#------------------------------------------------------------------------------ #$Date: 2020-04-10 04:23:44 +0300 (Fri, 10 Apr 2020) $ #$Revision: 250578 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557770.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_1557770 loop_ _publ_author_name 'Cliffe, Matthew' 'Grey, Clare P.' 'Keyzer, Evan N.' 'Bond, Andrew David' 'Astle, Maxwell A.' _publ_section_title ; The structures of ordered defects in thiocyanate analogues of Prussian Blue  ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC01246G _journal_year 2020 _chemical_formula_moiety 'C7 H10 Bi Mn2 N7 O5 S7, 2(H2 O)' _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 91.208(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.3698(3) _cell_length_b 26.0037(9) _cell_length_c 12.2466(4) _cell_measurement_reflns_used 6808 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 66.60 _cell_measurement_theta_min 3.40 _cell_volume 2664.83(16) _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 300(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.1315 _diffrn_reflns_av_unetI/netI 0.0734 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _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 30850 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 66.717 _diffrn_reflns_theta_max 66.717 _diffrn_reflns_theta_min 3.399 _diffrn_source 'Incoatec I\mS Cu microsource' _exptl_absorpt_coefficient_mu 25.858 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.3751 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.122 _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 3.391 _refine_diff_density_min -1.432 _refine_diff_density_rms 0.217 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 4712 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0553 _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^)+(0.0867P)^2^+0.2708P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1326 _refine_ls_wR_factor_ref 0.1544 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3248 _reflns_number_total 4712 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01246g3.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1557770 _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 0.122 _shelx_estimated_absorpt_t_max 0.782 _shelx_res_file ; TITL MC_B2_0002 in P2(1)/n 1.res created by SHELXL-2018/1 at 23:15:05 on 29-Oct-2019 CELL 1.5418 8.3698 26.0037 12.2466 90.00 91.208 90.00 ZERR 4.00 0.0003 0.0009 0.0004 0.00 0.002 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 