#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:30:00 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296460 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/94/7249422.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_7249422 loop_ _publ_author_name 'Islam, Md Faizul' 'Wijesekera, Gamage Isuri P.' 'Sindt, Ammon J.' 'Smith, Mark D.' 'Shimizu, Linda S.' _publ_section_title ; Examination of photoinduced radicals in two crystal forms of triphenylamine bis-urea macrocycles ; _journal_issue 42 _journal_name_full CrystEngComm _journal_page_first 6025 _journal_page_last 6033 _journal_paper_doi 10.1039/D4CE00839A _journal_volume 26 _journal_year 2024 _chemical_formula_moiety 'C42 H36 Br2 N6 O2, 0.716(C2 H6 O S)' _chemical_formula_sum 'C43.43 H40.29 Br2 N6 O2.72 S0.71' _chemical_formula_weight 872.45 _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' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2021-11-30 _audit_creation_method ; Olex2 1.5 (compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429) ; _audit_update_record ; 2024-03-31 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.584(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.878(2) _cell_length_b 4.6413(6) _cell_length_c 26.735(3) _cell_measurement_reflns_used 8762 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.271 _cell_measurement_theta_min 2.602 _cell_volume 1942.7(4) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2016)' _computing_data_collection 'Bruker APEX3 v2019.1-0 (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2016)' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material 'OLEX2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector PHOTON-II _diffrn_detector_area_resol_mean 7.39 _diffrn_detector_type 'area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Quest' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 26749 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.374 _diffrn_reflns_theta_min 1.847 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.173 _exptl_absorpt_correction_T_max 0.5624 _exptl_absorpt_correction_T_min 0.4717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0854 before and 0.0590 after correction. The Ratio of minimum to maximum transmission is 0.8387. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.491 _exptl_crystal_description needle _exptl_crystal_F_000 892 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.456 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 274 _refine_ls_number_reflns 3961 _refine_ls_number_restraints 14 _refine_ls_restrained_S_all 1.233 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0667 _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^)+(0.0001P)^2^+7.7180P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.1168 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3335 _reflns_number_total 3961 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00839a2.cif _cod_data_source_block mfi_brmc_tegme _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 7249420--7249422.cif. ; _cod_original_cell_volume 1942.8(4) _cod_database_code 7249422 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.958 _shelx_estimated_absorpt_t_min 0.751 _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, All N(H) groups 2. Restrained distances S1S-O1S 1.5 with sigma of 0.015 S1S-C1S = S1S-C2S 1.775 with sigma of 0.02 S2S-O2S 1.5 with sigma of 0.015 S2S-C3S = S2S-C4S 1.775 with sigma of 0.02 N1-H1 = N2-H2 0.85 with sigma of 0.02 O1S-C1S = O1S-C2S 2.623 with sigma of 0.04 C1S-C2S 2.66 with sigma of 0.04 O2S-C3S = O2S-C4S 2.623 with sigma of 0.04 C3S-C4S 2.66 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uiso(C2S) = Uiso(O2S) 4. Others Sof(S1S)=Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)= Sof(H2SB)=Sof(H2SC)=FVAR(1) Sof(S2S)=Sof(O2S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=Sof(C4S)=Sof(H4SA)= Sof(H4SB)=Sof(H4SC)=FVAR(2) 5.