#------------------------------------------------------------------------------ #$Date: 2021-11-03 23:18:52 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270258 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/91/4519118.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_4519118 loop_ _publ_author_name 'Alanazi, Abdulaziz M.' 'McNaughter, Paul D.' 'Alam, Firoz' 'Vitorica-Yrezabal, Inigo J' 'Whitehead, George F. S.' 'Tuna, Floriana' 'O'Brien, Paul' 'Collison, David' 'Lewis, David J.' _publ_section_title ; Structural Investigations of \a-MnS Nanocrystals and Thin Films Synthesized from Manganese(II) Xanthates by Hot Injection, Solvent-Less Thermolysis, and Doctor Blade Routes. ; _journal_issue 42 _journal_name_full 'ACS omega' _journal_page_first 27716 _journal_page_last 27725 _journal_paper_doi 10.1021/acsomega.1c02907 _journal_volume 6 _journal_year 2021 _chemical_formula_sum 'C14 H30 Mn N2 O2 S4' _chemical_formula_weight 441.58 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 106.751(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8338(5) _cell_length_b 11.9042(4) _cell_length_c 15.5003(6) _cell_measurement_reflns_used 4421 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 72.06 _cell_measurement_theta_min 5.39 _cell_volume 2090.90(14) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 16722 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.180 _diffrn_reflns_theta_min 4.762 _exptl_absorpt_coefficient_mu 8.936 _exptl_absorpt_correction_T_max 0.616 _exptl_absorpt_correction_T_min 0.468703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.403 _exptl_crystal_description block _exptl_crystal_F_000 932 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.339 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 214 _refine_ls_number_reflns 4099 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0282 _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^)+(0.0306P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.0660 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3538 _reflns_number_total 4099 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao1c02907_si_003.cif _cod_data_source_block s4606ma _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4519118 _shelx_shelxl_version_number 2014/7 _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 0.223 _shelx_estimated_absorpt_t_max 0.616 _shelx_res_file ; s4606ma.res created by SHELXL-2014/7 TITL s4606ma in P2(1)/c CELL 1.54178 11.8338 11.9042 15.5003 90.000 106.751 90.000 ZERR 4.00 0.0005 0.0004 0.0006 0.000 0.002 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O S Mn UNIT 56 120 8 8 16 4 L.S. 16 ACTA BOND $H FMAP 2 PLAN 0 HTAB C14 S1 HTAB C13 S3_$1 EQIV $1 -x+1, y-1/2, -z+1/2 HTAB C13 S3 HTAB C11 S3 SIZE 0.060 0.130 0.240 CONF HTAB TEMP -173.000 WGHT 0.030600 FVAR 0.11704 C1 1 1.010978 0.694969 0.161102 11.00000 0.01088 0.01504 = 0.00829 0.00094 0.00176 -0.00070 C2 1 1.156635 0.608781 0.102032 11.00000 0.01358 0.01338 = 0.01521 -0.00126 0.00646 0.00048 AFIX 23 H2A 2 1.100019 0.575258 0.048302 11.00000 -1.20000 H2B 2 1.176391 0.551787 0.150593 11.00000 -1.20000 AFIX 0 C3 1 1.267182 0.646308 0.079651 11.00000 0.01449 0.01757 = 0.02456 -0.00037 0.01133 -0.00145 AFIX 23 H3A 2 1.322232 0.681719 0.133238 11.00000 -1.20000 H3B 2 1.246470 0.702752 0.030698 11.00000 -1.20000 AFIX 0 C4 1 1.326749 0.545863 0.050157 11.00000 0.01513 0.01976 = 0.02214 -0.00248 0.00884 0.00029 AFIX 137 H4A 2 1.352056 0.492523 0.100189 11.00000 -1.50000 H4B 2 1.395621 0.571483 0.032522 11.00000 -1.50000 H4C 2 1.270885 0.508974 -0.001210 11.00000 -1.50000 AFIX 0 C5 1 0.582854 0.801899 0.112175 11.00000 0.01160 0.01328 = 0.01368 0.00244 0.00300 0.00110 C6 1 0.437671 0.841071 -0.028169 11.00000 0.01534 0.02089 = 0.01087 0.00046 0.00190 0.00282 