#------------------------------------------------------------------------------ #$Date: 2021-11-04 01:58:51 +0200 (Thu, 04 Nov 2021) $ #$Revision: 270276 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708693.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_7708693 loop_ _publ_author_name 'Zhang, Yue' 'Chen, Dian' 'Jin, Kai-Hang' 'Zang, Shuang-Quan' 'Wang, Qing-Lun' _publ_section_title ; Room-temperature phosphorescence of manganese-based metal halides ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03206B _journal_year 2021 _chemical_formula_moiety 'Cl6 Mn, 2(C8 H14 N2)' _chemical_formula_sum 'C16 H28 Cl6 Mn N4' _chemical_formula_weight 544.06 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2020-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-09-17 deposited with the CCDC. 2021-11-01 downloaded from the CCDC. ; _cell_angle_alpha 101.991(3) _cell_angle_beta 99.889(3) _cell_angle_gamma 112.943(3) _cell_formula_units_Z 1 _cell_length_a 7.5206(3) _cell_length_b 8.4873(3) _cell_length_c 10.5291(3) _cell_measurement_reflns_used 3780 _cell_measurement_temperature 296.6(6) _cell_measurement_theta_max 72.7890 _cell_measurement_theta_min 5.9230 _cell_volume 581.08(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)' _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 air _diffrn_ambient_temperature 296.6(6) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.955 _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 -57.00 0.00 0.50 0.50 -- 0.00 -38.00 90.00 114 2 \w -56.00 12.00 0.50 0.50 -- 0.00 -37.00-176.00 136 3 \w -13.00 29.00 0.50 0.50 -- 0.00 -38.00 -60.00 84 4 \w -87.00 -37.00 0.50 0.50 -- 0.00 -38.00 -60.00 100 5 \w 8.00 135.00 0.50 0.50 -- 97.60 -82.00 0.00 254 6 \w 9.00 61.00 0.50 0.50 -- 97.60 -61.00-150.00 104 7 \w 133.00 159.00 0.50 0.50 -- 97.60 77.00 60.00 52 8 \w 8.00 127.00 0.50 0.50 -- 97.60 -82.00-150.00 238 9 \w 92.00 118.00 0.50 0.50 -- 97.60 -82.00 120.00 52 10 \w 64.00 186.00 0.50 0.50 -- 97.60 30.00 90.00 244 11 \w 101.00 130.00 0.50 0.50 -- 97.60 -30.00 120.00 58 12 \w 86.00 123.00 0.50 0.50 -- 97.60 45.00 120.00 74 13 \w 21.00 47.00 0.50 0.50 -- 97.60 -30.00 120.00 52 14 \w 69.00 128.00 0.50 0.50 -- 97.60 -61.00-150.00 118 15 \w 33.00 58.00 0.50 0.50 -- 97.60 -82.00 120.00 50 16 \w 128.00 161.00 0.50 0.50 -- 97.60 45.00 120.00 66 17 \w 71.00 105.00 0.50 0.50 -- 97.60 77.00 60.00 68 18 \w 89.00 114.00 0.50 0.50 -- 97.60 -82.00 -90.00 50 19 \w 65.00 135.00 0.50 0.50 -- 97.60 -82.00 60.00 140 20 \w 98.00 130.00 0.50 0.50 -- 97.60 45.00-180.00 64 21 \w 89.00 115.00 0.50 0.50 -- 97.60 -82.00 90.00 52 22 \w 81.00 183.00 0.50 0.50 -- 97.60 61.00 150.00 204 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0169878000 _diffrn_orient_matrix_UB_12 -0.1730990000 _diffrn_orient_matrix_UB_13 0.0074552000 _diffrn_orient_matrix_UB_21 0.2272625000 _diffrn_orient_matrix_UB_22 0.1104245000 _diffrn_orient_matrix_UB_23 0.0694795000 _diffrn_orient_matrix_UB_31 -0.0415583000 _diffrn_orient_matrix_UB_32 0.0242963000 _diffrn_orient_matrix_UB_33 0.1391190000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5478 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_unetI/netI 0.0274 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.955 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4761 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.955 _diffrn_reflns_theta_full 68.230 _diffrn_reflns_theta_max 73.781 _diffrn_reflns_theta_min 4.490 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.160 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.35881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.555 _exptl_crystal_description block _exptl_crystal_F_000 279 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.334 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.122 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 126 _refine_ls_number_reflns 2227 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0376 _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^)+(0.0690P)^2^+0.0868P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.0981 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2139 _reflns_number_total 2227 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL hy_a.res in P-1 hy.res created by SHELXL-2016/4 at 14:14:12 on 26-Feb-2020 REM Old TITL HY in P-1 #2 REM SHELXT solution in P-1 REM R1 0.098, Rweak 0.011, Alpha 0.064, Orientation as input REM Formula found by SHELXT: C16 Cl6 Mn N4 CELL 1.5478 7.520645 8.487334 10.529076 101.9911 99.8891 112.9432 ZERR 1 0.000251 0.000265 0.000315 0.0026 0.0027 0.0031 LATT 1 SFAC C H Cl Mn N DISP C 0.0193 0.0097 90.8895 DISP Cl 0.3694 0.7045 6304.002 DISP H -0 0 0.6551 DISP Mn -0.5661 2.8539 24854.1133 DISP N 0.0328 0.0186 175.0453 UNIT 16 28 6 1 4 L.S. 4 0 0 PLAN 20 BOND $H list 4 htab fmap 2 53 acta OMIT 4 -5 10 OMIT 3 -6 11 OMIT 2 -5 7 OMIT 2 4 1 OMIT 6 -9 4 OMIT 2 -5 1 OMIT 0 -2 2 REM REM REM WGHT 0.069000 0.086800 FVAR 9.66284 MN1 4 0.000000 0.500000 0.000000 10.50000 0.02319 0.02430 = 0.01953 0.00696 0.00653 0.01333 CL1 3 0.141977 0.267621 -0.005359 11.00000 0.02333 0.02245 = 0.02467 0.00417 0.00526 0.01178 CL2 3 0.012136 0.523404 0.243581 11.00000 0.02924 0.03107 = 0.01952 0.00512 0.00490 0.01539 CL3 3 -0.372601 0.238261 -0.069372 11.00000 0.02039 0.02545 = 0.03526 0.00791 0.00116 0.00740 N1 5 0.581104 0.529805 0.186603 11.00000 0.02684 0.02860 = 0.01794 0.00507 0.00247 0.01121 AFIX 137 H1A 2 0.518004 0.428913 0.117647 11.00000 -1.20000 H1B 2 0.713410 0.570909 0.200135 11.00000 -1.20000 H1C 2 0.543435 0.611554 0.167770 11.00000 -1.20000 AFIX 0 N2 5 1.169827 0.910435 0.835935 11.00000 0.02393 0.02489 = 0.02814 0.00741 -0.00053 0.00882 AFIX 137 H2A 2 1.099317 0.799823 0.838726 11.00000 -1.20000 H2B 2 1.124336 0.983506 0.876826 11.00000 -1.20000 H2C 2 1.298999 0.948631 0.878021 11.00000 -1.20000 AFIX 0 C1 1 0.528433 0.493126 0.310628 11.00000 0.03941 0.02938 = 0.01672 0.00629 0.00190 0.00029 AFIX 23 H1D 2 0.563041 0.399367 0.328132 11.00000 -1.20000 H1E 2 0.384471 0.450284 0.296102 11.00000 -1.20000 AFIX 0 C2 1 0.637208 0.658543 0.432024 11.00000 0.02950 0.02603 = 0.01283 0.00704 0.00280 0.00423 C3 1 0.542083 0.761859 0.473137 11.00000 0.02938 0.03915 = 0.02593 0.01374 0.00004 0.01520 AFIX 43 H3 2 0.411391 0.730776 0.424801 11.00000 -1.20000 AFIX 0 C4 1 0.641528 0.912577 0.586891 11.00000 0.04229 0.03598 = 0.03347 0.00825 0.00343 0.02534 AFIX 43 H4 2 0.576380 0.980927 0.615123 11.00000 -1.20000 AFIX 0 C5 1 0.836097 0.960631 0.657663 11.00000 0.04031 0.02552 = 0.02346 0.00322 0.00079 0.01335 AFIX 43 H5 2 0.902655 1.062862 0.732390 11.00000 -1.20000 AFIX 0 C6 1 0.933665 0.857667 0.618334 11.00000 0.02528 