#------------------------------------------------------------------------------ #$Date: 2020-04-23 01:17:33 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251061 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126444.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_7126444 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 'C17 H15 B F2 O3' _chemical_formula_sum 'C17 H15 B F2 O3' _chemical_formula_weight 316.10 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _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 103.133(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.7481(4) _cell_length_b 19.1442(7) _cell_length_c 10.2334(4) _cell_measurement_reflns_used 6493 _cell_measurement_temperature 199.98(10) _cell_measurement_theta_max 29.9670 _cell_measurement_theta_min 2.6730 _cell_volume 1478.23(11) _computing_cell_refinement 'CrysAlisPro 1.171.39.29a (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.29a (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.29a (Rigaku OD, 2015)' _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 N~2~ _diffrn_ambient_temperature 199.98(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.851 _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 -26.00 58.00 0.50 1.07 -- 17.58 -95.00-101.00 168 2 \w 4.00 30.00 0.50 1.07 -- -18.36 -99.00 0.00 52 3 \w -18.00 30.00 0.50 1.07 -- -18.36 -99.00 90.00 96 4 \w -24.00 42.00 0.50 1.07 -- -18.36 19.00 120.00 132 5 \w -60.00 30.00 0.50 1.07 -- -18.36 95.00 8.00 180 6 \w 48.00 77.00 0.50 1.07 -- 17.58 178.00-120.00 58 7 \w -67.00 -42.00 0.50 1.07 -- -18.36-178.00 60.00 50 8 \w -104.00 -71.00 0.50 1.07 -- -18.36-178.00 60.00 66 ; _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 0.0711410000 _diffrn_orient_matrix_UB_12 0.0237632000 _diffrn_orient_matrix_UB_13 0.0213256000 _diffrn_orient_matrix_UB_21 0.0450656000 _diffrn_orient_matrix_UB_22 -0.0251622000 _diffrn_orient_matrix_UB_23 0.0462673000 _diffrn_orient_matrix_UB_31 0.0418454000 _diffrn_orient_matrix_UB_32 -0.0132165000 _diffrn_orient_matrix_UB_33 -0.0496846000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.851 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 13362 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.851 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.653 _diffrn_reflns_theta_min 2.304 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.420 _exptl_crystal_description block _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.239 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 3886 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0446 _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^)+(0.0509P)^2^+0.3605P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1124 _refine_ls_wR_factor_ref 0.1211 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2906 _reflns_number_total 3886 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 200K in P2(1)/c 200k.res created by SHELXL-2018/3 at 12:38:19 on 18-Oct-2019 CELL 0.71073 7.7481 19.1442 10.2334 90 103.133 90 ZERR 4 0.0004 0.0007 0.0004 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F O UNIT 68 60 4 8 12 L.S. 4 PLAN 5 SIZE 0.28 0.24 0.11 TEMP -73 ACTA BOND $H CONF fmap 2 REM REM REM WGHT 0.050900 0.360500 FVAR 2.81427 F1 4 0.246854 0.701083 0.338903 11.00000 0.05602 0.03074 = 0.04657 0.00212 -0.01256 0.00390 F2 4 0.487434 0.636273 0.326264 11.00000 0.04101 0.06515 = 0.03737 -0.00260 0.00973 -0.00976 O1 5 0.415995 0.651813 0.532741 11.00000 0.04598 0.02981 = 0.02585 0.00297 -0.00052 -0.00948 O2 5 0.232963 0.581230 0.355433 11.00000 0.04440 0.03107 = 0.02637 0.00299 -0.00059 -0.00866 O3 5 -0.116696 0.411377 0.062495 11.00000 0.04785 0.03889 = 0.02813 -0.00246 -0.00325 -0.00773 C1 1 -0.209768 0.351305 -0.000175 11.00000 0.04839 0.04779 = 0.03321 -0.01194 0.00269 -0.01311 AFIX 137 H1A 2 -0.259669 0.361284 -0.095181 11.00000 -1.50000 H1B 2 -0.305697 0.339690 0.044116 11.00000 -1.50000 H1C 2 -0.127741 0.311762 0.007580 11.00000 -1.50000 AFIX 0 C2 1 -0.041570 0.407355 0.196477 11.00000 0.02809 0.03092 = 0.02850 -0.00368 0.00275 0.00085 C3 1 -0.055263 0.350233 0.277436 11.00000 0.03079 0.02543 = 0.03779 -0.00465 0.00537 -0.00107 AFIX 43 H3 2 -0.120273 0.310038 0.240448 11.00000 -1.20000 AFIX 