#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:10:30 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257320 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557767.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_1557767 loop_ _publ_author_name 'Cliffe, Matthew J.' 'Keyzer, Evan N.' 'Bond, Andrew D.' 'Astle, Maxwell A.' 'Grey, Clare P.' _publ_section_title ; The structures of ordered defects in thiocyanate analogues of Prussian Blue ; _journal_issue 17 _journal_name_full 'Chemical Science' _journal_page_first 4430 _journal_page_last 4438 _journal_paper_doi 10.1039/D0SC01246G _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C7 H14 Bi Mn2 N7 O7 S7' _chemical_formula_sum 'C7 H14 Bi Mn2 N7 O7 S7' _chemical_formula_weight 851.53 _chemical_name_systematic 'manganese hexathiocyanatobismuthate thiocyanate heptahydrate' _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' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2020-02-27 deposited with the CCDC. 2020-04-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.2358(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.3065(2) _cell_length_b 25.8428(6) _cell_length_c 12.2664(3) _cell_measurement_reflns_used 9893 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 66.59 _cell_measurement_theta_min 3.42 _cell_volume 2633.12(11) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction SAINT _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material SHELXL _computing_structure_refinement 'SHELXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8-QUEST PHOTON-100' _diffrn_measurement_method '\w and \f-scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.0797 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_Laue_measured_fraction_full 0.998 _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 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 33300 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 66.654 _diffrn_reflns_theta_max 66.654 _diffrn_reflns_theta_min 3.420 _diffrn_source 'Incoatec I\mS Cu microsource' _exptl_absorpt_coefficient_mu 26.169 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.3997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.148 _exptl_crystal_description plate _exptl_crystal_F_000 1624 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water' _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.010 _refine_diff_density_max 2.364 _refine_diff_density_min -1.633 _refine_diff_density_rms 0.175 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 4657 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0376 _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^)+(0.0442P)^2^+9.0260P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.0927 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3697 _reflns_number_total 4657 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01246g3.cif _cod_data_source_block 1a _cod_depositor_comments ;Adding full bibliography for 1557765--1557770.cif. Adding full bibliography for 1557765--1557770.cif. ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557767 _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 0.121 _shelx_estimated_absorpt_t_max 0.780 _shelx_res_file ; TITL MC_B2_0001 in P2(1)/n 1a.res created by SHELXL-2018/1 at 11:13:18 on 30-Oct-2019 CELL 1.5418 8.3065 25.8428 12.2664 90.00 90.2358 90.00 ZERR 4.00 0.0002 0.0006 0.0003 0.00 0.0013 0.00 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Bi Mn N O S UNIT 28 56 4 8 28 28 28 SIZE 0.14 0.06 0.01 TEMP -93 L.S. 20 EXYZ S7 S7A EADP S7 S7A ACTA BOND $H CONF LIST 4 FMAP 2 PLAN -10 WGHT 0.044200 9.026000 FVAR 0.20417 0.52839 BI1 3 0.462675 0.333981 -0.064416 11.00000 0.02206 0.01860 = 0.01856 -0.00099 0.00219 0.00054 MN1 4 0.000000 0.500000 0.000000 10.50000 0.02389 0.02094 = 0.02280 -0.00311 0.00139 0.00304 MN2 4 0.458028 0.338360 0.429852 11.00000 0.02351 0.02120 = 0.01899 -0.00093 0.00282 -0.00061 MN3 4 1.000000 0.500000 0.500000 10.50000 0.03228 0.02236 = 0.02371 -0.00161 0.00040 -0.00439 S1 7 0.257768 0.648350 0.190412 11.00000 0.04444 0.03904 = 0.03449 -0.01388 0.01558 -0.01672 S2 7 0.529020 0.425506 0.049166 11.00000 0.02660 0.02837 = 0.05122 -0.01235 0.00051 0.00136 S3 7 -0.055057 0.256828 0.307847 11.00000 0.03439 0.03428 = 0.04641 0.01418 -0.01621 -0.00781 S4 7 0.702916 0.177637 0.579959 11.00000 0.04437 0.03686 = 0.03137 0.01221 0.01521 0.01636 S5 7 0.670595 0.279256 0.075226 11.00000 0.04647 0.04882 = 0.02599 -0.00956 -0.00567 0.02501 S6 7 0.216955 0.371490 0.794391 11.00000 0.04310 0.06457 = 0.02350 0.00070 0.00301 0.02737 N1 5 0.104397 0.572430 0.062147 11.00000 0.02920 0.02731 = 0.04108 -0.00748 0.00632 0.00185 N2 5 0.209640 0.459112 0.063785 11.00000 0.03540 0.02652 = 0.04579 -0.00313 -0.00822 0.00623 N3 5 0.225662 0.304017 0.382514 11.00000 0.04487 0.03403 = 0.02506 0.00791 -0.00162 -0.00953 N4 5 0.570402 0.268323 0.491782 11.00000 0.02970 0.02861 = 0.04273 0.00260 0.00957 0.00797 N5 5 0.560365 0.322291 0.269684 11.00000 0.05337 0.05966 = 0.02023 0.00626 0.00939 0.02397 N6 5 0.364959 0.357873 0.591923 11.00000 0.05843 0.03490 = 0.01923 0.00049 -0.00156 0.00998 C1 1 0.168687 0.603654 0.114703 11.00000 0.03060 0.02517 = 0.02941 0.00078 0.01331 0.00730 C2 1 0.340190 0.445385 0.057681 11.00000 0.03727 0.01827 = 0.02623 0.00234 0.00441 0.00658 C3 1 0.110862 0.284302 0.351754 11.00000 