#------------------------------------------------------------------------------ #$Date: 2021-03-05 04:30:53 +0200 (Fri, 05 Mar 2021) $ #$Revision: 262732 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/08/1560816.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_1560816 loop_ _publ_author_name 'MIKURIYA, Masahiro' 'ONO, Sayuri' 'KOYAMA, Yoshiki' 'MITSUHASHI, Ryoji' 'TSUBOI, Motohiro' _publ_section_title ; Crystal Structure of \m-Oxido-\m-phenolato-bridged Dinuclear Manganese(III) Complex of Schiff-base Ligand with Bromido Coordination ; _journal_issue 0 _journal_name_full 'X-ray Structure Analysis Online' _journal_page_first 9 _journal_page_last 11 _journal_paper_doi 10.2116/xraystruct.37.9 _journal_volume 37 _journal_year 2021 _chemical_formula_sum 'C41 H56 Br2 Mn2 N8 O12' _chemical_formula_weight 1122.63 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.890(2) _cell_length_b 20.903(3) _cell_length_c 14.7765(19) _cell_measurement_reflns_used 28119 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 27.499 _cell_measurement_theta_min 1.688 _cell_volume 4599.1(11) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 90(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1311 _diffrn_reflns_av_unetI/netI 0.1201 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 28119 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_min 1.688 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 2.356 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_correction_T_min 0.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour dark-brown _exptl_crystal_density_diffrn 1.621 _exptl_crystal_description needle _exptl_crystal_F_000 2296 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.659 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.124 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 5416 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0539 _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^)+(0.0120P)^2^+4.9675P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1065 _refine_ls_wR_factor_ref 0.1260 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3430 _reflns_number_total 5416 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 37_9_1.txt _cod_data_source_block MnSO161m_0ma_a _cod_original_cell_volume 4599.3(11) _cod_database_code 1560816 _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 0.519 _shelx_estimated_absorpt_t_max 0.834 _shelx_res_file ; MnSO161m_0ma_a.res created by SHELXL-2014/7 TITL MnSO161m_0ma_a.res in Pnma REM Yadorkari-X generated CELL 0.71073 14.8901 20.9035 14.7765 90.0000 90.0000 90.0000 ZERR 4.0 0.0020 0.0029 0.0019 0.0000 0.0000 0.0000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, 1/2-Z SYMM -X, 1/2+Y, -Z REM SPGR Pnma orthorhombic SFAC C H N O Mn Br UNIT 164 224 32 48 8 8 SIZE 0.32 0.12 0.08 TEMP -183.0 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H MERG 2 OMIT -10.000000 55.000000 WGHT 0.012000 4.967500 FVAR 0.22523 MN1 5 0.552067 0.679302 0.457514 11.00000 0.01808 0.01509 = 0.00843 0.00079 0.00060 -0.00027 O1 4 0.620880 0.750000 0.540397 10.50000 0.01763 0.02173 = 0.00718 0.00000 0.00187 0.00000 C1 1 0.611217 0.750000 0.629164 10.50000 0.01990 0.01272 = 0.00580 0.00000 0.00066 0.00000 C2 1 0.686713 0.750000 0.687762 10.50000 0.01154 0.01781 = 0.02374 0.00000 -0.00131 0.00000 AFIX 43 H1 2 0.745546 0.750000 0.662891 10.50000 -1.20000 AFIX 0 C3 1 0.675667 0.750000 0.780049 10.50000 0.02241 0.01728 = 0.00931 0.00000 -0.00335 0.00000 AFIX 43 H2 2 0.726482 0.750000 0.818926 10.50000 -1.20000 AFIX 0 C4 1 0.589241 0.750000 0.816059 10.50000 0.01816 0.01701 = 0.00713 0.00000 -0.00428 0.00000 C5 1 0.514406 0.750000 0.760808 10.50000 0.01631 0.00920 = 0.01528 0.00000 -0.00157 0.00000 AFIX 43 H3 2 0.455914 0.750000 0.786485 10.50000 -1.20000 AFIX 0 C6 1 0.525184 0.750000 0.668243 10.50000 0.01176 0.01387 = 0.01213 0.00000 0.00072 0.00000 N1 3 0.576600 0.750000 0.913514 10.50000 0.02796 0.02282 = 0.00845 0.00000 -0.00614 0.00000 O2 4 0.643518 0.750000 0.962034 10.50000 0.03266 0.02395 = 0.01269 0.00000 -0.00920 0.00000 O3 4 0.499221 0.750000 0.943002 10.50000 0.02659 0.04789 = 0.00875 0.00000 0.00319 0.00000 C7 1 0.443396 0.750000 0.607338 10.50000 0.01524 0.01656 = 0.00786 0.00000 0.00079 0.00000 AFIX 13 H4 2 0.388996 0.750000 0.647023 10.50000 -1.20000 AFIX 0 N2 3 0.435432 0.694766 0.544190 11.00000 