0 C4 1 0.027096 0.352527 0.412998 11.00000 0.03615 0.02584 = 0.03580 0.00327 0.00622 -0.00005 AFIX 43 H4 2 0.016891 0.313672 0.468495 11.00000 -1.20000 AFIX 0 C5 1 0.123679 0.410311 0.468711 11.00000 0.03145 0.02966 = 0.02834 -0.00003 0.00367 0.00127 AFIX 43 H5 2 0.180037 0.410949 0.561411 11.00000 -1.20000 AFIX 0 C6 1 0.137575 0.467782 0.387279 11.00000 0.02465 0.02644 = 0.02719 -0.00280 0.00601 0.00175 C7 1 0.053610 0.466315 0.251191 11.00000 0.03043 0.02748 = 0.02807 -0.00003 0.00504 -0.00025 AFIX 43 H7 2 0.061373 0.505518 0.195899 11.00000 -1.20000 AFIX 0 C8 1 0.241410 0.530017 0.440820 11.00000 0.02434 0.02530 = 0.02722 -0.00044 0.00686 0.00256 C9 1 0.340495 0.536317 0.571225 11.00000 0.03030 0.02600 = 0.02604 0.00101 0.00300 0.00065 AFIX 43 H9 2 0.351386 0.497690 0.630820 11.00000 -1.20000 AFIX 0 C10 1 0.424125 0.599210 0.615013 11.00000 0.02418 0.02796 = 0.02537 0.00049 0.00462 0.00233 C11 1 0.521271 0.612762 0.753261 11.00000 0.02473 0.03097 = 0.02485 -0.00070 0.00411 0.00009 C12 1 0.570026 0.681159 0.792886 11.00000 0.03520 0.03030 = 0.02916 0.00153 0.00076 -0.00264 AFIX 43 H12 2 0.539481 0.718294 0.730320 11.00000 -1.20000 AFIX 0 C13 1 0.662787 0.695268 0.923021 11.00000 0.03594 0.03421 = 0.03180 -0.00316 0.00121 -0.00572 AFIX 43 H13 2 0.692641 0.742178 0.948944 11.00000 -1.20000 AFIX 0 C14 1 0.712728 0.641820 1.016078 11.00000 0.02595 0.04376 = 0.02538 -0.00094 0.00432 -0.00210 C15 1 0.665099 0.573505 0.975553 11.00000 0.03489 0.03782 = 0.02764 0.00551 0.00405 0.00159 AFIX 43 H15 2 0.698866 0.536268 1.037447 11.00000 -1.20000 AFIX 0 C16 1 0.569684 0.559036 0.846995 11.00000 0.03534 0.02967 = 0.03007 0.00013 0.00511 -0.00084 AFIX 43 H16 2 0.536780 0.512246 0.822170 11.00000 -1.20000 AFIX 0 C17 1 0.814184 0.657183 1.157251 11.00000 0.03944 0.05367 = 0.02753 -0.00043 0.00106 -0.00369 AFIX 137 H17A 2 0.871220 0.703007 1.159753 11.00000 -1.50000 H17B 2 0.904803 0.621204 1.186108 11.00000 -1.50000 H17C 2 0.732440 0.657319 1.217606 11.00000 -1.50000 AFIX 0 B1 3 0.346648 0.644100 0.386498 11.00000 0.03443 0.02838 = 0.02609 0.00270 0.00058 -0.00359 HKLF 4 REM 200K in P2(1)/c REM wR2 = 0.1211, GooF = S = 1.070, Restrained GooF = 1.070 for all data REM R1 = 0.0446 for 2906 Fo > 4sig(Fo) and 0.0612 for all 3886 data REM 210 parameters refined using 0 restraints END WGHT 0.0509 0.3608 REM Highest difference peak 0.239, deepest hole -0.232, 1-sigma level 0.044 Q1 1 0.1864 0.4985 0.4177 11.00000 0.05 0.24 Q2 1 0.4036 0.5640 0.5907 11.00000 0.05 0.22 Q3 1 0.4217 0.6696 0.2995 11.00000 0.05 0.21 Q4 1 0.7828 0.7099 1.1789 11.00000 0.05 0.20 Q5 1 0.9698 0.6542 1.1599 11.00000 0.05 0.19 REM The information below was added by Olex2. REM REM R1 = 0.0446 for 2906 Fo > 4sig(Fo) and 0.0612 for all 13592 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.24, deepest hole -0.23 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0612 REM R1_gt = 0.0446 REM wR_ref = 0.1211 REM GOOF = 1.070 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 13592 REM Reflections_gt = 2906 REM Parameters = n/a REM Hole = -0.23 REM Peak = 0.24 REM Flack = n/a ; _cod_data_source_file d0cc01505a2.cif _cod_data_source_block 200k_CCDC1 _cod_database_code 7126444 _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 0.969 _reflns_odcompleteness_completeness 99.69 _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: C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C17(H17A,H17B,H17C) ; _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 1.156 _oxdiff_exptl_absorpt_empirical_full_min 0.876 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 F1 F 0.24685(13) 0.70108(4) 0.33890(9) 0.0483(3) Uani 1 1 d . . . . . F2 F 0.48743(13) 0.63627(5) 0.32626(9) 0.0477(3) Uani 1 1 d . . . . . O1 O 0.41600(14) 0.65181(5) 0.53274(10) 0.0353(3) Uani 1 1 d . . . . . O2 O 0.23296(14) 0.58123(5) 0.35543(9) 0.0353(2) Uani 1 1 d . . . . . O3 O -0.11670(14) 0.41138(5) 0.06249(10) 0.0402(3) Uani 1 1 d . . . . . C1 C -0.2098(2) 0.35131(9) -0.00017(16) 0.0442(4) Uani 1 1 d . . . . . H1A H -0.259669 0.361284 -0.095181 0.066 Uiso 1 1 calc GR . . . . H1B H -0.305697 0.339690 0.044116 0.066 Uiso 1 1 calc GR . . . . H1C H -0.127741 0.311762 0.007580 0.066 Uiso 1 1 calc GR . . . . C2 C -0.04157(18) 