#------------------------------------------------------------------------------ #$Date: 2024-10-04 01:13:05 +0300 (Fri, 04 Oct 2024) $ #$Revision: 295024 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572766.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_1572766 loop_ _publ_author_name 'Zhang, Chonghe' 'Gilliard, Robert J.' 'Cummins, Christopher' _publ_section_title ; Arene extrusion as an approach to reductive elimination at boron: Implication of carbene-ligated haloborylene as a transient reactive intermediate ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC05524A _journal_year 2024 _chemical_absolute_configuration unk _chemical_formula_moiety 'C22 H36 B Cl N' _chemical_formula_sum 'C22 H36 B Cl N' _chemical_formula_weight 360.78 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2023-07-12 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-09-26 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.192(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.2417(5) _cell_length_b 10.0889(6) _cell_length_c 11.8541(8) _cell_measurement_reflns_used 9808 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.985 _cell_measurement_theta_min 2.727 _cell_volume 1037.33(11) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_unetI/netI 0.0278 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 59900 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.141 _diffrn_reflns_theta_min 1.830 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0800 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.8845. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.155 _exptl_crystal_description block _exptl_crystal_F_000 394 _exptl_crystal_size_max 0.065 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.012 _refine_diff_density_max 1.495 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.075 _refine_ls_abs_structure_details ; Flack x determined using 2712 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.254(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 233 _refine_ls_number_reflns 6660 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0482 _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^)+(0.0928P)^2^+0.1825P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1274 _refine_ls_wR_factor_ref 0.1303 _reflns_Friedel_coverage 0.899 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.991 _reflns_number_gt 6089 _reflns_number_total 6660 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc05524a3.cif _cod_data_source_block 3 _cod_database_code 1572766 _shelx_shelxl_version_number 2016/6 _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 0.998 _shelx_estimated_absorpt_t_min 0.988 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C20(H20), C4(H4), C17(H17), B1(H1) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B) 2.c Aromatic/amide H refined with riding coordinates: C15(H15), C14(H14), C13(H13) 2.d Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C19(H19A,H19B, H19C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C) ; _shelx_res_file ; TITL mo_P8_23081_0m_a.res in P2(1) mo_p8_23081_0m_a.res created by SHELXL-2016/6 at 21:17:53 on 12-Jul-2023 CELL 0.71073 9.2417 10.0889 11.8541 90 110.192 90 ZERR 2 0.0005 0.0006 0.0008 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H B Cl N UNIT 44 72 2 2 2 L.S. 10 PLAN 7 0 0 SIZE 0.065 0.056 0.012 TEMP -173.15 CONF HTAB BOND $H fmap 2 acta MORE -1 REM REM REM WGHT 0.092800 0.182500 FVAR 0.96060 CL1 4 0.616760 0.195118 0.380290 11.00000 0.02852 0.01331 = 0.02371 0.00128 0.01143 -0.00279 N1 5 0.603759 0.581958 0.271872 11.00000 0.01064 0.01202 = 0.01178 -0.00045 0.00385 0.00054 C21 1 0.155246 0.643669 0.265820 11.00000 0.01847 0.02807 = 0.03044 -0.00496 0.01082 0.00392 AFIX 137 H21A 2 0.182163 0.735221 0.253688 11.00000 -1.50000 H21B 2 0.141240 0.636257 0.343843 11.00000 -1.50000 H21C 2 0.059300 0.618984 0.201731 11.00000 -1.50000 AFIX 0 C20 1 0.284635 0.551025 0.263015 11.00000 0.01298 0.02120 = 0.01892 -0.00086 0.00628 -0.00046 AFIX 13 H20 2 0.377721 0.571198 0.334781 11.00000 -1.20000 AFIX 0 C12 1 0.328294 0.568845 0.151515 11.00000 0.01150 0.01122 = 0.01622 -0.00024 0.00330 0.00049 C11 1 0.481208 0.576731 0.154475 11.00000 0.01142 0.01022 = 0.01180 -0.00031 0.00190 -0.00016 C4 1 0.659385 0.478164 0.335526 11.00000 0.00964 0.01493 = 0.01474 0.00118 0.00578 0.00023 AFIX 13 H4 2 0.571757 0.461248 0.364842 11.00000 -1.20000 AFIX 0 C3 1 0.779766 0.514168 0.455513 11.00000 0.01207 0.01231 = 0.01529 0.00211 0.00316 -0.00143 C7 1 0.714753 0.495073 0.558118 11.00000 0.01783 0.01733 = 0.01713 0.00002 0.00772 -0.00158 AFIX 23 H7A 2 0.623784 0.553219 0.543390 11.00000 -1.20000 H7B 2 0.679853 0.402194 0.557335 11.00000 -1.20000 AFIX 0 C8 1 0.832451 0.526401 0.682473 