#------------------------------------------------------------------------------ #$Date: 2021-11-10 03:40:58 +0200 (Wed, 10 Nov 2021) $ #$Revision: 270557 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061060.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_7061060 loop_ _publ_author_name 'Kaim, Vishakha' 'Kaur-Ghumaan, Sandeep' _publ_section_title ; Mononuclear Mn complexes featuring N,S-/N,N-donor and 1,3,5-triaza-7-phosphaadamantane ligands: synthesis and electrocatalytic properties ; _journal_issue 43 _journal_name_full 'New Journal of Chemistry' _journal_page_first 20272 _journal_page_last 20279 _journal_paper_doi 10.1039/D1NJ02104D _journal_volume 45 _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_moiety 'C16 H16 Mn N4 O3 P S2' _chemical_formula_sum 'C16 H16 Mn N4 O3 P S2' _chemical_formula_weight 462.36 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-03-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-04-28 deposited with the CCDC. 2021-09-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0708(7) _cell_length_b 11.9149(8) _cell_length_c 15.6475(11) _cell_measurement_reflns_used 5050 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 29.3120 _cell_measurement_theta_min 2.3930 _cell_volume 1877.6(2) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -25.75 154.25 1.00 2.00 -25.75 0.00 73.76 -- 180 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Saxi-CrysAlisPro-abstract goniometer imported SAXI images' _diffrn_measurement_method '\f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0295276000 _diffrn_orient_matrix_UB_12 -0.0523731000 _diffrn_orient_matrix_UB_13 -0.0101018000 _diffrn_orient_matrix_UB_21 -0.0254480000 _diffrn_orient_matrix_UB_22 0.0036960000 _diffrn_orient_matrix_UB_23 -0.0421560000 _diffrn_orient_matrix_UB_31 0.0586762000 _diffrn_orient_matrix_UB_32 0.0280191000 _diffrn_orient_matrix_UB_33 -0.0132734000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 11170 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.668 _diffrn_reflns_theta_min 2.405 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.27891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic yellowish yellow' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.636 _exptl_crystal_description block _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.96 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.5 _refine_diff_density_max 2.643 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.098 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.48(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 259 _refine_ls_number_reflns 3498 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0503 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+3.9220P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1255 _refine_ls_wR_factor_ref 0.1276 _reflns_Friedel_coverage 0.751 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 3314 _reflns_number_total 3498 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj02104d2.cif _cod_data_source_block fastscan_autored _cod_database_code 7061060 _shelx_shelxl_version_number 2017/1 _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. ; _reflns_odcompleteness_completeness 87.16 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.53 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.52(4) 0.48(4) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 3.a Secondary CH2 refined with riding coordinates: C16(H16A,H16B), C15(H15A,H15B), C12(H12A,H12B), C11(H11A,H11B), C13(H13A,H13B) 3.b Aromatic/amide H refined with riding coordinates: C9(H9), C6(H6) ; _shelx_res_file ; TITL fastscan_autored_a.res in P2(1)2(1)2(1) fastscan_autored.res created by SHELXL-2017/1 at 22:51:55 on 15-Mar-2021 REM Old TITL fastscan_autored in P21212 #18 REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.247, Rweak 0.064, Alpha 0.007, Orientation as input REM Flack x = 0.494 ( 0.004 ) from Parsons' quotients REM Formula found by SHELXT: C17 N3 O6 Br CELL 0.71073 10.0708 11.9149 15.6475 90 90 90 ZERR 4 0.0007 0.0008 0.0011 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Mn N O P S UNIT 64 64 4 16 12 4 8 L.S. 10 PLAN 5 TEMP -123 CONN 3 C4 BOND $H list 4 fmap 2 acta SHEL 100 0.82 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 1 1 OMIT 0 1 3 OMIT 0 0 2 OMIT 3 0 1 OMIT 0 3 8 OMIT 2 0 0 OMIT 0 2 0 OMIT 0 2 3 REM REM REM WGHT 0.064900 3.922000 BASF 0.47517 FVAR 0.43524 MN1 3 0.145942 0.605928 0.580027 11.00000 0.02260 0.01129 = 0.01906 0.00191 -0.00049 -0.00001 P1 6 0.340375 0.590215 0.656811 11.00000 0.02416 0.01198 = 0.01519 0.00015 -0.00144 -0.00049 S2 7 0.033658 0.291356 0.699312 11.00000 0.04517 0.02040 = 0.02998 0.00403 0.00455 -0.00233 S1 7 0.024193 0.552839 0.708926 11.00000 0.04317 0.02004 = 0.03596 -0.00244 0.00528 0.00378 N1 4 0.132883 0.433840 0.591616 11.00000 0.03457 0.02251 = 0.02744 -0.00133 0.00085 0.00582 O1 5 0.137777 0.849438 0.615106 11.00000 0.04230 0.01310 = 0.04631 -0.00124 0.00387 0.00210 O3 5 -0.103632 0.631686 0.480255 11.00000 0.03156 0.03167 = 0.05219 0.01035 -0.01741 -0.00348 O2 5 0.293421 0.627042 0.425645 11.00000 0.04820 0.03398 = 0.03948 0.01140 -0.01722 -0.00938 N4 4 0.499670 0.473511 0.769034 11.00000 0.03249 0.01928 = 0.02203 0.00480 -0.00738 -0.00344 N2 4 0.613799 0.578122 0.654222 11.00000 0.02312 0.02343 = 0.03035 0.00535 -0.00212 -0.00026 N3 4 0.514089 0.680716 0.775003 11.00000 0.04342 0.01898 = 0.02476 -0.00106 -0.01182 -0.00479 C16 1 0.369429 0.466969 0.726686 11.00000 0.02832 0.01800 = 0.02063 0.00461 -0.00459 -0.00368 AFIX 23 H16A 2 0.298716 0.463173 