#------------------------------------------------------------------------------ #$Date: 2021-01-13 07:12:41 +0200 (Wed, 13 Jan 2021) $ #$Revision: 260910 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/20/7242063.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_7242063 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_sum 'C10 H24 Br4 Mn N2' _chemical_formula_weight 546.89 _chemical_properties_physical Moisture-sensitive,Heat-sensitive _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-07-31 deposited with the CCDC. 2020-12-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.4500(3) _cell_length_b 9.1134(2) _cell_length_c 16.4176(5) _cell_measurement_reflns_used 3427 _cell_measurement_temperature 223(2) _cell_measurement_theta_max 70.3380 _cell_measurement_theta_min 4.2390 _cell_volume 2012.39(9) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 223(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.943 _diffrn_measurement_device_type 'ROD, Synergy Custom DW system, HyPix' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.943 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 7663 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.943 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 76.943 _diffrn_reflns_theta_min 4.249 _exptl_absorpt_coefficient_mu 14.522 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.07347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.805 _exptl_crystal_description block _exptl_crystal_F_000 1052 _exptl_crystal_preparation 'Magnetic properties,Luminescent' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.238 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 96 _refine_ls_number_reflns 2135 _refine_ls_number_restraints 113 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.1182 _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^)+(0.0800P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2712 _refine_ls_wR_factor_ref 0.2835 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1372 _reflns_number_total 2135 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ra08795e2.cif _cod_data_source_block Pnma _cod_original_cell_volume 2012.40(9) _cod_database_code 7242063 _shelx_shelxl_version_number 2018/3 _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_estimated_absorpt_t_min 0.325 _shelx_estimated_absorpt_t_max 0.476 _shelx_res_file ; TITL Pnma in Pnma Pnma.res created by SHELXL-2018/3 at 18:08:56 on 27-Jul-2020 CELL 1.54178 13.45000 9.11344 16.41763 90.0000 90.0000 90.0000 ZERR 4 0.00029 0.00020 0.00054 0.0000 0.0000 0.0000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, 0.5-Z SYMM -X, 0.5+Y, -Z SFAC C H N MN BR UNIT 40 96 8 4 16 LIST 4 MERG 2 FMAP 2 EQIV $1 +x, 1/2-y, +z PLAN 5 TEMP -50 SIZE 0.1 0.1 0.06 BOND ISOR $C DFIX 1.52 N1 C3 DFIX 1.28 C4 C3 DFIX 2.46 N1 C4 DFIX 1.52 N2 C7 DFIX 1.28 C7 C8 DFIX 2.46 N2 C8 DFIX 1.52 N1 C1 N1 C2 DFIX 1.52 N2 C5 N2 C6 DFIX 2.42 0.01 C1 C2 C2 C3 C1 C3 C5 C6 C6 C7 C5 C7 C1 C1_$1 OMIT 9 0 1 L.S. 20 simu 0.01 0.02 2 omit 2 1 0 omit 2 3 0 ACTA WGHT 0.080000 15.000000 FVAR 0.09281 MN1 4 0.248509 0.250000 0.601116 10.50000 0.07585 0.08882 = 0.11752 0.00000 0.00724 0.00000 BR2 5 0.186413 0.250000 0.457447 10.50000 0.14564 0.18000 = 0.14012 0.00000 -0.00171 0.00000 BR3 5 0.432251 0.250000 0.607826 10.50000 0.07721 0.17471 = 0.24236 