#------------------------------------------------------------------------------ #$Date: 2024-07-12 01:06:49 +0300 (Fri, 12 Jul 2024) $ #$Revision: 293371 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572123.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_1572123 loop_ _publ_author_name 'Seki, Tomohiro' 'Kobayashi, Shiori' 'Ishikawa, Rintaro' 'Yano, Keigo' 'Matsuo, Takumi' 'Hayashi, Shotaro' _publ_section_title ; Preparation of intrinsically fragile bent crystals ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02918F _journal_year 2024 _chemical_formula_moiety 'C15 H12 F3 N O2' _chemical_formula_sum 'C15 H12 F3 N O2' _chemical_formula_weight 295.26 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-12-04 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-04-24 deposited with the CCDC. 2024-07-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 12.3091(2) _cell_length_b 5.07340(10) _cell_length_c 41.7053(4) _cell_measurement_reflns_used 24943 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 76.9450 _cell_measurement_theta_min 2.0780 _cell_volume 2604.45(7) _computing_cell_refinement 'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)' _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_environment N~2~ _diffrn_ambient_temperature 173.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.985 _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 37.00 106.00 0.50 0.16 -- 107.12 -99.00 90.00 138 2 \w 37.00 106.00 0.50 0.16 -- 107.12 -99.00 60.00 138 3 \w 38.00 112.00 0.50 0.16 -- 107.12-125.00 -30.00 148 4 \w 37.00 106.00 0.50 0.16 -- 107.12 -99.00-120.00 138 5 \w 19.00 93.00 0.50 0.05 -- 47.44-125.00 -90.00 148 6 \w 37.00 106.00 0.50 0.16 -- 107.12 -99.00 90.00 138 7 \w 35.00 109.00 0.50 0.16 -- 107.12 -77.00 120.00 148 8 \w 35.00 69.00 0.50 0.16 -- 107.12 -57.00 90.00 68 9 \w 35.00 69.00 0.50 0.16 -- 107.12 -57.00 30.00 68 10 \w 35.00 69.00 0.50 0.16 -- 107.12 -57.00 -30.00 68 11 \w -27.00 30.00 0.50 0.05 -- 47.44 -19.00 0.00 114 12 \w 35.00 69.00 0.50 0.16 -- 107.12 -57.00-120.00 68 13 \w 35.00 69.00 0.50 0.16 -- 107.12 -57.00 -90.00 68 14 \w 94.00 178.00 0.50 0.16 -- 107.12 38.00-150.00 168 15 \w 92.00 178.00 0.50 0.16 -- 107.12 57.00 90.00 172 16 \w 85.00 178.00 0.50 0.16 -- 107.12 77.00 150.00 186 17 \w 85.00 178.00 0.50 0.16 -- 107.12 77.00 150.00 186 18 \w 25.00 120.00 0.50 0.05 -- 47.44 77.00 -60.00 190 19 \w 25.00 120.00 0.50 0.05 -- 47.44 77.00-120.00 190 20 \w 25.00 120.00 0.50 0.05 -- 47.44 77.00-180.00 190 21 \w -23.00 28.00 0.50 0.05 -- -47.44 19.00 -90.00 102 22 \w -39.00 26.00 0.50 0.05 -- -47.44 38.00-120.00 130 23 \w -62.00 25.00 0.50 0.05 -- -47.44 57.00-150.00 174 24 \w -39.00 26.00 0.50 0.05 -- -47.44 38.00 0.00 130 25 \w -62.00 -32.00 0.50 0.16 -- -104.50 57.00-120.00 60 26 \w -62.00 -32.00 0.50 0.16 -- -104.50 57.00 -90.00 60 27 \w -107.00 -34.00 0.50 0.16 -- -104.50 104.00-155.00 146 28 \w -111.00 -35.00 0.50 0.16 -- -104.50 125.00 -60.00 152 29 \w -111.00 -35.00 0.50 0.16 -- -104.50 125.00 120.00 152 30 \w -174.00 -91.00 0.50 0.16 -- -104.50 -38.00 -30.00 166 31 \w -174.00 -91.00 0.50 0.16 -- -104.50 -38.00 -30.00 166 32 \w -174.00 -89.00 0.50 0.16 -- -104.50 -57.00 120.00 170 33 \w -174.00 -91.00 0.50 0.16 -- -104.50 -49.00 38.40 166 34 \w -174.00-106.00 0.50 0.16 -- -104.50 -51.00 -50.71 136 35 \w -174.00 -89.00 0.50 0.16 -- -104.50 -57.00-180.00 170 36 \w -120.00 -34.00 0.50 0.05 -- -47.44 -38.00-180.00 172 37 \w -119.00 -25.00 0.50 0.05 -- -47.44 -77.00 30.00 188 38 \w -119.00 -32.00 0.50 0.05 -- -47.44 -57.00 60.00 174 39 \w -120.00 -34.00 0.50 0.05 -- -47.44 -38.00 90.00 172 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0310431000 _diffrn_orient_matrix_UB_12 -0.0313673000 _diffrn_orient_matrix_UB_13 -0.1416575000 _diffrn_orient_matrix_UB_21 -0.1203999000 _diffrn_orient_matrix_UB_22 0.0058995000 _diffrn_orient_matrix_UB_23 0.0670075000 _diffrn_orient_matrix_UB_31 -0.0141180000 _diffrn_orient_matrix_UB_32 0.0185781000 _diffrn_orient_matrix_UB_33 -0.2602354000 _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 0.0464 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_number 45890 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.721 _diffrn_reflns_theta_min 2.119 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet R (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.506 _exptl_crystal_description needle _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.259 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.043 _refine_ls_abs_structure_details ; Flack x determined using 2351 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 386 _refine_ls_number_reflns 5415 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0406 _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^)+(0.0540P)^2^+1.1426P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1075 _refine_ls_wR_factor_ref 0.1087 _reflns_Friedel_coverage 0.946 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.959 _reflns_number_gt 5152 _reflns_number_total 5415 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02918f3.cif _cod_data_source_block kby-ffa4ch3-y_auto _cod_database_code 1572123 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHONF _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 N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: N00A(H00A), N00C(H00C), C00D(H00D), C00G(H00G), C00M(H00M), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013) 2.b Idealised Me refined as rotating group: C014(H01D,H01E,H01F), C015(H01A,H01B,H01C) 2.c Idealised tetrahedral OH refined as rotating group: O007(H007) ; _shelx_res_file ; TITL kby-ffa4ch3-y_auto_a.res in Pna2(1) kby-ffa4ch3-y_auto.res created by SHELXL-2018/3 at 12:39:39 on 04-Dec-2023 REM Old TITL kby-ffa4ch3-y_auto_a.res in Pna2(1) REM SHELXT solution in Pna2(1): R1 0.114, Rweak 0.004, Alpha 0.002 REM 0.833 for 463 systematic absences, Orientation as input REM Flack x = 0.142 ( 0.053 ) from 2397 Parsons' quotients REM Formula found by SHELXT: C30 F7 N2 O3 CELL 1.54184 12.3091 5.0734 41.7053 90 90 90 ZERR 8 0.0002 0.0001 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H F N O UNIT 120 96 24 8 16 L.S. 10 PLAN 10 TEMP -100 CONF list 4 fmap 2 ACTA MORE -1 BOND $H REM REM REM WGHT 0.054000 1.142600 FVAR 0.39506 F001 3 0.406451 0.741312 0.267219 11.00000 0.06799 0.06215 = 0.02894 0.00511 0.00367 0.00634 O8 5 0.479696 0.759563 0.498770 11.00000 0.03982 0.03363 = 0.02614 0.00490 -0.00502 -0.00809 O003 5 0.410584 0.361542 0.534047 11.00000 0.03730 0.03428 = 0.02846 0.00504 -0.00119 -0.00706 O004 5 0.345111 0.635825 0.466101 11.00000 0.03815 0.03268 = 0.02725 0.00388 -0.00111 -0.00639 F005 3 0.242311 0.593475 0.709621 11.00000 0.04837 0.06193 = 0.06038 -0.00957 0.01414 0.01178 F006 3 0.509895 0.458582 0.289205 11.00000 0.05586 0.07019 = 0.05324 0.00036 0.01378 0.02009 O007 5 0.277059 0.237658 0.501515 11.00000 0.04203 0.03385 = 0.02599 0.00557 -0.00560 -0.00640 AFIX 147 H007 2 0.300171 0.366999 0.490951 11.00000 -1.50000 AFIX 0 F008 3 0.219211 0.185748 0.698412 11.00000 0.07006 0.08477 = 0.04847 -0.02313 0.02664 -0.04272 F009 3 0.340996 0.301854 0.732230 11.00000 0.07394 0.07611 = 0.02677 0.00621 0.00789 0.00136 N00A 4 0.413652 0.157167 0.593201 11.00000 0.03176 0.03113 = 0.02511 0.00153 0.00164 -0.00281 AFIX 43 H00A 2 0.463211 0.196414 0.578762 11.00000 -1.20000 AFIX 0 F00B 3 0.525096 0.867492 0.300876 11.00000 0.08063 0.09677 = 0.04605 -0.01825 0.02387 -0.04922 N00C 4 0.340357 0.845572 0.407289 11.00000 0.03357 0.03220 = 0.02406 0.00096 0.00230 -0.00449 AFIX 43 H00C 2 0.291849 0.801390 0.421828 11.00000 -1.20000 AFIX 0 C00D 1 0.392856 0.773188 0.350688 11.00000 0.03272 0.02915 = 0.02395 -0.00022 -0.00163 -0.00183 AFIX 43 H00D 2 0.454152 0.885954 0.352535 11.00000 -1.20000 AFIX 0 C00E 1 0.424162 0.778373 0.471641 11.00000 0.02984 0.02420 = 0.02575 0.00096 0.00121 -0.00017 C00F 1 0.323292 0.741106 0.376554 11.00000 0.03083 0.02493 = 0.02674 0.00257 -0.00360 0.00376 C00G 1 0.465172 1.212687 0.398539 11.00000 0.03949 0.02259 = 0.02648 0.00144 0.00195 0.00372 AFIX 43 H00G 2 0.436175 1.240108 0.377695 11.00000 -1.20000 AFIX 0 C00H 1 0.331549 0.219075 0.528611 11.00000 0.03607 0.02590 = 0.02271 -0.00116 0.00227 0.00278 C00I 1 0.330853 -0.005546 0.582760 11.00000 0.02919 0.02416 = 0.02722 -0.00023 0.00272 0.00390 C00J 1 0.289714 0.018448 0.550935 11.00000 0.03084 0.02150 = 0.02693 -0.00120 0.00226 0.00228 C00K 1 0.422709 1.007929 0.417822 11.00000 0.03055 0.02239 = 0.02859 -0.00128 0.00341 0.00381 C00L 1 0.376343 0.392073 0.677500 11.00000 0.03454 0.02968 = 0.02698 0.00356 0.00015 0.00318 C00M 1 0.206519 -0.150533 0.540640 11.00000 0.03188 0.03102 = 0.02818 -0.00102 0.00019 0.00088 AFIX 43 H00M 2 0.178990 -0.133587 0.519459 11.00000 -1.20000 AFIX 0 C00N 1 0.464846 0.982323 0.449257 11.00000 0.03319 0.02303 = 0.02655 0.00084 0.00295 0.00199 C00O 1 0.452802 0.677485 0.295063 11.00000 0.04551 0.04678 = 0.03012 -0.00397 0.00259 -0.00381 C00P 1 0.546966 1.371884 0.409231 11.00000 0.03999 0.02269 = 0.03546 0.00146 0.00709 0.00090 AFIX 43 H00P 2 0.574385 1.506247 0.395585 11.00000 -1.20000 AFIX 0 C00Q 1 0.429721 0.269019 0.623789 11.00000 0.02953 0.02811 = 0.02362 0.00287 -0.00143 0.00269 C00R 1 0.463858 0.563081 0.680758 11.00000 0.03422 0.03252 = 0.03023 -0.00060 -0.00259 0.00263 C00S 1 0.535496 0.577374 0.654709 11.00000 0.03075 0.03795 = 0.03738 -0.00107 -0.00279 -0.00371 AFIX 43 H00S 2 0.597163 0.689339 0.656154 11.00000 -1.20000 AFIX 0 C00T 1 0.163881 -0.340685 0.560624 11.00000 0.03738 0.02900 = 0.03822 -0.00333 0.00419 -0.00451 AFIX 43 H00T 2 0.106326 -0.450910 0.553516 11.00000 -1.20000 AFIX 0 C00U 1 0.233958 0.574105 0.372769 11.00000 0.03310 0.03696 = 0.03027 0.00111 0.00104 -0.00186 AFIX 43 H00U 2 0.184248 0.552698 0.389998 11.00000 -1.20000 AFIX 0 C00V 1 0.206322 -0.368824 0.591330 11.00000 0.03623 0.02404 = 0.03658 0.00315 0.00752 -0.00027 AFIX 43 H00V 2 0.178528 -0.502413 0.605023 11.00000 -1.20000 AFIX 0 C00W 1 