0.770542 11.00000 -1.20000 H16B 2 0.364959 0.397557 0.692029 11.00000 -1.20000 AFIX 0 C15 1 0.607616 0.475700 0.705860 11.00000 0.02631 0.02159 = 0.03145 0.00653 -0.00381 0.00114 AFIX 23 H15A 2 0.693176 0.466612 0.736237 11.00000 -1.20000 H15B 2 0.597081 0.410637 0.667098 11.00000 -1.20000 AFIX 0 C7 1 0.263292 0.193460 0.464283 11.00000 0.02897 0.04483 = 0.02087 -0.00809 0.00031 -0.00202 C5 1 0.167564 0.329486 0.557816 11.00000 0.02519 0.01952 = 0.02915 -0.00726 -0.01650 0.00603 C12 1 0.384995 0.701821 0.732638 11.00000 0.03989 0.01533 = 0.01820 -0.00238 -0.00388 0.00046 AFIX 23 H12A 2 0.389300 0.774308 0.701837 11.00000 -1.20000 H12B 2 0.314797 0.707878 0.776689 11.00000 -1.20000 AFIX 0 C11 1 0.499349 0.585309 0.597737 11.00000 0.02504 0.02173 = 0.02217 0.00300 0.00248 -0.00031 AFIX 23 H11A 2 0.498996 0.519482 0.559131 11.00000 -1.20000 H11B 2 0.507360 0.653539 0.562000 11.00000 -1.20000 AFIX 0 C9 1 0.135978 0.131530 0.587249 11.00000 0.03789 0.02305 = 0.02651 0.00259 -0.00548 -0.00185 AFIX 43 H9 2 0.099436 0.073038 0.621148 11.00000 -1.20000 AFIX 0 C4 1 0.064762 0.427254 0.663321 11.00000 0.03233 0.02511 = 0.02394 -0.00196 -0.00066 -0.00455 C8 1 0.210344 0.108195 0.514303 11.00000 0.03483 0.01911 = 0.03707 -0.00992 -0.00929 0.00565 C6 1 0.242452 0.304894 0.485595 11.00000 0.02595 0.03215 = 0.02825 0.00009 -0.00906 -0.00752 AFIX 43 H6 2 0.278632 0.363370 0.451520 11.00000 -1.20000 AFIX 0 C2 1 0.243682 0.619835 0.479203 11.00000 0.03068 0.02076 = 0.03477 -0.00545 -0.01749 0.00496 C13 1 0.621495 0.673610 0.711533 11.00000 0.02823 0.02805 = 0.03876 0.00757 -0.00617 -0.00549 AFIX 23 H13A 2 0.620953 0.743136 0.676891 11.00000 -1.20000 H13B 2 0.707403 0.670555 0.742200 11.00000 -1.20000 AFIX 0 C14 1 0.511983 0.573874 0.823153 11.00000 0.03907 0.02706 = 0.02237 0.00113 -0.00656 -0.00271 H14A 2 0.447457 0.585290 0.865124 11.00000 -1.20000 H14B 2 0.600116 0.570127 0.850638 11.00000 -1.20000 C10 1 0.117568 0.242164 0.608226 11.00000 0.02823 0.03290 = 0.02003 -0.00424 -0.00497 0.00273 C3 1 -0.009219 0.618204 0.519527 11.00000 0.02902 0.01191 = 0.03253 0.00568 -0.00066 -0.00005 C1 1 0.142482 0.755291 0.599946 11.00000 0.02424 0.02555 = 0.02185 0.00141 0.00196 0.00042 H8 2 0.228018 0.033531 0.493820 11.00000 0.00401 H7 2 0.315012 0.184819 0.412767 11.00000 0.01481 HKLF 4 REM fastscan_autored_a.res in P2(1)2(1)2(1) REM R1 = 0.0503 for 3314 Fo > 4sig(Fo) and 0.0536 for all 3498 data REM 259 parameters refined using 0 restraints END WGHT 0.0650 3.9221 REM Highest difference peak 2.643, deepest hole -0.373, 1-sigma level 0.098 Q1 1 0.3365 0.3847 0.4035 11.00000 0.05 2.64 Q2 1 0.1900 0.4589 0.5304 11.00000 0.05 0.65 Q3 1 0.0665 0.5747 0.6532 11.00000 0.05 0.54 Q4 1 0.2518 0.4912 0.4626 11.00000 0.05 0.43 Q5 1 0.5381 0.6141 0.9014 11.00000 0.05 