0.01626 0.02101 = 0.01097 0.00037 -0.00143 -0.00249 C8 1 0.420013 0.633195 0.591964 11.00000 0.01823 0.01883 = 0.01512 0.00163 0.00465 -0.00187 AFIX 23 H5 2 0.388418 0.603259 0.550955 11.00000 -1.20000 H6 2 0.381027 0.640730 0.645178 11.00000 -1.20000 AFIX 0 C9 1 0.507339 0.603135 0.622843 11.00000 0.01968 0.01931 = 0.01402 0.00419 0.00139 -0.00039 AFIX 23 H7 2 0.532327 0.627117 0.674841 11.00000 -1.20000 H8 2 0.497149 0.558288 0.641772 11.00000 -1.20000 AFIX 0 N3 3 0.570400 0.605447 0.545095 11.00000 0.01907 0.01443 = 0.00874 0.00083 0.00149 -0.00058 C10 1 0.624325 0.558332 0.533856 11.00000 0.02042 0.01378 = 0.01269 0.00188 -0.00349 -0.00486 AFIX 43 H9 2 0.622495 0.524914 0.577389 11.00000 -1.20000 AFIX 0 C11 1 0.687798 0.551895 0.460214 11.00000 0.01566 0.01951 = 0.01339 -0.00070 -0.00195 -0.00280 C12 1 0.734398 0.494296 0.454786 11.00000 0.01724 0.02104 = 0.01886 0.00035 -0.00085 -0.00210 AFIX 43 H10 2 0.725125 0.461987 0.499024 11.00000 -1.20000 AFIX 0 C13 1 0.794383 0.484352 0.384500 11.00000 0.02403 0.01810 = 0.02446 0.00192 0.00174 -0.00071 C14 1 0.812345 0.531766 0.321782 11.00000 0.01855 0.01855 = 0.01760 -0.00322 0.00373 -0.00548 AFIX 43 H11 2 0.854521 0.524257 0.274726 11.00000 -1.20000 AFIX 0 C15 1 0.769473 0.589368 0.327479 11.00000 0.02332 0.02160 = 0.01315 0.00372 0.00226 -0.00201 AFIX 43 H12 2 0.783881 0.622061 0.285246 11.00000 -1.20000 AFIX 0 C16 1 0.703160 0.601679 0.395768 11.00000 0.01965 0.01478 = 0.01334 -0.00108 -0.00441 -0.00235 N4 3 0.838319 0.423131 0.376553 11.00000 0.03054 0.01731 = 0.04002 -0.00289 0.00862 -0.00262 O4 4 0.830126 0.383901 0.438633 11.00000 0.03943 0.02459 = 0.05550 0.01239 0.01971 0.01107 O5 4 0.882953 0.412113 0.308231 11.00000 0.04300 0.02465 = 0.04398 -0.00503 0.01965 0.00584 O6 4 0.663094 0.656478 0.397081 11.00000 0.01817 0.01772 = 0.01245 0.00063 0.00211 0.00199 BR1 6 0.457177 0.594326 0.356425 11.00000 0.02911 0.01952 = 0.01311 -0.00042 -0.00374 -0.00448 O7 4 0.527857 0.750000 0.388454 10.50000 0.02308 0.01527 = 0.00957 0.00000 -0.00169 0.00000 C17 1 0.354510 0.713595 0.489847 11.00000 0.01551 0.03026 = 0.01277 0.00067 -0.00615 0.00107 AFIX 23 H13 2 0.298944 0.696851 0.517997 11.00000 -1.20000 H14 2 0.358906 0.696851 0.427332 11.00000 -1.20000 AFIX 0 O8 4 0.363539 0.593648 0.795731 11.00000 0.05400 0.14462 = 0.03178 0.03732 -0.00666 -0.01115 C18 1 0.360938 0.623875 0.881517 11.00000 0.04785 0.06401 = 0.05864 0.02681 0.00490 -0.00495 AFIX 23 H15 2 0.298848 0.624707 0.905449 11.00000 -1.20000 H16 2 0.383426 0.668343 0.877283 11.00000 -1.20000 AFIX 0 C19 1 0.421689 0.583736 0.942310 11.00000 0.03565 0.03765 = 0.03875 0.00542 0.00057 -0.00046 AFIX 23 H17 2 0.395784 0.579487 1.003720 11.00000 -1.20000 H18 2 0.482213 0.603040 0.947140 11.00000 -1.20000 AFIX 0 C20 1 0.425874 0.518324 0.894310 11.00000 0.04533 0.05049 = 0.03605 -0.00715 0.00222 -0.01013 AFIX 23 H19 2 0.487838 0.508429 0.874459 11.00000 -1.20000 H20 2 0.404404 0.483685 0.934552 11.00000 -1.20000 AFIX 0 C21 1 0.364228 0.526670 0.814276 11.00000 0.06794 0.11021 = 0.02170 0.00191 -0.00134 -0.04488 AFIX 23 H21 2 0.386913 0.502476 0.761410 11.00000 -1.20000 H22 2 0.302999 0.511376 0.828900 11.00000 -1.20000 AFIX 0 N5 3 0.501688 0.750000 0.200903 10.50000 0.02493 0.02754 = 0.01168 0.00000 0.00131 0.00000 AFIX 13 H23 2 0.527473 0.750001 0.263391 10.50000 -1.20000 AFIX 0 C22 1 0.531506 0.689214 0.156352 11.00000 0.03756 0.02229 = 0.01776 0.00110 0.00442 0.01031 AFIX 23 H24 2 0.520929 0.692803 0.090402 11.00000 -1.20000 H25 2 0.494024 0.653586 0.179197 11.00000 -1.20000 AFIX 0 C23 1 0.628358 0.673100 0.171909 11.00000 0.05095 0.07358 = 0.01839 0.00151 -0.00120 0.02543 AFIX 127 H26 2 0.644362 0.635214 0.136328 10.50000 -1.50000 H27 2 0.638084 0.664300 0.236310 10.50000 -1.50000 H28 2 0.665960 0.709249 0.153262 10.50000 -1.50000 H29 2 0.654575 0.703961 0.214272 10.50000 -1.50000 H30 2 0.660853 0.674876 0.114290 10.50000 -1.50000 H31 2 0.632977 0.629926 0.197338 10.50000 -1.50000 AFIX 0 C24 1 0.399428 0.750000 0.211017 10.50000 0.02434 0.02765 = 0.02329 0.00000 0.00117 0.00000 AFIX 23 H32 2 0.381100 0.711739 0.245919 10.50000 -1.20000 H33 2 0.381100 0.788261 0.245919 10.50000 -1.20000 AFIX 0 C25 1 0.350248 0.750000 0.120207 10.50000 0.02428 0.03529 = 0.02912 0.00000 -0.00303 0.00000 AFIX 33 H34 2 0.285270 0.750000 0.130756 10.50000 -1.50000 H35 2 0.366973 0.788279 0.085825 