#------------------------------------------------------------------------------ #$Date: 2018-02-13 09:20:21 +0200 (Tue, 13 Feb 2018) $ #$Revision: 206397 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/01/7230136.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_7230136 loop_ _publ_author_name 'Filatov, Mikhail A.' 'Karuthedath, Safakath' 'Polestshuk, Pavel M.' 'Callaghan, Susan' 'Flanagan, Keith' 'Telitchko, Maxime' 'Wiesner, Thomas' 'Laquai, Fr\'ed\'eric' 'Senge, Mathias O.' _publ_section_title ; Control of triplet state generation in heavy atom-free BODIPY-anthracene dyads by media polarity and structural factors ; _journal_name_full 'Physical Chemistry Chemical Physics' _journal_paper_doi 10.1039/C7CP08472B _journal_year 2018 _chemical_formula_moiety 'C32 H33 B F2 N2' _chemical_formula_sum 'C32 H33 B F2 N2' _chemical_formula_weight 494.41 _chemical_name_systematic 2,6-Diethyl-1,3,5,7-tetramethyl-8-(10-methylanthracen-9-yl)-4,4-difluoro-4-bora-3a,4a-diaza-s-indacene _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-10-05 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2017-11-12 deposited with the CCDC. 2018-02-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.878(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.836(6) _cell_length_b 20.573(7) _cell_length_c 7.781(3) _cell_measurement_reflns_used 7289 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.07 _cell_measurement_theta_min 2.37 _cell_volume 2480.7(16) _computing_data_collection 'APEX 3 (Bruker, 2016) ' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'Kappa diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1328 _diffrn_reflns_av_unetI/netI 0.0715 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 58475 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.500 _diffrn_reflns_theta_max 25.500 _diffrn_reflns_theta_min 1.645 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6215 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1266 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.8339. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 1048 _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of DCM and methanol by slow evaporation' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.186 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 341 _refine_ls_number_reflns 4627 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0483 _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^)+(0.0543P)^2^+0.0763P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0937 _refine_ls_wR_factor_ref 0.1125 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2793 _reflns_number_total 4627 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cp08472b2.cif _cod_data_source_block kjf145_a _cod_original_cell_volume 2480.7(15) _cod_database_code 7230136 _shelx_shelxl_version_number 2014/7 _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 0.996 _shelx_estimated_absorpt_t_min 0.950 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C31(H31A,H31B), C35(H35A,H35B) 2.b Aromatic/amide H refined with riding coordinates: C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27) 2.c Idealised Me refined as rotating group: C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C37(H37A,H37B, H37C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C29(H29A,H29B,H29C) ; _shelx_res_file ; kjf145_a.res created by SHELXL-2014/7 TITL kjf145_a.res in P2(1)/c REM Old TITL kjf145 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.172, Rweak 0.020, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C24 B N2 F2 CELL 0.71073 15.8356 20.5725 7.7813 90 101.878 90 ZERR 4 0.0055 0.0069 0.0026 0 0.008 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F N UNIT 128 132 4 8 8 L.S. 10 PLAN 20 SIZE 0.05 0.05 0.6 TEMP -173.15 HTAB C33 F14 BOND $H HTAB MORE -1 CONF fmap 2 acta 52 OMIT -2 51 OMIT 1 0 0 REM REM REM WGHT 0.054300 0.076300 FVAR 0.41750 N10 5 0.753297 0.591203 0.821054 11.00000 0.02147 0.01300 = 0.02346 -0.00149 0.00143 0.00093 C3 1 0.726266 0.616963 0.956419 11.00000 0.01828 0.01839 = 0.02574 -0.00045 -0.00144 0.00383 C2 1 0.678045 0.571574 1.028511 11.00000 0.02188 0.01967 = 0.02264 0.00100 -0.00001 0.00493 C1 1 0.677788 0.515319 0.934259 11.00000 0.02008 0.01816 = 0.02111 0.00137 -0.00036 0.00202 C9 1 0.724965 0.527320 0.802647 11.00000 0.01870 0.01403 = 0.02238 -0.00081 -0.00042 0.00055 C8 1 0.745352 0.488904 0.670912 11.00000 0.01596 0.01587 = 0.02219 0.00068 -0.00332 0.00237 C12 1 0.790934 0.513946 0.552614 11.00000 0.01873 0.01346 = 0.02432 -0.00009 0.00158 -0.00133 C7 1 0.818388 0.486064 0.409633 11.00000 0.01964 0.01947 = 0.02304 -0.00005 0.00145 0.00080 C6 1 0.862281 0.533135 0.338253 11.00000 0.01924 0.01999 = 0.02402 0.00121 0.00112 0.00077 C5 1 0.863001 0.588547 0.440089 11.00000 0.01794 0.01985 = 0.02630 0.00489 0.00110 0.00122 N11 5 0.819634 0.577680 0.567041 11.00000 