#------------------------------------------------------------------------------ #$Date: 2020-07-06 04:52:11 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253795 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126446.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_7126446 loop_ _publ_author_name 'Wang, Jian-Xin' 'Yu, Yi-Shuai' 'Niu, Li-Ya' 'Zou, Bo' 'Wang, Kai' 'Yang, Qing-Zheng' _publ_section_title ; A difluoroboron \b-diketonate based thermometer with temperature-dependent emission wavelength. ; _journal_issue 46 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 6269 _journal_page_last 6272 _journal_paper_doi 10.1039/d0cc01505a _journal_volume 56 _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 7.2099(10) _cell_length_b 10.1738(9) _cell_length_c 49.415(6) _cell_measurement_reflns_used 3802 _cell_measurement_temperature 300.00(17) _cell_measurement_theta_max 28.3110 _cell_measurement_theta_min 2.9160 _cell_volume 3624.7(7) _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 300.00(17) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.883 _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 -18.00 71.00 0.25 0.60 -- 17.58 77.00 90.00 356 2 \w -17.00 31.00 0.25 0.60 -- 17.58 77.00-120.00 192 3 \w 60.00 96.00 0.25 0.60 -- 17.58 77.00-120.00 144 4 \w -56.00 56.00 0.25 0.60 -- -18.36 77.00 150.00 448 ; _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 -0.0750308000 _diffrn_orient_matrix_UB_12 -0.0011965000 _diffrn_orient_matrix_UB_13 -0.0092673000 _diffrn_orient_matrix_UB_21 0.0624956000 _diffrn_orient_matrix_UB_22 -0.0131340000 _diffrn_orient_matrix_UB_23 -0.0107647000 _diffrn_orient_matrix_UB_31 -0.0107777000 _diffrn_orient_matrix_UB_32 -0.0684603000 _diffrn_orient_matrix_UB_33 0.0022017000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_unetI/netI 0.0687 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.883 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 67 _diffrn_reflns_limit_l_min -69 _diffrn_reflns_number 21132 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.883 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.565 _diffrn_reflns_theta_min 2.473 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.02848 _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 1.313 _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 0.338 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 239 _refine_ls_number_reflns 4923 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0887 _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^)+(0.1332P)^2^+1.5942P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2518 _refine_ls_wR_factor_ref 0.2803 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2801 _reflns_number_total 4923 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 300K in Pbca 300k.res created by SHELXL-2018/3 at 13:28:53 on 18-Oct-2019 CELL 0.71073 7.2099 10.1738 49.4149 90 90 90 ZERR 8 0.001 0.0009 0.0056 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 27 BOND $H CONF fmap 2 acta OMIT 1 6 2 OMIT 0 10 8 OMIT 0 6 28 OMIT 0 8 14 OMIT 0 6 2 OMIT 0 8 18 REM REM REM WGHT 0.133200 1.594200 FVAR 1.42416 F1 4 0.203040 0.634531 0.591409 11.00000 0.05863 0.07504 = 0.08104 0.01859 -0.01942 -0.01557 F2 4 0.222043 0.785149 0.624085 11.00000 0.06774 0.06873 = 0.08317 0.01417 0.02061 0.01981 O1 5 0.434642 0.791520 0.588922 11.00000 0.02951 0.06423 = 0.07627 0.02888 0.00116 0.00337 O2 5 0.438199 0.617627 0.623183 11.00000 0.02927 0.05996 = 0.07317 0.02533 -0.00057 -0.00009 O3 5 0.592296 1.140524 0.520483 11.00000 0.05609 0.07583 = 0.07649 0.03610 0.00404 0.00171 C1 1 0.394456 1.144262 0.522100 11.00000 0.05969 0.07991 = 0.07538 0.03166 -0.00537 0.00758 AFIX 137 H1A 2 0.347084 1.203800 0.508706 11.00000 -1.50000 H1B 2 0.357879 1.173605 0.539776 11.00000 -1.50000 H1C 2 0.345511 1.057892 0.518904 11.00000 -1.50000 AFIX 0 C2 1 0.684104 1.055412 0.537226 11.00000 0.04858 0.05110 = 0.05179 0.01434 -0.00008 0.00035 C3 1 0.875561 1.060379 0.535793 11.00000 0.05024 0.06594 = 0.07325 0.02404 0.01084 -0.00756 AFIX 43 H3 2 0.932964 1.118326 0.523889 11.00000 -1.20000 AFIX 0 C4 1 0.981462 0.979403 0.552017 11.00000 0.03662 0.07436 = 0.09126 0.02475 0.00628 -0.00572 AFIX 43 