0.40735(7) 0.19648(14) 0.0298(3) Uani 1 1 d . . . . . C3 C -0.05526(19) 0.35023(7) 0.27744(15) 0.0317(3) Uani 1 1 d . . . . . H3 H -0.120273 0.310038 0.240448 0.038 Uiso 1 1 calc R . . . . C4 C 0.0271(2) 0.35253(7) 0.41300(15) 0.0329(3) Uani 1 1 d . . . . . H4 H 0.016891 0.313672 0.468495 0.039 Uiso 1 1 calc R . . . . C5 C 0.12368(18) 0.41031(7) 0.46871(14) 0.0303(3) Uani 1 1 d . . . . . H5 H 0.180037 0.410949 0.561411 0.036 Uiso 1 1 calc R . . . . C6 C 0.13757(17) 0.46778(7) 0.38728(13) 0.0261(3) Uani 1 1 d . . . . . C7 C 0.05361(18) 0.46632(7) 0.25119(14) 0.0289(3) Uani 1 1 d . . . . . H7 H 0.061373 0.505518 0.195899 0.035 Uiso 1 1 calc R . . . . C8 C 0.24141(17) 0.53002(7) 0.44082(13) 0.0255(3) Uani 1 1 d . . . . . C9 C 0.34049(18) 0.53632(7) 0.57122(13) 0.0280(3) Uani 1 1 d . . . . . H9 H 0.351386 0.497690 0.630820 0.034 Uiso 1 1 calc R . . . . C10 C 0.42413(17) 0.59921(7) 0.61501(13) 0.0260(3) Uani 1 1 d . . . . . C11 C 0.52127(17) 0.61276(7) 0.75326(13) 0.0271(3) Uani 1 1 d . . . . . C12 C 0.57003(19) 0.68116(7) 0.79289(14) 0.0326(3) Uani 1 1 d . . . . . H12 H 0.539481 0.718294 0.730320 0.039 Uiso 1 1 calc R . . . . C13 C 0.6628(2) 0.69527(8) 0.92302(14) 0.0350(3) Uani 1 1 d . . . . . H13 H 0.692641 0.742178 0.948944 0.042 Uiso 1 1 calc R . . . . C14 C 0.71273(19) 0.64182(8) 1.01608(14) 0.0319(3) Uani 1 1 d . . . . . C15 C 0.6651(2) 0.57350(8) 0.97555(14) 0.0339(3) Uani 1 1 d . . . . . H15 H 0.698866 0.536268 1.037447 0.041 Uiso 1 1 calc R . . . . C16 C 0.56968(19) 0.55904(7) 0.84699(14) 0.0321(3) Uani 1 1 d . . . . . H16 H 0.536780 0.512246 0.822170 0.038 Uiso 1 1 calc R . . . . C17 C 0.8142(2) 0.65718(9) 1.15725(15) 0.0413(4) Uani 1 1 d . . . . . H17A H 0.871220 0.703007 1.159753 0.062 Uiso 1 1 calc GR . . . . H17B H 0.904803 0.621204 1.186108 0.062 Uiso 1 1 calc GR . . . . H17C H 0.732440 0.657319 1.217606 0.062 Uiso 1 1 calc GR . . . . B1 B 0.3466(2) 0.64410(8) 0.38650(16) 0.0306(3) Uani 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 F1 0.0560(6) 0.0307(5) 0.0466(6) 0.0021(4) -0.0126(4) 0.0039(4) F2 0.0410(6) 0.0652(6) 0.0374(5) -0.0026(4) 0.0097(4) -0.0098(4) O1 0.0460(6) 0.0298(5) 0.0258(5) 0.0030(4) -0.0005(4) -0.0095(4) O2 0.0444(6) 0.0311(5) 0.0264(5) 0.0030(4) -0.0006(4) -0.0087(4) O3 0.0478(7) 0.0389(6) 0.0281(5) -0.0025(4) -0.0033(5) -0.0077(5) C1 0.0484(10) 0.0478(9) 0.0332(8) -0.0119(7) 0.0027(7) -0.0131(7) C2 0.0281(7) 0.0309(7) 0.0285(7) -0.0037(5) 0.0028(5) 0.0008(5) C3 0.0308(8) 0.0254(6) 0.0378(8) -0.0046(5) 0.0054(6) -0.0011(5) C4 0.0362(8) 0.0258(7) 0.0358(8) 0.0033(5) 0.0062(6) -0.0001(5) C5 0.0314(7) 0.0297(7) 0.0283(7) 0.0000(5) 0.0037(5) 0.0013(5) C6 0.0246(7) 0.0264(6) 0.0272(7) -0.0028(5) 0.0060(5) 0.0018(5) C7 0.0304(7) 0.0275(7) 0.0281(7) 0.0000(5) 0.0050(5) -0.0002(5) C8 0.0243(6) 0.0253(6) 0.0272(7) -0.0004(5) 0.0069(5) 0.0026(5) C9 0.0303(7) 0.0260(6) 0.0260(7) 0.0010(5) 0.0030(5) 0.0007(5) C10 0.0242(7) 0.0280(6) 0.0254(6) 0.0005(5) 0.0046(5) 0.0023(5) C11 0.0247(7) 0.0310(7) 0.0248(6) -0.0007(5) 0.0041(5) 0.0001(5) C12 0.0352(8) 0.0303(7) 0.0292(7) 0.0015(5) 0.0008(6) -0.0026(5) C13 0.0359(8) 0.0342(7) 0.0318(7) -0.0032(6) 0.0012(6) -0.0057(6) C14 0.0259(7) 0.0438(8) 0.0254(7) -0.0009(6) 0.0043(5) -0.0021(5) C15 0.0349(8) 0.0378(8) 0.0276(7) 0.0055(6) 0.0041(6) 0.0016(6) C16 0.0353(8) 0.0297(7) 0.0301(7) 0.0001(5) 0.0051(6) -0.0008(5) C17 0.0394(9) 0.0537(10) 0.0275(8) -0.0004(6) 0.0011(6) -0.0037(7) B1 0.0344(9) 0.0284(8) 0.0261(8) 0.0027(6) 0.0006(6) -0.0036(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 O1 B1 121.96(11) . . ? C8 O2 B1 121.96(11) . . ? C2 O3 C1 117.51(11) . . ? 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 . . ? O3 C2 C3 124.76(12) . . ? O3 C2 C7 115.07(12) . . ? C3 C2 C7 120.16(12) . . ? C2 C3 H3 120.3 . . ? C4 C3 C2 119.34(12) . . ? C4 C3 H3 120.3 . . ? C3 C4 H4 119.4 . . ? C5 C4 C3 121.28(13) . . ? C5 C4 H4 119.4 . . ? C4 C5 H5 120.3 . . ? C4 C5 C6 119.40(13) . . ? C6 C5 H5 120.3 . . ? C5 C6 C8 121.63(12) . . ? C7 C6 C5 119.77(12) . . ? C7 C6 C8 118.60(12) . . ? C2 C7 C6 120.04(12) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O2 C8 C6 114.76(11) . . ? O2 C8 C9 120.80(12) . . ? C9 C8 C6 124.43(12) . . ? C8 C9 H9 120.0 . . ? C8 C9 C10 120.06(12) . . ? C10 C9 H9 120.0 . . ? O1 C10 C9 120.60(12) . . ? O1 C10 C11 115.14(11) . . ? C9 C10 C11 124.24(12) . . ? C12 C11 C10 119.43(12) . . ? C12 C11 C16 118.53(12) . . ? C16 C11 C10 122.03(12) . . ? C11 C12 H12 119.7 . . ? C13 C12 C11 120.50(13) . . ? C13 C12 H12 119.7 . . ? C12 C13 H13 119.5 . . ? C12 C13 C14 121.08(13) . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 118.16(13) . . ? C13 C14 C17 121.03(13) . . ? C15 C14 C17 120.81(13) . . ? C14 C15 H15 119.4 . . ? C16 C15 C14 121.22(13) . . ? C16 C15 H15 119.4 . . ? C11 C16 H16 119.8 . . ? C15 C16 C11 120.49(13) . . ? C15 C16 H16 119.8 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F1 B1 F2 111.72(12) . . ? F1 B1 O1 109.17(12) . . ? F1 B1 O2 108.20(12) . . ? F2 B1 O1 108.74(12) . . ? F2 B1 O2 107.94(12) . . ? O1 B1 O2 111.09(11) . . ? 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 F1 B1 1.3616(17) . ? F2 B1 1.378(2) . ? O1 C10 1.3049(16) . ? O1 B1 1.4781(18) . ? O2 C8 1.3050(15) . ? O2 B1 1.4827(18) . ? O3 C1 1.4296(17) . ? O3 C2 1.3645(16) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.390(2) . ? C2 C7 1.3942(18) . ? C3 H3 0.9500 . ? C3 C4 1.390(2) . ? C4 H4 0.9500 . ? C4 C5 1.3838(19) . ? C5 H5 0.9500 . ? C5 C6 1.3990(18) . ? C6 C7 1.3971(18) . ? C6 C8 1.4720(17) . ? C7 H7 0.9500 . ? C8 C9 1.3854(18) . ? C9 H9 0.9500 . ? C9 C10 1.3923(18) . ? C10 C11 1.4668(18) . ? C11 C12 1.3972(19) . ? C11 C16 1.3983(19) . ? C12 H12 0.9500 . ? C12 C13 1.3885(19) . ? C13 H13 0.9500 . ? C13 C14 1.391(2) . ? C14 C15 1.396(2) . ? C14 C17 1.5085(19) . ? C15 H15 0.9500 . ? C15 C16 1.383(2) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 O1 C10 C11 C12 10.82(19) . . . . ? O1 C10 C11 C16 -168.13(13) . . . . ? O2 C8 C9 C10 3.8(2) . . . . ? O3 C2 C3 C4 -179.83(13) . . . . ? O3 C2 C7 C6 -179.42(12) . . . . ? C1 O3 C2 C3 -2.8(2) . . . . ? C1 O3 C2 C7 177.48(13) . . . . ? C2 C3 C4 C5 -0.5(2) . . . . ? C3 C2 C7 C6 0.9(2) . . . . ? C3 C4 C5 C6 0.5(2) . . . . ? C4 C5 C6 C7 0.2(2) . . . . ? C4 C5 C6 C8 -178.83(13) . . . . ? C5 C6 C7 C2 -0.9(2) . . . . ? C5 C6 C8 O2 -175.75(12) . . . . ? C5 C6 C8 C9 3.5(2) . . . . ? C6 C8 C9 C10 -175.45(12) . . . . ? C7 C2 C3 C4 -0.1(2) . . . . ? C7 C6 C8 O2 5.20(18) . . . . ? C7 C6 C8 C9 -175.52(12) . . . . ? C8 O2 B1 F1 -139.64(13) . . . . ? C8 O2 B1 F2 99.30(14) . . . . ? C8 O2 B1 O1 -19.82(19) . . . . ? C8 C6 C7 C2 178.17(12) . . . . ? C8 C9 C10 O1 -2.7(2) . . . . ? C8 C9 C10 C11 175.49(12) . . . . ? C9 C10 C11 C12 -167.45(13) . . . . ? C9 C10 C11 C16 13.6(2) . . . . ? C10 O1 B1 F1 140.18(13) . . . . ? C10 O1 B1 F2 -97.70(15) . . . . ? C10 O1 B1 O2 20.95(19) . . . . ? C10 C11 C12 C13 -179.69(13) . . . . ? C10 C11 C16 C15 178.38(13) . . . . ? C11 C12 C13 C14 1.4(2) . . . . ? C12 C11 C16 C15 -0.6(2) . . . . ? C12 C13 C14 C15 -0.8(2) . . . . ? C12 C13 C14 C17 179.73(14) . . . . ? C13 C14 C15 C16 -0.5(2) . . . . ? C14 C15 C16 C11 1.2(2) . . . . ? C16 C11 C12 C13 -0.7(2) . . . . ? C17 C14 C15 C16 178.97(14) . . . . ? B1 O1 C10 C9 -10.9(2) . . . . ? B1 O1 C10 C11 170.81(12) . . . . ? B1 O2 C8 C6 -172.05(12) . . . . ? B1 O2 C8 C9 8.6(2) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 2 8016.7 204.14 4 0 0 2 8044.54 209.242 8 0 0 -2 8210.52 213.198 1 0 0 -2 8127.79 203.297 4 0 0 -2 7833.9 201.176 2 0 0 2 8004.74 212.59 1 0 0 2 7474.63 200.698 2 0 0 -3 -1.92415 8.6396 1 0 0 -3 -3.26506 7.62953 8 0 0 3 3.43005 6.28753 4 0 0 3 -3.06986 8.08156 8 0 0 3 1.83826 9.67862 1 0 0 4 117.067 17.6267 8 0 0 -4 132.662 19.9578 1 0 0 4 114.075 19.9264 1 0 0 4 76.9343 13.1598 4 0 0 5 1.92196 10.4218 4 0 0 -5 -3.28754 13.4755 1 0 0 5 12.5908 12.8506 8 0 0 6 1863.13 77.5589 4 0 0 -6 2167 98.7387 1 0 0 -7 -9.5007 16.2914 1 0 0 7 2.11179 10.0584 6 0 0 7 34.6914 15.0779 4 0 0 8 20.8708 15.9472 4 0 0 -8 5.54244 21.5616 1 0 0 8 41.2694 14.5731 6 0 0 9 -6.51424 16.0762 4 0 0 -9 44.3999 30.7619 1 0 0 -10 1390.47 100.678 1 0 0 -11 -15.8443 28.1241 1 0 0 -12 372.814 63.7102 1 0 1 1 18840.1 465.263 1 0 1 2 22176.7 554.951 8 0 1 2 21975.6 548.674 6 0 1 2 21242.3 556.395 1 0 1 2 22321.2 546.054 4 0 -1 -2 22494.8 545.604 4 0 1 -2 22595.5 557.878 1 0 -1 3 9746.05 254.378 4 0 1 -3 9633.38 246.113 2 0 1 3 9507.77 247.251 4 0 -1 3 9244.19 255.085 8 0 -1 -3 9238.17 258.911 8 0 1 3 9493.21 258.613 8 0 -1 -3 9357.93 