AFIX 23 H6A 2 0.418819 0.760466 -0.039885 11.00000 -1.20000 H6B 2 0.495323 0.863066 -0.060401 11.00000 -1.20000 AFIX 0 C7 1 0.326967 0.910669 -0.060953 11.00000 0.01400 0.01597 = 0.01346 0.00126 0.00224 0.00183 AFIX 23 H7A 2 0.346511 0.991173 -0.049401 11.00000 -1.20000 H7B 2 0.270385 0.889371 -0.027569 11.00000 -1.20000 AFIX 0 C8 1 0.270574 0.892049 -0.161807 11.00000 0.01741 0.02688 = 0.01567 0.00197 0.00051 0.00053 AFIX 137 H8A 2 0.327593 0.910920 -0.194534 11.00000 -1.50000 H8B 2 0.200816 0.940140 -0.182857 11.00000 -1.50000 H8C 2 0.247162 0.813150 -0.172684 11.00000 -1.50000 AFIX 0 C9 1 0.810464 0.604580 0.414658 11.00000 0.02152 0.02009 = 0.01109 0.00099 0.00605 -0.00103 AFIX 23 H9A 2 0.737270 0.641890 0.418430 11.00000 -1.20000 H9B 2 0.856509 0.582396 0.476326 11.00000 -1.20000 AFIX 0 C10 1 0.778964 0.500556 0.355831 11.00000 0.02485 0.01601 = 0.01499 0.00352 0.00608 -0.00159 AFIX 23 H10A 2 0.852204 0.462808 0.352658 11.00000 -1.20000 H10B 2 0.734709 0.447441 0.383088 11.00000 -1.20000 AFIX 0 C11 1 0.875645 0.797159 0.415744 11.00000 0.02044 0.01816 = 0.01349 -0.00487 0.00133 0.00204 AFIX 137 H11A 2 0.793521 0.822760 0.400173 11.00000 -1.50000 H11B 2 0.922069 0.849642 0.391018 11.00000 -1.50000 H11C 2 0.908255 0.794020 0.481428 11.00000 -1.50000 AFIX 0 C12 1 1.005186 0.647958 0.402717 11.00000 0.01527 0.02543 = 0.01473 0.00062 0.00055 0.00439 AFIX 137 H12A 2 1.037503 0.648889 0.468468 11.00000 -1.50000 H12B 2 1.050509 0.699441 0.376136 11.00000 -1.50000 H12C 2 1.010297 0.571694 0.380327 11.00000 -1.50000 AFIX 0 C13 1 0.584368 0.557781 0.264115 11.00000 0.01610 0.02513 = 0.02954 0.00370 0.00925 -0.00450 AFIX 137 H13A 2 0.536521 0.575845 0.202780 11.00000 -1.50000 H13B 2 0.585978 0.622559 0.303469 11.00000 -1.50000 H13C 2 0.549989 0.493096 0.286514 11.00000 -1.50000 AFIX 0 C14 1 0.700415 0.431908 0.204652 11.00000 0.03534 0.01514 = 0.02315 -0.00450 0.01276 -0.00902 AFIX 137 H14A 2 0.780409 0.410385 0.204813 11.00000 -1.50000 H14B 2 0.653910 0.450740 0.143112 11.00000 -1.50000 H14C 2 0.663054 0.369164 0.226916 11.00000 -1.50000 AFIX 0 MN1 6 0.796929 0.684671 0.222877 11.00000 0.00952 0.01031 = 0.00924 0.00063 0.00268 0.00061 N1 3 0.880314 0.683947 0.377395 11.00000 0.01257 0.01519 = 0.01157 -0.00007 0.00287 0.00042 N2 3 0.706237 0.530332 0.263484 11.00000 0.01505 0.01405 = 0.01452 -0.00116 0.00574 -0.00162 O1 4 1.105315 0.707740 0.131269 11.00000 0.01361 0.01223 = 0.01797 -0.00142 0.00824 -0.00115 O2 4 0.487299 0.860135 0.067968 11.00000 0.01241 0.01787 = 0.01255 -0.00061 0.00063 0.00495 S1 5 0.949175 0.567884 0.166306 11.00000 0.01232 0.01016 = 0.01477 0.00027 0.00536 -0.00078 S2 5 0.957627 0.815807 0.192886 11.00000 0.01637 0.01017 = 0.01887 -0.00168 0.00840 -0.00067 S3 5 0.638540 0.834363 0.223231 11.00000 0.01769 0.01729 = 0.01139 -0.00217 0.00066 0.00637 S4 5 0.644937 0.703772 0.061675 11.00000 0.01477 0.01762 = 0.01172 -0.00158 0.00231 0.00475 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM s4606ma in P2(1)/c REM R1 = 0.0282 for 3538 Fo > 4sig(Fo) and 0.0356 for all 4099 data REM 214 parameters refined using 0 restraints END WGHT 0.0303 0.0000 REM Instructions for potential hydrogen bonds HTAB C11 S3 HTAB C13 S3 HTAB C13 S3_$1 HTAB C14 S1 REM Highest difference peak 0.339, deepest hole -0.242, 1-sigma level 0.061 Q1 1 0.6002 0.8200 0.1671 11.00000 0.05 0.34 Q2 1 0.5980 0.7543 0.0911 11.00000 0.05 0.29 Q3 1 0.8445 0.6899 0.3106 11.00000 0.05 0.28 Q4 1 0.2912 0.9067 -0.1132 11.00000 0.05 0.27 Q5 1 1.2975 0.5934 0.0636 11.00000 0.05 0.27 Q6 1 0.7961 0.5559 0.3853 11.00000 0.05 0.27 Q7 1 0.3857 0.8723 -0.0494 11.00000 0.05 0.26 Q8 1 0.4462 0.9008 0.0848 11.00000 0.05 0.26 Q9 1 0.7184 0.7178 0.0948 11.00000 0.05 0.26 Q10 1 0.6861 0.6635 0.1069 11.00000 0.05 0.26 Q11 1 1.2097 0.6369 0.0885 11.00000 0.05 0.23 