0.02887 = 0.01676 0.00708 0.00366 0.00672 C7 1 0.832504 0.705491 0.505541 11.00000 0.03066 0.02772 = 0.01831 0.00563 0.00799 0.01106 AFIX 43 H7 2 0.895938 0.634737 0.479164 11.00000 -1.20000 AFIX 0 C8 1 1.147924 0.909346 0.693308 11.00000 0.02354 0.04488 = 0.02555 0.00467 0.00384 0.00801 AFIX 23 H8A 2 1.191679 0.825223 0.648035 11.00000 -1.20000 H8B 2 1.234288 1.027753 0.690750 11.00000 -1.20000 AFIX 0 HKLF 4 REM hy_a.res in P-1 REM R1 = 0.0376 for 2139 Fo > 4sig(Fo) and 0.0398 for all 2227 data REM 126 parameters refined using 0 restraints END WGHT 0.0690 0.0868 REM Instructions for potential hydrogen bonds HTAB N1 CL1 EQIV $1 x+1, y, HTAB N1 CL3_$1 EQIV $2 -x+1, -y+1, - HTAB N1 CL1_$2 HTAB N1 CL2_$1 EQIV $3 -x, -y+1, - HTAB N1 CL3_$3 EQIV $4 -x+1, -y+1, -z+ HTAB N2 CL1_$4 HTAB N2 CL2_$4 EQIV $5 x+1, y+1, z+ HTAB N2 CL1_$5 EQIV $6 x+2, y+1, z+ HTAB N2 CL3_$6 HTAB N2 CL3_$4 REM Highest difference peak 0.334, deepest hole -0.681, 1-sigma level 0.122 Q1 1 -0.0603 0.1041 -0.0871 11.00000 0.05 0.33 Q2 1 0.8719 0.6057 0.1980 11.00000 0.05 0.31 Q3 1 -0.1015 0.2933 0.0240 11.00000 0.05 0.30 Q4 1 -0.2376 0.1600 -0.0200 11.00000 0.05 0.30 Q5 1 0.0154 0.3424 -0.0556 11.00000 0.05 0.30 Q6 1 0.0271 0.3359 0.0433 11.00000 0.05 0.29 Q7 1 0.1766 0.1240 0.0367 11.00000 0.05 0.29 Q8 1 -0.5075 0.2637 -0.0413 11.00000 0.05 0.28 Q9 1 -0.4263 0.3772 -0.0104 11.00000 0.05 0.28 Q10 1 -0.2016 0.3714 0.0206 11.00000 0.05 0.28 Q11 1 0.3300 0.2708 -0.0127 11.00000 0.05 0.28 Q12 1 0.2929 0.4823 -0.0232 11.00000 0.05 0.28 Q13 1 1.0401 0.9797 0.9831 11.00000 0.05 0.27 Q14 1 0.1632 0.2942 -0.0762 11.00000 0.05 0.27 Q15 1 0.3008 0.1988 0.0365 11.00000 0.05 0.27 Q16 1 1.0641 0.8622 0.8911 11.00000 0.05 0.27 Q17 1 -0.3131 0.0937 -0.0364 11.00000 0.05 0.27 Q18 1 0.8004 0.5428 0.3420 11.00000 0.05 0.26 Q19 1 -0.0548 0.1207 -0.0004 11.00000 0.05 0.26 Q20 1 1.3993 1.0922 0.8892 11.00000 0.05 0.26 REM The information below was added by Olex2. REM REM R1 = 0.0376 for 2139 Fo > 4sig(Fo) and 0.0398 for all 4773 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.33, deepest hole -0.68 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0398 REM R1_gt = 0.0376 REM wR_ref = 0.0981 REM GOOF = 1.100 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 4773 REM Reflections_gt = 2139 REM Parameters = n/a REM Hole = -0.68 REM Peak = 0.33 REM Flack = n/a ; _cod_data_source_file d1dt03206b2.cif _cod_data_source_block 2 _cod_original_cell_volume 581.09(3) _cod_database_code 7708693 _shelx_shelxl_version_number 2016/4 _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 98.22 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C1(H1D,H1E), C8(H8A,H8B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C7(H7) 2.c Idealised Me refined as rotating group: N1(H1A,H1B,H1C), N2(H2A,H2B,H2C) ; _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 3.013 _oxdiff_exptl_absorpt_empirical_full_min 0.643 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 0.000000 0.500000 0.000000 0.02126(15) Uani 1 2 d S T P . . Cl1 Cl 0.14198(7) 0.26762(6) -0.00536(5) 0.02363(15) Uani 1 1 d . . . . . Cl2 Cl 0.01214(7) 0.52340(7) 0.24358(5) 0.02661(16) Uani 1 1 d . . . . . Cl3 Cl -0.37260(7) 0.23826(7) -0.06937(6) 0.02908(16) Uani 1 1 d . . . . . N1 N 0.5811(3) 0.5298(2) 0.18660(18) 0.0257(4) Uani 1 1 d . . . . . H1A H 0.518004 0.428913 