#------------------------------------------------------------------------------ #$Date: 2020-08-06 16:30:52 +0300 (Thu, 06 Aug 2020) $ #$Revision: 254934 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557900.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_1557900 loop_ _publ_author_name 'Okude, Ryo' 'Mori, Genki' 'Yagi, Akiko' 'Itami, Kenichiro' _publ_section_title ; Programmable synthesis of multiply arylated cubanes through C--H metalation and arylation ; _journal_issue 29 _journal_name_full 'Chemical Science' _journal_page_first 7672 _journal_paper_doi 10.1039/D0SC01909G _journal_volume 11 _journal_year 2020 _chemical_formula_sum 'C30 H26 F3 N3 O' _chemical_formula_weight 501.54 _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_method SHELXL-2016/6 _audit_update_record ; 2020-03-30 deposited with the CCDC. 2020-04-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 108.846(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.0809(7) _cell_length_b 10.9917(4) _cell_length_c 17.1659(8) _cell_measurement_reflns_used 6785 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.8020 _cell_measurement_theta_min 1.6430 _cell_volume 2514.4(2) _computing_cell_refinement 'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution SHELXS _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'ROD, Synergy Custom system, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_unetI/netI 0.0508 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13618 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.634 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.325 _exptl_crystal_description block _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.340 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 375 _refine_ls_number_reflns 4418 _refine_ls_number_restraints 20 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0615 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+3.3237P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1401 _refine_ls_wR_factor_ref 0.1466 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3506 _reflns_number_total 4418 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01909g2.cif _cod_data_source_block 3a _cod_depositor_comments 'Adding full bibliography for 1557900--1557907.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557900 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL cn_4_cn_4_cf3_diaryl_etoac_hex_a.res CN_4_CN_4_CF3_diaryl_EtOAc_Hex.res created by SHELXL-2016/6 at 11:26:40 on 29-May-2019 REM Yadorkari-X generated CELL 0.71073 14.0809 10.9917 17.1659 90.0000 108.8460 90.0000 ZERR 4.0 0.0007 0.0004 0.0008 0.0000 0.0050 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H N O F UNIT 120 104 12 4 12 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 MERG 2 OMIT -10.000000 50.000000 DFIX 1.33 0.01 C23 F1 C23 F2 C23 F3 C30 F4 C30 F5 C30 F6 DFIX 2.15 0.01 F1 F2 F2 F3 F3 F1 F4 F5 F5 F6 F6 F4 DFIX 1.15 0.01 C23 N3 C30 N4 DFIX 2.69 0.01 C20 N3 C27 N4 DFIX 3.59 0.01 C19 N3 C21 N3 C26 N4 C28 N4 WGHT 0.031900 3.323700 FVAR 0.46507 0.84455 C1 1 0.675132 0.879924 0.837837 11.00000 0.03137 0.03217 = 0.02616 -0.00134 0.00571 -0.01132 C2 1 0.572357 0.941865 0.789141 11.00000 0.03614 0.02392 = 0.02779 -0.00131 0.00868 -0.00736 AFIX 13 H1 2 0.564193 1.026676 0.770548 11.00000 -1.20000 AFIX 0 C3 1 0.523696 0.884053 0.849978 11.00000 0.03580 0.02321 = 0.02570 -0.00422 0.01152 -0.00574 AFIX 13 H2 2 0.480546 0.927910 0.875266 11.00000 -1.20000 AFIX 0 C4 1 0.624635 0.823063 0.898619 11.00000 0.03278 0.02952 = 0.02167 -0.00265 0.00554 -0.01127 AFIX 13 H3 2 0.654138 0.822267 0.958729 11.00000 -1.20000 AFIX 0 C5 1 0.643919 0.765133 0.781126 11.00000 0.02492 0.03280 = 0.02309 -0.00087 0.00633 -0.00547 AFIX 13 H4 2 0.688136 0.721870 0.756599 11.00000 -1.20000 AFIX 0 C6 1 0.543677 0.827553 0.731292 11.00000 0.02650 0.02487 = 0.02335 -0.00114 0.00883 -0.00469 C7 1 0.490420 0.770496 0.793235 11.00000 0.02846 0.02372 = 0.02121 -0.00139 0.00856 -0.00225 C8 1 0.596118 0.707499 0.842982 11.00000 0.02446 0.02640 = 0.02270 -0.00113 0.00473 -0.00538 C9 1 0.772936 0.936907 0.859343 11.00000 0.04038 0.04300 = 0.02569 -0.00271 0.00707 -0.01420 N1 3 0.850579 0.980395 0.874394 11.00000 0.04932 0.06020 = 0.03925 -0.00294 0.00875 -0.02718 C10 1 0.383164 0.728537 0.772777 11.00000 0.02714 0.02744 = 0.02463 0.00053 0.00804 -0.00322 O1 4 0.328352 0.788128 0.801792 11.00000 0.02960 0.04434 = 0.05093 -0.02008 0.01697 -0.00483 N2 3 0.348393 0.632066 0.722464 11.00000 0.02305 0.02657 = 0.02651 -0.00358 0.00774 -0.00345 C11 1 0.410751 0.558167 0.685634 11.00000 0.02630 0.02298 = 0.02987 -0.00292 0.00973 -0.00561 AFIX 13 H5 2 0.478656 0.592393 0.703951 11.00000 -1.20000 AFIX 0 C12 1 0.372143 0.562597 0.591733 11.00000 0.03771 0.03180 = 0.03221 -0.00714 0.01099 -0.00751 AFIX 137 H6 2 0.309814 0.519132 0.571795 11.00000 -1.50000 H7 2 0.420503 0.525706 0.570487 11.00000 -1.50000 H8 2 0.361831 0.645740 0.573862 11.00000 -1.50000 AFIX 0 C13 1 0.417781 0.426541 0.716255 11.00000 0.03305 0.02460 = 0.04577 -0.00171 0.00814 -0.00216 AFIX 137 H9 2 0.441053 0.425751 0.775345 11.00000 -1.50000 H10 2 0.463938 0.382185 0.696283 11.00000 -1.50000 H11 2 0.352757 0.389182 0.696330 11.00000 -1.50000 AFIX 0 C14 1 0.240639 0.598340 0.700525 11.00000 0.02436 0.03496 = 0.03444 -0.01022 0.00856 -0.00717 AFIX 13 H12 2 0.230943 0.525508 0.665898 11.00000 -1.20000 AFIX 0 C15 1 0.173381 0.696880 0.648664 11.00000 0.02868 0.05217 = 0.04527 -0.00848 0.00212 0.00329 AFIX 137 H13 2 0.178445 0.769139 0.681172 11.00000 -1.50000 H14 2 0.105100 0.669044 0.630267 11.00000 -1.50000 H15 2 0.194190 0.714593 0.601852 11.00000 -1.50000 AFIX 0 C16 1 0.210844 0.564228 0.775248 11.00000 0.03623 0.05651 = 0.04958 -0.00805 0.01919 -0.01661 AFIX 137 H16 2 0.256774 0.504509 0.807267 11.00000 -1.50000 H17 2 0.144122 0.531298 0.757469 11.00000 -1.50000 H18 2 0.212816 0.635331 0.808212 11.00000 -1.50000 AFIX 0 C17 1 0.505538 0.832674 0.640225 11.00000 0.02363 0.02465 = 0.02533 0.00160 0.00815 -0.00708 C18 1 0.553125 0.767332 0.594187 11.00000 0.03034 0.03104 = 0.02743 0.00087 0.00676 0.00281 AFIX 43 H19 2 0.609184 0.720628 0.621163 11.00000 -1.20000 AFIX 0 C19 1 0.518974 0.770322 0.509440 11.00000 0.03774 0.03829 = 0.03050 -0.00566 0.01515 -0.00340 AFIX 43 H20 2 0.551055 0.725072 0.479529 11.00000 -1.20000 AFIX 0 C20 1 0.436249 0.841463 0.469043 11.00000 0.03627 0.03031 = 0.02306 0.00074 0.00897 -0.01162 C21 1 0.388358 0.909012 0.514003 11.00000 0.03158 0.03465 = 