#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:50:46 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242545 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132599.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_4132599 loop_ _publ_author_name 'Schwamb, C. Benjamin' 'Fitzpatrick, Keegan P.' 'Brueckner, Alexander C.' 'Richardson, H. Camille' 'Cheong, Paul H.-Y.' 'Scheidt, Karl A.' _publ_section_title ; Enantioselective Synthesis of \a-Amidoboronates Catalyzed by Planar-Chiral NHC-Cu(I) Complexes. ; _journal_issue 34 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 10644 _journal_page_last 10648 _journal_paper_doi 10.1021/jacs.8b05045 _journal_volume 140 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C17 H26 B N O3, C18 H20 N2 O2' _chemical_formula_sum 'C35 H46 B N3 O5' _chemical_formula_weight 599.56 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2017-08-25 _audit_creation_method ; Olex2 1.2 (compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370) ; _cell_angle_alpha 90 _cell_angle_beta 91.805(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.9592(17) _cell_length_b 9.3307(12) _cell_length_c 16.2386(19) _cell_measurement_reflns_used 1677 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 63.620 _cell_measurement_theta_min 4.036 _cell_volume 1659.7(4) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection 'APEX2 V2014.11-0 (Bruker, 2014)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.01 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'MX optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_unetI/netI 0.1119 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 12226 _diffrn_reflns_point_group_measured_fraction_full 0.946 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 65.080 _diffrn_reflns_theta_max 65.080 _diffrn_reflns_theta_min 2.722 _diffrn_source microsource _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_T_max 0.7526 _exptl_absorpt_correction_T_min 0.6357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0913 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.8190. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.200 _exptl_crystal_description needle _exptl_crystal_F_000 644 _exptl_crystal_recrystallization_method 'The material was recrystallised from --- by as supplied' _exptl_crystal_size_max 0.232 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.011 _refine_diff_density_max 0.221 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.058 _refine_ls_abs_structure_details ; Flack x determined using 1185 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.1(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 5335 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0574 _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^)+(0.0566P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1173 _refine_ls_wR_factor_ref 0.1361 _reflns_Friedel_coverage 0.792 _reflns_Friedel_fraction_full 0.898 _reflns_Friedel_fraction_max 0.897 _reflns_number_gt 3632 _reflns_number_total 5335 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05045_si_005.cif _cod_data_source_block cx1055 _cod_database_code 4132599 _shelx_shelxl_version_number 2017/1 _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 0.993 _shelx_estimated_absorpt_t_min 0.867 _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 Ternary CH refined with riding coordinates: C8(H8), C9(H9), C25(H25), C26(H26) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35) 2.c Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B, H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C28(H28A, H28B,H28C) ; _shelx_res_file ; TITL cx1055 in P2(1) cx1055.res created by SHELXL-2017/1 at 13:37:48 on 25-Aug-2017 REM Best SHELXD solution FINAL CC 84.80 REM Fragments: 22 13 8 CELL 1.54178 10.9592 9.3307 16.2386 90 91.8047 90 ZERR 2 0.0017 0.0012 0.0019 0 0.0107 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H B N O UNIT 70 92 2 6 10 EQIV $1 2-X,0.5+Y,-Z EQIV $2 2-X,-0.5+Y,1-Z L.S. 4 0 0 PLAN 20 SIZE 0.011 0.015 0.232 TEMP -173.14 HTAB N1 O2_$1 HTAB N2 O5_$2 fmap 2 53 ACTA REM REM REM WGHT 0.056600 FVAR 0.77558 O1 5 0.916656 0.269022 0.129958 11.00000 0.02662 0.02424 = 0.01543 -0.00007 0.00199 -0.00784 O2 5 0.829205 0.074284 0.045872 11.00000 0.02005 0.01687 = 0.01911 -0.00323 0.00227 -0.00122 O3 5 0.708541 0.273349 0.067522 11.00000 0.02023 0.01846 = 0.02480 0.00046 0.00346 -0.00119 N1 4 1.013881 0.371298 0.028899 11.00000 0.02329 0.01987 = 0.01653 0.00140 -0.00153 -0.00299 C1 1 1.104284 0.380487 0.170655 11.00000 0.02840 0.01521 = 0.01603 -0.00195 -0.00307 -0.00048 C2 1 1.096198 0.322442 0.249346 11.00000 0.03455 0.01968 = 0.01867 0.00309 0.00422 -0.00239 AFIX 43 H2 2 1.031043 0.259587 0.261618 11.00000 -1.20000 AFIX 0 C3 1 1.183634 0.356819 0.309627 11.00000 0.04003 0.02964 = 0.01579 0.00385 -0.00198 -0.00170 AFIX 43 H3 2 1.178016 0.318376 0.363547 11.00000 -1.20000 AFIX 0 C4 1 1.278998 0.447041 0.291273 11.00000 0.03223 0.02465 = 0.02588 -0.00111 -0.00503 -0.00200 AFIX 43 H4 2 1.339714 0.468970 0.332393 11.00000 -1.20000 AFIX 0 C5 1 1.286533 0.505709 0.213188 11.00000 0.03590 0.02533 = 0.02314 