0.288516 -0.205209 0.602300 11.00000 0.03522 0.02377 = 0.02926 -0.00008 0.00260 0.00306 AFIX 43 H00W 2 0.316477 -0.228813 0.623336 11.00000 -1.20000 AFIX 0 C00X 1 0.285756 0.467965 0.317932 11.00000 0.03884 0.03416 = 0.03088 -0.00271 -0.00588 0.00223 C00Y 1 0.591179 1.340756 0.439938 11.00000 0.03828 0.03079 = 0.03520 -0.00151 0.00179 -0.00680 AFIX 43 H00Y 2 0.648953 1.450173 0.447076 11.00000 -1.20000 AFIX 0 C00Z 1 0.519234 0.433842 0.627022 11.00000 0.03048 0.03460 = 0.03175 0.00255 0.00160 -0.00045 AFIX 43 H00Z 2 0.569928 0.447875 0.609932 11.00000 -1.20000 AFIX 0 C010 1 0.373097 0.639930 0.321835 11.00000 0.03497 0.03198 = 0.02590 0.00123 -0.00231 0.00305 C011 1 0.357773 0.246616 0.649736 11.00000 0.03163 0.02638 = 0.03098 0.00229 0.00076 -0.00087 AFIX 43 H011 2 0.296684 0.132739 0.648365 11.00000 -1.20000 AFIX 0 C012 1 0.216575 0.439487 0.344423 11.00000 0.03361 0.03725 = 0.03816 -0.00327 -0.00131 -0.00512 AFIX 43 H012 2 0.155977 0.324260 0.342837 11.00000 -1.20000 AFIX 0 C013 1 0.548844 1.147287 0.459606 11.00000 0.03462 0.02836 = 0.03268 -0.00196 -0.00072 -0.00159 AFIX 43 H013 2 0.577390 1.125829 0.480608 11.00000 -1.20000 AFIX 0 C014 1 0.486371 0.729797 0.710032 11.00000 0.04322 0.04800 = 0.03358 -0.00567 -0.00221 -0.00509 AFIX 137 H01D 2 0.418773 0.756300 0.722020 11.00000 -1.50000 H01E 2 0.515424 0.901039 0.703347 11.00000 -1.50000 H01F 2 0.539519 0.640187 0.723717 11.00000 -1.50000 AFIX 0 C015 1 0.262337 0.313629 0.287678 11.00000 0.04527 0.04983 = 0.03884 -0.01292 -0.00558 -0.00074 AFIX 137 H01A 2 0.230940 0.431360 0.271517 11.00000 -1.50000 H01B 2 0.210851 0.171669 0.292476 11.00000 -1.50000 H01C 2 0.330048 0.237871 0.279441 11.00000 -1.50000 AFIX 0 C016 1 0.295002 0.366749 0.704247 11.00000 0.04361 0.04409 = 0.03283 -0.00537 0.00535 -0.00304 H8 2 0.455903 0.609536 0.511335 11.00000 0.06512 HKLF 4 REM kby-ffa4ch3-y_auto_a.res in Pna2(1) REM wR2 = 0.1087, GooF = S = 1.072, Restrained GooF = 1.072 for all data REM R1 = 0.0406 for 5152 Fo > 4sig(Fo) and 0.0422 for all 5415 data REM 386 parameters refined using 1 restraints END WGHT 0.0540 1.1427 REM Highest difference peak 0.259, deepest hole -0.308, 1-sigma level 0.043 Q1 1 0.3299 0.6859 0.4215 11.00000 0.05 0.26 Q2 1 0.4230 0.3006 0.5796 11.00000 0.05 0.25 Q3 1 0.3523 0.8055 0.4688 11.00000 0.05 0.21 Q4 1 0.2436 0.8910 0.7098 11.00000 0.05 0.19 Q5 1 0.2016 -0.3004 0.5425 11.00000 0.05 0.17 Q6 1 0.4070 0.1939 0.5311 11.00000 0.05 0.17 Q7 1 0.5222 0.0686 0.6290 11.00000 0.05 0.17 Q8 1 0.3771 0.2820 0.6305 11.00000 0.05 0.16 Q9 1 0.4668 0.9509 0.6807 11.00000 0.05 0.16 Q10 1 0.5388 1.2092 0.4014 11.00000 0.05 0.16 ; _shelx_res_checksum 67787 _shelx_hkl_file ; 0 -1 0 7.70 0.95 0 1 0 -0.41 0.47 0 2 0 2761.14 90.15 0 2 0 2681.15 90.60 0 -2 0 2877.46 91.26 0 2 0 2933.60 91.06 0 -2 0 2847.95 90.72 0 3 0 2.80 1.95 0 -3 0 8.07 1.67 0 3 0 2.24 1.71 0 4 0 15.96 2.35 0 -4 0 14.26 1.52 0 -4 0 17.14 1.57 0 -4 0 16.95 1.74 0 -4 0 16.01 2.14 0 -4 0 15.19 1.55 0 -5 0 -0.13 0.75 0 -5 0 -0.21 0.98 0 -6 0 -1.23 0.80 0 -1 -1 2046.75 82.92 0 -1 1 2009.67 82.97 0 1 1 1978.81 82.42 0 -1 -1 2008.01 82.82 0 -1 1 2006.74 82.71 0 1 1 1948.65 82.73 0 1 1 2147.39 82.90 0 2 -1 76.05 2.26 0 -2 1 211.32 5.97 0 3 1 392.19 18.52 0 3 -1 416.75 18.68 0 -3 -1 407.67 18.28 0 -3 1 426.66 18.21 0 3 -1 392.22 18.09 0 3 1 389.26 18.03 0 -4 1 0.07 0.92 0 -4 -1 -0.80 0.99 0 -4 -1 -0.28 0.79 0 -4 1 0.28 0.81 0 -4 -1 1.17 1.11 0 -4 1 0.15 0.96 0 -4 -1 -0.17 0.60 0 4 1 -1.48 1.62 0 4 -1 -1.14 1.64 0 -4 -1 0.32 0.94 0 -4 -1 -0.74 1.02 0 -4 1 0.75 1.01 0 -4 1 1.00 1.00 0 -5 -1 5.86 1.27 0 -5 1 6.89 1.23 0 -5 -1 3.65 0.91 0 -5 1 5.11 0.90 0 -5 -1 11.07 1.33 0 -5 1 13.18 1.39 0 -5 -1 8.31 1.20 0 -6 -1 13.88 1.10 0 -6 1 -0.33 0.76 0 0 2 2.27 0.22 0 0 2 2.07 0.26 0 0 2 1.97 0.26 0 1 2 0.63 0.40 0 1 2 0.93 0.84 0 -1 -2 0.87 0.84 0 -1 2 0.82 0.89 0 -1 2 0.44 0.43 0 -1 -2 0.16 0.33 0 1 2 -0.48 0.42 0 1 2 0.45 0.79 0 -1 -2 0.54 0.58 0 -1 2 0.15 0.50 0 -2 -2 58.74 3.40 0 -2 2 61.13 3.23 0 2 -2 48.13 2.54 0 -2 -2 57.67 3.65 0 -2 2 59.40 3.73 0 -2 2 51.20 2.57 0 2 2 60.87 3.32 0 2 -2 53.96 3.35 0 2 2 57.81 2.67 0 2 2 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6 972.70 42.36 -2 1 6 1091.76 41.84 2 -1 -6 1024.52 42.18 2 1 6 1029.67 41.86 -2 1 6 968.55 42.34 2 -1 6 1004.77 42.01 2 1 -6 921.83 41.74 -2 -1 -6 995.67 42.35 -2 -1 6 1032.44 42.24 -2 -1 6 1072.59 42.51 2 -1 6 989.93 42.44 -2 -1 -6 1085.84 41.74 -2 -1 -6 1027.18 41.69 2 1 -6 1018.42 42.47 2 -1 -6 989.89 41.71 2 1 6 1023.24 42.10 2 1 -6 962.73 41.98 -2 2 6 134.49 6.43 -2 -2 6 133.92 6.63 -2 -2 6 139.15 6.64 -2 -2 6 156.28 7.66 -2 2 -6 140.77 6.98 -2 2 6 146.79 6.87 -2 -2 -6 145.20 6.76 -2 2 6 159.88 6.75 2 2 6 159.97 7.60 2 -2 6 138.98 6.49 -2 -2 6 137.03 6.47 2 -2 6 139.50 6.26 2 2 -6 141.67 6.53 2 -2 -6 142.83 7.27 2 2 6 148.36 6.66 2 2 -6 148.53 7.34 -2 2 6 142.89 7.31 2 -2 -6 150.01 7.06 2 2 6 148.97 6.56 -2 3 -6 94.24 5.91 -2 3 6 82.67 5.47 -2 -3 -6 88.49 5.65 2 -3 -6 96.07 5.59 -2 -3 -6 87.12 4.38 2 -3 -6 88.94 5.15 -2 -3 6 95.12 6.10 2 3 -6 89.22 5.33 2 -3 6 82.69 4.42 2 -3 6 87.39 4.30 2 -3 -6 83.44 4.40 2 3 6 93.19 5.79 -2 3 6 93.15 4.90 -2 3 -6 82.80 5.15 2 3 -6 92.84 6.15 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-8 2.88 1.51 -2 -3 -8 4.28 0.92 -2 -3 -8 4.31 0.99 2 -3 -8 3.91 1.10 -2 -3 8 3.63 1.85 -2 -3 8 3.43 1.02 -2 -3 8 4.13 1.00 -2 -3 -8 3.45 0.90 2 -3 8 3.53 0.99 -2 3 8 3.51 1.08 2 3 -8 2.71 1.52 2 3 8 4.78 1.61 -2 3 -8 3.04 1.15 2 -4 8 30.85 2.24 -2 -4 -8 34.58 2.41 2 -4 8 32.52 2.46 2 -4 8 32.01 2.25 -2 -4 -8 32.35 2.31 -2 -4 8 32.83 2.22 -2 -4 -8 32.73 2.36 -2 -4 8 32.27 2.09 2 -4 8 37.87 2.24 -2 -4 -8 31.86 3.56 2 -4 -8 37.68 3.60 -2 -4 8 30.69 2.40 -2 -4 -8 40.82 2.50 2 -4 8 35.37 2.51 -2 -4 8 33.87 3.99 -2 4 -8 30.51 3.38 -2 4 8 35.48 3.42 2 4 -8 24.61 3.51 2 -4 -8 30.51 2.37 2 4 8 34.97 3.57 2 -4 -8 29.62 2.21 2 -4 8 30.50 2.24 2 -4 8 29.41 2.31 2 -4 -8 33.11 2.40 -2 -4 -8 31.72 2.20 2 -4 8 32.71 2.29 -2 -4 8 32.45 2.40 2 -4 8 31.82 1.92 -2 -4 8 31.08 2.21 -2 -4 -8 32.84 2.38 -2 -4 -8 37.16 2.54 -2 -4 8 30.29 2.29 -2 -5 -8 15.65 1.54 -2 -5 8 14.87 1.40 2 -5 -8 15.45 1.58 2 -5 -8 17.18 1.58 2 -5 8 10.91 1.36 -2 -5 8 18.97 1.74 2 -5 8 17.14 1.58 -2 -5 -8 17.72 1.43 2 -5 -8 23.56 1.62 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1.30 -2 -4 -9 11.15 1.39 -2 -4 9 10.69 1.26 -2 -4 9 8.83 1.27 2 -4 9 10.26 0.97 2 -4 -9 7.28 1.20 2 -4 9 6.71 1.21 2 -4 9 8.45 1.28 2 -5 -9 62.60 3.66 -2 -5 9 71.25 3.57 -2 -5 9 75.36 4.00 2 -5 9 78.45 3.79 -2 -5 9 68.83 3.82 -2 -5 -9 70.47 3.75 2 -5 -9 61.49 3.65 2 -5 -9 66.66 3.57 2 -5 9 61.76 3.52 -2 -5 9 75.25 3.69 -2 -5 -9 70.42 3.72 -2 -6 9 4.21 0.76 -2 -6 9 5.89 0.73 -2 -6 -9 4.14 0.57 -2 0 10 18.11 1.70 2 0 10 16.55 1.38 -2 0 -10 15.58 1.30 2 0 10 19.71 1.72 -2 0 10 18.16 1.48 2 0 -10 18.72 1.68 -2 0 -10 19.25 1.50 -2 0 10 19.73 1.83 2 0 10 19.21 1.21 2 0 -10 16.99 1.69 -2 -1 -10 680.43 27.00 2 -1 -10 655.64 27.55 2 -1 -10 639.44 26.84 2 1 10 627.88 27.21 2 1 -10 614.88 27.26 -2 -1 -10 635.02 27.45 -2 1 10 627.58 27.41 -2 1 -10 630.22 27.34 -2 1 10 661.02 27.02 2 1 10 629.06 27.38 -2 -1 -10 649.15 27.52 2 1 10 642.80 27.16 2 -1 10 653.08 27.52 -2 -1 10 627.47 27.48 2 1 10 640.65 27.07 2 -1 -10 658.74 27.43 -2 1 10 655.47 27.48 -2 -1 10 630.91 27.49 -2 1 10 705.96 27.67 -2 1 10 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-14 2 4 28.32 1.68 14 -2 -4 26.28 1.57 -14 -2 4 26.20 1.50 14 -2 4 25.61 1.56 14 -2 4 25.46 1.75 14 -2 4 26.15 1.78 -14 2 4 30.51 1.63 14 -2 -4 26.30 1.67 -14 -2 -4 30.79 1.76 -14 -2 4 27.89 1.75 14 0 -5 2.73 0.93 -14 0 -5 2.79 0.77 -14 0 -5 3.74 0.91 14 0 5 4.13 0.83 14 -1 5 9.32 1.18 14 1 -5 6.68 0.92 -14 -1 -5 8.30 1.08 -14 -1 5 9.53 1.13 -14 1 5 8.21 0.91 -14 -1 -5 10.02 1.05 14 -1 -5 8.80 1.16 14 -1 5 9.60 1.21 14 1 5 7.01 0.89 -14 1 5 6.86 0.97 -14 2 5 21.75 1.44 14 -2 -5 22.01 1.37 -14 -2 5 18.08 1.27 14 -2 5 22.81 1.41 -14 -2 -5 23.10 1.52 -14 -2 5 20.79 1.51 14 -2 5 24.40 1.59 14 -2 5 18.80 1.52 14 -2 -5 21.97 1.49 -14 2 5 22.68 1.37 -14 0 -6 11.82 1.08 14 0 -6 11.31 1.24 -14 0 -6 12.04 1.21 14 0 6 9.86 1.09 14 -1 6 1.62 0.84 14 1 -6 -0.07 0.59 14 -1 -6 0.63 0.83 -14 -1 -6 0.63 0.74 -14 -1 6 0.25 0.70 -14 -1 -6 1.17 0.72 -14 1 -6 2.39 0.81 14 -1 6 0.99 0.82 -14 1 6 0.04 0.66 14 1 6 1.58 0.67 -14 2 6 16.70 1.24 14 -2 6 15.93 1.34 14 -2 6 16.44 1.32 -14 -2 -6 16.22 1.28 -14 -2 6 18.88 1.33 14 -2 -6 17.02 1.13 -14 -2 6 16.21 1.13 14 -2 6 15.62 1.16 14 -2 -6 17.12 1.29 -14 2 6 15.97 1.11 14 0 -7 1.01 0.83 -14 0 -7 0.04 0.61 -14 0 -7 2.42 0.87 14 0 7 0.83 0.70 -14 -1 7 12.94 1.08 14 -1 7 9.33 1.16 14 -1 7 10.32 1.18 14 -1 -7 16.88 1.39 -14 -1 -7 14.76 1.26 -14 -1 7 12.50 1.20 -14 1 -7 13.81 1.30 14 1 -7 10.38 1.00 -14 -1 -7 14.11 1.20 -14 1 7 11.52 1.11 14 1 7 13.52 1.07 14 -2 7 5.10 0.69 14 -2 -7 5.90 0.70 -14 -2 7 4.15 0.65 14 -2 7 5.13 0.85 14 -2 -7 3.78 0.73 14 -2 7 5.12 0.88 -14 -2 -7 4.71 0.78 -14 -2 7 3.68 0.78 -14 2 7 5.15 0.76 -14 -2 7 5.05 0.73 14 0 -8 12.40 1.29 -14 0 -8 12.63 1.13 -14 0 -8 12.54 1.25 14 0 8 13.95 1.22 -14 -1 8 3.08 0.70 14 -1 8 3.26 0.83 14 -1 8 3.53 0.86 14 1 -8 2.05 0.62 14 -1 -8 2.86 0.86 -14 -1 -8 1.83 0.77 -14 -1 8 3.97 0.81 -14 -1 -8 3.75 0.79 -14 1 8 2.91 0.71 14 1 8 2.74 0.68 -14 2 8 10.07 0.93 14 -2 -8 8.34 0.79 -14 -2 8 10.30 0.87 14 -2 8 8.81 0.98 14 -2 8 8.56 0.98 -14 -2 -8 9.85 0.99 -14 -2 8 10.58 1.00 -14 2 -8 12.31 1.06 14 -2 -8 9.48 0.97 -14 -2 8 9.98 0.94 14 0 -9 18.38 1.50 -14 0 -9 18.54 1.37 -14 0 -9 19.82 1.55 14 0 9 18.34 1.41 -14 -1 9 -0.30 0.57 14 -1 9 0.49 0.70 14 -1 9 -0.04 0.68 14 1 -9 -0.45 0.51 14 -1 -9 -1.08 0.77 -14 -1 -9 1.19 0.68 -14 -1 9 0.23 0.64 -14 -1 -9 0.96 0.70 -14 1 9 -1.21 0.66 14 1 9 -0.04 0.56 -14 2 9 22.94 1.41 14 -2 -9 19.51 1.21 -14 -2 9 21.30 1.31 14 -2 9 19.29 1.40 14 -2 9 18.08 1.39 -14 -2 -9 21.72 1.44 -14 -2 9 22.76 1.43 -14 2 -9 24.54 1.47 -14 -2 -9 20.05 1.24 14 -2 -9 21.73 1.41 -14 -2 9 21.73 1.33 14 0 -10 21.38 1.59 -14 0 -10 24.01 1.65 14 0 10 23.01 1.54 -14 -1 10 1.13 0.54 14 -1 10 1.97 