#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:00:03 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293750 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571926.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_1571926 loop_ _publ_author_name 'Biswas, Soumen' 'Empel, Claire' 'Sanchez-Palestino, Luis Mario' 'Arman, Hadi' 'Koenigs, Rene M.' 'Doyle, Michael P.' _publ_section_title ; Denitrogenative dismantling of heteroaromatics by nucleophilic substitution reactions with diazomethyl compounds. ; _journal_issue 28 _journal_name_full 'Chemical science' _journal_page_first 11065 _journal_page_last 11071 _journal_paper_doi 10.1039/d4sc01578a _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C14 H11 F3 O3' _chemical_formula_sum 'C14 H11 F3 O3' _chemical_formula_weight 284.23 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-06-02 _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2023-07-29 deposited with the CCDC. 2024-06-17 downloaded from the CCDC. ; _cell_angle_alpha 97.571(3) _cell_angle_beta 107.127(4) _cell_angle_gamma 95.412(4) _cell_formula_units_Z 2 _cell_length_a 7.1427(3) _cell_length_b 9.1744(4) _cell_length_c 9.7896(4) _cell_measurement_reflns_used 6959 _cell_measurement_temperature 100.01(11) _cell_measurement_theta_max 75.7210 _cell_measurement_theta_min 4.7990 _cell_volume 601.69(5) _computing_cell_refinement 'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(11) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.924 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 36.00 111.00 0.50 0.60 -- 106.29-125.00 150.00 150 2 \w 36.00 111.00 0.50 0.60 -- 106.29-125.00 120.00 150 3 \w 33.00 105.00 0.50 0.60 -- 106.29 -94.00 0.00 144 4 \w 33.00 105.00 0.50 0.60 -- 106.29 -94.00 120.00 144 5 \w 36.00 111.00 0.50 0.60 -- 106.29-125.00 -30.00 150 6 \w 33.00 105.00 0.50 0.60 -- 106.29 -94.00 -60.00 144 7 \w 33.00 105.00 0.50 0.60 -- 106.29 -94.00-180.00 144 8 \w 33.00 101.00 0.50 0.60 -- 106.29 -77.00-180.00 136 9 \w 33.00 71.00 0.50 0.60 -- 106.29 -61.00-120.00 76 10 \w -26.00 62.00 0.50 0.15 -- 45.90 -57.00-120.00 176 11 \w 33.00 71.00 0.50 0.60 -- 106.29 -61.00 120.00 76 12 \w -29.00 33.00 0.50 0.15 -- 45.90 -24.00 105.00 124 13 \w 92.00 178.00 0.50 0.60 -- 106.29 24.00 -90.00 172 14 \w 31.00 120.00 0.50 0.15 -- 45.90 37.00 -60.00 178 15 \w 31.00 120.00 0.50 0.15 -- 45.90 37.00 0.00 178 16 \w 32.00 122.00 0.50 0.15 -- 45.90 24.00 -90.00 180 17 \w 31.00 120.00 0.50 0.15 -- 45.90 37.00-120.00 178 18 \w 31.00 120.00 0.50 0.15 -- 45.90 37.00-150.00 178 19 \w 31.00 120.00 0.50 0.15 -- 45.90 37.00-180.00 178 20 \w -43.00 28.00 0.50 0.15 -- -45.90 37.00 -60.00 142 21 \w -33.00 30.00 0.50 0.15 -- -45.90 24.00 -90.00 126 22 \w -30.00 30.00 0.50 0.15 -- -45.90 19.00 60.00 120 23 \w -51.00 -19.00 0.50 0.60 -- -91.75 45.00 150.00 64 24 \w -101.00 -19.00 0.50 0.60 -- -91.75 77.00 60.00 164 25 \w -71.00 -19.00 0.50 0.60 -- -91.75 61.00 -30.00 104 26 \w -51.00 -19.00 0.50 0.60 -- -91.75 45.00 -30.00 64 27 \w -51.00 -19.00 0.50 0.60 -- -91.75 45.00 -90.00 64 28 \w -51.00 -19.00 0.50 0.60 -- -91.75 45.00-180.00 64 29 \w -51.00 -19.00 0.50 0.60 -- -91.75 45.00-120.00 64 30 \w -51.00 -19.00 0.50 0.60 -- -91.75 45.00 90.00 64 31 \w -85.00 -22.00 0.50 0.60 -- -91.75 125.00 150.00 126 32 \w -122.00 -31.00 0.50 0.15 -- -45.90 -24.00 105.00 182 33 \w -120.00 -31.00 0.50 0.15 -- -45.90 -37.00 30.00 178 34 \w -120.00 -31.00 0.50 0.15 -- -45.90 -37.00 -30.00 178 35 \w -120.00 -31.00 0.50 0.15 -- -45.90 -37.00 -90.00 178 36 \w -164.00 -77.00 0.50 0.60 -- -91.75 -45.00 0.00 174 37 \w -164.00 -77.00 0.50 0.60 -- -91.75 -45.00 60.00 174 38 \w -167.00 -77.00 0.50 0.60 -- -91.75 -24.00 105.00 180 39 \w -164.00-100.00 0.50 0.60 -- -91.75 -94.00 -90.00 128 40 \w -164.00-100.00 0.50 0.60 -- -91.75 -94.00-120.00 128 41 \w -164.00-100.00 0.50 0.60 -- -91.75 -94.00-150.00 128 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.2263709000 _diffrn_orient_matrix_UB_12 -0.0437319000 _diffrn_orient_matrix_UB_13 -0.0524841000 _diffrn_orient_matrix_UB_21 -0.0267797000 _diffrn_orient_matrix_UB_22 0.1638379000 _diffrn_orient_matrix_UB_23 -0.0067646000 _diffrn_orient_matrix_UB_31 0.0013897000 _diffrn_orient_matrix_UB_32 -0.0227552000 _diffrn_orient_matrix_UB_33 -0.1584312000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0211 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.924 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 9968 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.924 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.802 _diffrn_reflns_theta_min 4.795 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.220 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.569 _exptl_crystal_description plate _exptl_crystal_F_000 292 _exptl_crystal_size_max 0.119 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.091 _refine_diff_density_max 0.278 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 185 _refine_ls_number_reflns 2315 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0365 _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^)+(0.0625P)^2^+0.1901P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.1034 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2023 _reflns_number_total 2315 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01578a2.cif _cod_data_source_block hpd718_auto _cod_depositor_comments 'Adding full bibliography for 1571926--1571927.cif.' _cod_database_code 1571926 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H N O' _chemical_oxdiff_usercomment SB2-167A _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.897 _shelx_estimated_absorpt_t_min 0.868 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, H7 of C7, H5 of C5, H6 of C6, H4 of C4, H1A of C1 At 1.5 times of: All