#------------------------------------------------------------------------------ #$Date: 2026-05-22 01:33:39 +0100 (Fri, 22 May 2026) $ #$Revision: 306061 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064415.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_7064415 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 'C8 H11 Cl2 Mn N5' _chemical_formula_sum 'C8 H11 Cl2 Mn N5' _chemical_formula_weight 303.06 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens 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 90 _cell_angle_beta 92.2570(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.62890(10) _cell_length_b 15.5631(2) _cell_length_c 11.48390(10) _cell_measurement_reflns_used 8853 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 76.5850 _cell_measurement_theta_min 4.7770 _cell_volume 1183.83(3) _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 'SHELXL 2025/1 (Sheldrick, 2015)' _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 0.999 _diffrn_measured_fraction_theta_max 0.952 _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 35.00 93.00 0.50 0.06 -- 47.37-125.00 150.00 116 2 \w 41.00 82.00 0.50 0.23 -- 105.94 -95.00 60.00 82 3 \w 35.00 76.00 0.50 0.23 -- 105.94 -77.00 60.00 82 4 \w 80.00 105.00 0.50 0.23 -- 105.94 -77.00 60.00 50 5 \w 45.00 105.00 0.50 0.23 -- 105.94 -77.00 -30.00 120 6 \w 33.00 68.00 0.50 0.23 -- 105.94 -61.00 0.00 70 7 \w 34.00 66.00 0.50 0.23 -- 105.94 -65.00 -59.00 64 8 \w 35.00 71.00 0.50 0.23 -- 105.94 -61.00-120.00 72 9 \w 55.00 104.00 0.50 0.23 -- 105.94 -95.00-150.00 98 10 \w 35.00 69.00 0.50 0.23 -- 105.94 -61.00-180.00 68 11 \w -24.00 24.00 0.50 0.06 -- 47.37 -65.00 -59.00 96 12 \w 33.00 67.00 0.50 0.23 -- 105.94 -61.00 -90.00 68 13 \w 33.00 71.00 0.50 0.23 -- 105.94 -61.00 -30.00 76 14 \w 33.00 71.00 0.50 0.23 -- 105.94 -61.00 90.00 76 15 \w 35.00 70.00 0.50 0.06 -- 47.37 38.00 150.00 70 16 \w 53.00 79.00 0.50 0.06 -- 47.37 65.00 76.00 52 17 \w 84.00 147.00 0.50 0.23 -- 105.94 77.00 0.00 126 18 \w 109.00 134.00 0.50 0.23 -- 105.94 65.00 76.00 50 19 \w 78.00 104.00 0.50 0.06 -- 47.37 38.00 150.00 52 20 \w -64.00 -13.00 0.50 0.06 -- -47.37 65.00 76.00 102 21 \w -51.00 -25.00 0.50 0.23 -- -91.75 65.00 76.00 52 22 \w -50.00 -23.00 0.50 0.23 -- -91.75 45.00 120.00 54 23 \w -39.00 25.00 0.50 0.06 -- -47.37 38.00 -60.00 128 24 \w -50.00 -20.00 0.50 0.23 -- -91.75 45.00-150.00 60 25 \w -51.00 -24.00 0.50 0.23 -- -91.75 45.00-180.00 54 26 \w -85.00 -51.00 0.50 0.06 -- -47.37 125.00-180.00 68 27 \w -86.00 -37.00 0.50 0.06 -- -47.37 -38.00-180.00 98 28 \w -47.00 -14.00 0.50 0.06 -- -47.37 125.00-180.00 66 29 \w -117.00 -59.00 0.50 0.06 -- -47.37 -65.00 -59.00 116 30 \w -112.00 -83.00 0.50 0.23 -- -91.75 -77.00-120.00 58 31 \w -162.00 -69.00 0.50 0.23 -- -91.75 -77.00-150.00 186 32 \w -150.00-123.00 0.50 0.23 -- -91.75 -77.00-120.00 54 33 \w -166.00 -82.00 0.50 0.23 -- -91.75 -30.00-120.00 168 34 \w -155.00-129.00 0.50 0.23 -- -91.75 -15.00-180.00 52 35 \w -122.00 -84.00 0.50 0.23 -- -91.75 -15.00-180.00 76 36 \w -162.00 -91.00 0.50 0.23 -- -91.75 -65.00 -59.00 142 37 \w -150.00-101.00 0.50 0.23 -- -91.75 -45.00 0.00 98 38 \w -163.00 -79.00 0.50 0.23 -- -91.75 -45.00 150.00 168 39 \w -164.00-125.00 0.50 0.23 -- -91.75 -15.00 150.00 78 ; _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 -0.0541956000 _diffrn_orient_matrix_UB_12 -0.0731659000 _diffrn_orient_matrix_UB_13 -0.0860303000 _diffrn_orient_matrix_UB_21 -0.2055698000 _diffrn_orient_matrix_UB_22 -0.0108762000 _diffrn_orient_matrix_UB_23 0.0562562000 _diffrn_orient_matrix_UB_31 -0.0943480000 _diffrn_orient_matrix_UB_32 0.0657948000 _diffrn_orient_matrix_UB_33 -0.0863363000 _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 0.0336 _diffrn_reflns_av_unetI/netI 0.0212 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14177 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.795 _diffrn_reflns_theta_min 4.788 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type PhotonJet-S _exptl_absorpt_coefficient_mu 13.067 _exptl_absorpt_correction_T_max 0.953 _exptl_absorpt_correction_T_min 0.283 _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 1.700 _exptl_crystal_description block _exptl_crystal_F_000 612 _exptl_crystal_size_max 0.226 _exptl_crystal_size_mid 0.115 _exptl_crystal_size_min 0.084 _refine_diff_density_max 0.358 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 162 _refine_ls_number_reflns 2382 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0224 _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^)+(0.0280P)^2^+0.5982P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.0593 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2280 _reflns_number_total 2382 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj00370b2.cif _cod_data_source_block aa-3-2_auto _cod_database_code 7064415 _shelx_shelxl_version_number 2025/1 _chemical_oxdiff_formula C8H11Cl2MnN5 _chemical_oxdiff_usercomment 'Methanol-ether, yellow/orange block' _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 90.0099(15) _cell_oxdiff_angle_beta 92.2826(15) _cell_oxdiff_angle_gamma 89.9834(15) _cell_oxdiff_length_a 6.62880(12) _cell_oxdiff_length_b 15.5616(3) _cell_oxdiff_length_c 11.4854(2) _cell_oxdiff_measurement_reflns_used 8853 _cell_oxdiff_volume 1183.84(4) _diffrn_oxdiff_digest_hkl ; 01891b87b9e1c1c2db8bd6718a3a4a33043e1d ; _diffrn_oxdiff_digest_od_ed ; ; _diffrn_oxdiff_measurement_exp_name AA-3-2.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) ; _shelx_res_file ; TITL aa-3-2_auto_c.res in P2(1)/n aa-3-2_auto.res created by SHELXL-2025/1 at 13:58:27 on 12-May-2026 REM Old TITL AA-3-2_auto in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.140, Rweak 0.010, Alpha 0.018 REM 0.435 for 102 systematic absences, Orientation as input REM Formula found by SHELXT: C8 N4 Cl2 Mn CELL 1.54184 6.6289 15.5631 11.4839 90 92.257 90 ZERR 4 0.0001 0.0002 0.0001 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl Mn N UNIT 32 44 8 4 20 L.S. 10 PLAN 20 TEMP -173 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta OMIT -1 0 1 REM REM REM WGHT 0.028000 0.598200 FVAR 4.46493 MN1 4 0.293573 0.639711 0.675605 11.00000 0.01707 0.01355 = 0.01697 0.00119 0.00276 -0.00049 CL1 3 0.412455 0.644998 0.877010 11.00000 