0.42 ; _shelx_res_checksum 98673 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.554 _oxdiff_exptl_absorpt_empirical_full_min 0.487 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 0.14594(10) 0.60593(7) 0.58003(6) 0.0177(3) Uani 1 1 d . . . . . P1 P 0.34037(16) 0.59021(13) 0.65681(9) 0.0171(3) Uani 1 1 d . . . . . S2 S 0.0337(2) 0.29136(15) 0.69931(12) 0.0318(5) Uani 1 1 d . . . . . S1 S 0.0242(2) 0.55284(15) 0.70893(13) 0.0331(5) Uani 1 1 d . . . . . N1 N 0.1329(6) 0.4338(5) 0.5916(4) 0.0282(13) Uani 1 1 d . . . . . O1 O 0.1378(6) 0.8494(4) 0.6151(3) 0.0339(12) Uani 1 1 d . . . . . O3 O -0.1036(5) 0.6317(5) 0.4803(4) 0.0385(14) Uani 1 1 d . . . . . O2 O 0.2934(6) 0.6270(5) 0.4256(4) 0.0406(14) Uani 1 1 d . . . . . N4 N 0.4997(6) 0.4735(5) 0.7690(4) 0.0246(13) Uani 1 1 d . . . . . N2 N 0.6138(5) 0.5781(5) 0.6542(4) 0.0256(12) Uani 1 1 d . . . . . N3 N 0.5141(7) 0.6807(5) 0.7750(4) 0.0291(14) Uani 1 1 d . . . . . C16 C 0.3694(7) 0.4670(5) 0.7267(4) 0.0223(14) Uani 1 1 d . . . . . H16A H 0.298716 0.463173 0.770542 0.027 Uiso 1 1 calc R . . . . H16B H 0.364959 0.397557 0.692029 0.027 Uiso 1 1 calc R . . . . C15 C 0.6076(7) 0.4757(6) 0.7059(5) 0.0264(15) Uani 1 1 d . . . . . H15A H 0.693176 0.466612 0.736237 0.032 Uiso 1 1 calc R . . . . H15B H 0.597081 0.410637 0.667098 0.032 Uiso 1 1 calc R . . . . C7 C 0.2633(8) 0.1935(7) 0.4643(5) 0.0316(17) Uani 1 1 d . . . . . C5 C 0.1676(7) 0.3295(6) 0.5578(4) 0.0246(15) Uani 1 1 d . . . . . C12 C 0.3850(8) 0.7018(6) 0.7326(4) 0.0245(15) Uani 1 1 d . . . . . H12A H 0.389300 0.774308 0.701837 0.029 Uiso 1 1 calc R . . . . H12B H 0.314797 0.707878 0.776689 0.029 Uiso 1 1 calc R . . . . C11 C 0.4993(6) 0.5853(6) 0.5977(4) 0.0230(14) Uani 1 1 d . . . . . H11A H 0.498996 0.519482 0.559131 0.028 Uiso 1 1 calc R . . . . H11B H 0.507360 0.653539 0.562000 0.028 Uiso 1 1 calc R . . . . C9 C 0.1360(8) 0.1315(6) 0.5872(4) 0.0291(15) Uani 1 1 d . . . . . H9 H 0.099436 0.073038 0.621148 0.035 Uiso 1 1 calc R . . . . C4 C 0.0648(7) 0.4273(6) 0.6633(4) 0.0271(15) Uani 1 1 d . . . . . C8 C 0.2103(7) 0.1082(6) 0.5143(5) 0.0303(16) Uani 1 1 d . . . . . C6 C 0.2425(7) 0.3049(7) 0.4856(5) 0.0288(16) Uani 1 1 d . . . . . H6 H 0.278632 0.363370 0.451520 0.035 Uiso 1 1 calc R . . . . C2 C 0.2437(8) 0.6198(6) 0.4792(6) 0.0287(16) Uani 1 1 d . . . . . C13 C 0.6215(7) 0.6736(6) 0.7115(5) 0.0317(17) Uani 1 1 d . . . . . H13A H 0.620953 0.743136 0.676891 0.038 Uiso 1 1 calc R . . . . H13B H 0.707403 0.670555 0.742200 0.038 Uiso 1 1 calc R . . . . C14 C 0.5120(8) 0.5739(6) 0.8232(4) 0.0295(16) Uani 1 1 d . . . . . H14A H 0.447(8) 0.585(8) 0.865(5) 0.035 Uiso 1 1 d R . . . . H14B H 0.600(8) 0.570(7) 0.851(5) 0.035 Uiso 1 1 d R . . . . C10 C 0.1176(7) 0.2422(6) 0.6082(4) 0.0271(16) Uani 1 1 d . . . . . C3 C -0.0092(7) 