#------------------------------------------------------------------------------ #$Date: 2023-09-19 10:04:27 +0300 (Tue, 19 Sep 2023) $ #$Revision: 286402 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/75/8107513.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_8107513 loop_ _publ_author_name 'Shi, Zheng' 'Zhang, Zhongyu' 'Han, Bing' 'Li, Yunyun' _publ_section_title ; The crystal structure of diaqua-methanol-\k1 O- (3-thiophenecarboxylato-\kO)-(2,2′-dipyridyl-\k2 N,N′)manganese(II) 3-thiophenecarboxylate, C21H22N2O7S2Mn ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 623 _journal_page_last 625 _journal_paper_doi 10.1515/ncrs-2023-0123 _journal_volume 238 _journal_year 2023 _chemical_formula_moiety 'C16 H19 Mn N2 O5 S, C5 H3 O2 S' _chemical_formula_sum 'C21 H22 Mn N2 O7 S2' _chemical_formula_weight 533.46 _chemical_name_systematic ; 3-thiophenecarboxylato-? O-( 2,2'-dipyridyl -?2 N, N') manganese(II), ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 96.664(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.544(6) _cell_length_b 9.636(4) _cell_length_c 17.087(7) _cell_measurement_reflns_used 6603 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 26.090 _cell_measurement_theta_min 2.400 _cell_volume 2378.5(17) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 14425 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.121 _diffrn_reflns_theta_min 2.400 _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_meas . _exptl_crystal_description block _exptl_crystal_F_000 1100 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.836 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.053 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 318 _refine_ls_number_reflns 4715 _refine_ls_number_restraints 22 _refine_ls_restrained_S_all 1.156 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0349 _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^)+(0.0522P)^2^+1.5232P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0967 _refine_ls_wR_factor_ref 0.1036 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3960 _reflns_number_total 4715 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_j_ncrs-2023-0123_suppl.cif _cod_data_source_block 1_a _cod_database_code 8107513 _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_res_file ; 1_a.res created by SHELXL-2014/7 TITL 1_a.res in P2(1)/c REM Old TITL 1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.137, Rweak 