#------------------------------------------------------------------------------ #$Date: 2017-11-21 10:50:44 +0200 (Tue, 21 Nov 2017) $ #$Revision: 203412 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/24/7042456.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_7042456 loop_ _publ_author_name 'Lunsford, Allen M.' 'Goldstein, Kristina F.' 'Cohan, Matthew A.' 'Denny, Jason A.' 'Bhuvanesh, Nattamai' 'Ding, Shengda' 'Hall, Michael B.' 'Darensbourg, Marcetta Y.' _publ_section_title ; Comparisons of MN2S2vs. bipyridine as redox-active ligands to manganese and rhenium in (L-L)M'(CO)3Cl complexes. ; _journal_issue 16 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 5175 _journal_page_last 5182 _journal_paper_doi 10.1039/c7dt00600d _journal_volume 46 _journal_year 2017 _chemical_formula_sum 'C12 H18 Br Co Mn N3 O4 S2' _chemical_formula_weight 526.19 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-11-21 deposited with the CCDC. 2017-03-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.553(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.5578(12) _cell_length_b 14.564(2) _cell_length_c 32.747(5) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.33 _cell_measurement_theta_min 2.33 _cell_volume 3604.4(9) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 90482 _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 27.567 _diffrn_reflns_theta_min 1.530 _exptl_absorpt_coefficient_mu 4.091 _exptl_absorpt_correction_T_max 0.7914 _exptl_absorpt_correction_T_min 0.2722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.939 _exptl_crystal_description needle _exptl_crystal_F_000 2096 _exptl_crystal_size_max 0.430 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.826 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 433 _refine_ls_number_reflns 8308 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0332 _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^)+(0.0409P)^2^+7.9418P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.0892 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7274 _reflns_number_total 8308 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00600d3.cif _cod_data_source_block CodachMn _cod_depositor_comments ; Adding full bibliography for 7042451--7042457.cif. 2017-11-04 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C24 H36 Br2 Co2 Mn2 N6 O8 S4' _cod_original_formula_weight 1052.39 _cod_original_formula_units_Z 4 _cod_original_cell_volume 3604.5(10) _cod_database_code 7042456 _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 0.272 _shelx_estimated_absorpt_t_max 0.791 _shelx_res_file ; TITL Mono in P2(1)/n CELL 0.71073 7.5578 14.5643 32.7474 90.000 90.553 90.000 ZERR 4.0000 0.0012 0.0024 0.0053 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O S MN CO BR UNIT 96 144 24 32 16 8 8 8 MERG 2 FMAP 2 GRID PLAN 5 0 0 TEMP -123 SIZE 0.06 0.06 0.43 HTAB BOND $H CONF WPDB -1 L.S. 10 ACTA WGHT 0.040900 7.941800 FVAR 0.05517 BR1 8 0.040780 0.971883 -0.066842 11.00000 0.03516 0.02318 = 0.02539 -0.00361 -0.00331 -0.00629 BR2 8 1.254479 0.238659 0.370825 11.00000 0.02965 0.02035 = 0.02219 -0.00103 -0.00871 -0.00067 MN1 6 -0.219380 0.904695 -0.105775 11.00000 0.01952 0.01818 = 0.01453 0.00095 0.00077 -0.00052 CO1 7 -0.107939 0.732663 -0.046930 11.00000 0.01204 0.01436 = 0.01503 -0.00266 -0.00011 -0.00068 MN2 6 1.104286 0.088477 0.351106 11.00000 0.01593 0.01391 = 0.01582 0.00175 -0.00193 0.00157 CO2 7 0.971123 0.224607 0.277630 11.00000 0.01223 0.01141 = 0.01271 -0.00060 -0.00053 -0.00032 S1 5 -0.079665 0.756832 -0.113166 11.00000 0.01660 0.02207 = 0.01532 -0.00488 0.00066 -0.00065 S2 5 -0.340583 0.823696 -0.048837 11.00000 0.01452 0.01791 = 0.01621 0.00004 0.00195 0.00120 S3 5 0.830705 0.158882 0.328648 11.00000 0.01450 0.01778 = 0.01778 0.00323 0.00149 0.00042 S4 5 1.161658 0.108685 0.279121 11.00000 0.01595 0.01438 = 0.01745 -0.00153 0.00067 0.00248 O4 4 -0.339155 0.604174 -0.066779 11.00000 0.02645 0.02464 = 0.05987 -0.00932 -0.00874 -0.00502 O3 4 -0.050630 0.986740 -0.177959 11.00000 0.03446 0.04016 = 0.02283 0.00888 0.00338 -0.00495 O1 4 -0.510287 0.845846 -0.159273 11.00000 0.02258 0.05709 = 0.02794 0.00146 -0.00185 -0.00256 O6 4 1.448149 0.004670 0.373942 11.00000 0.02352 0.03228 = 0.03800 0.00334 -0.00419 0.00841 O5 4 0.957280 -0.094144 0.333637 11.00000 0.03627 0.02018 = 0.03859 -0.00217 -0.00371 -0.00586 N6 3 0.833218 0.190886 0.235698 11.00000 0.02066 0.02110 = 0.02073 -0.00043 -0.00791 -0.00188 O8 4 0.772220 0.118238 0.230372 11.00000 0.02759 0.02274 = 0.03502 -0.00700 -0.00932 -0.00243 O7 4 0.959883 0.077565 0.434476 11.00000 0.03224 0.04166 = 0.02309 0.00550 0.00670 0.00839 N2 3 -0.077789 0.753173 0.012558 11.00000 0.01923 0.01676 = 0.01615 0.00092 -0.00166 -0.00136 N1 3 0.145366 0.695891 -0.041653 11.00000 0.01241 0.01970 = 0.02252 -0.00365 -0.00105 0.00084 N3 3 -0.214039 0.623494 -0.047536 11.00000 0.02173 0.01511 = 0.03026 -0.00185 -0.00342 -0.00193 O2 4 -0.428580 1.067616 -0.082619 11.00000 0.05654 0.02723 = 0.04268 0.00637 0.01795 0.01476 N4 3 0.869141 0.346484 0.291651 11.00000 0.01884 0.01420 = 0.01771 -0.00134 -0.00314 -0.00045 N5 3 1.142517 0.304582 0.248785 11.00000 0.01576 0.01631 = 0.01542 0.00017 -0.00124 -0.00255 C10 1 -0.053903 0.665589 0.035836 11.00000 0.02640 0.01975 = 0.01996 0.00480 -0.00209 0.00039 AFIX 23 H10A 2 -0.151475 0.622969 0.028720 11.00000 -1.20000 H10B 2 -0.060369 0.678634 0.065454 11.00000 -1.20000 AFIX 0 C9 1 0.123016 0.619420 0.026647 11.00000 0.02438 0.02309 = 0.02927 0.00435 -0.00665 0.00241 AFIX 23 H9A 2 0.122524 0.557643 0.039257 11.00000 -1.20000 H9B 2 0.217955 0.655284 0.040255 11.00000 -1.20000 AFIX 0 C8 1 0.170791 0.608677 -0.018263 11.00000 0.02061 0.02095 = 0.03546 -0.00134 -0.00642 0.00546 AFIX 23 H8A 2 0.295847 0.589106 -0.020275 11.00000 -1.20000 H8B 2 0.096156 0.560020 -0.030634 11.00000 -1.20000 AFIX 0 C6 1 0.223059 0.774271 -0.017926 11.00000 0.01546 0.02481 = 0.02455 -0.00347 -0.00367 -0.00400 AFIX 23 H6A 2 0.251993 0.825137 -0.036771 11.00000 -1.20000 H6B 2 0.333972 0.754199 -0.004298 11.00000 -1.20000 AFIX 0 C7 1 0.090550 0.808584 0.014606 11.00000 0.02133 0.02028 = 0.01831 -0.00297 -0.00318 -0.00334 AFIX 23 H7A 2 0.144521 0.802832 0.042154 11.00000 -1.20000 H7B 2 0.063296 0.874194 0.009757 11.00000 -1.20000 AFIX 0 C5 1 0.228198 0.686309 -0.082965 11.00000 0.01510 0.03175 = 0.02513 -0.00865 0.00356 0.00285 AFIX 23 H5A 2 0.358451 0.690621 -0.080093 11.00000 -1.20000 H5B 2 0.199282 0.625119 -0.094378 11.00000 -1.20000 AFIX 0 C4 1 0.163436 0.759716 -0.111972 