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C21(H21A,H21B) 5.b Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20) 5.c Idealised Me refined with riding coordinates: C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB, H4SC) ; _shelx_res_file ; TITL mfi_brmc_tegme_a.res in P2(1)/c mfi_brmc_tegme.res created by SHELXL-2018/3 at 14:43:46 on 30-Nov-2021 REM Old TITL mfi_brmc_tegme in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.154, Rweak 0.021, Alpha 0.071 REM 0.868 for 510 systematic absences, Orientation as input REM Formula found by SHELXT: C23 N2 O Br CELL 0.71073 15.8782 4.6413 26.7352 90 99.584 90 ZERR 2 0.0022 0.0006 0.0034 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N O S UNIT 86.86 80.59 4 12 5.43 1.43 EQIV $1 +X,-1+Y,+Z DFIX 1.5 0.015 S1S O1S DFIX 1.775 S1S C1S S1S C2S DANG 2.623 O1S C1S O1S C2S DANG 2.66 C1S C2S DFIX 1.5 0.015 S2S O2S DFIX 1.775 S2S C3S S2S C4S DANG 2.623 O2S C3S O2S C4S DANG 2.66 C3S C4S EADP C2S O2S DFIX 0.85 N1 H1 N2 H2 L.S. 7 PLAN 9 SIZE 0.02 0.04 0.14 TEMP -173(2) CONF HTAB N1 O1_$1 HTAB N2 O1_$1 BOND $H list 4 fmap 2 53 MORE -1 ACTA REM REM REM WGHT 0.000100 7.718000 FVAR 0.38989 0.26786 0.08999 BR1 3 1.176160 0.836587 0.720351 11.00000 0.03489 0.05076 = 0.02295 -0.00280 0.00616 -0.00617 O1 5 0.600574 0.924451 0.338194 11.00000 0.03636 0.01081 = 0.03980 0.00001 -0.00702 -0.00073 N1 4 0.533305 0.497120 0.319556 11.00000 0.02433 0.01980 = 0.04153 -0.00444 -0.00540 0.00055 H1 2 0.540564 0.316539 0.321919 11.00000 -1.50000 N2 4 0.672315 0.507924 0.358857 11.00000 0.02463 0.02078 = 0.02946 0.00214 -0.00137 0.00036 H2 2 0.665926 0.326695 0.359425 11.00000 -1.50000 N3 4 0.823198 0.647895 0.596530 11.00000 0.03326 0.04931 = 0.02360 -0.00300 0.00316 0.00231 C1 1 0.601980 0.653640 0.338755 11.00000 0.02551 0.01746 = 0.02126 -0.00265 0.00094 -0.00390 C2 1 0.752970 0.641519 0.378805 11.00000 0.02433 0.02735 = 0.02820 0.00032 0.00235 -0.00234 AFIX 23 H2A 2 0.752650 0.841254 0.365779 11.00000 -1.20000 H2B 2 0.799061 0.535740 0.365886 11.00000 -1.20000 AFIX 0 C3 1 0.773255 0.649777 0.435874 11.00000 0.02694 0.02008 = 0.02560 -0.00022 0.00148 -0.00085 C4 1 0.847667 0.531878 0.462368 11.00000 0.02840 0.03210 = 0.02831 0.00313 0.00613 0.00500 AFIX 43 H4 2 0.887974 0.448947 0.444033 11.00000 -1.20000 AFIX 0 C5 1 0.864880 0.531703 0.514948 11.00000 0.03042 0.03178 = 0.02669 0.00724 0.00200 0.00838 AFIX 43 H5 2 0.916363 0.448161 0.532011 11.00000 -1.20000 AFIX 0 C6 1 0.808409 0.650708 0.542450 11.00000 0.03631 0.02928 = 0.02737 0.00026 0.00220 -0.00330 C7 1 0.734025 0.771534 0.516492 11.00000 0.04582 0.05189 = 0.03084 -0.01727 0.00142 0.02236 AFIX 43 H7 2 0.694168 0.856906 0.534871 11.00000 -1.20000 AFIX 0 C8 1 0.717267 0.768982 0.464048 11.00000 0.03912 0.03744 = 0.03375 -0.00862 -0.00366 0.01638 AFIX 43 H8 2 0.665643 0.851906 0.447051 11.00000 -1.20000 AFIX 0 C9 1 0.906814 0.685127 0.624000 11.00000 0.03344 0.02717 = 0.02338 -0.00125 0.00488 0.00707 C10 1 0.963552 0.872360 0.607430 11.00000 0.05795 0.02704 = 0.02753 0.00521 -0.00516 -0.00622 AFIX 43 H10 2 0.947133 0.973380 0.576436 11.00000 -1.20000 AFIX 0 C11 1 1.044255 0.915529 0.635318 11.00000 0.04485 0.02818 = 0.03250 0.00377 0.00431 -0.01038 AFIX 43 H11 2 1.082752 1.047169 0.623889 11.00000 -1.20000 AFIX 0 C12 1 1.067784 0.765694 0.679624 11.00000 0.03011 0.02780 = 0.02314 -0.00285 0.00704 0.00217 C13 1 1.013575 0.572900 0.696389 11.00000 0.02908 0.04049 = 0.02138 0.00855 0.00608 0.00807 AFIX 43 H13 2 1.030977 0.469289 0.727010 11.00000 -1.20000 AFIX 0 C14 1 0.932992 0.530190 0.668255 11.00000 0.03064 0.03967 = 0.02894 0.00623 0.01294 0.00128 AFIX 43 H14 2 0.895429 0.393927 0.679346 11.00000 -1.20000 AFIX 0 C15 1 0.754514 0.589661 0.623098 11.00000 0.03135 0.02639 = 0.02792 -0.00571 0.00274 0.00315 C16 1 0.747020 0.733888 0.667130 11.00000 0.02255 0.03346 = 0.03455 -0.01004 -0.00163 -0.00091 AFIX 43 H16 2 0.787251 0.878837 0.679733 11.00000 -1.20000 AFIX 0 C17 1 0.680526 0.667710 0.693269 