0.003, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C20 N3 O7 S2 Mn REM 1_a.res in P2(1)/c REM 304 parameters refined using 3 restraints REM Highest difference peak 2.512, deepest hole -1.220, 1-sigma level 0.137 REM 299 parameters refined using 3 restraints REM 300 parameters refined using 8 restraints REM Highest difference peak 2.540, deepest hole -1.218, 1-sigma level 0.140 REM 305 parameters refined using 8 restraints REM Highest difference peak 2.492, deepest hole -1.230, 1-sigma level 0.135 REM Highest difference peak 2.464, deepest hole -1.229, 1-sigma level 0.134 REM 308 parameters refined using 12 restraints REM Highest difference peak 1.528, deepest hole -0.652, 1-sigma level 0.075 CELL 0.71073 14.5437 9.6358 17.0874 90 96.664 90 ZERR 4 0.0062 0.004 0.007 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Mn N O S UNIT 84 88 4 8 28 8 EQIV $1 1-X,2-Y,1-Z EQIV $2 1-X,1-Y,1-Z DFIX 0.85 0.01 O5 H5 SADI S2 C18 S1 C3 S1A C5 SADI S2 C19 S1 C4 S1A C4A SADI C18 C19 C4A C5 C4 C3 SADI C19 C20 C4 C5 C4A C3 DANG 1.868878 0.02 C21 H5 DANG 2.704932 0.02 Mn1 H5 DELU 0.001 0.001 S2 C19 SIMU 0.001 0.002 2 S2 C19 L.S. 20 PLAN 20 SIZE 0.3 0.2 0.2 TEMP 0 HTAB O6 O4_$1 HTAB O6 O4 HTAB O7 O3 HTAB O7 O3_$2 GRID BOND $H fmap 2 acta MERG 2 REM REM REM WGHT 0.052200 1.523200 FVAR 0.37353 0.62390 MN1 3 0.674224 0.754839 0.412598 11.00000 0.02840 0.03000 = 0.02552 -0.00306 0.00366 -0.00061 PART 1 S1 6 1.015307 0.882807 0.721381 21.00000 0.04269 0.04790 = 0.04646 -0.01106 -0.01168 0.00662 PART 0 S2 6 0.101122 0.609189 0.428443 11.00000 0.03668 0.08615 = 0.06864 0.01680 -0.00496 -0.01109 PART 2 S1A 6 0.936864 0.764813 0.751850 -21.00000 0.05014 0.04404 = 0.03788 -0.00221 -0.00269 0.00471 PART 0 O1 5 0.774924 0.755332 0.512290 11.00000 0.03650 0.04883 = 0.03675 0.00221 -0.00456 -0.01158 O2 5 0.889937 0.876778 0.469888 11.00000 0.03483 0.06378 = 0.04485 0.00725 0.00597 -0.00698 O3 5 0.410714 0.628127 0.443107 11.00000 0.02918 0.03107 = 0.07937 0.00744 0.00447 0.00430 O4 5 0.396654 0.856337 0.455269 11.00000 0.04124 0.02972 = 0.05211 -0.00651 0.00341 -0.00815 O5 5 0.753437 0.920490 0.359443 11.00000 0.04746 0.05396 = 0.06810 0.02408 -0.00355 -0.01249 AFIX 3 H5 2 0.808227 0.928760 0.384133 11.00000 -1.50000 AFIX 0 O6 5 0.579211 0.908354 0.450503 11.00000 0.03858 0.03820 = 0.05240 -0.01725 0.01219 -0.00309 AFIX 3 H6A 2 0.606511 0.955414 0.488513 11.00000 -1.50000 H6B 2 0.532521 0.867374 0.465733 11.00000 -1.50000 AFIX 0 O7 5 0.591591 0.595237 0.456520 