Q12 1 0.5426 0.5193 0.1685 11.00000 0.05 0.23 Q13 1 0.9646 0.8223 0.2678 11.00000 0.05 0.22 Q14 1 0.7039 0.7750 0.2084 11.00000 0.05 0.22 Q15 1 0.9772 0.7536 0.1663 11.00000 0.05 0.22 Q16 1 0.7980 0.8173 0.5333 11.00000 0.05 0.21 Q17 1 0.4613 0.8429 0.0173 11.00000 0.05 0.21 Q18 1 0.8820 0.7447 0.2034 11.00000 0.05 0.21 Q19 1 0.8318 0.6454 0.3845 11.00000 0.05 0.21 Q20 1 0.5236 0.8270 0.0915 11.00000 0.05 0.20 ; _shelx_res_checksum 59439 _shelx_hkl_file ; 2 0 0 24.11 0.89 3 0 0 144.20 4.70 4 0 0 0.37 0.21 5 0 0 38.29 1.50 6 0 0 36.02 1.49 7 0 0 95.61 4.02 8 0 0 9.88 1.11 -8 0 0 8.47 1.03 -9 0 0 2.47 1.47 -9 0 0 1.70 0.72 -10 0 0 4.00 1.03 -10 0 0 3.86 0.90 -10 0 0 4.15 1.56 -11 0 0 1.62 0.84 -11 0 0 0.58 1.32 -12 0 0 60.06 4.13 -13 0 0 95.27 5.43 0 -1 0 0.09 0.11 0 -1 0 0.31 0.10 1 -1 0 260.26 9.56 -1 -1 0 278.75 8.59 1 -1 0 274.13 8.60 2 -1 0 3.19 0.27 -2 -1 0 3.45 0.25 2 -1 0 2.41 0.35 -3 -1 0 82.50 2.66 3 -1 0 78.37 3.06 3 -1 0 77.96 2.67 4 -1 0 3.68 0.36 4 -1 0 3.03 0.48 5 -1 0 22.75 1.02 5 -1 0 23.67 1.33 5 1 0 23.82 1.08 6 -1 0 378.60 13.91 6 1 0 375.16 12.43 -6 1 0 397.02 14.48 7 -1 0 23.16 1.45 -7 1 0 20.38 1.51 -8 -1 0 18.72 1.28 8 -1 0 19.63 1.50 -8 1 0 16.44 1.54 8 1 0 18.45 1.48 -9 -1 0 3.02 1.36 -9 -1 0 3.57 0.78 -9 1 0 3.64 1.56 -9 1 0 3.10 1.13 -9 1 0 4.01 0.95 -10 -1 0 1.48 0.70 -10 -1 0 0.62 1.35 -10 -1 0 1.02 0.82 -10 1 0 1.44 0.84 -10 1 0 0.46 0.78 -10 1 0 1.41 1.42 -11 -1 0 6.77 1.09 -11 -1 0 6.55 1.65 -11 1 0 6.61 1.09 -11 1 0 6.20 1.72 -12 -1 0 13.75 1.87 -12 1 0 14.01 2.01 -13 -1 0 70.43 4.31 -13 1 0 75.60 4.38 0 -2 0 204.61 7.46 0 -2 0 215.28 6.73 -1 -2 0 28.71 1.05 1 -2 0 26.33 1.24 1 -2 0 29.87 1.09 2 -2 0 31.03 1.17 -2 -2 0 31.34 1.14 2 -2 0 29.26 1.42 3 -2 0 8.16 0.72 3 -2 0 7.94 0.51 -3 -2 0 7.92 0.48 -3 2 0 8.86 0.87 -4 -2 0 49.37 1.73 4 -2 0 44.84 1.73 4 -2 0 45.79 2.09 -4 2 0 48.43 2.28 5 -2 0 53.09 2.43 -5 -2 0 55.63 2.00 5 -2 0 53.06 2.00 -5 2 0 56.40 2.64 6 -2 0 4.30 0.70 6 2 0 5.22 0.59 -6 2 0 4.80 0.85 7 -2 0 44.66 2.24 -7 2 0 40.38 2.37 8 -2 0 29.84 1.87 -8 2 0 26.74 1.99 -9 -2 0 24.21 1.52 -9 -2 0 25.54 2.62 -9 2 0 22.77 2.57 -9 2 0 30.68 2.12 -9 2 0 23.69 2.03 -10 -2 0 0.05 1.18 -10 -2 0 0.91 0.56 -10 2 0 1.02 0.85 -10 2 0 1.92 1.43 -10 2 0 -0.75 0.77 -11 -2 0 13.73 1.91 -11 2 0 17.70 2.22 -12 -2 0 13.20 1.79 -12 2 0 13.73 1.92 -13 -2 0 28.33 2.19 -13 2 0 29.27 2.28 0 -3 0 -0.08 0.29 0 -3 0 -0.01 0.25 1 -3 0 168.28 6.08 1 -3 0 168.93 5.43 -1 -3 0 158.72 5.40 2 -3 0 52.49 1.95 -2 -3 0 55.06 1.93 2 -3 0 53.90 2.30 -3 -3 0 39.58 1.49 3 -3 0 38.11 1.81 3 -3 0 37.66 1.49 -3 3 0 40.46 2.08 -4 -3 0 -0.01 0.27 4 -3 0 0.01 0.43 4 -3 0 0.59 0.28 -4 3 0 0.18 0.61 -5 -3 0 59.22 2.22 5 -3 0 60.03 2.20 5 -3 0 59.96 2.72 -5 3 0 59.05 2.96 6 -3 0 2.43 0.65 -6 3 0 2.03 0.76 7 -3 0 1.36 0.59 7 3 0 1.32 0.50 -7 3 0 0.88 0.75 8 -3 0 11.10 1.25 -8 3 0 12.81 1.55 -9 -3 0 3.27 0.58 -9 -3 0 4.11 1.45 -9 3 0 5.06 1.12 -9 3 0 5.11 1.50 -9 3 0 2.10 1.02 -10 -3 0 1.21 1.21 -10 -3 0 0.52 0.46 -10 3 0 1.34 0.96 -10 3 0 1.21 1.36 -11 -3 0 0.12 1.04 -11 3 0 1.06 1.30 -12 -3 0 2.98 1.06 -12 3 0 3.69 1.18 13 -3 0 0.62 0.43 -13 3 0 -0.18 0.69 0 -4 0 92.68 3.51 0 -4 0 88.26 3.13 1 -4 0 1.15 0.34 1 -4 0 1.39 0.48 -1 -4 0 1.33 0.34 2 -4 0 4.98 0.67 -2 -4 0 5.20 0.50 2 -4 0 4.80 0.50 3 -4 0 3.54 0.45 3 -4 0 3.12 0.65 -3 -4 0 3.36 0.45 -3 4 0 4.64 0.86 4 -4 0 21.65 1.10 -4 -4 0 24.10 1.11 4 -4 0 22.81 1.43 -4 4 0 23.11 1.74 -5 -4 0 0.33 0.33 5 -4 0 0.78 0.51 -5 4 0 0.17 0.64 6 -4 0 10.55 1.11 -6 -4 0 9.87 0.80 -6 4 0 10.34 1.38 7 -4 0 0.42 0.58 -7 4 0 0.02 0.79 7 4 0 -0.86 0.47 8 -4 0 0.56 0.64 -8 4 0 0.11 0.85 -9 4 0 14.28 2.06 -9 4 0 11.99 1.68 -9 4 0 10.48 0.99 -10 4 0 1.92 1.13 -10 4 0 2.93 1.35 -11 4 0 1.10 1.15 12 -4 0 0.63 0.56 -12 4 0 0.81 0.85 13 -4 0 0.53 0.39 -13 4 0 0.25 0.59 0 -5 0 0.23 0.42 0 -5 0 