#------------------------------------------------------------------------------ #$Date: 2021-07-31 04:53:19 +0300 (Sat, 31 Jul 2021) $ #$Revision: 267843 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564281.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_1564281 loop_ _publ_author_name 'Zhai, Yizhan' 'Zhang, Xue' 'Ma, Shengming' _publ_section_title ; Stereoselective rhodium-catalyzed 2-C--H 1,3-dienylation of indoles: dual functions of the directing group ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02167B _journal_year 2021 _chemical_formula_moiety 'C23 H18 Br N3 O' _chemical_formula_sum 'C23 H18 Br N3 O' _chemical_formula_weight 432.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-12 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-04 deposited with the CCDC. 2021-07-16 downloaded from the CCDC. ; _cell_angle_alpha 95.198(4) _cell_angle_beta 91.243(4) _cell_angle_gamma 108.491(4) _cell_formula_units_Z 2 _cell_length_a 7.4828(5) _cell_length_b 7.7696(6) _cell_length_c 16.9566(12) _cell_measurement_reflns_used 6086 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 54.86 _cell_measurement_theta_min 4.56 _cell_volume 929.76(12) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 170.0 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_unetI/netI 0.0740 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 9015 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 54.991 _diffrn_reflns_theta_min 4.563 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.163 _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.4688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1691 before and 0.0925 after correction. The Ratio of minimum to maximum transmission is 0.6244. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.544 _exptl_crystal_description block _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _refine_diff_density_max 2.110 _refine_diff_density_min -2.097 _refine_diff_density_rms 0.201 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 3490 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0808 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1960P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2228 _refine_ls_wR_factor_ref 0.2407 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2968 _reflns_number_total 3490 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02167b2.cif _cod_data_source_block mj19656_0m _cod_database_code 1564281 _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 0.881 _shelx_estimated_absorpt_t_min 0.797 _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 Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C14(H14), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22) 2.b X=CH2 refined with riding coordinates: C1(H1A,H1B) 2.c Idealised Me refined as rotating group: C23(H23A,H23B,H23C) ; _shelx_res_file ; TITL mj19656_0m_a.res in P-1 mj19656_0m.res created by SHELXL-2016/6 at 10:05:36 on 12-Oct-2019 REM Old TITL mj19656_0m in P-1 REM SHELXT solution in P-1 REM R1 0.142, Rweak 0.008, Alpha 0.047, Orientation as input REM Formula found by SHELXT: C23 N3 O Br CELL 1.34139 7.4828 7.7696 16.9566 95.198 91.243 108.491 ZERR 2 0.0005 0.0006 0.0012 0.004 0.004 0.004 LATT 1 SFAC C H Br N O DISP Br -0.9502 1.041 8191.5115 DISP C 0.0148 0.007 57.7477 DISP H -0 0 0.6481 DISP N 0.0253 0.0136 110.5121 DISP O 0.0412 0.025 193.9543 