245.747 4 0 1 3 9731.19 249.359 6 0 1 3 9093.67 261.233 1 0 1 -3 10007.2 264.337 1 0 1 3 9800.1 247.811 2 0 1 4 15501.9 395.842 6 0 1 4 15284.6 408.027 8 0 1 4 15132.6 414.341 1 0 -1 4 15418 402.107 4 0 1 -4 15908.9 417.187 1 0 1 -4 15169.4 391.452 2 0 1 4 15641.5 394.073 2 0 -1 -4 15010.9 409.196 8 0 -1 -4 15342.2 392.211 4 0 -1 4 15141.2 405.201 8 0 1 4 15686.4 395.189 4 0 -1 -5 16875.6 448.091 8 0 1 5 16594 424.578 2 0 1 5 16509.9 428.255 6 0 -1 5 15974.9 434.666 4 0 1 -5 16488.7 453.719 1 0 1 -5 16801.4 424.364 2 0 -1 5 16195 440.402 8 0 1 5 16576.3 428.488 4 0 1 5 16640.2 443.785 8 0 1 -6 92.0191 21.7693 1 0 1 6 54.3318 14.3193 4 0 1 6 90.2532 15.55 6 0 -1 6 76.4788 17.1064 4 0 1 7 19.3099 11.7159 4 0 1 -7 4.76221 15.7445 1 0 1 7 30.1706 13.2584 6 0 -1 7 20.3037 12.7583 4 0 -1 8 50.2693 14.5278 6 0 1 8 34.9654 16.1816 4 0 1 8 28.9028 13.6278 6 0 1 -8 38.947 24.4671 1 0 -1 8 6.54931 14.0965 4 0 1 9 -11.6189 13.5773 4 0 1 -9 -6.35687 21.0085 1 0 -1 9 -10.6609 18.1361 4 0 1 -10 1664.24 112.548 1 0 1 -11 277.393 52.8068 1 0 1 -12 182.412 51.1666 1 0 2 -1 21826.4 545.759 1 0 2 1 22582.7 545.613 1 0 2 1 21796.1 549.292 7 0 -2 -1 22566.8 547.707 6 0 -2 -1 21958 550.723 7 0 -2 -2 3460.13 104.058 6 0 2 2 3528.71 103.435 6 0 -2 -2 3784.13 98.3612 4 0 2 2 3538.25 108.426 7 0 2 -2 3714.91 108.832 1 0 2 2 3749.99 108.693 1 0 -2 -3 2235.84 68.3788 4 0 2 3 2278.35 69.1275 4 0 2 3 2289.18 82.925 1 0 2 -3 2309.46 83.7924 1 0 2 3 2285.93 74.5739 6 0 2 4 537.585 28.0278 4 0 2 4 531.285 30.4869 6 0 -2 -4 518.139 36.9941 8 0 -2 4 585.343 35.7736 4 0 -2 4 586.077 35.0633 8 0 -2 -4 555.49 27.7089 4 0 2 4 511.878 37.7065 1 0 2 -4 589.655 39.7951 1 0 2 -5 88472.7 2120.52 1 0 2 5 83881.2 2087.31 4 0 -2 -5 81003.8 2110.8 8 0 2 5 88658.2 2091.78 2 0 -2 5 84799 2103.65 4 0 2 -5 83197.8 2087.32 2 0 2 5 89610.4 2093.3 6 0 -2 -5 84245.3 2084.16 4 0 -2 5 86069.1 2102.37 8 0 2 6 4193.11 131.256 2 0 2 6 4268.76 130.945 4 0 2 -6 4301.93 158.505 1 0 -2 -6 4285.1 153.64 8 0 -2 6 3686.99 138.823 4 0 2 -6 4223.03 128.533 2 0 2 6 4243.08 133.631 6 0 -2 -7 1450.73 81.1295 8 0 2 -7 1337.45 82.448 1 0 -2 7 1386.34 71.1074 4 0 2 7 1334.86 60.0054 4 0 2 7 1313.82 62.5999 6 0 -2 8 124.721 24.8622 4 0 2 -8 122.662 30.8256 1 0 2 8 141.556 21.4434 4 0 2 -9 12.738 21.8488 1 0 -2 9 19.457 17.4817 4 0 2 9 31.1331 15.2362 4 0 -2 10 824.322 61.8577 4 0 2 -10 787.328 76.465 1 0 2 -11 500.071 66.1783 1 0 2 -12 60.8836 36.5604 1 0 -3 0 -0.65336 4.97424 3 0 3 1 3343.98 90.7748 1 0 -3 -1 3280.05 98.4377 7 0 -3 1 3414.31 91.3465 1 0 -3 -1 3261.38 90.441 1 0 3 -1 3306.87 90.9912 1 0 -3 -2 1971.75 66.4994 1 0 -3 2 1907.82 65.8912 1 0 -3 -2 2070.23 67.5296 6 0 3 2 1887.03 65.0144 6 0 3 2 1867.72 68.4411 7 0 3 -2 2026.25 67.2565 1 0 3 2 1937.36 65.8068 1 0 -3 3 14423.4 382.99 1 0 -3 -3 14649.9 367.044 4 0 3 3 14510.5 383.731 1 0 3 3 14720.7 376.044 6 0 -3 -3 14285 378.578 6 0 3 -3 14426.8 384.889 1 0 -3 -3 14652.1 384.508 1 0 3 3 14855.8 385.314 7 0 -3 -4 6259.43 196.767 1 0 -3 -4 6556.38 175.467 4 0 3 4 6848.77 197.913 1 0 3 4 6404.19 193.886 7 0 3 4 6420.62 184.539 6 0 -3 -4 6384.62 198.426 8 0 3 -4 6309.92 197.79 1 0 -3 4 6721.64 196.975 1 0 -3 -5 566.318 43.1678 8 0 -3 -5 501.247 28.0566 4 0 -3 -5 561.446 42.8695 1 0 3 5 560.531 34.6916 6 0 -3 5 480.481 37.5826 4 0 -3 5 547.52 38.0265 8 0 3 -5 573.843 43.9201 1 0 -3 -6 316.966 23.2034 4 0 -3 -6 343.448 36.3053 8 0 -3 6 305.211 32.8688 4 0 3 6 302.025 26.453 2 0 3 6 314.842 24.2874 4 0 3 -6 273.567 24.375 2 0 -3 -6 401.96 40.7879 1 0 3 -6 274.137 35.0406 1 0 3 6 268.011 26.6047 6 0 3 7 988.104 47.2757 4 0 3 -7 996.181 69.9256 1 0 3 7 902.354 50.3407 6 0 -3 7 837.536 56.336 4 0 3 7 1009.16 51.1093 2 0 -3 -7 1011.79 67.174 8 0 3 -7 896.767 46.4227 2 0 -3 -7 931.435 68.0311 1 0 -3 8 1255.05 72.3859 4 0 -3 -8 1151.59 78.1666 8 0 -3 -8 1264.05 83.9273 1 0 3 -8 1084.28 80.2479 1 0 -3 9 320.084 39.5041 4 0 -3 -9 390.604 52.6423 1 0 3 -9 356.967 51.6204 1 0 3 -10 315.26 51.0292 1 0 -3 10 307.749 42.3956 4 0 -3 -10 347.066 54.8602 1 0 -3 -11 86.3341 36.7764 1 0 3 -11 143.072 42.5623 1 0 -3 -12 654.609 77.6613 1 0 3 -12 617.806 78.4259 1 0 4 0 206047 4990.88 3 0 -4 0 206574 4990.3 3 0 -4 -1 27760.7 675.268 1 0 4 1 27703.7 675.682 1 0 -4 -1 27682.1 689.987 7 0 4 -1 