#------------------------------------------------------------------------------ #$Date: 2021-06-18 00:30:25 +0300 (Fri, 18 Jun 2021) $ #$Revision: 266539 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/88/4518826.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_4518826 loop_ _publ_author_name 'Wang, Lixian' 'Lin, Jin' 'Sun, Qiangsheng' 'Xia, Chungu' 'Sun, Wei' _publ_section_title ; Amino Acid Derived Chiral Aminobenzimidazole Manganese Catalysts for Asymmetric Transfer Hydrogenation of Ketones ; _journal_name_full 'ACS Catalysis' _journal_page_first 8033 _journal_page_last 8041 _journal_paper_doi 10.1021/acscatal.1c00616 _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_sum 'C16 H19 Br Mn N3 O3' _chemical_formula_weight 436.19 _space_group_crystal_system hexagonal _space_group_IT_number 170 _space_group_name_Hall 'P 65' _space_group_name_H-M_alt 'P 65' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 12 _cell_length_a 10.2602(9) _cell_length_b 10.2602(9) _cell_length_c 61.043(5) _cell_measurement_reflns_used 9850 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 27.59 _cell_measurement_theta_min 2.32 _cell_volume 5565.2(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 153(2) _diffrn_detector_area_resol_mean 'fine-focus sealed tube' _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_unetI/netI 0.0502 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.962 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_limit_l_min -83 _diffrn_reflns_number 46178 _diffrn_reflns_point_group_measured_fraction_full 0.893 _diffrn_reflns_point_group_measured_fraction_max 0.843 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.100 _diffrn_reflns_theta_min 2.292 _exptl_absorpt_coefficient_mu 2.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.562 _exptl_crystal_description block _exptl_crystal_F_000 2640 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_transmission_factor_max 0.7458 _exptl_transmission_factor_min 0.3394 _refine_diff_density_max 1.051 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.092 _refine_ls_abs_structure_details ; Flack x determined using 2815 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 441 _refine_ls_number_reflns 8368 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0390 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.1816P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1022 _refine_ls_wR_factor_ref 0.1068 _reflns_Friedel_coverage 0.737 _reflns_Friedel_fraction_full 0.803 _reflns_Friedel_fraction_max 0.721 _reflns_number_gt 7612 _reflns_number_total 8368 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c00616_si_002.cif _cod_data_source_block 1_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 5565.2(11) _cod_database_code 4518826 _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_min 0.478 _shelx_estimated_absorpt_t_max 0.596 _shelx_res_file ; 1_a.res created by SHELXL-2014/7 TITL 1_a.res in P6(5) CELL 0.71073 10.2602 10.2602 61.0434 90.000 90.000 120.000 ZERR 12.000 0.0009 0.0009 0.0051 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, 2/3+Z SYMM -X+Y, -X, 1/3+Z SYMM -X, -Y, 1/2+Z SYMM Y, -X+Y, 1/6+Z SYMM X-Y, X, 5/6+Z SFAC C H Mn N O Br UNIT 192 228 12 36 36 12 omit 0 3 -55 omit -4 6 -14 omit -2 7 -21 omit -1 4 -28 omit 0 1 5 omit -1 4 -51 omit 0 2 -37 omit -1 3 -48 omit -3 4 -53 omit 0 2 -53 omit 0 1 -39 omit 0 3 -48 omit -2 7 -51 omit 0 5 -40 omit -5 6 -56 omit -1 7 -50 omit -5 6 -32 omit 0 3 -36 omit -2 4 -52 omit 0 4 -57 omit -4 10 -46 omit -3 6 -61 omit -3 7 -31 omit -3 6 -70 omit -2 7 -46 omit -1 4 -58 omit -3 5 -41 omit -3 7 -42 omit -6 9 -43 omit -3 6 -28 omit -3 6 -59 omit -7 10 -50 omit -1 7 -28 omit -1 5 -12 omit -4 5 -59 omit -4 9 -31 omit 0 10 -27 omit -7 9 -36 omit 0 1 -73 omit -4 8 -54 omit 0 8 -36 omit -3 4 -43 omit -5 6 -64 omit -2 3 -55 omit 0 1 -27 omit -3 8 -29 omit 0 1 -47 omit -2 3 -51 omit -2 3 -37 omit -1 3 -53 omit -1 2 -43 omit 0 3 -60 omit 0 1 -42 omit -3 4 -56 omit -1 3 -61 omit 0 2 -47 omit -2 3 -53 omit -1 4 -53 omit 0 1 -36 omit -6 7 -39 omit -6 9 -45 omit -3 5 -58 omit 0 1 -54 omit 0 6 -62 omit 0 2 -49 omit -2 3 -60 omit -1 5 -54 omit -1 6 -42 omit -1 3 -50 omit -3 4 -50 omit -2 3 -49 omit 0 3 -78 omit 0 1 -33 omit -5 8 -34 omit -2 7 -65 omit 0 1 -57 omit 0 4 -67 omit 0 1 -69 omit 0 7 -38 omit -1 4 -38 omit 0 1 -45 omit -1 5 -68 omit -3 8 -47 omit 0 3 -57 omit 0 3 -45 omit 0 6 -60 omit -1 2 -59 omit -1 7 -52 omit -1 4 -43 omit -2 5 -49 omit -7 8 -52 