0.01830 0.01482 = 0.02489 0.00259 0.00128 -0.00029 B4 3 0.804991 0.626068 0.705530 11.00000 0.02169 0.01574 = 0.02918 0.00012 0.00139 -0.00016 F13 4 0.759676 0.678611 0.627666 11.00000 0.04502 0.01668 = 0.04445 0.00824 0.01664 0.00731 F14 4 0.883115 0.646504 0.804653 11.00000 0.02753 0.03326 = 0.04165 -0.01469 0.00834 -0.01220 C33 1 0.746243 0.684580 1.013897 11.00000 0.03443 0.01894 = 0.03580 -0.00676 0.00605 -0.00212 AFIX 137 H33A 2 0.805436 0.695088 1.004149 11.00000 -1.50000 H33B 2 0.740572 0.689407 1.136306 11.00000 -1.50000 H33C 2 0.705990 0.714157 0.939412 11.00000 -1.50000 AFIX 0 C31 1 0.635992 0.584973 1.177477 11.00000 0.03369 0.02303 = 0.02674 -0.00007 0.00794 0.00247 AFIX 23 H31A 2 0.680377 0.599692 1.278889 11.00000 -1.20000 H31B 2 0.611011 0.544030 1.211675 11.00000 -1.20000 AFIX 0 C32 1 0.565787 0.635530 1.138733 11.00000 0.02892 0.03561 = 0.04145 -0.00055 0.01030 0.00373 AFIX 137 H32A 2 0.522942 0.622505 1.034789 11.00000 -1.50000 H32B 2 0.590914 0.677473 1.116688 11.00000 -1.50000 H32C 2 0.537845 0.639491 1.239526 11.00000 -1.50000 AFIX 0 C30 1 0.633658 0.454108 0.962964 11.00000 0.03368 0.02047 = 0.02997 0.00337 0.00888 0.00053 AFIX 137 H30A 2 0.586156 0.446024 0.862719 11.00000 -1.50000 H30B 2 0.610741 0.457733 1.070355 11.00000 -1.50000 H30C 2 0.674841 0.418014 0.974835 11.00000 -1.50000 AFIX 0 C37 1 0.804722 0.418627 0.343162 11.00000 0.03117 0.02352 = 0.02820 -0.00541 0.00784 -0.00404 AFIX 137 H37A 2 0.840116 0.388798 0.426351 11.00000 -1.50000 H37B 2 0.821300 0.415395 0.228868 11.00000 -1.50000 H37C 2 0.743705 0.407060 0.330277 11.00000 -1.50000 AFIX 0 C35 1 0.905323 0.524858 0.188484 11.00000 0.02555 0.02243 = 0.02539 0.00038 0.00324 -0.00170 AFIX 23 H35A 2 0.918807 0.568136 0.145410 11.00000 -1.20000 H35B 2 0.865617 0.502469 0.091659 11.00000 -1.20000 AFIX 0 C36 1 0.987604 0.485933 0.239106 11.00000 0.02471 0.03221 = 0.02819 0.00167 0.00300 0.00084 AFIX 137 H36A 2 1.013254 0.479966 0.135818 11.00000 -1.50000 H36B 2 0.974612 0.443379 0.284005 11.00000 -1.50000 H36C 2 1.028316 0.509208 0.330331 11.00000 -1.50000 AFIX 0 C34 1 0.906221 0.651194 0.424297 11.00000 0.03094 0.02114 = 0.03642 0.00373 0.00899 -0.00549 AFIX 137 H34A 2 0.863939 0.686507 0.413999 11.00000 -1.50000 H34B 2 0.931639 0.650506 0.319636 11.00000 -1.50000 H34C 2 0.951777 0.658159 0.528770 11.00000 -1.50000 AFIX 0 C15 1 0.721786 0.419124 0.659657 11.00000 0.01938 0.01370 = 0.01977 0.00042 0.00416 -0.00009 C16 1 0.643420 0.398451 0.561025 11.00000 0.02209 0.01448 = 0.01960 -0.00071 0.00512 -0.00072 C17 1 0.582956 0.442767 0.467849 11.00000 0.02500 0.01910 = 0.02364 0.00015 0.00456 0.00168 AFIX 43 H17 2 0.596594 0.487784 0.472041 11.00000 -1.20000 AFIX 0 C18 1 0.506482 0.422946 0.373206 11.00000 0.02268 0.02954 = 0.02579 -0.00156 0.00001 0.00585 AFIX 43 H18 2 0.467347 0.453807 0.310188 11.00000 -1.20000 AFIX 0 C19 1 0.484431 0.357262 0.367247 11.00000 0.02007 0.03418 = 0.02873 -0.00611 -0.00012 -0.00487 AFIX 43 H19 2 0.429566 0.343614 0.303470 11.00000 -1.20000 AFIX 0 C20 1 0.540532 0.313411 0.451353 11.00000 0.02551 0.02141 = 0.02972 -0.00351 0.00474 -0.00604 AFIX 43 H20 2 0.524448 0.268855 0.446140 11.00000 -1.20000 AFIX 0 C21 1 0.623062 0.331340 0.547808 11.00000 0.02308 0.01809 = 0.02086 -0.00107 0.00641 -0.00211 C22 1 0.683351 0.285690 0.628020 11.00000 0.02564 0.01553 = 0.02145 -0.00146 0.00865 -0.00219 C23 1 0.761662 0.306679 0.730118 11.00000 0.02630 0.01446 = 0.01918 -0.00048 0.00745 0.00112 C24 1 0.823693 0.262923 0.821637 11.00000 0.03184 0.01433 = 0.03327 0.00297 0.00649 0.00397 AFIX 43 H24 2 0.812044 0.217612 0.812724 11.00000 -1.20000 AFIX 0 C25 1 0.898640 0.283344 0.920885 11.00000 0.02956 0.02454 = 0.03394 0.00347 0.00040 0.01046 AFIX 43 H25 2 0.938491 0.252574 0.982174 11.00000 -1.20000 AFIX 0 C26 1 0.918290 0.349518 0.934463 11.00000 0.02145 0.02729 = 0.02836 -0.00153 -0.00012 0.00146 AFIX 43 H26 2 0.971716 0.363692 1.003538 11.00000 -1.20000 AFIX 0 C27 1 0.861618 0.393054 0.849828 11.00000 0.02340 0.01767 = 0.02399 -0.00069 0.00282 -0.00097 AFIX 43 H27 2 0.875815 0.437954 0.859574 11.00000 -1.20000 AFIX 0 C28 1 0.781244 0.373891 0.746405 11.00000 0.02040 0.01836 = 0.02023 -0.00176 0.00495 0.00022 C29 1 0.665338 0.214754 0.604289 11.00000 0.03720 0.01982 = 0.03329 0.00080 0.00609 -0.00496 AFIX 137 H29A 2 0.638389 0.198952 0.699000 11.00000 -1.50000 H29B 2 0.719540 0.191360 0.607390 11.00000 -1.50000 H29C 2 0.626246 0.207329 0.490881 11.00000 -1.50000 AFIX 0 HKLF 4 REM kjf145_a.res in P2(1)/c REM R1 = 0.0483 for 2793 Fo > 4sig(Fo) and 0.1076 for all 4627 data REM 341 parameters refined using 0 restraints END WGHT 0.0543 0.0763 REM Instructions for potential hydrogen bonds HTAB C33 F14 HTAB C34 F13 REM Highest difference peak 0.186, deepest hole -0.230, 1-sigma level 0.049 Q1 1 0.7186 0.5128 0.7064 11.00000 0.05 0.19 Q2 1 0.6707 0.2072 0.4660 11.00000 0.05 0.18 Q3 1 