#------------------------------------------------------------------------------ #$Date: 2026-05-22 01:33:39 +0100 (Fri, 22 May 2026) $ #$Revision: 306061 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064414.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_7064414 loop_ _publ_author_name 'Wani, Aabid' 'Bhujbal, Shivkanya Madhavrao' 'Mehta, Kriti' 'Chourasiya, Sumit S.' 'Kathuria, Deepika' 'Gr\"utzmacher, Hansj\"org' 'W\"orle, Michael' 'Bharatam, Prasad V.' _publ_section_title ; Aminoazine-Based Unsymmetric Multidentate Ligands in Mn(II & I) Complexes and Application in Hydrophosphination Reactions ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ00370B _journal_year 2026 _chemical_formula_moiety 'C12 H17 Mn N5 O4' _chemical_formula_sum 'C12 H17 Mn N5 O4' _chemical_formula_weight 350.24 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2026-05-12 _audit_creation_method ; Olex2 1.5 (compiled 2026.04.10 svn.r48fbca5a for OlexSys, GUI svn.r7537) ; _audit_update_record ; 2026-05-14 deposited with the CCDC. 2026-05-21 downloaded from the CCDC. ; _cell_angle_alpha 73.241(3) _cell_angle_beta 83.832(3) _cell_angle_gamma 60.862(3) _cell_formula_units_Z 2 _cell_length_a 8.3343(3) _cell_length_b 8.4136(3) _cell_length_c 12.5945(4) _cell_measurement_reflns_used 12519 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 79.0240 _cell_measurement_theta_min 3.6430 _cell_volume 738.05(5) _computing_cell_refinement 'CrysAlisPro 1.171.44.140a (Rigaku OD, 2026)' _computing_data_collection 'CrysAlisPro system (CCD 42.94a 64-bit (release 21-06-2023))' _computing_data_reduction 'CrysAlisPro 1.171.44.140a (Rigaku OD, 2026)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Rigaku HyPix-6000 area detector' _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HPC area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 3.00 28.00 0.50 0.07 -- 34.00 95.00 -99.42 50 2 \w -10.00 15.00 0.50 0.07 -- 22.00 99.00 5.44 50 3 \w 5.00 30.00 0.50 0.07 -- 34.00 91.00 21.01 50 4 \w -60.00 -35.00 0.50 0.07 -- 10.00 161.00 144.07 50 5 \w -8.00 17.00 0.50 0.07 -- 22.00 99.00 179.90 50 6 \w 10.00 35.00 0.50 0.07 -- 38.00 89.00 67.27 50 7 \w 32.00 57.00 0.50 0.07 -- 50.00 76.00 122.07 50 8 \w 36.00 62.00 0.50 0.07 -- 50.00 74.00 82.29 52 9 \w 35.00 61.00 0.50 0.07 -- 58.00 77.00 28.69 52 10 \w 91.00 139.00 0.50 0.29 -- 113.25 77.00 120.00 96 11 \w 105.00 178.00 0.50 0.29 -- 113.25 77.00 30.00 146 12 \w 103.00 171.00 0.50 0.29 -- 113.25 77.00 0.00 136 13 \w 139.00 164.00 0.50 0.29 -- 113.25 77.00-180.00 50 14 \w 92.00 131.00 0.50 0.29 -- 113.25 77.00-180.00 78 15 \w 31.00 57.00 0.50 0.07 -- 54.00 77.00-122.10 52 16 \w 36.00 62.00 0.50 0.07 -- 58.00 76.00-152.88 52 17 \w 48.00 76.00 0.50 0.07 -- 47.37 38.00 -60.00 56 18 \w 34.00 60.00 0.50 0.07 -- 54.00 75.00 -90.53 52 19 \w 37.00 63.00 0.50 0.07 -- 58.00 76.00 -37.02 52 20 \w 37.00 63.00 0.50 0.07 -- 58.00 74.00 -8.23 52 21 \w 96.00 122.00 0.50 0.07 -- 54.00 74.00 -59.31 52 22 \w 35.00 61.00 0.50 0.07 -- 54.00 74.00 -59.31 52 23 \w 41.00 66.00 0.50 0.07 -- 62.00 74.00 45.39 50 24 \w 45.00 71.00 0.50 0.07 -- 66.00 73.00 70.26 52 25 \w 40.00 66.00 0.50 0.07 -- 62.00 76.00 104.70 52 26 \w 56.00 82.00 0.50 0.07 -- 78.00 75.00 124.82 52 27 \w 45.00 71.00 0.50 0.07 -- 66.00 73.00 137.82 52 28 \w 41.00 66.00 0.50 0.07 -- 62.00 74.00 172.17 50 29 \w 97.00 178.00 0.50 0.29 -- 113.25 61.00 150.00 162 30 \w 118.00 144.00 0.50 0.29 -- 113.25 45.00 -30.00 52 31 \w 103.00 170.00 0.50 0.29 -- 113.25 61.00 -60.00 134 32 \w 102.00 139.00 0.50 0.29 -- 113.25 61.00-120.00 74 33 \w 103.00 