#------------------------------------------------------------------------------ #$Date: 2023-11-17 01:42:48 +0200 (Fri, 17 Nov 2023) $ #$Revision: 287658 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247748.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_7247748 loop_ _publ_author_name 'Kumar, Jayasree' 'Tarannum, Ibtesham' 'Zheng, Yan-Zhen' 'Singh, Saurabh Kumar' 'Mondal, Kartik Chandra' _publ_section_title ; Assembly of MnIII ions into Di-, Tetra-, Deca-nuclear Coordination Complexes, Zero- to Three-Dimensional Molecular Framework: Molecular Spin Flop to and short Range Bulk Magnetic Spin Flop Ordering ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00967J _journal_year 2023 _chemical_formula_moiety 'C30 H28 Mn2 N6 O8' _chemical_formula_sum 'C30 H28 Mn2 N6 O8' _chemical_formula_weight 710.46 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2018-08-08 deposited with the CCDC. 2023-11-08 downloaded from the CCDC. ; _cell_angle_alpha 68.52(4) _cell_angle_beta 73.73(4) _cell_angle_gamma 71.10(6) _cell_formula_units_Z 2 _cell_length_a 10.063(12) _cell_length_b 12.143(15) _cell_length_c 15.195(17) _cell_measurement_reflns_used 7649 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 28.038 _cell_measurement_theta_min 2.931 _cell_volume 1607(3) _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-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 53693 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.038 _diffrn_reflns_theta_min 2.931 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.468 _exptl_crystal_description BLOCK _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 1.705 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.132 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 424 _refine_ls_number_reflns 7649 _refine_ls_number_restraints 38 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0684 _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^)+(0.0779P)^2^+8.6806P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1855 _refine_ls_wR_factor_ref 0.2105 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5494 _reflns_number_total 7649 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00967j2.cif _cod_data_source_block Mn-CP _cod_database_code 7247748 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.849 _shelx_estimated_absorpt_t_max 0.884 _shelx_res_file ; TITL shelxt_a.res in P-1 shelx.res created by SHELXL-2018/3 at 12:44:54 on 04-Aug-2018 CELL 0.71073 10.0632 12.1432 15.1946 68.521 73.726 71.096 ZERR 2.00 0.0120 0.0146 0.0168 0.039 0.038 0.059 LATT 1 SFAC C H N O MN UNIT 60 56 12 16 4 MERG 2 DELU 0.010 0.010 O8 O8A C33 C33A SIMU 0.040 0.080 1.700 O8 O8A C33 C33A EADP O8 O8A C33 C33A FMAP 2 PLAN 20 SIZE 0.150 0.150 0.200 ACTA BOND LIST 6 L.S. 20 TEMP -73 WGHT 0.077900 8.680600 FVAR 0.47559 0.48672 MN1 5 0.599965 0.536848 0.901136 11.00000 0.01884 0.03390 = 0.02136 -0.01027 -0.00381 -0.00724 MN2 5 0.102159 0.882964 0.473247 11.00000 