0.02814 0.02413 = 0.02207 0.00363 -0.00454 -0.00487 C4 1 0.624574 0.231110 0.526971 11.00000 0.02162 0.03380 = 0.02401 -0.00028 0.00647 0.00222 C5 1 0.601597 0.305345 0.189673 11.00000 0.03410 0.03272 = 0.02554 0.00590 -0.00011 0.00740 C6 1 0.308034 0.363412 0.675836 11.00000 0.03860 0.03007 = 0.01855 0.00289 -0.00456 0.00748 O1 6 -0.121712 0.491075 0.163176 11.00000 0.03344 0.02982 = 0.03004 -0.00050 0.00373 0.00976 AFIX 3 H11 2 -0.130512 0.459725 0.183096 11.00000 -1.50000 H12 2 -0.206412 0.508886 0.173077 11.00000 -1.50000 AFIX 0 O4 6 1.080186 0.528319 0.340146 11.00000 0.05187 0.05945 = 0.03197 0.00631 -0.00377 -0.01594 AFIX 3 H41 2 1.020586 0.517470 0.288506 11.00000 -1.50000 H42 2 1.180266 0.525999 0.326826 11.00000 -1.50000 AFIX 0 O5 6 0.942798 0.578965 0.550485 11.00000 0.05704 0.02749 = 0.05858 0.00120 0.01343 0.00541 AFIX 3 H51 2 0.964569 0.605415 0.512136 11.00000 -1.50000 H52 2 0.987438 0.587325 0.610436 11.00000 -1.50000 AFIX 0 PART 1 S7 7 0.489285 0.518810 0.285667 21.00000 0.07849 0.03304 = 0.04912 0.00883 -0.01861 -0.00096 N7 5 0.750937 0.501532 0.434379 21.00000 0.05356 C7 1 0.646455 0.508397 0.372164 21.00000 0.02816 O2 6 0.367569 0.410411 0.360401 21.00000 0.03238 AFIX 3 H21 2 0.273569 0.413541 0.386721 21.00000 -1.50000 H22 2 0.402039 0.439951 0.341050 21.00000 -1.50000 AFIX 0 O3 6 0.669951 0.383840 0.497978 21.00000 0.05403 AFIX 3 H31 2 0.755010 0.369920 0.523187 21.00000 -1.50000 H32 2 0.691022 0.415060 0.481528 21.00000 -1.50000 AFIX 0 PART 2 S7A 7 0.489285 0.518810 0.285667 -21.00000 0.07849 0.03304 = 0.04912 0.00883 -0.01861 -0.00096 N7A 5 0.390569 0.417939 0.379568 -21.00000 0.03492 C7A 1 0.423972 0.458954 0.334328 -21.00000 0.03513 O2A 6 1.235210 0.516531 0.555935 -21.00000 0.04040 AFIX 3 H21A 2 1.254408 0.549031 0.555855 -21.00000 -1.50000 H22A 2 1.309608 0.506781 0.598775 -21.00000 -1.50000 AFIX 0 O3A 6 0.700153 0.375254 0.445047 -21.00000 0.02535 AFIX 3 H31A 2 0.775363 0.364025 0.485857 -21.00000 -1.50000 H32A 2 0.756903 0.380274 0.388517 -21.00000 -1.50000 AFIX 0 PART 0 O1W 6 -0.097350 0.392626 0.242463 11.00000 0.07106 0.04114 = 0.05788 0.00605 0.00427 -0.00867 AFIX 3 H1W 2 -0.027710 0.376476 0.204963 11.00000 -1.50000 H2W 2 -0.183040 0.374966 0.249243 11.00000 -1.50000 AFIX 0 O2W 6 0.951137 0.338782 0.577435 11.00000 0.04335 0.04857 = 0.02995 -0.00195 0.00426 0.01113 AFIX 3 H3W 2 1.003835 0.310592 0.576683 11.00000 -1.50000 H4W 2 0.898266 0.342042 0.636213 11.00000 -1.50000 AFIX 0 HKLF 4 REM MC_B2_0001 in P2(1)/n REM R1 = 0.0376 for 3697 Fo > 4sig(Fo) and 0.0547 for all 4657 data REM 280 parameters refined using 0 restraints END WGHT 0.0443 8.9954 REM Highest difference peak 2.364, deepest