150.00 0.50 0.29 -- 113.25 61.00 -90.00 94 34 \w 128.00 177.00 0.50 0.29 -- 113.25 45.00-180.00 98 35 \w 122.00 149.00 0.50 0.29 -- 113.25 45.00 -90.00 54 36 \w 105.00 177.00 0.50 0.29 -- 113.25 45.00-120.00 144 37 \w 153.00 178.00 0.50 0.29 -- 113.25 45.00 -30.00 50 38 \w 132.00 157.00 0.50 0.29 -- 113.25 15.00-120.00 50 39 \w 113.00 138.00 0.50 0.29 -- 113.25 45.00 0.00 50 40 \w 107.00 173.00 0.50 0.29 -- 113.25 45.00 120.00 132 41 \w 109.00 164.00 0.50 0.29 -- 113.25 30.00 90.00 110 42 \w 44.00 69.00 0.50 0.29 -- 113.25 -61.00 30.00 50 43 \w 69.00 105.00 0.50 0.29 -- 113.25 -77.00 30.00 72 44 \w 74.00 104.00 0.50 0.29 -- 113.25 -77.00 -60.00 60 45 \w 45.00 90.00 0.50 0.29 -- 113.25 -77.00 -90.00 90 46 \w 43.00 92.00 0.50 0.29 -- 113.25 -77.00-150.00 98 47 \w 43.00 70.00 0.50 0.29 -- 113.25 -61.00 -60.00 54 48 \w 45.00 70.00 0.50 0.29 -- 113.25 -61.00 120.00 50 49 \w 45.00 70.00 0.50 0.29 -- 113.25 -61.00 150.00 50 50 \w 95.00 135.00 0.50 0.29 -- 113.25 125.00-107.00 80 51 \w 99.00 124.00 0.50 0.29 -- 113.25 148.00 57.00 50 52 \w 43.00 69.00 0.50 0.29 -- 113.25 -61.00 60.00 52 53 \w 43.00 70.00 0.50 0.29 -- 113.25 -61.00 -30.00 54 54 \w 50.00 104.00 0.50 0.07 -- 47.37-148.00 9.00 108 55 \w 44.00 111.00 0.50 0.29 -- 113.25-125.00-120.00 134 56 \w 94.00 126.00 0.50 0.29 -- 113.25-148.00 9.00 64 57 \w 44.00 70.00 0.50 0.29 -- 113.25-125.00 0.00 52 58 \w 45.00 70.00 0.50 0.29 -- 113.25-125.00 90.00 50 59 \w 43.00 94.00 0.50 0.29 -- 113.25 -95.00 30.00 102 60 \w 83.00 108.00 0.50 0.29 -- 113.25-125.00 90.00 50 61 \w 55.00 101.00 0.50 0.29 -- 113.25 -95.00 120.00 92 62 \w 77.00 102.00 0.50 0.29 -- 113.25-125.00 174.00 50 63 \w 44.00 93.00 0.50 0.07 -- 47.37-125.00 174.00 98 64 \w 80.00 105.00 0.50 0.29 -- 113.25 -95.00-120.00 50 65 \w 65.00 105.00 0.50 0.29 -- 113.25 -95.00-150.00 80 66 \w -26.00 25.00 0.50 0.07 -- -47.37 19.00 90.00 102 67 \w -102.00 -65.00 0.50 0.07 -- -47.37 148.00 57.00 74 68 \w -67.00 -27.00 0.50 0.07 -- -47.37 125.00-107.00 80 69 \w -72.00 -47.00 0.50 0.29 -- -91.75 125.00-107.00 50 70 \w -86.00 -38.00 0.50 0.07 -- -47.37 -19.00 -60.00 96 71 \w -73.00 -26.00 0.50 0.07 -- -47.37 -77.00 120.00 94 72 \w -62.00 -37.00 0.50 0.07 -- -47.37 -19.00 120.00 50 73 \w -121.00 -66.00 0.50 0.07 -- -47.37 -19.00 120.00 110 74 \w -52.00 -26.00 0.50 0.07 -- -47.37 -77.00 -30.00 52 75 \w -70.00 -35.00 0.50 0.07 -- -47.37 -38.00 30.00 70 76 \w -99.00 -62.00 0.50 0.07 -- -78.00 -59.00 53.99 74 77 \w -97.00 -71.00 0.50 0.29 -- -91.75 -77.00 60.00 52 78 \w -150.00-123.00 0.50 0.29 -- -91.75 -77.00 60.00 54 79 \w -96.00 -71.00 0.50 0.29 -- -91.75 -77.00 90.00 50 80 \w -94.00 -69.00 0.50 0.29 -- -91.75 -77.00 0.00 50 81 \w -98.00 -73.00 0.50 0.29 -- -91.75 -77.00-120.00 50 82 \w -68.00 -43.00 0.50 0.07 -- -66.00 -77.00-150.99 50 83 \w -94.00 -69.00 0.50 0.29 -- -91.75 -77.00-150.00 50 84 \w -95.00 -69.00 0.50 0.29 -- -91.75 -77.00-180.00 52 85 \w -126.00-100.00 0.50 0.07 -- -66.00 -77.00-150.99 52 86 \w -162.00-137.00 0.50 0.29 -- -91.75 -77.00-150.00 50 87 \w -89.00 -63.00 0.50 0.29 -- -86.00 -76.00-112.39 52 88 \w -98.00 -70.00 0.50 0.29 -- -91.75 -77.00 -60.00 56 89 \w -94.00 -64.00 0.50 0.29 -- -82.00 -75.00 -88.73 60 90 \w -84.00 -59.00 0.50 0.29 -- -82.00 -76.00 -61.68 50 91 \w -162.00-119.00 0.50 0.29 -- -90.00 -76.00 37.62 86 92 \w -94.00 -68.00 0.50 0.29 -- -90.00 -76.00 37.62 52 93 \w -96.00 -71.00 0.50 0.29 -- -91.75 -74.00 11.91 50 94 \w -86.00 -60.00 0.50 0.29 -- -82.00 -74.00 46.33 52 95 \w -85.00 -60.00 0.50 0.29 -- -82.00 -75.00 60.15 50 96 \w -101.00 -71.00 0.50 0.29 -- -91.75 -75.00 