0.117647 0.031 Uiso 1 1 calc GR . . . . H1B H 0.713410 0.570909 0.200135 0.031 Uiso 1 1 calc GR . . . . H1C H 0.543435 0.611554 0.167770 0.031 Uiso 1 1 calc GR . . . . N2 N 1.1698(3) 0.9104(2) 0.83594(19) 0.0275(4) Uani 1 1 d . . . . . H2A H 1.099317 0.799823 0.838726 0.033 Uiso 1 1 calc GR . . . . H2B H 1.124336 0.983506 0.876826 0.033 Uiso 1 1 calc GR . . . . H2C H 1.298999 0.948631 0.878021 0.033 Uiso 1 1 calc GR . . . . C1 C 0.5284(4) 0.4931(3) 0.3106(2) 0.0344(5) Uani 1 1 d . . . . . H1D H 0.563041 0.399367 0.328132 0.041 Uiso 1 1 calc R . . . . H1E H 0.384471 0.450284 0.296102 0.041 Uiso 1 1 calc R . . . . C2 C 0.6372(3) 0.6585(3) 0.4320(2) 0.0257(4) Uani 1 1 d . . . . . C3 C 0.5421(4) 0.7619(3) 0.4731(2) 0.0319(5) Uani 1 1 d . . . . . H3 H 0.411391 0.730776 0.424801 0.038 Uiso 1 1 calc R . . . . C4 C 0.6415(4) 0.9126(3) 0.5869(3) 0.0359(5) Uani 1 1 d . . . . . H4 H 0.576380 0.980927 0.615123 0.043 Uiso 1 1 calc R . . . . C5 C 0.8361(4) 0.9606(3) 0.6577(2) 0.0320(5) Uani 1 1 d . . . . . H5 H 0.902655 1.062862 0.732390 0.038 Uiso 1 1 calc R . . . . C6 C 0.9337(3) 0.8577(3) 0.6183(2) 0.0257(4) Uani 1 1 d . . . . . C7 C 0.8325(3) 0.7055(3) 0.5055(2) 0.0262(4) Uani 1 1 d . . . . . H7 H 0.895938 0.634737 0.479164 0.031 Uiso 1 1 calc R . . . . C8 C 1.1479(3) 0.9093(4) 0.6933(2) 0.0351(5) Uani 1 1 d . . . . . H8A H 1.191679 0.825223 0.648035 0.042 Uiso 1 1 calc R . . . . H8B H 1.234288 1.027753 0.690750 0.042 Uiso 1 1 calc R . . . . 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 0.0232(3) 0.0243(3) 0.0195(3) 0.00696(18) 0.00653(19) 0.0133(2) Cl1 0.0233(3) 0.0225(2) 0.0247(3) 0.00417(19) 0.0053(2) 0.01178(19) Cl2 0.0292(3) 0.0311(3) 0.0195(3) 0.00512(19) 0.0049(2) 0.0154(2) Cl3 0.0204(3) 0.0254(3) 0.0353(3) 0.0079(2) 0.0012(2) 0.0074(2) N1 0.0268(9) 0.0286(9) 0.0179(9) 0.0051(7) 0.0025(7) 0.0112(7) N2 0.0239(9) 0.0249(8) 0.0281(10) 0.0074(7) -0.0005(7) 0.0088(7) C1 0.0394(13) 0.0294(11) 0.0167(11) 0.0063(9) 0.0019(9) 0.0003(10) C2 0.0295(10) 0.0260(10) 0.0128(10) 0.0070(8) 0.0028(8) 0.0042(8) C3 0.0294(11) 0.0391(12) 0.0259(12) 0.0137(9) 0.0000(9) 0.0152(10) C4 0.0423(13) 0.0360(12) 0.0335(13) 0.0083(10) 0.0034(11) 0.0253(11) C5 0.0403(13) 0.0255(10) 0.0235(11) 0.0032(8) 0.0008(9) 0.0133(9) C6 0.0253(10) 0.0289(10) 0.0168(10) 0.0071(8) 0.0037(8) 0.0067(8) C7 0.0307(11) 0.0277(10) 0.0183(11) 0.0056(8) 0.0080(9) 0.0111(9) C8 0.0235(11) 0.0449(13) 0.0255(12) 0.0047(10) 0.0038(9) 0.0080(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0193 0.0097 '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 0.3694 0.7045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5661 2.8539 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0328 0.0186 '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 Cl1 Mn1 Cl1 180.0 2_565 . ? Cl1 Mn1 Cl3 89.852(15) . 2_565 ? Cl1 Mn1 Cl3 89.851(15) 2_565 . ? Cl1 Mn1 Cl3 90.149(15) 2_565 2_565 ? Cl1 Mn1 Cl3 90.149(15) . . ? Cl2 Mn1 Cl1 88.831(16) . . ? Cl2 Mn1 Cl1 91.169(16) 2_565 . ? Cl2 Mn1 Cl1 91.168(16) . 2_565 ? Cl2 Mn1 Cl1 88.832(16) 2_565 2_565 ? Cl2 Mn1 Cl2 180.0 2_565 . ? Cl2 Mn1 Cl3 91.587(17) . 2_565 ? Cl2 Mn1 Cl3 88.413(17) 2_565 2_565 ? Cl2 Mn1 Cl3 91.586(17) 2_565 . ? Cl2 Mn1 Cl3 88.414(17) . . ? Cl3 Mn1 Cl3 180.0 2_565 . ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H2A N2 H2B 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C8 N2 H2A 109.5 . . ? C8 N2 H2B 109.5 . . ? C8 N2 H2C 109.5 . . ? N1 C1 H1D 109.3 . . ? N1 C1 H1E 109.3 . . ? N1 C1 C2 111.72(17) . . ? H1D C1 H1E 107.9 . . ? C2 C1 H1D 109.3 . . ? C2 C1 H1E 109.3 . . ? C3 C2 C1 120.2(2) . . ? C3 C2 C7 119.5(2) . . ? C7 C2 C1 120.2(2) . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.1(2) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.5(2) . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.1(2) . . ? C5 C6 C8 121.4(2) . . ? C7 C6 C8 119.5(2) . . ? C2 C7 C6 120.5(2) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? N2 C8 C6 112.21(18) . . ? N2 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C6 C8 H8A 109.2 . . ? C6 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? 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 2.5787(4) . ? Mn1 Cl1 2.5786(4) 2_565 ? Mn1 Cl2 2.5138(5) . ? Mn1 Cl2 2.5138(5) 2_565 ? Mn1 Cl3 2.6627(5) 2_565 ? Mn1 Cl3 2.6628(5) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 C1 1.486(3) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N2 C8 1.480(3) . ? C1 H1D 0.9700 . ? C1 H1E 0.9700 . ? C1 C2 1.508(3) . ? C2 C3 1.381(3) . ? C2 C7 1.393(3) . ? C3 H3 0.9300 . ? C3 C4 1.393(3) . ? C4 H4 0.9300 . ? C4 C5 1.377(3) . ? C5 H5 0.9300 . ? C5 C6 1.388(3) . ? C6 C7 1.394(3) . ? C6 C8 1.510(3) . ? C7 H7 0.9300 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 -1 101854 1500.14 1 0 0 1 104475 1501.04 1 0 0 -2 112253 1710.18 1 0 0 2 116044 1707.2 1 0 0 3 143101 2187.37 1 0 0 -3 147038 2211.49 1 0 0 -4 213827 3271.16 3 0 0 4 209748 3183.28 1 0 0 -5 71171.7 1322.65 3 0 0 6 23776.1 713.644 5 0 0 7 10916.5 510.932 15 0 0 7 9743.01 485.568 5 0 0 8 22407.5 809.768 15 0 0 8 21935.6 834.925 5 0 0 9 12833.6 706.348 5 0 0 9 12284.5 620.593 15 0 0 10 7533.84 493.532 19 0 0 10 6967.38 575.673 5 0 0 11 5865.52 404.176 19 0 0 11 6637.22 526.305 5 0 0 12 51995.9 1165.62 19 0 0 12 54635.6 1178.09 5 0 -1 12 14569.8 546.527 19 0 -1 12 17559.5 662.574 5 0 -1 11 462.879 168.373 19 0 -1 11 -127.753 358.766 5 0 -1 10 599.485 254.398 5 0 -1 9 23112.9 721.981 18 0 -1 9 21770.7 871.786 5 0 -1 8 15221.5 550.305 18 0 -1 8 15519.4 663.792 5 0 -1 7 20022 591.029 18 0 -1 7 18185.8 657.474 5 0 -1 6 4058.72 278.689 22 0 -1 6 3412 238.231 5 0 1 -5 326036 4939.72 3 0 1 -4 461640 6248.23 3 0 -1 4 460809 6064.5 1 0 -1 3 79987 1175.23 1 0 1 -3 77242.5 1291.13 3 0 -1 2 53577.5 864.98 3 0 1 -2 50651 853.439 3 0 -1 1 120362 1744.81 1 0 -1 0 138962 2070.09 1 0 1 0 141421 2076.69 1 0 -1 0 142832 2074.17 4 0 1 0 139176 2069.72 4 0 -1 -1 81080.5 1226.23 4 0 1 1 82418.5 1256.69 4 0 -1 -2 102599 1653.27 1 0 -1 -2 100240 1635.29 4 0 -1 -3 37642.1 748.16 1 0 1 3 36861.9 614.535 2 0 -1 -3 39269.4 744.639 4 0 1 4 166660 2675.66 1 0 -1 -4 169173 2654.52 4 0 -1 -4 170622 2724.94 1 0 1 5 17606.9 558.404 5 0 -1 -5 19713.8 487.536 4 0 1 6 2990.43 259.706 5 0 1 7 1550.81 240.194 5 0 1 7 1229.44 208.152 15 0 1 8 40273.1 1226.38 15 0 1 8 40529.1 1220.09 5 0 1 9 21474.5 892.988 5 0 1 9 20322.1 838.451 15 0 1 9 18933.6 796.878 19 0 1 10 1737.42 263.324 19 0 1 10 2841 428.211 5 0 1 11 10905.3 502.078 5 0 1 11 7603.14 435.701 19 0 -2 12 3150.37 393.197 5 0 -2 12 2890.58 222.285 19 0 -2 11 6713.84 413.991 19 0 -2 11 8585.54 545.415 5 0 -2 10 3947.84 324.765 18 0 -2 10 824.139 250.585 5 0 -2 9 12497.9 545.994 18 0 -2 9 11871.6 625.127 5 0 -2 8 27115.9 875.029 5 0 -2 8 26844 785.655 18 0 -2 7 11681 496.573 5 0 -2 7 11645.1 544.601 22 0 -2 6 4377.15 266.345 5 0 -2 6 4474.13 294.092 22 0 2 -5 11748.4 398.99 3 0 2 -5 10892.5 282.58 2 0 -2 4 29323.7 678.62 3 0 -2 3 12058.8 215.254 1 0 -2 3 12472 341.151 3 0 -2 2 710901 10104.3 1 0 -2 2 709208 10206.8 3 0 -2 1 75097 1204.49 1 0 2 -1 76673.7 1247.43 4 0 2 0 19006.4 423.464 4 0 -2 0 20726.4 451.547 1 0 2 1 243265 3805.6 4 0 -2 -1 261826 3781.18 4 0 2 2 349482 5092.78 1 0 -2 -2 334536 5018.52 4 0 -2 -2 335326 5084.88 1 0 -2 -3 1605.88 137.695 1 0 -2 -3 1867.22 126.505 4 0 2 4 35089.1 923.077 5 0 -2 -4 37291.9 883.741 1 0 -2 -4 35289.6 760.448 4 0 2 5 22356.4 734.413 5 0 2 6 455.402 169.226 5 0 2 7 6732.51 435.985 19 0 2 7 7816.16 521.998 15 0 2 7 6938.52 483.134 5 0 2 8 1223.37 251.542 15 0 2 8 1854.48 390.296 5 0 2 8 1069.19 227.63 19 0 2 9 7065.41 571.584 5 0 2 9 6769.17 486.638 15 0 2 9 6334.85 458.231 19 0 2 10 7145 439.066 19 0 2 10 9779.39 511.141 5 0 2 11 432.374 104.53 19 0 2 11 614.955 120.374 5 0 -3 12 13836.2 674.592 5 0 -3 11 4574.85 332.636 18 0 -3 11 1068.36 260.149 5 0 -3 10 4304.21 415.749 5 0 -3 10 5604.68 387.427 18 0 -3 9 9739.71 494.772 18 0 -3 9 10363.2 567.037 5 0 -3 8 6906.39 427.833 5 0 -3 8 6934.97 392.907 18 0 -3 8 6716.07 458.265 22 0 -3 7 18018.6 633.735 8 0 -3 7 16354 681.084 22 0 -3 7 17601.4 650.71 5 0 -3 6 4237.36 292.036 5 0 -3 6 4363.46 294.209 8 0 -3 6 4266.66 311.463 22 0 -3 6 4138.47 254.135 14 0 -3 5 15257.8 542.312 5 0 -3 5 17734.9 581.17 3 0 -3 4 1411.36 138.073 3 0 -3 3 93488.8 1625.5 3 0 -3 3 93963.1 1468.39 1 0 3 -2 66921.9 1238.28 4 0 -3 2 69388.7 1162.76 1 0 -3 1 2527.66 145.988 1 0 3 -1 2388.94 156.024 4 0 -3 0 141477 2256.76 1 0 3 0 136218 2247.83 4 0 3 1 157286 2616.36 4 0 -3 -1 160946 2603.42 1 0 -3 -2 31167.9 717.076 4 0 3 3 167301 2757.48 19 0 -3 -3 159844 2662.27 4 0 3 4 113702 2074.1 19 0 3 4 105035 2194.99 5 0 3 5 15975.8 611.186 19 0 3 5 15337.4 658.801 5 0 3 6 723.228 229.453 5 0 3 6 987.501 196.692 19 0 3 7 10415.3 635.513 15 0 3 7 9810.66 543.388 19 0 3 7 9630.91 574.525 5 0 3 8 13112 652.05 5 0 3 8 12678.5 625.781 19 0 3 8 12408.8 702.282 15 0 3 9 2241.52 273.754 5 0 3 9 1766.97 264.833 15 0 3 9 1494.37 223.096 19 0 3 10 1936.53 196.305 19 0 3 10 1686.71 178.565 5 0 -4 12 23292.7 823.206 5 0 -4 11 820.853 233.345 5 0 -4 11 4843.87 345.215 18 0 -4 10 2384.12 298.822 18 0 -4 10 1319.2 271.202 5 0 -4 9 28759 918.858 18 0 -4 9 27601 1023.09 22 0 -4 8 15828.3 671.758 8 0 -4 8 15951.5 736.165 22 0 -4 8 17583.4 730.783 5 0 -4 7 603.444 171.439 22 0 -4 7 297.648 119.987 14 0 -4 7 260.884 144.999 5 0 -4 7 112.205 113.703 8 0 -4 6 22197.3 810.641 22 0 -4 6 21687.6 717.14 14 0 -4 6 23168.7 776.654 8 0 -4 6 23470.3 806.915 5 0 -4 5 17793 682.108 22 0 -4 5 18146.7 701.097 5 0 -4 5 18761.4 633.49 14 0 -4 5 19187.7 670.217 8 0 -4 5 19310.7 747.522 16 0 -4 4 223298 3750.04 8 0 -4 4 223967 3708.58 14 0 -4 4 226615 3822.61 16 0 -4 3 51900.8 1235.11 10 0 -4 3 50974.2 1148.89 8 0 -4 3 50563.8 960.692 1 0 -4 3 51189.5 1185.4 16 0 -4 2 123041 2130.73 3 0 -4 2 120996 2044.05 1 0 4 -2 121475 2135.6 4 0 4 -1 439389 6707.23 4 0 -4 1 431913 6663.73 1 0 -4 0 367096 5578.26 12 0 4 0 352011 5545.74 4 0 -4 0 360671 5520.54 1 0 4 1 48682.9 1148.77 4 0 -4 -1 51015.1 1130.85 12 0 -4 -2 24955.2 747.371 12 0 4 2 