27 L.S. 30 EXYZ S7 S7A EADP S7 S7A ACTA BOND $H LIST 4 FMAP 2 PLAN -10 WGHT 0.086700 0.270800 FVAR 0.20370 0.69770 BI1 3 0.462999 0.334130 -0.057785 11.00000 0.03725 0.03827 = 0.03299 -0.00264 0.00350 0.00044 MN1 4 0.000000 0.500000 0.000000 10.50000 0.03526 0.04073 = 0.04448 -0.00637 0.00664 0.00260 MN2 4 0.455885 0.337066 0.440385 11.00000 0.04297 0.04399 = 0.03475 -0.00142 0.00595 0.00043 MN3 4 1.000000 0.500000 0.500000 10.50000 0.05756 0.05528 = 0.04314 0.00051 0.00100 -0.00551 S1 7 0.262988 0.648477 0.184894 11.00000 0.06867 0.06967 = 0.05484 -0.02235 0.02118 -0.02154 S2 7 0.523548 0.426588 0.054633 11.00000 0.04228 0.05739 = 0.09269 -0.02576 -0.00227 0.00237 S3 7 -0.056788 0.257410 0.320978 11.00000 0.05373 0.06335 = 0.08536 0.02964 -0.02239 -0.00775 S4 7 0.708824 0.178216 0.586713 11.00000 0.08037 0.06884 = 0.05324 0.01973 0.02654 0.02911 S5 7 0.674228 0.284496 0.086951 11.00000 0.08529 0.10757 = 0.03837 -0.01680 -0.00513 0.04905 S6 7 0.210885 0.368628 0.800795 11.00000 0.05439 0.10514 = 0.04072 0.00154 0.01051 0.02804 N1 5 0.109565 0.571542 0.062209 11.00000 0.04829 0.03857 = 0.07801 -0.00596 0.02461 -0.00087 N2 5 0.207975 0.458538 0.066962 11.00000 0.05596 0.05706 = 0.07851 -0.01136 -0.00346 -0.00303 N3 5 0.231269 0.301694 0.389646 11.00000 0.07510 0.06741 = 0.05094 -0.00628 -0.00399 -0.01166 N4 5 0.573374 0.267533 0.500749 11.00000 0.06542 0.06993 = 0.06925 0.00518 0.02609 0.01792 N5 5 0.563861 0.325402 0.281545 11.00000 0.08173 0.09622 = 0.03648 0.00303 0.01168 0.02094 N6 5 0.352004 0.355038 0.598923 11.00000 0.07940 0.06649 = 0.04193 -0.00761 0.00918 0.01455 C1 1 0.174447 0.602512 0.110155 11.00000 0.04865 0.03736 = 0.05732 -0.00063 0.02294 -0.00614 C2 1 0.338700 0.445398 0.061633 11.00000 0.04289 0.03829 = 0.04525 0.00225 0.00613 0.01118 C3 1 0.115312 0.283358 0.360745 11.00000 0.05520 0.04534 = 0.02655 0.00800 -0.00382 0.00624 C4 1 0.629992 0.231062 0.535412 11.00000 0.04780 0.04629 = 0.03674 0.00057 0.01994 0.00793 C5 1 0.605980 0.308013 0.203452 11.00000 0.06027 0.06745 = 0.03803 -0.00381 0.01056 0.01945 C6 1 0.298342 0.361052 0.684320 11.00000 0.05000 0.06510 = 0.04382 -0.00403 0.00384 0.01546 O1 6 -0.124280 0.492867 0.161255 11.00000 0.05429 0.08065 = 0.04610 -0.00372 0.01248 0.00344 AFIX 3 H11 2 -0.133080 0.461517 0.181175 11.00000 -1.50000 H12 2 -0.208980 0.510678 0.171156 11.00000 -1.50000 AFIX 0 O4 6 1.084593 0.526925 0.340405 11.00000 0.09282 0.11994 = 0.04832 0.00830 0.00821 -0.03339 AFIX 3 H41 2 1.024992 0.516075 0.288765 11.00000 -1.50000 