11.00000 0.01499 0.03246 = 0.02295 -0.00862 0.00522 -0.00179 AFIX 23 H4A 2 0.210192 0.748417 -0.139657 11.00000 -1.20000 H4B 2 0.205142 0.820744 -0.102680 11.00000 -1.20000 AFIX 0 C11 1 -0.230590 0.805765 0.030037 11.00000 0.02327 0.02439 = 0.01524 -0.00076 0.00434 0.00110 AFIX 23 H11A 2 -0.193166 0.835090 0.055990 11.00000 -1.20000 H11B 2 -0.328507 0.762843 0.036055 11.00000 -1.20000 AFIX 0 C12 1 -0.295634 0.879041 0.000438 11.00000 0.02389 0.02226 = 0.01539 -0.00337 0.00484 0.00402 AFIX 23 H12A 2 -0.204520 0.927295 -0.002710 11.00000 -1.20000 H12B 2 -0.404728 0.907985 0.010890 11.00000 -1.20000 AFIX 0 C3 1 -0.115174 0.955392 -0.150016 11.00000 0.02123 0.02124 = 0.02259 0.00178 -0.00221 -0.00117 C1 1 -0.399340 0.866307 -0.137497 11.00000 0.02164 0.02620 = 0.01859 0.00198 0.00531 0.00493 C2 1 -0.344653 1.006166 -0.092217 11.00000 0.03516 0.02328 = 0.01905 0.00597 0.00602 0.00173 C14 1 1.316288 0.037159 0.364540 11.00000 0.02299 0.01970 = 0.01796 0.00073 -0.00098 -0.00094 C13 1 1.012633 -0.022580 0.339776 11.00000 0.01870 0.02346 = 0.01981 0.00516 -0.00138 0.00372 C18 1 1.028150 0.398737 0.306253 11.00000 0.02813 0.01363 = 0.02453 -0.00464 -0.00660 -0.00220 AFIX 23 H18A 2 1.051346 0.384306 0.335358 11.00000 -1.20000 H18B 2 1.004924 0.465449 0.303986 11.00000 -1.20000 AFIX 0 C19 1 1.192656 0.373660 0.280740 11.00000 0.02110 0.01335 = 0.02558 0.00114 -0.00426 -0.00625 AFIX 23 H19A 2 1.240129 0.429525 0.267557 11.00000 -1.20000 H19B 2 1.285980 0.347949 0.298818 11.00000 -1.20000 AFIX 0 C23 1 1.299180 0.250213 0.235063 11.00000 0.01953 0.02918 = 0.02399 0.00321 0.00795 0.00199 AFIX 23 H23A 2 1.399221 0.292383 0.229887 11.00000 -1.20000 H23B 2 1.269575 0.218583 0.209125 11.00000 -1.20000 AFIX 0 C24 1 1.354484 0.179913 0.266658 11.00000 0.01428 0.02415 = 0.03186 0.00351 0.00462 0.00369 AFIX 23 H24A 2 1.399086 0.211198 0.291544 11.00000 -1.20000 H24B 2 1.450474 0.140927 0.255801 11.00000 -1.20000 AFIX 0 C22 1 1.062953 0.353588 0.212611 11.00000 0.02709 0.02550 = 0.01632 0.00655 -0.00184 -0.00313 AFIX 23 H22A 2 1.005283 0.308066 0.194402 11.00000 -1.20000 H22B 2 1.158520 0.383707 0.197073 11.00000 -1.20000 AFIX 0 C21 1 0.927892 0.425305 0.224875 11.00000 0.02683 0.02182 = 0.02786 0.01021 -0.00844 -0.00197 AFIX 23 H21A 2 0.866450 0.447198 0.199878 11.00000 -1.20000 H21B 2 0.991905 0.478332 0.236829 11.00000 -1.20000 AFIX 0 C20 1 0.788175 0.393788 0.255313 11.00000 0.02182 0.01675 = 0.02868 0.00382 -0.00594 0.00395 AFIX 23 H20A 2 0.719884 0.447714 0.264665 11.00000 -1.20000 H20B 2 0.704922 0.351254 0.241455 11.00000 -1.20000 AFIX 0 C17 1 0.733224 0.339020 0.324709 11.00000 0.02043 0.02224 = 0.02631 -0.00288 0.00538 0.00595 AFIX 23 H17A 2 0.617033 0.323580 0.312294 11.00000 -1.20000 H17B 2 0.721767 0.399076 0.338595 11.00000 -1.20000 AFIX 0 C16 1 0.782809 0.266226 0.355909 11.00000 0.02304 0.02750 = 0.02050 -0.00343 0.00631 0.00692 AFIX 23 H16A 2 0.684020 0.256706 0.375086 11.00000 -1.20000 H16B 2 0.888166 0.286060 0.371795 11.00000 -1.20000 AFIX 0 C15 1 1.019434 0.081041 0.402547 11.00000 0.01952 0.01982 = 0.02556 0.00089 -0.00494 0.00380 HKLF 4 REM Mono in P2(1)/n REM R1 = 0.0332 for 7274 Fo > 4sig(Fo) and 0.0416 for all 8308 data REM 433 parameters refined using 0 restraints END WGHT 0.0320 8.4953 REM