#------------------------------------------------------------------------------ #$Date: 2021-01-13 07:12:41 +0200 (Wed, 13 Jan 2021) $ #$Revision: 260910 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/20/7242059.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_7242059 loop_ _publ_author_name 'Li, Yanyan' 'Lin, Liting' 'Yang, Jie' 'Qian, Kun' 'Jiang, Tao' 'Li, Hong' _publ_section_title ; Red/green-light emission in continuous dielectric phase transition materials: [Me3NVinyl]2[MnX4] (X = Cl, Br) ; _journal_issue 4 _journal_name_full 'RSC Advances' _journal_page_first 2329 _journal_page_last 2336 _journal_paper_doi 10.1039/D0RA08795E _journal_volume 11 _journal_year 2021 _chemical_formula_moiety 'Cl4 Mn, 2(C5 H12 N)' _chemical_formula_sum 'C10 H24 Cl4 Mn N2' _chemical_formula_weight 369.05 _chemical_properties_physical Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2020-07-31 _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _audit_update_record ; 2020-07-31 deposited with the CCDC. 2020-12-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 119.224(7) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.2344(10) _cell_length_b 12.6038(4) _cell_length_c 18.1345(10) _cell_measurement_reflns_used 6523 _cell_measurement_temperature 200.00(10) _cell_measurement_theta_max 75.5030 _cell_measurement_theta_min 10.6670 _cell_volume 3637.2(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine 1.3 (Bourhis et al., 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 200.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.957 _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 -25.00 16.00 0.50 0.08 -- 46.37 -72.00 92.00 82 2 \w 25.00 52.00 0.50 0.08 -- 46.37 -72.00 92.00 54 3 \w 36.00 87.00 0.50 0.31 -- 107.75 -72.00 92.00 102 4 \w 71.00 101.00 0.50 0.31 -- 107.75 -77.00 120.00 60 5 \w 76.00 107.00 0.50 0.31 -- 107.75-125.00 90.00 62 6 \w 39.00 65.00 0.50 0.31 -- 107.75-125.00 90.00 52 7 \w 37.00 68.00 0.50 0.31 -- 107.75 -61.00 0.00 62 8 \w 40.00 68.00 0.50 0.31 -- 107.75 -61.00 -60.00 56 9 \w 37.00 67.00 0.50 0.31 -- 107.75 -61.00-120.00 60 10 \w 50.00 95.00 0.50 0.31 -- 107.75 -77.00-120.00 90 11 \w 93.00 157.00 0.50 0.31 -- 107.75 15.00 0.00 128 12 \w 143.00 168.00 0.50 0.31 -- 107.75 72.00-137.00 50 13 \w 100.00 165.00 0.50 0.31 -- 107.75 45.00-180.00 130 14 \w 47.00 72.00 0.50 0.08 -- 46.37 72.00-137.00 50 15 \w -29.00 22.00 0.50 0.08 -- 46.37 -19.00 -60.00 102 16 \w -21.00 14.00 0.50 0.08 -- 46.37 -19.00 90.00 70 17 \w 37.00 65.00 0.50 0.31 -- 107.75 -61.00 120.00 56 18 \w -58.00 -32.00 0.50 0.08 -- -46.37 -72.00 92.00 52 19 \w -104.00 -63.00 0.50 0.08 -- -46.37 -72.00 92.00 82 20 \w -58.00 27.00 0.50 0.08 -- -46.37 72.00-137.00 170 21 \w -54.00 -28.00 0.50 0.31 -- -100.00 45.00 -30.00 52 22 \w -53.00 -28.00 0.50 0.31 -- -100.00 45.00 30.00 50 23 \w -85.00 -36.00 0.50 0.31 -- -100.00 72.00-137.00 98 24 \w -110.00 -83.00 0.50 0.31 -- -100.00 -77.00 -30.00 54 25 \w -158.00-119.00 0.50 0.31 -- -100.00 -77.00 -30.00 78 26 \w -167.00 -85.00 0.50 0.31 -- -100.00 -72.00 92.00 164 27 \w -163.00 -86.00 0.50 0.31 -- -100.00 -30.00 150.00 154 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0615506000 _diffrn_orient_matrix_UB_12 -0.0906627000 _diffrn_orient_matrix_UB_13 0.0109350000 _diffrn_orient_matrix_UB_21 0.0613643000 _diffrn_orient_matrix_UB_22 0.0394265000 _diffrn_orient_matrix_UB_23 0.0893483000 _diffrn_orient_matrix_UB_31 -0.0439617000 _diffrn_orient_matrix_UB_32 -0.0717501000 _diffrn_orient_matrix_UB_33 0.0354991000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_unetI/netI 0.0169 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.957 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 12898 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 77.257 _diffrn_reflns_theta_min 2.777 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.178 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.42374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.348 _exptl_crystal_description block _exptl_crystal_F_000 1528 _exptl_crystal_preparation 'Magnetic properties,Luminescent' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.576 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.114 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 320 _refine_ls_number_reflns 12898 _refine_ls_number_restraints 221 _refine_ls_restrained_S_all 1.108 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0655 _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^)+(0.0783P)^2^+11.8541P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1787 _refine_ls_wR_factor_ref 0.2027 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11061 _reflns_number_total 12898 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL P21c_a.res in P2(1)/c QK-LYY-200621-CL-200K-AGAIN_twin1_hklf5.res created by SHELXL-2018/3 at 11:47:27 on 31-Jul-2020 REM Old TITL P21c_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.313, Rweak 0.073, Alpha 0.137 REM 2.510 for 349 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N7 Mn2 Cl8 CELL 1.54178 18.2344 12.6038 18.1345 90.000 119.224 90.000 ZERR 8 0.0010 0.0004 0.0010 0.000 