0.12 0.35 1 -5 0 37.29 1.86 1 -5 0 35.84 1.56 -1 -5 0 37.95 1.57 2 -5 0 -0.67 0.44 -2 -5 0 0.09 0.35 2 -5 0 -0.11 0.31 -3 -5 0 6.38 0.63 3 -5 0 5.21 0.80 3 -5 0 5.78 0.59 4 -5 0 1.68 0.42 4 -5 0 1.81 0.68 -4 -5 0 0.93 0.38 -5 -5 0 73.01 2.80 5 -5 0 78.55 3.42 -5 5 0 68.49 3.75 -6 -5 0 27.51 1.40 6 -5 0 29.10 1.90 -6 5 0 29.71 2.28 7 -5 0 -0.01 0.57 -7 5 0 0.58 0.86 -8 5 0 28.78 2.10 -8 5 0 33.09 2.57 -9 5 0 0.12 0.63 -9 5 0 0.52 1.08 -9 5 0 1.12 1.23 -10 5 0 2.48 1.19 11 -5 0 5.88 0.93 -11 5 0 7.18 1.29 12 -5 0 5.07 0.72 -12 5 0 5.55 1.01 0 -6 0 208.74 6.83 0 -6 0 193.72 7.57 -1 -6 0 1.27 0.44 1 -6 0 0.87 0.47 1 -6 0 0.83 0.55 2 -6 0 3.59 0.77 2 -6 0 3.74 0.57 -2 -6 0 3.62 0.60 3 -6 0 1.23 0.44 3 -6 0 1.33 0.65 -3 -6 0 1.97 0.50 3 -6 0 2.64 0.71 -4 -6 0 1.80 0.48 4 -6 0 1.52 0.65 4 -6 0 1.61 0.42 -5 -6 0 53.12 2.34 5 -6 0 61.43 2.90 -6 -6 0 5.89 0.79 6 -6 0 5.02 0.96 -7 -6 0 36.17 1.80 7 -6 0 35.78 2.19 -7 6 0 31.07 2.58 -8 6 0 17.07 1.72 -9 6 0 16.74 1.58 10 -6 0 4.41 0.91 11 -6 0 9.26 0.97 12 -6 0 22.51 1.42 0 -7 0 -0.33 0.46 0 -7 0 -0.48 0.38 1 -7 0 207.15 7.92 1 -7 0 204.51 7.01 -1 -7 0 202.33 7.03 2 -7 0 1.78 0.69 2 -7 0 1.83 0.52 -2 -7 0 2.01 0.55 -3 -7 0 4.44 0.69 3 -7 0 2.67 0.82 3 -7 0 5.03 0.64 4 -7 0 1.26 0.69 -4 -7 0 1.09 0.51 5 -7 0 0.28 0.69 -5 -7 0 -0.11 0.44 6 -7 0 80.24 4.21 -6 -7 0 79.23 3.22 6 -7 0 80.39 3.83 -7 -7 0 6.79 0.84 7 -7 0 7.69 1.08 -7 7 0 6.33 1.26 -8 -7 0 1.69 0.61 8 -7 0 0.89 0.77 -8 7 0 1.13 0.89 9 -7 0 3.43 0.87 9 -7 0 2.62 1.06 -9 7 0 3.21 0.87 10 -7 0 -0.30 0.60 -10 7 0 0.10 0.37 11 -7 0 11.77 1.08 12 -7 0 4.66 0.55 -12 7 0 4.13 0.44 0 -8 0 407.44 13.52 1 -8 0 55.56 2.98 1 -8 0 62.10 2.57 -1 -8 0 61.46 2.60 2 -8 0 4.67 0.73 2 -8 0 5.53 1.00 -2 -8 0 4.70 0.67 -2 -8 0 5.75 0.82 3 -8 0 30.58 2.00 3 -8 0 31.45 1.62 -3 -8 0 30.67 1.70 -4 -8 0 9.94 1.04 4 -8 0 10.11 1.35 -5 -8 0 36.64 1.63 -5 -8 0 37.25 2.22 -5 -8 0 37.88 2.03 5 -8 0 35.89 2.45 -5 -8 0 44.07 2.60 5 -8 0 37.69 2.42 -6 -8 0 0.21 0.60 -6 -8 0 -0.29 0.68 6 -8 0 0.09 0.67 -7 -8 0 54.48 3.01 7 -8 0 49.90 2.99 -7 -8 0 48.40 2.65 -7 8 0 48.97 3.23 -8 -8 0 24.36 1.63 8 -8 0 25.93 1.92 -8 8 0 22.80 2.10 9 -8 0 0.00 0.63 -9 8 0 -0.29 0.70 10 -8 0 2.97 0.68 -10 8 0 2.78 0.46 11 -8 0 8.94 0.87 0 -9 0 0.56 0.58 1 -9 0 62.60 2.73 -1 -9 0 59.19 2.72 2 -9 0 7.72 1.21 -2 -9 0 13.56 1.26 2 -9 0 12.19 1.13 -3 -9 0 17.76 1.51 3 -9 0 15.35 1.64 3 -9 0 18.93 1.61 -3 -9 0 16.08 1.40 -3 -9 0 18.21 1.50 -3 -9 0 17.09 1.14 -4 -9 0 5.41 0.57 -4 -9 0 4.69 0.90 -4 -9 0 4.62 0.93 4 -9 0 3.40 0.94 -5 -9 0 10.61 0.61 -5 -9 0 11.66 1.25 -5 -9 0 11.35 1.32 5 -9 0 9.56 1.26 6 -9 0 86.89 4.64 -6 -9 0 88.60 4.31 -6 -9 0 94.64 4.79 -7 -9 0 19.19 1.68 -7 -9 0 17.15 1.47 7 -9 0 17.70 1.67 -7 9 0 19.27 2.02 -8 -9 0 0.40 0.64 8 -9 0 1.51 0.71 -8 -9 0 2.22 0.66 -8 9 0 1.07 0.84 -9 -9 0 4.06 0.63 9 -9 0 3.00 0.68 -9 9 0 3.62 0.80 10 -9 0 0.95 0.47 11 -9 0 2.45 0.41 -11 9 0 2.28 0.41 0 -10 0 43.17 2.21 0 -10 0 41.13 2.59 0 -10 0 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-17 7.38 0.83 -6 -1 17 11.20 1.37 6 -1 -17 11.51 0.94 -6 -1 17 10.78 2.02 -6 1 17 7.87 1.75 -5 -1 17 44.47 3.94 5 -1 -17 43.85 2.36 -5 1 17 52.98 3.95 5 1 -17 45.25 2.47 -4 -1 17 1.60 1.81 4 -1 -17 2.75 0.60 4 1 -17 3.90 0.68 -4 1 17 4.73 1.87 -3 -1 17 -1.08 1.71 3 -1 -17 0.54 0.43 3 1 -17 -0.50 0.44 -3 1 17 0.11 1.68 -2 -1 17 16.01 2.59 2 -1 -17 19.64 1.19 2 1 -17 20.29 1.31 -2 1 17 18.69 2.65 1 -1 -17 2.27 0.57 1 -1 -17 3.35 0.35 -1 -1 17 1.77 1.83 -1 1 17 1.32 1.61 1 1 -17 3.04 0.49 0 -1 -17 0.41 0.42 0 -1 17 -0.12 1.61 0 1 -17 0.23 0.46 0 1 17 0.50 1.55 1 -1 17 3.18 1.59 -1 -1 -17 4.52 0.50 1 1 17 1.82 1.49 -1 1 -17 4.33 0.52 -2 -1 -17 7.69 0.49 2 -1 17 3.79 1.40 2 1 17 3.35 1.51 -2 1 -17 7.95 0.59 -9 -2 17 5.89 1.15 9 -2 -17 7.45 0.66 -9 2 17 7.03 1.25 -9 2 17 8.02 0.84 9 2 -17 8.13 