UNIT 46 36 2 6 2 L.S. 4 PLAN 20 SIZE 0.06 0.06 0.11 TEMP -103.15 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.196000 FVAR 0.75145 BR1 3 0.850690 0.064983 0.588427 11.00000 0.05317 0.03465 = 0.03010 0.01051 0.00327 0.01973 O1 5 1.093201 0.251704 0.000730 11.00000 0.02462 0.03940 = 0.02683 -0.00065 0.01224 0.00736 N1 4 0.554785 0.341947 0.205112 11.00000 0.02418 0.02537 = 0.01653 0.00260 0.00412 0.00756 N2 4 0.279773 0.106281 0.160078 11.00000 0.02798 0.02679 = 0.02313 0.00439 0.00502 0.00616 N3 4 0.282788 0.309818 0.274530 11.00000 0.02876 0.03193 = 0.02227 0.00229 0.00706 0.00605 C1 1 0.480987 0.764996 0.213782 11.00000 0.04233 0.03191 = 0.03529 0.01094 0.00683 0.01628 AFIX 93 H1A 2 0.516172 0.694962 0.171733 11.00000 -1.20000 H1B 2 0.423169 0.853170 0.202352 11.00000 -1.20000 AFIX 0 C2 1 0.512677 0.739598 0.288658 11.00000 0.03223 0.02654 = 0.03128 0.00773 0.00929 0.01107 AFIX 43 H2 2 0.475020 0.812864 0.328608 11.00000 -1.20000 AFIX 0 C3 1 0.600778 0.608432 0.315618 11.00000 0.02717 0.02303 = 0.01956 0.00344 0.00754 0.00459 C4 1 0.634601 0.605661 0.393951 11.00000 0.02836 0.02846 = 0.02027 0.00426 0.00721 0.00895 AFIX 43 H4 2 0.614030 0.701816 0.427343 11.00000 -1.20000 AFIX 0 C5 1 0.698692 0.475303 0.435070 11.00000 0.02933 0.02694 = 0.01843 0.00423 0.00686 0.00767 C6 1 0.757014 0.523231 0.515411 11.00000 0.03124 0.02657 = 0.02206 0.00338 0.01049 0.01027 AFIX 43 H6 2 0.763784 0.640546 0.539493 11.00000 -1.20000 AFIX 0 C7 1 0.804961 0.402533 0.560321 11.00000 0.03238 0.03528 = 0.02028 0.00474 0.00612 0.01086 AFIX 43 H7 2 0.845039 0.436554 0.614664 11.00000 -1.20000 AFIX 0 C8 1 0.793627 0.232764 0.525005 11.00000 0.02965 0.02786 = 0.02357 0.00791 0.00758 0.00910 C9 1 0.736372 0.179571 0.445577 11.00000 0.04171 0.02306 = 0.02626 0.00578 0.00726 0.00945 AFIX 43 H9 2 0.730510 0.062116 0.421980 11.00000 -1.20000 AFIX 0 C10 1 0.687925 0.301613 0.401430 11.00000 0.03940 0.03180 = 0.01758 0.00185 0.00024 0.01196 AFIX 43 H10 2 0.646654 0.266112 0.347274 11.00000 -1.20000 AFIX 0 C11 1 0.666944 0.499873 0.252595 11.00000 0.02955 0.02198 = 0.01816 0.00719 0.00394 0.00705 C12 1 0.845824 0.549305 0.227635 11.00000 0.03037 0.02389 = 0.02007 0.00497 0.00197 0.00640 AFIX 43 H12 2 0.948904 0.649882 0.250181 11.00000 -1.20000 AFIX 0 C13 1 0.851875 0.424607 0.162057 11.00000 0.02789 0.02481 = 0.01919 0.00813 0.00550 0.01016 C14 1 1.001845 0.419765 0.113230 11.00000 0.02531 0.02547 = 0.02209 0.00499 0.00484 0.00621 AFIX 43 H14 2 1.122780 0.509636 0.121711 11.00000 -1.20000 AFIX 0 C15 1 0.965536 0.279025 0.052630 11.00000 0.02557 0.03242 = 0.01911 0.00604 0.00701 0.01244 C16 1 0.785809 0.143995 0.041332 11.00000 0.02865 0.03148 = 0.02048 0.00201 0.00522 0.01197 AFIX 43 H16 2 0.765933 0.046260 0.000703 11.00000 -1.20000 AFIX 0 C17 1 0.637659 0.150899 0.088239 11.00000 0.02581 0.02704 = 0.02103 0.00169 0.00445 0.00658 AFIX 43 H17 2 0.516588 0.061309 0.079597 11.00000 -1.20000 AFIX 0 C18 1 0.673262 0.294477 0.148608 11.00000 0.02565 0.02587 = 0.01664 0.00630 0.00428 0.01005 C19 1 0.362608 0.247665 0.213976 11.00000 0.02711 0.02215 = 0.01803 0.00962 0.00397 0.00870 C20 1 0.098037 0.018653 0.169402 11.00000 0.02846 0.03244 = 0.02515 0.00255 0.00360 0.00650 AFIX 43 H20 2 0.033742 -0.083301 0.132684 11.00000 -1.20000 AFIX 0 C21 1 -0.000650 0.069586 0.230029 11.00000 0.02549 0.02926 = 0.02678 0.00716 0.00807 0.00354 AFIX 43 H21 