#------------------------------------------------------------------------------ #$Date: 2026-06-28 00:02:23 +0100 (Sun, 28 Jun 2026) $ #$Revision: 306671 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721173.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_7721173 loop_ _publ_author_name 'Yu, Kaijian' 'Ye, Qiong' 'Wu, Yuechuan' 'Yang, Yawen' _publ_section_title ; Halogen Substitution of Aromatic Cations for Phase Transition Control and High-Efficiency Luminescence in 0D Manganese-Based Hybrid Perovskites ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT01114D _journal_year 2026 _chemical_formula_moiety 'Br4 Mn, 2(C10 H14 Cl F P)' _chemical_formula_sum 'C20 H28 Br4 Cl2 F2 Mn P2' _chemical_formula_weight 813.84 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2026-05-11 _audit_creation_method ; Olex2 1.5 (compiled 2026.04.10 svn.r48fbca5a for OlexSys, GUI svn.r7537) ; _audit_update_record ; 2026-05-11 deposited with the CCDC. 2026-06-19 downloaded from the CCDC. ; _cell_angle_alpha 99.426(5) _cell_angle_beta 90.233(7) _cell_angle_gamma 93.680(6) _cell_formula_units_Z 2 _cell_length_a 9.4186(8) _cell_length_b 10.5532(6) _cell_length_c 15.3860(12) _cell_measurement_reflns_used 4542 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.7980 _cell_measurement_theta_min 2.0010 _cell_volume 1505.4(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.988 _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 -74.00 63.00 0.50 2.50 -- 20.00 54.00 -90.00 274 2 \w 73.00 106.00 0.50 2.50 -- 20.00 54.00 -90.00 66 3 \w -73.00 83.00 0.50 2.50 -- 20.00 54.00 120.00 312 4 \w -63.00 -38.00 0.50 2.50 -- 20.00 54.00-120.00 50 5 \w -10.00 33.00 0.50 2.50 -- 20.00 54.00-120.00 86 6 \w 85.00 110.00 0.50 2.50 -- 20.00 54.00-120.00 50 7 \w -70.00 -28.00 0.50 2.50 -- 20.00 54.00 -30.00 84 8 \w -20.00 55.00 0.50 2.50 -- 20.00 54.00 -30.00 150 9 \w 67.00 98.00 0.50 2.50 -- 20.00 54.00 -30.00 62 10 \w -74.00 -25.00 0.50 2.50 -- 20.00 54.00 60.00 98 11 \w 70.00 107.00 0.50 2.50 -- 20.00 54.00 60.00 74 12 \w -62.00 68.00 0.50 2.50 -- 20.00 54.00-150.00 260 13 \w -67.00 -41.00 0.50 2.50 -- 20.00 54.00 0.00 52 14 \w -66.00 9.00 0.50 2.50 -- 20.00 54.00 90.00 150 15 \w 35.00 60.00 0.50 2.50 -- 20.00 54.00 90.00 50 16 \w 75.00 100.00 0.50 2.50 -- 20.00 54.00 90.00 50 17 \w -66.00 -40.00 0.50 2.50 -- 20.00 54.00 -60.00 52 18 \w -70.00 59.00 0.50 2.50 -- 20.00 54.00-180.00 258 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0198520000 _diffrn_orient_matrix_UB_12 0.0160611000 _diffrn_orient_matrix_UB_13 -0.0414688000 _diffrn_orient_matrix_UB_21 0.0172966000 _diffrn_orient_matrix_UB_22 0.0645281000 _diffrn_orient_matrix_UB_23 