0.72 -8 -2 17 12.96 1.13 -8 -2 17 7.48 1.47 8 -2 -17 12.45 0.94 8 2 -17 11.48 0.92 -8 2 17 9.85 1.49 -8 2 17 10.91 1.13 7 -2 -17 12.11 1.06 -7 -2 17 15.52 1.38 -7 -2 17 8.11 1.72 7 -2 -17 13.68 1.05 -7 2 17 9.18 1.64 -6 -2 17 2.97 1.61 6 -2 -17 5.05 0.70 6 -2 -17 4.46 0.66 -6 -2 17 3.57 0.91 -6 2 17 5.22 1.58 5 -2 -17 6.07 0.75 -5 -2 17 5.04 1.82 -5 -2 17 6.18 1.13 -5 2 17 5.65 1.72 4 -2 -17 20.31 1.29 -4 -2 17 13.41 2.38 4 2 -17 21.43 1.45 -4 2 17 15.88 2.29 -3 -2 17 0.31 1.76 3 -2 -17 0.72 0.44 3 2 -17 1.50 0.56 -3 2 17 0.88 1.57 -2 -2 17 2.22 1.80 2 -2 -17 2.75 0.44 2 -2 -17 2.50 0.57 -2 2 17 3.26 1.68 2 2 -17 2.21 0.56 -1 -2 17 8.46 2.06 1 -2 -17 13.76 1.01 1 2 -17 12.46 0.95 -1 2 17 7.23 1.83 0 -2 -17 16.36 1.02 0 -2 17 9.54 2.07 0 2 17 12.32 2.06 0 2 -17 17.02 1.20 0 2 -17 17.56 0.86 -1 -2 -17 43.02 1.82 1 2 17 29.84 2.98 -1 2 -17 44.21 1.97 2 -2 17 1.52 1.18 -2 2 -17 3.22 0.39 2 2 17 2.87 1.15 9 -3 -17 18.25 1.08 9 3 -17 17.33 1.06 -9 3 17 17.23 1.57 -9 3 17 17.22 1.25 8 -3 -17 3.96 0.57 -8 -3 17 4.52 0.56 8 -3 -17 3.54 0.52 -8 -3 17 2.72 1.12 -8 3 17 3.20 1.02 8 3 -17 2.38 0.45 -8 3 17 1.74 0.68 7 -3 -17 3.21 0.54 -7 -3 17 2.56 1.26 7 -3 -17 4.14 0.59 -7 -3 17 3.46 0.80 -7 -3 17 3.51 0.74 -7 3 17 3.67 1.21 -7 3 17 2.03 0.78 6 -3 -17 11.36 0.94 -6 -3 17 9.24 1.16 -6 -3 17 6.87 1.69 6 -3 -17 12.09 0.97 -6 -3 17 10.29 1.14 -6 3 17 7.86 1.58 5 -3 -17 32.78 1.79 5 -3 -17 32.85 1.73 -5 -3 17 34.17 2.30 -5 -3 17 31.41 3.15 -5 3 17 32.98 2.89 4 -3 -17 4.74 0.60 -4 -3 17 0.61 1.61 -4 -3 17 3.17 0.89 -4 3 17 2.02 1.43 4 3 -17 3.89 0.70 3 -3 -17 2.64 0.44 -3 -3 17 2.60 1.74 3 3 -17 1.55 0.58 -3 3 17 1.91 1.41 -2 -3 17 12.85 2.30 2 -3 -17 21.39 1.26 -2 3 17 15.27 2.15 2 3 -17 20.46 1.33 -1 -3 17 0.75 1.57 1 -3 -17 1.38 0.43 -1 3 17 0.57 1.31 1 3 -17 1.67 0.46 0 -3 -17 1.10 0.35 0 -3 17 0.91 1.38 0 3 -17 0.97 0.29 0 3 17 2.79 1.31 1 -3 17 3.05 1.31 -1 -3 -17 3.68 0.34 -1 3 -17 4.10 0.53 1 3 17 2.38 1.18 -2 3 -17 28.13 1.32 8 -4 -17 1.78 0.39 -8 -4 17 1.57 0.54 8 -4 -17 1.22 0.38 -8 4 17 1.50 0.59 -7 -4 17 1.11 0.57 7 -4 -17 1.41 0.42 7 -4 -17 1.34 0.39 -7 -4 17 0.02 0.50 -7 4 17 0.78 0.84 6 -4 -17 0.99 0.41 -6 -4 17 1.12 1.15 -6 -4 17 0.24 0.62 -6 -4 17 0.18 0.62 6 -4 -17 0.15 0.37 -6 4 17 0.11 0.95 -5 -4 17 36.33 2.23 5 -4 -17 34.66 1.77 -5 -4 17 32.76 2.86 -5 -4 17 35.47 2.18 5 -4 -17 35.39 1.76 -5 4 17 31.90 2.65 4 -4 -17 33.61 1.68 -4 -4 17 33.08 2.96 -4 -4 17 36.75 2.21 -4 -4 17 39.81 2.32 -4 4 17 34.08 2.69 4 4 -17 29.90 2.01 3 -4 -17 4.40 0.57 -3 -4 17 3.11 1.51 -3 -4 17 4.06 0.83 3 -4 -17 4.73 0.41 -3 4 17 3.22 1.29 3 4 -17 4.59 0.71 -2 -4 17 1.39 1.39 2 -4 -17 1.70 0.44 -2 -4 17 2.44 0.72 2 4 -17 2.32 0.55 -1 -4 17 5.77 0.82 1 -4 -17 6.13 0.56 -1 -4 17 2.12 1.33 1 4 -17 5.94 0.62 0 -4 17 -1.02 1.12 0 -4 -17 0.61 0.27 0 4 -17 1.20 0.28 8 -5 -17 0.35 0.27 8 -5 -17 0.26 0.27 7 -5 -17 2.04 0.39 7 -5 -17 2.16 0.37 -7 -5 17 1.12 0.53 6 -5 -17 8.94 0.70 6 -5 -17 8.81 0.73 -6 -5 17 9.77 0.90 -6 -5 17 8.92 0.95 -5 -5 17 8.15 0.99 -5 -5 17 9.41 1.00 5 -5 -17 7.63 0.70 5 -5 -17 7.81 0.62 -4 -5 17 8.27 0.98 -4 -5 17 8.72 1.00 4 -5 -17 8.48 0.76 -3 -5 17 0.57 0.66 3 -5 -17 0.52 0.34 -3 -5 17 1.46 0.63 3 5 -17 -0.39 0.44 -2 -5 17 10.71 1.03 2 -5 -17 9.99 0.73 2 5 -17 8.05 0.78 1 -5 -17 0.77 0.28 -1 -5 17 0.71 0.51 1 5 -17 1.08 0.38 0 -5 -17 2.57 0.23 0 5 -17 2.90 0.30 -6 -6 17 10.87 1.00 6 -6 -17 9.14 0.64 5 -6 -17 12.80 0.80 -5 -6 17 14.38 1.15 -5 -6 17 12.90 1.01 -4 -6 17 1.39 0.56 4 -6 -17 1.29 0.33 -4 -6 17 0.90 0.56 -3 -6 17 1.11 0.54 3 -6 -17 0.33 0.29 -3 -6 17 0.93 0.52 3 6 -17 0.08 0.41 2 -6 -17 1.14 0.33 2 -6 -17 1.67 0.29 -2 -6 17 1.20 0.58 -2 -6 17 1.88 0.54 2 6 -17 1.16 0.38 1 -6 -17 6.68 0.42 1 -6 -17 7.28 0.62 1 6 -17 7.69 0.60 -8 0 18 1.94 0.53 -8 0 18 1.06 0.92 -7 0 18 71.34 3.49 7 0 -18 69.24 3.26 -6 0 18 -0.77 