#------------------------------------------------------------------------------ #$Date: 2020-04-23 01:17:33 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251061 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126442.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_7126442 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 104.183(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.9445(7) _cell_length_b 19.2382(16) _cell_length_c 10.3606(11) _cell_measurement_reflns_used 3690 _cell_measurement_temperature 400.0(2) _cell_measurement_theta_max 25.8850 _cell_measurement_theta_min 2.6110 _cell_volume 1535.2(3) _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 air _diffrn_ambient_temperature 400.0(2) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.854 _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 -1.00 95.00 0.50 1.50 -- 17.58 57.00-180.00 192 2 \w -8.00 39.00 0.50 1.50 -- 17.58 57.00 -90.00 94 3 \w 49.00 94.00 0.50 1.50 -- 17.58 57.00 -90.00 90 4 \w -4.00 60.00 0.50 1.50 -- 17.58 57.00 0.00 128 5 \w -45.00 -5.00 0.50 1.50 -- -18.36 57.00 60.00 80 ; _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 0.0570648000 _diffrn_orient_matrix_UB_12 0.0158089000 _diffrn_orient_matrix_UB_13 0.0557290000 _diffrn_orient_matrix_UB_21 -0.0018996000 _diffrn_orient_matrix_UB_22 -0.0305686000 _diffrn_orient_matrix_UB_23 0.0378286000 _diffrn_orient_matrix_UB_31 0.0723753000 _diffrn_orient_matrix_UB_32 -0.0132796000 _diffrn_orient_matrix_UB_33 -0.0208787000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.854 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 10149 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.854 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.662 _diffrn_reflns_theta_min 2.644 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90597 _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 1.368 _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 0.174 _refine_diff_density_min -0.167 _refine_diff_density_rms 0.035 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 4058 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0540 _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^)+(0.0778P)^2^+0.0596P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1451 _refine_ls_wR_factor_ref 0.1742 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1992 _reflns_number_total 4058 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 400K in P2(1)/c 400k.res created by SHELXL-2018/3 at 12:45:38 on 18-Oct-2019 CELL 0.71073 7.9445 19.2382 10.3606 90 104.183 90 ZERR 4 0.0007 0.0016 0.0011 0 0.01 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 127 ACTA BOND $H CONF fmap 2 OMIT 0 12 0 OMIT -6 0 6 REM REM REM WGHT 0.077800 0.059600 FVAR 2.76970 F1 4 0.024315 0.363224 0.674396 11.00000 0.10525 0.13888 = 0.08285 -0.00687 0.02507 -0.02679 F2 4 0.259645 0.302620 0.658126 11.00000 0.13428 0.06978 = 0.10380 0.00370 -0.02577 0.00694 O1 5 0.265954 0.421169 0.645459 11.00000 0.10423 0.06951 = 0.05927 0.00635 0.00083 -0.01920 O2 5 0.085383 0.350929 0.469581 11.00000 0.10398 0.06713 = 0.06011 0.00573 0.00069 -0.01897 O3 5 0.614858 0.589854 0.935195 11.00000 0.11463 0.08994 = 0.06829 -0.00420 -0.00681 -0.02004 C1 1 0.705895 0.648250 0.999454 11.00000 0.11631 0.11326 = 0.07779 -0.02547 0.00762 -0.03303 AFIX 137 H1A 2 0.795797 0.660705 0.956480 11.00000 -1.50000 H1B 2 0.756729 0.637222 1.091091 11.00000 -1.50000 H1C 2 0.627074 0.686540 0.994495 11.00000 -1.50000 AFIX 0 C2 1 0.539190 0.593630 0.802248 11.00000 0.06925 0.06809 = 0.06576 -0.00916 0.00796 -0.00138 C3 1 0.550887 0.649600 0.722352 11.00000 0.07642 0.05798 = 0.08312 -0.00779 0.01043 -0.00531 AFIX 43 H3 2 0.613945 0.688750 0.758179 11.00000 -1.20000 AFIX 0 C4 1 0.469036 0.647326 0.589596 11.00000 0.09047 0.05875 = 0.08174 0.00711 0.01354 -0.00338 AFIX 43 H4 2 0.477964 0.685161 0.535795 11.00000 -1.20000 AFIX 0 C5 1 0.373976 0.590278 0.534256 11.00000 0.07973 0.06432 = 0.06544 0.00161 0.01018 -0.00081 AFIX 43 H5 2 0.318424 0.589831 0.444125 11.00000 -1.20000 