11.00000 0.02543 0.04457 = 0.03177 -0.01173 -0.00011 0.00111 AFIX 43 H17 2 0.676513 0.767391 0.723818 11.00000 -1.20000 AFIX 0 C18 1 0.619951 0.459200 0.675660 11.00000 0.02650 0.02273 = 0.03066 -0.00260 0.00022 0.00294 C19 1 0.627358 0.322846 0.630547 11.00000 0.06207 0.04837 = 0.04256 -0.01828 0.01028 -0.02505 AFIX 43 H19 2 0.586185 0.182710 0.617020 11.00000 -1.20000 AFIX 0 C20 1 0.693612 0.387171 0.604882 11.00000 0.07214 0.04574 = 0.03834 -0.02394 0.02375 -0.02177 AFIX 43 H20 2 0.697276 0.289885 0.574055 11.00000 -1.20000 AFIX 0 C21 1 0.548270 0.387606 0.703744 11.00000 0.02388 0.02641 = 0.03723 -0.00065 -0.00244 0.00113 AFIX 23 H21A 2 0.543493 0.175488 0.705984 11.00000 -1.20000 H21B 2 0.562426 0.463383 0.738751 11.00000 -1.20000 AFIX 0 PART -1 S1S 6 0.473618 0.898423 0.491540 21.00000 0.08887 O1S 5 0.485460 1.198092 0.490189 21.00000 0.05636 C1S 1 0.525596 0.613136 0.467147 21.00000 0.07449 AFIX 133 H1SA 2 0.587322 0.630221 0.478558 21.00000 -1.50000 H1SB 2 0.513317 0.618435 0.430002 21.00000 -1.50000 H1SC 2 0.505368 0.430372 0.479170 21.00000 -1.50000 AFIX 0 C2S 1 0.472109 0.761068 0.552720 21.00000 0.08835 AFIX 133 H2SA 2 0.459198 0.917014 0.574971 21.00000 -1.50000 H2SB 2 0.528062 0.678414 0.566257 21.00000 -1.50000 H2SC 2 0.428225 0.611267 0.551010 21.00000 -1.50000 AFIX 0 PART -2 S2S 6 0.457534 0.651320 0.497042 31.00000 0.07081 O2S 5 0.478342 0.665267 0.553726 31.00000 0.08835 C3S 1 0.512223 0.940171 0.473051 31.00000 0.07068 AFIX 133 H3SA 2 0.478542 1.009884 0.441293 31.00000 -1.50000 H3SB 2 0.568003 0.873061 0.466697 31.00000 -1.50000 H3SC 2 0.520332 1.097106 0.497912 31.00000 -1.50000 AFIX 0 C4S 1 0.518844 0.370103 0.476343 31.00000 0.04285 AFIX 133 H4SA 2 0.485689 0.191024 0.473482 31.00000 -1.50000 H4SB 2 0.571411 0.343844 0.500911 31.00000 -1.50000 H4SC 2 0.533355 0.419838 0.443181 31.00000 -1.50000 AFIX 0 HKLF 4 REM mfi_brmc_tegme_a.res in P2(1)/c REM wR2 = 0.116812, GooF = S = 1.22246, Restrained GooF = 1.23330 for all data REM R1 = 0.066713 for 3335 Fo > 4sig(Fo) and 0.082257 for all 3961 data REM 274 parameters refined using 14 restraints END WGHT 0.0001 7.7131 REM Highest difference peak 0.456, deepest hole -1.061, 1-sigma level 0.088 Q1 1 0.4539 1.0380 0.4775 11.00000 0.05 0.46 Q2 1 0.4867 1.1199 0.4994 11.00000 0.05 0.39 Q3 1 1.1533 0.6747 0.7406 11.00000 0.05 0.35 Q4 1 0.6039 0.2668 0.3418 11.00000 0.05 0.35 Q5 1 1.1708 1.2592 0.7183 11.00000 0.05 0.35 Q6 1 1.1981 0.6328 0.7180 11.00000 0.05 0.33 Q7 1 0.9198 0.5225 0.6254 11.00000 0.05 0.32 Q8 1 1.1992 0.7011 0.7010 11.00000 0.05 0.32 Q9 1 1.2040 0.9650 0.6972 11.00000 0.05 0.31 ; _shelx_res_checksum 55794 _shelx_hkl_file ; 2 0 0 1065.79 34.60 -2 0 0 1138.49 35.30 -2 0 0 1008.20 35.30 -2 0 0 1084.69 35.20 2 0 0 1198.98 35.40 3 0 0 1680.93 50.49 3 0 0 1539.65 49.40 3 0 0 1577.54 50.79 -3 0 0 1462.65 50.29 -3 0 0 1540.35 50.19 -3 0 0 1602.74 50.19 -3 0 0 1536.75 49.30 3 0 0 1551.94 50.29 -4 0 0 64.69 4.90 -4 0 0 64.09 5.50 -4 0 0 61.59 6.30 -4 0 0 69.49 5.90 -4 0 0 61.69 5.40 4 0 0 62.99 4.90 4 0 0 56.89 6.00 4 0 0 67.09 5.90 4 0 0 66.19 5.80 -5 0 0 647.54 24.30 -5 0 0 680.23 24.40 -5 0 0 633.24 23.10 5 0 0 684.63 25.40 5 0 0 651.03 24.60 5 0 0 646.34 23.10 -5 0 0 661.23 25.10 -5 0 0 612.44 23.60 5 0 0 694.03 24.90 6 0 0 694.23 26.90 -6 0 0 715.73 27.40 6 0 0 702.33 25.10 6 0 0 739.93 27.80 6 0 0 730.23 27.10 -6 0 0 685.63 26.50 -6 0 0 676.53 25.70 -6 0 0 685.13 25.00 7 0 0 8.80 5.20 7 0 0 8.00 5.30 -7 0 0 9.70 5.60 -7 0 0 6.60 5.20 -7 0 0 4.70 5.50 -7 0 0 11.50 4.70 7 0 0 5.60 5.70 8 0 0 831.62 29.90 -8 0 0 799.82 29.80 -8 0 0 817.52 32.70 -8 0 0 799.52 30.70 8 0 0 842.02 32.30 8 0 0 841.52 32.90 9 0 0 1357.86 49.10 -9 0 0 1252.67 45.20 9 0 0 1370.16 45.90 9 0 0 1367.46 48.80 -9 0 0 1266.37 47.50 -9 0 0 1294.47 46.50 -10 0 0 42.90 6.50 10 0 0 51.19 10.30 -10 0 0 37.20 8.60 10 0 0 53.09 10.20 -11 0 0 418.26 19.20 11 0 0 437.96 23.10 -11 0 0 421.16 21.60 11 0 0 423.56 22.10 12 0 0 385.66 21.70 -12 0 0 383.76 20.60 -12 0 0 360.66 18.00 12 0 0 367.86 22.10 -13 0 0 58.79 8.30 13 0 0 57.99 13.30 13 0 0 65.69 13.60 -13 0 0 56.19 11.50 -14 0 0 1023.70 42.40 -14 0 0 1028.90 39.10 14 0 0 954.00 43.80 14 0 0 1032.60 44.70 15 0 0 17.00 12.60 16 0 0 77.89 17.60 -16 0 0 84.59 11.30 -16 0 0 88.19 13.30 17 0 0 84.69 19.20 17 0 0 101.79 19.10 -17 0 0 129.99 15.60 -17 0 0 90.89 12.40 -18 0 0 21.10 13.90 18 0 0 1.20 12.40 -18 0 0 13.40 11.20 18 0 0 -15.00 14.00 19 0 0 25.70 16.50 19 0 0 58.39 19.00 -19 0 0 81.69 18.80 0 -1 0 1.40 2.10 0 -1 0 2.50 3.20 0 -1 0 -0.20 3.50 0 -1 0 -4.00 3.00 0 1 0 0.00 2.10 0 1 0 4.00 3.30 0 1 0 -1.40 3.30 0 1 0 1.10 3.40 -1 -1 0 370.56 15.10 1 -1 0 373.66 13.60 -1 -1 0 384.56 15.60 1 -1 0 391.46 15.20 1 -1 0 376.76 15.40 1 -1 0 376.26 14.50 -1 -1 0 373.56 13.40 -1 -1 0 383.66 14.50 1 1 0 377.56 14.40 -1 1 0 368.66 13.50 1 1 0 369.86 13.30 1 1 0 373.16 13.40 -1 1 0 382.76 15.10 -1 1 0 370.86 15.40 1 1 0 379.66 15.20 1 1 0 370.96 15.20 -1 1 0 350.46 14.20 -2 -1 0 351.26 15.30 2 -1 0 372.86 15.20 -2 -1 0 376.66 13.60 -2 -1 0 362.66 13.60 -2 -1 0 370.96 14.00 2 -1 0 375.86 14.30 -2 -1 0 381.56 15.60 2 -1 0 369.66 14.00 -2 1 0 351.16 13.80 2 1 0 363.06 15.40 2 1 0 367.36 15.40 2 1 0 361.96 13.50 2 1 0 359.16 13.50 2 1 0 367.06 14.00 -2 1 0 383.36 15.70 -2 1 0 358.96 15.50 -2 1 0 369.36 13.90 -2 1 0 341.27 15.00 -3 -1 0 1068.59 38.00 3 -1 0 1103.79 38.50 3 -1 0 1056.39 37.30 -3 -1 0 1093.39 36.10 -3 -1 0 1067.69 38.30 3 -1 0 1058.49 36.30 -3 -1 0 1102.29 36.20 3 -1 0 1148.09 37.00 -3 1 0 1104.99 36.60 3 1 0 1117.79 36.20 -3 1 0 1021.60 37.60 -3 1 0 1091.39 37.90 3 1 0 1102.59 38.30 3 1 0 1111.09 36.50 3 1 0 1131.99 36.40 3 1 0 1085.69 37.70 4 -1 0 881.61 30.70 4 -1 0 880.31 32.00 4 -1 0 830.92 30.70 -4 -1 0 919.11 30.20 -4 -1 0 870.71 29.20 -4 -1 0 840.22 31.60 -4 -1 0 871.91 31.50 -4 1 0 872.01 31.30 -4 1 0 748.43 30.60 4 1 0 888.71 29.40 -4 1 0 862.91 30.30 4 1 0 883.91 29.90 4 1 0 826.82 30.90 4 1 0 859.41 31.90 -5 -1 0 831.32 32.20 -5 -1 0 873.21 32.10 -5 -1 0 866.21 30.60 5 -1 0 943.71 31.90 5 -1 0 759.32 30.80 -5 -1 0 864.41 29.30 -5 -1 0 892.81 29.50 5 -1 0 879.81 32.70 5 1 0 886.61 30.00 -5 1 0 845.42 31.80 -5 1 0 844.42 31.00 -5 1 0 823.92 31.40 5 1 0 843.52 31.60 5 1 0 887.31 30.80 6 -1 0 42.30 5.30 -6 -1 0 63.59 9.10 6 -1 0 61.19 9.10 -6 -1 0 41.30 8.00 6 -1 0 56.39 8.40 -6 1 0 46.70 6.90 6 1 0 42.40 6.10 6 1 0 37.10 6.00 -6 1 0 36.30 6.90 6 1 0 56.09 8.50 7 -1 0 1773.02 67.89 -7 -1 0 2015.70 69.59 -7 -1 0 2027.70 69.29 -7 -1 0 2099.69 65.89 7 -1 0 2153.08 70.49 7 -1 0 2071.99 69.09 -7 -1 0 2025.10 65.39 -7 1 0 1937.71 68.09 7 1 0 2084.09 68.09 -7 1 0 2026.80 68.89 7 1 0 2056.09 69.19 7 1 0 2083.59 66.29 -8 -1 0 29.10 5.80 -8 -1 0 25.30 8.20 8 -1 0 28.20 7.30 -8 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16.30 5 1 -31 45.90 15.40 5 1 -31 70.59 16.00 -5 1 31 70.39 18.80 4 -1 -31 35.80 13.90 4 -1 -31 12.00 15.30 -4 -1 31 4.10 10.00 4 -1 -31 17.90 9.00 -4 1 31 -2.80 16.10 -4 1 31 16.60 10.20 4 1 -31 -13.20 12.00 4 1 -31 11.70 12.30 4 1 -31 5.90 10.60 3 -1 -31 0.60 13.00 3 -1 -31 5.30 9.90 3 -1 -31 62.89 20.10 -3 -1 31 2.80 10.60 -3 1 31 2.40 16.50 3 1 -31 -12.00 12.30 3 1 -31 -7.00 10.30 3 1 -31 13.00 11.10 -3 1 31 -1.80 10.80 -2 -1 31 39.40 13.90 2 -1 -31 38.20 11.90 2 -1 -31 52.39 18.60 2 -1 -31 35.00 17.00 -2 1 31 32.90 19.30 -2 1 31 40.00 13.10 2 1 -31 79.89 18.40 2 1 -31 90.29 21.00 2 1 -31 48.80 14.30 1 -1 -31 43.80 17.30 1 -1 -31 74.19 21.30 1 -1 -31 33.30 10.70 -1 -1 31 50.59 14.10 -1 1 31 16.80 17.50 1 1 -31 50.79 18.20 1 1 -31 58.19 13.80 0 -1 31 5.20 10.40 0 -1 -31 -2.20 15.90 0 -1 -31 3.90 8.90 0 -1 -31 0.70 14.30 0 1 -31 -1.40 9.40 0 1 31 38.70 18.30 0 1 31 4.70 11.00 0 1 -31 17.60 14.90 -1 -1 -31 23.70 16.10 1 -1 31 5.10 10.90 -1 -1 -31 30.30 17.50 -1 -1 -31 29.20 10.30 1 1 31 -4.70 10.90 -1 1 -31 34.00 15.80 -1 1 -31 14.20 11.40 1 1 31 9.80 19.50 -2 -1 -31 43.40 18.10 -2 -1 -31 7.70 10.10 -2 -1 -31 74.79 16.60 2 -1 