10.50000 -1.50000 H36 2 0.366973 0.711721 0.085825 10.50000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM MnSO161m_0ma_a.res in Pnma REM R1 = 0.0539 for 3430 Fo > 4sig(Fo) and 0.1054 for all 5416 data REM 317 parameters refined using 0 restraints END WGHT 0.0122 4.9496 REM Highest difference peak 0.659, deepest hole -0.629, 1-sigma level 0.124 Q1 1 0.4012 0.6085 0.3745 11.00000 0.05 0.66 Q2 1 0.4209 0.6419 0.3580 11.00000 0.05 0.63 Q3 1 0.5447 0.7500 0.4478 10.50000 0.05 0.61 Q4 1 0.4699 0.6491 0.3484 11.00000 0.05 0.61 Q5 1 0.4663 0.5418 0.3526 11.00000 0.05 0.58 Q6 1 0.4492 0.5135 0.3570 11.00000 0.05 0.58 Q7 1 0.5983 0.7500 0.4776 10.50000 0.05 0.53 Q8 1 0.4120 0.5584 0.3628 11.00000 0.05 0.52 Q9 1 0.3069 0.6007 0.7631 11.00000 0.05 0.48 Q10 1 0.7460 0.4811 0.3377 11.00000 0.05 0.47 Q11 1 0.5255 0.6206 0.4473 11.00000 0.05 0.47 Q12 1 0.6033 0.6417 0.4494 11.00000 0.05 0.46 Q13 1 0.9369 0.3694 0.2829 11.00000 0.05 0.45 Q14 1 0.5642 0.6195 0.6386 11.00000 0.05 0.44 Q15 1 0.2089 0.2500 0.8524 10.50000 0.05 0.44 Q16 1 0.6579 0.7500 0.4242 10.50000 0.05 0.44 Q17 1 0.3772 0.7500 0.4920 10.50000 0.05 0.44 Q18 1 0.5212 0.6226 0.3692 11.00000 0.05 0.44 Q19 1 0.2767 0.7500 0.1679 10.50000 0.05 0.43 Q20 1 0.6872 0.7500 0.7354 10.50000 0.05 0.43 ; _shelx_res_checksum 14329 _shelx_hkl_file ; 0 0 -1 -0.90 0.90 0 0 -2 3337.77 473.25 0 0 -2 3388.96 473.65 0 0 -3 0.80 6.20 0 0 -3 -1.30 2.90 0 0 -4 6640.84 933.31 0 0 -4 6615.44 934.11 0 0 -5 -4.70 4.30 0 0 -5 29.60 10.90 0 0 -6 829.42 123.59 0 0 -6 969.70 125.59 0 0 -7 -7.10 12.60 0 0 -7 0.50 6.40 0 0 -8 193.48 41.50 0 0 -8 285.27 38.80 0 0 -9 -6.60 16.00 0 0 -9 11.30 9.30 0 0 -10 2516.75 365.16 0 0 -10 2700.43 367.46 0 0 -11 5.60 12.40 0 0 -11 0.00 18.80 0 0 -12 2620.04 384.16 0 0 -12 2752.12 382.36 0 0 -13 19.00 22.10 0 0 -14 316.97 55.59 0 0 -15 -9.70 25.70 0 0 -16 144.39 37.30 0 0 -17 -26.20 30.80 0 0 -18 83.99 35.80 0 0 -19 25.20 36.70 -1 0 0 0.70 1.90 -1 0 -1 7565.74 1004.10 -1 0 1 6729.13 1003.80 -1 0 -2 1716.73 244.48 -1 0 -2 1844.22 244.88 1 0 -2 1695.83 244.68 1 0 -2 1703.83 244.08 1 0 -3 1561.94 225.78 1 0 -3 1648.44 226.68 -1 0 -3 1640.94 226.28 -1 0 -3 1577.94 226.58 -1 0 -4 1946.61 271.47 1 0 -4 1918.01 271.47 1 0 -4 1853.11 270.37 -1 0 -4 1981.00 270.87 1 0 -5 1055.49 150.38 1 0 -5 1049.20 148.79 -1 0 -5 1103.39 150.48 -1 0 -5 1027.10 149.29 1 0 -6 259.57 38.50 1 0 -6 217.48 40.80 -1 0 -6 292.87 41.70 -1 0 -6 283.07 39.50 1 0 -7 3295.27 493.25 -1 0 -7 3606.74 493.75 -1 0 -7 3716.93 494.95 1 0 -7 3458.15 494.85 -1 0 -8 103.49 27.70 -1 0 -8 146.59 24.30 1 0 -8 176.58 23.70 1 0 -8 122.19 27.90 -1 0 -9 613.94 83.59 1 0 -9 581.94 83.99 -1 0 -9 521.65 80.19 1 0 -9 544.55 79.49 -1 0 -10 -36.20 16.80 1 0 -10 -2.60 9.70 -1 0 -10 -1.20 11.10 1 0 -10 -14.90 17.50 -1 0 -11 3687.83 524.95 -1 0 -11 3749.52 526.65 1 0 -11 3662.13 524.45 1 0 -11 3812.22 526.85 -1 0 -12 180.88 39.80 1 0 -12 171.78 39.40 -1 0 -12 248.38 36.00 1 0 -13 125.29 27.60 -1 0 -13 14.60 25.10 1 0 -14 29.60 24.50 -1 0 -14 -12.30 23.40 -1 0 -15 9.70 26.80 1 0 -15 16.60 25.90 -1 0 -16 446.56 81.19 1 0 -16 587.04 83.69 1 0 -17 488.85 83.99 -1 0 -17 535.95 84.59 1 0 -18 82.39 35.90 -1 0 -18 26.40 34.00 1 0 -19 49.20 36.40 -1 0 -19 64.89 37.70 2 0 0 8859.71 1246.98 -2 0 0 8860.21 1247.28 2 0 1 193.78 26.50 -2 0 1 174.78 26.70 2 0 -1 185.68 26.40 -2 0 -1 182.78 27.60 2 0 -2 273.67 40.70 2 0 -2 284.57 41.40 -2 0 2 282.87 40.70 -2 0 -2 336.87 42.20 -2 0 -3 368.36 43.40 -2 0 -3 284.17 43.20 2 0 -3 277.47 43.20 -2 0 3 283.27 41.70 2 0 -4 971.10 152.38 -2 0 -4 1051.19 152.38 -2 0 -4 1159.58 152.28 2 0 -4 1081.19 151.18 -2 0 -5 1016.10 134.59 2 0 -5 920.61 133.49 -2 0 -5 943.81 135.19 2 0 -5 911.31 135.09 -2 0 -6 276.77 35.80 2 0 -6 226.38 33.70 -2 0 -6 252.37 36.90 2 0 -6 167.18 35.90 -2 0 -7 41.50 13.40 2 0 -7 91.39 12.10 -2 0 -7 41.40 17.30 2 0 -7 52.09 16.90 2 0 -8 53.69 18.90 2 0 -8 92.99 13.80 -2 0 -8 65.39 19.70 -2 0 -8 63.69 15.90 2 0 -9 450.15 65.39 -2 0 -9 475.45 69.69 -2 0 -9 505.45 67.49 2 0 -9 360.56 68.39 2 0 -10 2732.63 415.86 -2 0 -10 3107.79 418.36 2 0 -10 2938.21 418.36 -2 0 -10 3123.49 416.86 2 0 -11 57.39 25.20 -2 0 -11 101.09 21.30 -2 0 -11 131.99 26.60 -2 0 -12 678.63 92.29 -2 0 -12 600.04 88.89 2 0 -12 524.15 91.59 -2 0 -13 248.28 37.40 2 0 -13 208.98 41.50 -2 0 -13 144.59 40.40 -2 0 -14 275.87 47.50 2 0 -14 224.98 46.70 2 0 -15 336.67 60.79 -2 0 -15 368.26 61.39 -2 0 -16 115.89 34.00 2 0 -16 101.59 34.40 2 0 -17 466.15 75.39 -2 0 -17 422.86 74.49 -2 0 -18 226.48 46.30 2 0 -18 157.18 45.50 -2 0 -19 21.20 37.10 2 0 -19 -22.60 35.00 3 0 0 2.70 2.60 -3 0 0 -1.90 6.30 3 0 -1 3312.47 486.95 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25.60 6 15 -8 40.90 27.90 -6 -15 -8 -23.70 25.00 6 -15 -8 23.00 22.20 -6 15 -8 28.80 29.30 -6 15 -8 12.60 21.00 -6 -15 -9 -7.40 26.90 -6 15 9 -8.50 25.00 6 15 -9 -12.00 28.90 -6 15 -9 -48.50 30.90 6 -15 -9 32.00 24.10 -6 15 -9 -28.50 21.20 -6 -15 -10 382.96 70.89 6 15 -10 598.94 76.79 -6 15 10 381.06 67.09 6 -15 -10 355.56 68.09 -6 15 -10 329.87 71.09 -6 15 -10 480.55 67.49 -6 15 11 -41.10 27.10 -6 -15 -11 44.30 32.40 6 15 -11 -28.20 36.50 -6 15 -11 6.90 24.40 6 -15 -11 28.90 29.70 -6 15 -11 -20.40 35.80 -6 15 12 69.99 33.60 -6 -15 -12 82.29 38.80 6 15 -12 141.09 45.90 6 -15 -12 84.29 36.60 -6 15 -12 118.39 33.60 -6 -15 -13 57.49 38.30 6 15 -13 -3.50 42.60 -6 15 -13 -41.30 30.90 6 -15 -13 -22.50 33.70 -6 -15 -14 54.19 40.70 6 15 -14 32.40 47.10 6 -15 -14 -29.80 36.50 -6 15 -14 -9.80 36.20 6 15 -15 12.10 49.20 6 -15 -15 14.90 40.80 -6 15 -15 16.90 40.70 7 15 0 -17.50 15.20 -7 -15 0 9.80 17.60 -7 15 0 -8.50 18.50 7 15 0 16.60 13.20 7 15 -1 328.07 47.30 7 15 -1 266.27 45.20 -7 -15 -1 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38.40 -7 15 -9 97.09 28.40 7 15 -10 -7.80 36.60 -7 -15 -10 -14.20 32.00 -7 15 10 -23.10 28.20 -7 15 -10 10.00 24.20 7 -15 -10 -25.50 26.70 -7 15 -10 33.40 36.00 -7 -15 -11 214.58 45.90 -7 15 11 131.39 38.30 7 15 -11 271.67 52.59 -7 15 -11 93.89 45.90 7 -15 -11 153.68 40.80 -7 15 -11 128.69 36.10 7 15 -12 -7.60 43.60 -7 -15 -12 40.40 38.10 -7 15 -12 61.09 31.30 7 -15 -12 86.89 38.10 -7 -15 -13 12.50 39.00 7 15 -13 197.28 48.40 7 -15 -13 9.20 35.60 -7 15 -13 -45.50 33.40 -7 -15 -14 -5.10 46.60 7 15 -14 98.59 49.60 -7 15 -14 47.40 38.10 7 -15 -14 2.00 39.50 7 15 -15 22.00 49.10 -7 15 -15 -16.00 41.40 7 -15 -15 22.50 42.40 -8 15 0 284.27 66.59 -8 -15 0 564.84 68.69 8 15 0 452.95 63.99 8 15 -1 16.60 15.10 -8 15 1 -24.80 21.60 -8 -15 -1 91.59 23.80 8 15 1 25.10 13.90 -8 -15 1 17.50 18.60 -8 15 -1 3.00 22.00 -8 15 2 41.70 22.30 -8 -15 -2 -38.80 21.60 8 15 -2 -6.70 15.30 8 15 -2 14.70 19.40 8 15 2 -3.40 13.50 -8 15 -2 -19.60 20.80 -8 -15 2 5.10 17.60 -8 -15 -3 212.98 39.80 -8 15 3 215.48 38.60 8 15 -3 196.18 33.40 8 15 -3 178.08 36.50 -8 15 -3 150.08 38.20 8 15 3 191.38 31.80 8 15 -4 0.60 16.90 -8 -15 -4 -3.20 23.80 8 15 -4 3.80 22.00 -8 15 4 2.60 21.60 -8 15 -4 -26.60 22.80 -8 -15 -5 373.96 65.59 8 15 -5 375.56 64.59 -8 15 5 403.96 64.99 8 15 -5 426.16 61.29 -8 15 -5 350.06 61.29 -8 15 -5 435.06 66.49 -8 15 6 59.89 31.20 8 15 -6 51.19 32.10 8 15 -6 124.99 25.80 -8 -15 -6 70.49 31.70 -8 15 -6 170.48 36.40 -8 15 -6 130.19 26.40 -8 -15 -7 116.89 35.20 -8 15 7 127.49 33.00 8 15 -7 88.69 35.50 -8 15 -7 83.99 37.80 -8 15 -7 131.39 28.70 -8 15 8 -4.70 25.70 -8 -15 -8 -12.20 29.40 8 15 -8 -36.50 32.50 8 -15 -8 -4.20 24.40 -8 15 -8 8.70 32.90 -8 15 -8 -33.80 21.10 -8 -15 -9 236.58 48.20 8 15 -9 171.28 51.99 -8 15 9 210.28 43.30 8 -15 -9 205.58 43.20 -8 15 -9 217.58 41.00 -8 15 -9 168.58 48.60 -8 15 10 209.78 47.00 8 15 -10 192.18 55.79 -8 -15 -10 311.17 54.29 8 -15 -10 304.37 50.99 -8 15 -10 261.97 55.19 -8 15 -10 179.38 44.40 -8 15 11 -1.80 30.30 -8 -15 -11 22.40 37.30 8 15 -11 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-4 42.60 32.80 -3 26 -4 48.80 35.30 3 26 4 2.80 44.60 -3 26 -4 1.30 36.60 3 26 -5 14.50 33.10 -3 26 -5 -21.90 37.20 -3 26 -5 -59.89 33.20 3 26 -6 147.09 41.90 -3 26 -6 103.09 41.70 4 26 0 59.39 36.70 -4 26 0 50.19 38.40 -4 26 1 120.49 44.70 4 26 -1 153.98 37.40 -4 26 -1 71.09 38.10 4 26 1 23.70 37.90 4 26 -2 34.00 32.00 4 26 2 27.40 35.90 -4 26 -2 59.69 35.80 4 26 -3 8.70 32.20 -4 26 -3 -53.89 35.00 4 26 3 -22.10 36.30 4 26 -4 83.39 35.80 -4 26 -4 98.89 37.10 -4 26 -4 47.00 38.00 4 26 -5 215.88 51.79 -4 26 -5 252.67 55.39 -4 26 -5 246.08 50.89 4 26 -6 46.70 36.50 -4 26 -6 -16.90 35.20 5 26 0 -18.80 39.90 5 26 0 -18.60 32.30 5 26 -1 12.30 31.00 -5 26 -1 -35.10 58.49 5 26 1 19.00 36.40 5 26 -2 -5.50 31.70 -5 26 -2 -22.10 40.60 5 26 2 -40.90 38.20 5 26 -3 30.30 33.40 5 26 3 -25.90 39.70 -5 26 -3 14.90 40.10 5 26 -4 258.47 48.10 -5 26 -4 140.69 45.80 -5 26 -4 150.38 52.99 5 26 -5 1.30 36.30 -5 26 -5 47.10 35.70 -5 26 -5 -35.70 65.39 6 26 1 71.19 