0.007 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N MN CL UNIT 80 192 16 8 32 DFIX_NC5 2.4 0.01 N1 C5 SAME_NC5 N1 > C5 DFIX_NC5 1.34 0.01 C4 C5 SIMU 0.04 0.08 1 L.S. 10 BOND LIST 4 acta merg 0 simu 0.01 0.02 2 FMAP 2 PLAN 20 WGHT 0.0783 11.8543 BASF 0.49815 FVAR 3.27949 MN01 4 0.334740 0.241260 0.419379 11.00000 0.03192 0.03899 = 0.02899 -0.00220 0.01484 -0.00365 CL03 5 0.423191 0.217753 0.566675 11.00000 0.05238 0.05238 = 0.03168 0.00044 0.01134 0.00121 CL06 5 0.314145 0.424158 0.383439 11.00000 0.05480 0.04063 = 0.04740 0.00604 0.01555 -0.00232 CL09 5 0.398140 0.161917 0.346451 11.00000 0.08562 0.06390 = 0.07142 -0.00894 0.06069 0.00102 CL0A 5 0.201575 0.164917 0.372982 11.00000 0.03640 0.06760 = 0.06994 0.00702 0.01744 -0.01449 RESI NC5 1 N1 3 0.511148 1.013316 0.822648 11.00000 0.02981 0.03158 = 0.03245 -0.00057 0.01311 0.00288 C1 1 0.529441 1.008950 0.912146 11.00000 0.06021 0.07504 = 0.02763 -0.00278 0.01751 0.00030 AFIX 137 H1A 2 0.530960 0.936296 0.928728 11.00000 -1.50000 H1B 2 0.486314 1.046098 0.917498 11.00000 -1.50000 H1C 2 0.582837 1.041642 0.947879 11.00000 -1.50000 AFIX 0 C2 1 0.500108 1.125358 0.794012 11.00000 0.05125 0.04267 = 0.05341 0.00977 0.00750 -0.00053 AFIX 137 H2A 2 0.489708 1.128051 0.736795 11.00000 -1.50000 H2B 2 0.550152 1.164711 0.829796 11.00000 -1.50000 H2C 2 0.453324 1.155790 0.796921 11.00000 -1.50000 AFIX 0 C3 1 0.585250 0.967518 0.819151 11.00000 0.04036 0.04936 = 0.07437 -0.01641 0.03547 -0.00418 AFIX 137 H3A 2 0.573747 0.965555 0.761555 11.00000 -1.50000 H3B 2 0.595639 0.896840 0.841751 11.00000 -1.50000 H3C 2 0.633826 1.010828 0.851906 11.00000 -1.50000 AFIX 0 C4 1 0.432450 0.956024 0.770061 11.00000 0.03318 0.03666 = 0.03665 0.00084 0.01639 -0.00119 AFIX 43 H4 2 0.386217 0.970845 0.776994 11.00000 -1.20000 AFIX 0 C5 1 0.424322 0.885301 0.714063 11.00000 0.04606 0.05128 = 0.06132 -0.01455 0.02295 -0.00844 AFIX 93 H5A 2 0.469691 0.869165 0.706018 11.00000 -1.20000 H5B 2 0.373156 0.851003 0.682176 11.00000 -1.20000 AFIX 0 RESI 0 RESI NC5 2 N1 3 0.322474 0.827825 0.377503 11.00000 0.05100 0.04978 = 0.04717 0.00179 0.02680 -0.00456 C1 1 0.341445 0.712348 0.392811 11.00000 0.10081 0.03677 = 0.07257 0.00560 0.05218 0.00784 AFIX 137 H1A 2 0.329872 0.688612 0.436395 11.00000 -1.50000 H1B 2 0.399635 0.700382 0.410158 11.00000 -1.50000 H1C 2 0.307049 0.673667 0.341740 11.00000 -1.50000 AFIX 0 C2 1 0.345566 0.861440 0.311907 11.00000 0.07409 0.07883 = 0.06337 0.01093 0.04214 -0.00774 AFIX 137 H2A 2 0.333451 0.935524 0.299778 11.00000 -1.50000 H2B 2 0.313565 0.820956 0.261238 11.00000 -1.50000 H2C 2 0.404423 0.849301 0.332824 11.00000 -1.50000 AFIX 0 C3 1 0.232827 0.845438 0.345284 11.00000 0.05577 0.08427 = 0.09186 -0.01133 0.04115 0.00576 AFIX 137 H3A 2 0.219859 0.918828 0.330481 11.00000 -1.50000 H3B 2 0.218469 0.826889 0.388009 11.00000 -1.50000 H3C 2 0.201188 0.802184 0.296169 11.00000 -1.50000 AFIX 0 C4 1 0.379134 0.883357 0.455615 11.00000 0.08612 0.06460 = 0.05182 -0.00131 0.02913 -0.01750 AFIX 43 H4 2 0.436789 0.875399 0.477615 11.00000 -1.20000 AFIX 0 C5 1 0.352132 0.943415 0.495543 11.00000 0.18032 0.07963 = 0.06292 -0.00235 0.04373 -0.00075 AFIX 93 H5A 2 0.294706 0.952375 0.474553 11.00000 -1.20000 H5B 2 0.390227 0.977447 0.545115 11.00000 -1.20000 AFIX 0 RESI 0 RESI NC5 3 N1 3 0.051846 0.507100 0.317245 11.00000 0.04649 0.04935 = 0.03895 0.00295 0.02332 0.00350 C1 1 0.108642 0.539403 0.405067 11.00000 0.18030 0.10533 = 0.04273 -0.01505 0.04332 -0.04780 AFIX 137 H1A 2 0.076144 0.559712 0.431421 11.00000 -1.50000 H1B 2 0.142160 0.598433 0.405580 11.00000 -1.50000 H1C 2 0.144685 0.481145 0.435510 11.00000 -1.50000 AFIX 0 C2 1 0.061890 0.391094 0.312946 11.00000 0.13039 0.05240 = 0.07178 0.00060 0.06446 -0.00589 AFIX 137 H2A 2 0.022197 0.365804 0.257680 11.00000 -1.50000 H2B 2 0.052078 0.356403 0.354464 11.00000 -1.50000 H2C 2 0.117909 0.375846 0.323905 11.00000 -1.50000 AFIX 0 C3 1 -0.035246 0.531080 0.292474 11.00000 0.08333 0.16595 = 0.15859 0.10098 0.08927 0.05566 AFIX 137 H3A 2 -0.070135 0.516544 0.233358 11.00000 -1.50000 H3B 2 -0.040153 0.604622 0.303154 11.00000 -1.50000 H3C 2 -0.052894 0.487889 0.324572 11.00000 -1.50000 AFIX 0 C4 1 0.080965 0.560417 0.263863 11.00000 0.04067 0.06278 = 0.05075 0.00569 0.02396 -0.00091 AFIX 43 H4 2 0.136418 0.550716 0.276368 11.00000 -1.20000 AFIX 0 C5 1 0.032876 0.620105 0.200395 11.00000 0.06045 0.08668 = 0.09173 0.04052 0.04630 0.01459 AFIX 93 H5A 2 -0.022797 0.630935 0.186722 11.00000 -1.20000 H5B 2 0.053984 0.652178 0.168449 11.00000 -1.20000 AFIX 0 RESI 0 RESI NC5 4 N1 3 0.826517 0.702619 0.895359 11.00000 0.04668 0.05642 = 0.03982 -0.00593 0.01460 -0.00270 C1 1 0.881868 0.640522 0.972629 11.00000 0.07549 0.08359 = 0.04506 0.01015 0.01696 -0.00444 AFIX 137 H1A 2 0.864257 0.650926 1.014096 11.00000 -1.50000 H1B 2 0.938903 0.664012 0.995067 11.00000 -1.50000 H1C 2 0.878158 0.566562 0.958580 11.00000 -1.50000 AFIX 0 C2 1 0.851748 0.671270 0.830927 11.00000 0.08966 0.09044 = 0.05688 0.00153 0.04231 -0.01006 AFIX 137 H2A 2 0.818664 0.710144 0.779621 11.00000 -1.50000 H2B 2 0.842531 0.596607 0.819756 11.00000 -1.50000 H2C 2 0.910169 0.687031 