Instructions for potential hydrogen bonds HTAB C10 N3 HTAB C8 N3 HTAB C6 Br1 EQIV $1 -x+3/2, y+1/2, -z+1/2 HTAB C7 Br2_$1 HTAB C7 Br1 EQIV $2 -x, -y+2, -z HTAB C7 Br1_$2 EQIV $3 x+1, y, z HTAB C5 O4_$3 HTAB C4 O1_$3 HTAB C4 Br1 HTAB C11 Br1_$2 HTAB C12 Br1 HTAB C12 Br1_$2 HTAB C18 Br2 HTAB C19 Br2 EQIV $4 -x+1, -y+1, -z HTAB C23 O1_$4 HTAB C24 Br2 HTAB C24 O8_$3 HTAB C22 S1_$4 HTAB C22 N6 HTAB C20 O8_$1 HTAB C20 N6 HTAB C16 Br2 REM Highest difference peak 0.826, deepest hole -1.077, 1-sigma level 0.105 Q1 1 -0.3560 0.5993 -0.0306 11.00000 0.05 0.83 Q2 1 0.9695 0.2554 0.2651 11.00000 0.05 0.58 Q3 1 1.1598 0.2457 0.3814 11.00000 0.05 0.57 Q4 1 0.9823 0.2200 0.2995 11.00000 0.05 0.55 Q5 1 1.0597 0.2251 0.2731 11.00000 0.05 0.52 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 Br1 Br 0.04078(5) 0.97188(2) -0.06684(2) 0.02793(9) Uani 1 1 d . . Br2 Br 1.25448(5) 0.23866(2) 0.37082(2) 0.02412(9) Uani 1 1 d . . Mn1 Mn -0.21938(6) 0.90470(3) -0.10578(2) 0.01740(11) Uani 1 1 d . . Co1 Co -0.10794(5) 0.73266(3) -0.04693(2) 0.01381(9) Uani 1 1 d . . Mn2 Mn 1.10429(6) 0.08848(3) 0.35111(2) 0.01523(10) Uani 1 1 d . . Co2 Co 0.97112(5) 0.22461(3) 0.27763(2) 0.01212(9) Uani 1 1 d . . S1 S -0.07967(10) 0.75683(6) -0.11317(2) 0.01799(16) Uani 1 1 d . . S2 S -0.34058(10) 0.82370(5) -0.04884(2) 0.01620(15) Uani 1 1 d . . S3 S 0.83071(10) 0.15888(5) 0.32865(2) 0.01668(15) Uani 1 1 d . . S4 S 1.16166(10) 0.10868(5) 0.27912(2) 0.01593(15) Uani 1 1 d . . O4 O -0.3392(4) 0.60417(18) -0.06678(10) 0.0370(7) Uani 1 1 d . . O3 O -0.0506(4) 0.98674(19) -0.17796(8) 0.0325(6) Uani 1 1 d . . O1 O -0.5103(3) 0.8458(2) -0.15927(8) 0.0359(6) Uani 1 1 d . . O6 O 1.4481(3) 0.00467(19) 0.37394(8) 0.0313(6) Uani 1 1 d . . O5 O 0.9573(4) -0.09414(17) 0.33364(8) 0.0317(6) Uani 1 1 d . . N6 N 0.8332(4) 0.19089(19) 0.23570(8) 0.0209(6) Uani 1 1 d . . O8 O 0.7722(3) 0.11824(17) 0.23037(8) 0.0285(6) Uani 1 1 d . . O7 O 0.9599(4) 0.0776(2) 0.43448(8) 0.0323(6) Uani 1 1 d . . N2 N -0.0778(4) 0.75317(18) 0.01256(8) 0.0174(5) Uani 1 1 d . . N1 N 0.1454(3) 0.69589(19) -0.04165(8) 0.0182(5) Uani 1 1 d . . N3 N -0.2140(4) 0.62349(19) -0.04754(9) 0.0224(6) Uani 1 1 d . . O2 O -0.4286(4) 1.06762(19) -0.08262(9) 0.0420(7) Uani 1 1 d . . N4 N 0.8691(3) 0.34648(18) 0.29165(8) 0.0169(5) Uani 1 1 d . . N5 N 1.1425(3) 0.30458(18) 0.24878(8) 0.0158(5) Uani 1 1 d . . C10 C -0.0539(5) 0.6656(2) 0.03584(10) 0.0220(7) Uani 1 1 d . . H10A H -0.1515 0.6230 0.0287 0.026 Uiso 1 1 calc R U H10B H -0.0604 0.6786 0.0655 0.026 Uiso 1 1 calc R U C9 C 0.1230(5) 0.6194(2) 0.02665(11) 0.0256(7) Uani 1 1 d . . H9A H 0.1225 0.5576 0.0393 0.031 Uiso 1 1 calc R U H9B H 0.2180 0.6553 0.0403 0.031 Uiso 1 1 calc R U C8 C 0.1708(5) 0.6087(2) -0.01826(11) 0.0257(7) Uani 1 1 d . . H8A H 0.2958 0.5891 -0.0203 0.031 Uiso 1 1 calc R U H8B H 0.0962 0.5600 -0.0306 0.031 Uiso 1 1 calc R U C6 C 0.2231(4) 0.7743(2) -0.01793(10) 0.0216(7) Uani 1 1 d . . H6A H 0.2520 0.8251 -0.0368 0.026 Uiso 1 1 calc R U H6B H 0.3340 0.7542 -0.0043 0.026 Uiso 1 1 calc R U C7 C 0.0905(4) 0.8086(2) 0.01461(10) 0.0200(6) Uani 1 1 d . . H7A H 0.1445 0.8028 0.0422 0.024 Uiso 1 1 calc R U H7B H 0.0633 0.8742 0.0098 0.024 Uiso 1 1 calc R U C5 C 0.2282(4) 0.6863(3) -0.08296(10) 0.0240(7) Uani 1 1 d . . H5A H 