0.72 14 -1 10 1.63 0.69 14 -1 -10 1.52 0.76 -14 -1 -10 2.03 0.71 -14 -1 10 1.56 0.65 -14 -1 -10 2.09 0.76 -14 1 10 2.00 0.68 14 1 10 2.72 0.67 -14 2 10 0.81 0.50 14 -2 -10 1.47 0.45 -14 -2 10 0.50 0.49 14 -2 10 2.77 0.66 14 -2 -10 1.02 0.59 14 -2 10 1.29 0.64 -14 -2 -10 1.66 0.61 -14 -2 10 1.23 0.59 -14 2 -10 2.66 0.66 -14 -2 -10 1.37 0.49 -14 -2 10 1.33 0.55 -14 0 -11 7.18 0.87 14 0 -11 6.38 0.98 14 0 11 7.72 0.94 -14 -1 11 2.97 0.60 14 -1 11 1.62 0.67 14 -1 11 1.97 0.67 14 -1 -11 3.26 0.83 -14 -1 11 3.13 0.70 -14 -1 -11 2.91 0.74 -14 1 -11 2.84 0.80 -14 -1 -11 2.33 0.75 -14 1 11 2.24 0.64 14 1 11 2.50 0.66 -14 2 11 2.53 0.60 -14 -2 11 2.38 0.54 14 -2 11 3.61 0.66 14 -2 -11 3.43 0.62 14 -2 11 3.10 0.67 -14 -2 -11 3.10 0.62 -14 2 -11 2.98 0.66 -14 -2 -11 3.48 0.55 -14 -2 11 2.47 0.58 -14 0 -12 1.82 0.63 14 0 12 1.68 0.72 14 0 -12 0.77 0.69 14 -1 12 0.74 0.60 14 -1 12 1.55 0.62 14 -1 -12 0.94 0.73 -14 -1 12 0.08 0.54 -14 -1 -12 0.23 0.62 -14 1 -12 0.32 0.71 -14 -1 -12 0.84 0.64 -14 1 12 0.24 0.55 14 1 12 0.83 0.60 -14 2 12 0.23 0.47 -14 -2 12 0.14 0.45 14 -2 12 -0.32 0.52 14 -2 -12 0.03 0.46 14 -2 12 -0.24 0.53 -14 -2 -12 0.34 0.48 -14 -2 12 0.15 0.42 -14 2 -12 0.45 0.54 -14 -2 -12 -0.10 0.42 14 0 -13 14.22 1.26 14 0 13 16.49 1.27 -14 0 -13 14.19 1.16 14 -1 -13 12.81 1.21 -14 -1 -13 14.44 1.19 -14 1 -13 14.71 1.25 -14 -1 -13 15.07 1.22 -14 1 13 11.55 1.02 14 1 13 14.53 1.10 -14 2 13 1.51 0.48 14 -2 13 1.21 0.49 14 -2 -13 1.17 0.47 14 -2 13 0.35 0.45 -14 -2 -13 1.81 0.52 -14 -2 13 1.85 0.49 -14 2 -13 1.98 0.59 -14 -2 -13 1.75 0.46 14 0 -14 44.05 2.40 14 0 14 44.02 2.36 -14 0 -14 41.09 2.27 14 -1 -14 17.78 1.40 -14 -1 -14 19.01 1.37 -14 1 -14 19.48 1.41 -14 -1 -14 19.06 1.39 14 1 14 17.97 1.27 14 -2 -14 2.28 0.49 -14 -2 14 1.87 0.44 -14 2 -14 1.98 0.51 -14 -2 -14 1.90 0.45 -14 2 14 1.83 0.45 -14 -2 -14 2.22 0.52 14 0 -15 107.20 5.15 -14 0 -15 117.99 5.26 14 0 15 115.96 5.16 -14 0 -15 108.40 5.06 14 -1 -15 58.56 3.13 -14 1 -15 66.36 3.15 14 1 15 60.43 3.00 -14 -1 -15 61.39 3.11 -14 -2 -15 0.33 0.40 -14 -2 15 0.54 0.37 -14 2 -15 0.83 0.43 -14 0 -16 9.85 0.91 14 0 -16 9.65 1.02 -14 0 -16 13.10 1.14 14 0 16 10.80 1.01 -14 -1 -16 3.11 0.67 14 -1 -16 2.54 0.71 -14 1 -16 3.50 0.72 14 1 16 3.15 0.62 -14 0 -17 52.15 2.66 14 0 -17 54.93 2.78 -14 0 -17 55.67 2.85 14 0 17 57.36 2.78 -14 -1 -17 6.48 0.78 14 -1 -17 5.03 0.77 14 1 17 5.43 0.71 -14 1 -17 5.82 0.82 -14 0 -18 25.32 1.58 14 0 -18 22.72 1.45 -14 -1 -18 1.75 0.57 14 -1 -18 2.00 0.61 14 1 18 1.90 0.54 -14 -1 -18 1.86 0.60 -14 1 -18 1.47 0.57 14 0 -19 7.44 0.81 -14 0 -19 9.83 0.91 -14 -1 -19 2.18 0.56 -14 1 -19 1.83 0.57 -14 -1 -19 2.79 0.55 14 1 19 1.55 0.49 -14 -1 19 0.58 0.52 14 -1 -19 1.21 0.54 -14 0 -20 1.56 0.59 14 0 -20 0.59 0.43 14 -1 20 2.31 0.55 14 1 20 2.05 0.47 -14 -1 -20 1.57 0.53 -14 1 -20 1.95 0.51 14 -1 -20 1.56 0.50 -14 -1 20 0.14 0.43 14 0 21 31.56 1.67 -14 0 -21 31.91 1.73 14 -1 21 0.23 0.40 14 -1 -21 0.13 0.40 -14 -1 -21 0.39 0.43 14 0 22 28.42 1.70 -14 0 -22 34.99 1.71 14 0 23 11.93 0.86 -15 1 0 4.17 0.54 15 -1 0 2.67 0.67 15 -1 0 2.25 0.61 -15 1 -1 4.86 0.60 15 -1 1 1.66 0.61 15 -1 -1 1.73 0.61 15 -1 -1 3.82 0.68 15 -1 1 4.71 0.66 -15 1 -2 3.96 0.58 15 -1 2 0.23 0.53 15 -1 -2 1.36 0.63 15 -1 2 3.42 0.61 15 -1 -2 2.93 0.67 -15 0 -3 -0.73 0.50 -15 1 -3 1.02 0.50 15 -1 3 0.11 0.48 15 -1 -3 0.45 0.59 15 -1 -3 0.40 0.59 -15 0 -4 0.22 0.48 -15 1 -4 1.76 0.53 15 -1 -4 1.23 0.57 -15 0 -5 -0.52 0.50 -15 1 -5 5.14 0.66 15 -1 -5 5.19 0.74 -15 0 -6 0.18 0.49 15 0 -6 -0.09 0.50 -15 1 -6 3.34 0.61 15 -1 -6 3.42 0.64 -15 0 -7 0.59 0.48 15 0 -7 -0.42 0.51 15 -1 -7 6.43 0.74 -15 1 -7 5.28 0.67 -15 0 -8 0.80 0.50 15 0 -8 -0.52 0.49 -15 1 -8 4.47 0.63 15 -1 -8 3.63 0.61 -15 0 -9 0.47 0.49 15 0 -9 -0.05 0.43 -15 1 -9 2.10 0.52 15 -1 -9 1.70 0.51 -15 0 -10 -0.20 0.48 15 0 -10 -0.30 0.45 15 -1 -10 1.19 0.47 -15 0 -11 0.75 0.46 15 -1 -11 0.48 0.39 -15 0 -12 0.11 0.44 0 0 0 0.00 0.00 TITL KBY-FFA4CH3-Y_auto in Pnma REM Pnma (#62, found as Pbnm in bca setting) CELL 1.54184 12.309081 41.705336 5.073418 90.0000 90.0000 90.0000 ZERR 37.00 0.000154 0.000428 0.000060 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z SYMM x+1/2,-y+1/2,-z+1/2 SFAC C H N O F UNIT 37.00 37.00 37.00 37.00 37.00 REM CrysAlisPro recorded range (K): Min=173.0; max=173.0; aver:173.0 TEMP -100 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 96552 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.356 _oxdiff_exptl_absorpt_empirical_full_min 0.601 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, 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 F001 F 0.4065(3) 0.7413(5) 0.26722(7) 0.0530(7) Uani 1 1 d . . . . . O8 O 0.4797(2) 0.7596(5) 0.49877(7) 0.0332(6) Uani 1 1 d . . . . . O003 O 0.4106(2) 0.3615(5) 0.53405(6) 0.0333(5) Uani 1 1 d . . . . . O004 O 0.3451(2) 0.6358(5) 0.46610(6) 0.0327(5) Uani 1 1 d . . . . . F005 F 0.2423(2) 0.5935(5) 0.70962(7) 0.0569(6) Uani 1 1 d . . . . . F006 F 0.5099(2) 0.4586(6) 0.28920(6) 0.0598(7) Uani 1 1 d . . . . . O007 O 0.2771(3) 0.2377(5) 0.50151(7) 0.0340(6) Uani 1 1 d . . . . . H007 H 0.300171 0.366999 0.490951 0.051 Uiso 1 1 calc R U . . . F008 F 0.2192(3) 0.1857(6) 0.69841(7) 0.0678(9) Uani 1 1 d . . . . . F009 F 0.3410(3) 0.3019(6) 0.73223(7) 0.0589(7) Uani 1 1 d . . . . . N00A N 0.4137(2) 0.1572(6) 0.59320(6) 0.0293(6) Uani 1 1 d . . . . . H00A H 0.463211 0.196414 0.578762 0.035 Uiso 1 1 calc R U . . . F00B F 0.5251(3) 0.8675(7) 0.30088(7) 0.0745(10) Uani 1 1 d . . . . . N00C N 0.3404(2) 0.8456(5) 0.40729(6) 0.0299(6) Uani 1 1 d . . . . . H00C H 0.291849 0.801390 0.421828 0.036 Uiso 1 1 calc R U . . . C00D C 0.3929(3) 0.7732(6) 0.35069(9) 0.0286(8) Uani 1 1 d . . . . . H00D H 0.454152 0.885954 0.352535 0.034 Uiso 1 1 calc R U . . . C00E C 0.4242(3) 0.7784(6) 0.47164(9) 0.0266(7) Uani 1 1 d . . . . . C00F C 0.3233(3) 0.7411(6) 0.37655(10) 0.0275(8) Uani 1 1 d . . . . . C00G C 0.4652(3) 1.2127(6) 0.39854(9) 0.0295(7) Uani 1 1 d . . . . . H00G H 0.436175 1.240108 0.377695 0.035 Uiso 1 1 calc R U . . . C00H C 0.3315(3) 0.2191(6) 0.52861(9) 0.0282(7) Uani 1 1 d . . . . . C00I C 0.3309(3) -0.0055(6) 0.58276(7) 0.0269(6) Uani 1 1 d . . . . . C00J C 0.2897(2) 0.0184(6) 0.55093(8) 0.0264(6) Uani 1 1 d . . . . . C00K C 0.4227(3) 1.0079(6) 0.41782(8) 0.0272(6) Uani 1 1 d . . . . . C00L C 0.3763(3) 0.3921(6) 0.67750(8) 0.0304(6) Uani 1 1 d . . . . . C00M C 0.2065(3) -0.1505(6) 0.54064(8) 0.0304(7) Uani 1 1 d . . . . . H00M H 0.178990 -0.133587 0.519459 0.036 Uiso 1 1 calc R U . . . C00N C 0.4648(2) 0.9823(6) 0.44926(7) 0.0276(6) Uani 1 1 d . . . . . C00O C 0.4528(3) 0.6775(8) 0.29506(9) 0.0408(8) Uani 1 1 d . . . . . C00P C 0.5470(3) 1.3719(6) 0.40923(8) 0.0327(7) Uani 1 1 d . . . . . H00P H 0.574385 1.506247 0.395585 0.039 Uiso 1 1 calc R U . . . C00Q C 0.4297(3) 0.2690(6) 0.62379(9) 0.0271(8) Uani 1 1 d . . . . . C00R C 0.4639(3) 0.5631(7) 0.68076(8) 0.0323(7) Uani 1 1 d . . . . . C00S C 0.5355(3) 0.5774(7) 0.65471(8) 0.0354(7) Uani 1 1 d . . . . . H00S H 0.597163 0.689339 0.656154 0.042 Uiso 1 1 calc R U . . . C00T C 0.1639(3) -0.3407(7) 0.56062(9) 0.0349(7) Uani 1 1 d . . . . . H00T H 0.106326 -0.450910 0.553516 0.042 Uiso 1 1 calc R U . . . C00U C 0.2340(3) 0.5741(7) 0.37277(8) 0.0334(7) Uani 1 1 d . . . . . H00U H 0.184248 0.552698 0.389998 0.040 Uiso 1 1 calc R U . . . C00V C 0.2063(3) -0.3688(6) 0.59133(8) 0.0323(7) Uani 1 1 d . . . . . H00V H 0.178528 -0.502413 0.605023 0.039 Uiso 1 1 calc R U . . . C00W C 0.2885(3) -0.2052(6) 0.60230(9) 0.0294(7) Uani 1 1 d . . . . . H00W H 0.316477 -0.228813 0.623336 0.035 Uiso 1 1 calc R U . . . C00X C 0.2858(3) 0.4680(7) 0.31793(8) 0.0346(7) Uani 1 1 d . . . . . C00Y C 0.5912(3) 1.3408(7) 0.43994(9) 0.0348(7) Uani 1 1 d . . . . . H00Y H 0.648953 1.450173 0.447076 0.042 Uiso 1 1 calc R U . . . C00Z C 0.5192(3) 0.4338(7) 0.62702(8) 0.0323(7) Uani 1 1 d . . . . . H00Z H 0.569928 0.447875 0.609932 0.039 Uiso 1 1 calc R U . . . C010 C 0.3731(3) 0.6399(6) 0.32183(8) 0.0309(7) Uani 1 1 d . . . . . C011 C 0.3578(3) 0.2466(6) 0.64974(10) 0.0297(8) Uani 1 1 d . . . . . H011 H 0.296684 0.132739 0.648365 0.036 Uiso 1 1 calc R U . . . C012 C 0.2166(3) 0.4395(7) 0.34442(9) 0.0363(7) Uani 1 1 d . . . . . H012 H 0.155977 0.324260 0.342837 0.044 Uiso 1 1 calc R U . . . C013 C 0.5488(3) 1.1473(6) 0.45961(9) 0.0319(7) Uani 1 1 d . . . . . H013 H 0.577390 1.125829 0.480608 0.038 Uiso 1 1 calc R U . . . C014 C 0.4864(4) 0.7298(8) 0.71003(11) 0.0416(9) Uani 1 1 d . . . . . H01D H 0.418773 0.756300 0.722020 0.062 Uiso 1 1 calc R U . . . H01E H 0.515424 0.901039 0.703347 0.062 Uiso 1 1 calc R U . . . H01F H 0.539519 0.640187 0.723717 0.062 Uiso 1 1 calc R U . . . C015 C 0.2623(4) 0.3136(9) 0.28768(11) 0.0446(9) Uani 1 1 d . . . . . H01A H 0.230940 0.431360 0.271517 0.067 Uiso 1 1 calc R U . . . H01B H 0.210851 0.171669 0.292476 0.067 Uiso 1 1 calc R U . . . H01C H 0.330048 0.237871 0.279441 0.067 Uiso 1 1 calc R U . . . C016 C 0.2950(3) 0.3667(8) 0.70425(9) 0.0402(8) Uani 1 1 d . . . . . H8 H 0.456(4) 0.610(11) 0.5113(12) 0.065(15) Uiso 1 1 d . . . . . 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 F001 0.0680(18) 0.0622(15) 0.0289(14) 0.0051(10) 0.0037(12) 0.0063(12) O8 0.0398(15) 0.0336(13) 0.0261(15) 0.0049(9) -0.0050(12) -0.0081(9) O003 0.0373(12) 0.0343(13) 0.0285(12) 0.0050(9) -0.0012(9) -0.0071(10) O004 0.0382(12) 0.0327(12) 0.0273(12) 0.0039(9) -0.0011(9) -0.0064(10) F005 0.0484(13) 0.0619(14) 0.0604(15) -0.0096(12) 0.0141(11) 0.0118(11) F006 0.0559(14) 0.0702(17) 0.0532(14) 0.0004(12) 0.0138(11) 0.0201(13) O007 0.0420(15) 0.0338(13) 0.0260(15) 0.0056(9) -0.0056(12) -0.0064(10) F008 0.0701(19) 0.0848(18) 0.0485(15) -0.0231(13) 0.0266(13) -0.0427(15) F009 0.074(2) 0.0761(17) 0.0268(14) 0.0062(11) 0.0079(13) 0.0014(14) N00A 0.0318(14) 0.0311(15) 0.0251(13) 0.0015(10) 0.0016(10) -0.0028(11) F00B 0.081(2) 0.097(2) 0.0460(15) -0.0183(15) 0.0239(14) -0.0492(18) N00C 0.0336(14) 0.0322(14) 0.0241(13) 0.0010(11) 0.0023(10) -0.0045(11) C00D 0.0327(19) 