hole -1.633, 1-sigma level 0.175 Q1 1 0.4634 0.2944 -0.0634 11.00000 0.05 2.36 Q2 1 0.4628 0.3741 -0.0608 11.00000 0.05 2.34 Q3 1 0.3645 0.4011 -0.0443 11.00000 0.05 0.92 Q4 1 0.3685 0.2703 -0.0621 11.00000 0.05 0.85 Q5 1 0.5462 0.2614 -0.0753 11.00000 0.05 0.80 Q6 1 0.4654 0.2915 -0.1929 11.00000 0.05 0.78 Q7 1 0.5457 0.2697 -0.0438 11.00000 0.05 0.77 Q8 1 0.5322 0.3945 -0.0141 11.00000 0.05 0.75 Q9 1 0.9611 0.5064 0.4273 11.00000 0.05 0.73 Q10 1 0.5743 0.3324 -0.0760 11.00000 0.05 0.72 ; _shelx_res_checksum 30379 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.46267(3) 0.33398(2) -0.06442(2) 0.01974(10) Uani 1 1 d . . . . . Mn1 Mn 0.000000 0.500000 0.000000 0.0225(3) Uani 1 2 d S . P . . Mn2 Mn 0.45803(13) 0.33836(4) 0.42985(9) 0.0212(2) Uani 1 1 d . . . . . Mn3 Mn 1.000000 0.500000 0.500000 0.0261(4) Uani 1 2 d S . P . . S1 S 0.2578(3) 0.64835(8) 0.19041(17) 0.0393(5) Uani 1 1 d . . . . . S2 S 0.5290(2) 0.42551(8) 0.04917(18) 0.0354(5) Uani 1 1 d . . . . . S3 S -0.0551(3) 0.25683(8) 0.30785(18) 0.0384(5) Uani 1 1 d . . . . . S4 S 0.7029(3) 0.17764(8) 0.57996(17) 0.0375(5) Uani 1 1 d . . . . . S5 S 0.6706(3) 0.27926(9) 0.07523(16) 0.0404(5) Uani 1 1 d . . . . . S6 S 0.2170(3) 0.37149(10) 0.79439(16) 0.0437(6) Uani 1 1 d . . . . . N1 N 0.1044(8) 0.5724(3) 0.0621(6) 0.0325(15) Uani 1 1 d . . . . . N2 N 0.2096(8) 0.4591(3) 0.0638(6) 0.0359(16) Uani 1 1 d . . . . . N3 N 0.2257(9) 0.3040(3) 0.3825(5) 0.0347(16) Uani 1 1 d . . . . . N4 N 0.5704(8) 0.2683(3) 0.4918(6) 0.0337(16) Uani 1 1 d . . . . . N5 N 0.5604(9) 0.3223(3) 0.2697(6) 0.044(2) Uani 1 1 d . . . . . N6 N 0.3650(9) 0.3579(3) 0.5919(5) 0.0375(17) Uani 1 1 d . . . . . C1 C 0.1687(9) 0.6037(3) 0.1147(6) 0.0284(17) Uani 1 1 d . . . . . C2 C 0.3402(10) 0.4454(3) 0.0577(6) 0.0272(17) Uani 1 1 d . . . . . C3 C 0.1109(9) 0.2843(3) 0.3518(6) 0.0248(16) Uani 1 1 d . . . . . C4 C 0.6246(9) 0.2311(3) 0.5270(6) 0.0265(17) Uani 1 1 d . . . . . C5 C 0.6016(10) 0.3053(3) 0.1897(6) 0.0308(18) Uani 1 1 d . . . . . C6 C 0.3080(10) 0.3634(3) 0.6758(6) 0.0291(18) Uani 1 1 d . . . . . O1 O -0.1217(6) 0.4911(2) 0.1632(4) 0.0311(12) Uani 1 1 d . . . . . H11 H -0.130512 0.459725 0.183096 0.047 Uiso 1 1 d R U . . . H12 H -0.206412 0.508886 0.173077 0.047 Uiso 1 1 d R U . . . O4 O 1.0802(8) 0.5283(2) 0.3401(5) 0.0478(16) Uani 1 1 d . . . . . H41 H 1.020586 0.517470 0.288506 0.072 Uiso 1 1 d R U . . . H42 H 1.180266 0.525999 0.326826 0.072 Uiso 1 1 d R U . . . O5 O 0.9428(7) 0.5790(2) 0.5505(5) 0.0477(16) Uani 1 1 d . . . . . H51 H 0.964569 0.605415 0.512136 0.071 Uiso 1 1 d R U . . . H52 H 0.987438 0.587325 0.610436 0.071 Uiso 1 1 d R U . . . S7 S 0.4893(3) 0.51881(9) 0.2857(2) 