0.6504 0.5577 0.9476 11.00000 0.05 0.18 Q4 1 0.6894 0.6049 0.9751 11.00000 0.05 0.17 Q5 1 0.5729 0.4910 1.2113 11.00000 0.05 0.17 Q6 1 0.7103 0.7395 1.0383 11.00000 0.05 0.16 Q7 1 0.9613 0.6647 0.7445 11.00000 0.05 0.16 Q8 1 0.7884 0.3823 0.8364 11.00000 0.05 0.15 Q9 1 0.8490 0.6915 0.8419 11.00000 0.05 0.15 Q10 1 0.8050 0.6097 0.5983 11.00000 0.05 0.15 Q11 1 0.7429 0.4043 0.2765 11.00000 0.05 0.15 Q12 1 0.5240 0.4804 1.1006 11.00000 0.05 0.15 Q13 1 0.8935 0.3623 0.3447 11.00000 0.05 0.15 Q14 1 0.8746 0.3633 0.4668 11.00000 0.05 0.15 Q15 1 1.0131 0.6379 0.4973 11.00000 0.05 0.15 Q16 1 0.7588 0.7154 0.9436 11.00000 0.05 0.15 Q17 1 0.6700 0.3840 0.9179 11.00000 0.05 0.15 Q18 1 0.9498 0.5627 0.1007 11.00000 0.05 0.15 Q19 1 0.7601 0.3381 0.9054 11.00000 0.05 0.14 Q20 1 0.8607 0.3537 1.0692 11.00000 0.05 0.14 ; _shelx_res_checksum 4089 _shelx_hkl_file ; 0 0 -1 -3.40 5.30 0 0 -1 8.20 6.80 0 0 -1 -2.20 7.60 0 0 -1 -1.00 4.40 0 0 -1 -3.00 5.60 0 0 -1 4.20 7.40 0 0 -1 -3.70 4.30 0 0 -1 -3.00 1.40 0 0 -1 -8.10 3.80 0 0 -1 0.40 4.40 0 0 1 -0.50 5.30 0 0 1 -4.40 5.50 0 0 1 -1.40 4.50 0 0 1 -1.00 7.80 0 0 1 1.00 3.30 0 0 1 7.70 5.00 0 0 1 3.50 4.70 0 0 1 -11.30 6.80 0 0 -2 145.09 11.10 0 0 -2 154.78 14.50 0 0 -2 158.88 18.30 0 0 -2 134.49 11.70 0 0 -2 178.98 18.10 0 0 -2 158.78 12.80 0 0 -2 195.58 14.30 0 0 2 197.88 22.90 0 0 2 151.58 12.40 0 0 2 139.79 12.50 0 0 2 169.98 14.20 0 0 2 174.38 24.40 0 0 2 141.99 11.90 0 0 2 154.88 14.90 0 0 2 147.49 11.50 0 0 -3 -1.00 8.10 0 0 -3 -4.70 10.10 0 0 -3 6.40 14.10 0 0 -3 0.80 8.30 0 0 -3 -11.90 8.90 0 0 3 8.10 17.00 0 0 3 19.40 14.20 0 0 3 -5.50 9.60 0 0 3 4.20 7.30 0 0 3 -6.30 9.90 0 0 3 -1.20 10.40 0 0 -4 204.58 17.50 0 0 -4 189.48 15.10 0 0 -4 218.18 18.40 0 0 -4 160.68 14.10 0 0 -4 196.18 22.60 0 0 4 166.78 16.50 0 0 4 253.57 33.90 0 0 4 182.88 12.90 0 0 4 220.68 24.30 0 0 4 221.38 17.20 0 0 4 202.38 17.40 0 0 -5 -4.50 9.00 0 0 -5 -0.60 9.50 0 0 -5 2.70 10.30 0 0 -5 8.40 16.30 0 0 -5 -9.60 8.60 0 0 5 -0.90 10.80 0 0 5 22.10 22.60 0 0 5 -41.10 21.90 0 0 5 -3.30 11.60 0 0 5 -2.70 11.10 0 0 5 -6.70 16.80 0 0 5 -10.00 6.90 0 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5 5 53.69 33.00 8 5 5 17.10 57.59 -8 -5 -6 4.50 12.80 -8 -5 -6 3.50 16.10 -8 -5 -6 8.90 14.60 8 5 6 15.10 25.20 8 5 6 -27.50 32.70 8 5 6 23.90 15.40 -8 -5 -7 -1.70 12.50 -8 -5 -7 -17.70 21.60 -8 -5 -7 -7.10 16.80 8 5 7 -30.40 26.00 8 5 7 7.40 19.40 8 5 7 41.00 41.10 -9 -5 9 6.70 16.20 9 5 -9 9.10 20.00 9 5 -9 43.90 27.50 -9 -5 8 47.10 15.70 -9 -5 8 16.70 15.30 9 5 -8 4.50 24.90 9 5 -8 -3.20 19.50 9 5 -8 45.90 15.90 -9 -5 7 98.99 16.10 -9 -5 7 106.49 18.70 -9 -5 7 101.19 17.10 9 5 -7 71.19 20.00 9 5 -7 85.19 19.10 9 5 -7 73.39 23.70 -9 -5 6 38.60 15.60 -9 -5 6 55.59 14.70 -9 -5 6 81.99 16.00 9 5 -6 72.09 15.40 9 5 -6 70.29 25.30 9 5 -6 53.99 16.80 -9 -5 5 0.90 12.40 -9 -5 5 28.20 13.10 9 5 -5 14.70 11.60 9 5 -5 32.50 16.70 9 5 -5 21.00 17.40 9 5 -5 23.10 13.10 -9 -5 4 152.08 15.00 -9 -5 4 154.98 15.90 -9 -5 4 163.68 14.80 9 5 -4 158.08 17.50 9 5 -4 203.58 24.10 9 5 -4 148.69 15.80 9 5 -4 141.99 22.80 9 5 -4 119.79 20.00 -9 -5 3 7.20 8.20 -9 -5 3 -5.70 6.50 -9 -5 3 -4.40 9.00 -9 -5 3 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11 5 -1 6.10 17.60 11 5 -1 10.00 11.70 11 5 -1 3.20 8.50 11 5 -1 -4.30 11.60 -11 -5 0 10.40 5.50 -11 -5 0 -0.60 8.30 -11 -5 0 21.20 10.20 -11 -5 0 7.10 8.90 11 5 0 -23.40 40.90 11 5 0 -15.00 11.50 11 5 0 17.00 11.90 -11 -5 -1 50.19 11.90 -11 -5 -1 68.09 9.00 -11 -5 -1 63.99 7.20 -11 -5 -1 58.29 9.60 11 5 1 86.49 46.00 11 5 1 61.19 13.70 11 5 1 50.59 13.10 11 5 1 60.29 13.20 -11 -5 -2 15.90 10.40 -11 -5 -2 -5.50 9.40 11 5 2 26.80 13.40 11 5 2 9.10 10.60 11 5 2 27.90 16.30 -11 -5 -3 254.07 19.50 -11 -5 -3 256.67 19.90 -11 -5 -3 245.58 22.20 11 5 3 260.77 23.60 11 5 3 256.17 29.10 -11 -5 -4 20.60 10.60 -11 -5 -4 13.30 15.40 -11 -5 -4 -8.40 9.90 11 5 4 26.10 21.60 11 5 4 18.80 18.30 -11 -5 -5 -6.70 13.70 -11 -5 -5 34.80 12.20 -11 -5 -5 20.80 17.70 11 5 5 -9.50 18.70 11 5 5 52.49 32.30 11 5 5 17.70 23.60 -11 -5 -6 6.30 19.00 -11 -5 -6 2.90 11.80 -11 -5 -6 20.20 12.90 11 5 6 -12.10 24.90 11 5 6 19.10 16.50 -12 -5 8 -12.00 16.40 -12 -5 8 24.00 19.40 12 5 -8 24.10 19.50 12 5 -8 21.30 24.80 12 5 -8 -14.40 17.00 12 5 -8 14.70 20.20 -12 -5 7 12.50 13.30 -12 -5 7 -12.80 16.90 -12 -5 7 4.10 14.20 12 5 -7 34.50 20.30 12 5 -7 29.90 18.90 12 5 -7 -15.90 21.80 -12 -5 6 3.50 12.40 -12 -5 6 -2.70 15.00 12 5 -6 10.40 14.10 12 5 -6 -29.10 23.40 12 5 -6 1.60 15.30 -12 -5 5 155.98 15.90 -12 -5 5 159.78 18.30 12 5 -5 143.99 19.20 12 5 -5 138.29 27.60 12 5 -5 189.08 18.80 12 5 -5 178.28 24.50 -12 -5 4 7.20 10.70 -12 -5 4 3.00 12.70 -12 -5 4 -1.40 13.40 12 5 -4 1.40 13.70 12 5 -4 76.29 23.30 12 5 -4 11.80 17.80 12 5 -4 5.20 14.70 -12 -5 3 -1.90 9.80 -12 -5 3 6.90 12.50 -12 -5 3 -6.70 11.20 12 5 -3 -12.20 13.40 12 5 -3 -0.10 12.20 12 5 -3 12.40 28.90 12 5 -3 -11.40 