0.0291(17) 0.0239(19) -0.0002(11) -0.0016(15) -0.0018(12) C00E 0.0298(18) 0.0242(15) 0.0258(18) 0.0010(11) 0.0012(14) -0.0002(12) C00F 0.0308(19) 0.0249(16) 0.027(2) 0.0026(11) -0.0036(15) 0.0038(11) C00G 0.039(2) 0.0226(15) 0.0265(18) 0.0014(11) 0.0019(14) 0.0037(13) C00H 0.036(2) 0.0259(15) 0.0227(17) -0.0012(12) 0.0023(15) 0.0028(13) C00I 0.0292(15) 0.0242(14) 0.0272(14) -0.0002(11) 0.0027(12) 0.0039(12) C00J 0.0308(14) 0.0215(14) 0.0269(14) -0.0012(11) 0.0023(12) 0.0023(11) C00K 0.0306(14) 0.0224(14) 0.0286(14) -0.0013(11) 0.0034(12) 0.0038(12) C00L 0.0345(17) 0.0297(15) 0.0270(15) 0.0036(12) 0.0002(12) 0.0032(12) C00M 0.0319(16) 0.0310(17) 0.0282(16) -0.0010(12) 0.0002(13) 0.0009(13) C00N 0.0332(15) 0.0230(14) 0.0266(14) 0.0008(11) 0.0029(12) 0.0020(12) C00O 0.046(2) 0.047(2) 0.0301(17) -0.0040(14) 0.0026(15) -0.0038(17) C00P 0.0400(17) 0.0227(14) 0.0355(17) 0.0015(12) 0.0071(14) 0.0009(12) C00Q 0.0295(18) 0.0281(17) 0.0236(19) 0.0029(11) -0.0014(15) 0.0027(11) C00R 0.0342(17) 0.0325(16) 0.0302(16) -0.0006(13) -0.0026(12) 0.0026(13) C00S 0.0307(16) 0.0380(17) 0.0374(18) -0.0011(14) -0.0028(13) -0.0037(14) C00T 0.0374(18) 0.0290(17) 0.0382(19) -0.0033(14) 0.0042(14) -0.0045(14) C00U 0.0331(17) 0.0370(17) 0.0303(16) 0.0011(13) 0.0010(12) -0.0019(14) C00V 0.0362(17) 0.0240(15) 0.0366(17) 0.0031(12) 0.0075(14) -0.0003(12) C00W 0.0352(19) 0.0238(14) 0.0293(18) -0.0001(12) 0.0026(14) 0.0031(14) C00X 0.0388(18) 0.0342(17) 0.0309(16) -0.0027(13) -0.0059(13) 0.0022(14) C00Y 0.0383(18) 0.0308(17) 0.0352(17) -0.0015(14) 0.0018(14) -0.0068(14) C00Z 0.0305(16) 0.0346(17) 0.0317(16) 0.0025(13) 0.0016(12) -0.0005(13) C010 0.0350(17) 0.0320(16) 0.0259(15) 0.0012(12) -0.0023(12) 0.0031(13) C011 0.0316(19) 0.0264(17) 0.031(2) 0.0023(12) 0.0008(16) -0.0009(12) C012 0.0336(17) 0.0373(17) 0.0382(18) -0.0033(14) -0.0013(14) -0.0051(14) C013 0.0346(17) 0.0284(16) 0.0327(16) -0.0020(13) -0.0007(14) -0.0016(13) C014 0.043(2) 0.048(2) 0.0336(19) -0.0057(15) -0.0022(16) -0.0051(16) C015 0.045(2) 0.050(2) 0.039(2) -0.0129(17) -0.0056(17) -0.0007(19) C016 0.044(2) 0.044(2) 0.0328(18) -0.0054(15) 0.0054(15) -0.0030(15) 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' 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 C00E O8 H8 111(3) . . ? C00H O007 H007 109.5 . . ? C00I N00A H00A 115.5 . . ? C00I N00A C00Q 129.0(3) . . ? C00Q N00A H00A 115.5 . . ? C00F N00C H00C 115.6 . . ? C00K N00C H00C 115.6 . . ? C00K N00C C00F 128.8(3) . . ? C00F C00D H00D 119.9 . . ? C00F C00D C010 120.3(3) . . ? C010 C00D H00D 119.9 . . ? O8 C00E C00N 114.5(3) . . ? O004 C00E O8 121.6(3) . . ? O004 C00E C00N 123.9(3) . . ? C00D C00F N00C 125.0(3) . . ? C00D C00F C00U 118.0(3) . . ? C00U C00F N00C 116.8(3) . . ? C00K C00G H00G 119.3 . . ? C00P C00G H00G 119.3 . . ? C00P C00G C00K 121.4(3) . . ? O003 C00H O007 121.2(3) . . ? O003 C00H C00J 124.4(3) . . ? O007 C00H C00J 114.4(3) . . ? N00A C00I C00J 120.3(3) . . ? N00A C00I C00W 121.5(3) . . ? C00W C00I C00J 118.1(3) . . ? C00I C00J C00H 121.6(3) . . ? C00M C00J C00H 119.0(3) . . ? C00M C00J C00I 119.5(3) . . ? N00C C00K C00G 122.0(3) . . ? N00C C00K C00N 120.7(3) . . ? C00G C00K C00N 117.3(3) . . ? C00R C00L C011 122.7(3) . . ? C00R C00L C016 119.8(3) . . ? C011 C00L C016 117.5(3) . . ? C00J C00M H00M 119.3 . . ? C00T C00M C00J 121.4(3) . . ? C00T C00M H00M 119.3 . . ? C00K C00N C00E 121.6(3) . . ? C013 C00N C00E 118.3(3) . . ? C013 C00N C00K 120.1(3) . . ? F001 C00O F006 105.5(3) . . ? F001 C00O F00B 105.6(3) . . ? F001 C00O C010 113.5(3) . . ? F006 C00O C010 112.0(3) . . ? F00B C00O F006 106.4(4) . . ? F00B C00O C010 113.2(3) . . ? C00G C00P H00P 119.4 . . ? C00G C00P C00Y 121.2(3) . . ? C00Y C00P H00P 119.4 . . ? C00Z C00Q N00A 116.2(3) . . ? C00Z C00Q C011 118.3(3) . . ? C011 C00Q N00A 125.2(3) . . ? C00L C00R C00S 116.4(3) . . ? C00L C00R C014 124.8(3) . . ? C00S C00R C014 118.8(3) . . ? C00R C00S H00S 119.0 . . ? C00Z C00S C00R 122.0(3) . . ? C00Z C00S H00S 119.0 . . ? C00M C00T H00T 120.5 . . ? C00M C00T C00V 119.1(3) . . ? C00V C00T H00T 120.5 . . ? C00F C00U H00U 119.4 . . ? C012 C00U C00F 121.2(3) . . ? C012 C00U H00U 119.4 . . ? C00T C00V H00V 119.4 . . ? C00W C00V C00T 121.1(3) . . ? C00W C00V H00V 119.4 . . ? C00I C00W H00W 119.6 . . ? C00V C00W C00I 120.8(3) . . ? C00V C00W H00W 119.6 . . ? C010 C00X C012 116.2(3) . . ? C010 C00X C015 124.6(3) . . ? C012 C00X C015 119.2(3) . . ? C00P C00Y H00Y 120.8 . . ? C013 C00Y C00P 118.5(3) . . ? C013 C00Y H00Y 120.8 . . ? C00Q C00Z H00Z 119.5 . . ? C00S C00Z C00Q 120.9(3) . . ? C00S C00Z H00Z 119.5 . . ? C00D C010 C00O 117.7(3) . . ? C00X C010 C00D 122.4(3) . . ? C00X C010 C00O 119.8(3) . . ? C00L C011 C00Q 119.7(3) . . ? C00L C011 H011 120.2 . . ? C00Q C011 H011 120.2 . . ? C00U C012 C00X 121.9(3) . . ? C00U C012 H012 119.0 . . ? C00X C012 H012 119.0 . . ? C00N C013 H013 119.3 . . ? C00Y C013 C00N 121.4(3) . . ? C00Y C013 H013 119.3 . . ? C00R C014 H01D 109.5 . . ? C00R C014 H01E 109.5 . . ? C00R C014 H01F 