0.02438 0.02579 = 0.02247 -0.00544 -0.00826 -0.00569 O2 4 0.548201 0.426121 0.855197 11.00000 0.02356 0.03586 = 0.02537 -0.01250 -0.00294 -0.00942 O6 4 0.060281 1.053468 0.410156 11.00000 0.02841 0.02715 = 0.01931 -0.00410 -0.00601 -0.00563 O4 4 0.261398 0.880735 0.523277 11.00000 0.02623 0.02754 = 0.02556 -0.00686 -0.01077 -0.00346 O3 4 0.412678 0.605631 0.956927 11.00000 0.01762 0.03476 = 0.02425 -0.01151 -0.00364 -0.00458 O1 4 0.683295 0.638771 0.925697 11.00000 0.02225 0.04148 = 0.03669 -0.01819 -0.00424 -0.00977 O5 4 -0.026028 0.847223 0.423786 11.00000 0.03211 0.03811 = 0.02861 -0.00583 -0.01191 -0.01324 N6 3 0.139789 0.713626 0.561764 11.00000 0.02394 0.02639 = 0.02502 -0.00732 -0.00761 -0.00382 N3 3 0.791007 0.451020 0.847326 11.00000 0.02150 0.03299 = 0.02111 -0.00971 -0.00237 -0.00875 N1 3 0.565469 0.674730 0.751857 11.00000 0.02323 0.03751 = 0.02302 -0.00659 -0.00706 -0.00648 N5 3 0.253719 0.680390 0.610988 11.00000 0.02763 0.03028 = 0.02985 -0.00738 -0.01035 -0.00465 N2 3 0.719728 0.167099 0.656870 11.00000 0.03022 0.03476 = 0.03018 -0.01372 -0.00475 -0.00959 N4 3 0.792039 0.363304 0.806336 11.00000 0.02324 0.04130 = 0.03167 -0.02181 -0.00077 -0.00738 O7 4 0.730810 0.807731 0.974984 11.00000 0.04982 0.07648 = 0.08485 -0.05555 0.01514 -0.03519 C8 1 0.659446 0.361016 0.814346 11.00000 0.03040 0.02827 = 0.02136 -0.00949 -0.00209 -0.00948 PART 1 O8 4 -0.209187 0.839478 0.321660 21.00000 0.06716 0.06179 = 0.05647 -0.00444 -0.03414 -0.02564 PART 2 O8A 4 -0.243373 0.857470 0.342159 -21.00000 0.06716 0.06179 = 0.05647 -0.00444 -0.03414 -0.02564 PART 0 C19 1 0.428921 0.765966 0.626589 11.00000 0.02403 0.02539 = 0.02680 -0.00934 -0.00517 -0.00391 C10 1 0.738224 0.238176 0.699943 11.00000 0.02385 0.03233 = 0.02804 -0.01217 -0.00069 -0.00786 AFIX 43 H10 2 0.825304 0.262686 0.680037 11.00000 -1.20000 AFIX 0 C22 1 0.063073 0.634756 0.585745 11.00000 0.03131 0.02477 = 0.02484 -0.00711 -0.00280 -0.00458 C7 1 0.914206 0.466310 0.843896 11.00000 0.02040 0.03471 = 0.03034 -0.01245 -0.00498 -0.00370 C11 1 0.635940 0.277866 0.772497 11.00000 0.02685 0.03651 = 0.02579 -0.01219 -0.00483 -0.00878 C21 1 0.307385 0.774897 0.584560 11.00000 0.02722 0.02622 = 0.01991 -0.00807 -0.00415 -0.00324 C20 1 0.458821 0.679542 0.712500 11.00000 0.02122 0.03495 = 0.02419 -0.00800 -0.00281 -0.00815 AFIX 43 H20 2 0.402421 0.621892 0.744663 11.00000 -1.20000 AFIX 0 C28 1 -0.087640 0.754959 0.459516 11.00000 0.02346 0.03349 = 0.02796 -0.01163 -0.00117 -0.01007 C6 1 0.817907 0.639899 0.913569 11.00000 0.02704 0.03979 = 0.02034 -0.00684 -0.00633 -0.01350 C23 1 -0.052638 0.652431 0.540640 11.00000 0.02733 0.03070 = 0.03102 -0.01325 -0.00029 -0.00645 C16 1 0.647116 0.754794 0.704491 11.00000 0.02648 0.03975 = 0.03063 -0.01075 -0.00726 -0.01163 AFIX 43 H16 2 0.721743 0.751629 0.732894 11.00000 -1.20000 AFIX 0 C17 1 0.627656 0.842344 0.615639 11.00000 0.03251 0.03298 = 0.04086 -0.00894 -0.00561 -0.01161 AFIX 43 H17 2 0.688875 0.895997 