139.14 60 97 \w -161.00-124.00 0.50 0.29 -- -91.75 -75.00 139.14 74 98 \w -89.00 -62.00 0.50 0.29 -- -82.00 -73.00 15.52 54 99 \w -97.00 -71.00 0.50 0.29 -- -91.75 -71.00 -39.87 52 100 \w -103.00 -71.00 0.50 0.29 -- -91.75 -71.00 -24.49 64 101 \w -107.00 -72.00 0.50 0.29 -- -91.75 -72.00 -81.42 70 102 \w -155.00-128.00 0.50 0.29 -- -91.75 -72.00 -81.42 54 103 \w -94.00 -63.00 0.50 0.29 -- -82.00 -71.00 -14.02 62 104 \w -98.00 -72.00 0.50 0.29 -- -91.75 -70.00 105.25 52 105 \w -84.00 -58.00 0.50 0.07 -- -78.00 -71.00 138.15 52 106 \w -96.00 -71.00 0.50 0.29 -- -91.75 -71.00 162.08 50 107 \w -94.00 -69.00 0.50 0.29 -- -86.00 -63.00 164.08 50 108 \w -84.00 -59.00 0.50 0.07 -- -74.00 -64.00 150.72 50 109 \w -161.00-115.00 0.50 0.29 -- -91.75 -70.00 105.25 92 110 \w -102.00 -76.00 0.50 0.29 -- -91.75 -63.00 14.20 52 111 \w -89.00 -63.00 0.50 0.29 -- -82.00 -67.00 -8.99 52 112 \w -74.00 -48.00 0.50 0.07 -- -66.00 -64.00-117.38 52 113 \w -83.00 -57.00 0.50 0.07 -- -74.00 -63.00 -65.71 52 114 \w -86.00 -61.00 0.50 0.07 -- -78.00 -63.00 -47.86 50 115 \w -87.00 -61.00 0.50 0.07 -- -78.00 -62.00 -56.36 52 116 \w -104.00 -57.00 0.50 0.07 -- -74.00 -61.00-139.92 94 117 \w -106.00 -77.00 0.50 0.29 -- -91.75 -61.00-150.00 58 118 \w -103.00 -77.00 0.50 0.29 -- -91.75 -61.00-180.00 52 119 \w -156.00-130.00 0.50 0.29 -- -91.75 -61.00-150.00 52 120 \w -89.00 -51.00 0.50 0.07 -- -66.00 -61.00 -87.74 76 121 \w -91.00 -66.00 0.50 0.29 -- -82.00 -60.00-168.47 50 122 \w -102.00 -76.00 0.50 0.29 -- -91.75 -61.00 30.00 52 123 \w -112.00 -75.00 0.50 0.29 -- -91.75 -61.00 78.86 74 124 \w -82.00 -57.00 0.50 0.07 -- -74.00 -63.00 165.07 50 125 \w -116.00 -91.00 0.50 0.29 -- -91.75 -95.00 60.00 50 126 \w -112.00 -67.00 0.50 0.07 -- -47.37-148.00 9.00 90 127 \w -149.00 -77.00 0.50 0.29 -- -91.75-148.00 9.00 144 128 \w -122.00 -96.00 0.50 0.29 -- -91.75-125.00 174.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0687750000 _diffrn_orient_matrix_UB_12 -0.1658883000 _diffrn_orient_matrix_UB_13 0.1061475000 _diffrn_orient_matrix_UB_21 -0.0600599000 _diffrn_orient_matrix_UB_22 0.1406983000 _diffrn_orient_matrix_UB_23 0.0704814000 _diffrn_orient_matrix_UB_31 -0.1910978000 _diffrn_orient_matrix_UB_32 0.0117029000 _diffrn_orient_matrix_UB_33 0.0104665000 _diffrn_radiation_monochromator 'multi-layer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_unetI/netI 0.0244 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 21434 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.019 _diffrn_reflns_theta_min 3.668 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type PhotonJet-S _exptl_absorpt_coefficient_mu 7.526 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.44.140a (Rigaku Oxford Diffraction, 2026) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light red' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.576 _exptl_crystal_description block _exptl_crystal_F_000 362 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.357 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 218 _refine_ls_number_reflns 3124 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0284 _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^)+(0.0425P)^2^+0.3133P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.0805 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3006 _reflns_number_total 3124 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj00370b2.cif _cod_data_source_block aa310_auto _cod_database_code 7064414 _shelx_shelxl_version_number 2019/1 _chemical_oxdiff_formula C12H17MnN5O4 _chemical_oxdiff_usercomment 