27078.5 675.812 1 0 -4 1 27493.3 675.857 1 0 -4 1 27761.4 678.321 3 0 -4 2 2441.04 76.9263 1 0 4 2 2424.61 82.2398 7 0 4 2 2462.51 76.8758 1 0 -4 -2 2329.19 79.4338 6 0 -4 -2 2335.72 75.6972 1 0 4 -2 2327.39 76.2332 1 0 4 -3 1939.14 74.3901 1 0 -4 -3 2030.41 63.2018 4 0 -4 -3 1932.69 72.6102 6 0 -4 3 1894.67 73.1251 1 0 4 3 1889.17 75.9329 7 0 -4 -3 1943.42 73.9695 1 0 4 3 1988.7 73.7632 1 0 -4 4 4837.27 149.168 1 0 4 4 4549.78 147.592 1 0 4 4 4551.95 149.233 7 0 4 4 4704.26 140.404 6 0 -4 -4 4394.57 152.213 8 0 -4 -4 4279.02 147.594 1 0 -4 -4 4519.28 143.468 6 0 4 -4 4596.23 150.755 1 0 -4 -4 4548.7 129.05 4 0 4 5 3825.31 122.59 6 0 -4 -5 3859.26 111.361 4 0 -4 -5 3450.91 135.225 8 0 -4 5 3426.83 130.495 4 0 4 -5 3752.33 137.52 1 0 -4 -5 3704.22 136.578 1 0 4 -6 4857.54 173.868 1 0 -4 -6 4884.86 173.848 8 0 -4 -6 4734.81 137.694 4 0 -4 6 4779.45 164.374 4 0 -4 -6 4559.94 170.068 1 0 4 6 4683.72 149.83 6 0 4 6 4530.01 150.89 2 0 -4 -7 680.967 55.4037 8 0 -4 -7 657.408 56.1384 1 0 4 -7 631.516 38.277 2 0 -4 7 663.867 50.5547 4 0 4 7 490.695 37.0462 2 0 4 -7 736.287 58.733 1 0 -4 -8 539.327 52.1564 8 0 4 8 575.946 39.9893 2 0 -4 8 473.617 46.5469 4 0 4 -8 475.924 34.5241 2 0 4 -8 386.524 50.1733 1 0 -4 -8 539.819 54.5355 1 0 4 -9 976.501 80.164 1 0 -4 9 1013.43 69.8664 4 0 -4 -9 986.725 79.8849 1 0 4 -10 251.019 47.2308 1 0 -4 -10 169.624 39.745 1 0 -4 10 236.394 38.8973 4 0 4 -11 31.7691 29.1408 1 0 -4 -11 70.477 33.6841 1 0 4 -12 -17.4183 33.8671 1 0 -4 -12 -8.55804 28.2827 1 0 5 0 6.70631 7.17282 3 0 -5 -1 808.73 40.5647 7 0 5 -1 853.106 29.9567 1 0 -5 1 885.328 34.0235 3 0 -5 -1 838.648 29.268 1 0 5 1 831.243 29.2523 1 0 -5 1 822.064 29.7336 1 0 -5 -2 7998.51 223.688 6 0 5 2 7919.12 225.164 7 0 5 2 8128.25 214.864 1 0 5 -2 8041.72 215.714 1 0 -5 -2 7850.73 214.389 1 0 -5 -2 8238.98 229.701 7 0 -5 2 8088.48 215.125 1 0 5 3 1829.04 68.3958 1 0 -5 -3 1608.83 66.3248 1 0 5 3 1583.63 69.5956 7 0 5 -3 1664.03 67.4995 1 0 -5 3 1712.29 66.9435 1 0 -5 -3 1803.47 70.7328 6 0 -5 -4 3279.87 114.449 6 0 -5 -4 3297.15 116.757 1 0 -5 -4 3297.78 98.9724 4 0 5 4 3429.1 115.699 1 0 5 -4 3248.63 116.971 1 0 -5 4 3252.89 114.747 1 0 5 4 3036.52 115.293 7 0 5 -5 555.966 43.4527 1 0 -5 -5 532.24 44.4853 8 0 -5 -5 426.205 38.7236 1 0 -5 -5 596.543 30.6503 4 0 5 5 520.134 36.2515 6 0 -5 -6 3067.98 98.5383 4 0 -5 6 3265.35 127.089 4 0 -5 -6 3091.05 128.698 1 0 5 -6 3374.58 133.35 1 0 -5 -6 3011.4 130.455 8 0 -5 7 627.005 51.4503 4 0 5 -7 585.996 37.7159 2 0 -5 -7 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895.177 65.0535 1 1 -6 -7 930.452 70.3048 8 1 6 -6 -7.73196 14.1739 1 1 -6 -6 -3.78153 12.4972 1 1 -6 -5 2106.12 92.1794 1 1 6 -5 2172.61 93.5592 1 -1 6 4 546.975 36.6232 1 -1 -6 4 502.801 34.4283 5 -1 6 4 477.713 33.8961 5 1 -6 -4 514.163 36.5728 1 1 6 -4 392.342 32.8975 1 1 -6 -4 414.807 39.3065 8 -1 6 4 496.184 36.4093 6 -1 -6 4 542.552 36.242 1 1 -6 -3 2146.78 77.845 1 -1 6 3 2087.72 75.1465 5 -1 -6 3 2120.81 75.8675 5 1 -6 -3 2098.2 86.3846 6 1 -6 -3 2175.56 90.0823 8 -1 6 3 2145.92 77.0786 1 -1 -6 3 2105.07 76.6226 1 1 6 -3 2015.85 76.5918 1 -1 6 2 3239.08 97.1482 1 -1 -6 2 2978.99 96.5808 1 1 6 -2 3272.07 97.4357 1 -1 6 2 3218.64 95.8792 5 1 -6 -2 3150.34 97.4465 5 -1 -6 2 3331.66 96.7193 5 -1 6 2 3138.84 107.044 6 1 -6 -2 3191.62 96.9053 1 1 -6 -2 3227.13 112.122 7 1 -6 -2 3057.53 109.766 6 1 6 -2 3048.67 96.5876 5 1 6 -1 31798.7 771.863 3 1 -6 -1 31531.2 797.979 3 1 6 -1 30540.8 777.159 5 -1 -6 1 31494.1 776.871 1 -1 -6 1 32533.2 776.583 5 1 -6 -1 32226.2 777.613 5 -1 6 1 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29.3372 16.7613 2 -3 2 6 43.4766 20.5066 3 -3 2 5 6709.19 214.688 2 -3 2 5 6108.19 172.025 4 -3 -2 5 6571.39 192.457 3 3 2 -5 6764.75 210.409 1 3 2 -5 6517.78 209.737 5 -3 2 4 5999.9 204.515 2 -3 2 4 6278.26 176.308 4 3 2 -4 6648.4 202.363 1 -3 2 4 5781.62 196.953 3 -3 -2 4 6366.55 184.759 3 3 2 -4 6485.31 200.629 5 -3 -2 3 21.846 10.0117 3 -3 2 3 34.7895 15.3581 2 3 2 -3 28.0812 14.8054 2 -3 2 3 33.1388 11.2169 4 -3 2 3 43.3104 14.9772 8 3 2 -3 26.2724 11.7798 3 3 -2 -3 32.0921 15.1976 3 -3 2 3 38.2262 13.5206 5 -3 2 3 47.6112 14.8185 1 -3 2 3 21.4465 13.0246 3 3 2 -3 45.9012 15.6707 5 -3 2 2 2301.17 85.0354 4 3 2 -2 2198.62 89.5092 