#------------------------------------------------------------------------------ #$Date: 2019-05-21 04:38:42 +0300 (Tue, 21 May 2019) $ #$Revision: 215339 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/00/7700034.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_7700034 loop_ _publ_author_name 'Das, Avijit' 'Chakraborty, Maharudra' 'Maity, Souvik' 'Ghosh, Ashutosh' _publ_section_title ; The catalytic activities and magnetic behaviours of a \m3-chlorido and a \m1,1,1-azido bridged rare defective dicubane tetranuclear Mn(II) complexes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C9DT01567A _journal_year 2019 _chemical_formula_moiety 'C22 H30 Cl2 Mn2 N2 O4, 2[CH3OH]' _chemical_formula_sum 'C44 H60 Cl4 Mn4 N4 O8' _chemical_formula_weight 1134.52 _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_date 2019-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _audit_update_record ; 2019-05-08 deposited with the CCDC. 2019-05-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.235(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.134(5) _cell_length_b 10.725(4) _cell_length_c 18.983(7) _cell_measurement_reflns_used 8621 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 22.69 _cell_measurement_theta_min 2.18 _cell_volume 2831.8(18) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 298 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'CCD AREA DETECTOR' _diffrn_measurement_method OMEGA-SCAN _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2268 _diffrn_reflns_av_unetI/netI 0.1080 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 57421 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.243 _diffrn_reflns_theta_min 2.190 _diffrn_source 'FINE FOCUS SEALED TUBE' _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1438 before and 0.1028 after correction. The Ratio of minimum to maximum transmission is 0.7311. The \l/2 correction factor is Not present. ; _exptl_crystal_colour WHITE _exptl_crystal_density_diffrn 1.331 _exptl_crystal_description NEEDLE _exptl_crystal_F_000 1168 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.165 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.134 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 5085 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.1789 _refine_ls_R_factor_gt 0.1012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1739P)^2^+4.3508P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2647 _refine_ls_wR_factor_ref 0.3210 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2491 _reflns_number_total 5085 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt01567a2.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to 'empirical' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 2831.9(18) _cod_database_code 7700034 _shelx_shelxl_version_number 2016/6 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C22) = Uanis(C17) 3.