C(H,H,H) groups, H1 of C12 2.a Secondary CH2 refined with riding coordinates: C12(H12A,H12B) 2.b Aromatic/amide H refined with riding coordinates: C4(H4), C1(H1A), C7(H7), C6(H6), C5(H5) 2.c Idealised Me refined as rotating group: C13(H13A,H13B,H13C) ; _shelx_res_file ; TITL hpd718_auto_a.res in P-1 hpd718_auto.res created by SHELXL-2018/3 at 11:26:26 on 02-Jun-2023 REM Old TITL hpd718_auto in P-1 REM SHELXT solution in P-1: R1 0.117, Rweak 0.004, Alpha 0.017 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C14 O6 CELL 1.54184 7.1427 9.1744 9.7896 97.571 107.127 95.412 ZERR 2 0.0003 0.0004 0.0004 0.003 0.004 0.004 LATT 1 SFAC C H F O UNIT 28 22 6 6 L.S. 4 0 0 PLAN 5 SIZE 0.091 0.103 0.119 TEMP -173 list 4 fmap 2 53 ACTA REM REM REM WGHT 0.062500 0.190100 FVAR 0.74174 F3 3 0.424143 0.246676 0.089868 11.00000 0.02477 0.03265 = 0.02117 -0.00187 0.00198 0.00143 F2 3 0.713350 0.300982 0.073019 11.00000 0.03088 0.04200 = 0.01863 -0.00111 0.01021 0.00095 F1 3 0.652354 0.115303 0.174938 11.00000 0.05360 0.02405 = 0.02241 -0.00179 0.00378 0.01331 O3 4 0.918080 0.199107 0.692832 11.00000 0.03019 0.02057 = 0.01621 0.00168 0.00461 0.00613 O1 4 0.871351 0.578630 0.782971 11.00000 0.03055 0.02115 = 0.01499 -0.00115 0.00404 0.00467 O2 4 1.000491 0.352830 0.906660 11.00000 0.03140 0.02559 = 0.01618 0.00166 0.00465 0.00468 C2 1 0.786768 0.443300 0.548868 11.00000 0.01994 0.02116 = 0.01804 0.00156 0.00541 0.00219 C9 1 0.675842 0.354661 0.304967 11.00000 0.02176 0.02292 = 0.01803 0.00099 0.00661 0.00299 C10 1 0.859428 0.450862 0.694606 11.00000 0.02046 0.02022 = 0.01864 -0.00055 0.00591 0.00171 C11 1 0.933094 0.328786 0.775720 11.00000 0.02110 0.02133 = 0.01786 0.00128 0.00666 0.00231 C4 1 0.716412 0.714850 0.524418 11.00000 0.02444 0.02299 = 0.01847 0.00008 0.00557 0.00211 AFIX 43 H4 2 0.761778 0.752562 0.625428 11.00000 -1.20000 AFIX 0 C3 1 0.719909 0.566980 0.473535 11.00000 0.01977 0.02337 = 0.01829 0.00237 0.00613 0.00245 C1 1 0.755687 0.314682 0.435286 11.00000 0.02326 0.02177 = 0.01832 0.00033 0.00629 0.00346 AFIX 43 H1A 2 0.786682 0.218515 0.450716 11.00000 -1.20000 AFIX 0 C7 1 0.580316 0.603972 0.223955 11.00000 0.02371 0.02691 = 0.01753 0.00219 0.00529 0.00365 AFIX 43 H7 2 0.534343 0.566729 0.122851 11.00000 -1.20000 AFIX 0 C14 1 0.617722 0.254953 0.162662 11.00000 0.02488 0.02325 = 0.01811 0.00155 0.00428 0.00413 C8 1 0.651716 0.511977 0.322967 11.00000 0.02008 0.02249 = 0.01795 0.00119 0.00617 0.00210 C6 1 0.577384 0.752181 0.275810 11.00000 0.02676 0.02529 = 0.02404 0.00781 0.00771 0.00612 AFIX 43 H6 2 0.528811 0.816789 0.209348 11.00000 -1.20000 AFIX 0 C5 1 0.644848 0.806896 0.424042 11.00000 0.02787 0.02075 = 0.02530 0.00205 0.00812 0.00369 AFIX 43 H5 2 0.642056 0.908499 0.457260 11.00000 -1.20000 AFIX 0 C13 1 0.834785 0.009242 0.826519 11.00000 0.03333 0.02368 = 0.02277 0.00234 0.00774 0.00583 AFIX 137 H13A 2 0.709067 -0.018832 0.748085 