#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:46:44 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242534 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132590.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_4132590 loop_ _publ_author_name 'Wei, Zhenhong' 'Liao, Wei-Qiang' 'Tang, Yuan-Yuan' 'Li, Peng-Fei' 'Shi, Ping-Ping' 'Cai, Hu' 'Xiong, Ren-Gen' _publ_section_title ; Discovery of an Antiperovskite Ferroelectric in [(CH3)3NH]3(MnBr3)(MnBr4). ; _journal_issue 26 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 8110 _journal_page_last 8113 _journal_paper_doi 10.1021/jacs.8b05037 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety '3(C3 H10 N),Br3 Mn, Br4 Mn' _chemical_formula_sum 'C9 H30 Br7 Mn2 N3' _chemical_formula_weight 849.61 _space_group_crystal_system hexagonal _space_group_IT_number 186 _space_group_name_Hall 'P 6c -2c' _space_group_name_H-M_alt 'P 63 m c' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 2 _cell_length_a 14.6822(5) _cell_length_b 14.6822(5) _cell_length_c 6.6323(3) _cell_measurement_reflns_used 5153 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 27.4700 _cell_measurement_theta_min 1.7529 _cell_volume 1238.16(8) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.916 _diffrn_measurement_device_type 'Rigaku saturn 724' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.916 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 6278 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.911 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.188 _diffrn_reflns_theta_min 2.775 _exptl_absorpt_coefficient_mu 12.312 _exptl_absorpt_correction_T_max 0.067 _exptl_absorpt_correction_T_min 0.045 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 2.279 _exptl_crystal_description needle _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _refine_diff_density_max 1.298 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.204 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 1171 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0385 _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^)+(0.0333P)^2^+2.8325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.0789 _reflns_Friedel_coverage 0.841 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.905 _reflns_number_gt 1067 _reflns_number_total 1171 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05037_si_002.cif _cod_data_source_block P63mc _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_original_cell_volume 1238.16(10) _cod_database_code 4132590 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; P63mc.res created by SHELXL-2014/7 TITL P63mc in P6(3)mc CELL 0.71073 14.6822 14.6822 6.6323 90.000 90.000 120.000 ZERR 2.00 0.0005 0.0005 0.0003 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -X, -Y, 0.5+Z SYMM Y, -X+Y, 0.5+Z SYMM