0.00426 0.00023 -0.00432 AFIX 43 H5 2 1.351862 0.568538 0.201261 11.00000 -1.20000 AFIX 0 C6 1 1.199346 0.473245 0.152448 11.00000 0.03081 0.02861 = 0.01503 0.00219 -0.00012 -0.00319 AFIX 43 H6 2 1.204302 0.513757 0.098986 11.00000 -1.20000 AFIX 0 C7 1 1.010374 0.341027 0.107414 11.00000 0.02520 0.01422 = 0.01569 -0.00040 0.00167 0.00035 C8 1 0.907603 0.313964 -0.019953 11.00000 0.02758 0.02219 = 0.01444 -0.00189 -0.00276 -0.00472 AFIX 13 H8 2 0.938910 0.240842 -0.059049 11.00000 -1.20000 AFIX 0 C9 1 0.849959 0.436207 -0.071297 11.00000 0.03365 0.02184 = 0.01764 0.00189 -0.00309 0.00095 AFIX 13 H9 2 0.914970 0.478035 -0.105853 11.00000 -1.20000 AFIX 0 C10 1 0.800873 0.555707 -0.017592 11.00000 0.03669 0.01699 = 0.03001 0.00233 -0.00422 0.00403 AFIX 137 H10A 2 0.733292 0.518922 0.014397 11.00000 -1.50000 H10B 2 0.771655 0.634826 -0.052665 11.00000 -1.50000 H10C 2 0.866107 0.590215 0.020025 11.00000 -1.50000 AFIX 0 C11 1 0.749135 0.378733 -0.129229 11.00000 0.03612 0.03162 = 0.02752 0.00094 -0.00819 0.00234 AFIX 137 H11A 2 0.682194 0.341482 -0.096814 11.00000 -1.50000 H11B 2 0.781812 0.301577 -0.163042 11.00000 -1.50000 H11C 2 0.718642 0.456224 -0.165039 11.00000 -1.50000 AFIX 0 C12 1 0.729182 0.027674 0.096583 11.00000 0.02663 0.01788 = 0.01411 0.00038 0.00254 -0.00249 C13 1 0.688495 -0.119721 0.068240 11.00000 0.03524 0.02482 = 0.03176 -0.00339 0.00269 -0.00717 AFIX 137 H13A 2 0.669217 -0.117634 0.008910 11.00000 -1.50000 H13B 2 0.615742 -0.148121 0.097798 11.00000 -1.50000 H13C 2 0.754171 -0.188878 0.079655 11.00000 -1.50000 AFIX 0 C14 1 0.772185 0.019177 0.185766 11.00000 0.02931 0.02616 = 0.03037 0.00621 -0.00096 -0.00268 AFIX 137 H14A 2 0.846186 -0.039630 0.190270 11.00000 -1.50000 H14B 2 0.708173 -0.024174 0.218422 11.00000 -1.50000 H14C 2 0.790091 0.115823 0.206454 11.00000 -1.50000 AFIX 0 C15 1 0.633631 0.148035 0.079253 11.00000 0.02772 0.02018 = 0.02390 -0.00180 0.00127 -0.00084 C16 1 0.548458 0.177961 0.149237 11.00000 0.02878 0.03504 = 0.02912 -0.00717 0.00757 -0.00034 AFIX 137 H16A 2 0.596320 0.208887 0.198046 11.00000 -1.50000 H16B 2 0.503284 0.090568 0.162131 11.00000 -1.50000 H16C 2 0.490823 0.253735 0.132684 11.00000 -1.50000 AFIX 0 C17 1 0.558141 0.123217 0.000136 11.00000 0.02883 0.03706 = 0.02673 0.00019 0.00077 0.00359 AFIX 137 H17A 2 0.512270 0.210398 -0.014079 11.00000 -1.50000 H17B 2 0.501089 0.043952 0.008233 11.00000 -1.50000 H17C 2 0.612510 0.099340 -0.044630 11.00000 -1.50000 AFIX 0 B1 3 0.831925 0.229552 0.050083 11.00000 0.02350 0.01820 = 0.01251 -0.00299 0.00025 -0.00281 O4 5 1.089595 0.707699 0.605653 11.00000 0.03653 0.01733 = 0.02040 -0.00110 0.00006 -0.00101 O5 5 0.818956 0.709665 0.495545 11.00000 0.03156 0.01578 = 0.02212 -0.00338 -0.00365 0.00204 N2 4 1.080141 0.482591 0.552886 11.00000 0.02523 0.01761 = 0.02525 -0.00276 -0.00028 0.00030 N3 4 0.888450 0.483872 0.476234 11.00000 0.02944 0.01743 = 0.02129 -0.00369 -0.00546 -0.00375 H3A 2 0.885829 0.405810 0.440846 11.00000 0.02780 C18 1 1.277964 0.598876 0.573089 11.00000 0.02977 0.01635 = 0.01766 0.00433 -0.00125 -0.00063 C19 1 1.339777 0.510925 0.518919 11.00000 0.03902 0.01910 = 0.01522 -0.00493 0.00206 -0.00403 AFIX 43 H19 2 1.295974 0.445382 0.484355 11.00000 -1.20000 AFIX 0 C20 1 1.466288 0.520139 0.516004 11.00000 0.03586 0.02722 = 0.03087 -0.00361 0.00906 0.00145 AFIX 43 H20 2 1.508747 0.460921 0.478901 11.00000 -1.20000 AFIX 0 C21 1 1.530667 0.614085 0.566269 11.00000 0.03064 0.02594 = 0.03493 0.00462 0.00282 -0.00546 AFIX 43 H21 2 1.617005 0.619429 0.563491 11.00000 -1.20000 AFIX 0 C22 1 1.470363 0.700457 0.620627 11.00000 0.03333 0.02974 = 0.02546 -0.00046 -0.00018 -0.00539 AFIX 43 H22 2 1.515063 0.764187 0.655818 11.00000 -1.20000 AFIX 0 C23 1 1.343008 0.693779 0.623704 11.00000 0.03024 0.01951 = 0.02330 -0.00063 0.00010 0.00249 AFIX 43 H23 2 1.300994 0.754178 0.660426 11.00000 -1.20000 AFIX 0 C24 1 1.141838 0.600945 0.578367 11.00000 0.03389 0.01434 = 0.01457 -0.00071 -0.00353 -0.00204 C25 1 0.947347 0.472305 0.557912 11.00000 0.02491 0.01880 = 0.02207 -0.00235 -0.00182 0.00102 AFIX 13 H25 2 0.919457 0.555497 0.591280 11.00000 -1.20000 AFIX 0 C26 1 0.909745 0.336034 0.602109 11.00000 0.02796 0.02407 = 0.02157 -0.00037 0.00543 0.00205 AFIX 13 H26 2 0.934817 0.251800 0.568530 11.00000 -1.20000 AFIX 0 C27 1 0.770230 0.331866 0.609955 11.00000 0.03177 0.02714 = 0.03382 0.00181 -0.00070 -0.00245 AFIX 137 H27A 2 0.746874 0.242805 0.637300 11.00000 -1.50000 H27B 2 0.730888 0.336104 0.554971 11.00000 -1.50000 H27C 2 0.744073 0.414034 0.642591 11.00000 -1.50000 AFIX 0 C28 1 0.972582 0.325100 0.686917 11.00000 0.03437 0.03023 = 0.02566 0.00500 -0.00237 0.00432 AFIX 137 H28A 2 0.949237 0.407232 0.720582 11.00000 -1.50000 H28B 2 1.061301 0.324891 0.681017 11.00000 -1.50000 H28C 2 0.947624 0.236144 0.713701 11.00000 -1.50000 AFIX 0 C29 1 0.826133 0.602344 0.451556 11.00000 0.02769 0.01475 = 0.01866 0.00133 0.00326 -0.00246 C30 1 0.763674 0.595422 0.368891 11.00000 0.02954 0.01586 = 0.02018 0.00091 0.00112 -0.00466 C31 1 0.802839 0.510756 0.304039 11.00000 0.03699 0.01859 = 0.02217 -0.00200 0.00224 0.00635 AFIX 43 H31 2 0.874309 0.453875 0.311045 11.00000 -1.20000 AFIX 0 C32 1 0.737769 0.509300 0.229293 11.00000 0.04383 0.02437 = 0.02136 -0.00381 0.00053 0.00240 AFIX 43 H32 2 0.765206 0.451412 0.185450 11.00000 -1.20000 AFIX 0 C33 1 0.632975 0.591591 0.217943 11.00000 0.03789 0.03126 = 0.02369 0.00025 -0.00646 -0.00716 AFIX 43 H33 2 0.588407 0.589195 0.166827 11.00000 -1.20000 AFIX 0 C34 1 0.593885 0.677112 0.281577 11.00000 0.03578 0.03295 = 0.02429 0.00071 -0.00646 0.00150 AFIX 43 H34 2 0.522251 0.733513 0.273941 11.00000 -1.20000 AFIX 0 C35 1 0.658612 0.681161 0.356612 11.00000 0.03182 0.02007 = 0.02685 -0.00018 0.00061 -0.00086 AFIX 43 H35 2 0.632091 0.741635 0.399580 11.00000 -1.20000 AFIX 0 H2A 2 1.116132 0.395851 0.543261 11.00000 0.04725 H1 2 1.066069 0.429021 0.007902 11.00000 0.03844 HKLF 4 REM cx1055 in P2(1) REM R1 = 0.0574 for 3632 Fo > 4sig(Fo) and 0.0989 for all 5335 data REM 417 parameters refined using 1 restraints END WGHT 0.0566 0.0000 REM Highest difference peak 0.221, deepest hole -0.270, 1-sigma level 0.058 Q1 1 0.8956 0.2402 0.2205 11.00000 0.05 0.22 Q2 1 1.4768 0.4975 0.3004 11.00000 0.05 0.21 Q3 1 0.8173 0.5950 0.1639 11.00000 0.05 0.20 Q4 1 0.8219 0.6302 0.1067 11.00000 0.05 0.20 Q5 1 0.9377 0.0614 0.1768 11.00000 0.05 0.19 Q6 1 0.9366 0.3982 0.5824 11.00000 0.05 0.19 Q7 1 0.9725 0.6098 -0.1591 11.00000 0.05 0.19 Q8 1 1.3822 0.3806 0.3384 11.00000 0.05 0.19 Q9 1 1.0232 0.2019 0.2807 11.00000 0.05 0.19 Q10 1 1.2008 0.3787 0.6808 11.00000 0.05 0.18 Q11 1 1.4203 0.5001 0.1603 11.00000 0.05 0.18 Q12 1 1.1236 0.5485 0.5403 11.00000 0.05 0.18 Q13 1 1.1583 0.5620 0.4841 11.00000 0.05 0.18 Q14 1 0.8452 0.1368 0.0805 11.00000 0.05 0.18 Q15 1 0.5102 0.8265 0.2803 11.00000 0.05 0.18 Q16 1 0.8239 0.2024 0.5605 11.00000 0.05 0.18 Q17 1 0.7853 0.5398 0.3411 11.00000 0.05 0.18 Q18 1 1.5033 0.2926 0.5358 11.00000 0.05 0.17 Q19 1 1.2591 0.5499 0.1005 11.00000 0.05 0.17 Q20 1 0.8015 0.0974 0.6160 11.00000 0.05 0.17 ; _shelx_res_checksum 45192 _shelx_hkl_file ; -1 0 0 2922.63 33.4772 9 1 0 0 2883.72 32.1826 9 -2 0 0 2077.38 37.2452 9 -2 0 0 2103.64 35.7065 10 -3 0 0 571.603 27.8409 10 -4 0 0 25.6982 15.8713 10 -5 0 0 613.971 38.0860 10 -6 0 0 34.8841 14.1007 1 -6 0 0 18.1786 20.8844 10 -7 0 0 101.247 18.1805 1 -7 0 0 99.0070 27.3387 10 8 0 0 62.9002 23.0049 2 -8 0 0 38.5746 18.9588 1 -8 0 0 48.2587 22.5606 8 8 0 0 47.9951 27.0936 4 -8 0 0 71.2462 31.0441 10 8 0 0 54.7508 25.8973 7 -8 0 0 123.195 36.1215 2 9 0 0 13.0600 26.4383 7 9 0 0 -13.165 25.6570 2 9 0 0 26.5758 28.1072 4 -9 0 0 -11.839 25.7444 8 -9 0 0 7.72110 20.0948 1 10 0 0 49.8431 28.5103 2 -10 0 0 48.6584 44.5451 8 10 0 0 100.624 30.3791 4 -10 0 0 26.7215 20.7901 1 11 0 0 448.811 38.2992 4 11 0 0 515.163 45.4696 2 0 -1 0 1.90000 6.47650 12 0 -1 0 0.15679 5.29160 13 0 1 0 -8.0509 4.64794 13 -1 -1 0 1117.97 24.8215 9 1 1 0 1197.09 25.0677 9 2 -1 0 779.323 24.2759 7 -2 -1 0 759.464 25.4423 10 -2 -1 0 789.492 27.4101 9 -2 1 0 811.621 23.3674 10 2 1 0 862.057 28.1114 9 -3 -1 0 351.155 27.3750 10 -3 1 0 341.947 23.8350 10 3 1 0 335.799 27.7525 9 -4 -1 0 855.226 37.8577 10 -4 1 0 811.985 34.7378 10 4 1 0 810.816 36.5006 9 -5 -1 0 554.733 39.1208 10 -5 1 0 506.432 36.4988 10 -6 -1 0 780.280 47.0410 10 6 -1 0 742.368 44.9906 7 -6 -1 0 719.975 28.0781 1 -6 1 0 777.881 30.2634 1 -6 1 0 825.171 46.0951 10 7 -1 0 219.852 28.6692 4 7 -1 0 128.953 27.4804 7 -7 -1 0 213.470 33.2285 10 -7 -1 0 246.833 24.7097 1 -7 1 0 265.941 26.9901 1 -7 1 0 231.672 34.2270 10 8 -1 0 28.4512 21.7952 2 8 -1 0 53.2539 25.9353 7 -8 -1 0 30.4650 31.6997 2 -8 -1 0 46.1417 27.9352 10 8 -1 0 19.3125 26.6519 4 -8 -1 0 57.4193 24.4908 8 -8 -1 0 20.8590 18.3299 1 -8 1 0 33.9028 19.6196 1 9 -1 0 46.0613 23.0126 2 -9 -1 0 2.14900 19.6301 1 9 -1 0 44.7731 30.0751 4 -9 -1 0 52.0535 31.6069 2 9 -1 0 15.2271 27.8407 7 -9 -1 0 12.2042 35.3889 14 -9 -1 0 -25.247 32.5215 10 -9 1 0 48.8936 24.3173 8 -9 1 0 4.01861 20.9464 1 -10 -1 0 61.6417 36.3326 2 10 -1 0 25.1717 26.7032 2 -10 -1 0 42.7896 20.2023 1 10 -1 0 69.1888 32.7629 4 -10 1 0 66.4687 22.6630 1 10 1 0 42.5922 27.4491 4 -10 1 0 74.0882 30.5540 8 11 -1 0 -21.423 24.1066 2 -11 -1 0 50.8135 27.9625 2 -11 1 0 33.3825 22.3240 1 11 1 0 53.0063 27.7443 4 12 -1 0 3.38842 20.7432 2 -12 1 0 30.6449 20.1206 1 12 1 0 45.9110 26.7506 4 0 -2 0 599.071 26.8177 12 0 -2 0 637.330 23.2729 13 0 2 0 621.103 23.0251 13 -1 -2 0 6454.27 72.0689 13 -1 -2 0 6245.25 74.6042 14 1 -2 0 6285.11 66.4351 7 1 -2 0 6435.44 71.9276 12 -1 2 0 6644.81 77.9958 13 1 2 0 6806.29 80.8902 9 -2 -2 0 2633.75 52.0716 14 2 -2 0 2537.84 44.2491 7 -2 -2 0 2587.31 45.2338 10 2 2 0 2727.63 53.5819 9 -3 -2 0 1160.31 39.1406 10 -3 -2 0 1161.98 42.6647 14 3 -2 0 1208.13 37.6357 7 3 2 0 1229.97 41.5092 9 4 -2 0 528.973 34.1520 7 -4 -2 0 582.277 36.0162 10 4 2 0 587.645 36.0637 9 -4 2 0 503.228 30.1287 10 5 -2 0 392.458 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405.261 30.0168 2 7 5 -3 393.589 50.5677 6 -7 5 3 383.565 33.6980 1 7 5 -3 408.814 29.5768 1 -6 -5 3 230.544 22.3339 5 6 -5 -3 197.256 27.5643 2 -6 -5 3 234.476 33.2997 8 -6 -5 3 240.618 39.4057 10 -6 -5 3 313.236 36.9689 2 6 5 -3 323.774 27.5386 1 6 5 -3 263.762 34.9564 6 -6 5 3 337.597 29.6745 1 -5 -5 3 565.457 47.6553 2 -5 -5 3 558.237 49.5138 10 5 -5 -3 492.167 28.9266 2 -5 -5 3 502.566 34.1532 8 -5 -5 3 527.005 24.4044 5 5 5 -3 699.164 47.1040 6 5 5 -3 617.005 29.4971 1 -4 -5 3 129.373 28.4615 10 -4 -5 3 143.413 15.0182 5 -4 -5 3 126.071 18.3399 8 -4 -5 3 144.434 27.5403 2 4 5 -3 152.610 20.5264 1 4 5 -3 163.475 26.8433 6 3 -5 -3 330.466 24.9875 3 -3 -5 3 250.737 25.4091 8 3 5 -3 298.666 35.0386 6 3 5 -3 309.854 21.4204 1 2 -5 -3 973.260 30.6161 3 2 5 -3 1175.00 43.8577 6 2 5 -3 1103.78 30.3028 1 1 -5 -3 20.9900 12.7818 3 1 5 -3 1.63408 15.2568 6 1 5 -3 1.50365 10.3540 1 -1 5 3 -0.1509 16.7127 9 0 -5 -3 236.637 35.0327 12 0 -5 -3 245.613 22.4599 3 0 5 -3 276.765 26.7625 6 0 5 -3 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305.315 25.5083 1 -4 -6 -3 18.8131 21.6730 2 4 -6 3 65.7010 12.5380 16 -4 -6 -3 49.8564 39.6941 12 -4 -6 -3 47.3177 12.2462 5 -4 6 -3 67.3004 18.9169 1 -5 -6 -3 15.8496 25.4597 2 5 -6 3 13.6321 11.0272 16 -5 -6 -3 31.3794 12.0419 5 -5 6 -3 10.9044 20.3164 1 6 -6 3 23.8050 18.3047 2 6 -6 3 38.3707 11.9464 16 -6 -6 -3 85.4021 27.5622 2 -6 6 -3 19.6442 21.8109 1 -6 6 -3 104.401 50.1091 11 6 6 3 34.5377 17.7396 1 7 -6 3 23.0755 12.2187 16 -7 -6 -3 27.3748 26.7193 2 7 -6 3 21.3175 18.6063 2 -7 6 -3 70.6915 24.8733 1 -7 6 -3 49.6201 42.0404 11 8 -6 3 126.247 21.1926 2 8 -6 3 70.3398 14.8334 16 -8 -6 -3 114.127 30.0792 2 -8 6 -3 126.099 27.0423 1 -8 6 -3 173.945 36.7386 11 -9 -6 -3 -20.257 22.8023 2 9 -6 3 23.2461 17.6999 2 -9 6 -3 -2.3231 20.3779 1 10 -6 3 13.5753 15.3068 2 -10 -6 -3 20.7291 18.9653 2 9 -7 -3 -9.1695 14.8324 2 8 -7 -3 8.52062 15.1124 2 8 7 -3 -10.850 16.0095 1 -7 -7 3 51.5847 20.6397 8 7 -7 -3 87.5258 17.6941 2 -7 -7 3 96.8711 15.6998 5 7 7 -3 78.6118 19.0962 1 7 7 -3 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53.4248 15.4286 3 -7 4 -9 79.8681 23.0319 1 -7 4 -9 94.2023 19.9381 4 8 -4 9 60.9655 19.9257 15 -8 -4 -9 15.7465 26.0051 2 -8 4 -9 1.16225 15.6110 3 -8 4 -9 19.5929 15.8350 4 -9 -4 -9 7.09804 23.2907 2 9 -4 9 21.4010 15.5389 15 -9 4 -9 33.8247 16.2588 3 -9 4 -9 10.5979 13.6568 4 -10 -4 -9 38.7963 17.2280 2 -9 -5 9 27.5822 17.2669 8 9 5 -9 63.5142 20.3954 4 -9 5 9 36.1672 26.9485 8 -8 -5 9 74.2536 20.5843 8 -8 -5 9 58.0038 14.9622 5 8 5 -9 29.0499 18.6009 4 -8 5 9 30.7352 28.2308 8 -7 -5 9 122.476 23.8311 8 -7 -5 9 144.121 17.6836 5 7 5 -9 102.349 19.7317 4 -7 5 9 108.925 30.1920 8 7 5 -9 71.9602 30.5228 6 7 5 -9 80.3754 17.3620 1 -6 -5 9 88.2837 18.8431 1 -6 -5 9 175.943 19.0845 5 -6 -5 9 181.671 26.2541 8 6 5 -9 174.105 24.2851 1 6 5 -9 173.815 34.4155 6 6 5 -9 203.204 23.3657 4 -5 -5 9 86.8792 18.3765 1 -5 -5 9 43.7276 36.5714 10 -5 -5 9 159.619 24.6125 8 5 5 -9 104.647 31.6740 6 5 5 -9 82.7354 16.8335 4 5 5 -9 98.6598 17.6083 1 -4 -5 9 35.1506 18.4756 8 -4 -5 9 33.9371 17.1286 1 -4 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254.588 44.6868 2 -4 -1 10 329.592 42.9091 10 -4 -1 10 292.249 25.6617 1 -4 -1 10 235.067 34.9099 8 4 -1 -10 236.557 39.6711 2 4 1 -10 236.097 40.9649 2 -4 1 10 268.734 25.0784 1 4 1 -10 240.200 38.8907 6 -4 1 10 269.165 38.2615 10 -3 -1 10 368.069 27.0586 1 -3 -1 10 364.420 46.9014 7 3 1 -10 395.804 41.1201 2 -3 1 10 413.371 42.4086 10 3 1 -10 391.685 38.6348 6 -2 -1 10 247.865 37.8817 7 2 1 -10 201.497 34.2431 6 -1 -1 10 271.901 43.7045 7 1 1 -10 212.125 34.9225 6 0 -1 -10 14.9127 9.98218 3 0 -1 10 24.2157 23.5055 7 0 1 -10 27.4343 18.7646 6 0 1 -10 22.6657 9.01087 3 -1 -1 -10 102.208 13.3065 3 1 -1 10 122.340 29.9764 7 -1 1 -10 94.7632 11.4276 3 -1 1 -10 117.916 23.5019 6 -1 1 -10 107.756 7.04199 4 1 1 10 98.4583 25.5436 7 2 -1 10 221.282 35.3007 7 -2 -1 -10 239.044 20.1354 3 -2 1 -10 225.888 8.69672 4 -2 1 -10 212.408 17.5635 3 -2 1 -10 262.927 32.0899 2 2 1 10 201.222 29.6097 7 3 -1 10 382.395 49.8752 7 -3 -1 -10 396.915 23.0622 3 -3 -1 -10 327.844 48.5699 2 -3 1 -10 406.960 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42.1399 2 -8 1 -10 137.433 20.8157 3 -9 -1 -10 58.6629 29.0868 2 9 -1 10 70.7540 22.3944 15 -9 1 -10 65.7926 18.3893 3 9 1 10 122.402 25.2319 15 -9 1 -10 97.6306 35.1261 2 -10 -1 -10 23.1052 24.2809 2 10 -1 10 11.3300 20.1256 15 -10 1 -10 -0.6787 24.7675 2 -10 -2 10 12.1100 18.2187 8 10 -2 -10 27.0591 21.4009 2 -10 -2 10 -0.0353 18.5403 1 10 2 -10 -12.611 19.9140 2 -10 2 10 -11.216 21.7037 8 -10 2 10 3.91753 21.6388 1 -9 -2 10 -4.6992 19.5917 8 9 -2 -10 35.9271 25.0954 2 -9 -2 10 23.1115 18.7332 1 -9 2 10 14.7903 23.9398 8 -9 2 10 8.09592 20.5150 1 9 2 -10 10.7020 25.6673 2 -8 -2 10 158.373 25.0458 8 8 -2 -10 141.854 29.9584 2 -8 -2 10 120.171 23.6898 1 8 2 -10 149.253 31.4111 2 -8 2 10 169.337 26.2829 1 -8 2 10 171.537 29.9491 8 -7 -2 10 44.7194 21.7460 8 -7 -2 10 38.8186 19.3672 1 7 -2 -10 12.4488 26.5447 2 -7 2 10 69.3655 21.3030 1 -7 2 10 80.6024 27.8710 8 7 2 -10 16.7120 28.7850 2 6 -2 -10 55.5620 27.4073 2 -6 -2 10 36.6872 36.8160 10 -6 -2 10 61.7967 21.8871 8 -6 -2 10 57.7984 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19.4809 3 -3 4 -15 8.18715 16.1491 3 -3 4 -15 1.65913 33.4780 2 4 -4 15 29.3417 25.0817 15 -4 -4 -15 -7.1397 20.3959 3 -4 4 -15 25.7968 34.0499 2 -4 4 -15 21.7962 17.6413 3 -5 -4 -15 