0.03393 0.00420 0.00279 0.00099 AFIX 43 H21 2 0.333425 0.957430 0.486982 11.00000 -1.20000 AFIX 0 C22 1 0.422743 0.903776 0.598717 11.00000 0.03240 0.03306 = 0.02882 -0.00278 0.00990 0.00261 AFIX 43 H22 2 0.390230 0.948334 0.628625 11.00000 -1.20000 AFIX 0 C23 1 0.400522 0.842394 0.379556 11.00000 0.04023 0.03834 = 0.03541 0.00402 0.00965 -0.01141 PART 1 N3 3 0.367393 0.838789 0.308126 21.00000 0.04530 0.05854 = 0.02411 0.00102 0.00647 -0.02100 PART 2 F1 5 0.491364 0.846790 0.355158 -21.00000 0.07918 0.06067 = 0.04128 0.01636 0.02739 0.03053 F2 5 0.358502 0.942980 0.346714 -21.00000 0.03770 0.09975 = 0.05253 0.02851 0.01907 0.00986 F3 5 0.359986 0.744525 0.342639 -21.00000 0.10969 0.09854 = 0.03198 -0.00174 -0.00334 -0.03052 PART 0 C24 1 0.614859 0.580916 0.875561 11.00000 0.02166 0.03000 = 0.02296 0.00087 0.00383 -0.00315 C25 1 0.647487 0.490239 0.833996 11.00000 0.02824 0.03341 = 0.02421 0.00007 0.00621 -0.00106 AFIX 43 H23 2 0.659217 0.508737 0.785028 11.00000 -1.20000 AFIX 0 C26 1 0.662860 0.372416 0.864411 11.00000 0.03249 0.03353 = 0.03024 -0.00347 0.00719 0.00663 AFIX 43 H24 2 0.683580 0.312079 0.835494 11.00000 -1.20000 AFIX 0 C27 1 0.647259 0.345217 0.937755 11.00000 0.03182 0.03075 = 0.03008 0.00358 0.00489 0.00226 C28 1 0.617806 0.434854 0.982150 11.00000 0.03579 0.03785 = 0.02662 0.00420 0.01139 -0.00009 AFIX 43 H25 2 0.609389 0.416491 1.032400 11.00000 -1.20000 AFIX 0 C29 1 0.601032 0.552333 0.950701 11.00000 0.03119 0.03408 = 0.02854 -0.00044 0.01151 -0.00275 AFIX 43 H26 2 0.580439 0.612510 0.979811 11.00000 -1.20000 AFIX 0 C30 1 0.663919 0.219197 0.972815 11.00000 0.05606 0.03704 = 0.04391 0.00981 0.01277 0.01121 PART 1 F4 5 0.673964 0.138692 0.920887 21.00000 0.20845 0.02469 = 0.04861 -0.00031 0.04126 0.01666 F5 5 0.748681 0.214128 1.038823 21.00000 0.05898 0.04257 = 0.05851 0.01553 -0.00675 0.01299 F6 5 0.592396 0.184386 1.002066 21.00000 0.07022 0.05014 = 0.09503 0.03525 0.02772 -0.00098 PART 2 N4 3 0.648905 0.110710 0.980755 -21.00000 0.11076 0.03284 = 0.08843 -0.00607 -0.01511 -0.00266 PART 0 HKLF 4 REM cn_4_cn_4_cf3_diaryl_etoac_hex_a.res REM R1 = 0.0615 for 3506 Fo > 4sig(Fo) and 0.0774 for all 4418 data REM 375 parameters refined using 20 restraints END WGHT 0.0319 3.3245 REM Highest difference peak 0.340, deepest hole -0.337, 1-sigma level 0.051 Q1 1 0.5198 0.8552 0.3512 11.00000 0.05 0.34 Q2 1 0.7674 0.1871 0.9811 11.00000 0.05 0.31 Q3 1 0.6033 0.1613 0.9358 11.00000 0.05 0.31 Q4 1 0.6645 0.2035 1.0480 11.00000 0.05 0.29 Q5 1 0.3862 0.7609 0.3496 11.00000 0.05 0.24 Q6 1 0.5032 0.7931 0.7506 11.00000 0.05 0.22 Q7 1 0.8051 1.0349 0.8792 11.00000 0.05 0.22 Q8 1 0.6448 0.0742 0.9686 11.00000 0.05 0.22 Q9 1 0.5348 0.7212 0.8156 11.00000 0.05 0.22 Q10 1 0.5725 0.3727 0.9455 11.00000 0.05 0.22 Q11 1 0.6747 0.8236 0.8110 11.00000 0.05 0.17 Q12 1 0.3744 0.8474 0.3866 11.00000 0.05 0.17 Q13 1 0.3528 0.7261 0.8291 11.00000 0.05 0.16 Q14 1 0.4852 0.8318 0.8136 11.00000 0.05 0.16 Q15 1 0.3825 0.9364 0.3629 11.00000 0.05 0.16 Q16 1 0.6252 0.7190 0.8100 11.00000 0.05 0.15 Q17 1 0.3185 0.7940 0.8723 11.00000 0.05 0.15 Q18 1 0.5593 0.8896 0.7579 11.00000 0.05 0.15 Q19 1 0.4400 0.8489 0.9169 11.00000 0.05 0.15 Q20 1 0.6411 0.2802 0.9473 11.00000 0.05 0.15 ; _shelx_res_checksum 27200 _shelx_hkl_file ; 0 0 -2 892.15 44.27 0 0 2 901.65 44.31 0 0 3 0.10 1.21 0 0 -3 1.54 1.07 0 0 -4 7.75 1.62 0 0 4 5.33 1.63 0 0 -5 15.10 2.18 0 0 5 14.97 2.35 0 0 -6 898.11 45.99 0 0 6 869.44 46.13 0 0 6 920.98 44.99 0 0 7 3.55 2.11 0 0 7 7.05 0.60 0 0 -7 2.68 1.66 0 0 7 7.86 1.45 0 0 8 187.07 9.19 0 0 8 181.30 10.43 0 0 -8 161.30 11.28 0 0 8 174.47 11.68 0 0 9 0.48 1.21 0 0 9 0.05 0.34 0 0 -9 -0.28 1.73 0 0 -10 121.58 9.57 0 0 10 135.42 8.68 0 0 10 148.13 7.18 0 0 10 132.10 7.60 0 0 11 9.72 2.17 0 0 11 11.93 0.87 0 0 11 6.57 1.15 0 0 -11 7.68 2.53 0 0 12 236.91 11.50 0 0 -12 212.31 14.59 0 0 12 236.01 13.63 0 0 12 213.62 12.01 0 0 13 3.49 2.04 0 0 13 3.14 1.02 0 0 -13 1.59 2.54 0 0 14 247.41 14.70 0 0 -14 234.39 15.82 0 0 14 239.37 12.72 0 0 -15 1.39 3.05 0 0 15 0.61 2.46 0 0 -16 207.15 14.80 0 0 16 207.26 13.66 0 0 17 0.72 2.93 0 0 -17 1.55 3.11 0 0 -18 -0.54 3.77 0 0 18 4.65 3.46 0 0 -19 -1.73 4.13 0 1 0 20.20 1.31 0 -1 0 29.47 1.37 0 1 1 42.11 2.37 0 1 -1 62.47 2.31 0 1 1 41.45 2.16 0 1 -1 29.80 2.07 0 -1 -1 45.97 2.18 0 -1 -2 194.83 10.42 0 -1 2 207.86 10.49 0 1 -2 198.70 10.00 0 -1 3 1657.58 80.62 0 1 3 1670.79 79.73 0 -1 -3 1592.03 80.53 0 1 -3 1597.20 79.82 0 -1 4 2285.66 119.23 0 -1 4 2559.34 118.21 0 1 4 2444.04 118.07 0 -1 -4 2275.83 119.14 0 1 4 2274.93 118.69 0 -1 5 12.84 2.49 0 -1 5 16.09 1.37 0 1 5 22.03 2.02 0 -1 -5 16.12 2.21 0 1 5 20.61 1.27 0 -1 6 625.04 28.86 0 -1 6 641.24 30.69 0 1 6 563.84 28.60 0 1 6 546.76 29.50 0 -1 6 578.55 29.18 0 -1 -6 547.81 30.30 0 1 7 454.60 26.07 0 1 7 513.71 25.05 0 -1 7 488.37 25.76 0 -1 7 551.75 25.37 0 -1 -7 451.01 26.82 0 -1 7 512.92 27.28 0 1 8 32.03 3.09 0 -1 -8 31.19 3.79 0 1 8 29.70 1.94 0 -1 8 36.48 2.32 0 -1 8 31.13 2.75 0 -1 8 31.11 4.16 0 1 9 41.11 2.01 0 1 9 26.41 2.96 0 -1 9 20.88 2.01 0 -1 -9 27.60 3.62 0 -1 9 20.34 2.51 0 1 10 112.25 8.19 0 -1 10 118.28 7.89 0 -1 10 119.22 7.14 0 -1 -10 113.33 9.00 0 1 10 149.42 6.89 0 -1 -11 33.45 4.26 0 -1 11 34.54 3.41 0 -1 11 38.28 2.72 0 1 11 37.37 3.83 0 1 11 35.71 2.26 0 1 12 0.66 0.59 0 1 12 1.97 1.90 0 -1 12 0.95 0.95 0 -1 -12 2.94 2.30 0 -1 12 1.62 1.62 0 1 13 5.08 1.07 0 1 13 5.83 0.86 0 -1 -13 5.19 2.74 0 1 13 7.29 2.44 0 -1 13 7.47 1.33 0 -1 13 6.22 2.28 0 1 14 65.49 4.44 0 -1 -14 63.06 7.04 0 1 14 67.67 6.35 0 -1 14 78.95 4.82 0 1 14 80.15 4.20 0 -1 14 78.76 6.26 0 -1 -15 24.96 4.69 0 1 15 28.28 4.30 0 -1 15 29.06 4.05 0 1 16 51.04 5.82 0 -1 -16 35.37 5.78 0 -1 16 46.59 5.25 0 1 17 87.72 7.76 0 -1 -17 67.15 8.09 0 -1 -18 68.11 8.17 0 1 18 80.42 7.76 0 1 19 11.91 4.51 0 -1 -19 3.46 4.05 0 2 0 1742.11 84.72 0 2 0 1730.72 84.79 0 2 -1 30.90 1.41 0 -2 -1 15.60 1.28 0 2 1 16.75 1.32 0 2 -2 160.79 7.94 0 2 -2 134.26 7.44 0 2 -2 137.02 7.62 0 2 2 164.82 8.01 0 -2 2 150.44 7.98 0 -2 -2 160.47 7.93 0 -2 2 152.64 7.48 0 -2 -3 37.69 3.13 0 2 -3 51.04 2.84 0 2 3 25.09 2.88 0 -2 3 53.56 3.53 0 -2 3 55.74 2.57 0 2 3 41.35 3.29 0 2 -3 49.86 3.34 0 -2 -4 669.65 35.40 0 -2 4 729.74 34.66 0 -2 4 678.16 35.52 0 -2 4 720.49 34.29 0 2 4 672.89 35.15 0 2 -4 718.42 35.49 0 2 4 727.60 34.52 0 2 -4 623.19 34.59 0 2 4 713.23 35.56 0 -2 5 296.06 14.73 0 -2 5 286.98 15.03 0 -2 5 299.39 16.39 0 2 5 299.40 15.83 0 2 -5 289.60 16.20 0 2 -5 271.08 15.13 0 2 5 312.30 16.47 0 -2 