0.0536(6) Uani 0.528(16) 1 d . . P A 1 N7 N 0.751(2) 0.5015(9) 0.4344(16) 0.054(5) Uiso 0.528(16) 1 d . . P A 1 C7 C 0.6465(17) 0.5084(6) 0.3722(12) 0.028(4) Uiso 0.528(16) 1 d . . P A 1 O2 O 0.3676(18) 0.4104(6) 0.3604(12) 0.032(4) Uiso 0.528(16) 1 d . . P A 1 H21 H 0.273569 0.413541 0.386721 0.049 Uiso 0.528(16) 1 d R U P A 1 H22 H 0.402039 0.439951 0.341050 0.049 Uiso 0.528(16) 1 d R U P A 1 O3 O 0.6700(16) 0.3838(5) 0.4980(13) 0.054(4) Uiso 0.528(16) 1 d . . P A 1 H31 H 0.755010 0.369920 0.523187 0.081 Uiso 0.528(16) 1 d R U P A 1 H32 H 0.691022 0.415060 0.481528 0.081 Uiso 0.528(16) 1 d R U P A 1 S7A S 0.4893(3) 0.51881(9) 0.2857(2) 0.0536(6) Uani 0.472(16) 1 d . . P A 2 N7A N 0.391(3) 0.4179(8) 0.3796(17) 0.035(6) Uiso 0.472(16) 1 d . . P A 2 C7A C 0.424(2) 0.4590(7) 0.3343(14) 0.035(5) Uiso 0.472(16) 1 d . . P A 2 O2A O 1.2352(18) 0.5165(7) 0.5559(12) 0.040(4) Uiso 0.472(16) 1 d . . P A 2 H21A H 1.254408 0.549031 0.555855 0.061 Uiso 0.472(16) 1 d R U P A 2 H22A H 1.309608 0.506781 0.598775 0.061 Uiso 0.472(16) 1 d R U P A 2 O3A O 0.7002(13) 0.3753(4) 0.4450(11) 0.025(3) Uiso 0.472(16) 1 d . . P A 2 H31A H 0.775363 0.364025 0.485857 0.038 Uiso 0.472(16) 1 d R U P A 2 H32A H 0.756903 0.380274 0.388517 0.038 Uiso 0.472(16) 1 d R U P A 2 O1W O -0.0973(9) 0.3926(2) 0.2425(5) 0.0567(18) Uani 1 1 d . . . . . H1W H -0.027710 0.376476 0.204963 0.085 Uiso 1 1 d R U . . . H2W H -0.183040 0.374966 0.249243 0.085 Uiso 1 1 d R U . . . O2W O 0.9511(7) 0.3388(2) 0.5774(4) 0.0406(14) Uani 1 1 d . . . . . H3W H 1.003835 0.310592 0.576683 0.061 Uiso 1 1 d R U . . . H4W H 0.898266 0.342042 0.636213 0.061 Uiso 1 1 d R U . . . 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 Bi1 0.02206(15) 0.01860(14) 0.01856(15) -0.00099(11) 0.00219(10) 0.00054(12) Mn1 0.0239(8) 0.0209(8) 0.0228(9) -0.0031(7) 0.0014(7) 0.0030(7) Mn2 0.0235(6) 0.0212(6) 0.0190(6) -0.0009(4) 0.0028(4) -0.0006(5) Mn3 0.0323(9) 0.0224(8) 0.0237(9) -0.0016(7) 0.0004(7) -0.0044(8) S1 0.0444(12) 0.0390(11) 0.0345(11) -0.0139(9) 0.0156(10) -0.0167(10) S2 0.0266(10) 0.0284(10) 0.0512(13) -0.0123(9) 0.0005(9) 0.0014(8) S3 0.0344(11) 0.0343(11) 0.0464(13) 0.0142(9) -0.0162(10) -0.0078(9) S4 0.0444(12) 0.0369(12) 0.0314(11) 0.0122(8) 0.0152(9) 0.0164(9) S5 0.0465(13) 0.0488(13) 0.0260(11) -0.0096(9) -0.0057(9) 0.0250(11) S6 0.0431(13) 0.0646(15) 0.0235(11) 0.0007(10) 0.0030(9) 0.0274(11) N1 0.029(4) 0.027(4) 0.041(4) -0.007(3) 0.006(3) 0.002(3) N2 0.035(4) 0.027(4) 0.046(4) -0.003(3) -0.008(3) 0.006(3) N3 0.045(4) 0.034(4) 0.025(4) 0.008(3) -0.002(3) -0.010(3) N4 0.030(4) 0.029(4) 0.043(4) 0.003(3) 0.010(3) 0.008(3) N5 0.053(5) 0.060(5) 0.020(4) 0.006(3) 0.009(3) 