0.00000 0.00473 0.00000 BR1 5 0.187645 0.022991 0.666802 11.00000 0.16023 0.13685 = 0.20370 0.05482 0.01243 -0.02755 N2 3 0.507141 0.250000 0.347762 10.50000 0.16196 0.16418 = 0.17956 0.00000 0.00839 0.00000 C8 1 0.632013 0.250000 0.240906 10.50000 0.24596 0.21504 = 0.23540 0.00000 0.01758 0.00000 AFIX 93 H8A 2 0.682877 0.250000 0.280172 10.50000 -1.20000 H8B 2 0.648089 0.250000 0.185186 10.50000 -1.20000 AFIX 0 N1 3 0.872911 0.250000 0.590073 10.50000 0.10402 0.24792 = 0.31502 0.00000 -0.01497 0.00000 C3 1 0.763119 0.250000 0.588661 10.50000 0.11679 0.26161 = 0.32169 0.00000 -0.00696 0.00000 AFIX 43 H3 2 0.734529 0.250000 0.536415 10.50000 -1.20000 AFIX 0 C6 1 0.591938 0.250000 0.405543 10.50000 0.18536 0.23563 = 0.17793 0.00000 -0.00515 0.00000 part -1 AFIX 33 H6A 2 0.566940 0.250000 0.460963 10.50000 -1.50000 H6B 2 0.632160 0.163095 0.396723 10.50000 -1.50000 H6C 2 0.632160 0.336905 0.396724 10.50000 -1.50000 AFIX 0 part 0 C5 1 0.449578 0.108591 0.361939 11.00000 0.24091 0.17738 = 0.22934 -0.01299 0.00208 -0.04038 AFIX 137 H5A 2 0.495112 0.026066 0.361106 11.00000 -1.50000 H5B 2 0.400305 0.096530 0.319319 11.00000 -1.50000 H5C 2 0.416615 0.113015 0.414432 11.00000 -1.50000 AFIX 0 C1 1 0.910945 0.117232 0.630976 11.00000 0.16453 0.24494 = 0.35393 0.03789 -0.01663 0.00035 AFIX 137 H1A 2 0.961118 0.144846 0.670552 11.00000 -1.50000 H1B 2 0.940047 0.051999 0.590837 11.00000 -1.50000 H1C 2 0.856675 0.067559 0.658431 11.00000 -1.50000 AFIX 0 C2 1 0.908576 0.250000 0.503094 10.50000 0.12370 0.29180 = 0.30724 0.00000 0.01108 0.00000 part -1 AFIX 33 H2A 2 0.883998 0.163101 0.475554 10.50000 -1.50000 H2B 2 0.884011 0.336911 0.475558 10.50000 -1.50000 H2C 2 0.980686 0.249988 0.502164 10.50000 -1.50000 AFIX 0 part 0 C4 1 0.703818 0.250000 0.644932 10.50000 0.15684 0.29704 = 0.35110 0.00000 -0.00326 0.00000 AFIX 93 H4A 2 0.726795 0.250000 0.699005 10.50000 -1.20000 H4B 2 0.635168 0.250000 0.634198 10.50000 -1.20000 AFIX 0 C7 1 0.542040 0.250000 0.263022 10.50000 0.17736 0.17502 = 0.19767 0.00000 0.01537 0.00000 AFIX 43 H7 2 0.493466 0.250000 0.221856 10.50000 -1.20000 AFIX 0 HKLF 4 REM Pnma in Pnma REM wR2 = 0.283501, GooF = S = 1.05075, Restrained GooF = 1.05746 for all data REM R1 = 0.118189 for 1372 Fo > 4sig(Fo) and 0.141681 for all 2135 data REM 96 parameters refined using 113 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.238, deepest hole -0.798, 1-sigma level 0.166 Q1 1 0.6602 0.2500 0.7640 10.50000 0.05 0.81 Q2 1 0.2099 0.0551 0.5239 11.00000 0.05 0.80 Q3 1 0.2406 0.1672 0.4754 11.00000 0.05 0.77 Q4 1 0.2602 0.1912 0.4635 11.00000 0.05 0.74 Q5 1 0.1733 0.1293 0.7172 11.00000 0.05 0.68 ; _shelx_res_checksum 64057 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.24851(18) 0.250000 0.60112(17) 0.0941(9) Uani 1 2 d S T P . . Br2 Br 0.1864(2) 0.250000 0.45745(17) 0.1553(12) Uani 1 2 d S T P . . Br3 Br 0.43225(16) 0.250000 0.6078(2) 0.1648(13) Uani 1 2 d S T P . . Br1 Br 0.18765(16) 0.0230(2) 0.66680(14) 0.1669(10) Uani 1 1 d . . . . . N2 N 0.5071(15) 0.250000 0.3478(10) 0.169(6) Uani 1 2 d DS TU P . . C8 C 0.632(2) 0.250000 0.2409(19) 0.232(10) Uani 1 2 d DS TU P . . H8A H 0.682877 0.250000 0.280172 0.279 Uiso 1 2 calc R U P . . H8B H 0.648089 0.250000 0.185186 0.279 Uiso 1 2 calc R U P . . N1 N 0.8729(12) 0.250000 0.5901(13) 0.222(8) Uani 1 2 d DS TU P . . C3 C 0.7631(11) 0.250000 0.5887(16) 0.233(9) Uani 1 2 d DS TU P . . H3 H 0.734529 0.250000 0.536415 0.280 Uiso 1 2 calc R U P . . C6 C 0.5919(16) 0.250000 0.4055(12) 0.200(9) Uani 1 2 d DS TU P . . H6A H 0.566940 0.250000 0.460963 0.299 Uiso 0.5 1 calc R U P A -1 H6B H 0.632160 0.163095 0.396723 0.299 Uiso 0.5 1 calc R U P A -1 H6C H 0.632160 0.336905 0.396724 0.299 Uiso 0.5 1 calc R U P A -1 C5 C 0.4496(14) 0.109(2) 0.3619(11) 0.216(8) Uani 1 1 d D U . . . H5A H 0.495112 0.026066 0.361106 0.324 Uiso 1 1 calc R U . . . H5B H 0.400305 0.096530 0.319319 0.324 Uiso 1 1 calc R U . . . H5C H 0.416615 0.113015 0.414432 0.324 Uiso 1 1 calc R U . . . C1 C 0.9109(13) 0.1172(5) 0.6310(12) 0.254(10) Uani 1 1 d D U . . . H1A H 0.961118 0.144846 0.670552 0.382 Uiso 1 1 calc R U . . . H1B H 0.940047 0.051999 0.590837 0.382 Uiso 1 1 calc R U . . . H1C H 0.856675 0.067559 0.658431 0.382 Uiso 1 1 calc R U . . . C2 C 0.9086(18) 0.250000 0.5031(12) 0.241(11) Uani 1 2 d DS TU P . . H2A H 0.883998 0.163101 0.475554 0.361 Uiso 0.5 1 calc R U P B -1 H2B H 0.884011 0.336911 0.475558 0.361 Uiso 0.5 1 calc R U P B -1 H2C H 0.980686 0.249988 0.502164 0.361 Uiso 0.5 1 calc R U P B -1 C4 C 0.7038(19) 0.250000 0.645(2) 0.268(12) Uani 1 2 d DS TU P . . H4A H 0.726795 0.250000 0.699005 0.322 Uiso 1 2 calc R U P . . H4B H 0.635168 0.250000 0.634198 0.322 Uiso 1 2 calc R U P . . C7 C 0.5420(18) 0.250000 0.2630(10) 0.183(7) Uani 1 2 d DS TU P . . H7 H 0.493466 0.250000 0.221856 0.220 Uiso 1 2 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0758(15) 0.0888(17) 0.118(2) 0.000 0.0072(14) 0.000 Br2 0.146(2) 0.180(3) 0.140(2) 0.000 -0.0017(16) 0.000 Br3 0.0772(12) 0.175(3) 0.242(3) 0.000 0.0047(16) 0.000 Br1 0.1602(17) 0.1368(15) 0.204(2) 0.0548(14) 0.0124(14) -0.0276(12) N2 0.162(14) 0.164(11) 0.180(12) 0.000 0.008(11) 0.000 C8 0.25(2) 0.215(18) 0.24(2) 0.000 0.02(2) 0.000 N1 0.104(10) 0.248(19) 0.32(2) 0.000 -0.015(13) 0.000 C3 0.117(12) 0.26(2) 0.32(2) 0.000 -0.007(14) 0.000 C6 0.185(19) 0.236(19) 0.178(18) 0.000 -0.005(16) 0.000 C5 0.241(19) 0.177(15) 0.229(16) -0.013(14) 0.002(15) -0.040(14) C1 0.165(14) 0.24(2) 0.35(3) 0.038(16) -0.017(17) 0.000(14) C2 0.124(15) 0.29(2) 0.31(3) 0.000 0.011(18) 0.000 C4 0.157(19) 0.30(3) 0.35(3) 0.000 0.00(2) 0.000 C7 0.177(15) 0.175(12) 0.198(14) 0.000 0.015(13) 0.000 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' Br Br -0.6763 1.2805 '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 Br1 113.60(15) 8_565 . ? Br1 Mn1 Br3 108.14(9) 8_565 . ? Br1 Mn1 Br3 108.14(9) . . ? Br1 Mn1 Br2 107.50(10) 8_565 . ? Br1 Mn1 Br2 107.50(10) . . ? Br3 Mn1 Br2 112.05(15) . . ? C7 N2 C6 111.1(12) . . ? C7 N2 C5 107.9(9) . . ? C6 N2 C5 107.1(9) . . ? C7 N2 C5 107.9(9) . 8_565 ? C6 N2 C5 107.1(9) . 8_565 ? C5 N2 C5 116(2) . 8_565 ? C1 N1 C1 110.2(13) 8_565 . ? C1 N1 C3 110.7(8) 8_565 . ? C1 N1 C3 110.7(8) . . ? C1 N1 C2 108.7(8) 8_565 . ? C1 N1 C2 108.7(8) . . ? C3 N1 C2 107.7(12) . . ? C4 C3 N1 130(2) . . ? C8 C7 N2 125(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Br1 2.472(2) 8_565 ? Mn1 Br1 2.472(2) . ? Mn1 Br3 2.474(3) . ? Mn1 Br2 2.502(4) . ? N2 C7 1.468(15) . ? N2 C6 1.483(16) . ? N2 C5 1.521(12) . ? N2 C5 1.521(12) 8_565 ? C8 C7 1.263(17) . ? N1 C1 1.475(11) 8_565 ? N1 C1 1.475(11) . ? N1 C3 1.477(15) . ? N1 C2 1.506(17) . ? C3 C4 1.221(18) . ?