26633.8 773.155 19 0 -4 -3 93367.6 1837.68 12 0 4 3 94453.2 1893.71 19 0 -4 -4 146831 2629.19 12 0 4 4 143456 2707.93 19 0 4 5 4354.92 351.346 19 0 -4 -5 4374.82 314.36 12 0 4 5 3543.09 369.617 5 0 4 6 1902.03 248.895 19 0 4 6 1867.17 291.127 15 0 -4 -6 1955.84 214.707 12 0 4 6 1593.82 267.184 5 0 4 7 582.63 203.299 5 0 4 7 463.863 164.508 19 0 4 8 24228.4 791.521 19 0 4 8 23610.2 894.13 15 0 4 8 21430.4 756.769 5 0 4 9 9394.13 400.284 19 0 4 9 9113.43 399.825 5 0 -5 12 10714.1 514.417 5 0 -5 11 427.79 212.466 5 0 -5 11 4078.22 321.165 18 0 -5 10 691.594 231.218 5 0 -5 9 29795 955.801 18 0 -5 9 27942.6 1004.5 22 0 -5 9 31583 1083.88 5 0 -5 8 20365.3 792.961 14 0 -5 8 19860.9 851.848 22 0 -5 8 20903.7 832.101 8 0 -5 8 21375.6 763.418 18 0 -5 8 22566.5 900.692 5 0 -5 7 24119.2 946.772 22 0 -5 7 24909 915.18 8 0 -5 7 24550.4 873.033 14 0 -5 6 100614 2089.14 14 0 -5 6 99134.4 2147.3 8 0 -5 6 103333 2259.42 5 0 -5 6 96107.6 2201.98 22 0 -5 5 183239 3523.08 16 0 -5 5 182292 3508.51 22 0 -5 5 195075 3646.67 10 0 -5 5 187330 3401.23 8 0 -5 5 186538 3338.3 14 0 -5 4 149928 2968.62 16 0 -5 4 152406 3091.97 22 0 -5 3 25739.8 800.051 14 0 -5 3 27613 960.684 22 0 -5 2 43057.2 1230.86 22 0 -5 2 41174.4 1140.04 10 0 -5 1 63182 1412.6 14 0 -5 1 64560.4 1525.34 10 0 -5 1 66242.3 1491.64 12 0 -5 1 67627.7 1622.55 22 0 -5 0 186419 3239.31 14 0 -5 0 184673 3269.97 10 0 -5 0 179851 3241.58 12 0 -5 -1 2097.35 231.088 10 0 -5 -1 1825.69 219.462 12 0 -5 -2 16478.7 647.123 12 0 5 3 8503.52 488.306 19 0 -5 -3 8095.94 450.033 12 0 -5 -4 25523.7 820.957 12 0 5 4 25837.6 889.622 19 0 5 4 23544.4 894.119 15 0 5 5 267.197 151.912 15 0 5 5 80.8501 191.092 5 0 -5 -5 411.266 141.971 12 0 5 5 160.672 137.409 19 0 5 6 110.254 165.278 5 0 5 6 186.285 167.43 15 0 5 6 84.6299 119.579 19 0 5 7 26463.5 784.179 19 0 5 7 24917 806.338 5 0 -6 12 4211.8 285.614 5 0 -6 11 3676.33 334.726 5 0 -6 10 5122.54 427.216 5 0 -6 10 7903.16 450.242 18 0 -6 9 33648.6 984.625 18 0 -6 9 37363.1 1157.07 5 0 -6 8 10684 529.061 18 0 -6 8 9821.8 581.741 22 0 -6 8 10696.8 606.537 14 0 -6 7 433.099 164.426 18 0 -6 7 550.576 229.781 5 0 -6 7 618.569 203.142 14 0 -6 7 629.462 212.619 22 0 -6 6 1721.34 211.442 18 0 -6 6 2067.47 333.066 5 0 -6 6 1706.23 282.409 22 0 -6 6 1897.91 284.675 14 0 -6 5 10124.1 571.194 14 0 -6 5 10466.7 642.112 16 0 -6 5 11059.8 674.848 22 0 -6 4 1353.7 253.37 16 0 -6 4 1535.37 294.062 22 0 -6 4 1477.59 241.689 14 0 -6 3 27773.6 954.223 14 0 -6 3 30394 1165.22 22 0 -6 2 23640.2 855.628 14 0 -6 2 25911.6 1063.54 22 0 -6 2 24989.4 992.98 10 0 -6 1 2000.13 262.797 14 0 -6 1 2013.19 277.14 10 0 -6 1 2149.05 316.115 22 0 -6 0 4497.69 381.932 12 0 -6 0 4297.03 378.949 10 0 -6 0 3969.39 402.914 22 0 -6 -1 38522.1 1153.07 12 0 -6 -1 39577.7 1290.72 22 0 -6 -1 40663 1191.97 10 0 -6 -2 21953.9 817.796 12 0 6 2 21037.1 750.131 15 0 6 3 15553.2 652.761 15 0 -6 -3 16057.7 664.549 12 0 6 4 7820.09 460.937 15 0 -6 -4 8077.64 438.025 12 0 6 5 668.473 172.342 15 0 6 6 2670.95 251.873 15 0 -6 -6 2575.07 249.872 22 0 -6 -7 2005.27 171.457 22 0 -7 11 3229.57 265.453 5 0 -7 10 386.565 165.411 5 0 -7 9 3356.45 349.315 5 0 -7 9 5558.85 345.873 18 0 -7 8 1413.67 225.669 22 0 -7 8 1923.43 320.922 5 0 -7 7 3806.82 396.73 14 0 -7 7 4908.71 315.059 18 0 -7 7 5122.38 474.654 5 0 -7 7 3596.82 373.696 22 0 -7 6 8744.57 606.054 22 0 -7 