2 3 -2 -2 2310.92 88.546 3 3 2 -2 2286.24 79.9894 3 -3 2 2 2368.98 88.5846 5 3 2 -2 2278.48 89.5132 5 -3 2 2 2390.23 91.9922 3 -3 2 2 2320.78 84.6112 8 3 -2 -2 2377.1 87.211 4 -3 2 1 15188.5 416.231 2 -3 2 1 14853.4 413.063 4 3 -2 -1 16132.4 418.987 4 -3 2 1 15861.5 401.522 8 -3 -2 1 15760.3 417.113 4 -3 2 1 15201.7 412.377 5 3 2 -1 15261.9 414.383 5 3 -2 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4 -3 3 0 255.067 17.1565 8 3 -3 0 266.124 26.5635 5 3 3 0 242.769 26.0447 5 -3 3 0 216.447 26.3062 4 3 3 1 1535.06 74.1793 5 -3 3 -1 1644.86 67.4194 2 -3 3 -1 1769.28 79.3628 4 3 -3 1 1651.91 75.4174 5 -3 3 -1 1735.62 60.3671 6 -3 3 -2 2639.53 88.6928 2 3 -3 2 2551.02 112.91 4 -3 3 -2 2648.68 78.2335 6 3 -3 3 38.1893 18.3193 4 -3 -3 -3 75.3951 14.463 7 -3 3 -3 79.1581 11.639 2 -3 3 -4 269.842 14.6285 2 -3 -3 -4 294.641 27.4962 7 3 -3 4 272.159 36.5857 4 -3 -3 -5 17.0649 11.6599 8 -3 -3 -5 10.4927 7.60598 6 -3 -3 -5 -5.04369 17.9051 1 3 -3 5 10.271 17.6128 4 -3 3 -5 -5.1055 18.1244 1 -3 -3 -6 5.67089 18.0067 1 -3 3 -6 57.3615 24.0937 1 -3 -3 -6 13.0466 14.3389 8 3 -3 6 5.64479 23.71 4 3 -3 6 9.56946 9.21079 7 3 3 6 -4.78265 18.0753 4 -3 -3 -7 166.506 38.2813 1 -3 -3 -7 180.005 28.6945 8 3 -3 7 164.237 37.2305 4 -3 3 -7 207.262 42.1959 1 -3 3 -8 1521.31 107.113 1 3 -3 8 1554.92 102.119 4 -3 -3 -8 1604.41 109.434 1 -3 -3 -8 1336.69 78.5085 8 3 -3 9 48.0767 33.318 4 -3 -3 -9 7.79809 28.599 1 -3 3 -9 47.2675 33.0968 1 -3 -3 -10 8.52012 31.2383 1 -3 3 -10 17.2169 30.5601 1 3 -3 10 21.4072 26.9685 4 -3 -3 -11 9.30772 35.1838 1 -3 3 -11 75.1836 43.9288 1 3 4 -13 159.794 48.3052 1 3 -4 -13 175.336 49.042 1 3 -4 -12 306.481 54.9276 1 3 4 -12 375.575 60.4167 1 3 4 -11 -14.8971 27.3074 1 3 -4 -11 29.4169 31.6153 1 3 -4 -10 8309.9 298.547 1 3 4 -10 8383.62 299.389 1 3 -4 -9 238.429 43.0129 1 3 4 -9 229.21 42.0899 1 -3 4 9 212.695 36.3051 2 3 4 -8 525.687 54.2349 1 -3 4 8 450.644 51.0375 2 3 -4 -8 487.737 51.6121 1 -3 4 7 2239.99 113.224 2 3 -4 -7 2223.61 110.921 1 3 4 -7 2415.46 114.235 1 -3 4 6 2064.97 104.528 2 -3 4 6 2018.07 104.365 3 3 -4 -6 2135.35 102.284 1 3 4 -6 2145.68 103.069 1 3 4 -6 2178.18 103.921 5 3 -4 -6 2443.57 109.129 5 -3 4 5 2669.57 79.1653 4 -3 4 5 2696.66 119.477 2 -3 -4 5 2860.98 96.2713 3 -3 4 5 2646.58 117.098 3 3 -4 -5 2917.33 117.273 1 3 4 -5 2951.65 117.296 1 3 4 -5 2912.72 117.573 5 3 -4 -5 2843.83 116.414 5 -3 4 4 1136.71 46.381 4 -3 4 4 1240.28 71.5198 2 3 -4 -4 1309.1 66.6968 1 3 4 -4 1180.22 65.0355 1 -3 -4 4 1242.41 49.9383 3 3 4 -4 1126.52 63.0186 5 3 -4 -4 1186.53 64.4583 5 -3 4 4 1266.22 70.0278 3 -3 4 3 13.3665 10.9388 4 -3 -4 3 3.51259 6.87575 3 -3 4 3 10.4609 13.5614 2 -3 4 3 5.23658 12.4719 8 -3 4 3 31.0823 13.5108 1 -3 -4 3 7.12595 12.5086 1 3 -4 -3 11.0167 10.2394 4 -3 -4 3 4.79728 10.7729 5 -3 4 3 26.2452 13.6587 5 -3 4 3 6.50733 12.6543 3 3 4 -3 16.1702 12.8373 5 3 -4 -3 18.7913 12.056 5 -3 4 2 714.925 41.0863 4 3 -4 -2 812.166 45.3858 4 -3 4 2 750.134 43.214 1 -3 -4 2 709.429 42.2669 1 -3 -4 2 780.106 44.1505 5 -3 4 2 761.172 43.7654 5 3 4 -2 819.014 34.4124 3 3 4 -2 753.11 45.1323 5 3 -4 -2 769.017 44.6497 5 -3 4 2 806.641 50.644 3 -3 4 2 775.396 43.2583 8 -3 4 1 2088.84 79.1604 6 -3 4 1 2089.9 82.8399 4 3 -4 -1 1893.05 83.5108 4 -3 4 1 2054.95 72.7714 8 -3 4 1 2047.84 79.9373 5 -3 -4 1 2041.65 79.4701 5 3 -4 -1 1964.22 80.0201 5 -3 4 1 2008.42 86.9283 3 3 4 -1 2011.9 80.9789 5 -3 4 0 6353.26 200.935 4 3 -4 0 6570.78 207.521 4 -3 4 0 6612.84 175.998 7 -3 4 0 6636.14 187.654 6 3 -4 0 6655.37 199.668 5 3 4 0 6488.3 199.511 5 3 -4 0 6503.62 201.765 3 3 4 1 11386 324.816 5 3 -4 1 11649.7 325.048 5 -3 4 -1 11566.8 302.829 6 3 -4 2 1998.66 97.3179 4 3 -4 3 10023.4 310.815 4 -3 -4 -3 9907.04 279.568 7 -3 4 -4 103.844 11.9867 2 -3 -4 -4 83.8568 17.9018 7 3 -4 4 88.0317 27.3651 4 -3 -4 -5 220.707 36.3158 1 -3 -4 -5 311.843 32.5454 8 -3 -4 -5 304.473 23.8914 6 -3 4 -5 310.965 41.8742 1 3 -4 5 322.524 42.6918 4 -3 4 -6 5.73491 19.6672 1 -3 -4 -6 -3.60184 12.7857 8 -3 -4 -6 -5.64686 20.0449 1 3 -4 6 -5.79147 23.1375 4 -3 -4 -7 2431.27 129.556 1 -3 4 -7 2117.94 122.979 1 3 -4 7 2229.27 124.141 4 -3 -4 -7 2232.16 104.993 8 3 -4 8 128.332 37.2942 4 -3 -4 -8 168.111 31.5367 8 -3 -4 -8 127.821 35.8054 1 -3 4 -8 122.415 35.699 1 -3 4 -9 -7.87432 27.9517 1 -3 -4 -9 4.79146 17.0084 8 -3 -4 -9 7.76471 24.6527 1 3 -4 9 -7.1494 27.8007 4 -3 -4 -10 25.4797 29.127 1 -3 4 -10 8.60536 30.5473 1 3 -4 10 -7.46871 28.2247 4 -3 -4 -11 1223.64 111.43 1 -3 4 -11 1427.93 118.571 1 3 -5 -13 52.5201 36.7798 1 3 5 -13 35.5171 34.5432 1 3 -5 -12 1352.41 107.07 1 3 5 -12 1356.65 106.462 1 3 -5 -11 227.658 46.1061 1 3 5 -11 320.474 52.422 1 -3 5 10 3507.33 155.459 2 3 -5 -10 3362.03 163.173 1 3 5 -10 3308.72 162.815 1 3 -5 -9 119.284 34.4249 1 3 5 -9 229.483 41.657 1 -3 5 9 229.039 39.5775 2 -3 5 8 383.391 47.8583 2 3 -5 -8 444.981 50.0357 1 3 5 -8 413.102 47.9514 1 -3 5 7 4396.11 175.081 2 3 5 -7 4724.53 175.563 1 3 -5 -7 4372.12 171.608 1 -3 5 7 4209.81 176.689 3 3 5 -6 91.7014 22.297 5 3 -5 -6 75.7837 21.8498 5 3 -5 -6 32.5131 17.0968 1 3 5 -6 12.2837 14.0746 1 -3 -5 6 33.4491 12.9619 3 -3 5 6 51.5416 19.2297 3 -3 5 6 37.0919 18.5481 2 -3 5 5 7080.28 238.141 2 -3 5 5 6795.59 234.923 3 3 -5 -5 7236.86 229.548 1 3 5 -5 7451.27 231.16 1 -3 -5 5 7207.77 200.155 3 3 5 -5 7162.44 229.063 5 3 -5 -5 7396.56 230.524 5 3 -5 -5 6721.18 235.152 8 3 -5 -4 1560.91 77.3684 1 3 5 -4 1740.2 82.1317 1 3 -5 -4 1662.54 84.2065 8 -3 5 4 1768.14 88.1516 3 3 -5 -4 1731.43 80.1976 5 -3 -5 4 1694.99 58.0197 3 3 5 -4 1855.74 82.8518 5 3 -5 -4 1689.43 62.0042 4 -3 5 3 625.598 34.5478 4 3 -5 -3 590.031 41.5661 5 3 -5 -3 570.159 35.3709 4 -3 5 3 522.063 39.0907 8 3 -5 -3 504.614 40.4141 8 -3 5 3 618.984 40.0762 1 -3 5 3 617.859 40.0995 5 -3 -5 3 571.685 38.5483 1 -3 -5 3 647.443 41.1703 5 -3 5 3 606.703 46.9396 3 3 5 -3 563.121 40.4752 5 -3 5 2 460.112 33.4814 4 3 -5 -2 494.701 35.5495 4 -3 5 2 531.037 35.0783 8 -3 5 2 448.772 35.1115 6 3 5 -2 546.801 36.8152 5 -3 5 2 497.35 33.9794 1 -3 -5 2 396.505 33.7575 1 -3 5 2 484.16 34.176 5 3 5 -2 476.802 23.4164 3 3 -5 -2 472.913 34.5058 5 -3 5 2 502.359 40.4891 3 -3 -5 2 498.072 34.6938 5 3 -5 -2 521.331 36.2713 8 3 -5 -1 562.396 41.0416 4 3 5 -1 581.922 37.8758 5 -3 5 1 556.596 32.1222 7 3 -5 -1 472.754 31.5977 8 -3 5 1 508.36 35.4008 5 -3 5 1 496.563 34.651 6 -3 -5 1 641.877 38.5011 5 3 -5 -1 589.707 38.3909 5 3 -5 -1 581.105 42.0323 3 -3 5 1 536.914 42.4401 3 -3 5 1 572.111 39.3788 4 3 -5 0 28383.3 717.985 5 -3 5 0 28509.6 723.28 4 3 -5 0 26146.1 725.585 4 3 -5 0 27940.3 695.962 8 -3 5 0 27965.2 693.206 7 -3 5 0 28097.5 706.269 6 3 5 0 27972.6 717.515 5 -3 5 -1 6547.93 182.32 6 3 -5 1 6510.23 200.572 5 3 5 1 6362.19 200.51 5 3 -5 2 77.7617 24.9527 4 3 -5 3 49.952 19.993 4 -3 -5 -3 45.8535 13.8112 7 3 -5 4 418.695 47.2374 4 -3 -5 -4 420.875 37.2431 7 3 -5 5 3924.86 166.899 4 -3 -5 -5 4327.57 166.954 1 -3 5 -5 4059.52 165.003 1 3 -5 5 3760.93 103.736 7 -3 -5 -5 4013.99 125.886 6 3 -5 6 3099.71 146.754 4 -3 -5 -6 2879.47 139.08 1 -3 5 -6 3039.39 142.997 1 -3 -5 -6 2856.29 99.7765 6 -3 -5 -6 2621.93 117.85 8 -3 -5 -7 25.4673 21.8395 1 -3 5 -7 25.9406 22.2452 1 -3 -5 -7 12.9661 17.722 8 3 -5 7 19.5679 25.3681 4 -3 -5 -8 273.96 39.7185 8 3 -5 8 277.512 49.6662 4 -3 -5 -8 246.91 45.7079 1 -3 5 -8 258.505 47.8859 1 3 -5 9 215.517 46.9976 4 -3 -5 -9 306.969 42.8538 8 -3 -5 -9 185.577 44.5762 1 -3 5 -9 165.252 44.7763 1 -3 5 -10 189.265 48.3844 1 3 -5 10 272.308 50.322 4 -3 -5 -10 252.677 41.0878 8 3 -5 11 320.713 58.312 4 -3 -5 -11 369.212 65.3817 1 -3 5 -11 225.193 57.5006 1 3 -6 -13 43.7041 36.7341 1 3 6 -13 62.1819 38.209 1 3 -6 -12 48.2584 34.5932 1 3 6 -12 40.8696 33.521 1 3 -6 -11 425.804 58.8672 1 3 6 -11 462.236 60.9118 1 -3 6 11 446.965 54.8538 2 -3 6 10 72.4246 31.3334 2 3 -6 -10 86.4276 32.8536 1 3 6 -10 47.2024 29.0336 1 -3 6 9 465.514 55.2096 2 3 6 -9 435.941 54.0445 1 3 -6 -9 453.207 54.9181 1 3 -6 -8 137.42 31.1316 1 3 6 -8 112.566 29.5967 1 -3 6 8 87.343 27.074 2 -3 6 7 449.487 49.2983 2 3 6 -7 559.14 50.8278 1 -3 6 7 433.341 49.8368 3 3 -6 -7 408.998 45.5656 1 -3 6 6 3462.07 147.858 2 -3 6 6 3285.87 146.574 3 3 -6 -6 3866.95 144.749 1 3 6 -6 3624.81 141.775 1 -3 -6 6 3531.68 114.451 3 3 6 -6 3369.97 139.843 5 3 -6 -6 3188.49 137.05 5 3 -6 -6 3307.44 148.051 8 3 -6 -5 8518.12 276.4 8 -3 -6 5 8650.79 232.27 3 3 -6 -5 8650.95 266.518 1 3 6 -5 8883.18 267.967 1 -3 6 5 8226.54 276.242 3 3 6 -5 9162.36 268.895 5 3 -6 -5 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