#------------------------------------------------------------------------------ #$Date: 2020-04-23 01:17:33 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251061 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126445.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_7126445 loop_ _publ_author_name 'Wang, Jian-Xin' 'Yu, Yishuai' 'Niu, Li-Ya' 'Zou, Bo' 'Wang, Kai' 'Yang, Qing-Zheng' _publ_section_title ; Difluoroboron \b-diketonate based Thermometer with Temperature-Dependent Emission Wavelength ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC01505A _journal_year 2020 _chemical_formula_moiety 'C20 H21 B F2 O3' _chemical_formula_sum 'C20 H21 B F2 O3' _chemical_formula_weight 358.18 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-10-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-01-13 deposited with the CCDC. 2020-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.1936(15) _cell_length_b 10.205(3) _cell_length_c 50.76(4) _cell_measurement_reflns_used 3323 _cell_measurement_temperature 399.9(3) _cell_measurement_theta_max 29.4450 _cell_measurement_theta_min 2.9240 _cell_volume 3726(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_environment air _diffrn_ambient_temperature 399.9(3) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.872 _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 -4.00 87.00 0.25 2.00 -- 17.58 57.00 30.00 364 2 \w 33.00 72.00 0.25 2.00 -- 17.58 77.00 120.00 156 3 \w -1.00 30.00 0.25 2.00 -- 17.58 77.00 120.00 124 4 \w -12.00 93.00 0.25 2.00 -- 17.58 57.00 90.00 420 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0873854000 _diffrn_orient_matrix_UB_12 -0.0050135000 _diffrn_orient_matrix_UB_13 0.0063195000 _diffrn_orient_matrix_UB_21 -0.0437850000 _diffrn_orient_matrix_UB_22 -0.0046267000 _diffrn_orient_matrix_UB_23 0.0125548000 _diffrn_orient_matrix_UB_31 -0.0034466000 _diffrn_orient_matrix_UB_32 -0.0689288000 _diffrn_orient_matrix_UB_33 -0.0015158000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_unetI/netI 0.0870 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.872 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -70 _diffrn_reflns_number 20217 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.872 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.856 _diffrn_reflns_theta_min 2.407 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.47240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.277 _exptl_crystal_description block _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.283 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.075 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 239 _refine_ls_number_reflns 5122 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.1737 _refine_ls_R_factor_gt 0.1104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3171 _refine_ls_wR_factor_ref 0.3638 