41.40 6 26 2 -49.80 40.30 6 26 -4 57.69 38.70 -6 26 -4 39.30 36.60 7 26 2 114.89 49.00 0 27 0 30.10 36.70 0 27 1 -21.10 38.00 0 27 -1 -16.50 35.40 0 27 -2 11.00 36.20 0 27 -3 1.20 34.40 0 27 -4 17.20 35.50 0 27 -5 -5.70 35.40 1 27 0 -74.59 36.60 -1 27 0 -3.70 36.50 1 27 -1 62.99 36.60 -1 27 1 44.40 48.50 -1 27 -1 72.79 37.50 1 27 1 -17.10 37.60 1 27 -2 -25.60 35.20 1 27 -2 -5.50 32.10 1 27 2 19.50 61.49 -1 27 -2 6.80 37.80 1 27 -3 0.30 32.50 -1 27 -3 -22.80 35.50 -1 27 -3 -10.10 33.60 1 27 -4 47.10 34.00 -1 27 -4 32.00 34.00 1 27 -5 31.30 33.70 -1 27 -5 21.80 34.90 2 27 0 -70.69 37.00 -2 27 0 14.30 46.40 2 27 -1 5.60 37.30 2 27 1 -11.10 37.00 -2 27 -1 -67.59 37.40 2 27 -2 56.49 33.50 2 27 2 22.90 48.60 -2 27 -2 43.60 37.30 2 27 -3 12.80 32.20 -2 27 -3 45.40 37.60 -2 27 -3 15.80 35.70 2 27 -4 51.99 34.10 -2 27 -4 61.89 39.40 -2 27 -4 -0.40 36.00 2 27 -5 -14.50 34.70 -2 27 -5 16.30 35.60 3 27 0 -34.10 36.50 3 27 -1 22.00 33.10 3 27 1 27.50 37.60 3 27 -2 132.19 37.90 -3 27 -2 43.80 43.80 3 27 2 213.18 69.79 3 27 -3 80.49 35.70 -3 27 -3 47.10 35.70 -3 27 -3 38.00 39.50 3 27 -4 73.19 36.30 -3 27 -4 32.90 36.70 -3 27 -4 10.00 40.60 4 27 0 110.29 43.50 4 27 0 130.99 39.90 4 27 -1 -1.00 34.40 4 27 1 55.59 39.30 4 27 -2 173.28 44.60 4 27 -3 48.10 35.20 5 27 -1 98.49 38.20 5 27 1 71.19 43.20 5 27 -2 -30.70 34.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 67447 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.55207(4) 0.67930(3) 0.45751(4) 0.01387(16) Uani 1 1 d . . . . . O1 O 0.6209(3) 0.7500 0.5404(3) 0.0155(9) Uani 1 2 d S T P . . C1 C 0.6112(4) 0.7500 0.6292(4) 0.0128(13) Uani 1 2 d S T P . . C2 C 0.6867(4) 0.7500 0.6878(4) 0.0177(14) Uani 1 2 d S T P . . H1 H 0.7455 0.7500 0.6629 0.021 Uiso 1 2 calc R U P . . C3 C 0.6757(4) 0.7500 0.7800(4) 0.0163(13) Uani 1 2 d S T P . . H2 H 0.7265 0.7500 0.8189 0.020 Uiso 1 2 calc R U P . . C4 C 0.5892(4) 0.7500 0.8161(4) 0.0141(13) Uani 1 2 d S T P . . C5 C 0.5144(4) 0.7500 0.7608(4) 0.0136(13) Uani 1 2 d S T P . . H3 H 0.4559 0.7500 0.7865 0.016 Uiso 1 2 calc R U P . . C6 C 0.5252(4) 0.7500 0.6682(4) 0.0126(13) Uani 1 2 d S T P . . N1 N 0.5766(4) 0.7500 0.9135(3) 0.0197(12) Uani 1 2 d S T P . . O2 O 0.6435(3) 0.7500 0.9620(3) 0.0231(10) Uani 1 2 d S T P . . O3 O 0.4992(3) 0.7500 0.9430(3) 0.0277(11) Uani 1 2 d S T P . . C7 C 0.4434(4) 0.7500 0.6073(4) 0.0132(13) Uani 1 2 d S T P . . H4 H 0.3890 0.7500 0.6470 0.016 Uiso 1 2 calc R U P . . N2 N 0.4354(2) 0.69477(17) 0.5442(2) 0.0161(8) Uani 1 1 d . . . . . C8 C 0.4200(3) 0.6332(2) 0.5920(3) 0.0174(10) Uani 1 1 d . . . . . H5 H 0.3884 0.6033 0.5510 0.021 Uiso 1 1 calc R U . . . H6 H 0.3810 0.6407 0.6452 0.021 Uiso 1 1 calc R U . . . C9 C 0.5073(3) 0.6031(2) 0.6228(3) 0.0177(10) Uani 1 1 d . . . . . H7 H 0.5323 0.6271 0.6748 0.021 Uiso 1 1 calc R U . . . H8 H 0.4971 0.5583 0.6418 0.021 Uiso 1 1 calc R U . . . N3 N 0.5704(2) 0.60545(16) 0.5451(2) 0.0141(8) Uani 1 1 d . . . . . C10 C 0.6243(3) 0.5583(2) 0.5339(3) 0.0156(10) Uani 1 1 d . . . . . H9 H 0.6225 0.5249 0.5774 0.019 Uiso 1 1 calc R U . . . C11 C 0.6878(3) 0.5519(2) 0.4602(3) 0.0162(9) Uani 1 1 d . . . . . C12 C 0.7344(3) 0.4943(2) 0.4548(3) 0.0190(10) Uani 1 1 d . . . . . H10 H 0.7251 0.4620 0.4990 0.023 Uiso 1 1 calc R U . . . C13 C 0.7944(3) 0.4844(2) 0.3845(3) 0.0222(11) Uani 1 1 d . . . . . C14 C 0.8123(3) 0.5318(2) 0.3218(3) 0.0182(10) Uani 1 1 d . . . . . H11 H 0.8545 0.5243 0.2747 0.022 Uiso 1 1 calc R U . . . C15 C 0.7695(3) 0.5894(2) 0.3275(3) 0.0194(10) Uani 1 1 d . . . . . H12 H 0.7839 0.6221 0.2852 0.023 Uiso 1 1 calc R U . . . C16 C 0.7032(3) 0.6017(2) 0.3958(3) 0.0159(9) Uani 1 1 d . . . . . N4 N 0.8383(3) 0.4231(2) 0.3766(3) 0.0293(10) Uani 1 1 d . . . . . O4 O 0.8301(2) 0.38390(17) 0.4386(3) 0.0398(10) Uani 1 1 d . . . . . O5 O 0.8830(2) 0.41211(17) 0.3082(3) 0.0372(9) Uani 1 1 d . . . . . O6 O 0.66309(19) 0.65648(14) 0.39708(19) 0.0161(7) Uani 1 1 d . . . . . Br1 Br 0.45718(3) 0.59433(2) 0.35642(3) 0.02058(13) Uani 1 1 d . . . . . O7 O 0.5279(3) 0.7500 0.3885(3) 0.0160(9) Uani 1 2 d S T P . . C17 C 0.3545(3) 0.7136(2) 0.4898(3) 0.0195(10) Uani 1 1 d . . . . . H13 H 0.2989 0.6969 0.5180 0.023 Uiso 1 1 calc R U . . . H14 H 0.3589 0.6969 0.4273 0.023 Uiso 1 1 calc R U . . . O8 O 0.3635(3) 0.5936(3) 0.7957(3) 0.0768(17) Uani 1 1 d . . . . . C18 C 0.3609(4) 0.6239(4) 0.8815(4) 0.0568(19) Uani 1 1 d . . . . . H15 