5 315.78 15.24 0 2 5 332.05 15.07 0 -2 -5 292.77 16.21 0 2 -6 25.41 2.77 0 -2 6 19.87 1.63 0 -2 6 25.65 1.15 0 2 6 12.83 2.49 0 2 6 12.14 1.96 0 -2 6 21.06 1.70 0 2 6 9.41 1.24 0 -2 -6 12.04 2.32 0 -2 6 20.87 2.99 0 -2 7 20.27 1.70 0 2 7 19.96 3.11 0 -2 7 13.91 1.65 0 2 -7 13.03 2.51 0 2 7 18.77 1.42 0 -2 -7 20.90 2.77 0 -2 7 17.95 3.11 0 2 7 13.01 2.14 0 -2 8 2.81 0.90 0 2 8 2.50 0.68 0 2 -8 1.97 1.61 0 -2 8 1.92 0.99 0 2 8 2.71 1.46 0 -2 -8 0.99 1.82 0 -2 9 218.11 11.42 0 2 9 226.51 11.13 0 2 -9 203.83 13.16 0 -2 9 210.62 11.74 0 -2 -9 183.97 12.96 0 2 9 210.97 12.59 0 2 10 13.86 1.37 0 -2 10 20.73 1.83 0 2 -10 16.62 3.16 0 2 10 11.57 2.38 0 -2 -10 15.20 2.94 0 -2 10 19.21 2.21 0 2 11 7.23 0.94 0 -2 11 6.12 1.24 0 2 -11 8.00 2.52 0 -2 11 5.79 1.65 0 2 11 1.96 1.89 0 -2 -11 2.01 2.28 0 2 -12 2.56 2.53 0 -2 -12 2.57 2.34 0 -2 12 3.09 1.17 0 2 12 1.60 1.88 0 -2 12 2.24 1.65 0 2 12 4.99 0.95 0 2 13 1.37 0.76 0 -2 13 -0.21 1.85 0 -2 -13 1.98 2.62 0 2 -13 1.19 2.31 0 -2 13 1.45 1.12 0 2 13 1.17 2.22 0 2 14 7.89 1.12 0 -2 14 4.01 2.26 0 -2 -14 6.01 3.08 0 -2 14 3.30 1.30 0 2 -14 5.14 3.19 0 2 14 7.43 3.20 0 -2 -15 46.88 6.39 0 -2 15 71.83 5.95 0 2 -15 53.43 6.65 0 2 15 73.84 6.71 0 2 -16 28.27 5.45 0 -2 -16 31.24 5.37 0 2 16 36.97 5.15 0 2 17 0.41 3.41 0 2 -17 -0.51 3.35 0 -2 -17 2.54 3.51 0 2 -18 -1.63 3.97 0 -2 -18 2.72 3.68 0 2 18 -0.88 3.46 0 -2 -19 -3.46 4.60 0 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0.62 2.28 2 7 -11 -0.28 1.64 -2 7 11 1.53 0.89 2 7 -11 1.93 1.43 2 7 -10 91.28 5.44 2 7 -10 78.27 5.52 -2 7 10 76.23 4.79 2 7 -10 83.53 6.72 2 -7 -10 69.56 6.41 -2 7 10 77.74 7.39 2 7 -9 98.17 6.84 -2 7 9 97.84 8.45 2 -7 -9 115.00 6.51 -2 7 9 106.59 6.21 2 7 -9 103.53 7.74 2 -7 -9 102.64 7.71 2 7 -9 114.71 6.55 2 7 -8 14.04 2.68 2 -7 -8 10.28 2.41 -2 7 8 16.96 3.49 2 7 -8 15.02 1.78 2 -7 -8 15.18 1.74 -2 7 8 12.22 1.59 2 7 -8 14.24 1.59 2 7 -8 17.03 2.22 2 7 -7 34.65 2.59 -2 7 7 26.00 2.47 2 7 -7 33.35 2.48 -2 7 7 35.96 4.36 2 -7 -7 30.85 2.44 2 7 -7 38.17 3.58 2 7 -7 36.45 3.19 2 -7 -7 30.99 3.43 2 7 -6 104.23 6.51 2 -7 -6 119.21 7.01 2 7 -6 109.65 6.31 2 -7 -6 122.66 6.40 2 7 -6 107.39 7.09 -2 7 6 127.40 8.64 -2 7 6 121.25 6.75 2 -7 -6 113.77 7.32 2 7 -6 117.13 7.37 2 7 -5 4.50 1.49 2 -7 -5 2.39 1.34 -2 7 5 4.10 1.09 2 7 -5 2.69 1.02 2 -7 -5 4.02 1.20 -2 7 5 3.98 2.23 2 -7 -5 3.82 0.85 2 7 -5 4.93 0.89 2 -7 -4 171.46 8.98 2 7 -4 165.76 9.52 2 7 -4 173.92 8.98 2 -7 -4 166.40 9.80 2 7 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7.54 4 -4 -10 134.97 7.55 4 4 -10 136.13 7.53 4 4 -10 124.81 7.63 4 -4 -10 143.46 8.00 4 4 -10 143.17 8.03 4 -4 -9 12.55 1.46 4 -4 -9 13.97 1.78 4 4 -9 10.75 1.63 -4 -4 9 8.77 1.33 4 4 -9 15.05 1.69 4 -4 -9 12.03 2.54 4 -4 -8 19.62 2.87 4 -4 -8 13.65 1.56 4 -4 -8 15.24 1.83 4 4 -8 25.43 2.12 4 -4 -7 70.82 4.13 4 -4 -7 75.10 4.24 4 4 -7 51.77 3.94 4 -4 -7 55.03 4.95 4 4 -6 65.33 4.18 4 -4 -6 60.04 4.08 4 4 -6 73.69 4.18 4 -4 -6 67.54 5.29 4 -4 -6 62.50 4.11 -4 4 5 8.79 1.09 4 -4 -5 8.00 1.13 4 4 -5 9.45 1.45 -4 -4 5 5.16 1.00 4 -4 -5 6.32 2.19 4 -4 -5 7.95 1.20 4 4 -5 5.04 1.04 4 -4 -4 151.46 8.46 4 4 -4 176.98 8.55 4 -4 -4 140.66 8.57 4 -4 -4 128.90 9.31 4 -4 -4 157.55 8.35 4 4 -4 181.21 8.68 -4 4 4 155.45 8.39 -4 -4 4 157.69 8.44 -4 4 3 88.66 6.25 4 -4 -3 88.88 5.04 -4 4 3 86.25 4.95 -4 -4 3 89.00 4.99 4 -4 -3 84.37 5.08 4 4 -3 90.68 5.06 4 -4 -2 129.23 6.31 -4 4 2 121.61 6.07 -4 -4 2 89.85 5.93 -4 4 2 112.11 7.09 4 -4 -2 128.40 6.32 4 4 -2 92.63 6.00 4 -4 -1 50.89 3.33 4 4 -1 48.28 3.31 -4 4 1 55.73 4.02 4 -4 -1 47.36 3.37 -4 4 1 52.17 3.20 -4 -4 1 50.20 3.21 4 -4 0 71.48 4.38 4 -4 0 66.30 4.43 -4 4 0 72.73 4.75 4 4 0 71.98 4.41 -4 4 0 70.47 4.22 -4 -4 0 72.27 4.29 4 -4 0 62.29 4.88 4 -4 1 442.30 21.59 4 4 1 407.41 21.35 4 -4 1 404.12 21.22 -4 4 -1 439.82 21.44 -4 4 -1 432.18 21.17 -4 -4 -1 387.52 21.11 4 -4 1 397.37 21.59 4 -4 2 1038.92 52.09 4 4 2 1053.06 51.96 4 -4 2 1016.54 51.66 -4 4 -2 1013.47 51.63 -4 -4 -2 1067.03 51.75 4 -4 2 1053.76 51.90 4 -4 3 462.96 24.22 4 4 3 462.16 24.06 4 -4 3 459.54 23.62 -4 4 -3 479.59 23.75 -4 -4 -3 443.63 23.73 4 -4 3 448.83 23.56 4 4 4 15.35 2.61 -4 -4 -4 15.04 2.15 4 -4 4 21.73 2.34 -4 4 -4 30.25 2.62 4 -4 4 25.15 3.08 -4 -4 -5 55.44 4.12 4 -4 5 41.76 3.28 -4 4 -5 36.14 3.59 4 -4 5 37.05 4.18 4 4 5 48.91 4.40 -4 4 -6 31.22 3.53 4 -4 6 40.17 3.18 4 4 6 41.52 4.29 -4 -4 -6 44.45 4.04 4 -4 6 37.04 3.18 4 -4 6 33.81 4.11 -4 4 -7 104.45 7.86 -4 -4 -7 135.16 8.48 4 -4 7 113.84 7.29 4 -4 7 111.87 8.74 4 4 7 144.97 9.13 4 -4 8 18.67 3.77 4 4 8 20.14 3.93 -4 4 -8 13.56 2.69 -4 -4 -8 15.75 2.95 -4 -4 -9 270.29 16.53 -4 4 -9 285.80 16.58 -4 4 -10 66.22 6.35 -4 -4 -10 81.86 6.73 -4 4 -11 12.10 3.13 -4 -4 -11 16.00 3.47 -4 -4 -12 67.06 6.59 -4 4 -12 52.15 6.06 -4 -4 -13 144.48 11.01 -4 4 -13 147.27 11.09 -4 -4 -14 23.31 4.56 -4 4 -14 14.32 4.13 4 4 14 19.32 4.16 -4 4 -15 39.63 5.76 -4 -4 -15 35.77 5.46 4 4 15 26.54 4.96 -4 4 -16 11.95 4.40 4 4 16 7.93 3.74 -4 -4 -16 7.79 3.85 4 5 -19 -0.60 4.16 4 -5 -19 -2.92 4.46 4 5 -18 -1.72 4.22 4 -5 -18 -3.37 4.14 4 5 -17 7.75 4.58 4 -5 -17 6.53 4.13 4 5 -16 3.19 3.87 4 -5 -16 -3.63 4.04 4 5 -15 40.84 6.28 4 -5 -15 49.34 6.43 4 5 -14 23.30 2.47 4 -5 -14 17.56 4.47 4 5 -14 16.08 4.48 4 5 -13 8.78 1.63 4 5 -13 9.42 3.66 4 -5 -13 8.00 3.47 4 5 -12 101.65 6.65 4 -5 -12 119.82 6.58 4 5 -12 98.77 8.90 4 -5 -12 104.65 8.98 4 5 -11 7.10 3.11 4 -5 -11 1.25 1.35 4 5 -11 5.26 1.36 4 5 -11 4.24 1.63 4 -5 -11 2.88 1.07 4 -5 -11 -2.20 2.56 4 -5 -10 4.15 1.39 4 5 -10 2.67 1.38 4 -5 -10 2.91 0.97 4 5 -10 4.85 0.79 4 5 -10 0.68 2.23 4 -5 -10 2.99 2.33 4 5 -10 4.84 1.27 4 5 -9 115.50 6.37 4 -5 -9 117.25 6.93 4 5 -9 118.52 6.46 4 -5 -9 112.48 6.95 4 5 -9 134.28 7.14 4 5 -8 43.65 3.00 4 -5 -8 55.15 3.59 4 -5 -8 54.98 3.57 4 5 -8 47.38 3.45 4 -5 -8 48.36 4.57 4 -5 -7 167.50 9.63 4 5 -7 181.80 9.59 4 -5 -7 181.30 9.61 4 -5 -7 164.95 10.70 4 -5 -6 68.38 4.63 4 -5 -6 73.14 4.55 4 5 -6 76.65 4.54 4 -5 -6 76.28 5.79 4 5 -6 78.26 4.56 4 -5 -5 13.60 1.38 4 -5 -5 14.98 1.54 4 5 -5 5.85 1.10 4 5 -5 9.10 1.41 4 -5 -5 10.99 2.31 4 -5 -4 17.68 1.83 4 -5 -4 15.70 2.60 4 -5 -4 14.69 1.56 4 5 -4 19.14 1.62 -4 5 4 16.26 1.51 -4 -5 4 16.95 1.55 4 -5 -3 107.66 6.43 -4 5 3 111.80 7.54 4 -5 -3 100.52 7.13 -4 5 3 109.81 6.01 -4 -5 3 109.19 6.03 4 -5 -3 111.74 6.16 4 5 -3 110.67 6.09 4 -5 -2 229.18 13.44 -4 5 2 268.29 14.52 -4 -5 2 257.24 13.15 4 5 -2 251.51 13.22 -4 5 2 262.89 13.11 4 -5 -2 260.36 13.31 4 -5 -2 263.66 13.45 4 -5 -1 865.15 39.43 -4 5 1 806.77 39.08 -4 -5 