1.26 -6 0 18 0.19 0.66 6 0 -18 0.70 0.40 -5 0 18 38.85 3.23 5 0 -18 38.62 1.98 -4 0 18 3.86 1.68 4 0 -18 5.61 0.62 3 0 -18 8.17 0.74 -3 0 18 6.03 1.68 -2 0 18 2.67 1.51 2 0 -18 2.72 0.35 -1 0 18 4.74 1.55 1 0 -18 8.36 0.71 0 0 -18 51.53 2.25 -8 -1 18 20.29 1.22 -8 -1 18 17.72 1.78 -8 1 18 20.46 1.35 -8 1 18 16.56 1.71 -7 -1 18 13.97 1.21 7 -1 -18 11.60 0.88 7 -1 -18 12.55 0.81 -7 -1 18 5.70 1.29 -7 1 18 10.24 1.07 -7 1 18 7.68 1.45 -6 -1 18 26.21 1.82 -6 -1 18 24.05 2.36 6 -1 -18 23.68 1.38 6 1 -18 22.80 1.43 -6 1 18 23.33 2.44 -6 1 18 24.71 1.78 5 -1 -18 7.32 0.73 -5 -1 18 6.65 0.95 -5 -1 18 5.15 1.54 5 1 -18 5.73 0.69 -5 1 18 6.32 1.52 -4 -1 18 5.99 1.76 4 -1 -18 8.11 0.77 -4 1 18 8.26 1.74 4 1 -18 8.62 0.82 -3 -1 18 3.88 1.56 3 -1 -18 2.93 0.43 3 1 -18 2.35 0.48 -3 1 18 2.23 1.43 -2 -1 18 4.72 1.61 2 -1 -18 7.42 0.67 -2 1 18 5.59 1.63 2 1 -18 8.86 0.65 1 -1 -18 16.46 0.98 -1 -1 18 8.70 1.77 1 1 -18 17.01 1.01 -1 1 18 12.35 1.94 0 -1 18 2.09 1.25 0 1 18 2.22 1.21 -8 -2 18 0.14 0.79 -8 2 18 0.63 0.74 -8 2 18 0.80 0.51 -7 -2 18 19.74 1.31 7 -2 -18 15.64 0.98 7 -2 -18 15.12 0.87 -7 -2 18 9.47 1.48 -7 2 18 14.76 1.35 -7 2 18 16.59 1.79 -6 -2 18 -0.14 1.13 -6 -2 18 0.93 0.63 6 -2 -18 1.41 0.36 -6 2 18 0.78 1.10 6 2 -18 0.41 0.46 5 -2 -18 23.42 1.26 -5 -2 18 20.45 1.67 -5 -2 18 22.10 2.41 -5 2 18 21.34 2.18 5 2 -18 21.25 1.35 4 -2 -18 5.57 0.54 -4 -2 18 3.10 1.48 -4 2 18 7.59 1.57 4 2 -18 5.76 0.64 -3 -2 18 1.73 1.42 3 -2 -18 1.68 0.28 3 2 -18 1.81 0.45 -3 2 18 1.17 1.26 2 -2 -18 4.99 0.55 -2 -2 18 3.02 1.45 2 2 -18 4.48 0.51 -2 2 18 5.41 1.35 -1 -2 18 8.32 1.56 -1 2 18 11.33 1.50 0 -2 18 1.30 1.06 7 -3 -18 3.65 0.44 -7 -3 18 4.36 0.57 -7 3 18 3.14 0.88 -6 -3 18 -0.34 0.53 6 -3 -18 0.38 0.31 -6 -3 18 0.61 1.02 -6 3 18 -0.30 0.79 -5 -3 18 9.81 1.55 5 -3 -18 15.54 0.87 -5 -3 18 15.92 1.35 -5 3 18 9.82 1.48 5 3 -18 14.44 1.04 -4 -3 18 30.22 1.97 -4 -3 18 27.36 2.49 4 -3 -18 31.57 1.41 -4 3 18 28.82 2.36 4 3 -18 28.93 1.63 -3 -3 18 1.80 1.26 3 -3 -18 2.80 0.44 -3 3 18 2.88 1.15 3 3 -18 2.77 0.47 2 -3 -18 7.46 0.63 -2 -3 18 4.94 1.29 2 3 -18 8.04 0.66 -2 3 18 5.49 1.33 -1 -3 18 1.20 1.04 1 -3 -18 3.33 0.38 6 -4 -18 0.54 0.25 -6 -4 18 0.39 0.46 -5 -4 18 0.13 0.49 5 -4 -18 -0.08 0.20 -4 -4 18 0.53 0.53 4 4 -18 0.22 0.35 3 -4 -18 -0.32 0.25 -3 -4 18 -0.15 0.56 3 4 -18 0.35 0.33 2 -4 -18 2.22 0.33 2 4 -18 2.16 0.36 -5 0 19 -0.84 0.95 5 0 -19 -0.30 0.26 4 0 -19 -0.11 0.23 -4 0 19 0.50 0.99 -3 0 19 -0.06 0.93 5 -1 -19 3.94 0.37 -5 -1 19 1.86 0.98 5 1 -19 3.85 0.42 -5 1 19 2.89 1.04 -4 -1 19 0.11 0.93 4 1 -19 0.58 0.27 -4 1 19 1.84 0.98 -3 -1 19 0.79 1.04 -3 1 19 0.35 0.98 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 43106 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 C1 C 1.01098(17) 0.69497(15) 0.16110(11) 0.0116(4) Uani 1 1 d . . . . . C2 C 1.15663(17) 0.60878(15) 0.10203(12) 0.0136(4) Uani 1 1 d . . . . . H2A H 1.1000 0.5753 0.0483 0.016 Uiso 1 1 calc R U . . . H2B H 1.1764 0.5518 0.1506 0.016 Uiso 1 1 calc R U . . . C3 C 1.26718(19) 0.64631(16) 0.07965(14) 0.0177(4) Uani 1 1 d . . . . . H3A H 1.3222 0.6817 0.1332 0.021 Uiso 1 1 calc R U . . . H3B H 1.2465 0.7028 0.0307 0.021 Uiso 1 1 calc R U . . . C4 C 1.32675(18) 0.54586(16) 0.05016(13) 0.0183(4) Uani 1 1 d . . . . . H4A H 1.3521 0.4925 0.1002 0.027 Uiso 1 1 calc R U . . . H4B H 1.3956 0.5715 0.0325 0.027 Uiso 1 1 calc R U . . . H4C H 1.2709 0.5090 -0.0012 0.027 Uiso 1 1 calc R U . . . C5 C 0.58285(18) 0.80190(15) 0.11217(12) 0.0130(4) Uani 1 1 d . . . . . C6 C 0.43767(18) 0.84107(16) -0.02817(12) 0.0161(4) Uani 1 1 d . . . . . H6A H 0.4188 0.7605 -0.0399 0.019 Uiso 1 1 calc R U . . . H6B H 0.4953 0.8631 -0.0604 0.019 Uiso 1 1 calc R U . . . C7 C 0.32697(18) 0.91067(15) -0.06095(12) 0.0148(4) Uani 1 1 d . . . . . H7A H 0.3465 0.9912 -0.0494 0.018 Uiso 1 1 