omit -6 9 -39 omit -2 4 -54 omit -3 5 -72 omit 0 2 -63 omit 0 3 -2 omit 0 1 -5 L.S. 50 ACTA BOND $H FMAP 2 PLAN 20 CONF SIZE 0.30 0.20 0.20 ISOR 0.01 C19 TEMP -120.000 WGHT 0.075000 0.181600 FVAR 0.31759 MN1 3 0.327107 0.223811 0.514182 11.00000 0.01720 0.02255 = 0.01531 0.00380 0.00135 0.01163 MN2 3 -0.042420 0.410196 0.443986 11.00000 0.01577 0.01322 = 0.01572 0.00079 -0.00307 0.00449 BR1 6 0.459802 0.445858 0.541133 11.00000 0.02121 0.02725 = 0.02290 -0.00038 -0.00253 0.00622 BR2 6 0.030914 0.240372 0.464660 11.00000 0.04120 0.02473 = 0.02007 0.00149 -0.00674 0.01957 C1 1 0.291028 0.023167 0.555968 11.00000 0.01860 0.01658 = 0.01612 0.00469 -0.00288 0.00670 C2 1 0.414202 0.001348 0.555278 11.00000 0.02307 0.02027 = 0.02557 0.00609 0.00019 0.01248 AFIX 43 H2 2 0.479440 0.031327 0.542956 11.00000 -1.20000 AFIX 0 C3 1 0.437599 -0.065905 0.573313 11.00000 0.03252 0.02978 = 0.03285 0.00615 -0.00708 0.02217 AFIX 43 H3 2 0.520208 -0.083377 0.573246 11.00000 -1.20000 AFIX 0 C4 1 0.343134 -0.109112 0.591699 11.00000 0.03570 0.02891 = 0.02072 0.00692 -0.00448 0.02021 AFIX 43 H4 2 0.363389 -0.155034 0.603731 11.00000 -1.20000 AFIX 0 C5 1 0.221298 -0.086554 0.592754 11.00000 0.03147 0.01971 = 0.02439 0.00703 0.00372 0.01110 AFIX 43 H5 2 0.157783 -0.114599 0.605257 11.00000 -1.20000 AFIX 0 C6 1 0.196567 -0.019867 0.574316 11.00000 0.01851 0.01659 = 0.01916 0.00045 -0.00395 0.00729 C7 1 0.114982 0.076809 0.549507 11.00000 0.01372 0.01858 = 0.01592 -0.00296 -0.00386 0.00618 C8 1 0.025696 0.131365 0.536898 11.00000 0.01274 0.02541 = 0.01973 -0.00207 -0.00493 0.01068 AFIX 13 H8 2 -0.002167 0.189337 0.547187 11.00000 -1.20000 AFIX 0 C9 1 -0.121560 0.005460 0.526233 11.00000 0.01456 0.02528 = 0.01975 -0.00149 -0.00616 0.00612 C10 1 -0.089873 -0.075390 0.507887 11.00000 0.02375 0.02372 = 0.03426 -0.00607 -0.00806 0.00899 AFIX 137 H10A 2 -0.031483 -0.119554 0.513671 11.00000 -1.50000 H10B 2 -0.032476 -0.003407 0.496267 11.00000 -1.50000 H10C 2 -0.185262 -0.155254 0.501911 11.00000 -1.50000 AFIX 0 C11 1 -0.206883 0.082375 0.517538 11.00000 0.01520 0.04483 = 0.03885 -0.00405 -0.00887 0.01633 AFIX 137 H11A 2 -0.145465 0.157351 0.506472 11.00000 -1.50000 H11B 2 -0.227526 0.132083 0.529658 11.00000 -1.50000 H11C 2 -0.302067 0.006739 0.510939 11.00000 -1.50000 AFIX 0 C12 1 -0.220476 -0.110953 0.543433 11.00000 0.01689 0.04041 = 0.03095 -0.00087 -0.00464 -0.00136 AFIX 137 H12A 2 -0.315476 -0.185629 0.536677 11.00000 -1.50000 H12B 2 -0.241266 -0.060370 0.555414 11.00000 -1.50000 H12C 2 -0.167963 -0.161330 0.549212 11.00000 -1.50000 AFIX 0 C13 1 0.257873 0.075715 0.493964 11.00000 0.02949 0.02977 = 0.02550 0.00330 0.00457 0.01540 C14 1 0.394578 0.356628 0.491864 11.00000 0.02951 0.02819 = 0.02357 0.00469 0.00303 0.01686 C15 1 0.505190 0.231198 0.513761 11.00000 0.03658 0.04462 = 0.02292 0.01667 0.00957 0.02946 C16 1 -0.022423 0.007879 0.586052 11.00000 0.01388 0.03446 = 0.02390 0.00359 0.00444 0.00740 AFIX 137 H16A 2 -0.061302 0.073958 0.581682 11.00000 -1.50000 H16B 2 0.026258 0.039225 0.600410 11.00000 -1.50000 H16C 2 -0.105712 -0.096169 0.586912 11.00000 -1.50000 AFIX 0 C17 1 0.211637 0.655142 0.498711 11.00000 0.03900 0.02244 = 0.02429 -0.00447 -0.00848 0.00888 C18 1 0.228234 0.683174 0.521287 11.00000 0.05872 0.03932 = 0.01472 -0.00963 -0.01042 0.01012 AFIX 43 H18 2 0.324442 0.728200 0.528055 11.00000 -1.20000 AFIX 0 C19 1 0.101010 0.643417 0.533238 11.00000 0.08138 0.04889 = 0.02081 -0.00719 -0.00352 0.01497 AFIX 43 H19 2 0.109068 0.661368 0.548579 11.00000 -1.20000 AFIX 0 C20 1 -0.041028 0.576697 0.523285 11.00000 0.06342 0.03143 = 0.03482 -0.00062 0.01913 0.01128 AFIX 43 H20 2 -0.126966 0.552911 0.531964 11.00000 -1.20000 AFIX 0 C21 1 -0.058916 0.544716 0.501130 11.00000 0.03804 0.02680 = 0.03368 -0.00379 0.00968 0.00705 AFIX 43 H21 2 -0.155846 0.496485 0.494564 11.00000 -1.20000 AFIX 0 C22 1 0.070138 0.585634 0.488732 11.00000 0.03973 0.01659 = 0.02176 -0.00478 0.00045 0.01145 C23 1 0.236699 0.630803 0.463206 11.00000 0.02445 0.01329 = 0.02546 -0.00734 -0.00634 0.00582 C24 1 0.477034 0.750301 0.485976 11.00000 0.03247 0.05184 = 0.04248 -0.01395 -0.02329 0.00941 AFIX 137 H24A 2 0.520941 0.718734 0.474316 11.00000 -1.50000 H24B 2 0.494418 0.717022 0.500174 11.00000 -1.50000 H24C 2 0.524203 0.860224 0.485912 11.00000 -1.50000 AFIX 0 C25 1 0.297427 0.629891 0.441082 11.00000 0.02069 0.02148 = 0.01606 -0.00814 -0.00769 0.01077 AFIX 13 H25 2 0.381820 0.608520 0.442899 11.00000 -1.20000 AFIX 0 C26 1 0.358004 