'yellow plate' _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. ; _cell_oxdiff_angle_alpha 73.241(3) _cell_oxdiff_angle_beta 83.832(3) _cell_oxdiff_angle_gamma 60.862(3) _cell_oxdiff_length_a 8.3343(3) _cell_oxdiff_length_b 8.4136(3) _cell_oxdiff_length_c 12.5945(4) _cell_oxdiff_measurement_reflns_used 12519 _cell_oxdiff_volume 738.04(4) _shelx_estimated_absorpt_t_max 0.584 _shelx_estimated_absorpt_t_min 0.379 _diffrn_oxdiff_digest_od_ed ; ; _diffrn_oxdiff_measurement_exp_name aa310.par _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3A), C4(H4) 2.b Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C) ; _shelx_res_file ; TITL aa310_auto_a.res in P-1 aa310_auto.res created by SHELXL-2019/1 at 10:19:07 on 12-May-2026 REM Old TITL aa310_auto in P-1 REM SHELXT solution in P-1: R1 0.101, Rweak 0.012, Alpha 0.031 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C13 Mn N5 O3 CELL 1.54184 8.3343 8.4136 12.5945 73.241 83.832 60.862 ZERR 2 0.0003 0.0003 0.0004 0.003 0.003 0.003 LATT 1 SFAC C H Mn N O UNIT 24 34 2 10 8 L.S. 10 PLAN 5 SIZE 0.08 0.12 0.16 TEMP -173 CONF LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.042500 0.313300 FVAR 8.29366 MN1 3 0.688099 0.371254 0.768844 11.00000 0.01756 0.02109 = 0.01879 -0.00584 -0.00003 -0.01274 O1 5 0.672500 0.649208 0.708171 11.00000 0.02458 0.02403 = 0.01898 -0.00629 -0.00161 -0.01447 O2 5 0.764332 0.518356 0.884727 11.00000 0.02324 0.02282 = 0.01988 -0.00519 -0.00012 -0.01440 O3 5 0.893616 0.092640 0.842508 11.00000 0.01903 0.02534 = 0.02815 -0.00651 0.00021 -0.01368 O4 5 1.062543 0.231324 0.770673 11.00000 0.02252 0.02741 = 0.02500 -0.00741 0.00043 -0.01658 N1 4 0.756970 0.325767 0.590678 11.00000 0.01735 0.02075 = 0.01915 -0.00481 -0.00087 -0.01137 N2 4 0.481817 0.310567 0.700738 11.00000 0.01628 0.01993 = 0.01770 -0.00493 0.00052 -0.01113 N3 4 0.346054 0.309330 0.770035 11.00000 0.01912 0.02732 = 0.01879 -0.00968 0.00317 -0.01699 H3 2 0.270877 0.279955 0.758777 11.00000 0.03327 N4 4 0.183824 0.398392 0.920186 11.00000 0.02158 0.03799 = 0.02042 -0.01329 0.00357 -0.01910 H4A 2 0.181270 0.424271 0.980677 11.00000 0.03177 H4B 2 0.104166 0.370328 0.901873 11.00000 0.03565 N5 4 0.459848 0.413593 0.878262 11.00000 0.01919 0.02946 = 0.02099 -0.01190 0.00146 -0.01480 H5 2 0.437919 0.452498 0.938536 11.00000 0.03303 C1 1 0.897007 0.339877 0.534404 11.00000 0.01931 0.02504 = 0.02367 -0.00533 -0.00090 -0.01452 AFIX 43 H1 2 0.963126 0.383028 0.564813 11.00000 -1.20000 AFIX 0 C2 1 0.951389 0.295200 0.434229 11.00000 0.01912 0.02915 = 0.02395 -0.00686 0.00290 -0.01399 AFIX 43 H2 2 1.051830 0.307338 0.396979 11.00000 -1.20000 AFIX 0 C3 1 0.854235 0.232072 0.390035 11.00000 0.02215 0.02888 = 0.01980 -0.00832 0.00333 -0.01389 AFIX 43 H3A 2 0.888235 0.198518 0.322050 11.00000 -1.20000 AFIX 0 C4 1 0.707095 0.218735 0.446484 11.00000 0.02088 0.02415 = 0.02050 -0.00765 0.00084 -0.01293 AFIX 43 H4 2 0.638048 0.177628 0.416997 11.00000 -1.20000 AFIX 0 C5 1 0.661464 0.266111 0.546730 11.00000 0.01543 0.01680 = 0.01968 -0.00279 -0.00181 -0.00898 C6 1 0.506294 0.256051 0.612081 11.00000 0.01687 0.01769 = 0.01736 -0.00325 -0.00144 -0.00986 C7 1 0.398940 0.179242 0.575980 11.00000 0.02124 0.02868 = 0.02052 -0.01077 0.00253 -0.01646 AFIX 137 H7A 2 0.470983 0.041129 0.593711 11.00000 -1.50000 H7B 2 0.372315 0.231617 0.495760 11.00000 -1.50000 H7C 2 0.283301 0.214741 0.614857 11.00000 -1.50000 AFIX 0 C8 1 0.332395 0.376578 0.860102 11.00000 0.01801 0.01913 = 0.01799 -0.00530 0.00004 -0.00932 C9 1 0.726228 0.652637 0.797793 11.00000 0.01439 0.02190 = 0.02036 -0.00729 