31 30.60 14.70 -2 1 -31 72.79 18.70 -2 1 -31 31.80 13.00 2 1 31 20.60 20.10 2 1 31 10.80 12.00 3 -1 31 27.30 13.90 -3 -1 -31 17.50 17.20 -3 -1 -31 31.30 12.00 -3 -1 -31 13.60 14.00 3 1 31 15.60 12.30 3 1 31 24.60 20.80 -3 1 -31 14.80 12.70 -3 1 -31 20.30 15.80 5 -2 -31 17.20 15.60 5 -2 -31 35.40 20.00 -5 -2 31 40.90 14.40 -5 2 31 33.80 17.60 5 2 -31 37.80 14.40 5 2 -31 30.80 13.20 4 -2 -31 70.59 20.10 4 -2 -31 42.20 19.80 -4 -2 31 36.20 14.30 -4 2 31 67.09 20.10 4 2 -31 33.20 14.80 4 2 -31 64.19 16.80 3 -2 -31 70.29 22.00 -3 -2 31 181.68 20.50 3 -2 -31 107.09 24.30 3 2 -31 122.29 20.50 -3 2 31 120.09 24.30 3 2 -31 125.59 16.90 2 -2 -31 14.90 14.90 2 -2 -31 9.70 14.90 -2 -2 31 11.40 12.00 -2 2 31 11.40 16.30 2 2 -31 21.20 13.80 2 2 -31 13.00 12.20 1 -2 -31 91.19 23.40 -1 -2 31 102.49 20.50 1 -2 -31 129.79 27.00 1 2 -31 95.39 18.70 -1 2 31 104.09 24.40 1 2 -31 144.69 18.70 8 0 -32 41.60 16.00 -8 0 32 18.50 20.80 8 0 -32 -6.80 14.90 8 0 -32 7.80 11.80 7 0 -32 0.70 14.50 7 0 -32 26.20 15.00 -7 0 32 1.80 18.30 -7 0 32 -4.10 10.40 7 0 -32 8.40 10.90 6 0 -32 113.79 21.70 6 0 -32 146.69 19.60 -6 0 32 93.09 18.30 6 0 -32 105.99 15.50 5 0 -32 29.10 14.30 5 0 -32 41.90 16.30 -5 0 32 62.09 22.40 -5 0 32 31.00 14.30 4 0 -32 83.39 16.10 4 0 -32 114.19 21.20 -4 0 32 96.89 17.90 -4 0 32 61.99 24.30 4 0 -32 86.49 18.70 -3 0 32 179.48 19.60 3 0 -32 230.58 21.90 3 0 -32 214.78 22.70 -3 0 32 246.28 28.10 2 0 -32 72.19 17.80 2 0 -32 88.79 21.70 2 0 -32 55.79 13.60 -2 0 32 75.89 25.40 -2 0 32 48.60 14.80 1 0 -32 31.90 17.80 1 0 -32 40.70 13.40 -1 0 32 70.49 23.80 1 0 -32 54.49 15.80 -1 0 32 52.39 15.10 0 0 -32 104.89 22.90 0 0 32 85.29 17.70 0 0 -32 107.39 18.00 0 0 32 116.29 26.10 1 0 32 -10.80 10.70 1 0 32 12.30 19.30 -1 0 -32 5.80 9.60 -1 0 -32 18.40 16.10 -2 0 -32 127.99 16.50 -2 0 -32 150.78 22.20 2 0 32 99.49 17.70 7 -1 -32 102.39 14.90 7 -1 -32 54.99 19.50 7 -1 -32 57.69 21.10 -7 -1 32 84.09 17.40 -7 1 32 50.79 21.30 7 1 -32 85.49 17.70 7 1 -32 78.29 19.90 7 1 -32 59.79 16.20 6 -1 -32 -12.10 13.40 6 -1 -32 -6.60 9.30 6 -1 -32 20.70 16.30 -6 -1 32 23.70 14.30 6 1 -32 7.80 14.10 6 1 -32 -6.20 9.80 -6 1 32 20.70 19.40 -5 -1 32 120.39 17.90 5 -1 -32 106.39 22.50 5 -1 -32 153.48 21.60 5 -1 -32 101.39 13.90 5 1 -32 156.58 18.20 -5 1 32 175.48 24.80 5 1 -32 147.19 17.30 4 -1 -32 142.09 21.20 4 -1 -32 62.29 13.50 4 -1 -32 92.69 21.60 -4 -1 32 109.29 18.10 4 1 -32 101.19 18.70 -4 1 32 121.19 26.40 -4 1 32 80.39 15.70 4 1 -32 94.39 17.10 4 1 -32 115.79 20.60 3 -1 -32 62.39 20.40 -3 -1 32 -0.30 9.80 3 -1 -32 12.60 15.50 3 -1 -32 3.60 9.50 -3 1 32 14.30 19.20 3 1 -32 39.60 21.40 -3 1 32 11.80 11.60 3 1 -32 42.30 14.20 3 1 -32 29.00 16.00 2 -1 -32 101.89 22.20 -2 -1 32 118.29 20.20 2 -1 -32 75.09 22.30 2 -1 -32 106.29 14.60 2 1 -32 90.99 20.60 2 1 -32 142.99 17.80 -2 1 32 126.99 27.50 -2 1 32 89.29 17.20 1 -1 -32 18.80 13.20 1 -1 -32 -7.40 9.00 -1 -1 32 0.40 11.70 1 1 -32 12.40 10.50 1 1 -32 -6.70 14.80 -1 1 32 27.20 18.20 -1 1 32 -2.30 10.60 0 -1 32 2.00 11.40 0 -1 -32 9.10 9.70 0 -1 -32 18.30 16.00 0 -1 -32 21.10 18.40 0 1 -32 1.90 14.40 0 1 32 15.80 19.20 0 1 -32 -7.80 9.70 0 1 32 -9.50 11.60 -1 -1 -32 77.19 15.00 -1 -1 -32 100.39 22.10 -1 -1 -32 76.39 18.70 1 -1 32 56.89 16.00 -1 1 -32 81.79 19.30 1 1 32 57.09 15.70 1 1 32 47.80 23.00 6 0 -33 -3.80 9.70 6 0 -33 54.69 17.10 6 0 -33 23.50 17.50 -6 0 33 9.30 11.90 -6 0 33 15.60 21.70 -5 0 33 22.90 22.80 5 0 -33 16.60 11.80 5 0 -33 55.49 18.90 5 0 -33 -8.40 11.90 -5 0 33 5.60 11.40 4 0 -33 20.50 10.30 -4 0 33 -20.90 11.50 4 0 -33 74.39 18.40 4 0 -33 8.90 13.90 -3 0 33 75.59 28.70 2 0 -33 8.30 11.20 -2 0 33 34.10 13.60 -2 0 33 16.60 21.60 2 0 -33 2.10 13.50 2 0 -33 -6.20 15.50 1 0 -33 8.80 11.30 1 0 -33 -20.20 12.60 1 0 -33 4.40 11.80 -1 0 33 7.20 19.60 -1 0 33 8.00 12.