2 -0.129995 0.005731 0.236103 11.00000 -1.20000 AFIX 0 C22 1 0.099488 0.218210 0.281057 11.00000 0.03165 0.03135 = 0.02363 0.00680 0.01156 0.00988 AFIX 43 H22 2 0.035748 0.258265 0.323152 11.00000 -1.20000 AFIX 0 C23 1 1.276702 0.383278 0.007557 11.00000 0.02999 0.03800 = 0.02439 0.00971 0.00850 0.01033 AFIX 137 H23A 2 1.354964 0.349234 -0.032640 11.00000 -1.50000 H23B 2 1.334290 0.387729 0.060482 11.00000 -1.50000 H23C 2 1.267219 0.503479 -0.000469 11.00000 -1.50000 AFIX 0 HKLF 4 REM mj19656_0m_a.res in P-1 REM R1 = 0.0808 for 2968 Fo > 4sig(Fo) and 0.0914 for all 3490 data REM 254 parameters refined using 0 restraints END WGHT 0.1960 0.0000 REM Highest difference peak 2.110, deepest hole -2.097, 1-sigma level 0.201 Q1 1 0.8833 -0.0398 0.5673 11.00000 0.05 2.11 Q2 1 0.8360 0.1773 0.6109 11.00000 0.05 1.86 Q3 1 0.7271 0.0053 0.5598 11.00000 0.05 1.53 Q4 1 0.9853 0.1441 0.6179 11.00000 0.05 1.49 Q5 1 0.9651 0.2017 0.6281 11.00000 0.05 1.30 Q6 1 0.7330 0.3383 0.5382 11.00000 0.05 0.61 Q7 1 0.6983 0.4222 0.5474 11.00000 0.05 0.59 Q8 1 0.3314 0.1366 0.1780 11.00000 0.05 0.55 Q9 1 0.6018 0.0271 0.5272 11.00000 0.05 0.54 Q10 1 -0.0098 0.1722 0.2523 11.00000 0.05 0.53 Q11 1 0.7980 0.2974 0.1865 11.00000 0.05 0.51 Q12 1 0.5850 0.8038 0.5077 11.00000 0.05 0.51 Q13 1 0.5375 0.5691 0.3689 11.00000 0.05 0.51 Q14 1 0.2756 0.1963 0.1840 11.00000 0.05 0.51 Q15 1 0.8888 0.1321 0.4930 11.00000 0.05 0.50 Q16 1 0.5582 0.4288 0.2191 11.00000 0.05 0.50 Q17 1 0.5652 0.2496 0.3707 11.00000 0.05 0.50 Q18 1 0.8306 -0.0288 0.6829 11.00000 0.05 0.48 Q19 1 0.7008 0.1797 0.0312 11.00000 0.05 0.47 Q20 1 0.6705 0.1998 0.5023 11.00000 0.05 0.46 ; _shelx_res_checksum 7474 _shelx_hkl_file ; 1 0 0 383.96 33.80 1 0 0 411.46 34.10 -2 0 0 1174.28 100.39 2 0 0 1156.08 98.19 -3 0 0 107.29 9.10 -3 0 0 97.29 12.10 3 0 0 105.69 11.80 -4 0 0 179.28 20.00 -4 0 0 199.98 20.80 -4 0 0 175.48 16.40 4 0 0 207.48 18.10 4 0 0 200.58 20.20 -5 0 0 86.19 13.90 -5 0 0 87.39 14.50 5 0 0 102.79 13.00 5 0 0 98.59 11.20 -6 0 0 274.27 31.20 -6 0 0 272.97 30.10 6 0 0 254.67 26.70 6 0 0 296.87 29.50 -7 0 0 122.49 19.40 -7 0 0 145.69 18.30 7 0 0 89.79 16.10 7 0 0 105.89 14.50 -8 0 0 37.90 9.70 -8 0 0 45.70 12.30 -8 1 0 2.80 6.20 -8 1 0 5.90 5.10 7 -1 0 96.09 14.20 -7 1 0 79.39 15.90 -7 1 0 74.49 14.30 6 -1 0 10.40 3.90 6 -1 0 12.10 5.60 -6 1 0 15.10 7.20 -6 1 0 11.80 6.40 5 -1 0 14.80 5.30 5 -1 0 18.50 4.30 -5 1 0 15.10 2.80 -5 1 0 13.80 5.40 -5 1 0 14.90 5.70 4 -1 0 35.40 7.20 4 -1 0 37.80 4.80 -4 1 0 37.00 3.60 -4 1 0 26.60 6.40 -4 1 0 37.50 7.40 -3 1 0 560.24 44.80 -3 1 0 509.85 47.30 -2 1 0 16.10 4.20 -2 1 0 37.20 8.50 -2 1 0 24.10 2.50 1 -1 0 366.76 33.00 -1 1 0 380.76 32.90 0 -1 0 29.10 4.30 0 1 0 43.40 5.20 0 1 0 35.10 5.00 -1 -1 0 3320.67 315.47 1 1 0 4339.07 315.67 1 1 0 3730.63 314.37 2 1 0 317.77 26.80 2 1 0 269.17 25.20 -3 -1 0 1650.93 130.99 3 1 0 1389.96 129.09 3 1 0 1591.44 130.79 -4 -1 0 870.91 76.99 -4 -1 0 758.62 75.29 4 1 0 956.30 74.09 -5 -1 0 51.09 11.50 -5 -1 0 59.59 11.70 5 1 0 46.00 7.80 5 1 0 66.89 10.20 -6 -1 0 14.50 7.70 -6 -1 0 28.60 9.20 6 1 0 24.70 6.10 6 1 0 19.30 6.70 -7 -1 0 196.88 23.70 -7 -1 0 207.88 25.30 7 1 0 150.68 19.90 -8 -1 0 18.90 6.50 -9 2 0 65.19 12.40 -8 2 0 3.20 6.50 -8 2 0 2.70 5.40 7 -2 0 541.25 54.89 -7 2 0 575.84 54.39 -7 2 0 566.14 55.59 6 -2 0 97.39 11.30 6 -2 0 102.49 15.50 -6 2 0 119.09 15.60 -6 2 0 134.49 17.60 5 -2 0 