0.024(4) N6 0.058(5) 0.035(4) 0.019(4) 0.000(3) -0.002(3) 0.010(4) C1 0.031(4) 0.025(4) 0.029(4) 0.001(3) 0.013(3) 0.007(3) C2 0.037(5) 0.018(4) 0.026(4) 0.002(3) 0.004(3) 0.007(3) C3 0.028(4) 0.024(4) 0.022(4) 0.004(3) -0.005(3) -0.005(3) C4 0.022(4) 0.034(5) 0.024(4) 0.000(3) 0.006(3) 0.002(3) C5 0.034(4) 0.033(4) 0.026(4) 0.006(3) 0.000(3) 0.007(4) C6 0.039(5) 0.030(4) 0.019(4) 0.003(3) -0.005(3) 0.007(4) O1 0.033(3) 0.030(3) 0.030(3) 0.000(2) 0.004(2) 0.010(2) O4 0.052(4) 0.059(4) 0.032(3) 0.006(3) -0.004(3) -0.016(3) O5 0.057(4) 0.027(3) 0.059(4) 0.001(3) 0.013(3) 0.005(3) S7 0.0785(18) 0.0330(12) 0.0491(14) 0.0088(10) -0.0186(13) -0.0010(12) S7A 0.0785(18) 0.0330(12) 0.0491(14) 0.0088(10) -0.0186(13) -0.0010(12) O1W 0.071(5) 0.041(4) 0.058(4) 0.006(3) 0.004(4) -0.009(3) O2W 0.043(3) 0.049(4) 0.030(3) -0.002(3) 0.004(3) 0.011(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 S2 Bi1 S5 90.15(6) . . ? S2 Bi1 S4 85.80(6) . 4_565 ? S5 Bi1 S4 91.93(7) . 4_565 ? S2 Bi1 S3 171.03(6) . 4_665 ? S5 Bi1 S3 87.16(6) . 4_665 ? S4 Bi1 S3 102.83(6) 4_565 4_665 ? S2 Bi1 S1 88.58(6) . 3_665 ? S5 Bi1 S1 84.86(7) . 3_665 ? S4 Bi1 S1 173.52(6) 4_565 3_665 ? S3 Bi1 S1 82.66(6) 4_665 3_665 ? S2 Bi1 S6 98.89(7) . 1_554 ? S5 Bi1 S6 168.96(7) . 1_554 ? S4 Bi1 S6 82.49(7) 4_565 1_554 ? S3 Bi1 S6 84.82(6) 4_665 1_554 ? S1 Bi1 S6 101.59(7) 3_665 1_554 ? N2 Mn1 N2 180.0 3_565 . ? N2 Mn1 N1 91.4(2) 3_565 . ? N2 Mn1 N1 88.6(2) . . ? N2 Mn1 N1 88.6(2) 3_565 3_565 ? N2 Mn1 N1 91.4(2) . 3_565 ? N1 Mn1 N1 180.0 . 3_565 ? N2 Mn1 O1 90.4(2) 3_565 . ? N2 Mn1 O1 89.6(2) . . ? N1 Mn1 O1 87.5(2) . . ? N1 Mn1 O1 92.5(2) 3_565 . ? N2 Mn1 O1 89.6(2) 3_565 3_565 ? N2 Mn1 O1 90.4(2) . 3_565 ? N1 Mn1 O1 92.5(2) . 3_565 ? N1 Mn1 O1 87.5(2) 3_565 3_565 ? O1 Mn1 O1 180.0(2) . 3_565 ? N4 Mn2 O2 174.4(4) . . ? N4 Mn2 N5 89.3(3) . . ? O2 Mn2 N5 86.9(4) . . ? N4 Mn2 N6 91.6(2) . . ? O2 Mn2 N6 92.0(4) . . ? N5 Mn2 N6 176.9(3) . . ? N4 Mn2 N3 97.6(3) . . ? O2 Mn2 N3 86.6(4) . . ? N5 Mn2 N3 91.7(3) . . ? N6 Mn2 N3 91.1(3) . . ? N4 Mn2 N7A 167.8(6) . . ? N5 Mn2 N7A 91.4(6) . . ? N6 Mn2 N7A 87.1(6) . . ? N3 Mn2 N7A 94.6(6) . . ? N4 Mn2 O3A 86.6(3) . . ? N5 Mn2 O3A 78.6(4) . . ? N6 Mn2 O3A 98.4(4) . . ? N3 Mn2 O3A 169.5(4) . . ? N7A Mn2 O3A 81.6(6) . . ? N4 Mn2 O3 88.4(4) . . ? O2 Mn2 O3 88.1(5) . . ? N5 Mn2 O3 97.2(5) . . ? N6 Mn2 O3 79.8(5) . . ? N3 Mn2 O3 169.4(5) . . ? O2A Mn3 O2A 180.0 3_766 . ? O2A Mn3 O5 94.5(5) 3_766 . ? O2A Mn3 O5 85.5(5) . . ? O5 Mn3 O5 180.0 3_766 . ? O5 Mn3 O4 90.5(2) 3_766 3_766 ? O5 Mn3 O4 89.5(2) . 3_766 ? O2A Mn3 O4 93.5(4) 3_766 . ? O2A Mn3 O4 86.5(4) . . ? O5 Mn3 O4 89.5(2) 3_766 . ? O5 Mn3 O4 90.5(2) . . ? O4 Mn3 O4 180.0 3_766 . ? O5 Mn3 N7 83.3(6) 3_766 3_766 ? O5 Mn3 N7 96.7(6) . 