11.00000 -1.50000 H13B 2 0.817156 0.081042 0.903643 11.00000 -1.50000 H13C 2 0.877761 -0.079311 0.865599 11.00000 -1.50000 AFIX 0 C12 1 0.988955 0.078096 0.768501 11.00000 0.02898 0.02167 = 0.02055 0.00426 0.00482 0.00767 AFIX 23 H12A 2 1.111447 0.116845 0.849609 11.00000 -1.20000 H12B 2 1.020829 0.001500 0.700891 11.00000 -1.20000 AFIX 0 H1 2 0.920758 0.563235 0.874202 11.00000 -1.50000 HKLF 4 REM hpd718_auto_a.res in P-1 REM wR2 = 0.1034, GooF = S = 1.056, Restrained GooF = 1.056 for all data REM R1 = 0.0365 for 2023 Fo > 4sig(Fo) and 0.0414 for all 2315 data REM 185 parameters refined using 0 restraints END WGHT 0.0597 0.2046 REM Highest difference peak 0.278, deepest hole -0.236, 1-sigma level 0.050 Q1 1 0.6879 0.5424 0.4009 11.00000 0.05 0.28 Q2 1 0.7545 0.5070 0.5197 11.00000 0.05 0.25 Q3 1 0.8127 0.4419 0.6192 11.00000 0.05 0.25 Q4 1 0.6541 0.3179 0.2424 11.00000 0.05 0.24 Q5 1 0.7126 0.3234 0.3594 11.00000 0.05 0.24 ; _shelx_res_checksum 23277 _shelx_hkl_file ; 0 0 1 0.86 0.20 0 0 -2 910.95 27.65 0 0 2 887.65 27.46 0 0 2 910.64 27.40 0 0 2 908.61 27.56 0 0 -2 898.33 27.36 0 0 -2 918.92 27.48 0 0 3 824.11 25.56 0 0 3 839.27 25.24 0 0 -3 845.49 25.46 0 0 3 817.81 25.42 0 0 -3 827.28 25.73 0 0 4 50.82 2.18 0 0 4 48.28 1.98 0 0 4 47.25 2.23 0 0 -5 317.79 9.95 0 0 -5 324.31 9.98 0 0 -5 322.90 9.97 0 0 5 298.66 10.55 0 0 -6 56.63 2.17 0 0 -6 55.03 2.17 0 0 -6 57.79 2.19 0 0 -6 52.87 2.18 0 0 -7 33.67 1.68 0 0 -7 35.56 1.71 0 0 -7 39.08 1.80 0 0 -7 38.96 1.78 0 0 -7 35.69 1.70 0 0 -8 374.00 12.09 0 0 -8 374.88 12.07 0 0 -8 402.28 12.14 0 0 -8 368.73 12.09 0 0 -8 391.52 12.16 0 0 -9 36.72 1.80 0 0 -9 36.68 1.80 0 0 -9 37.27 1.85 0 0 -9 36.61 1.78 0 0 -9 41.23 1.84 0 0 -10 31.52 1.57 0 0 -10 34.51 1.58 0 0 -10 31.79 1.54 0 0 -11 0.21 0.50 0 1 -11 0.52 0.53 0 1 -10 133.99 4.59 0 1 -10 140.57 4.68 0 1 -10 133.43 4.58 0 1 -9 160.10 5.50 0 1 -9 156.94 5.46 0 1 -9 165.55 5.56 0 1 -9 164.18 5.51 0 1 -8 1.29 0.82 0 1 -8 2.27 0.89 0 1 -8 1.14 0.89 0 1 -8 1.66 0.88 0 1 -7 172.58 5.89 0 1 -7 179.67 5.96 0 1 -7 181.86 5.94 0 1 -7 175.30 5.87 0 1 -6 145.92 4.79 0 1 -6 144.33 4.77 0 1 -6 147.82 4.78 0 1 -6 144.99 4.68 0 1 -5 102.48 3.23 0 1 -5 99.51 3.23 0 1 -4 198.79 6.18 0 -1 4 201.13 6.42 0 1 -3 317.01 10.02 0 -1 3 327.00 10.23 0 -1 3 319.85 9.87 0 1 -2 348.18 10.90 0 -1 2 356.62 10.87 0 1 -1 158.99 5.00 0 -1 1 156.55 5.01 0 -1 0 1291.79 38.52 0 1 0 1264.55 38.54 0 1 0 1257.65 38.58 0 1 1 527.40 15.74 0 1 1 524.07 15.89 0 -1 -1 508.18 15.73 0 1 1 506.68 15.76 0 -1 -1 513.57 15.62 0 1 1 509.34 15.69 0 -1 -2 1171.37 35.74 0 1 2 1175.38 35.76 0 -1 -2 1187.72 36.00 0 1 2 1199.77 36.00 0 1 2 1173.49 35.87 0 1 3 1191.79 35.90 0 -1 -3 1158.72 36.12 0 -1 -3 1178.14 35.84 0 1 3 1172.82 35.42 0 1 3 1155.68 35.84 0 -1 -4 33.91 1.73 0 1 4 36.14 1.81 0 1 4 39.55 2.16 0 -1 -4 40.34 2.31 0 1 4 37.12 1.93 0 1 5 346.50 11.65 0 1 5 351.18 11.43 0 -1 -5 