0.3585 0.6906 -0.0801 0.029 Uiso 1 1 calc R U H5B H 0.1993 0.6251 -0.0944 0.029 Uiso 1 1 calc R U C4 C 0.1634(4) 0.7597(3) -0.11197(10) 0.0234(7) Uani 1 1 d . . H4A H 0.2102 0.7484 -0.1397 0.028 Uiso 1 1 calc R U H4B H 0.2051 0.8207 -0.1027 0.028 Uiso 1 1 calc R U C11 C -0.2306(4) 0.8058(2) 0.03004(10) 0.0209(7) Uani 1 1 d . . H11A H -0.1932 0.8351 0.0560 0.025 Uiso 1 1 calc R U H11B H -0.3285 0.7628 0.0361 0.025 Uiso 1 1 calc R U C12 C -0.2956(4) 0.8790(2) 0.00044(9) 0.0205(6) Uani 1 1 d . . H12A H -0.2045 0.9273 -0.0027 0.025 Uiso 1 1 calc R U H12B H -0.4047 0.9080 0.0109 0.025 Uiso 1 1 calc R U C3 C -0.1152(4) 0.9554(2) -0.15002(10) 0.0217(7) Uani 1 1 d . . C1 C -0.3993(4) 0.8663(2) -0.13750(10) 0.0221(7) Uani 1 1 d . . C2 C -0.3447(5) 1.0062(2) -0.09222(10) 0.0258(7) Uani 1 1 d . . C14 C 1.3163(4) 0.0372(2) 0.36454(10) 0.0202(6) Uani 1 1 d . . C13 C 1.0126(4) -0.0226(2) 0.33978(10) 0.0207(7) Uani 1 1 d . . C18 C 1.0281(4) 0.3987(2) 0.30625(10) 0.0221(7) Uani 1 1 d . . H18A H 1.0513 0.3843 0.3354 0.027 Uiso 1 1 calc R U H18B H 1.0049 0.4654 0.3040 0.027 Uiso 1 1 calc R U C19 C 1.1927(4) 0.3737(2) 0.28074(10) 0.0200(6) Uani 1 1 d . . H19A H 1.2401 0.4295 0.2676 0.024 Uiso 1 1 calc R U H19B H 1.2860 0.3479 0.2988 0.024 Uiso 1 1 calc R U C23 C 1.2992(4) 0.2502(2) 0.23506(11) 0.0242(7) Uani 1 1 d . . H23A H 1.3992 0.2924 0.2299 0.029 Uiso 1 1 calc R U H23B H 1.2696 0.2186 0.2091 0.029 Uiso 1 1 calc R U C24 C 1.3545(4) 0.1799(2) 0.26666(11) 0.0234(7) Uani 1 1 d . . H24A H 1.3991 0.2112 0.2915 0.028 Uiso 1 1 calc R U H24B H 1.4505 0.1409 0.2558 0.028 Uiso 1 1 calc R U C22 C 1.0630(5) 0.3536(2) 0.21261(10) 0.0230(7) Uani 1 1 d . . H22A H 1.0053 0.3081 0.1944 0.028 Uiso 1 1 calc R U H22B H 1.1585 0.3837 0.1971 0.028 Uiso 1 1 calc R U C21 C 0.9279(5) 0.4253(2) 0.22488(11) 0.0256(7) Uani 1 1 d . . H21A H 0.8664 0.4472 0.1999 0.031 Uiso 1 1 calc R U H21B H 0.9919 0.4783 0.2368 0.031 Uiso 1 1 calc R U C20 C 0.7882(4) 0.3938(2) 0.25531(11) 0.0225(7) Uani 1 1 d . . H20A H 0.7199 0.4477 0.2647 0.027 Uiso 1 1 calc R U H20B H 0.7049 0.3513 0.2415 0.027 Uiso 1 1 calc R U C17 C 0.7332(4) 0.3390(2) 0.32471(10) 0.0230(7) Uani 1 1 d . . H17A H 0.6170 0.3236 0.3123 0.028 Uiso 1 1 calc R U H17B H 0.7218 0.3991 0.3386 0.028 Uiso 1 1 calc R U C16 C 0.7828(5) 0.2662(2) 0.35591(10) 0.0236(7) Uani 1 1 d . . H16A H 0.6840 0.2567 0.3751 0.028 Uiso 1 1 calc R U H16B H 0.8882 0.2861 0.3718 0.028 Uiso 1 1 calc R U C15 C 1.0194(4) 0.0810(2) 0.40255(10) 0.0217(7) 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 Br1 0.0352(2) 0.02318(18) 0.02539(18) -0.00361(13) -0.00331(14) -0.00629(14) Br2 0.02965(18) 0.02035(16) 0.02219(16) -0.00103(12) -0.00871(13) -0.00067(13) Mn1 0.0195(2) 0.0182(2) 0.0145(2) 0.00095(18) 0.00077(18) -0.00052(19) Co1 0.01204(19) 0.0144(2) 0.01503(19) -0.00266(15) -0.00011(15) -0.00068(15) Mn2 0.0159(2) 0.0139(2) 0.0158(2) 0.00175(17) -0.00193(17) 0.00157(17) Co2 0.01223(19) 0.01141(19) 0.01271(19) -0.00060(14) -0.00053(14) -0.00032(14) S1 0.0166(4) 0.0221(4) 0.0153(3) -0.0049(3) 0.0007(3) -0.0006(3) S2 0.0145(3) 0.0179(4) 0.0162(3) 0.0000(3) 0.0019(3) 0.0012(3) S3 0.0145(3) 0.0178(4) 0.0178(4) 0.0032(3) 0.0015(3) 0.0004(3) S4 0.0160(3) 0.0144(3) 0.0175(3) -0.0015(3) 0.0007(3) 0.0025(3) O4 0.0265(14) 