H 0.2988 0.6247 0.9054 0.068 Uiso 1 1 calc R U . . . H16 H 0.3834 0.6683 0.8773 0.068 Uiso 1 1 calc R U . . . C19 C 0.4217(4) 0.5837(3) 0.9423(4) 0.0374(14) Uani 1 1 d . . . . . H17 H 0.3958 0.5795 1.0037 0.045 Uiso 1 1 calc R U . . . H18 H 0.4822 0.6030 0.9471 0.045 Uiso 1 1 calc R U . . . C20 C 0.4259(4) 0.5183(3) 0.8943(4) 0.0440(15) Uani 1 1 d . . . . . H19 H 0.4878 0.5084 0.8745 0.053 Uiso 1 1 calc R U . . . H20 H 0.4044 0.4837 0.9346 0.053 Uiso 1 1 calc R U . . . C21 C 0.3642(5) 0.5267(4) 0.8143(4) 0.067(2) Uani 1 1 d . . . . . H21 H 0.3869 0.5025 0.7614 0.080 Uiso 1 1 calc R U . . . H22 H 0.3030 0.5114 0.8289 0.080 Uiso 1 1 calc R U . . . N5 N 0.5017(4) 0.7500 0.2009(3) 0.0214(13) Uani 1 2 d S T P . . H23 H 0.5275 0.7500 0.2634 0.026 Uiso 1 2 calc R U P . . C22 C 0.5315(3) 0.6892(2) 0.1564(3) 0.0259(11) Uani 1 1 d . . . . . H24 H 0.5209 0.6928 0.0904 0.031 Uiso 1 1 calc R U . . . H25 H 0.4940 0.6536 0.1792 0.031 Uiso 1 1 calc R U . . . C23 C 0.6284(4) 0.6731(3) 0.1719(4) 0.0476(17) Uani 1 1 d . . . . . H26 H 0.6444 0.6352 0.1363 0.071 Uiso 0.5 1 calc R U P . . H27 H 0.6381 0.6643 0.2363 0.071 Uiso 0.5 1 calc R U P . . H28 H 0.6660 0.7092 0.1533 0.071 Uiso 0.5 1 calc R U P . . H29 H 0.6546 0.7040 0.2143 0.071 Uiso 0.5 1 calc R U P . . H30 H 0.6609 0.6749 0.1143 0.071 Uiso 0.5 1 calc R U P . . H31 H 0.6330 0.6299 0.1973 0.071 Uiso 0.5 1 calc R U P . . C24 C 0.3994(4) 0.7500 0.2110(4) 0.0251(16) Uani 1 2 d S T P . . H32 H 0.3811 0.7117 0.2459 0.030 Uiso 0.5 1 calc R U P . . H33 H 0.3811 0.7883 0.2459 0.030 Uiso 0.5 1 calc R U P . . C25 C 0.3502(4) 0.7500 0.1202(5) 0.0296(17) Uani 1 2 d S T P . . H34 H 0.2853 0.7500 0.1308 0.044 Uiso 1 2 calc R U P . . H35 H 0.3670 0.7883 0.0858 0.044 Uiso 0.5 1 calc R U P . . H36 H 0.3670 0.7117 0.0858 0.044 Uiso 0.5 1 calc R U P . . 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 0.0181(3) 0.0151(3) 0.0084(3) 0.0008(3) 0.0006(3) -0.0003(3) O1 0.018(2) 0.022(2) 0.007(2) 0.000 0.0019(17) 0.000 C1 0.020(3) 0.013(3) 0.006(3) 0.000 0.001(2) 0.000 C2 0.012(3) 0.018(4) 0.024(4) 0.000 -0.001(3) 0.000 C3 0.022(3) 0.017(3) 0.009(3) 0.000 -0.003(3) 0.000 C4 0.018(3) 0.017(3) 0.007(3) 0.000 -0.004(3) 0.000 C5 0.016(3) 0.009(3) 0.015(3) 0.000 -0.002(3) 0.000 C6 0.012(3) 0.014(3) 0.012(3) 0.000 0.001(2) 0.000 N1 0.028(3) 0.023(3) 0.008(3) 0.000 -0.006(2) 0.000 O2 0.033(3) 0.024(3) 0.013(2) 0.000 -0.009(2) 0.000 O3 0.027(3) 0.048(3) 0.009(2) 0.000 0.003(2) 0.000 C7 0.015(3) 0.017(3) 0.008(3) 0.000 0.001(2) 0.000 N2 0.0163(19) 0.021(2) 0.0110(18) 0.0004(16) -0.0014(14) -0.0025(15) C8 0.018(2) 0.019(3) 0.015(2) 0.0016(19) 0.0046(18) -0.002(2) C9 0.020(2) 0.019(3) 0.014(2) 0.0042(18) 0.0014(18) -0.0004(19) N3 0.0191(19) 0.014(2) 0.0087(18) 0.0008(15) 0.0015(14) -0.0006(15) C10 0.020(2) 0.014(2) 0.013(2) 0.0019(17) -0.0035(19) -0.0049(18) C11 0.016(2) 0.020(2) 0.013(2) -0.0007(19) -0.0020(19) -0.0028(18) C12 0.017(2) 0.021(3) 0.019(2) 0.000(2) -0.0009(19) -0.0021(19) C13 0.024(3) 0.018(3) 0.024(3) 0.002(2) 0.002(2) -0.001(2) C14 0.019(2) 0.019(3) 0.018(2) -0.0032(19) 0.0037(19) -0.005(2) C15 0.023(2) 0.022(3) 0.013(2) 0.0037(19) 0.0023(19) -0.002(2) C16 0.020(2) 0.015(2) 0.013(2) -0.0011(18) -0.0044(18) -0.0023(19) N4 0.031(2) 0.017(2) 0.040(3) -0.0029(19) 0.009(2) -0.0026(19) O4 0.039(2) 0.025(2) 0.055(3) 0.0124(19) 0.0197(19) 0.0111(17) O5 0.043(2) 0.025(2) 0.044(2) -0.0050(18) 0.0196(18) 0.0058(18) O6 0.0182(16) 0.0177(17) 0.0125(16) 0.0006(13) 0.0021(13) 0.0020(13) Br1 0.0291(3) 0.0195(2) 0.0131(2) -0.00042(19) -0.0037(2) -0.0045(2) O7 0.023(2) 0.015(2) 0.010(2) 0.000 -0.0017(17) 0.000 C17 0.016(2) 0.030(3) 0.013(2) 0.0007(19) -0.0062(18) 0.001(2) O8 0.054(3) 0.145(6) 0.032(3) 0.037(3) -0.007(2) -0.011(3) C18 0.048(4) 0.064(5) 0.059(5) 0.027(4) 0.005(3) -0.005(4) C19 0.036(3) 0.038(4) 0.039(3) 0.005(3) 0.001(3) 0.000(3) C20 0.045(4) 0.050(4) 0.036(4) -0.007(3) 0.002(3) -0.010(3) C21 0.068(5) 0.110(7) 0.022(3) 0.002(4) -0.001(3) -0.045(5) N5 0.025(3) 0.028(3) 0.012(3) 0.000 0.001(2) 0.000 C22 0.038(3) 0.022(3) 0.018(3) 0.001(2) 0.004(2) 0.010(2) C23 0.051(4) 0.074(5) 0.018(3) 0.002(3) -0.001(3) 0.025(3) C24 0.024(4) 0.028(4) 0.023(4) 0.000 0.001(3) 0.000 C25 0.024(4) 0.035(5) 0.029(4) 0.000 -0.003(3) 0.000 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' 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' Mn Mn 0.3368 0.7283 '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 O7 Mn1 O6 96.30(15) . . ? O7 Mn1 N3 173.60(15) . . ? O6 Mn1 N3 89.53(13) . . ? O7 Mn1 O1 81.85(12) . . ? O6 Mn1 O1 91.42(13) . . ? N3 Mn1 O1 95.41(12) . . ? O7 Mn1 N2 92.91(15) . . ? O6 Mn1 N2 170.27(13) . . ? N3 Mn1 N2 81.12(14) . . ? O1 Mn1 N2 86.78(14) . . ? O7 Mn1 Br1 96.82(10) . . ? O6 Mn1 Br1 91.68(9) . . ? N3 Mn1 Br1 85.60(10) . . ? O1 Mn1 Br1 176.74(10) . . ? N2 Mn1 Br1 90.32(9) . . ? O7 Mn1 Mn1 36.22(10) . 