15.90 12 5 -3 -0.30 19.40 -12 -5 2 11.30 10.10 -12 -5 2 3.90 7.60 -12 -5 2 4.50 9.60 12 5 -2 -0.30 12.60 12 5 -2 22.20 14.20 12 5 -2 26.00 30.40 12 5 -2 6.00 15.90 -12 -5 1 4.10 9.10 -12 -5 1 14.40 11.20 -12 -5 1 -6.20 5.80 -12 -5 1 17.70 9.60 12 5 -1 12.50 8.20 12 5 -1 -2.60 12.60 12 5 -1 21.30 12.90 12 5 -1 -0.20 44.90 -12 -5 0 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293.67 19.10 -9 -6 0 291.87 17.20 -9 -6 0 273.17 13.80 9 6 0 286.37 20.20 9 6 0 296.27 18.30 9 6 0 331.57 22.60 9 6 0 295.97 41.70 9 6 0 278.27 37.70 -9 -6 -1 77.19 9.00 -9 -6 -1 66.69 9.50 9 6 1 51.49 9.90 9 6 1 48.60 11.90 9 6 1 49.60 38.80 9 6 1 31.00 13.00 -9 -6 -2 38.30 8.90 -9 -6 -2 25.60 8.90 -9 -6 -2 44.50 9.10 9 6 2 84.79 42.40 9 6 2 34.70 12.40 9 6 2 32.90 10.30 9 6 2 44.30 16.30 -9 -6 -3 44.70 12.30 -9 -6 -3 52.69 12.00 -9 -6 -3 36.70 9.80 -9 -6 -3 48.90 12.70 9 6 3 43.50 13.40 9 6 3 35.30 19.70 9 6 3 40.00 11.60 9 6 3 29.50 46.10 -9 -6 -4 48.40 16.80 -9 -6 -4 47.40 13.40 -9 -6 -4 12.10 12.50 9 6 4 23.00 17.40 9 6 4 -5.30 31.70 9 6 4 -11.00 21.40 -9 -6 -5 29.90 18.10 -9 -6 -5 5.00 11.90 -9 -6 -5 14.60 13.50 9 6 5 -3.10 24.10 9 6 5 -9.60 14.20 9 6 5 -22.10 40.10 -9 -6 -6 9.90 12.00 -9 -6 -6 5.50 19.80 -9 -6 -6 8.90 15.70 9 6 6 -11.10 25.40 9 6 6 26.40 19.80 9 6 6 20.70 41.70 -9 -6 -7 -23.40 14.80 -9 -6 -7 -1.70 13.40 -9 -6 -7 -4.90 16.90 9 6 7 -51.19 42.70 9 6 7 -9.80 27.00 9 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39.50 13.90 16 -10 -1 27.60 17.70 16 -10 -1 -2.20 25.70 -16 10 1 5.40 13.60 -16 10 1 5.20 14.00 -16 10 1 -8.90 14.00 16 -10 -2 27.70 22.90 16 -10 -2 -1.80 16.10 -16 10 2 18.80 12.00 -16 10 2 8.00 14.80 -16 10 2 -7.00 11.60 16 -10 -3 28.70 24.40 16 -10 -3 39.80 19.60 -16 10 3 19.30 13.00 -16 10 3 24.30 15.60 -16 10 3 26.00 13.60 16 -10 -4 13.10 24.20 -16 10 4 -18.00 13.40 -16 10 4 31.00 25.10 -16 10 4 1.10 17.10 -16 10 4 -9.30 13.70 15 -10 1 9.50 19.10 -15 10 -1 5.50 13.50 -15 10 -1 21.70 12.50 -15 10 -1 20.70 12.70 15 -10 0 47.20 18.60 15 -10 0 66.19 47.50 15 -10 0 48.10 19.70 -15 10 0 23.10 13.10 -15 10 0 16.20 11.10 -15 10 0 19.30 13.00 15 -10 -1 45.80 43.20 15 -10 -1 129.39 20.30 15 -10 -1 118.99 23.30 -15 10 1 77.49 15.10 -15 10 1 99.39 13.50 -15 10 1 61.19 15.20 15 -10 -2 -3.70 26.40 15 -10 -2 51.89 41.30 15 -10 -2 15.00 16.40 -15 10 2 17.30 14.30 -15 10 2 11.20 13.80 -15 10 2 13.40 11.80 15 -10 -3 23.80 22.90 15 -10 -3 23.30 18.90 15 -10 -3 6.90 17.70 -15 10 3 10.90 12.30 -15 10 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14.90 12 -14 -3 66.49 27.20 12 -14 -3 68.19 47.50 -12 14 3 45.50 12.20 -12 14 3 87.09 27.80 -12 14 3 59.79 14.60 -12 14 3 45.00 15.90 12 -14 -4 62.39 23.30 11 -14 2 50.89 20.60 11 -14 2 49.20 15.80 11 -14 1 40.30 19.10 11 -14 1 30.20 14.00 11 -14 1 5.20 45.00 -11 14 -1 9.90 10.90 -11 14 -1 38.20 10.30 11 -14 0 -0.20 42.30 11 -14 0 36.90 19.10 11 -14 0 -1.70 17.00 -11 14 0 -0.90 10.60 -11 14 0 2.20 10.00 11 -14 -1 93.09 19.40 11 -14 -1 130.69 23.90 11 -14 -1 75.39 44.20 -11 14 1 102.19 12.40 -11 14 1 110.79 12.80 -11 14 1 102.09 13.40 11 -14 -2 12.20 16.50 11 -14 -2 28.20 19.60 11 -14 -2 59.89 43.40 -11 14 2 25.00 13.60 -11 14 2 2.00 11.60 -11 14 2 -28.40 21.00 -11 14 2 10.70 11.10 11 -14 -3 17.40 20.10 11 -14 -3 -48.30 44.10 -11 14 3 19.90 11.10 -11 14 3 16.90 12.00 -11 14 3 4.00 25.20 -11 14 3 -0.50 13.20 11 -14 -4 70.99 45.60 11 -14 -4 119.49 24.30 -11 14 4 88.29 28.10 -11 14 4 111.89 16.00 -11 14 4 86.09 14.50 -11 14 4 92.09 16.90 11 -14 -7 53.99 29.70 -11 14 7 16.50 22.30 -11 14 7 7.80 23.30 -11 14 7 61.69 17.20 10 -14 5 -4.50 25.90 10 -14 5 33.60 16.70 10 -14 2 17.10 12.70 10 -14 2 8.50 18.70 10 -14 2 98.69 53.39 -10 14 -2 12.60 10.90 -10 14 -2 8.70 8.90 10 -14 1 24.60 18.10 10 -14 1 25.10 13.60 10 -14 1 -23.10 51.59 -10 14 -1 16.50 9.10 -10 14 -1 17.70 12.70 10 -14 0 391.66 53.89 10 -14 0 397.06 30.50 10 -14 0 379.56 37.40 -10 14 0 364.36 22.40 -10 14 0 407.46 25.90 -10 14 0 390.16 23.60 10 -14 -1 22.20 16.30 10 -14 -1 51.99 41.00 10 -14 -1 35.00 21.00 -10 14 1 27.80 11.50 -10 14 1 18.00 9.50 -10 14 1 14.00 10.60 10 -14 -2 25.60 19.00 10 -14 -2 34.70 41.50 10 -14 -2 21.80 15.80 -10 14 2 3.40 12.70 -10 14 2 11.70 10.70 -10 14 2 4.70 13.10 -10 14 2 5.10 25.40 10 -14 -3 8.50 24.30 10 -14 -3 33.80 51.69 -10 14 3 5.40 24.40 -10 14 3 -7.00 12.30 -10 14 3 4.00 11.50 -10 14 3 9.80 12.60 10 -14 -4 40.10 44.80 10 -14 -4 72.29 22.80 -10 14 4 89.79 17.60 -10 14 4 58.59 15.40 -10 14 4 83.19 27.20 -10 14 4 96.39 16.40 10 -14 -6 53.39 23.80 -10 14 6 22.30 16.10 -10 14 6 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-5 -23 1 104.09 16.80 5 23 -1 81.69 10.30 -5 -23 0 6.50 13.90 5 23 0 29.20 9.10 -5 -23 -1 2.90 11.40 5 23 1 19.70 10.10 5 23 1 10.90 24.80 -5 -23 -2 -4.30 13.70 -5 -23 -2 -39.60 21.50 5 23 2 0.30 10.40 5 23 2 0.10 34.00 5 23 3 1.40 12.20 -6 -23 3 4.90 13.60 -6 -23 3 15.30 14.50 6 23 -3 44.40 21.70 6 23 -3 -1.20 9.60 -6 -23 2 -2.90 13.10 6 23 -2 12.90 8.90 -6 -23 1 8.10 17.30 -6 -23 1 17.70 12.60 6 23 -1 3.80 8.70 -6 -23 0 5.60 16.00 -6 -23 0 16.00 14.60 6 23 0 12.90 9.70 -6 -23 -1 28.30 12.10 6 23 1 20.20 11.10 6 23 1 15.80 31.80 -6 -23 -2 30.60 14.90 6 23 2 -5.10 12.80 6 23 2 18.00 35.60 -7 -23 3 7.60 19.40 -7 -23 3 0.40 17.90 7 23 -3 41.20 27.10 7 23 -3 -1.70 10.20 -7 -23 2 -0.80 16.00 7 23 -2 46.70 23.00 7 23 -2 2.10 9.00 -7 -23 1 71.49 14.10 7 23 -1 42.10 10.80 -7 -23 0 0.60 12.20 -7 -23 0 10.50 16.40 7 23 0 19.90 9.70 -7 -23 -1 -10.00 11.50 7 23 1 -15.00 39.00 7 23 1 2.70 10.70 -8 -23 2 -9.20 16.40 8 23 -2 7.90 10.40 8 23 -2 55.29 24.00 -8 -23 1 -27.20 14.80 -8 -23 1 5.10 17.60 8 23 -1 -3.80 10.80 -8 -23 0 48.70 13.60 -8 -23 0 30.70 16.70 8 23 0 36.60 12.70 8 23 1 7.20 11.30 -7 24 0 17.30 13.80 -7 24 1 11.30 12.00 -7 24 1 15.90 7.30 6 -24 1 24.40 22.80 -6 24 -1 -5.40 13.00 -6 24 -1 15.60 26.80 6 -24 -2 5.50 20.80 -6 24 2 12.90 31.40 -6 24 2 10.90 14.90 -6 24 2 33.80 9.50 -5 24 3 9.10 15.90 -5 24 3 23.40 12.00 4 -24 2 -0.60 21.80 4 -24 2 24.80 17.00 -4 24 -2 13.00 23.10 -4 24 -2 -22.90 10.70 4 -24 -1 33.20 18.80 -4 24 1 8.00 23.70 -4 24 1 -3.70 16.60 -4 24 1 19.80 6.80 4 -24 -2 88.79 21.90 -4 24 2 47.20 32.80 -4 24 2 54.89 9.70 4 -24 -3 11.60 21.00 -4 24 3 5.80 10.60 -4 24 3 -0.50 27.20 3 -24 -1 50.09 21.90 -3 24 1 44.00 7.30 -3 24 1 56.29 30.90 3 -24 -2 22.80 20.30 -3 24 2 6.70 25.30 -3 24 2 11.40 9.00 3 -24 -3 -15.70 20.70 -3 24 3 17.30 33.20 -3 24 3 3.60 10.70 2 -24 3 22.40 17.60 2 -24 0 26.20 17.10 -2 24 0 38.80 27.20 2 -24 -1 14.90 17.60 -2 24 1 28.80 6.90 -2 24 1 2.30 23.40 2 -24 -2 47.90 23.90 -2 24 2 17.70 31.60 -2 24 2 20.00 9.60 2 -24 -3 -35.70 24.40 -2 24 3 4.30 10.70 -2 24 3 -31.40 26.90 1 -24 3 5.20 14.00 -1 24 -3 32.60 22.80 1 -24 2 46.60 14.60 -1 24 -2 100.99 22.80 1 -24 1 8.80 15.20 -1 24 -1 64.19 18.20 -1 24 -1 28.00 24.10 1 -24 0 17.30 20.30 -1 24 0 -1.50 26.10 1 -24 -1 21.40 22.50 -1 24 1 29.40 7.70 -1 24 1 9.70 24.00 1 -24 -2 6.90 18.90 -1 24 2 -4.50 9.50 -1 24 2 55.49 27.50 1 -24 -3 8.20 19.90 -1 24 3 13.20 11.40 -1 24 3 8.80 35.10 0 -24 3 -39.60 12.80 0 24 -3 44.00 23.00 0 -24 2 22.70 13.60 0 24 -2 39.50 22.90 0 -24 1 36.10 19.00 0 24 -1 60.69 19.20 0 24 -1 39.80 24.00 0 -24 0 17.00 16.80 0 24 0 24.00 26.30 0 24 0 5.70 5.30 0 -24 -1 59.99 19.30 0 24 1 39.50 7.90 0 24 1 19.90 29.80 0 -24 -2 6.70 22.60 0 24 2 8.70 26.30 0 24 2 7.90 10.30 0 -24 -3 18.90 24.70 0 24 3 4.50 11.40 0 24 3 8.70 28.90 -1 -24 3 14.40 17.00 1 24 -3 93.09 24.80 -1 -24 2 -2.40 15.30 1 24 -2 37.20 23.70 -1 -24 1 19.70 15.70 -1 -24 1 8.70 16.40 1 24 -1 1.70 27.70 -1 -24 0 11.70 12.90 -1 -24 0 12.10 16.70 1 24 0 30.50 27.20 1 24 0 2.80 6.20 -1 -24 -1 -3.60 18.00 -1 -24 -1 26.50 12.50 1 24 1 34.50 8.40 1 24 1 -12.90 28.60 -1 -24 -2 43.80 13.20 -1 -24 -2 69.39 21.20 1 24 2 51.29 33.80 1 24 2 57.99 10.70 -1 -24 -3 30.10 20.20 -1 -24 -3 12.10 12.80 1 24 3 19.80 12.10 1 24 3 18.80 28.90 -2 -24 3 6.60 15.90 -2 -24 3 24.40 13.80 2 24 -3 30.00 23.90 -2 -24 2 -9.20 14.90 -2 -24 1 20.60 14.10 2 24 -1 11.10 5.00 -2 -24 0 21.80 13.60 -2 -24 0 32.20 17.50 2 24 0 45.00 7.60 2 24 0 27.00 27.30 -2 -24 -1 -2.50 17.80 -2 -24 -1 13.40 12.70 2 24 1 32.60 30.10 2 24 1 -7.00 7.70 -2 -24 -2 27.90 19.90 -2 -24 -2 8.20 10.60 2 24 2 14.00 10.30 2 24 2 28.60 33.30 -2 -24 -3 -27.50 24.30 2 24 3 -0.10 12.50 2 24 3 43.40 36.30 -3 -24 3 7.20 12.70 -3 -24 3 -8.70 13.40 3 24 -3 29.90 20.40 -3 -24 2 -4.70 15.20 3 24 -2 19.40 19.70 -3 -24 1 50.49 15.20 3 24 -1 44.60 7.40 -3 -24 0 14.40 17.30 -3 -24 0 23.60 13.70 3 24 0 12.90 7.50 3 24 0 7.80 26.50 -3 -24 -1 15.40 13.20 -3 -24 -1 -11.60 17.60 3 24 1 -15.80 29.20 3 24 1 12.10 9.50 -3 -24 -2 2.80 18.70 -3 -24 -2 12.80 13.40 3 24 2 13.80 33.60 3 24 2 -7.40 10.40 -4 -24 3 -4.00 12.00 -4 -24 3 -2.40 13.80 4 24 -3 33.70 20.60 -4 -24 2 69.29 17.30 4 24 -2 62.79 8.20 4 24 -2 104.79 23.20 -4 -24 1 29.30 15.30 4 24 -1 29.20 7.80 -4 -24 0 4.70 13.80 4 24 0 2.60 8.60 -4 -24 -1 22.80 18.10 -4 -24 -1 -0.50 11.20 4 24 1 -6.60 24.20 4 24 1 9.90 9.20 -4 -24 -2 -0.50 13.90 -4 -24 -2 15.70 19.60 4 24 2 34.90 34.20 4 24 2 -9.70 11.20 5 24 -3 9.70 8.20 -5 -24 2 4.60 13.30 5 24 -2 77.89 22.10 5 24 -2 -9.00 7.70 -5 -24 1 25.60 13.00 5 24 -1 17.00 8.70 -5 -24 0 61.89 15.70 5 24 0 65.49 11.00 -5 -24 -1 -2.50 14.10 5 24 1 6.20 9.70 5 24 1 34.90 31.60 -6 -24 2 0.10 16.70 6 24 -2 76.69 27.30 6 24 -2 15.40 8.90 -6 -24 1 -4.20 15.70 6 24 -1 6.60 9.70 -6 -24 0 45.20 13.40 -6 -24 0 9.80 16.80 6 24 0 43.50 10.40 6 24 1 -0.70 40.10 6 24 1 7.00 11.20 7 24 -1 27.70 10.30 7 24 0 15.30 9.50 -4 25 0 84.09 30.40 4 -25 -1 25.70 17.90 -4 25 1 6.50 29.90 -4 25 1 3.00 6.10 -3 25 -1 40.60 21.70 3 -25 -1 -15.20 21.60 -3 25 1 3.00 24.60 -3 25 1 3.20 6.30 -3 25 2 14.50 8.60 2 -25 1 -2.60 20.00 -2 25 -1 15.30 24.40 2 -25 0 8.90 16.90 -2 25 0 24.90 28.00 2 -25 -1 1.90 17.70 -2 25 1 -4.50 6.40 -2 25 1 -9.60 23.90 2 -25 -2 19.50 