11.00000 0.02847 0.04190 = 0.06157 0.01544 0.00486 -0.00218 AFIX 3 H7A 2 0.609651 0.528397 0.488240 11.00000 -1.50000 H7B 2 0.531901 0.594377 0.448800 11.00000 -1.50000 AFIX 0 N1 4 0.742560 0.599038 0.340769 11.00000 0.03482 0.03390 = 0.02835 -0.00005 0.00459 0.00473 N2 4 0.589762 0.745163 0.291087 11.00000 0.03647 0.04240 = 0.02776 -0.00365 0.00045 0.00950 C1 1 0.852791 0.815464 0.522434 11.00000 0.02779 0.03278 = 0.03797 -0.00463 0.00157 0.00318 C2 1 0.901391 0.815262 0.603937 11.00000 0.03121 0.03019 = 0.03966 -0.00661 0.00001 0.00451 C3 1 0.979249 0.893715 0.626519 11.00000 0.03383 0.04163 = 0.04776 -0.00442 -0.00159 -0.00039 AFIX 3 H3 2 1.008849 0.947695 0.591909 11.00000 -1.20000 AFIX 0 PART 1 C4 1 0.931088 0.770919 0.736281 21.00000 0.08960 0.05275 = 0.05058 0.00253 0.01233 0.02355 AFIX 43 H4 2 0.924182 0.731964 0.785052 21.00000 -1.20000 AFIX 0 PART 0 C5 1 0.872152 0.742228 0.667501 11.00000 0.04434 0.03569 = 0.04286 -0.00428 0.00106 -0.00149 AFIX 3 H5A 2 0.820672 0.684258 0.662861 11.00000 -1.20000 AFIX 0 C6 1 0.813433 0.518968 0.370324 11.00000 0.04284 0.04649 = 0.03587 0.00255 0.00212 0.01103 AFIX 43 H6 2 0.838685 0.532751 0.422276 11.00000 -1.20000 AFIX 0 C7 1 0.850473 0.417106 0.327018 11.00000 0.04681 0.04266 = 0.05580 0.00248 0.00519 0.01694 AFIX 43 H7 2 0.899909 0.363400 0.349174 11.00000 -1.20000 AFIX 0 C8 1 0.812970 0.396436 0.250512 11.00000 0.05427 0.03764 = 0.05237 -0.01235 0.00969 0.01116 AFIX 43 H8 2 0.836449 0.327798 0.220119 11.00000 -1.20000 AFIX 0 C9 1 0.740483 0.477939 0.219196 11.00000 0.04667 0.03953 = 0.03683 -0.01025 0.00457 0.00336 AFIX 43 H9 2 0.714502 0.465311 0.167345 11.00000 -1.20000 AFIX 0 C10 1 0.706296 0.579628 0.265840 11.00000 0.03056 0.02815 = 0.02992 -0.00171 0.00681 -0.00167 C11 1 0.628004 0.671597 0.236252 11.00000 0.03258 0.03072 = 0.02785 -0.00189 0.00378 -0.00094 C12 1 0.596161 0.682226 0.157254 11.00000 0.05801 0.06539 = 0.02916 -0.00756 0.00065 0.01731 AFIX 43 H12 2 0.624404 0.632193 0.120093 11.00000 -1.20000 AFIX 0 C13 1 0.522384 0.767369 0.134036 11.00000 0.06775 0.07950 = 0.03138 0.00116 -0.00907 0.02224 AFIX 43 H13 2 0.500002 0.775543 0.081003 11.00000 -1.20000 AFIX 0 C14 1 0.482194 0.839998 0.189750 11.00000 0.05915 0.06994 = 0.04383 0.00011 -0.00822 0.03076 AFIX 43 H14 2 0.431687 0.897500 0.175402 11.00000 -1.20000 AFIX 0 C15 1 0.517882 0.826367 0.267334 11.00000 0.05318 0.06454 = 0.03828 -0.00906 -0.00196 0.02822 AFIX 43 H15 2 0.490535 0.876241 0.305089 11.00000 -1.20000 AFIX 0 C16 1 0.363643 0.735807 0.448593 11.00000 0.03147 0.02769 = 0.03030 0.00166 -0.00179 -0.00005 C17 1 0.261383 0.717962 0.446159 11.00000 0.02948 0.03075 = 0.02982 0.00450 0.00122 0.00193 C18 1 0.217660 0.596375 0.426055 11.00000 0.03160 0.03906 = 0.05794 -0.00027 -0.00415 -0.00365 AFIX 43 H18 2 0.247608 0.516024 0.412639 11.00000 -1.20000 AFIX 0 C19 1 0.106153 0.775062 0.455845 11.00000 0.03001 0.08171 = 0.05937 0.01754 0.00762 0.01539 AFIX 43 H19 2 0.055378 0.828879 0.464927 11.00000 -1.20000 AFIX 0 C20 1 0.198798 0.822262 0.463310 11.00000 0.04638 0.04253 = 0.05578 0.00061 0.01372 0.01040 AFIX 43 H20 2 0.216491 0.912212 0.477926 11.00000 -1.20000 AFIX 0 C21 1 0.731702 1.047663 0.323710 11.00000 0.07932 0.07208 = 0.10743 0.04475 -0.00366 -0.01076 AFIX 137 H21A 2 0.666822 1.050361 0.305230 11.00000 -1.50000 H21B 2 0.766896 1.059647 0.280010 11.00000 -1.50000 H21C 2 0.746366 1.120869 0.361193 11.00000 -1.50000 AFIX 0 PART 2 C4A 1 1.007457 0.872752 0.708825 -21.00000 0.04212 0.07719 = 0.11337 -0.04631 -0.01422 0.00126 AFIX 43 H4A 2 1.059438 0.914420 0.735845 -21.00000 -1.20000 AFIX 0 HKLF 4 REM 1_a.res in P2(1)/c REM R1 = 0.0349 for 3960 Fo > 4sig(Fo) and 0.0434 for all 4715 data REM 318 parameters refined using 22 restraints END WGHT 0.0522 1.5227 REM Highest difference peak 0.836, deepest hole -0.589, 1-sigma level 0.053 Q1 1 0.0855 0.7570 0.4460 11.00000 0.05 0.84 Q2 1 0.5839 1.0015 0.4683 11.00000 0.05 0.30 Q3 1 0.5162 0.9098 0.4424 11.00000 0.05 0.27 Q4 1 0.7170 0.5238 0.2470 11.00000 0.05 0.26 Q5 1 0.1681 0.5978 0.4247 11.00000 0.05 0.25 Q6 1 0.8868 0.8066 0.5670 11.00000 0.05 0.24 Q7 1 0.6622 0.6176 0.2522 11.00000 0.05 0.23 Q8 1 0.7437 0.7576 0.4627 11.00000 0.05 0.22 Q9 1 0.8906 0.7715 0.6192 11.00000 0.05 0.22 Q10 1 0.4005 0.6568 0.4801 11.00000 0.05 0.21 Q11 1 0.3083 0.7329 0.4437 11.00000 0.05 0.20 Q12 1 0.8840 0.8212 0.4849 11.00000 0.05 0.20 Q13 1 0.7362 0.6037 0.2995 11.00000 0.05 0.20 Q14 1 0.6200 0.7359 0.2626 11.00000 0.05 0.20 Q15 1 0.6975 1.0121 0.2688 11.00000 0.05 0.20 Q16 1 0.5986 0.6378 0.4992 11.00000 0.05 0.18 Q17 1 0.9172 0.8637 0.6140 11.00000 0.05 0.18 Q18 1 0.4857 0.8011 0.2354 11.00000 0.05 0.18 Q19 1 0.8060 0.3912 0.3025 11.00000 0.05 0.18 Q20 1 0.6212 0.7456 0.3410 11.00000 0.05 0.18 ; _shelx_res_checksum 79336 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Mn1 Mn 0.67422(2) 0.75484(3) 0.41260(2) 0.02793(11) Uani 1 1 d D . . . . S1 S 1.0153(2) 0.8828(3) 0.72138(19) 