0.0202346000 _diffrn_orient_matrix_UB_31 0.0707303000 _diffrn_orient_matrix_UB_32 -0.0154985000 _diffrn_orient_matrix_UB_33 0.0074292000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_unetI/netI 0.0749 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 22555 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.167 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.051 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.36289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.795 _exptl_crystal_description plate _exptl_crystal_F_000 790 _refine_diff_density_max 0.432 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.107 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 6081 _refine_ls_number_restraints 91 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0574 _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^)+(0.0317P)^2^+0.9077P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.0953 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4086 _reflns_number_total 6081 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt01114d2.cif _cod_data_source_block pm-10-mnbr _cod_database_code 7721173 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H P F Br Mn Cl' _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C2-C1 = C6-C1 = C6-C5 = C5-C4 = C4-C3 = C3-C2 = C12-C11 = C16-C11 = C16-C15 = C15-C14 = C14-C13 = C13-C12 1.395 with sigma of 0.01 F1-C5 1.36 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(C3) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4.a Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C7(H7A,H7B) 4.b Aromatic/amide H refined with riding coordinates: C16(H16), C13(H13), C14(H14), C3(H3) 4.c Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B, H20C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C) ; _shelx_res_file ; TITL pm-10-mnbr_a.res in P-1 pm-10-mnbr.res created by SHELXL-2018/3 at 16:57:19 on 11-May-2026 REM Old TITL pm-10-mnbr in P-1 REM SHELXT solution in P-1: R1 0.183, Rweak 0.063, Alpha 0.066 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C21 F P2 Cl2 Br5 CELL 0.71073 9.4186 10.5532 15.386 99.426 90.233 93.68 ZERR 2 0.0008 0.0006 0.0012 0.005 0.007 0.006 LATT 1 SFAC C H Br Cl F Mn P UNIT 40 56 8 4 4 2 4 DFIX 1.395 0.01 C2 C1 C6 C1 C6 C5 C5 C4 C4 C3 C3 C2 C12 C11 C16 C11 C16 C15 = C15 C14 C14 C13 C13 C12 DFIX 1.36 0.01 F1 C5 ISOR 0.01 0.02 C3 P1 C9 C10 C7 C8 C1 C6 C2 C5 Cl1 F1 C4 L.S. 11 0 0 PLAN 16 CONF list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 999 0.8 OMIT -1 0 1 OMIT 0 -1 1 OMIT 0 1 0 REM REM REM WGHT 0.031700 0.907700 FVAR 0.43491 BR2 3 0.970793 0.524305 0.804845 11.00000 0.04006 0.04072 = 0.05281 0.01164 -0.00300 0.00669 BR1 3 0.669721 0.632650 0.652826 11.00000 0.04280 0.07571 = 0.04090 0.00600 -0.00959 0.00459 BR4 3 0.958867 0.906260 0.794142 11.00000 0.04766 0.03620 = 0.07414 0.00473 0.00522 -0.00005 BR3 3 0.649641 0.720877 0.928001 11.00000 0.05209 0.05782 = 0.05264 0.01140 0.01649 0.01044 MN1 6 0.804116 0.702711 0.796878 11.00000 0.03363 0.03796 = 0.03616 0.00557 -0.00172 0.00258 P2 7 0.796008 0.241080 0.952811 11.00000 0.03149 0.04484 = 0.03234 0.00492 -0.00093 0.00152 P1 7 0.759131 0.353846 0.393440 11.00000 0.03834 0.03429 = 0.03386 0.00516 0.00061 0.00092 CL2 4 0.523501 -0.023274 0.824701 11.00000 0.06494 0.03779 = 0.10741 0.01356 -0.02060 -0.01133 CL1 4 0.859612 0.272997 0.627124 11.00000 0.13859 0.09061 = 0.04237 0.01413 -0.01663 -0.01605 F2 5 0.358187 0.490713 0.798221 11.00000 0.10038 0.07299 = 0.06718 0.01121 -0.00901 0.04648 C11 1 0.580700 0.232208 0.825322 11.00000 0.02750 0.03519 = 0.02997 0.00405 0.00096 0.00089 F1 5 0.607398 -0.183068 0.399667 11.00000 0.17998 0.05422 = 0.09263 -0.00068 0.03614 -0.03127 C17 1 0.736752 0.213704 0.839295 11.00000 0.03863 0.02795 = 0.03175 0.00339 -0.00062 -0.00494 AFIX 23 H17A 2 0.792738 0.271691 0.808036 11.00000 -1.20000 H17B 2 0.755686 0.126473 0.813218 11.00000 -1.20000 AFIX 0 C12 1 0.476082 0.131765 0.819190 11.00000 0.03824 0.03964 = 0.04058 0.00625 -0.00829 -0.00241 C9 1 0.716452 0.271698 0.285016 11.00000 0.04578 0.04181 = 0.04103 -0.00401 -0.00317 -0.00008 AFIX 137 H9A 2 0.770601 0.311918 0.243061 11.00000 -1.50000 H9B 2 0.616742 0.275485 0.273346 11.00000 -1.50000 H9C 2 0.739010 0.183413 0.280201 11.00000 -1.50000 AFIX 0 C1 1 0.694158 0.154150 0.488140 11.00000 0.05138 0.04274 = 0.04240 0.00964 0.01592 0.00419 C15 1 0.395073 0.369404 0.805554 11.00000 0.07208 0.05032 = 0.03244 0.00591 0.00085 0.03079 C16 1 0.537752 0.353910 0.818013 11.00000 0.05200 0.04298 = 0.03382 0.00578 -0.00472 0.00684 AFIX 43 H16 2 0.604206 0.423711 0.821474 11.00000 -1.20000 AFIX 0 C6 1 0.636762 0.043406 0.434324 11.00000 0.06503 0.05286 = 0.05121 0.01646 0.01230 -0.00261 C10 1 0.722851 0.519039 0.402943 11.00000 0.08141 0.03317 = 0.04817 0.00144 -0.00706 0.00019 AFIX 137 H10A 2 0.783267 0.559616 0.364006 11.00000 -1.50000 H10B 2 0.740661 0.561074 0.462536 11.00000 -1.50000 H10C 2 0.625064 0.525489 0.387410 11.00000 -1.50000 AFIX 0 C7 1 0.651137 0.285473 0.473083 11.00000 0.04377 0.04775 = 0.05259 0.01711 0.00980 0.00961 AFIX 23 H7A 2 0.657502 0.344102 0.528736 11.00000 -1.20000 H7B 2 0.552611 0.277553 0.453220 11.00000 -1.20000 AFIX 0 C2 1 0.786192 0.138602 0.555511 11.00000 0.07899 0.05377 = 0.03961 0.01516 0.00342 0.00400 C13 1 0.332366 0.148904 0.806436 11.00000 0.04459 0.06200 = 0.06031 0.01502 -0.00487 -0.00815 AFIX 43 H13 2 0.265038 0.079681 0.802347 11.00000 -1.20000 AFIX 0 C14 1 0.291923 0.270139 0.800006 11.00000 0.03745 0.09179 = 0.04500 0.01282 -0.00017 0.00970 AFIX 43 H14 2 0.196714 0.284554 0.792067 11.00000 -1.20000 AFIX 0 C19 1 0.985137 0.240914 0.952752 11.00000 0.03160 0.08694 = 0.06115 0.00704 -0.00672 0.00833 AFIX 137 H19A 2 1.012958 0.159510 0.922563 11.00000 -1.50000 H19B 2 1.020540 0.254604 1.012378 11.00000 -1.50000 H19C 2 1.023831 0.308536 0.923285 11.00000 -1.50000 AFIX 0 C20 1 0.744905 0.394084 1.006201 11.00000 0.05880 0.05019 = 0.04508 -0.01111 -0.00289 0.00990 AFIX 137 H20A 2 0.770640 0.458143 0.970380 11.00000 -1.50000 H20B 2 0.792705 0.416191 1.062381 11.00000 -1.50000 H20C 2 0.643867 0.390258 1.014572 11.00000 -1.50000 AFIX 0 C8 1 0.943715 0.340922 0.415185 11.00000 0.04274 0.07837 = 0.05156 0.01562 -0.00191 0.00024 AFIX 137 H8A 2 0.965969 0.252479 0.400941 11.00000 -1.50000 H8B 2 0.964447 0.371790 0.476416 11.00000 -1.50000 H8C 2 0.999886 0.391554 0.379880 11.00000 -1.50000 AFIX 0 C5 1 0.670156 -0.076850 0.451647 11.00000 0.09217 0.04451 = 0.06882 0.00440 0.02857 -0.00872 C18 1 0.725462 0.117701 1.010131 11.00000 0.07501 0.06171 = 0.05594 0.02649 -0.00084 -0.00244 AFIX 137 H18A 2 0.624516 0.123291 1.015943 11.00000 -1.50000 H18B 2 0.769160 0.128413 1.067572 11.00000 -1.50000 H18C 2 0.744758 0.035025 0.977714 11.00000 -1.50000 AFIX 0 C3 1 0.818527 0.017477 0.572187 11.00000 0.09893 0.07895 = 0.07822 0.03928 -0.00549 0.01515 AFIX 43 H3 2 0.879219 0.010326 0.618718 11.00000 -1.20000 AFIX 0 C4 1 0.760193 -0.090711 0.519507 11.00000 0.10510 0.06425 = 0.08708 0.03263 0.01449 0.01550 H4 2 0.781778 -0.179869 0.525984 11.00000 0.10437 H6 2 0.572807 0.047636 0.389539 11.00000 0.04521 HKLF 4 REM pm-10-mnbr_a.res in P-1 REM wR2 = 0.0953, GooF = S = 1.058, Restrained GooF = 1.061 for all data REM R1 = 0.0574 for 4086 Fo > 4sig(Fo) and 0.1020 for all 6081 data REM 294 parameters refined using 91 restraints END WGHT 0.0316 0.8971 REM Highest difference peak 0.432, deepest hole -0.710, 1-sigma level 0.107 Q1 1 0.5986 0.7191 0.8836 11.00000 0.05 0.43 Q2 1 0.5810 0.0025 0.7681 11.00000 0.05 0.39 Q3 1 0.7351 0.0641 1.1350 11.00000 0.05 0.39 Q4 1 0.8060 -0.1906 0.3799 11.00000 0.05 0.37 Q5 1 0.9810 0.5771 0.7164 11.00000 0.05 0.37 Q6 1 0.7255 0.3518 1.0609 11.00000 0.05 0.37 Q7 1 0.8596 0.0620 0.6625 11.00000 0.05 0.36 Q8 1 0.5783 0.6681 0.7039 11.00000 0.05 0.36 Q9 1 0.4628 0.3039 0.9221 11.00000 0.05 0.36 Q10 1 0.7778 0.3045 0.7074 11.00000 0.05 0.35 Q11 1 0.7793 0.4452 1.1362 11.00000 0.05 0.34 Q12 1 1.0864 0.4649 0.7375 11.00000 0.05 0.34 Q13 1 0.2036 0.5114 0.7755 11.00000 