0.02255 0.02163 = 0.01858 -0.00073 0.00034 0.00246 CL2 3 0.054249 0.526856 0.664657 11.00000 0.01998 0.01692 = 0.02944 -0.00014 0.00199 -0.00261 N1 5 0.071091 0.750103 0.695085 11.00000 0.01651 0.01894 = 0.01785 -0.00083 0.00128 -0.00110 N2 5 0.402827 0.757416 0.584649 11.00000 0.01666 0.01762 = 0.01654 0.00004 0.00328 0.00056 N3 5 0.574292 0.746054 0.525328 11.00000 0.02088 0.01562 = 0.02101 0.00257 0.00878 0.00011 H3 2 0.630569 0.785968 0.492256 11.00000 0.02406 N4 5 0.806445 0.653508 0.455435 11.00000 0.02609 0.01888 = 0.02711 0.00239 0.01118 0.00378 H4A 2 0.855937 0.696897 0.424887 11.00000 0.02978 H4B 2 0.855431 0.601036 0.440418 11.00000 0.04056 N5 5 0.544410 0.603061 0.572061 11.00000 0.02361 0.01441 = 0.02390 0.00189 0.00635 0.00388 H5 2 0.601511 0.552594 0.561407 11.00000 0.03261 C1 1 -0.098084 0.744165 0.754771 11.00000 0.01905 0.02638 = 0.02143 -0.00046 0.00159 -0.00275 AFIX 43 H1 2 -0.140665 0.689076 0.779619 11.00000 -1.20000 AFIX 0 C2 1 -0.213389 0.815260 0.781677 11.00000 0.01612 0.03588 = 0.02658 -0.00461 0.00446 0.00086 AFIX 43 H2 2 -0.332253 0.808816 0.824437 11.00000 -1.20000 AFIX 0 C3 1 -0.153219 0.895459 0.745536 11.00000 0.02109 0.02671 = 0.02982 -0.00803 -0.00102 0.00579 AFIX 43 H3A 2 -0.229343 0.945080 0.763640 11.00000 -1.20000 AFIX 0 C4 1 0.020356 0.902606 0.682263 11.00000 0.02016 0.01841 = 0.02465 -0.00302 -0.00131 0.00177 AFIX 43 H4 2 0.063862 0.957030 0.655438 11.00000 -1.20000 AFIX 0 C5 1 0.129185 0.828657 0.658932 11.00000 0.01833 0.01859 = 0.01700 -0.00116 -0.00141 -0.00057 C6 1 0.316455 0.830991 0.592229 11.00000 0.01870 0.01509 = 0.01724 -0.00072 -0.00020 -0.00025 C7 1 0.387603 0.913160 0.540896 11.00000 0.02235 0.01519 = 0.02750 0.00223 0.00361 -0.00018 AFIX 137 H7A 2 0.513420 0.902937 0.501047 11.00000 -1.50000 H7B 2 0.411481 0.955528 0.603050 11.00000 -1.50000 H7C 2 0.284629 0.934974 0.484882 11.00000 -1.50000 AFIX 0 C8 1 0.642782 0.662700 0.518657 11.00000 0.01798 0.01990 = 0.01875 -0.00091 0.00209 0.00254 HKLF 4 REM aa-3-2_auto_c.res in P2(1)/n REM wR2 = 0.0593, GooF = S = 1.084, Restrained GooF = 1.084 for all data REM R1 = 0.0224 for 2280 Fo > 4sig(Fo) and 0.0239 for all 2382 data REM 162 parameters refined using 0 restraints END WGHT 0.0279 0.5989 REM Highest difference peak 0.358, deepest hole -0.289, 1-sigma level 0.056 Q1 1 0.3653 0.6320 0.7757 11.00000 0.05 0.36 Q2 1 0.1017 0.8631 0.6796 11.00000 0.05 0.32 Q3 1 0.1372 0.6723 0.7022 11.00000 0.05 0.30 Q4 1 0.3472 0.8728 0.5763 11.00000 0.05 0.27 Q5 1 0.4643 0.5856 0.8493 11.00000 0.05 0.26 Q6 1 0.2225 0.8281 0.6278 11.00000 0.05 0.26 Q7 1 0.3449 0.7138 0.6050 11.00000 0.05 0.22 Q8 1 0.4697 0.6168 0.6224 11.00000 0.05 0.21 Q9 1 -0.0224 0.7461 0.7064 11.00000 0.05 0.21 Q10 1 0.4616 0.9126 0.4508 11.00000 0.05 0.20 Q11 1 0.4005 0.6202 0.5837 11.00000 0.05 0.20 Q12 1 0.4853 0.5969 0.9777 11.00000 0.05 0.20 Q13 1 -0.1563 0.7823 0.7616 11.00000 0.05 0.20 Q14 1 -0.0035 0.5185 0.5732 11.00000 0.05 0.19 Q15 1 0.4810 0.7523 0.5591 11.00000 0.05 0.19 Q16 1 -0.0157 0.5997 0.6615 11.00000 0.05 0.19 Q17 1 0.1223 0.5938 0.6821 11.00000 0.05 0.18 Q18 1 0.4822 0.9209 0.5675 11.00000 