0.852242 11.00000 -1.50000 AFIX 0 C3 1 0.738413 0.669981 0.862824 11.00000 0.03986 0.10513 = 0.12119 -0.02467 0.03595 -0.00351 AFIX 137 H3A 2 0.703191 0.707273 0.811250 11.00000 -1.50000 H3B 2 0.721264 0.686416 0.903857 11.00000 -1.50000 H3C 2 0.733404 0.594997 0.852175 11.00000 -1.50000 AFIX 0 C4 1 0.846060 0.813512 0.913843 11.00000 0.10344 0.05293 = 0.07026 -0.01473 -0.00427 -0.00257 AFIX 43 H4 2 0.897849 0.829025 0.960443 11.00000 -1.20000 AFIX 0 C5 1 0.800475 0.893212 0.873626 11.00000 0.09074 0.07594 = 0.11890 -0.02922 0.02052 0.00270 AFIX 93 H5A 2 0.748042 0.882524 0.826490 11.00000 -1.20000 H5B 2 0.819803 0.961780 0.891556 11.00000 -1.20000 AFIX 0 RESI 0 RESI 5 MnCl sadi_MnCl Mn1 Cl1 Mn1 Cl2 Mn1 Cl3 Mn1 Cl4 sadi_MnCl Cl1 Cl2 Cl2 Cl3 Cl1 Cl3 Cl1 Cl4 Cl2 Cl4 Cl3 Cl4 MN1 4 0.158639 0.771031 0.556866 11.00000 0.03020 0.03809 = 0.03200 -0.00129 0.01426 0.00074 CL2 5 0.212345 0.888853 0.672145 11.00000 0.04998 0.05559 = 0.04966 -0.01749 0.02305 -0.00533 CL3 5 0.273525 0.678299 0.561911 11.00000 0.03521 0.05505 = 0.05334 -0.00410 0.01699 0.01025 CL4 5 0.084660 0.857219 0.426177 11.00000 0.05228 0.08174 = 0.04637 0.02361 0.02063 0.01833 CL1 5 0.067885 0.651245 0.572603 11.00000 0.06093 0.05560 = 0.07086 0.00023 0.04318 -0.01365 HKLF 5 1 0 0 1 0 -1 0 1 0 0 REM P21c_a.res in P2(1)/c REM wR2 = 0.202655, GooF = S = 1.08854, Restrained GooF = 1.10819 for all data REM R1 = 0.065452 for 11061 Fo > 4sig(Fo) and 0.080911 for all 12898 data REM 320 parameters refined using 221 restraints END WGHT 0.0783 11.8543 REM Highest difference peak 0.576, deepest hole -0.583, 1-sigma level 0.114 Q1 1 0.2305 0.3382 0.4209 11.00000 0.05 0.58 Q2 1 0.3580 0.5848 0.4515 11.00000 0.05 0.54 Q3 1 0.1099 0.8431 0.5067 11.00000 0.05 0.52 Q4 1 0.1781 0.7412 0.5900 11.00000 0.05 0.52 Q5 1 0.8021 0.7955 0.9261 11.00000 0.05 0.52 Q6 1 -0.0017 0.5728 0.3404 11.00000 0.05 0.52 Q7 1 0.2915 0.4135 0.4086 11.00000 0.05 0.50 Q8 1 0.1079 0.7298 0.2324 11.00000 0.05 0.48 Q9 1 0.8450 0.5190 1.0116 11.00000 0.05 0.48 Q10 1 0.3399 0.3564 0.4227 11.00000 0.05 0.48 Q11 1 0.4480 1.1517 0.9438 11.00000 0.05 0.48 Q12 1 0.2195 0.1448 0.3376 11.00000 0.05 0.47 Q13 1 0.0077 0.4118 0.2806 11.00000 0.05 0.46 Q14 1 0.1575 0.8434 0.5037 11.00000 0.05 0.45 Q15 1 0.2864 0.0911 0.3413 11.00000 0.05 0.45 Q16 1 0.6517 0.5316 0.8472 11.00000 0.05 0.44 Q17 1 0.1893 0.7768 0.6272 11.00000 0.05 0.44 Q18 1 0.3807 0.2336 0.4978 11.00000 0.05 0.44 Q19 1 0.4130 0.1175 0.5602 11.00000 0.05 0.44 Q20 1 -0.0283 0.4284 0.2370 11.00000 0.05 0.44 ; _twin_special_details ; Component 2 rotated by -179.9884\% around [1.00 -0.00 0.00] (reciprocal) or [0.90 -0.00 0.44] (direct) ; _cod_data_source_file d0ra08795e2.cif _cod_data_source_block QK-LYY-200621-CL-200K-AGAIN_twin1_hklf5 _cod_database_code 7242059 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'MnCl4 C4HN' _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. Twinned data refinement Scales: 0.5019(15) 0.4981(15) 2. 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 3. Restrained distances N1_1-C5_1 N1_2-C5_2 N1_3-C5_3 N1_4-C5_4 2.4 with sigma of 0.01 C4_1-C5_1 C4_2-C5_2 C4_3-C5_3 C4_4-C5_4 1.34 with sigma of 0.01 Mn1_5-Cl1_5 \\sim Mn1_5-Cl2_5 \\sim Mn1_5-Cl3_5 \\sim Mn1_5-Cl4_5 with sigma of 0.02 Cl1_5-Cl2_5 \\sim Cl2_5-Cl3_5 \\sim Cl1_5-Cl3_5 \\sim Cl1_5-Cl4_5 \\sim Cl2_5-Cl4_5 \\sim Cl3_5- Cl4_5 with sigma of 0.02 4. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1A All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 5. Same fragment restrains {N1_2, C1_2, C2_2, C3_2, C4_2, C5_2} {N1_3, C1_3, C2_3, C3_3, C4_3, C5_3} {N1_4, C1_4, C2_4, C3_4, C4_4, C5_4} as {N1_1, C1_1, C2_1, C3_1, C4_1, C5_1} sigma for 1-2: 0.02 1-3: 0.04 6.a Aromatic/amide H refined with riding coordinates: C4(H4), C4(H4), C4(H4), C4(H4) 6.b X=CH2 refined with riding coordinates: C5(H5A,H5B), C5(H5A,H5B), C5(H5A,H5B), C5(H5A,H5B) 6.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A, H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C) ; _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 2.331 _oxdiff_exptl_absorpt_empirical_full_min 0.591 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn01 Mn 0.33474(5) 0.24126(8) 0.41938(6) 0.0333(2) Uani 1 1 d . . . . . Cl03 Cl 0.42319(10) 0.21775(15) 0.56667(10) 0.0494(4) Uani 1 1 d . . . . . Cl06 Cl 0.31414(11) 0.42416(14) 0.38344(11) 0.0516(4) Uani 1 1 d . . . . . Cl09 Cl 0.39814(14) 0.16192(18) 0.34645(14) 0.0641(5) Uani 1 1 d . . . . . Cl0A Cl 0.20158(10) 0.16492(18) 0.37298(14) 0.0616(5) Uani 1 1 d . . . . . N1_1 N 0.5111(3) 1.0133(4) 0.8226(3) 0.0322(10) Uani 1 1 d D U . . . C1_1 C 0.5294(5) 1.0089(8) 0.9121(4) 0.0560(19) Uani 1 1 d D U . . . H1A_1 H 0.530960 0.936296 0.928728 0.084 Uiso 1 1 calc GR . . . . H1B_1 H 0.486314 1.046098 0.917498 0.084 Uiso 1 1 calc GR . . . . H1C_1 H 0.582837 1.041642 0.947879 0.084 Uiso 1 1 calc GR . . . . C2_1 C 0.5001(5) 1.1254(6) 0.7940(5) 0.0568(19) Uani 1 1 d D U . . . H2A_1 H 0.489708 1.128051 0.736795 0.085 Uiso 1 1 calc GR . . . . H2B_1 H 0.550152 1.164711 0.829796 0.085 Uiso 1 1 calc GR . . . . H2C_1 H 0.453324 1.155790 0.796921 0.085 Uiso 1 1 calc GR . . . . C3_1 C 0.5853(4) 0.9675(6) 0.8192(5) 0.0515(18) Uani 1 1 d D U . . . H3A_1 H 0.573747 0.965555 0.761555 0.077 Uiso 1 1 calc GR . . . . H3B_1 H 0.595639 0.896840 0.841751 0.077 Uiso 1 1 calc GR . . . . H3C_1 H 0.633826 1.010828 0.851906 0.077 Uiso 1 1 calc GR . . . . C4_1 C 0.4325(3) 0.9560(5) 0.7701(4) 0.0358(12) Uani 1 1 d D U . . . H4_1 H 0.386217 0.970845 0.776994 0.043 Uiso 1 1 calc R . . . . C5_1 C 0.4243(4) 0.8853(6) 0.7141(5) 0.0543(18) Uani 1 1 d D U . . . H5A_1 H 0.469691 0.869165 0.706018 0.065 Uiso 1 1 calc R . . . . H5B_1 H 0.373156 0.851003 0.682176 0.065 Uiso 1 1 calc R . . . . N1_2 N 0.3225(4) 0.8278(5) 0.3775(4) 0.0481(13) Uani 1 1 d D U . . . C1_2 C 0.3414(6) 0.7123(6) 0.3928(6) 0.066(2) Uani 1 1 d D U . . . H1A_2 H 0.329872 0.688612 0.436395 0.099 Uiso 1 1 calc GR . . . . H1B_2 H 0.399635 0.700382 0.410158 0.099 Uiso 1 1 calc GR . . . . H1C_2 H 0.307049 0.673667 0.341740 0.099 Uiso 1 1 calc GR . . . . C2_2 C 0.3456(6) 0.8614(9) 0.3119(6) 0.068(2) Uani 1 1 d D U . . . H2A_2 H 0.333451 0.935524 0.299778 0.103 Uiso 1 1 calc GR . . . . H2B_2 H 0.313565 0.820956 0.261238 0.103 Uiso 1 1 calc GR . . . . H2C_2 H 0.404423 0.849301 0.332824 0.103 Uiso 1 1 calc GR . . . . C3_2 C 0.2328(5) 0.8454(9) 0.3453(7) 0.075(3) Uani 1 1 d D U . . . H3A_2 H 0.219859 0.918828 0.330481 0.113 Uiso 1 1 calc GR . . . . H3B_2 H 0.218469 0.826889 0.388009 0.113 Uiso 1 1 calc GR . . . . H3C_2 H 0.201188 0.802184 0.296169 0.113 Uiso 1 1 calc GR . . . . C4_2 C 0.3791(6) 0.8834(8) 0.4556(5) 0.069(2) Uani 1 1 d D U . . . H4_2 H 0.436789 0.875399 0.477615 0.083 Uiso 1 1 calc R . . . . C5_2 C 0.3521(10) 0.9434(10) 0.4955(7) 0.114(4) Uani 1 1 d D U . . . H5A_2 H 0.294706 0.952375 0.474553 0.137 Uiso 1 1 calc R . . . . H5B_2 H 0.390227 0.977447 0.545115 0.137 Uiso 1 1 calc R . . . . N1_3 N 0.0518(3) 0.5071(5) 0.3172(3) 0.0439(12) Uani 1 1 d D U . . . C1_3 C 0.1086(9) 0.5394(12) 0.4051(6) 0.114(5) Uani 1 1 d D U . . . H1A_3 H 0.076144 0.559712 0.431421 0.171 Uiso 1 1 calc GR . . . . H1B_3 H 0.142160 0.598433 0.405580 0.171 Uiso 1 1 calc GR . . . . H1C_3 H 0.144685 0.481145 0.435510 0.171 Uiso 1 1 calc GR . . . . C2_3 C 0.0619(7) 0.3911(7) 0.3129(7) 0.078(3) Uani 1 1 d D U . . . H2A_3 H 0.022197 0.365804 0.257680 0.118 Uiso 1 1 calc GR . . . . H2B_3 H 0.052078 0.356403 0.354464 0.118 Uiso 1 1 calc GR . . . . H2C_3 H 0.117909 0.375846 0.323905 0.118 Uiso 1 1 calc GR . . . . C3_3 C -0.0352(7) 0.5311(13) 0.2925(10) 0.123(5) Uani 1 1 d D U . . . H3A_3 H -0.070135 0.516544 0.233358 0.185 Uiso 1 1 calc GR . . . . H3B_3 H -0.040153 0.604622 0.303154 0.185 Uiso 1 1 calc GR . . . . H3C_3 H -0.052894 0.487889 0.324572 0.185 Uiso 1 1 calc GR . . . . C4_3 C 0.0810(4) 0.5604(7) 0.2639(5) 0.0507(17) Uani 1 1 d D U . . . H4_3 H 0.136418 0.550716 0.276368 0.061 Uiso 1 1 calc R . . . . C5_3 C 0.0329(5) 0.6201(9) 0.2004(6) 0.076(3) Uani 1 1 d D U . . . H5A_3 H -0.022797 0.630935 0.186722 0.091 Uiso 1 1 calc R . . . . H5B_3 H 0.053984 0.652178 0.168449 0.091 Uiso 1 1 calc R . . . . N1_4 N 0.8265(3) 0.7026(5) 0.8954(4) 0.0504(14) Uani 1 1 d D U . . . C1_4 C 0.8819(6) 0.6405(9) 0.9726(5) 0.073(3) Uani 1 1 d D U . . . H1A_4 H 0.864257 0.650926 1.014096 0.110 Uiso 1 1 calc GR . . . . H1B_4 H 0.938903 0.664012 0.995067 0.110 Uiso 1 1 calc GR . . . . H1C_4 H 0.878158 0.566562 0.958580 0.110 Uiso 1 1 calc GR . . . . C2_4 C 0.8517(6) 0.6713(10) 0.8309(6) 0.076(3) Uani 1 1 d D U . . . H2A_4 H 0.818664 0.710144 0.779621 0.114 Uiso 1 1 calc GR . . . . H2B_4 H 0.842531 0.596607 0.819756 0.114 Uiso 1 1 calc GR . . . . H2C_4 H 0.910169 0.687031 0.852242 0.114 Uiso 1 1 calc GR . . . . C3_4 C 0.7384(5) 0.6700(10) 0.8628(8) 0.090(4) Uani 1 1 d D U . . . H3A_4 H 0.703191 0.707273 0.811250 0.135 Uiso 1 1 calc GR . . . . H3B_4 H 0.721264 0.686416 0.903857 0.135 Uiso 1 1 calc GR . . . . H3C_4 H 0.733404 0.594997 0.852175 0.135 Uiso 1 1 calc GR . . . . C4_4 C 0.8461(7) 0.8135(7) 0.9138(7) 0.095(3) Uani 1 1 d D U . . . H4_4 H 0.897849 0.829025 0.960443 0.115 Uiso 1 1 calc R . . . . C5_4 C 0.8005(7) 0.8932(7) 0.8736(8) 0.108(4) Uani 1 1 d D U . . . H5A_4 H 0.748042 0.882524 0.826490 0.130 Uiso 1 1 calc R . . . . H5B_4 H 0.819803 0.961780 0.891556 0.130 Uiso 1 1 calc R . . . . Mn1_5 Mn 0.15864(5) 0.77103(8) 0.55687(6) 0.0338(2) Uani 1 1 d D . . . . Cl2_5 Cl 0.21234(10) 0.88885(15) 0.67215(11) 0.0523(4) Uani 1 1 d D . . . . Cl3_5 Cl 0.27353(9) 0.67830(15) 0.56191(11) 0.0498(4) Uani 1 1 d D . . . . Cl4_5 Cl 0.08466(11) 0.85722(19) 0.42618(12) 0.0616(5) Uani 1 1 d D . . . . Cl1_5 Cl 0.06789(12) 0.65124(16) 0.57260(14) 0.0578(5) Uani 1 1 d 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 Mn01 0.0319(4) 0.0390(5) 0.0290(5) -0.0022(4) 0.0148(4) -0.0037(4) Cl03 0.0524(8) 0.0524(10) 0.0317(7) 0.0004(7) 0.0113(6) 0.0012(7) Cl06 0.0548(9) 0.0406(9) 0.0474(9) 0.0060(7) 0.0155(7) -0.0023(7) Cl09 0.0856(13) 0.0639(13) 0.0714(13) -0.0089(10) 0.0607(12) 0.0010(10) Cl0A 0.0364(8) 0.0676(13) 0.0699(12) 0.0070(10) 0.0174(8) -0.0145(7) N1_1 0.030(2) 0.032(3) 0.032(2) -0.001(2) 0.0131(19) 0.0029(18) C1_1 0.060(4) 0.075(6) 0.028(3) -0.003(3) 0.018(3) 0.000(4) C2_1 0.051(4) 0.043(4) 0.053(4) 0.010(3) 