1 724.95 39.05 -4 5 1 833.22 40.22 4 5 -1 740.56 39.20 4 -5 -1 822.61 39.48 4 -5 0 25.51 2.29 4 -5 0 26.16 2.45 -4 5 0 28.74 2.14 -4 -5 0 29.78 2.20 -4 5 0 30.30 2.91 4 5 0 30.33 2.46 4 -5 0 30.02 2.51 4 -5 1 12.45 1.67 4 5 1 22.20 2.09 -4 5 -1 16.10 1.94 4 -5 1 10.53 1.75 -4 5 -1 9.59 1.36 -4 -5 -1 22.45 1.81 4 -5 2 98.78 6.16 4 5 2 87.60 5.92 4 -5 2 86.45 6.07 4 -5 2 98.67 5.90 -4 5 -2 99.38 5.79 -4 5 -2 88.42 5.49 -4 -5 -2 93.59 5.63 4 5 3 35.74 3.31 4 -5 3 35.68 2.96 4 -5 3 33.42 3.08 -4 5 -3 33.89 2.90 -4 -5 -3 31.91 2.86 4 -5 3 38.59 3.56 4 -5 4 6.98 2.14 4 5 4 4.71 1.88 4 -5 4 7.31 1.76 -4 5 -4 5.41 1.40 -4 -5 -4 5.97 1.50 4 -5 4 7.10 1.51 4 -5 5 8.29 2.45 4 5 5 10.46 2.47 -4 -5 -5 12.42 2.04 -4 5 -5 9.16 1.82 4 -5 5 14.78 2.04 -4 -5 -6 196.24 12.07 -4 5 -6 202.18 11.97 4 -5 6 209.32 11.30 4 -5 6 218.85 12.95 4 5 6 193.15 12.45 -4 5 -7 303.10 17.21 -4 -5 -7 310.73 17.42 4 -5 7 303.00 16.18 4 -5 7 300.81 18.17 4 5 7 311.17 18.01 4 -5 8 2.84 3.08 4 5 8 0.66 2.73 -4 5 -8 2.24 2.01 -4 -5 -8 2.10 1.95 4 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45.53 5.30 -4 -6 -8 40.17 4.24 -4 6 -8 45.36 4.37 4 -6 8 41.22 5.25 4 -6 9 4.86 1.33 -4 6 -9 3.45 2.32 -4 -6 -9 3.95 2.30 4 -6 10 17.74 1.96 -4 6 -10 23.85 3.65 -4 -6 -10 15.57 3.45 -4 6 -11 6.77 3.02 -4 -6 -11 2.71 2.74 4 6 11 5.96 3.06 4 -6 11 6.40 1.30 -4 6 -12 -1.40 2.70 -4 -6 -12 4.40 3.00 4 6 12 2.69 3.02 -4 6 -13 16.69 4.01 -4 -6 -13 19.31 4.05 4 6 13 10.16 3.58 -4 6 -14 2.04 3.09 4 6 14 4.79 3.48 -4 -6 -14 3.79 3.42 -4 6 -15 17.85 4.56 -4 -6 -15 18.39 4.56 4 6 15 22.31 5.04 -4 -6 -16 1.90 3.54 -4 6 -16 1.38 3.62 4 7 -19 -0.57 4.49 4 7 -18 50.81 7.49 4 7 -17 2.56 4.45 4 -7 -17 -1.50 4.20 4 7 -16 4.90 3.86 4 -7 -16 9.58 4.26 4 7 -15 14.55 4.52 4 -7 -15 12.82 4.23 4 7 -15 15.15 2.36 4 7 -14 6.68 3.83 4 -7 -14 9.18 3.75 4 7 -14 5.74 1.72 4 7 -13 21.11 4.48 4 -7 -13 24.96 4.61 4 7 -13 19.22 2.54 4 7 -12 -2.65 3.29 4 -7 -12 0.75 2.88 4 7 -12 1.46 1.48 4 -7 -11 112.23 6.73 4 7 -11 107.48 6.71 4 7 -11 105.22 8.57 4 -7 -11 106.05 8.49 4 7 -11 95.24 6.79 4 -7 -10 24.49 2.61 4 7 -10 27.13 2.69 -4 7 10 25.84 2.13 4 7 -10 35.59 4.48 4 7 -10 27.25 2.90 4 -7 -10 23.60 3.91 4 -7 -9 235.85 13.82 4 7 -9 273.43 13.75 -4 7 9 270.05 13.42 4 7 -9 237.82 14.06 4 7 -9 269.95 15.70 4 -7 -9 229.85 15.19 -4 7 8 45.28 3.09 4 -7 -8 42.24 3.18 4 -7 -8 37.46 3.30 4 7 -8 39.76 3.00 4 7 -8 44.22 3.16 4 7 -8 43.95 4.60 4 -7 -8 40.79 4.39 4 -7 -7 48.13 3.18 4 7 -7 40.81 3.03 4 7 -7 35.09 2.95 -4 7 7 48.89 3.24 4 -7 -7 42.23 3.37 4 7 -6 -0.29 0.91 4 -7 -6 -0.43 0.92 4 -7 -6 1.00 0.96 -4 7 6 0.75 0.94 4 7 -6 0.82 0.89 4 7 -6 1.88 1.05 4 -7 -5 8.14 1.49 4 7 -5 16.34 1.69 4 -7 -5 8.49 1.32 4 -7 -5 8.77 2.40 -4 7 5 8.74 1.48 4 7 -5 11.34 1.36 4 7 -4 13.04 1.65 4 -7 -4 9.16 1.60 4 -7 -4 10.83 1.40 4 -7 -4 12.47 2.53 4 7 -4 14.05 1.43 -4 7 4 13.78 1.72 4 7 -3 225.49 12.48 -4 7 3 243.90 14.16 4 -7 -3 225.12 12.74 4 -7 -3 242.93 12.18 4 7 -3 217.31 12.04 4 -7 -3 246.57 13.63 -4 7 3 254.57 12.80 4 7 -2 276.50 14.92 4 7 -2 265.87 14.46 -4 7 2 282.94 16.12 4 -7 -2 295.26 14.65 4 -7 -2 305.90 15.97 -4 7 2 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3.18 2.37 -13 6 0 189.21 11.82 -13 -6 0 184.27 12.01 -13 6 -1 1.05 2.41 -13 -6 -1 2.02 2.68 -13 6 -2 6.86 2.79 -13 -6 -2 6.59 2.95 -13 6 -3 3.18 2.72 -13 -6 -3 3.47 2.87 -13 6 -4 14.91 3.53 -13 -6 -4 7.97 3.42 -13 6 -5 18.06 3.80 -13 -6 -5 15.16 3.88 13 -7 -14 1.58 1.93 13 -7 -13 0.92 1.90 13 -7 -12 27.75 3.44 13 -7 -11 6.47 2.22 -13 7 11 1.92 4.29 -13 7 11 5.57 2.31 -13 -7 11 4.17 2.41 13 -7 -10 5.21 2.07 -13 7 10 4.15 3.93 -13 7 10 2.96 2.24 -13 -7 10 11.65 2.89 -13 7 9 -1.08 1.89 -13 -7 9 0.96 2.05 -13 7 9 -0.44 3.50 -13 7 8 12.54 2.44 -13 -7 8 6.29 2.53 -13 7 8 11.40 4.48 -13 7 7 5.09 2.22 -13 -7 7 6.37 2.50 -13 7 7 2.02 3.45 -13 7 6 36.46 5.48 -13 7 6 42.98 4.26 -13 -7 6 44.06 4.38 -13 7 5 -1.14 3.46 -13 7 5 6.34 2.22 -13 -7 5 0.94 2.12 -13 7 4 65.27 5.24 -13 -7 4 57.37 5.27 -13 7 3 -0.22 2.08 -13 -7 3 5.14 2.43 -13 7 2 19.80 3.11 -13 -7 2 21.56 3.43 -13 7 1 11.72 2.60 -13 -7 1 10.64 3.00 -13 7 0 99.86 7.68 -13 -7 0 117.96 8.21 -13 7 -1 -0.25 2.33 -13 -7 -1 0.28 2.55 -13 7 -2 74.30 6.51 -13 -7 -2 88.69 7.18 -13 7 -3 3.07 2.46 -13 7 -4 50.34 5.41 -13 7 -5 15.22 3.72 -13 8 10 0.64 1.95 -13 8 9 10.05 4.38 -13 8 9 16.92 2.88 13 -8 -8 8.64 2.48 -13 8 8 8.14 2.33 -13 8 8 3.93 4.12 -13 8 7 2.04 2.05 13 -8 -7 1.71 1.87 -13 8 7 3.37 3.88 -13 8 6 38.56 5.77 -13 8 6 31.83 3.73 -13 8 5 2.50 2.03 -13 8 5 1.17 3.73 -13 8 4 9.57 2.44 -13 8 3 1.06 2.04 -13 8 2 11.97 2.75 -13 8 1 0.22 2.06 -13 8 0 8.15 2.57 -13 8 -1 31.66 3.96 -13 8 -2 0.26 2.46 -13 9 7 8.78 4.41 -13 9 6 -2.49 4.08 -13 9 5 0.81 3.85 -14 0 18 13.87 4.73 -14 0 17 0.87 3.99 -14 0 16 2.91 3.53 -14 0 15 -0.40 3.54 -14 0 14 -0.39 3.30 -14 0 14 2.20 2.12 -14 0 13 -2.29 3.33 -14 0 13 0.28 2.10 -14 0 12 21.54 3.32 -14 0 11 1.03 1.86 -14 0 10 35.27 4.12 -14 0 9 0.25 1.98 -14 0 8 16.64 2.94 -14 0 7 -0.75 1.87 -14 0 6 146.14 9.68 -14 0 5 1.28 1.85 -14 0 4 14.00 2.73 -14 0 3 -1.35 2.23 -14 0 2 55.17 5.18 -14 0 1 -2.62 2.16 -14 0 0 2.97 2.24 -14 0 -1 0.62 1.96 -14 0 -2 12.77 3.19 -14 0 -3 0.68 2.54 -14 0 -4 3.87 2.74 -14 0 -5 -0.73 2.64 -14 -1 17 -5.62 4.12 -14 1 17 -3.64 4.25 -14 -1 16 4.70 3.83 -14 1 16 1.77 3.73 -14 -1 15 2.68 3.40 -14 1 15 0.43 3.70 -14 1 14 19.37 4.65 -14 -1 14 28.02 3.71 -14 1 13 4.37 3.48 -14 -1 13 10.61 2.73 -14 1 12 26.97 4.78 -14 -1 12 16.62 3.12 -14 1 11 36.39 5.45 -14 -1 11 40.79 4.31 -14 -1 10 8.82 2.67 -14 -1 9 32.07 3.83 -14 -1 8 9.15 2.48 -14 -1 7 10.65 2.59 -14 -1 6 133.03 9.06 -14 -1 5 1.29 1.95 -14 -1 4 8.18 2.54 -14 -1 3 69.10 5.99 -14 -1 2 11.56 2.89 -14 -1 1 5.54 2.63 -14 -1 0 2.70 2.42 -14 -1 -1 -0.31 2.37 -14 -1 -2 7.59 3.14 -14 -1 -3 -0.34 2.48 -14 -1 -4 17.36 3.66 -14 -1 -5 0.37 2.93 -14 2 16 13.92 4.83 -14 2 15 10.29 4.48 -14 2 14 15.22 4.66 -14 2 14 18.63 3.34 -14 -2 14 26.72 3.62 -14 2 13 17.76 4.60 -14 2 13 17.91 3.13 -14 -2 13 26.88 3.65 -14 2 12 -5.25 3.56 -14 2 12 1.05 2.06 -14 -2 12 0.81 1.92 -14 2 11 3.04 2.16 -14 -2 11 2.88 2.09 -14 2 11 0.39 3.02 -14 2 10 8.37 2.45 -14 -2 10 4.46 2.41 -14 2 10 9.56 3.73 -14 2 9 4.46 2.23 -14 -2 9 1.28 2.06 -14 2 8 1.73 2.11 -14 -2 8 1.28 2.00 -14 2 7 37.95 3.98 -14 -2 7 24.50 3.62 -14 2 6 2.70 2.21 -14 -2 6 2.04 2.10 -14 2 5 119.20 8.22 -14 -2 5 108.41 8.09 -14 2 4 2.05 2.10 -14 -2 4 2.92 2.22 -14 2 3 -0.27 2.12 -14 -2 3 -2.20 2.20 -14 2 2 13.66 2.87 -14 -2 2 7.36 2.67 -14 2 1 1.41 2.18 -14 -2 1 0.88 2.18 -14 2 0 22.39 3.62 -14 -2 0 22.56 3.66 -14 2 -1 11.34 3.08 -14 -2 -1 8.56 3.00 -14 2 -2 26.23 3.92 -14 -2 -2 18.50 3.78 -14 2 -3 70.03 6.74 -14 -2 -3 79.46 7.02 -14 2 -4 17.98 3.91 -14 -2 -4 21.39 4.05 -14 3 15 37.00 6.29 -14 3 14 1.36 4.03 -14 3 14 0.80 2.15 -14 -3 14 1.68 2.30 -14 3 13 40.42 4.48 -14 -3 13 39.86 4.39 -14 3 13 32.04 5.65 -14 3 12 3.45 3.72 -14 3 12 3.42 2.21 -14 -3 12 3.31 2.33 -14 3 11 7.58 2.45 -14 -3 11 6.62 2.48 -14 3 11 7.79 3.91 -14 3 10 57.72 6.61 -14 3 10 66.45 5.47 -14 -3 10 53.93 5.29 -14 3 9 2.21 1.95 -14 -3 9 1.55 1.94 -14 3 9 2.32 3.12 -14 3 8 20.91 3.23 -14 -3 8 25.10 3.49 -14 3 7 5.83 2.32 -14 -3 7 0.51 1.94 -14 3 6 12.67 2.66 -14 -3 6 15.84 2.99 -14 3 5 5.21 2.22 -14 -3 5 8.10 2.52 -14 3 4 0.76 2.00 -14 -3 4 -0.27 2.07 -14 3 3 6.92 2.50 -14 -3 3 0.84 2.09 -14 3 2 0.54 1.92 -14 -3 2 2.26 2.18 -14 3 1 3.62 2.21 -14 -3 1 1.46 2.37 -14 3 0 0.87 2.19 -14 -3 0 -0.30 2.36 -14 3 -1 70.02 6.35 -14 -3 -1 71.31 6.55 -14 3 -2 11.36 3.02 -14 -3 -2 8.91 3.14 -14 3 -3 1.98 2.76 -14 -3 -3 -0.35 2.80 -14 3 -4 13.32 3.59 -14 -3 -4 23.24 4.14 -14 4 14 1.45 4.30 -14 4 13 -1.84 3.86 -14 4 13 1.05 2.00 -14 -4 13 0.28 2.18 -14 4 12 -1.77 3.77 -14 4 12 1.05 2.16 -14 -4 12 4.21 2.42 -14 -4 11 27.80 3.90 -14 4 11 33.96 5.59 -14 4 11 43.66 4.31 -14 4 10 14.01 2.86 -14 -4 10 17.01 2.97 -14 4 10 11.20 4.16 -14 4 9 2.44 2.09 -14 -4 9 2.87 2.20 -14 4 8 15.27 2.81 -14 -4 8 6.17 2.37 -14 -4 7 2.84 2.10 -14 4 7 2.40 2.01 -14 4 6 13.92 2.79 -14 -4 6 12.85 2.78 -14 4 5 26.39 3.54 -14 -4 5 25.64 3.54 -14 4 4 17.66 3.17 -14 -4 4 17.86 3.24 -14 4 3 12.98 2.85 -14 -4 3 18.47 3.30 -14 4 2 6.08 2.60 -14 -4 2 6.80 2.61 -14 -4 1 47.69 4.90 -14 4 1 31.36 4.22 -14 4 0 2.01 2.66 -14 -4 0 0.61 2.34 -14 4 -1 2.35 2.41 -14 -4 -1 0.31 2.57 -14 4 -2 16.35 3.53 -14 -4 -2 19.73 3.75 -14 4 -3 5.54 2.95 -14 -4 -3 3.45 2.89 -14 4 -4 0.34 2.88 -14 -4 -4 -2.86 3.08 14 -5 -15 -0.62 1.92 -14 5 13 2.56 2.15 -14 -5 13 4.11 2.42 -14 5 12 12.09 4.49 -14 5 12 7.18 2.60 -14 -5 12 9.68 2.83 -14 5 11 0.25 2.17 -14 -5 11 0.27 2.22 -14 5 10 25.65 3.46 -14 -5 10 24.37 3.58 -14 5 9 1.46 2.11 -14 -5 9 1.32 2.19 -14 5 9 -1.25 3.65 -14 5 8 2.15 1.98 -14 -5 8 0.26 2.10 -14 5 8 1.61 3.50 -14 5 7 8.60 2.47 -14 -5 7 7.29 2.54 -14 5 7 5.95 3.49 -14 5 6 13.61 2.76 -14 -5 6 16.30 3.11 -14 5 5 2.39 2.05 -14 -5 5 3.12 2.26 -14 5 4 -0.98 2.04 -14 -5 4 0.80 2.18 -14 5 3 25.53 3.46 -14 -5 3 16.60 3.32 -14 5 2 46.36 4.76 -14 -5 2 38.27 4.62 -14 5 1 22.02 3.52 -14 -5 1 24.51 3.79 -14 5 0 6.69 2.67 -14 -5 0 7.23 3.00 -14 5 -1 96.85 7.97 -14 -5 -1 118.81 8.60 -14 5 -2 5.14 2.87 -14 -5 -2 7.20 3.07 -14 5 -3 3.81 2.86 -14 -5 -3 5.46 3.03 -14 5 -4 72.57 6.71 -14 -5 -4 57.38 6.38 14 -6 -15 0.67 1.81 14 -6 -14 3.16 2.05 14 -6 -13 6.22 2.17 -14 6 12 1.50 2.17 -14 -6 12 1.90 2.25 -14 6 11 8.84 4.58 -14 6 11 2.01 2.14 -14 -6 11 2.76 2.57 -14 6 10 34.95 5.91 -14 6 10 29.86 3.83 -14 -6 10 31.65 4.06 -14 6 9 26.97 3.54 -14 -6 9 26.04 3.68 -14 6 9 21.29 5.12 -14 6 8 10.38 2.63 -14 -6 8 8.82 2.77 -14 6 8 11.29 4.18 -14 6 7 4.90 2.22 -14 -6 7 7.44 2.55 -14 6 7 3.67 3.56 -14 -6 6 2.33 2.61 -14 6 6 1.17 2.08 -14 6 5 56.60 5.32 -14 -6 5 69.50 5.93 -14 6 4 0.24 2.29 -14 -6 4 0.26 2.40 -14 6 3 5.88 2.45 -14 -6 3 4.59 2.63 -14 6 2 39.01 4.56 -14 -6 2 60.73 5.44 -14 6 1 0.79 2.27 -14 -6 1 0.29 2.52 -14 6 0 5.20 2.70 -14 -6 0 8.71 3.00 -14 6 -1 139.18 9.83 -14 -6 -1 142.72 10.12 -14 6 -2 16.15 3.41 -14 -6 -2 8.07 3.26 -14 6 -3 19.18 3.73 -14 -6 -3 17.62 3.90 -14 7 12 2.18 2.25 -14 7 11 11.89 2.84 -14 7 10 0.48 2.29 -14 -7 10 -0.53 2.32 -14 7 9 26.78 3.44 -14 -7 9 16.54 3.29 -14 7 9 19.58 5.16 -14 7 8 8.98 2.64 -14 -7 8 9.48 2.86 -14 7 8 10.84 4.49 -14 7 7 -1.38 2.17 -14 -7 7 1.03 2.38 -14 7 7 -4.20 3.83 -14 7 6 17.87 3.14 -14 -7 6 18.85 3.37 -14 7 5 3.93 2.42 -14 -7 5 1.55 2.32 -14 7 4 3.49 2.29 -14 -7 4 5.71 2.52 -14 7 3 4.79 2.43 -14 -7 3 6.43 2.67 -14 7 2 3.68 2.44 -14 -7 2 7.67 2.83 -14 7 1 38.68 4.34 -14 7 0 4.23 2.46 -14 7 -1 6.09 2.78 -14 7 -2 1.44 2.52 -14 7 -3 -0.30 2.68 -14 8 9 2.08 2.25 -14 8 8 1.12 2.06 -14 8 7 9.24 2.67 -14 8 6 39.05 6.05 -14 8 6 45.44 4.53 -14 8 5 1.14 2.13 -14 8 4 0.46 2.03 -14 8 3 50.65 4.83 -14 8 2 19.77 3.30 -15 0 16 -2.16 3.85 -15 0 15 1.27 3.67 -15 0 14 1.18 2.32 -15 0 13 22.52 3.45 -15 0 12 -1.13 2.39 -15 0 11 34.12 4.16 -15 0 10 -0.55 2.11 -15 0 9 4.89 2.42 -15 0 8 -0.54 2.14 -15 0 7 145.84 9.84 -15 0 6 2.72 2.14 -15 0 5 10.85 2.77 -15 0 4 -0.85 2.13 -15 0 3 4.45 2.59 -15 0 2 -0.90 2.30 -15 0 1 47.65 5.20 -15 0 0 -2.26 2.68 -15 0 -1 50.82 5.52 -15 0 -2 -0.35 2.61 -15 -1 17 -0.42 4.20 -15 1 15 21.99 5.02 -15 1 14 0.43 3.48 -15 -1 14 6.26 2.52 -15 1 13 0.84 3.43 -15 -1 13 -1.19 2.51 -15 -1 12 28.56 3.92 -15 -1 11 1.10 2.11 -15 -1 10 68.80 6.06 -15 -1 9 3.56 2.34 -15 -1 8 4.39 2.38 -15 -1 7 175.81 11.42 -15 -1 6 11.27 2.83 -15 -1 5 1.96 2.28 -15 -1 4 16.34 3.17 -15 -1 3 0.30 2.29 -15 -1 2 -0.30 2.26 -15 -1 1 4.37 2.64 -15 -1 0 4.55 2.69 -15 -1 -1 5.73 2.90 -15 -1 -2 0.35 2.77 -15 2 14 46.39 4.89 -15 -2 14 45.79 4.91 -15 2 14 29.62 5.90 -15 2 13 8.24 3.79 -15 2 13 9.95 3.06 -15 -2 13 6.05 2.76 -15 2 12 11.71 2.97 -15 -2 12 22.18 3.54 -15 2 12 18.25 4.64 -15 2 11 4.59 2.39 -15 -2 11 10.89 2.75 -15 2 10 9.24 2.75 -15 -2 10 7.87 2.59 -15 2 9 0.27 2.26 -15 -2 9 0.55 2.30 -15 2 8 -2.41 2.24 -15 -2 8 0.83 2.10 -15 2 7 52.41 5.17 -15 -2 7 55.66 5.33 -15 2 6 81.16 6.62 -15 -2 6 82.44 6.74 -15 2 5 40.96 4.58 -15 -2 5 49.10 4.93 -15 2 4 1.95 2.41 -15 -2 4 -1.15 2.52 -15 2 3 27.50 3.98 -15 -2 3 33.34 4.39 -15 2 2 0.59 2.34 -15 -2 2 -0.31 2.31 -15 2 1 6.39 2.73 -15 -2 1 12.94 3.19 -15 2 0 9.83 3.15 -15 -2 0 4.59 2.59 -15 2 -1 3.26 2.71 -15 -2 -1 0.34 2.67 -15 2 -2 2.38 2.81 -15 -2 -2 1.76 2.83 -15 3 14 0.85 2.36 -15 -3 14 -1.19 2.46 -15 3 13 -0.91 4.12 -15 3 13 0.29 2.35 -15 -3 13 1.51 2.34 -15 3 12 0.44 3.42 -15 3 12 3.32 2.41 -15 -3 12 2.92 2.29 -15 3 11 16.68 3.21 -15 -3 11 28.84 3.76 -15 3 11 18.00 4.49 -15 3 10 6.49 2.55 -15 -3 10 10.23 2.79 -15 3 10 7.58 3.88 -15 3 9 36.36 4.25 -15 -3 9 36.31 4.32 -15 3 8 0.27 2.05 -15 -3 8 0.56 2.04 -15 3 7 12.42 2.81 -15 -3 7 13.36 2.89 -15 3 6 -0.53 2.05 -15 -3 6 2.78 2.31 -15 3 5 4.04 2.25 -15 -3 5 5.11 2.42 -15 3 4 3.56 2.33 -15 -3 4 0.87 2.23 -15 3 3 2.88 2.46 -15 -3 3 3.92 2.56 -15 3 2 2.33 2.35 -15 -3 2 5.21 2.69 -15 3 1 2.12 2.49 -15 -3 1 1.27 2.43 -15 3 0 1.88 2.54 -15 -3 0 0.99 2.49 -15 3 -1 0.64 2.70 -15 -3 -1 1.35 2.67 -15 3 -2 -2.37 2.74 -15 -3 -2 -0.71 2.82 -15 4 13 -0.28 2.25 -15 -4 13 0.30 2.36 -15 4 12 2.22 2.33 -15 -4 12 0.89 2.46 -15 4 11 9.10 2.74 -15 -4 11 12.28 2.95 -15 