0.05 0.18 Q19 1 0.0882 0.7981 0.6737 11.00000 0.05 0.18 Q20 1 0.9164 0.5190 0.4425 11.00000 0.05 0.18 ; _shelx_res_checksum 45209 _shelx_hkl_file ; 0 0 -1 4.99694 4.45661 11 0 0 -1-5.35704 32.3845 20 0 0 -1 3.31210 19.5827 26 0 0 -2 62795.7 590.698 26 0 0 -2 62957.2 646.499 19 0 0 -3 30.8322 33.6678 11 0 0 -3 10.5648 58.8122 26 0 0 -4 35348.3 1426.11 11 0 0 -5 114.600 161.549 11 0 0 -6 96865.7 3592.34 11 0 0 -6 93398.5 3303.69 31 0 0 -7 23.4450 107.064 38 0 0 -7-102.089 139.819 31 0 0 -7-47.3483 283.100 11 0 0 -7 47.8696 98.9186 39 0 0 -8 26267.3 1418.54 23 0 0 -8 28642.1 1165.37 8 0 0 -8 28224.1 1192.69 31 0 0 -8 28892.2 1110.80 39 0 0 -8 27568.1 1103.87 38 0 0 -8 30073.3 1159.47 12 0 0 -9-24.4978 204.838 31 0 0 -9-61.5464 181.025 12 0 0 -10 3376.74 372.891 31 0 0 -10 3296.02 358.269 7 0 0 -10 3045.75 341.345 12 0 0 -11 25.2437 226.136 7 0 0 -11-257.655 247.354 31 0 0 -11 24.2174 224.335 12 0 0 -12 17164.1 821.178 12 0 0 -12 17085.6 831.265 7 0 0 -13 82.4381 143.928 13 0 0 -13-64.5447 171.990 7 0 0 -14 26260.4 960.676 5 0 0 -14 25518.6 968.592 7 0 1 0 10.0995 18.4998 28 0 -1 0 7.95821 43.7268 27 0 -1 -1-6.34138 7.99803 19 0 -1 -1 20548.8 298.785 20 0 1 -1-7.42241 9.35999 1 0 1 -1 19702.6 334.621 23 0 1 -2 191925. 6554.19 26 0 -1 -2 195154. 6577.44 20 0 -1 -3 51576.8 1929.31 19 0 1 -3 53710.1 1911.43 26 0 1 -4 36226.4 1413.79 26 0 -1 -4 37059.5 1476.68 11 0 1 -5 74909.0 2761.62 26 0 -1 -5 75537.0 2853.21 11 0 -1 -6 57085.3 2159.08 31 0 1 -6 60796.1 2156.48 31 0 -1 -6 61179.2 2143.48 34 0 -1 -6 60880.3 2436.11 11 0 -1 -7 72.9427 109.470 38 0 1 -7 70.5095 101.589 38 0 -1 -7 94.7244 235.056 11 0 1 -7 50.2633 147.102 31 0 -1 -7 17.6080 144.719 31 0 -1 -7 134.610 123.657 34 0 1 -7 206.517 211.499 23 0 -1 -8 22285.6 878.123 38 0 1 -8 21134.3 865.522 38 0 -1 -8 21878.5 916.427 12 0 1 -8 21488.0 1180.93 23 0 1 8 19302.2 867.457 37 0 -1 -8 20849.7 948.614 31 0 1 -8 21179.5 944.166 31 0 1 -8 22149.8 922.416 8 0 1 -8 20746.9 902.080 12 0 -1 -8 22186.1 895.469 39 0 -1 -9 68813.8 2455.05 38 0 1 -9 68549.1 2564.11 31 0 1 -9 67545.4 2517.90 12 0 -1 -9 68968.6 2533.85 12 0 1 -9 66288.4 2523.01 8 0 -1 -9 69274.0 2578.71 31 0 -1 -9 68309.5 2467.73 39 0 -1 -10 87170.6 3164.99 7 0 1 -10 89280.9 3193.09 31 0 -1 -10 88166.3 3193.15 31 0 -1 -10 82697.2 3141.57 12 0 1 -10 83212.8 3135.67 12 0 -1 -11 19891.3 908.075 31 0 -1 -11 16968.9 877.649 7 0 1 -11 18088.4 873.185 12 0 -1 -11 16860.0 858.810 12 0 -1 -12 15841.2 785.401 7 0 1 -12 15626.2 770.124 12 0 -1 -13 6409.59 392.086 7 0 -1 -13 5803.47 359.036 13 0 1 -14 16484.1 650.326 5 0 -1 -14 17210.8 666.502 7 0 2 0 178534. 5831.97 28 0 -2 0 161413. 5925.83 27 0 2 0 171035. 5827.67 1 0 -2 0 173199. 