H42 2 1.184675 0.524605 0.327085 11.00000 -1.50000 AFIX 0 O5 6 0.963206 0.580283 0.551002 11.00000 0.08593 0.07104 = 0.08216 -0.01132 0.00698 0.01757 AFIX 3 H51 2 0.984976 0.606733 0.512652 11.00000 -1.50000 H52 2 1.007846 0.588643 0.610952 11.00000 -1.50000 AFIX 0 PART 1 S7 7 0.495945 0.519485 0.289098 21.00000 0.09396 0.06701 = 0.07504 0.00565 -0.02309 -0.00287 N7 5 0.750298 0.505937 0.432890 21.00000 0.06706 C7 1 0.643514 0.509046 0.374024 21.00000 0.04359 O2 6 0.350759 0.409323 0.366980 21.00000 0.06277 AFIX 3 H21 2 0.256759 0.412453 0.393299 21.00000 -1.50000 H22 2 0.385229 0.438863 0.347630 21.00000 -1.50000 AFIX 0 O3 6 0.657048 0.386041 0.512527 21.00000 0.08045 AFIX 3 H31 2 0.742108 0.372121 0.537736 21.00000 -1.50000 H32 2 0.678118 0.417261 0.496077 21.00000 -1.50000 AFIX 0 PART 2 S7A 7 0.495945 0.519485 0.289098 -21.00000 0.09396 0.06701 = 0.07504 0.00565 -0.02309 -0.00287 N7A 5 0.396609 0.414977 0.396523 -21.00000 0.03402 C7A 1 0.425232 0.459078 0.353457 -21.00000 0.10312 O2A 6 1.231994 0.514570 0.564741 -21.00000 0.06993 AFIX 3 H21A 2 1.251192 0.547070 0.564661 -21.00000 -1.50000 H22A 2 1.306392 0.504820 0.607581 -21.00000 -1.50000 AFIX 0 O3A 6 0.687943 0.377231 0.474146 -21.00000 0.05265 AFIX 3 H31A 2 0.763153 0.366002 0.514956 -21.00000 -1.50000 H32A 2 0.744693 0.382251 0.417616 -21.00000 -1.50000 AFIX 0 PART 0 O1W 6 -0.093150 0.393506 0.238204 11.00000 0.16366 0.07711 = 0.10857 -0.00316 -0.00353 -0.02163 AFIX 3 H1W 2 -0.023510 0.377356 0.200704 11.00000 -1.50000 H2W 2 -0.178840 0.375846 0.244984 11.00000 -1.50000 AFIX 0 O2W 6 0.943156 0.338329 0.582006 11.00000 0.11189 0.13412 = 0.07583 -0.01899 0.00861 0.01223 AFIX 3 H3W 2 0.995855 0.310139 0.581256 11.00000 -1.50000 H4W 2 0.890285 0.341589 0.640786 11.00000 -1.50000 AFIX 0 HKLF 4 REM MC_B2_0002 in P2(1)/n REM R1 = 0.0553 for 3248 Fo > 4sig(Fo) and 0.0913 for all 4712 data REM 280 parameters refined using 0 restraints END WGHT 0.0867 0.2708 REM Highest difference peak 3.391, deepest hole -1.432, 1-sigma level 0.217 Q1 1 0.4659 0.2931 -0.0571 11.00000 0.05 3.39 Q2 1 0.4649 0.3745 -0.0567 11.00000 0.05 3.11 Q3 1 0.5383 0.3953 -0.0097 11.00000 0.05 1.24 Q4 1 0.3952 0.2786 -0.1179 11.00000 0.05 1.13 Q5 1 0.0114 0.5407 -0.0057 11.00000 0.05 1.06 Q6 1 0.4790 0.3331 0.0108 11.00000 0.05 0.93 Q7 1 0.4495 0.3737 0.4101 11.00000 0.05 0.92 Q8 1 0.5711 0.2836 -0.0903 11.00000 0.05 0.78 Q9 1 0.5519 0.4724 0.0859 11.00000 0.05 0.75 Q10 1 0.7437 0.3204 -0.1647 11.00000 0.05 0.74 ; _shelx_res_checksum 94426 