AFIX 0 C6 1 0.361399 0.533154 0.614037 11.00000 0.05951 0.05592 = 0.05923 -0.00443 0.01206 0.00172 C7 1 0.446116 0.535338 0.748219 11.00000 0.06995 0.05875 = 0.06453 0.00085 0.00997 -0.00109 AFIX 43 H7 2 0.440236 0.497269 0.802263 11.00000 -1.20000 AFIX 0 C8 1 0.259648 0.471302 0.561098 11.00000 0.05953 0.05632 = 0.05880 0.00029 0.01360 0.00351 C9 1 0.163509 0.463947 0.431864 11.00000 0.07276 0.05658 = 0.06007 0.00399 0.00862 -0.00028 AFIX 43 H9 2 0.154794 0.501103 0.373172 11.00000 -1.20000 AFIX 0 C10 1 0.079778 0.402309 0.387909 11.00000 0.06007 0.06163 = 0.05784 0.00280 0.01227 0.00384 C11 1 -0.016480 0.388958 0.250577 11.00000 0.05980 0.06615 = 0.05581 0.00047 0.01035 0.00095 C12 1 -0.062683 0.321738 0.209389 11.00000 0.08527 0.06866 = 0.06805 0.00516 0.00019 -0.00615 AFIX 43 H12 2 -0.032550 0.285279 0.269571 11.00000 -1.20000 AFIX 0 C13 1 -0.152964 0.308004 0.080105 11.00000 0.08791 0.07764 = 0.07115 -0.00710 0.00007 -0.01367 AFIX 43 H13 2 -0.180884 0.262303 0.054232 11.00000 -1.20000 AFIX 0 C14 1 -0.202268 0.360616 -0.010960 11.00000 0.06315 0.09236 = 0.05885 -0.00077 0.00986 -0.00072 C15 1 -0.157618 0.428134 0.031365 11.00000 0.08745 0.08428 = 0.06276 0.01380 0.00784 0.00329 AFIX 43 H15 2 -0.191088 0.464675 -0.028162 11.00000 -1.20000 AFIX 0 C16 1 -0.065130 0.442226 0.159151 11.00000 0.08652 0.06795 = 0.06473 0.00238 0.01067 0.00128 AFIX 43 H16 2 -0.035030 0.487840 0.184370 11.00000 -1.20000 AFIX 0 C17 1 -0.300098 0.345978 -0.151939 11.00000 0.09675 0.13283 = 0.06496 -0.00548 0.00319 -0.00893 AFIX 137 H17A 2 -0.219787 0.342573 -0.207426 11.00000 -1.50000 H17B 2 -0.380661 0.383030 -0.183358 11.00000 -1.50000 H17C 2 -0.362310 0.302986 -0.155051 11.00000 -1.50000 AFIX 0 B1 3 0.159027 0.357946 0.613772 11.00000 0.08433 0.05951 = 0.06141 0.00705 0.00349 -0.00356 HKLF 4 REM 400K in P2(1)/c REM wR2 = 0.1742, GooF = S = 1.037, Restrained GooF = 1.037 for all data REM R1 = 0.0540 for 1992 Fo > 4sig(Fo) and 0.1104 for all 4058 data REM 210 parameters refined using 0 restraints END WGHT 0.0778 0.0596 REM Highest difference peak 0.174, deepest hole -0.167, 1-sigma level 0.035 Q1 1 0.1046 0.3235 0.6953 11.00000 0.05 0.17 Q2 1 0.1655 0.4403 0.6441 11.00000 0.05 0.15 Q3 1 -0.2558 0.2815 -0.1530 11.00000 0.05 0.14 Q4 1 -0.4564 0.3455 -0.1550 11.00000 0.05 0.13 Q5 1 0.2463 0.4924 0.3597 11.00000 0.05 0.12 REM The information below was added by Olex2. REM REM R1 = 0.0540 for 1992 Fo > 4sig(Fo) and 0.1104 for all 10369 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.17, deepest hole -0.17 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1104 REM R1_gt = 0.0540 REM wR_ref = 0.1742 REM GOOF = 1.037 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 10369 REM Reflections_gt = 1992 REM Parameters = n/a REM Hole = -0.17 REM Peak = 0.17 REM Flack = n/a ; _cod_data_source_file d0cc01505a2.cif _cod_data_source_block 400k_CCDC1 _cod_database_code 7126442 _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 0.971 _reflns_odcompleteness_completeness 99.78 _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 1.191 _oxdiff_exptl_absorpt_empirical_full_min 0.775 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 0.02432(18) 0.36322(7) 0.67440(13) 0.1086(5) Uani 1 1 d . . . . . F2 F 0.25965(18) 0.30262(6) 0.65813(13) 0.1122(5) Uani 1 1 d . . . . . O1 O 0.26595(17) 0.42117(7) 0.64546(12) 0.0810(4) Uani 1 1 d . . . . . O2 O 0.08538(18) 0.35093(7) 0.46958(13) 0.0804(4) Uani 1 1 d . . . . . O3 O 0.61486(19) 0.58985(8) 0.93520(14) 0.0960(5) Uani 1 1 d . . . . . C1 C 0.7059(3) 0.64825(13) 0.9995(2) 0.1053(8) Uani 1 1 d . . . . . H1A H 0.795797 0.660705 0.956480 0.158 Uiso 1 1 calc GR . . . . H1B H 0.756729 0.637222 1.091091 0.158 Uiso 1 1 calc GR . . . . H1C H 0.627074 0.686540 0.994495 0.158 Uiso 1 1 calc GR . . . . C2 C 0.5392(2) 0.59363(10) 0.80225(19) 0.0692(5) Uani 1 1 d . . . . . C3 C 0.5509(3) 0.64960(10) 0.7224(2) 0.0741(5) Uani 1 1 d . . . . . H3 H 0.613945 0.688750 0.758179 0.089 Uiso 1 1 calc R . . . . C4 C 0.4690(3) 0.64733(10) 0.5896(2) 0.0783(6) Uani 