H4 2 1.110157 0.983984 0.551167 11.00000 -1.20000 AFIX 0 C5 1 0.897986 0.891690 0.569492 11.00000 0.03693 0.05868 = 0.07506 0.02025 0.00043 0.00032 AFIX 43 H5 2 0.970196 0.837213 0.580327 11.00000 -1.20000 AFIX 0 C6 1 0.706762 0.885042 0.570844 11.00000 0.03641 0.04009 = 0.04692 0.00449 0.00077 -0.00091 C7 1 0.598244 0.968445 0.554697 11.00000 0.03759 0.04792 = 0.04982 0.01012 0.00062 -0.00021 AFIX 43 H7 2 0.469532 0.965248 0.555740 11.00000 -1.20000 AFIX 0 C8 1 0.614785 0.792207 0.589469 11.00000 0.03231 0.04302 = 0.04466 0.00395 -0.00029 0.00087 C9 1 0.711166 0.709433 0.606295 11.00000 0.02896 0.04963 = 0.05659 0.01309 -0.00174 -0.00111 AFIX 43 H9 2 0.840108 0.711788 0.606455 11.00000 -1.20000 AFIX 0 C10 1 0.618332 0.622601 0.623007 11.00000 0.03203 0.03791 = 0.04656 0.00225 -0.00290 0.00220 C11 1 0.712899 0.533046 0.641870 11.00000 0.03606 0.03840 = 0.04620 0.00382 -0.00161 0.00249 C12 1 0.610794 0.440461 0.656251 11.00000 0.03401 0.04402 = 0.05930 0.00611 -0.00456 -0.00409 AFIX 43 H12 2 0.484579 0.430739 0.652924 11.00000 -1.20000 AFIX 0 C13 1 0.697324 0.362397 0.675604 11.00000 0.04441 0.04440 = 0.05649 0.01084 0.00071 -0.00480 AFIX 43 H13 2 0.627552 0.300184 0.684905 11.00000 -1.20000 AFIX 0 C14 1 0.884991 0.374717 0.681436 11.00000 0.04401 0.03815 = 0.05097 0.00360 -0.00285 0.00360 C15 1 0.985158 0.465746 0.666237 11.00000 0.03462 0.06335 = 0.06995 0.01949 -0.00685 0.00149 AFIX 43 H15 2 1.111839 0.474475 0.669292 11.00000 -1.20000 AFIX 0 C16 1 0.902169 0.543193 0.646823 11.00000 0.03246 0.05728 = 0.06739 0.02298 -0.00081 -0.00253 AFIX 43 H16 2 0.973225 0.602619 0.636973 11.00000 -1.20000 AFIX 0 C17 1 0.980123 0.301070 0.704660 11.00000 0.05478 0.05179 = 0.05580 0.00850 -0.00809 0.00845 C18 1 0.857327 0.190413 0.715917 11.00000 0.09485 0.05580 = 0.06965 0.01970 -0.01127 0.00273 AFIX 137 H18A 2 0.746784 0.227516 0.723594 11.00000 -1.50000 H18B 2 0.924038 0.143247 0.729642 11.00000 -1.50000 H18C 2 0.824434 0.131336 0.701549 11.00000 -1.50000 AFIX 0 C19 1 1.010964 0.399771 0.727558 11.00000 0.10365 0.07574 = 0.07505 0.00618 -0.03408 -0.00360 AFIX 137 H19A 2 1.100618 0.464078 0.721988 11.00000 -1.50000 H19B 2 1.055678 0.354479 0.743303 11.00000 -1.50000 H19C 2 0.895957 0.442725 0.731758 11.00000 -1.50000 AFIX 0 C20 1 1.163037 0.240461 0.695304 11.00000 0.07265 0.12438 = 0.10553 0.05087 0.01050 0.04636 AFIX 137 H20A 2 1.141362 0.186667 0.679659 11.00000 -1.50000 H20B 2 1.213766 0.187470 0.709573 11.00000 -1.50000 H20C 2 1.248943 0.309155 0.690799 11.00000 -1.50000 AFIX 0 B1 3 0.321022 0.708144 0.607017 11.00000 0.02864 0.05473 = 0.06377 0.01662 -0.00095 0.00204 HKLF 4 REM 300K in Pbca REM wR2 = 0.2803, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0887 for 2801 Fo > 4sig(Fo) and 0.1356 for all 4923 data REM 239 parameters refined using 0 restraints END WGHT 0.1335 1.5615 REM Highest difference peak 0.338, deepest hole -0.365, 1-sigma level 0.069 Q1 1 0.3729 1.1487 0.5000 11.00000 0.05 0.34 Q2 1 0.2126 0.6384 0.5702 11.00000 0.05 0.34 Q3 1 0.5954 1.1416 0.4992 11.00000 0.05 0.30 Q4 1 0.4278 0.6250 0.6459 11.00000 0.05 0.30 Q5 1 0.6981 0.7207 0.6255 11.00000 0.05 0.29 REM The information below was added by Olex2. REM REM R1 = 0.0887 for 2801 Fo > 4sig(Fo) and 0.1356 for all 23317 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.34, deepest hole -0.37 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1356 REM R1_gt = 0.0887 REM wR_ref = 0.2803 REM GOOF = 1.046 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 23317 REM Reflections_gt = 2801 REM Parameters = n/a REM Hole = -0.37 REM Peak = 0.34 REM Flack = n/a ; _cod_data_source_file d0cc01505a2.cif _cod_data_source_block 300k_CCDC2 _cod_depositor_comments 'Adding full bibliography for 7126433--7126447.cif.' _cod_database_code 7126446 _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 0.947 _reflns_odcompleteness_completeness 99.77 _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), C18(H18A,H18B,H18C), 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 21.696 _oxdiff_exptl_absorpt_empirical_full_min 0.434 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 F1 F 0.2030(3) 0.63453(19) 0.59141(4) 0.0716(6) Uani 1 1 d . . . . . F2 F 0.2220(3) 