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 0.46300(5) 0.33413(2) -0.05778(3) 0.03613(16) Uani 1 1 d . . . . . Mn1 Mn 0.000000 0.500000 0.000000 0.0401(6) Uani 1 2 d S . P . . Mn2 Mn 0.4559(2) 0.33707(7) 0.44039(15) 0.0405(4) Uani 1 1 d . . . . . Mn3 Mn 1.000000 0.500000 0.500000 0.0520(7) Uani 1 2 d S . P . . S1 S 0.2630(5) 0.64848(16) 0.1849(3) 0.0641(10) Uani 1 1 d . . . . . S2 S 0.5235(4) 0.42659(15) 0.0546(4) 0.0642(10) Uani 1 1 d . . . . . S3 S -0.0568(5) 0.25741(16) 0.3210(4) 0.0678(11) Uani 1 1 d . . . . . S4 S 0.7088(5) 0.17822(15) 0.5867(3) 0.0671(11) Uani 1 1 d . . . . . S5 S 0.6742(6) 0.28450(19) 0.0870(3) 0.0772(14) Uani 1 1 d . . . . . S6 S 0.2109(5) 0.36863(18) 0.8008(3) 0.0666(11) Uani 1 1 d . . . . . N1 N 0.1096(14) 0.5715(4) 0.0622(10) 0.055(3) Uani 1 1 d . . . . . N2 N 0.2080(16) 0.4585(5) 0.0670(11) 0.064(3) Uani 1 1 d . . . . . N3 N 0.2313(17) 0.3017(5) 0.3896(10) 0.065(3) Uani 1 1 d . . . . . N4 N 0.5734(16) 0.2675(5) 0.5007(11) 0.068(4) Uani 1 1 d . . . . . N5 N 0.5639(18) 0.3254(6) 0.2815(10) 0.071(4) Uani 1 1 d . . . . . N6 N 0.3520(17) 0.3550(5) 0.5989(10) 0.062(3) Uani 1 1 d . . . . . C1 C 0.1744(16) 0.6025(5) 0.1102(11) 0.047(3) Uani 1 1 d . . . . . C2 C 0.3387(15) 0.4454(5) 0.0616(10) 0.042(3) Uani 1 1 d . . . . . C3 C 0.1153(16) 0.2834(5) 0.3607(9) 0.042(3) Uani 1 1 d . . . . . C4 C 0.6300(15) 0.2311(5) 0.5354(10) 0.043(3) Uani 1 1 d . . . . . C5 C 0.6060(18) 0.3080(6) 0.2035(11) 0.055(4) Uani 1 1 d . . . . . C6 C 0.2983(17) 0.3611(6) 0.6843(11) 0.053(3) Uani 1 1 d . . . . . O1 O -0.1243(11) 0.4929(4) 0.1613(7) 0.060(3) Uani 1 1 d . . . . . H11 H -0.133080 0.461517 0.181175 0.090 Uiso 1 1 d R U . . . H12 H -0.208980 0.510678 0.171156 0.090 Uiso 1 1 d R U . . . O4 O 1.0846(15) 0.5269(5) 0.3404(9) 0.087(4) Uani 1 1 d . . . . . H41 H 1.024992 0.516075 0.288765 0.130 Uiso 1 1 d R U . . . H42 H 1.184675 0.524605 0.327085 0.130 Uiso 1 1 d R U . . . O5 O 0.9632(14) 0.5803(5) 0.5510(10) 0.080(3) Uani 1 1 d . . . . . H51 H 0.984976 0.606733 0.512652 0.119 Uiso 1 1 d R U . . . H52 H 1.007846 0.588643 0.610952 0.119 Uiso 1 1 d R U . . . S7 S 0.4959(6) 0.51949(17) 0.2891(4) 0.0790(13) Uani 0.70(3) 1 d . . P A 1 N7 N 0.750(3) 0.5059(10) 0.4329(19) 0.067(6) Uiso 0.70(3) 1 d . . P A 1 C7 C 0.644(2) 0.5090(7) 0.3740(15) 0.044(5) Uiso 0.70(3) 1 d . . P A 1 O2 O 0.351(2) 0.4093(7) 0.3670(15) 0.063(5) Uiso 0.70(3) 1 d . . P A 1 H21 H 0.256759 0.412453 0.393299 0.094 Uiso 0.70(3) 1 d R U P A 1 H22 H 0.385229 0.438863 0.347630 0.094 Uiso 0.70(3) 1 d R U