0.780467 0.427366 11.00000 0.01915 0.01529 = 0.03024 -0.00212 0.00009 0.00444 C27 1 0.472068 0.915666 0.441299 11.00000 0.02834 0.01741 = 0.04344 -0.00800 0.00174 -0.00351 AFIX 137 H27A 2 0.504030 1.009278 0.433185 11.00000 -1.50000 H27B 2 0.559909 0.904963 0.444454 11.00000 -1.50000 H27C 2 0.424516 0.918392 0.455082 11.00000 -1.50000 AFIX 0 C28 1 0.437229 0.768687 0.406995 11.00000 0.02911 0.02571 = 0.03307 0.00170 0.00933 0.01003 AFIX 137 H28A 2 0.363328 0.690729 0.397273 11.00000 -1.50000 H28B 2 0.513122 0.742202 0.411286 11.00000 -1.50000 H28C 2 0.486212 0.865550 0.399318 11.00000 -1.50000 AFIX 0 C29 1 0.229982 0.808406 0.421255 11.00000 0.02682 0.01803 = 0.04886 0.01054 0.00637 0.00997 AFIX 137 H29A 2 0.270541 0.903617 0.413239 11.00000 -1.50000 H29B 2 0.179725 0.813641 0.434603 11.00000 -1.50000 H29C 2 0.157368 0.725922 0.411993 11.00000 -1.50000 AFIX 0 C30 1 -0.101233 0.526823 0.430780 11.00000 0.01528 0.02136 = 0.02678 0.00080 -0.00235 0.00319 C31 1 -0.137279 0.266209 0.423739 11.00000 0.01970 0.01677 = 0.02456 0.00462 0.00172 0.00605 C32 1 -0.218404 0.323246 0.458358 11.00000 0.02569 0.02551 = 0.02808 -0.00136 -0.00437 0.01074 N1 4 0.236658 0.085431 0.540659 11.00000 0.01457 0.01723 = 0.02036 0.00137 -0.00162 0.00682 N2 4 0.087504 0.017783 0.569825 11.00000 0.01264 0.02386 = 0.02651 0.00188 -0.00120 0.00757 N3 4 0.132291 0.239021 0.520216 11.00000 0.01545 0.01766 = 0.02334 -0.00053 -0.00355 0.00796 AFIX 23 H3A 2 0.161622 0.334365 0.524701 11.00000 -1.20000 H3B 2 0.081695 0.223590 0.507361 11.00000 -1.20000 AFIX 0 N4 4 0.315308 0.683088 0.482289 11.00000 0.03362 0.02433 = 0.02292 -0.00839 -0.01375 0.00950 N5 4 0.089162 0.568574 0.466575 11.00000 0.02218 0.01663 = 0.01750 -0.00157 -0.00042 0.00823 N6 4 0.170941 0.498890 0.429218 11.00000 0.01552 0.01488 = 0.01892 -0.00196 -0.00122 0.00581 AFIX 23 H6A 2 0.193793 0.424102 0.428131 11.00000 -1.20000 H6B 2 0.165461 0.528680 0.415373 11.00000 -1.20000 AFIX 0 O1 5 0.228307 -0.011659 0.480611 11.00000 0.05548 0.04010 = 0.05209 -0.01390 0.00340 0.02279 O2 5 0.443505 0.438738 0.477583 11.00000 0.04712 0.04277 = 0.03038 0.01753 0.00910 0.02236 O3 5 0.623030 0.245779 0.513354 11.00000 0.03299 0.07705 = 0.05513 0.02983 0.01426 0.03937 O4 5 -0.336783 0.262111 0.466218 11.00000 0.02757 0.04389 = 0.03871 -0.00309 0.00762 0.00568 O5 5 -0.206113 0.169659 0.411345 11.00000 0.02703 0.02298 = 0.02358 -0.00649 -0.00538 0.00075 O6 5 -0.148039 0.597458 0.423194 11.00000 0.02294 0.02930 = 0.07004 0.01233 -0.01113 0.01224 HKLF 4 REM 1_a.res in P6(5) REM R1 = 0.0390 for 7612 Fo > 4sig(Fo) and 0.0479 for all 8368 data REM 441 parameters refined using 7 restraints END WGHT 0.0374 3.4660 REM Highest difference peak 1.051, deepest hole -0.881, 1-sigma level 0.092 Q1 1 0.4592 0.4459 0.5278 11.00000 0.05 1.05 Q2 1 0.0295 0.2370 0.4780 11.00000 0.05 1.00 Q3 1 0.0350 0.2457 0.4515 11.00000 0.05 0.87 Q4 1 0.4567 0.4424 0.5545 11.00000 0.05 0.81 Q5 1 0.3258 0.2148 0.5281 11.00000 0.05 0.72 Q6 1 -0.0394 0.4035 0.4577 11.00000 0.05 0.66 Q7 1 -0.0436 0.4091 0.4298 11.00000 0.05 0.64 Q8 1 0.3207 0.2240 0.5003 11.00000 0.05 0.64 Q9 1 0.0658 0.5717 0.4782 11.00000 0.05 0.37 Q10 1 -0.2053 0.0589 0.6140 11.00000 0.05 0.37 Q11 1 0.0463 0.1163 0.5502 11.00000 0.05 0.36 Q12 1 0.3990 0.1780 0.5125 11.00000 0.05 0.35 Q13 1 0.2624 0.1129 0.5112 11.00000 0.05 0.35 Q14 1 0.4799 0.3769 0.5404 11.00000 0.05 0.34 Q15 1 -0.1296 0.2026 0.5370 11.00000 0.05 0.34 Q16 1 -0.4608 -0.1150 0.5116 11.00000 0.05 0.34 Q17 1 0.5574 0.6776 0.4631 11.00000 0.05 0.33 Q18 1 -0.3324 0.5444 0.4929 11.00000 0.05 0.33 Q19 1 0.5961 0.6797 0.4825 11.00000 0.05 0.33 Q20 1 -0.0760 0.1533 0.4637 11.00000 0.05 0.32 ; _shelx_res_checksum 89113 _shelx_hkl_file ; 0 -1 0 8.70 2.00 0 -1 0 10.90 2.30 1 0 0 6.90 2.10 -1 1 0 13.60 1.80 -1 1 0 7.20 2.00 0 1 0 7.00 2.00 0 1 0 10.30 2.00 1 -1 0 9.70 2.30 -1 0 0 12.00 2.50 1 -2 0 21.10 4.70 1 1 0 23.20 4.20 -2 1 0 30.30 4.10 -1 2 0 35.70 4.70 2 -1 0 34.60 4.40 -1 -1 0 31.00 4.80 -1 -1 0 27.90 4.10 2 -1 0 28.70 4.50 0 -2 0 4204.08 284.27 -2 2 0 4104.89 276.77 -2 2 0 4282.97 283.97 2 0 0 4046.70 286.87 0 -2 0 4051.19 306.87 2 -2 0 3720.83 306.77 0 2 0 4287.27 276.67 -2 0 0 4047.80 284.87 0 2 0 4445.56 286.57 -3 1 0 498.25 34.10 2 -3 0 441.36 38.30 -3 1 0 465.25 35.70 1 2 0 503.45 35.50 -1 -2 0 523.25 37.80 -1 -2 0 471.65 35.50 -2 3 0 479.55 34.50 3 -1 0 526.85 37.40 3 -1 0 466.25 35.60 1 -3 0 4923.31 395.56 -3 2 0 5387.56 356.56 -3 2 0 5572.24 366.36 2 1 0 5171.38 