351.18 10.88 0 -1 -5 344.13 10.84 0 -1 -6 9.88 0.91 0 -1 -6 7.14 0.77 0 -1 -6 7.06 0.74 0 -1 -6 9.02 0.87 0 1 6 5.55 1.20 0 -1 -6 6.78 0.82 0 -1 -6 7.75 0.73 0 -1 -7 2.26 0.83 0 -1 -7 1.45 0.73 0 -1 -7 2.16 0.85 0 -1 -7 0.84 0.79 0 -1 -7 -0.13 0.76 0 -1 -7 1.22 0.80 0 -1 -8 11.78 1.05 0 -1 -8 12.22 1.15 0 -1 -8 13.53 1.16 0 -1 -8 12.94 1.12 0 -1 -8 11.87 1.07 0 -1 -9 64.90 2.49 0 -1 -9 56.92 2.37 0 -1 -9 59.44 2.40 0 -1 -9 57.13 2.39 0 -1 -10 23.83 1.24 0 -1 -10 25.70 1.29 0 -1 -10 25.53 1.28 0 2 -11 9.88 0.83 0 2 -10 43.91 1.89 0 2 -10 46.28 2.00 0 2 -10 40.06 1.88 0 2 -9 60.49 2.55 0 2 -9 61.08 2.60 0 2 -9 66.41 2.67 0 2 -8 -0.13 0.91 0 2 -8 0.50 0.85 0 2 -8 0.08 0.83 0 2 -8 0.18 0.88 0 2 -7 0.42 0.79 0 2 -7 0.33 0.73 0 2 -7 0.43 0.69 0 2 -7 0.26 0.80 0 2 -7 -0.17 0.83 0 2 -7 -0.54 0.66 0 2 -7 0.73 0.65 0 2 -7 -0.37 0.83 0 -2 6 221.21 8.13 0 2 -6 227.49 7.22 0 2 -6 221.95 7.12 0 2 -6 227.56 7.20 0 2 -6 218.42 7.18 0 2 -6 228.34 7.24 0 2 -6 227.80 7.23 0 2 -6 222.93 7.27 0 -2 5 57.80 2.91 0 2 -5 61.06 2.17 0 2 -5 60.58 2.14 0 -2 4 1.09 0.92 0 2 -3 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19.40 1.05 4 7 -9 21.32 1.10 4 7 -8 0.35 0.71 4 7 -8 0.99 0.69 4 7 -7 9.58 0.98 4 7 -7 10.56 1.04 4 7 -7 8.19 0.91 4 7 -6 2.97 0.80 4 7 -6 2.42 0.77 -4 -7 6 2.17 0.80 4 7 -6 2.89 0.76 4 7 -5 41.88 1.88 -4 -7 5 40.85 1.96 4 7 -5 40.01 1.90 4 7 -4 2.18 0.72 -4 -7 4 1.36 0.87 -4 -7 3 37.40 1.86 4 7 -3 34.41 1.80 4 7 -3 37.25 1.76 4 7 -3 32.75 1.66 4 7 -2 24.53 1.48 4 7 -2 26.64 1.46 4 7 -2 24.18 1.31 -4 -7 1 4.25 0.87 4 7 -1 4.15 0.81 4 7 -1 3.27 0.78 4 7 0 20.30 1.25 -4 -7 0 22.32 1.30 -4 -7 -1 88.01 3.00 4 7 1 79.49 3.03 -4 -7 -2 41.81 1.82 -4 -7 -3 3.36 0.59 4 8 -8 -0.10 0.55 4 8 -8 -0.31 0.50 4 8 -7 15.79 0.99 4 8 -7 10.48 0.81 -4 -8 6 24.12 1.25 4 8 -5 59.31 2.43 -4 -8 5 60.04 2.37 -4 -8 4 12.90 1.06 4 8 -3 105.37 3.57 -4 -8 3 96.12 3.60 4 8 -2 1.32 0.67 -4 -8 1 3.10 0.70 -4 -8 0 58.98 2.21 -4 -8 -1 11.66 0.80 -4 -9 5 10.89 0.76 4 9 -5 9.49 0.80 -4 -9 4 5.41 0.65 4 9 -4 5.21 0.73 4 9 -3 62.71 2.31 -4 -9 2 14.48 0.85 -5 10 1 1.00 0.36 5 -9 -4 0.24 0.43 -5 9 3 13.95 0.85 5 -9 -2 -0.21 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-2 5.09 0.68 7 1 3 -0.56 0.43 7 2 -8 2.42 0.66 7 2 -8 1.60 0.59 7 2 -8 2.51 0.71 7 2 -7 11.51 0.93 7 2 -7 10.37 0.97 7 2 -7 12.11 1.05 7 2 -7 10.45 0.84 7 2 -7 13.43 1.13 7 2 -6 3.07 0.73 7 2 -6 3.70 0.90 7 2 -6 3.05 0.95 7 2 -5 51.93 2.26 7 2 -5 51.05 2.21 7 2 -5 57.59 2.28 7 2 -4 30.05 1.57 7 2 -4 32.79 1.58 7 2 -3 1.41 0.69 7 2 -2 32.00 1.67 -7 -2 1 14.76 1.14 7 2 -1 13.26 1.09 -7 -2 0 6.19 0.85 7 2 1 -1.23 0.70 7 2 2 1.36 0.51 7 3 -8 -0.08 0.60 7 3 -7 0.46 0.53 7 3 -7 0.53 0.82 7 3 -7 -0.07 0.64 7 3 -7 0.64 0.72 7 3 -6 2.68 0.85 7 3 -6 3.51 0.88 7 3 -6 4.10 0.69 7 3 -5 12.51 0.95 7 3 -5 10.35 1.04 7 3 -4 64.01 2.45 7 3 -4 53.43 2.26 -7 -3 3 27.72 1.48 7 3 -3 27.72 1.48 -7 -3 2 6.40 0.89 7 3 -2 6.51 