0.0246(14) 0.0599(19) -0.0093(13) -0.0087(13) -0.0050(11) O3 0.0345(14) 0.0402(15) 0.0228(13) 0.0089(11) 0.0034(11) -0.0050(12) O1 0.0226(13) 0.0571(19) 0.0279(14) 0.0015(13) -0.0019(11) -0.0026(13) O6 0.0235(13) 0.0323(14) 0.0380(15) 0.0033(12) -0.0042(11) 0.0084(11) O5 0.0363(15) 0.0202(13) 0.0386(15) -0.0022(11) -0.0037(12) -0.0059(11) N6 0.0207(14) 0.0211(14) 0.0207(13) -0.0004(11) -0.0079(11) -0.0019(11) O8 0.0276(13) 0.0227(13) 0.0350(14) -0.0070(10) -0.0093(11) -0.0024(10) O7 0.0322(14) 0.0417(16) 0.0231(13) 0.0055(11) 0.0067(11) 0.0084(12) N2 0.0192(13) 0.0168(13) 0.0162(12) 0.0009(10) -0.0017(10) -0.0014(10) N1 0.0124(12) 0.0197(13) 0.0225(13) -0.0036(11) -0.0010(10) 0.0008(10) N3 0.0217(14) 0.0151(13) 0.0303(15) -0.0019(11) -0.0034(12) -0.0019(11) O2 0.0565(19) 0.0272(15) 0.0427(17) 0.0064(12) 0.0179(14) 0.0148(14) N4 0.0188(13) 0.0142(12) 0.0177(13) -0.0013(10) -0.0031(10) -0.0004(10) N5 0.0158(12) 0.0163(12) 0.0154(12) 0.0002(10) -0.0012(10) -0.0026(10) C10 0.0264(17) 0.0197(16) 0.0200(16) 0.0048(13) -0.0021(13) 0.0004(13) C9 0.0244(17) 0.0231(17) 0.0293(18) 0.0044(14) -0.0067(14) 0.0024(14) C8 0.0206(16) 0.0210(17) 0.0355(19) -0.0013(14) -0.0064(14) 0.0055(13) C6 0.0155(15) 0.0248(17) 0.0246(17) -0.0035(13) -0.0037(12) -0.0040(13) C7 0.0213(16) 0.0203(16) 0.0183(15) -0.0030(12) -0.0032(12) -0.0033(13) C5 0.0151(15) 0.0318(19) 0.0251(17) -0.0087(14) 0.0036(13) 0.0028(13) C4 0.0150(15) 0.0325(19) 0.0230(16) -0.0086(14) 0.0052(12) -0.0018(13) C11 0.0233(16) 0.0244(16) 0.0152(15) -0.0008(12) 0.0043(12) 0.0011(13) C12 0.0239(16) 0.0223(16) 0.0154(14) -0.0034(12) 0.0048(12) 0.0040(13) C3 0.0212(16) 0.0212(16) 0.0226(16) 0.0018(13) -0.0022(13) -0.0012(13) C1 0.0216(16) 0.0262(17) 0.0186(15) 0.0020(13) 0.0053(13) 0.0049(13) C2 0.035(2) 0.0233(17) 0.0191(16) 0.0060(13) 0.0060(14) 0.0017(15) C14 0.0230(17) 0.0197(16) 0.0180(15) 0.0007(12) -0.0010(12) -0.0009(13) C13 0.0187(15) 0.0235(17) 0.0198(15) 0.0052(13) -0.0014(12) 0.0037(13) C18 0.0281(17) 0.0136(15) 0.0245(16) -0.0046(12) -0.0066(13) -0.0022(13) C19 0.0211(16) 0.0133(14) 0.0256(16) 0.0011(12) -0.0043(13) -0.0062(12) C23 0.0195(16) 0.0292(18) 0.0240(17) 0.0032(14) 0.0080(13) 0.0020(14) C24 0.0143(15) 0.0241(17) 0.0319(18) 0.0035(14) 0.0046(13) 0.0037(13) C22 0.0271(17) 0.0255(17) 0.0163(15) 0.0065(13) -0.0018(13) -0.0031(14) C21 0.0268(18) 0.0218(17) 0.0279(17) 0.0102(14) -0.0084(14) -0.0020(14) C20 0.0218(16) 0.0167(15) 0.0287(17) 0.0038(13) -0.0059(13) 0.0040(12) C17 0.0204(16) 0.0222(17) 0.0263(17) -0.0029(13) 0.0054(13) 0.0060(13) C16 0.0230(16) 0.0275(18) 0.0205(16) -0.0034(13) 0.0063(13) 0.0069(14) C15 0.0195(16) 0.0198(16) 0.0256(17) 0.0009(13) -0.0049(13) 0.0038(13) 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' S S 0.1246 0.1234 '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' Co Co 0.3494 0.9721 '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 C1 Mn1 C3 89.83(15) C1 Mn1 C2 90.06(16) C3 Mn1 C2 95.49(15) C1 Mn1 S2 90.22(11) C3 Mn1 S2 174.15(11) C2 Mn1 S2 90.36(11) C1 Mn1 S1 89.65(11) C3 Mn1 S1 95.13(11) C2 Mn1 S1 169.37(11) S2 Mn1 S1 79.02(3) C1 Mn1 Br1 173.80(11) C3 Mn1 Br1 84.47(11) C2 Mn1 Br1 88.08(12) S2 Mn1 Br1 95.70(3) S1 Mn1 Br1 93.27(3) N3 Co1 N2 101.13(12) N3 Co1 N1 101.13(12) N2 Co1 N1 81.61(11) N3 