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C8(H8A,H8B), C10(H10A,H10B), C7(H7A,H7B) 3.b Aromatic/amide H refined with riding coordinates: C5(H5), C14(H14), C12(H12), C3(H3) 3.c Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C18(H18A,H18B, H18C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C) ; _shelx_res_file ; TITL pks_adm_0m_a.res in P2(1)/n pks_adm_0m.res created by SHELXL-2016/6 at 20:43:21 on 26-Feb-2019 REM Old TITL PKS_ADM_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.259, Rweak 0.043, Alpha 0.089 REM 0.714 for 296 systematic absences, Orientation as input REM Formula found by SHELXT: C23 N3 O4 Cl3 Mn2 CELL 0.71073 14.1338 10.7254 18.9833 90 100.235 90 ZERR 4 0.0052 0.0039 0.0069 0 0.007 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl Mn N O UNIT 88 120 8 8 8 16 EADP C22 C17 L.S. 10 PLAN 10 TEMP 18.52 list 4 ABIN fmap 2 acta OMIT 6 1 10 OMIT 6 2 0 OMIT -7 1 2 OMIT 0 4 1 OMIT -6 2 2 OMIT -3 6 5 OMIT -1 1 1 OMIT -3 8 5 OMIT -12 2 2 REM REM REM WGHT 0.173900 4.350801 FVAR 0.44420 MN2 4 0.415076 0.349196 0.608571 11.00000 0.06491 0.03363 = 0.06474 0.00171 0.01216 0.00030 MN1 4 0.448651 0.638047 0.528628 11.00000 0.06988 0.02936 = 0.05827 0.00016 0.01065 0.00227 CL1 3 0.375921 0.432597 0.476985 11.00000 0.07265 0.03907 = 0.06855 -0.00027 0.00990 0.00149 CL2 3 0.291512 0.196986 0.587952 11.00000 0.07497 0.05423 = 0.08457 -0.00039 0.01375 -0.01424 O1 6 0.450698 0.538535 0.625891 11.00000 0.07807 0.03979 = 0.05655 -0.00273 0.02170 0.00565 O3 6 0.451384 0.701926 0.422466 11.00000 0.06654 0.03884 = 0.06001 0.00656 0.00390 -0.00010 O4 6 0.508068 0.782135 0.305384 11.00000 0.08325 0.04663 = 0.06440 0.01240 0.02607 0.00391 N1 5 0.501879 0.804155 0.597963 11.00000 0.05939 0.03710 = 0.05650 -0.00458 0.00762 -0.00271 O2 6 0.346935 0.428147 0.710233 11.00000 0.07126 0.05518 = 0.09412 0.00228 0.03798 -0.00285 N2 5 0.309576 0.746935 0.520828 11.00000 0.05691 0.03600 = 0.06706 -0.00478 0.01050 -0.00750 C11 1 0.299197 0.803702 0.389361 11.00000 0.06431 0.03037 = 0.05723 0.00042 -0.00694 -0.00703 C16 1 0.390206 0.773589 0.378245 11.00000 0.06821 0.02609 = 0.06454 -0.00646 0.01657 -0.00802 C9 1 0.337771 0.874468 0.541687 11.00000 0.07654 0.02827 = 0.07442 -0.00453 0.02203 0.00327 AFIX 23 H9A 2 0.282083 0.920296 0.550924 11.00000 -1.20000 H9B 2 0.361490 0.915472 0.502726 11.00000 -1.20000 AFIX 0 C6 1 0.503312 0.692283 0.715901 11.00000 0.04767 0.04713 = 0.05792 -0.00436 0.00094 -0.00076 C8 1 0.415855 0.876145 0.608675 11.00000 0.08647 0.02953 = 0.07970 -0.00973 0.01265 0.00229 AFIX 23 H8A 2 0.434368 0.961701 0.620630 11.00000 -1.20000 H8B 2 0.390374 0.840904 0.648500 11.00000 -1.20000 AFIX 0 C10 1 0.251958 0.743040 0.447024 11.00000 0.06057 0.03422 = 0.08636 0.00113 0.00870 0.00778 AFIX 23 H10A 2 0.190923 0.784085 0.447508 11.00000 -1.20000 H10B 2 0.238398 0.656583 0.433996 11.00000 -1.20000 AFIX 0 C5 1 0.505087 0.736495 0.784814 11.00000 0.06278 0.06636 = 0.07028 -0.01979 0.00312 -0.00006 AFIX 43 H5 2 0.540176 0.808088 0.799601 11.00000 -1.20000 AFIX 0 C15 1 0.416261 0.819531 0.317791 11.00000 0.05784 0.04712 = 0.05812 -0.00429 0.01501 -0.00377 C1 1 0.451735 