0.582878 11.00000 -1.20000 AFIX 0 C5 1 0.935448 0.556898 0.875425 11.00000 0.02278 0.03833 = 0.02463 -0.00535 -0.00568 -0.00999 C1 1 0.848749 0.728555 0.939736 11.00000 0.03393 0.04784 = 0.03263 -0.01539 -0.00555 -0.01578 C27 1 -0.192727 0.753974 0.414295 11.00000 0.03508 0.03762 = 0.04159 -0.01160 -0.01336 -0.01171 C18 1 0.516180 0.847369 0.577814 11.00000 0.04009 0.03038 = 0.03187 -0.00345 -0.01374 -0.00929 AFIX 43 H18 2 0.498128 0.906515 0.518110 11.00000 -1.20000 AFIX 0 C4 1 1.076513 0.562177 0.866499 11.00000 0.02270 0.04447 = 0.03359 -0.00718 -0.00607 -0.00956 AFIX 43 H4 2 1.154157 0.505969 0.841191 11.00000 -1.20000 AFIX 0 C32 1 0.044335 1.102874 0.312924 11.00000 0.04933 0.03328 = 0.02196 -0.00167 -0.01015 -0.00881 AFIX 33 H32A 2 0.023089 1.192174 0.294133 11.00000 -1.50000 H32B 2 0.133069 1.072154 0.272365 11.00000 -1.50000 H32C 2 -0.034232 1.078616 0.304723 11.00000 -1.50000 AFIX 0 C26 1 -0.265511 0.663460 0.451754 11.00000 0.03366 0.05017 = 0.06030 -0.02402 -0.01355 -0.01353 AFIX 43 H26 2 -0.337072 0.666853 0.420571 11.00000 -1.20000 AFIX 0 C14 1 0.597357 0.131949 0.686339 11.00000 0.03648 0.05417 = 0.04613 -0.02733 -0.00381 -0.01696 AFIX 43 H14 2 0.583521 0.080998 0.656586 11.00000 -1.20000 AFIX 0 C25 1 -0.236438 0.567360 0.534154 11.00000 0.03305 0.03745 = 0.05505 -0.02002 0.00064 -0.01419 AFIX 43 H25 2 -0.289199 0.506737 0.560375 11.00000 -1.20000 AFIX 0 C2 1 0.987461 0.732928 0.929936 11.00000 0.04184 0.06037 = 0.03777 -0.01446 -0.01195 -0.02595 AFIX 43 H2 2 1.005755 0.793462 0.947397 11.00000 -1.20000 AFIX 0 C3 1 1.102849 0.647320 0.893867 11.00000 0.02699 0.06134 = 0.04109 -0.01202 -0.00721 -0.02010 AFIX 43 H3 2 1.198454 0.649130 0.888721 11.00000 -1.20000 AFIX 0 C24 1 -0.130460 0.561655 0.576817 11.00000 0.03618 0.03841 = 0.04013 -0.01500 0.00197 -0.01606 AFIX 43 H24 2 -0.108438 0.494990 0.632227 11.00000 -1.20000 AFIX 0 C30 1 0.368023 0.733132 0.948368 11.00000 0.03228 0.04412 = 0.03748 -0.01198 -0.00950 -0.00353 AFIX 33 H30A 2 0.268616 0.753082 0.981238 11.00000 -1.50000 H30B 2 0.429232 0.752515 0.977808 11.00000 -1.50000 H30C 2 0.375659 0.781058 0.880199 11.00000 -1.50000 AFIX 0 C12 1 0.508480 0.240654 0.801628 11.00000 0.03632 0.06346 = 0.03789 -0.02662 0.00578 -0.02211 AFIX 43 H12 2 0.435710 0.266137 0.850619 11.00000 -1.20000 AFIX 0 C13 1 0.490336 0.166383 0.758011 11.00000 0.03789 0.07600 = 0.05438 -0.03876 0.01121 -0.03320 AFIX 43 H13 2 0.405132 0.139181 0.777050 11.00000 -1.20000 AFIX 0 C29 1 0.741858 0.918203 0.980801 11.00000 0.09880 0.08479 = 0.15952 -0.06247 -0.00329 -0.02314 AFIX 33 H29A 2 0.647921 0.962326 1.007411 11.00000 -1.50000 H29B 2 0.809664 0.899819 1.022655 11.00000 -1.50000 H29C 2 0.775627 0.968850 0.916361 11.00000 -1.50000 AFIX 0 PART 1 C33 1 -0.141614 0.889327 0.255223 21.00000 0.06716 0.06179 = 0.05647 -0.00444 -0.03414 -0.02564 AFIX 33 H33A 2 -0.201314 0.941310 0.206910 21.00000 -1.50000 H33B 2 -0.100606 0.940052 0.272387 21.00000 -1.50000 H33C 