0.6182(5) 0.5195(4) 0.0245(15) Uani 1 1 d . . . . . C1 C 0.1425(7) 0.7553(6) 0.5999(4) 0.0239(14) Uani 1 1 d . . . . . H8 H 0.228(6) 0.034(5) 0.494(4) 0.004(14) Uiso 1 1 d . . . . . H7 H 0.315(7) 0.185(6) 0.413(5) 0.015(17) Uiso 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 Mn1 0.0226(5) 0.0113(4) 0.0191(5) 0.0019(4) -0.0005(4) 0.0000(4) P1 0.0242(8) 0.0120(7) 0.0152(7) 0.0002(6) -0.0014(6) -0.0005(7) S2 0.0452(11) 0.0204(8) 0.0300(9) 0.0040(7) 0.0045(8) -0.0023(8) S1 0.0432(11) 0.0200(8) 0.0360(10) -0.0024(7) 0.0053(9) 0.0038(8) N1 0.035(3) 0.023(3) 0.027(3) -0.001(2) 0.001(3) 0.006(3) O1 0.042(3) 0.013(2) 0.046(3) -0.001(2) 0.004(3) 0.002(2) O3 0.032(3) 0.032(3) 0.052(3) 0.010(3) -0.017(3) -0.003(2) O2 0.048(3) 0.034(3) 0.039(3) 0.011(3) -0.017(3) -0.009(3) N4 0.032(3) 0.019(3) 0.022(3) 0.005(2) -0.007(2) -0.003(3) N2 0.023(3) 0.023(3) 0.030(3) 0.005(3) -0.002(2) 0.000(2) N3 0.043(4) 0.019(3) 0.025(3) -0.001(2) -0.012(3) -0.005(3) C16 0.028(4) 0.018(3) 0.021(3) 0.005(2) -0.005(3) -0.004(3) C15 0.026(4) 0.022(3) 0.031(4) 0.007(3) -0.004(3) 0.001(3) C7 0.029(4) 0.045(5) 0.021(4) -0.008(3) 0.000(3) -0.002(4) C5 0.025(3) 0.020(3) 0.029(4) -0.007(3) -0.016(3) 0.006(3) C12 0.040(4) 0.015(3) 0.018(3) -0.002(3) -0.004(3) 0.000(3) C11 0.025(3) 0.022(3) 0.022(3) 0.003(3) 0.002(2) 0.000(3) C9 0.038(4) 0.023(3) 0.027(3) 0.003(3) -0.005(3) -0.002(3) C4 0.032(4) 0.025(3) 0.024(3) -0.002(3) -0.001(3) -0.005(3) C8 0.035(4) 0.019(4) 0.037(4) -0.010(3) -0.009(3) 0.006(3) C6 0.026(4) 0.032(4) 0.028(3) 0.000(3) -0.009(3) -0.008(3) C2 0.031(4) 0.021(4) 0.035(4) -0.005(3) -0.017(3) 0.005(3) C13 0.028(4) 0.028(4) 0.039(4) 0.008(3) -0.006(3) -0.005(3) C14 0.039(4) 0.027(4) 0.022(3) 0.001(3) -0.007(3) -0.003(3) C10 0.028(4) 0.033(4) 0.020(3) -0.004(3) -0.005(3) 0.003(3) C3 0.029(4) 0.012(3) 0.033(3) 0.006(3) -0.001(3) 0.000(3) C1 0.024(3) 0.026(3) 0.022(3) 0.001(3) 0.002(3) 0.000(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' P P 0.1023 0.0942 '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 _geom_angle_publ_flag P1 Mn1 S1 88.57(7) . . ? P1 Mn1 C4 86.56(16) . . ? S1 Mn1 C4 39.15(16) . . ? N1 Mn1 P1 85.85(18) . . ? N1 Mn1 S1 68.78(17) . . ? N1 Mn1 C4 29.6(2) . . ? C2 Mn1 P1 90.0(2) . . ? C2 Mn1 S1 170.1(2) . . ? C2 Mn1 N1 101.3(3) . . ? C2 Mn1 C4 130.9(3) . . ? C3 Mn1 P1 179.7(2) . . ? C3 Mn1 S1 91.1(2) . . ? C3 Mn1 N1 94.0(3) . . ? C3 Mn1 C4 93.2(3) . . ? C3 Mn1 C2 90.3(3) . . ? C1 Mn1 P1 90.4(2) . . ? C1 Mn1 S1 95.9(2) . . ? C1 Mn1 N1 164.3(2) . . ? C1 Mn1 C4 135.0(3) . . ? C1 Mn1 C2 93.9(3) . . ? C1 Mn1 C3 89.7(3) . . ? C16 P1 Mn1 120.4(2) . . ? C12 P1 Mn1 119.0(2) . . ? C12 P1 C16 98.8(3) . . ? C12 P1 C11 97.7(3) . . ? C11 P1 Mn1 118.5(2) . . ? C11 P1 C16 97.6(3) . . ? C4 S2 C10 87.8(3) . . ? C4 S1 Mn1 76.2(2) . . ? C5 N1 