0.008(3) -0.001(3) C3_1 0.040(3) 0.049(4) 0.074(5) -0.016(4) 0.035(3) -0.004(3) C4_1 0.033(3) 0.037(3) 0.037(3) 0.001(3) 0.016(2) -0.001(2) C5_1 0.046(4) 0.051(5) 0.061(5) -0.015(4) 0.023(3) -0.008(3) N1_2 0.051(3) 0.050(3) 0.047(3) 0.002(3) 0.027(3) -0.005(2) C1_2 0.101(6) 0.037(4) 0.073(6) 0.006(4) 0.052(5) 0.008(4) C2_2 0.074(5) 0.079(7) 0.063(5) 0.011(5) 0.042(4) -0.008(5) C3_2 0.056(4) 0.084(7) 0.092(7) -0.011(6) 0.041(5) 0.006(4) C4_2 0.086(5) 0.065(5) 0.052(4) -0.001(4) 0.029(4) -0.018(4) C5_2 0.180(12) 0.080(9) 0.063(7) -0.002(6) 0.044(8) -0.001(8) N1_3 0.046(3) 0.049(3) 0.039(3) 0.003(2) 0.023(2) 0.003(2) C1_3 0.180(11) 0.105(10) 0.043(5) -0.015(6) 0.043(7) -0.048(9) C2_3 0.130(8) 0.052(6) 0.072(6) 0.001(5) 0.064(6) -0.006(5) C3_3 0.083(6) 0.166(12) 0.159(11) 0.101(10) 0.089(7) 0.056(7) C4_3 0.041(3) 0.063(5) 0.051(4) 0.006(3) 0.024(3) -0.001(3) C5_3 0.060(5) 0.087(7) 0.092(7) 0.041(6) 0.046(5) 0.015(4) N1_4 0.047(3) 0.056(4) 0.040(3) -0.006(3) 0.015(2) -0.003(3) C1_4 0.075(5) 0.084(7) 0.045(5) 0.010(5) 0.017(4) -0.004(5) C2_4 0.090(6) 0.090(8) 0.057(5) 0.002(5) 0.042(5) -0.010(5) C3_4 0.040(4) 0.105(9) 0.121(9) -0.025(7) 0.036(5) -0.004(4) C4_4 0.103(6) 0.053(5) 0.070(6) -0.015(5) -0.004(5) -0.003(5) C5_4 0.091(7) 0.076(8) 0.119(10) -0.029(7) 0.021(7) 0.003(6) Mn1_5 0.0302(4) 0.0381(5) 0.0320(5) -0.0013(4) 0.0143(4) 0.0007(4) Cl2_5 0.0500(8) 0.0556(10) 0.0497(9) -0.0175(8) 0.0231(7) -0.0053(7) Cl3_5 0.0352(7) 0.0550(10) 0.0533(9) -0.0041(8) 0.0170(7) 0.0103(6) Cl4_5 0.0523(9) 0.0817(14) 0.0464(9) 0.0236(9) 0.0206(8) 0.0183(9) Cl1_5 0.0609(10) 0.0556(11) 0.0709(12) 0.0002(9) 0.0432(9) -0.0136(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u _diffrn_refln_scale_group_code -1 0 1 6.60461 13.2921 -2 0 0 -1 6.60461 13.2921 1 0 0 -2 48572.9 275.411 1 0 0 -3 60.1834 55.5108 1 0 0 -4 95419.2 561.342 1 0 0 -5 486.838 101.613 1 0 0 -6 2125.75 160.116 1 6 0 -6 20623.4 349.885 -2 0 0 6 20623.4 349.885 1 7 0 -7 23865.2 418.219 -2 0 0 7 23865.2 418.219 1 8 0 -8 212898 1254.55 -2 0 0 8 212898 1254.55 1 0 0 -9 3934.96 197.464 1 0 0 10 337.58 115.989 1 0 0 11 15639.4 250.929 1 0 0 -12 53898.2 442.427 1 0 0 13 1533.9 184.866 1 0 0 14 11545.9 281.456 1 0 0 15 10133.4 215.822 1 0 0 -16 10362.2 352.589 1 0 0 -17 13691.3 356.276 1 0 0 -18 2100.19 225.845 1 0 0 -19 5237.24 199.201 1 0 -1 0 4.84951 15.4571 -2 0 1 0 4.84951 15.4571 1 -1 -1 1 2214.32 36.2713 -2 0 1 -1 2214.32 36.2713 1 -2 -1 2 345107 703.133 -2 0 1 -2 345107 703.133 1 0 1 -3 882.944 75.6455 1 0 1 -4 67314 470.334 1 0 1 5 29662.1 263.346 1 0 1 -6 1621.88 154.186 1 6 -1 -6 12300.2 281.481 -2 0 1 6 12300.2 281.481 1 0 1 7 6221.75 237.052 1 0 1 8 3772.84 231.934 1 0 1 9 11814 269.083 1 0 -1 10 74593.2 357.444 1 0 -1 11 6065.02 111.821 1 0 1 12 3913.31 108.646 1 0 -1 13 6919.2 172.79 1 0 1 -14 28404.2 280.772 1 0 1 15 9150.16 206.558 1 0 1 16 178.329 188.037 1 0 1 17 2292.13 127.421 1 0 1 -18 355.124 100.577 1 0 1 -19 651.065 77.5759 1 0 1 20 1547.38 36.1639 1 0 -2 0 572741 1162.15 -2 0 2 0 572741 1162.15 1 1 2 -1 173.174 21.791 -2 0 -2 1 173.174 21.791 1 -2 -2 2 407765 541.262 -2 0 2 -2 407765 541.262 1 -3 -2 3 158188 439.253 -2 0 2 -3 158188 439.253 1 0 -2 -4 86449.1 384.109 1 0 -2 -5 14822.4 280.358 1 5 2 -5 145867 544.269 -2 0 -2 5 145867 544.269 1 0 2 6 35389.7 438.122 1 6 2 -6 62851.3 587.131 -2 0 -2 6 62851.3 587.131 1 0 -2 7 17128.1 368.503 1 7 -2 -7 18760.3 372.485 -2 0 2 7 18760.3 372.485 1 0 -2 -8 10863.5 242.031 1 8 -2 -8 10575.6 246.69 -2 0 2 8 10575.6 246.69 1 0 2 -9 937.061 113.376 1 0 -2 -10 22710.4 186.712 1 0 -2 11 1324.41 74.5516 1 0 -2 12 39951.2 220.876 1 0 2 13 979.925 91.3098 1 0 -2 14 737.888 112.962 1 0 2 -15 3671.17 120.666 1 0 -2 -16 12017.1 210.077 1 0 2 17 1914.2 107.883 1 0 2 18 5792.71 107.274 1 0 2 19 78.2548 61.2206 1 0 -3 0 256.333 53.9696 -2 0 3 0 256.333 53.9696 1 -1 -3 1 72948.1 135.028 -2 0 3 -1 72948.1 135.028 1 2 -3 -2 148453 261.492 -2 0 3 2 148453 261.492 1 3 3 -3 65973.8 275.77 -2 0 -3 3 65973.8 275.77 1 4 3 -4 1651.21 87.7148 -2 0 -3 4 1651.21 87.7148 1 5 3 -5 32774 267.37 -2 0 -3 5 32774 267.37 1 0 3 -6 34245.1 455.182 1 6 -3 -6 101764 511.237 -2 0 3 6 101764 511.237 1 0 3 -7 3152.64 121.157 1 7 -3 -7 3829.29 231.881 -2 0 3 7 3829.29 231.881 1 0 -3 -8 86661.1 493.933 1 8 3 -8 154789 1125.33 -2 0 -3 8 154789 1125.33 1 0 3 9 10002.8 139.974 1 0 -3 -10 14444.5 136.962 1 0 -3 11 3875.47 96.2938 1 0 3 12 9907.4 130.884 1 0 -3 -13 -14.343 91.4911 1 0 3 -14 13739.1 129.923 1 0 3 -15 2263.66 118.477 1 0 -3 16 1329.13 85.4692 1 0 3 17 111.936 87.8215 1 0 3 18 267.88 76.8335 1 0 3 19 1119.59 54.6641 1 0 4 0 108051 412.543 -2 0 -4 0 108051 412.543 1 1 -4 -1 115137 584.69 -2 0 4 1 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223.609 2 11 -4 -19 3349.75 274.535 2 11 -4 -17 2179.03 203.995 2 11 -4 -16 634.695 121.919 2 -11 4 15 2891.06 85.0692 2 -11 4 14 27865.6 148.112 2 11 4 -13 479.473 85.4394 2 -11 4 12 3057.1 92.4947 2 -11 4 11 5081.13 103.593 2 11 -4 -10 4004.7 83.7335 2 -11 4 9 4553.73 76.7721 2 -11 4 8 9759.88 105.592 2 -11 4 7 1802.95 90.7191 2 -11 -4 6 12604.7 196.59 2 -11 4 -6 4595.6 111.004 2 -11 4 -7 451.437 109.281 2 -11 4 -8 3554.25 91.7756 2 -11 4 -9 191.834 67.8146 2 -11 4 -10 306.607 75.7385 2 11 -5 -20 1772.65 216.669 2 11 -5 -19 273.807 225.846 2 -11 5 16 3548.32 111.769 2 11 5 -15 425.339 79.9005 2 -11 5 14 8754.3 108.93 2 -11 5 13 4112.93 99.004 2 -11 5 12 946.318 103.146 2 -11 5 11 14926.7 117.849 2 -11 5 10 7533.09 92.4781 2 11 -5 -9 3270.89 85.0463 2 -11 5 8 550.699 60.675 2 -11 5 7 309.169 83.4971 2 -11 5 6 -94.7449 145.074 2 -11 5 -4 1116.03 326.875 2 -11 -5 -5 1614.61 239.271 2 -11 5 -6 4350.88 107.639 2 -11 -5 -7 1041.73 93.5598 2 -11 5 -8 1832.3 75.235 2 -11 5 -9 710.485 63.9785 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10 490.626 173.715 2 -11 10 9 6633.75 155.368 2 11 -10 -8 26.1054 239.682 2 11 -10 -7 1532.64 242.359 2 -11 -10 -5 856.561 115.684 2 -11 10 -6 860.162 74.8613 2 11 -11 -15 -4.52032 77.1484 2 -11 11 14 686.203 77.9149 2 -11 11 13 1466.69 96.4257 2 -11 11 12 -77.3138 113.966 2 -11 11 11 85.6965 122.815 2 -11 11 10 -600.267 213.466 2 -11 11 9 623.946 167.905 2 11 -11 -8 13526.9 318.905 2 11 -11 -7 4189.48 245.245 2 -11 11 -5 172.115 54.2873 2 11 12 -13 74.8395 74.8318 2 -11 12 12 544.786 75.6968 2 -11 12 11 1798.55 104.727 2 11 12 -10 851.536 130.863 2 -11 12 9 1098.74 200.758 2 11 13 -11 117.44 66.2006 2 -11 13 10 146.256 68.9222 2 -11 13 9 163.775 73.1908 2 12 0 -18 14012.3 322.42 2 12 0 -17 1246.34 188.958 2 -12 0 16 1340.46 170.596 2 -12 0 15 11728 297.445 2 -12 0 14 6009.54 243.932 2 -12 0 13 11400 274.682 2 12 0 -12 12897.6 270.015 2 12 0 -11 32197.1 357.711 2 -12 0 10 346.409 141.994 2 12 0 -9 1330.98 113.638 2 -12 0 8 31794 340.754 2 -12 0 7 70852.1 481.815 2 -12 0 6 185.071 139.629 2 -12 0 5 1901.88 355.323 2 -12 0 -5 889.236 183.98 2 -12 0 -6 9822.33 197.397 2 -12 0 -7 1545.46 142.242 2 -12 0 -8 8424.28 296.381 2 -12 0 -9 2233.98 212.128 2 -12 0 -10 1258.16 156.961 2 12 -1 -18 10650.1 241.96 2 12 -1 -17 14624.9 207.116 2 -12 -1 16 8698.24 149.184 2 -12 -1 15 4371.93 180.017 2 -12 -1 14 438.9 141.739 2 -12 -1 13 11348.2 203.367 2 12 1 -12 5786.71 121.693 2 12 -1 -11 32438.4 205.523 2 -12 -1 10 45396.7 231.445 2 -12 -1 9 96399.9 291.805 2 -12 -1 8 4690.39 125.086 2 -12 -1 7 249.768 132.627 2 -12 -1 6 43933.3 389.82 2 -12 -1 -5 13182.2 250.959 2 -12 -1 -6 2458.35 119.564 2 -12 -1 -7 4840.46 124.586 2 -12 -1 -8 3443.56 257.881 2 -12 -1 -9 287.193 190.89 2 -12 -1 -10 355.454 151.279 2 12 -2 -18 10937.7 235.411 2 12 2 -17 -19.6588 132.417 2 -12 2 16 661.192 114.939 2 -12 2 15 3519.75 109.585 2 -12 2 14 6007.67 141.757 2 -12 2 13 725.803 90.763 2 -12 2 12 3481.39 119.264 2 12 -2 -11 2453.25 105.816 2 -12 2 10 389.171 76.2641 2 -12 2 9 6792.96 85.961 2 -12 2 8 31409.5 166.909 2 -12 2 7 955.092 72.0704 2 -12 -2 6 11176 157.283 2 -12 -2 -5 872.935 214.877 2 -12 2 -6 1470.07 101.495 2 -12 2 -7 554.504 173.581 2 -12 2 -8 1158.68 160.418 2 -12 2 -9 2647.28 102.15 2 -12 2 -10 794.969 101.029 2 12 -3 -20 -613.714 225.546 2 12 -3 -18 6894.34 352.63 2 12 3 -17 205.305 130.695 2 12 3 -16 19798.1 173.376 2 -12 3 15 6901.8 118.747 2 -12 3 14 427.544 96.2948 2 12 3 -13 1877.77 101.272 2 -12 3 12 10046.6 153.7 2 12 -3 -11 11293.1 151.92 2 12 -3 -10 22714.1 136.369 2 -12 3 9 159.877 57.1827 2 -12 3 8 8501.53 87.3786 2 -12 3 7 19546 166.782 2 -12 3 6 22996.1 213.321 2 -12 3 -4 770.285 256.296 2 -12 -3 -5 10580.6 173.978 2 -12 3 -6 6186.84 129.44 2 -12 3 -7 3486.2 185.317 2 -12 3 -8 35.6559 14.5742 2 -12 3 -9 2198.96 96.9476 2 -12 3 -10 484.519 116.541 2 12 -4 -20 572.641 222.809 2 12 -4 -18 5331.63 314.181 2 12 -4 -17 3555.65 136.298 2 12 4 -16 2007.41 106.023 2 12 4 -15 53.0528 82.048 2 -12 4 14 22405.8 144.314 2 -12 4 13 25155.4 166.457 2 -12 4 12 5934.23 121.665 2 -12 4 11 3834.83 89.2507 2 12 -4 -10 2087.84 76.3805 2 -12 4 9 15366.8 112.553 2 -12 4 8 13147.3 104.829 2 -12 4 7 255.085 77.6478 2 -12 4 6 13214.5 401.608 2 -12 -4 -5 2634.35 138.785 2 -12 4 -6 6468.51 133.512 2 -12 -4 -7 402.877 78.9698 2 -12 4 -8 21.0412 15.2809 2 -12 4 -9 1034.04 78.8123 2 12 -5 -20 259.565 199.21 2 -12 5 19 166.14 166.474 2 -12 -5 18 65.0444 141.609 2 12 -5 -17 379.536 108.379 2 12 5 -16 16447.1 152.729 2 -12 5 15 20774.7 140.415 2 -12 5 14 2233.1 81.5608 2 -12 5 13 2698.97 84.9839 2 12 5 -12 198.327 71.1101 2 -12 5 11 19008.4 121.734 2 12 5 -10 5285.07 83.3621 2 -12 5 9 6072.63 96.18 2 -12 5 8 21705.8 160.239 2 -12 5 7 6591.3 113.658 2 -12 5 6 5441.67 238.401 2 -12 -5 -5 403.895 102.487 2 -12 5 -6 7282.59 113.711 2 -12 5 -7 256.799 73.5433 2 -12 5 -8 33.1787 12.9417 2 12 5 9 832.148 119.473 2 12 -6 -20 230.865 169.62 2 -12 6 18 7.12622 21.6622 2 -12 6 17 1516.75 151.361 2 12 6 -16 145.16 74.6723 2 -12 6 15 1882.23 76.5704 2 -12 6 14 6138.27 91.9655 2 12 -6 -13 41303 206.217 2 -12 6 12 6206.74 109.511 2 -12 6 11 124.258 89.1387 2 -12 6 10 1162.1 92.807 2 -12 6 9 41397.9 225.654 2 -12 6 8 5327.4 134.998 2 -12 6 7 5920.07 164.7 2 -12 -6 -5 342.423 110.934 2 -12 6 -6 50.9434 29.5481 2 -12 6 -7 468.891 78.8162 2 -12 6 -8 -2.72283 10.108 2 12 -7 -20 2001.62 149.259 2 12 7 -18 141.028 113.318 2 12 -7 -17 769.343 229.932 2 -12 7 16 320.32 158.04 2 -12 7 15 4068.3 145.969 2 -12 7 14 1572.94 114.474 2 12 7 -13 43.0846 94.5856 2 -12 7 12 