11.00000 0.02904 0.02173 = 0.01728 -0.00057 0.00670 -0.00364 AFIX 137 H8A 2 0.923260 0.469672 0.697502 11.00000 -1.50000 H8B 2 0.786007 0.509940 0.744026 11.00000 -1.50000 H8C 2 0.863340 0.619623 0.685403 11.00000 -1.50000 AFIX 0 C22 1 0.239080 0.405447 0.272713 11.00000 0.02237 0.02304 = 0.02787 0.00231 0.01253 -0.00217 AFIX 137 H22A 2 0.147700 0.383237 0.203327 11.00000 -1.50000 H22B 2 0.216065 0.393472 0.346814 11.00000 -1.50000 H22C 2 0.324542 0.347175 0.274158 11.00000 -1.50000 AFIX 0 C16 1 0.520142 0.577393 0.049307 11.00000 0.01370 0.00967 = 0.01378 0.00042 0.00410 0.00014 C15 1 0.397653 0.577493 -0.060735 11.00000 0.01944 0.01041 = 0.01266 0.00004 0.00221 -0.00149 AFIX 43 H15 2 0.419569 0.578950 -0.133348 11.00000 -1.20000 AFIX 0 C14 1 0.245329 0.575522 -0.066374 11.00000 0.01649 0.01504 = 0.01572 -0.00070 -0.00138 -0.00063 AFIX 43 H14 2 0.164328 0.579009 -0.142032 11.00000 -1.20000 AFIX 0 C13 1 0.211477 0.568449 0.038649 11.00000 0.01108 0.01718 = 0.02063 0.00001 0.00153 0.00015 AFIX 43 H13 2 0.106900 0.563231 0.033909 11.00000 -1.20000 AFIX 0 C17 1 0.683466 0.571084 0.047918 11.00000 0.01506 0.01410 = 0.01454 0.00178 0.00611 0.00019 AFIX 13 H17 2 0.756432 0.576246 0.132720 11.00000 -1.20000 AFIX 0 C19 1 0.711703 0.440155 -0.006647 11.00000 0.02435 0.01680 = 0.02466 -0.00084 0.01351 0.00157 AFIX 137 H19A 2 0.686243 0.365845 0.036378 11.00000 -1.50000 H19B 2 0.820353 0.434437 0.000437 11.00000 -1.50000 H19C 2 0.646575 0.436445 -0.091654 11.00000 -1.50000 AFIX 0 C18 1 0.717866 0.687375 -0.023138 11.00000 0.02124 0.01757 = 0.02297 0.00369 0.00925 -0.00147 AFIX 137 H18A 2 0.656122 0.677824 -0.108510 11.00000 -1.50000 H18B 2 0.827624 0.687177 -0.013219 11.00000 -1.50000 H18C 2 0.691742 0.771122 0.007100 11.00000 -1.50000 AFIX 0 C1 1 0.864254 0.342415 0.339524 11.00000 0.01666 0.01725 = 0.02067 -0.00035 0.00676 0.00339 AFIX 23 H1A 2 0.912166 0.253487 0.348235 11.00000 -1.20000 H1B 2 0.897989 0.394780 0.282427 11.00000 -1.20000 AFIX 0 C2 1 0.911163 0.413390 0.463580 11.00000 0.01272 0.01722 = 0.01921 0.00022 0.00444 0.00252 AFIX 23 H2A 2 1.010573 0.460243 0.480647 11.00000 -1.20000 H2B 2 0.922125 0.348232 0.528458 11.00000 -1.20000 AFIX 0 C5 1 0.813059 0.660755 0.436315 11.00000 0.01500 0.01283 = 0.01749 -0.00059 0.00404 -0.00118 AFIX 23 H5A 2 0.906705 0.668097 0.414180 11.00000 -1.20000 H5B 2 0.829446 0.712208 0.510820 11.00000 -1.20000 AFIX 0 C6 1 0.670778 0.713932 0.333441 11.00000 0.01294 0.01084 = 0.01430 -0.00114 0.00373 -0.00154 C9 1 0.553903 0.786190 0.375729 11.00000 0.01942 0.01322 = 0.02287 -0.00289 0.00715 0.00147 AFIX 137 H9A 2 0.598695 0.869595 0.414644 11.00000 -1.50000 H9B 2 0.526910 0.730412 0.433202 11.00000 -1.50000 H9C 2 0.460957 0.805022 0.306529 11.00000 -1.50000 AFIX 0 C10 1 0.717319 0.804637 0.248925 11.00000 0.02310 0.01312 = 0.02079 0.00048 0.00645 -0.00436 AFIX 137 H10A 2 0.625712 0.828362 0.180297 11.00000 -1.50000 H10B 2 0.791295 0.758610 0.220146 11.00000 -1.50000 H10C 2 0.764873 0.885252 0.291996 11.00000 -1.50000 AFIX 0 B1 3 0.676116 0.329936 0.291330 11.00000 0.01757 0.01160 = 0.01937 -0.00079 0.00607 0.00034 AFIX 13 H1 2 0.629374 0.318354 0.202270 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_P8_23081_0m_a.res in P2(1) REM R1 = 0.0482 for 6089 Fo > 4sig(Fo) and 0.0533 for all 6660 data REM 233 parameters refined using 1 restraints END WGHT 0.0928 0.1825 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y+1/2, -z+1 HTAB C9 Cl1_$1 REM Highest difference peak 1.495, deepest hole -0.520, 1-sigma level 0.075 Q1 1 0.6166 0.9500 0.3799 11.00000 0.05 1.49 Q2 1 0.6566 0.6564 0.3301 11.00000 0.05 0.56 Q3 1 0.8223 0.4754 0.4384 11.00000 0.05 0.55 Q4 1 0.6666 0.4093 0.3246 11.00000 0.05 0.53 Q5 1 0.7858 0.6063 0.4519 11.00000 0.05 0.52 Q6 1 0.7191 0.3317 0.2463 11.00000 0.05 0.49 Q7 1 0.6734 0.8101 0.2954 11.00000 0.05 0.48 ; _shelx_res_checksum 73844 _shelx_hkl_file ; 1 0 0 5512.74 227.55 1 0 0 5196.41 227.55 1 0 0 5435.89 227.55 1 0 0 5220.68 227.54 1 0 0 5209.08 227.53 1 0 0 5235.81 227.53 1 0 0 5956.94 227.57 1 0 0 5475.88 227.55 1 0 0 5182.62 227.54 -1 0 0 5273.13 227.54 -1 0 0 5237.41 227.53 -1 0 0 5956.09 227.57 -1 0 0 5289.69 227.54 -1 0 0 5450.95 227.54 -1 0 0 5417.45 227.55 -1 0 0 5081.76 227.55 2 0 0 8513.48 376.53 2 0 0 8308.60 376.49 2 0 0 8949.09 376.50 -2 0 0 8953.80 376.49 2 0 0 8415.46 376.53 -2 0 0 8366.59 376.51 -2 0 0 8955.45 376.51 -2 0 0 8555.87 376.52 -2 0 0 8939.77 376.57 -2 0 0 8594.14 376.50 -2 0 0 9281.75 376.52 2 0 0 8981.08 376.51 2 0 0 9414.32 376.52 2 0 0 9999.00 376.52 2 0 0 8902.11 376.49 2 0 0 9384.31 376.58 3 0 0 364.32 15.61 -3 0 0 367.42 15.77 3 0 0 352.46 15.63 3 0 0 355.76 15.58 3 0 0 366.78 15.56 3 0 0 365.59 15.55 3 0 0 372.93 15.71 3 0 0 361.91 15.61 3 0 0 387.56 15.63 3 0 