0.00149 -0.01017 C10 1 0.744426 0.821726 0.799587 11.00000 0.02926 0.02301 = 0.02480 -0.00548 -0.00316 -0.01575 AFIX 137 H10A 2 0.637925 0.904390 0.834802 11.00000 -1.50000 H10B 2 0.750106 0.891607 0.723412 11.00000 -1.50000 H10C 2 0.857065 0.778999 0.841712 11.00000 -1.50000 AFIX 0 C11 1 1.047179 0.089431 0.827936 11.00000 0.02064 0.02464 = 0.01974 -0.00905 0.00141 -0.01242 C12 1 1.216909 -0.090949 0.881097 11.00000 0.02186 0.02950 = 0.03510 -0.00422 -0.00207 -0.00782 AFIX 137 H12A 2 1.270969 -0.069344 0.937340 11.00000 -1.50000 H12B 2 1.306477 -0.130211 0.824248 11.00000 -1.50000 H12C 2 1.183453 -0.190374 0.916209 11.00000 -1.50000 AFIX 0 HKLF 4 REM aa310_auto_a.res in P-1 REM wR2 = 0.0805, GooF = S = 1.126, Restrained GooF = 1.126 for all data REM R1 = 0.0284 for 3006 Fo > 4sig(Fo) and 0.0299 for all 3124 data REM 218 parameters refined using 0 restraints END WGHT 0.0425 0.3133 REM Highest difference peak 0.357, deepest hole -0.442, 1-sigma level 0.055 Q1 1 0.7241 0.3757 0.6856 11.00000 0.05 0.36 Q2 1 0.6584 0.3734 0.8419 11.00000 0.05 0.30 Q3 1 0.5780 0.2679 0.5726 11.00000 0.05 0.28 Q4 1 0.6754 0.2549 0.4960 11.00000 0.05 0.27 Q5 1 0.9354 0.3019 0.4786 11.00000 0.05 0.25 ; _shelx_res_checksum 54606 _shelx_hkl_file ; 0 0 -1 7767.85 388.225 75 0 0 1 8149.93 408.622 66 0 0 2 249055. 10668.4 15 0 0 2 256490. 10723.4 66 0 0 -2 238985. 10674.6 75 0 0 -2 253383. 10649.5 6 0 0 2 246232. 10610.3 1 0 0 3 447433. 19246.4 82 0 0 3 449688. 19224.9 66 0 0 -3 447603. 19183.5 23 0 0 3 443423. 19147.1 15 0 0 -3 443453. 19114.0 6 0 0 -4 2134.69 330.267 23 0 0 4 1943.99 329.416 82 0 0 4 1771.90 237.897 15 0 0 4 1980.71 331.651 66 0 0 -4 1820.89 275.351 76 0 0 -5 57546.3 2567.58 23 0 0 -5 52649.3 2498.03 76 0 0 5 52935.5 2590.20 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45 -9 -6 0 2309.51 333.860 64 -9 -6 -1 946.538 308.472 56 -9 -6 -1 515.414 260.613 45 -9 -6 -1 991.731 303.385 64 -9 -6 -2 7075.70 486.279 45 -9 -6 -2 6940.17 487.558 65 -9 -6 -2 7294.00 549.366 56 -9 -6 -3 528.894 223.553 46 -9 -6 -4 2418.99 261.863 55 -9 -6 -4 2384.17 330.014 56 -9 -6 -4 2019.16 283.988 65 -9 -6 -4 2651.69 300.774 46 -9 -6 -5 2279.59 305.376 56 -9 -6 -5 2373.34 252.402 55 -9 -6 -5 2531.28 280.995 65 -9 -6 -5 2906.96 295.149 46 -9 -6 -6 1610.04 195.242 55 -9 -6 -6 1581.82 243.335 56 -9 -6 -6 1403.33 227.443 65 -9 -6 -6 1986.63 257.419 46 -9 -6 -7 515.464 131.609 55 -9 -6 -7 498.959 196.179 46 -9 -6 -7 630.424 177.187 65 -9 -6 -8 6384.25 393.210 46 -9 -6 -8 6279.68 368.637 65 -9 -6 -9 3919.16 241.190 65 -9 -6 -10 3430.96 210.714 64 -9 -7 3 10996.6 583.958 44 -9 -7 2-50.6652 244.698 44 -9 -7 2-6.13523 114.182 56 -9 -7 1 3308.81 352.937 44 -9 -7 1 3155.81 294.117 56 -9 -7 0 1125.93 270.357 56 -9 -7 0 1097.77 294.176 44 -9 -7 0 800.861 257.788 45 -9 -7 -1 7532.94 509.196 44 -9 -7 -1 8126.80 548.274 56 -9 -7 -1 7432.37 507.933 45 -9 -7 -1 7374.78 503.550 64 -9 -7 -2 1131.25 309.131 56 -9 -7 -2 987.165 279.968 45 -9 -7 -2 1126.65 266.232 64 -9 -7 -3 2256.46 313.168 45 -9 -7 -3 2002.25 296.796 64 -9 -7 -4 3712.08 357.602 45 -9 -7 -4 3929.62 355.091 64 -9 -7 -4 3499.24 320.372 65 -9 -7 -4 4221.02 390.245 56 -9 -7 -5 4921.71 384.150 45 -9 -7 -5 5063.19 377.975 46 -9 -7 -5 5268.45 413.841 56 -9 -7 -5 5620.20 405.769 64 -9 -7 -5 5322.93 369.745 65 -9 -7 -6 1944.09 249.404 56 -9 -7 -6 1731.85 213.269 65 -9 -7 -6 1580.73 256.549 64 -9 -7 -7 189.626 131.407 65 -9 -7 -7 206.539 182.690 64 -9 -7 -8 961.486 143.484 65 -9 -7 -8 1129.18 190.722 64 -9 -7 -9 161.299 111.027 46 -9 -7 -9 144.029 111.810 64 -9 -8 2 551.421 142.477 44 -9 -8 