8_575 ? O6 Mn1 Mn1 104.25(9) . 8_575 ? N3 Mn1 Mn1 139.41(10) . 8_575 ? O1 Mn1 Mn1 47.22(7) . 8_575 ? N2 Mn1 Mn1 81.48(10) . 8_575 ? Br1 Mn1 Mn1 130.823(17) . 8_575 ? C1 O1 Mn1 120.5(2) . 8_575 ? C1 O1 Mn1 120.5(2) . . ? Mn1 O1 Mn1 85.57(14) 8_575 . ? O1 C1 C6 120.5(5) . . ? O1 C1 C2 121.3(5) . . ? C6 C1 C2 118.1(5) . . ? C3 C2 C1 120.7(6) . . ? C3 C2 H1 119.6 . . ? C1 C2 H1 119.6 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H2 120.3 . . ? C4 C3 H2 120.3 . . ? C5 C4 C3 121.3(5) . . ? C5 C4 N1 118.8(5) . . ? C3 C4 N1 119.9(5) . . ? C6 C5 C4 119.5(6) . . ? C6 C5 H3 120.2 . . ? C4 C5 H3 120.2 . . ? C5 C6 C1 121.0(5) . . ? C5 C6 C7 119.8(5) . . ? C1 C6 C7 119.3(5) . . ? O2 N1 O3 123.5(5) . . ? O2 N1 C4 118.3(5) . . ? O3 N1 C4 118.2(5) . . ? N2 C7 N2 101.7(4) . 8_575 ? N2 C7 C6 115.9(3) . . ? N2 C7 C6 115.9(3) 8_575 . ? N2 C7 H4 107.6 . . ? N2 C7 H4 107.6 8_575 . ? C6 C7 H4 107.6 . . ? C8 N2 C7 112.7(3) . . ? C8 N2 C17 110.9(3) . . ? C7 N2 C17 101.3(3) . . ? C8 N2 Mn1 105.9(3) . . ? C7 N2 Mn1 114.8(3) . . ? C17 N2 Mn1 111.3(3) . . ? N2 C8 C9 111.7(3) . . ? N2 C8 H5 109.3 . . ? C9 C8 H5 109.3 . . ? N2 C8 H6 109.3 . . ? C9 C8 H6 109.3 . . ? H5 C8 H6 107.9 . . ? N3 C9 C8 107.2(3) . . ? N3 C9 H7 110.3 . . ? C8 C9 H7 110.3 . . ? N3 C9 H8 110.3 . . ? C8 C9 H8 110.3 . . ? H7 C9 H8 108.5 . . ? C10 N3 C9 118.1(4) . . ? C10 N3 Mn1 125.8(3) . . ? C9 N3 Mn1 115.6(3) . . ? N3 C10 C11 125.3(4) . . ? N3 C10 H9 117.3 . . ? C11 C10 H9 117.3 . . ? C12 C11 C16 120.8(4) . . ? C12 C11 C10 116.7(4) . . ? C16 C11 C10 122.5(4) . . ? C13 C12 C11 119.6(4) . . ? C13 C12 H10 120.2 . . ? C11 C12 H10 120.2 . . ? C14 C13 C12 121.3(4) . . ? C14 C13 N4 119.6(4) . . ? C12 C13 N4 119.1(4) . . ? C15 C14 C13 120.0(4) . . ? C15 C14 H11 120.0 . . ? C13 C14 H11 120.0 . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H12 119.2 . . ? C16 C15 H12 119.2 . . ? O6 C16 C11 124.2(4) . . ? O6 C16 C15 119.2(4) . . ? C11 C16 C15 116.6(4) . . ? O5 N4 O4 122.5(4) . . ? O5 N4 C13 118.6(4) . . ? O4 N4 C13 118.9(4) . . ? C16 O6 Mn1 128.2(3) . . ? Mn1 O7 Mn1 107.6(2) 8_575 . ? N2 C17 C17 105.2(2) . 8_575 ? N2 C17 H13 110.7 . . ? C17 C17 H13 110.7 8_575 . ? N2 C17 H14 110.7 . . ? C17 C17 H14 110.7 8_575 . ? H13 C17 H14 108.8 . . ? C18 O8 C21 105.4(5) . . ? O8 C18 C19 105.4(5) . . ? O8 C18 H15 110.7 . . ? C19 C18 H15 110.7 . . ? O8 C18 H16 110.7 . . ? C19 C18 H16 110.7 . . ? H15 C18 H16 108.8 . . ? C18 C19 C20 103.9(5) . . ? C18 C19 H17 111.0 . . ? C20 C19 H17 111.0 . . ? C18 C19 H18 111.0 . . ? C20 C19 H18 111.0 . . ? H17 C19 H18 109.0 . . ? C21 C20 C19 103.5(5) . . ? C21 C20 H19 111.1 . . ? C19 C20 H19 111.1 . . ? C21 C20 H20 111.1 . . ? C19 C20 H20 111.1 . . ? H19 C20 H20 109.0 . . ? O8 C21 C20 105.6(5) . . ? O8 C21 H21 110.6 . . ? C20 C21 H21 110.6 . . ? O8 C21 H22 110.6 . . ? C20 C21 H22 110.6 . . ? H21 C21 H22 108.8 . . ? C22 N5 C22 116.0(5) 8_575 . ? C22 N5 C24 109.7(3) 8_575 . ? C22 N5 C24 109.7(3) . . ? C22 N5 H23 107.0 8_575 . ? C22 N5 H23 107.0 . . ? C24 N5 H23 107.0 . . ? N5 C22 C23 114.1(5) . . ? N5 C22 H24 108.7 . . ? C23 C22 H24 108.7 . . ? N5 C22 H25 108.7 . . ? C23 C22 H25 108.7 . . ? H24 C22 H25 107.6 . . ? C22 C23 H26 109.5 . . ? C22 C23 H27 109.5 . . ? H26 C23 H27 109.5 . . ? C22 C23 H28 109.5 . . ? H26 C23 H28 109.5 . . ? H27 C23 H28 109.5 . . ? C22 C23 H29 109.5 . . ? H26 C23 H29 141.1 . . ? H27 C23 H29 56.3 . . ? H28 C23 H29 56.3 . . ? C22 C23 H30 109.5 . . ? H26 C23 H30 56.3 . . ? H27 C23 H30 141.1 . . ? H28 C23 H30 56.3 . . ? H29 C23 H30 109.5 . . ? C22 C23 H31 109.5 . . ? H26 C23 H31 56.3 . . ? H27 C23 H31 56.3 . . ? H28 C23 H31 141.1 . . ? H29 C23 H31 109.5 . . ? H30 C23 H31 109.5 . . ? C25 C24 N5 113.0(5) . . ? C25 C24 H32 109.0 . . ? N5 C24 H32 109.0 . . ? C25 C24 H33 109.0 . . ? N5 C24 H33 109.0 . . ? H32 C24 H33 107.8 . . ? C24 C25 H34 109.5 . . ? C24 C25 H35 109.5 . . ? H34 C25 H35 109.5 . . ? C24 C25 H36 109.5 . . ? H34 C25 H36 109.5 . . ? H35 C25 H36 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 Mn1 O7 1.832(2) . ? Mn1 O6 1.939(3) . ? Mn1 N3 2.033(3) . ? Mn1 O1 2.176(3) . ? Mn1 N2 2.182(3) . ? Mn1 Br1 2.7171(8) . ? Mn1 Mn1 2.9556(14) 8_575 ? O1 C1 1.320(6) . ? O1 Mn1 2.176(3) 8_575 ? C1 C6 1.405(8) . ? C1 C2 1.419(8) . ? C2 C3 1.374(8) . ? C2 H1 0.9500 . ? C3 C4 1.393(8) . ? C3 H2 0.9500 . ? C4 C5 1.381(8) . ? C4 N1 1.452(7) . ? C5 C6 1.377(8) . ? C5 H3 0.9500 . ? C6 C7 1.514(8) . ? N1 O2 1.228(6) . ? N1 O3 1.232(6) . ? C7 N2 1.489(5) . ? C7 N2 1.489(5) 8_575 ? C7 H4 1.0000 . ? N2 C8 1.486(5) . ? N2 C17 1.501(5) . ? C8 C9 1.515(6) . ? C8 H5 0.9900 . ? C8 H6 0.9900 . ? C9 N3 1.485(5) . ? C9 H7 0.9900 . ? C9 H8 0.9900 . ? N3 C10 1.282(5) . ? C10 C11 1.448(6) . ? C10 H9 0.9500 . ? C11 C12 1.392(6) . ? C11 C16 1.429(6) . ? C12 C13 1.386(6) . ? C12 H10 0.9500 . ? C13 C14 1.383(6) . ? C13 N4 1.442(6) . ? C14 C15 1.365(6) . ? C14 H11 0.9500 . ? C15 C16 1.435(6) . ? C15 H12 0.9500 . ? C16 O6 1.292(5) . ? N4 O5 1.230(5) . ? N4 O4 1.236(5) . ? O7 Mn1 1.832(2) 8_575 ? C17 C17 1.522(9) 8_575 ? C17 H13 0.9900 . ? C17 H14 0.9900 . ? O8 C18 1.417(8) . ? O8 C21 1.427(9) . ? C18 C19 1.526(8) . ? C18 H15 0.9900 . ? C18 H16 0.9900 . ? C19 C20 1.542(8) . ? C19 H17 0.9900 . ? C19 H18 0.9900 . ? C20 C21 1.507(8) . ? C20 H19 0.9900 . ? C20 H20 0.9900 . ? C21 H21 0.9900 . ? C21 H22 0.9900 . ? N5 C22 1.498(5) 8_575 ? N5 C22 1.498(5) . ? N5 C24 1.530(8) . ? N5 H23 1.0000 . ? C22 C23 1.499(7) . ? C22 H24 0.9900 . ? C22 H25 0.9900 . ? C23 H26 0.9800 . ? C23 H27 0.9800 . ? C23 H28 0.9800 . ? C23 H29 0.9800 . ? C23 H30 0.9800 . ? C23 H31 0.9800 . ? C24 C25 1.529(9) . ? C24 H32 0.9900 . ? C24 H33 0.9900 . ? C25 H34 0.9800 . ? C25 H35 0.9800 . ? C25 H36 0.9800 . ? 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 Mn1 O1 C1 C6 52.1(2) 8_575 . . . ? Mn1 O1 C1 C6 -52.1(2) . . . . ? Mn1 O1 C1 C2 -127.9(2) 8_575 . . . ? Mn1 O1 C1 C2 127.9(2) . . . . ? O1 C1 C2 C3 180.000(1) . . . . ? C6 C1 C2 C3 0.000(2) . . . . ? C1 C2 C3 C4 0.000(2) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 N1 180.000(1) . . . . ? C3 C4 C5 C6 0.000(2) . . . . ? N1 C4 C5 C6 180.000(1) . . . . ? C4 C5 C6 C1 0.000(2) . . . . ? C4 C5 C6 C7 180.000(1) . . . . ? O1 C1 C6 C5 180.000(1) . . . . ? C2 C1 C6 C5 0.000(1) . . . . ? O1 C1 C6 C7 0.000(1) . . . . ? C2 C1 C6 C7 180.000(1) . . . . ? C5 C4 N1 O2 180.000(1) . . . . ? C3 C4 N1 O2 0.000(2) . . . . ? C5 C4 N1 O3 0.000(2) . . . . ? C3 C4 N1 O3 180.000(1) . . . . ? C5 C6 C7 N2 -120.5(4) . . . . ? C1 C6 C7 N2 59.5(4) . . . . ? C5 C6 C7 N2 120.5(4) . . . 8_575 ? C1 C6 C7 N2 -59.5(4) . . . 8_575 ? N2 C7 N2 C8 -166.6(3) 8_575 . . . ? C6 C7 N2 C8 66.8(5) . . . . ? N2 C7 N2 C17 -48.0(5) 8_575 . . . ? C6 C7 N2 C17 -174.6(4) . . . . ? N2 C7 N2 Mn1 72.0(4) 8_575 . . . ? C6 C7 N2 Mn1 -54.5(5) . . . . ? C7 N2 C8 C9 -84.8(5) . . . . ? C17 N2 C8 C9 162.4(3) . . . . ? Mn1 N2 C8 C9 41.5(4) . . . . ? N2 C8 C9 N3 -47.2(5) . . . . ? C8 C9 N3 C10 -143.6(4) . . . . ? C8 C9 N3 Mn1 29.4(4) . . . . ? C9 N3 C10 C11 177.8(4) . . . . ? Mn1 N3 C10 C11 5.6(6) . . . . ? N3 C10 C11 C12 -173.9(4) . . . . ? N3 C10 C11 C16 6.4(7) . . . . ? C16 C11 C12 C13 -2.0(6) . . . . ? C10 C11 C12 C13 178.3(4) . . . . ? C11 C12 C13 C14 3.2(7) . . . . ? C11 C12 C13 N4 -176.4(4) . . . . ? C12 C13 C14 C15 -1.1(7) . . . . ? N4 C13 C14 C15 178.4(4) . . . . ? C13 C14 C15 C16 -2.1(7) . . . . ? C12 C11 C16 O6 -179.3(4) . . . . ? C10 C11 C16 O6 0.4(7) . . . . ? C12 C11 C16 C15 -1.1(6) . . . . ? C10 C11 C16 C15 178.6(4) . . . . ? C14 C15 C16 O6 -178.5(4) . . . . ? C14 C15 C16 C11 3.2(6) . . . . ? C14 C13 N4 O5 -8.2(7) . . . . ? C12 C13 N4 O5 171.4(4) . . . . ? C14 C13 N4 O4 171.5(4) . . . . ? C12 C13 N4 O4 -8.9(7) . . . . ? C11 C16 O6 Mn1 -19.6(6) . . . . ? C15 C16 O6 Mn1 162.2(3) . . . . ? O6 Mn1 O7 Mn1 -105.56(19) . . . 8_575 ? O1 Mn1 O7 Mn1 -15.02(19) . . . 8_575 ? N2 Mn1 O7 Mn1 71.30(19) . . . 8_575 ? Br1 Mn1 O7 Mn1 161.98(15) . . . 8_575 ? C8 N2 C17 C17 149.0(3) . . . 8_575 ? C7 N2 C17 C17 29.1(3) . . . 8_575 ? Mn1 N2 C17 C17 -93.36(18) . . . 8_575 ? C21 O8 C18 C19 38.5(6) . . . . ? O8 C18 C19 C20 -21.3(6) . . . . ? C18 C19 C20 C21 -2.6(6) . . . . ? C18 O8 C21 C20 -40.6(6) . . . . ? C19 C20 C21 O8 25.5(6) . . . . ? C22 N5 C22 C23 75.4(6) 8_575 . . . ? C24 N5 C22 C23 -159.5(4) . . . . ? C22 N5 C24 C25 64.3(3) 8_575 . . . ? C22 N5 C24 C25 -64.3(3) . . . . ?