P A 1 O3 O 0.657(3) 0.3860(8) 0.5125(18) 0.080(6) Uiso 0.70(3) 1 d . . P A 1 H31 H 0.742108 0.372121 0.537736 0.121 Uiso 0.70(3) 1 d R U P A 1 H32 H 0.678118 0.417261 0.496077 0.121 Uiso 0.70(3) 1 d R U P A 1 S7A S 0.4959(6) 0.51949(17) 0.2891(4) 0.0790(13) Uani 0.30(3) 1 d . . P A 2 N7A N 0.397(5) 0.4150(13) 0.397(3) 0.034(8) Uiso 0.30(3) 1 d . . P A 2 C7A C 0.425(9) 0.459(3) 0.353(6) 0.10(3) Uiso 0.30(3) 1 d . . P A 2 O2A O 1.232(5) 0.515(2) 0.565(3) 0.070(12) Uiso 0.30(3) 1 d . . P A 2 H21A H 1.251192 0.547070 0.564661 0.105 Uiso 0.30(3) 1 d R U P A 2 H22A H 1.306392 0.504820 0.607581 0.105 Uiso 0.30(3) 1 d R U P A 2 O3A O 0.688(4) 0.3772(14) 0.474(3) 0.053(9) Uiso 0.30(3) 1 d . . P A 2 H31A H 0.763153 0.366002 0.514956 0.079 Uiso 0.30(3) 1 d R U P A 2 H32A H 0.744693 0.382251 0.417616 0.079 Uiso 0.30(3) 1 d R U P A 2 O1W O -0.093(2) 0.3935(5) 0.2382(12) 0.117(5) Uani 1 1 d . . . . . H1W H -0.023510 0.377356 0.200704 0.175 Uiso 1 1 d R U . . . H2W H -0.178840 0.375846 0.244984 0.175 Uiso 1 1 d R U . . . O2W O 0.9432(19) 0.3383(6) 0.5820(11) 0.107(5) Uani 1 1 d . . . . . H3W H 0.995855 0.310139 0.581256 0.161 Uiso 1 1 d R U . . . H4W H 0.890285 0.341589 0.640786 0.161 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 0.0373(3) 0.0383(2) 0.0330(2) -0.00264(19) 0.00350(16) 0.0004(2) Mn1 0.0353(13) 0.0407(14) 0.0445(15) -0.0064(12) 0.0066(12) 0.0026(12) Mn2 0.0430(10) 0.0440(10) 0.0347(9) -0.0014(8) 0.0060(8) 0.0004(9) Mn3 0.0576(18) 0.0553(17) 0.0431(16) 0.0005(14) 0.0010(14) -0.0055(15) S1 0.069(2) 0.070(2) 0.055(2) -0.0223(17) 0.0212(18) -0.0215(19) S2 0.0423(18) 0.057(2) 0.093(3) -0.0258(19) -0.0023(18) 0.0024(16) S3 0.054(2) 0.063(2) 0.085(3) 0.030(2) -0.022(2) -0.0078(17) S4 0.080(3) 0.069(2) 0.053(2) 0.0197(17) 0.0265(19) 0.029(2) S5 0.085(3) 0.108(3) 0.0384(19) -0.0168(19) -0.0051(19) 0.049(3) S6 0.054(2) 0.105(3) 0.0407(18) 0.0015(18) 0.0105(16) 0.028(2) N1 0.048(6) 0.039(6) 0.078(8) -0.006(6) 0.025(6) -0.001(5) N2 0.056(8) 0.057(7) 0.079(9) -0.011(6) -0.003(7) -0.003(6) N3 0.075(9) 0.067(8) 0.051(7) -0.006(6) -0.004(7) -0.012(7) N4 0.065(8) 0.070(9) 0.069(8) 0.005(7) 0.026(7) 0.018(7) N5 0.082(9) 0.096(11) 0.036(6) 0.003(7) 0.012(6) 0.021(8) N6 0.079(9) 0.066(8) 0.042(7) -0.008(6) 0.009(6) 0.015(7) C1 0.049(8) 0.037(7) 0.057(8) -0.001(6) 0.023(6) -0.006(6) C2 0.043(7) 0.038(6) 0.045(7) 0.002(5) 0.006(6) 0.011(5) C3 0.055(8) 0.045(7) 0.027(6) 0.008(5) -0.004(6) 0.006(6) C4 0.048(7) 0.046(7) 0.037(6) 0.001(5) 0.020(6) 0.008(6) C5 0.060(9) 0.067(9) 