5811.11 19 0 2 -1 71697.0 2576.40 28 0 2 -1 72912.8 2526.40 11 0 -2 -1 73711.8 2528.08 11 0 2 -1 79552.4 2628.99 23 0 -2 -1 75410.5 2664.02 27 0 2 -2-15.7590 19.8658 1 0 2 -2 2886.57 167.960 11 0 -2 -2 2828.49 171.526 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167.967 38 0 -2 -9 469.733 237.942 31 0 2 -9 861.655 253.054 31 0 -2 -9 854.351 196.408 39 0 2 9 906.573 200.416 37 0 -2 -9 1163.18 245.196 12 0 -2 -10 11293.7 650.451 31 0 -2 -10 9596.22 527.901 39 0 2 -10 9964.09 605.384 7 0 -2 -10 11209.5 632.438 7 0 -2 -10 10728.0 621.492 12 0 -2 -11 732.604 292.317 31 0 -2 -11 641.386 240.427 7 0 2 -11 373.926 248.967 7 0 -2 -11 304.527 244.945 12 0 2 -12 2374.06 310.844 7 0 -2 -12 2742.77 318.092 7 0 2 -12 2684.87 320.147 12 0 2 -12 2396.49 253.637 13 0 2 -13 4276.58 301.322 5 0 2 -13 4515.22 313.887 7 0 -2 -13 4491.74 318.265 7 0 -2 -14 89.9516 86.5517 13 0 -2 -14 197.638 95.6489 7 0 2 -14 30.9465 82.8318 7 0 -2 -14 249.982 103.343 5 0 2 -14 62.6383 79.6321 5 0 -3 0 112.944 56.1785 19 0 3 0 72.1041 66.2208 28 0 -3 0 91.9729 151.995 27 0 3 0-29.3497 66.9943 1 0 3 1 1911.20 132.097 1 0 -3 -1 1891.05 249.205 27 0 -3 1 1433.41 93.5983 19 0 -3 -1 1874.92 115.177 11 0 3 -1 1581.26 108.631 11 0 3 -1 1694.98 159.569 28 0 3 -1 1591.45 201.781 23 0 3 -2 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213.670 121.936 18 -7 6 3 222.224 146.909 14 -7 -6 3 314.974 147.632 33 -7 6 3 226.788 143.158 22 -7 -6 2 8256.20 395.146 36 -7 -6 2 9141.33 437.867 33 -7 6 2 9208.38 439.579 22 7 -6 -2 8864.27 425.734 18 -7 6 1 1985.97 206.196 14 -7 -6 1 1325.02 161.085 21 -7 6 1 1468.30 180.047 3 -7 -6 1 1817.71 188.880 33 -7 6 1 1821.93 193.954 22 -7 6 0 5906.74 323.045 14 -7 6 0 5812.69 331.078 3 -7 -6 0 5683.79 316.769 33 -7 -6 0 4983.17 290.623 35 -7 6 0 5267.03 312.830 22 -7 -6 0 5322.45 289.708 21 -7 6 -1 5345.54 301.646 22 -7 -6 -1 5115.57 281.796 21 -7 6 -1 5359.97 298.951 14 -7 6 -1 5505.83 325.018 3 -7 -6 -1 4940.15 293.749 33 -7 -6 -2 4383.90 266.833 2 -7 -6 -2 5467.49 278.547 21 -7 -6 -2 5001.79 283.303 33 -7 6 -2 6171.10 327.442 3 -7 6 -3 10688.4 472.035 2 -7 -6 -3 9843.37 460.055 2 -7 -6 -3 11082.4 465.110 33 -7 6 -4 2922.47 196.644 2 -7 -6 -4 2656.07 192.825 2 -7 -6 -5 483.584 105.074 2 -7 6 -5 658.739 104.645 3 -7 7 5 856.880 118.365 14 -7 7 4 19988.0 787.251 22 -7 7 4 21050.5 796.376 14 -7 -7 4 20031.4 796.262 33 -7 7 3 584.057 133.430 22 -7 7 3 836.369 155.024 14 -7 -7 3 472.362 134.848 33 -7 7 2 378.375 126.579 22 -7 -7 2 460.511 143.211 33 -7 7 1 13924.4 602.640 22 -7 7 1 15218.9 625.131 14 -7 -7 1 14912.4 618.440 33 -7 -7 0 10624.5 479.572 35 -7 -7 0 11520.6 501.098 33 -7 7 0 10688.2 498.258 3 -7 7 0 11600.6 501.905 14 -7 7 0 11766.6 489.884 22 -7 7 -1 42.4263 135.361 3 -7 -7 -1-67.2482 114.566 33 -7 7 -1 8.74695 107.469 14 -7 7 -1 140.945 99.4244 22 -7 -7 -2 24800.8 935.514 33 -7 7 -2 24913.8 953.097 3 -7 -7 -3 527.177 107.211 33 -7 7 -3 575.701 134.772 3 -7 -7 -3 518.502 110.230 2 -7 -7 -4 447.154 102.104 2 -7 -7 -5 733.410 88.8341 2 -7 8 5 694.274 96.2822 14 -7 8 4 314.526 104.008 14 -7 8 3 2359.59 168.415 22 -7 8 3 2108.51 181.414 14 -7 8 2 516.404 106.908 22 -7 -8 2 507.881 127.176 33 -7 8 1 1273.17 133.915 4 -7 8 1 1283.11 135.728 22 -7 -8 1 1469.63 155.185 33 -7 -8 1 1143.60 144.982 35 -7 -8 0 348.675 116.590 33 -7 8 0 425.771 120.850 14 -7 -8 0 338.052 104.676 35 -7 -8 -1 121.477 103.812 33 -7 8 -1 80.3183 94.3681 14 -7 8 -2 11208.4 474.346 3 -7 -8 -2 10611.4 457.916 33 -7 -8 -3 3973.32 200.190 2 -7 9 4 620.664 93.3074 14 -7 9 3 20104.5 760.950 14 -7 9 1 452.238 87.9314 4 -7 9 1 510.242 