0.0470(5) Uani 0.624(5) 1 d D . P A 1 S2 S 0.10112(5) 0.60919(9) 0.42844(5) 0.0647(2) Uani 1 1 d D U . . . S1A S 0.9369(4) 0.7648(7) 0.7518(4) 0.0446(8) Uani 0.376(5) 1 d D . P A 2 O1 O 0.77492(11) 0.75533(16) 0.51229(9) 0.0414(4) Uani 1 1 d . . . . . O2 O 0.88994(11) 0.87678(19) 0.46989(9) 0.0477(4) Uani 1 1 d . . . . . O3 O 0.41071(10) 0.62813(16) 0.44311(11) 0.0467(4) Uani 1 1 d . . . . . O4 O 0.39665(11) 0.85634(16) 0.45527(9) 0.0412(4) Uani 1 1 d . . . . . O5 O 0.75344(12) 0.92049(19) 0.35944(11) 0.0573(5) Uani 1 1 d D . . . . H5 H 0.8082 0.9288 0.3841 0.086 Uiso 1 1 d DR . . . . O6 O 0.57921(11) 0.90835(16) 0.45050(9) 0.0425(4) Uani 1 1 d . . . . . H6A H 0.6065 0.9554 0.4885 0.064 Uiso 1 1 d R . . . . H6B H 0.5325 0.8674 0.4657 0.064 Uiso 1 1 d R . . . . O7 O 0.59159(10) 0.59524(17) 0.45652(10) 0.0440(4) Uani 1 1 d . . . . . H7A H 0.6097 0.5284 0.4882 0.066 Uiso 1 1 d R . . . . H7B H 0.5319 0.5944 0.4488 0.066 Uiso 1 1 d R . . . . N1 N 0.74256(12) 0.59904(18) 0.34077(10) 0.0323(4) Uani 1 1 d . . . . . N2 N 0.58976(13) 0.74516(19) 0.29109(10) 0.0358(4) Uani 1 1 d . . . . . C1 C 0.85279(14) 0.8155(2) 0.52243(12) 0.0330(4) Uani 1 1 d . . . . . C2 C 0.90139(14) 0.8153(2) 0.60394(13) 0.0340(5) Uani 1 1 d . . . . . C3 C 0.97925(16) 0.8937(2) 0.62652(14) 0.0416(5) Uani 1 1 d D . . . . H3 H 1.0088 0.9477 0.5919 0.050 Uiso 1 1 d R . . A . C4 C 0.9311(10) 0.7709(16) 0.7363(7) 0.064(6) Uani 0.624(5) 1 d D . P A 1 H4 H 0.9242 0.7320 0.7851 0.077 Uiso 0.624(5) 1 calc R . P A 1 C5 C 0.87215(17) 0.7422(2) 0.66750(14) 0.0413(5) Uani 1 1 d D . . . . H5A H 0.8207 0.6843 0.6629 0.050 Uiso 1 1 d R . . A . C6 C 0.81343(16) 0.5190(2) 0.37032(13) 0.0419(5) Uani 1 1 d . . . . . H6 H 0.8387 0.5328 0.4223 0.050 Uiso 1 1 calc R . . . . C7 C 0.85047(18) 0.4171(3) 0.32702(15) 0.0485(6) Uani 1 1 d . . . . . H7 H 0.8999 0.3634 0.3492 0.058 Uiso 1 1 calc R . . . . C8 C 0.81297(18) 0.3964(3) 0.25051(15) 0.0478(6) Uani 1 1 d . . . . . H8 H 0.8364 0.3278 0.2201 0.057 Uiso 1 1 calc R . . . . C9 C 0.74048(16) 0.4779(2) 0.21920(13) 0.0410(5) Uani 1 1 d . . . . . H9 H 0.7145 0.4653 0.1673 0.049 Uiso 1 1 calc R . . . . C10 C 0.70630(14) 0.5796(2) 0.26584(11) 0.0293(4) Uani 1 1 d . . . . . C11 C 0.62800(14) 0.6716(2) 0.23625(11) 0.0304(4) Uani 1 1 d . . . . . C12 C 0.59616(19) 0.6822(3) 0.15725(13) 0.0512(6) Uani 1 1 d . . . . . H12 H 0.6244 0.6322 0.1201 0.061 Uiso 1 1 calc R . . . . C13 C 0.5224(2) 0.7674(3) 0.13404(15) 0.0607(8) Uani 1 1 d . . . . . H13 H 0.5000 0.7755 0.0810 0.073 Uiso 1 1 calc R . . . . C14 C 0.4822(2) 0.8400(3) 0.18975(15) 0.0588(7) Uani 1 1 d . . . . . H14 H 0.4317 0.8975 0.1754 0.071 Uiso 1 1 calc R . . . . C15 C 0.51788(18) 0.8264(3) 0.26733(14) 0.0526(7) Uani 1 1 d . . . . . H15 H 0.4905 0.8762 0.3051 0.063 Uiso 1 1 calc R . . . . C16 C 0.36364(14) 0.7358(2) 0.44859(12) 0.0302(4) Uani 1 1 d . . . . . C17 C 0.26138(14) 0.7180(2) 0.44616(12) 0.0302(4) Uani 1 1 d . . . . . C18 C 0.21766(15) 0.5964(2) 0.42606(14) 0.0436(5) Uani 1 1 d D . . . . H18 H 0.2476 0.5160 0.4126 0.052 Uiso 1 1 calc R . . . . C19 C 0.10615(17) 0.7751(3) 0.45584(17) 0.0568(4) Uani 1 1 d D U . . . H19 H 0.0554 0.8289 0.4649 0.068 Uiso 1 1 calc R . . . . C20 C 0.19880(17) 0.8223(3) 0.46331(15) 0.0476(6) Uani 1 1 d D . . . . H20 H 0.2165 0.9122 0.4779 0.057 Uiso 1 1 calc R . . . . C21 C 0.7317(3) 1.0477(4) 0.3237(2) 0.0874(11) Uani 1 1 d D . . . . H21A H 0.6668 1.0504 0.3052 0.131 Uiso 1 1 calc GR . . . . H21B H 0.7669 1.0596 0.2800 0.131 Uiso 1 1 calc GR . . . . H21C H 0.7464 1.1209 0.3612 0.131 Uiso 1 1 calc GR . . . . C4A C 1.0075(13) 0.873(2) 0.7088(9) 0.079(10) Uani 0.376(5) 1 d D . P A 2 H4A H 1.0594 0.9144 0.7358 0.095 Uiso 0.376(5) 1 calc R . P A 2 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 0.02840(18) 0.03000(18) 0.02552(17) -0.00306(12) 0.00366(12) -0.00061(12) S1 0.0427(10) 0.0479(10) 0.0465(7) -0.0111(7) -0.0117(6) 0.0066(7) S2 0.0367(3) 0.0862(6) 0.0686(5) 0.0168(4) -0.0050(3) -0.0111(3) S1A 0.0501(16) 0.0440(17) 0.0379(17) -0.0022(11) -0.0027(10) 0.0047(12) O1 0.0365(9) 0.0488(10) 0.0367(8) 0.0022(7) -0.0046(7) -0.0116(7) O2 0.0348(8) 0.0638(11) 0.0449(9) 0.0072(8) 0.0060(7) -0.0070(8) O3 0.0292(8) 0.0311(8) 0.0794(12) 0.0074(8) 0.0045(8) 0.0043(6) O4 0.0412(9) 0.0297(8) 0.0521(9) -0.0065(7) 0.0034(7) -0.0082(7) O5 0.0475(10) 0.0540(11) 0.0681(12) 0.0241(9) -0.0036(8) -0.0125(8) O6 0.0386(8) 0.0382(9) 0.0524(9) -0.0172(7) 0.0122(7) -0.0031(7) O7 0.0285(8) 0.0419(9) 0.0616(10) 0.0154(8) 0.0049(7) -0.0022(7) N1 0.0348(9) 0.0339(9) 0.0284(8) -0.0001(7) 0.0046(7) 0.0047(7) N2 0.0365(10) 0.0424(11) 0.0278(9) -0.0036(7) 0.0005(7) 0.0095(8) C1 0.0278(10) 0.0328(11) 0.0380(11) -0.0046(9) 0.0016(8) 0.0032(8) C2 0.0312(11) 0.0302(11) 0.0397(11) -0.0066(9) 0.0000(9) 0.0045(8) C3 0.0338(12) 0.0416(13) 0.0478(13) -0.0044(10) -0.0016(10) -0.0004(9) C4 0.090(9) 0.053(5) 0.051(8) 0.003(4) 0.012(5) 0.024(5) C5 0.0443(13) 0.0357(12) 0.0429(13) -0.0043(10) 