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 855 _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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.17616(3) 0.83659(13) 0.72035(2) 0.03605(15) Uani 1 1 d . . . . . O1 O 0.6006(2) 0.9245(6) 0.33819(12) 0.0305(8) Uani 1 1 d . . . . . N1 N 0.5333(3) 0.4971(9) 0.31956(16) 0.0298(9) Uani 1 1 d D . . . . H1 H 0.541(3) 0.317(5) 0.322(2) 0.045 Uiso 1 1 d D U . . . N2 N 0.6723(2) 0.5079(8) 0.35886(15) 0.0256(9) Uani 1 1 d D . . . . H2 H 0.666(3) 0.327(5) 0.3594(19) 0.038 Uiso 1 1 d D U . . . N3 N 0.8232(2) 0.6479(11) 0.59653(14) 0.0356(10) Uani 1 1 d . . . . . C1 C 0.6020(3) 0.6536(10) 0.33876(15) 0.0217(9) Uani 1 1 d . . . . . C2 C 0.7530(3) 0.6415(11) 0.37881(16) 0.0269(10) Uani 1 1 d . . . . . H2A H 0.752650 0.841254 0.365779 0.032 Uiso 1 1 calc R U . . . H2B H 0.799061 0.535740 0.365886 0.032 Uiso 1 1 calc R U . . . C3 C 0.7733(3) 0.6498(10) 0.43587(15) 0.0245(9) Uani 1 1 d . . . . . C4 C 0.8477(3) 0.5319(11) 0.46237(17) 0.0294(11) Uani 1 1 d . . . . . H4 H 0.887974 0.448947 0.444033 0.035 Uiso 1 1 calc R U . . . C5 C 0.8649(3) 0.5317(11) 0.51495(17) 0.0299(11) Uani 1 1 d . . . . . H5 H 0.916363 0.448161 0.532011 0.036 Uiso 1 1 calc R U . . . C6 C 0.8084(3) 0.6507(12) 0.54245(16) 0.0313(11) Uani 1 1 d . . . . . C7 C 0.7340(3) 0.7715(13) 0.51649(18) 0.0434(15) Uani 1 1 d . . . . . H7 H 0.694168 0.856906 0.534871 0.052 Uiso 1 1 calc R U . . . C8 C 0.7173(3) 0.7690(11) 0.46405(18) 0.0379(13) Uani 1 1 d . . . . . H8 H 0.665643 0.851906 0.447051 0.045 Uiso 1 1 calc R U . . . C9 C 0.9068(3) 0.6851(11) 0.62400(16) 0.0280(10) Uani 1 1 d . . . . . C10 C 0.9636(3) 0.8724(12) 0.60743(18) 0.0389(13) Uani 1 1 d . . . . . H10 H 0.947133 0.973380 0.576436 0.047 Uiso 1 1 calc R U . . . C11 C 1.0443(3) 0.9155(11) 0.63532(18) 0.0354(12) Uani 1 1 d . . . . . H11 H 1.082752 1.047169 0.623889 0.043 Uiso 1 1 calc R U . . . C12 C 1.0678(3) 0.7657(10) 0.67962(16) 0.0267(10) Uani 1 1 d . . . . . C13 C 1.0136(3) 0.5729(11) 0.69639(16) 0.0301(11) Uani 1 1 d . . . . . H13 H 1.030977 0.469289 0.727010 0.036 Uiso 1 1 calc R U . . . C14 C 0.9330(3) 0.5302(12) 0.66826(17) 0.0322(11) Uani 1 1 d . . . . . H14 H 0.895429 0.393927 0.679346 0.039 Uiso 1 1 calc R U . . . C15 C 0.7545(3) 0.5897(10) 0.62310(17) 0.0288(11) Uani 1 1 d . . . . . C16 C 0.7470(3) 0.7339(11) 0.66713(17) 0.0309(11) Uani 1 1 d . . . . . H16 H 0.787251 0.878837 0.679733 0.037 Uiso 1 1 calc R U . . . C17 C 0.6805(3) 0.6677(12) 0.69327(17) 0.0345(11) Uani 1 1 d . . . . . H17 H 0.676513 0.767391 0.723818 0.041 Uiso 1 1 calc R U . . . C18 C 0.6200(3) 0.4592(10) 0.67566(17) 0.0271(10) Uani 1 1 d . . . . . C19 C 0.6274(4) 0.3228(14) 0.6305(2) 0.0508(15) Uani 1 1 d . . . . . H19 H 0.586185 0.182710 0.617020 0.061 Uiso 1 1 calc R U . . . C20 C 0.6936(4) 0.3872(13) 0.6049(2) 0.0504(16) Uani 1 1 d . . . . . H20 H 0.697276 0.289885 0.574055 0.060 Uiso 1 1 calc R U . . . C21 C 0.5483(3) 0.3876(11) 0.70374(17) 0.0300(11) Uani 1 1 d . . . . . H21A H 0.543493 0.175488 0.705984 0.036 Uiso 1 1 calc R U . . . H21B H 0.562426 0.463383 0.738751 0.036 Uiso 1 1 calc R U . . . S1S S 0.4736(6) 0.898(2) 0.4915(4) 0.089(3) Uiso 0.268(6) 1 d D . P A -1 O1S O 0.4855(11) 1.198(3) 0.4902(6) 0.056(5) Uiso 0.268(6) 1 d D . P A -1 C1S C 0.5256(17) 0.613(5) 0.4671(9) 0.074(8) Uiso 0.268(6) 1 d D . P A -1 H1SA H 0.587322 0.630221 0.478558 0.112 Uiso 0.268(6) 1 calc R U P A -1 H1SB H 0.513317 0.618435 0.430002 0.112 Uiso 0.268(6) 1 calc R U P A -1 H1SC H 0.505368 0.430372 0.479170 0.112 Uiso 0.268(6) 1 calc R U P A -1 C2S C 0.472(2) 0.761(7) 0.5527(8) 0.088(8) Uiso 0.268(6) 1 d D . P A -1 H2SA H 0.459198 0.917014 0.574971 0.133 Uiso 0.268(6) 1 calc R U P A -1 H2SB H 0.528062 0.678414 0.566257 0.133 Uiso 0.268(6) 1 calc R U P A -1 H2SC H 0.428225 0.611267 0.551010 0.133 Uiso 0.268(6) 1 calc R U P A -1 S2S S 0.4575(14) 0.651(6) 0.4970(8) 0.071(8) Uiso 0.090(6) 1 d D . P B -2 O2S O 0.478(4) 0.665(14) 0.5537(9) 0.088(8) Uiso 0.090(6) 1 d D . P B -2 C3S C 0.512(5) 0.940(11) 0.473(3) 0.07(2) Uiso 0.090(6) 1 d D . P B -2 H3SA H 0.478542 1.009884 0.441293 0.106 Uiso 0.090(6) 1 calc R U P B -2 