4 11 6.22 3.94 -15 4 10 1.32 2.09 -15 -4 10 -1.97 2.34 -15 4 10 0.87 3.65 -15 4 9 4.21 2.37 -15 -4 9 3.10 2.40 -15 4 8 2.63 2.13 -15 -4 8 -1.12 2.27 -15 4 7 11.20 2.86 -15 -4 7 9.75 2.79 -15 4 6 1.04 2.15 -15 -4 6 0.28 2.08 -15 4 5 2.13 2.16 -15 -4 5 0.85 2.28 -15 4 4 7.03 2.72 -15 -4 4 1.45 2.34 -15 4 3 1.67 2.27 -15 -4 3 -1.19 2.41 -15 4 2 13.54 3.10 -15 -4 2 8.33 2.84 -15 4 1 9.21 2.84 -15 -4 1 13.27 3.36 -15 4 0 13.47 3.26 -15 -4 0 14.40 3.42 -15 4 -1 53.74 5.76 -15 -4 -1 52.91 5.81 -15 4 -2 15.54 3.59 -15 5 13 0.28 2.21 -15 -5 13 0.59 2.45 -15 5 12 3.34 2.48 -15 -5 12 5.42 2.88 -15 5 11 8.24 2.71 -15 -5 11 6.04 2.67 -15 5 10 0.52 2.23 -15 -5 10 0.28 2.16 -15 5 9 28.43 5.57 -15 5 9 32.06 4.10 -15 -5 9 32.57 4.26 -15 5 8 0.77 2.25 -15 -5 8 -0.28 2.43 -15 5 7 0.52 2.23 -15 -5 7 4.22 2.61 -15 5 6 11.41 2.85 -15 -5 6 7.33 2.79 -15 5 5 0.26 2.09 -15 -5 5 2.55 2.47 -15 5 4 1.86 2.22 -15 -5 4 5.50 2.67 -15 5 3 11.70 2.99 -15 -5 3 14.21 3.26 -15 5 2 3.44 2.45 -15 -5 2 2.18 2.63 -15 5 1 20.63 3.61 -15 -5 1 21.10 4.04 -15 5 0 -1.81 2.73 -15 -5 0 -1.97 2.74 -15 5 -1 0.63 2.78 -15 -5 -1 3.39 2.86 -15 6 12 42.65 4.69 -15 -6 12 37.50 4.71 -15 6 11 1.87 2.37 -15 -6 11 3.51 2.78 -15 6 10 9.53 2.85 -15 -6 10 14.71 3.32 -15 6 9 4.59 2.47 -15 -6 9 4.72 2.58 -15 6 8 -1.28 2.26 -15 -6 8 2.25 2.46 -15 6 7 9.67 2.75 -15 -6 7 6.46 2.82 -15 6 6 -0.25 2.27 -15 -6 6 -2.24 2.52 -15 6 5 2.81 2.40 -15 -6 5 0.57 2.26 -15 6 4 1.82 2.37 -15 -6 4 0.86 2.31 -15 6 3 33.01 4.20 -15 -6 3 31.41 4.32 -15 6 2 36.98 4.44 -15 -6 2 27.78 4.16 -15 6 1 2.02 2.57 -15 -6 1 3.51 3.05 -15 6 0 -0.29 2.53 -15 -6 0 3.23 2.84 -15 7 12 4.15 2.58 -15 7 11 2.63 2.60 -15 7 10 5.12 2.57 -15 7 9 4.74 2.57 -15 7 8 1.01 2.30 -15 7 7 -0.25 2.25 -15 7 6 -0.50 2.26 -15 7 5 -0.25 2.24 -15 7 4 2.53 2.60 -15 7 3 4.95 2.62 -15 7 2 65.58 5.96 -15 7 1 8.25 2.90 -15 7 0 -0.86 2.68 -16 0 12 23.81 3.81 -16 0 11 1.78 2.25 -16 0 10 37.05 4.41 -16 0 9 -0.88 2.13 -16 0 8 167.70 11.22 -16 0 7 2.35 2.52 -16 0 6 98.21 7.73 -16 0 5 -0.60 2.42 -16 0 4 38.96 4.66 -16 0 3 -2.25 2.75 -16 0 2 4.87 2.77 -16 0 1 0.34 2.55 -16 -1 11 8.92 2.86 -16 -1 10 16.75 3.46 -16 -1 9 9.74 2.92 -16 -1 8 1.78 2.37 -16 -1 7 69.61 6.27 -16 -1 6 70.97 6.36 -16 -1 5 3.03 2.50 -16 -1 4 21.64 3.74 -16 -1 3 0.32 2.34 -16 -1 2 -0.65 2.61 -16 -1 1 21.71 3.96 -16 2 11 -0.29 2.27 -16 -2 11 -1.48 2.31 -16 2 10 12.23 3.16 -16 -2 10 14.47 3.06 -16 2 9 3.73 2.49 -16 -2 9 6.86 2.76 -16 2 8 0.87 2.46 -16 -2 8 0.30 2.39 -16 2 7 19.36 3.51 -16 -2 7 19.75 3.59 -16 2 6 4.05 2.46 -16 -2 6 3.59 2.61 -16 2 5 3.25 2.38 -16 -2 5 3.97 2.50 -16 2 4 11.70 2.96 -16 -2 4 9.63 2.96 -16 2 3 0.94 2.48 -16 -2 3 -1.30 2.75 -16 2 2 11.14 3.02 -16 -2 2 11.55 3.34 -16 2 1 -0.33 2.42 -16 -2 1 2.05 2.96 -16 3 11 5.44 2.72 -16 -3 11 1.20 2.54 -16 3 10 32.96 4.17 -16 -3 10 21.60 3.79 -16 3 9 3.71 2.61 -16 -3 9 1.80 2.44 -16 3 8 7.75 2.90 -16 -3 8 8.76 3.00 -16 3 7 1.71 2.36 -16 -3 7 4.80 2.57 -16 3 6 5.42 2.60 -16 -3 6 9.01 2.77 -16 3 5 1.46 2.37 -16 -3 5 1.85 2.29 -16 3 4 4.74 2.65 -16 -3 4 2.50 2.56 -16 3 3 1.84 2.47 -16 -3 3 2.88 2.74 -16 3 2 -1.26 2.58 -16 -3 2 1.00 2.49 -16 4 11 3.13 2.44 -16 4 10 0.57 2.43 -16 -4 10 0.30 2.51 -16 4 9 3.67 2.49 -16 -4 9 -1.81 2.29 -16 4 8 3.96 2.52 -16 -4 8 3.64 2.62 -16 4 7 60.43 5.62 -16 -4 7 56.00 5.73 -16 4 6 10.71 2.83 -16 -4 6 5.77 2.79 -16 4 5 7.16 2.68 -16 -4 5 1.83 2.51 -16 4 4 13.16 3.23 -16 -4 4 16.59 3.53 -16 4 3 44.50 5.01 -16 -4 3 40.60 5.09 -16 4 2 9.46 3.16 -16 -4 2 7.39 3.12 -16 5 10 -0.55 2.27 -16 5 9 0.84 2.38 -16 -5 9 -0.61 2.48 -16 5 8 1.66 2.51 -16 -5 8 -0.60 2.56 -16 5 7 1.96 2.58 -16 -5 7 3.95 2.94 -16 5 6 5.04 2.58 -16 -5 6 6.69 3.07 -16 5 5 2.53 2.48 -16 -5 5 3.05 2.69 -16 5 4 21.60 3.67 -16 -5 4 22.23 4.05 -16 5 3 12.61 3.11 -16 -5 3 7.65 3.09 -16 6 9 0.55 2.32 -16 6 8 43.00 4.84 -16 -6 8 55.37 5.60 -16 6 7 1.10 2.34 -16 -6 7 3.64 2.79 -16 6 6 5.49 2.61 -16 -6 6 9.08 3.15 -16 6 5 -0.56 2.36 -16 -6 5 0.31 2.54 -16 6 4 10.92 3.03 0 0 0 0.00 0.00 TITL CN_4_CN_4_CF3_diaryl_EtOAc_Hex in P2/n REM P2/n (#13 in standard setting) CELL 0.71073 14.080897 10.991732 17.165856 90.0000 108.8459 90.0000 ZERR 4.00 0.000686 0.000383 0.000785 0.0000 0.0052 0.0000 LATT 1 SYMM -x+1/2, y,-z+1/2 SFAC C H N O F UNIT 120.00 104.00 12.00 4.00 12.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 6002 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 C1 C 0.6751(2) 0.8799(3) 0.83784(17) 0.0308(6) Uani 1 1 d . . . . . C2 C 0.5724(2) 0.9419(2) 0.78914(17) 0.0297(6) Uani 1 1 d . . . . . H1 H 0.564193 1.026676 0.770548 0.036 Uiso 1 1 calc R U . . . C3 C 0.5237(2) 0.8841(2) 0.84998(16) 0.0279(6) Uani 1 1 d . . . . . H2 H 0.480546 0.927910 0.875266 0.033 Uiso 1 1 calc R U . . . C4 C 0.6246(2) 0.8231(2) 0.89862(17) 0.0288(6) Uani 1 1 d . . . . . H3 H 0.654138 0.822267 0.958729 0.035 Uiso 1 1 calc R U . . . C5 C 0.6439(2) 0.7651(3) 0.78113(16) 0.0273(6) Uani 1 1 d . . . . . H4 H 0.688136 0.721870 0.756599 0.033 Uiso 1 1 calc R U . . . C6 C 0.5437(2) 0.8276(2) 0.73129(16) 0.0247(6) Uani 1 1 d . . . . . C7 C 0.4904(2) 0.7705(2) 0.79324(16) 0.0243(6) Uani 1 1 d . . . . . C8 C 0.5961(2) 0.7075(2) 0.84298(16) 0.0252(6) Uani 1 1 d . . . . . C9 C 0.7729(2) 0.9369(3) 0.85934(18) 0.0372(7) Uani 1 1 d . . . . . N1 N 0.8506(2) 0.9804(3) 0.87439(17) 0.0509(8) Uani 1 1 d . . . . . C10 C 0.3832(2) 0.7285(2) 0.77278(16) 0.0265(6) Uani 1 1 d . . . . . O1 O 0.32835(15) 0.78813(19) 0.80179(14) 0.0407(5) Uani 1 1 d . . . . . N2 N 0.34839(16) 0.6321(2) 0.72246(13) 0.0254(5) Uani 1 1 d . . . . . C11 C 0.4108(2) 0.5582(2) 0.68563(17) 0.0262(6) Uani 1 1 d . . . . . H5 H 0.478656 0.592393 0.703951 0.031 Uiso 1 1 calc R U . . . C12 C 0.3721(2) 0.5626(3) 0.59173(17) 0.0340(7) Uani 1 1 d . . . . . H6 H 0.309814 0.519132 0.571795 0.051 Uiso 1 1 calc R U . . . H7 H 0.420503 0.525706 0.570487 0.051 Uiso 1 1 calc R U . . . H8 H 0.361831 0.645740 0.573862 0.051 Uiso 1 1 calc R U . . . C13 C 0.4178(2) 0.4265(2) 0.7163(2) 0.0356(7) Uani 1 1 d . . . . . H9 H 0.441053 0.425751 0.775345 0.053 Uiso 1 1 calc R U . . . H10 H 0.463938 0.382185 0.696283 0.053 Uiso 1 1 calc R U . . . H11 H 0.352757 0.389182 0.696330 0.053 Uiso 1 1 calc R U . . . C14 C 0.2406(2) 0.5983(3) 0.70052(18) 0.0315(7) Uani 1 1 d . . . . . H12 H 0.230943 0.525508 0.665898 0.038 Uiso 1 1 calc R U . . . C15 C 0.1734(2) 0.6969(3) 0.6487(2) 0.0444(8) Uani 1 1 d . . . . . H13 H 0.178445 0.769139 0.681172 0.067 Uiso 1 1 calc R U . . . H14 H 0.105100 0.669044 0.630267 0.067 Uiso 1 1 calc R U . . . H15 H 0.194190 