469.15 44.40 5 -2 0 582.74 49.60 -5 2 0 493.95 48.30 -5 2 0 535.35 43.40 -5 2 0 507.05 47.20 4 -2 0 31.40 4.40 -4 2 0 26.70 6.30 -4 2 0 23.80 5.90 -4 2 0 61.09 15.80 -4 2 0 36.80 3.40 3 -2 0 395.16 36.70 -3 2 0 428.16 36.00 -3 2 0 412.46 38.70 -3 2 0 487.95 40.90 2 -2 0 840.32 74.89 -2 2 0 947.11 76.19 1 -2 0 0.30 1.50 -1 2 0 2.40 6.50 -1 2 0 2.30 2.40 0 -2 0 25.80 3.80 0 2 0 29.00 3.60 0 2 0 30.00 7.60 0 2 0 17.30 5.70 -1 -2 0 4267.77 383.56 1 2 0 4988.50 383.76 -2 -2 0 91.99 9.60 2 2 0 118.39 12.20 2 2 0 91.49 10.20 -3 -2 0 156.08 18.70 -3 -2 0 181.38 16.60 -3 -2 0 179.88 20.60 3 2 0 218.88 20.00 3 2 0 188.38 17.60 -4 -2 0 413.36 44.50 -4 -2 0 487.95 46.50 4 2 0 483.25 42.70 4 2 0 532.95 45.40 -5 -2 0 20.80 8.40 -5 -2 0 16.10 6.60 5 2 0 24.10 5.80 5 2 0 35.30 7.90 -6 -2 0 85.39 14.60 -6 -2 0 91.19 16.60 6 2 0 77.89 14.50 6 2 0 65.19 10.90 -7 -2 0 26.50 15.40 -7 -2 0 54.99 12.40 7 2 0 57.09 9.80 -9 3 0 2.50 6.10 -8 3 0 18.50 7.40 -8 3 0 36.10 9.00 -7 3 0 55.79 11.80 -7 3 0 61.89 13.00 6 -3 0 174.48 22.00 -6 3 0 184.98 15.40 -6 3 0 149.49 19.50 -6 3 0 202.58 22.80 -5 3 0 416.56 35.30 -5 3 0 416.16 38.40 -5 3 0 390.46 40.60 -5 3 0 444.66 43.20 4 -3 0 65.99 7.80 -4 3 0 76.49 6.70 -4 3 0 79.69 13.40 -4 3 0 65.79 10.60 -4 3 0 63.69 8.60 3 -3 0 516.15 49.20 -3 3 0 631.74 53.49 -3 3 0 578.74 50.99 2 -3 0 937.71 87.99 -2 3 0 1111.79 87.19 -2 3 0 984.20 88.79 -2 3 0 1146.19 91.49 1 -3 0 264.17 26.80 -1 3 0 296.47 27.50 -1 3 0 349.77 26.90 -1 3 0 310.27 29.80 0 -3 0 122.59 12.80 0 3 0 124.09 16.40 0 3 0 156.78 13.10 0 3 0 129.89 15.50 -1 -3 0 422.26 38.20 1 3 0 454.85 41.90 1 3 0 434.26 40.50 1 3 0 447.66 38.30 -2 -3 0 2527.55 205.68 -2 -3 0 2482.15 206.68 2 3 0 2305.77 208.98 2 3 0 2540.05 206.18 -3 -3 0 97.49 13.20 -3 -3 0 118.39 11.10 3 3 0 118.29 12.20 3 3 0 94.99 14.50 -4 -3 0 244.48 29.10 -4 -3 0 222.58 24.90 4 3 0 242.08 23.10 4 3 0 215.58 25.70 -5 -3 0 238.08 25.20 -5 -3 0 226.68 27.50 5 3 0 218.68 22.60 5 3 0 173.58 25.50 -6 -3 0 36.80 9.10 -6 -3 0 24.10 10.60 6 3 0 17.20 6.30 -7 -3 0 7.70 4.40 7 3 0 20.70 5.90 -9 4 0 1.10 6.10 -8 4 0 91.89 16.10 7 -4 0 176.48 25.00 -7 4 0 231.18 25.50 6 -4 0 99.09 10.60 -6 4 0 93.89 15.50 -6 4 0 105.29 13.50 -6 4 0 100.39 9.30 5 -4 0 34.50 5.30 -5 4 0 20.20 7.20 -5 4 0 26.00 3.50 -5 4 0 24.70 12.90 4 -4 0 83.99 10.30 -4 4 0 103.69 18.80 -4 4 0 96.09 8.90 -4 4 0 93.49 13.20 3 -4 0 508.65 47.30 -3 4 0 575.04 52.29 -3 4 0 547.85 46.00 -3 4 0 538.75 49.00 2 -4 0 207.88 20.90 -2 4 0 226.58 21.80 -2 4 0 219.68 25.30 -2 4 0 216.58 20.20 -2 4 0 239.68 19.60 1 -4 0 100.29 11.60 -1 4 0 111.39 16.10 -1 4 0 112.99 12.70 -1 4 0 123.69 11.70 0 -4 0 99.69 10.90 0 4 0 115.09 11.10 0 4 0 105.79 14.80 0 4 0 82.49 14.40 -1 -4 0 422.16 34.70 -1 -4 0 324.07 34.00 1 4 0 377.46 39.60 1 4 0 389.46 37.20 1 4 0 432.36 35.10 -2 -4 0 408.06 38.60 -2 -4 0 477.55 37.90 2 4 0 393.06 42.40 2 4 0 409.36 40.10 -3 -4 0 131.89 12.10 -3 -4 0 77.19 18.50 3 4 0 89.89 15.70 3 4 0 127.49 13.40 3 4 0 102.19 15.90 -4 -4 0 74.29 14.50 -4 -4 0 61.19 11.80 4 4 0 60.29 9.30 4 4 0 43.80 11.50 5 4 0 285.67 35.70 5 4 0 366.06 33.00 -6 -4 0 -11.30 8.70 6 4 0 8.40 4.30 -8 5 0 110.69 16.90 7 -5 0 159.28 23.60 6 -5 0 -0.40 2.50 -6 5 0 -0.40 4.60 -6 5 0 0.90 1.50 -6 5 0 -1.00 13.50 5 -5 0 610.24 59.49 -5 5 0 626.04 59.19 -5 5 0 665.43 54.09 4 -5 0 53.29 7.50 -4 5 0 35.60 14.00 -4 5 0 45.00 5.50 -4 5 0 48.90 10.60 3 -5 0 -1.70 2.40 -3 5 0 1.50 12.30 -3 5 0 6.60 4.50 -3 5 0 -2.10 1.30 2 -5 0 92.89 11.20 -2 5 0 104.59 17.30 -2 5 0 89.79 12.20 -2 5 0 75.49 10.50 -2 5 0 88.69 9.00 1 -5 0 162.18 16.50 -1 5 0 152.38 21.80 -1 5 0 154.18 16.00 0 -5 0 150.48 16.00 0 5 0 157.58 20.70 0 5 0 159.08 16.30 -1 -5 0 86.29 9.90 1 5 0 64.59 14.30 1 5 0 80.89 10.20 1 5 0 67.49 15.00 -2 -5 0 366.36 33.80 2 5 0 398.16 34.70 2 5 0 309.07 38.50 -3 -5 0 30.60 5.70 -3 -5 0 11.90 7.70 -3 -5 0 31.30 6.60 3 5 0 28.80 6.80 -4 -5 0 12.50 10.20 4 5 0 12.50 8.10 4 5 0 26.90 7.10 -5 -5 0 10.30 7.70 5 5 0 5.70 3.70 -8 6 0 199.08 23.90 -7 6 0 84.69 8.40 -7 6 0 90.19 15.00 6 -6 0 45.90 7.40 -6 6 0 48.30 13.80 -6 6 0 46.50 5.50 5 -6 0 1.40 2.80 -5 6 0 -1.60 15.10 -5 6 0 -2.80 1.40 -5 6 0 0.70 5.20 4 -6 0 896.61 80.59 -4 6 0 935.31 78.19 -4 6 0 941.71 83.09 3 -6 0 592.34 52.49 -3 6 0 551.44 49.60 -3 6 0 594.74 54.09 2 -6 0 680.03 53.99 -2 6 0 621.54 50.79 -2 6 0 529.25 59.29 -2 6 0 537.05 52.19 1 -6 0 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2.30 2.80 2 2 17 -15.10 9.50 -3 -2 -17 4.70 7.70 -3 -2 -17 8.90 4.10 3 2 17 18.20 8.60 4 -3 -17 75.39 9.70 -4 3 17 89.59 8.90 3 -3 -17 56.89 7.90 -3 3 17 55.89 6.90 2 -3 -17 122.09 13.30 -2 3 17 103.09 11.10 1 -3 -17 5.00 9.80 1 -3 -17 0.90 2.50 0 -3 -17 11.20 9.00 0 -3 -17 9.60 4.10 -1 -3 -17 75.29 10.20 -2 -3 -17 120.69 12.60 -2 -3 -17 103.19 18.80 2 3 17 82.99 21.30 -4 4 17 2.80 2.30 3 -4 -17 2.20 2.80 -3 4 17 -0.70 2.00 2 -4 -17 100.49 13.50 -2 4 17 89.09 9.40 1 -4 -17 203.28 24.20 0 -4 -17 72.29 9.70 0 5 -18 11.30 3.40 0 -5 18 3.50 5.90 -1 5 -18 162.88 16.70 1 -5 18 135.59 23.10 1 -5 18 180.58 21.10 2 -5 18 223.78 25.00 2 4 -18 -0.60 3.20 -2 -4 18 5.90 5.40 0 4 -18 32.90 6.30 0 -4 18 37.80 9.30 1 -4 18 357.76 36.90 2 -4 18 105.79 28.10 2 -4 18 154.68 19.80 -3 4 -18 22.40 6.60 3 -4 18 34.90 10.00 3 3 -18 415.66 38.60 -3 -3 18 435.76 42.80 2 3 -18 12.20 4.20 -2 -3 18 9.10 7.20 1 3 -18 149.79 16.70 -1 -3 18 178.88 22.20 0 3 -18 85.29 11.40 0 -3 18 116.89 16.40 -1 3 -18 8.00 3.60 1 -3 18 3.20 5.60 1 -3 18 -1.00 8.70 -2 3 -18 87.39 10.60 2 -3 18 77.99 16.20 -3 3 -18 208.68 21.40 3 -3 18 229.98 33.30 4 -3 18 23.20 9.50 -3 -2 18 20.30 8.40 2 2 -18 13.10 4.40 -2 -2 18 17.50 7.50 1 2 -18 58.09 8.70 0 2 -18 209.78 21.10 -1 2 -18 6.90 3.40 1 -2 18 8.90 6.60 -2 2 -18 191.88 18.40 2 -2 18 139.09 23.00 -3 2 -18 78.19 13.90 3 -2 18 64.79 14.40 4 -2 18 -9.00 6.10 4 1 -18 3.30 3.10 -4 -1 18 0.00 6.20 3 1 -18 68.79 9.50 2 1 -18 149.99 16.10 1 1 -18 82.69 10.50 0 1 -18 326.07 30.70 -1 1 -18 5.60 3.20 1 -1 18 0.60 9.10 -2 1 -18 3.70 3.10 2 -1 18 11.70 8.40 -3 1 -18 150.58 17.60 3 -1 18 141.29 21.70 4 -1 18 135.19 20.30 4 0 -18 35.10 6.70 -4 0 18 61.69 12.60 3 0 -18 187.78 19.20 2 0 -18 69.39 9.60 1 0 -18 69.09 9.40 0 0 -18 16.20 4.50 1 0 18 39.00 12.30 -2 0 -18 0.40 3.20 2 0 18 5.80 8.40 -3 0 -18 5.10 8.00 3 0 18 3.70 7.50 4 -1 -18 6.70 3.20 -4 1 18 6.10 6.80 3 -1 -18 102.69 11.40 -3 1 18 76.79 9.30 2 -1 -18 173.78 17.30 -2 1 18 150.88 15.40 1 -1 -18 22.60 5.40 -1 1 18 23.50 6.20 0 -1 -18 14.90 4.30 0 1 18 23.10 6.70 -1 -1 -18 376.76 34.00 1 1 18 315.77 38.80 1 1 18 379.26 35.40 -2 -1 -18 62.49 8.90 -2 -1 -18 46.40 12.90 2 1 18 43.30 13.10 -3 -1 -18 12.70 4.70 -3 -1 -18 6.70 8.20 3 1 18 11.80 9.00 4 -2 -18 8.50 3.40 -4 2 18 4.90 2.60 3 -2 -18 30.10 6.20 -3 2 18 5.30 4.80 2 -2 -18 17.00 4.50 -2 2 18 8.70 3.50 1 -2 -18 99.09 11.80 0 -2 -18 