0.85 -7 -3 1 3.43 0.76 -7 -3 0 107.83 3.72 -7 -3 -1 4.43 0.63 7 3 1 4.59 0.63 7 4 -8 0.77 0.58 7 4 -7 17.05 0.96 7 4 -7 16.82 1.06 7 4 -7 16.14 0.94 7 4 -6 1.39 0.70 7 4 -6 0.59 0.54 7 4 -6 0.43 0.74 -7 -4 6 0.74 0.70 7 4 -5 24.13 1.31 7 4 -5 26.49 1.34 7 4 -4 1.26 0.61 7 4 -4 0.99 0.59 -7 -4 4 1.91 0.66 -7 -4 3 -0.43 0.63 7 4 -3 0.44 0.58 -7 -4 2 5.26 0.70 7 4 -2 3.55 0.67 -7 -4 1 1.81 0.93 -7 -4 1 6.70 0.73 7 4 0 1.88 0.52 -7 -4 0 0.88 0.52 7 5 -8 1.05 0.41 7 5 -7 7.26 0.68 7 5 -6 -0.28 0.65 7 5 -5 6.60 0.65 -7 -5 5 8.75 0.78 7 5 -4 6.66 0.71 7 5 -4 5.60 0.63 -7 -5 4 6.72 0.77 7 5 -3 5.66 0.66 7 5 -3 3.89 0.58 -7 -5 2 1.60 0.57 7 5 -1 1.03 0.44 -8 6 3 65.26 2.24 8 -5 -3 0.18 0.53 8 -5 -2 55.86 2.11 8 -4 -4 0.93 0.61 8 -4 -4 1.23 0.54 8 -4 -3 1.79 0.65 8 -4 -3 1.81 0.58 -8 4 2 1.39 0.60 8 -4 -2 -0.22 0.62 8 -4 -2 1.03 0.56 8 -4 -1 2.11 0.56 -8 4 1 1.65 0.56 8 -4 -1 1.48 0.56 8 -4 0 12.27 0.82 8 -4 0 14.20 0.84 8 -3 -7 11.11 0.68 8 -3 -6 61.83 2.16 8 -3 -6 53.51 2.02 8 -3 -5 0.21 0.55 8 -3 -5 -0.08 0.57 8 -3 -4 6.38 0.78 8 -3 -3 47.11 1.97 -8 3 3 53.91 2.04 8 -3 -2 4.86 0.75 -8 3 2 6.52 0.78 -8 3 1 -0.28 0.58 -8 3 0 0.58 0.50 8 -2 -8 0.22 0.37 8 -2 -7 9.57 0.72 8 -2 -6 36.73 1.52 8 -2 -5 34.40 1.52 8 -2 -5 33.43 1.47 8 -2 -4 6.50 0.80 8 -2 -4 5.22 0.69 8 -2 -4 5.08 0.81 8 -2 -3 0.55 0.66 8 -2 -3 0.90 0.72 -8 2 3 0.86 0.68 8 -2 -2 18.44 1.13 -8 2 2 18.01 1.05 8 -2 -1 119.59 3.92 -8 2 1 118.41 3.80 8 -2 0 0.19 0.57 -8 2 0 0.69 0.55 8 -2 1 0.02 0.49 8 -1 -8 1.30 0.46 8 -1 -7 4.52 0.62 8 -1 -7 4.34 0.63 8 -1 -6 -0.08 0.57 8 -1 -6 0.88 0.61 8 -1 -5 5.01 0.75 8 -1 -5 3.83 0.71 8 -1 -4 8.51 0.92 8 -1 -4 9.48 0.84 -8 1 3 26.38 1.27 8 -1 -3 28.28 1.41 -8 1 2 10.09 0.82 8 -1 -2 9.75 0.91 -8 1 1 17.46 1.05 -8 1 1 16.80 0.99 8 -1 -1 18.64 1.11 8 -1 0 12.09 0.88 -8 1 0 11.07 0.80 -8 1 0 10.88 0.78 8 -1 0 10.26 0.75 8 0 -8 0.23 0.42 8 0 -7 6.87 0.69 8 0 -7 6.87 0.70 8 0 -7 6.95 0.65 8 0 -6 0.21 0.59 8 0 -6 -0.65 0.64 8 0 -6 -0.41 0.56 8 0 -5 -0.69 0.73 8 0 -5 1.31 0.64 8 0 -4 6.89 0.79 8 0 -4 6.17 0.81 8 0 -3 6.35 0.76 8 0 -3 7.81 0.83 8 0 -2 -0.32 0.62 -8 0 1 1.09 0.60 8 0 -1 0.30 0.51 8 0 -1 0.77 0.59 8 0 0 0.59 0.47 -8 0 0 0.59 0.52 8 1 -8 1.83 0.46 8 1 -7 0.20 0.53 8 1 -6 -0.11 0.54 8 1 -5 58.60 2.27 8 1 -5 62.73 2.36 8 1 -4 182.63 5.94 8 1 -2 6.27 0.68 8 1 -1 18.86 1.03 -8 -1 0 20.29 0.99 8 2 -7 -0.37 0.49 8 2 -6 29.85 1.29 8 2 -5 78.17 3.05 8 2 -5 99.29 3.05 8 2 -4 324.12 10.38 -8 -2 4 351.63 10.51 -8 -2 3 3.68 0.69 8 2 -2 1.16 0.50 -8 -2 2 0.38 0.55 -8 -2 1 0.63 0.48 8 3 -7 4.60 0.47 8 3 -7 5.77 0.50 8 3 -6 1.24 0.49 8 3 -5 6.95 0.61 8 3 -5 8.64 0.67 8 3 -4 35.37 1.39 0 0 0 0.00 0.00 TITL hpd718_auto in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 7.142703 9.174402 9.789558 97.5709 107.1270 95.4120 ZERR 11.00 0.000333 0.000380 0.000374 0.0033 0.0038 0.0036 LATT 1 SFAC C H N O UNIT 11.00 11.00 11.00 11.