110.305 14 -7 -9 0 94.4574 96.8391 33 -7 9 0 190.278 90.5136 14 -7 9 0 163.832 93.0138 4 -7 -9 -1 14405.0 562.493 33 -7 9 -1 13762.6 556.232 4 -7 9 -2 5104.75 255.172 4 -7 9 -3 1440.50 119.530 4 -7 10 3 1333.72 108.159 14 -7 10 1 93.2396 72.7835 14 -7 10 0 3260.16 176.991 4 -7 10 0 3871.65 184.044 14 -7 10 -1 723.563 88.3122 4 -7 10 -2 547.575 76.7882 4 8 0 -4 314.152 93.8198 18 8 0 -3-17.0569 103.672 18 8 0 -2 10591.6 441.309 18 -8 0 2 8961.44 401.243 36 -8 0 1-14.8143 96.5811 21 -8 0 0 19894.2 781.578 3 -8 0 0 25054.1 825.890 21 -8 0 -1-36.6302 92.0716 3 -8 0 -1-137.788 98.0734 21 -8 0 -2-79.6185 93.1583 3 -8 0 -3-16.0446 72.4528 3 8 -1 -4 10999.2 449.903 18 8 -1 -3 12787.5 528.348 18 8 -1 -2 152.102 102.872 18 -8 -1 1 871.971 119.090 21 -8 1 0 21378.0 827.574 3 -8 -1 0 26158.1 870.152 21 -8 -1 -1 18356.9 715.239 3 -8 1 -1 20370.0 721.817 3 -8 -1 -2 3491.38 197.450 3 -8 1 -2 3793.23 201.168 3 -8 -1 -3 3574.15 181.399 3 -8 1 -3 3198.42 177.692 3 -8 2 4 102.185 70.0668 14 8 -2 -4 72.5661 75.5576 18 8 2 -4 170.058 71.9203 18 8 -2 -3 1418.33 137.870 18 8 2 -3 1609.79 140.933 18 8 -2 -2 3848.46 221.730 18 8 2 -2 3540.56 215.256 18 8 2 -1 11355.3 475.561 18 8 -2 -1 11126.9 475.553 18 -8 -2 -1 5527.88 252.645 3 -8 2 -1 5433.01 255.189 3 -8 2 -2 92.1527 77.1904 3 -8 -2 -2 5.55239 75.5585 3 -8 2 -3 649.239 85.2862 3 -8 -2 -3 617.115 83.6635 3 -8 3 4 6435.94 274.698 14 -8 3 3 1115.44 117.684 14 8 -3 -3 895.238 101.400 18 8 3 -3 1308.00 114.904 18 -8 3 2 980.800 112.515 14 8 -3 -2 1079.79 115.915 18 8 3 -2 856.208 112.408 18 -8 3 1 6064.81 287.839 14 8 -3 -1 6311.20 297.824 18 8 3 -1 6746.41 302.820 18 -8 3 0 4451.31 217.732 14 -8 3 -1 2359.91 150.918 3 -8 3 -2 292.773 78.0620 3 -8 -3 -2 244.759 71.5792 3 -8 4 3 58.7989 68.5753 14 -8 4 2 372.560 85.8414 14 8 4 -1 504.462 80.1260 18 8 -4 -1 424.184 76.2320 18 -8 4 1 378.630 83.8729 14 -8 4 0 215.195 68.9378 14 8 -4 0 96.8512 60.9720 18 8 4 0 129.318 68.5496 18 -8 5 2 2304.44 136.537 14 -8 5 1 372.469 68.8465 14 0 0 0 0.00 0.00 0 TITL AA-3-2_auto in P2(1)/n REM P2(1)/n (#14 in standard setting (mkl: cell=2,tostdtrans=2,'abc')) CELL 1.54184 6.628906 15.563132 11.483936 90.0000 92.2565 90.0000 ZERR 3.00 0.000073 0.000177 0.000133 0.0000 0.0010 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H Cl Mn N UNIT 24.00 33.00 6.00 3.00 15.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.08 0.12 0.23 TREF HKLF 4 END ; _shelx_hkl_checksum 49876 _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 1.555 _oxdiff_exptl_absorpt_empirical_full_min 0.812 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.29357(4) 0.63971(2) 0.67561(2) 0.01581(9) Uani 1 1 d . . . . . Cl1 Cl 0.41246(6) 0.64500(2) 0.87701(3) 0.02093(10) Uani 1 1 d . . . . . Cl2 Cl 0.05425(6) 0.52686(2) 0.66466(4) 0.02209(11) Uani 1 1 d . . . . . N1 N 0.0711(2) 0.75010(9) 0.69508(12) 0.0178(3) Uani 1 1 d . . . . . N2 N 0.4028(2) 0.75742(9) 0.58465(11) 0.0169(3) Uani 1 1 d . . . . . N3 N 0.5743(2) 0.74605(9) 0.52533(12) 0.0190(3) Uani 1 1 d . . . . . H3 H 0.631(3) 0.7860(15) 0.4923(19) 0.024(5) Uiso 1 1 d . . . . . N4 N 0.8064(2) 0.65351(11) 0.45544(14) 0.0238(3) Uani 