2 -0.064445 0.829757 0.228878 21.00000 -1.50000 AFIX 0 PART 2 C33A 1 -0.267294 0.958426 0.322996 -21.00000 0.06716 0.06179 = 0.05647 -0.00444 -0.03414 -0.02564 AFIX 33 H33D 2 -0.302873 0.995817 0.262207 -21.00000 -1.50000 H33E 2 -0.340075 0.985912 0.373955 -21.00000 -1.50000 H33F 2 -0.180050 0.982674 0.315910 -21.00000 -1.50000 AFIX 0 PART 0 H7 2 0.992206 0.420336 0.816274 11.00000 0.03291 H22 2 0.082838 0.560790 0.636256 11.00000 0.04218 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.2105, GooF = S = 1.068, Restrained GooF = 1.065 for all data REM R1 = 0.0684 for 5494 Fo > 4sig(Fo) and 0.1026 for all 7649 data REM 424 parameters refined using 38 restraints END WGHT 0.0779 8.4193 REM Highest difference peak 1.705, deepest hole -0.579, 1-sigma level 0.132 Q1 1 -0.0052 0.8702 0.1355 11.00000 0.05 1.70 Q2 1 0.6633 0.8969 0.9283 11.00000 0.05 1.16 Q3 1 0.6010 0.8805 0.5561 11.00000 0.05 0.73 Q4 1 0.3980 0.7782 0.7742 11.00000 0.05 0.72 Q5 1 0.1008 1.1976 0.3277 11.00000 0.05 0.71 Q6 1 0.7009 0.0381 0.7279 11.00000 0.05 0.68 Q7 1 0.8060 0.2988 0.8495 11.00000 0.05 0.63 Q8 1 1.0979 0.5481 0.8059 11.00000 0.05 0.56 Q9 1 0.0989 1.0854 0.2681 11.00000 0.05 0.53 Q10 1 1.0000 1.0000 1.0000 10.50000 0.05 0.53 Q11 1 0.8390 0.2024 0.7085 11.00000 0.05 0.48 Q12 1 0.5156 0.5822 0.9348 11.00000 0.05 0.47 Q13 1 0.9119 0.7820 0.8516 11.00000 0.05 0.47 Q14 1 0.5803 0.7581 0.5118 11.00000 0.05 0.46 Q15 1 0.5174 0.4210 0.6859 11.00000 0.05 0.46 Q16 1 0.4193 0.8411 0.9717 11.00000 0.05 0.44 Q17 1 0.7355 0.7819 0.8212 11.00000 0.05 0.44 Q18 1 0.7963 0.3955 0.8243 11.00000 0.05 0.43 Q19 1 0.4447 0.9156 0.8519 11.00000 0.05 0.42 Q20 1 0.1782 0.8348 0.4398 11.00000 0.05 0.41 ; _shelx_res_checksum 81022 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.59996(7) 0.53685(7) 0.90114(5) 0.02393(19) Uani 1 1 d . . . . . Mn2 Mn 0.10216(7) 0.88296(6) 0.47325(5) 0.02404(19) Uani 1 1 d . . . . . O2 O 0.5482(3) 0.4261(3) 0.8552(2) 0.0271(7) Uani 1 1 d . . . . . O6 O 0.0603(3) 1.0535(3) 0.4102(2) 0.0258(7) Uani 1 1 d . . . . . O4 O 0.2614(3) 0.8807(3) 0.5233(2) 0.0263(7) Uani 1 1 d . . . . . O3 O 0.4127(3) 0.6056(3) 0.9569(2) 0.0253(7) Uani 1 1 d . . . . . O1 O 0.6833(3) 0.6388(3) 0.9257(3) 0.0314(8) Uani 1 1 d . . . . . O5 O -0.0260(4) 0.8472(3) 0.4238(2) 0.0317(8) Uani 1 1 d . . . . . N6 N 0.1398(4) 0.7136(4) 0.5618(3) 0.0252(8) Uani 1 1 d . . . . . N3 N 0.7910(4) 0.4510(4) 0.8473(3) 0.0246(8) Uani 1 1 d . . . . . N1 N 0.5655(4) 0.6747(4) 0.7519(3) 0.0283(9) Uani 1 1 d . . . . . N5 N 0.2537(4) 0.6804(4) 0.6110(3) 0.0293(9) Uani 1 1 d . . . . . N2 N 0.7197(4) 0.1671(4) 0.6569(3) 0.0303(9) Uani 1 1 d . . . . . N4 N 0.7920(4) 0.3633(4) 0.8063(3) 0.0300(9) Uani 1 1 d . . . . . O7 O 0.7308(5) 0.8077(5) 0.9750(4) 0.0622(14) Uani 1 1 d . . . . . C8 C 0.6594(5) 0.3610(4) 0.8143(3) 0.0261(9) Uani 1 1 d . . . . . O8 O -0.209(2) 0.839(2) 0.3217(15) 0.058(2) Uani 0.487(11) 1 d . U P A 1 O8A O -0.2434(19) 0.857(2) 0.3422(13) 0.058(2) Uani 