0.7851(2) 0.62408(4) 0.0732(6) Uani 1 1 d . . . . . O1 O 0.4346(2) 0.7915(2) 0.58892(4) 0.0567(6) Uani 1 1 d . . . . . O2 O 0.4382(2) 0.6176(2) 0.62318(4) 0.0541(5) Uani 1 1 d . . . . . O3 O 0.5923(3) 1.1405(2) 0.52048(5) 0.0695(7) Uani 1 1 d . . . . . C1 C 0.3945(5) 1.1443(4) 0.52210(7) 0.0717(10) Uani 1 1 d . . . . . H1A H 0.347084 1.203800 0.508706 0.107 Uiso 1 1 calc GR . . . . H1B H 0.357879 1.173605 0.539776 0.107 Uiso 1 1 calc GR . . . . H1C H 0.345511 1.057892 0.518904 0.107 Uiso 1 1 calc GR . . . . C2 C 0.6841(4) 1.0554(3) 0.53723(5) 0.0505(7) Uani 1 1 d . . . . . C3 C 0.8756(4) 1.0604(3) 0.53579(7) 0.0631(8) Uani 1 1 d . . . . . H3 H 0.932964 1.118326 0.523889 0.076 Uiso 1 1 calc R . . . . C4 C 0.9815(4) 0.9794(4) 0.55202(7) 0.0674(9) Uani 1 1 d . . . . . H4 H 1.110157 0.983984 0.551167 0.081 Uiso 1 1 calc R . . . . C5 C 0.8980(4) 0.8917(3) 0.56949(6) 0.0569(8) Uani 1 1 d . . . . . H5 H 0.970196 0.837213 0.580327 0.068 Uiso 1 1 calc R . . . . C6 C 0.7068(3) 0.8850(2) 0.57084(5) 0.0411(6) Uani 1 1 d . . . . . C7 C 0.5982(4) 0.9684(3) 0.55470(5) 0.0451(6) Uani 1 1 d . . . . . H7 H 0.469532 0.965248 0.555740 0.054 Uiso 1 1 calc R . . . . C8 C 0.6148(3) 0.7922(2) 0.58947(5) 0.0400(6) Uani 1 1 d . . . . . C9 C 0.7112(3) 0.7094(3) 0.60630(5) 0.0451(6) Uani 1 1 d . . . . . H9 H 0.840108 0.711788 0.606455 0.054 Uiso 1 1 calc R . . . . C10 C 0.6183(3) 0.6226(2) 0.62301(5) 0.0388(5) Uani 1 1 d . . . . . C11 C 0.7129(3) 0.5330(2) 0.64187(5) 0.0402(6) Uani 1 1 d . . . . . C12 C 0.6108(4) 0.4405(3) 0.65625(5) 0.0458(6) Uani 1 1 d . . . . . H12 H 0.484579 0.430739 0.652924 0.055 Uiso 1 1 calc R . . . . C13 C 0.6973(4) 0.3624(3) 0.67560(5) 0.0484(6) Uani 1 1 d . . . . . H13 H 0.627552 0.300184 0.684905 0.058 Uiso 1 1 calc R . . . . C14 C 0.8850(4) 0.3747(2) 0.68144(5) 0.0444(6) Uani 1 1 d . . . . . C15 C 0.9852(4) 0.4657(3) 0.66624(6) 0.0560(8) Uani 1 1 d . . . . . H15 H 1.111839 0.474475 0.669292 0.067 Uiso 1 1 calc R . . . . C16 C 0.9022(4) 0.5432(3) 0.64682(6) 0.0524(7) Uani 1 1 d . . . . . H16 H 0.973225 0.602619 0.636973 0.063 Uiso 1 1 calc R . . . . C17 C 0.9801(4) 0.3011(3) 0.70466(6) 0.0541(7) Uani 1 1 d . . . . . C18 C 0.8573(5) 0.1904(3) 0.71592(7) 0.0734(10) Uani 1 1 d . . . . . H18A H 0.746784 0.227516 0.723594 0.110 Uiso 1 1 calc GR . . . . H18B H 0.924038 0.143247 0.729642 0.110 Uiso 1 1 calc GR . . . . H18C H 0.824434 0.131336 0.701549 0.110 Uiso 1 1 calc GR . . . . C19 C 1.0110(6) 0.3998(4) 0.72756(8) 0.0848(12) Uani 1 1 d . . . . . H19A H 1.100618 0.464078 0.721988 0.127 Uiso 1 1 calc GR . . . . H19B H 1.055678 0.354479 0.743303 0.127 Uiso 1 1 calc GR . . . . H19C H 0.895957 0.442725 0.731758 0.127 Uiso 1 1 calc GR . . . . C20 C 1.1630(5) 0.2405(5) 0.69530(9) 0.1009(16) Uani 1 1 d . . . . . H20A H 1.141362 0.186667 0.679659 0.151 Uiso 1 1 calc GR . . . . H20B H 1.213766 0.187470 0.709573 0.151 Uiso 1 1 calc GR . . . . H20C H 1.248943 0.309155 0.690799 0.151 Uiso 1 1 calc GR . . . . B1 B 0.3210(4) 0.7081(3) 0.60702(7) 0.0490(8) 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 0.0586(11) 0.0750(12) 0.0810(12) 0.0186(10) -0.0194(9) -0.0156(9) F2 0.0677(13) 0.0687(12) 0.0832(12) 0.0142(10) 0.0206(10) 0.0198(10) O1 0.0295(10) 0.0642(12) 0.0763(14) 0.0289(10) 0.0012(8) 0.0034(9) O2 0.0293(10) 0.0600(12) 0.0732(13) 0.0253(10) -0.0006(8) -0.0001(8) O3 0.0561(13) 0.0758(15) 0.0765(14) 0.0361(12) 0.0040(11) 0.0017(12) C1 0.060(2) 0.080(2) 0.075(2) 0.0317(18) -0.0054(16) 0.0076(18) C2 0.0486(16) 0.0511(15) 0.0518(15) 0.0143(12) -0.0001(12) 0.0003(13) C3 0.0502(18) 0.0659(19) 0.0733(19) 0.0240(16) 0.0108(14) -0.0076(15) C4 0.0366(15) 0.074(2) 0.091(2) 0.0247(18) 0.0063(14) -0.0057(14) C5 0.0369(15) 0.0587(17) 0.0751(19) 0.0203(15) 0.0004(13) 0.0003(13) C6 0.0364(13) 0.0401(12) 0.0469(13) 0.0045(10) 0.0008(10) -0.0009(10) C7 0.0376(13) 0.0479(13) 0.0498(14) 0.0101(11) 0.0006(10) -0.0002(11) C8 0.0323(12) 0.0430(12) 0.0447(13) 0.0040(10) -0.0003(10) 0.0009(10) C9 0.0290(12) 0.0496(14) 0.0566(15) 0.0131(12) -0.0017(10) -0.0011(11) C10 0.0320(12) 0.0379(12) 0.0466(13) 0.0022(10) -0.0029(10) 0.0022(10) C11 0.0361(13) 0.0384(11) 0.0462(13) 0.0038(10) -0.0016(10) 0.0025(10) C12 0.0340(13) 0.0440(13) 0.0593(15) 