1 1 d . . . . . H4 H 0.477964 0.685161 0.535795 0.094 Uiso 1 1 calc R . . . . C5 C 0.3740(2) 0.59028(10) 0.53426(19) 0.0712(5) Uani 1 1 d . . . . . H5 H 0.318424 0.589831 0.444125 0.085 Uiso 1 1 calc R . . . . C6 C 0.3614(2) 0.53315(9) 0.61404(17) 0.0586(4) Uani 1 1 d . . . . . C7 C 0.4461(2) 0.53534(9) 0.74822(18) 0.0655(5) Uani 1 1 d . . . . . H7 H 0.440236 0.497269 0.802263 0.079 Uiso 1 1 calc R . . . . C8 C 0.2596(2) 0.47130(9) 0.56110(17) 0.0584(4) Uani 1 1 d . . . . . C9 C 0.1635(2) 0.46395(9) 0.43186(18) 0.0645(5) Uani 1 1 d . . . . . H9 H 0.154794 0.501103 0.373172 0.077 Uiso 1 1 calc R . . . . C10 C 0.0798(2) 0.40231(9) 0.38791(18) 0.0602(4) Uani 1 1 d . . . . . C11 C -0.0165(2) 0.38896(9) 0.25058(17) 0.0613(5) Uani 1 1 d . . . . . C12 C -0.0627(2) 0.32174(11) 0.2094(2) 0.0772(6) Uani 1 1 d . . . . . H12 H -0.032550 0.285279 0.269571 0.093 Uiso 1 1 calc R . . . . C13 C -0.1530(3) 0.30800(11) 0.0801(2) 0.0823(6) Uani 1 1 d . . . . . H13 H -0.180884 0.262303 0.054232 0.099 Uiso 1 1 calc R . . . . C14 C -0.2023(2) 0.36062(11) -0.01096(19) 0.0723(5) Uani 1 1 d . . . . . C15 C -0.1576(3) 0.42813(11) 0.0314(2) 0.0800(6) Uani 1 1 d . . . . . H15 H -0.191088 0.464675 -0.028162 0.096 Uiso 1 1 calc R . . . . C16 C -0.0651(2) 0.44223(10) 0.1592(2) 0.0744(5) Uani 1 1 d . . . . . H16 H -0.035030 0.487840 0.184370 0.089 Uiso 1 1 calc R . . . . C17 C -0.3001(3) 0.34598(15) -0.1519(2) 0.1011(7) Uani 1 1 d . . . . . H17A H -0.219787 0.342573 -0.207426 0.152 Uiso 1 1 calc GR . . . . H17B H -0.380661 0.383030 -0.183358 0.152 Uiso 1 1 calc GR . . . . H17C H -0.362310 0.302986 -0.155051 0.152 Uiso 1 1 calc GR . . . . B1 B 0.1590(3) 0.35795(11) 0.6138(2) 0.0709(6) 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 0.1053(10) 0.1389(12) 0.0828(9) -0.0069(8) 0.0251(7) -0.0268(8) F2 0.1343(11) 0.0698(8) 0.1038(10) 0.0037(7) -0.0258(8) 0.0069(7) O1 0.1042(10) 0.0695(8) 0.0593(8) 0.0064(6) 0.0008(7) -0.0192(7) O2 0.1040(10) 0.0671(8) 0.0601(8) 0.0057(7) 0.0007(7) -0.0190(7) O3 0.1146(11) 0.0899(10) 0.0683(9) -0.0042(8) -0.0068(8) -0.0200(9) C1 0.1163(19) 0.1133(19) 0.0778(16) -0.0255(14) 0.0076(13) -0.0330(14) C2 0.0692(11) 0.0681(12) 0.0658(12) -0.0092(10) 0.0080(9) -0.0014(9) C3 0.0764(12) 0.0580(11) 0.0831(15) -0.0078(10) 0.0104(10) -0.0053(9) C4 0.0905(14) 0.0588(11) 0.0817(15) 0.0071(11) 0.0135(11) -0.0034(10) C5 0.0797(12) 0.0643(11) 0.0654(12) 0.0016(10) 0.0102(9) -0.0008(10) C6 0.0595(10) 0.0559(10) 0.0592(11) -0.0044(8) 0.0121(8) 0.0017(7) C7 0.0700(11) 0.0587(10) 0.0645(12) 0.0008(9) 0.0100(9) -0.0011(8) C8 0.0595(9) 0.0563(10) 0.0588(11) 0.0003(9) 0.0136(8) 0.0035(7) C9 0.0728(11) 0.0566(10) 0.0601(11) 0.0040(9) 0.0086(8) -0.0003(8) C10 0.0601(10) 0.0616(11) 0.0578(11) 0.0028(9) 0.0123(8) 0.0038(8) C11 0.0598(10) 0.0662(11) 0.0558(11) 0.0005(9) 0.0103(8) 0.0009(8) C12 0.0853(13) 0.0687(12) 0.0680(13) 0.0052(10) 0.0002(10) -0.0061(10) C13 0.0879(14) 0.0776(14) 0.0711(14) -0.0071(11) 0.0001(11) -0.0137(10) C14 0.0631(11) 0.0924(15) 0.0588(12) -0.0008(11) 0.0099(9) -0.0007(10) C15 0.0874(13) 0.0843(14) 0.0628(12) 0.0138(11) 0.0078(10) 0.0033(11) C16 0.0865(13) 0.0679(12) 0.0647(12) 0.0024(10) 0.0107(10) 0.0013(10) C17 0.0967(16) 0.133(2) 0.0650(14) -0.0055(13) 0.0032(12) -0.0089(14) B1 0.0843(15) 0.0595(13) 0.0614(13) 0.0070(11) 0.0035(11) -0.0036(11) 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 C8 O1 B1 122.66(15) . . ? C10 O2 B1 122.35(14) . . ? C2 O3 C1 118.84(17) . . ? 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 124.88(17) . . ? O3 C2 C7 115.16(17) . . ? C3 C2 C7 119.95(18) . . ? C2 C3 H3 120.2 . . ? C4 C3 C2 119.58(18) . . ? C4 C3 H3 120.2 . . ? C3 C4 H4 119.3 . . ? C3 C4 C5 121.39(19) . . ? C5 C4 H4 119.3 . . ? C4 C5 H5 120.2 . . ? C4 C5 C6 119.60(18) . . ? C6 C5 H5 120.2 . . ? C5 C6 C8 122.07(16) . . ? C7 C6 C5 118.84(16) . . ? C7 C6 C8 119.09(16) . . ? C2 C7 C6 120.62(17) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? O1 C8 C6 115.17(15) . . ? O1 C8 C9 120.04(16) . . ? C9 C8 C6 124.79(16) . . ? C8 C9 H9 119.4 . . ? C8 C9 C10 121.10(17) . . ? C10 C9 H9 119.4 . . ? O2 C10 C9 120.22(16) . . ? O2 C10 C11 115.31(15) . . ? C9 C10 C11 124.47(16) . . ? C12 C11 C10 120.00(16) . . ? C12 C11 C16 118.20(17) . . ? C16 C11 C10 121.80(16) . . ? C11 C12 H12 119.5 . . ? C13 C12 C11 120.91(19) . . ? C13 C12 H12 119.5 . . ? C12 C13 H13 119.4 . . ? C14 C13 C12 121.20(19) . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 117.68(18) . . ? C13 C14 C17 121.5(2) . . ? C15 C14 C17 120.9(2) . . ? C14 C15 H15 119.2 . . ? C16 C15 C14 121.56(19) . . ? C16 C15 H15 119.2 . . ? C11 C16 H16 119.8 . . ? C15 C16 C11 120.44(18) . . ? 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 O1 107.99(17) . . ? F1 B1 O2 108.13(17) . . ? F2 B1 F1 111.59(18) . . ? F2 B1 O1 108.40(17) . . ? F2 B1 O2 109.27(17) . . ? O2 B1 O1 111.47(16) . . ? 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 1.371(3) . ? F2 B1 1.343(2) . ? O1 C8 1.294(2) . ? O1 B1 1.474(2) . ? O2 C10 1.295(2) . ? O2 B1 1.471(3) . ? O3 C1 1.412(3) . ? O3 C2 1.363(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.375(3) . ? C2 C7 1.384(2) . ? C3 H3 0.9300 . ? C3 C4 1.371(3) . ? C4 H4 0.9300 . ? C4 C5 1.375(3) . ? C5 H5 0.9300 . ? C5 C6 1.393(2) . ? C6 C7 1.389(2) . ? C6 C8 1.467(2) . ? C7 H7 0.9300 . ? C8 C9 1.377(2) . ? C9 H9 0.9300 . ? C9 C10 1.381(2) . ? C10 C11 1.464(2) . ? C11 C12 1.383(3) . ? C11 C16 1.385(2) . ? C12 H12 0.9300 . ? C12 C13 1.381(3) . ? C13 H13 0.9300 . ? C13 C14 1.374(3) . ? C14 C15 1.389(3) . ? C14 C17 1.503(3) . ? C15 H15 0.9300 . ? C15 C16 1.375(3) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 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 O1 C8 C9 C10 -3.3(3) . . . . ? O2 C10 C11 C12 -13.3(2) . . . . ? O2 C10 C11 C16 166.12(16) . . . . ? O3 C2 C3 C4 179.95(18) . . . . ? O3 C2 C7 C6 179.28(15) . . . . ? C1 O3 C2 C3 3.2(3) . . . . ? C1 O3 C2 C7 -177.26(18) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C3 C2 C7 C6 -1.1(3) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C4 C5 C6 C8 179.02(16) . . . . ? C5 C6 C7 C2 1.0(3) . . . . ? C5 C6 C8 O1 177.15(15) . . . . ? C5 C6 C8 C9 -2.2(3) . . . . ? C6 C8 C9 C10 176.02(15) . . . . ? C7 C2 C3 C4 0.4(3) . . . . ? C7 C6 C8 O1 -3.7(2) . . . . ? C7 C6 C8 C9 176.90(15) . . . . ? C8 O1 B1 F1 -103.1(2) . . . . ? C8 O1 B1 F2 135.80(18) . . . . ? C8 O1 B1 O2 15.5(3) . . . . ? C8 C6 C7 C2 -178.18(15) . . . . ? C8 C9 C10 O2 2.5(3) . . . . ? C8 C9 C10 C11 -176.34(15) . . . . ? C9 C10 C11 C12 165.62(17) . . . . ? C9 C10 C11 C16 -15.0(3) . . . . ? C10 O2 B1 F1 102.27(19) . . . . ? C10 O2 B1 F2 -136.08(18) . . . . ? C10 O2 B1 O1 -16.3(3) . . . . ? C10 C11 C12 C13 -179.76(16) . . . . ? C10 C11 C16 C15 -179.08(17) . . . . ? C11 C12 C13 C14 -1.1(3) . . . . ? C12 C11 C16 C15 0.3(3) . . . . ? C12 C13 C14 C15 0.2(3) . . . . ? C12 C13 C14 C17 179.82(19) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? C14 C15 C16 C11 -1.2(3) . . . . ? C16 C11 C12 C13 0.8(3) . . . . ? C17 C14 C15 C16 -178.65(19) . . . . ? B1 O1 C8 C6 173.96(16) . . . . ? B1 O1 C8 C9 -6.6(3) . . . . ? B1 O2 C10 C9 8.2(3) . . . . ? B1 O2 C10 C11 -172.80(16) . . . . ? 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 6927.27 213.195 1 0 0 3 -2.82812 7.21349 1 0 0 -4 20.4983 9.95734 1 0 0 4 -1.93558 7.89352 2 0 0 4 5.71072 7.76303 1 0 0 5 -9.89279 17.3392 2 0 0 -5 -2.10414 15.2847 1 0 0 5 -2.42489 13.6756 1 0 0 6 510.53 37.698 2 0 0 6 486.869 36.9178 1 0 0 7 7.03134 11.5816 1 0 0 7 21.1787 13.4252 2 0 0 8 8.15298 14.2903 1 0 0 8 4.07408 14.2819 2 0 0 9 46.9746 19.9791 1 0 0 9 9.20901 15.1757 2 0 0 10 324.487 41.7165 1 0 0 10 213.941 35.9892 2 0 0 11 -5.57946 20.1245 2 0 0 11 11.5066 20.1669 1 0 0 12 86.3526 29.3039 2 0 0 13 -13.1779 27.4449 2 0 1 2 20041.9 595.788 1 0 1 -2 20269.5 594.621 2 0 -1 2 19840.4 594.773 1 0 1 -3 7651.27 237.856 1 0 1 3 7572.62 239.887 1 0 -1 3 7646.53 238.953 1 0 1 -3 7620.17 238.221 2 0 1 4 10372.4 322.094 2 0 -1 4 9894.37 319.773 2 0 1 -4 10526.1 318.786 2 0 1 4 9754.22 320.064 1 0 -1 -4 10129.4 317.44 1 0 -1 4 10379.9 320.357 1 0 1 -4 10359.5 318.14 1 0 -1 5 11967.6 363.215 