23.90 -2 25 2 43.80 9.70 -2 25 2 22.80 26.80 -1 25 -2 77.99 22.90 -1 25 -1 21.50 24.10 -1 25 -1 66.49 22.10 1 -25 0 24.60 17.50 -1 25 0 23.80 27.80 1 -25 -1 10.30 18.60 -1 25 1 26.70 7.10 -1 25 1 -18.00 29.30 1 -25 -2 6.80 19.30 -1 25 2 16.10 33.30 -1 25 2 -1.70 9.20 0 -25 2 36.60 17.90 0 25 -2 70.49 23.60 0 -25 1 -12.50 16.90 0 25 -1 41.90 23.30 0 -25 0 20.80 20.20 0 25 0 -11.90 26.30 0 25 0 0.00 4.70 0 -25 -1 36.70 22.50 0 25 1 -18.40 7.10 0 25 1 -21.20 29.80 0 -25 -2 22.80 19.90 0 25 2 22.30 10.10 0 25 2 -7.20 33.60 -1 -25 2 -8.10 16.90 1 25 -2 61.29 19.90 -1 -25 1 20.40 19.40 1 25 -1 85.59 21.90 -1 -25 0 61.59 18.40 1 25 0 23.60 27.70 1 25 0 44.20 7.00 -1 -25 -1 28.50 19.10 1 25 1 22.00 7.90 1 25 1 13.80 30.50 -1 -25 -2 -23.40 23.40 1 25 2 8.10 9.50 2 25 -2 71.09 21.30 -2 -25 1 -2.80 11.50 -2 -25 0 -12.80 16.80 -2 -25 0 6.10 13.70 2 25 0 11.30 6.60 2 25 0 -12.30 27.10 -2 -25 -1 2.00 13.10 -2 -25 -1 -8.10 22.10 2 25 1 1.90 8.50 2 25 1 8.60 30.10 3 25 -2 64.99 21.30 -3 -25 1 -8.40 11.60 3 25 -1 -1.00 6.50 -3 -25 0 -0.40 11.30 -3 -25 0 34.10 21.50 3 25 0 -3.40 7.80 -3 -25 -1 29.00 18.80 -3 -25 -1 15.40 13.70 3 25 1 16.20 30.50 3 25 1 28.20 8.70 4 25 -1 5.40 7.60 -4 -25 0 53.99 15.50 4 25 0 54.99 9.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 41147 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN micromount with oil' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn N10 N 0.75330(11) 0.59120(7) 0.8211(2) 0.0198(4) Uani 1 1 d . C3 C 0.72627(13) 0.61696(10) 0.9564(3) 0.0217(5) Uani 1 1 d . C2 C 0.67805(14) 0.57157(10) 1.0285(3) 0.0221(5) Uani 1 1 d . C1 C 0.67779(13) 0.51532(10) 0.9343(3) 0.0204(5) Uani 1 1 d . C9 C 0.72496(13) 0.52732(9) 0.8026(3) 0.0190(5) Uani 1 1 d . C8 C 0.74535(13) 0.48890(9) 0.6709(3) 0.0190(5) Uani 1 1 d . C12 C 0.79093(13) 0.51395(9) 0.5526(3) 0.0192(5) Uani 1 1 d . C7 C 0.81839(13) 0.48606(10) 0.4096(3) 0.0211(5) Uani 1 1 d . C6 C 0.86228(13) 0.53313(10) 0.3383(3) 0.0216(5) Uani 1 1 d . C5 C 0.86300(13) 0.58855(10) 0.4401(3) 0.0219(5) Uani 1 1 d . N11 N 0.81963(11) 0.57768(8) 0.5670(2) 0.0198(4) Uani 1 1 d . B4 B 0.80499(16) 0.62607(11) 0.7055(4) 0.0228(6) Uani 1 1 d . F13 F 0.75968(8) 0.67861(5) 0.62767(18) 0.0343(4) Uani 1 1 d . F14 F 0.88311(8) 0.64650(6) 0.80465(18) 0.0340(4) Uani 1 1 d . C33 C 0.74624(15) 0.68458(10) 1.0139(3) 0.0299(6) Uani 1 1 d . H33A H 0.8054 0.6951 1.0041 0.045 Uiso 1 1 calc GR H33B H 0.7406 0.6894 1.1363 0.045 Uiso 1 1 calc GR H33C H 0.7060 0.7142 0.9394 0.045 Uiso 1 1 calc GR C31 C 0.63599(15) 0.58497(10) 1.1775(3) 0.0276(6) Uani 1 1 d . H31A H 0.6804 0.5997 1.2789 0.033 Uiso 1 1 calc R H31B H 0.6110 0.5440 1.2117 0.033 Uiso 1 1 calc R C32 C 0.56579(15) 0.63553(11) 1.1387(3) 0.0349(6) Uani 1 1 d . H32A H 0.5229 0.6225 1.0348 0.052 Uiso 1 1 calc GR H32B H 0.5909 0.6775 1.1167 0.052 Uiso 1 1 calc GR H32C H 0.5378 0.6395 1.2395 0.052 Uiso 1 1 calc GR C30 C 0.63366(15) 0.45411(10) 0.9630(3) 0.0277(6) Uani 1 1 d . H30A H 0.5862 0.4460 0.8627 0.042 Uiso 1 1 calc GR H30B H 0.6107 0.4577 1.0704 0.042 Uiso 1 1 calc GR H30C H 0.6748 0.4180 0.9748 0.042 Uiso 1 1 calc GR C37 C 0.80472(15) 0.41863(10) 0.3432(3) 0.0274(6) Uani 1 1 d . H37A H 0.8401 0.3888 0.4264 0.041 Uiso 1 1 calc GR H37B H 0.8213 0.4154 0.2289 0.041 Uiso 1 1 calc GR H37C H 0.7437 0.4071 0.3303 0.041 Uiso 1 1 calc GR C35 C 0.90532(14) 0.52486(10) 0.1885(3) 0.0247(5) Uani 1 1 d . H35A H 0.9188 0.5681 0.1454 0.030 Uiso 1 1 calc R H35B H 0.8656 0.5025 0.0917 0.030 Uiso 1 1 calc R C36 C 0.98760(14) 0.48593(11) 0.2391(3) 0.0287(6) Uani 1 1 d . H36A H 1.0133 0.4800 0.1358 0.043 Uiso 1 1 calc GR H36B H 0.9746 0.4434 0.2840 0.043 Uiso 1 1 calc GR H36C H 1.0283 0.5092 0.3303 0.043 Uiso 1 1 calc GR C34 C 0.90622(15) 0.65119(10) 0.4243(3) 0.0292(6) Uani 1 1 d . H34A H 0.8639 0.6865 0.4140 0.044 Uiso 1 1 calc GR H34B H 0.9316 0.6505 0.3196 0.044 Uiso 1 1 calc GR H34C H 0.9518 0.6582 0.5288 0.044 Uiso 1 1 calc GR C15 C 0.72179(13) 0.41912(9) 0.6597(3) 0.0176(5) Uani 1 1 d . C16 C 0.64342(13) 0.39845(9) 0.5610(3) 0.0186(5) Uani 1 1 d . C17 C 0.58296(14) 0.44277(10) 0.4678(3) 0.0226(5) Uani 1 1 d . H17 H 0.5966 0.4878 0.4720 0.027 Uiso 1 1 calc R C18 C 0.50648(14) 0.42295(11) 0.3732(3) 0.0267(6) Uani 1 1 d . H18 H 0.4673 0.4538 0.3102 0.032 Uiso 1 1 calc R C19 C 0.48443(14) 0.35726(11) 0.3672(3) 0.0284(6) Uani 1 1 d . H19 H 0.4296 0.3436 0.3035 0.034 Uiso 1 1 calc R C20 C 0.54053(14) 0.31341(11) 0.4514(3) 0.0257(5) Uani 1 1 d . H20 H 0.5244 0.2689 0.4461 0.031 Uiso 1 1 calc R C21 C 0.62306(14) 0.33134(10) 0.5478(3) 0.0204(5) Uani 1 1 d . C22 C 0.68335(14) 0.28569(9) 0.6280(3) 0.0203(5) Uani 1 1 d . C23 C 0.76166(14) 0.30668(9) 0.7301(3) 0.0196(5) Uani 1 1 d . C24 C 0.82369(14) 0.26292(10) 0.8216(3) 0.0265(6) Uani 1 1 d . H24 H 0.8120 0.2176 0.8127 0.032 Uiso 1 1 calc R C25 C 0.89864(15) 0.28334(11) 0.9209(3) 0.0302(6) Uani 1 1 d . H25 H 0.9385 0.2526 0.9822 0.036 