0.0061(12) -0.0046(11) -0.0041(11) C13 0.0444(15) 0.0444(13) 0.0565(15) 0.0108(12) 0.0007(12) -0.0048(12) C14 0.0440(14) 0.0381(12) 0.0510(14) 0.0036(11) -0.0029(11) 0.0036(11) C15 0.0346(14) 0.0634(18) 0.0700(18) 0.0195(15) -0.0069(12) 0.0015(13) C16 0.0325(13) 0.0573(16) 0.0674(17) 0.0230(14) -0.0008(12) -0.0025(12) C17 0.0548(17) 0.0518(16) 0.0558(16) 0.0085(13) -0.0081(13) 0.0084(13) C18 0.095(3) 0.0558(18) 0.070(2) 0.0197(16) -0.0113(18) 0.0027(18) C19 0.104(3) 0.076(2) 0.075(2) 0.0062(19) -0.034(2) -0.004(2) C20 0.073(3) 0.124(4) 0.106(3) 0.051(3) 0.011(2) 0.046(3) B1 0.0286(14) 0.0547(17) 0.0638(19) 0.0166(15) -0.0009(13) 0.0020(13) 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 123.0(2) . . ? C10 O2 B1 122.8(2) . . ? C2 O3 C1 117.8(2) . . ? 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 115.4(2) . . ? O3 C2 C7 124.5(3) . . ? C7 C2 C3 120.1(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 119.7 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.7 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(3) . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 119.9(2) . . ? C5 C6 C8 120.6(2) . . ? C7 C6 C8 119.4(2) . . ? C2 C7 C6 119.5(2) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? O1 C8 C6 116.1(2) . . ? O1 C8 C9 121.0(2) . . ? C9 C8 C6 122.9(2) . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.6(2) . . ? C10 C9 H9 119.7 . . ? O2 C10 C9 120.8(2) . . ? O2 C10 C11 115.8(2) . . ? C9 C10 C11 123.4(2) . . ? C12 C11 C10 119.9(2) . . ? C16 C11 C10 121.4(2) . . ? C16 C11 C12 118.7(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C12 C13 H13 119.1 . . ? C14 C13 C12 121.9(2) . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 116.9(2) . . ? C13 C14 C17 123.2(2) . . ? C15 C14 C17 119.8(2) . . ? C14 C15 H15 119.0 . . ? C16 C15 C14 122.0(3) . . ? C16 C15 H15 119.0 . . ? C11 C16 H16 119.8 . . ? C15 C16 C11 120.4(2) . . ? C15 C16 H16 119.8 . . ? C14 C17 C18 111.8(3) . . ? C19 C17 C14 107.3(3) . . ? C19 C17 C18 107.3(3) . . ? C20 C17 C14 110.9(3) . . ? C20 C17 C18 108.1(3) . . ? C20 C17 C19 111.3(3) . . ? 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 . . ? 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 . . ? F1 B1 O1 108.5(2) . . ? F1 B1 O2 108.5(2) . . ? F2 B1 F1 109.8(2) . . ? F2 B1 O1 109.7(3) . . ? F2 B1 O2 108.9(2) . . ? O1 B1 O2 111.5(2) . . ? 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(4) . ? F2 B1 1.354(4) . ? O1 C8 1.299(3) . ? O1 B1 1.480(4) . ? O2 C10 1.300(3) . ? O2 B1 1.483(3) . ? O3 C1 1.429(4) . ? O3 C2 1.368(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.383(4) . ? C2 C7 1.383(4) . ? C3 H3 0.9300 . ? C3 C4 1.380(4) . ? C4 H4 0.9300 . ? C4 C5 1.380(4) . ? C5 H5 0.9300 . ? C5 C6 1.382(4) . ? C6 C7 1.403(3) . ? C6 C8 1.476(3) . ? C7 H7 0.9300 . ? C8 C9 1.372(3) . ? C9 H9 0.9300 . ? C9 C10 1.382(3) . ? C10 C11 1.471(3) . ? C11 C12 1.391(3) . ? C11 C16 1.390(4) . ? C12 H12 0.9300 . ? C12 C13 1.391(4) . ? C13 H13 0.9300 . ? C13 C14 1.389(4) . ? C14 C15 1.394(4) . ? C14 C17 1.533(4) . ? C15 H15 0.9300 . ? C15 C16 1.378(4) . ? C16 H16 0.9300 . ? C17 C18 1.536(5) . ? C17 C19 1.529(5) . ? C17 C20 1.527(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 O1 C8 C9 C10 0.3(4) . . . . ? O2 C10 C11 C12 7.0(4) . . . . ? O2 C10 C11 C16 -169.6(3) . . . . ? O3 C2 C3 C4 179.4(3) . . . . ? O3 C2 C7 C6 179.6(3) . . . . ? C1 O3 C2 C3 -176.9(3) . . . . ? C1 O3 C2 C7 3.2(5) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C2 C7 C6 -0.3(4) . . . . ? C3 C4 C5 C6 -0.2(6) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? C4 C5 C6 C8 -179.8(3) . . . . ? C5 C6 C7 C2 1.0(4) . . . . ? C5 C6 C8 O1 -178.8(3) . . . . ? C5 C6 C8 C9 0.4(4) . . . . ? C6 C8 C9 C10 -178.8(2) . . . . ? C7 C2 C3 C4 -0.7(5) . . . . ? C7 C6 C8 O1 2.2(4) . . . . ? C7 C6 C8 C9 -178.6(2) . . . . ? C8 O1 B1 F1 -125.5(3) . . . . ? C8 O1 B1 F2 114.5(3) . . . . ? C8 O1 B1 O2 -6.2(4) . . . . ? C8 C6 C7 C2 -180.0(2) . . . . ? C8 C9 C10 O2 -0.1(4) . . . . ? C8 C9 C10 C11 -178.8(2) . . . . ? C9 C10 C11 C12 -174.3(2) . . . . ? C9 C10 C11 C16 9.2(4) . . . . ? C10 O2 B1 F1 125.7(3) . . . . ? C10 O2 B1 F2 -114.7(3) . . . . ? C10 O2 B1 O1 6.4(4) . . . . ? C10 C11 C12 C13 -175.1(2) . . . . ? C10 C11 C16 C15 174.5(3) . . . . ? C11 