2 0 -1 5 11131.1 361.107 1 0 1 5 11629.4 363.41 1 0 1 -5 11353.7 358.154 1 0 1 5 11457.1 363.773 2 0 -1 -5 11074 357.67 1 0 -1 6 8.74994 10.226 1 0 1 6 24.1064 12.0178 1 0 -1 6 23.3947 11.1206 2 0 1 6 -6.13184 11.6588 2 0 -1 7 27.9833 12.2722 1 0 1 7 24.9882 13.5821 1 0 -1 7 6.90087 11.3729 2 0 1 7 14.5099 12.726 2 0 1 8 4.15565 13.6835 1 0 -1 8 3.95212 14.646 2 0 -1 8 -4.05244 14.2054 1 0 1 8 12.4526 14.5505 2 0 1 9 -4.71391 17.0026 1 0 -1 9 -13.3565 16.0586 2 0 1 9 18.8871 18.3956 2 0 -1 9 13.6926 19.0095 1 0 -1 10 340.858 42.1206 2 0 1 10 325.027 42.0738 2 0 -1 10 464.251 46.6045 1 0 1 10 409.699 46.9963 1 0 -1 11 66.9481 24.7484 2 0 1 11 88.8117 29.4371 1 0 1 11 80.5545 25.9825 2 0 1 12 6.40328 23.7337 1 0 -1 12 18.0103 23.944 2 0 1 12 24.7179 23.4992 2 0 -1 13 25.7679 26.8411 2 0 1 13 27.0001 26.3086 2 0 2 1 23838.9 698.447 1 0 -2 -1 23627.9 698.01 1 0 2 2 2560.77 87.0612 1 0 2 -2 2527.07 85.267 2 0 -2 -2 2555.2 86.2292 1 0 2 -3 1722.34 65.713 1 0 2 3 1826.86 69.1241 1 0 2 -3 1729.64 66.375 2 0 2 -4 267.446 21.5344 2 0 2 -4 237.337 20.9802 1 0 -2 4 260.795 21.841 1 0 -2 4 247.42 20.6466 2 0 2 4 225.626 21.2867 1 0 2 -5 63485.9 1871.24 2 0 -2 5 63253.8 1874.24 1 0 2 -5 64215.1 1870.56 1 0 2 5 62923 1877.97 2 0 2 5 61726 1875.78 1 0 -2 5 64605.1 1873.9 2 0 2 6 1836.88 88.4066 1 0 2 6 2097.33 92.0049 2 0 -2 6 2111.17 89.4129 2 0 -2 6 2019.3 88.9197 1 0 -2 7 430.72 36.4134 1 0 -2 7 422.212 36.2555 2 0 2 7 469.529 39.9314 2 0 2 7 434.777 38.3951 1 0 -2 8 3.89873 14.0623 2 0 2 8 4.24919 13.991 2 0 2 8 -8.40556 13.369 1 0 2 9 4.82274 16.4031 2 0 2 9 9.62817 15.854 1 0 -2 9 17.8012 15.1368 2 0 -2 10 341.479 40.7465 2 0 2 10 329.364 42.7823 1 0 2 10 376.961 44.597 2 0 2 11 78.0155 27.1414 1 0 -2 11 81.2559 27.3887 2 0 2 11 141.347 31.7899 2 0 2 12 -6.59955 23.8061 1 0 -2 12 -11.805 23.5388 2 0 2 12 -12.7671 23.658 2 0 2 13 21.1065 27.4129 1 0 2 13 6.7701 23.7349 2 0 -2 13 19.2538 25.0073 2 0 3 0 5.99548 4.0852 3 0 -3 0 1.42262 3.67977 3 0 3 1 3535.93 108.455 1 0 -3 -1 3448.19 107.296 1 0 3 1 3196.76 103.227 4 0 3 -1 3401.15 106.997 3 0 3 2 1548.04 50.7159 5 0 -3 -2 1601.76 59.3247 1 0 3 2 1695.93 61.1026 1 0 3 -2 1680.37 58.9996 2 0 3 -3 10966.7 336.631 1 0 3 -3 10804.8 336.678 2 0 -3 3 11000.4 337.119 2 0 3 3 11182.4 340.1 1 0 3 -4 5506.01 180.036 2 0 3 -4 5023.92 177.584 1 0 3 4 5591.82 184.803 1 0 -3 4 5691.88 181.282 2 0 3 -5 842.954 44.5926 1 0 3 5 802.693 47.8376 1 0 3 -5 904.311 46.6303 2 0 -3 5 759.348 44.5399 2 0 3 6 237.348 28.0975 2 0 3 6 256.637 27.753 1 0 3 7 406.703 37.291 1 0 -3 7 338.23 31.7933 2 0 3 8 632.88 50.645 2 0 -3 8 572.771 45.8075 2 0 3 8 609.161 49.5153 1 0 3 9 63.4556 20.8162 1 0 -3 9 30.3393 16.9681 2 0 -3 10 218.267 33.3457 2 0 3 10 231.291 36.8215 1 0 3 10 209.021 36.7801 2 0 3 11 6.04944 18.545 2 0 -3 11 26.9401 19.4357 2 0 3 11 -6.08176 19.3477 1 0 -3 12 129.818 32.2068 2 0 3 12 73.8628 31.3546 1 0 3 12 52.3133 26.1799 2 0 3 13 166.466 39.5614 1 0 3 13 97.5735 34.7344 2 0 -3 13 114.391 36.818 2 0 -4 0 191418 5577.44 4 0 4 0 192451 5584.62 3 0 -4 -1 25181.6 721.697 1 0 4 -1 23978.2 721.782 3 0 4 1 23849.2 722.434 1 0 4 1 24348.8 716.029 4 0 -4 -1 24596 716.658 4 0 4 2 2124.25 72.457 4 0 4 2 2137.7 78.2682 1 0 -4 -2 2009.93 76.2086 1 0 -4 -2 2197.04 66.9682 5 0 4 -3 2092.71 75.0485 2 0 4 3 1994.34 64.1671 5 0 -4 -3 1908.25 74.7381 1 0 4 3 1935.75 77.3063 1 0 4 -4 3504.17 120.409 1 0 -4 4 3364.95 121.007 2 0 4 4 3518.33 125.51 1 0 4 -4 3268.06 120.289 2 0 4 5 1274.47 65.8879 1 0 4 -5 1372.23 61.7749 1 0 -4 5 1424.74 64.4834 2 0 4 6 2378.88 103.943 1 0 -4 6 2377.95 99.8047 2 0 4 7 188.248 27.1638 2 0 4 7 170.069 26.7857 1 0 -4 7 172.999 24.5435 2 0 4 8 335.294 38.6083 2 0 -4 8 417.599 38.6967 2 0 4 8 369.385 39.7297 1 0 -4 9 165.221 27.5682 2 0 4 9 187.077 32.51 2 0 4 9 140.249 27.9963 1 0 -4 10 73.0166 24.2559 2 0 4 10 89.8666 26.2696 2 0 4 10 95.2053 29.0653 1 0 4 11 6.22938 20.5138 1 0 -4 11 10.7826 18.9009 2 0 4 11 18.5247 22.2747 2 0 4 12 26.8883 25.5577 2 0 -4 12 -29.0508 21.5313 2 0 4 12 6.79422 23.816 1 0 -4 13 68.3859 