0.038(7) -0.004(6) 0.011(7) 0.019(7) C6 0.050(8) 0.065(9) 0.044(8) -0.004(6) 0.004(6) 0.015(7) O1 0.054(6) 0.081(7) 0.046(5) -0.004(5) 0.012(4) 0.003(5) O4 0.093(9) 0.120(11) 0.048(6) 0.008(6) 0.008(6) -0.033(8) O5 0.086(8) 0.071(7) 0.082(8) -0.011(6) 0.007(7) 0.018(6) S7 0.094(3) 0.067(3) 0.075(3) 0.006(2) -0.023(2) -0.003(2) S7A 0.094(3) 0.067(3) 0.075(3) 0.006(2) -0.023(2) -0.003(2) O1W 0.164(16) 0.077(9) 0.109(11) -0.003(8) -0.004(11) -0.022(10) O2W 0.112(11) 0.134(13) 0.076(9) -0.019(8) 0.009(8) 0.012(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 S5 Bi1 S3 88.47(12) . 4_665 ? S5 Bi1 S2 88.81(13) . . ? S3 Bi1 S2 172.64(12) 4_665 . ? S5 Bi1 S4 91.43(14) . 4_565 ? S3 Bi1 S4 101.47(12) 4_665 4_565 ? S2 Bi1 S4 85.44(11) . 4_565 ? S5 Bi1 S1 85.04(14) . 3_665 ? S3 Bi1 S1 83.36(12) 4_665 3_665 ? S2 Bi1 S1 89.59(11) . 3_665 ? S4 Bi1 S1 173.97(11) 4_565 3_665 ? S5 Bi1 S6 169.40(15) . 1_554 ? S3 Bi1 S6 84.88(12) 4_665 1_554 ? S2 Bi1 S6 98.75(13) . 1_554 ? S4 Bi1 S6 81.84(13) 4_565 1_554 ? S1 Bi1 S6 102.33(12) 3_665 1_554 ? N2 Mn1 N2 180.0 3_565 . ? N2 Mn1 N1 88.0(4) 3_565 3_565 ? N2 Mn1 N1 92.0(4) . 3_565 ? N2 Mn1 N1 92.0(4) 3_565 . ? N2 Mn1 N1 88.0(4) . . ? N1 Mn1 N1 180.0(5) 3_565 . ? N2 Mn1 O1 89.5(5) 3_565 . ? N2 Mn1 O1 90.5(5) . . ? N1 Mn1 O1 92.1(4) 3_565 . ? N1 Mn1 O1 87.9(4) . . ? N2 Mn1 O1 90.5(5) 3_565 3_565 ? N2 Mn1 O1 89.5(5) . 3_565 ? N1 Mn1 O1 87.9(4) 3_565 3_565 ? N1 Mn1 O1 92.1(4) . 3_565 ? O1 Mn1 O1 180.0 . 3_565 ? N7A Mn2 N3 97.7(12) . . ? N7A Mn2 N4 165.0(12) . . ? N3 Mn2 N4 97.3(5) . . ? N7A Mn2 N5 90.3(10) . . ? N3 Mn2 N5 93.3(5) . . ? N4 Mn2 N5 89.7(5) . . ? N7A Mn2 N6 85.8(10) . . ? N3 Mn2 N6 89.2(5) . . ? N4 Mn2 N6 93.5(5) . . ? N5 Mn2 N6 175.6(6) . . ? N7A Mn2 O3A 78.5(14) . . ? N3 Mn2 O3A 173.7(11) . . ? N4 Mn2 O3A 86.6(10) . . ? N5 Mn2 O3A 81.7(12) . . ? N6 Mn2 O3A 95.5(12) . . ? N3 Mn2 O2 84.9(6) . . ? N4 Mn2 O2 175.1(6) . . ? N5 Mn2 O2 85.7(6) . . ? N6 Mn2 O2 91.0(6) . . ? N3 Mn2 O3 167.8(7) . . ? N4 Mn2 O3 90.4(7) . . ? N5 Mn2 O3 96.1(8) . . ? N6 Mn2 O3 80.8(7) . . ? O2 Mn2 O3 88.2(7) . . ? O2A Mn3 O2A 180.0 . 3_766 ? O2A Mn3 O5 81.8(15) . . ? O2A Mn3 O5 98.2(15) 3_766 . ? O5 Mn3 O5 180.0 . 3_766 ? O5 Mn3 O4 90.0(5) . 3_766 ? O5 Mn3 O4 90.0(5) 3_766 3_766 ? O2A Mn3 O4 88.1(12) . . ? O2A Mn3 O4 91.9(12) 3_766 . ? O5 Mn3 O4 90.0(5) . . ? O5 Mn3 O4 90.0(5) 3_766 . ? O4 Mn3 O4 180.0 3_766 . ? O5 Mn3 N7 95.5(7) . 3_766 ? O5 Mn3 N7 84.5(7) 3_766 3_766 ? O4 Mn3 N7 88.1(7) 3_766 3_766 ? O4 Mn3 N7 91.9(7) . 