0.714593 0.601852 0.067 Uiso 1 1 calc R U . . . C16 C 0.2108(2) 0.5642(3) 0.7752(2) 0.0462(8) Uani 1 1 d . . . . . H16 H 0.256774 0.504509 0.807267 0.069 Uiso 1 1 calc R U . . . H17 H 0.144122 0.531298 0.757469 0.069 Uiso 1 1 calc R U . . . H18 H 0.212816 0.635331 0.808212 0.069 Uiso 1 1 calc R U . . . C17 C 0.50554(19) 0.8327(2) 0.64023(16) 0.0245(6) Uani 1 1 d . . . . . C18 C 0.5531(2) 0.7673(3) 0.59419(17) 0.0302(6) Uani 1 1 d . . . . . H19 H 0.609184 0.720628 0.621163 0.036 Uiso 1 1 calc R U . . . C19 C 0.5190(2) 0.7703(3) 0.50944(18) 0.0345(7) Uani 1 1 d D . . . . H20 H 0.551055 0.725072 0.479529 0.041 Uiso 1 1 calc R U . . . C20 C 0.4362(2) 0.8415(3) 0.46904(16) 0.0300(6) Uani 1 1 d D . . . . C21 C 0.3884(2) 0.9090(3) 0.51400(18) 0.0353(7) Uani 1 1 d D . . . . H21 H 0.333425 0.957430 0.486982 0.042 Uiso 1 1 calc R U . . . C22 C 0.4227(2) 0.9038(3) 0.59872(17) 0.0314(6) Uani 1 1 d . . . . . H22 H 0.390230 0.948334 0.628625 0.038 Uiso 1 1 calc R U . . . C23 C 0.4005(2) 0.8424(3) 0.37956(19) 0.0386(7) Uani 1 1 d D . . . . N3 N 0.3674(2) 0.8388(3) 0.30813(17) 0.0438(9) Uani 0.845(3) 1 d D . P A 1 F1 F 0.4914(7) 0.8468(10) 0.3552(7) 0.058(4) Uani 0.155(3) 1 d D . P A 2 F2 F 0.3585(8) 0.9430(9) 0.3467(8) 0.062(4) Uani 0.155(3) 1 d D . P A 2 F3 F 0.3600(10) 0.7445(9) 0.3426(8) 0.086(6) Uani 0.155(3) 1 d D . P A 2 C24 C 0.61486(19) 0.5809(2) 0.87556(16) 0.0257(6) Uani 1 1 d . . . . . C25 C 0.6475(2) 0.4902(2) 0.83400(17) 0.0292(6) Uani 1 1 d . . . . . H23 H 0.659217 0.508737 0.785028 0.035 Uiso 1 1 calc R U . . . C26 C 0.6629(2) 0.3724(3) 0.86441(17) 0.0328(7) Uani 1 1 d D . . . . H24 H 0.683580 0.312079 0.835494 0.039 Uiso 1 1 calc R U . . . C27 C 0.6473(2) 0.3452(3) 0.93776(18) 0.0321(7) Uani 1 1 d D . . . . C28 C 0.6178(2) 0.4349(3) 0.98215(18) 0.0331(7) Uani 1 1 d D . . . . H25 H 0.609389 0.416491 1.032400 0.040 Uiso 1 1 calc R U . . . C29 C 0.6010(2) 0.5523(3) 0.95070(17) 0.0308(6) Uani 1 1 d . . . . . H26 H 0.580439 0.612510 0.979811 0.037 Uiso 1 1 calc R U . . . C30 C 0.6639(3) 0.2192(3) 0.9728(2) 0.0465(8) Uani 1 1 d D . . . . F4 F 0.6740(3) 0.1387(2) 0.92089(16) 0.0940(13) Uani 0.845(3) 1 d D . P A 1 F5 F 0.74868(18) 0.2141(2) 1.03882(15) 0.0595(8) Uani 0.845(3) 1 d D . P A 1 F6 F 0.5924(2) 0.1844(2) 1.00207(18) 0.0715(9) Uani 0.845(3) 1 d D . P A 1 N4 N 0.6489(19) 0.1107(6) 0.9808(11) 0.089(9) Uani 0.155(3) 1 d D . P A 2 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 C1 0.0314(16) 0.0322(15) 0.0262(15) -0.0013(12) 0.0057(12) -0.0113(12) C2 0.0361(16) 0.0239(14) 0.0278(15) -0.0013(11) 0.0087(13) -0.0074(12) C3 0.0358(16) 0.0232(14) 0.0257(14) -0.0042(11) 0.0115(12) -0.0057(12) C4 0.0328(16) 0.0295(15) 0.0217(14) -0.0026(11) 0.0055(12) -0.0113(12) C5 0.0249(14) 0.0328(15) 0.0231(14) -0.0009(11) 0.0063(12) -0.0055(12) C6 0.0265(15) 0.0249(14) 0.0234(14) -0.0011(11) 0.0088(12) -0.0047(11) C7 0.0285(15) 0.0237(13) 0.0212(14) -0.0014(11) 0.0086(12) -0.0022(11) C8 0.0245(14) 0.0264(14) 0.0227(14) -0.0011(11) 0.0047(11) -0.0054(11) C9 0.0404(18) 0.0430(18) 0.0257(15) -0.0027(13) 0.0071(14) -0.0142(15) N1 0.0493(18) 0.0602(19) 0.0392(16) -0.0029(14) 0.0088(14) -0.0272(15) C10 0.0271(15) 0.0274(14) 0.0246(14) 0.0005(11) 0.0080(12) -0.0032(11) O1 0.0296(11) 0.0443(13) 0.0509(14) -0.0201(10) 0.0170(10) -0.0048(9) N2 0.0231(12) 0.0266(12) 0.0265(12) -0.0036(9) 0.0077(10) -0.0034(9) C11 0.0263(14) 0.0230(14) 0.0299(15) -0.0029(11) 0.0097(12) -0.0056(11) C12 0.0377(17) 0.0318(16) 0.0322(16) -0.0071(13) 0.0110(14) -0.0075(13) C13 0.0330(16) 0.0246(15) 0.0458(18) -0.0017(13) 0.0081(14) -0.0022(12) C14 0.0244(15) 0.0350(16) 0.0344(16) -0.0102(13) 0.0086(13) -0.0072(12) C15 0.0287(17) 0.052(2) 0.0453(19) -0.0085(16) 0.0021(15) 0.0033(14) C16 0.0362(18) 0.057(2) 0.050(2) -0.0080(16) 0.0192(16) -0.0166(16) C17 0.0236(14) 0.0246(14) 0.0253(14) 0.0016(11) 0.0082(12) -0.0071(11) C18 0.0303(16) 0.0310(15) 0.0274(15) 0.0009(12) 0.0068(13) 0.0028(12) C19 0.0377(18) 0.0383(17) 0.0305(16) -0.0057(13) 0.0151(14) -0.0034(13) C20 0.0363(16) 0.0303(15) 0.0231(14) 0.0007(12) 0.0090(13) -0.0116(12) C21 0.0316(16) 0.0347(16) 0.0339(17) 0.0042(13) 0.0028(13) 0.0010(13) C22 0.0324(16) 0.0331(15) 0.0288(15) -0.0028(12) 0.0099(13) 0.0026(12) C23 0.0402(18) 0.0383(18) 0.0354(19) 0.0040(14) 0.0097(15) -0.0114(14) N3 0.045(2) 0.059(2) 0.0241(18) 0.0010(16) 0.0065(15) -0.0210(17) F1 0.079(10) 0.061(8) 0.041(7) 0.016(6) 0.027(7) 0.031(7) F2 0.038(7) 0.100(12) 0.053(8) 0.029(8) 0.019(6) 0.010(7) F3 0.110(14) 0.099(13) 0.032(8) -0.002(8) -0.003(8) -0.031(11) C24 0.0217(13) 0.0300(15) 0.0230(14) 0.0009(11) 0.0038(11) -0.0031(11) C25 0.0282(15) 0.0334(15) 0.0242(14) 0.0001(12) 0.0062(12) -0.0011(12) C26 0.0325(16) 0.0335(16) 0.0302(16) -0.0035(12) 0.0072(13) 0.0066(12) C27 0.0318(16) 0.0308(15) 0.0301(16) 0.0036(12) 0.0049(13) 0.0023(12) C28 0.0358(17) 0.0378(17) 0.0266(15) 0.0042(13) 0.0114(13) -0.0001(13) C29 0.0312(16) 0.0341(16) 0.0285(15) -0.0004(12) 0.0115(13) -0.0028(12) C30 0.056(2) 0.0370(19) 0.044(2) 0.0098(15) 0.0128(17) 0.0112(16) F4 0.208(4) 0.0247(13) 0.0486(16) -0.0003(12) 0.041(2) 0.0167(17) F5 0.0590(16) 0.0426(13) 0.0585(16) 0.0155(11) -0.0067(12) 0.0130(11) F6 0.0702(19) 0.0501(16) 0.095(2) 0.0352(15) 0.0277(17) -0.0010(13) N4 0.11(2) 0.033(13) 0.09(2) -0.006(13) -0.015(17) -0.003(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C1 C5 124.0(3) . . ? C9 C1 C4 126.9(2) . . ? C5 C1 C4 89.8(2) . . ? C9 C1 C2 125.7(2) . . ? C5 C1 C2 89.6(2) . . ? C4 C1 C2 89.4(2) . . ? C3 C2 C6 91.06(19) . . ? C3 C2 C1 89.7(2) . . ? C6 C2 C1 89.7(2) . . ? C4 C3 C2 90.7(2) . . ? C4 C3 C7 91.6(2) . . ? C2 C3 C7 90.9(2) . . ? C3 C4 C8 90.7(2) . . ? C3 C4 C1 90.2(2) . . ? C8 C4 C1 90.0(2) . . ? C6 C5 C8 92.2(2) . . ? C6 C5 C1 90.5(2) . . ? C8 C5 C1 90.0(2) . . ? C17 C6 C5 123.6(2) . . ? C17 C6 C2 124.6(2) . . ? C5 C6 C2 90.2(2) . . ? C17 C6 C7 128.6(2) . . ? C5 C6 C7 89.91(19) . . ? C2 C6 C7 88.49(19) . . ? C10 C7 C3 117.8(2) . . ? C10 C7 C6 127.5(2) . . ? C3 C7 C6 89.47(19) . . ? C10 C7 C8 132.5(2) . . ? C3 C7 C8 88.47(19) . . ? C6 C7 C8 88.28(18) . . ? C24 C8 C4 123.4(2) . . ? C24 C8 C5 124.8(2) . . ? C4 C8 C5 90.21(19) . . ? C24 C8 C7 128.3(2) . . ? C4 C8 C7 89.2(2) . . ? C5 C8 C7 89.57(19) . . ? N1 C9 C1 178.0(3) . . ? O1 C10 N2 121.9(2) . . ? O1 C10 C7 117.0(2) . . ? N2 C10 C7 121.1(2) . . ? C10 N2 C11 124.0(2) . . ? C10 N2 C14 119.0(2) . . ? C11 N2 C14 116.9(2) . . ? N2 C11 C12 112.1(2) . . ? N2 C11 C13 110.7(2) . . ? C12 C11 C13 110.7(2) . . ? N2 C14 C16 112.6(2) . . ? N2 C14 C15 111.2(2) . . ? C16 C14 C15 112.3(3) . . ? C18 C17 C22 118.5(2) . . ? C18 C17 C6 120.2(2) . . ? C22 C17 C6 121.3(2) . . ? C19 C18 C17 121.4(3) . . ? C18 C19 C20 119.4(3) . . ? C19 C20 C21 120.1(3) . . ? C19 C20 C23 118.7(3) . . ? C21 C20 C23 121.2(3) . . ? C22 C21 C20 119.7(3) . . ? C21 C22 C17 120.9(3) . . ? F3 C23 F2 115.6(7) . . ? N3 C23 C20 176.0(3) . . ? F3 C23 C20 117.5(6) . . ? F2 C23 C20 114.8(7) . . ? F3 C23 F1 100.1(6) . . ? F2 C23 F1 99.5(6) . . ? C20 C23 F1 105.4(5) . . ? C25 C24 C29 118.7(3) . . ? C25 C24 C8 121.7(2) . . ? C29 C24 C8 119.6(2) . . ? C26 C25 C24 121.0(3) . . ? C27 C26 C25 119.6(3) . . ? C26 C27 C28 120.7(3) . . ? C26 C27 C30 121.1(3) . . ? C28 C27 C30 118.1(3) . . ? C27 C28 C29 119.3(3) . . ? C28 C29 C24 120.6(3) . . ? F4 C30 F6 109.3(3) . . ? F4 C30 F5 106.5(3) . . ? F6 C30 F5 104.1(3) . . ? N4 C30 C27 159.0(11) . . ? F4 C30 C27 113.1(3) . . ? F6 C30 C27 112.4(3) . . ? F5 C30 C27 110.8(3) . . ? 