1 5892.12 368.596 44 -9 -8 0 6853.05 410.525 56 -9 -8 0 7546.64 446.526 44 -9 -8 -1 9470.67 540.182 44 -9 -8 -1 9113.50 538.350 56 -9 -8 -1 9215.55 522.084 45 -9 -8 -2 715.929 241.047 56 -9 -8 -2 758.735 223.816 45 -9 -8 -3 29480.7 1349.62 45 -9 -8 -3 30020.4 1397.85 56 -9 -8 -3 26951.8 1334.23 64 -9 -8 -4 206.369 201.911 45 -9 -8 -4 90.6033 166.713 64 -9 -8 -5 1987.63 266.316 56 -9 -8 -5 2124.71 251.213 45 -9 -8 -5 1586.37 220.230 64 -9 -8 -6 1426.61 209.119 56 -9 -8 -6 1833.74 197.174 64 -9 -8 -6 1756.96 216.537 45 -9 -8 -7 2327.14 201.483 64 -9 -8 -8 8268.65 406.984 64 -9 -9 -1 2566.51 179.284 44 -9 -9 -2 5684.30 323.667 56 -9 -9 -2 5896.89 317.021 44 -9 -9 -3 7542.06 415.482 56 -9 -9 -4 4569.58 282.234 45 -9 -9 -5 7606.32 405.823 56 -9 -9 -5 7299.12 386.909 45 -9 -9 -6 3163.38 206.239 56 -9 -9 -6 3644.61 211.516 45 -10 -3 -4 784.885 120.503 55 -10 -4 -3 897.755 186.796 55 -10 -4 -4 3046.69 221.063 65 -10 -4 -4 3050.98 245.983 55 -10 -4 -5 1099.82 136.323 65 -10 -4 -5 1193.88 156.430 55 -10 -4 -6 3828.23 220.986 55 -10 -5 -3 11764.2 635.805 64 -10 -5 -3 12839.9 635.624 65 -10 -5 -4 7685.78 440.655 64 -10 -5 -4 7960.48 443.988 65 -10 -5 -5 27674.0 1297.41 64 -10 -5 -5 29656.0 1312.95 65 -10 -6 -1 5575.90 385.948 56 -10 -6 -2 491.464 185.090 64 -10 -6 -2 246.549 189.245 56 -10 -6 -3 19619.5 961.913 64 -10 -6 -4 937.539 195.825 64 -10 -6 -4 960.466 160.080 65 -10 -6 -5 19676.8 943.052 64 -10 -6 -6 2668.99 218.705 64 -10 -6 -6 2773.56 203.060 65 -10 -7 -1 313.240 158.945 56 -10 -7 -2 2820.62 257.779 56 -10 -7 -4 15814.7 775.474 56 -10 -7 -6 1612.37 157.380 64 -10 -8 -2 8636.51 424.839 56 -10 -8 -3 5202.51 292.875 56 0 0 0 0.00 0.00 0 TITL aa310_auto in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.334328 8.413569 12.594497 73.2410 83.8322 60.8620 ZERR 1.00 0.000289 0.000257 0.000368 0.0026 0.0026 0.0034 LATT 1 SFAC C H Mn N O UNIT 12.00 17.00 1.00 5.00 4.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.08 0.12 0.16 TREF HKLF 4 END ; _shelx_hkl_checksum 89071 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.740 _oxdiff_exptl_absorpt_empirical_full_min 0.635 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 0.68810(3) 0.37125(4) 0.76884(2) 0.01744(10) Uani 1 1 d . . . . . O1 O 0.67250(17) 0.64921(17) 0.70817(10) 0.0210(3) Uani 1 1 d . . . . . O2 O 0.76433(17) 0.51836(17) 0.88473(10) 0.0206(2) Uani 1 1 d . . . . . O3 O 0.89362(17) 0.09264(17) 0.84251(11) 0.0229(3) Uani 1 1 d . . . . . O4 O 1.06254(17) 0.23132(18) 0.77067(10) 0.0228(3) Uani 1 1 d . . . . . N1 N 0.75697(19) 0.32577(19) 0.59068(12) 0.0181(3) Uani 1 1 d . . . . . N2 N 0.48182(19) 0.31057(19) 0.70074(11) 0.0169(3) Uani 1 1 d . . . . . N3 N 0.3461(2) 0.3093(2) 0.77003(12) 0.0185(3) Uani 1 1 d . . . . . H3 H 0.271(4) 0.280(3) 0.759(2) 0.033(6) Uiso 1 1 d . . . . . N4 N 0.1838(2) 0.3984(2) 0.92019(13) 0.0235(3) Uani 1 1 d . . . . . H4A H 0.181(3) 0.424(3) 0.981(2) 0.032(6) Uiso 1 1 d . . . . . H4B H 0.104(4) 0.370(4) 0.902(2) 0.036(6) Uiso 1 1 d . . . . . N5 N 0.4598(2) 0.4136(2) 0.87826(12) 0.0207(3) Uani 1 1 d . . . . . H5 H 0.438(3) 0.452(3) 0.939(2) 0.033(6) Uiso 1 1 d . . . . . C1 C 0.8970(2) 0.3399(2) 0.53440(15) 0.0211(3) Uani 1 1 d . . . . . H1 H 0.963126 0.383028 0.564813 0.025 Uiso 1 1 calc R U . . . C2 C 0.9514(2) 0.2952(3) 0.43423(15) 0.0233(4) Uani 1 1 d . . . . . H2 H 1.051830 0.307338 0.396979 0.028 Uiso 1 1 calc R U . . . C3 C 0.8542(2) 0.2321(3) 0.39004(15) 0.0227(4) Uani 1 1 d . . . . . H3A H 0.888235 0.198518 0.322050 0.027 Uiso 1 1 calc R U . . . C4 C 0.7071(2) 0.2187(2) 0.44648(14) 0.0205(3) Uani 1 