Uiso 1 1 calc R C26 C 0.91829(15) 0.34952(10) 0.9345(3) 0.0265(6) Uani 1 1 d . H26 H 0.9717 0.3637 1.0035 0.032 Uiso 1 1 calc R C27 C 0.86162(13) 0.39305(10) 0.8498(3) 0.0220(5) Uani 1 1 d . H27 H 0.8758 0.4380 0.8596 0.026 Uiso 1 1 calc R C28 C 0.78124(13) 0.37389(10) 0.7464(3) 0.0195(5) Uani 1 1 d . C29 C 0.66534(15) 0.21475(10) 0.6043(3) 0.0303(6) Uani 1 1 d . H29A H 0.6384 0.1990 0.6990 0.045 Uiso 1 1 calc GR H29B H 0.7195 0.1914 0.6074 0.045 Uiso 1 1 calc GR H29C H 0.6262 0.2073 0.4909 0.045 Uiso 1 1 calc GR 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 N10 0.0215(10) 0.0130(9) 0.0235(11) -0.0015(8) 0.0014(8) 0.0009(8) C3 0.0183(11) 0.0184(11) 0.0257(13) -0.0005(10) -0.0014(10) 0.0038(10) C2 0.0219(12) 0.0197(12) 0.0226(13) 0.0010(10) 0.0000(10) 0.0049(10) C1 0.0201(12) 0.0182(11) 0.0211(13) 0.0014(10) -0.0004(10) 0.0020(10) C9 0.0187(11) 0.0140(11) 0.0224(13) -0.0008(9) -0.0004(10) 0.0005(9) C8 0.0160(11) 0.0159(11) 0.0222(13) 0.0007(10) -0.0033(10) 0.0024(9) C12 0.0187(12) 0.0135(11) 0.0243(13) -0.0001(9) 0.0016(10) -0.0013(9) C7 0.0196(12) 0.0195(11) 0.0230(13) -0.0001(10) 0.0015(10) 0.0008(10) C6 0.0192(12) 0.0200(12) 0.0240(13) 0.0012(10) 0.0011(10) 0.0008(10) C5 0.0179(12) 0.0198(12) 0.0263(13) 0.0049(10) 0.0011(10) 0.0012(10) N11 0.0183(9) 0.0148(9) 0.0249(11) 0.0026(8) 0.0013(8) -0.0003(8) B4 0.0217(14) 0.0157(13) 0.0292(16) 0.0001(11) 0.0014(12) -0.0002(12) F13 0.0450(9) 0.0167(7) 0.0445(9) 0.0082(6) 0.0166(7) 0.0073(6) F14 0.0275(8) 0.0333(8) 0.0417(9) -0.0147(6) 0.0083(7) -0.0122(6) C33 0.0344(14) 0.0189(12) 0.0358(15) -0.0068(11) 0.0060(12) -0.0021(11) C31 0.0337(14) 0.0230(12) 0.0267(14) -0.0001(10) 0.0079(11) 0.0025(11) C32 0.0289(14) 0.0356(14) 0.0414(16) -0.0006(12) 0.0103(12) 0.0037(12) C30 0.0337(14) 0.0205(12) 0.0300(14) 0.0034(10) 0.0089(12) 0.0005(11) C37 0.0312(14) 0.0235(12) 0.0282(14) -0.0054(10) 0.0078(11) -0.0040(11) C35 0.0255(12) 0.0224(12) 0.0254(13) 0.0004(10) 0.0032(11) -0.0017(10) C36 0.0247(13) 0.0322(13) 0.0282(14) 0.0017(11) 0.0030(11) 0.0008(11) C34 0.0309(14) 0.0211(12) 0.0364(15) 0.0037(11) 0.0090(12) -0.0055(11) C15 0.0194(12) 0.0137(11) 0.0198(12) 0.0004(9) 0.0042(10) -0.0001(9) C16 0.0221(12) 0.0145(11) 0.0196(12) -0.0007(9) 0.0051(10) -0.0007(9) C17 0.0250(13) 0.0191(12) 0.0236(13) 0.0002(10) 0.0046(11) 0.0017(10) C18 0.0227(13) 0.0295(13) 0.0258(13) -0.0016(11) 0.0000(11) 0.0059(11) C19 0.0201(13) 0.0342(14) 0.0287(14) -0.0061(11) -0.0001(11) -0.0049(11) C20 0.0255(13) 0.0214(12) 0.0297(14) -0.0035(10) 0.0047(11) -0.0060(11) C21 0.0231(12) 0.0181(11) 0.0209(12) -0.0011(9) 0.0064(10) -0.0021(10) C22 0.0256(13) 0.0155(11) 0.0214(13) -0.0015(9) 0.0086(11) -0.0022(10) C23 0.0263(13) 0.0145(11) 0.0192(12) -0.0005(9) 0.0075(10) 0.0011(10) C24 0.0318(14) 0.0143(11) 0.0333(14) 0.0030(10) 0.0065(12) 0.0040(11) C25 0.0296(14) 0.0245(13) 0.0339(15) 0.0035(11) 0.0004(12) 0.0105(11) C26 0.0215(12) 0.0273(13) 0.0284(14) -0.0015(10) -0.0001(11) 0.0015(11) C27 0.0234(13) 0.0177(11) 0.0240(13) -0.0007(10) 0.0028(11) -0.0010(10) C28 0.0204(12) 0.0184(11) 0.0202(12) -0.0018(9) 0.0050(10) 0.0002(10) C29 0.0372(14) 0.0198(12) 0.0333(15) 0.0008(11) 0.0061(12) -0.0050(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C3 N10 C9 108.08(17) C3 N10 B4 125.74(18) C9 N10 B4 126.18(18) N10 C3 C2 110.17(18) N10 C3 C33 122.2(2) C2 C3 C33 127.6(2) C3 C2 C31 124.28(19) C1 C2 C3 107.0(2) C1 C2 C31 128.7(2) C2 C1 C9 107.32(18) C2 C1 C30 126.0(2) C9 C1 C30 126.65(19) N10 C9 C1 107.45(18) C8 C9 N10 119.86(19) C8 C9 C1 132.69(19) C9 C8 C15 120.2(2) C12 C8 C9 120.94(19) C12 C8 C15 118.81(19) C8 C12 C7 131.92(19) C8 C12 N11 120.47(19) N11 C12 C7 107.60(18) C12 C7 C37 127.97(19) C6 C7 C12 107.37(18) C6 C7 C37 124.7(2) C7 C6 C5 107.1(2) C7 C6 C35 126.30(19) C5 C6 C35 126.52(19) C6 C5 C34 128.3(2) N11 C5 C6 109.92(18) N11 C5 C34 121.8(2) C12 N11 B4 125.62(18) C5 N11 C12 108.02(17) C5 N11 B4 126.36(18) N10 B4 N11 106.89(17) F13 B4 N10 109.79(18) F13 B4 N11 110.3(2) F13 B4 F14 109.55(18) F14 B4 N10 110.11(19) F14 B4 N11 110.21(19) C3 C33 H33A 109.5 C3 C33 H33B 109.5 C3 C33 H33C 109.5 H33A C33 H33B 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C2 C31 H31A 108.8 C2 C31 H31B 108.8 C2 C31 C32 113.90(19) H31A C31 H31B 107.7 C32 C31 H31A 108.8 C32 C31 H31B 108.8 C31 C32 H32A 109.5 C31 C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32B 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C1 C30 H30A 109.5 C1 C30 H30B 109.5 C1 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C7 C37 H37A 109.5 C7 C37 H37B 109.5 C7 C37 H37C 109.5 H37A C37 H37B 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 C6 C35 H35A 109.3 C6 C35 H35B 109.3 C6 C35 C36 111.65(19) H35A C35 H35B 108.0 C36 C35 H35A 109.3 C36 C35 H35B 109.3 C35 C36 H36A 109.5 C35 C36 H36B 109.5 C35 C36 H36C 109.5 H36A C36 H36B 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C5 C34 H34A 109.5 