X-Y, X, 0.5+Z SYMM -Y, -X, Z SYMM -X+Y, Y, Z SYMM X, X-Y, Z SYMM Y, X, 0.5+Z SYMM X-Y, -Y, 0.5+Z SYMM -X, -X+Y, 0.5+Z SFAC C H N Br Mn UNIT 18 60 6 14 4 L.S. 40 ACTA BOND $H FMAP 2 PLAN 20 twin CONF TEMP -180 WGHT 0.033300 2.832500 BASF -0.01553 FVAR 0.09488 C1 1 0.348212 0.174106 0.627510 10.50000 0.00592 0.02000 = 0.01678 -0.00123 -0.00246 0.00296 AFIX 3 H1A 2 0.363161 0.129810 0.549940 11.00000 0.03369 H1B 2 0.276152 0.138076 0.664349 10.50000 0.02432 AFIX 0 MN2 5 0.333333 0.666667 0.849906 10.16667 0.01089 0.01089 = 0.01023 0.00000 0.00000 0.00545 BR2 4 0.427118 0.854237 0.963610 10.50000 0.01420 0.01047 = 0.01714 -0.00255 -0.00127 0.00523 BR1 4 0.166374 0.083187 0.248456 10.50000 0.00590 0.01072 = 0.00805 -0.00001 -0.00003 0.00295 MN1 5 0.000000 0.000000 -0.001458 10.16667 0.00867 0.00867 = 0.00668 0.00000 0.00000 0.00433 BR3 4 0.333333 0.666667 0.467292 10.16667 0.01089 0.01089 = 0.01039 0.00000 0.00000 0.00544 N1 3 0.415086 0.207543 0.808371 10.50000 0.00474 0.01371 = 0.02034 0.00114 0.00228 0.00237 AFIX 3 H1D 2 0.481986 0.240993 0.769011 10.50000 0.08670 AFIX 0 C2 1 0.399003 0.283677 0.930485 11.00000 0.01199 0.01436 = 0.01811 -0.00340 -0.00090 0.00605 AFIX 3 H2A 2 0.442304 0.302927 1.047126 11.00000 0.04480 H2B 2 0.416573 0.344647 0.852945 11.00000 0.04402 H2C 2 0.327403 0.251267 0.970195 11.00000 0.02435 AFIX 0 HKLF 4 REM P63mc in P6(3)mc REM R1 = 0.0385 for 1067 Fo > 4sig(Fo) and 0.0465 for all 1171 data REM 50 parameters refined using 0 restraints END WGHT 0.0157 3.6738 REM Highest difference peak 1.298, deepest hole -1.257, 1-sigma level 0.204 Q1 1 0.3333 0.6667 0.9558 10.16667 0.05 1.30 Q2 1 0.0241 0.0482 -0.0650 10.50000 0.05 1.05 Q3 1 0.1027 0.0513 0.2035 10.50000 0.05 0.87 Q4 1 0.5784 0.4216 0.9573 10.50000 0.05 0.85 Q5 1 -0.0784 -0.0392 0.0645 10.50000 0.05 0.84 Q6 1 0.4295 0.8590 1.1496 10.50000 0.05 0.83 Q7 1 0.0000 0.0000 0.1699 10.16667 0.05 0.78 Q8 1 0.2176 0.1088 0.6632 10.50000 0.05 0.77 Q9 1 0.4924 0.8899 0.8890 11.00000 0.05 0.76 Q10 1 0.1554 0.0297 0.1597 11.00000 0.05 0.76 Q11 1 0.0991 0.0496 0.3384 10.50000 0.05 0.75 Q12 1 0.5646 0.3524 0.9702 11.00000 0.05 0.74 Q13 1 0.5242 0.9804 0.9881 11.00000 0.05 0.73 Q14 1 0.5494 0.4506 1.0312 10.50000 0.05 0.73 Q15 1 0.2247 0.0913 0.1687 11.00000 0.05 0.72 Q16 1 0.4970 0.3160 1.0321 11.00000 0.05 0.71 Q17 1 0.1720 0.0860 0.4247 10.50000 0.05 0.71 Q18 1 0.3942 0.7883 1.0523 10.50000 0.05 0.71 Q19 1 0.2279 0.1140 0.3176 10.50000 0.05 0.71 Q20 1 0.4595 0.9189 1.0176 10.50000 0.05 0.70 ; _shelx_res_checksum 17122 _shelx_hkl_file ; 0 0 -6 144.10 9.46 0 0 -5 -0.26 2.17 0 0 -4 641.28 36.19 0 0 -3 0.24 1.18 0 0 -2 328.28 18.53 0 0 -1 -0.05 0.35 0 0 1 0.15 0.16 0 0 2 305.51 17.02 0 0 3 0.41 0.54 0 0 4 612.05 34.10 0 0 5 0.92 1.05 0 0 6 145.74 8.57 0 0 7 2.91 1.62 0 0 8 114.10 7.07 -1 0 -6 76.07 5.80 0 -1 -6 68.38 5.57 1 -1 -6 71.55 5.66 -1 1 -6 74.94 5.67 0 -1 -5 0.26 2.15 -1 1 -5 0.27 2.19 1 -1 -5 0.13 2.13 -1 0 -5 -0.26 2.09 0 -1 -4 96.70 6.39 1 -1 -4 99.37 6.46 -1 1 -4 99.45 6.50 -1 0 -4 103.09 6.50 -1 1 -3 4.55 1.36 -1 0 -3 4.53 1.36 1 -1 -3 5.44 1.35 0 -1 -3 4.35 1.30 0 -1 -2 333.35 18.38 1 -1 -2 343.86 18.41 -1 1 -2 323.11 18.12 -1 0 -2 323.64 18.02 -1 0 -2 326.37 18.15 1 -1 -1 23.34 1.63 0 -1 -1 27.64 1.65 -1 1 1 27.35 1.81 0 1 1 28.05 1.69 1 -1 1 28.36 1.66 1 0 1 28.02 1.69 -1 0 1 30.78 1.81 0 1 2 301.39 17.23 0 1 2 310.49 17.09 0 -1 2 307.10 17.15 1 0 2 308.78 17.24 -1 0 2 313.63 17.09 1 -1 2 292.80 17.19 -1 1 2 310.73 17.47 -1 0 2 316.62 17.48 0 -1 3 4.13 0.56 -1 1 3 2.40 1.25 -1 0 3 3.65 0.56 1 -1 3 3.35 0.61 -1 1 3 2.65 0.63 1 0 3 2.98 0.74 0 1 3 2.41 0.65 1 0 4 94.04 5.43 -1 0 4 86.60 5.30 1 -1 4 90.66 5.36 -1 1 4 88.28 5.36 0 -1 4 95.66 5.32 0 1 4 91.68 5.42 1 0 5 0.34 1.09 1 -1 5 0.25 0.99 -1 0 5 0.87 0.91 -1 1 5 0.89 0.99 0 -1 5 0.47 0.93 0 1 5 1.72 1.19 1 0 6 65.82 4.28 -1 1 6 60.41 4.18 -1 0 6 62.59 4.12 0 1 6 64.71 4.28 1 -1 6 67.23 4.19 0 -1 6 66.88 4.11 0 1 7 6.26 1.78 -1 0 7 4.53 1.50 1 0 7 5.07 1.83 1 -1 7 5.27 1.52 -1 1 7 6.00 1.70 0 -1 7 4.12 1.43 -1 1 8 58.15 4.29 -1 0 8 63.18 4.11 1 -1 8 58.14 4.09 1 0 8 58.53 4.25 0 1 8 58.91 4.35 1 -2 -6 10.56 2.83 -2 1 -6 13.93 3.14 -1 -1 -6 7.83 2.80 1 1 -6 9.74 3.03 -2 1 -5 -1.11 2.31 -1 -1 -5 -1.53 2.13 1 -2 -5 0.38 2.15 -1 -1 -4 103.86 6.45 -2 1 -4 94.28 6.49 1 -2 -4 101.46 6.47 -2 1 -3 0.34 0.61 1 -2 -3 0.48 1.26 -1 -1 -3 0.32 1.25 1 -2 -2 61.93 3.86 -1 -1 -2 65.55 3.87 -2 1 -2 59.99 3.62 -1 2 -2 61.80 3.53 1 1 -1 0.23 0.22 -1 -1 -1 -0.18 0.30 1 -2 -1 0.71 0.51 2 -1 -1 0.04 0.54 -1 -1 -1 0.36 0.21 -1 -1 0 456.66 23.95 1 1 0 432.63 23.95 -1 -1 0 408.33 23.95 1 1 1 0.02 0.31 -2 1 1 0.92 0.55 -1 -1 1 0.46 0.37 2 -1 1 0.25 0.30 1 1 2 58.70 3.46 2 -1 2 58.99 3.43 -2 1 2 59.26 3.70 1 -2 2 56.64 3.31 -2 1 3 2.26 1.38 2 -1 3 0.07 0.67 1 -2 3 0.16 0.45 1 1 3 1.00 0.73 -1 -1 3 0.19 0.38 2 -1 4 102.85 6.03 -1 2 4 97.91 6.01 -2 1 4 101.66 6.60 1 1 4 103.76 6.08 1 -2 4 99.67 5.88 -1 -1 4 104.52 5.86 2 -1 5 0.11 1.14 -1 2 5 2.12 1.16 1 -2 5 1.16 0.88 -1 -1 5 0.53 0.79 -2 1 5 0.10 0.94 1 1 5 0.46 1.25 1 1 6 14.27 1.87 -2 1 6 15.91 1.68 2 -1 6 14.29 1.77 -1 2 6 12.86 1.78 -1 -1 6 16.13 1.50 1 -2 6 11.71 1.45 1 -2 7 0.83 1.24 -1 -1 7 2.22 1.27 1 1 7 0.97 1.84 -2 1 7 -0.97 1.46 -1 2 7 2.33 1.82 2 -1 7 1.50 1.62 1 1 8 43.88 3.54 -2 1 8 38.65 3.23 2 -1 8 39.23 3.26 -1 2 8 38.08 3.46 -2 0 -6 1.29 2.76 0 2 -6 0.80 3.04 2 -2 -6 0.31 2.63 0 -2 -6 5.45 2.72 -2 0 -5 33.82 3.39 2 -2 -5 37.91 3.46 0 -2 -5 32.98 3.33 0 2 -5 29.06 3.41 -2 2 -5 31.77 3.55 2 -2 -4 59.79 4.50 -2 0 -4 63.08 4.53 0 -2 -4 64.98 4.47 -2 0 -3 58.29 3.33 2 -2 -3 57.66 3.77 -2 0 -3 54.41 3.07 0 -2 -3 62.64 3.78 0 2 -3 48.99 3.07 -2 2 -3 58.75 3.25 -2 0 -2 13.29 1.11 0 -2 -2 14.95 1.37 2 -2 -2 15.19 1.38 -2 2 -2 14.42 1.01 -2 0 -2 13.37 0.91 2 -2 -1 16.91 1.38 0 -2 -1 17.81 1.22 -2 0 0 11.73 0.81 -2 0 1 15.09 1.16 2 0 1 14.94 1.07 0 2 1 16.01 1.05 -2 2 1 15.21 1.34 -2 2 2 13.83 1.48 -2 0 2 14.21 1.37 0 2 2 16.60 1.18 2 -2 2 14.12 1.08 2 0 3 58.80 3.58 -2 2 3 56.09 3.97 0 -2 3 54.53 3.33 2 -2 3 53.20 3.43 0 2 3 59.52 3.31 0 2 3 54.48 3.54 -2 0 3 56.66 3.95 -2 0 3 62.36 3.31 0 2 4 59.20 3.73 0 -2 4 61.24 3.50 -2 0 4 54.40 3.53 -2 2 4 61.30 4.38 2 -2 4 59.45 3.61 2 0 4 62.50 3.80 2 -2 5 34.70 2.33 0 -2 5 32.71 2.14 -2 0 5 30.15 2.20 0 2 5 30.91 2.48 -2 2 5 29.52 2.36 2 0 5 35.94 2.57 0 -2 6 1.47 0.96 2 -2 6 0.98 1.18 0 2 6 1.32 1.54 2 0 6 3.33 1.59 -2 2 6 2.68 1.36 -2 0 6 2.14 1.15 0 -2 7 5.90 1.24 2 0 7 5.76 1.89 -2 0 7 4.49 1.40 -2 2 7 3.65 1.73 2 -2 7 4.41 1.46 0 2 7 2.98 1.84 -2 2 8 7.00 2.04 0 2 8 2.53 2.21 2 0 8 6.50 2.09 -1 -2 -6 6.27 2.83 -1 3 -6 9.09 3.03 1 2 -6 9.09 2.96 -3 2 -6 7.09 3.07 1 -3 -6 10.53 2.94 -2 -1 -6 6.64 2.81 2 -3 -6 8.47 2.94 -3 1 -6 4.89 2.95 2 1 -6 8.98 3.05 -2 -1 -5 35.41 3.55 -1 3 -5 37.37 3.81 1 -3 -5 39.69 3.62 1 2 -5 39.12 3.74 -1 -2 -5 37.91 3.64 2 1 -5 40.36 3.73 3 -2 -5 41.43 3.73 -3 1 -5 36.14 3.68 2 -3 -5 37.70 3.63 -3 2 -5 34.07 3.72 3 -2 -4 11.27 2.08 -1 3 -4 7.66 0.65 -1 -2 -4 8.74 1.84 2 1 -4 6.97 2.01 -3 2 -4 9.70 1.14 1 -3 -4 11.01 1.94 2 -3 -4 10.81 2.05 -1 3 -4 7.39 2.14 1 2 -4 7.04 1.90 -2 -1 -4 5.21 1.76 -3 1 -4 7.82 0.68 -3 1 -4 10.04 1.22 -3 2 -3 191.57 10.97 1 -3 -3 192.56 11.31 -3 1 -3 194.72 11.01 -1 -2 -3 184.00 11.26 1 2 -3 197.72 11.31 2 1 -3 197.44 11.32 -2 3 -3 198.61 10.86 -2 -1 -3 194.76 11.02 2 -3 -3 188.41 11.32 3 -2 -3 177.86 11.34 -2 -1 -3 194.37 11.31 1 -3 -2 10.52 1.27 3 -2 -2 10.69 1.42 -1 3 -2 11.57 0.77 1 2 -2 10.83 0.85 -3 2 -2 12.40 1.03 -2 3 -2 12.85 0.90 -3 1 -2 10.78 1.06 2 1 -2 10.95 1.25 1 2 -2 14.33 1.37 -2 -1 -2 13.93 0.86 2 -3 -2 10.40 1.34 -1 -2 -2 13.27 1.23 2 -3 -1 91.20 5.69 -1 -2 -1 97.44 5.47 1 2 -1 101.08 5.49 1 2 -1 98.16 5.35 3 -2 -1 90.91 5.77 -1 -2 -1 105.71 5.50 2 1 -1 86.61 5.49 1 -3 -1 88.58 5.57 -2 -1 -1 95.12 5.50 1 2 -1 91.04 5.41 -2 -1 -1 96.13 5.41 -2 -1 0 2.70 0.39 -1 -2 0 3.22 0.38 2 1 0 2.37 0.38 -2 -1 0 2.84 0.42 1 2 0 3.07 0.37 -1 -2 1 101.27 5.77 -2 -1 1 105.68 5.94 3 -1 1 106.44 5.94 -2 -1 1 101.47 5.82 -3 2 1 103.06 6.26 -3 1 1 108.51 6.20 1 2 1 106.58 5.93 2 1 1 104.44 5.95 1 2 2 8.13 0.74 3 -2 2 8.32 0.84 -3 1 2 9.01 1.25 -2 -1 2 9.72 0.72 1 2 2 8.91 0.93 -3 2 2 9.98 1.35 3 -1 2 10.03 0.93 2 1 2 8.96 0.94 -2 -1 2 9.90 1.15 3 -1 3 192.93 11.17 -3 1 3 191.75 11.53 3 -2 3 188.59 11.12 -3 2 3 202.09 11.61 -1 -2 3 195.39 10.91 -1 3 3 191.99 11.17 1 2 3 201.19 10.98 1 2 3 199.94 11.22 2 1 3 199.48 11.22 3 -2 4 5.32 0.99 -3 1 4 7.93 1.96 3 -1 4 6.64 1.17 -1 3 4 6.16 1.17 2 -3 4 4.61 0.78 1 2 4 9.28 1.22 -3 1 4 6.42 0.61 2 1 4 5.14 1.17 1 -3 4 5.74 0.72 -3 2 4 6.63 2.00 -1 -2 4 4.96 0.66 -1 3 4 6.39 0.59 -2 -1 4 5.29 0.70 2 1 5 37.59 2.70 3 -2 5 34.84 2.47 1 2 5 36.48 2.72 1 -3 5 33.16 2.18 3 -1 5 36.76 2.65 -2 -1 5 32.48 2.21 -1 3 5 31.37 2.54 -1 -2 5 34.00 2.15 -3 1 5 31.27 2.34 -2 3 5 33.43 2.57 -3 2 5 31.28 2.42 2 -3 5 34.31 2.26 3 -1 6 5.36 1.56 -2 -1 6 3.00 1.01 2 1 6 3.91 1.73 1 -3 6 3.89 0.93 -1 3 6 4.50 1.67 -3 2 6 3.12 1.34 -1 -2 6 4.78 0.98 -2 3 6 4.52 1.54 1 2 6 3.33 1.62 2 -3 6 4.20 1.10 3 -2 6 4.51 1.40 -3 1 6 4.23 1.26 -2 -1 7 42.06 2.89 3 -1 7 43.87 3.36 -3 2 7 44.60 3.29 -1 -2 7 39.84 2.75 2 -3 7 41.35 2.87 1 2 7 45.62 3.61 2 1 7 47.00 3.57 -3 1 7 41.47 3.09 3 -2 7 44.16 3.22 -2 3 7 42.96 3.45 1 -3 7 41.33 2.78 -1 3 7 42.20 3.48 -1 3 8 7.24 2.39 -3 2 8 4.12 2.00 -2 3 8 5.47 2.29 1 2 8 8.84 2.51 3 -2 8 4.81 1.81 2 1 8 10.59 2.43 3 -1 8 5.41 2.13 -3 0 -6 46.26 4.45 3 0 -6 50.55 4.60 0 -3 -6 47.49 4.32 0 3 -6 42.18 4.61 0 -3 -5 201.76 12.73 0 3 -5 214.66 12.90 3 -3 -5 218.14 12.89 -3 0 -5 209.06 12.89 3 0 -5 217.88 12.85 3 0 -4 19.63 2.34 -3 0 -4 19.70 1.67 0 -3 -4 13.06 2.10 0 3 -4 15.06 1.12 0 3 -4 17.06 2.33 3 -3 -4 16.60 2.42 -3 0 -4 15.64 2.28 -3 3 -4 18.87 1.44 0 -3 -3 57.91 3.81 -3 0 -3 56.76 3.23 3 -3 -3 55.57 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3.90 6 4 -4 79.87 5.06 -10 6 -4 66.63 4.65 4 -10 -4 73.35 5.10 -10 4 -4 70.99 4.76 -10 4 -3 16.30 2.20 6 4 -3 20.87 2.44 4 6 -3 15.94 1.93 -6 -4 -3 19.69 2.10 -6 -4 -3 18.98 2.09 -4 -6 -3 18.93 1.89 -10 6 -3 19.40 2.28 4 6 -3 22.93 2.26 -6 -4 -2 32.72 2.54 -4 -6 -2 30.79 2.46 4 6 -2 28.52 2.50 -10 6 -2 31.78 2.68 -4 -6 -2 29.80 2.15 4 6 -2 35.41 2.39 -6 -4 -1 3.24 1.24 4 6 -1 4.27 1.27 -10 4 -1 3.84 1.52 -6 -4 -1 6.27 1.12 -4 -6 -1 4.46 1.18 4 6 -1 5.44 1.35 -6 -4 0 64.82 4.11 -6 -4 0 74.73 4.07 -4 -6 0 63.99 4.01 4 6 0 59.63 4.17 6 4 0 67.86 4.39 -6 -4 0 60.10 3.76 4 6 0 64.56 4.25 -6 -4 1 4.05 1.08 4 6 1 2.79 1.61 6 4 1 5.19 1.65 -4 10 1 5.98 2.39 -10 4 1 -0.46 3.14 -6 -4 1 6.72 1.13 -6 10 1 6.73 2.99 -6 -4 1 4.80 0.82 -4 -6 1 3.66 0.90 -6 10 2 28.02 4.15 -4 -6 2 33.93 2.19 -10 4 2 37.16 4.66 4 6 2 33.24 2.63 -6 -4 2 35.26 2.43 -4 10 2 31.11 3.44 -10 6 2 44.48 5.44 4 6 2 36.02 2.98 -6 -4 2 30.68 2.24 4 6 3 22.68 2.12 -4 10 3 22.91 3.19 -6 10 3 28.52 3.90 -10 4 3 22.42 4.28 -6 -4 3 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195.22 10.20 -10 7 -3 179.51 10.49 3 7 -3 191.22 10.34 -3 -7 -3 161.62 10.20 -10 3 -3 178.24 10.57 7 3 -3 188.22 10.59 -7 -3 -2 14.28 1.88 3 7 -2 15.19 1.50 -7 -3 -2 16.91 1.62 3 7 -2 12.44 1.69 3 7 -2 16.40 1.56 -3 -7 -2 15.26 1.42 -7 -3 -1 92.20 5.91 -7 -3 -1 108.39 5.81 -10 3 -1 100.75 6.13 3 7 -1 102.33 5.87 -7 -3 0 50.11 3.06 3 7 0 38.75 3.11 -10 3 0 44.25 3.30 -7 -3 0 45.63 3.16 3 7 0 46.10 3.23 7 3 0 48.04 3.35 -7 -3 0 40.44 3.07 3 7 1 107.87 6.44 7 3 1 114.08 6.57 -7 -3 1 95.92 6.10 -3 10 1 95.51 6.63 -10 3 1 95.09 7.75 -7 10 1 100.33 7.58 -7 -3 1 95.78 6.13 -7 -3 1 116.96 6.21 -3 10 2 11.80 2.33 -7 -3 2 11.36 1.38 -7 10 2 15.66 3.98 -7 -3 2 14.11 1.56 3 7 2 10.92 1.99 -10 7 2 11.24 4.61 -10 3 2 15.99 3.82 3 7 2 11.72 1.65 -7 -3 2 13.49 1.57 3 7 3 180.84 10.64 -7 -3 3 208.80 10.55 -7 -3 3 173.90 10.78 -3 10 3 174.52 11.15 7 3 3 184.49 11.03 -10 3 3 185.84 12.04 -7 10 3 183.70 12.10 -10 7 3 192.98 12.85 -7 -3 3 169.31 10.42 -10 3 4 12.84 3.83 -7 -3 4 11.05 1.20 -7 10 4 9.53 3.93 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30.49 4.63 -6 11 5 30.49 5.12 5 6 6 2.22 3.12 -6 11 6 0.64 2.67 -5 11 6 7.42 2.79 -5 11 6 2.24 4.42 -6 11 6 9.02 5.03 6 5 6 3.84 3.12 -11 5 6 7.96 5.33 -11 6 6 10.01 5.25 5 6 7 35.67 4.21 -5 11 7 24.40 3.80 -6 11 7 29.09 3.96 -6 11 7 34.21 6.36 6 5 7 33.98 4.38 -11 5 7 41.20 6.65 -11 6 7 35.82 6.91 -7 -4 -5 110.45 7.80 -4 -7 -5 116.32 7.58 4 7 -5 136.05 7.99 7 4 -5 134.43 8.13 -7 11 -5 116.48 7.06 -11 7 -5 121.10 7.57 -11 7 -4 15.98 2.42 -4 -7 -4 15.77 2.01 4 7 -4 15.76 2.62 -11 4 -4 16.10 2.45 7 4 -4 19.50 2.86 -7 11 -4 14.89 1.78 -4 11 -4 14.96 1.25 -7 -4 -4 18.34 2.40 -7 -4 -3 47.29 3.45 4 7 -3 42.07 3.32 -7 -4 -3 44.00 3.36 -11 7 -3 46.01 3.59 -4 -7 -3 40.91 3.06 4 7 -3 48.95 3.39 -11 4 -3 46.48 3.65 -11 7 -2 15.61 2.01 4 7 -2 15.31 1.60 -7 -4 -2 14.30 1.87 -4 -7 -2 15.39 1.34 4 7 -2 14.97 1.50 4 7 -2 11.46 1.88 -7 -4 -1 151.01 8.83 -7 -4 -1 163.93 8.72 4 7 -1 125.92 8.76 -11 4 -1 147.02 8.99 4 7 -1 154.83 8.83 -7 -4 0 3.65 1.12 4 7 0 0.80 1.63 -7 -4 0 2.76 0.84 -11 4 0 3.07 1.37 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290.98 17.48 7 7 0 337.62 17.92 -7 14 1 -1.96 3.47 -7 -7 1 -0.70 1.19 7 7 1 0.12 2.47 -7 -7 2 104.74 6.34 7 7 2 112.08 7.27 -7 14 2 102.01 7.96 -14 7 2 121.46 10.16 -7 14 3 0.56 3.89 -14 7 3 -3.40 5.89 -7 -7 3 0.36 0.97 7 7 3 -0.27 2.61 -7 14 4 111.70 8.64 -14 7 4 113.36 10.41 -14 7 5 -0.38 6.42 7 7 5 0.48 3.34 -7 14 5 3.12 4.85 -14 7 6 45.02 8.09 -7 14 6 30.35 6.10 -8 14 -4 7.86 1.78 6 8 -4 17.01 2.68 -8 -6 -3 19.83 1.96 -6 -8 -3 20.83 1.78 -8 -6 -2 16.57 1.39 -8 -6 -1 12.77 1.90 6 8 -1 14.06 2.35 -6 -8 0 9.99 1.61 8 6 0 9.95 2.53 -6 14 0 14.07 3.30 6 8 0 8.74 2.16 6 8 0 13.04 2.41 -8 -6 0 9.37 1.62 -14 6 1 8.97 4.68 -6 14 1 10.93 3.59 -8 14 1 4.85 3.84 -14 8 1 9.73 5.14 8 6 1 9.58 2.63 -8 -6 1 7.14 1.48 6 8 1 9.58 2.67 -8 -6 2 15.70 1.61 -6 14 2 8.13 3.65 -8 14 2 13.50 4.59 -14 6 2 19.86 5.54 -14 8 2 13.81 5.87 8 6 2 13.31 2.89 6 8 2 13.56 2.91 6 8 3 25.04 3.32 -6 14 3 19.08 3.91 -8 14 3 10.18 4.40 -8 -6 3 18.01 1.63 -14 6 3 19.60 5.95 -14 8 3 14.84 6.41 8 6 3 15.76 3.20 -6 14 4 7.16 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4.44 -10 19 2 4.91 4.92 -19 9 2 1.67 7.04 -19 10 2 3.70 8.45 10 9 2 5.50 4.05 9 10 2 6.06 4.04 -9 19 3 12.24 4.62 -10 19 3 11.86 5.11 -9 19 4 8.42 4.98 -10 19 4 -2.80 5.14 -8 19 -1 29.70 4.11 -8 19 0 0.40 3.38 -11 19 0 8.73 5.20 8 11 0 1.85 3.33 -19 8 0 -4.67 5.98 -8 19 1 24.00 4.26 -11 19 1 30.23 5.98 -19 8 1 31.48 7.47 8 11 1 36.48 4.42 -8 19 2 17.57 4.08 -11 19 2 11.02 5.60 -19 8 2 23.29 7.60 11 8 2 16.98 4.29 8 11 2 20.33 4.20 -8 19 3 11.65 4.25 -11 19 3 6.39 5.47 -7 19 -2 32.73 3.70 -7 19 -1 17.84 3.12 7 12 -1 16.21 3.29 -7 19 -1 11.83 3.22 -7 19 0 -2.26 3.21 -12 19 0 -2.00 5.90 -19 7 0 2.83 4.90 7 12 0 0.39 3.26 -7 19 0 -3.06 2.88 -7 19 1 8.41 3.44 -19 7 1 19.49 5.74 -7 19 1 10.32 3.06 7 12 1 12.04 3.92 -7 19 2 28.59 4.15 -12 19 2 23.62 6.38 -19 7 2 43.22 7.06 7 12 2 28.10 4.59 -7 19 2 28.67 3.63 -12 19 3 19.00 6.40 -6 19 -1 7.00 2.78 6 13 -1 4.40 2.92 -19 6 0 2.42 4.28 -13 19 0 13.85 6.82 6 13 0 4.47 3.38 -6 19 0 0.83 2.64 -19 6 1 8.17 5.11 -13 19 1 1.95 6.27 6 13 1 4.50 3.40 -6 19 1 2.91 2.85 -19 6 2 7.67 5.08 -13 19 2 12.95 6.45 -6 19 2 6.38 2.89 6 13 2 6.85 3.88 -19 6 3 18.32 5.62 5 14 -1 2.92 2.89 -5 19 -1 0.38 2.57 -5 19 0 85.80 6.18 5 14 0 86.04 6.55 -19 5 0 92.08 7.57 -14 19 0 107.12 10.29 -5 19 1 2.33 2.81 -19 5 1 2.47 4.36 -14 19 1 12.72 6.89 5 14 1 0.14 3.39 -19 5 2 22.38 5.16 -14 19 2 24.08 7.52 5 14 2 25.52 4.23 -19 5 3 5.05 4.75 -4 19 -1 3.31 2.82 4 15 -1 3.75 3.00 -4 19 0 6.59 2.88 -19 4 0 11.28 3.91 4 15 0 9.17 3.35 -19 4 1 6.50 3.89 -4 19 1 5.05 3.09 4 15 1 6.59 3.59 -19 4 2 25.70 4.50 3 16 0 5.84 3.27 -3 19 0 11.28 3.06 3 16 1 2.91 3.41 -3 19 1 7.33 3.13 2 17 0 22.59 3.85 -2 19 0 16.06 3.36 2 17 1 1.17 3.42 -2 19 1 1.54 3.16 -10 20 -1 8.38 4.30 -10 20 0 30.01 4.96 -10 20 1 -3.93 4.35 10 10 1 6.39 3.85 -10 20 2 56.97 6.15 -10 20 3 -0.37 4.61 -9 20 -1 8.19 3.71 -11 20 -1 6.15 4.92 -9 20 0 10.02 3.84 -11 20 0 9.86 5.13 -9 20 1 7.32 3.87 -11 20 1 12.62 5.15 9 11 1 8.03 4.12 -9 20 2 10.66 4.12 -11 20 2 19.79 5.37 -11 20 3 8.52 5.48 -8 20 -1 39.17 4.54 -12 20 0 14.21 5.85 8 12 0 8.22 3.63 -20 8 0 15.03 5.66 -8 20 0 17.33 3.58 -8 20 1 38.39 4.42 -12 20 1 41.25 6.72 8 12 1 42.09 5.09 -12 20 2 10.05 5.68 -7 20 -1 23.16 3.63 -7 20 0 -1.19 2.99 -20 7 0 1.29 4.97 7 13 0 5.52 3.72 -7 20 1 14.41 3.48 -13 20 1 12.64 6.50 -20 7 1 19.33 5.91 7 13 1 20.40 4.26 -13 20 2 3.96 6.46 -6 20 -1 13.68 3.37 -6 20 0 -2.28 2.96 -20 6 0 3.85 4.48 -14 20 0 2.17 6.90 6 14 0 2.59 3.49 -6 20 1 14.54 3.30 -20 6 1 13.80 4.89 6 14 1 16.09 4.10 -20 5 -1 2.58 3.40 -20 5 0 12.32 4.29 -5 20 0 18.72 3.45 5 15 0 20.29 3.89 -20 5 1 5.61 4.22 5 15 1 6.82 3.70 -4 20 0 83.96 6.20 4 16 0 81.48 6.36 -11 21 -1 18.95 4.79 -11 21 0 21.31 5.08 -11 21 1 15.31 4.77 -9 21 -1 8.63 4.79 -12 21 -1 12.55 5.22 -12 21 0 19.37 5.53 -9 21 0 18.19 4.39 -12 21 1 2.69 5.25 -8 21 0 16.60 4.03 8 13 0 8.72 3.71 -7 21 0 19.40 4.02 7 14 0 18.04 3.99 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 98572 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, 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 C1 C 0.3482(8) 0.1741(4) 0.6275(15) 0.016(2) Uani 1 2 d S T P H1A H 0.3632 0.1298 0.5499 0.03(3) Uiso 1 1 d R . . H1B H 0.2762 0.1381 0.6643 0.02(4) Uiso 1 2 d R . P Mn2 Mn 0.3333 0.6667 0.8499(4) 0.0107(6) Uani 1 6 d S T P Br2 Br 0.42712(4) 0.85424(8) 0.9636(2) 0.0144(2) Uani 1 2 d S T P Br1 Br 0.16637(7) 0.08319(4) 0.24846(12) 0.0088(2) Uani 1 2 d S T P Mn1 Mn 0.0000 0.0000 -0.0015(4) 0.0080(5) Uani 1 6 d S T P Br3 Br 0.3333 0.6667 0.4673(3) 0.0107(3) Uani 1 6 d S T P N1 N 0.4151(7) 0.2075(3) 0.8084(14) 0.0139(19) Uani 1 2 d S T P H1D H 0.4820 0.2410 0.7690 0.09(8) Uiso 1 2 d R . P C2 C 0.3990(6) 0.2837(6) 0.9305(11) 0.0151(17) Uani 1 1 d . . . H2A H 0.4423 0.3029 1.0471 0.04(3) Uiso 1 1 d R . . H2B H 0.4166 0.3446 0.8529 0.04(3) Uiso 1 1 d R . . H2C H 0.3274 0.2513 0.9702 0.02(2) Uiso 1 1 d 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 C1 0.006(5) 0.020(4) 0.017(6) -0.001(2) -0.002(4) 0.003(3) Mn2 0.0109(8) 0.0109(8) 0.0102(13) 0.000 0.000 0.0054(4) Br2 0.0142(4) 0.0105(5) 0.0171(5) -0.0025(5) -0.0013(3) 0.0052(2) Br1 0.0059(4) 0.0107(3) 0.0080(4) 0.0000(2) 0.0000(4) 0.0029(2) Mn1 0.0087(7) 0.0087(7) 0.0067(12) 0.000 0.000 0.0043(3) Br3 0.0109(5) 0.0109(5) 0.0104(7) 0.000 0.000 0.0054(2) N1 0.005(4) 0.014(3) 0.020(5) 0.0011(17) 0.002(3) 0.002(2) C2 0.012(3) 0.014(4) 0.018(5) -0.003(3) -0.001(3) 0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N1 C1 H1A 109.3 . . N1 C1 H1B 110.4 . . H1A C1 H1B 109.7 . . Br2 Mn2 Br2 111.33(7) 3_565 . Br2 Mn2 Br2 111.33(7) 3_565 2_665 Br2 Mn2 Br2 111.32(7) . 2_665 Br2 Mn2 Br3 107.55(7) 3_565 . Br2 Mn2 Br3 107.55(7) . . Br2 Mn2 Br3 107.55(7) 2_665 . Mn1 Br1 Mn1 76.18(2) . 4 Br1 Mn1 Br1 85.95(8) . 3 Br1 Mn1 Br1 85.95(8) . 2 Br1 Mn1 Br1 85.95(8) 3 2 Br1 Mn1 Br1 179.98(10) . 4_554 Br1 Mn1 Br1 94.059(18) 3 4_554 Br1 Mn1 Br1 94.061(18) 2 4_554 Br1 Mn1 Br1 94.060(18) . 6_554 Br1 Mn1 Br1 179.98(10) 3 6_554 Br1 Mn1 Br1 94.061(18) 2 6_554 Br1 Mn1 Br1 85.93(8) 4_554 6_554 Br1 Mn1 Br1 94.060(18) . 5_554 Br1 Mn1 Br1 94.061(18) 3 5_554 Br1 Mn1 Br1 179.98(10) 2 5_554 Br1 Mn1 Br1 85.93(8) 4_554 5_554 Br1 Mn1 Br1 85.93(8) 6_554 5_554 C1 N1 C2 111.3(5) . . C1 N1 C2 111.3(5) . 9 C2 N1 C2 111.9(8) . 9 C1 N1 H1D 108.3 . . C2 N1 H1D 106.9 . . C2 N1 H1D 106.9 9 . N1 C2 H2A 109.4 . . N1 C2 H2B 110.0 . . H2A C2 H2B 109.5 . . N1 C2 H2C 109.0 . . H2A C2 H2C 109.4 . . H2B C2 H2C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N1 1.470(13) . C1 H1A 0.9373 . C1 H1B 0.9483 . Mn2 Br2 2.5013(14) 3_565 Mn2 Br2 2.5014(14) . Mn2 Br2 2.5014(14) 2_665 Mn2 Br3 2.538(4) . Br1 Mn1 2.687(2) . Br1 Mn1 2.688(2) 4 Mn1 Br1 2.687(2) 3 Mn1 Br1 2.688(2) 2 Mn1 Br1 2.688(2) 4_554 Mn1 Br1 2.688(2) 6_554 Mn1 Br1 2.688(2) 5_554 N1 C2 1.492(9) . N1 C2 1.492(9) 9 N1 H1D 0.8898 . C2 H2A 0.9502 . C2 H2B 0.9494 . C2 H2C 0.9490 .