C12 C13 C14 0.8(4) . . . . ? C12 C11 C16 C15 -2.1(4) . . . . ? C12 C13 C14 C15 -2.4(4) . . . . ? C12 C13 C14 C17 173.2(3) . . . . ? C13 C14 C15 C16 1.9(5) . . . . ? C13 C14 C17 C18 13.5(4) . . . . ? C13 C14 C17 C19 -103.9(3) . . . . ? C13 C14 C17 C20 134.3(4) . . . . ? C14 C15 C16 C11 0.4(5) . . . . ? C15 C14 C17 C18 -171.0(3) . . . . ? C15 C14 C17 C19 71.6(4) . . . . ? C15 C14 C17 C20 -50.2(4) . . . . ? C16 C11 C12 C13 1.5(4) . . . . ? C17 C14 C15 C16 -173.9(3) . . . . ? B1 O1 C8 C6 -177.6(3) . . . . ? B1 O1 C8 C9 3.2(4) . . . . ? B1 O2 C10 C9 -3.6(4) . . . . ? B1 O2 C10 C11 175.2(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 6 2391.46 231.966 2 0 0 -7 63.3584 8.10246 1 0 0 7 60.364 7.69455 2 0 0 8 5184.59 451.683 2 0 0 -8 4147.92 451.659 1 0 0 -9 7.8056 5.14682 1 0 0 9 7.03791 3.90147 1 0 0 9 11.6502 4.54987 2 0 0 10 4850.87 450.44 2 0 0 -10 4749.47 450.967 1 0 0 10 4410.72 450.11 1 0 0 -11 54.8657 11.6799 1 0 0 11 69.7493 10.5658 1 0 0 -12 12958.7 1432.34 1 0 0 12 16139.8 1431.95 2 0 0 12 15034.7 1431.56 1 0 0 13 369.324 36.8634 1 0 0 -13 285.05 37.6187 1 0 0 13 393.843 37.2408 2 0 0 14 3647.63 324.587 2 0 0 -14 3328.74 325.387 1 0 0 14 3106.6 323.785 1 0 0 -15 16.5531 8.46103 1 0 0 15 37.0748 9.24874 2 0 0 16 10694.7 926.194 2 0 0 16 9680.5 925.44 1 0 0 -16 8167.96 926.469 1 0 0 17 20.9094 5.61618 1 0 0 -17 13.761 8.87433 1 0 0 17 13.0835 6.40032 2 0 0 18 2207.96 219.983 1 0 0 -18 2141.54 221.903 1 0 0 18 2389.62 220.909 2 0 0 19 103.927 14.0357 2 0 0 19 83.8996 11.0567 1 0 0 -20 10903.5 1237.78 1 0 0 20 13079.5 1236 1 0 0 20 14003.4 1237.19 2 0 0 21 11.4805 7.68684 2 0 0 -21 2.86213 10.5784 1 0 0 21 11.8785 6.44381 1 0 0 -22 351.915 46.5233 1 0 0 22 449.295 45.6871 2 0 0 22 433.207 44.0422 1 0 0 -23 9.80568 10.7869 1 0 0 23 13.6807 6.44266 1 0 0 23 18.7742 9.05847 2 0 0 24 532.999 57.0945 1 0 0 24 633.066 59.2474 2 0 0 -24 485.776 60.2148 1 0 0 25 38.3334 11.4455 2 0 0 25 44.8027 9.72278 1 0 0 -26 1920.56 230.748 1 0 0 26 2606.04 228.82 1 0 0 27 167.972 18.4614 1 0 0 -27 39.8225 18.7064 1 0 0 28 9780.97 842.56 1 0 0 -28 7144.9 844.56 1 0 0 29 48.7697 11.6556 1 0 0 -29 7.99173 17.6872 1 0 0 30 2494.3 208.306 1 0 0 -30 1626.6 209.392 1 0 0 31 49.3282 12.7929 1 0 0 -31 17.0122 15.5809 1 0 0 32 2939.8 232.657 1 0 0 -32 1720.65 232.86 1 0 0 33 110.742 16.9084 1 0 0 -33 -2.25834 19.1218 1 0 0 34 5443.7 379.933 1 0 0 -34 2537.38 378.495 1 0 0 35 81.0497 15.5139 1 0 0 -35 22.0069 20.3902 1 0 0 36 2864.64 191.543 1 0 0 -36 1143.63 189.342 1 0 0 37 71.6332 15.9469 1 0 0 -37 10.391 22.9695 1 0 0 38 2895.62 189.599 1 0 0 -38 1089.74 187.001 1 0 0 -39 58.0353 23.4011 1 0 0 39 40.3642 14.0015 1 0 0 40 861.892 90.478 1 0 0 41 13.1539 11.5226 1 0 0 42 60.3524 16.6458 1 0 0 43 15.3724 12.7517 1 0 0 44 116.202 20.8488 1 0 0 45 12.4861 13.4734 1 0 0 46 5.56681 13.8705 1 0 0 47 5.72656 15.6472 1 0 0 48 213.869 31.3431 1 0 0 49 -5.89661 15.4184 1 0 0 50 7.76063 16.5675 1 0 0 51 13.4258 18.7791 1 0 0 52 429.357 52.0255 1 0 0 53 56.941 20.0301 4 0 0 54 528.307 60.4603 4 0 0 55 501.476 60.2971 4 0 0 56 5336.88 523.93 4 0 0 -57 387.472 83.3074 3 0 0 57 129.85 29.0407 4 0 0 -58 391.516 100.047 3 0 0 58 770.445 77.9982 4 0 0 -59 186.996 81.4938 3 0 0 -60 419.526 94.163 3 0 0 -61 225.618 91.3237 3 0 0 -62 352.533 92.553 3 0 0 -63 76.4621 61.5543 3 0 0 -64 -15.2426 62.4516 3 0 0 -65 7.89862 61.9221 3 0 0 -66 8.13045 60.2921 3 0 0 -67 126 72.2877 3 0 -1 3 30.0995 9.34726 2 0 -1 4 -0.95119 6.16788 2 0 1 4 3.28627 4.26197 4 0 1 -4 -0.42603 3.22821 4 0 1 4 -2.16259 4.25073 1 0 -1 -4 -0.7099 4.0876 4 0 -1 -4 -0.69279 3.98905 1 0 1 4 6.16038 4.27323 3 0 -1 5 -3.47433 6.15055 2 0 1 -5 -0.7115 4.47944 2 0 1 5 -2.82482 5.00104 4 0 1 -5 1.68408 3.93546 4 0 1 5 0.78435 5.32565 1 0 -1 -5 3.66566 5.23334 1 0 1 5 4.90485 4.13031 3 0 1 -6 4.05133 3.81365 4 0 -1 -6 3.22707 6.2878 1 0 1 -6 2.68682 4.76285 2 0 -1 6 -1.5977 6.50979 2 0 1 6 3.08035 4.21364 3 0 1 -7 3.05198 3.86278 4 0 1 7 10.4442 6.07752 3 0 -1 -7 -0.87645 6.87373 1 0 1 -7 -0.69939 5.96987 2 0 -1 7 -3.05803 6.77381 2 0 -1 8 -0.8166 4.84343 4 0 1 -8 1.68971 4.22216 4 0 1 8 -4.20926 6.42093 3 0 -1 8 3.03072 7.46363 2 0 1 -8 6.29183 6.2866 2 0 -1 -8 -1.88086 7.97799 1 0 1 -9 2.41576 3.98815 