Co1 S2 100.25(9) N2 Co1 S2 91.22(8) N1 Co1 S2 158.39(8) N3 Co1 S1 100.32(10) N2 Co1 S1 158.36(8) N1 Co1 S1 91.49(8) S2 Co1 S1 87.77(3) C13 Mn2 C15 89.94(15) C13 Mn2 C14 90.97(15) C15 Mn2 C14 93.98(14) C13 Mn2 S3 89.55(10) C15 Mn2 S3 89.93(10) C14 Mn2 S3 176.05(11) C13 Mn2 S4 88.89(11) C15 Mn2 S4 169.08(10) C14 Mn2 S4 96.89(10) S3 Mn2 S4 79.20(3) C13 Mn2 Br2 175.04(10) C15 Mn2 Br2 88.65(11) C14 Mn2 Br2 84.38(10) S3 Mn2 Br2 95.21(3) S4 Mn2 Br2 93.38(3) N6 Co2 N5 100.02(12) N6 Co2 N4 101.44(12) N5 Co2 N4 80.95(11) N6 Co2 S3 100.46(10) N5 Co2 S3 159.16(8) N4 Co2 S3 91.26(8) N6 Co2 S4 100.46(10) N5 Co2 S4 91.75(8) N4 Co2 S4 157.81(8) S3 Co2 S4 88.28(3) C4 S1 Co1 95.10(11) C4 S1 Mn1 114.59(12) Co1 S1 Mn1 89.84(3) C12 S2 Co1 95.66(11) C12 S2 Mn1 113.56(11) Co1 S2 Mn1 90.42(3) C16 S3 Co2 95.58(12) C16 S3 Mn2 112.65(12) Co2 S3 Mn2 89.89(3) C24 S4 Co2 94.67(11) C24 S4 Mn2 115.79(12) Co2 S4 Mn2 89.52(3) O8 N6 Co2 126.3(2) C10 N2 C11 109.3(2) C10 N2 C7 109.6(2) C11 N2 C7 111.2(2) C10 N2 Co1 112.6(2) C11 N2 Co1 111.69(19) C7 N2 Co1 102.32(18) C8 N1 C6 109.5(3) C8 N1 C5 109.3(3) C6 N1 C5 111.9(3) C8 N1 Co1 113.0(2) C6 N1 Co1 102.21(19) C5 N1 Co1 110.8(2) O4 N3 Co1 125.8(3) C18 N4 C20 109.9(3) C18 N4 C17 111.0(3) C20 N4 C17 109.1(2) C18 N4 Co2 102.45(19) C20 N4 Co2 112.5(2) C17 N4 Co2 111.74(19) C23 N5 C22 109.0(2) C23 N5 C19 111.7(3) C22 N5 C19 109.2(2) C23 N5 Co2 110.7(2) C22 N5 Co2 113.27(19) C19 N5 Co2 102.90(19) N2 C10 C9 112.1(3) N2 C10 H10A 109.2 C9 C10 H10A 109.2 N2 C10 H10B 109.2 C9 C10 H10B 109.2 H10A C10 H10B 107.9 C10 C9 C8 116.8(3) C10 C9 H9A 108.1 C8 C9 H9A 108.1 C10 C9 H9B 108.1 C8 C9 H9B 108.1 H9A C9 H9B 107.3 N1 C8 C9 112.1(3) N1 C8 H8A 109.2 C9 C8 H8A 109.2 N1 C8 H8B 109.2 C9 C8 H8B 109.2 H8A C8 H8B 107.9 N1 C6 C7 110.4(3) N1 C6 H6A 109.6 C7 C6 H6A 109.6 N1 C6 H6B 109.6 C7 C6 H6B 109.6 H6A C6 H6B 108.1 N2 C7 C6 110.3(2) N2 C7 H7A 109.6 C6 C7 H7A 109.6 N2 C7 H7B 109.6 C6 C7 H7B 109.6 H7A C7 H7B 108.1 C4 C5 N1 111.4(3) C4 C5 H5A 109.3 N1 C5 H5A 109.3 C4 C5 H5B 109.3 N1 C5 H5B 109.3 H5A C5 H5B 108.0 C5 C4 S1 108.4(2) C5 C4 H4A 110.0 S1 C4 H4A 110.0 C5 C4 H4B 110.0 S1 C4 H4B 110.0 H4A C4 H4B 108.4 N2 C11 C12 111.1(3) N2 C11 H11A 109.4 C12 C11 H11A 109.4 N2 C11 H11B 109.4 C12 C11 H11B 109.4 H11A C11 H11B 108.0 C11 C12 S2 108.0(2) C11 C12 H12A 110.1 S2 C12 H12A 110.1 C11 C12 H12B 110.1 S2 C12 H12B 110.1 H12A C12 H12B 108.4 O3 C3 Mn1 179.4(3) O1 C1 Mn1 175.9(3) O2 C2 Mn1 176.8(3) O6 C14 Mn2 178.3(3) O5 C13 Mn2 177.8(3) N4 C18 C19 110.7(2) N4 C18 H18A 109.5 C19 C18 H18A 109.5 N4 C18 H18B 109.5 C19 C18 H18B 109.5 H18A C18 H18B 108.1 N5 C19 C18 109.7(2) N5 C19 H19A 109.7 C18 C19 H19A 109.7 N5 C19 H19B 109.7 C18 C19 H19B 109.7 H19A C19 H19B 108.2 N5 C23 C24 111.5(3) N5 C23 H23A 109.3 C24 C23 H23A 109.3 N5 C23 H23B 109.3 C24 C23 H23B 109.3 H23A C23 H23B 108.0 C23 C24 S4 108.6(2) C23 C24 H24A 110.0 S4 C24 H24A 110.0 C23 C24 H24B 110.0 S4 C24 H24B 110.0 H24A C24 H24B 108.3 N5 C22 C21 112.5(3) N5 C22 H22A 109.1 C21 C22 H22A 109.1 N5 C22 H22B 109.1 C21 C22 H22B 109.1 H22A C22 H22B 107.8 C22 C21 C20 115.9(3) C22 C21 H21A 108.3 C20 C21 H21A 108.3 C22 C21 H21B 108.3 C20 C21 H21B 108.3 H21A C21 H21B 107.4 N4 C20 C21 112.1(3) N4 C20 H20A 109.2 C21 C20 H20A 109.2 N4 C20 H20B 109.2 C21 C20 H20B 109.2 H20A C20 H20B 