66.1861 28.3701 3 5 -4 15 17.4944 15.8399 15 -5 4 -15 38.5969 29.0274 2 -5 4 -15 3.25907 19.1896 3 6 -4 15 17.0234 13.8802 15 -6 4 -15 -11.674 26.6346 2 -5 -5 15 62.0427 14.0177 5 5 5 -15 38.3337 19.1307 2 -4 -5 15 4.55478 12.8282 5 -4 -5 15 2.82078 24.9425 1 4 5 -15 38.2078 21.3430 2 -3 -5 15 3.31450 15.1266 1 3 5 -15 6.35631 21.8430 2 -2 -5 15 123.073 19.7118 1 2 5 -15 151.960 31.9110 2 -1 -5 15 5.73059 14.9690 1 1 5 -15 14.4577 26.4737 2 0 -5 15 130.104 19.6706 1 0 -5 -15 157.831 24.0130 3 0 5 -15 154.211 32.9814 2 1 -5 15 91.1523 18.4050 1 -1 -5 -15 78.1895 22.5270 3 -1 5 -15 71.3867 32.3199 2 -2 -5 -15 7.09650 22.4343 3 2 -5 15 2.34455 15.3162 1 -2 5 -15 2.76025 31.9194 2 -3 -5 -15 14.4767 23.7015 3 3 -5 15 54.1136 19.0220 1 -3 5 -15 78.1455 32.5130 2 -4 -5 -15 9.98728 27.1327 3 -4 5 -15 13.8269 29.3870 2 -4 -6 15 13.4630 11.4854 5 -3 -6 15 50.7514 13.2111 5 -2 -6 15 10.6812 9.88465 5 0 -6 -15 48.0006 25.8962 3 0 -6 15 55.8978 10.4893 16 -1 -6 -15 -0.6767 24.7226 3 1 -6 15 7.42032 9.61444 16 7 0 -16 5.65961 15.2672 2 6 0 -16 -5.6477 17.9106 2 -6 0 16 50.5639 20.1502 1 -5 0 16 34.7835 19.1490 1 5 0 -16 12.0209 20.1426 2 4 0 -16 4.10608 19.7159 2 -4 0 16 2.21247 19.4549 1 3 0 -16 59.0093 22.1753 2 -3 0 16 276.216 32.5987 1 2 0 -16 2.57702 21.6434 2 -2 0 16 26.7296 19.0890 1 -1 0 16 240.274 30.1464 1 1 0 -16 214.024 38.9174 2 0 0 -16 11.5472 22.8349 2 -1 0 -16 32.4251 28.7771 2 -2 0 -16 51.9399 18.2584 3 -2 0 -16 77.8406 32.5147 2 -3 0 -16 5.61445 30.3080 2 -3 0 -16 -4.8311 17.1128 3 -4 0 -16 166.610 21.9716 3 -4 0 -16 164.818 33.5116 2 4 0 16 146.422 27.4031 15 -5 0 -16 6.85477 27.8982 2 5 0 16 22.1593 21.9146 15 -5 0 -16 -0.8366 18.3520 3 -6 0 -16 23.2047 24.6126 2 -6 0 -16 2.02604 22.1983 3 6 0 16 27.6313 18.4408 15 7 1 -16 15.6380 15.8381 2 -6 -1 16 68.1778 22.0448 1 6 -1 -16 6.32493 15.6834 2 6 1 -16 28.1935 19.4438 2 -5 -1 16 38.1186 18.3930 1 5 -1 -16 -4.5704 16.7355 2 5 1 -16 40.0414 21.7879 2 4 -1 -16 -4.7244 16.9089 2 -4 -1 16 18.9398 19.4742 1 4 1 -16 -19.066 19.9279 2 -3 -1 16 111.210 22.7861 1 3 -1 -16 33.7274 19.4262 2 3 1 -16 36.3876 22.4270 2 2 -1 -16 8.95969 19.6175 2 -2 -1 16 77.9657 20.6918 1 2 1 -16 44.4256 23.7458 2 1 -1 -16 6.44925 20.1047 2 -1 -1 16 27.9857 20.0666 1 1 1 -16 20.0282 23.3219 2 0 -1 -16 4.00383 22.0303 2 0 1 -16 76.1664 28.5940 2 -1 -1 -16 127.425 24.1291 3 -1 -1 -16 63.1179 29.3453 2 -1 1 -16 150.496 31.1912 2 -2 -1 -16 85.2620 29.1485 2 -2 -1 -16 109.835 20.8319 3 -2 1 -16 49.8421 31.1296 2 -2 1 -16 131.425 19.8905 3 -3 -1 -16 -10.095 29.2641 2 -3 -1 -16 74.6474 20.2135 3 -3 1 -16 31.7616 32.4457 2 -3 1 -16 70.4501 18.7908 3 -4 -1 -16 -7.5296 17.2928 3 -4 -1 -16 33.4964 29.8903 2 4 -1 16 -10.956 24.0065 15 4 1 16 8.42457 26.1367 15 -4 1 -16 9.02289 32.1326 2 -4 1 -16 -0.9084 16.8012 3 -5 -1 -16 47.7339 26.4866 2 -5 -1 -16 42.1667 20.9244 3 5 -1 16 6.17373 20.3796 15 -5 1 -16 23.4815 30.1738 2 5 1 16 48.2116 23.3359 15 -5 1 -16 5.67526 18.6911 3 6 -1 16 71.7015 17.7307 15 -6 -1 -16 36.2944 21.1373 2 -6 1 -16 95.0995 28.8402 2 6 1 16 71.7804 20.9217 15 -6 -2 16 7.50718 30.9482 1 6 2 -16 -5.9202 16.2079 2 -5 -2 16 31.3322 18.5338 1 5 2 -16 -2.3712 18.8537 2 -4 -2 16 32.5754 18.5196 1 4 2 -16 -2.6372 21.3454 2 -3 -2 16 102.408 20.9841 1 3 2 -16 26.9723 22.0030 2 -2 -2 16 46.7844 18.4644 1 2 2 -16 39.2170 24.5443 2 -1 -2 16 95.7453 21.3059 1 1 2 -16 26.4716 25.3779 2 0 -2 16 104.746 21.6555 1 0 2 -16 68.5989 28.7652 2 -1 -2 -16 115.332 23.2530 3 -1 2 -16 101.739 30.6967 2 -2 -2 -16 68.2176 21.3716 3 -2 2 -16 74.9257 32.5564 2 -3 -2 -16 15.6115 18.7884 3 3 -2 16 29.9818 25.0950 15 -3 2 -16 -20.669 16.3348 3 3 2 16 -49.522 25.5630 15 -3 2 -16 2.63829 32.1418 2 -4 -2 -16 41.1721 20.1074 3 4 -2 16 23.8833 23.4434 15 -4 2 -16 24.5142 18.6559 3 -4 2 -16 31.6006 32.1362 2 -5 -2 -16 15.8657 23.7699 3 5 -2 16 13.0395 20.0341 15 -5 2 -16 -13.911 20.3319 3 -5 2 -16 -5.0017 28.3802 2 6 -2 16 9.11203 15.0468 15 -6 2 -16 29.1251 26.0810 2 6 3 -16 27.2598 17.4792 2 -5 -3 16 32.6758 19.4907 1 5 3 -16 36.9851 19.9712 2 -4 -3 16 4.24974 17.0256 1 4 3 -16 -14.428 18.1809 2 -3 -3 16 40.9337 18.8248 1 3 3 -16 19.5410 21.3234 2 -2 -3 16 10.6106 15.8360 1 2 3 -16 -25.766 21.1623 2 -1 -3 16 10.3857 15.7556 1 1 3 -16 38.6229 26.7332 2 0 -3 16 262.610 29.7120 1 0 3 -16 302.820 47.6196 2 -1 -3 -16 85.3507 22.2273 3 1 -3 16 85.7325 19.9445 1 -1 3 -16 78.9683 30.7996 2 -2 -3 -16 14.3927 20.1430 3 -2 3 -16 68.9580 33.3357 2 3 -3 16 12.2515 24.0327 15 -3 -3 -16 31.6919 21.1316 3 -3 3 -16 17.4516 31.9743 2 -3 3 -16 23.2397 17.4043 3 -4 -3 -16 30.5245 22.5068 3 4 -3 16 47.9782 22.1251 15 -4 3 -16 82.1593 19.3590 3 -4 3 -16 46.1182 32.1003 2 5 -3 16 81.8730 17.7866 15 -5 -3 -16 53.3119 28.5372 3 -5 3 -16 104.336 30.1852 2 5 4 -16 18.4353 17.8429 2 -4 -4 16 37.4920 18.9376 1 4 4 -16 44.4872 21.3031 2 -3 -4 16 5.86315 17.1565 1 3 4 -16 -10.635 20.5371 2 -2 -4 16 17.5804 16.5045 1 2 4 -16 7.46000 23.9394 2 -1 -4 16 146.606 20.5964 1 1 4 -16 134.121 28.8142 2 0 -4 16 -2.5008 14.4002 1 0 4 -16 9.30357 27.4078 2 1 -4 16 46.6894 17.0165 1 -1 -4 -16 24.6755 20.9165 3 1 -4 16 59.8746 29.1278 15 -1 4 -16 -8.9935 29.5846 2 -2 -4 -16 60.7469 23.0531 3 