1 1 d . . . . . H4A H 0.856(3) 0.6969(16) 0.425(2) 0.030(6) Uiso 1 1 d . . . . . H4B H 0.855(4) 0.6010(18) 0.440(2) 0.041(7) Uiso 1 1 d . . . . . N5 N 0.5444(2) 0.60306(9) 0.57206(13) 0.0205(3) Uani 1 1 d . . . . . H5 H 0.602(3) 0.5526(16) 0.561(2) 0.033(6) Uiso 1 1 d . . . . . C1 C -0.0981(3) 0.74417(12) 0.75477(15) 0.0223(3) Uani 1 1 d . . . . . H1 H -0.140665 0.689076 0.779619 0.027 Uiso 1 1 calc R U . . . C2 C -0.2134(3) 0.81526(13) 0.78168(16) 0.0261(4) Uani 1 1 d . . . . . H2 H -0.332253 0.808816 0.824437 0.031 Uiso 1 1 calc R U . . . C3 C -0.1532(3) 0.89546(12) 0.74554(16) 0.0259(4) Uani 1 1 d . . . . . H3A H -0.229343 0.945080 0.763640 0.031 Uiso 1 1 calc R U . . . C4 C 0.0204(3) 0.90261(11) 0.68226(15) 0.0211(3) Uani 1 1 d . . . . . H4 H 0.063862 0.957030 0.655438 0.025 Uiso 1 1 calc R U . . . C5 C 0.1292(2) 0.82866(11) 0.65893(14) 0.0180(3) Uani 1 1 d . . . . . C6 C 0.3165(2) 0.83099(10) 0.59223(14) 0.0170(3) Uani 1 1 d . . . . . C7 C 0.3876(3) 0.91316(10) 0.54090(16) 0.0216(3) Uani 1 1 d . . . . . H7A H 0.513420 0.902937 0.501047 0.032 Uiso 1 1 calc R U . . . H7B H 0.411481 0.955528 0.603050 0.032 Uiso 1 1 calc R U . . . H7C H 0.284629 0.934974 0.484882 0.032 Uiso 1 1 calc R U . . . C8 C 0.6428(2) 0.66270(11) 0.51866(14) 0.0188(3) 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 Mn1 0.01707(14) 0.01355(14) 0.01697(14) 0.00119(9) 0.00276(10) -0.00049(9) Cl1 0.0225(2) 0.0216(2) 0.0186(2) -0.00073(14) 0.00034(14) 0.00246(14) Cl2 0.01998(19) 0.0169(2) 0.0294(2) -0.00014(15) 0.00199(15) -0.00261(14) N1 0.0165(6) 0.0189(7) 0.0178(6) -0.0008(5) 0.0013(5) -0.0011(5) N2 0.0167(6) 0.0176(7) 0.0165(6) 0.0000(5) 0.0033(5) 0.0006(5) N3 0.0209(7) 0.0156(7) 0.0210(7) 0.0026(6) 0.0088(5) 0.0001(6) N4 0.0261(8) 0.0189(7) 0.0271(8) 0.0024(6) 0.0112(6) 0.0038(6) N5 0.0236(7) 0.0144(7) 0.0239(7) 0.0019(6) 0.0064(6) 0.0039(6) C1 0.0191(8) 0.0264(9) 0.0214(8) -0.0005(7) 0.0016(6) -0.0028(7) C2 0.0161(8) 0.0359(10) 0.0266(9) -0.0046(8) 0.0045(6) 0.0009(7) C3 0.0211(8) 0.0267(9) 0.0298(9) -0.0080(8) -0.0010(7) 0.0058(7) C4 0.0202(8) 0.0184(8) 0.0247(8) -0.0030(6) -0.0013(6) 0.0018(6) C5 0.0183(8) 0.0186(8) 0.0170(8) -0.0012(6) -0.0014(6) -0.0006(6) C6 0.0187(8) 0.0151(7) 0.0172(7) -0.0007(6) -0.0002(6) -0.0002(6) C7 0.0224(8) 0.0152(8) 0.0275(9) 0.0022(7) 0.0036(7) -0.0002(6) C8 0.0180(8) 0.0199(8) 0.0188(8) -0.0009(6) 0.0021(6) 0.0025(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Cl Cl 0.3639 0.7018 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -2 1 0.0400 0 1 0 0.0578 0 -1 0 0.0559 1 2 2 0.0553 -1 -2 -1 0.0566 1 -1 2 0.0604 -1 2 -1 0.0443 -1 2 1 0.0608 0 -1 2 0.0988 0 0 -1 0.0768 2 1 2 0.0364 0 2 -1 0.0723 1 1 0 0.0670 -1 -9 -2 0.0439 -2 -5 -5 0.0595 -4 2 0 0.0559 0 6 6 0.0653 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 Cl2 Mn1 Cl1 105.598(16) . . ? N1 Mn1 Cl1 93.91(4) . . ? N1 Mn1 Cl2 97.44(4) . . ? N2 Mn1 Cl1 108.60(4) . . ? N2 Mn1 Cl2 144.04(4) . . ? N2 Mn1 N1 69.66(5) . . ? N5 Mn1 Cl1 107.89(4) . . ? N5 Mn1 Cl2 107.69(4) . . ? N5 Mn1 N1 140.18(5) . . ? N5 Mn1 N2 71.91(5) . . ? C1 N1 Mn1 123.74(12) . . ? C1 N1 C5 118.27(15) . . ? C5 N1 Mn1 