0.589644 0.692348 11.00000 0.05358 0.03504 = 0.05974 0.00317 0.00311 0.00335 C7 1 0.559791 0.763678 0.666502 11.00000 0.07712 0.04470 = 0.06741 -0.00663 -0.00081 0.00208 AFIX 23 H7A 2 0.588781 0.836636 0.691800 11.00000 -1.20000 H7B 2 0.611499 0.710819 0.656499 11.00000 -1.20000 AFIX 0 C14 1 0.359504 0.900092 0.270332 11.00000 0.07523 0.05150 = 0.06683 0.01553 -0.01331 -0.00218 AFIX 43 H14 2 0.380342 0.930310 0.229782 11.00000 -1.20000 AFIX 0 C2 1 0.399357 0.530844 0.738612 11.00000 0.06015 0.04819 = 0.06856 -0.00264 0.02503 -0.00711 C13 1 0.271789 0.932925 0.285864 11.00000 0.07139 0.04530 = 0.08111 -0.01273 -0.01156 -0.00665 C12 1 0.239865 0.882306 0.343329 11.00000 0.06418 0.05537 = 0.08039 0.00568 -0.00832 -0.00392 AFIX 43 H12 2 0.178422 0.900566 0.351540 11.00000 -1.20000 AFIX 0 C3 1 0.401951 0.573642 0.806050 11.00000 0.07102 0.08441 = 0.07001 -0.00527 0.03016 -0.01048 AFIX 43 H3 2 0.366402 0.532545 0.835735 11.00000 -1.20000 AFIX 0 C19 1 0.248313 0.692179 0.570330 11.00000 0.07480 0.08905 = 0.05798 0.00263 0.01554 -0.00208 AFIX 137 H19A 2 0.239163 0.604759 0.560579 11.00000 -1.50000 H19B 2 0.187017 0.733305 0.562913 11.00000 -1.50000 H19C 2 0.279698 0.703559 0.619061 11.00000 -1.50000 AFIX 0 C4 1 0.456095 0.677016 0.832155 11.00000 0.07071 0.08084 = 0.07095 -0.00682 0.00531 0.00333 C20 1 0.564751 0.877257 0.559980 11.00000 0.09323 0.04702 = 0.06770 -0.00600 0.00968 -0.01129 AFIX 137 H20A 2 0.615247 0.824904 0.548951 11.00000 -1.50000 H20B 2 0.592211 0.945150 0.589713 11.00000 -1.50000 H20C 2 0.527940 0.909556 0.516420 11.00000 -1.50000 AFIX 0 C17 1 0.553348 0.845203 0.254325 11.00000 0.08397 0.07961 = 0.12176 -0.01995 0.04210 -0.00908 AFIX 137 H17A 2 0.561435 0.931614 0.267175 11.00000 -1.50000 H17B 2 0.514060 0.838156 0.207740 11.00000 -1.50000 H17C 2 0.615079 0.808364 0.253634 11.00000 -1.50000 AFIX 0 C18 1 0.206700 1.028430 0.235566 11.00000 0.10904 0.05516 = 0.10288 0.01631 -0.00836 -0.00754 AFIX 137 H18A 2 0.228579 1.111815 0.247455 11.00000 -1.50000 H18B 2 0.141189 1.020168 0.242121 11.00000 -1.50000 H18C 2 0.210772 1.011351 0.186553 11.00000 -1.50000 AFIX 0 C22 1 0.264514 0.395367 0.737796 11.00000 0.08397 0.07961 = 0.12176 -0.01995 0.04210 -0.00908 AFIX 137 H22A 2 0.218018 0.461284 0.728503 11.00000 -1.50000 H22B 2 0.281547 0.382292 0.788496 11.00000 -1.50000 H22C 2 0.237616 0.320109 0.715235 11.00000 -1.50000 AFIX 0 C21 1 0.460435 0.723644 0.907758 11.00000 0.08908 0.13773 = 0.09315 -0.03419 0.03246 -0.02215 AFIX 137 H21A 2 0.524087 0.753383 0.926182 11.00000 -1.50000 H21B 2 0.444798 0.656807 0.937314 11.00000 -1.50000 H21C 2 0.415179 0.790372 0.907818 11.00000 -1.50000 AFIX 0 HKLF 4 REM pks_adm_0m_a.res in P2(1)/n REM R1 = 0.1012 for 2491 Fo > 4sig(Fo) and 0.1789 for all 5085 data REM 289 parameters refined using 0 restraints END WGHT 0.1735 4.5862 REM Highest difference peak 1.165, deepest hole -0.757, 1-sigma level 0.134 Q1 1 0.3482 0.3458 0.5560 11.00000 0.05 1.16 Q2 1 0.3817 0.6390 0.4778 11.00000 0.05 1.12 Q3 1 0.4829 0.3484 0.6592 