369.56 3 -2 0 5514.45 395.26 3 -2 0 5458.85 369.46 -1 3 0 5454.75 356.76 -2 -1 0 5460.15 394.46 -2 -1 0 5030.30 366.96 0 -3 0 35.80 5.40 3 0 0 24.10 5.40 -3 3 0 37.80 5.70 -3 3 0 38.40 4.70 0 -3 0 28.40 6.10 3 -3 0 32.90 6.10 0 3 0 33.90 5.40 0 3 0 38.10 5.30 -3 0 0 32.00 6.40 3 -3 0 20.80 4.30 1 3 0 978.60 67.69 1 3 0 952.60 65.29 3 -4 0 854.01 72.89 -4 1 0 895.91 68.19 4 -1 0 964.00 71.59 -1 -3 0 939.01 72.49 4 -1 0 971.50 68.19 -3 4 0 988.30 66.09 -1 -3 0 984.90 67.79 2 -4 0 5652.73 439.96 -4 2 0 6067.49 396.46 2 2 0 5781.22 410.86 -2 4 0 5959.20 396.76 -2 -2 0 6170.28 438.86 4 -2 0 6089.29 439.06 -2 -2 0 5850.31 408.16 4 -2 0 5807.52 410.96 -4 3 0 4508.85 301.57 3 1 0 4347.67 304.47 -4 3 0 4329.37 293.77 1 -4 0 4251.27 326.07 1 -4 0 4423.36 301.37 4 -3 0 4510.55 325.67 -3 -1 0 4173.58 302.67 4 -3 0 4353.96 304.27 -1 4 0 4385.56 293.97 -1 4 0 4483.85 303.77 0 -4 0 3611.64 250.67 0 -4 0 3644.34 270.97 -4 4 0 3812.32 244.48 4 0 0 3664.13 253.17 -4 4 0 3726.73 249.88 4 -4 0 3502.45 252.37 0 4 0 3651.93 244.08 4 -4 0 3537.65 270.87 -4 0 0 3541.35 251.97 0 4 0 3600.94 252.47 -5 1 0 751.82 56.29 4 -5 0 729.93 59.59 1 4 0 730.13 52.99 1 4 0 774.52 54.99 -1 -4 0 739.13 54.99 -4 5 0 723.73 53.69 5 -1 0 774.02 55.59 -4 5 0 775.62 53.29 -1 -4 0 759.42 59.29 -5 2 0 718.33 51.99 3 -5 0 710.83 56.09 2 3 0 684.63 51.19 -5 2 0 697.03 49.50 -2 -3 0 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466.65 45.50 5 6 -28 500.95 43.90 -6 11 28 511.05 51.79 6 5 -28 487.55 45.00 5 -11 -28 504.45 50.59 -11 6 -28 496.35 47.20 -6 -5 28 483.25 54.59 -5 11 28 588.04 51.59 7 4 -28 31.90 20.20 -11 7 -28 43.00 19.70 4 -11 -28 57.59 23.20 7 4 -28 42.80 17.70 -7 -4 28 22.20 26.20 3 -11 -28 35.70 22.50 8 3 -28 55.39 21.10 8 3 -28 32.10 18.40 -8 -3 28 38.80 29.20 11 -8 28 37.10 22.80 9 2 -28 68.39 21.10 2 -11 -28 49.00 24.50 9 2 -28 39.00 20.10 11 -9 28 58.39 24.10 -9 -2 28 -17.00 28.90 1 -11 -28 169.78 30.70 10 1 -28 150.78 26.30 11 -10 28 136.39 30.50 -10 -1 28 170.38 41.10 0 -11 -28 138.79 31.90 -11 11 -28 164.08 26.20 -11 0 28 110.79 41.90 10 -12 -28 140.49 28.90 2 10 -28 151.18 30.60 12 -2 28 128.79 31.10 9 -12 -28 67.19 24.60 3 9 -28 43.40 21.80 -12 3 -28 10.40 22.50 -9 12 28 -19.40 25.60 12 -3 28 37.00 26.20 8 -12 -28 37.90 23.70 -12 4 -28 31.50 23.20 4 8 -28 16.60 21.50 -8 12 28 -10.10 25.80 7 -12 -28 27.20 23.30 5 7 -28 28.30 20.50 -12 5 -28 6.40 21.60 -7 12 28 -14.50 24.10 -12 6 -28 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254.67 33.30 5 -4 -75 258.37 35.40 -4 0 -75 22.00 20.20 -4 1 -75 155.68 27.70 3 -4 -75 143.79 28.80 -4 2 -75 35.80 20.60 2 -4 -75 58.99 23.70 3 1 -75 18.80 18.60 1 -4 -75 47.60 23.50 -4 3 -75 26.80 21.30 4 0 -75 -2.00 19.40 0 -4 -75 32.70 23.20 -4 4 -75 22.50 21.20 -5 0 -75 26.80 20.70 -5 1 -75 143.59 28.20 1 4 -75 163.68 27.40 -5 2 -75 91.99 24.80 2 3 -75 84.49 23.80 3 -5 -75 112.09 26.60 2 -5 -75 15.10 23.50 3 2 -75 -14.40 20.20 4 1 -75 262.57 34.20 4 -6 -75 41.10 21.80 1 -1 -76 243.58 35.20 0 1 -76 251.87 31.70 -1 1 -76 234.98 31.70 -1 2 -76 42.20 20.70 -1 3 -76 120.69 26.40 0 2 -76 138.59 26.10 -2 0 -76 141.79 25.10 1 -2 -76 76.19 23.40 -2 1 -76 56.59 21.60 0 -2 -76 145.39 30.50 -2 2 -76 141.99 26.60 -1 -2 -76 200.58 34.90 -2 3 -76 190.08 31.00 -2 4 -76 126.19 27.70 -2 -2 -76 119.29 29.60 5 -3 -76 95.19 25.10 -1 4 -76 371.46 44.10 4 -3 -76 418.56 41.10 -3 0 -76 119.39 24.80 2 -3 -76 176.78 30.00 -3 1 -76 210.98 29.30 1 -3 -76 145.09 28.60 -3 2 -76 122.99 25.20 -3 3 -76 140.39 27.80 0 -3 -76 122.39 29.80 -1 -3 -76 6.70 25.10 -3 4 -76 34.10 22.20 -4 0 -76 118.79 25.50 -4 1 -76 19.20 19.70 3 -4 -76 39.70 22.40 -4 2 -76 132.79 27.80 2 -4 -76 149.49 29.00 -4 3 -76 416.46 46.40 1 -4 -76 451.95 50.49 4 0 -76 58.79 22.90 1 4 -76 43.40 21.60 3 -5 -76 32.40 22.30 2 3 -76 28.70 19.90 2 -5 -76 138.69 29.00 3 2 -76 101.59 25.60 4 1 -76 74.59 23.90 0 1 -77 216.38 31.00 1 -1 -77 286.47 37.00 -1 1 -77 224.38 30.60 -1 2 -77 102.19 24.80 -1 3 -77 106.99 25.40 0 2 -77 40.30 20.90 -2 0 -77 30.00 18.30 1 -2 -77 88.09 26.70 -2 1 -77 85.99 23.30 0 -2 -77 20.10 22.10 -2 2 -77 27.40 20.90 -2 3 -77 34.00 21.90 -1 -2 -77 63.09 25.90 -2 4 -77 216.78 33.80 5 -3 -77 89.19 24.00 -1 4 -77 40.60 22.70 4 -3 -77 81.89 23.40 -3 0 -77 350.56 38.30 0 3 -77 341.67 40.80 -3 1 -77 57.79 22.00 2 -3 -77 77.19 24.50 -3 2 -77 141.29 26.40 1 -3 -77 118.89 29.10 -3 3 -77 310.47 40.00 0 -3 -77 375.76 44.80 -4 0 -77 148.49 26.20 -4 1 -77 47.50 22.60 -4 2 -77 199.48 31.20 2 -4 -77 228.88 34.70 -4 3 -77 73.09 25.20 1 -4 -77 129.49 28.40 2 3 -77 16.70 20.60 3 -5 -77 32.10 23.30 3 2 -77 83.39 23.70 0 1 -78 51.79 20.20 1 -1 -78 51.89 23.40 0 -1 -78 33.20 24.50 -1 1 -78 57.29 20.00 -1 2 -78 188.88 30.00 -1 3 -78 287.57 37.00 0 2 -78 53.29 21.40 -2 1 -78 205.98 29.40 1 -2 -78 180.98 32.00 0 -2 -78 64.59 24.90 -2 2 -78 -5.80 20.10 -1 -2 -78 56.69 26.30 -2 3 -78 50.99 23.50 4 -3 -78 46.10 22.80 -3 0 -78 87.89 23.80 0 3 -78 87.59 24.70 2 -3 -78 41.50 22.20 -3 1 -78 41.50 20.70 1 2 -78 47.10 20.80 1 -3 -78 336.57 42.60 -3 2 -78 340.07 40.30 0 -3 -78 78.59 28.50 -3 3 -78 134.29 26.70 -4 0 -78 218.78 31.80 -4 1 -78 84.99 23.50 2 -4 -78 85.89 26.50 -4 2 -78 79.99 25.10 -1 1 -79 176.78 28.20 0 -1 -79 152.08 31.40 -1 2 -79 57.39 22.90 -1 3 -79 29.90 22.00 0 2 -79 47.00 21.20 1 -2 -79 104.69 27.80 -2 1 -79 96.79 24.00 -2 2 -79 19.90 21.30 0 -2 -79 32.50 25.40 -1 -2 -79 71.19 29.10 -2 3 -79 75.49 23.90 4 -3 -79 62.09 22.30 -3 0 -79 163.88 26.60 0 3 -79 122.39 27.50 2 -3 -79 51.29 25.00 1 2 -79 57.19 21.40 -3 1 -79 85.59 23.80 -3 2 -79 49.80 22.90 1 -3 -79 48.40 25.10 2 -4 -79 34.90 23.60 -1 1 -80 124.09 25.50 0 -1 -80 83.29 26.60 -1 2 -80 24.10 21.30 -1 3 -80 69.29 24.40 0 2 -80 64.79 23.20 -2 1 -80 11.90 20.20 1 -2 -80 38.50 24.30 0 -2 -80 50.29 25.10 -2 2 -80 18.00 20.30 -3 1 -80 59.49 22.50 2 -3 -80 1.30 20.90 1 2 -80 23.60 20.70 1 -3 -80 67.29 25.40 -3 2 -80 45.20 22.20 0 -1 -81 17.70 24.10 -1 2 -81 42.50 22.40 0 2 -81 23.00 21.30 1 -2 -81 37.70 23.60 -2 1 -81 16.70 21.00 0 -2 -81 51.09 26.80 -2 2 -81 56.09 22.50 1 2 -81 197.98 31.70 -3 1 -81 208.08 30.70 0 -1 -82 72.49 28.20 -1 2 -82 49.50 23.40 0 2 -82 114.19 27.20 -2 1 -82 62.89 22.20 1 -2 -82 27.80 25.00 0 -1 -83 80.89 28.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 48318 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' 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 Mn1 Mn 0.32711(8) 0.22381(9) 0.51418(2) 0.01761(17) Uani 1 1 d . . . . . Mn2 Mn -0.04242(8) 0.41020(8) 0.44399(2) 0.01613(16) Uani 1 1 d . . . . . Br1 Br 0.45980(6) 0.44586(6) 0.54113(2) 0.02641(14) Uani 1 1 d . . . . . Br2 Br 0.03091(7) 0.24037(6) 0.46466(2) 0.02730(14) Uani 1 1 d . . . . . C1 C 0.2910(5) 0.0232(5) 0.55597(9) 0.0180(10) Uani 1 1 d . . . . . C2 C 0.4142(6) 0.0013(6) 0.55528(11) 0.0222(11) Uani 1 1 d . . . . . H2 H 0.4794 0.0313 0.5430 0.027 Uiso 1 1 calc R U . . . C3 C 0.4376(7) -0.0659(7) 0.57331(12) 0.0288(13) Uani 1 1 d . . . . . H3 H 0.5202 -0.0834 0.5732 0.035 Uiso 1 1 calc R U . . . C4 C 0.3431(7) -0.1091(6) 0.59170(11) 0.0266(12) Uani 1 1 d . . . . . H4 H 0.3634 -0.1550 0.6037 0.032 Uiso 1 1 calc R U . . . C5 C 0.2213(6) -0.0866(6) 0.59275(11) 0.0259(12) Uani 1 1 d . . . . . H5 H 0.1578 -0.1146 0.6053 0.031 Uiso 1 1 calc R U . . . C6 C 0.1966(6) -0.0199(5) 0.57432(10) 0.0188(10) Uani 1 1 d . . . . . C7 C 0.1150(5) 0.0768(5) 0.54951(9) 0.0169(10) Uani 1 1 d . . . . . C8 C 0.0257(5) 0.1314(6) 0.53690(9) 0.0188(10) Uani 1 1 d . . . . . H8 H -0.0022 0.1893 0.5472 0.023 Uiso 1 1 calc R U . . . C9 C -0.1216(6) 0.0055(6) 0.52623(10) 0.0216(11) Uani 1 1 d . . . . . C10 C -0.0899(6) -0.0754(6) 0.50789(11) 0.0285(13) Uani 1 1 d . . . . . H10A H -0.0315 -0.1196 0.5137 0.043 Uiso 1 1 calc R U . . . H10B H -0.0325 -0.0034 0.4963 0.043 Uiso 1 1 calc R U . . . H10C H -0.1853 -0.1553 0.5019 0.043 Uiso 1 1 calc R U . . . C11 C -0.2069(6) 0.0824(8) 0.51754(13) 0.0324(14) Uani 1 1 d . . . . . H11A H -0.1455 0.1574 0.5065 0.049 Uiso 1 1 calc R U . . . H11B H -0.2275 0.1321 0.5297 0.049 Uiso 1 1 calc R U . . . H11C H -0.3021 0.0067 0.5109 0.049 Uiso 1 1 calc R U . . . C12 C -0.2205(6) -0.1110(8) 0.54343(12) 0.0364(15) Uani 1 1 d . . . . . H12A H -0.3155 -0.1856 0.5367 0.055 Uiso 1 1 calc R U . . . H12B H -0.2413 -0.0604 0.5554 0.055 Uiso 1 1 calc R U . . . H12C H -0.1680 -0.1613 0.5492 0.055 Uiso 1 1 calc R U . . . C13 C 0.2579(7) 0.0757(7) 0.49396(11) 0.0280(13) Uani 1 1 d . . . . . C14 C 0.3946(6) 0.3566(7) 0.49186(11) 0.0260(12) Uani 1 1 d . . . . . C15 C 0.5052(7) 0.2312(7) 0.51376(11) 0.0306(14) Uani 1 1 d . . . . . C16 C -0.0224(6) 0.0079(7) 0.58605(11) 0.0262(12) Uani 1 1 d . . . . . H16A H -0.0613 0.0740 0.5817 0.039 Uiso 1 1 calc R U . . . H16B H 0.0263 0.0392 0.6004 0.039 Uiso 1 1 calc R U . . . H16C H -0.1057 -0.0962 0.5869 0.039 Uiso 1 1 calc R U . . . C17 C 0.2116(7) 0.6551(7) 0.49871(12) 0.0315(14) Uani 1 1 d . . . . . C18 C 0.2282(9) 0.6832(8) 0.52129(12) 0.0440(18) Uani 1 1 d . . . . . H18 H 0.3244 0.7282 0.5281 0.053 Uiso 1 1 calc R U . . . C19 C 