1 d . . . . . H4 H 0.638048 0.177628 0.416997 0.025 Uiso 1 1 calc R U . . . C5 C 0.6615(2) 0.2661(2) 0.54673(13) 0.0170(3) Uani 1 1 d . . . . . C6 C 0.5063(2) 0.2561(2) 0.61208(13) 0.0168(3) Uani 1 1 d . . . . . C7 C 0.3989(2) 0.1792(3) 0.57598(14) 0.0207(3) Uani 1 1 d . . . . . H7A H 0.470983 0.041129 0.593711 0.031 Uiso 1 1 calc R U . . . H7B H 0.372315 0.231617 0.495760 0.031 Uiso 1 1 calc R U . . . H7C H 0.283301 0.214741 0.614857 0.031 Uiso 1 1 calc R U . . . C8 C 0.3324(2) 0.3766(2) 0.86010(14) 0.0181(3) Uani 1 1 d . . . . . C9 C 0.7262(2) 0.6526(2) 0.79779(14) 0.0179(3) Uani 1 1 d . . . . . C10 C 0.7444(3) 0.8217(2) 0.79959(15) 0.0241(4) Uani 1 1 d . . . . . H10A H 0.637925 0.904390 0.834802 0.036 Uiso 1 1 calc R U . . . H10B H 0.750106 0.891607 0.723412 0.036 Uiso 1 1 calc R U . . . H10C H 0.857065 0.778999 0.841712 0.036 Uiso 1 1 calc R U . . . C11 C 1.0472(2) 0.0894(2) 0.82794(14) 0.0203(3) Uani 1 1 d . . . . . C12 C 1.2169(3) -0.0909(3) 0.88110(18) 0.0316(4) Uani 1 1 d . . . . . H12A H 1.270969 -0.069344 0.937340 0.047 Uiso 1 1 calc R U . . . H12B H 1.306477 -0.130211 0.824248 0.047 Uiso 1 1 calc R U . . . H12C H 1.183453 -0.190374 0.916209 0.047 Uiso 1 1 calc 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 Mn1 0.01756(15) 0.02109(15) 0.01879(15) -0.00584(10) -0.00003(10) -0.01274(11) O1 0.0246(6) 0.0240(6) 0.0190(6) -0.0063(5) -0.0016(5) -0.0145(5) O2 0.0232(6) 0.0228(6) 0.0199(6) -0.0052(5) -0.0001(5) -0.0144(5) O3 0.0190(6) 0.0253(6) 0.0282(6) -0.0065(5) 0.0002(5) -0.0137(5) O4 0.0225(6) 0.0274(6) 0.0250(6) -0.0074(5) 0.0004(5) -0.0166(5) N1 0.0173(7) 0.0208(7) 0.0191(7) -0.0048(5) -0.0009(5) -0.0114(6) N2 0.0163(7) 0.0199(6) 0.0177(6) -0.0049(5) 0.0005(5) -0.0111(5) N3 0.0191(7) 0.0273(7) 0.0188(7) -0.0097(6) 0.0032(5) -0.0170(6) N4 0.0216(8) 0.0380(9) 0.0204(7) -0.0133(6) 0.0036(6) -0.0191(7) N5 0.0192(7) 0.0295(7) 0.0210(7) -0.0119(6) 0.0015(6) -0.0148(6) C1 0.0193(8) 0.0250(8) 0.0237(8) -0.0053(7) -0.0009(6) -0.0145(7) C2 0.0191(8) 0.0292(9) 0.0240(9) -0.0069(7) 0.0029(7) -0.0140(7) C3 0.0222(9) 0.0289(9) 0.0198(8) -0.0083(7) 0.0033(7) -0.0139(7) C4 0.0209(8) 0.0241(8) 0.0205(8) -0.0077(6) 0.0008(6) -0.0129(7) C5 0.0154(8) 0.0168(7) 0.0197(8) -0.0028(6) -0.0018(6) -0.0090(6) C6 0.0169(8) 0.0177(7) 0.0174(7) -0.0032(6) -0.0014(6) -0.0099(6) C7 0.0212(8) 0.0287(9) 0.0205(8) -0.0108(7) 0.0025(6) -0.0165(7) C8 0.0180(8) 0.0191(7) 0.0180(8) -0.0053(6) 0.0000(6) -0.0093(6) C9 0.0144(8) 0.0219(8) 0.0204(8) -0.0073(6) 0.0015(6) -0.0102(6) C10 0.0293(10) 0.0230(8) 0.0248(9) -0.0055(7) -0.0032(7) -0.0157(7) C11 0.0206(8) 0.0246(8) 0.0197(8) -0.0091(6) 0.0014(6) -0.0124(7) C12 0.0219(9) 0.0295(10) 0.0351(10) -0.0042(8) -0.0021(8) -0.0078(8) 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' 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 -1 0.0266 3 0 -6 0.0796 -5 -3 0 0.0791 5 3 0 0.0686 -3 -3 -7 0.0614 0 -4 -7 0.0488 0 -5 -2 0.0486 0 -4 0 0.0419 0 0 8 0.0495 -3 3 2 0.0501 0 5 2 0.0514 -3 0 -6 0.0425 -3 -5 0 0.0578 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 Mn1 O2 56.35(4) . . ? O1 Mn1 N1 90.24(5) . . ? O1 Mn1 N2 120.30(5) . . ? O3 Mn1 O1 136.14(5) . . ? O3 Mn1 O2 95.24(5) . . ? O3 Mn1 N1 91.35(5) . . ? O3 Mn1 N2 100.50(5) . . ? O3 Mn1 N5 104.12(5) . . ? N1 Mn1 O2 136.26(5) . . ? N2 Mn1 O2 151.46(5) . . ? N2 Mn1 N1 67.34(5) . . ? N5 Mn1 O1 104.35(5) . . ? N5 Mn1 O2 83.07(5) . . ? N5 Mn1 N1 136.67(5) . . ? N5 Mn1 N2 70.11(5) . . ? C9 O1 Mn1 97.39(10) . . ? C9 O2 Mn1 84.77(9) . . ? C11 O3 Mn1 107.74(11) . . ? C1 N1 Mn1 122.93(11) . . ? C1 N1 C5 118.08(14) . . ? C5 