3_766 ? O5 Mn3 N7 84.5(7) . . ? O5 Mn3 N7 95.5(7) 3_766 . ? O4 Mn3 N7 91.9(7) 3_766 . ? O4 Mn3 N7 88.1(7) . . ? N7 Mn3 N7 180.0 3_766 . ? C1 S1 Bi1 99.7(4) . 3_665 ? C2 S2 Bi1 97.0(5) . . ? C3 S3 Bi1 98.6(4) . 4_566 ? C4 S4 Bi1 99.1(4) . 4_666 ? C5 S5 Bi1 98.6(5) . . ? C6 S6 Bi1 98.8(5) . 1_556 ? C1 N1 Mn1 167.0(12) . . ? C2 N2 Mn1 151.0(13) . . ? C3 N3 Mn2 178.4(12) . . ? C4 N4 Mn2 177.2(12) . . ? C5 N5 Mn2 163.6(15) . . ? C6 N6 Mn2 175.4(13) . . ? N1 C1 S1 177.3(12) . . ? N2 C2 S2 179.7(15) . . ? N3 C3 S3 178.5(14) . . ? N4 C4 S4 179.0(13) . . ? N5 C5 S5 177.3(17) . . ? N6 C6 S6 176.1(14) . . ? Mn1 O1 H11 111.8 . . ? Mn1 O1 H12 118.5 . . ? H11 O1 H12 113.5 . . ? Mn3 O4 H41 111.2 . . ? Mn3 O4 H42 118.6 . . ? H41 O4 H42 113.4 . . ? Mn3 O5 H51 125.0 . . ? Mn3 O5 H52 115.4 . . ? H51 O5 H52 100.1 . . ? C7 N7 Mn3 162(2) . . ? N7 C7 S7 174(2) . . ? Mn2 O2 H21 106.4 . . ? Mn2 O2 H22 136.7 . . ? H21 O2 H22 109.6 . . ? Mn2 O3 H31 120.6 . . ? Mn2 O3 H32 126.5 . . ? H31 O3 H32 108.3 . . ? C7A N7A Mn2 154(4) . . ? N7A C7A S7A 172(6) . . ? Mn3 O2A H21A 110.2 . . ? Mn3 O2A H22A 146.9 . . ? H21A O2A H22A 99.2 . . ? Mn2 O3A H31A 125.4 . . ? Mn2 O3A H32A 114.5 . . ? H31A O3A H32A 96.4 . . ? H1W O1W H2W 111.6 . . ? H3W O2W H4W 111.7 . . ? 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 S5 2.793(4) . ? Bi1 S3 2.808(4) 4_665 ? Bi1 S2 2.811(4) . ? Bi1 S4 2.814(4) 4_565 ? Bi1 S1 2.835(4) 3_665 ? Bi1 S6 2.847(4) 1_554 ? Mn1 N2 2.192(13) 3_565 ? Mn1 N2 2.192(13) . ? Mn1 N1 2.203(12) 3_565 ? Mn1 N1 2.203(12) . ? Mn1 O1 2.259(9) . ? Mn1 O1 2.259(9) 3_565 ? Mn2 N7A 2.15(3) . ? Mn2 N3 2.172(14) . ? Mn2 N4 2.180(14) . ? Mn2 N5 2.183(13) . ? Mn2 N6 2.194(12) . ? Mn2 O3A 2.24(3) . ? Mn2 O2 2.254(17) . ? Mn2 O3 2.27(2) . ? Mn3 O2A 2.12(4) . ? Mn3 O2A 2.12(4) 3_766 ? Mn3 O5 2.203(11) . ? Mn3 O5 2.203(11) 3_766 ? Mn3 O4 2.207(11) 3_766 ? Mn3 O4 2.207(11) . ? Mn3 N7 2.23(3) 3_766 ? Mn3 N7 2.23(3) . ? S1 C1 1.669(14) . ? S2 C2 1.627(12) . ? S3 C3 1.655(14) . ? S4 C4 1.643(13) . ? S5 C5 1.664(14) . ? S6 C6 1.629(14) . ? N1 C1 1.129(17) . ? N2 C2 1.149(17) . ? N3 C3 1.131(17) . ? N4 C4 1.138(18) . ? N5 C5 1.121(18) . ? N6 C6 1.157(17) . ? O1 H11 0.8546 . ? O1 H12 0.8576 . ? O4 H41 0.8456 . ? O4 H42 0.8589 . ? O5 H51 0.8547 . ? O5 H52 0.8452 . ? S7 C7 1.621(18) . ? N7 C7 1.14(3) . ? O2 H21 0.8603 . ? O2 H22 0.8558 . ? O3 H31 0.8508 . ? O3 H32 0.8557 . ? S7A C7A 1.86(8) . ? N7A C7A 1.29(8) . ? O2A H21A 0.8603 . ? O2A H22A 0.8447 . ? O3A H31A 0.8474 . ? O3A H32A 0.8578 . ? O1W H1W 0.8592 . ? O1W H2W 0.8571 . ? O2W H3W 0.8557 . ? O2W H4W 0.8571 . ?