0 339.42 15.74 -3 0 0 357.43 15.67 -3 0 0 365.91 15.60 -3 0 0 350.61 15.56 -3 0 0 377.29 15.57 -3 0 0 379.59 15.62 -3 0 0 378.54 15.61 -3 0 0 364.05 15.66 -4 0 0 255.52 10.92 -4 0 0 237.29 10.83 -4 0 0 261.05 10.83 -4 0 0 239.33 11.28 4 0 0 239.77 10.83 4 0 0 250.72 10.81 -4 0 0 243.63 11.04 -4 0 0 242.94 10.89 4 0 0 258.05 10.81 4 0 0 247.25 11.07 4 0 0 250.29 10.92 4 0 0 253.35 10.93 4 0 0 265.16 10.95 4 0 0 249.44 11.03 4 0 0 251.36 10.95 -4 0 0 253.06 11.04 -4 0 0 262.82 10.88 5 0 0 30.00 2.75 5 0 0 27.17 3.09 -5 0 0 28.43 2.70 -5 0 0 36.39 2.47 5 0 0 31.61 2.41 -5 0 0 34.19 2.78 -5 0 0 27.96 2.69 -5 0 0 27.43 2.74 5 0 0 26.15 3.13 5 0 0 28.41 2.35 5 0 0 29.34 3.25 -5 0 0 30.50 3.65 5 0 0 32.38 2.26 5 0 0 31.17 2.38 5 0 0 34.04 3.10 5 0 0 27.59 3.20 -5 0 0 24.87 3.35 -5 0 0 32.39 3.00 6 0 0 51.14 3.43 -6 0 0 49.60 3.56 6 0 0 42.72 4.46 6 0 0 41.04 4.73 6 0 0 58.92 3.46 6 0 0 50.33 4.47 -6 0 0 42.76 4.30 6 0 0 35.38 4.33 6 0 0 59.49 4.46 -6 0 0 56.23 3.81 -6 0 0 52.18 3.73 -6 0 0 39.88 4.94 6 0 0 49.83 4.33 -6 0 0 56.33 5.33 7 0 0 13.77 2.80 7 0 0 9.87 3.44 -7 0 0 6.33 2.90 -7 0 0 9.85 3.78 7 0 0 10.95 3.85 -7 0 0 11.98 3.09 -7 0 0 5.48 4.24 -7 0 0 6.69 2.72 7 0 0 14.45 2.44 7 0 0 12.33 2.14 7 0 0 13.16 2.98 7 0 0 18.20 5.22 8 0 0 17.88 4.35 8 0 0 9.74 3.51 8 0 0 12.56 4.13 8 0 0 13.32 2.80 8 0 0 13.00 3.15 -8 0 0 12.08 3.77 -8 0 0 8.56 3.69 -8 0 0 10.54 6.49 -8 0 0 12.82 3.67 8 0 0 13.14 5.09 -8 0 0 15.40 4.86 8 0 0 12.37 3.77 8 0 0 6.78 3.09 9 0 0 90.68 6.63 -9 0 0 80.66 9.60 9 0 0 85.78 8.57 9 0 0 94.47 7.64 9 0 0 80.19 8.52 -9 0 0 91.03 7.52 9 0 0 90.87 6.15 9 0 0 89.66 9.30 9 0 0 89.56 6.65 -9 0 0 79.86 7.62 -10 0 0 84.58 9.64 10 0 0 104.31 7.51 10 0 0 89.98 9.84 10 0 0 111.39 8.11 10 0 0 93.58 10.52 10 0 0 110.30 10.85 10 0 0 120.35 9.41 10 0 0 103.34 7.94 -10 0 0 101.18 11.73 10 0 0 105.48 10.89 11 0 0 19.06 6.30 11 0 0 20.80 8.08 11 0 0 13.94 5.38 11 0 0 12.04 5.96 11 0 0 16.41 8.81 11 0 0 25.30 7.22 12 0 0 2.44 7.81 12 0 0 2.47 11.69 12 0 0 -8.43 7.67 12 0 0 0.77 7.55 12 0 0 10.76 10.22 12 0 0 5.33 10.77 0 -1 0 0.41 0.39 0 -1 0 0.26 0.33 0 -1 0 0.17 0.33 0 -1 0 0.72 0.28 0 -1 0 -0.18 0.27 0 -1 0 -0.05 0.22 0 -1 0 -0.20 0.29 0 -1 0 0.45 0.23 0 -1 0 0.10 0.22 0 -1 0 -0.25 0.31 0 -1 0 0.88 0.30 0 -1 0 -0.06 0.31 0 -1 0 0.18 0.30 0 1 0 -0.35 0.35 0 1 0 -0.19 0.30 0 1 0 0.21 0.22 0 1 0 0.06 0.35 0 1 0 -0.17 0.31 0 1 0 0.17 0.29 0 1 0 -0.44 0.23 0 1 0 0.23 0.30 0 1 0 0.58 0.26 0 1 0 0.04 0.21 0 1 0 0.34 0.31 0 1 0 0.41 0.23 0 1 0 0.12 0.37 -1 -1 0 570.90 22.45 1 -1 0 527.92 22.46 1 -1 0 501.04 22.44 -1 -1 0 519.13 22.47 -1 -1 0 536.96 22.44 -1 -1 0 546.52 22.50 -1 -1 0 510.77 22.43 -1 -1 0 519.19 22.42 -1 -1 0 528.49 22.45 1 -1 0 529.61 22.44 1 -1 0 513.31 22.41 -1 -1 0 505.70 22.44 -1 -1 0 513.04 22.44 1 -1 0 535.52 22.44 1 -1 0 511.63 22.43 1 -1 0 517.25 22.43 1 -1 0 531.04 22.44 1 -1 0 515.51 22.42 -1 -1 0 511.09 22.45 1 -1 0 509.11 22.43 -1 1 0 520.60 22.43 -1 1 0 541.71 22.41 -1 1 0 530.74 22.44 -1 1 0 514.11 22.44 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83.29 0 -8 0 1880.76 83.34 0 -8 0 2090.05 83.41 0 -8 0 1929.09 83.40 0 8 0 1913.31 83.53 0 8 0 1965.01 83.34 0 8 0 1957.54 83.52 0 8 0 1852.23 83.22 0 8 0 1926.57 83.46 0 8 0 1944.14 83.69 0 8 0 2003.91 83.41 -1 -8 0 1044.57 43.33 -1 -8 0 1013.63 43.44 1 -8 0 1045.55 43.35 1 -8 0 1048.25 43.49 -1 -8 0 983.05 43.30 1 -8 0 1002.07 43.38 1 -8 0 976.89 43.77 1 -8 0 1023.71 43.32 -1 -8 0 987.57 43.79 -1 -8 0 1017.70 43.54 -1 -8 0 1013.17 43.30 1 -8 0 1011.60 43.46 -1 -8 0 1029.86 43.60 -1 -8 0 1023.65 43.50 1 8 0 1002.84 43.22 1 8 0 1004.76 43.54 1 8 0 1063.15 43.52 -1 8 0 1025.27 43.59 -1 8 0 1026.70 43.52 -1 8 0 1037.33 43.59 1 8 0 943.90 43.29 1 8 0 1021.70 43.39 -1 8 0 1016.01 43.77 -1 8 0 1035.44 43.44 -1 8 0 1026.18 43.38 1 8 0 1000.61 43.74 -1 8 0 997.97 43.26 1 8 0 1012.10 43.65 -2 -8 0 61.62 5.89 -2 -8 0 43.51 4.99 -2 -8 0 47.25 4.54 2 -8 0 50.87 4.34 2 -8 0 56.14 3.80 2 -8 0 65.85 5.45 2 -8 0 56.77 3.84 -2 -8 0 58.56 4.13 2 -8 0 54.28 4.75 2 -8 0 45.25 4.51 -2 -8 0 51.69 5.98 -2 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-3 -15 29.23 8.39 2 3 -15 10.26 6.72 2 3 -15 7.42 10.55 2 3 -15 20.60 9.10 2 3 -15 14.47 7.05 -1 -3 15 31.75 9.39 1 -3 -15 37.32 9.48 1 -3 -15 49.79 9.53 1 -3 -15 36.97 6.62 -1 -3 15 43.43 9.66 1 -3 -15 32.67 6.97 -1 -3 15 31.57 12.96 1 3 -15 34.21 11.27 -1 3 15 -8.46 13.78 1 3 -15 24.88 7.51 -1 3 15 37.31 9.04 1 3 -15 42.81 7.63 1 3 -15 36.53 9.59 0 -3 -15 11.71 10.11 0 -3 -15 26.21 7.73 0 -3 15 23.29 10.14 0 -3 15 11.79 18.46 0 -3 15 25.25 10.12 0 -3 -15 29.28 7.66 0 -3 15 27.64 13.92 0 3 -15 22.39 8.21 0 3 -15 25.28 12.01 0 3 15 32.14 9.92 0 3 -15 15.83 9.69 0 3 -15 19.92 10.11 0 3 15 2.65 14.45 1 -3 15 23.29 11.79 1 -3 15 12.69 15.20 1 -3 