11.00000 0.05 1.09 Q4 1 0.5202 0.6362 0.5781 11.00000 0.05 0.98 Q5 1 0.4378 0.4322 0.5273 11.00000 0.05 0.94 Q6 1 0.2203 0.1836 0.5341 11.00000 0.05 0.67 Q7 1 0.2997 0.6470 0.4338 11.00000 0.05 0.64 Q8 1 0.4790 0.5642 0.4243 11.00000 0.05 0.59 Q9 1 0.3718 0.1990 0.6438 11.00000 0.05 0.57 Q10 1 0.4989 0.8810 0.5051 11.00000 0.05 0.52 ; _shelx_res_checksum 41307 _shelx_fab_file ; -16 0 -2 -0.0371 -0.0184 -16 0 0 0.5904 0.0049 -16 0 2 3.2231 0.0035 -16 0 4 1.9578 -0.1235 -16 0 6 1.2808 -0.1824 -16 0 8 3.4236 -0.0962 -16 0 10 0.0397 -0.0052 -16 1 -3 -2.0097 0.0023 -16 1 -2 0.8549 0.1168 -16 1 -1 -0.8177 -0.0017 -16 1 0 -0.4725 0.1162 -16 1 1 -1.1797 -0.0304 -16 1 2 -0.8388 0.0171 -16 1 3 -3.0435 -0.0471 -16 1 4 2.1729 -0.0118 -16 1 5 -0.3004 -0.0473 -16 1 6 0.3762 0.0464 -16 1 7 0.9167 -0.0504 -16 1 8 -0.9990 -0.0039 -16 1 9 -3.7145 0.0006 -16 1 10 4.0891 -0.0125 -16 2 -2 0.5570 -0.0159 -16 2 -1 -0.8072 0.1216 -16 2 0 1.5700 -0.0040 -16 2 1 0.4296 0.1071 -16 2 2 0.8370 -0.0096 -16 2 3 -0.8109 -0.0042 -16 2 4 1.2801 0.0121 -16 2 5 1.8647 0.0337 -16 2 6 3.1296 -0.0104 -16 2 7 7.5748 0.0345 -16 2 8 -3.4356 0.0037 -16 2 9 4.9302 0.0083 -16 2 10 -6.2347 -0.0170 -16 3 -1 -1.3740 -0.0667 -16 3 0 -1.9188 0.1112 -16 3 1 -2.7380 -0.0364 -16 3 2 -2.9144 0.0465 -16 3 3 -2.2815 0.0244 -16 3 4 0.5187 -0.0082 -16 3 5 -2.9784 0.1073 -16 3 6 4.2480 -0.0167 -16 3 7 0.5850 0.0720 -16 3 8 1.3462 0.0133 -16 3 9 4.5721 -0.0194 -16 4 2 -0.2281 -0.0198 -16 4 3 -2.8207 -0.0242 -16 4 4 -2.2384 0.1200 -16 4 5 -0.1925 -0.0024 -16 4 6 1.8730 0.0944 -15 0 -5 0.7043 -0.0494 -15 0 -3 1.0644 -0.0189 -15 0 -1 -0.5188 -0.0108 -15 0 1 -2.4837 -0.0215 -15 0 3 -1.4810 -0.0036 -15 0 5 -1.7350 0.0569 -15 0 7 -5.1727 0.0579 -15 0 9 -2.9778 0.0055 -15 0 11 3.7318 -0.0047 -15 0 13 2.8662 0.0172 -15 1 -6 -0.9438 0.0400 -15 1 -5 -3.2326 -0.0239 -15 1 -4 -0.4033 0.0536 -15 1 -3 -1.8943 0.0034 -15 1 -2 0.8208 -0.0197 -15 1 -1 -0.5078 -0.0508 -15 1 0 -0.5645 -0.0086 -15 1 1 0.5643 -0.0145 -15 1 2 1.9112 0.0086 -15 1 3 0.0877 0.0073 -15 1 4 2.7728 0.0024 -15 1 5 0.2455 -0.0284 -15 1 6 -2.6480 0.0246 -15 1 7 2.0152 -0.0215 -15 1 8 -1.6566 0.0218 -15 1 9 -1.3991 0.0092 -15 1 10 4.2169 -0.0342 -15 1 11 -5.8555 -0.0760 -15 1 12 0.3900 0.0144 -15 1 13 -1.5856 -0.0881 -15 2 -6 -1.3891 -0.0529 -15 2 -5 1.5294 0.0353 -15 2 -4 -3.2419 0.0534 -15 2 -3 -1.8308 0.0391 -15 2 -2 0.0807 0.0304 -15 2 -1 -3.3464 -0.0129 -15 2 0 -0.1415 -0.0674 -15 2 1 -2.8721 0.0050 -15 2 2 -0.7313 -0.0183 -15 2 3 -1.2068 -0.0150 -15 2 4 2.1656 -0.0248 -15 2 5 -4.3578 -0.0227 -15 2 6 -1.9376 -0.0676 -15 2 7 -2.5980 0.0085 -15 2 8 -8.2001 0.0022 -15 2 9 8.2987 -0.0116 -15 2 10 -4.0270 -0.0518 -15 2 11 6.5118 0.0173 -15 2 12 1.2233 -0.0708 -15 2 13 -1.9833 -0.0004 -15 3 -5 0.4530 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2.7621 0.0158 8 3 11 -4.7232 0.0167 8 3 12 2.0359 0.0050 8 3 13 2.3501 0.0055 8 3 14 0.6015 0.0353 8 3 15 0.6158 -0.0199 8 3 16 0.4086 0.0244 8 3 17 -0.8797 0.0193 8 4 8 -0.7164 0.0129 8 4 9 4.6495 0.0001 8 4 10 -3.4251 0.0017 8 4 11 -1.3147 -0.0195 8 4 12 -1.8366 0.0096 8 4 13 3.4045 -0.0144 8 4 14 1.9743 0.0215 8 4 15 2.8800 -0.0181 8 4 16 1.1866 0.0367 8 5 8 -4.5881 -0.0025 8 5 9 -3.0737 0.0123 8 5 10 -0.2581 0.0084 8 5 11 -3.7241 0.0018 8 5 12 -2.3114 -0.0049 8 5 13 0.0936 0.0017 8 5 14 -2.0884 0.0393 8 5 15 2.8872 -0.0368 8 6 8 -0.9722 -0.0052 8 6 9 1.8754 0.0037 8 6 10 -5.6381 -0.0208 8 6 11 -1.7392 -0.0033 8 6 12 0.8721 -0.0208 8 6 13 -1.7818 0.0089 8 6 14 1.8391 -0.0010 8 7 8 1.1759 0.0214 8 7 9 -0.0386 0.0233 8 7 10 -0.0474 0.0086 8 7 11 -0.8084 0.0346 8 7 12 -0.9726 0.0515 8 7 13 0.2872 0.0080 8 8 8 -3.6709 0.0716 8 8 9 -1.4710 -0.0042 8 8 10 -4.4404 -0.0866 8 8 11 1.4705 0.0416 8 9 8 0.7835 0.1551 8 9 9 -0.6989 -0.0404 8 9 10 -0.4728 0.2016 9 0 9 1.9391 -0.0054 9 0 11 4.5915 -0.0086 9 0 13 -1.0834 -0.0302 9 0 15 -6.8939 -0.0103 9 1 9 -2.9467 0.0051 9 1 10 -1.8026 -0.0054 9 1 11 2.1171 0.0147 9 1 12 -1.7117 -0.0042 9 1 13 4.2593 0.0041 9 1 14 4.8860 0.0350 9 1 15 2.7276 -0.0686 9 1 16 4.4374 -0.0105 9 2 9 -3.9316 -0.0151 9 2 10 3.3425 0.0005 9 2 11 -1.6224 -0.0252 9 2 12 -8.1603 -0.0013 9 2 13 -1.4465 0.0117 9 2 14 -6.0585 0.0165 9 2 15 -1.0550 0.0291 9 2 16 2.3698 -0.0226 9 3 9 2.8533 0.0161 9 3 10 7.3961 0.0164 9 3 11 -1.2546 0.0028 9 3 12 0.3979 0.0184 9 3 13 -0.2408 0.0102 9 3 14 -4.4498 0.0942 9 3 15 -0.7644 -0.0445 9 3 16 0.3903 0.0937 9 4 9 0.2909 0.0156 9 4 10 0.5787 0.0167 9 4 11 2.6259 0.0044 9 4 12 0.0765 0.0172 9 4 13 -1.1063 0.0198 9 4 14 -4.6924 0.0246 9 4 15 -0.8846 0.0129 9 5 9 -0.2006 0.0155 9 5 10 5.0578 -0.0232 9 5 11 -0.3896 0.0364 9 5 12 1.7390 -0.0124 9 5 13 3.6553 0.0484 9 5 14 -2.7054 0.0053 9 6 9 2.1040 0.0030 9 6 10 0.2133 0.0047 9 6 11 -1.0957 -0.0027 9 6 12 2.8383 0.0101 9 6 13 -3.9308 0.0451 9 7 9 0.8894 -0.0070 9 7 10 1.0017 -0.0047 9 7 11 -0.1812 0.0090 9 7 12 -0.3845 -0.0124 9 8 9 6.0547 -0.0881 9 8 10 -0.5007 0.0342 10 0 10 -4.0867 0.0179 10 0 12 -3.7335 -0.0168 10 0 14 0.5614 0.0087 10 1 10 0.5055 0.0102 10 1 11 4.0700 -0.0012 10 1 12 -0.9304 -0.0149 10 1 13 1.8154 -0.0211 10 1 14 -1.6583 -0.0728 10 1 15 -6.5193 -0.0296 10 2 10 0.9989 0.0129 10 2 11 1.4153 -0.0399 10 2 12 0.4879 0.0212 10 2 13 11.7422 -0.0670 10 2 14 2.1112 -0.0272 10 2 15 5.7881 -0.0524 10 3 10 -2.7256 -0.0146 10 3 11 -3.0877 0.0162 10 3 12 0.8452 -0.0353 10 3 13 2.5912 -0.0879 10 3 14 -0.7495 -0.0317 10 4 10 -1.9174 -0.0066 10 4 11 -1.0652 0.0125 10 4 12 -0.9204 -0.0300 10 4 13 3.2065 0.0217 10 4 14 0.7734 -0.0558 10 5 10 1.1237 0.0123 10 5 11 -2.9438 0.0102 10 5 12 -0.8338 -0.0460 10 5 13 1.4479 0.0135 10 6 10 -1.0466 0.0272 10 6 11 -2.0206 -0.0279 10 6 12 2.4839 0.0253 10 7 10 -0.7468 -0.0031 11 0 11 2.8900 -0.0032 11 0 13 3.4934 0.0578 11 1 11 -0.3758 -0.0606 11 1 12 -6.1988 0.0380 11 1 13 -1.1615 0.0015 11 1 14 -1.0211 0.0176 11 2 11 0.7783 0.0204 11 2 12 -3.8499 0.0874 11 2 13 1.9887 -0.0126 11 2 14 -10.1570 0.1217 11 3 11 1.5822 -0.0184 11 3 12 0.1508 -0.0559 11 3 13 -1.5657 0.0493 11 4 11 3.3352 -0.0135 11 4 12 -1.1395 -0.0540 11 5 11 0.0743 -0.0710 12 0 12 -2.0437 -0.0078 12 1 12 1.3549 0.0776 12 2 12 -2.1655 -0.0515 12 3 12 0.2047 0.0437 0 0 0 0.0 0.0 ; _shelx_fab_checksum 44844 _olex2_submission_special_instructions 'No special instructions were received' 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 Mn2 Mn 0.41508(12) 0.34920(13) 0.60857(9) 0.0543(5) Uani 1 1 d . Mn1 Mn 0.44865(12) 0.63805(13) 0.52863(8) 0.0526(5) Uani 1 1 d . Cl1 Cl 0.3759(2) 0.4326(2) 0.47698(15) 0.0604(8) Uani 1 1 d . Cl2 Cl 0.2915(2) 0.1970(3) 0.58795(17) 0.0713(9) Uani 1 1 d . O1 O 0.4507(5) 0.5385(6) 0.6259(4) 0.0569(18) Uani 1 1 d . O3 O 0.4514(5) 0.7019(6) 0.4225(4) 0.0560(18) Uani 1 1 d . O4 O 0.5081(6) 0.7821(6) 0.3054(4) 0.063(2) Uani 1 1 d . N1 N 0.5019(6) 0.8042(7) 0.5980(4) 0.051(2) Uani 1 1 d . O2 O 0.3469(5) 0.4281(7) 0.7102(4) 0.071(2) Uani 1 1 d . N2 N 0.3096(6) 0.7469(7) 0.5208(5) 0.053(2) Uani 1 1 d . C11 C 0.2992(8) 0.8037(8) 0.3894(5) 0.053(3) Uani 1 1 d . C16 C 0.3902(8) 0.7736(8) 0.3782(6) 0.052(3) Uani 1 1 d . C9 C 0.3378(8) 0.8745(8) 0.5417(6) 0.059(3) Uani 1 1 d . H9A H 0.282083 0.920296 0.550924 0.070 Uiso 1 1 calc R H9B H 0.361490 0.915472 0.502726 0.070 Uiso 1 1 calc R C6 C 0.5033(7) 0.6923(9) 0.7159(6) 0.052(3) Uani 1 1 d . C8 C 0.4159(8) 0.8761(9) 0.6087(6) 0.065(3) Uani 1 1 d . H8A H 0.434368 0.961701 0.620630 0.079 Uiso 1 1 calc R H8B H 0.390374 0.840904 0.648500 0.079 Uiso 1 1 calc R C10 C 0.2520(8) 0.7430(9) 0.4470(6) 0.061(3) Uani 1 1 d . H10A H 0.190923 0.784085 0.447508 0.073 Uiso 1 1 calc R H10B H 0.238398 0.656583 0.433996 0.073 Uiso 1 1 calc R C5 C 0.5051(8) 0.7365(11) 0.7848(6) 0.068(3) Uani 1 1 d . H5 H 0.540176 0.808088 0.799601 0.081 Uiso 1 1 calc R C15 C 0.4163(8) 0.8195(9) 0.3178(6) 0.054(3) Uani 1 1 d . C1 C 0.4517(7) 0.5896(9) 0.6923(6) 0.050(3) Uani 1 1 d . C7 C 0.5598(8) 0.7637(10) 0.6665(6) 0.065(3) Uani 1 1 d . H7A H 0.588781 0.836636 0.691800 0.078 Uiso 1 1 calc R H7B H 0.611499 0.710819 0.656499 0.078 Uiso 1 1 calc R C14 C 0.3595(9) 0.9001(10) 0.2703(6) 0.068(3) Uani 1 1 d . H14 H 0.380342 0.930310 0.229782 0.081 Uiso 1 1 calc R C2 C 0.3994(8) 0.5308(9) 0.7386(6) 0.057(3) Uani 1 1 d . C13 C 0.2718(9) 0.9329(10) 0.2859(7) 0.069(3) Uani 1 1 d . C12 C 0.2399(9) 0.8823(10) 0.3433(7) 0.069(3) Uani 1 1 d . H12 H 0.178422 0.900566 0.351540 0.083 Uiso 1 1 calc R C3 C 0.4020(9) 0.5736(12) 0.8061(6) 0.073(3) Uani 1 1 d . H3 H 0.366402 0.532545 0.835735 0.088 Uiso 1 1 calc R C19 C 0.2483(9) 0.6922(12) 0.5703(6) 0.073(3) Uani 1 1 d . H19A H 0.239163 0.604759 0.560579 0.110 Uiso 1 1 calc GR H19B H 0.187017 0.733305 0.562913 0.110 Uiso 1 1 calc GR H19C H 0.279698 0.703559 0.619061 0.110 Uiso 1 1 calc GR C4 C 0.4561(9) 0.6770(12) 0.8322(7) 0.075(3) Uani 1 1 d . C20 C 0.5648(9) 0.8773(10) 0.5600(6) 0.070(3) Uani 1 1 d . H20A H 0.615247 0.824904 0.548951 0.105 Uiso 1 1 calc GR H20B H 0.592211 0.945150 0.589713 0.105 Uiso 1 1 calc GR H20C H 0.527940 0.909556 0.516420 0.105 Uiso 1 1 calc GR C17 C 0.5533(10) 0.8452(12) 0.2543(8) 0.092(3) Uani 1 1 d . H17A H 0.561435 0.931614 