) 0.165(3) Uani 1 1 d . . . . . H9 H 0.698181 0.306561 0.740887 0.198 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 0.1494(13) 0.1001(11) 0.1102(9) 0.0165(9) 0.0155(9) 0.0073(11) F1 0.360(5) 0.267(5) 0.278(4) -0.067(4) -0.180(3) 0.051(4) F2 0.414(4) 0.365(5) 0.283(4) 0.108(3) 0.222(3) 0.257(3) F3 0.213(4) 0.321(4) 0.410(4) 0.221(3) 0.132(3) 0.040(3) F4 0.258(5) 0.235(5) 0.334(5) -0.006(4) -0.106(4) -0.038(4) F5 0.325(5) 0.222(4) 0.353(5) 0.130(3) 0.055(4) -0.057(4) F6 0.385(5) 0.294(4) 0.240(4) -0.077(3) 0.008(4) 0.185(4) O1 0.120(2) 0.135(3) 0.0922(19) -0.0121(19) 0.0029(18) 0.005(2) O2 0.154(3) 0.108(3) 0.148(3) 0.017(2) 0.033(2) -0.006(2) O3 0.111(2) 0.089(2) 0.150(3) -0.019(2) 0.006(2) -0.027(2) O4 0.115(2) 0.153(3) 0.098(2) 0.025(2) 0.0286(18) 0.010(2) O5 0.150(3) 0.117(3) 0.182(3) -0.059(2) 0.035(2) -0.056(2) O6 0.117(3) 0.175(3) 0.108(2) -0.024(2) -0.008(2) 0.011(3) C3 0.117(5) 0.226(7) 0.163(5) -0.077(5) -0.007(4) -0.033(5) C5 0.161(5) 0.171(5) 0.139(4) -0.068(4) 0.026(4) -0.059(4) C7 0.150(5) 0.158(5) 0.185(5) -0.102(4) 0.010(4) -0.041(4) C10 0.133(5) 0.241(7) 0.094(4) 0.014(4) -0.002(3) 0.040(5) C11 0.133(5) 0.139(5) 0.213(6) 0.065(4) 0.001(5) 0.020(4) C12 0.158(3) 0.140(3) 0.115(2) 0.021(2) 0.025(2) 0.024(2) C13 0.185(6) 0.098(4) 0.293(7) -0.016(5) 0.104(5) -0.050(4) C14 0.158(3) 0.140(3) 0.115(2) 0.021(2) 0.025(2) 0.024(2) C15 0.133(4) 0.225(6) 0.094(3) 0.044(4) 0.037(3) 0.068(4) C16 0.133(5) 0.220(7) 0.114(4) -0.024(4) -0.019(4) -0.050(5) C17 0.248(7) 0.108(5) 0.242(7) 0.033(5) 0.092(5) -0.024(5) C18 0.128(4) 0.070(4) 0.240(6) 0.004(4) 0.041(4) -0.012(3) N1 0.089(2) 0.074(2) 0.082(2) -0.0061(19) 0.0143(19) -0.014(2) N2 0.155(4) 0.085(3) 0.364(6) -0.020(4) 0.137(4) 0.000(3) C1 0.073(3) 0.064(3) 0.136(3) 0.006(3) 0.021(3) -0.007(2) C2 0.220(7) 0.120(5) 0.230(6) -0.068(4) 0.083(5) 0.006(5) C4 0.127(4) 0.137(5) 0.100(3) -0.009(3) 0.037(3) -0.005(4) C6 0.085(3) 0.118(4) 0.153(4) -0.010(3) 0.039(3) -0.023(3) C8 0.103(4) 0.161(5) 0.135(4) 0.028(4) 0.027(3) 0.037(4) C9 0.088(4) 0.121(5) 0.284(7) 0.068(5) 0.031(4) 0.040(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 F1 P1 F2 86.1(3) . . ? F1 P1 F3 109.2(3) . . ? F1 P1 F4 164.4(4) . . ? F1 P1 F5 84.9(3) . . ? F1 P1 F6 86.1(3) . . ? F2 P1 F3 84.6(3) . . ? F2 P1 F4 105.7(3) . . ? F2 P1 F5 82.3(3) . . ? F3 P1 F4 82.5(3) . . ? F5 P1 F3 160.1(3) . . ? F5 P1 F4 86.7(3) . . ? F6 P1 F2 165.6(4) . . ? F6 P1 F3 86.5(3) . . ? F6 P1 F4 84.2(3) . . ? F6 P1 F5 109.1(4) . . ? C14 O1 C16 113.4(4) . . ? C17 O2 C12 114.4(5) . . ? C5 O3 C18 113.9(4) . . ? C15 O4 C11 112.0(4) . . ? C7 O5 C13 116.1(4) . . ? C3 O6 C10 112.9(4) . . ? O6 C3 H3A 109.3 . . ? O6 C3 H3B 109.3 . . ? O6 C3 C7 111.5(4) . . ? H3A C3 H3B 108.0 . . ? C7 C3 H3A 109.3 . . ? C7 C3 H3B 109.3 . . ? O3 C5 H5A 109.6 . . ? O3 C5 H5B 109.6 . . ? O3 C5 C16 110.4(5) . . ? H5A C5 H5B 108.1 . . ? C16 C5 H5A 109.6 . . ? C16 C5 H5B 109.6 . . ? O5 C7 C3 111.7(5) . . ? O5 C7 H7A 109.3 . . ? O5 C7 H7B 109.3 . . ? C3 C7 H7A 109.3 . . ? C3 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? O6 C10 H10A 109.7 . . ? O6 C10 H10B 109.7 . . ? O6 C10 C15 109.8(4) . . ? H10A C10 H10B 108.2 . . ? C15 C10 H10A 109.7 . . ? C15 C10 H10B 109.7 . . ? O4 C11 H11A 109.0 . . ? O4 C11 H11B 109.0 . . ? O4 C11 C18 112.9(5) . . ? H11A C11 H11B 107.8 . . ? C18 C11 H11A 109.0 . . ? C18 C11 H11B 109.0 . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? O2 C12 C14 110.7(5) . . ? H12A C12 H12B 108.1 . . ? C14 C12 H12A 109.5 . . ? C14 C12 H12B 109.5 . . ? O5 C13 H13A 109.4 . . ? O5 C13 H13B 109.4 . . ? O5 C13 C17 111.0(5) . . ? H13A C13 H13B 108.0 . . ? C17 C13 H13A 109.4 . . ? C17 C13 H13B 109.4 . . ? O1 C14 C12 110.8(4) . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O4 C15 C10 107.8(4) . . ? O4 C15 H15A 110.2 . . ? O4 C15 H15B 110.2 . . ? C10 C15 H15A 110.2 . . ? C10 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? O1 C16 C5 110.8(5) . . ? O1 C16 H16A 109.5 . . ? O1 C16 H16B 109.5 . . ? C5 C16 H16A 109.5 . . ? C5 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? O2 C17 C13 108.7(6) . . ? O2 C17 H17A 110.0 . . ? O2 C17 H17B 110.0 . . ? C13 C17 H17A 110.0 . . ? C13 C17 H17B 110.0 . . ? H17A C17 H17B 108.3 . . ? O3 C18 C11 107.1(4) . . ? O3 C18 H18A 110.3 . . ? O3 C18 H18B 110.3 . . ? C11 C18 H18A 110.3 . . ? C11 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C6 N1 H1A 109.5 . . ? C6 N1 H1B 109.5 . . ? C6 N1 H1C 109.5 . . ? C9 N2 C2 108.4(5) . . ? C4 C1 C6 123.8(5) . . ? C8 C1 C4 115.2(5) . . ? C8 C1 C6 121.0(5) . . ? N2 C2 H2 114.7 . . ? N2 C2 C4 130.6(6) . . ? C4 C2 H2 114.7 . . ? C1 C4 H4 120.8 . . ? C2 C4 C1 118.4(5) . . ? C2 C4 H4 120.8 . . ? N1 C6 C1 114.0(4) . . ? N1 C6 H6A 108.8 . . ? N1 C6 H6B 108.8 . . ? C1 C6 H6A 108.8 . . ? C1 C6 H6B 108.8 . . ? H6A C6 H6B 107.6 . . ? C1 C8 H8 120.8 . . ? C1 C8 C9 118.3(5) . . ? C9 C8 H8 120.8 . . ? N2 C9 C8 128.7(6) . . ? N2 C9 H9 115.6 . . ? C8 C9 H9 115.6 . . ? 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 1.416(5) . ? P1 F2 1.433(5) . ? P1 F3 1.464(5) . ? P1 F4 1.470(5) . ? P1 F5 1.433(5) . ? P1 F6 1.420(5) . ? O1 C14 1.410(6) . ? O1 C16 1.404(6) . ? O2 C12 1.406(6) . ? O2 C17 1.351(7) . ? O3 C5 1.395(6) . ? O3 C18 1.407(6) . ? O4 C11 1.394(7) . ? O4 C15 1.397(5) . ? O5 C7 1.376(6) . ? O5 C13 1.432(7) . ? O6 C3 1.386(7) . ? O6 C10 1.424(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C7 1.474(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C16 1.460(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C15 1.488(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C18 1.479(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C14 1.444(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C17 1.465(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 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 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 C6 1.456(5) . ? N2 C2 1.294(8) . ? N2 C9 1.288(9) . ? C1 C4 1.361(6) . ? C1 C6 1.467(6) . ? C1 C8 1.344(6) . ? C2 H2 0.9300 . ? C2 C4 1.318(8) . ? C4 H4 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 H8 0.9300 . ? C8 C9 1.364(8) . ? C9 H9 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 C12 C14 O1 -66.7(6) . . . . ? O3 C5 C16 O1 65.2(6) . . . . ? O4 C11 C18 O3 -60.4(6) . . . . ? O5 C13 C17 O2 61.6(7) . . . . ? O6 C3 C7 O5 -59.6(7) . . . . ? O6 C10 C15 O4 65.3(6) . . . . ? C3 O6 C10 C15 175.9(5) . . . . ? C5 O3 C18 C11 -172.6(5) . . . . ? C7 O5 C13 C17 -178.4(5) . . . . ? C10 O6 C3 C7 176.7(5) . . . . ? C11 O4 C15 C10 176.2(5) . . . . ? C12 O2 C17 C13 171.0(5) . . . . ? C13 O5 C7 C3 -177.6(5) . . . . ? C14 O1 C16 C5 -179.2(5) . . . . ? C15 O4 C11 C18 177.1(4) . . . . ? C16 O1 C14 C12 177.0(4) . . . . ? C17 O2 C12 C14 -177.2(5) . . . . ? C18 O3 C5 C16 -179.0(5) . . . . ? N2 C2 C4 C1 4.0(11) . . . . ? C1 C8 C9 N2 -6.4(10) . . . . ? C2 N2 C9 C8 7.6(9) . . . . ? C4 C1 C6 N1 84.3(6) . . . . ? C4 C1 C8 C9 2.5(7) . . . . ? C6 C1 C4 C2 178.7(5) . . . . ? C6 C1 C8 C9 -177.7(5) . . . . ? C8 C1 C4 C2 -1.5(8) . . . . ? C8 C1 C6 N1 -95.5(5) . . . . ? C9 N2 C2 C4 -6.5(10) . . . . ?