15 20.13 11.05 -1 -3 -15 17.98 11.57 1 -3 15 23.72 10.81 -1 -3 -15 20.09 7.90 -1 -3 -15 7.30 8.22 -1 3 -15 15.64 11.83 1 3 15 20.16 11.18 1 3 15 2.47 15.99 1 3 15 11.65 11.23 -1 3 -15 8.67 9.12 9 -4 -15 69.82 9.32 9 -4 -15 71.87 10.54 -9 -4 15 70.68 11.82 9 -4 -15 97.61 10.95 9 4 -15 49.65 19.80 9 4 -15 84.82 11.24 9 4 -15 73.47 10.40 -8 -4 15 9.17 10.27 8 -4 -15 10.36 8.69 8 -4 -15 20.59 9.60 8 -4 -15 9.59 7.92 8 4 -15 8.39 9.40 8 4 -15 9.02 10.41 8 4 -15 4.75 13.07 -7 -4 15 236.53 17.27 7 -4 -15 229.01 14.47 7 -4 -15 260.64 16.88 7 4 -15 235.60 15.38 7 4 -15 261.83 17.26 7 4 -15 264.98 23.91 7 4 -15 228.41 15.79 -6 -4 15 300.28 18.10 6 -4 -15 243.61 15.20 6 -4 -15 297.82 17.34 6 4 -15 256.75 16.17 6 4 -15 248.82 27.21 6 4 -15 280.93 15.75 6 4 -15 287.81 17.80 5 -4 -15 143.79 13.27 5 -4 -15 134.50 11.11 5 -4 -15 181.86 13.70 -5 -4 15 161.74 15.32 5 4 -15 163.56 15.98 5 4 -15 152.50 10.99 5 4 -15 168.56 14.24 5 4 -15 138.41 12.72 4 -4 -15 3.86 8.15 -4 -4 15 1.71 8.83 4 -4 -15 11.59 8.21 4 -4 -15 -1.44 6.69 4 4 -15 -3.68 10.09 4 4 -15 -4.77 7.74 4 4 -15 -6.52 8.78 4 4 -15 7.01 6.47 3 -4 -15 24.98 6.83 3 -4 -15 31.38 12.41 -3 -4 15 29.10 9.21 3 4 -15 14.63 7.73 3 4 -15 21.26 8.92 3 4 -15 25.00 10.99 3 4 -15 27.17 6.94 -2 -4 15 -10.22 9.74 -2 -4 15 6.82 8.90 2 -4 -15 7.83 5.82 2 -4 -15 3.59 6.59 2 -4 -15 1.10 8.88 2 4 -15 -0.84 11.17 2 4 -15 6.53 7.72 2 4 -15 5.19 7.15 2 4 -15 10.72 9.22 1 -4 -15 24.67 7.28 1 -4 -15 26.95 6.82 -1 -4 15 20.17 9.94 -1 -4 15 22.17 9.89 1 -4 -15 14.53 9.77 1 4 -15 -0.28 11.69 1 4 -15 23.00 8.32 1 4 -15 10.71 9.63 1 4 -15 23.00 7.75 0 -4 15 -4.39 10.12 0 -4 15 -7.57 10.77 0 -4 -15 10.41 9.58 0 -4 15 -8.06 14.55 0 -4 -15 11.77 10.79 0 -4 -15 1.50 8.90 0 -4 15 18.45 10.40 0 4 -15 0.19 9.02 0 4 -15 9.52 10.25 0 4 -15 -6.57 12.37 0 4 15 0.13 10.13 0 4 -15 -2.07 8.54 1 -4 15 14.20 15.99 -1 -4 -15 7.00 8.91 1 -4 15 -0.40 12.29 1 -4 15 4.98 11.18 -1 -4 -15 17.06 8.43 -1 4 -15 4.27 13.22 1 4 15 4.02 11.45 -1 4 -15 -6.97 9.57 -1 4 -15 -1.72 10.53 -8 -5 15 -1.89 10.84 8 -5 -15 -1.97 9.25 8 -5 -15 -5.39 8.50 8 -5 -15 -5.24 10.05 8 5 -15 5.36 10.31 8 5 -15 5.74 11.64 8 5 -15 -5.38 13.33 8 5 -15 -3.30 9.29 -7 -5 15 28.67 10.43 7 -5 -15 14.12 7.93 7 -5 -15 18.20 9.85 7 5 -15 10.26 9.80 7 5 -15 18.92 12.69 7 5 -15 31.70 15.18 -6 -5 15 26.28 10.21 6 -5 -15 20.22 7.56 6 -5 -15 24.13 9.48 6 5 -15 36.65 11.73 6 5 -15 31.56 9.96 6 5 -15 24.69 9.13 6 5 -15 47.53 9.50 6 5 -15 42.59 8.60 6 5 -15 35.92 7.02 5 -5 -15 16.76 9.12 -5 -5 15 13.01 10.05 5 -5 -15 10.27 7.11 5 -5 -15 16.89 8.87 5 5 -15 11.20 7.70 5 5 -15 15.12 11.56 5 5 -15 15.18 9.73 5 5 -15 14.68 6.61 5 5 -15 12.47 8.72 4 -5 -15 92.37 10.25 4 -5 -15 97.17 10.33 -4 -5 15 102.57 11.06 4 5 -15 113.94 12.48 4 5 -15 117.02 12.61 4 5 -15 124.27 14.27 4 5 -15 132.42 11.09 3 -5 -15 2.84 9.59 -3 -5 15 21.32 9.76 3 -5 -15 10.09 6.90 3 5 -15 7.92 11.28 3 5 -15 13.89 7.43 3 5 -15 17.38 9.44 3 5 -15 15.00 8.51 2 -5 -15 31.88 7.98 2 -5 -15 35.37 10.20 2 -5 -15 37.14 7.78 -2 -5 15 30.70 10.02 -2 -5 15 48.99 10.51 2 5 -15 38.51 10.06 2 5 -15 32.47 8.19 2 5 -15 38.06 8.96 2 5 -15 38.23 11.96 -1 -5 15 8.86 10.51 1 -5 -15 2.84 7.89 -1 -5 15 3.27 10.34 1 -5 -15 -4.55 9.94 1 -5 -15 7.97 8.04 1 5 -15 -2.05 12.67 1 5 -15 -2.80 11.25 1 5 -15 0.07 10.45 1 5 -15 -7.31 14.14 0 -5 -15 28.54 7.97 0 -5 15 45.80 11.32 0 -5 15 38.98 15.36 0 -5 -15 40.95 8.28 0 -5 15 41.35 10.63 0 -5 15 45.19 12.05 0 -5 -15 24.17 11.16 0 5 -15 17.61 9.65 0 5 -15 50.13 13.79 0 5 -15 43.22 11.13 0 5 15 3.53 12.06 7 -6 -15 70.11 11.19 7 -6 -15 83.61 11.33 -7 -6 15 93.27 12.19 7 6 -15 105.59 10.96 7 6 -15 89.88 14.32 7 6 -15 74.48 12.09 7 6 -15 78.80 11.32 7 6 -15 93.18 10.15 -6 -6 15 276.85 18.99 6 -6 -15 221.86 15.42 6 -6 -15 264.83 17.81 6 6 -15 257.13 16.14 6 6 -15 200.04 18.51 6 6 -15 256.83 18.21 6 6 -15 255.93 14.82 6 6 -15 270.44 21.39 6 6 -15 232.88 17.47 -5 -6 15 10.44 10.57 5 -6 -15 8.44 8.29 5 -6 -15 10.01 8.97 5 6 -15 8.98 12.13 5 6 -15 4.53 9.93 5 6 -15 15.41 9.25 5 6 -15 20.83 9.30 5 6 -15 11.12 10.67 5 6 -15 25.49 12.04 -4 -6 15 28.39 10.56 4 -6 -15 17.11 13.20 4 6 -15 24.38 12.65 4 6 -15 9.44 9.83 4 6 -15 17.10 15.86 4 6 -15 22.74 14.80 3 -6 -15 21.71 8.97 3 -6 -15 35.33 9.98 -3 -6 15 34.20 10.52 3 6 -15 42.55 12.86 3 6 -15 25.37 9.93 2 -6 -15 49.98 10.59 -2 -6 15 48.81 11.00 2 -6 -15 49.68 8.07 2 -6 -15 49.48 6.96 -2 -6 15 52.62 11.32 2 6 -15 58.47 16.62 2 6 -15 44.46 10.14 2 6 -15 53.14 11.32 2 6 -15 48.52 13.15 -1 -6 15 6.26 10.36 -1 -6 15 3.28 8.52 1 -6 -15 8.18 11.42 -1 -6 15 7.11 11.49 1 -6 -15 -0.25 7.17 1 -6 -15 0.17 7.78 1 6 -15 -2.39 11.68 1 6 -15 -5.31 9.99 1 6 -15 2.32 9.33 1 6 -15 -0.82 13.25 5 -7 -15 57.03 9.61 -5 -7 15 69.83 12.64 5 7 -15 73.32 14.53 5 7 -15 61.17 11.76 5 7 -15 68.80 12.21 5 7 -15 69.19 9.85 