0.267175 0.138 Uiso 1 1 calc GR H17B H 0.514060 0.838156 0.207740 0.138 Uiso 1 1 calc GR H17C H 0.615079 0.808364 0.253634 0.138 Uiso 1 1 calc GR C18 C 0.2067(10) 1.0284(11) 0.2356(7) 0.092(4) Uani 1 1 d . H18A H 0.228579 1.111815 0.247455 0.139 Uiso 1 1 calc GR H18B H 0.141189 1.020168 0.242121 0.139 Uiso 1 1 calc GR H18C H 0.210772 1.011351 0.186553 0.139 Uiso 1 1 calc GR C22 C 0.2645(9) 0.3954(13) 0.7378(8) 0.092(3) Uani 1 1 d . H22A H 0.218018 0.461284 0.728503 0.138 Uiso 1 1 calc GR H22B H 0.281547 0.382292 0.788496 0.138 Uiso 1 1 calc GR H22C H 0.237616 0.320109 0.715235 0.138 Uiso 1 1 calc GR C21 C 0.4604(10) 0.7236(15) 0.9078(7) 0.105(5) Uani 1 1 d . H21A H 0.524087 0.753383 0.926182 0.157 Uiso 1 1 calc GR H21B H 0.444798 0.656807 0.937314 0.157 Uiso 1 1 calc GR H21C H 0.415179 0.790372 0.907818 0.157 Uiso 1 1 calc GR 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 Mn2 0.0649(11) 0.0336(8) 0.0647(11) 0.0017(7) 0.0122(8) 0.0003(7) Mn1 0.0699(11) 0.0294(8) 0.0583(10) 0.0002(7) 0.0106(8) 0.0023(7) Cl1 0.0726(18) 0.0391(13) 0.0685(18) -0.0003(12) 0.0099(14) 0.0015(12) Cl2 0.075(2) 0.0542(16) 0.085(2) -0.0004(14) 0.0138(16) -0.0142(14) O1 0.078(5) 0.040(4) 0.057(4) -0.003(3) 0.022(4) 0.006(3) O3 0.067(5) 0.039(4) 0.060(4) 0.007(3) 0.004(4) 0.000(3) O4 0.083(6) 0.047(4) 0.064(5) 0.012(3) 0.026(4) 0.004(4) N1 0.059(5) 0.037(4) 0.057(5) -0.005(4) 0.008(4) -0.003(4) O2 0.071(5) 0.055(5) 0.094(6) 0.002(4) 0.038(5) -0.003(4) N2 0.057(5) 0.036(4) 0.067(6) -0.005(4) 0.010(5) -0.007(4) C11 0.064(7) 0.030(5) 0.057(7) 0.000(4) -0.007(6) -0.007(5) C16 0.068(8) 0.026(5) 0.065(7) -0.006(5) 0.017(6) -0.008(5) C9 0.077(8) 0.028(5) 0.074(8) -0.005(5) 0.022(6) 0.003(5) C6 0.048(6) 0.047(6) 0.058(7) -0.004(5) 0.001(5) -0.001(5) C8 0.086(8) 0.030(5) 0.080(8) -0.010(5) 0.013(7) 0.002(5) C10 0.061(7) 0.034(5) 0.086(8) 0.001(5) 0.009(6) 0.008(5) C5 0.063(7) 0.066(8) 0.070(8) -0.020(6) 0.003(6) 0.000(6) C15 0.058(7) 0.047(6) 0.058(7) -0.004(5) 0.015(6) -0.004(5) C1 0.054(6) 0.035(5) 0.060(7) 0.003(5) 0.003(5) 0.003(5) C7 0.077(8) 0.045(6) 0.067(7) -0.007(5) -0.001(6) 0.002(6) C14 0.075(8) 0.051(6) 0.067(8) 0.016(6) -0.013(7) -0.002(6) C2 0.060(7) 0.048(6) 0.069(7) -0.003(5) 0.025(6) -0.007(5) C13 0.071(8) 0.045(6) 0.081(9) -0.013(6) -0.012(7) -0.007(6) C12 0.064(7) 0.055(7) 0.080(9) 0.006(6) -0.008(7) -0.004(6) C3 0.071(8) 0.084(9) 0.070(8) -0.005(7) 0.030(7) -0.010(7) C19 0.075(8) 0.089(9) 0.058(7) 0.003(6) 0.016(6) -0.002(7) C4 0.071(8) 0.081(9) 0.071(9) -0.007(7) 0.005(7) 0.003(7) C20 0.093(9) 0.047(6) 0.068(8) -0.006(5) 0.010(7) -0.011(6) C17 0.084(7) 0.080(7) 0.122(8) -0.020(6) 0.042(6) -0.009(5) C18 0.109(11) 0.055(7) 0.103(10) 0.016(7) -0.008(9) -0.008(7) C22 0.084(7) 0.080(7) 0.122(8) -0.020(6) 0.042(6) -0.009(5) C21 0.089(11) 0.138(14) 0.093(11) -0.034(10) 0.032(9) -0.022(10) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl2 Mn2 Cl1 93.04(11) . . Cl2 Mn2 O2 89.3(2) . . O1 Mn2 Cl1 79.8(2) . . O1 Mn2 Cl2 147.0(2) . . O1 Mn2 O3 95.3(3) . 3_666 O1 Mn2 O4 114.5(3) . 