0.1010(11) 0.6434(9) 0.53324(15) 0.058(2) Uani 1 1 d . U . . . H19 H 0.1091 0.6614 0.5486 0.070 Uiso 1 1 calc R U . . . C20 C -0.0410(10) 0.5767(8) 0.52329(14) 0.049(2) Uani 1 1 d . . . . . H20 H -0.1270 0.5529 0.5320 0.059 Uiso 1 1 calc R U . . . C21 C -0.0589(8) 0.5447(7) 0.50113(13) 0.0369(16) Uani 1 1 d . . . . . H21 H -0.1558 0.4965 0.4946 0.044 Uiso 1 1 calc R U . . . C22 C 0.0701(7) 0.5856(6) 0.48873(11) 0.0272(13) Uani 1 1 d . . . . . C23 C 0.2367(6) 0.6308(5) 0.46321(11) 0.0227(11) Uani 1 1 d . . . . . C24 C 0.4770(8) 0.7503(9) 0.48598(15) 0.0474(19) Uani 1 1 d . . . . . H24A H 0.5209 0.7187 0.4743 0.071 Uiso 1 1 calc R U . . . H24B H 0.4944 0.7170 0.5002 0.071 Uiso 1 1 calc R U . . . H24C H 0.5242 0.8602 0.4859 0.071 Uiso 1 1 calc R U . . . C25 C 0.2974(6) 0.6299(6) 0.44108(9) 0.0193(10) Uani 1 1 d . . . . . H25 H 0.3818 0.6085 0.4429 0.023 Uiso 1 1 calc R U . . . C26 C 0.3580(6) 0.7805(6) 0.42737(11) 0.0234(12) Uani 1 1 d . . . . . C27 C 0.4721(7) 0.9157(6) 0.44130(14) 0.0364(16) Uani 1 1 d . . . . . H27A H 0.5040 1.0093 0.4332 0.055 Uiso 1 1 calc R U . . . H27B H 0.5599 0.9050 0.4445 0.055 Uiso 1 1 calc R U . . . H27C H 0.4245 0.9184 0.4551 0.055 Uiso 1 1 calc R U . . . C28 C 0.4372(7) 0.7687(7) 0.40700(12) 0.0309(14) Uani 1 1 d . . . . . H28A H 0.3633 0.6907 0.3973 0.046 Uiso 1 1 calc R U . . . H28B H 0.5131 0.7422 0.4113 0.046 Uiso 1 1 calc R U . . . H28C H 0.4862 0.8655 0.3993 0.046 Uiso 1 1 calc R U . . . C29 C 0.2300(6) 0.8084(6) 0.42125(13) 0.0318(15) Uani 1 1 d . . . . . H29A H 0.2705 0.9036 0.4132 0.048 Uiso 1 1 calc R U . . . H29B H 0.1797 0.8136 0.4346 0.048 Uiso 1 1 calc R U . . . H29C H 0.1574 0.7259 0.4120 0.048 Uiso 1 1 calc R U . . . C30 C -0.1012(6) 0.5268(6) 0.43078(11) 0.0238(12) Uani 1 1 d . . . . . C31 C -0.1373(6) 0.2662(6) 0.42374(10) 0.0217(11) Uani 1 1 d . . . . . C32 C -0.2184(7) 0.3232(7) 0.45836(11) 0.0273(13) Uani 1 1 d . . . . . N1 N 0.2367(4) 0.0854(5) 0.54066(8) 0.0179(9) Uani 1 1 d . . . . . N2 N 0.0875(5) 0.0178(5) 0.56982(9) 0.0217(10) Uani 1 1 d . . . . . N3 N 0.1323(5) 0.2390(5) 0.52022(8) 0.0190(9) Uani 1 1 d . . . . . H3A H 0.1616 0.3344 0.5247 0.023 Uiso 1 1 calc R U . . . H3B H 0.0817 0.2236 0.5074 0.023 Uiso 1 1 calc R U . . . N4 N 0.3153(6) 0.6831(5) 0.48229(9) 0.0292(11) Uani 1 1 d . . . . . N5 N 0.0892(5) 0.5686(5) 0.46658(8) 0.0194(9) Uani 1 1 d . . . . . N6 N 0.1709(4) 0.4989(5) 0.42922(8) 0.0172(9) Uani 1 1 d . . . . . H6A H 0.1938 0.4241 0.4281 0.021 Uiso 1 1 calc R U . . . H6B H 0.1655 0.5287 0.4154 0.021 Uiso 1 1 calc R U . . . O1 O 0.2283(6) -0.0117(6) 0.48061(11) 0.0497(15) Uani 1 1 d . . . . . O2 O 0.4435(6) 0.4387(6) 0.47758(9) 0.0401(12) Uani 1 1 d . . . . . O3 O 0.6230(5) 0.2458(7) 0.51335(10) 0.0498(15) Uani 1 1 d . . . . . O4 O -0.3368(5) 0.2621(5) 0.46622(9) 0.0421(12) Uani 1 1 d . . . . . O5 O -0.2061(4) 0.1697(5) 0.41134(8) 0.0298(9) Uani 1 1 d . . . . . O6 O -0.1480(5) 0.5975(5) 0.42319(10) 0.0411(13) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0172(3) 0.0226(4) 0.0153(4) 0.0038(3) 0.0013(3) 0.0116(3) Mn2 0.0158(3) 0.0132(3) 0.0157(4) 0.0008(3) -0.0031(3) 0.0045(3) Br1 0.0212(2) 0.0272(3) 0.0229(3) -0.0004(2) -0.0025(2) 0.0062(2) Br2 0.0412(3) 0.0247(3) 0.0201(3) 0.0015(2) -0.0067(2) 0.0196(2) C1 0.019(2) 0.017(2) 0.016(3) 0.0047(19) -0.0029(19) 0.0067(18) C2 0.023(2) 0.020(2) 0.026(3) 0.006(2) 0.000(2) 0.012(2) C3 0.033(3) 0.030(3) 0.033(4) 0.006(3) -0.007(2) 0.022(2) C4 0.036(3) 0.029(3) 0.021(3) 0.007(2) -0.004(2) 0.020(2) C5 0.031(3) 0.020(2) 0.024(3) 0.007(2) 0.004(2) 0.011(2) C6 0.019(2) 0.017(2) 0.019(3) 0.000(2) -0.0039(19) 0.0073(19) C7 0.014(2) 0.019(2) 0.016(3) -0.0030(19) -0.0039(18) 0.0062(18) C8 0.013(2) 0.025(2) 0.020(3) -0.002(2) -0.0049(19) 0.0107(19) C9 0.015(2) 0.025(3) 0.020(3) -0.001(2) -0.006(2) 0.006(2) C10 0.024(3) 0.024(3) 0.034(4) -0.006(2) -0.008(2) 0.009(2) C11 0.015(2) 0.045(3) 0.039(4) -0.004(3) -0.009(2) 0.016(2) C12 0.017(3) 0.040(3) 0.031(4) -0.001(3) -0.005(2) -0.001(2) C13 0.029(3) 0.030(3) 0.026(3) 0.003(2) 0.005(2) 0.015(2) C14 0.030(3) 0.028(3) 0.024(3) 0.005(2) 0.003(2) 0.017(2) C15 0.037(3) 0.045(3) 0.023(3) 0.017(3) 0.010(3) 0.029(3) C16 0.014(2) 0.034(3) 0.024(3) 0.004(2) 0.004(2) 0.007(2) C17 0.039(3) 0.022(3) 0.024(4) -0.004(2) -0.008(3) 0.009(2) C18 0.059(4) 0.039(4) 0.015(3) -0.010(3) -0.010(3) 0.010(3) C19 0.081(6) 0.049(4) 0.021(4) -0.007(3) -0.004(4) 0.015(4) C20 0.063(5) 0.031(3) 0.035(5) -0.001(3) 0.019(4) 0.011(3) C21 0.038(3) 0.027(3) 0.034(4) -0.004(3) 