5 7 -15 55.51 11.50 5 7 -15 55.69 8.87 -4 -7 15 37.02 13.14 4 -7 -15 38.69 10.78 4 -7 -15 40.00 8.74 4 7 -15 15.31 13.66 4 7 -15 45.10 19.32 4 7 -15 32.58 9.31 4 7 -15 32.75 11.47 4 7 -15 39.35 8.67 3 -7 -15 9.11 10.70 3 -7 -15 4.02 7.88 3 7 -15 9.02 8.73 3 7 -15 9.16 10.79 3 7 -15 10.64 9.02 3 7 -15 19.33 11.63 8 0 -16 55.52 10.88 8 0 -16 37.46 8.95 8 0 -16 30.20 9.05 7 0 -16 229.18 16.27 7 0 -16 197.89 14.12 7 0 -16 198.58 14.47 6 0 -16 340.88 18.70 6 0 -16 277.33 16.72 6 0 -16 294.36 19.27 5 0 -16 115.49 13.10 -5 0 16 100.65 10.35 5 0 -16 86.37 11.12 5 0 -16 87.85 10.72 4 0 -16 10.66 7.66 4 0 -16 17.20 9.02 -4 0 16 12.80 8.93 3 0 -16 31.29 10.59 3 0 -16 19.83 6.29 3 0 -16 24.60 9.04 -3 0 16 23.91 9.89 3 0 -16 25.62 7.47 2 0 -16 -3.38 7.32 -2 0 16 3.58 12.32 2 0 -16 0.86 11.35 2 0 -16 5.32 9.92 2 0 -16 -1.14 7.29 -1 0 16 17.31 10.90 1 0 -16 12.00 17.68 1 0 -16 -4.40 12.17 1 0 -16 15.75 9.06 1 0 -16 8.37 11.41 0 0 -16 0.85 13.41 0 0 16 17.48 11.68 0 0 -16 16.81 11.15 0 0 -16 -1.86 9.16 0 0 -16 12.89 8.61 8 -1 -16 62.09 9.40 8 -1 -16 46.34 8.92 8 -1 -16 64.84 10.76 8 1 -16 64.17 9.59 8 1 -16 49.92 11.09 8 1 -16 42.24 9.44 7 -1 -16 145.76 13.32 7 -1 -16 143.80 12.88 7 -1 -16 198.49 15.39 7 1 -16 144.73 13.25 7 1 -16 176.77 15.77 7 1 -16 149.97 13.21 7 1 -16 158.53 17.14 6 -1 -16 69.15 10.62 6 -1 -16 81.49 10.03 6 -1 -16 61.00 8.38 -6 -1 16 66.56 9.62 6 1 -16 78.97 10.14 6 1 -16 55.79 11.20 6 1 -16 58.63 8.93 -5 -1 16 5.32 9.82 5 -1 -16 16.40 9.08 5 -1 -16 17.23 7.55 5 -1 -16 17.86 10.13 5 1 -16 10.82 9.28 5 1 -16 12.00 8.01 5 1 -16 8.49 10.63 4 -1 -16 14.79 9.15 4 -1 -16 21.84 14.71 -4 -1 16 13.77 9.19 4 -1 -16 4.62 7.02 4 1 -16 14.28 9.13 4 1 -16 21.57 6.23 4 1 -16 22.79 8.00 4 1 -16 17.98 10.76 -3 -1 16 26.45 11.00 3 -1 -16 30.48 10.23 3 -1 -16 18.54 7.43 3 -1 -16 40.01 9.38 3 1 -16 26.32 6.78 -3 1 16 22.07 9.76 3 1 -16 23.02 11.15 3 1 -16 25.36 9.17 3 1 -16 32.38 8.07 2 -1 -16 44.05 11.02 2 -1 -16 51.30 9.11 2 -1 -16 47.23 10.28 2 -1 -16 42.73 8.01 -2 -1 16 57.79 10.48 2 1 -16 47.33 8.38 2 1 -16 60.75 8.89 2 1 -16 46.28 11.73 2 1 -16 67.30 10.38 -2 1 16 58.74 10.58 1 -1 -16 -0.98 8.22 1 -1 -16 -7.35 7.71 -1 -1 16 1.36 10.76 1 -1 -16 2.54 13.19 1 -1 -16 6.41 11.27 1 1 -16 -2.42 8.06 -1 1 16 -3.36 10.93 1 1 -16 7.99 16.42 1 1 -16 1.18 12.11 1 1 -16 3.61 9.56 0 -1 -16 2.65 11.22 0 -1 16 -6.66 17.29 0 -1 -16 2.62 8.34 0 -1 -16 2.08 12.44 0 -1 16 2.02 11.80 0 -1 -16 3.13 8.88 0 1 -16 1.04 11.22 0 1 -16 5.26 8.67 0 1 16 12.33 11.74 0 1 -16 2.42 9.08 -8 -2 16 23.70 10.62 8 -2 -16 13.65 9.09 8 -2 -16 19.76 10.65 8 -2 -16 14.56 8.50 8 2 -16 17.07 12.58 8 2 -16 9.06 16.10 8 2 -16 14.36 9.44 7 -2 -16 41.32 8.64 7 -2 -16 70.27 10.31 -7 -2 16 77.81 10.35 7 2 -16 50.84 12.15 7 2 -16 55.30 10.92 7 2 -16 46.31 9.16 7 2 -16 65.10 9.50 6 -2 -16 90.84 10.82 -6 -2 16 77.25 10.77 6 -2 -16 89.86 10.51 6 2 -16 82.12 12.08 6 2 -16 72.75 10.62 6 2 -16 78.09 9.37 -5 -2 16 59.91 10.55 5 -2 -16 45.71 7.91 5 -2 -16 41.81 10.13 5 -2 -16 62.36 9.70 5 2 -16 53.95 11.65 5 2 -16 61.54 10.04 5 2 -16 42.07 8.60 4 -2 -16 25.98 12.60 4 -2 -16 54.54 9.59 4 -2 -16 37.20 7.58 -4 -2 16 35.51 17.26 4 2 -16 70.68 10.04 4 2 -16 59.91 7.12 4 2 -16 41.13 8.38 4 2 -16 42.76 11.60 3 -2 -16 6.11 9.37 -3 -2 16 10.30 10.12 3 -2 -16 -5.02 6.98 3 -2 -16 -11.61 10.07 3 -2 -16 0.65 6.40 3 2 -16 -5.23 8.02 3 2 -16 3.70 11.34 3 2 -16 0.52 9.77 3 2 -16 1.63 6.97 2 -2 -16 29.27 10.80 -2 -2 16 47.47 10.73 2 2 -16 39.55 17.95 2 2 -16 47.41 12.17 -2 2 16 59.05 10.56 2 2 -16 29.46 9.86 1 -2 -16 21.29 7.59 1 -2 -16 17.32 11.45 1 -2 -16 25.30 7.58 -1 -2 16 30.39 11.44 1 -2 -16 27.67 10.60 -1 -2 16 -0.50 18.32 1 2 -16 15.11 8.31 1 2 -16 29.39 12.87 -1 2 16 31.29 11.24 1 2 -16 37.07 12.43 1 2 -16 37.87 8.60 0 -2 -16 34.95 12.04 0 2 -16 14.51 9.02 0 2 -16 23.21 11.34 8 -3 -16 53.46 10.10 8 -3 -16 67.54 11.04 8 -3 -16 42.48 9.49 -8 -3 16 51.78 11.47 8 3 -16 69.71 11.96 8 3 -16 68.03 9.93 8 3 -16 63.11 17.58 8 3 -16 64.01 10.61 7 -3 -16 103.32 12.03 7 -3 -16 145.29 15.46 -7 -3 16 106.17 11.83 7 3 -16 133.37 12.92 7 3 -16 104.16 16.04 7 3 -16 98.55 11.16 6 -3 -16 31.94 9.84 6 -3 -16 11.48 8.01 -6 -3 16 22.70 10.53 6 3 -16 2.88 13.19 6 3 -16 39.04 18.25 6 3 -16 28.28 11.75 6 3 -16 32.22 9.08 5 -3 -16 4.20 10.03 5 -3 -16 -1.66 7.83 5 -3 -16 -4.42 9.46 -5 -3 16 -4.57 10.82 5 3 -16 8.67 8.00 5 3 -16 7.80 8.67 5 3 -16 -0.64 11.99 5 3 -16 14.62 11.56 4 -3 -16 6.72 9.80 -4 -3 16 4.61 9.98 4 -3 -16 2.48 7.48 4 3 -16 9.49 12.30 4 3 -16 2.66 8.47 4 3 -16 -3.79 11.83 4 3 -16 3.78 10.27 3 -3 -16 70.81 17.09 -3 -3 16 81.49 11.14 3 -3 -16 66.01 10.98 3 -3 -16 69.13 12.80 3 3 -16 55.31 12.26 3 3 -16 49.32 9.13 2 -3 -16 33.37 8.32 2 -3 -16 23.87 7.48 2 -3 -16 37.08 10.88 2 -3 -16 30.35 11.10 -2 -3 16 29.15 11.56 2 3 -16 30.05 13.14 