4 0 -1 -9 13.0983 9.54609 1 0 -1 9 0.78348 7.01088 2 0 1 -9 -5.01221 5.76017 2 0 -1 9 2.79536 4.73831 4 0 1 -10 8.86679 5.90335 2 0 -1 -10 -3.22734 8.37276 1 0 -1 10 -0.81948 7.0901 2 0 -1 10 21.9071 5.32957 4 0 -1 11 -2.58639 4.0878 4 0 -1 -11 -9.17995 9.05603 1 0 1 -11 6.15682 5.87484 2 0 -1 11 -3.456 6.86386 2 0 -1 -12 12.1983 9.44156 1 0 -1 12 -1.81884 6.18294 2 0 -1 12 -0.45146 4.25153 4 0 -1 -12 10.4605 7.65553 3 0 1 12 9.38577 6.50549 1 0 1 -13 -1.19082 3.01838 1 0 -1 -13 3.13791 7.286 3 0 -1 -13 7.76366 8.14517 1 0 -1 13 -1.89981 6.39265 2 0 -1 13 6.7046 4.15398 4 0 1 13 -1.08189 6.52671 1 0 -1 -14 2.73707 8.78811 1 0 -1 14 -1.94667 6.3113 2 0 1 -14 1.65673 3.06757 1 0 -1 14 -1.54799 4.04493 4 0 -1 14 0.66419 2.97126 1 0 1 14 -3.34391 6.57239 1 0 -1 15 2.01708 7.02633 2 0 -1 -15 -2.88893 8.21618 1 0 -1 15 6.09498 4.48681 4 0 1 15 1.17318 7.23386 1 0 -1 15 -0.68808 3.03508 1 0 1 -15 3.14629 3.35854 1 0 -1 16 0.59507 4.17925 4 0 -1 -16 9.12466 9.375 1 0 1 -16 -2.66602 3.74817 1 0 -1 16 5.26036 6.48565 2 0 -1 16 1.11114 3.17717 1 0 1 16 -1.17417 7.16088 1 0 1 17 -1.1942 6.44421 1 0 -1 17 1.57039 3.27633 1 0 -1 17 -1.09415 6.67409 2 0 1 -17 -0.50455 4.00897 1 0 -1 -17 -11.2011 9.86517 1 0 -1 17 -3.77105 4.30601 4 0 -1 18 0.42558 3.69188 1 0 1 -18 5.29355 4.90577 1 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1390.62 150.931 4 2 -4 3 13.4508 12.2449 1 -2 4 3 -1.81704 9.1509 1 2 -4 -3 7.68989 10.6874 1 2 4 3 23.255 11.3068 4 -2 4 -3 10.6346 8.74264 1 2 -4 3 29.7906 17.2046 4 2 4 3 18.7382 8.39633 2 2 -4 -3 3.12891 13.3342 4 2 -4 -4 68.9288 18.5799 1 2 -4 4 64.0273 16.2235 1 2 4 -4 84.6744 20.2442 4 -2 4 4 94.1559 16.7765 1 2 4 -4 114.322 15.2348 2 2 4 4 77.124 14.3976 2 2 -4 -4 88.9676 21.8496 4 -2 4 -4 79.3228 14.8672 1 2 -4 -5 683.651 78.4082 1 2 -4 5 697.773 76.7445 1 -2 4 5 729.941 78.0907 1 2 -4 -5 546.576 80.7208 4 -2 4 -5 687.539 75.6778 1 2 4 -5 765.453 75.2501 2 2 4 5 726.448 74.2219 2 2 4 -5 714.182 79.3708 4 2 -4 -6 1943.39 238.191 4 2 -4 6 2208.9 233.086 1 2 4 6 2408.54 231.162 2 -2 4 -6 2065.26 231.979 1 -2 4 6 2305.09 234.651 1 2 4 -6 2495.87 232.192 2 2 4 -6 2249.14 235.216 4 2 4 7 10520.2 1026.2 2 2 -4 7 10167.6 1028.26 1 2 -4 -7 9826.98 1034.81 4 -2 4 -7 10167.2 1027.41 1 -2 4 7 9981.06 1029.61 1 2 4 -7 10871.3 1027.45 2 2 4 -7 9623.08 1029.64 4 -2 -4 8 35287.6 3159.96 2 2 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1844.35 179.134 4 2 4 13 1425.91 166.885 3 -2 4 -13 1651.2 168.318 1 -2 4 13 1804.27 173.972 1 2 -4 13 1959.54 171.926 1 2 4 -13 1908.21 171.637 2 -2 -4 13 1857.1 176.069 2 2 4 -13 1927.09 170.669 4 2 -4 -13 1598.1 177.551 4 2 -4 -14 60.0178 20.9905 4 -2 4 14 36.6646 13.1266 1 2 -4 14 31.0065 13.3215 1 2 4 -14 79.3026 15.2221 2 2 4 14 68.6754 11.0874 3 2 -4 14 37.0823 17.6496 4 -2 4 -14 34.5824 8.82828 1 2 4 -14 27.2825 12.3891 4 -2 4 15 1699.2 176.445 1 -2 4 -15 1727.46 170.682 1 2 -4 15 1588.95 179.641 4 2 -4 15 1898.87 175.218 1 2 4 -15 1629.2 172.143 4 2 4 -15 1821.35 174.047 2 2 -4 -15 1782.48 181.93 4 -2 4 -16 1973.4 205.549 1 2 4 -16 2159.49 209.153 2 2 -4 16 2292.45 210.663 1 -2 4 16 2170.21 212.265 1 2 -4 16 2170.42 216.046 4 2 4 -16 2006.71 206.8 4 2 -4 -16 2294.08 217.919 4 2 -4 -17 111.834 26.9373 4 -2 4 -17 128.759 16.6277 1 2 4 -17 188.942 22.0648 2 2 4 -17 138.446 19.0733 4 -2 4 17 99.2729 22.4019 1 2 -4 17 140.222 27.148 4 2 -4 17 133.573 23.1897 1 2 -4 -18 16.9249 16.7722 4 2 -4 18 -7.27411 15.4491 1 -2 4 -18 9.88378 15.2169 2 -2 4 -18 10.694 6.4261 1 2 4 -18 34.3674 9.16586 4 2 -4 18 14.7494 14.6439 4 -2 4 -19 1643.04 147.705 1 -2 4 -19 1315.26 156.584 2 2 4 -19 1531.89 147.308 4 2 -4 19 1064.71 150.83 1 2 -4 19 1711.06 158.697 4 2 -4 -19 1654.98 160.303 4 2 -4 20 2443.86 210.851 4 2 4 -20 2109.19 198.094 4 2 -4 -20 2683.08 214.884 4 -2 4 -20 2313.64 211.787 2 2 -4 21 2575.12 195.102 4 -2 4 -21 2430.65 196.49 2 2 4 -21 1696.23 179.332 4 2 4 21 1849.63 210.33 1 2 -4 -21 2570.81 197.739 4 2 -4 22 957.868 103.48 4 -2 4 -22 1018.5 105.085 2 2 4 22 641.351 115.382 1 2 -4 -22 987.993 105.252 4 2 -4 -23 49.0968 20.3775 4 2 -4 23 58.1188 19.0261 4 -2 4 -23 57.604 20.4114 2 2 4 23 39.3148 47.1909 1 2 4 24 1016.99 147.919 1 -2 4 24 1254.29 130.949 1 2 -4 24 1305.95 