0.0011(10) -0.0015(10) C6 0.0428(13) 0.0465(13) 0.0359(11) 0.0026(10) 0.0021(9) 0.0110(10) C7 0.0468(14) 0.0427(13) 0.0558(15) 0.0025(11) 0.0052(11) 0.0169(11) C8 0.0543(15) 0.0376(13) 0.0524(14) -0.0124(11) 0.0097(11) 0.0112(11) C9 0.0467(13) 0.0395(12) 0.0368(11) -0.0103(10) 0.0046(10) 0.0034(10) C10 0.0306(10) 0.0281(10) 0.0299(10) -0.0017(8) 0.0068(8) -0.0017(8) C11 0.0326(10) 0.0307(11) 0.0279(10) -0.0019(8) 0.0038(8) -0.0009(8) C12 0.0580(16) 0.0654(17) 0.0292(11) -0.0076(11) 0.0006(10) 0.0173(13) C13 0.0678(19) 0.079(2) 0.0314(12) 0.0012(12) -0.0091(12) 0.0222(15) C14 0.0592(17) 0.0699(19) 0.0438(14) 0.0001(13) -0.0082(12) 0.0308(14) C15 0.0532(15) 0.0645(17) 0.0383(13) -0.0091(12) -0.0020(11) 0.0282(13) C16 0.0315(10) 0.0277(10) 0.0303(10) 0.0017(8) -0.0018(8) 0.0000(8) C17 0.0295(10) 0.0307(10) 0.0298(10) 0.0045(8) 0.0012(8) 0.0019(8) C18 0.0316(11) 0.0391(13) 0.0579(14) -0.0003(11) -0.0042(10) -0.0036(10) C19 0.0300(8) 0.0817(9) 0.0594(9) 0.0175(8) 0.0076(8) 0.0154(8) C20 0.0464(14) 0.0425(14) 0.0558(15) 0.0006(11) 0.0137(11) 0.0104(11) C21 0.079(2) 0.072(2) 0.107(3) 0.045(2) -0.004(2) -0.0108(18) C4A 0.042(8) 0.077(12) 0.11(2) -0.046(10) -0.014(8) 0.001(6) 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' 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' S S 0.1246 0.1234 '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 O1 Mn1 O5 89.10(7) . . O1 Mn1 O6 99.40(7) . . O1 Mn1 O7 94.80(7) . . O1 Mn1 N1 97.64(7) . . O1 Mn1 N2 168.55(7) . . O5 Mn1 N1 88.48(8) . . O5 Mn1 N2 84.70(7) . . O6 Mn1 O5 90.61(8) . . O6 Mn1 N1 162.92(6) . . O6 Mn1 N2 90.30(6) . . O7 Mn1 O5 176.09(6) . . O7 Mn1 O6 88.98(7) . . O7 Mn1 N1 90.77(7) . . O7 Mn1 N2 91.42(7) . . N1 Mn1 N2 72.63(7) . . C3 S1 C4 92.0(5) . . C19 S2 C18 93.72(12) . . C5 S1A C4A 90.9(6) . . C1 O1 Mn1 129.53(14) . . Mn1 O5 H5 111.1 . . C21 O5 Mn1 135.3(2) . . C21 O5 H5 106.5 . . Mn1 O6 H6A 109.5 . . Mn1 O6 H6B 109.4 . . H6A O6 H6B 109.4 . . Mn1 O7 H7A 127.9 . . Mn1 O7 H7B 123.3 . . H7A O7 H7B 108.4 . . C6 N1 Mn1 123.37(14) . . C6 N1 C10 118.72(18) . . C10 N1 Mn1 117.77(13) . . C11 N2 Mn1 115.56(14) . . C15 N2 Mn1 124.94(15) . . C15 N2 C11 118.09(19) . . O1 C1 C2 116.62(19) . . O2 C1 O1 124.9(2) . . O2 C1 C2 118.41(19) . . C3 C2 C1 123.2(2) . . C3 C2 C5 111.8(2) . . C5 C2 C1 124.9(2) . . S1 C3 H3 122.9 . . C2 C3 S1 113.4(2) . . C2 C3 H3 123.7 . . C2 C3 C4A 109.2(6) . . C4A C3 H3 127.0 . . S1 C4 H4 123.6 . . C5 C4 S1 112.8(8) . . C5 C4 H4 123.6 . . S1A C5 H5A 121.9 . . C2 C5 S1A 114.8(2) . . C2 C5 H5A 123.3 . . C4 C5 C2 109.9(5) . . C4 C5 H5A 126.8 . . N1 C6 H6 118.6 . . N1 C6 C7 122.7(2) . . C7 C6 H6 118.6 . . C6 C7 H7 120.7 . . C8 C7 C6 118.6(2) . . C8 C7 H7 120.7 . . C7 C8 H8 120.3 . . C7 C8 C9 119.4(2) . . C9 C8 H8 120.3 . . C8 C9 H9 120.4 . . C8 C9 C10 119.3(2) . . C10 C9 H9 120.4 . . N1 C10 C9 121.24(19) . . N1 C10 C11 116.32(17) . . C9 C10 C11 122.44(18) . . N2 C11 C10 116.10(17) . . N2 C11 C12 121.6(2) . . C12 C11 C10 122.33(19) . . C11 C12 H12 120.3 . . C13 C12 C11 119.3(2) . . C13 C12 H12 120.3 . . C12 C13 H13 120.4 . . C14 C13 C12 119.2(2) . . C14 C13 H13 120.4 . . C13 C14 H14 120.7 . . C13 C14 C15 118.7(2) . . C15 C14 H14 120.7 . . N2 C15 C14 123.1(2) . . N2 C15 H15 118.4 . . C14 C15 H15 118.4 . . O3 C16 O4 124.5(2) . . O3 C16 C17 116.99(18) . . O4 C16 C17 118.54(18) . . C18 C17 C16 122.83(19) . . C18 C17 C20 111.9(2) . . C20 C17 C16 125.3(2) . . S2 C18 H18 124.2 . . C17 C18 S2 111.66(18) . . C17 C18 H18 124.2 . . S2 C19 H19 124.9 . . C20 C19 S2 110.2(2) . . C20 C19 H19 124.9 . . C17 C20 C19 112.6(2) . . C17 C20 H20 123.7 . . C19 C20 H20 123.7 . . O5 C21 H21A 109.5 . . O5 C21 H21B 109.5 . . O5 C21 H21C 109.5 . . H21A C21 H21B 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . S1A C4A H4A 123.4 . . C3 C4A S1A 113.3(9) . . C3 C4A H4A 123.4 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mn1 O1 2.1137(17) . Mn1 O5 2.2232(18) . Mn1 O6 2.1737(16) . Mn1 O7 2.1406(16) . Mn1 N1 2.2430(18) . Mn1 N2 2.2884(19) . S1 C3 1.648(4) . S1 C4 1.673(11) . S2 C18 1.705(2) . S2 C19 1.665(3) . S1A C5 1.642(7) . S1A C4A 1.689(13) . O1 C1 1.266(3) . O2 C1 1.249(3) . O3 C16 1.253(3) . O4 C16 1.257(2) . O5 H5 0.8610 . O5 C21 1.389(4) . O6 H6A 0.8516 . O6 H6B 0.8519 . O7 H7A 0.8629 . O7 H7B 0.8629 . N1 C6 1.339(3) . N1 C10 1.340(3) . N2 C11 1.346(3) . N2 C15 1.331(3) . C1 C2 1.487(3) . C2 C3 1.379(3) . C2 C5 1.401(3) . C3 H3 0.9299 . C3 C4A 1.433(14) . C4 H4 0.9300 . C4 C5 1.400(12) . C5 H5A 0.9301 . C6 H6 0.9300 . C6 C7 1.376(3) . C7 H7 0.9300 . C7 C8 1.371(4) . C8 H8 0.9300 . C8 C9 1.372(3) . C9 H9 0.9300 . C9 C10 1.391(3) . C10 C11 1.485(3) . C11 C12 1.379(3) . C12 H12 0.9300 . C12 C13 1.372(4) . C13 H13 0.9300 . C13 C14 1.366(4) . C14 H14 0.9300 . C14 C15 1.373(3) . C15 H15 0.9300 . C16 C17 1.493(3) . C17 C18 1.358(3) . C17 C20 1.409(3) . C18 H18 0.9300 . C19 H19 0.9300 . C19 C20 1.414(4) . C20 H20 0.9300 . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 . C4A H4A 0.9300 .