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0 TEMP -173 SIZE 0.09 0.10 0.12 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 20211 _olex2_exptl_crystal_mounting_method 'nylo loop' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.439 _oxdiff_exptl_absorpt_empirical_full_min 0.737 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 F3 F 0.42414(12) 0.24668(10) 0.08987(9) 0.0281(2) Uani 1 1 d . . . . . F2 F 0.71335(13) 0.30098(11) 0.07302(9) 0.0308(2) Uani 1 1 d . . . . . F1 F 0.65235(15) 0.11530(10) 0.17494(10) 0.0351(3) Uani 1 1 d . . . . . O3 O 0.91808(15) 0.19911(11) 0.69283(10) 0.0229(2) Uani 1 1 d . . . . . O1 O 0.87135(15) 0.57863(11) 0.78297(11) 0.0232(2) Uani 1 1 d . . . . . O2 O 1.00049(16) 0.35283(11) 0.90666(10) 0.0251(3) Uani 1 1 d . . . . . C2 C 0.7868(2) 0.44330(15) 0.54887(15) 0.0200(3) Uani 1 1 d . . . . . C9 C 0.6758(2) 0.35466(16) 0.30497(15) 0.0211(3) Uani 1 1 d . . . . . C10 C 0.8594(2) 0.45086(15) 0.69461(15) 0.0202(3) Uani 1 1 d . . . . . C11 C 0.9331(2) 0.32879(15) 0.77572(15) 0.0202(3) Uani 1 1 d . . . . . C4 C 0.7164(2) 0.71485(16) 0.52442(15) 0.0226(3) Uani 1 1 d . . . . . H4 H 0.761778 0.752562 0.625428 0.027 Uiso 1 1 calc R U . . . C3 C 0.7199(2) 0.56698(16) 0.47353(15) 0.0206(3) Uani 1 1 d . . . . . C1 C 0.7557(2) 0.31468(16) 0.43529(15) 0.0214(3) Uani 1 1 d . . . . . H1A H 0.786682 0.218515 0.450716 0.026 Uiso 1 1 calc R U . . . C7 C 0.5803(2) 0.60397(16) 0.22395(16) 0.0231(3) Uani 1 1 d . . . . . H7 H 0.534343 0.566729 0.122851 0.028 Uiso 1 1 calc R U . . . C14 C 0.6177(2) 0.25495(16) 0.16266(15) 0.0227(3) Uani 1 1 d . . . . . C8 C 0.6517(2) 0.51198(16) 0.32297(15) 0.0204(3) Uani 1 1 d . . . . . C6 C 0.5774(2) 0.75218(17) 0.27581(16) 0.0249(3) Uani 1 1 d . . . . . H6 H 0.528811 0.816789 0.209348 0.030 Uiso 1 1 calc R U . . . C5 C 0.6448(2) 0.80690(16) 0.42404(16) 0.0248(3) Uani 1 1 d . . . . . H5 H 0.642056 0.908499 0.457260 0.030 Uiso 1 1 calc R U . . . C13 C 0.8348(2) 0.00924(17) 0.82652(16) 0.0268(3) Uani 1 1 d . . . . . H13A H 0.709067 -0.018832 0.748085 0.040 Uiso 1 1 calc R U . . . H13B H 0.817156 0.081042 0.903643 0.040 Uiso 1 1 calc R U . . . H13C H 0.877761 -0.079311 0.865599 0.040 Uiso 1 1 calc R U . . . C12 C 0.9890(2) 0.07810(16) 0.76850(16) 0.0240(3) Uani 1 1 d . . . . . H12A H 1.111447 0.116845 0.849609 0.029 Uiso 1 1 calc R U . . . H12B H 1.020829 0.001500 0.700891 0.029 Uiso 1 1 calc R U . . . H1 H 0.921(3) 0.563(2) 0.874(2) 0.036 Uiso 1 1 d . 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 F3 0.0248(5) 0.0327(5) 0.0212(4) -0.0019(4) 0.0020(3) 0.0014(4) F2 0.0309(5) 0.0420(5) 0.0186(4) -0.0011(4) 0.0102(4) 0.0010(4) F1 0.0536(6) 0.0240(5) 0.0224(5) -0.0018(4) 0.0038(4) 0.0133(4) O3 0.0302(6) 0.0206(5) 0.0162(5) 0.0017(4) 0.0046(4) 0.0061(4) O1 0.0305(6) 0.0211(5) 0.0150(5) -0.0011(4) 0.0040(4) 0.0047(4) O2 0.0314(6) 0.0256(5) 0.0162(5) 0.0017(4) 0.0046(4) 0.0047(4) C2 0.0199(7) 0.0212(7) 