29.9664 2 0 4 13 35.8085 32.2807 2 0 4 13 119.238 38.5913 1 0 -5 0 8.57839 3.12083 4 0 5 0 18.7643 6.70821 3 0 5 -1 888.199 37.9389 3 0 -5 -1 826.756 31.9524 4 0 5 1 904.992 31.8312 4 0 -5 -1 871.314 36.8733 1 0 5 2 5098.31 159.576 4 0 -5 -2 4981.56 165.093 1 0 -5 -2 5092 154.001 5 0 5 2 5341.43 168.242 1 0 5 3 790.371 29.1717 5 0 5 -3 821.109 39.5607 2 0 -5 -3 921.756 41.7563 1 0 5 3 799.065 42.2368 1 0 -5 3 805.912 40.1696 3 0 5 4 1623.99 70.943 1 0 5 4 1502.34 53.0071 5 0 5 -4 1645.12 65.7182 1 0 5 -4 1580.04 66.4517 2 0 5 5 233.348 25.4228 1 0 5 5 273.321 16.1944 5 0 -5 6 1231.02 64.0917 2 0 5 6 1316.94 70.5618 1 0 5 6 1319.68 51.4441 5 0 -5 7 282.411 30.0617 2 0 5 7 353.108 35.6218 1 0 -5 8 1714.34 87.2381 2 0 5 8 1856.89 94.7465 1 0 5 8 1605.41 90.5921 2 0 5 9 236.346 36.5419 2 0 -5 9 276.375 33.8923 2 0 5 9 263.444 38.0199 1 0 5 10 57.7181 23.0986 2 0 5 10 80.0967 26.7124 1 0 -5 10 67.3308 23.2117 2 0 5 11 12.7152 22.9325 2 0 5 11 -6.33021 20.8445 1 0 -5 11 -15.8129 20.0417 2 0 -5 12 68.5692 25.716 2 0 5 12 6.8525 24.7272 2 0 5 12 6.94229 24.3458 1 0 5 13 37.3758 30.4893 1 0 5 13 22.0105 27.9075 2 0 -6 0 10304.8 300.435 4 0 6 0 9603.74 310.941 3 0 6 -1 2705.02 95.9549 3 0 6 1 2751.29 87.3431 4 0 -6 -1 2793.17 88.7688 4 0 -6 -2 193.675 11.1703 5 0 6 2 212.166 13.9009 4 0 6 -2 208.601 17.1813 3 0 -6 -2 225.09 18.1654 1 0 6 2 177.161 17.6718 1 0 6 3 243.625 18.3401 4 0 -6 3 297.936 22.3454 3 0 6 -3 286.403 21.97 2 0 -6 -3 268.366 22.1401 1 0 6 3 314.613 25.5053 1 0 6 -4 1134.91 53.6427 2 0 6 4 1152.61 57.7894 1 0 6 4 1097.25 39.7922 5 0 -6 4 1190.91 55.625 3 0 6 5 641.691 42.981 1 0 6 5 570.191 25.3396 5 0 6 6 52.1931 8.35201 5 0 6 6 65.0659 17.4563 1 0 6 7 53.6423 19.5655 1 0 6 7 36.4075 9.18759 5 0 6 8 4.66279 9.15609 5 0 6 8 9.45799 19.2817 1 0 6 9 21.1348 20.6062 1 0 6 9 42.7761 19.8369 2 0 6 10 236.085 38.9271 1 0 6 10 276.756 41.3406 2 0 6 11 -6.46844 19.0502 2 0 6 11 19.3236 19.7445 1 0 6 12 -7.01435 23.0959 2 0 6 12 14.1519 24.8034 1 0 6 13 44.9922 30.602 2 0 6 13 45.6002 32.3328 1 0 7 0 47.2117 9.96859 3 0 -7 0 51.5119 6.15592 4 0 7 -1 4416.44 147.504 3 0 -7 -1 4417.92 138.898 4 0 7 1 4484.47 137.173 4 0 7 -2 38.9874 10.202 3 0 -7 -2 37.856 9.90914 1 0 7 2 33.51 6.87961 4 0 -7 -3 37.1308 11.8891 1 0 7 3 30.1024 10.6878 1 0 7 3 30.3732 7.94961 4 0 -7 3 68.1889 12.9441 3 0 -7 -3 59.9435 6.26882 5 0 7 4 300.331 21.5072 4 0 -7 4 266.475 24.2263 3 0 7 4 279.059 26.9852 1 0 -7 5 225.274 24.1983 3 0 7 5 210.836 26.2863 1 0 7 5 195.714 12.3 5 0 7 6 18.4495 13.6849 1 0 7 6 19.0548 5.74742 5 0 7 7 3896.03 153.183 1 0 7 7 3452.88 116.085 5 0 7 8 58.4483 24.1493 1 0 7 8 9.31408 9.27038 5 0 7 9 44.0205 23.4115 2 0 7 9 27.2021 20.1855 1 0 7 10 -6.05068 20.5777 2 0 7 10 36.3135 21.8314 1 0 7 11 -19.8968 23.2496 2 0 7 11 6.61318 23.1826 1 0 7 12 -7.15606 26.5186 2 0 7 12 7.19462 25.9503 1 0 7 13 83.9391 36.2026 2 0 8 0 4014.8 140.154 3 0 -8 0 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4826.23 153.832 1 -2 -4 2 5388.28 169.144 3 2 4 -1 11465.4 345.124 3 2 4 -1 10939.9 337.125 1 -2 -4 1 11452.4 336.375 1 -2 4 1 11536.9 336.246 4 -2 -4 1 11412.3 345.969 3 -2 -4 0 17471.4 515.349 3 2 -4 0 16917.8 506.902 4 2 4 0 17256 512.368 1 -2 -4 0 17865.3 511.648 1 2 4 0 17356.1 513.693 3 -2 4 0 16981.5 508.679 4 2 4 0 16832 514.61 4 2 4 1 4150.96 139.592 1 2 4 1 4181.26 135.513 3 2 -4 1 4199.28 130.652 3 2 4 1 4118.39 137.758 5 -2 4 -1 4090.01 129.304 3 2 4 1 4430.68 137.593 4 -2 -4 -1 4195.76 137.434 5 2 -4 1 4052.28 131.959 4 -2 -4 -1 4356.28 137.985 1 2 4 2 1556.97 61.9791 5 2 -4 2 1597.51 55.7365 3 2 4 2 1574.13 66.5414 1 -2 -4 -2 1625.07 62.0257 5 2 -4 2 1549.56 59.6649 4 -2 -4 -2 1565.44 63.9222 1 -2 4 -2 1476.08 54.8108 2 2 4 2 1611.63 62.3424 4 2 4 3 127.512 17.163 1 -2 -4 -3 123.82 18.0063 1 2 4 3 134.773 14.7145 5 2 -4 3 149.239 13.1581 3 -2 4 -3 148.661 13.7546 2 2 4 4 422.027 28.5387 5 -2 4 -4 455.827 27.5037 2 -2 4 -5 307.007 24.343 2 2 4 5 283.939 23.8786 5 2 4 6 8.14982 13.8689 1 2 4 6 40.8012 11.9113 5 2 -4 6 11.8477 9.24901 2 2 4 7 79.2651 22.5048 