109.5 . . ? H01D C014 H01E 109.5 . . ? H01D C014 H01F 109.5 . . ? H01E C014 H01F 109.5 . . ? C00X C015 H01A 109.5 . . ? C00X C015 H01B 109.5 . . ? C00X C015 H01C 109.5 . . ? H01A C015 H01B 109.5 . . ? H01A C015 H01C 109.5 . . ? H01B C015 H01C 109.5 . . ? F005 C016 C00L 111.9(3) . . ? F008 C016 F005 106.5(4) . . ? F008 C016 F009 106.6(3) . . ? F008 C016 C00L 112.9(3) . . ? F009 C016 F005 105.7(3) . . ? F009 C016 C00L 112.7(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 F001 C00O 1.334(5) . ? O8 C00E 1.325(5) . ? O8 H8 0.97(5) . ? O003 C00H 1.233(4) . ? O004 C00E 1.234(4) . ? F005 C016 1.339(5) . ? F006 C00O 1.337(5) . ? O007 H007 0.8400 . ? O007 C00H 1.317(5) . ? F008 C016 1.331(5) . ? F009 C016 1.338(5) . ? N00A H00A 0.8800 . ? N00A C00I 1.382(4) . ? N00A C00Q 1.410(5) . ? F00B C00O 1.334(5) . ? N00C H00C 0.8800 . ? N00C C00F 1.403(5) . ? N00C C00K 1.378(4) . ? C00D H00D 0.9500 . ? C00D C00F 1.387(6) . ? C00D C010 1.401(5) . ? C00E C00N 1.481(4) . ? C00F C00U 1.397(5) . ? C00G H00G 0.9500 . ? C00G C00K 1.414(5) . ? C00G C00P 1.366(5) . ? C00H C00J 1.472(5) . ? C00I C00J 1.426(4) . ? C00I C00W 1.401(5) . ? C00J C00M 1.403(4) . ? C00K C00N 1.416(4) . ? C00L C00R 1.390(5) . ? C00L C011 1.392(5) . ? C00L C016 1.504(5) . ? C00M H00M 0.9500 . ? C00M C00T 1.379(5) . ? C00N C013 1.398(5) . ? C00O C010 1.498(5) . ? C00P H00P 0.9500 . ? C00P C00Y 1.400(5) . ? C00Q C00Z 1.390(5) . ? C00Q C011 1.403(6) . ? C00R C00S 1.401(5) . ? C00R C014 1.511(5) . ? C00S H00S 0.9500 . ? C00S C00Z 1.380(5) . ? C00T H00T 0.9500 . ? C00T C00V 1.390(5) . ? C00U H00U 0.9500 . ? C00U C012 1.382(5) . ? C00V H00V 0.9500 . ? C00V C00W 1.386(5) . ? C00W H00W 0.9500 . ? C00X C010 1.394(5) . ? C00X C012 1.402(5) . ? C00X C015 1.513(5) . ? C00Y H00Y 0.9500 . ? C00Y C013 1.381(5) . ? C00Z H00Z 0.9500 . ? C011 H011 0.9500 . ? C012 H012 0.9500 . ? C013 H013 0.9500 . ? C014 H01D 0.9800 . ? C014 H01E 0.9800 . ? C014 H01F 0.9800 . ? C015 H01A 0.9800 . ? C015 H01B 0.9800 . ? C015 H01C 0.9800 . ? 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 F001 C00O C010 C00D -129.7(3) . . . . ? F001 C00O C010 C00X 53.0(5) . . . . ? O8 C00E C00N C00K 172.7(3) . . . . ? O8 C00E C00N C013 -5.6(5) . . . . ? O003 C00H C00J C00I 7.5(5) . . . . ? O003 C00H C00J C00M -173.2(3) . . . . ? O004 C00E C00N C00K -7.5(5) . . . . ? O004 C00E C00N C013 174.2(3) . . . . ? F006 C00O C010 C00D 110.9(4) . . . . ? F006 C00O C010 C00X -66.4(4) . . . . ? O007 C00H C00J C00I -172.3(3) . . . . ? O007 C00H C00J C00M 6.9(4) . . . . ? N00A C00I C00J C00H -1.5(4) . . . . ? N00A C00I C00J C00M 179.3(3) . . . . ? N00A C00I C00W C00V -179.2(3) . . . . ? N00A C00Q C00Z C00S 172.4(3) . . . . ? N00A C00Q C011 C00L -172.3(3) . . . . ? F00B C00O C010 C00D -9.4(5) . . . . ? F00B C00O C010 C00X 173.3(4) . . . . ? N00C C00F C00U C012 -173.1(3) . . . . ? N00C C00K C00N C00E 1.3(5) . . . . ? N00C C00K C00N C013 179.6(3) . . . . ? C00D C00F C00U C012 1.6(5) . . . . ? C00E C00N C013 C00Y 179.6(3) . . . . ? C00F N00C C00K C00G 38.2(5) . . . . ? C00F N00C C00K C00N -144.6(3) . . . . ? C00F C00D C010 C00O -178.5(3) . . . . ? C00F C00D C010 C00X -1.3(5) . . . . ? C00F C00U C012 C00X -1.5(6) . . . . ? C00G C00K C00N C00E 178.6(3) . . . . ? C00G C00K C00N C013 -3.1(4) . . . . ? C00G C00P C00Y C013 -1.1(5) . . . . ? C00H C00J C00M C00T -179.6(3) . . . . ? C00I N00A C00Q C00Z -177.8(3) . . . . ? C00I N00A C00Q C011 -4.2(5) . . . . ? C00I C00J C00M C00T -0.3(5) . . . . ? C00J C00I C00W C00V -2.2(5) . . . . ? C00J C00M C00T C00V -1.6(5) . . . . ? C00K N00C C00F C00D 3.9(5) . . . . ? C00K N00C C00F C00U 178.2(3) . . . . ? C00K C00G C00P C00Y -0.8(5) . . . . ? C00K C00N C013 C00Y 1.2(5) . . . . ? C00L C00R C00S C00Z 1.2(5) . . . . ? C00M C00T C00V C00W 1.6(5) . . . . ? C00P C00G C00K N00C -179.9(3) . . . . ? C00P C00G C00K C00N 2.9(5) . . . . ? C00P C00Y C013 C00N 0.9(5) . . . . ? C00Q N00A C00I C00J 143.6(3) . . . . ? C00Q N00A C00I C00W -39.4(5) . . . . ? C00R C00L C011 C00Q 0.5(5) . . . . ? C00R C00L C016 F005 63.3(4) . . . . ? C00R C00L C016 F008 -176.6(3) . . . . ? C00R C00L C016 F009 -55.7(4) . . . . ? C00R C00S C00Z C00Q 0.4(5) . . . . ? C00T C00V C00W C00I 0.3(5) . . . . ? C00W C00I C00J C00H -178.6(3) . . . . ? C00W C00I C00J C00M 2.2(4) . . . . ? C00Z C00Q C011 C00L 1.2(5) . . . . ? C010 C00D C00F N00C 174.0(3) . . . . ? C010 C00D C00F C00U -0.2(5) . . . . ? C010 C00X C012 C00U 0.0(5) . . . . ? C011 C00L C00R C00S -1.7(5) . . . . ? C011 C00L C00R C014 178.6(4) . . . . ? C011 C00L C016 F005 -114.6(4) . . . . ? C011 C00L C016 F008 5.5(5) . . . . ? C011 C00L C016 F009 126.5(3) . . . . ? C011 C00Q C00Z C00S -1.7(5) . . . . ? C012 C00X C010 C00D 1.4(5) . . . . ? C012 C00X C010 C00O 178.5(3) . . . . ? C014 C00R C00S C00Z -179.0(3) . . . . ? C015 C00X C010 C00D -178.3(4) . . . . ? C015 C00X C010 C00O -1.2(5) . . . . ? C015 C00X C012 C00U 179.7(4) . . . . ? C016 C00L C00R C00S -179.5(3) . . . . ? C016 C00L C00R C014 0.8(5) . . . . ? C016 C00L C011 C00Q 178.3(3) . . . . ?