117.25(11) . . ? N3 N2 Mn1 114.76(10) . . ? C6 N2 Mn1 122.92(11) . . ? C6 N2 N3 122.24(14) . . ? N2 N3 H3 122.3(15) . . ? N2 N3 C8 115.74(14) . . ? C8 N3 H3 121.8(15) . . ? H4A N4 H4B 120(2) . . ? C8 N4 H4A 118.9(16) . . ? C8 N4 H4B 120.6(16) . . ? Mn1 N5 H5 131.0(15) . . ? C8 N5 Mn1 118.83(12) . . ? C8 N5 H5 110.1(15) . . ? N1 C1 H1 118.7 . . ? N1 C1 C2 122.59(17) . . ? C2 C1 H1 118.7 . . ? C1 C2 H2 120.4 . . ? C3 C2 C1 119.12(17) . . ? C3 C2 H2 120.4 . . ? C2 C3 H3A 120.5 . . ? C2 C3 C4 119.02(17) . . ? C4 C3 H3A 120.5 . . ? C3 C4 H4 120.6 . . ? C3 C4 C5 118.77(17) . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.22(16) . . ? N1 C5 C6 115.76(14) . . ? C4 C5 C6 122.01(15) . . ? N2 C6 C5 113.40(14) . . ? N2 C6 C7 126.04(15) . . ? C5 C6 C7 120.56(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 114.04(15) . . ? N5 C8 N3 118.23(15) . . ? N5 C8 N4 127.73(16) . . ? 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 Cl1 2.4153(4) . ? Mn1 Cl2 2.3668(4) . ? Mn1 N1 2.2810(14) . ? Mn1 N2 2.2430(14) . ? Mn1 N5 2.1587(15) . ? N1 C1 1.340(2) . ? N1 C5 1.352(2) . ? N2 N3 1.3595(19) . ? N2 C6 1.285(2) . ? N3 H3 0.82(2) . ? N3 C8 1.378(2) . ? N4 H4A 0.83(3) . ? N4 H4B 0.90(3) . ? N4 C8 1.337(2) . ? N5 H5 0.88(2) . ? N5 C8 1.302(2) . ? C1 H1 0.9500 . ? C1 C2 1.387(3) . ? C2 H2 0.9500 . ? C2 C3 1.379(3) . ? C3 H3A 0.9500 . ? C3 C4 1.389(3) . ? C4 H4 0.9500 . ? C4 C5 1.390(2) . ? C5 C6 1.485(2) . ? C6 C7 1.492(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 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 N1 C1 C2 169.09(12) . . . . ? Mn1 N1 C5 C4 -170.11(12) . . . . ? Mn1 N1 C5 C6 10.11(18) . . . . ? Mn1 N2 N3 C8 7.00(17) . . . . ? Mn1 N2 C6 C5 -4.58(19) . . . . ? Mn1 N2 C6 C7 175.75(12) . . . . ? Mn1 N5 C8 N3 -3.8(2) . . . . ? Mn1 N5 C8 N4 176.67(14) . . . . ? N1 C1 C2 C3 0.3(3) . . . . ? N1 C5 C6 N2 -3.9(2) . . . . ? N1 C5 C6 C7 175.81(14) . . . . ? N2 N3 C8 N4 177.22(14) . . . . ? N2 N3 C8 N5 -2.4(2) . . . . ? N3 N2 C6 C5 178.85(13) . . . . ? N3 N2 C6 C7 -0.8(3) . . . . ? C1 N1 C5 C4 0.4(2) . . . . ? C1 N1 C5 C6 -179.38(14) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C3 C4 C5 N1 0.4(2) . . . . ? C3 C4 C5 C6 -179.81(15) . . . . ? C4 C5 C6 N2 176.34(15) . . . . ? C4 C5 C6 C7 -4.0(2) . . . . ? C5 N1 C1 C2 -0.8(2) . . . . ? C6 N2 N3 C8 -176.17(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 0.9998 -1.9986 1.0000 0.0060 -0.1275 -0.3122 -0.0001 0.9993 -0.0001 -0.0731 -0.0108 0.0658 0.0001 -0.9993 0.0001 0.0731 0.0108 -0.0658 0.9993 1.9987 1.9989 -0.3724 -0.1147 -0.1354 -0.9992 -1.9985 -0.9994 0.2864 0.1709 0.0491 0.9997 -0.9991 1.9993 -0.1531 -0.0822 -0.3327 -0.9998 1.9986 -1.0000 -0.0060 0.1275 0.3122 -0.9996 1.9991 0.9989 -0.1780 0.2399 0.1396 0.0003 -0.9988 1.9990 -0.0989 0.1233 -0.2383 -0.0001 -0.0002 -0.9994 0.0860 -0.0562 0.0863 1.9988 0.9992 1.9993 -0.3534 -0.3093 -0.2955 -0.0003 1.9983 -0.9997 -0.0602 -0.0779 0.2178 0.9993 0.9990 0.0001 -0.1273 -0.2163 -0.0286 -1.0434 -9.1846 -2.4485 0.9392 0.1767 -0.2945 -2.0520 -4.7737 -5.3792 0.9233 0.1711 0.3439 -4.1710 2.4778 0.2534 0.0230 0.8447 0.5347 -0.2162 5.6937 6.1560 -0.9345 0.3288 -0.1365