1 2 4 7 58.6561 19.5571 2 2 4 7 63.8291 16.8766 5 2 -4 7 65.2307 16.4643 2 2 4 8 128.714 25.4239 2 2 4 8 126.589 29.2477 1 2 -4 8 121.852 22.2916 2 2 4 8 93.9169 18.9614 5 2 4 9 165.831 24.5676 5 2 4 9 164.514 33.477 1 2 -4 9 153.43 26.0917 2 2 4 9 177.803 30.6699 2 2 4 10 15.5251 19.1785 2 2 -4 10 4.16377 14.161 2 2 4 10 38.8878 24.019 1 2 4 10 -3.44165 13.7255 5 2 4 11 -5.63621 23.4746 2 2 -4 11 27.386 21.2543 2 2 4 11 -7.16519 25.1164 1 2 4 12 7.63509 25.9647 1 2 4 12 6.01714 23.9946 2 2 4 13 -12.5726 25.0697 2 -2 5 14 -21.269 26.962 1 -2 5 13 15.5315 23.8091 2 -2 5 13 6.62804 25.8268 1 -2 -5 13 27.0575 24.4033 2 -2 5 12 -6.0598 21.8614 1 -2 -5 12 -12.5892 23.9361 2 -2 5 12 -28.8172 25.2568 2 -2 5 11 27.8176 22.718 1 -2 5 11 59.6452 26.4562 2 -2 -5 11 46.4022 24.6873 2 -2 5 10 64.4552 24.2794 1 -2 -5 10 57.9653 24.1908 2 -2 5 9 4.45966 16.9584 1 -2 -5 9 18.982 19.7669 2 -2 5 8 1657.05 91.4874 2 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1 -2 6 8 24.5696 19.1441 2 -2 6 7 156.051 8.07444 5 -2 6 7 172.12 24.8672 1 -2 6 6 259.126 27.1686 1 2 6 -6 235.019 21.5115 1 2 6 -5 7109.66 220.926 1 -2 6 5 6753.82 234.714 1 2 6 -4 138.893 12.8114 1 -2 -6 4 158.312 19.799 3 -2 6 4 146.738 18.1893 1 -2 6 3 4888.03 163.264 1 -2 -6 3 4831.25 164.939 3 2 -6 -3 4740.27 144.438 5 -2 -6 2 433.691 28.8072 3 -2 6 2 444.15 27.5992 1 2 6 -2 424.951 20.4609 1 -2 -6 1 2376.03 85.321 3 2 6 -1 2288.26 82.3998 3 2 6 -1 2251.39 75.5299 1 -2 -6 1 2315.68 80.5019 4 -2 6 1 2123.19 67.5456 4 -2 -6 0 71.3827 10.6023 4 -2 -6 0 97.1195 10.9128 1 -2 -6 0 89.6263 13.1818 3 2 6 0 57.9567 11.2274 3 -2 6 0 89.4671 10.6228 3 2 6 0 82.5925 10.876 1 2 -6 0 91.9644 6.26176 4 2 6 0 102.612 11.8356 4 -2 -6 -1 1713.54 69.2547 5 2 6 1 1852.28 69.7379 4 2 6 1 1908.45 73.4318 1 -2 -6 -1 1942.4 71.2142 1 -2 6 -1 1885.95 66.9049 3 2 6 1 1720.19 70.7106 3 2 -6 1 1984.4 64.5835 4 -2 -6 -1 1879.34 72.4585 4 -2 -6 -2 3985.33 139.087 1 2 6 2 3923.55 137.207 5 -2 -6 -2 4074.46 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32.6897 1 -2 7 9 77.5153 25.8201 1 -2 7 8 25.2732 17.5587 1 -2 7 7 18.6488 13.0851 1 2 7 -6 38.324 11.2328 1 -2 7 6 29.4994 12.8089 1 -2 7 5 65.8863 15.5022 1 -2 -7 5 67.0658 17.4736 3 2 7 -5 54.4128 11.5551 1 -2 7 4 17.4975 12.229 1 -2 -7 4 31.8702 11.9694 3 2 -7 -3 17963.9 531.424 5 -2 -7 3 18350.9 555.326 3 -2 7 3 18221 553.299 1 -2 7 2 575.369 34.5314 1 -2 -7 2 581.339 35.0864 3 2 7 -2 595.285 27.1592 1 -2 -7 1 18855.2 567.932 3 2 7 -1 18995.6 565.39 3 2 7 -1 18822.9 557.729 1 -2 -7 1 18097.2 561.387 4 2 -7 0 558.94 20.2313 4 -2 -7 0 548.875 28.5355 1 -2 7 0 560.991 29.7066 3 -2 -7 0 633.794 35.5494 3 2 7 0 596.413 32.9925 3 -2 -7 0 591.396 31.5391 4 2 7 0 627.775 31.9411 1 2 7 0 587.765 29.842 4 2 7 1 16094.7 489.59 4 2 -7 1 15866.5 481.433 4 -2 -7 -1 16476.7 490.928 5 2 7 1 16172.6 495.032 1 -2 -7 -1 16722.6 494.083 4 -2 -7 -1 16637.3 491.455 1 -2 7 -1 16115.8 488.025 3 2 7 1 16219.5 493.952 3 -2 7 -2 127.059 14.4354 3 2 7 2 182.622 20.404 1 2 7 2 144.94 15.6951 4 -2 -7 -2 165.173 16.2023 5 2 -7 2 172.703 15.6781 3 -2 -7 -2 167.309 18.515 4 -2 -7 -2 161.74 18.1709 1 -2 7 -3 763.447 37.4872 2 2 7 3 837.486 47.4225 1 2 -7 3 681.008 36.5921 3 2 7 3 696.32 37.3621 5 -2 -7 -3 765.642 43.0287 4 -2 -7 -3 784.057 38.4279 5 2 7 4 26.6675 14.1827 1 -2 7 -4 1.83037 8.25655 2 2 -7 4 42.2414 10.2122 3 2 7 4 31.3497 10.4172 5 2 7 5 8035.24 250.699 5 2 -7 5 7468.8 252.218 3 2 -7 6 1618.78 74.0406 3 2 7 6 1596.27 69.5452 5 2 -7 7 2716.42 112.744 3 2 7 7 2795.66 106.849 5 2 7 8 -5.12375 11.3172 5 2 7 8 16.8516 19.6899 1 2 7 9 67.887 26.803 1 2 7 9 46.776 23.8504 2 2 7 10 5.65985 19.8393 2 2 7 10 -6.83094 22.4918 1 2 7 11 7.42593 26.7846 1 2 7 11 -6.15567 22.2029 2 2 7 12 -6.58513 25.0374 2 -2 8 13 21.448 29.1559 1 -2 8 12 -6.66305 24.6915 1 -2 8 12 7.62681 24.2608 2 -2 8 11 -12.2705 22.131 1 -2 8 11 -7.01255 23.8487 2 -2 8 10 66.4958 25.8754 1 -2 8 9 65.6122 23.1853 1 -2 8 8 -4.392 17.9075 1 -2 8 7 182.079 27.8462 1 -2 8 6 239.044 28.9239 1 2 8 -6 247.943 22.5208 1 2 8 -5 3033.56 105.337 