0.0180(7) 0.0016(5) 0.0054(5) 0.0022(5) C9 0.0218(7) 0.0229(7) 0.0180(7) 0.0010(5) 0.0066(5) 0.0030(5) C10 0.0205(7) 0.0202(7) 0.0186(7) -0.0006(5) 0.0059(5) 0.0017(5) C11 0.0211(7) 0.0213(7) 0.0179(7) 0.0013(5) 0.0067(5) 0.0023(6) C4 0.0244(7) 0.0230(7) 0.0185(7) 0.0001(5) 0.0056(6) 0.0021(6) C3 0.0198(7) 0.0234(7) 0.0183(7) 0.0024(5) 0.0061(5) 0.0025(5) C1 0.0233(7) 0.0218(7) 0.0183(7) 0.0003(5) 0.0063(5) 0.0035(5) C7 0.0237(7) 0.0269(8) 0.0175(7) 0.0022(5) 0.0053(6) 0.0037(6) C14 0.0249(7) 0.0233(7) 0.0181(7) 0.0015(5) 0.0043(6) 0.0041(6) C8 0.0201(7) 0.0225(7) 0.0179(7) 0.0012(5) 0.0062(5) 0.0021(5) C6 0.0268(8) 0.0253(7) 0.0240(7) 0.0078(6) 0.0077(6) 0.0061(6) C5 0.0279(8) 0.0207(7) 0.0253(7) 0.0020(6) 0.0081(6) 0.0037(6) C13 0.0333(8) 0.0237(7) 0.0228(7) 0.0023(6) 0.0077(6) 0.0058(6) C12 0.0290(8) 0.0217(7) 0.0206(7) 0.0043(5) 0.0048(6) 0.0077(6) 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 -2 -5 0.0460 2 -2 -6 0.0515 -2 6 -2 0.0646 -2 1 6 0.0397 2 -6 1 0.0206 -1 -1 -5 0.0513 -4 -2 -1 0.0418 -1 0 6 0.0363 4 2 -2 0.0556 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 C11 O3 C12 116.11(11) . . ? C10 C2 C3 125.68(13) . . ? C10 C2 C1 128.29(13) . . ? C1 C2 C3 106.03(12) . . ? C1 C9 C14 125.65(13) . . ? C1 C9 C8 110.30(12) . . ? C8 C9 C14 124.04(13) . . ? O1 C10 C2 119.83(13) . . ? O1 C10 C11 112.72(12) . . ? C2 C10 C11 127.45(13) . . ? O3 C11 C10 114.78(12) . . ? O2 C11 O3 124.91(13) . . ? O2 C11 C10 120.32(12) . . ? C3 C4 C5 118.54(13) . . ? C4 C3 C2 132.02(13) . . ? C4 C3 C8 120.25(13) . . ? C8 C3 C2 107.72(12) . . ? C9 C1 C2 108.98(13) . . ? C8 C7 C6 118.54(13) . . ? F3 C14 F2 105.18(11) . . ? F3 C14 C9 112.36(12) . . ? F2 C14 C9 112.77(12) . . ? F1 C14 F3 106.54(12) . . ? F1 C14 F2 106.73(11) . . ? F1 C14 C9 112.71(12) . . ? C3 C8 C9 106.96(12) . . ? C7 C8 C9 132.17(13) . . ? C7 C8 C3 120.88(13) . . ? C7 C6 C5 120.77(13) . . ? C6 C5 C4 121.02(13) . . ? O3 C12 C13 110.74(12) . . ? 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 F3 C14 1.3457(17) . ? F2 C14 1.3458(17) . ? F1 C14 1.3416(17) . ? O3 C11 1.3250(17) . ? O3 C12 1.4627(17) . ? O1 C10 1.3417(17) . ? O2 C11 1.2106(17) . ? C2 C10 1.357(2) . ? C2 C3 1.4747(19) . ? C2 C1 1.4620(19) . ? C9 C1 1.350(2) . ? C9 C14 1.4838(19) . ? C9 C8 1.4634(19) . ? C10 C11 1.504(2) . ? C4 C3 1.387(2) . ? C4 C5 1.394(2) . ? C3 C8 1.414(2) . ? C7 C8 1.385(2) . ? C7 C6 1.392(2) . ? C6 C5 1.393(2) . ? C13 C12 1.505(2) . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.1518 -2.4762 -5.2959 -0.1009 -0.4275 0.8984 1.9920 -1.8040 -5.7062 -0.0726 -0.3103 0.9479 -1.6561 5.5055 -1.8467 0.2311 0.9588 0.1650 -1.6973 0.7656 6.1313 0.0289 0.1294 -0.9912 1.9355 -5.5862 0.7630 -0.2339 -0.9722 0.0089 -0.9683 -1.1703 -5.0965 0.5379 -0.1313 0.8327 -3.6494 -2.0393 -0.8132 0.9580 -0.2309 0.1702 -0.5844 0.4755 6.0913 -0.2082 0.0524 -0.9767 4.2205 1.9258 -2.4151 -0.9129 0.2188 0.3447