2 -4 16 72.2026 19.6134 1 2 -4 16 98.5225 28.7580 15 -2 4 -16 123.969 34.3749 2 3 -4 16 32.2245 25.1155 15 3 -4 16 17.4536 17.8754 1 -3 -4 -16 -3.3497 23.3059 3 -3 4 -16 -18.107 30.0974 2 4 -4 16 39.9905 16.2187 15 -4 -4 -16 -24.766 27.9353 3 -4 4 -16 -36.837 28.0500 2 -4 -5 16 36.9622 12.8560 5 4 5 -16 30.8871 19.6014 2 -3 -5 16 -0.6470 11.9846 5 3 5 -16 19.4378 20.9977 2 -2 -5 16 27.8969 10.7479 5 2 5 -16 26.5156 23.5428 2 -1 -5 16 121.074 27.2920 1 1 5 -16 81.8670 27.0290 2 0 -5 16 75.1009 27.8349 1 0 5 -16 90.2049 29.3444 2 -1 -5 -16 108.360 27.3357 3 -1 5 -16 33.1989 27.4568 2 -2 5 -16 27.4630 27.8878 2 -3 5 -16 12.5329 27.2976 2 6 0 -17 2.35514 14.2737 2 5 0 -17 29.3090 16.4067 2 4 0 -17 56.1698 19.5552 2 -4 0 17 129.560 22.0833 1 3 0 -17 6.53966 18.7979 2 -3 0 17 15.7319 20.0348 1 2 0 -17 -34.548 18.9434 2 -2 0 17 -2.5972 19.4348 1 -1 0 17 34.9389 19.2305 1 1 0 -17 1.89978 20.8424 2 0 0 17 -6.9257 19.1107 1 0 0 -17 -17.186 25.4120 2 -1 0 -17 5.41749 28.3749 2 -2 0 -17 160.473 35.7976 3 -2 0 -17 102.122 29.8179 2 -3 0 -17 29.3613 19.0516 3 3 0 17 18.9820 23.0658 15 -3 0 -17 27.9893 28.9921 2 -4 0 -17 5.55060 26.1170 2 -4 0 -17 52.3869 21.9403 3 4 0 17 28.8750 21.6936 15 -5 0 -17 -13.414 22.1626 2 5 0 17 -5.3560 17.8605 15 6 1 -17 -8.2046 13.6076 2 5 1 -17 -9.4351 15.3853 2 -4 -1 17 33.4978 19.9916 1 4 1 -17 16.9752 17.8052 2 -3 -1 17 32.8809 20.0785 1 3 1 -17 55.9221 22.1289 2 -2 -1 17 23.0016 18.9607 1 2 1 -17 -11.654 21.2933 2 -1 -1 17 143.671 22.9296 1 1 1 -17 56.4347 24.7637 2 0 -1 17 112.750 22.8277 1 0 1 -17 38.5330 24.6714 2 -1 1 -17 26.0152 28.7628 2 -2 -1 -17 73.3086 21.2216 3 -2 -1 -17 -7.7846 33.2544 2 -2 1 -17 7.64639 29.4863 2 -3 -1 -17 9.14291 19.7326 3 3 -1 17 56.2231 23.4564 15 -3 -1 -17 -11.991 28.7579 2 3 1 17 -26.974 23.4309 15 -3 1 -17 29.0092 29.3853 2 -3 1 -17 10.6384 18.0983 3 -4 -1 -17 1.28230 34.0768 2 4 -1 17 9.45459 20.8720 15 -4 -1 -17 0.18856 22.7765 3 4 1 17 -1.5668 22.0806 15 -4 1 -17 32.9256 26.6631 2 -4 1 -17 -4.4240 20.4933 3 5 -1 17 4.29195 17.0877 15 5 1 17 37.9991 18.5694 15 -5 1 -17 10.1883 23.4203 2 5 2 -17 3.57804 14.9776 2 -4 -2 17 -2.3859 18.5585 1 4 2 -17 16.0771 18.3681 2 -3 -2 17 39.6228 19.1963 1 3 2 -17 31.8425 20.6822 2 -2 -2 17 8.53991 16.4782 1 2 2 -17 -10.619 20.3254 2 -1 -2 17 20.1647 17.1749 1 1 2 -17 17.4817 23.8226 2 0 -2 17 -7.0509 16.3332 1 0 2 -17 1.39864 24.7566 2 1 -2 17 45.5575 18.9149 1 -1 2 -17 25.8329 28.0712 2 -2 -2 -17 32.7785 20.6816 3 -2 2 -17 -9.1956 29.5903 2 -3 -2 -17 1.45967 21.5566 3 3 -2 17 17.3924 21.6878 15 -3 2 -17 54.2841 30.3263 2 3 2 17 -53.958 29.4699 15 4 -2 17 25.7207 19.4339 15 -4 -2 -17 -36.055 26.1604 3 -4 2 -17 14.2353 27.6650 2 5 -2 17 35.3592 15.3721 15 4 3 -17 14.2558 17.7262 2 -3 -3 17 9.95521 20.5068 1 3 3 -17 0.52676 18.9431 2 -2 -3 17 195.341 29.8221 1 2 3 -17 111.253 24.8202 2 -1 -3 17 29.6132 16.5219 1 1 3 -17 -16.694 20.0597 2 0 -3 17 -2.9121 15.8795 1 0 3 -17 40.6953 26.2029 2 1 -3 17 31.2247 18.4008 1 -1 3 -17 -5.5256 26.5851 2 -2 -3 -17 10.1294 20.7596 3 2 -3 17 5.61039 19.5663 1 2 -3 17 2.49095 22.5091 15 -2 3 -17 41.5329 29.5979 2 3 -3 17 85.1004 22.3272 15 -3 -3 -17 69.7970 27.9982 3 -3 3 -17 59.2623 30.0050 2 4 -3 17 0.48714 16.9963 15 -4 3 -17 16.7552 27.0356 2 3 4 -17 12.6116 19.2266 2 2 4 -17 11.6051 20.9574 2 -1 -4 17 15.8667 31.4921 1 1 4 -17 26.8752 23.0132 2 0 -4 17 -59.435 23.7861 15 0 -4 17 -11.955 19.9975 1 0 4 -17 26.8983 25.5558 2 1 -4 17 12.3462 24.6852 15 -1 4 -17 -3.8123 25.4097 2 2 -4 17 18.1025 23.0966 15 -2 4 -17 0.69515 26.2454 2 3 -4 17 19.0145 14.7200 15 -3 4 -17 0.95862 25.7783 2 4 0 -18 -8.0953 16.3009 2 3 0 -18 -5.3903 16.0527 2 2 0 -18 5.84754 18.1683 2 1 0 -18 -16.805 22.5491 2 0 0 -18 -26.837 23.5539 2 -1 0 -18 -16.657 23.3116 2 -2 0 -18 -19.132 24.2469 2 3 0 18 4.58174 19.3917 15 -3 0 -18 -37.911 22.0838 2 4 1 -18 14.7286 16.6814 2 3 1 -18 -7.0120 16.8824 2 2 1 -18 8.32131 19.6110 2 -1 -1 18 77.3185 21.6865 1 1 1 -18 35.2713 21.6443 2 0 -1 18 46.3304 20.8501 1 0 1 -18 10.1248 24.3053 2 1 -1 18 39.6654 23.9601 1 2 -1 18 35.8266 20.4224 15 -2 1 -18 46.6499 26.1557 2 2 1 18 4.67770 22.3140 15 3 -1 18 58.3358 20.2465 15 -3 1 -18 14.0440 24.1138 2 3 1 18 24.5570 21.4965 15 3 2 -18 52.5154 18.8172 2 2 2 -18 15.9283 20.0086 2 -1 -2 18 29.2048 25.1343 1 1 2 -18 -13.158 20.1568 2 0 -2 18 28.3272 20.3060 1 0 2 -18 17.3107 24.3307 2 -1 2 -18 7.32005 25.3983 2 2 -2 18 34.2501 19.7883 15 -2 2 -18 58.0711 26.8578 2 2 2 18 59.0232 32.6574 15 3 -2 18 24.5532 18.2509 15 -3 2 -18 44.3191 25.2052 2 2 3 -18 14.3893 18.3676 2 1 3 -18 48.3383 21.1490 2 0 3 -18 19.1653 21.3891 2 1 -3 18 42.3869 20.7420 15 -1 3 -18 43.5688 24.6789 2 2 -3 18 28.3190 18.9871 15 0 0 0 0.00 0.00 0 _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 0.7526 _exptl_absorpt_correction_T_min 0.6357 _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 1.54184 10.955 9.334 16.228 90.027 91.787 89.960 ) ; _shelx_hkl_checksum 58687 _olex2_date_sample_data_collection 2017-08-24 _olex2_date_sample_submission 2017-08-19 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in Paratone oil' _olex2_submission_original_sample_id cx1055 _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 O1 O 0.9167(3) 0.2690(4) 0.1300(2) 0.0221(9) Uani 1 1 d . O2 O 0.8292(3) 0.0743(4) 0.0459(2) 0.0186(9) Uani 1 1 d . O3 O 0.7085(3) 0.2733(4) 0.0675(2) 0.0211(9) Uani 1 1 d . N1 N 1.0139(5) 0.3713(5) 0.0289(3) 0.0199(11) Uani 1 1 d . C1 C 1.1043(5) 0.3805(6) 0.1707(3) 0.0200(13) Uani 1 1 d . C2 C 1.0962(6) 0.3224(6) 0.2493(3) 0.0242(14) Uani 1 1 d . H2 H 1.031043 0.259587 0.261618 0.029 Uiso 1 1 calc R C3 C 1.1836(6) 0.3568(7) 0.3096(4) 0.0285(15) Uani 1 1 d . H3 H 1.178016 0.318376 0.363547 0.034 Uiso 1 1 calc R C4 C 1.2790(6) 0.4470(6) 0.2913(4) 0.0277(15) Uani 1 1 d . H4 H 1.339714 0.468970 0.332393 0.033 Uiso 1 1 calc R C5 C 1.2865(6) 0.5057(7) 0.2132(4) 0.0281(15) Uani 1 1 d . H5 H 1.351862 0.568538 0.201261 0.034 Uiso 1 1 calc R C6 C 1.1993(6) 0.4732(7) 0.1524(4) 0.0248(14) Uani 1 1 d . H6 H 1.204302 0.513757 0.098986 0.030 Uiso 1 1 calc R C7 C 1.0104(5) 0.3410(6) 0.1074(3) 0.0183(13) Uani 1 1 d . C8 C 0.9076(5) 0.3140(6) -0.0200(4) 0.0215(14) Uani 1 1 d . H8 H 0.938910 0.240842 -0.059049 0.026 Uiso 1 1 calc R C9 C 0.8500(6) 0.4362(6) -0.0713(4) 0.0245(14) Uani 1 1 d . H9 H 0.914970 0.478035 -0.105853 0.029 Uiso 1 1 calc R C10 C 0.8009(6) 0.5557(6) -0.0176(4) 0.0280(15) Uani 1 1 d . H10A H 0.733292 0.518922 0.014397 0.042 Uiso 1 1 calc GR H10B H 0.771655 0.634826 -0.052665 0.042 Uiso 1 1 calc GR H10C H 0.866107 0.590215 0.020025 0.042 Uiso 1 1 calc GR C11 C 0.7491(6) 0.3787(7) -0.1292(4) 0.0319(16) Uani 1 1 d . H11A H 0.682194 0.341482 -0.096814 0.048 Uiso 1 1 calc GR H11B H 0.781812 0.301577 -0.163042 0.048 Uiso 1 1 calc GR H11C H 0.718642 0.456224 -0.165039 0.048 Uiso 1 1 calc GR C12 C 0.7292(5) 0.0277(6) 0.0966(3) 0.0195(13) Uani 1 1 d . C13 C 0.6885(6) -0.1197(6) 0.0682(4) 0.0306(15) Uani 1 1 d . H13A H 0.669217 -0.117634 0.008910 0.046 Uiso 1 1 calc GR H13B H 0.615742 -0.148121 0.097798 0.046 Uiso 1 1 calc GR H13C H 0.754171 -0.188878 0.079655 0.046 Uiso 1 1 calc GR C14 C 0.7722(6) 0.0192(7) 0.1858(4) 0.0287(15) Uani 1 1 d . H14A H 0.846186 -0.039630 0.190270 0.043 Uiso 1 1 calc GR H14B H 0.708173 -0.024174 0.218422 0.043 Uiso 1 1 calc GR H14C H 0.790091 0.115823 0.206454 0.043 Uiso 1 1 calc GR C15 C 0.6336(6) 0.1480(6) 0.0793(4) 0.0239(14) Uani 1 1 d . C16 C 0.5485(6) 0.1780(7) 0.1492(4) 0.0308(16) Uani 1 1 d . H16A H 0.596320 0.208887 0.198046 0.046 Uiso 1 1 calc GR H16B H 0.503284 0.090568 0.162131 0.046 Uiso 1 1 calc GR H16C H 0.490823 0.253735 0.132684 0.046 Uiso 1 1 calc GR C17 C 0.5581(6) 0.1232(7) 0.0001(4) 0.0309(16) Uani 1 1 d . H17A H 0.512270 0.210398 -0.014079 0.046 Uiso 1 1 calc GR H17B H 0.501089 0.043952 0.008233 0.046 Uiso 1 1 calc GR H17C H 0.612510 0.099340 -0.044630 0.046 Uiso 1 1 calc GR B1 B 0.8319(6) 0.2296(7) 0.0501(4) 0.0181(15) Uani 1 1 d . O4 O 1.0896(4) 0.7077(4) 0.6057(2) 0.0248(10) Uani 1 1 d . O5 O 0.8190(4) 0.7097(4) 0.4955(2) 0.0233(9) Uani 1 1 d . N2 N 1.0801(5) 0.4826(5) 0.5529(3) 0.0227(12) Uani 1 1 d . N3 N 0.8884(5) 0.4839(5) 0.4762(3) 0.0229(12) Uani 1 1 d . H3A H 0.886(6) 0.406(7) 0.441(4) 0.028(18) Uiso 1 1 d . C18 C 1.2780(5) 0.5989(6) 0.5731(3) 0.0213(13) Uani 1 1 d . C19 C 1.3398(6) 0.5109(6) 0.5189(4) 0.0244(14) Uani 1 1 d . H19 H 1.295974 0.445382 0.484355 0.029 Uiso 1 1 calc R C20 C 1.4663(6) 0.5201(7) 0.5160(4) 0.0312(16) Uani 1 1 d . H20 H 1.508747 0.460921 0.478901 0.037 Uiso 1 1 calc R C21 C 1.5307(6) 0.6141(6) 0.5663(4) 0.0305(16) Uani 1 1 d . H21 H 1.617005 0.619429 0.563491 0.037 Uiso 1 1 calc R C22 C 1.4704(6) 0.7005(7) 0.6206(4) 0.0295(15) Uani 1 1 d . H22 H 1.515063 0.764187 0.655818 0.035 Uiso 1 1 calc R C23 C 1.3430(6) 0.6938(6) 0.6237(4) 0.0244(14) Uani 1 1 d . H23 H 1.300994 0.754178 0.660426 0.029 Uiso 1 1 calc R C24 C 1.1418(5) 0.6009(6) 0.5784(3) 0.0210(13) Uani 1 1 d . C25 C 0.9473(5) 0.4723(6) 0.5579(3) 0.0220(14) Uani 1 1 d . H25 H 0.919457 0.555497 0.591280 0.026 Uiso 1 1 calc R C26 C 0.9097(6) 0.3360(7) 0.6021(4) 0.0244(14) Uani 1 1 d . H26 H 0.934817 0.251800 0.568530 0.029 Uiso 1 1 calc R C27 C 0.7702(6) 0.3319(7) 0.6100(4) 0.0309(15) Uani 1 1 d . H27A H 0.746874 0.242805 0.637300 0.046 Uiso 1 1 calc GR H27B H 0.730888 0.336104 0.554971 0.046 Uiso 1 1 calc GR H27C H 0.744073 0.414034 0.642591 0.046 Uiso 1 1 calc GR C28 C 0.9726(6) 0.3251(7) 0.6869(4) 0.0302(15) Uani 1 1 d . H28A H 0.949237 0.407232 0.720582 0.045 Uiso 1 1 calc GR H28B H 1.061301 0.324891 0.681017 0.045 Uiso 1 1 calc GR H28C H 0.947624 0.236144 0.713701 0.045 Uiso 1 1 calc GR C29 C 0.8261(5) 0.6023(6) 0.4516(3) 0.0203(13) Uani 1 1 d . C30 C 0.7637(5) 0.5954(6) 0.3689(3) 0.0219(13) Uani 1 1 d . C31 C 0.8028(6) 0.5108(6) 0.3040(4) 0.0259(15) Uani 1 1 d . H31 H 0.874309 0.453875 0.311045 0.031 Uiso 1 1 calc R C32 C 0.7378(6) 0.5093(7) 0.2293(4) 0.0299(15) Uani 1 1 d . H32 H 0.765206 0.451412 0.185450 0.036 Uiso 1 1 calc R C33 C 0.6330(6) 0.5916(7) 0.2179(4) 0.0311(15) Uani 1 1 d . H33 H 0.588407 0.589195 0.166827 0.037 Uiso 1 1 calc R C34 C 0.5939(6) 0.6771(7) 0.2816(4) 0.0312(16) Uani 1 1 d . H34 H 0.522251 0.733513 0.273941 0.037 Uiso 1 1 calc R C35 C 0.6586(6) 0.6812(6) 0.3566(4) 0.0263(14) Uani 1 1 d . H35 H 0.632091 0.741635 0.399580 0.032 Uiso 1 1 calc R H2A