H3SB H 0.568003 0.873061 0.466697 0.106 Uiso 0.090(6) 1 calc R U P B -2 H3SC H 0.520332 1.097106 0.497912 0.106 Uiso 0.090(6) 1 calc R U P B -2 C4S C 0.519(4) 0.370(10) 0.476(2) 0.043(17) Uiso 0.090(6) 1 d D . P B -2 H4SA H 0.485689 0.191024 0.473482 0.064 Uiso 0.090(6) 1 calc R U P B -2 H4SB H 0.571411 0.343844 0.500911 0.064 Uiso 0.090(6) 1 calc R U P B -2 H4SC H 0.533355 0.419838 0.443181 0.064 Uiso 0.090(6) 1 calc R U P B -2 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 0.0349(3) 0.0508(3) 0.0229(2) -0.0028(3) 0.00616(18) -0.0062(3) O1 0.0364(19) 0.0108(16) 0.0398(19) 0.0000(14) -0.0070(15) -0.0007(14) N1 0.024(2) 0.020(2) 0.042(2) -0.004(2) -0.0054(17) 0.0006(18) N2 0.025(2) 0.021(2) 0.029(2) 0.0021(18) -0.0014(16) 0.0004(18) N3 0.033(2) 0.049(3) 0.0236(19) -0.003(2) 0.0032(16) 0.002(2) C1 0.026(2) 0.017(2) 0.021(2) -0.003(2) 0.0009(17) -0.004(2) C2 0.024(2) 0.027(3) 0.028(2) 0.000(2) 0.0024(18) -0.002(2) C3 0.027(2) 0.020(2) 0.026(2) 0.000(2) 0.0015(18) -0.001(2) C4 0.028(2) 0.032(3) 0.028(2) 0.003(2) 0.006(2) 0.005(2) C5 0.030(3) 0.032(3) 0.027(2) 0.007(2) 0.002(2) 0.008(2) C6 0.036(3) 0.029(3) 0.027(2) 0.000(2) 0.002(2) -0.003(2) C7 0.046(3) 0.052(4) 0.031(3) -0.017(3) 0.001(2) 0.022(3) C8 0.039(3) 0.037(3) 0.034(3) -0.009(2) -0.004(2) 0.016(2) C9 0.033(2) 0.027(3) 0.023(2) -0.001(2) 0.0049(19) 0.007(2) C10 0.058(3) 0.027(3) 0.028(2) 0.005(2) -0.005(2) -0.006(3) C11 0.045(3) 0.028(3) 0.033(3) 0.004(2) 0.004(2) -0.010(2) C12 0.030(2) 0.028(3) 0.023(2) -0.0029(19) 0.0070(19) 0.002(2) C13 0.029(2) 0.040(3) 0.021(2) 0.009(2) 0.0061(19) 0.008(2) C14 0.031(3) 0.040(3) 0.029(2) 0.006(2) 0.013(2) 0.001(2) C15 0.031(3) 0.026(3) 0.028(2) -0.006(2) 0.003(2) 0.003(2) C16 0.023(2) 0.033(3) 0.035(2) -0.010(2) -0.0016(19) -0.001(2) C17 0.025(2) 0.045(3) 0.032(2) -0.012(3) -0.0001(19) 0.001(3) C18 0.027(2) 0.023(2) 0.031(2) -0.003(2) 0.0002(19) 0.003(2) C19 0.062(4) 0.048(4) 0.043(3) -0.018(3) 0.010(3) -0.025(3) C20 0.072(4) 0.046(4) 0.038(3) -0.024(3) 0.024(3) -0.022(3) C21 0.024(2) 0.026(3) 0.037(3) -0.001(2) -0.002(2) 0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 N1 H1 115(4) . . ? C1 N1 C21 125.4(4) . 3_666 ? C21 N1 H1 120(4) 3_666 . ? C1 N2 H2 114(4) . . ? C1 N2 C2 124.1(4) . . ? C2 N2 H2 121(4) . . ? C9 N3 C6 120.4(4) . . ? C9 N3 C15 119.6(4) . . ? C15 N3 C6 119.8(4) . . ? O1 C1 N1 121.7(4) . . ? O1 C1 N2 121.4(4) . . ? N1 C1 N2 116.8(4) . . ? N2 C2 H2A 108.7 . . ? N2 C2 H2B 108.7 . . ? N2 C2 C3 114.3(4) . . ? H2A C2 H2B 107.6 . . ? C3 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C4 C3 C2 121.9(4) . . ? C8 C3 C2 121.1(4) . . ? C8 C3 C4 117.0(4) . . ? C3 C4 H4 119.1 . . ? C3 C4 C5 121.7(4) . . ? C5 C4 H4 119.1 . . ? C4 C5 H5 119.7 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C5 C6 N3 122.0(4) . . ? C5 C6 C7 118.4(4) . . ? C7 C6 N3 119.6(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 C6 120.6(5) . . ? C8 C7 H7 119.7 . . ? C3 C8 C7 121.8(5) . . ? C3 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 N3 121.1(4) . . ? C10 C9 C14 118.8(4) . . ? C14 C9 N3 120.0(4) . . ? C9 C10 H10 119.5 . . ? C9 C10 C11 120.9(4) . . ? C11 C10 H10 119.5 . . ? C10 C11 H11 120.5 . . ? C12 C11 C10 119.1(5) . . ? C12 C11 H11 120.5 . . ? C11 C12 Br1 119.8(4) . . ? C13 C12 Br1 118.9(3) . . ? C13 C12 C11 121.3(4) . . ? C12 C13 H13 120.3 . . ? C12 C13 C14 119.3(4) . . ? C14 C13 H13 120.3 . . ? C9 C14 H14 119.8 . . ? C13 C14 C9 120.5(5) . . ? C13 C14 H14 119.8 . . ? C16 C15 N3 121.1(4) . . ? C16 C15 C20 118.6(5) . . ? C20 C15 N3 120.3(4) . . ? C15 C16 H16 119.9 . . ? C15 C16 C17 120.1(5) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 119.2 . . ? C18 C17 C16 121.5(4) . . ? C18 C17 H17 119.2 . . ? C17 C18 C21 121.6(4) . . ? C19 C18 C17 117.3(5) . . ? C19 C18 C21 121.1(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 C18 121.1(5) . . ? C20 C19 H19 119.5 . . ? C15 C20 C19 121.3(5) . . ? C15 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? N1 C21 C18 113.7(4) 3_666 . ? N1 C21 H21A 108.8 3_666 . ? N1 C21 H21B 108.8 3_666 . ? C18 C21 H21A 108.8 . . ? C18 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? O1S S1S C1S 132.0(13) . . ? O1S S1S C2S 113.9(13) . . ? C1S S1S C2S 98.8(14) . . ? S1S C1S H1SA 109.5 . . ? S1S C1S H1SB 109.5 . . ? S1S C1S H1SC 109.5 . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? S1S C2S H2SA 109.5 . . ? S1S C2S H2SB 109.5 . . ? S1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O2S S2S C3S 107(2) . . ? O2S S2S C4S 108(2) . . ? C4S S2S C3S 96.7(19) . . ? S2S C3S H3SA 109.5 . . ? S2S C3S H3SB 109.5 . . ? S2S C3S H3SC 109.5 . . ? H3SA C3S H3SB 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? S2S C4S H4SA 109.5 . . ? S2S C4S H4SB 109.5 . . ? S2S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 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 C12 1.906(5) . ? O1 C1 1.257(5) . ? N1 H1 0.85(2) . ? N1 C1 1.339(6) . ? N1 C21 1.443(6) 3_666 ? N2 H2 0.85(2) . ? N2 C1 1.339(6) . ? N2 C2 1.443(6) . ? N3 C6 1.426(6) . ? N3 C9 1.417(6) . ? N3 C15 1.423(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.506(6) . ? C3 C4 1.385(6) . ? C3 C8 1.374(6) . ? C4 H4 0.9500 . ? C4 C5 1.387(6) . ? C5 H5 0.9500 . ? C5 C6 1.367(7) . ? C6 C7 1.385(7) . ? C7 H7 0.9500 . ? C7 C8 1.383(7) . ? C8 H8 0.9500 . ? C9 C10 1.377(7) . ? C9 C14 1.388(6) . ? C10 H10 0.9500 . ? C10 C11 1.386(7) . ? C11 H11 0.9500 . ? C11 C12 1.371(6) . ? C12 C13 1.368(7) . ? C13 H13 0.9500 . ? C13 C14 1.386(6) . ? C14 H14 0.9500 . ? C15 C16 1.376(6) . ? C15 C20 1.378(7) . ? C16 H16 0.9500 . ? C16 C17 1.394(7) . ? C17 H17 0.9500 . ? C17 C18 1.390(7) . ? C18 C19 1.384(7) . ? C18 C21 1.501(6) . ? C19 H19 0.9500 . ? C19 C20 1.381(8) . ? C20 H20 0.9500 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? S1S O1S 1.405(12) . ? S1S C1S 1.743(16) . ? S1S C2S 1.759(16) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? S2S O2S 1.498(15) . ? S2S C3S 1.77(2) . ? S2S C4S 1.771(19) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 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 _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 O1 0.85(2) 2.07(3) 2.877(5) 160(5) 1_545 yes N2 H2 O1 0.85(2) 2.17(3) 2.954(5) 155(5) 1_545 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 C12 C13 C14 176.9(4) . . . . ? N2 C2 C3 C4 123.8(5) . . . . ? N2 C2 C3 C8 -54.5(7) . . . . ? N3 C6 C7 C8 -178.1(5) . . . . ? N3 C9 C10 C11 177.8(5) . . . . ? N3 C9 C14 C13 -177.6(5) . . . . ? N3 C15 C16 C17 -178.2(5) . . . . ? N3 C15 C20 C19 178.7(6) . . . . ? C1 N2 C2 C3 104.3(5) . . . . ? C2 N2 C1 O1 -3.6(7) . . . . ? C2 N2 C1 N1 176.7(4) . . . . ? C2 C3 C4 C5 -177.9(5) . . . . ? C2 C3 C8 C7 178.3(5) . . . . ? C3 C4 C5 C6 -0.4(8) . . . . ? C4 C3 C8 C7 -0.1(8) . . . . ? C4 C5 C6 N3 178.5(5) . . . . ? C4 C5 C6 C7 -0.2(8) . . . . ? C5 C6 C7 C8 0.6(9) . . . . ? C6 N3 C9 C10 37.2(7) . . . . ? C6 N3 C9 C14 -142.4(5) . . . . ? C6 N3 C15 C16 -141.7(5) . . . . ? C6 N3 C15 C20 38.0(7) . . . . ? C6 C7 C8 C3 -0.4(9) . . . . ? C8 C3 C4 C5 0.5(8) . . . . ? C9 N3 C6 C5 37.3(8) . . . . ? C9 N3 C6 C7 -144.1(5) . . . . ? C9 N3 C15 C16 42.2(7) . . . . ? C9 N3 C15 C20 -138.1(5) . . . . ? C9 C10 C11 C12 0.9(8) . . . . ? C10 C9 C14 C13 2.8(7) . . . . ? C10 C11 C12 Br1 -176.7(4) . . . . ? C10 C11 C12 C13 0.7(8) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C12 C13 C14 C9 -1.2(7) . . . . ? C14 C9 C10 C11 -2.7(8) . . . . ? C15 N3 C6 C5 -138.8(5) . . . . ? C15 N3 C6 C7 39.8(8) . . . . ? C15 N3 C9 C10 -146.7(5) . . . . ? C15 N3 C9 C14 33.7(7) . . . . ? C15 C16 C17 C18 -0.7(8) . . . . ? C16 C15 C20 C19 -1.6(9) . . . . ? C16 C17 C18 C19 -1.1(8) . . . . ? C16 C17 C18 C21 -180.0(4) . . . . ? C17 C18 C19 C20 1.6(9) . . . . ? C17 C18 C21 N1 104.7(5) . . . 3_666 ? C18 C19 C20 C15 -0.2(10) . . . . ? C19 C18 C21 N1 -74.2(6) . . . 3_666 ? C20 C15 C16 C17 2.1(7) . . . . ? C21 N1 C1 O1 0.4(7) 3_666 . . . ? C21 N1 C1 N2 -179.9(4) 3_666 . . . ? C21 C18 C19 C20 -179.5(5) . . . . ?