1 -2 -8 5 2946.95 121.064 3 -2 8 5 2806.82 117.959 1 -2 8 4 951.891 51.94 1 -2 -8 4 834.873 50.2679 3 -2 -8 3 75.946 14.9551 3 2 -8 -3 80.2796 7.2672 5 -2 -8 2 794.219 44.0862 3 2 8 -2 759.863 34.4016 1 -2 8 2 781.815 43.0155 1 2 8 -1 9.34546 7.00036 1 -2 -8 1 9.33329 7.71452 4 -2 -8 1 15.6224 10.0424 3 2 8 -1 1.94184 9.62878 3 -2 -8 0 8567.1 268.964 1 -2 8 0 8671.26 271.68 3 2 8 0 8502.93 275.044 3 2 8 0 8720.84 272.927 1 2 8 0 8742.53 269.129 4 -2 -8 0 8828.65 272.838 4 2 8 1 1615.32 62.7592 4 -2 -8 -1 1690.51 65.6255 1 -2 8 -1 1591.49 62.756 3 2 8 1 1585.06 67.923 1 -2 -8 -1 1628.86 63.9298 5 -2 -8 -1 1669.47 66.846 4 2 8 1 1522.68 66.6259 3 2 -8 1 1506.96 54.2384 4 -2 8 -2 10017.3 307.668 3 2 -8 2 9651.26 308.963 3 -2 -8 -2 9923.82 314.753 4 2 8 2 10182.2 318.815 1 -2 -8 -2 9857.8 307.657 5 -2 -8 -3 96.6099 16.2572 4 2 -8 3 111.459 14.7104 3 -2 -8 -3 90.395 13.373 5 2 8 3 75.2975 16.1883 1 2 8 4 1078.42 50.2626 5 2 8 4 1180.13 64.2521 1 -2 8 -4 1105.32 51.1947 2 2 -8 5 2013.97 84.402 3 2 8 5 1903.67 96.1053 1 2 8 5 2059.62 80.6331 5 2 -8 6 42.7129 15.1446 3 2 8 6 72.4382 15.9794 5 2 -8 7 257.704 29.2457 3 2 8 7 249.397 25.0078 5 2 8 8 -5.75449 20.7562 1 2 -8 8 14.0304 14.9104 3 2 8 8 2.45544 11.6232 5 2 8 9 31.6179 22.8116 1 2 -8 9 3.92014 15.6364 3 2 8 9 16.2759 17.8674 2 2 8 10 52.9983 29.3511 2 2 -8 10 116.971 25.6995 3 2 8 10 166.341 37.8529 1 2 8 11 -6.35296 22.9153 2 2 8 11 -7.55886 29.4492 1 2 -8 11 28.2934 21.9588 3 2 -8 12 30.4608 23.6615 3 2 8 12 40.6555 28.2389 2 -2 9 13 14.7656 26.6326 1 -2 9 12 -13.5861 27.1042 1 -2 9 12 -46.7184 29.619 2 -2 9 11 25.3531 25.8529 1 -2 9 10 11.5412 22.4842 1 -2 9 9 113.968 28.394 1 -2 9 8 1666.73 90.4875 1 -2 -9 8 1600.22 89.8328 3 -2 9 7 4.19233 14.257 1 -2 9 6 90.5061 20.3813 1 2 9 -6 62.2915 13.7154 1 -2 -9 5 240.546 27.0773 3 -2 9 5 289.966 29.9656 1 -2 -9 4 48.4067 14.1346 3 -2 9 4 32.4816 12.6045 1 -2 -9 3 248.662 25.6301 3 -2 9 3 275.662 26.5515 1 -2 -9 2 1996.5 78.5275 4 -2 9 2 2010.91 85.6288 1 -2 -9 2 2118.56 88.3931 3 2 9 -2 2096.85 76.0346 1 -2 -9 1 1395.08 64.8747 3 2 9 -1 1413.31 57.4275 1 -2 -9 1 1318.37 57.3336 4 -2 9 0 19217.4 572.327 3 2 9 0 19235.5 573.629 1 -2 -9 0 18303.9 570.813 4 2 -9 1 25.5555 5.5183 4 -2 -9 -1 45.0345 10.8357 4 2 9 1 27.0254 11.5031 1 -2 -9 -1 7.13587 8.59976 1 2 9 1 20.1309 8.75253 4 -2 -9 -1 11.4911 8.27759 5 -2 9 -1 11.7314 8.32885 3 2 9 2 4368.84 154.895 1 -2 9 -2 4124.76 143.195 3 2 -9 2 4168.78 146.885 3 -2 -9 -2 4145.28 142.715 5 -2 -9 -2 4479.42 150.544 4 2 -9 3 579.654 34.7604 3 2 9 3 523.602 39.212 1 -2 -9 -3 522.783 35.5255 4 -2 -9 -3 515.756 31.1768 5 2 -9 4 4369.97 150.753 3 2 9 4 4055.71 161.828 1 2 9 5 942.108 61.9921 1 2 -9 5 891.836 50.3161 3 2 -9 6 2740.02 110.66 3 2 9 6 2680.12 102.569 5 2 -9 7 80.4185 21.0812 3 2 9 7 51.0592 15.4357 5 2 -9 8 219.746 29.5985 3 2 9 8 219.549 24.0104 5 2 -9 9 3.96502 15.8115 3 2 9 9 6.51714 21.459 1 2 9 10 12.1784 23.1552 2 2 -9 10 8.76221 17.4754 3 2 9 10 35.2618 28.1252 1 2 9 11 6.50514 25.9431 2 2 -9 11 19.0285 21.4045 3 2 9 11 15.3795 29.9613 1 2 9 12 13.9084 27.0939 2 2 -9 12 5.08369 21.1744 3 -2 10 12 31.688 28.5923 2 -2 10 12 28.2003 24.7338 1 -2 -10 12 46.746 26.6488 3 -2 10 11 13.0633 23.559 1 -2 -10 11 -12.3895 21.7143 3 -2 -10 10 11.4074 19.3991 3 -2 10 10 12.0459 19.8342 1 -2 10 9 261.461 39.4674 1 -2 -10 9 343.538 41.9531 3 -2 -10 8 639.573 52.9755 3 -2 10 8 511.399 49.8744 1 -2 10 7 -4.41224 15.915 1 -2 10 6 71.5003 20.0866 1 -2 10 5 1728.53 84.9828 1 -2 -10 5 1646.04 83.8021 3 -2 -10 4 901.753 53.7516 3 -2 10 4 840.598 52.6701 1 -2 10 3 431.548 19.6703 4 -2 -10 3 440.977 35.3534 3 -2 10 2 2.65235 9.02315 1 -2 -10 2 3.53902 6.56218 4 -2 -10 2 19.8384 11.5578 3 2 10 -2 17.4084 8.07657 1 -2 -10 1 2233.16 84.7762 4 -2 -10 1 2144.32 93.5315 3 2 10 -1 2298.82 85.7149 1 -2 -10 0 374.804 26.3922 4 2 10 0 451.215 30.3822 1 2 10 1 174.68 21.0595 1 -2 10 -1 212.111 20.1927 3 2 -10 1 184.244 11.4194 4 -2 -10 -1 209.779 19.7991 4 -2 -10 -2 3023.21 111.042 5 2 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