0.513(11) 1 d . U P A 2 C19 C 0.4289(5) 0.7660(4) 0.6266(3) 0.0254(9) Uani 1 1 d . . . . . C10 C 0.7382(5) 0.2382(4) 0.6999(3) 0.0278(10) Uani 1 1 d . . . . . H10 H 0.825304 0.262686 0.680037 0.033 Uiso 1 1 calc R U . . . C22 C 0.0631(5) 0.6348(4) 0.5857(3) 0.0282(10) Uani 1 1 d . . . . . C7 C 0.9142(5) 0.4663(5) 0.8439(4) 0.0285(10) Uani 1 1 d . . . . . C11 C 0.6359(5) 0.2779(5) 0.7725(3) 0.0287(10) Uani 1 1 d . . . . . C21 C 0.3074(5) 0.7749(4) 0.5846(3) 0.0250(9) Uani 1 1 d . . . . . C20 C 0.4588(5) 0.6795(5) 0.7125(3) 0.0271(10) Uani 1 1 d . . . . . H20 H 0.402421 0.621892 0.744663 0.032 Uiso 1 1 calc R U . . . C28 C -0.0876(5) 0.7550(5) 0.4595(3) 0.0276(10) Uani 1 1 d . . . . . C6 C 0.8179(5) 0.6399(5) 0.9136(3) 0.0280(10) Uani 1 1 d . . . . . C23 C -0.0526(5) 0.6524(5) 0.5406(4) 0.0298(10) Uani 1 1 d . . . . . C16 C 0.6471(5) 0.7548(5) 0.7045(4) 0.0309(10) Uani 1 1 d . . . . . H16 H 0.721743 0.751629 0.732894 0.037 Uiso 1 1 calc R U . . . C17 C 0.6277(6) 0.8423(5) 0.6156(4) 0.0355(11) Uani 1 1 d . . . . . H17 H 0.688875 0.895997 0.582878 0.043 Uiso 1 1 calc R U . . . C5 C 0.9354(5) 0.5569(5) 0.8754(3) 0.0289(10) Uani 1 1 d . . . . . C1 C 0.8487(6) 0.7286(5) 0.9397(4) 0.0359(11) Uani 1 1 d . . . . . C27 C -0.1927(6) 0.7540(5) 0.4143(4) 0.0361(11) Uani 1 1 d . . . . . C18 C 0.5162(6) 0.8474(5) 0.5778(4) 0.0342(11) Uani 1 1 d . . . . . H18 H 0.498128 0.906515 0.518110 0.041 Uiso 1 1 calc R U . . . C4 C 1.0765(5) 0.5622(5) 0.8665(4) 0.0344(11) Uani 1 1 d . . . . . H4 H 1.154157 0.505969 0.841191 0.041 Uiso 1 1 calc R U . . . C32 C 0.0443(6) 1.1029(5) 0.3129(3) 0.0364(12) Uani 1 1 d . . . . . H32A H 0.023089 1.192174 0.294133 0.055 Uiso 1 1 calc R U . . . H32B H 0.133069 1.072154 0.272365 0.055 Uiso 1 1 calc R U . . . H32C H -0.034232 1.078616 0.304723 0.055 Uiso 1 1 calc R U . . . C26 C -0.2655(6) 0.6635(6) 0.4518(5) 0.0440(14) Uani 1 1 d . . . . . H26 H -0.337072 0.666853 0.420571 0.053 Uiso 1 1 calc R U . . . C14 C 0.5974(6) 0.1319(6) 0.6863(4) 0.0414(13) Uani 1 1 d . . . . . H14 H 0.583521 0.080998 0.656586 0.050 Uiso 1 1 calc R U . . . C25 C -0.2364(6) 0.5674(5) 0.5342(4) 0.0406(13) Uani 1 1 d . . . . . H25 H -0.289199 0.506737 0.560375 0.049 Uiso 1 1 calc R U . . . C2 C 0.9875(6) 0.7329(6) 0.9299(4) 0.0423(13) Uani 1 1 d . . . . . H2 H 1.005755 0.793462 0.947397 0.051 Uiso 1 1 calc R U . . . C3 C 1.1028(6) 0.6473(6) 0.8939(4) 0.0416(13) Uani 1 1 d . . . . . H3 H 1.198454 0.649130 0.888721 0.050 Uiso 1 1 calc R U . . . C24 C -0.1305(6) 0.5617(5) 0.5768(4) 0.0375(12) Uani 1 1 d . . . . . H24 H -0.108438 0.494990 0.632227 0.045 Uiso 1 1 calc R U . . . C30 C 0.3680(6) 0.7331(5) 0.9484(4) 0.0389(12) Uani 1 1 d . . . . . H30A H 0.268616 0.753082 0.981238 0.058 Uiso 1 1 calc R U . . . H30B H 0.429232 0.752515 0.977808 0.058 Uiso 1 1 calc R U . . . H30C H 0.375659 0.781058 0.880199 0.058 Uiso 1 1 calc R U . . . C12 C 0.5085(6) 0.2407(6) 0.8016(4) 0.0428(14) Uani 1 1 d . . . . . H12 H 0.435710 