231.149 114.389 2 -12 7 11 6244.8 126.311 2 -12 7 10 2954.82 111.43 2 -12 7 9 102.039 129.437 2 -12 7 8 1957.87 133.578 2 -12 7 7 3682.72 179.423 2 -12 -7 -5 1462.21 97.9272 2 -12 7 -6 2609.47 108.704 2 -12 7 -7 1281.87 72.3023 2 12 7 8 331.948 57.8631 2 12 -8 -17 1860.06 215.238 2 12 -8 -16 800.383 242.286 2 -12 8 15 5300.82 202.076 2 -12 8 14 3151.47 141.262 2 -12 8 13 431.513 95.2913 2 -12 8 12 3063.2 116.289 2 -12 8 11 1367.79 133.924 2 -12 8 10 622.94 108.967 2 -12 8 9 6693.65 149.976 2 -12 8 8 16861.5 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160.41 55.8168 2 19 3 -17 190.691 67.118 2 -19 3 16 1029.77 79.046 2 -19 -3 15 492.666 81.0002 2 19 3 -14 825.408 93.1636 2 -19 3 13 6674.57 124.108 2 -19 3 12 263.63 146.212 2 -19 3 11 453.48 148.964 2 -19 3 10 1254.97 154.863 2 -19 3 9 2271.81 162.007 2 -19 3 8 962.36 154.834 2 -19 3 7 465.541 147.119 2 19 3 -6 183.223 90.2552 2 19 3 -5 280.209 82.96 2 -19 -3 4 5978.39 221.859 2 19 -4 -18 26.8738 350.079 2 19 4 -17 6.73583 15.7764 2 19 -4 -16 1079.31 52.6771 2 -19 4 15 1248.15 61.4695 2 -19 4 14 1570.61 88.9366 2 -19 4 13 2178.36 99.9577 2 -19 4 12 345.581 129.165 2 -19 4 11 1120.02 137.751 2 -19 4 10 58.2405 132.732 2 -19 4 9 -134.02 130.239 2 -19 4 8 21.8274 130.827 2 19 4 -7 2567.39 102.873 2 19 4 -6 3383.67 100.355 2 19 4 -5 308.495 81.1743 2 19 4 -4 217.31 94.2089 2 19 5 -16 1195.88 60.8867 2 19 5 -15 10.0607 8.50777 2 19 5 -14 -0.93847 12.435 2 -19 5 13 4185.48 117.745 2 -19 5 12 210.552 103.428 2 -19 5 11 5011.49 103.124 2 -19 5 10 130.247 110.34 2 -19 5 9 1381.2 117.171 2 19 5 -8 1999.99 91.7271 2 19 5 -7 190.935 80.4028 2 19 5 -6 129.827 75.7688 2 19 5 -5 231.278 84.3333 2 19 5 -4 1022.09 100.616 2 19 6 -15 484.142 90.0501 2 19 6 -14 2189.62 117.72 2 19 6 -13 563.506 115.708 2 19 6 -12 1896.59 134.307 2 -19 6 11 3495.98 129.676 2 -19 6 10 628.692 131.048 2 -19 6 9 1336.04 147.444 2 -19 6 8 468.597 147.563 2 -19 6 7 1215.96 75.4058 2 -19 6 6 8.86218 70.7955 2 -19 6 5 229.095 80.3924 2 -19 6 4 188.551 71.027 2 19 7 -15 754.591 71.4603 2 19 7 -14 1202.79 91.4651 2 19 7 -13 1096.55 101.266 2 19 7 -12 16.2877 102.026 2 19 7 -11 195.015 110.173 2 19 7 -10 322.643 75.8223 2 -19 7 9 1691.01 122.701 2 -19 7 8 228.731 121.401 2 -19 7 7 1360.88 127.603 2 -19 7 6 128.165 56.7201 2 -19 7 5 335.603 54.2455 2 -19 7 4 69.0163 57.802 2 19 8 -14 61.3545 53.3125 2 19 8 -13 98.3003 68.035 2 19 8 -12 223.174 74.6583 2 19 8 -11 1204.57 89.9315 2 -19 8 9 1007.67 293.398 2 19 8 -8 82.5131 58.8874 2 -19 8 7 455.871 59.3004 2 19 8 -6 395.469 54.458 2 -19 8 5 1056.41 80.4087 2 -20 0 18 441.408 135.296 2 -20 0 17 508.919 156.439 2 -20 0 16 1828.58 184.296 2 -20 0 15 -25.8428 176.883 2 -20 0 14 7106.87 250.066 2 -20 0 13 1040.81 211.007 2 -20 0 12 131.687 200.994 2 -20 0 11 6493.07 262.937 2 -20 0 10 63.9044 211.365 2 -20 0 9 10120.4 288.213 2 -20 0 8 14903.5 319.416 2 -20 0 7 10115.7 277.606 2 -20 0 6 1363.78 192.484 2 -20 0 5 983.308 183.138 2 -20 0 4 1338.27 176.493 2 20 1 -19 259.108 56.23 2 -20 -1 18 2861.44 73.2714 2 20 1 -17 572.162 76.9255 2 -20 -1 16 394.251 165.057 2 -20 -1 15 1053.93 189.166 2 -20 -1 14 598.657 193.6 2 -20 -1 13 1624.85 211.03 2 -20 -1 12 3886.99 229.184 2 -20 -1 11 6433.51 255.21 2 -20 -1 10 2502.72 227.283 2 -20 -1 9 16460.4 324.871 2 -20 -1 8 155.076 202.712 2 -20 -1 7 642.633 206.666 2 -20 -1 6 1580.24 191.243 2 -20 -1 5 3460.87 198.85 2 -20 -1 4 412.115 167.385 2 20 -2 -19 2750.92 82.923 2 20 2 -18 488.261 50.4524 2 20 2 -17 658.063 63.7733 2 -20 2 16 373.009 83.3821 2 -20 2 15 167.975 120.933 2 -20 2 14 327.767 127.775 2 -20 2 13 7956.75 175.393 2 -20 2 12 462.439 140.053 2 -20 2 11 4312.74 162.868 2 -20 2 10 61.4238 138.775 2 -20 2 9 4919.45 168.902 2 -20 2 8 1537.61 147.325 2 -20 2 7 7330.08 170.732 2 -20 2 6 1208.71 128.857 2 -20 2 5 491.414 118.82 2 -20 2 4 144.542 110.45 2 20 -3 -18 166.986 72.3784 2 -20 3 17 2593.5 60.5898 2 -20 3 16 2472.94 68.7147 2 -20 3 15 7583.39 146.467 2 -20 3 14 358.072 73.4789 2 -20 3 13 1246.9 86.0227 2 -20 3 12 220.299 125.18 2 -20 3 11 9337.58 175.873 2 -20 3 10 803.702 133.782 2 -20 3 9 4435.08 154.564 2 -20 3 8 3057.07 143.515 2 -20 3 7 276.746 115.882 2 -20 3 6 225.625 111.762 2 -20 3 5 707.682 107.468 2 -20 3 4 515.16 101.612 2 20 4 -16 -1.53396 11.1656 2 -20 4 15 24.6614 15.1533 2 -20 4 14 3888.47 81.2128 2 -20 4 13 11289.6 112.802 2 -20 4 12 835.752 109.893 2 -20 4 11 170.209 108.106 2 -20 4 10 1379.98 116.025 2 -20 4 9 565.684 109.195 2 -20 4 8 197.361 104.236 2 -20 4 7 682.678 105.702 2 -20 4 6 974.596 101.409 2 -20 4 5 1498.95 97.7996 2 -20 4 4 -5.9123 117.263 2 -20 4 3 1011.97 99.9907 2 20 5 -15 5124.22 92.7618 2 20 5 -14 223.798 55.3195 2 20 5 -13 171.696 99.1868 2 -20 5 12 69.5572 21.2631 2 -20 5 11 92.5139 20.566 2 -20 5 10 -2.31763 20.4984 2 -20 5 9 3.85127 19.9438 2 -20 5 8 29.6318 20.7805 2 -20 5 7 262.698 98.5053 2 -20 5 6 115.17 79.0624 2 -20 5 5 807.735 116.241 2 -20 5 3 3717.52 94.9963 2 20 6 -14 1082.52 77.838 2 20 6 -13 3070.47 102.139 2 20 6 -12 1051.36 100.19 2 20 6 -11 4.14058 97.6495 2 -20 6 10 -98.9396 91.1889 2 -20 6 9 1649.71 114.762 2 -20 6 8 421.894 109.052 2 -20 6 7 401.548 105.711 2 -20 6 6 -14.0084 98.5749 2 -20 6 5 1570.09 98.1634 2 20 7 -13 317.927 61.3895 2 20 7 -12 42.8693 68.4237 2 20 7 -11 1470.4 87.5951 2 20 7 -10 264.349 81.9041 2 20 7 -9 483.113 84.4892 2 -20 7 8 -80.1647 75.8407 2 -20 7 7 608.091 78.7307 2 -20 7 6 1048.23 72.6185 2 -21 0 17 85.7279 119.421 2 -21 0 16 -70.4281 132.428 2 -21 0 15 -15.1621 149.272 2 -21 0 14 120.01 157.055 2 -21 0 13 143.76 162.84 2 -21 0 12 279.406 171.995 2 -21 0 11 139.441 168.362 2 -21 0 10 -170.081 169.585 2 -21 0 9 -62.9526 171.89 2 -21 0 8 292.751 160.21 2 -21 0 7 546.596 155.248 2 -21 0 6 218.105 143.623 2 -21 0 5 86.2862 136.729 2 -21 0 4 -131.915 116.361 2 21 1 -18 -16.9663 45.4629 2 -21 -1 17 1240.51 59.3451 2 21 1 -16 235.154 63.7138 2 -21 -1 15 268.382 143.001 2 -21 -1 14 60.2627 151.711 2 -21 -1 13 1091.27 170.748 2 -21 -1 12 8.63943 167.049 2 -21 -1 11 85.1381 170.131 2 -21 -1 10 390.902 173.319 2 -21 -1 9 78.2235 167.151 2 -21 -1 8 361.009 157.862 2 -21 -1 7 1857.03 163.972 2 -21 -1 6 314.39 145.812 2 -21 -1 5 318.72 128.03 2 -21 -1 4 -108.164 117.425 2 21 -2 -17 66.5724 53.1093 2 21 2 -16 73.2031 50.9901 2 -21 2 15 59.8371 96.888 2 -21 2 14 156.286 99.8708 2 -21 2 13 4727 134.167 2 -21 2 12 202.058 112.373 2 -21 2 11 246.393 114.96 2 -21 2 10 113.015 112.404 2 -21 2 9 3794.35 132.234 2 -21 2 8 639.24 107.455 2 -21 2 7 304.33 100.495 2 -21 2 6 125.773 93.5938 2 -21 2 5 37.8124 84.1812 2 21 3 -16 68.564 50.1953 2 21 3 -15 172.137 54.7496 2 -21 3 14 589.686 91.5777 2 -21 3 13 105.606 95.2257 2 -21 3 12 388.906 66.3981 2 -21 3 11 2263.69 112.431 2 -21 3 10 -110.637 99.0963 2 -21 3 9 2127.04 108.087 2 -21 3 8 126.019 91.8908 2 -21 -3 7 863.976 93.6304 2 -21 3 6 73.0734 76.2798 2 21 -4 -14 147.753 347.228 2 21 4 -13 3391.8 89.5291 2 -21 4 12 1023.26 72.2016 2 -21 4 11 164.01 69.5573 2 -21 4 10 369.391 77.0903 2 -21 4 9 323.84 114.801 2 -21 4 6 281.603 58.6245 2 -21 4 5 156.899 78.1144 2 21 5 -13 789.419 64.7525 2 21 5 -12 370.608 73.4235 2 21 5 -11 386.689 80.6674 2 -21 5 10 38.4947 289.821 2 -21 5 9 317.608 84.9207 2 -21 5 8 97.3596 87.0441 2 -21 5 7 412.441 84.0889 2 -21 5 6 24.8907 71.6219 2 21 6 -11 144.85 58.3634 2 21 6 -10 274.973 63.0465 2 21 6 -9 167.665 60.3173 2 21 6 -8 132.639 57.6942 2 -22 0 14 344.778 114.386 2 -22 0 13 1775.73 141.688 2 -22 0 12 117.891 129.431 2 -22 0 11 3532.36 157.286 2 -22 0 10 1066.4 135.11 2 -22 0 9 594.018 125.261 2 -22 0 8 1487.07 122.931 2 -22 0 7 627.949 107.29 2 22 1 -16 44.2359 43.1528 2 22 1 -15 1858.79 60.0407 2 -22 -1 14 126.235 107.435 2 -22 -1 13 2405.89 133.723 2 -22 -1 12 91.431 127.796 2 -22 -1 11 80.2294 122.479 2 -22 -1 10 1530.89 127.274 2 -22 -1 9 5110.47 148.62 2 -22 -1 8 266.691 106.987 2 22 -2 -15 985.099 71.4904 2 -22 2 13 3498.59 137.37 2 -22 2 12 31.7259 80.9745 2 -22 2 11 2526.7 92.9926 2 -22 2 10 198.415 76.8515 2 -22 2 9 672.324 75.9168 2 -22 3 9 506.552 76.536 2 -22 3 8 239.947 71.732 2 -22 3 7 1345.2 72.0566 2 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 Cl03 Mn01 Cl06 111.10(7) . . ? Cl09 Mn01 Cl03 109.17(8) . . ? Cl09 Mn01 Cl06 108.20(8) . . ? Cl0A Mn01 Cl03 111.57(8) . . ? Cl0A Mn01 Cl06 107.55(8) . . ? Cl0A Mn01 Cl09 109.17(9) . . ? C1_1 N1_1 C3_1 107.7(5) . . ? C2_1 N1_1 C1_1 109.7(6) . . ? C2_1 N1_1 C3_1 108.8(5) . . ? C4_1 N1_1 C1_1 108.5(5) . . ? C4_1 N1_1 C2_1 108.6(5) . . ? C4_1 N1_1 C3_1 113.5(5) . . ? C5_1 C4_1 N1_1 123.1(5) . . ? C1_2 N1_2 C2_2 107.1(6) . . ? C3_2 N1_2 C1_2 109.6(7) . . ? C3_2 N1_2 C2_2 109.4(7) . . ? C3_2 N1_2 C4_2 116.0(7) . . ? C4_2 N1_2 C1_2 107.3(7) . . ? C4_2 N1_2 C2_2 107.1(6) . . ? C5_2 C4_2 N1_2 122.6(9) . . ? C1_3 N1_3 C2_3 106.9(8) . . ? C1_3 N1_3 C4_3 107.2(7) . . ? C3_3 N1_3 C1_3 111.2(10) . . ? C3_3 N1_3 C2_3 109.5(9) . . ? C3_3 N1_3 C4_3 113.0(6) . . ? C4_3 N1_3 C2_3 108.8(6) . . ? C5_3 C4_3 N1_3 123.0(6) . . ? C1_4 N1_4 C2_4 105.6(7) . . ? C3_4 N1_4 C1_4 109.6(7) . . ? C3_4 N1_4 C2_4 107.6(7) . . ? C4_4 N1_4 C1_4 108.3(7) . . ? C4_4 N1_4 C2_4 107.5(8) . . ? C4_4 N1_4 C3_4 117.5(7) . . ? C5_4 C4_4 N1_4 127.6(9) . . ? Cl2_5 Mn1_5 Cl3_5 107.54(7) . . ? Cl2_5 Mn1_5 Cl1_5 107.99(8) . . ? Cl4_5 Mn1_5 Cl2_5 112.97(9) . . ? Cl4_5 Mn1_5 Cl3_5 109.29(7) . . ? Cl4_5 Mn1_5 Cl1_5 109.12(8) . . ? Cl1_5 Mn1_5 Cl3_5 109.89(8) . . ? 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 Mn01 Cl03 2.3701(18) . ? Mn01 Cl06 2.375(2) . ? Mn01 Cl09 2.3619(18) . ? Mn01 Cl0A 2.3526(18) . ? N1_1 C1_1 1.490(8) . ? N1_1 C2_1 1.484(8) . ? N1_1 C3_1 1.499(7) . ? N1_1 C4_1 1.468(7) . ? C4_1 C5_1 1.304(7) . ? N1_2 C1_2 1.490(9) . ? N1_2 C2_2 1.504(9) . ? N1_2 C3_2 1.460(9) . ? N1_2 C4_2 1.461(9) . ? C4_2 C5_2 1.299(9) . ? N1_3 C1_3 1.471(10) . ? N1_3 C2_3 1.480(10) . ? N1_3 C3_3 1.456(9) . ? N1_3 C4_3 1.474(8) . ? C4_3 C5_3 1.294(8) . ? N1_4 C1_4 1.488(10) . ? N1_4 C2_4 1.503(10) . ? N1_4 C3_4 1.474(9) . ? N1_4 C4_4 1.441(10) . ? C4_4 C5_4 1.281(9) . ? Mn1_5 Cl2_5 2.3528(19) . ? Mn1_5 Cl3_5 2.3613(17) . ? Mn1_5 Cl4_5 2.3441(19) . ? Mn1_5 Cl1_5 2.3581(18) . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.5019(15) 14551 13490 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4981(15) 14628 13490 nmt 0.9997 0.0001 0.9696 -0.0001 -0.9999 0.0001 0.0007 -0.0003 -0.9997