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2367 _reflns_number_total 5122 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 400K in Pbca 400k.res created by SHELXL-2018/3 at 13:29:09 on 18-Oct-2019 CELL 0.71073 7.1936 10.2053 50.7636 90 90 90 ZERR 8 0.0015 0.0028 0.0433 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H B F O UNIT 160 168 8 16 24 L.S. 4 PLAN 5 SIZE 0.55 0.21 0.12 TEMP 127 BOND $H CONF fmap 2 acta OMIT 1 8 17 REM REM REM WGHT 0.200000 FVAR 1.33452 O2 5 0.439469 0.629594 0.622908 11.00000 0.04870 0.08999 = 0.10398 0.03871 0.00083 0.00013 O1 5 0.435382 0.800068 0.588891 11.00000 0.04592 0.09732 = 0.10870 0.04469 -0.00025 0.00527 C11 1 0.712751 0.546439 0.641507 11.00000 0.05261 0.06160 = 0.07158 0.00830 -0.00333 0.00077 C10 1 0.619782 0.633666 0.622730 11.00000 0.05103 0.05591 = 0.07104 0.00728 -0.00406 -0.00047 C6 1 0.704881 0.891329 0.570858 11.00000 0.05645 0.06697 = 0.06957 0.01073 0.00281 -0.00004 C8 1 0.615675 0.799887 0.589245 11.00000 0.04885 0.06569 = 0.06957 0.00509 0.00022 0.00087 C9 1 0.710599 0.717931 0.606006 11.00000 0.04984 0.07798 = 0.08512 0.01954 -0.00249 -0.00146 AFIX 43 H9 2 0.839860 0.719579 0.606024 11.00000 -1.20000 AFIX 0 F2 4 0.223480 0.793756 0.623375 11.00000 0.09606 0.10888 = 0.12350 0.02876 0.02893 0.02601 F1 4 0.206606 0.644801 0.591588 11.00000 0.08370 0.12087 = 0.11769 0.02834 -0.02608 -0.02123 C7 1 0.597716 0.973048 0.554608 11.00000 0.05708 0.07612 = 0.07548 0.01595 0.00187 0.00056 AFIX 43 H7 2 0.468679 0.969319 0.555447 11.00000 -1.20000 AFIX 0 C14 1 0.886963 0.393354 0.680886 11.00000 0.06586 0.06409 = 0.07661 0.00905 -0.00316 0.00788 C13 1 0.698558 0.380346 0.675197 11.00000 0.06847 0.07131 = 0.08619 0.02232 -0.00038 -0.00573 AFIX 43 H13 2 0.628263 0.319754 0.684579 11.00000 -1.20000 AFIX 0 C2 1 0.682473 1.058708 0.537429 11.00000 0.07285 0.08614 = 0.07445 0.02470 0.00052 -0.00481 O3 5 0.591763 1.142022 0.520716 11.00000 0.08795 0.12247 = 0.11454 0.06096 0.00662 0.00088 C16 1 0.901426 0.556392 0.646295 11.00000 0.05200 0.09592 = 0.09863 0.03656 -0.00008 -0.00223 AFIX 43 H16 2 0.972860 0.614798 0.636534 11.00000 -1.20000 AFIX 0 C12 1 0.613569 0.454699 0.656073 11.00000 0.05453 0.07130 = 0.09460 0.01715 -0.00502 -0.00130 AFIX 43 H12 2 0.487351 0.443379 0.652827 11.00000 -1.20000 AFIX 0 C5 1 0.896040 0.897873 0.569327 11.00000 0.05814 0.09236 = 0.10826 0.03538 0.00195 -0.00108 AFIX 43 H5 2 0.969103 0.844638 0.579999 11.00000 -1.20000 AFIX 0 C15 1 0.984764 0.480267 0.665469 11.00000 0.05965 0.09588 = 0.10709 0.02736 -0.01203 -0.00234 AFIX 43 H15 2 1.112262 0.488102 0.668061 11.00000 -1.20000 AFIX 0 C3 1 0.873232 1.062572 0.535729 11.00000 0.07420 0.09930 = 0.11155 0.04334 0.01565 -0.01242 AFIX 43 H3 2 0.930822 1.118152 0.523721 11.00000 -1.20000 AFIX 0 B1 3 0.322017 0.716990 0.606638 11.00000 0.05194 0.08348 = 0.09096 0.02121 -0.00213 0.00213 C17 1 0.981340 0.320028 0.704011 11.00000 0.08640 0.08157 = 0.08149 0.01819 -0.01366 0.01188 C4 1 0.978314 0.983722 0.551898 11.00000 0.06297 0.12023 = 0.13818 0.04323 0.01221 -0.00947 AFIX 43 H4 2 1.107287 0.988419 0.551055 11.00000 -1.20000 AFIX 0 C18 1 0.859547 0.211903 0.715471 11.00000 0.14265 0.10440 = 0.11304 0.04019 -0.02018 -0.00070 AFIX 137 H18A 2 0.743846 0.248671 0.721317 11.00000 -1.50000 H18B 2 0.922148 0.171954 0.730115 11.00000 -1.50000 H18C 2 0.835947 0.146989 0.702199 11.00000 -1.50000 AFIX 0 C1 1 0.393392 1.146000 0.522013 11.00000 0.08323 0.13015 = 0.11705 0.05253 -0.00458 0.01151 AFIX 137 H1A 2 0.347520 1.210731 0.509929 11.00000 -1.50000 H1B 2 0.355463 1.168243 0.539584 11.00000 -1.50000 H1C 2 0.343937 1.061699 0.517398 11.00000 -1.50000 AFIX 0 C19 1 1.008242 0.420337 0.726497 11.00000 0.16988 0.11182 = 0.11499 0.01131 -0.05376 -0.00364 AFIX 137 H19A 2 1.091350 0.488246 0.720791 11.00000 -1.50000 H19B 2 1.059764 0.376989 0.741609 11.00000 -1.50000 H19C 2 0.890322 0.458089 0.731058 11.00000 -1.50000 AFIX 0 C20 1 1.161055 0.263007 0.694679 11.00000 0.12339 0.21715 = 0.16269 0.09634 0.02261 0.09181 AFIX 137 H20A 2 1.141894 0.219425 0.678141 11.00000 -1.50000 H20B 2 1.205969 0.201165 0.707429 11.00000 -1.50000 H20C 2 1.250721 0.331809 0.692473 11.00000 -1.50000 AFIX 0 HKLF 4 REM 400K in Pbca REM wR2 = 0.3638, GooF = S = 1.072, Restrained GooF = 1.072 for all data REM R1 = 0.1104 for 2367 Fo > 4sig(Fo) and 0.1737 for all 5122 data REM 239 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.283, deepest hole -0.488, 1-sigma level 0.075 Q1 1 0.2229 0.7671 0.6462 11.00000 0.05 0.28 Q2 1 0.1939 0.6645 0.5702 11.00000 0.05 0.27 Q3 1 0.9347 0.3666 0.6992 11.00000 0.05 0.24 Q4 1 0.3567 1.1326 0.5006 11.00000 0.05 0.24 Q5 1 0.4499 0.8218 0.5677 11.00000 0.05 0.23 REM The information below was added by Olex2. REM REM R1 = 0.1104 for 2367 Fo > 4sig(Fo) and 0.1737 for all 22087 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.28, deepest hole -0.49 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1737 REM R1_gt = 0.1104 REM wR_ref = 0.3638 REM GOOF = 1.072 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 22087 REM Reflections_gt = 2367 REM Parameters = n/a REM Hole = -0.49 REM Peak = 0.28 REM Flack = n/a ; _cod_data_source_file d0cc01505a2.cif _cod_data_source_block 400k_CCDC2 _cod_original_cell_volume 3727(3) _cod_database_code 7126445 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.988 _shelx_estimated_absorpt_t_min 0.949 _diffrn_oxdiff_digest_frames ; 0108a728e287377d75bb0c93cfff91b747010649025 ; _diffrn_oxdiff_digest_hkl ; 0130a798f802ce23d34316331725435b733665 ; _reflns_odcompleteness_completeness 99.