C5 C34 H34B 109.5 C5 C34 H34C 109.5 H34A C34 H34B 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C16 C15 C8 121.10(18) C16 C15 C28 120.12(18) C28 C15 C8 118.75(18) C15 C16 C17 121.51(18) C15 C16 C21 120.27(18) C17 C16 C21 118.20(19) C16 C17 H17 119.2 C18 C17 C16 121.7(2) C18 C17 H17 119.2 C17 C18 H18 119.9 C17 C18 C19 120.2(2) C19 C18 H18 119.9 C18 C19 H19 120.0 C20 C19 C18 120.0(2) C20 C19 H19 120.0 C19 C20 H20 119.0 C19 C20 C21 122.1(2) C21 C20 H20 119.0 C20 C21 C16 117.64(19) C22 C21 C16 120.01(19) C22 C21 C20 122.35(19) C21 C22 C23 119.56(18) C21 C22 C29 120.6(2) C23 C22 C29 119.86(19) C22 C23 C24 122.27(19) C22 C23 C28 120.33(19) C24 C23 C28 117.40(19) C23 C24 H24 119.0 C25 C24 C23 122.1(2) C25 C24 H24 119.0 C24 C25 H25 119.8 C24 C25 C26 120.4(2) C26 C25 H25 119.8 C25 C26 H26 120.1 C27 C26 C25 119.9(2) C27 C26 H26 120.1 C26 C27 H27 119.1 C26 C27 C28 121.7(2) C28 C27 H27 119.1 C15 C28 C23 119.61(19) C15 C28 C27 121.87(19) C27 C28 C23 118.52(19) C22 C29 H29A 109.5 C22 C29 H29B 109.5 C22 C29 H29C 109.5 H29A C29 H29B 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N10 C3 1.326(3) N10 C9 1.387(3) N10 B4 1.515(3) C3 C2 1.395(3) C3 C33 1.475(3) C2 C1 1.370(3) C2 C31 1.477(3) C1 C9 1.408(3) C1 C30 1.479(3) C9 C8 1.384(3) C8 C12 1.381(3) C8 C15 1.481(3) C12 C7 1.398(3) C12 N11 1.385(2) C7 C6 1.374(3) C7 C37 1.481(3) C6 C5 1.387(3) C6 C35 1.476(3) C5 N11 1.333(3) C5 C34 1.476(3) N11 B4 1.520(3) B4 F13 1.368(3) B4 F14 1.382(3) C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C31 H31A 0.9900 C31 H31B 0.9900 C31 C32 1.507(3) C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C37 H37A 0.9800 C37 H37B 0.9800 C37 H37C 0.9800 C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.511(3) C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C15 C16 1.385(3) C15 C28 1.395(3) C16 C17 1.410(3) C16 C21 1.417(3) C17 H17 0.9500 C17 C18 1.345(3) C18 H18 0.9500 C18 C19 1.394(3) C19 H19 0.9500 C19 C20 1.339(3) C20 H20 0.9500 C20 C21 1.415(3) C21 C22 1.392(3) C22 C23 1.396(3) C22 C29 1.491(3) C23 C24 1.412(3) C23 C28 1.417(3) C24 H24 0.9500 C24 C25 1.343(3) C25 H25 0.9500 C25 C26 1.396(3) C26 H26 0.9500 C26 C27 1.341(3) C27 H27 0.9500 C27 C28 1.415(3) C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 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 C33 H33A F14 0.98 2.39 3.068(3) 125.9 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 N10 C3 C2 C1 1.4(2) N10 C3 C2 C31 -177.99(19) N10 C9 C8 C12 -2.5(3) N10 C9 C8 C15 174.79(18) C3 N10 C9 C1 0.6(2) C3 N10 C9 C8 -179.36(19) C3 N10 B4 N11 -179.12(18) C3 N10 B4 F13 -59.5(3) C3 N10 B4 F14 61.2(3) C3 C2 C1 C9 -1.0(2) C3 C2 C1 C30 -179.3(2) C3 C2 C31 C32 64.2(3) C2 C1 C9 N10 0.3(2) C2 C1 C9 C8 -179.8(2) C1 C2 C31 C32 -115.0(3) C1 C9 C8 C12 177.5(2) C1 C9 C8 C15 -5.2(3) C9 N10 C3 C2 -1.3(2) C9 N10 C3 C33 179.25(19) C9 N10 B4 N11 -0.1(3) C9 N10 B4 F13 119.5(2) C9 N10 B4 F14 -119.8(2) C9 C8 C12 C7 -179.3(2) C9 C8 C12 N11 2.1(3) C9 C8 C15 C16 90.5(3) C9 C8 C15 C28 -91.3(2) C8 C12 C7 C6 -179.4(2) C8 C12 C7 C37 0.3(4) C8 C12 N11 C5 178.57(19) C8 C12 N11 B4 -0.6(3) C8 C15 C16 C17 -0.1(3) C8 C15 C16 C21 178.20(19) C8 C15 C28 C23 -176.9(2) C8 C15 C28 C27 2.5(3) C12 C8 C15 C16 -92.1(3) C12 C8 C15 C28 86.0(3) C12 C7 C6 C5 1.4(2) C12 C7 C6 C35 177.77(19) C12 N11 B4 N10 -0.3(3) C12 N11 B4 F13 -119.6(2) C12 N11 B4 F14 119.3(2) C7 C12 N11 C5 -0.3(2) C7 C12 N11 B4 -179.51(19) C7 C6 C5 N11 -1.6(2) C7 C6 C5 C34 176.2(2) C7 C6 C35 C36 -73.2(3) C6 C5 N11 C12 1.2(2) C6 C5 N11 B4 -179.62(19) C5 C6 C35 C36 102.5(2) C5 N11 B4 N10 -179.40(18) C5 N11 B4 F13 61.3(3) C5 N11 B4 F14 -59.7(3) N11 C12 C7 C6 -0.7(2) N11 C12 C7 C37 179.0(2) B4 N10 C3 C2 177.92(19) B4 N10 C3 C33 -1.6(3) B4 N10 C9 C1 -178.56(19) B4 N10 C9 C8 1.5(3) C33 C3 C2 C1 -179.1(2) C33 C3 C2 C31 1.5(4) C31 C2 C1 C9 178.4(2) C31 C2 C1 C30 0.1(4) C30 C1 C9 N10 178.5(2) C30 C1 C9 C8 -1.5(4) C37 C7 C6 C5 -178.3(2) C37 C7 C6 C35 -1.9(3) C35 C6 C5 N11 -178.00(19) C35 C6 C5 C34 -0.2(4) C34 C5 N11 C12 -176.8(2) C34 C5 N11 B4 2.4(3) C15 C8 C12 C7 3.4(3) C15 C8 C12 N11 -175.21(18) C15 C16 C17 C18 -179.4(2) C15 C16 C21 C20 177.3(2) C15 C16 C21 C22 -2.7(3) C16 C15 C28 C23 1.2(3) C16 C15 C28 C27 -179.4(2) C16 C17 C18 C19 1.0(4) C16 C21 C22 C23 3.9(3) C16 C21 C22 C29 -175.5(2) C17 C16 C21 C20 -4.3(3) C17 C16 C21 C22 175.7(2) C17 C18 C19 C20 -2.1(4) C18 C19 C20 C21 -0.1(3) C19 C20 C21 C16 3.3(3) C19 C20 C21 C22 -176.6(2) C20 C21 C22 C23 -176.2(2) C20 C21 C22 C29 4.5(3) C21 C16 C17 C18 2.2(3) C21 C22 C23 C24 176.9(2) C21 C22 C23 C28 -2.5(3) C22 C23 C24 C25 -179.4(2) C22 C23 C28 C15 0.0(3) C22 C23 C28 C27 -179.4(2) C23 C24 C25 C26 -1.0(4) C24 C23 C28 C15 -179.5(2) C24 C23 C28 C27 1.1(3) C24 C25 C26 C27 0.9(4) C25 C26 C27 C28 0.3(3) C26 C27 C28 C15 179.3(2) C26 C27 C28 C23 -1.3(3) C28 C15 C16 C17 -178.2(2) C28 C15 C16 C21 0.1(3) C28 C23 C24 C25 0.0(3) C29 C22 C23 C24 -3.7(3) C29 C22 C23 C28 176.8(2)