0.010(3) 0.007(3) C22 0.040(3) 0.017(2) 0.022(3) -0.005(2) 0.000(3) 0.011(2) C23 0.024(3) 0.013(2) 0.025(3) -0.007(2) -0.006(2) 0.0058(19) C24 0.032(3) 0.052(4) 0.042(5) -0.014(4) -0.023(3) 0.009(3) C25 0.021(2) 0.021(2) 0.016(3) -0.008(2) -0.008(2) 0.0108(19) C26 0.019(2) 0.015(2) 0.030(3) -0.002(2) 0.000(2) 0.0044(19) C27 0.028(3) 0.017(3) 0.043(5) -0.008(3) 0.002(3) -0.004(2) C28 0.029(3) 0.026(3) 0.033(4) 0.002(2) 0.009(3) 0.010(2) C29 0.027(3) 0.018(2) 0.049(5) 0.011(3) 0.006(3) 0.010(2) C30 0.015(2) 0.021(2) 0.027(3) 0.001(2) -0.002(2) 0.003(2) C31 0.020(2) 0.017(2) 0.025(3) 0.005(2) 0.002(2) 0.0061(19) C32 0.026(3) 0.026(3) 0.028(4) -0.001(2) -0.004(2) 0.011(2) N1 0.0146(18) 0.0172(18) 0.020(3) 0.0014(17) -0.0016(17) 0.0068(15) N2 0.0126(18) 0.024(2) 0.027(3) 0.0019(19) -0.0012(18) 0.0076(17) N3 0.0154(19) 0.0177(19) 0.023(3) -0.0005(17) -0.0036(17) 0.0080(16) N4 0.034(3) 0.024(2) 0.023(3) -0.008(2) -0.014(2) 0.009(2) N5 0.022(2) 0.0166(19) 0.018(3) -0.0016(17) -0.0004(18) 0.0082(17) N6 0.0155(19) 0.0149(19) 0.019(2) -0.0020(16) -0.0012(16) 0.0058(16) O1 0.055(3) 0.040(3) 0.052(4) -0.014(3) 0.003(3) 0.023(2) O2 0.047(3) 0.043(3) 0.030(3) 0.018(2) 0.009(2) 0.022(2) O3 0.033(2) 0.077(4) 0.055(4) 0.030(3) 0.014(2) 0.039(3) O4 0.028(2) 0.044(3) 0.039(3) -0.003(2) 0.008(2) 0.006(2) O5 0.027(2) 0.0230(19) 0.024(3) -0.0065(17) -0.0054(17) 0.0007(16) O6 0.023(2) 0.029(2) 0.070(4) 0.012(2) -0.011(2) 0.0122(18) 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' Mn Mn 0.3368 0.7283 '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' Br Br -0.2901 2.4595 '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 Mn1 C14 87.7(3) . . ? C15 Mn1 C13 89.4(3) . . ? C14 Mn1 C13 87.7(3) . . ? C15 Mn1 N1 98.1(2) . . ? C14 Mn1 N1 173.2(2) . . ? C13 Mn1 N1 96.0(2) . . ? C15 Mn1 N3 169.1(3) . . ? C14 Mn1 N3 95.5(2) . . ? C13 Mn1 N3 101.1(2) . . ? N1 Mn1 N3 78.21(18) . . ? C15 Mn1 Br1 84.0(2) . . ? C14 Mn1 Br1 88.9(2) . . ? C13 Mn1 Br1 172.68(19) . . ? N1 Mn1 Br1 87.99(13) . . ? N3 Mn1 Br1 85.68(13) . . ? C30 Mn2 C32 87.7(3) . . ? C30 Mn2 C31 90.9(3) . . ? C32 Mn2 C31 86.0(3) . . ? C30 Mn2 N5 94.7(2) . . ? C32 Mn2 N5 99.6(2) . . ? C31 Mn2 N5 172.2(2) . . ? C30 Mn2 N6 98.3(2) . . ? C32 Mn2 N6 173.9(2) . . ? C31 Mn2 N6 94.6(2) . . ? N5 Mn2 N6 79.31(18) . . ? C30 Mn2 Br2 176.7(2) . . ? C32 Mn2 Br2 89.2(2) . . ? C31 Mn2 Br2 90.13(18) . . ? N5 Mn2 Br2 84.61(13) . . ? N6 Mn2 Br2 84.78(12) . . ? C2 C1 N1 131.1(5) . . ? C2 C1 C6 121.0(5) . . ? N1 C1 C6 107.9(4) . . ? C3 C2 C1 117.1(6) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.5 . . ? C2 C3 C4 122.0(5) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 121.6(5) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 116.3(6) . . ? C4 C5 H5 121.8 . . ? C6 C5 H5 121.8 . . ? N2 C6 C1 106.4(5) . . ? N2 C6 C5 131.6(6) . . ? C1 C6 C5 122.0(5) . . ? N1 C7 N2 112.6(5) . . ? N1 C7 C8 119.8(5) . . ? N2 C7 C8 127.6(5) . . ? N3 C8 C7 105.5(4) . . ? N3 C8 C9 112.0(5) . . ? C7 C8 C9 115.1(4) . . ? N3 C8 H8 108.0 . . ? C7 C8 H8 108.0 . . ? C9 C8 H8 108.0 . . ? C10 C9 C12 108.5(5) . . ? C10 C9 C11 110.9(5) . . ? C12 C9 C11 108.2(5) . . ? C10 C9 C8 112.1(5) . . ? C12 C9 C8 110.5(5) . . ? C11 C9 C8 106.5(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 Mn1 173.4(6) . . ? O2 C14 Mn1 176.2(5) . . ? O3 C15 Mn1 175.6(6) . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C22 106.6(6) . . ? N4 C17 C18 132.0(6) . . ? C22 C17 C18 121.5(7) . . ? C19 C18 C17 117.6(7) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C18 C19 C20 121.3(8) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 121.5(8) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 117.8(7) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? N5 C22 C17 108.2(6) . . ? N5 C22 C21 131.4(6) . . ? C17 C22 C21 120.3(6) . . ? N5 C23 N4 111.3(6) . . ? N5 C23 C25 121.0(5) . . ? N4 C23 C25 127.6(5) . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 N6 105.4(4) . . ? C23 C25 C26 115.7(4) . . ? N6 C25 C26 111.0(4) . . ? C23 C25 H25 108.2 . . ? N6 C25 H25 108.2 . . ? C26 C25 H25 108.2 . . ? C28 C26 C29 111.1(6) . . ? C28 C26 C27 109.0(5) . . ? C29 C26 C27 107.6(5) . . ? C28 C26 C25 108.6(5) . . ? C29 C26 C25 111.0(4) . . ? C27 C26 C25 109.6(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C30 Mn2 175.1(6) . . ? O5 C31 Mn2 176.1(5) . . ? O4 C32 Mn2 175.0(6) . . ? C7 N1 C1 106.0(5) . . ? C7 N1 Mn1 117.1(4) . . ? C1 N1 Mn1 134.5(3) . . ? C7 N2 C6 107.0(5) . . ? C7 N2 C16 129.4(5) . . ? C6 N2 C16 123.3(5) . . ? C8 N3 Mn1 115.6(3) . . ? C8 N3 H3A 108.4 . . ? Mn1 N3 H3A 108.4 . . ? C8 N3 H3B 108.4 . . ? Mn1 N3 H3B 108.4 . . ? H3A N3 H3B 107.4 . . ? C23 N4 C17 107.2(5) . . ? C23 N4 C24 128.7(6) . . ? C17 N4 C24 124.1(6) . . ? C23 N5 C22 106.7(5) . . ? C23 N5 Mn2 114.7(4) . . ? C22 N5 Mn2 132.7(4) . . ? C25 N6 Mn2 115.1(3) . . ? C25 N6 H6A 108.5 . . ? Mn2 N6 H6A 108.5 . . ? C25 N6 H6B 108.5 . . ? Mn2 N6 H6B 108.5 . . ? H6A N6 H6B 107.5 . . ? 