0.05 0.34 Q14 1 0.7915 0.3247 0.5935 11.00000 0.05 0.34 Q15 1 0.6815 -0.1227 0.5987 11.00000 0.05 0.33 Q16 1 0.8366 0.0733 1.0240 11.00000 0.05 0.33 ; _shelx_res_checksum 93801 _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 2.071 _oxdiff_exptl_absorpt_empirical_full_min 0.661 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 Br2 Br 0.97079(6) 0.52430(5) 0.80484(4) 0.04392(16) Uani 1 1 d . . . . . Br1 Br 0.66972(6) 0.63265(6) 0.65283(4) 0.05354(19) Uani 1 1 d . . . . . Br4 Br 0.95887(6) 0.90626(5) 0.79414(4) 0.05326(18) Uani 1 1 d . . . . . Br3 Br 0.64964(6) 0.72088(6) 0.92800(4) 0.05358(19) Uani 1 1 d . . . . . Mn1 Mn 0.80412(8) 0.70271(8) 0.79688(5) 0.0360(2) Uani 1 1 d . . . . . P2 P 0.79601(14) 0.24108(14) 0.95281(9) 0.0364(4) Uani 1 1 d . . . . . P1 P 0.75913(15) 0.35385(13) 0.39344(9) 0.0356(3) Uani 1 1 d . U . . . Cl2 Cl 0.52350(18) -0.02327(15) 0.82470(12) 0.0706(5) Uani 1 1 d . . . . . Cl1 Cl 0.8596(2) 0.27300(19) 0.62712(11) 0.0912(6) Uani 1 1 d . U . . . F2 F 0.3582(4) 0.4907(3) 0.7982(2) 0.0785(12) Uani 1 1 d . . . . . C11 C 0.5807(5) 0.2322(4) 0.8253(3) 0.0311(12) Uani 1 1 d D . . . . F1 F 0.6074(5) -0.1831(4) 0.3997(3) 0.1120(16) Uani 1 1 d D U . . . C17 C 0.7368(5) 0.2137(5) 0.8393(3) 0.0333(12) Uani 1 1 d . . . . . H17A H 0.792738 0.271691 0.808036 0.040 Uiso 1 1 calc R U . . . H17B H 0.755686 0.126473 0.813218 0.040 Uiso 1 1 calc R U . . . C12 C 0.4761(5) 0.1318(5) 0.8192(3) 0.0398(13) Uani 1 1 d D . . . . C9 C 0.7165(6) 0.2717(5) 0.2850(3) 0.0442(14) Uani 1 1 d . U . . . H9A H 0.770601 0.311918 0.243061 0.066 Uiso 1 1 calc R U . . . H9B H 0.616742 0.275485 0.273346 0.066 Uiso 1 1 calc R U . . . H9C H 0.739010 0.183413 0.280201 0.066 Uiso 1 1 calc R U . . . C1 C 0.6942(6) 0.1542(5) 0.4881(3) 0.0451(15) Uani 1 1 d D U . . . C15 C 0.3951(6) 0.3694(6) 0.8056(3) 0.0505(16) Uani 1 1 d D . . . . C16 C 0.5378(6) 0.3539(5) 0.8180(3) 0.0428(14) Uani 1 1 d D . . . . H16 H 0.604206 0.423711 0.821474 0.051 Uiso 1 1 calc R U . . . C6 C 0.6368(7) 0.0434(6) 0.4343(4) 0.0557(17) Uani 1 1 d D U . . . C10 C 0.7229(6) 0.5190(5) 0.4029(4) 0.0550(16) Uani 1 1 d . U . . . H10A H 0.783267 0.559616 0.364006 0.083 Uiso 1 1 calc R U . . . H10B H 0.740661 0.561074 0.462536 0.083 Uiso 1 1 calc R U . . . H10C H 0.625064 0.525489 0.387410 0.083 Uiso 1 1 calc R U . . . C7 C 0.6511(6) 0.2855(5) 0.4731(4) 0.0467(15) Uani 1 1 d . U . . . H7A H 0.657502 0.344102 0.528736 0.056 Uiso 1 1 calc R U . . . H7B H 0.552611 0.277553 0.453220 0.056 Uiso 1 1 calc R U . . . C2 C 0.7862(7) 0.1386(6) 0.5555(4) 0.0566(17) Uani 1 1 d D U . . . C13 C 0.3324(6) 0.1489(6) 0.8064(4) 0.0556(16) Uani 1 1 d D . . . . H13 H 0.265038 0.079681 