7.10 3.70 -1 -2 -18 84.29 10.70 -2 -2 -18 104.19 21.20 -2 -2 -18 111.09 11.80 2 2 18 66.89 15.80 3 -3 -18 0.20 2.40 -3 3 18 3.50 2.30 -2 3 18 0.30 2.60 1 -3 -18 29.30 7.10 0 -3 -18 2.60 10.70 -1 -3 -18 12.30 9.20 0 4 -19 183.18 18.40 -1 4 -19 37.10 6.30 1 -4 19 26.30 7.20 -2 4 -19 35.60 6.70 2 -4 19 25.40 7.60 2 -4 19 32.50 10.60 2 3 -19 3.10 2.60 -2 -3 19 2.10 5.40 -1 -3 19 180.98 26.30 0 -3 19 543.55 52.29 -1 3 -19 31.80 7.50 1 -3 19 -10.40 11.20 1 -3 19 20.20 6.90 -2 3 -19 -4.00 2.90 2 -3 19 -6.60 6.30 2 -3 19 4.10 9.20 3 -3 19 37.60 11.20 -3 -2 19 385.76 39.50 -2 -2 19 14.70 9.50 1 2 -19 8.90 3.70 -1 -2 19 10.40 7.10 0 2 -19 38.50 7.00 -1 2 -19 155.28 16.90 1 -2 19 184.38 21.70 1 -2 19 130.39 25.10 -2 2 -19 -1.20 4.70 2 -2 19 23.20 10.70 -3 2 -19 73.19 10.10 3 -2 19 22.60 10.90 3 1 -19 3.30 3.50 -3 -1 19 11.30 6.80 2 1 -19 25.60 6.30 -2 -1 19 47.80 11.10 1 1 -19 -0.90 2.70 -1 -1 19 1.20 5.30 0 1 -19 26.30 6.00 0 -1 19 36.30 8.50 -1 1 -19 256.37 25.60 1 -1 19 284.17 29.40 -2 1 -19 13.70 6.40 2 -1 19 18.80 10.30 -3 1 -19 74.79 10.60 3 -1 19 67.69 14.80 3 0 -19 36.60 7.40 -3 0 19 58.69 12.70 2 0 -19 146.69 15.60 1 0 -19 26.90 6.10 0 0 -19 127.09 14.00 -1 0 -19 0.50 2.80 1 0 19 5.90 5.30 -2 0 -19 105.39 12.40 2 0 19 108.19 19.70 3 -1 -19 19.10 4.70 -3 1 19 30.30 8.60 2 -1 -19 137.39 14.90 1 -1 -19 97.19 11.80 0 -1 -19 3.00 2.50 0 1 19 8.30 5.40 -1 -1 -19 5.70 5.20 1 1 19 7.00 4.50 -2 -1 -19 18.20 4.60 2 1 19 10.40 4.80 3 -2 -19 10.30 3.70 2 -2 -19 96.99 11.40 1 -2 -19 151.88 18.00 0 -2 -19 31.90 5.70 -1 -2 -19 13.60 3.90 0 3 -20 19.00 5.00 -1 3 -20 16.00 4.80 1 -3 20 14.70 7.20 1 2 -20 32.50 6.50 0 2 -20 292.67 27.70 -1 2 -20 97.99 11.70 1 -2 20 115.89 16.00 -2 2 -20 97.39 10.60 2 -2 20 64.89 13.80 2 1 -20 25.40 5.50 1 1 -20 189.98 19.20 0 1 -20 9.70 3.60 0 -1 20 16.80 6.90 -1 1 -20 264.37 25.80 1 -1 20 278.17 28.70 2 0 -20 12.50 4.20 -2 0 20 20.00 7.20 1 0 -20 45.00 7.30 0 0 -20 29.10 5.60 0 0 20 28.40 7.50 -1 0 -20 207.48 18.90 1 0 20 161.38 20.20 2 -1 -20 44.90 6.80 -2 1 20 41.50 12.00 1 -1 -20 96.29 12.30 -1 1 20 131.79 16.50 0 -1 -20 -1.00 2.50 0 1 20 0.60 6.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 47589 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Br1 Br 0.85069(8) 0.06498(6) 0.58843(3) 0.0375(3) Uani 1 1 d . . . . . O1 O 1.0932(4) 0.2517(5) 0.00073(19) 0.0311(8) Uani 1 1 d . . . . . N1 N 0.5548(5) 0.3419(5) 0.2051(2) 0.0220(8) Uani 1 1 d . . . . . N2 N 0.2798(5) 0.1063(5) 0.1601(2) 0.0264(8) Uani 1 1 d . . . . . N3 N 0.2828(5) 0.3098(5) 0.2745(2) 0.0285(9) Uani 1 1 d . . . . . C1 C 0.4810(7) 0.7650(7) 0.2138(3) 0.0349(11) Uani 1 1 d . . . . . H1A H 0.516172 0.694962 0.171733 0.042 Uiso 1 1 calc R . . . . H1B H 0.423169 0.853170 0.202352 0.042 Uiso 1 1 calc R . . . . C2 C 0.5127(6) 0.7396(6) 0.2887(3) 0.0292(10) Uani 1 1 d . . . . . H2 H 0.475020 0.812864 0.328608 0.035 Uiso 1 1 calc R . . . . C3 C 0.6008(6) 0.6084(6) 0.3156(3) 0.0239(9) Uani 1 1 d . . . . . C4 C 0.6346(6) 0.6057(6) 0.3940(3) 0.0255(9) Uani 1 1 d . . . . . H4 H 0.614030 0.701816 0.427343 0.031 Uiso 1 1 calc R . . . . C5 C 0.6987(6) 0.4753(6) 0.4351(3) 0.0250(9) Uani 1 1 d . . . . . C6 C 0.7570(6) 0.5232(6) 0.5154(3) 0.0262(9) Uani 1 1 d . . . . . H6 H 0.763784 0.640546 0.539493 0.031 Uiso 1 1 calc R . . . . C7 C 0.8050(6) 0.4025(6) 0.5603(3) 0.0291(10) Uani 1 1 d . . . . . H7 H 0.845039 0.436554 0.614664 0.035 Uiso 1 