6 9190.45 593.288 14 0 -7 6 10699.9 702.24 5 0 -7 5 829.116 282.926 5 0 -7 5 495.835 230.019 14 0 -7 5 688.832 228.773 22 0 -7 5 531.387 229.644 16 0 -7 4 21065.4 1051.31 22 0 -7 4 19840.9 1009.45 10 0 -7 4 19351.3 846.85 14 0 -7 3 29224.3 1127.39 20 0 -7 3 32683.8 1302.39 22 0 -7 3 29786.8 1059.76 14 0 -7 3 26725.6 1098.66 16 0 -7 3 31714.6 1251.67 10 0 -7 2 8483.89 640.22 22 0 -7 2 9582.32 656.298 10 0 -7 2 7736.09 554.698 16 0 -7 1 14798.2 827.094 22 0 -7 1 15279.7 764.715 16 0 -7 1 16514 831.755 10 0 -7 0 24257.8 935.449 16 0 -7 0 27327.3 1065.23 10 0 -7 0 24502.7 1044.85 22 0 -7 -1 1190.19 236.498 16 0 -7 -1 1313.63 240.505 10 0 -7 -1 1193.88 283.706 22 0 -7 -2 749.08 188.974 16 0 -7 -2 762.444 229.467 22 0 -7 -3 20028.3 692.933 16 0 -7 -3 19751.5 784.202 22 0 -7 -4 20233.2 712.691 22 0 7 5 385.582 96.0467 13 0 -8 10 634.6 133.667 5 0 -8 9 10980.9 505.454 5 0 -8 8 1273.33 229.788 5 0 -8 7 1003.55 245.581 5 0 -8 6 7188.03 535.912 5 0 -8 6 5287.44 439.838 22 0 -8 5 32166.7 1185.39 22 0 -8 5 30042.7 1182.44 16 0 -8 4 19901.5 952.783 22 0 -8 3 22670 1025.06 22 0 -8 3 20142.7 896.297 16 0 -8 2 19546.7 911.561 22 0 -8 2 18411.2 828.379 16 0 -8 2 18608.6 812.778 20 0 -8 1 74441.4 1806.83 16 0 -8 1 74003.9 1879.46 22 0 -8 0 47049.2 1365.08 22 0 -8 0 48815.2 1304.85 16 0 -8 -1 4983.26 347.209 16 0 -8 -1 4899.8 381.366 22 0 -8 -2 9406.39 408.011 16 0 -8 -2 9328.39 460.728 22 0 8 3 14509.7 536.429 13 0 -8 -3 15497.3 523.955 22 0 -9 8 25193.6 681.396 5 0 -9 7 13735.9 534.95 5 0 -9 6 33581.1 958.72 5 0 -9 5 56333.5 1381.36 5 0 -9 4 17147.6 690.739 5 0 -9 4 13675.9 585.847 22 0 -9 3 16819.1 677.262 5 0 -9 3 16616.8 679.818 16 0 -9 3 15076.7 621.871 22 0 9 -2 16549.4 586.385 13 0 -9 2 17187.5 652.467 16 0 -9 2 16169.5 625.044 22 0 -9 1 28126 795.718 16 0 9 -1 26287.6 771.199 13 0 -9 1 27341 797.646 22 0 9 0 5646.66 307.565 13 0 -9 0 5625.95 282.526 16 0 -9 0 5569.43 302.822 22 1 -10 3 1448.56 137.298 5 1 -10 4 5934.69 269.85 5 1 -10 5 2327.03 163.499 5 1 -9 -2 6620.43 299.501 20 -1 9 2 6274.47 318.688 13 1 -9 -2 6869.58 313.014 22 1 -9 -1 4054.72 283.408 22 1 -9 -1 3975.91 267.87 20 -1 9 1 3908.06 287.511 13 -1 9 0 16017.9 628.31 13 1 -9 0 16485.4 614.464 20 1 -9 0 16958.1 652.314 22 1 -9 0 16511.2 576.391 16 1 -9 1 14481 592.773 16 1 -9 1 13729.8 587.181 20 -1 9 -1 14971.2 621.554 13 1 -9 1 15183.1 660.052 22 1 -9 2 35394.2 1058.12 16 1 -9 2 35039.3 1109.78 22 -1 9 -2 35437.9 1014.56 13 1 -9 2 32758 994.922 20 1 -9 3 2366.13 302.876 22 1 -9 4 17862.1 730.536 5 1 -9 4 17864.4 767.745 22 1 -9 5 7479.61 441.487 5 1 -9 5 7578.15 496.962 22 1 -9 6 2693.34 272.174 5 1 -9 6 2635.32 290.03 22 1 -9 7 6439.77 369.645 5 1 -9 7 5652.74 371.924 22 1 -9 8 4464.46 268.442 5 -1 8 4 25191.3 743.756 13 1 -8 -4 26641.4 730.542 22 -1 8 3 62397.9 1462.35 13 1 -8 -1 16510.5 759.182 22 1 -8 -1 17372.8 676.582 16 1 -8 0 33705.6 1056.33 16 1 -8 0 32806.9 1169.84 22 1 -8 1 39083 1287.47 22 1 -8 1 38531.2 1203.2 16 1 -8 2 676.498 238.632 22 1 -8 2 603.84 211.038 16 1 -8 2 645.167 200.267 20 1 -8 3 1113.94 301.404 22 1 -8 3 1031.15 242.83 20 1 -8 3 1066.04 261.768 16 -1 8 -3 1023.86 214.331 13 1 -8 4 14492.4 735.554 20 1 -8 4 12950.1 752.569 16 1 -8 4 14093.6 796.423 22 1 -8 5 30102.7 1170.4 22 1 -8 5 31341.6 1122.21 5 1 -8 6 20997.8 945.802 22 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