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 Mn1 C15 1.791(6) . ? Mn1 C14 1.802(6) . ? Mn1 C13 1.805(7) . ? Mn1 N1 2.042(5) . ? Mn1 N3 2.114(4) . ? Mn1 Br1 2.5786(10) . ? Mn2 C30 1.780(6) . ? Mn2 C32 1.793(6) . ? Mn2 C31 1.794(6) . ? Mn2 N5 2.042(5) . ? Mn2 N6 2.107(4) . ? Mn2 Br2 2.5507(9) . ? C1 C2 1.390(7) . ? C1 N1 1.396(7) . ? C1 C6 1.400(8) . ? C2 C3 1.383(8) . ? C2 H2 0.9500 . ? C3 C4 1.402(10) . ? C3 H3 0.9500 . ? C4 C5 1.382(8) . ? C4 H4 0.9500 . ? C5 C6 1.405(8) . ? C5 H5 0.9500 . ? C6 N2 1.382(7) . ? C7 N1 1.322(7) . ? C7 N2 1.347(8) . ? C7 C8 1.503(7) . ? C8 N3 1.498(7) . ? C8 C9 1.557(7) . ? C8 H8 1.0000 . ? C9 C10 1.522(9) . ? C9 C12 1.532(9) . ? C9 C11 1.537(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O1 1.135(9) . ? C14 O2 1.140(8) . ? C15 O3 1.142(7) . ? C16 N2 1.466(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N4 1.383(9) . ? C17 C22 1.397(9) . ? C17 C18 1.401(10) . ? C18 C19 1.367(13) . ? C18 H18 0.9500 . ? C19 C20 1.401(13) . ? C19 H19 0.9500 . ? C20 C21 1.382(11) . ? C20 H20 0.9500 . ? C21 C22 1.395(10) . ? C21 H21 0.9500 . ? C22 N5 1.390(8) . ? C23 N5 1.332(7) . ? C23 N4 1.365(8) . ? C23 C25 1.489(8) . ? C24 N4 1.461(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N6 1.507(6) . ? C25 C26 1.586(8) . ? C25 H25 1.0000 . ? C26 C28 1.523(9) . ? C26 C29 1.524(8) . ? C26 C27 1.547(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O6 1.148(7) . ? C31 O5 1.163(7) . ? C32 O4 1.156(8) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -179.4(5) . . . . ? C6 C1 C2 C3 0.7(8) . . . . ? C1 C2 C3 C4 -0.7(9) . . . . ? C2 C3 C4 C5 0.0(10) . . . . ? C3 C4 C5 C6 0.8(9) . . . . ? C2 C1 C6 N2 179.6(5) . . . . ? N1 C1 C6 N2 -0.3(6) . . . . ? C2 C1 C6 C5 0.0(8) . . . . ? N1 C1 C6 C5 -179.9(5) . . . . ? C4 C5 C6 N2 179.7(6) . . . . ? C4 C5 C6 C1 -0.8(8) . . . . ? N1 C7 C8 N3 -21.9(6) . . . . ? N2 C7 C8 N3 157.6(5) . . . . ? N1 C7 C8 C9 102.2(6) . . . . ? N2 C7 C8 C9 -78.3(7) . . . . ? N3 C8 C9 C10 53.1(6) . . . . ? C7 C8 C9 C10 -67.4(7) . . . . ? N3 C8 C9 C12 174.3(5) . . . . ? C7 C8 C9 C12 53.8(7) . . . . ? N3 C8 C9 C11 -68.4(6) . . . . ? C7 C8 C9 C11 171.1(5) . . . . ? N4 C17 C18 C19 178.9(7) . . . . ? C22 C17 C18 C19 -1.6(11) . . . . ? C17 C18 C19 C20 0.1(13) . . . . ? C18 C19 C20 C21 1.7(13) . . . . ? C19 C20 C21 C22 -2.1(11) . . . . ? N4 C17 C22 N5 1.6(6) . . . . ? C18 C17 C22 N5 -178.0(6) . . . . ? N4 C17 C22 C21 -179.2(6) . . . . ? C18 C17 C22 C21 1.2(10) . . . . ? C20 C21 C22 N5 179.6(6) . . . . ? C20 C21 C22 C17 0.6(10) . . . . ? N5 C23 C25 N6 -23.9(6) . . . . ? N4 C23 C25 N6 152.1(5) . . . . ? N5 C23 C25 C26 99.1(6) . . . . ? N4 C23 C25 C26 -84.9(7) . . . . ? C23 C25 C26 C28 171.3(5) . . . . ? N6 C25 C26 C28 -68.7(6) . . . . ? C23 C25 C26 C29 -66.4(6) . . . . ? N6 C25 C26 C29 53.6(6) . . . . ? C23 C25 C26 C27 52.3(6) . . . . ? N6 C25 C26 C27 172.3(5) . . . . ? N2 C7 N1 C1 2.0(6) . . . . ? C8 C7 N1 C1 -178.5(4) . . . . ? N2 C7 N1 Mn1 -163.1(4) . . . . ? C8 C7 N1 Mn1 16.4(6) . . . . ? C2 C1 N1 C7 179.1(6) . . . . ? C6 C1 N1 C7 -1.0(6) . . . . ? C2 C1 N1 Mn1 -19.6(9) . . . . ? C6 C1 N1 Mn1 160.3(4) . . . . ? N1 C7 N2 C6 -2.2(6) . . . . ? C8 C7 N2 C6 178.3(5) . . . . ? N1 C7 N2 C16 171.0(5) . . . . ? C8 C7 N2 C16 -8.5(9) . . . . ? C1 C6 N2 C7 1.4(6) . . . . ? C5 C6 N2 C7 -179.0(6) . . . . ? C1 C6 N2 C16 -172.2(5) . . . . ? C5 C6 N2 C16 7.3(9) . . . . ? C7 C8 N3 Mn1 17.5(5) . . . . ? C9 C8 N3 Mn1 -108.5(4) . . . . ? N5 C23 N4 C17 -1.3(6) . . . . ? C25 C23 N4 C17 -177.6(5) . . . . ? N5 C23 N4 C24 176.0(6) . . . . ? C25 C23 N4 C24 -0.3(10) . . . . ? C22 C17 N4 C23 -0.2(6) . . . . ? C18 C17 N4 C23 179.3(7) . . . . ? C22 C17 N4 C24 -177.7(6) . . . . ? C18 C17 N4 C24 1.8(11) . . . . ? N4 C23 N5 C22 2.3(6) . . . . ? C25 C23 N5 C22 178.8(5) . . . . ? N4 C23 N5 Mn2 -154.3(4) . . . . ? C25 C23 N5 Mn2 22.2(6) . . . . ? C17 C22 N5 C23 -2.4(6) . . . . ? C21 C22 N5 C23 178.6(6) . . . . ? C17 C22 N5 Mn2 148.2(4) . . . . ? C21 C22 N5 Mn2 -30.9(9) . . . . ? C23 C25 N6 Mn2 14.4(5) . . . . ? C26 C25 N6 Mn2 -111.6(4) . . . . ?