1 calc R . . . . C8 C 0.7936(6) 0.2328(6) 0.5250(3) 0.0266(9) Uani 1 1 d . . . . . C9 C 0.7364(7) 0.1796(6) 0.4456(3) 0.0303(10) Uani 1 1 d . . . . . H9 H 0.730510 0.062116 0.421980 0.036 Uiso 1 1 calc R . . . . C10 C 0.6879(7) 0.3016(6) 0.4014(3) 0.0295(10) Uani 1 1 d . . . . . H10 H 0.646654 0.266112 0.347274 0.035 Uiso 1 1 calc R . . . . C11 C 0.6669(6) 0.4999(6) 0.2526(2) 0.0231(9) Uani 1 1 d . . . . . C12 C 0.8458(6) 0.5493(6) 0.2276(2) 0.0251(9) Uani 1 1 d . . . . . H12 H 0.948904 0.649882 0.250181 0.030 Uiso 1 1 calc R . . . . C13 C 0.8519(6) 0.4246(6) 0.1621(3) 0.0231(9) Uani 1 1 d . . . . . C14 C 1.0018(6) 0.4198(6) 0.1132(3) 0.0245(9) Uani 1 1 d . . . . . H14 H 1.122780 0.509636 0.121711 0.029 Uiso 1 1 calc R . . . . C15 C 0.9655(6) 0.2790(6) 0.0526(2) 0.0246(9) Uani 1 1 d . . . . . C16 C 0.7858(6) 0.1440(6) 0.0413(3) 0.0263(10) Uani 1 1 d . . . . . H16 H 0.765933 0.046260 0.000703 0.032 Uiso 1 1 calc R . . . . C17 C 0.6377(6) 0.1509(6) 0.0882(3) 0.0251(9) Uani 1 1 d . . . . . H17 H 0.516588 0.061309 0.079597 0.030 Uiso 1 1 calc R . . . . C18 C 0.6733(6) 0.2945(6) 0.1486(2) 0.0220(9) Uani 1 1 d . . . . . C19 C 0.3626(6) 0.2477(6) 0.2140(2) 0.0217(9) Uani 1 1 d . . . . . C20 C 0.0980(6) 0.0187(6) 0.1694(3) 0.0294(10) Uani 1 1 d . . . . . H20 H 0.033742 -0.083301 0.132684 0.035 Uiso 1 1 calc R . . . . C21 C -0.0007(7) 0.0696(6) 0.2300(3) 0.0280(10) Uani 1 1 d . . . . . H21 H -0.129995 0.005731 0.236103 0.034 Uiso 1 1 calc R . . . . C22 C 0.0995(6) 0.2182(6) 0.2811(3) 0.0285(10) Uani 1 1 d . . . . . H22 H 0.035748 0.258265 0.323152 0.034 Uiso 1 1 calc R . . . . C23 C 1.2767(7) 0.3833(7) 0.0076(3) 0.0304(10) Uani 1 1 d . . . . . H23A H 1.354964 0.349234 -0.032640 0.046 Uiso 1 1 calc GR . . . . H23B H 1.334290 0.387729 0.060482 0.046 Uiso 1 1 calc GR . . . . H23C H 1.267219 0.503479 -0.000469 0.046 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 Br1 0.0532(5) 0.0347(4) 0.0301(4) 0.0105(3) 0.0033(3) 0.0197(3) O1 0.0246(16) 0.0394(18) 0.0268(16) -0.0006(14) 0.0122(13) 0.0074(14) N1 0.0242(18) 0.0254(18) 0.0165(17) 0.0026(14) 0.0041(14) 0.0076(14) N2 0.028(2) 0.0268(18) 0.0231(18) 0.0044(15) 0.0050(15) 0.0062(15) N3 0.029(2) 0.0319(19) 0.0223(18) 0.0023(15) 0.0071(15) 0.0060(16) C1 0.042(3) 0.032(2) 0.035(3) 0.011(2) 0.007(2) 0.016(2) C2 0.032(2) 0.027(2) 0.031(2) 0.0077(18) 0.0093(19) 0.0111(18) C3 0.027(2) 0.023(2) 0.020(2) 0.0034(17) 0.0075(17) 0.0046(17) C4 0.028(2) 0.028(2) 0.020(2) 0.0043(17) 0.0072(17) 0.0090(18) C5 0.029(2) 0.027(2) 0.018(2) 0.0042(17) 0.0069(17) 0.0077(17) C6 0.031(2) 0.027(2) 0.022(2) 0.0034(17) 0.0105(18) 0.0103(18) C7 0.032(2) 0.035(2) 0.020(2) 0.0047(18) 0.0061(18) 0.0109(19) C8 0.030(2) 0.028(2) 0.024(2) 0.0079(18) 0.0076(18) 0.0091(18) C9 0.042(3) 0.023(2) 0.026(2) 0.0058(18) 0.007(2) 0.0094(19) C10 0.039(3) 0.032(2) 0.018(2) 0.0018(19) 0.0002(18) 0.012(2) C11 0.030(2) 0.022(2) 0.018(2) 0.0072(16) 0.0039(17) 0.0071(17) C12 0.030(2) 0.024(2) 0.020(2) 0.0050(16) 0.0020(17) 0.0064(17) C13 0.028(2) 0.025(2) 0.019(2) 0.0081(17) 0.0055(17) 0.0102(17) C14 0.025(2) 0.025(2) 0.022(2) 0.0050(17) 0.0048(17) 0.0062(17) C15 0.026(2) 0.032(2) 0.019(2) 0.0060(18) 0.0070(17) 0.0124(18) C16 0.029(2) 0.031(2) 0.020(2) 0.0020(18) 0.0052(18) 0.0120(19) C17 0.026(2) 0.027(2) 0.021(2) 0.0017(17) 0.0045(17) 0.0066(17) C18 0.026(2) 0.026(2) 0.0166(19) 0.0063(16) 0.0043(17) 0.0101(17) C19 0.027(2) 