Mn1 146.8(5) . . ? C4 N1 Mn1 99.6(5) . . ? C4 N1 C5 113.6(6) . . ? C15 N4 C16 110.9(5) . . ? C15 N4 C14 108.1(6) . . ? C14 N4 C16 112.2(6) . . ? C11 N2 C15 110.5(5) . . ? C13 N2 C15 108.3(5) . . ? C13 N2 C11 111.8(5) . . ? C13 N3 C12 110.7(5) . . ? C13 N3 C14 107.8(6) . . ? C14 N3 C12 111.2(6) . . ? P1 C16 H16A 109.4 . . ? P1 C16 H16B 109.4 . . ? N4 C16 P1 111.4(4) . . ? N4 C16 H16A 109.4 . . ? N4 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C15 H15A 108.6 . . ? N4 C15 H15B 108.6 . . ? N2 C15 N4 114.7(6) . . ? N2 C15 H15A 108.6 . . ? N2 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C8 C7 H7 127(4) . . ? C6 C7 C8 120.5(7) . . ? C6 C7 H7 113(4) . . ? N1 C5 C10 111.0(6) . . ? C6 C5 N1 129.2(7) . . ? C6 C5 C10 119.8(6) . . ? P1 C12 H12A 109.1 . . ? P1 C12 H12B 109.1 . . ? N3 C12 P1 112.4(5) . . ? N3 C12 H12A 109.1 . . ? N3 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? P1 C11 H11A 109.1 . . ? P1 C11 H11B 109.1 . . ? N2 C11 P1 112.6(4) . . ? N2 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C8 C9 H9 121.3 . . ? C10 C9 H9 121.3 . . ? C10 C9 C8 117.4(7) . . ? S1 C4 S2 129.5(4) . . ? N1 C4 S2 115.1(5) . . ? N1 C4 S1 115.4(5) . . ? C7 C8 C9 121.5(7) . . ? C7 C8 H8 115(4) . . ? C9 C8 H8 124(4) . . ? C7 C6 C5 118.7(7) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? O2 C2 Mn1 178.9(7) . . ? N2 C13 N3 115.0(6) . . ? N2 C13 H13A 108.5 . . ? N2 C13 H13B 108.5 . . ? N3 C13 H13A 108.5 . . ? N3 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N4 C14 N3 114.1(5) . . ? N4 C14 H14A 118(6) . . ? N4 C14 H14B 107(5) . . ? N3 C14 H14A 104(6) . . ? N3 C14 H14B 104(5) . . ? H14A C14 H14B 109(7) . . ? C5 C10 S2 112.5(5) . . ? C9 C10 S2 125.4(6) . . ? C9 C10 C5 122.1(7) . . ? O3 C3 Mn1 176.1(6) . . ? O1 C1 Mn1 177.6(6) . . ? 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 Mn1 P1 2.3049(19) . ? Mn1 S1 2.444(2) . ? Mn1 N1 2.063(6) . ? Mn1 C4 2.627(7) . ? Mn1 C2 1.867(10) . ? Mn1 C3 1.833(7) . ? Mn1 C1 1.807(7) . ? P1 C16 1.854(6) . ? P1 C12 1.838(7) . ? P1 C11 1.850(7) . ? S2 C4 1.743(7) . ? S2 C10 1.758(7) . ? S1 C4 1.707(7) . ? N1 C5 1.396(9) . ? N1 C4 1.317(9) . ? O1 C1 1.148(8) . ? O3 C3 1.143(9) . ? O2 C2 0.980(9) . ? N4 C16 1.472(9) . ? N4 C15 1.470(9) . ? N4 C14 1.471(9) . ? N2 C15 1.465(8) . ? N2 C11 1.455(8) . ? N2 C13 1.451(10) . ? N3 C12 1.481(10) . ? N3 C13 1.471(10) . ? N3 C14 1.479(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C7 C8 1.389(12) . ? C7 C6 1.385(11) . ? C7 H7 0.97(7) . ? C5 C6 1.390(11) . ? C5 C10 1.399(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C9 H9 0.9500 . ? C9 C8 1.393(11) . ? C9 C10 1.371(10) . ? C8 H8 0.96(6) . ? C6 H6 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.93(8) . ? C14 H14B 0.99(8) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.52(4) 2 0.48(4)