N1 Mn1 118.72(11) . . ? N3 N2 Mn1 114.62(10) . . ? C6 N2 Mn1 123.36(11) . . ? C6 N2 N3 121.33(14) . . ? N2 N3 H3 124.4(18) . . ? N2 N3 C8 115.10(14) . . ? C8 N3 H3 120.3(18) . . ? H4A N4 H4B 123(2) . . ? C8 N4 H4A 115.8(16) . . ? C8 N4 H4B 120.8(17) . . ? Mn1 N5 H5 129.1(16) . . ? C8 N5 Mn1 120.70(12) . . ? C8 N5 H5 110.2(16) . . ? N1 C1 H1 118.1 . . ? N1 C1 C2 123.83(16) . . ? C2 C1 H1 118.1 . . ? C1 C2 H2 121.1 . . ? C1 C2 C3 117.89(16) . . ? C3 C2 H2 121.1 . . ? C2 C3 H3A 120.4 . . ? C4 C3 C2 119.14(16) . . ? C4 C3 H3A 120.4 . . ? C3 C4 H4 120.3 . . ? C3 C4 C5 119.41(16) . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.65(15) . . ? N1 C5 C6 115.56(14) . . ? C4 C5 C6 122.79(15) . . ? N2 C6 C5 113.90(14) . . ? N2 C6 C7 125.64(15) . . ? C5 C6 C7 120.40(14) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 N3 114.81(15) . . ? N5 C8 N3 118.51(15) . . ? N5 C8 N4 126.68(16) . . ? O1 C9 C10 118.99(15) . . ? O2 C9 O1 121.47(15) . . ? O2 C9 C10 119.54(15) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C11 O4 122.13(16) . . ? O3 C11 C12 118.32(16) . . ? O4 C11 C12 119.55(16) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 O1 2.1828(12) . ? Mn1 O2 2.4642(12) . ? Mn1 O3 2.1135(13) . ? Mn1 N1 2.3485(14) . ? Mn1 N2 2.3187(14) . ? Mn1 N5 2.1690(15) . ? O1 C9 1.271(2) . ? O2 C9 1.260(2) . ? O3 C11 1.261(2) . ? O4 C11 1.263(2) . ? N1 C1 1.337(2) . ? N1 C5 1.355(2) . ? N2 N3 1.355(2) . ? N2 C6 1.286(2) . ? N3 H3 0.81(3) . ? N3 C8 1.378(2) . ? N4 H4A 0.85(3) . ? N4 H4B 0.88(3) . ? N4 C8 1.341(2) . ? N5 H5 0.88(3) . ? N5 C8 1.301(2) . ? C1 H1 0.9500 . ? C1 C2 1.387(3) . ? C2 H2 0.9500 . ? C2 C3 1.391(3) . ? C3 H3A 0.9500 . ? C3 C4 1.387(3) . ? C4 H4 0.9500 . ? C4 C5 1.392(2) . ? C5 C6 1.481(2) . ? C6 C7 1.498(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C10 1.509(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.510(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 Mn1 O1 C9 O2 -1.37(18) . . . . ? Mn1 O1 C9 C10 178.66(13) . . . . ? Mn1 O2 C9 O1 1.21(15) . . . . ? Mn1 O2 C9 C10 -178.82(15) . . . . ? Mn1 O3 C11 O4 -4.93(19) . . . . ? Mn1 O3 C11 C12 175.13(13) . . . . ? Mn1 N1 C1 C2 173.27(13) . . . . ? Mn1 N1 C5 C4 -173.64(12) . . . . ? Mn1 N1 C5 C6 6.65(18) . . . . ? Mn1 N2 N3 C8 11.01(17) . . . . ? Mn1 N2 C6 C5 -9.75(19) . . . . ? Mn1 N2 C6 C7 167.43(12) . . . . ? Mn1 N5 C8 N3 0.2(2) . . . . ? Mn1 N5 C8 N4 -179.18(14) . . . . ? N1 C1 C2 C3 0.0(3) . . . . ? N1 C5 C6 N2 1.6(2) . . . . ? N1 C5 C6 C7 -175.70(14) . . . . ? N2 N3 C8 N4 171.64(14) . . . . ? N2 N3 C8 N5 -7.8(2) . . . . ? N3 N2 C6 C5 -179.72(13) . . . . ? N3 N2 C6 C7 -2.5(2) . . . . ? C1 N1 C5 C4 0.6(2) . . . . ? C1 N1 C5 C6 -179.14(14) . . . . ? C1 C2 C3 C4 0.8(3) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C3 C4 C5 N1 0.2(3) . . . . ? C3 C4 C5 C6 179.91(15) . . . . ? C4 C5 C6 N2 -178.06(15) . . . . ? C4 C5 C6 C7 4.6(2) . . . . ? C5 N1 C1 C2 -0.7(2) . . . . ? C6 N2 N3 C8 -178.20(14) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0005 1.0003 -0.9988 -0.2720 0.0704 0.0014 3.0818 0.1289 -6.1552 -0.4628 -0.6008 -0.6518 -5.3502 -2.5682 0.3146 0.0915 -0.0178 0.9956 5.3507 2.5649 -0.3109 -0.0905 0.0176 -0.9957 -3.3742 -3.4980 -6.7181 -0.3649 -0.7630 0.5336 -0.0303 -3.6045 -6.8186 -0.1279 -0.9859 -0.1078 -0.0484 -4.7935 -2.1233 0.5665 -0.8212 -0.0691 0.0556 -4.4929 0.4131 0.7930 -0.6064 -0.0589 -0.0142 0.0756 7.8567 0.8205 0.5652 0.0858 -2.6484 2.8546 1.7562 -0.4693 0.6845 0.5579 -0.0264 4.7569 2.1249 -0.5654 0.8206 0.0830 -2.9395 -0.0177 -5.9517 -0.8310 -0.2454 0.4992 -2.6288 -5.3068 -0.4417 0.6527 -0.6199 0.4356