0.266137 0.850619 0.051 Uiso 1 1 calc R U . . . C13 C 0.4903(6) 0.1664(7) 0.7580(5) 0.0499(16) Uani 1 1 d . . . . . H13 H 0.405132 0.139181 0.777050 0.060 Uiso 1 1 calc R U . . . C29 C 0.7419(13) 0.9182(10) 0.9808(10) 0.111(4) Uani 1 1 d . . . . . H29A H 0.647921 0.962326 1.007411 0.167 Uiso 1 1 calc R U . . . H29B H 0.809664 0.899819 1.022655 0.167 Uiso 1 1 calc R U . . . H29C H 0.775627 0.968850 0.916361 0.167 Uiso 1 1 calc R U . . . C33 C -0.1416(17) 0.8893(14) 0.2552(11) 0.058(2) Uani 0.487(11) 1 d . U P A 1 H33A H -0.201314 0.941310 0.206910 0.087 Uiso 0.487(11) 1 calc R U P A 1 H33B H -0.100606 0.940052 0.272387 0.087 Uiso 0.487(11) 1 calc R U P A 1 H33C H -0.064445 0.829757 0.228878 0.087 Uiso 0.487(11) 1 calc R U P A 1 C33A C -0.2673(16) 0.9584(13) 0.3230(10) 0.058(2) Uani 0.513(11) 1 d . U P A 2 H33D H -0.302873 0.995817 0.262207 0.087 Uiso 0.513(11) 1 calc R U P A 2 H33E H -0.340075 0.985912 0.373955 0.087 Uiso 0.513(11) 1 calc R U P A 2 H33F H -0.180050 0.982674 0.315910 0.087 Uiso 0.513(11) 1 calc R U P A 2 H7 H 0.992(6) 0.420(5) 0.816(4) 0.033(15) Uiso 1 1 d . . . . . H22 H 0.083(7) 0.561(6) 0.636(5) 0.042(16) Uiso 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 0.0188(3) 0.0339(4) 0.0214(3) -0.0103(3) -0.0038(3) -0.0072(3) Mn2 0.0244(4) 0.0258(4) 0.0225(3) -0.0054(3) -0.0083(3) -0.0057(3) O2 0.0236(16) 0.0359(18) 0.0254(16) -0.0125(14) -0.0029(13) -0.0094(14) O6 0.0284(16) 0.0271(17) 0.0193(15) -0.0041(13) -0.0060(12) -0.0056(13) O4 0.0262(16) 0.0275(17) 0.0256(16) -0.0069(13) -0.0108(13) -0.0035(13) O3 0.0176(14) 0.0348(18) 0.0242(16) -0.0115(13) -0.0036(12) -0.0046(13) O1 0.0223(16) 0.041(2) 0.0367(19) -0.0182(16) -0.0042(14) -0.0098(15) O5 0.0321(18) 0.038(2) 0.0286(17) -0.0058(15) -0.0119(14) -0.0132(15) N6 0.0239(19) 0.026(2) 0.0250(19) -0.0073(16) -0.0076(15) -0.0038(15) N3 0.0215(18) 0.033(2) 0.0211(18) -0.0097(16) -0.0024(14) -0.0087(16) N1 0.0232(19) 0.038(2) 0.0230(19) -0.0066(17) -0.0071(15) -0.0065(17) N5 0.028(2) 0.030(2) 0.030(2) -0.0074(17) -0.0104(16) -0.0046(17) N2 0.030(2) 0.035(2) 0.030(2) -0.0137(18) -0.0048(17) -0.0096(18) N4 0.0232(19) 0.041(2) 0.032(2) -0.0218(19) -0.0008(16) -0.0074(17) O7 0.050(3) 0.076(3) 0.085(4) -0.056(3) 0.015(2) -0.035(2) C8 0.030(2) 0.028(2) 0.021(2) -0.0095(18) -0.0021(18) -0.0095(19) O8 0.067(6) 0.062(5) 0.056(5) -0.004(3) -0.034(4) -0.026(4) O8A 0.067(6) 0.062(5) 0.056(5) -0.004(3) -0.034(4) -0.026(4) C19 0.024(2) 0.025(2) 0.027(2) -0.0093(18) -0.0052(18) -0.0039(18) C10 0.024(2) 0.032(3) 0.028(2) -0.012(2) -0.0007(18) -0.0079(19) C22 0.031(2) 0.025(2) 0.025(2) -0.0071(19) -0.0028(19) -0.0046(19) C7 0.020(2) 0.035(3) 0.030(2) -0.012(2) -0.0050(18) -0.0037(19) C11 0.027(2) 0.037(3) 0.026(2) -0.012(2) -0.0048(18) -0.009(2) C21 0.027(2) 0.026(2) 0.020(2) -0.0081(18) -0.0042(17) -0.0032(18) C20 0.021(2) 0.035(3) 0.024(2) -0.0080(19) -0.0028(17) -0.0082(19) C28 0.023(2) 0.033(3) 0.028(2) -0.012(2) -0.0012(18) -0.0101(19) C6 0.027(2) 