3_666 O1 Mn2 O2 70.2(3) . . O3 Mn2 Cl1 82.67(19) 3_666 . O3 Mn2 Cl2 115.9(2) 3_666 . O3 Mn2 O4 73.1(3) 3_666 3_666 O3 Mn2 O2 142.3(3) 3_666 . O4 Mn2 Cl1 152.5(2) 3_666 . O4 Mn2 Cl2 86.3(2) 3_666 . O4 Mn2 O2 81.6(3) 3_666 . O2 Mn2 Cl1 125.9(2) . . Cl1 Mn1 Cl1 93.11(10) . 3_666 O1 Mn1 Cl1 91.3(2) . 3_666 O1 Mn1 Cl1 80.95(19) . . O1 Mn1 O3 168.5(3) . . O1 Mn1 N1 86.5(3) . . O1 Mn1 N2 101.1(3) . . O3 Mn1 Cl1 89.32(19) . . O3 Mn1 Cl1 83.0(2) . 3_666 O3 Mn1 N1 103.7(3) . . O3 Mn1 N2 86.2(3) . . N1 Mn1 Cl1 166.6(2) . . N1 Mn1 Cl1 91.8(2) . 3_666 N1 Mn1 N2 80.1(3) . . N2 Mn1 Cl1 97.7(2) . . N2 Mn1 Cl1 164.6(2) . 3_666 Mn1 Cl1 Mn2 85.76(9) . . Mn1 Cl1 Mn2 84.18(9) 3_666 . Mn1 Cl1 Mn1 86.89(10) . 3_666 Mn2 O1 Mn1 112.5(3) . . C1 O1 Mn2 119.5(6) . . C1 O1 Mn1 126.4(6) . . Mn1 O3 Mn2 110.0(3) . 3_666 C16 O3 Mn2 118.5(6) . 3_666 C16 O3 Mn1 131.2(7) . . C15 O4 Mn2 112.9(6) . 3_666 C15 O4 C17 120.9(9) . . C17 O4 Mn2 124.5(8) . 3_666 C8 N1 Mn1 107.1(6) . . C7 N1 Mn1 110.9(6) . . C7 N1 C8 111.8(8) . . C20 N1 Mn1 107.6(6) . . C20 N1 C8 111.8(8) . . C20 N1 C7 107.5(8) . . C2 O2 Mn2 108.9(6) . . C2 O2 C22 118.5(9) . . C22 O2 Mn2 132.4(7) . . C9 N2 Mn1 105.8(6) . . C9 N2 C10 111.0(8) . . C9 N2 C19 110.8(9) . . C10 N2 Mn1 111.7(6) . . C10 N2 C19 107.3(8) . . C19 N2 Mn1 110.3(7) . . C16 C11 C10 123.3(9) . . C16 C11 C12 121.5(11) . . C12 C11 C10 114.8(11) . . O3 C16 C11 123.8(10) . . O3 C16 C15 119.8(10) . . C15 C16 C11 116.4(10) . . N2 C9 C8 111.0(8) . . C5 C6 C7 118.7(10) . . C1 C6 C5 120.6(11) . . C1 C6 C7 120.7(10) . . N1 C8 C9 111.6(9) . . N2 C10 C11 115.3(9) . . C4 C5 C6 121.8(11) . . C16 C15 O4 115.6(9) . . C16 C15 C14 124.0(11) . . C14 C15 O4 120.4(10) . . O1 C1 C2 118.5(9) . . C6 C1 O1 123.1(10) . . C6 C1 C2 118.4(10) . . N1 C7 C6 114.7(9) . . C13 C14 C15 117.3(12) . . O2 C2 C1 115.0(9) . . C3 C2 O2 124.1(10) . . C3 C2 C1 120.9(10) . . C14 C13 C18 119.2(12) . . C12 C13 C14 120.7(12) . . C12 C13 C18 120.1(12) . . C13 C12 C11 119.8(12) . . C2 C3 C4 121.9(12) . . C5 C4 C3 116.4(12) . . C5 C4 C21 121.6(12) . . C3 C4 C21 122.0(13) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn2 Cl1 2.618(3) . Mn2 Cl2 2.372(3) . Mn2 O1 2.104(7) . Mn2 O3 2.146(7) 3_666 Mn2 O4 2.281(7) 3_666 Mn2 O2 2.455(8) . Mn1 Cl1 2.552(3) . Mn1 Cl1 2.613(3) 3_666 Mn1 O1 2.128(7) . Mn1 O3 2.135(7) . Mn1 N1 2.263(8) . Mn1 N2 2.269(8) . O1 C1 1.373(12) . O3 C16 1.336(12) . O4 C15 1.417(12) . O4 C17 1.424(14) . N1 C8 1.484(13) . N1 C7 1.474(13) . N1 C20 1.467(13) . O2 C2 1.382(12) . O2 C22 1.404(14) . N2 C9 1.460(11) . N2 C10 1.491(13) . N2 C19 1.506(14) . C11 C16 1.378(14) . C11 C10 1.525(15) . C11 C12 1.385(14) . C16 C15 1.359(14) . C9 C8 1.529(14) . C6 C5 1.388(15) . C6 C1 1.352(13) . C6 C7 1.539(15) . C5 C4 1.384(16) . C15 C14 1.395(14) . C1 C2 1.396(14) . C14 C13 1.370(17) . C2 C3 1.354(15) . C13 C12 1.365(17) . C13 C18 1.580(16) . C3 C4 1.388(17) . C4 C21 1.511(17) . loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.807 0.500 326.1 75.2 '2 CH3OH' 2 0.500 -0.198 0.000 326.1 75.2 '2 CH3OH'