H 1.116(7) 0.396(8) 0.543(4) 0.05(2) Uiso 1 1 d . H1 H 1.066(6) 0.429(8) 0.008(4) 0.04(2) Uiso 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 O1 0.027(2) 0.024(2) 0.015(2) -0.0001(17) 0.0020(17) -0.008(2) O2 0.020(2) 0.017(2) 0.019(2) -0.0032(17) 0.0023(16) -0.0012(16) O3 0.020(2) 0.018(2) 0.025(2) 0.0005(17) 0.0035(17) -0.0012(17) N1 0.023(3) 0.020(3) 0.017(3) 0.001(2) -0.002(2) -0.003(2) C1 0.028(3) 0.015(3) 0.016(3) -0.002(2) -0.003(3) 0.000(2) C2 0.035(4) 0.020(3) 0.019(3) 0.003(3) 0.004(3) -0.002(3) C3 0.040(4) 0.030(4) 0.016(3) 0.004(3) -0.002(3) -0.002(3) C4 0.032(4) 0.025(3) 0.026(4) -0.001(3) -0.005(3) -0.002(3) C5 0.036(4) 0.025(3) 0.023(4) 0.004(3) 0.000(3) -0.004(3) C6 0.031(4) 0.029(4) 0.015(3) 0.002(3) 0.000(3) -0.003(3) C7 0.025(3) 0.014(3) 0.016(3) 0.000(2) 0.002(2) 0.000(2) C8 0.028(4) 0.022(3) 0.014(3) -0.002(2) -0.003(2) -0.005(3) C9 0.034(4) 0.022(3) 0.018(3) 0.002(2) -0.003(3) 0.001(3) C10 0.037(4) 0.017(3) 0.030(4) 0.002(3) -0.004(3) 0.004(3) C11 0.036(4) 0.032(4) 0.028(4) 0.001(3) -0.008(3) 0.002(3) C12 0.027(4) 0.018(3) 0.014(3) 0.000(2) 0.003(2) -0.002(2) C13 0.035(4) 0.025(3) 0.032(4) -0.003(3) 0.003(3) -0.007(3) C14 0.029(4) 0.026(3) 0.030(4) 0.006(3) -0.001(3) -0.003(3) C15 0.028(4) 0.020(3) 0.024(4) -0.002(3) 0.001(3) -0.001(3) C16 0.029(4) 0.035(4) 0.029(4) -0.007(3) 0.008(3) 0.000(3) C17 0.029(4) 0.037(4) 0.027(4) 0.000(3) 0.001(3) 0.004(3) B1 0.024(4) 0.018(4) 0.013(4) -0.003(3) 0.000(3) -0.003(3) O4 0.037(3) 0.017(2) 0.020(2) -0.0011(18) 0.0001(18) -0.0010(19) O5 0.032(3) 0.016(2) 0.022(2) -0.0034(18) -0.0037(18) 0.0020(18) N2 0.025(3) 0.018(3) 0.025(3) -0.003(2) 0.000(2) 0.000(2) N3 0.029(3) 0.017(3) 0.021(3) -0.004(2) -0.005(2) -0.004(2) C18 0.030(4) 0.016(3) 0.018(3) 0.004(3) -0.001(3) -0.001(3) C19 0.039(4) 0.019(3) 0.015(3) -0.005(2) 0.002(3) -0.004(3) C20 0.036(4) 0.027(4) 0.031(4) -0.004(3) 0.009(3) 0.001(3) C21 0.031(4) 0.026(4) 0.035(4) 0.005(3) 0.003(3) -0.005(3) C22 0.033(4) 0.030(4) 0.025(4) 0.000(3) 0.000(3) -0.005(3) C23 0.030(4) 0.020(3) 0.023(4) -0.001(3) 0.000(3) 0.002(3) C24 0.034(4) 0.014(3) 0.015(3) -0.001(2) -0.004(3) -0.002(3) C25 0.025(4) 0.019(3) 0.022(4) -0.002(3) -0.002(3) 0.001(3) C26 0.028(4) 0.024(3) 0.022(3) 0.000(3) 0.005(3) 0.002(3) C27 0.032(4) 0.027(3) 0.034(4) 0.002(3) -0.001(3) -0.002(3) C28 0.034(4) 0.030(4) 0.026(4) 0.005(3) -0.002(3) 0.004(3) C29 0.028(3) 0.015(3) 0.019(3) 0.001(3) 0.003(3) -0.002(3) C30 0.030(4) 0.016(3) 0.020(3) 0.001(3) 0.001(3) -0.005(3) C31 0.037(4) 0.019(3) 0.022(4) -0.002(3) 0.002(3) 0.006(3) C32 0.044(4) 0.024(3) 0.021(4) -0.004(3) 0.001(3) 0.002(3) C33 0.038(4) 0.031(3) 0.024(4) 0.000(3) -0.006(3) -0.007(3) C34 0.036(4) 0.033(4) 0.024(4) 0.001(3) -0.006(3) 0.002(3) C35 0.032(4) 0.020(3) 0.027(4) 0.000(3) 0.001(3) -0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C7 O1 B1 109.5(4) B1 O2 C12 106.6(4) C15 O3 B1 109.6(4) C7 N1 C8 113.3(5) C2 C1 C6 120.4(5) C2 C1 C7 118.5(5) C6 C1 C7 121.1(5) C3 C2 C1 119.7(6) C4 C3 C2 120.0(6) C3 C4 C5 120.3(6) C6 C5 C4 120.4(6) C5 C6 C1 119.2(5) O1 C7 N1 115.9(5) O1 C7 C1 118.4(5) N1 C7 C1 125.6(5) N1 C8 C9 108.9(5) N1 C8 B1 102.0(4) C9 C8 B1 121.8(5) C10 C9 C8 112.3(5) C10 C9 C11 110.4(5) C11 C9 C8 110.5(5) O2 C12 C13 108.6(5) O2 C12 C14 109.9(5) O2 C12 C15 101.3(4) C13 C12 C15 114.3(5) C14 C12 C13 108.9(5) C14 C12 C15 113.5(5) O3 C15 C12 103.1(4) O3 C15 C16 108.4(5) O3 C15 C17 107.9(5) C16 C15 C12 115.1(5) C16 C15 C17 109.2(5) C17 C15 C12 112.8(5) O1 B1 C8 99.1(4) O2 B1 O1 106.0(5) O2 B1 C8 117.4(5) O3 B1 O1 107.2(4) O3 B1 O2 105.8(5) O3 B1 C8 119.9(5) C24 N2 C25 121.7(5) C29 N3 C25 122.3(5) C19 C18 C24 123.3(5) C23 C18 C19 119.9(6) C23 C18 C24 116.8(5) C20 C19 C18 119.3(6) C21 C20 C19 120.8(6) C20 C21 C22 120.3(6) C21 C22 C23 119.7(6) C18 C23 C22 120.1(6) O4 C24 N2 122.3(6) O4 C24 C18 120.3(5) N2 C24 C18 117.5(5) N2 C25 C26 111.4(5) N3 C25 N2 110.9(5) N3 C25 C26 111.8(5) C25 C26 C27 110.1(5) C25 C26 C28 111.1(5) C28 C26 C27 110.2(5) O5 C29 N3 122.2(5) O5 C29 C30 121.4(5) N3 C29 C30 116.4(5) C31 C30 C29 124.2(5) C31 C30 C35 118.9(5) C35 C30 C29 116.9(5) C32 C31 C30 120.3(6) C31 C32 C33 120.7(6) C34 C33 C32 119.6(6) C33 C34 C35 120.6(6) C34 C35 C30 120.0(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C7 1.290(7) O1 B1 1.614(7) O2 C12 1.458(7) O2 B1 1.451(7) O3 C15 1.445(7) O3 B1 1.449(8) N1 C7 1.308(8) N1 C8 1.488(8) C1 C2 1.393(8) C1 C6 1.393(9) C1 C7 1.477(8) C2 C3 1.386(9) C3 C4 1.382(9) C4 C5 1.386(9) C5 C6 1.385(8) C8 C9 1.537(8) C8 B1 1.631(9) C9 C10 1.524(8) C9 C11 1.526(8) C12 C13 1.513(8) C12 C14 1.511(8) C12 C15 1.555(8) C15 C16 1.519(8) C15 C17 1.524(8) O4 C24 1.238(7) O5 C29 1.234(7) N2 C24 1.353(7) N2 C25 1.463(8) N3 C25 1.461(7) N3 C29 1.353(7) C18 C19 1.394(8) C18 C23 1.390(8) C18 C24 1.497(9) C19 C20 1.391(9) C20 C21 1.377(9) C21 C22 1.379(9) C22 C23 1.400(9) C25 C26 1.523(8) C26 C27 1.539(9) C26 C28 1.524(8) C29 C30 1.489(8) C30 C31 1.395(8) C30 C35 1.411(8) C31 C32 1.388(9) C32 C33 1.389(9) C33 C34 1.384(9) C34 C35 1.391(9) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N2 H2A O5 0.92(8) 1.99(8) 2.895(6) 171(7) 2_746 yes N1 H1 O2 0.86(7) 2.00(8) 2.855(7) 174(7) 2_755 yes