0.802347 0.067 Uiso 1 1 calc R U . . . C14 C 0.2919(6) 0.2701(6) 0.8000(4) 0.0577(18) Uani 1 1 d D . . . . H14 H 0.196714 0.284554 0.792067 0.069 Uiso 1 1 calc R U . . . C19 C 0.9851(5) 0.2409(6) 0.9528(4) 0.0603(18) Uani 1 1 d . . . . . H19A H 1.012958 0.159510 0.922563 0.090 Uiso 1 1 calc R U . . . H19B H 1.020540 0.254604 1.012378 0.090 Uiso 1 1 calc R U . . . H19C H 1.023831 0.308536 0.923285 0.090 Uiso 1 1 calc R U . . . C20 C 0.7449(6) 0.3941(5) 1.0062(3) 0.0532(16) Uani 1 1 d . . . . . H20A H 0.770640 0.458143 0.970380 0.080 Uiso 1 1 calc R U . . . H20B H 0.792705 0.416191 1.062381 0.080 Uiso 1 1 calc R U . . . H20C H 0.643867 0.390258 1.014572 0.080 Uiso 1 1 calc R U . . . C8 C 0.9437(5) 0.3409(6) 0.4152(4) 0.0572(17) Uani 1 1 d . U . . . H8A H 0.965969 0.252479 0.400941 0.086 Uiso 1 1 calc R U . . . H8B H 0.964447 0.371790 0.476416 0.086 Uiso 1 1 calc R U . . . H8C H 0.999886 0.391554 0.379880 0.086 Uiso 1 1 calc R U . . . C5 C 0.6702(7) -0.0768(6) 0.4516(4) 0.070(2) Uani 1 1 d D U . . . C18 C 0.7255(7) 0.1177(6) 1.0101(4) 0.0626(18) Uani 1 1 d . . . . . H18A H 0.624516 0.123291 1.015943 0.094 Uiso 1 1 calc R U . . . H18B H 0.769160 0.128413 1.067572 0.094 Uiso 1 1 calc R U . . . H18C H 0.744758 0.035025 0.977714 0.094 Uiso 1 1 calc R U . . . C3 C 0.8185(8) 0.0175(7) 0.5722(5) 0.082(2) Uani 1 1 d D U . . . H3 H 0.879219 0.010326 0.618718 0.098 Uiso 1 1 calc R U . . . C4 C 0.7602(9) -0.0907(8) 0.5195(5) 0.083(2) Uani 1 1 d D U . . . H4 H 0.782(7) -0.180(7) 0.526(4) 0.10(3) Uiso 1 1 d . . . . . H6 H 0.573(5) 0.048(5) 0.390(3) 0.045(16) Uiso 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 Br2 0.0401(3) 0.0407(4) 0.0528(4) 0.0116(3) -0.0030(3) 0.0067(3) Br1 0.0428(4) 0.0757(5) 0.0409(3) 0.0060(3) -0.0096(3) 0.0046(3) Br4 0.0477(4) 0.0362(4) 0.0741(4) 0.0047(3) 0.0052(3) -0.0001(3) Br3 0.0521(4) 0.0578(4) 0.0526(4) 0.0114(3) 0.0165(3) 0.0104(3) Mn1 0.0336(5) 0.0380(5) 0.0362(5) 0.0056(4) -0.0017(4) 0.0026(4) P2 0.0315(8) 0.0448(9) 0.0323(8) 0.0049(7) -0.0009(6) 0.0015(7) P1 0.0383(9) 0.0343(9) 0.0339(8) 0.0052(7) 0.0006(6) 0.0009(6) Cl2 0.0649(11) 0.0378(10) 0.1074(14) 0.0136(9) -0.0206(10) -0.0113(8) Cl1 0.1386(19) 0.0906(15) 0.0424(10) 0.0141(10) -0.0166(11) -0.0161(13) F2 0.100(3) 0.073(3) 0.067(2) 0.011(2) -0.009(2) 0.046(2) C11 0.028(3) 0.035(3) 0.030(3) 0.004(2) 0.001(2) 0.001(2) F1 0.180(5) 0.054(3) 0.093(3) -0.001(2) 0.036(3) -0.031(3) C17 0.039(3) 0.028(3) 0.032(3) 0.003(2) -0.001(2) -0.005(2) C12 0.038(3) 0.040(3) 0.041(3) 0.006(3) -0.008(3) -0.002(3) C9 0.046(3) 0.042(3) 0.041(3) -0.004(3) -0.003(3) 0.000(3) C1 0.051(4) 0.043(4) 0.042(3) 0.010(3) 0.016(3) 0.004(3) C15 0.072(5) 0.050(4) 0.032(3) 0.006(3) 0.001(3) 0.031(4) C16 0.052(4) 0.043(4) 0.034(3) 0.006(3) -0.005(3) 0.007(3) C6 0.065(4) 0.053(4) 0.051(4) 0.016(3) 0.012(3) -0.003(3) C10 0.081(5) 0.033(3) 0.048(4) 0.001(3) -0.007(3) 0.000(3) C7 0.044(3) 0.048(4) 0.053(3) 0.017(3) 0.010(3) 0.010(3) C2 0.079(4) 0.054(4) 0.040(3) 0.015(3) 0.003(3) 0.004(3) C13 0.045(4) 0.062(5) 0.060(4) 0.015(3) -0.005(3) -0.008(3) C14 0.037(4) 0.092(6) 0.045(4) 0.013(4) 0.000(3) 0.010(4) C19 0.032(3) 0.087(5) 0.061(4) 0.007(4) -0.007(3) 0.008(3) C20 0.059(4) 0.050(4) 0.045(4) -0.011(3) -0.003(3) 0.010(3) C8 0.043(4) 0.078(5) 0.052(4) 0.016(3) -0.002(3) 0.000(3) C5 0.092(5) 0.045(4) 0.069(4) 0.004(4) 0.029(4) -0.009(4) C18 0.075(5) 0.062(4) 0.056(4) 0.026(3) -0.001(3) -0.002(4) C3 0.099(5) 0.079(5) 0.078(5) 0.039(4) -0.005(4) 0.015(4) C4 0.105(6) 0.064(5) 0.087(5) 0.033(4) 0.014(4) 0.016(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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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 Br1 Mn1 Br2 104.40(3) . . ? Br4 Mn1 Br2 106.82(3) . . ? Br4 Mn1 Br1 111.23(3) . . ? Br3 Mn1 Br2 108.34(3) . . ? Br3 Mn1 Br1 113.64(4) . . ? Br3 Mn1 Br4 111.86(4) . . ? C19 P2 C17 107.1(3) . . ? C19 P2 C20 109.3(3) . . ? C19 P2 C18 109.1(3) . . ? C20 P2 C17 109.7(2) . . ? C20 P2 C18 109.9(3) . . ? C18 P2 C17 111.6(3) . . ? C9 P1 C7 110.2(3) . . ? C9 P1 C8 108.7(3) . . ? C10 P1 C9 110.2(3) . . ? C10 P1 C7 107.4(3) . . ? C10 P1 C8 109.7(3) . . ? C8 P1 C7 110.5(3) . . ? C12 C11 C17 122.7(4) . . ? C12 C11 C16 117.6(5) . . ? C16 C11 C17 119.7(4) . . ? P2 C17 H17A 108.5 . . ? P2 C17 H17B 108.5 . . ? C11 C17 P2 115.0(3) . . ? C11 C17 H17A 108.5 . . ? C11 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C11 C12 Cl2 119.8(4) . . ? C11 C12 C13 122.7(5) . . ? C13 C12 Cl2 117.5(4) . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C1 C7 119.7(5) . . ? C2 C1 C6 117.6(5) . . ? C2 C1 C7 122.7(5) . . ? F2 C15 C16 116.9(5) . . ? F2 C15 C14 119.9(5) . . ? C14 C15 C16 123.2(5) . . ? C11 C16 H16 120.5 . . ? C15 C16 C11 119.0(5) . . ? C15 C16 H16 120.5 . . ? C1 C6 H6 121(3) . . ? C5 C6 C1 119.4(6) . . ? C5 C6 H6 119(3) . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C7 H7A 108.8 . . ? P1 C7 H7B 108.8 . . ? C1 C7 P1 113.7(4) . . ? C1 C7 H7A 108.8 . . ? C1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C1 C2 Cl1 120.2(4) . . ? C1 C2 C3 122.4(6) . . ? C3 C2 Cl1 117.3(5) . . ? C12 C13 H13 120.6 . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 118.7(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? P2 C19 H19A 109.5 . . ? P2 C19 H19B 109.5 . . ? P2 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P2 C20 H20A 109.5 . . ? P2 C20 H20B 109.5 . . ? P2 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P1 C8 H8A 109.5 . . ? P1 C8 H8B 109.5 . . ? P1 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? F1 C5 C6 117.6(6) . . ? F1 C5 C4 120.0(6) . . ? C4 C5 C6 122.3(7) . . ? P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C3 H3 120.3 . . ? C4 C3 C2 119.5(7) . . ? C4 C3 H3 120.3 . . ? C5 C4 H4 117(4) . . ? C3 C4 C5 118.8(7) . . ? C3 C4 H4 124(4) . . ? 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 Br2 Mn1 2.5451(9) . ? Br1 Mn1 2.5262(10) . ? Br4 Mn1 2.5236(10) . ? Br3 Mn1 2.4813(10) . ? P2 C17 1.803(5) . ? P2 C19 1.781(5) . ? P2 C20 1.784(5) . ? P2 C18 1.785(5) . ? P1 C9 1.781(5) . ? P1 C10 1.781(5) . ? P1 C7 1.806(5) . ? P1 C8 1.787(5) . ? Cl2 C12 1.739(5) . ? Cl1 C2 1.749(6) . ? F2 C15 1.370(6) . ? C11 C17 1.514(6) . ? C11 C12 1.391(6) . ? C11 C16 1.393(5) . ? F1 C5 1.365(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C12 C13 1.394(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C1 C6 1.394(6) . ? C1 C7 1.522(7) . ? C1 C2 1.385(6) . ? C15 C16 1.380(6) . ? C15 C14 1.374(6) . ? C16 H16 0.9300 . ? C6 C5 1.394(6) . ? C6 H6 0.92(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C2 C3 1.396(6) . ? C13 H13 0.9300 . ? C13 C14 1.377(6) . ? C14 H14 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C5 C4 1.375(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C3 H3 0.9300 . ? C3 C4 1.369(7) . ? C4 H4 1.00(7) . ? 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 Cl2 C12 C13 C14 -178.7(4) . . . . ? Cl1 C2 C3 C4 178.1(6) . . . . ? F2 C15 C16 C11 -179.6(4) . . . . ? F2 C15 C14 C13 179.1(5) . . . . ? C11 C12 C13 C14 -0.3(8) . . . . ? F1 C5 C4 C3 -178.2(6) . . . . ? C17 C11 C12 Cl2 -1.7(7) . . . . ? C17 C11 C12 C13 179.9(5) . . . . ? C17 C11 C16 C15 -179.8(4) . . . . ? C12 C11 C17 P2 -92.3(5) . . . . ? C12 C11 C16 C15 0.3(7) . . . . ? C12 C13 C14 C15 0.6(9) . . . . ? C9 P1 C7 C1 73.2(5) . . . . ? C1 C6 C5 F1 177.4(5) . . . . ? C1 C6 C5 C4 -1.1(10) . . . . ? C1 C2 C3 C4 1.3(11) . . . . ? C16 C11 C17 P2 87.8(5) . . . . ? C16 C11 C12 Cl2 178.2(4) . . . . ? C16 C11 C12 C13 -0.2(8) . . . . ? C16 C15 C14 C13 -0.5(9) . . . . ? C6 C1 C7 P1 -87.5(6) . . . . ? C6 C1 C2 Cl1 -178.7(4) . . . . ? C6 C1 C2 C3 -2.1(9) . . . . ? C6 C5 C4 C3 0.3(11) . . . . ? C10 P1 C7 C1 -166.7(4) . . . . ? C7 C1 C6 C5 -176.3(5) . . . . ? C7 C1 C2 Cl1 -0.6(8) . . . . ? C7 C1 C2 C3 176.1(6) . . . . ? C2 C1 C6 C5 1.9(9) . . . . ? C2 C1 C7 P1 94.4(6) . . . . ? C2 C3 C4 C5 -0.4(12) . . . . ? C14 C15 C16 C11 0.1(8) . . . . ? C19 P2 C17 C11 -170.4(4) . . . . ? C20 P2 C17 C11 -51.8(4) . . . . ? C8 P1 C7 C1 -47.0(5) . . . . ? C18 P2 C17 C11 70.2(4) . . . . ?