0.040(3) 0.020(2) -0.0068(19) -0.0063(18) -0.014(2) C23 0.027(2) 0.031(3) 0.031(2) -0.013(2) -0.0003(19) -0.006(2) C16 0.026(2) 0.040(3) 0.031(2) -0.011(2) -0.0073(19) -0.012(2) C17 0.033(3) 0.033(3) 0.041(3) -0.009(2) -0.006(2) -0.012(2) C5 0.023(2) 0.038(3) 0.025(2) -0.005(2) -0.0057(18) -0.010(2) C1 0.034(3) 0.048(3) 0.033(3) -0.015(2) -0.006(2) -0.016(2) C27 0.035(3) 0.038(3) 0.042(3) -0.012(2) -0.013(2) -0.012(2) C18 0.040(3) 0.030(3) 0.032(3) -0.003(2) -0.014(2) -0.009(2) C4 0.023(2) 0.044(3) 0.034(3) -0.007(2) -0.006(2) -0.010(2) C32 0.049(3) 0.033(3) 0.022(2) -0.002(2) -0.010(2) -0.009(2) C26 0.034(3) 0.050(3) 0.060(4) -0.024(3) -0.014(3) -0.014(3) C14 0.036(3) 0.054(4) 0.046(3) -0.027(3) -0.004(2) -0.017(3) C25 0.033(3) 0.037(3) 0.055(3) -0.020(3) 0.001(2) -0.014(2) C2 0.042(3) 0.060(4) 0.038(3) -0.014(3) -0.012(2) -0.026(3) C3 0.027(3) 0.061(4) 0.041(3) -0.012(3) -0.007(2) -0.020(3) C24 0.036(3) 0.038(3) 0.040(3) -0.015(2) 0.002(2) -0.016(2) C30 0.032(3) 0.044(3) 0.037(3) -0.012(2) -0.010(2) -0.004(2) C12 0.036(3) 0.063(4) 0.038(3) -0.027(3) 0.006(2) -0.022(3) C13 0.038(3) 0.076(5) 0.054(4) -0.039(3) 0.011(3) -0.033(3) C29 0.099(8) 0.085(7) 0.160(12) -0.062(8) -0.003(8) -0.023(6) C33 0.067(6) 0.062(5) 0.056(5) -0.004(3) -0.034(4) -0.026(4) C33A 0.067(6) 0.062(5) 0.056(5) -0.004(3) -0.034(4) -0.026(4) 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' 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 O1 Mn1 O3 94.16(17) . . ? O1 Mn1 N3 89.99(18) . . ? O3 Mn1 N3 174.93(16) . . ? O1 Mn1 O2 168.30(14) . . ? O3 Mn1 O2 96.74(16) . . ? N3 Mn1 O2 79.35(17) . . ? O1 Mn1 O3 100.04(16) . 2_667 ? O3 Mn1 O3 81.79(16) . 2_667 ? N3 Mn1 O3 94.63(16) . 2_667 ? O2 Mn1 O3 85.75(16) . 2_667 ? O1 Mn1 N1 91.55(17) . . ? O3 Mn1 N1 90.59(16) . . ? N3 Mn1 N1 92.21(17) . . ? O2 Mn1 N1 84.11(17) . . ? O3 Mn1 N1 166.52(13) 2_667 . ? O1 Mn1 Mn1 99.69(13) . 2_667 ? O3 Mn1 Mn1 44.85(11) . 2_667 ? N3 Mn1 Mn1 131.48(13) . 2_667 ? O2 Mn1 Mn1 91.06(13) . 2_667 ? O3 Mn1 Mn1 36.94(9) 2_667 2_667 ? N1 Mn1 Mn1 134.36(12) . 2_667 ? O5 Mn2 O6 96.79(17) . . ? O5 Mn2 O4 166.20(15) . . ? O6 Mn2 O4 94.92(16) . . ? O5 Mn2 N6 90.22(18) . . ? O6 Mn2 N6 169.02(15) . . ? O4 Mn2 N6 79.36(16) . . ? O5 Mn2 O6 96.01(16) . 2_576 ? O6 Mn2 O6 80.61(16) . 2_576 ? O4 Mn2 O6 93.09(15) . 2_576 ? N6 Mn2 O6 90.28(16) . 2_576 ? O5 Mn2 N2 86.71(17) . 2_666 ? O6 Mn2 N2 94.66(16) . 2_666 ? O4 Mn2 N2 85.07(16) . 2_666 ? N6 Mn2 N2 94.17(17) . 2_666 ? O6 Mn2 N2 174.78(13) 2_576 2_666 ? O5 Mn2 Mn2 98.35(14) . 2_576 ? O6 Mn2 Mn2 44.23(12) . 2_576 ? O4 Mn2 Mn2 95.14(13) . 2_576 ? N6 Mn2 Mn2 126.41(14) . 2_576 ? O6 Mn2 Mn2 36.38(9) 2_576 2_576 ? N2 Mn2 Mn2 138.85(12) 2_666 2_576 ? C8 O2 Mn1 111.6(3) . . ? C32 O6 Mn2 122.2(3) . . ? C32 O6 Mn2 122.3(3) . 2_576 ? Mn2 O6 Mn2 99.39(16) . 2_576 ? C21 O4 Mn2 112.2(3) . . ? C30 O3 Mn1 120.3(3) . . ? C30 O3 Mn1 121.9(3) . 2_667 ? Mn1 O3 Mn1 98.21(16) . 2_667 ? C6 O1 Mn1 131.5(3) . . ? C28 O5 Mn2 129.5(3) . . ? C22 N6 N5 117.1(4) . . ? C22 N6 Mn2 127.1(3) . . ? N5 N6 Mn2 115.5(3) . . ? C7 N3 N4 116.5(4) . . ? C7 N3 Mn1 128.2(3) . . ? N4 N3 Mn1 115.3(3) . . ? C20 N1 C16 118.6(4) . . ? C20 N1 Mn1 120.2(3) . . ? C16 N1 Mn1 121.1(3) . . ? C21 N5 N6 107.9(4) . . ? C14 N2 C10 117.9(4) . . ? C14 N2 Mn2 122.7(3) . 2_666 ? C10 N2 Mn2 119.4(3) . 2_666 ? C8 N4 N3 108.6(4) . . ? C1 O7 C29 121.0(6) . . ? O2 C8 N4 125.1(4) . . ? O2 C8 C11 117.4(4) . . ? N4 C8 C11 117.4(4) . . ? C33 O8 C27 138.8(18) . . ? C33A O8A C27 139.4(17) . . ? C20 C19 C18 118.6(4) . . ? C20 C19 C21 122.1(4) . . ? C18 C19 C21 119.2(4) . . ? N2 C10 C11 123.1(4) . . ? N6 C22 C23 124.1(5) . . ? N3 C7 C5 125.1(5) . . ? C10 C11 C12 117.9(5) . . ? C10 C11 C8 120.8(4) . . ? C12 C11 C8 121.2(4) . . ? N5 C21 O4 125.0(4) . . ? N5 C21 C19 119.5(4) . . ? O4 C21 C19 115.5(4) . . ? N1 C20 C19 121.8(4) . . ? O5 C28 C27 119.4(5) . . ? O5 C28 C23 124.0(4) . . ? C27 C28 C23 116.6(5) . . ? O1 C6 C1 118.8(5) . . ? O1 C6 C5 123.8(4) . . ? C1 C6 C5 117.5(4) . . ? C24 C23 C28 119.7(5) . . ? C24 C23 C22 118.0(5) . . ? C28 C23 C22 122.3(5) . . ? N1 C16 C17 123.3(4) . . ? C18 C17 C16 117.0(5) . . ? C4 C5 C6 120.5(5) . . ? C4 C5 C7 118.2(5) . . ? C6 C5 C7 121.4(4) . . ? C2 C1 O7 123.7(5) . . ? C2 C1 C6 121.3(5) . . ? O7 C1 C6 115.0(5) . . ? C26 C27 O8A 118.1(10) . . ? C26 C27 C28 121.5(5) . . ? O8A C27 C28 119.2(10) . . ? C26 C27 O8 119.3(10) . . ? C28 C27 O8 118.6(10) . . ? C17 C18 C19 120.5(5) . . ? C3 C4 C5 120.7(5) . . ? C27 C26 C25 121.4(5) . . ? N2 C14 C13 123.0(5) . . ? C24 C25 C26 118.7(5) . . ? C1 C2 C3 120.1(5) . . ? C4 C3 C2 120.0(5) . . ? C25 C24 C23 121.8(5) . . ? C13 C12 C11 118.8(5) . . ? C12 C13 C14 119.2(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 O1 1.887(4) . ? Mn1 O3 1.890(4) . ? Mn1 N3 1.974(4) . ? Mn1 O2 1.978(4) . ? Mn1 O3 2.218(4) 2_667 ? Mn1 N1 2.313(5) . ? Mn1 Mn1 3.112(3) 2_667 ? Mn2 O5 1.887(4) . ? Mn2 O6 1.895(4) . ? Mn2 O4 1.946(4) . ? Mn2 N6 1.984(4) . ? Mn2 O6 2.229(4) 2_576 ? Mn2 N2 2.383(5) 2_666 ? Mn2 Mn2 3.152(4) 2_576 ? O2 C8 1.288(6) . ? O6 C32 1.411(6) . ? O4 C21 1.309(6) . ? O3 C30 1.432(7) . ? O1 C6 1.319(6) . ? O5 C28 1.323(6) . ? N6 C22 1.308(6) . ? N6 N5 1.413(5) . ? N3 C7 1.296(6) . ? N3 N4 1.413(6) . ? N1 C20 1.344(6) . ? N1 C16 1.346(7) . ? N5 C21 1.309(6) . ? N2 C14 1.338(7) . ? N2 C10 1.339(6) . ? N4 C8 1.314(6) . ? O7 C1 1.379(7) . ? O7 C29 1.417(11) . ? C8 C11 1.480(7) . ? O8 C33 1.13(3) . ? O8 C27 1.43(2) . ? O8A C33A 1.11(3) . ? O8A C27 1.39(2) . ? C19 C20 1.381(7) . ? C19 C18 1.400(7) . ? C19 C21 1.489(6) . ? C10 C11 1.392(7) . ? C22 C23 1.432(7) . ? C7 C5 1.443(7) . ? C11 C12 1.399(7) . ? C28 C27 1.418(7) . ? C28 C23 1.424(7) . ? C6 C1 1.419(7) . ? C6 C5 1.422(7) . ? C23 C24 1.416(7) . ? C16 C17 1.398(8) . ? C17 C18 1.373(7) . ? C5 C4 1.408(7) . ? C1 C2 1.378(8) . ? C27 C26 1.378(8) . ? C4 C3 1.366(8) . ? C26 C25 1.389(9) . ? C14 C13 1.380(8) . ? C25 C24 1.367(8) . ? C2 C3 1.417(9) . ? C12 C13 1.378(8) . ?