0.022(2) 0.018(2) 0.0096(16) 0.0040(17) 0.0087(16) C20 0.028(2) 0.032(2) 0.025(2) 0.0026(18) 0.0036(18) 0.0065(19) C21 0.025(2) 0.029(2) 0.027(2) 0.0072(18) 0.0081(18) 0.0035(17) C22 0.032(2) 0.031(2) 0.024(2) 0.0068(18) 0.0116(18) 0.0099(19) C23 0.030(2) 0.038(2) 0.024(2) 0.0097(19) 0.0085(19) 0.010(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 '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' Br Br -0.9502 1.0410 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 '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 C15 O1 C23 117.0(3) . . ? C11 N1 C18 107.1(3) . . ? C19 N1 C11 126.0(3) . . ? C19 N1 C18 126.9(3) . . ? C20 N2 C19 115.7(4) . . ? C19 N3 C22 115.2(4) . . ? H1A C1 H1B 120.0 . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? C1 C2 H2 116.9 . . ? C1 C2 C3 126.2(4) . . ? C3 C2 H2 116.9 . . ? C2 C3 C11 116.4(4) . . ? C4 C3 C2 119.6(4) . . ? C4 C3 C11 123.6(4) . . ? C3 C4 H4 115.3 . . ? C3 C4 C5 129.4(4) . . ? C5 C4 H4 115.3 . . ? C6 C5 C4 117.3(4) . . ? C10 C5 C4 124.1(4) . . ? C10 C5 C6 118.3(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 C5 121.2(4) . . ? C7 C6 H6 119.4 . . ? C6 C7 H7 120.5 . . ? C8 C7 C6 118.9(4) . . ? C8 C7 H7 120.5 . . ? C7 C8 Br1 118.5(3) . . ? C7 C8 C9 121.8(4) . . ? C9 C8 Br1 119.7(3) . . ? C8 C9 H9 120.7 . . ? C10 C9 C8 118.6(4) . . ? C10 C9 H9 120.7 . . ? C5 C10 H10 119.4 . . ? C9 C10 C5 121.2(4) . . ? C9 C10 H10 119.4 . . ? N1 C11 C3 126.6(4) . . ? C12 C11 N1 109.3(4) . . ? C12 C11 C3 123.9(4) . . ? C11 C12 H12 125.9 . . ? C11 C12 C13 108.1(4) . . ? C13 C12 H12 125.9 . . ? C14 C13 C12 130.5(4) . . ? C18 C13 C12 108.3(4) . . ? C18 C13 C14 121.2(4) . . ? C13 C14 H14 121.2 . . ? C15 C14 C13 117.5(4) . . ? C15 C14 H14 121.2 . . ? O1 C15 C14 125.5(4) . . ? O1 C15 C16 113.7(4) . . ? C14 C15 C16 120.8(4) . . ? C15 C16 H16 119.2 . . ? C17 C16 C15 121.6(4) . . ? C17 C16 H16 119.2 . . ? C16 C17 H17 121.2 . . ? C16 C17 C18 117.6(4) . . ? C18 C17 H17 121.2 . . ? C13 C18 N1 107.1(3) . . ? C13 C18 C17 121.2(4) . . ? C17 C18 N1 131.7(4) . . ? N2 C19 N1 116.5(4) . . ? N3 C19 N1 116.5(4) . . ? N3 C19 N2 127.0(4) . . ? N2 C20 H20 118.6 . . ? N2 C20 C21 122.9(4) . . ? C21 C20 H20 118.6 . . ? C20 C21 H21 122.0 . . ? C22 C21 C20 115.9(4) . . ? C22 C21 H21 122.0 . . ? N3 C22 C21 123.4(4) . . ? N3 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? O1 C23 H23A 109.5 . . ? O1 C23 H23B 109.5 . . ? O1 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 Br1 C8 1.904(5) . ? O1 C15 1.365(5) . ? O1 C23 1.423(6) . ? N1 C11 1.413(5) . ? N1 C18 1.421(5) . ? N1 C19 1.410(5) . ? N2 C19 1.337(6) . ? N2 C20 1.334(6) . ? N3 C19 1.328(5) . ? N3 C22 1.342(6) . ? C1 H1A 0.9500 . ? C1 H1B 0.9500 . ? C1 C2 1.330(7) . ? C2 H2 0.9500 . ? C2 C3 1.476(6) . ? C3 C4 1.350(6) . ? C3 C11 1.491(5) . ? C4 H4 0.9500 . ? C4 C5 1.471(6) . ? C5 C6 1.402(6) . ? C5 C10 1.394(6) . ? C6 H6 0.9500 . ? C6 C7 1.385(6) . ? C7 H7 0.9500 . ? C7 C8 1.375(6) . ? C8 C9 1.389(7) . ? C9 H9 0.9500 . ? C9 C10 1.388(7) . ? C10 H10 0.9500 . ? C11 C12 1.359(6) . ? C12 H12 0.9500 . ? C12 C13 1.418(6) . ? C13 C14 1.417(6) . ? C13 C18 1.396(6) . ? C14 H14 0.9500 . ? C14 C15 1.386(6) . ? C15 C16 1.415(6) . ? C16 H16 0.9500 . ? C16 C17 1.390(6) . ? C17 H17 0.9500 . ? C17 C18 1.399(6) . ? C20 H20 0.9500 . ? C20 C21 1.380(6) . ? C21 H21 0.9500 . ? C21 C22 1.373(7) . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ?