#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:46:10 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132588.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_4132588 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 14.9319(4) _cell_length_b 14.9319(4) _cell_length_c 6.7338(2) _cell_measurement_reflns_used 5153 _cell_measurement_temperature 373(2) _cell_measurement_theta_max 27.4700 _cell_measurement_theta_min 1.7529 _cell_volume 1300.23(6) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 373(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measurement_device_type 'Rigaku saturn 724' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.915 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 6442 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.909 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.379 _diffrn_reflns_theta_min 2.728 _exptl_absorpt_coefficient_mu 11.724 _exptl_absorpt_correction_T_max 0.076 _exptl_absorpt_correction_T_min 0.053 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 2.170 _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 0.994 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.103 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_extinction_coef 0.0271(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 45 _refine_ls_number_reflns 1292 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0347 _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^)+(0.0228P)^2^+1.0105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.0625 _reflns_Friedel_coverage 0.845 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.902 _reflns_number_gt 995 _reflns_number_total 1292 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05037_si_007.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 1300.23(8) _cod_database_code 4132588 _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 14.9319 14.9319 6.7338 90.000 90.000 120.000 ZERR 2.00 0.0004 0.0004 0.0002 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 100 WGHT 0.022800 1.010500 EXTI 0.027055 BASF -0.00836 FVAR 0.16030 C1 1 0.349127 0.174564 0.630306 10.50000 0.05991 0.10944 = 0.08859 -0.00776 -0.01553 0.02996 AFIX 3 H1A 2 0.364077 0.129810 0.552736 11.00000 -1.20000 H1B 2 0.277067 0.138534 0.667146 10.50000 -1.20000 AFIX 0 MN2 5 0.333333 0.666667 0.840429 10.16667 0.05658 0.05658 = 0.05335 0.00000 0.00000 0.02829 BR2 4 0.425250 0.850500 0.950801 10.50000 0.08046 0.06011 = 0.09051 -0.01306 -0.00653 0.03005 BR1 4 0.163460 0.081730 0.251872 10.50000 0.03771 0.05872 = 0.03510 -0.00013 -0.00027 0.01886 MN1 5 0.000000 0.000000 0.002115 10.16667 0.04442 0.04442 = 0.02712 0.00000 0.00000 0.02221 BR3 4 0.333333 0.666667 0.462009 10.16667 0.05786 0.05786 = 0.05242 0.00000 0.00000 0.02893 N1 3 0.414638 0.207319 0.809099 10.50000 0.04366 0.08334 = 0.07403 0.00061 0.00123 0.02183 AFIX 3 H1D 2 0.481538 0.240769 0.769739 10.50000 -1.20000 AFIX 0 C2 1 0.398040 0.280440 0.930130 11.00000 0.08377 0.10518 = 0.12322 -0.02489 0.01341 0.04452 AFIX 3 H2A 2 0.441340 0.299690 1.046767 11.00000 -1.20000 H2B 2 0.415610 0.341408 0.852588 11.00000 -1.20000 H2C 2 0.326440 0.248029 0.969839 11.00000 -1.20000 AFIX 0 HKLF 4 REM P63mc in P6(3)mc REM R1 = 0.0347 for 995 Fo > 4sig(Fo) and 0.0536 for all 1292 data REM 45 parameters refined using 0 restraints END WGHT 0.0304 0.0721 REM Highest difference peak 0.994, deepest hole -0.390, 1-sigma level 0.103 Q1 1 0.0000 0.0000 0.1375 10.16667 0.05 0.99 Q2 1 0.3333 0.6667 0.3181 10.16667 0.05 0.83 Q3 1 0.3333 0.6667 0.6118 10.16667 0.05 0.82 Q4 1 0.1652 0.0826 0.1233 10.50000 0.05 0.80 Q5 1 0.1625 0.0813 0.3777 10.50000 0.05 0.74 Q6 1 0.0000 0.0000 -0.1243 10.16667 0.05 0.63 Q7 1 0.4175 0.8351 1.1112 10.50000 0.05 0.51 Q8 1 0.3576 0.6424 0.5193 10.50000 0.05 0.50 Q9 1 0.5033 0.2516 1.1110 10.50000 0.05 0.46 Q10 1 0.4310 0.8620 0.8282 10.50000 0.05 0.45 Q11 1 0.3333 0.6667 0.7357 10.16667 0.05 0.44 Q12 1 0.3333 0.6667 1.0651 10.16667 0.05 0.39 Q13 1 0.0968 0.0484 0.1714 10.50000 0.05 0.35 Q14 1 0.3667 0.7334 0.6584 10.50000 0.05 0.35 Q15 1 0.3276 0.1638 0.8765 10.50000 0.05 0.35 Q16 1 0.3814 0.6186 0.2416 10.50000 0.05 0.32 Q17 1 0.4169 0.8338 1.2305 10.50000 0.05 0.32 Q18 1 0.4994 0.2497 0.3952 10.50000 0.05 0.31 Q19 1 0.4997 0.2499 1.2631 10.50000 0.05 0.31 Q20 1 0.4092 0.8184 0.6622 10.50000 0.05 0.31 ; _shelx_res_checksum 23499 _shelx_hkl_file ; 0 0 -6 109.80 3.57 0 0 -5 -0.17 0.75 0 0 -4 521.34 15.34 0 0 -3 -0.40 0.38 0 0 -2 417.81 12.22 0 0 -1 -0.11 0.10 0 0 1 0.09 0.08 0 0 2 434.82 12.84 0 0 2 447.91 12.84 0 0 3 0.58 0.26 0 0 3 0.70 0.27 0 0 4 519.80 15.18 0 0 5 0.10 0.47 0 0 6 123.84 3.81 0 0 7 -0.47 0.71 0 0 8 32.95 1.44 0 1 -6 41.20 1.74 1 -1 -6 42.58 1.76 -1 1 -6 42.85 1.73 1 0 -6 43.48 1.79 1 -1 -5 0.69 0.71 -1 1 -5 0.88 0.73 1 0 -5 0.62 0.70 0 1 -5 0.87 0.70 1 0 -4 243.85 7.01 1 -1 -4 232.59 6.99 0 1 -4 234.50 6.99 -1 1 -4 224.26 6.97 -1 1 -3 13.41 0.65 1 -1 -3 14.14 0.54 0 1 -3 15.58 0.68 1 0 -3 14.59 0.71 1 -1 -3 13.38 0.63 1 0 -3 13.58 0.57 1 0 -2 423.61 12.71 0 -1 -2 441.97 12.66 -1 1 -2 433.12 12.74 0 1 -2 458.20 12.75 1 -1 -2 425.77 12.69 1 -1 -2 430.99 12.69 0 1 -1 64.14 1.90 -1 1 -1 62.67 1.91 1 0 1 66.39 2.01 1 -1 1 67.88 2.02 0 -1 1 66.77 2.00 -1 0 1 65.34 2.00 -1 1 1 70.23 2.00 1 0 2 438.96 12.32 -1 0 2 411.85 12.36 1 0 2 394.45 12.40 0 -1 2 419.33 12.36 1 -1 2 404.65 12.41 0 1 2 429.62 12.33 -1 1 2 419.14 12.35 1 -1 3 11.12 0.62 1 -1 3 11.84 0.49 -1 1 3 12.15 0.48 1 0 3 11.57 0.46 -1 0 3 11.21 0.51 0 1 3 11.65 0.44 0 -1 3 11.03 0.51 0 -1 3 11.13 0.52 1 -1 4 222.79 6.60 0 -1 4 221.96 6.61 1 -1 4 225.87 6.60 -1 0 4 223.26 6.60 -1 1 4 222.47 6.59 1 0 4 222.06 6.57 0 1 4 223.74 6.57 1 0 4 223.79 6.57 0 -1 4 222.25 6.61 1 -1 5 0.50 0.51 0 1 5 0.12 0.42 1 0 5 0.58 0.46 1 -1 5 1.14 0.55 -1 1 5 0.37 0.49 -1 0 5 0.99 0.54 0 -1 5 0.30 0.52 -1 1 6 42.87 1.50 0 1 6 41.22 1.46 -1 0 6 41.79 1.54 1 -1 6 42.82 1.53 1 0 6 41.98 1.47 0 -1 6 39.77 1.54 1 -1 7 0.38 0.78 0 -1 7 -0.15 0.82 -1 1 7 1.42 0.76 -1 0 7 -0.80 0.79 1 0 7 -0.22 0.66 0 1 7 0.35 0.69 1 -1 8 41.13 1.70 -1 0 8 42.02 1.73 0 -1 8 44.91 1.78 -1 -1 -6 9.31 0.96 2 -1 -6 7.70 0.98 -1 2 -6 8.15 0.99 1 1 -6 7.83 1.01 -1 2 -5 -0.19 0.70 2 -1 -5 0.23 0.76 1 1 -5 0.44 0.76 2 -1 -4 146.98 4.44 -1 2 -4 153.50 4.54 1 1 -4 151.21 4.54 2 -1 -4 141.58 4.52 2 -1 -3 0.33 0.33 1 1 -3 0.27 0.35 1 -2 -3 0.05 0.21 -1 2 -3 -0.05 0.38 1 1 -3 0.32 0.42 2 -1 -3 0.28 0.32 2 -1 -2 135.87 4.06 -1 2 -2 133.88 4.08 1 -2 -2 138.10 4.01 1 1 -2 137.07 4.08 1 1 -1 0.23 0.12 -1 2 -1 0.47 0.21 -1 -1 -1 0.11 0.13 -1 -1 0 578.46 17.41 1 1 0 616.91 17.41 1 1 0 601.23 17.41 1 1 1 0.07 0.13 -1 -1 1 0.77 0.17 -1 -1 1 0.94 0.17 -2 1 1 1.43 0.19 2 -1 1 0.43 0.25 -1 -1 2 133.03 3.99 -1 -1 2 136.02 4.00 2 -1 2 136.04 4.05 -2 1 2 134.64 3.99 -1 2 3 0.32 0.24 1 -2 3 -0.10 0.34 -2 1 3 -0.01 0.28 2 -1 3 0.02 0.51 1 1 3 0.07 0.18 1 1 3 0.03 0.17 -1 -1 3 0.30 0.32 2 -1 4 157.12 4.87 2 -1 4 157.76 4.74 1 -2 4 160.93 4.77 -2 1 4 158.83 4.76 1 1 4 160.59 4.70 -1 2 4 156.70 4.72 -1 -1 4 162.15 4.78 2 -1 5 -0.05 0.49 2 -1 5 -0.02 0.47 -1 2 5 -0.03 0.44 -2 1 5 0.12 0.55 1 -2 5 -0.87 0.56 1 1 5 -0.15 0.38 -1 -1 5 1.35 0.59 1 -2 5 0.06 0.56 -1 -1 6 13.17 0.91 -2 1 6 12.44 0.84 1 1 6 12.45 0.67 1 -2 6 13.33 0.90 2 -1 6 13.18 0.81 -1 2 6 12.02 0.75 -2 1 7 -0.36 0.83 1 -2 7 0.75 0.86 -1 -1 7 0.24 0.88 2 -1 7 -0.64 0.75 1 1 7 0.09 0.59 -2 1 8 10.30 1.03 -1 -1 8 11.04 1.14 1 -2 8 10.96 1.09 2 0 -6 2.02 0.94 0 -2 -6 2.08 0.92 0 2 -6 0.83 0.92 -2 2 -6 1.65 0.88 0 -2 -5 52.47 1.87 0 2 -5 51.65 1.86 2 0 -5 50.39 1.89 2 -2 -5 48.54 1.86 -2 2 -5 51.69 1.86 0 2 -4 66.74 2.28 2 0 -4 69.67 2.22 2 0 -4 73.18 2.34 2 -2 -4 70.16 2.17 -2 2 -4 70.48 2.29 2 0 -3 90.90 2.59 2 -2 -3 89.65 2.64 2 0 -3 86.74 2.67 0 -2 -3 84.52 2.58 0 2 -3 82.33 2.70 2 -2 -3 88.01 2.64 -2 2 -3 87.33 2.72 2 -2 -2 16.55 0.60 0 2 -2 15.43 0.63 2 0 -2 16.46 0.62 -2 2 -2 17.60 0.68 0 2 -1 52.61 1.59 2 0 0 26.68 0.85 2 -2 1 50.93 1.58 0 -2 1 48.24 1.50 2 0 1 51.03 1.54 -2 0 1 49.46 1.51 0 -2 2 19.45 0.68 2 -2 2 20.13 0.76 -2 0 2 18.67 0.68 2 0 2 18.50 0.72 2 -2 3 94.49 2.85 0 -2 3 89.33 2.66 0 -2 3 91.62 2.75 0 2 3 88.42 2.66 2 0 3 87.53 2.83 2 0 3 94.47 2.67 -2 2 3 86.87 2.72 -2 0 3 87.77 2.74 -2 0 4 70.63 2.21 2 -2 4 70.60 2.18 0 -2 4 71.11 2.21 -2 2 4 68.45 2.17 0 2 4 66.21 2.10 2 -2 4 71.24 2.35 0 -2 4 70.13 2.21 2 0 4 72.26 2.13 2 0 5 47.44 1.57 -2 2 5 48.39 1.63 2 0 5 47.85 1.57 0 -2 5 49.32 1.70 -2 0 5 49.84 1.68 2 -2 5 51.09 1.67 0 2 5 48.04 1.54 2 0 6 0.89 0.51 2 -2 6 0.85 0.69 2 -2 6 1.48 0.67 0 -2 6 1.59 0.76 0 2 6 1.00 0.48 -2 2 6 1.25 0.62 -2 0 6 2.00 0.69 -2 0 7 2.39 0.89 2 0 7 3.86 0.66 0 -2 7 3.11 0.92 2 -2 7 2.49 0.85 -2 0 8 5.82 1.05 2 -2 8 6.44 1.06 0 -2 8 8.40 1.17 -2 -1 -6 12.90 1.04 1 -3 -6 12.47 1.05 2 1 -6 12.89 1.12 -1 -2 -6 12.80 1.00 3 -2 -6 13.19 1.10 1 2 -6 12.13 1.04 -1 3 -6 12.09 1.08 -2 3 -6 13.64 1.09 3 -1 -6 15.50 1.18 1 2 -5 17.00 0.97 -3 2 -5 13.53 0.95 -1 3 -5 15.53 0.97 1 -3 -5 18.08 0.99 -2 -1 -5 15.35 0.98 3 -2 -5 14.82 0.98 -2 3 -5 16.02 0.97 -1 -2 -5 16.61 0.94 2 1 -5 15.33 1.01 3 -2 -5 14.83 0.80 3 -1 -5 17.40 1.04 3 -1 -5 15.91 0.86 3 -2 -4 9.60 0.61 2 1 -4 10.51 0.68 2 -3 -4 10.92 0.50 1 -3 -4 9.73 0.42 3 -2 -4 9.77 0.61 -1 -2 -4 11.58 0.71 2 1 -4 10.69 0.78 -1 3 -4 10.04 0.73 3 -1 -4 11.04 0.65 -2 3 -4 11.46 0.75 -3 2 -4 10.54 0.75 1 2 -4 10.15 0.72 -2 -1 -4 10.65 0.71 1 -3 -4 10.44 0.76 3 -1 -4 10.70 0.44 -2 -1 -3 268.20 8.35 3 -1 -3 283.38 8.36 1 -3 -3 285.35 8.25 -1 -2 -3 264.11 8.27 2 1 -3 273.94 8.37 -2 3 -3 287.52 8.39 2 1 -3 289.66 8.36 3 -2 -3 285.63 8.34 -1 -2 -3 284.20 8.36 2 -3 -3 288.56 8.29 -1 3 -3 288.69 8.38 3 -1 -3 286.10 8.35 -3 2 -3 287.11 8.39 1 2 -3 282.11 8.37 1 -3 -3 289.75 8.25 2 1 -2 45.21 1.36 1 2 -2 42.63 1.40 3 -1 -2 43.77 1.43 3 -2 -2 42.65 1.42 -1 -2 -2 43.18 1.35 -3 2 -2 43.39 1.46 -2 3 -2 46.11 1.46 -2 -1 -2 41.54 1.39 -1 3 -2 43.38 1.43 -1 -2 -2 46.96 1.40 2 -3 -2 44.86 1.38 1 -3 -2 44.67 1.33 2 1 -1 181.05 5.43 -1 3 -1 187.14 5.45 -1 -2 -1 183.63 5.39 1 2 -1 181.98 5.42 -2 -1 -1 178.08 5.40 -1 -2 -1 181.07 5.41 -1 -2 -1 189.51 5.37 2 1 -1 187.05 5.41 1 2 -1 182.39 5.40 1 2 0 3.91 0.21 -1 -2 0 3.72 0.23 2 1 0 3.89 0.23 2 1 0 4.05 0.26 2 1 1 198.87 5.83 -2 -1 1 198.80 5.84 3 -1 1 195.29 5.93 1 2 1 199.94 5.79 2 1 1 196.08 5.81 -1 -2 1 200.24 5.84 -1 -2 1 199.27 5.83 2 1 2 36.35 1.24 3 -1 2 38.29 1.32 2 1 2 38.89 1.18 -1 -2 2 37.14 1.22 -3 1 2 38.01 1.23 -1 -2 2 37.64 1.22 3 -2 2 38.57 1.33 -1 -2 2 38.23 1.17 -2 -1 2 36.64 1.22 3 -2 3 306.31 8.79 -3 1 3 292.61 8.68 1 -3 3 295.51 8.68 -1 -2 3 302.61 8.68 -3 2 3 290.29 8.68 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3 4.36 1.42 12 -17 3 4.21 1.70 12 -17 4 -1.24 1.51 5 -17 4 1.37 0.86 17 -5 4 1.52 2.17 5 -17 5 4.95 1.21 17 -5 5 9.50 2.77 5 -17 5 7.46 1.08 4 -17 -5 -1.78 1.23 -4 -13 -3 4.08 1.38 13 4 -3 8.19 2.32 -4 -13 -3 5.38 0.92 4 -17 -2 15.51 1.02 -4 -13 -2 13.90 1.47 -4 -13 -2 16.23 1.13 13 4 -2 16.46 2.31 -4 -13 -1 4.35 1.01 -4 -13 -1 3.09 1.31 13 4 -1 5.34 1.91 -4 -13 0 2.39 1.06 -4 -13 0 -0.24 1.28 13 4 0 2.97 1.76 4 -17 0 2.62 0.54 -4 -13 1 4.40 1.11 -4 -13 1 4.36 1.31 13 4 1 6.27 1.69 4 -17 1 4.16 0.57 4 -17 2 15.85 0.84 -4 -13 2 12.97 1.46 13 4 2 16.04 1.68 17 -4 2 11.62 1.63 -4 -13 2 14.83 1.28 -4 -13 3 4.31 1.27 13 -17 3 4.35 2.01 17 -13 3 6.80 2.97 17 -4 3 5.91 1.99 -4 -13 3 4.25 1.32 4 -17 3 3.77 0.77 13 -17 4 0.86 1.68 4 -17 4 1.57 1.16 4 -17 4 0.15 0.80 17 -4 4 -1.78 2.35 17 -4 5 0.67 2.43 4 -17 5 2.24 1.17 3 -17 -4 1.07 1.13 -3 -14 -4 0.91 1.39 3 -17 -3 0.86 0.87 3 -17 -3 0.03 1.28 -3 -14 -3 0.27 1.30 -3 -14 -2 4.66 1.00 -3 -14 -2 3.41 1.34 14 3 -2 3.96 2.22 -3 -14 -1 2.12 0.99 3 -17 -1 2.41 0.46 -3 -14 -1 3.90 1.30 14 3 -1 4.90 2.18 -3 -14 0 4.62 1.09 -3 -14 0 3.01 1.27 14 3 0 6.08 2.02 3 -17 0 4.75 0.48 17 -3 1 1.31 1.17 -3 -14 1 2.95 1.13 3 -17 1 2.45 0.51 -3 -14 1 3.86 1.27 14 3 1 1.55 1.84 17 -3 2 3.55 1.55 -3 -14 2 2.90 1.19 -3 -14 2 4.28 1.39 14 3 2 4.73 1.70 -3 -14 3 0.56 1.32 17 -3 3 1.24 1.85 17 -14 3 -1.88 3.14 14 -17 3 -0.06 2.43 3 -17 3 0.82 1.22 -3 -14 3 0.56 1.33 3 -17 4 0.39 1.09 -3 -14 4 -0.64 1.40 17 -3 4 2.58 2.26 17 -3 5 2.81 2.66 3 -17 5 1.87 1.29 2 -17 -3 0.41 1.15 -2 -15 -3 0.22 1.30 -2 -15 -2 1.89 0.94 2 -17 -2 1.39 0.91 2 -17 -2 1.38 1.11 -2 -15 -2 1.57 1.33 15 2 -2 1.67 2.37 -2 -15 -1 1.80 1.02 2 -17 -1 1.82 0.89 2 -17 -1 -0.19 1.17 -2 -15 -1 2.36 1.29 15 2 -1 0.24 2.16 -2 -15 0 4.14 1.00 2 -17 0 4.20 0.98 2 -17 0 3.20 1.23 -2 -15 0 1.97 1.28 -2 -15 1 2.04 1.11 2 -17 1 1.06 1.14 2 -17 1 1.25 1.21 -2 -15 1 1.12 1.27 17 -2 1 1.89 1.23 -2 -15 2 1.19 1.19 2 -17 2 1.89 1.20 2 -17 2 1.28 1.12 -2 -15 2 0.53 1.27 17 -2 2 1.28 1.55 -2 -15 3 1.11 1.33 2 -17 3 2.90 1.24 2 -17 3 0.33 1.29 15 -17 3 4.81 3.21 -2 -15 3 -0.68 1.45 17 -2 3 1.25 1.86 2 -17 4 -0.08 1.20 17 -2 4 2.24 2.32 -2 -15 4 1.04 1.37 -1 -16 -2 5.56 1.04 1 -17 -2 6.98 1.05 1 -17 -2 3.34 1.30 -1 -16 -2 5.49 1.39 16 1 -2 7.20 2.51 -1 -16 -1 3.58 1.06 1 -17 -1 3.24 1.00 1 -17 -1 2.01 1.20 -1 -16 -1 0.78 1.30 -1 -16 0 1.28 1.02 1 -17 0 -0.32 1.03 1 -17 0 0.82 1.19 -1 -16 0 0.58 1.29 -1 -16 1 2.31 1.16 1 -17 1 4.36 1.21 17 -1 1 2.13 1.36 1 -17 1 3.08 1.22 -1 -16 1 2.94 1.33 -1 -16 2 4.55 1.25 1 -17 2 5.08 1.24 1 -17 2 5.42 1.35 -1 -16 2 3.69 1.38 0 -17 -2 1.02 1.03 0 -17 -1 5.95 1.09 0 -17 0 0.24 1.06 0 -17 1 4.77 1.27 0 -17 2 3.65 1.27 -9 -9 0 6.76 1.13 -9 -9 1 -0.13 1.16 9 -18 1 -0.10 1.04 -9 -9 2 0.90 1.24 9 -18 2 0.04 0.93 9 -18 3 -0.90 1.01 18 -9 3 1.02 2.27 -9 -9 3 2.04 1.23 9 -18 4 1.61 1.04 9 -18 5 1.21 1.21 10 8 -2 1.03 1.77 10 8 -1 -0.43 1.72 -8 -10 -1 0.69 1.10 10 8 0 9.31 1.61 -10 -8 0 8.02 1.18 -8 -10 0 6.74 1.10 8 -18 1 1.41 0.81 10 8 1 0.95 1.58 -10 -8 1 2.43 1.26 -8 -10 1 1.03 1.20 18 -8 2 0.46 1.69 10 -18 2 2.13 1.18 8 -18 2 1.48 0.87 -10 -8 2 -0.06 1.21 -8 -10 2 -0.03 1.24 18 -8 3 -1.67 2.01 10 -18 3 1.26 1.08 18 -10 3 -0.31 2.31 8 -18 3 2.75 0.93 -10 -8 3 1.02 1.28 -8 -10 3 1.45 1.35 8 -18 4 2.58 0.89 10 -18 4 2.16 1.18 8 -18 5 0.70 1.07 10 -18 5 1.48 1.17 11 7 -3 1.02 2.13 11 7 -2 -0.05 1.91 11 7 -1 3.66 1.74 -7 -11 -1 3.83 1.04 11 7 0 0.52 1.64 -7 -11 0 0.18 1.11 7 -18 1 3.87 0.76 11 7 1 3.51 1.50 -11 -7 1 3.44 1.28 -7 -11 1 4.85 1.15 7 -18 2 0.95 0.72 18 -7 2 0.20 1.56 11 -18 2 -0.28 1.58 11 7 2 2.62 1.43 -11 -7 2 -0.92 1.34 -7 -11 2 0.03 1.26 18 -7 3 -0.49 1.82 11 -18 3 3.70 1.39 7 -18 3 1.86 0.83 18 -11 3 6.20 2.72 -11 -7 3 4.36 1.35 -7 -11 3 3.18 1.32 18 -7 4 -0.66 2.10 7 -18 4 -0.74 0.92 11 -18 4 0.27 1.22 7 -18 5 2.97 1.08 12 6 -3 4.19 2.12 12 6 -2 1.97 1.92 -6 -12 -2 4.05 0.99 12 6 -1 2.49 1.87 -6 -12 -1 0.88 1.05 12 6 0 1.11 1.83 6 -18 0 0.56 0.64 -6 -12 0 2.13 1.11 -6 -12 1 1.13 1.12 6 -18 1 1.16 0.66 12 6 1 1.32 1.54 -6 -12 2 4.12 1.22 12 -18 2 7.34 2.14 18 -6 2 3.55 1.55 12 6 2 2.86 1.39 6 -18 2 3.82 0.74 -6 -12 3 2.28 1.31 6 -18 3 1.49 0.76 12 -18 3 2.74 1.56 18 -6 3 1.58 1.76 -12 -6 3 2.16 1.41 18 -12 3 -0.73 2.85 6 -18 4 -0.45 0.90 12 -18 4 -1.39 1.48 18 -6 4 -0.70 2.24 13 5 -2 4.06 2.13 -5 -13 -2 2.44 0.95 -5 -13 -1 1.56 1.33 13 5 -1 0.51 1.94 -5 -13 -1 4.10 1.06 -5 -13 0 0.91 1.08 5 -18 0 1.08 0.59 -5 -13 0 0.09 1.30 13 5 0 1.84 1.82 -5 -13 1 4.88 1.17 -5 -13 1 0.91 1.31 13 5 1 2.11 1.69 5 -18 1 1.47 0.60 -5 -13 2 2.88 1.28 5 -18 2 3.20 0.67 13 5 2 2.45 1.54 18 -5 2 0.76 1.47 -5 -13 3 1.64 1.32 18 -5 3 2.32 1.87 13 -18 3 1.07 1.92 18 -5 4 3.56 1.97 -4 -14 -2 2.06 1.40 14 4 -2 -0.06 2.38 -4 -14 -2 0.61 1.00 -4 -14 -1 0.21 1.07 -4 -14 -1 3.43 1.35 14 4 -1 3.54 2.15 -4 -14 0 1.85 1.15 -4 -14 0 1.77 1.27 14 4 0 4.22 1.86 -4 -14 1 -0.68 1.18 -4 -14 1 1.59 1.34 14 4 1 0.54 1.81 -4 -14 2 1.16 1.27 18 -4 2 1.16 1.43 -4 -14 2 1.53 1.39 14 4 2 0.64 1.73 14 -18 2 4.26 6.56 14 -18 3 0.82 2.68 18 -4 3 -0.54 1.76 18 -4 4 2.78 2.04 3 -18 -2 4.24 0.97 -3 -15 -2 5.94 1.09 -3 -15 -1 -0.02 1.03 3 -18 -1 0.88 1.00 3 -18 -1 0.62 1.17 -3 -15 -1 0.49 1.42 15 3 -1 -0.85 2.20 -3 -15 0 9.73 1.23 -3 -15 0 8.12 1.47 15 3 0 9.73 2.20 -3 -15 1 0.53 1.15 18 -3 1 0.35 1.16 3 -18 1 -0.43 1.28 -3 -15 1 -1.75 1.41 15 3 1 0.75 2.05 -3 -15 2 5.88 1.24 15 3 2 6.06 1.79 18 -3 3 1.15 1.90 2 -18 -2 1.17 0.99 -2 -16 -1 3.38 1.10 2 -18 -1 0.26 1.02 16 2 -1 -0.45 2.36 -2 -16 0 -0.02 1.13 2 -18 0 -0.53 1.15 16 2 0 1.57 2.39 -2 -16 1 1.73 1.20 2 -18 1 0.39 1.21 16 2 1 0.26 2.16 -2 -16 2 -1.03 1.27 16 2 2 -0.91 1.96 -1 -17 -1 0.84 1.06 1 -18 -1 2.17 1.06 -1 -17 0 1.02 1.16 1 -18 0 1.44 1.02 -1 -17 1 2.36 1.21 1 -18 1 3.55 1.14 0 -18 -1 0.93 1.12 0 -18 0 1.13 1.21 -10 -9 0 1.42 1.25 -9 -10 0 0.47 1.16 9 -19 1 1.64 1.04 10 -19 1 2.25 1.38 -10 -9 1 1.17 1.30 -9 -10 1 0.94 1.18 9 -19 2 -0.28 0.95 19 -9 2 -0.69 2.08 19 -10 2 1.06 2.57 -10 -9 2 0.51 1.30 -9 -10 2 1.77 1.23 10 -19 2 1.03 1.10 10 -19 3 1.39 1.06 9 -19 3 1.94 0.87 9 -19 4 -0.70 0.94 10 -19 4 -0.56 1.09 11 8 -2 2.52 2.06 11 8 -1 3.80 1.81 -8 -11 -1 3.42 1.14 11 8 0 -0.22 1.80 -8 -11 0 -0.48 1.18 8 -19 1 3.16 0.83 -11 -8 1 4.12 1.37 11 8 1 2.48 1.79 -8 -11 1 1.74 1.21 8 -19 2 2.52 0.81 11 -19 2 2.74 1.39 19 -8 2 1.09 1.76 -11 -8 2 0.76 1.42 -8 -11 2 2.63 1.27 19 -8 3 3.34 1.85 11 -19 3 1.29 1.19 8 -19 3 0.30 0.86 8 -19 4 -1.04 0.92 11 -19 4 1.11 1.24 12 7 -2 4.95 2.12 12 7 -1 1.82 1.91 -7 -12 -1 2.42 1.11 -7 -12 0 -0.29 1.22 7 -19 0 0.35 0.74 7 -19 1 1.66 0.76 12 7 1 2.53 1.69 -7 -12 1 0.93 1.23 12 -19 2 4.19 2.04 19 -7 2 4.07 1.59 7 -19 2 3.46 0.75 -7 -12 2 3.71 1.28 7 -19 3 0.69 0.78 12 -19 3 0.91 1.60 19 -7 3 -0.22 1.77 13 6 -2 1.44 2.14 -6 -13 -2 0.67 1.07 13 6 -1 -0.59 2.02 -6 -13 -1 1.62 1.10 13 6 0 -0.73 1.88 -6 -13 0 0.50 1.18 -6 -13 1 1.20 1.27 13 6 1 3.50 1.86 -6 -13 2 1.20 1.37 13 -19 2 5.72 3.39 19 -6 2 1.78 1.44 19 -6 3 -1.67 1.68 13 -19 3 2.06 2.09 14 5 -1 0.06 2.17 -5 -14 -1 0.59 1.09 -5 -14 0 8.17 1.27 14 5 0 9.76 2.07 -5 -14 1 0.38 1.26 14 5 1 0.59 1.72 -5 -14 2 3.23 1.29 19 -5 2 -0.47 1.36 19 -5 3 1.60 1.66 4 -19 -2 1.76 0.97 15 4 -1 -2.07 2.36 -4 -15 -1 -1.03 1.17 -4 -15 0 0.64 1.17 15 4 0 -0.44 2.31 -4 -15 1 0.38 1.29 19 -4 1 0.11 1.20 15 4 1 -1.66 1.97 19 -4 2 1.84 1.40 19 -4 3 2.37 1.60 -3 -16 -1 0.65 1.18 3 -19 -1 -0.86 1.11 -3 -16 0 2.04 1.19 3 -19 0 2.56 1.22 16 3 0 2.25 2.26 -3 -16 1 0.72 1.16 3 -19 1 0.41 1.20 16 3 1 2.01 2.07 -2 -17 -1 0.76 1.21 2 -19 -1 -0.64 1.08 -2 -17 0 3.43 1.24 2 -19 0 4.84 1.15 17 2 1 1.46 2.21 1 -19 -1 -1.33 1.15 -1 -18 0 0.81 1.21 1 -19 0 0.81 1.11 -10 -10 0 -0.13 1.26 -10 -10 1 0.14 1.36 10 -20 1 0.10 1.24 10 -20 2 4.96 1.11 10 -20 3 -0.48 0.99 10 -20 4 0.11 1.04 -9 -11 0 1.55 1.27 11 -20 1 -0.34 2.13 9 -20 1 1.38 0.97 -11 -9 1 1.57 1.46 -9 -11 1 0.99 1.26 9 -20 2 2.85 0.87 11 -20 2 3.21 1.31 11 -20 3 -0.10 1.20 9 -20 3 0.97 0.88 12 8 -1 2.89 2.09 -8 -12 -1 5.69 1.30 12 8 0 1.90 1.84 -8 -12 0 1.09 1.25 8 -20 0 2.33 0.92 12 -20 1 13.00 5.23 -8 -12 1 3.93 1.29 12 -20 2 3.46 1.83 12 -20 3 2.71 1.36 13 7 -1 1.19 2.13 -7 -13 -1 2.96 1.20 13 7 0 -2.06 2.11 -7 -13 0 1.61 1.16 13 7 1 0.70 1.71 -7 -13 1 2.17 1.25 13 -20 2 6.64 3.30 20 -7 2 0.97 1.64 -6 -14 -1 1.80 1.17 14 6 0 1.42 2.20 -6 -14 0 -0.96 1.31 14 6 1 2.24 2.02 -6 -14 1 2.33 1.26 20 -6 2 -0.09 1.49 -5 -15 -1 1.15 1.23 15 5 0 0.67 2.25 -5 -15 0 3.13 1.24 -5 -15 1 0.44 1.26 20 -5 1 1.57 1.30 15 5 1 1.35 2.16 20 -5 2 -0.99 1.44 4 -20 -1 -1.01 1.11 -4 -16 0 9.83 1.40 4 -20 0 8.69 1.38 16 4 1 2.11 2.15 3 -20 -1 1.11 1.16 -3 -17 0 2.35 1.25 10 -21 0 3.58 1.77 -10 -11 0 1.06 1.44 11 -21 1 2.64 1.71 11 -21 2 1.97 1.25 -9 -12 0 0.05 1.35 12 -21 1 6.44 3.32 12 -21 2 4.68 1.69 -8 -13 -1 -0.05 1.29 -8 -13 0 -0.54 1.34 13 -21 1 480.08 137.45 -7 -14 0 -1.28 1.27 -6 -15 0 2.14 1.26 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 87694 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 0.3491(8) 0.1746(4) 0.6303(15) 0.091(4) Uani 1 2 d S T P H1A H 0.3641 0.1298 0.5527 0.110 Uiso 1 1 d R U . H1B H 0.2771 0.1385 0.6671 0.110 Uiso 1 2 d R U P Mn2 Mn 0.3333 0.6667 0.8404(4) 0.0555(6) Uani 1 6 d S T P Br2 Br 0.42525(4) 0.85050(8) 0.95080(17) 0.0793(4) Uani 1 2 d S T P Br1 Br 0.16346(5) 0.08173(3) 0.25187(10) 0.0462(2) Uani 1 2 d S T P Mn1 Mn 0.0000 0.0000 0.0021(3) 0.0387(4) Uani 1 6 d S T P Br3 Br 0.3333 0.6667 0.4620(2) 0.0560(4) Uani 1 6 d S T P N1 N 0.4146(6) 0.2073(3) 0.8091(12) 0.071(2) Uani 1 2 d S T P H1D H 0.4815 0.2408 0.7697 0.086 Uiso 1 2 d R U P C2 C 0.3980(7) 0.2804(7) 0.9301(15) 0.105(3) Uani 1 1 d . . . H2A H 0.4413 0.2997 1.0468 0.126 Uiso 1 1 d R U . H2B H 0.4156 0.3414 0.8526 0.126 Uiso 1 1 d R U . H2C H 0.3264 0.2480 0.9698 0.126 Uiso 1 1 d 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 C1 0.060(6) 0.109(7) 0.089(8) -0.008(3) -0.016(6) 0.030(3) Mn2 0.0566(8) 0.0566(8) 0.0533(12) 0.000 0.000 0.0283(4) Br2 0.0805(5) 0.0601(6) 0.0905(8) -0.0131(6) -0.0065(3) 0.0301(3) Br1 0.0377(4) 0.0587(4) 0.0351(3) -0.00013(19) -0.0003(4) 0.01886(18) Mn1 0.0444(6) 0.0444(6) 0.0271(7) 0.000 0.000 0.0222(3) Br3 0.0579(5) 0.0579(5) 0.0524(7) 0.000 0.000 0.0289(3) N1 0.044(4) 0.083(4) 0.074(5) 0.0006(17) 0.001(3) 0.0218(19) C2 0.084(5) 0.105(6) 0.123(7) -0.025(6) 0.013(6) 0.045(5) 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 109.2 . . N1 C1 H1B 110.2 . . H1A C1 H1B 109.6 . . Br2 Mn2 Br2 111.50(6) 3_565 . Br2 Mn2 Br2 111.50(6) 3_565 2_665 Br2 Mn2 Br2 111.50(6) . 2_665 Br2 Mn2 Br3 107.36(6) 3_565 . Br2 Mn2 Br3 107.36(6) . . Br2 Mn2 Br3 107.36(6) 2_665 . Mn1 Br1 Mn1 77.069(18) . 4 Br1 Mn1 Br1 85.33(5) 2 3 Br1 Mn1 Br1 85.33(5) 2 . Br1 Mn1 Br1 85.33(5) 3 . Br1 Mn1 Br1 94.713(13) 2 4_554 Br1 Mn1 Br1 94.713(13) 3 4_554 Br1 Mn1 Br1 179.95(7) . 4_554 Br1 Mn1 Br1 179.95(7) 2 5_554 Br1 Mn1 Br1 94.713(13) 3 5_554 Br1 Mn1 Br1 94.714(13) . 5_554 Br1 Mn1 Br1 85.25(5) 4_554 5_554 Br1 Mn1 Br1 94.713(13) 2 6_554 Br1 Mn1 Br1 179.95(7) 3 6_554 Br1 Mn1 Br1 94.713(13) . 6_554 Br1 Mn1 Br1 85.25(5) 4_554 6_554 Br1 Mn1 Br1 85.25(5) 5_554 6_554 C1 N1 C2 111.5(5) . . C1 N1 C2 111.5(6) . 9 C2 N1 C2 110.5(9) . 9 C1 N1 H1D 108.1 . . C2 N1 H1D 107.5 . . C2 N1 H1D 107.5 9 . N1 C2 H2A 109.5 . . N1 C2 H2B 109.3 . . H2A C2 H2B 109.5 . . N1 C2 H2C 109.6 . . H2A C2 H2C 109.5 . . 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 1.472(11) . C1 H1A 0.9583 . C1 H1B 0.9643 . Mn2 Br2 2.4906(12) 3_565 Mn2 Br2 2.4907(12) . Mn2 Br2 2.4907(12) 2_665 Mn2 Br3 2.548(3) . Br1 Mn1 2.7012(14) . Br1 Mn1 2.7032(13) 4 Mn1 Br1 2.7012(14) 2 Mn1 Br1 2.7012(14) 3 Mn1 Br1 2.7033(13) 4_554 Mn1 Br1 2.7033(13) 5_554 Mn1 Br1 2.7033(13) 6_554 N1 C2 1.479(8) . N1 C2 1.479(8) 9 N1 H1D 0.9048 . C2 H2A 0.9652 . C2 H2B 0.9651 . C2 H2C 0.9651 .