3_766 ? O4 Mn3 N7 87.5(5) 3_766 3_766 ? O4 Mn3 N7 92.5(5) . 3_766 ? O5 Mn3 N7 96.7(6) 3_766 . ? O5 Mn3 N7 83.3(6) . . ? O4 Mn3 N7 92.5(5) 3_766 . ? O4 Mn3 N7 87.5(5) . . ? N7 Mn3 N7 180.0 3_766 . ? C1 S1 Bi1 99.9(3) . 3_665 ? C2 S2 Bi1 96.3(3) . . ? C3 S3 Bi1 97.8(3) . 4_566 ? C4 S4 Bi1 98.2(3) . 4_666 ? C5 S5 Bi1 95.6(3) . . ? C6 S6 Bi1 99.4(3) . 1_556 ? C1 N1 Mn1 164.6(7) . . ? C2 N2 Mn1 152.0(7) . . ? C3 N3 Mn2 174.9(7) . . ? C4 N4 Mn2 177.3(6) . . ? C5 N5 Mn2 167.5(8) . . ? C6 N6 Mn2 173.0(7) . . ? N1 C1 S1 179.2(7) . . ? N2 C2 S2 179.9(9) . . ? N3 C3 S3 179.2(8) . . ? N4 C4 S4 179.1(7) . . ? N5 C5 S5 177.1(8) . . ? N6 C6 S6 177.2(7) . . ? Mn1 O1 H11 113.1 . . ? Mn1 O1 H12 116.4 . . ? H11 O1 H12 113.8 . . ? Mn3 O4 H41 112.2 . . ? Mn3 O4 H42 116.6 . . ? H41 O4 H42 113.6 . . ? Mn3 O5 H51 123.2 . . ? Mn3 O5 H52 112.8 . . ? H51 O5 H52 100.5 . . ? C7 N7 Mn3 158.5(16) . . ? N7 C7 S7 177.8(16) . . ? Mn2 O2 H21 104.4 . . ? Mn2 O2 H22 139.5 . . ? H21 O2 H22 109.4 . . ? Mn2 O3 H31 123.8 . . ? Mn2 O3 H32 124.3 . . ? H31 O3 H32 108.4 . . ? C7A N7A Mn2 150.2(17) . . ? N7A C7A S7A 171.9(18) . . ? Mn3 O2A H21A 111.8 . . ? Mn3 O2A H22A 144.3 . . ? H21A O2A H22A 99.0 . . ? Mn2 O3A H31A 124.3 . . ? Mn2 O3A H32A 120.0 . . ? H31A O3A H32A 97.1 . . ? H1W O1W H2W 111.2 . . ? H3W O2W H4W 111.2 . . ? 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 Bi1 S2 2.7988(19) . ? Bi1 S5 2.809(2) . ? Bi1 S4 2.813(2) 4_565 ? Bi1 S3 2.825(2) 4_665 ? Bi1 S1 2.832(2) 3_665 ? Bi1 S6 2.842(2) 1_554 ? Mn1 N2 2.179(7) 3_565 ? Mn1 N2 2.179(7) . ? Mn1 N1 2.198(7) . ? Mn1 N1 2.198(7) 3_565 ? Mn1 O1 2.258(5) . ? Mn1 O1 2.258(5) 3_565 ? Mn2 N4 2.172(7) . ? Mn2 O2 2.180(14) . ? Mn2 N5 2.184(7) . ? Mn2 N6 2.195(7) . ? Mn2 N3 2.200(7) . ? Mn2 N7A 2.22(2) . ? Mn2 O3A 2.233(11) . ? Mn2 O3 2.273(13) . ? Mn3 O2A 2.112(15) 3_766 ? Mn3 O2A 2.112(15) . ? Mn3 O5 2.185(6) 3_766 ? Mn3 O5 2.185(6) . ? Mn3 O4 2.199(6) 3_766 ? Mn3 O4 2.199(6) . ? Mn3 N7 2.22(2) 3_766 ? Mn3 N7 2.22(2) . ? S1 C1 1.655(8) . ? S2 C2 1.654(8) . ? S3 C3 1.639(8) . ? S4 C4 1.659(8) . ? S5 C5 1.661(8) . ? S6 C6 1.655(8) . ? N1 C1 1.162(10) . ? N2 C2 1.144(10) . ? N3 C3 1.144(9) . ? N4 C4 1.145(10) . ? N5 C5 1.129(10) . ? N6 C6 1.143(9) . ? O1 H11 0.8495 . ? O1 H12 0.8499 . ? O4 H41 0.8499 . ? O4 H42 0.8500 . ? O5 H51 0.8497 . ? O5 H52 0.8501 . ? S7 C7 1.700(15) . ? N7 C7 1.17(2) . ? O2 H21 0.8500 . ? O2 H22 0.8495 . ? O3 H31 0.8500 . ? O3 H32 0.8500 . ? S7A C7A 1.745(18) . ? N7A C7A 1.23(3) . ? O2A H21A 0.8549 . ? O2A H22A 0.8479 . ? O3A H31A 0.8500 . ? O3A H32A 0.8500 . ? O1W H1W 0.8501 . ? O1W H2W 0.8499 . ? O2W H3W 0.8500 . ? O2W H4W 0.8500 . ?