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C9(H9), C7(H7), C13(H13), C16(H16), C12(H12), C5(H5), C15(H15), C3(H3), C4(H4) 2.b Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C) ; _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 4.630 _oxdiff_exptl_absorpt_empirical_full_min 0.409 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 O2 O 0.4395(3) 0.6296(2) 0.62291(4) 0.0809(7) Uani 1 1 d . . . . . O1 O 0.4354(3) 0.8001(2) 0.58889(4) 0.0840(7) Uani 1 1 d . . . . . C11 C 0.7128(4) 0.5464(3) 0.64151(5) 0.0619(7) Uani 1 1 d . . . . . C10 C 0.6198(4) 0.6337(3) 0.62273(5) 0.0593(7) Uani 1 1 d . . . . . C6 C 0.7049(4) 0.8913(3) 0.57086(5) 0.0643(7) Uani 1 1 d . . . . . C8 C 0.6157(4) 0.7999(3) 0.58925(5) 0.0614(7) Uani 1 1 d . . . . . C9 C 0.7106(4) 0.7179(3) 0.60601(6) 0.0710(8) Uani 1 1 d . . . . . H9 H 0.839860 0.719579 0.606024 0.085 Uiso 1 1 calc R . . . . F2 F 0.2235(3) 0.7938(2) 0.62338(4) 0.1095(8) Uani 1 1 d . . . . . F1 F 0.2066(3) 0.6448(2) 0.59159(4) 0.1074(8) Uani 1 1 d . . . . . C7 C 0.5977(4) 0.9730(3) 0.55461(5) 0.0696(8) Uani 1 1 d . . . . . H7 H 0.468679 0.969319 0.555447 0.083 Uiso 1 1 calc R . . . . C14 C 0.8870(4) 0.3934(3) 0.68089(5) 0.0689(8) Uani 1 1 d . . . . . C13 C 0.6986(4) 0.3803(3) 0.67520(6) 0.0753(8) Uani 1 1 d . . . . . H13 H 0.628263 0.319754 0.684579 0.090 Uiso 1 1 calc R . . . . C2 C 0.6825(4) 1.0587(3) 0.53743(6) 0.0778(9) Uani 1 1 d . . . . . O3 O 0.5918(4) 1.1420(3) 0.52072(5) 0.1083(9) Uani 1 1 d . . . . . C16 C 0.9014(4) 0.5564(4) 0.64630(6) 0.0822(9) Uani 1 1 d . . . . . H16 H 0.972860 0.614798 0.636534 0.099 Uiso 1 1 calc R . . . . C12 C 0.6136(4) 0.4547(3) 0.65607(6) 0.0735(8) Uani 1 1 d . . . . . H12 H 0.487351 0.443379 0.652827 0.088 Uiso 1 1 calc R . . . . C5 C 0.8960(4) 0.8979(4) 0.56933(7) 0.0863(10) Uani 1 1 d . . . . . H5 H 0.969103 0.844638 0.579999 0.104 Uiso 1 1 calc R . . . . C15 C 0.9848(4) 0.4803(4) 0.66547(7) 0.0875(10) Uani 1 1 d . . . . . H15 H 1.112262 0.488102 0.668061 0.105 Uiso 1 1 calc R . . . . C3 C 0.8732(5) 1.0626(4) 0.53573(7) 0.0950(11) Uani 1 1 d . . . . . H3 H 0.930822 1.118152 0.523721 0.114 Uiso 1 1 calc R . . . . B1 B 0.3220(5) 0.7170(4) 0.60664(7) 0.0755(10) Uani 1 1 d . . . . . C17 C 0.9813(5) 0.3200(4) 0.70401(6) 0.0832(10) Uani 1 1 d . . . . . C4 C 0.9783(4) 0.9837(5) 0.55190(9) 0.1071(13) Uani 1 1 d . . . . . H4 H 1.107287 0.988419 0.551055 0.129 Uiso 1 1 calc R . . . . C18 C 0.8595(7) 0.2119(5) 0.71547(9) 0.1200(14) Uani 1 1 d . . . . . H18A H 0.743846 0.248671 0.721317 0.180 Uiso 1 1 calc GR . . . . H18B H 0.922148 0.171954 0.730115 0.180 Uiso 1 1 calc GR . . . . H18C H 0.835947 0.146989 0.702199 0.180 Uiso 1 1 calc GR . . . . C1 C 0.3934(5) 1.1460(5) 0.52201(8) 0.1101(14) Uani 1 1 d . . . . . H1A H 0.347520 1.210731 0.509929 0.165 Uiso 1 1 calc GR . . . . H1B H 0.355463 1.168243 0.539584 0.165 Uiso 1 1 calc GR . . . . H1C H 0.343937 1.061699 0.517398 0.165 Uiso 1 1 calc GR . . . . C19 C 1.0082(6) 0.4203(5) 0.72650(9) 0.1322(18) Uani 1 1 d . . . . . H19A H 1.091350 0.488246 0.720791 0.198 Uiso 1 1 calc GR . . . . H19B H 1.059764 0.376989 0.741609 0.198 Uiso 1 1 calc GR . . . . H19C H 0.890322 0.458089 0.731058 0.198 Uiso 1 1 calc GR . . . . C20 C 1.1611(7) 0.2630(7) 0.69468(11) 0.168(3) Uani 1 1 d . . . . . H20A H 1.141894 0.219425 0.678141 0.252 Uiso 1 1 calc GR . . . . H20B H 1.205969 0.201165 0.707429 0.252 Uiso 1 1 calc GR . . . . H20C H 1.250721 0.331809 0.692473 0.252 Uiso 1 1 calc GR . . . . 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 O2 0.0487(11) 0.0900(15) 0.1040(15) 0.0387(12) 0.0008(10) 0.0001(10) O1 0.0459(11) 0.0973(16) 0.1087(16) 0.0447(13) -0.0002(10) 0.0053(10) C11 0.0526(16) 0.0616(15) 0.0716(15) 0.0083(13) -0.0033(11) 0.0008(11) C10 0.0510(15) 0.0559(14) 0.0710(15) 0.0073(12) -0.0041(12) -0.0005(11) C6 0.0564(16) 0.0670(16) 0.0696(15) 0.0107(13) 0.0028(12) 0.0000(12) C8 0.0488(14) 0.0657(15) 0.0696(15) 0.0051(12) 0.0002(12) 0.0009(11) C9 0.0498(15) 0.0780(18) 0.0851(18) 0.0195(15) -0.0025(13) -0.0015(13) F2 0.0961(16) 0.1089(16) 0.1235(15) 0.0288(12) 0.0289(12) 0.0260(12) F1 0.0837(14) 0.1209(17) 0.1177(15) 0.0283(13) -0.0261(11) -0.0212(12) C7 0.0571(15) 0.0761(17) 0.0755(16) 0.0159(14) 0.0019(13) 0.0006(13) C14 0.0659(18) 0.0641(16) 0.0766(17) 0.0091(14) -0.0032(14) 0.0079(13) C13 0.0685(19) 0.0713(17) 0.0862(18) 0.0223(15) -0.0004(15) -0.0057(14) C2 0.0728(19) 0.086(2) 0.0745(17) 0.0247(16) 0.0005(14) -0.0048(15) O3 0.0880(17) 0.122(2) 0.1145(17) 0.0610(16) 0.0066(14) 0.0009(15) C16 0.0520(17) 0.096(2) 0.099(2) 0.0366(18) -0.0001(15) -0.0022(15) C12 0.0545(16) 0.0713(17) 0.0946(19) 0.0171(15) -0.0050(14) -0.0013(13) C5 0.0581(18) 0.092(2) 0.108(2) 0.035(2) 0.0019(16) -0.0011(16) C15 0.0596(18) 0.096(2) 0.107(2) 0.027(2) -0.0120(16) -0.0023(16) C3 0.074(2) 0.099(2) 0.112(2) 0.043(2) 0.0156(19) -0.0124(18) B1 0.0519(18) 0.083(2) 0.091(2) 0.021(2) -0.0021(17) 0.0021(16) C17 0.086(2) 0.082(2) 0.0815(19) 0.0182(17) -0.0137(16) 0.0119(16) C4 0.063(2) 0.120(3) 0.138(3) 0.043(3) 0.0122(19) -0.0095(19) C18 0.143(4) 0.104(3) 0.113(3) 0.040(2) -0.020(3) -0.001(3) C1 0.083(3) 0.130(3) 0.117(3) 0.053(3) -0.005(2) 0.012(2) C19 0.170(5) 0.112(3) 0.115(3) 0.011(3) -0.054(3) -0.004(3) C20 0.123(4) 0.217(6) 0.163(4) 0.096(4) 0.023(3) 0.092(4) 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 '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 C10 O2 B1 123.2(2) . . ? C8 O1 B1 122.8(2) . . ? C16 C11 C10 121.2(2) . . ? C16 C11 C12 117.4(2) . . ? C12 C11 C10 121.4(2) . . ? O2 C10 C11 115.6(2) . . ? O2 C10 C9 120.0(2) . . ? C9 C10 C11 124.4(2) . . ? C7 C6 C8 120.8(2) . . ? C5 C6 C8 120.2(2) . . ? C5 C6 C7 119.1(2) . . ? O1 C8 C6 115.3(2) . . ? O1 C8 C9 120.4(2) . . ? C9 C8 C6 124.3(2) . . ? C10 C9 C8 121.8(3) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C6 C7 H7 119.8 . . ? C2 C7 C6 120.4(3) . . ? C2 C7 H7 119.8 . . ? C13 C14 C17 122.5(3) . . ? C15 C14 C13 116.2(3) . . ? C15 C14 C17 121.2(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 C14 121.8(3) . . ? C12 C13 H13 119.1 . . ? O3 C2 C7 125.2(3) . . ? O3 C2 C3 114.8(3) . . ? C3 C2 C7 120.0(3) . . ? C2 O3 C1 117.8(2) . . ? C11 C16 H16 119.7 . . ? C15 C16 C11 120.6(3) . . ? C15 C16 H16 119.7 . . ? C11 C12 H12 119.4 . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12 119.4 . . ? C6 C5 H5 120.2 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 H5 120.2 . . ? C14 C15 C16 122.7(3) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C2 C3 H3 120.2 . . ? C2 C3 C4 119.6(3) . . ? C4 C3 H3 120.2 . . ? O2 B1 O1 111.7(2) . . ? F2 B1 O2 107.3(3) . . ? F2 B1 O1 109.8(3) . . ? F1 B1 O2 109.8(3) . . ? F1 B1 O1 107.9(3) . . ? F1 B1 F2 110.4(3) . . ? C18 C17 C14 112.8(3) . . ? C18 C17 C19 105.6(3) . . ? C19 C17 C14 107.1(3) . . ? C20 C17 C14 109.1(3) . . ? C20 C17 C18 109.6(4) . . ? C20 C17 C19 112.6(4) . . ? C5 C4 H4 119.4 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4 119.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C1 H1A 109.5 . . ? O3 C1 H1B 109.5 . . ? O3 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? 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 O2 C10 1.298(3) . ? O2 B1 1.480(4) . ? O1 C8 1.297(3) . ? O1 B1 1.482(4) . ? C11 C10 1.466(3) . ? C11 C16 1.383(4) . ? C11 C12 1.390(4) . ? C10 C9 1.374(4) . ? C6 C8 1.468(4) . ? C6 C7 1.404(4) . ? C6 C5 1.379(4) . ? C8 C9 1.375(4) . ? C9 H9 0.9300 . ? F2 B1 1.356(4) . ? F1 B1 1.347(4) . ? C7 H7 0.9300 . ? C7 C2 1.377(4) . ? C14 C13 1.392(4) . ? C14 C15 1.376(4) . ? C14 C17 1.549(4) . ? C13 H13 0.9300 . ? C13 C12 1.375(4) . ? C2 O3 1.367(4) . ? C2 C3 1.376(5) . ? O3 C1 1.429(4) . ? C16 H16 0.9300 . ? C16 C15 1.382(4) . ? C12 H12 0.9300 . ? C5 H5 0.9300 . ? C5 C4 1.379(5) . ? C15 H15 0.9300 . ? C3 H3 0.9300 . ? C3 C4 1.376(5) . ? C17 C18 1.524(6) . ? C17 C19 1.545(6) . ? C17 C20 1.495(6) . ? C4 H4 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C10 C9 C8 0.3(4) . . . . ? O1 C8 C9 C10 0.3(4) . . . . ? C11 C10 C9 C8 -178.4(3) . . . . ? C11 C16 C15 C14 -1.0(6) . . . . ? C10 O2 B1 O1 4.7(4) . . . . ? C10 O2 B1 F2 -115.6(3) . . . . ? C10 O2 B1 F1 124.3(3) . . . . ? C10 C11 C16 C15 175.1(3) . . . . ? C10 C11 C12 C13 -174.7(3) . . . . ? C6 C8 C9 C10 -179.6(3) . . . . ? C6 C7 C2 O3 179.8(3) . . . . ? C6 C7 C2 C3 1.4(5) . . . . ? C6 C5 C4 C3 -0.6(7) . . . . ? C8 O1 B1 O2 -4.1(4) . . . . ? C8 O1 B1 F2 114.8(3) . . . . ? C8 O1 B1 F1 -124.8(3) . . . . ? C8 C6 C7 C2 179.9(3) . . . . ? C8 C6 C5 C4 179.7(4) . . . . ? C7 C6 C8 O1 0.9(4) . . . . ? C7 C6 C8 C9 -179.2(3) . . . . ? C7 C6 C5 C4 -0.2(5) . . . . ? C7 C2 O3 C1 3.4(5) . . . . ? C7 C2 C3 C4 -2.2(6) . . . . ? C14 C13 C12 C11 0.1(5) . . . . ? C13 C14 C15 C16 3.4(5) . . . . ? C13 C14 C17 C18 12.9(5) . . . . ? C13 C14 C17 C19 -102.9(4) . . . . ? C13 C14 C17 C20 135.0(5) . . . . ? C2 C3 C4 C5 1.8(7) . . . . ? O3 C2 C3 C4 179.2(4) . . . . ? C16 C11 C10 O2 -169.5(3) . . . . ? C16 C11 C10 C9 9.2(5) . . . . ? C16 C11 C12 C13 2.4(5) . . . . ? C12 C11 C10 O2 7.5(4) . . . . ? C12 C11 C10 C9 -173.8(3) . . . . ? C12 C11 C16 C15 -2.0(5) . . . . ? C5 C6 C8 O1 -179.1(3) . . . . ? C5 C6 C8 C9 0.9(5) . . . . ? C5 C6 C7 C2 -0.1(5) . . . . ? C15 C14 C13 C12 -2.9(5) . . . . ? C15 C14 C17 C18 -170.1(3) . . . . ? C15 C14 C17 C19 74.1(4) . . . . ? C15 C14 C17 C20 -48.0(5) . . . . ? C3 C2 O3 C1 -178.1(4) . . . . ? B1 O2 C10 C11 175.7(3) . . . . ? B1 O2 C10 C9 -3.0(4) . . . . ? B1 O1 C8 C6 -178.2(3) . . . . ? B1 O1 C8 C9 1.9(4) . . . . ? C17 C14 C13 C12 174.2(3) . . . . ? C17 C14 C15 C16 -173.8(3) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 6 11019.8 211.748 1 0 0 6 1960.46 190.298 4 0 0 7 304.611 23.8765 1 0 0 7 57.5107 6.51968 4 0 0 8 31825 547.319 1 0 0 8 5322.43 513.788 4 0 0 9 58.9455 22.0233 1 0 0 9 11.2162 3.38024 4 0 0 10 29779.7 550.499 1 0 0 10 5296.62 514.918 4 0 0 11 333.458 33.6978 1 0 0 11 90.3546 10.4786 4 0 0 -12 13330.8 1301.03 4 0 0 12 15429.9 1301.36 4 0 0 -13 401.861 37.0577 4 0 0 13 393.978 37.3428 4 0 0 -14 3111.11 283.062 4 0 0 14 3070.75 283.182 4 0 0 -15 43.9537 5.84996 4 0 0 15 35.0061 6.63448 4 0 0 16 8500.47 726.598 4 0 0 -16 7443.68 726.297 4 0 0 -17 4.3103 2.97688 4 0 0 17 6.57537 4.24369 4 0 0 -18 1295.59 119.106 3 0 0 18 1454.61 119.998 4 0 0 -19 20.4241 4.99159 4 0 0 19 28.0667 7.41582 4 0 0 -20 7722.48 724.814 3 0 0 -20 8480.68 725.477 4 0 0 20 8060.17 725.692 4 0 0 21 17.1965 5.89804 4 0 0 -21 12.8295 4.04217 3 0 0 -21 20.4359 4.9673 4 0 0 -22 144.685 14.3789 4 0 0 -22 135.964 13.509 3 0 0 22 123.529 14.491 4 0 0 23 1.52653 4.91576 4 0 0 -23 11.4449 3.71822 3 0 0 -23 2.57432 3.95917 4 0 0 -24 426.83 34.858 4 0 0 -24 372.531 33.6002 3 0 0 24 317.254 34.475 4 0 0 25 20.1218 7.76242 4 0 0 -25 22.4643 5.79083 4 0 0 -25 36.8923 5.55124 3 0 0 26 1123.95 113.565 4 0 0 -26 1371.82 112.583 3 0 0 -26 1352.98 113.781 4 0 0 -27 67.9888 11.2511 4 0 0 27 58.4171 13.4425 4 0 0 -28 4797.05 386.286 4 0 0 -28 4731.89 384.933 3 0 0 28 3767.36 386.227 4 0 0 -29 38.6178 8.41039 4 0 0 -29 55.7247 7.45142 3 0 0 -30 1200.08 111.035 3 0 0 -30 1442.69 113.248 4 0 0 -31 47.723 9.35843 4 0 0 -31 52.1033 7.46077 3 0 0 -32 1239.48 97.3171 4 0 0 -32 1020.18 94.8426 3 0 0 -33 94.0434 14.4612 4 0 0 -33 128.445 13.0338 3 0 0 -34 2842.2 227.749 4 0 0 -34 2506.64 225.32 3 0 0 -35 64.9783 11.7391 4 0 0 -35 77.4211 9.56433 3 0 0 -36 1312.52 102.565 4 0 0 -36 1069.75 99.4764 3 0 0 -37 84.9303 14.1091 4 0 0 -37 95.6709 11.2904 3 0 0 -38 1612.93 139.81 4 0 0 -38 1560.82 137.008 3 0 0 -39 73.1056 13.458 4 0 0 -39 85.2779 10.3611 3 0 0 -40 360.883 33.0709 3 0 0 -40 350.142 36.2476 4 0 0 -41 61.2875 11.7206 4 0 0 -41 51.6231 8.04368 3 0 0 -42 50.7225 