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 C1 C9 1.448(4) . ? C1 C5 1.567(4) . ? C1 C4 1.570(4) . ? C1 C2 1.573(4) . ? C2 C3 1.558(4) . ? C2 C6 1.571(4) . ? C3 C4 1.549(4) . ? C3 C7 1.559(4) . ? C4 C8 1.562(4) . ? C5 C6 1.554(4) . ? C5 C8 1.563(4) . ? C6 C17 1.481(4) . ? C6 C7 1.613(4) . ? C7 C10 1.508(4) . ? C7 C8 1.613(4) . ? C8 C24 1.491(4) . ? C9 N1 1.144(4) . ? C10 O1 1.233(3) . ? C10 N2 1.355(3) . ? N2 C11 1.480(3) . ? N2 C14 1.487(3) . ? C11 C12 1.526(4) . ? C11 C13 1.532(4) . ? C14 C16 1.520(4) . ? C14 C15 1.522(4) . ? C17 C18 1.390(4) . ? C17 C22 1.393(4) . ? C18 C19 1.377(4) . ? C19 C20 1.388(4) . ? C20 C21 1.392(4) . ? C20 C23 1.454(4) . ? C21 C22 1.378(4) . ? C23 N3 1.163(4) . ? C23 F3 1.285(8) . ? C23 F2 1.294(7) . ? C23 F1 1.470(7) . ? C24 C25 1.388(4) . ? C24 C29 1.401(4) . ? C25 C26 1.387(4) . ? C26 C27 1.379(4) . ? C27 C28 1.388(4) . ? C27 C30 1.498(4) . ? C28 C29 1.390(4) . ? C30 N4 1.226(7) . ? C30 F4 1.296(4) . ? C30 F6 1.319(4) . ? C30 F5 1.356(4) . ? 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 C9 C1 C2 C3 -137.3(3) . . . . ? C5 C1 C2 C3 89.55(19) . . . . ? C4 C1 C2 C3 -0.22(19) . . . . ? C9 C1 C2 C6 131.7(3) . . . . ? C5 C1 C2 C6 -1.52(19) . . . . ? C4 C1 C2 C6 -91.29(19) . . . . ? C6 C2 C3 C4 89.9(2) . . . . ? C1 C2 C3 C4 0.2(2) . . . . ? C6 C2 C3 C7 -1.8(2) . . . . ? C1 C2 C3 C7 -91.4(2) . . . . ? C2 C3 C4 C8 -90.2(2) . . . . ? C7 C3 C4 C8 0.7(2) . . . . ? C2 C3 C4 C1 -0.2(2) . . . . ? C7 C3 C4 C1 90.7(2) . . . . ? C9 C1 C4 C3 136.5(3) . . . . ? C5 C1 C4 C3 -89.4(2) . . . . ? C2 C1 C4 C3 0.2(2) . . . . ? C9 C1 C4 C8 -132.8(3) . . . . ? C5 C1 C4 C8 1.3(2) . . . . ? C2 C1 C4 C8 90.9(2) . . . . ? C9 C1 C5 C6 -132.9(3) . . . . ? C4 C1 C5 C6 90.9(2) . . . . ? C2 C1 C5 C6 1.5(2) . . . . ? C9 C1 C5 C8 134.9(3) . . . . ? C4 C1 C5 C8 -1.3(2) . . . . ? C2 C1 C5 C8 -90.7(2) . . . . ? C8 C5 C6 C17 -138.3(2) . . . . ? C1 C5 C6 C17 131.6(2) . . . . ? C8 C5 C6 C2 88.5(2) . . . . ? C1 C5 C6 C2 -1.5(2) . . . . ? C8 C5 C6 C7 0.01(19) . . . . ? C1 C5 C6 C7 -90.02(19) . . . . ? C3 C2 C6 C17 139.4(3) . . . . ? C1 C2 C6 C17 -130.9(3) . . . . ? C3 C2 C6 C5 -88.2(2) . . . . ? C1 C2 C6 C5 1.53(19) . . . . ? C3 C2 C6 C7 1.7(2) . . . . ? C1 C2 C6 C7 91.44(19) . . . . ? C4 C3 C7 C10 137.8(2) . . . . ? C2 C3 C7 C10 -131.4(2) . . . . ? C4 C3 C7 C6 -89.02(19) . . . . ? C2 C3 C7 C6 1.7(2) . . . . ? C4 C3 C7 C8 -0.73(19) . . . . ? C2 C3 C7 C8 90.0(2) . . . . ? C17 C6 C7 C10 -11.1(4) . . . . ? C5 C6 C7 C10 -146.0(3) . . . . ? C2 C6 C7 C10 123.8(3) . . . . ? C17 C6 C7 C3 -136.6(3) . . . . ? C5 C6 C7 C3 88.5(2) . . . . ? C2 C6 C7 C3 -1.7(2) . . . . ? C17 C6 C7 C8 134.9(3) . . . . ? C5 C6 C7 C8 -0.01(19) . . . . ? C2 C6 C7 C8 -90.18(19) . . . . ? C3 C4 C8 C24 -137.9(3) . . . . ? C1 C4 C8 C24 131.9(3) . . . . ? C3 C4 C8 C5 88.8(2) . . . . ? C1 C4 C8 C5 -1.3(2) . . . . ? C3 C4 C8 C7 -0.72(19) . . . . ? C1 C4 C8 C7 -90.9(2) . . . . ? C6 C5 C8 C24 138.6(3) . . . . ? C1 C5 C8 C24 -130.9(3) . . . . ? C6 C5 C8 C4 -89.2(2) . . . . ? C1 C5 C8 C4 1.3(2) . . . . ? C6 C5 C8 C7 -0.01(19) . . . . ? C1 C5 C8 C7 90.5(2) . . . . ? C10 C7 C8 C24 6.9(4) . . . . ? C3 C7 C8 C24 134.4(3) . . . . ? C6 C7 C8 C24 -136.1(3) . . . . ? C10 C7 C8 C4 -126.7(3) . . . . ? C3 C7 C8 C4 0.72(19) . . . . ? C6 C7 C8 C4 90.23(19) . . . . ? C10 C7 C8 C5 143.0(3) . . . . ? C3 C7 C8 C5 -89.50(19) . . . . ? C6 C7 C8 C5 0.01(18) . . . . ? C3 C7 C10 O1 0.8(4) . . . . ? C6 C7 C10 O1 -112.3(3) . . . . ? C8 C7 C10 O1 117.0(3) . . . . ? C3 C7 C10 N2 178.6(2) . . . . ? C6 C7 C10 N2 65.5(4) . . . . ? C8 C7 C10 N2 -65.2(4) . . . . ? O1 C10 N2 C11 179.6(2) . . . . ? C7 C10 N2 C11 1.8(4) . . . . ? O1 C10 N2 C14 1.0(4) . . . . ? C7 C10 N2 C14 -176.7(2) . . . . ? C10 N2 C11 C12 -118.8(3) . . . . ? C14 N2 C11 C12 59.8(3) . . . . ? C10 N2 C11 C13 117.1(3) . . . . ? C14 N2 C11 C13 -64.4(3) . . . . ? C10 N2 C14 C16 -61.1(3) . . . . ? C11 N2 C14 C16 120.3(3) . . . . ? C10 N2 C14 C15 66.0(3) . . . . ? C11 N2 C14 C15 -112.6(3) . . . . ? C5 C6 C17 C18 8.0(4) . . . . ? C2 C6 C17 C18 125.6(3) . . . . ? C7 C6 C17 C18 -113.8(3) . . . . ? C5 C6 C17 C22 -171.0(2) . . . . ? C2 C6 C17 C22 -53.4(4) . . . . ? C7 C6 C17 C22 67.2(4) . . . . ? C22 C17 C18 C19 -1.1(4) . . . . ? C6 C17 C18 C19 179.8(3) . . . . ? C17 C18 C19 C20 1.0(4) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C18 C19 C20 C23 -179.3(3) . . . . ? C19 C20 C21 C22 -0.8(4) . . . . ? C23 C20 C21 C22 178.5(3) . . . . ? C20 C21 C22 C17 0.6(4) . . . . ? C18 C17 C22 C21 0.3(4) . . . . ? C6 C17 C22 C21 179.3(3) . . . . ? C19 C20 C23 F3 68.9(8) . . . . ? C21 C20 C23 F3 -110.3(8) . . . . ? C19 C20 C23 F2 -149.9(6) . . . . ? C21 C20 C23 F2 30.8(6) . . . . ? C19 C20 C23 F1 -41.5(5) . . . . ? C21 C20 C23 F1 139.3(5) . . . . ? C4 C8 C24 C25 -140.4(3) . . . . ? C5 C8 C24 C25 -22.8(4) . . . . ? C7 C8 C24 C25 99.7(3) . . . . ? C4 C8 C24 C29 38.5(4) . . . . ? C5 C8 C24 C29 156.1(3) . . . . ? C7 C8 C24 C29 -81.4(3) . . . . ? C29 C24 C25 C26 2.2(4) . . . . ? C8 C24 C25 C26 -178.8(3) . . . . ? C24 C25 C26 C27 -1.2(4) . . . . ? C25 C26 C27 C28 -1.0(4) . . . . ? C25 C26 C27 C30 -179.5(3) . . . . ? C26 C27 C28 C29 2.0(4) . . . . ? C30 C27 C28 C29 -179.5(3) . . . . ? C27 C28 C29 C24 -0.8(4) . . . . ? C25 C24 C29 C28 -1.2(4) . . . . ? C8 C24 C29 C28 179.8(3) . . . . ? C26 C27 C30 N4 -74(3) . . . . ? C28 C27 C30 N4 108(3) . . . . ? C26 C27 C30 F4 -12.7(5) . . . . ? C28 C27 C30 F4 168.7(3) . . . . ? C26 C27 C30 F6 -137.1(3) . . . . ? C28 C27 C30 F6 44.3(4) . . . . ? C26 C27 C30 F5 106.8(3) . . . . ? C28 C27 C30 F5 -71.7(4) . . . . ?