2 3 -16 46.79 12.78 2 3 -16 30.39 9.29 2 3 -16 29.37 9.78 -1 -3 16 11.91 11.48 1 -3 -16 7.11 10.52 1 -3 -16 23.73 11.85 -1 -3 16 -10.01 20.08 1 -3 -16 10.17 7.60 1 -3 -16 5.73 7.79 1 3 -16 13.34 8.83 -1 3 16 7.55 11.67 1 3 -16 1.35 11.35 1 3 -16 6.21 13.71 1 3 -16 5.08 8.85 -7 -4 16 82.15 12.07 7 -4 -16 82.75 11.58 7 -4 -16 78.82 9.83 7 4 -16 62.13 11.09 7 4 -16 91.66 11.93 7 4 -16 78.23 13.73 7 4 -16 77.06 10.15 -6 -4 16 41.81 11.06 6 -4 -16 44.69 9.04 6 -4 -16 52.24 11.18 6 4 -16 55.08 9.16 6 4 -16 44.39 13.12 6 4 -16 39.91 7.32 6 4 -16 50.24 11.26 6 4 -16 43.23 10.09 5 -4 -16 106.89 14.34 5 -4 -16 93.66 10.80 -5 -4 16 85.83 12.21 5 -4 -16 84.85 11.22 5 4 -16 94.62 11.72 5 4 -16 72.14 8.59 5 4 -16 75.72 13.10 5 4 -16 79.38 10.34 -4 -4 16 105.28 12.19 4 -4 -16 102.17 12.28 4 4 -16 139.25 11.97 4 4 -16 114.68 12.83 4 4 -16 115.00 13.53 4 4 -16 117.09 12.54 3 -4 -16 13.57 11.10 3 -4 -16 7.83 7.61 -3 -4 16 20.22 11.07 3 -4 -16 2.88 10.24 3 4 -16 13.00 12.79 3 4 -16 5.27 8.00 3 4 -16 7.11 10.84 3 4 -16 18.24 15.84 2 -4 -16 85.07 11.38 2 -4 -16 49.07 8.23 2 -4 -16 49.06 7.49 -2 -4 16 78.87 12.16 2 -4 -16 60.51 11.74 2 4 -16 52.73 8.98 2 4 -16 35.92 11.30 2 4 -16 46.55 13.94 2 4 -16 39.37 9.58 6 -5 -16 28.43 13.73 6 5 -16 31.70 11.54 6 5 -16 9.27 10.94 6 5 -16 22.97 10.95 5 -5 -16 -1.09 10.89 -5 -5 16 -0.46 11.74 5 -5 -16 1.54 8.30 5 -5 -16 -2.16 11.10 5 5 -16 3.03 11.34 5 5 -16 -7.02 9.01 5 5 -16 -4.36 7.49 5 5 -16 1.34 11.03 5 5 -16 -3.23 13.54 4 -5 -16 10.25 8.38 4 -5 -16 14.64 10.73 4 -5 -16 13.32 10.66 -4 -5 16 3.17 11.28 4 5 -16 11.63 12.07 4 5 -16 12.38 11.23 4 5 -16 13.25 13.48 4 5 -16 15.62 8.17 -3 -5 16 13.84 11.89 3 -5 -16 11.90 6.55 3 -5 -16 25.85 11.64 3 -5 -16 19.59 8.34 3 5 -16 20.25 11.35 3 5 -16 25.53 13.59 3 5 -16 27.88 8.97 3 5 -16 30.02 10.15 6 0 -17 22.66 11.53 6 0 -17 18.36 11.30 5 0 -17 93.81 13.74 5 0 -17 132.71 15.54 -4 0 17 53.92 11.76 4 0 -17 52.45 13.10 4 0 -17 52.03 9.26 4 0 -17 72.12 11.27 3 0 -17 -5.52 12.68 3 0 -17 0.43 10.98 3 0 -17 2.43 8.55 3 0 -17 2.67 7.91 -6 -1 17 -3.37 14.00 6 -1 -17 16.17 16.06 6 -1 -17 25.93 11.10 6 -1 -17 -1.34 12.62 6 1 -17 28.12 11.43 6 1 -17 16.63 12.19 6 1 -17 5.09 13.16 5 -1 -17 3.23 10.52 5 -1 -17 27.33 12.40 -5 -1 17 12.19 11.88 5 -1 -17 27.83 10.82 5 1 -17 21.32 16.02 5 1 -17 12.06 13.04 5 1 -17 15.87 10.90 4 -1 -17 9.17 10.95 4 -1 -17 14.94 12.79 4 -1 -17 3.72 8.63 -4 -1 17 4.40 12.43 4 1 -17 -0.67 9.22 4 1 -17 13.10 13.22 4 1 -17 3.88 7.43 4 1 -17 6.47 10.94 3 -1 -17 -2.77 11.36 -3 -1 17 4.13 12.39 3 -1 -17 3.12 8.87 3 -1 -17 -0.83 12.84 3 1 -17 8.52 13.32 3 1 -17 1.70 10.89 -3 1 17 12.59 13.84 3 1 -17 5.94 9.12 5 -2 -17 9.44 12.13 5 -2 -17 24.38 9.09 -5 -2 17 17.83 12.34 5 -2 -17 15.33 11.20 5 2 -17 7.91 11.27 5 2 -17 21.91 13.71 5 2 -17 33.28 11.71 4 -2 -17 28.96 11.03 4 -2 -17 34.69 12.28 -4 -2 17 46.78 12.04 4 2 -17 44.89 13.74 4 2 -17 23.58 9.63 4 2 -17 43.52 11.60 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6600 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71081 9.246 10.093 11.859 89.993 110.247 90.004 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 47507 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 Cl1 Cl 0.61676(7) 0.19512(5) 0.38029(5) 0.02122(14) Uani 1 1 d . . . . . N1 N 0.60376(19) 0.58196(17) 0.27187(16) 0.0115(3) Uani 1 1 d . . . . . C21 C 0.1552(3) 0.6437(3) 0.2658(2) 0.0250(5) Uani 1 1 d . . . . . H21A H 0.182163 0.735221 0.253688 0.038 Uiso 1 1 calc R U . . . H21B H 0.141240 0.636257 0.343843 0.038 Uiso 1 1 calc R U . . . H21C H 0.059300 0.618984 0.201731 0.038 Uiso 1 1 calc R U . . . C20 C 0.2846(2) 0.5510(2) 0.2630(2) 0.0175(4) Uani 1 1 d . . . . . H20 H 0.377721 0.571198 0.334781 0.021 Uiso 1 1 calc R U . . . C12 C 0.3283(2) 0.5688(2) 0.15152(19) 0.0134(4) Uani 1 1 d . . . . . C11 C 0.4812(2) 0.57673(19) 0.15448(18) 0.0117(3) Uani 1 1 d . . . . . C4 C 0.6594(2) 0.4782(2) 0.33553(19) 0.0127(4) Uani 1 1 d . . . . . H4 H 0.571757 0.461248 0.364842 0.015 Uiso 1 1 calc R U . . . C3 C 0.7798(2) 0.5142(2) 0.45551(19) 0.0136(4) Uani 1 1 d . . . . . C7 C 0.7148(3) 0.4951(2) 0.5581(2) 0.0170(4) Uani 1 1 d . . . . . H7A H 0.623784 0.553219 0.543390 0.020 Uiso 1 1 calc R U . . . H7B H 0.679853 0.402194 0.557335 0.020 Uiso 1 1 calc R U . . . C8 C 0.8325(3) 0.5264(3) 0.6825(2) 0.0230(5) Uani 1 1 d . . . . . H8A H 0.923260 0.469672 0.697502 0.035 Uiso 1 1 calc R U . . . H8B H 0.786007 0.509940 0.744026 0.035 Uiso 1 1 calc R U . . . H8C H 0.863340 0.619623 0.685403 0.035 Uiso 1 1 calc R U . . . C22 C 0.2391(3) 0.4054(3) 0.2727(2) 0.0234(5) Uani 1 1 d . . . . . H22A H 0.147700 0.383237 0.203327 0.035 Uiso 1 1 calc R U . . . H22B H 0.216065 0.393472 0.346814 0.035 Uiso 1 1 calc R U . . . H22C H 0.324542 0.347175 0.274158 0.035 Uiso 1 1 calc R U . . . C16 C 0.5201(2) 0.5774(2) 0.04931(18) 0.0126(4) Uani 1 1 d . . . . . C15 C 0.3977(3) 0.5775(2) -0.06074(19) 0.0150(4) Uani 1 1 d . . . . . H15 H 0.419569 0.578950 -0.133348 0.018 Uiso 1 1 calc R U . . . C14 C 0.2453(3) 0.5755(2) -0.0664(2) 0.0176(4) Uani 1 1 d . . . . . H14 H 0.164328 0.579009 -0.142032 0.021 Uiso 1 1 calc R U . . . C13 C 0.2115(2) 0.5684(2) 0.0386(2) 0.0173(4) Uani 1 1 d . . . . . H13 H 0.106900 0.563231 0.033909 0.021 Uiso 1 1 calc R U . . . C17 C 0.6835(2) 0.5711(2) 0.04792(19) 0.0143(4) Uani 1 1 d . . . . . H17 H 0.756432 0.576246 0.132720 0.017 Uiso 1 1 calc R U . . . C19 C 0.7117(3) 0.4402(2) -0.0066(2) 0.0206(4) Uani 1 1 d . . . . . H19A H 0.686243 0.365845 0.036378 0.031 Uiso 1 1 calc R U . . . H19B H 0.820353 0.434437 0.000437 0.031 Uiso 1 1 calc R U . . . H19C H 0.646575 0.436445 -0.091654 0.031 Uiso 1 1 calc R U . . . C18 C 0.7179(3) 0.6874(3) -0.0231(2) 0.0202(4) Uani 1 1 d . . . . . H18A H 0.656122 0.677824 -0.108510 0.030 Uiso 1 1 calc R U . . . H18B H 0.827624 0.687177 -0.013219 0.030 Uiso 1 1 calc R U . . . H18C H 0.691742 0.771122 0.007100 0.030 Uiso 1 1 calc R U . . . C1 C 0.8643(3) 0.3424(2) 0.3395(2) 0.0181(4) Uani 1 1 d . . . . . H1A H 0.912166 0.253487 0.348235 0.022 Uiso 1 1 calc R U . . . H1B H 0.897989 0.394780 0.282427 0.022 Uiso 1 1 calc R U . . . C2 C 0.9112(2) 0.4134(2) 0.4636(2) 0.0167(4) Uani 1 1 d . . . . . H2A H 1.010573 0.460243 0.480647 0.020 Uiso 1 1 calc R U . . . H2B H 0.922125 0.348232 0.528458 0.020 Uiso 1 1 calc R U . . . C5 C 0.8131(2) 0.6608(2) 0.4363(2) 0.0155(4) Uani 1 1 d . . . . . H5A H 0.906705 0.668097 0.414180 0.019 Uiso 1 1 calc R U . . . H5B H 0.829446 0.712208 0.510820 0.019 Uiso 1 1 calc R U . . . C6 C 0.6708(2) 0.71393(19) 0.33344(18) 0.0129(4) Uani 1 1 d . . . . . C9 C 0.5539(3) 0.7862(2) 0.3757(2) 0.0185(4) Uani 1 1 d . . . . . H9A H 0.598695 0.869595 0.414644 0.028 Uiso 1 1 calc R U . . . H9B H 0.526910 0.730412 0.433202 0.028 Uiso 1 1 calc R U . . . H9C H 0.460957 0.805022 0.306529 0.028 Uiso 1 1 calc R U . . . C10 C 0.7173(3) 0.8046(2) 0.2489(2) 0.0193(4) Uani 1 1 d . . . . . H10A H 0.625712 0.828362 0.180297 0.029 Uiso 1 1 calc R U . . . H10B H 0.791295 0.758610 0.220146 0.029 Uiso 1 1 calc R U . . . H10C H 0.764873 0.885252 0.291996 0.029 Uiso 1 1 calc R U . . . B1 B 0.6761(3) 0.3299(2) 0.2913(2) 0.0163(4) Uani 1 1 d . . . . . H1 H 0.629374 0.318354 0.202270 0.020 Uiso 1 1 calc R U . . . 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 Cl1 0.0285(3) 0.0133(2) 0.0237(3) 0.00128(19) 0.0114(2) -0.00279(19) N1 0.0106(7) 0.0120(7) 0.0118(7) -0.0005(6) 0.0038(6) 0.0005(6) C21 0.0185(10) 0.0281(11) 0.0304(12) -0.0050(10) 0.0108(9) 0.0039(9) C20 0.0130(9) 0.0212(10) 0.0189(10) -0.0009(8) 0.0063(8) -0.0005(7) C12 0.0115(8) 0.0112(8) 0.0162(9) -0.0002(7) 0.0033(7) 0.0005(7) C11 0.0114(8) 0.0102(8) 0.0118(8) -0.0003(7) 0.0019(7) -0.0002(6) C4 0.0096(8) 0.0149(9) 0.0147(9) 0.0012(7) 0.0058(7) 0.0002(7) C3 0.0121(8) 0.0123(8) 0.0153(9) 0.0021(7) 0.0032(7) -0.0014(7) C7 0.0178(10) 0.0173(9) 0.0171(9) 0.0000(8) 0.0077(8) -0.0016(7) C8 0.0290(12) 0.0217(11) 0.0173(10) -0.0006(8) 0.0067(9) -0.0036(9) C22 0.0224(11) 0.0230(11) 0.0279(12) 0.0023(9) 0.0125(9) -0.0022(9) C16 0.0137(8) 0.0097(8) 0.0138(9) 0.0004(7) 0.0041(7) 0.0001(6) C15 0.0194(9) 0.0104(8) 0.0127(9) 0.0000(7) 0.0022(7) -0.0015(7) C14 0.0165(9) 0.0150(9) 0.0157(10) -0.0007(8) -0.0014(7) -0.0006(7) C13 0.0111(8) 0.0172(9) 0.0206(10) 0.0000(8) 0.0015(7) 0.0001(7) C17 0.0151(9) 0.0141(9) 0.0145(9) 0.0018(7) 0.0061(7) 0.0002(7) C19 0.0243(11) 0.0168(10) 0.0247(11) -0.0008(8) 0.0135(9) 0.0016(8) C18 0.0212(10) 0.0176(9) 0.0230(10) 0.0037(9) 0.0092(8) -0.0015(9) C1 0.0167(10) 0.0173(9) 0.0207(10) -0.0004(8) 0.0068(8) 0.0034(7) C2 0.0127(9) 0.0172(9) 0.0192(10) 0.0002(8) 0.0044(8) 0.0025(7) C5 0.0150(9) 0.0128(8) 0.0175(9) -0.0006(7) 0.0040(7) -0.0012(7) C6 0.0129(8) 0.0108(9) 0.0143(8) -0.0011(7) 0.0037(7) -0.0015(6) C9 0.0194(10) 0.0132(9) 0.0229(10) -0.0029(8) 0.0071(8) 0.0015(7) C10 0.0231(11) 0.0131(9) 0.0208(10) 0.0005(8) 0.0064(8) -0.0044(8) B1 0.0176(10) 0.0116(9) 0.0194(11) -0.0008(8) 0.0061(9) 0.0003(8) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 C11 N1 C6 122.33(15) . . ? C4 N1 C11 123.34(18) . . ? C4 N1 C6 114.24(16) . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? C21 C20 H20 107.9 . . ? C21 C20 C22 110.2(2) . . ? C12 C20 C21 113.04(19) . . ? C12 C20 H20 107.9 . . ? C12 C20 C22 109.79(19) . . ? C22 C20 H20 107.9 . . ? C11 C12 C20 123.51(18) . . ? C13 C12 C20 118.83(18) . . ? C13 C12 C11 117.51(19) . . ? C12 C11 N1 117.95(17) . . ? C12 C11 C16 122.64(17) . . ? C16 C11 N1 119.40(17) . . ? N1 C4 H4 97.8 . . ? N1 C4 C3 111.69(18) . . ? N1 C4 B1 128.89(19) . . ? C3 C4 H4 97.8 . . ? C3 C4 B1 113.95(17) . . ? B1 C4 H4 97.8 . . ? C4 C3 C7 110.49(17) . . ? C4 C3 C2 101.81(17) . . ? C4 C3 C5 102.14(16) . . ? C7 C3 C2 112.12(17) . . ? C5 C3 C7 112.80(18) . . ? C5 C3 C2 116.27(18) . . ? C3 C7 H7A 109.0 . . ? C3 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C8 C7 C3 113.09(19) . . ? C8 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C11 C16 C17 124.57(18) . . ? C15 C16 C11 116.86(19) . . ? C15 C16 C17 118.50(19) . . ? C16 C15 H15 119.1 . . ? C14 C15 C16 121.7(2) . . ? C14 C15 H15 119.1 . . ? C15 C14 H14 120.1 . . ? C15 C14 C13 119.84(19) . . ? C13 C14 H14 120.1 . . ? C12 C13 H13 119.3 . . ? C14 C13 C12 121.31(19) . . ? C14 C13 H13 119.3 . . ? C16 C17 H17 108.4 . . ? C16 C17 C19 110.85(18) . . ? C16 C17 C18 111.60(17) . . ? C19 C17 H17 108.4 . . ? C19 C17 C18 109.18(18) . . ? C18 C17 H17 108.4 . . ? 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 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 . . ? H1A C1 H1B 108.7 . . ? C2 C1 H1A 110.5 . . ? C2 C1 H1B 110.5 . . ? C2 C1 B1 106.32(18) . . ? B1 C1 H1A 110.5 . . ? B1 C1 H1B 110.5 . . ? C3 C2 H2A 110.4 . . ? C3 C2 H2B 110.4 . . ? C1 C2 C3 106.54(17) . . ? C1 C2 H2A 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? C3 C5 H5A 110.4 . . ? C3 C5 H5B 110.4 . . ? C3 C5 C6 106.85(16) . . ? H5A C5 H5B 108.6 . . ? C6 C5 H5A 110.4 . . ? C6 C5 H5B 110.4 . . ? N1 C6 C5 99.60(15) . . ? C9 C6 N1 110.75(17) . . ? C9 C6 C5 114.35(18) . . ? C9 C6 C10 108.77(18) . . ? C10 C6 N1 111.45(17) . . ? C10 C6 C5 111.72(18) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Cl1 B1 H1 113.4 . . ? C4 B1 Cl1 113.76(16) . . ? C4 B1 C1 91.42(17) . . ? C4 B1 H1 113.4 . . ? C1 B1 Cl1 109.53(16) . . ? C1 B1 H1 113.4 . . ? 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 Cl1 B1 1.914(3) . ? N1 C11 1.461(2) . ? N1 C4 1.289(3) . ? N1 C6 1.542(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 C20 1.527(3) . ? C20 H20 1.0000 . ? C20 C12 1.520(3) . ? C20 C22 1.543(3) . ? C12 C11 1.404(3) . ? C12 C13 1.399(3) . ? C11 C16 1.412(3) . ? C4 H4 1.0000 . ? C4 C3 1.517(3) . ? C4 B1 1.610(3) . ? C3 C7 1.543(3) . ? C3 C2 1.561(3) . ? C3 C5 1.543(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.533(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C16 C15 1.401(3) . ? C16 C17 1.516(3) . ? C15 H15 0.9500 . ? C15 C14 1.386(3) . ? C14 H14 0.9500 . ? C14 C13 1.386(3) . ? C13 H13 0.9500 . ? C17 H17 1.0000 . ? C17 C19 1.532(3) . ? C17 C18 1.540(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.557(3) . ? C1 B1 1.637(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.548(3) . ? C6 C9 1.524(3) . ? C6 C10 1.524(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? B1 H1 1.0000 . ? 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 N1 C11 C16 C15 -177.56(17) . . . . ? N1 C11 C16 C17 5.6(3) . . . . ? N1 C4 C3 C7 106.6(2) . . . . ? N1 C4 C3 C2 -134.16(19) . . . . ? N1 C4 C3 C5 -13.7(2) . . . . ? N1 C4 B1 Cl1 -136.2(2) . . . . ? N1 C4 B1 C1 111.7(2) . . . . ? C21 C20 C12 C11 134.5(2) . . . . ? C21 C20 C12 C13 -50.0(3) . . . . ? C20 C12 C11 N1 -6.6(3) . . . . ? C20 C12 C11 C16 172.24(19) . . . . ? C20 C12 C13 C14 -175.7(2) . . . . ? C12 C11 C16 C15 3.6(3) . . . . ? C12 C11 C16 C17 -173.21(19) . . . . ? C11 N1 C4 C3 -177.32(18) . . . . ? C11 N1 C4 B1 30.8(3) . . . . ? C11 N1 C6 C5 -168.72(17) . . . . ? C11 N1 C6 C9 70.5(2) . . . . ? C11 N1 C6 C10 -50.7(2) . . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C11 C16 C15 C14 -0.7(3) . . . . ? C11 C16 C17 C19 112.9(2) . . . . ? C11 C16 C17 C18 -125.2(2) . . . . ? C4 N1 C11 C12 82.7(2) . . . . ? C4 N1 C11 C16 -96.2(2) . . . . ? C4 N1 C6 C5 14.7(2) . . . . ? C4 N1 C6 C9 -106.0(2) . . . . ? C4 N1 C6 C10 132.8(2) . . . . ? C4 C3 C7 C8 178.49(19) . . . . ? C4 C3 C2 C1 7.9(2) . . . . ? C4 C3 C5 C6 22.4(2) . . . . ? C3 C4 B1 Cl1 72.4(2) . . . . ? C3 C4 B1 C1 -39.7(2) . . . . ? C3 C5 C6 N1 -22.1(2) . . . . ? C3 C5 C6 C9 95.9(2) . . . . ? C3 C5 C6 C10 -139.96(18) . . . . ? C7 C3 C2 C1 126.05(19) . . . . ? C7 C3 C5 C6 -96.2(2) . . . . ? C22 C20 C12 C11 -102.0(2) . . . . ? C22 C20 C12 C13 73.4(3) . . . . ? C16 C15 C14 C13 -2.4(3) . . . . ? C15 C16 C17 C19 -63.9(2) . . . . ? C15 C16 C17 C18 58.1(2) . . . . ? C15 C14 C13 C12 2.7(3) . . . . ? C13 C12 C11 N1 177.87(18) . . . . ? C13 C12 C11 C16 -3.3(3) . . . . ? C17 C16 C15 C14 176.29(19) . . . . ? C2 C3 C7 C8 65.7(2) . . . . ? C2 C3 C5 C6 132.23(19) . . . . ? C2 C1 B1 Cl1 -74.1(2) . . . . ? C2 C1 B1 C4 41.8(2) . . . . ? C5 C3 C7 C8 -67.9(2) . . . . ? C5 C3 C2 C1 -102.1(2) . . . . ? C6 N1 C11 C12 -93.6(2) . . . . ? C6 N1 C11 C16 87.5(2) . . . . ? C6 N1 C4 C3 -0.8(2) . . . . ? C6 N1 C4 B1 -152.7(2) . . . . ? B1 C4 C3 C7 -97.1(2) . . . . ? B1 C4 C3 C2 22.2(2) . . . . ? B1 C4 C3 C5 142.68(18) . . . . ? B1 C1 C2 C3 -34.2(2) . . . . ?