107.9 N4 C17 C16 111.7(3) N4 C17 H17A 109.3 C16 C17 H17A 109.3 N4 C17 H17B 109.3 C16 C17 H17B 109.3 H17A C17 H17B 107.9 C17 C16 S3 108.4(2) C17 C16 H16A 110.0 S3 C16 H16A 110.0 C17 C16 H16B 110.0 S3 C16 H16B 110.0 H16A C16 H16B 108.4 O7 C15 Mn2 177.4(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 Mn1 2.5300(7) Br2 Mn2 2.5447(7) Mn1 C1 1.793(4) Mn1 C3 1.813(3) Mn1 C2 1.813(4) Mn1 S2 2.3959(9) Mn1 S1 2.4117(10) Co1 N3 1.781(3) Co1 N2 1.982(3) Co1 N1 1.994(3) Co1 S2 2.2025(9) Co1 S1 2.2098(9) Mn2 C13 1.797(4) Mn2 C15 1.812(4) Mn2 C14 1.818(3) Mn2 S3 2.4162(9) Mn2 S4 2.4189(9) Co2 N6 1.785(3) Co2 N5 1.988(3) Co2 N4 1.991(3) Co2 S3 2.2064(9) Co2 S4 2.2193(9) S1 C4 1.838(3) S2 C12 1.833(3) S3 C16 1.838(3) S4 C24 1.838(3) O4 N3 1.166(4) O3 C3 1.137(4) O1 C1 1.135(4) O6 C14 1.143(4) O5 C13 1.140(4) N6 O8 1.167(4) O7 C15 1.143(4) N2 C10 1.496(4) N2 C11 1.504(4) N2 C7 1.508(4) N1 C8 1.495(4) N1 C6 1.498(4) N1 C5 1.503(4) O2 C2 1.143(4) N4 C18 1.497(4) N4 C20 1.500(4) N4 C17 1.503(4) N5 C23 1.497(4) N5 C22 1.504(4) N5 C19 1.498(4) C10 C9 1.529(5) C10 H10A 0.9900 C10 H10B 0.9900 C9 C8 1.526(5) C9 H9A 0.9900 C9 H9B 0.9900 C8 H8A 0.9900 C8 H8B 0.9900 C6 C7 1.552(5) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7A 0.9900 C7 H7B 0.9900 C5 C4 1.509(5) C5 H5A 0.9900 C5 H5B 0.9900 C4 H4A 0.9900 C4 H4B 0.9900 C11 C12 1.520(5) C11 H11A 0.9900 C11 H11B 0.9900 C12 H12A 0.9900 C12 H12B 0.9900 C18 C19 1.548(5) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19A 0.9900 C19 H19B 0.9900 C23 C24 1.512(5) C23 H23A 0.9900 C23 H23B 0.9900 C24 H24A 0.9900 C24 H24B 0.9900 C22 C21 1.517(5) C22 H22A 0.9900 C22 H22B 0.9900 C21 C20 1.530(5) C21 H21A 0.9900 C21 H21B 0.9900 C20 H20A 0.9900 C20 H20B 0.9900 C17 C16 1.517(5) C17 H17A 0.9900 C17 H17B 0.9900 C16 H16A 0.9900 C16 H16B 0.9900 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 N5 Co2 N6 O8 140.9(3) N4 Co2 N6 O8 -136.4(3) S3 Co2 N6 O8 -43.0(3) S4 Co2 N6 O8 47.2(3) N2 Co1 N3 O4 132.7(3) N1 Co1 N3 O4 -143.8(3) S2 Co1 N3 O4 39.4(3) S1 Co1 N3 O4 -50.2(3) C11 N2 C10 C9 -166.7(3) C7 N2 C10 C9 -44.6(3) Co1 N2 C10 C9 68.6(3) N2 C10 C9 C8 -48.8(4) C6 N1 C8 C9 45.8(4) C5 N1 C8 C9 168.7(3) Co1 N1 C8 C9 -67.4(3) C10 C9 C8 N1 48.3(4) C8 N1 C6 C7 -82.6(3) C5 N1 C6 C7 156.1(3) Co1 N1 C6 C7 37.5(3) C10 N2 C7 C6 82.4(3) C11 N2 C7 C6 -156.7(3) Co1 N2 C7 C6 -37.3(3) N1 C6 C7 N2 -0.3(4) C8 N1 C5 C4 163.8(3) C6 N1 C5 C4 -74.8(3) Co1 N1 C5 C4 38.6(3) N1 C5 C4 S1 -54.0(3) Co1 S1 C4 C5 39.9(2) Mn1 S1 C4 C5 132.1(2) C10 N2 C11 C12 -162.8(3) C7 N2 C11 C12 76.0(3) Co1 N2 C11 C12 -37.6(3) N2 C11 C12 S2 53.0(3) Co1 S2 C12 C11 -40.1(2) Mn1 S2 C12 C11 -133.0(2) C20 N4 C18 C19 -82.4(3) C17 N4 C18 C19 156.8(3) Co2 N4 C18 C19 37.4(3) C23 N5 C19 C18 -156.7(3) C22 N5 C19 C18 82.6(3) Co2 N5 C19 C18 -38.0(3) N4 C18 C19 N5 0.3(4) C22 N5 C23 C24 -164.4(3) C19 N5 C23 C24 74.9(3) Co2 N5 C23 C24 -39.1(3) N5 C23 C24 S4 54.1(3) Co2 S4 C24 C23 -39.2(2) Mn2 S4 C24 C23 -131.0(2) C23 N5 C22 C21 -168.2(3) C19 N5 C22 C21 -45.9(3) Co2 N5 C22 C21 68.1(3) N5 C22 C21 C20 -48.6(4) C18 N4 C20 C21 43.8(4) C17 N4 C20 C21 165.7(3) Co2 N4 C20 C21 -69.7(3) C22 C21 C20 N4 49.6(4) C18 N4 C17 C16 -77.7(3) C20 N4 C17 C16 161.0(3) Co2 N4 C17 C16 36.0(3) N4 C17 C16 S3 -51.9(3) Co2 S3 C16 C17 39.7(2) Mn2 S3 C16 C17 131.9(2)