calc R U . . . H7B H 0.2704 0.8894 -0.0276 0.018 Uiso 1 1 calc R U . . . C8 C 0.27057(19) 0.89205(17) -0.16181(13) 0.0209(4) Uani 1 1 d . . . . . H8A H 0.3276 0.9109 -0.1945 0.031 Uiso 1 1 calc R U . . . H8B H 0.2008 0.9401 -0.1829 0.031 Uiso 1 1 calc R U . . . H8C H 0.2472 0.8132 -0.1727 0.031 Uiso 1 1 calc R U . . . C9 C 0.81046(19) 0.60458(16) 0.41466(12) 0.0173(4) Uani 1 1 d . . . . . H9A H 0.7373 0.6419 0.4184 0.021 Uiso 1 1 calc R U . . . H9B H 0.8565 0.5824 0.4763 0.021 Uiso 1 1 calc R U . . . C10 C 0.7790(2) 0.50056(16) 0.35583(12) 0.0185(4) Uani 1 1 d . . . . . H10A H 0.8522 0.4628 0.3527 0.022 Uiso 1 1 calc R U . . . H10B H 0.7347 0.4474 0.3831 0.022 Uiso 1 1 calc R U . . . C11 C 0.87565(19) 0.79716(16) 0.41574(12) 0.0181(4) Uani 1 1 d . . . . . H11A H 0.7935 0.8228 0.4002 0.027 Uiso 1 1 calc R U . . . H11B H 0.9221 0.8496 0.3910 0.027 Uiso 1 1 calc R U . . . H11C H 0.9083 0.7940 0.4814 0.027 Uiso 1 1 calc R U . . . C12 C 1.00519(19) 0.64796(17) 0.40272(13) 0.0193(4) Uani 1 1 d . . . . . H12A H 1.0375 0.6489 0.4685 0.029 Uiso 1 1 calc R U . . . H12B H 1.0505 0.6994 0.3761 0.029 Uiso 1 1 calc R U . . . H12C H 1.0103 0.5717 0.3803 0.029 Uiso 1 1 calc R U . . . C13 C 0.58437(19) 0.55778(18) 0.26412(14) 0.0230(4) Uani 1 1 d . . . . . H13A H 0.5365 0.5758 0.2028 0.035 Uiso 1 1 calc R U . . . H13B H 0.5860 0.6226 0.3035 0.035 Uiso 1 1 calc R U . . . H13C H 0.5500 0.4931 0.2865 0.035 Uiso 1 1 calc R U . . . C14 C 0.7004(2) 0.43191(16) 0.20465(14) 0.0236(5) Uani 1 1 d . . . . . H14A H 0.7804 0.4104 0.2048 0.035 Uiso 1 1 calc R U . . . H14B H 0.6539 0.4507 0.1431 0.035 Uiso 1 1 calc R U . . . H14C H 0.6631 0.3692 0.2269 0.035 Uiso 1 1 calc R U . . . Mn1 Mn 0.79693(3) 0.68467(2) 0.22288(2) 0.00969(8) Uani 1 1 d . . . . . N1 N 0.88031(15) 0.68395(13) 0.37740(10) 0.0132(3) Uani 1 1 d . . . . . N2 N 0.70624(15) 0.53033(13) 0.26348(10) 0.0142(3) Uani 1 1 d . . . . . O1 O 1.10532(12) 0.70774(10) 0.13127(9) 0.0138(3) Uani 1 1 d . . . . . O2 O 0.48730(12) 0.86013(11) 0.06797(8) 0.0149(3) Uani 1 1 d . . . . . S1 S 0.94918(4) 0.56788(3) 0.16631(3) 0.01211(10) Uani 1 1 d . . . . . S2 S 0.95763(4) 0.81581(3) 0.19289(3) 0.01444(10) Uani 1 1 d . . . . . S3 S 0.63854(5) 0.83436(4) 0.22323(3) 0.01619(11) Uani 1 1 d . . . . . S4 S 0.64494(4) 0.70377(4) 0.06167(3) 0.01502(11) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0109(10) 0.0150(8) 0.0083(8) 0.0009(6) 0.0018(6) -0.0007(7) C2 0.0136(11) 0.0134(8) 0.0152(9) -0.0013(6) 0.0065(7) 0.0005(7) C3 0.0145(11) 0.0176(9) 0.0246(10) -0.0004(7) 0.0113(8) -0.0015(8) C4 0.0151(11) 0.0198(9) 0.0221(10) -0.0025(7) 0.0088(8) 0.0003(8) C5 0.0116(11) 0.0133(8) 0.0137(8) 0.0024(6) 0.0030(7) 0.0011(7) C6 0.0153(11) 0.0209(9) 0.0109(9) 0.0005(7) 0.0019(7) 0.0028(8) C7 0.0140(11) 0.0160(8) 0.0135(9) 0.0013(7) 0.0022(7) 0.0018(8) C8 0.0174(12) 0.0269(10) 0.0157(9) 0.0020(7) 0.0005(8) 0.0005(9) C9 0.0215(12) 0.0201(9) 0.0111(8) 0.0010(7) 0.0061(7) -0.0010(8) C10 0.0248(13) 0.0160(9) 0.0150(9) 0.0035(7) 0.0061(8) -0.0016(8) C11 0.0204(12) 0.0182(9) 0.0135(9) -0.0049(7) 0.0013(7) 0.0020(8) C12 0.0153(12) 0.0254(10) 0.0147(9) 0.0006(7) 0.0006(7) 0.0044(9) C13 0.0161(12) 0.0251(10) 0.0295(11) 0.0037(8) 0.0093(9) -0.0045(9) C14 0.0353(14) 0.0151(9) 0.0232(10) -0.0045(8) 0.0128(9) -0.0090(9) Mn1 0.00952(17) 0.01031(13) 0.00924(14) 0.00063(10) 0.00268(10) 0.00061(11) N1 0.0126(9) 0.0152(7) 0.0116(7) -0.0001(6) 0.0029(6) 0.0004(6) N2 0.0150(9) 0.0140(7) 0.0145(8) -0.0012(6) 0.0057(6) -0.0016(7) O1 0.0136(8) 0.0122(6) 0.0180(6) -0.0014(5) 0.0082(5) -0.0011(5) O2 0.0124(8) 0.0179(6) 0.0126(6) -0.0006(5) 0.0006(5) 0.0049(5) S1 0.0123(3) 0.01016(19) 0.0148(2) 0.00027(14) 0.00536(16) -0.00078(16) S2 0.0164(3) 0.01017(19) 0.0189(2) -0.00168(15) 0.00840(17) -0.00067(17) S3 0.0177(3) 0.0173(2) 0.0114(2) -0.00217(15) 0.00066(17) 0.00637(19) S4 0.0148(3) 0.0176(2) 0.0117(2) -0.00158(15) 0.00231(16) 0.00475(18) 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' 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' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 S1 122.31(14) . . ? O1 C1 S2 114.94(13) . . ? S1 C1 S2 122.75(12) . . ? O1 C2 C3 107.34(14) . . ? O1 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C2 C3 C4 110.01(16) . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 S4 122.61(14) . . ? O2 C5 S3 115.17(14) . . ? S4 C5 S3 122.22(11) . . ? O2 C6 C7 108.33(15) . . ? O2 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? O2 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 C7 C8 110.21(16) . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 110.77(15) . . ? N1 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N2 C10 C9 110.96(15) . . ? N2 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 Mn1 N1 78.90(6) . . ? N2 Mn1 S3 98.85(4) . . ? N1 Mn1 S3 95.37(4) . . ? N2 Mn1 S2 161.48(5) . . ? N1 Mn1 S2 94.10(4) . . ? S3 Mn1 S2 98.874(18) . . ? N2 Mn1 S1 95.03(4) . . ? N1 Mn1 S1 102.44(4) . . ? S3 Mn1 S1 159.232(18) . . ? S2 Mn1 S1 69.522(16) . . ? N2 Mn1 S4 94.79(4) . . ? N1 Mn1 S4 162.47(5) . . ? S3 Mn1 S4 69.241(16) . . ? S2 Mn1 S4 96.491(17) . . ? S1 Mn1 S4 94.346(17) . . ? C9 N1 C12 109.86(15) . . ? C9 N1 C11 109.59(15) . . ? C12 N1 C11 107.89(15) . . ? C9 N1 Mn1 106.70(11) . . ? C12 N1 Mn1 111.80(11) . . ? C11 N1 Mn1 111.00(11) . . ? C14 N2 C13 107.90(17) . . ? C14 N2 C10 108.50(15) . . ? C13 N2 C10 109.94(16) . . ? C14 N2 Mn1 114.02(12) . . ? C13 N2 Mn1 110.90(11) . . ? C10 N2 Mn1 105.51(11) . . ? C1 O1 C2 118.77(14) . . ? C5 O2 C6 118.51(15) . . ? C1 S1 Mn1 83.68(7) . . ? C1 S2 Mn1 84.02(7) . . ? C5 S3 Mn1 84.89(7) . . ? C5 S4 Mn1 83.64(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 C1 O1 1.334(2) . ? C1 S1 1.6924(18) . ? C1 S2 1.6999(18) . ? C2 O1 1.456(2) . ? C2 C3 1.514(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.524(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O2 1.335(2) . ? C5 S4 1.6877(19) . ? C5 S3 1.7009(18) . ? C6 O2 1.453(2) . ? C6 C7 1.509(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.529(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.478(2) . ? C9 C10 1.519(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.485(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N1 1.480(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N1 1.479(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N2 1.482(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N2 1.474(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? Mn1 N2 2.3050(16) . ? Mn1 N1 2.3125(15) . ? Mn1 S3 2.5874(6) . ? Mn1 S2 2.6036(6) . ? Mn1 S1 2.6188(5) . ? Mn1 S4 2.6343(5) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C14 H14A S1 0.98 2.92 3.556(2) 123.2 . C13 H13C S3 0.98 2.89 3.791(2) 152.5 2_645 C13 H13B S3 0.98 2.96 3.448(2) 112.2 . C11 H11A S3 0.98 2.83 3.485(2) 125.0 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 C4 178.92(15) . . . . ? O2 C6 C7 C8 -179.23(15) . . . . ? N1 C9 C10 N2 -61.1(2) . . . . ? C10 C9 N1 C12 -80.59(19) . . . . ? C10 C9 N1 C11 161.03(16) . . . . ? C10 C9 N1 Mn1 40.78(18) . . . . ? C9 C10 N2 C14 167.73(17) . . . . ? C9 C10 N2 C13 -74.5(2) . . . . ? C9 C10 N2 Mn1 45.16(18) . . . . ? S1 C1 O1 C2 0.1(2) . . . . ? S2 C1 O1 C2 -179.63(12) . . . . ? C3 C2 O1 C1 -175.23(15) . . . . ? S4 C5 O2 C6 -2.4(2) . . . . ? S3 C5 O2 C6 177.15(13) . . . . ? C7 C6 O2 C5 176.47(16) . . . . ? O1 C1 S1 Mn1 -177.79(15) . . . . ? S2 C1 S1 Mn1 1.93(10) . . . . ? O1 C1 S2 Mn1 177.80(13) . . . . ? S1 C1 S2 Mn1 -1.94(10) . . . . ? O2 C5 S3 Mn1 -179.23(14) . . . . ? S4 C5 S3 Mn1 0.31(11) . . . . ? O2 C5 S4 Mn1 179.20(16) . . . . ? S3 C5 S4 Mn1 -0.30(11) . . . . ?