133.375 4 -2 4 -24 1208.37 133.581 2 2 -4 -24 1324.01 136.274 4 -2 4 25 2.5679 12.1351 1 2 -4 25 14.7487 14.641 4 -2 4 -25 41.0844 19.3593 2 2 -4 -25 7.43601 16.8146 4 2 4 25 24.4024 8.12949 2 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2 -5 -4 1548.86 171.115 4 2 5 -4 1791.18 169.09 4 2 5 -5 103.835 23.3153 4 -2 5 -5 38.3555 14.3462 1 -2 5 5 50.313 14.3619 1 2 5 -5 91.5902 16.2584 2 2 -5 5 2.38029 15.6303 1 2 5 5 76.1746 15.7839 2 2 -5 -5 23.1685 19.0258 4 2 5 -6 115.769 24.4468 4 -2 5 -6 131.561 20.0553 1 2 -5 -6 68.8179 22.9116 4 -2 5 6 95.0375 19.491 1 2 -5 6 152.232 23.9842 1 2 5 -6 96.3138 17.9833 2 2 5 6 86.0932 17.7953 2 2 5 -7 27.5506 17.3451 4 -2 5 -7 60.0406 14.0804 1 -2 5 7 60.2927 15.3824 1 2 5 -7 69.063 14.4964 2 2 -5 7 57.3697 17.4404 1 2 5 7 61.5042 14.2395 2 2 -5 -7 23.0851 17.3855 4 2 -5 -8 259.854 44.2391 4 -2 -5 8 450.788 65.879 2 2 5 -8 319.675 41.6908 4 2 -5 8 252.33 40.2436 1 2 -5 8 287.919 45.4246 4 -2 5 -8 367.863 38.5131 1 2 5 -8 334.837 38.0251 2 -2 5 8 302.363 39.365 1 2 5 8 280.757 37.7317 2 2 -5 -9 7.71289 15.907 4 -2 5 -9 -4.94 9.27433 1 -2 5 9 -2.28076 9.86141 1 2 5 9 2.09238 16.6319 2 2 -5 9 -3.98848 18.3012 4 2 -5 9 -2.46598 14.7259 1 2 5 -9 20.5248 13.9265 4 2 5 -10 533.096 55.1436 2 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57.8953 35.2297 1 2 11 -29 61.1478 29.4668 2 -2 11 -29 108.66 30.3202 2 2 -11 30 39.0431 36.1582 4 -2 11 30 88.0804 36.3745 1 2 11 -30 70.8894 27.9385 2 -2 11 -30 64.4356 26.9626 2 -2 11 31 59.5331 33.9941 1 2 11 -31 18.9036 23.5059 2 -2 11 -31 21.5442 22.1293 2 2 -11 31 58.2569 36.4771 4 -2 11 32 48.3375 31.9753 1 2 11 32 -12.0236 57.3733 1 2 11 -32 48.7159 23.504 2 -2 11 -32 34.3012 24.7661 2 2 -11 32 96.7916 39.1636 4 2 11 -33 3.76393 21.6793 2 -2 11 -33 -12.9629 21.2891 2 2 11 -34 22.3672 22.3306 2 2 -11 34 19.1499 33.0373 4 2 11 -35 -3.72798 21.4675 2 2 11 -36 11.2803 22.1811 2 2 -11 36 -38.091 35.1961 4 2 11 -37 11.3911 21.6218 2 -2 12 0 33.9422 26.6606 1 2 -12 0 58.5072 35.6242 4 2 12 0 77.8143 32.4121 1 2 -12 1 175.458 52.5287 4 2 -12 -1 176.451 52.2775 4 -2 12 -1 134.074 36.202 1 -2 12 1 58.8632 29.7746 1 2 12 1 51.155 33.8684 1 2 12 -1 16.3928 26.4913 1 2 -12 2 25.0176 39.7777 4 2 -12 -2 59.2279 40.3564 4 -2 12 -2 42.5417 29.2737 1 -2 12 2 44.9228 29.2222 1 2 12 2 5.78943 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23.2141 29.0561 1 2 13 -5 5.2413 23.5656 1 -2 13 -6 -9.55787 45.5923 2 2 -13 6 17.2917 45.4471 4 2 -13 -6 83.1753 52.6573 4 -2 13 6 32.2814 30.7682 1 2 13 6 51.9612 31.3166 1 2 13 -6 31.0846 26.9562 1 -2 13 -7 90.8137 44.8662 2 2 -13 7 17.0952 40.8239 4 -2 13 7 38.0405 29.9334 1 2 13 7 35.3156 34.8857 1 2 13 -7 25.614 27.4803 1 -2 13 -8 8.46428 39.5494 2 2 -13 8 17.0638 40.5967 4 -2 13 8 -5.48571 29.598 1 2 13 8 -5.95092 28.3168 1 2 13 -8 -10.2644 26.9108 1 2 -13 9 -8.49718 41.2412 4 -2 13 9 22.1554 29.1757 1 2 13 9 60.7058 32.8713 1 -2 13 -9 40.2121 40.3616 2 2 13 -9 30.4949 26.0038 1 -2 13 -10 7.59344 37.9712 2 2 -13 10 150.689 53.1021 4 -2 13 10 122.968 38.5102 1 2 13 -10 50.3725 27.5904 1 -2 13 -11 80.4624 42.5472 2 2 -13 11 82.8018 47.4757 4 -2 13 11 67.6796 34.1785 1 2 13 -11 44.9523 27.9792 1 2 -13 12 -8.18677 36.0753 4 -2 13 12 34.1433 29.4084 1 2 13 -12 -29.7396 26.7571 1 -2 13 13 11.4828 27.8103 1 2 -13 13 40.415 41.7584 4 2 13 -13 -4.92281 24.6558 1 2 -13 15 15.787 38.9062 4 2 -13 16 7.84772 38.0088 4 2 -13 17 38.9905 41.6541 4 2 -13 18 -7.71571 38.0601 4 2 13 -18 44.4559 27.0346 2 2 -13 19 23.0281 38.5002 4 2 13 -19 24.481 25.2593 2 2 -13 20 45.5779 40.5404 4 2 13 -20 28.6002 26.4369 2 2 -13 21 -7.54057 37.7764 4 2 13 -21 -16.2279 22.2315 2 2 -13 22 -7.46462 38.0919 4 2 13 -22 52.7251 27.2177 2 2 -13 23 -7.42851 39.5176 4 2 13 -23 4.10845 25.327 2 2 -13 24 36.7822 39.7646 4 2 13 -24 21.0594 24.3736 2 2 -13 25 73.46 42.886 4 2 -13 26 14.5555 35.8713 4 2 -13 27 -14.4259 39.4764 4 2 -13 28 21.477 38.6797 4 -2 14 0 31.398 29.5416 1 3 0 0 18.0098 11.4285 4 -3 0 0 5.68165 11.4095 3 -3 0 -1 10.1463 11.9675 3 -3 0 1 5.58332 11.5316 3 3 0 -1 2.99724 8.65221 4 -3 0 -2 17793.8 1704.59 3 -3 0 2 19716.6 1704.72 3 3 0 -2 17625.4 1704.74 4 -3 0 2 15936.6 1701.68 4 3 0 2 18389.9 1705.09 4 3 0 3 7.83588 10.1795 4 -3 0 -3 -2.9781 11.3771 3 -3 0 3 12.3844 11.2204 3 3 0 -3 4.49722 8.43922 4 -3 0 3 7.84066 6.98833 4 3 0 -4 21.7235 14.2246 3 -3 0 4 14.7281 7.20206 4 -3 0 -4 29.6987 12.7516 3 -3 0 4 26.0177 12.0386 3 3 0 -4 13.6115 9.72357 4 3 0 4 30.1806 10.2924 4 3 0 -5 13.5592 12.5448 3 3 0 5 3.24977 9.03228 4 3 0 -5 5.92724 10.2571 1 -3 0 5 19.7278 11.1393 3 -3 0 5 0.85957 6.45613 4 3 0 -5 13.8094 10.4387 4 3 0 -6 5037.95 506.874 1 3 0 -6 6270.6 513.248 3 -3 0 6 6382.28 508.683 3 -3 0 6 4209.87 503.926 4 3 0 -6 5324.81 507.942 4 3 0 6 5919.27 509.076 4 3 0 -7 11.4902 14.7593 3 3 0 -7 -2.84743 9.58372 1 -3 0 7 -1.48868 11.2825 3 3 0 7 9.98645 10.0431 4 -3 0 7 5.92097 6.8924 4 3 0 -7 -3.2255 10.4607 4 3 0 -8 4643.06 469.641 1 3 0 -8 5879.47 475.666 3 -3 0 8 5230.4 471.237 3 3 0 8 5760.39 472.382 4 3 0 -8 4636.21 470.034 4 -3 0 8 4155.19 466.929 4 3 0 -9 -6.83907 13.9101 3 3 0 -9 -8.64036 10.843 1 3 0 9 -6.84185 10.0954 4 -3 0 9 3.45937 7.09872 4 3 0 -9 -7.42084 9.25673 4 3 0 -10 15.7326 12.5837 3 3 0 -10 26.6718 11.1296 1 3 0 10 7.02926 9.64558 4 -3 0 10 17.3772 7.70084 4 3 0 -10 29.8371 11.2834 4 3 0 -11 6.70543 12.0591 3 -3 0 11 -0.87671 6.87266 4 3 0 11 -3.54812 9.57146 4 3 0 -11 -1.48069 8.62873 4 3 0 -11 6.02566 9.28649 1 3 0 -12 561.339 57.2904 1 3 0 -12 512.547 59.5721 3 3 0 -12 515.557 56.6687 4 3 0 12 628.617 59.3192 4 -3 0 12 462.87 53.4832 4 3 0 -13 2.23068 11.1726 3 3 0 13 5.56769 8.99263 4 -3 0 13 2.57008 7.19244 4 3 0 -13 2.99465 9.62054 4 -3 0 -14 112.168 25.6445 2 3 0 -14 95.5954 20.1851 3 -3 0 14 66.1999 12.9291 4 3 0 14 108.03 18.3616 4 3 0 -14 124.592 17.9136 4 -3 0 -15 -18.1996 14.3211 2 3 0 15 -1.91207 10.1742 4 3 0 -15 -2.23183 11.5307 3 3 0 -15 15.963 10.7438 4 -3 0 15 -4.42149 6.65656 4 3 0 -16 562.014 60.7048 3 -3 0 16 449.254 54.0449 4 -3 0 -16 652.917 61.4179 2 3 0 -16 494.839 56.9997 4 3 0 16 636.039 60.2527 4 3 0 -17 9.19465 11.3219 3 -3 0 17 -3.54429 6.94718 4 3 0 17 1.9699 10.1763 4 -3 0 -17 5.42822 11.6199 2 3 0 -17 4.62757 8.88232 4 3 0 -18 75.8066 21.4715 3 3 0 18 150.259 22.1947 4 -3 0 18 105.646 16.3656 4 -3 0 -18 164.331 21.5959 2 3 0 -18 137.624 19.6622 4 3 0 -19 -2.75965 9.37312 4 3 0 -19 -21.8433 17.3252 3 -3 0 19 -4.48443 7.44265 4 -3 0 -19 9.00864 9.06266 2 -3 0 20 258.955 29.7119 4 3 0 -20 193.607 34.2131 3 -3 0 -20 290.857 32.9712 2 3 0 -20 298.191 32.7836 4 3 0 -21 4.00319 8.48617 4 -3 0 21 6.45189 7.59787 4 3 0 -21 7.60946 12.2837 3 -3 0 -21 -7.32641 9.31823 2 3 0 -22 160.19 20.7175 4 3 0 -22 127.454 23.9674 3 -3 0 22 105.196 17.0343 4 -3 0 -22 141.421 19.8535 2 3 0 -23 -7.18246 11.1159 4 3 0 -23 -2.65301 12.3998 3 -3 0 23 0.95992 7.53136 4 -3 0 -23 -6.99148 9.41432 2 3 0 -24 57.4544 20.5056 3 -3 0 24 89.2082 15.4332 4 -3 0 -24 103.402 17.3795 2 3 0 -25 -8.42482 14.9397 3 3 0 25 -2.17174 11.7175 4 -3 0 -25 -2.78805 8.50243 2 -3 0 25 3.78274 8.15711 4 3 0 -26 1540.14 150.976 3 -3 0 -26 1661.58 144.729 2 3 0 26 1675.73 148.716 4 -3 0 26 1203.48 141.261 4 -3 0 -27 4.27105 9.40732 2 3 0 -27 -9.10923 16.8309 3 3 0 27 15.5862 12.5034 4 -3 0 27 -5.68658 8.12974 4 3 0 28 67.6064 16.9976 4 3 0 -28 34.3618 19.5153 3 -3 0 -28 59.8755 13.9917 2 -3 0 28 29.812 10.5181 4 3 0 -29 3.21633 18.2972 3 3 0 29 -4.56076 12.3118 4 -3 0 -29 1.48154 10.3295 2 -3 0 29 -11.9031 9.45077 4 3 0 -30 2826.65 254.65 3 3 0 30 2877.03 249.973 4 -3 0 -30 2879.02 245.576 2 -3 0 30 2048.15 242.089 4 3 0 -31 17.2756 19.4045 3 3 0 31 14.0037 15.2816 4 -3 0 -31 2.91764 10.0804 2 -3 0 31 -6.22087 10.7156 4 3 0 -32 2012.88 181.559 3 -3 0 -32 2008.25 171.309 2 3 0 32 2008.65 175.559 4 3 0 33 26.2839 48.7445 1 3 0 -33 18.3695 21.71 3 -3 0 33 2.15579 11.2272 4 3 0 33 40.6319 16.983 4 3 0 -34 1451.48 129.582 3 -3 0 34 1070.39 113.197 4 3 0 34 1430.67 121.48 4 3 0 -35 3.91029 21.4022 3 3 0 35 4.88807 13.2095 4 -3 0 35 13.6863 10.8819 4 3 0 35 -17.4984 36.7222 1 3 0 36 12.4794 15.8107 4 3 0 36 -11.3806 37.2927 1 3 0 -36 12.1066 22.4398 3 -3 0 36 26.8238 11.5301 4 3 0 37 -11.465 38.5743 1 3 0 -37 -4.16538 24.2744 3 3 0 37 17.6637 13.8034 4 -3 0 37 -5.86557 11.5571 4 3 0 -38 348.191 50.7758 3 -3 0 38 255.963 35.2603 4 3 0 39 -21.384 37.8591 1 3 0 -39 4.4379 25.5638 3 -3 0 39 9.42298 12.8212 4 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