10.924 4 0 0 -42 42.9503 6.97801 3 0 0 -43 21.3877 9.88827 4 0 0 -44 73.5767 13.5317 4 0 0 -45 15.0205 9.18055 4 0 0 -46 14.6303 9.54842 4 0 0 -47 17.3274 10.1907 4 0 0 -48 3.69329 6.52619 2 0 0 -48 111.796 14.1675 4 0 0 -49 -0.34024 6.46914 2 0 0 -49 28.9629 11.975 4 0 0 -50 6.32661 6.92306 2 0 0 -50 21.9681 12.0401 4 0 0 -51 54.5821 14.7378 4 0 0 -52 337.326 37.5308 4 0 0 -53 43.5353 15.789 4 0 0 -54 110.522 20.3391 4 0 0 -55 77.1778 18.5806 4 0 0 -56 1044.23 98.018 4 0 0 -57 105.53 22.2785 4 0 0 -58 228.4 30.5352 4 0 0 -59 7.02235 16.1589 4 0 0 -60 109.15 21.9336 4 0 0 -61 7.26532 16.6178 4 0 0 -62 127.495 23.9702 4 0 0 -63 22.9925 17.4687 4 0 0 -64 27.2372 17.2301 4 0 0 -65 32.9888 17.139 4 0 0 -66 24.0642 17.3686 4 0 0 -67 -4.09362 17.7864 4 0 0 -68 4.1285 16.5613 4 0 -1 3 0.21977 2.4609 4 0 -1 4 -0.62971 2.486 4 0 1 -5 -0.45552 3.49462 1 0 1 -5 2.59532 2.73792 4 0 -1 5 3.31271 2.96229 4 0 -1 6 0.73701 3.33046 4 0 1 -6 2.18926 2.82707 4 0 1 6 0.93813 1.73075 4 0 1 -6 3.7221 3.70274 1 0 1 7 2.11209 1.91265 4 0 1 -7 -0.22195 2.83399 4 0 -1 7 -1.01564 3.33146 4 0 -1 -7 -0.39186 2.40376 4 0 1 -7 0.77075 4.40604 1 0 1 8 1.3798 1.89312 4 0 -1 8 0.8116 3.86527 4 0 1 -8 0.47609 3.24591 4 0 -1 -8 0.74221 2.22736 4 0 1 -8 1.84073 5.80392 1 0 1 9 2.2771 1.87019 4 0 -1 9 -0.56009 3.60267 4 0 -1 -9 1.18683 2.01027 4 0 1 -9 3.77125 5.98702 1 0 1 -10 0.88232 6.71133 1 0 1 10 0.99283 2.12197 4 0 -1 -10 1.27656 2.26326 4 0 -1 10 0.85968 3.96654 4 0 1 -11 3.11646 7.48121 1 0 1 11 0.51427 2.07732 4 0 -1 -11 -2.03963 2.42752 4 0 -1 11 0.59956 3.80053 4 0 1 -12 7.14889 9.61438 1 0 1 12 0.42114 2.18738 4 0 -1 -12 -1.6811 2.22733 4 0 -1 12 4.42226 4.18507 4 0 1 -13 4.38607 11.0429 1 0 1 13 2.06762 2.29042 4 0 -1 -13 -0.52604 2.46741 4 0 -1 13 7.81609 4.26135 4 0 1 -14 10.2543 16.422 1 0 1 14 1.70723 2.25534 4 0 -1 -14 0.56589 2.43484 4 0 -1 14 -0.6761 3.97095 4 0 1 15 8.82136 2.90427 4 0 -1 -15 1.04835 2.7016 4 0 -1 15 -2.48736 4.07848 4 0 1 -16 13.8073 22.087 1 0 1 16 1.45245 2.85615 4 0 -1 -16 0.88367 2.85188 4 0 -1 16 1.10639 4.22373 4 0 1 -17 4.2522 23.3701 1 0 1 17 1.69403 2.83289 4 0 -1 -17 -0.23427 2.77414 4 0 -1 17 -1.15756 4.35979 4 0 1 -18 2.46431 26.3103 1 0 1 -18 1.6868 4.22618 4 0 1 18 -1.7318 3.06984 4 0 -1 -18 5.40555 2.96012 4 0 -1 18 4.0273 4.75158 4 0 1 19 9.79553 17.6777 1 0 1 19 2.42307 3.25366 4 0 1 -19 -0.41221 3.88841 4 0 -1 -19 -1.02684 3.04167 4 0 -1 19 5.45379 4.69891 4 0 1 -20 2.19254 22.2071 1 0 1 20 16.6377 20.5533 1 0 1 20 0.52907 3.15768 4 0 1 -20 -2.12558 4.05956 4 0 -1 -20 0.27257 3.01019 4 0 -1 20 1.30881 4.86287 4 0 1 -21 -2.16387 22.3985 1 0 1 21 -8.17167 21.6535 1 0 1 21 4.80432 3.64626 4 0 1 -21 -1.30562 4.02441 4 0 -1 -21 -0.58106 3.17905 4 0 -1 21 0.45747 5.21518 4 0 1 22 1.90207 24.8712 1 0 1 -22 -2.03756 20.9787 1 0 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