#------------------------------------------------------------------------------
#$Date: 2020-02-29 01:43:40 +0200 (Sat, 29 Feb 2020) $
#$Revision: 248537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/42/4134270.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_4134270
loop_
_publ_author_name
'Gao, Ji-Xing'
'Zhang, Wan-Ying'
'Wu, Zheng-Guang'
'Zheng, You-Xuan'
'Fu, Da-Wei'
_publ_section_title
;
 Enantiomorphic Perovskite Ferroelectrics with Circularly Polarized
 Luminescence.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13291
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'Br3 Mn, C4 H9 F N'
_chemical_formula_sum            'C4 H9 Br3 F Mn N'
_chemical_formula_weight         384.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.669(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8558(4)
_cell_length_b                   6.7422(3)
_cell_length_c                   9.7844(5)
_cell_measurement_reflns_used    3447
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.3300
_cell_measurement_theta_min      2.8200
_cell_volume                     474.64(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    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5357
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.981
_diffrn_reflns_theta_max         24.981
_diffrn_reflns_theta_min         2.831
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    13.965
_exptl_absorpt_correction_T_max  0.075
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_description       Prism
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.255
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1661
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1233P)²+6.5174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.1968
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1462
_reflns_number_total             1661
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b13291_si_002.cif
_cod_data_source_block           P21
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4134270
_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_estimated_absorpt_t_min   0.157
_shelx_estimated_absorpt_t_max   0.167
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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 0.9967(4) 1.0018(4) 1.0015(4) 0.0285(4) Uani 1 1 d . . . . .
Br1 Br 1.17810(13) 0.7513(3) 0.88610(11) 0.0357(2) Uani 1 1 d . . . . .
Br2 Br 1.11878(14) 0.7462(3) 1.23681(11) 0.0373(3) Uani 1 1 d . . . . .
Br3 Br 0.70912(12) 0.7515(3) 0.89136(12) 0.0360(3) Uani 1 1 d . . . . .
N1 N 0.3608(16) 0.1459(10) 0.7678(8) 0.047(3) Uani 1 1 d D U . . .
H1A H 0.4601 0.0909 0.8409 0.056 Uiso 1 1 calc R U . . .
H1B H 0.2621 0.1339 0.7920 0.056 Uiso 1 1 calc R U . . .
C1 C 0.323(2) 0.0449(13) 0.6225(7) 0.070(5) Uani 1 1 d D U . . .
H1C H 0.2264 -0.0563 0.6022 0.084 Uiso 1 1 calc R U . . .
H1D H 0.4359 -0.0186 0.6240 0.084 Uiso 1 1 calc R U . . .
C2 C 0.2592(11) 0.2054(11) 0.5066(8) 0.084(5) Uani 1 1 d D U . . .
H2 H 0.1413 0.1810 0.4192 0.101 Uiso 1 1 calc R U . . .
C3 C 0.273(3) 0.3970(14) 0.5891(9) 0.095(6) Uani 1 1 d D U . . .
H3A H 0.3245 0.5015 0.5475 0.115 Uiso 1 1 calc R U . . .
H3B H 0.1494 0.4389 0.5804 0.115 Uiso 1 1 calc R U . . .
F1 F 0.4149(10) 0.198(3) 0.4826(12) 0.202(9) Uani 1 1 d D U . . .
C4 C 0.3975(16) 0.3605(11) 0.7495(9) 0.036(3) Uani 1 1 d D U . . .
H4A H 0.3639 0.4450 0.8163 0.043 Uiso 1 1 calc R U . . .
H4B H 0.5282 0.3829 0.7680 0.043 Uiso 1 1 calc R U . . .
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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
Br1 Mn1 Br3 94.15(10) 2_757 . ?
Br1 Mn1 Br2 85.48(9) 2_757 2_757 ?
Br3 Mn1 Br2 95.77(10) . 2_757 ?
Br1 Mn1 Br3 87.08(10) 2_757 2_757 ?
Br3 Mn1 Br3 178.70(16) . 2_757 ?
Br2 Mn1 Br3 83.89(10) 2_757 2_757 ?
Br1 Mn1 Br2 96.60(12) 2_757 . ?
Br3 Mn1 Br2 83.98(10) . . ?
Br2 Mn1 Br2 177.91(15) 2_757 . ?
Br3 Mn1 Br2 96.31(9) 2_757 . ?
Br1 Mn1 Br1 179.20(15) 2_757 . ?
Br3 Mn1 Br1 86.54(10) . . ?
Br2 Mn1 Br1 94.06(12) 2_757 . ?
Br3 Mn1 Br1 92.23(10) 2_757 . ?
Br2 Mn1 Br1 83.86(9) . . ?
Mn1 Br1 Mn1 77.25(3) 2_747 . ?
Mn1 Br2 Mn1 76.92(3) 2_747 . ?
Mn1 Br3 Mn1 77.57(2) . 2_747 ?
C1 N1 C4 107.4(7) . . ?
N1 C1 C2 105.6(7) . . ?
F1 C2 C1 93.1(10) . . ?
F1 C2 C3 104.7(14) . . ?
C1 C2 C3 106.5(7) . . ?
C4 C3 C2 107.2(7) . . ?
C3 C4 N1 102.0(7) . . ?
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 2.672(4) 2_757 ?
Mn1 Br3 2.676(3) . ?
Mn1 Br2 2.697(3) 2_757 ?
Mn1 Br3 2.707(3) 2_757 ?
Mn1 Br2 2.724(3) . ?
Mn1 Br1 2.729(4) . ?
Br1 Mn1 2.672(4) 2_747 ?
Br2 Mn1 2.697(3) 2_747 ?
Br3 Mn1 2.707(3) 2_747 ?
N1 C1 1.495(9) . ?
N1 C4 1.500(9) . ?
C1 C2 1.500(9) . ?
C2 F1 1.336(10) . ?
C2 C3 1.504(10) . ?
C3 C4 1.499(9) . ?
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
C4 N1 C1 C2 -23.2(13) . . . . ?
N1 C1 C2 F1 109.7(12) . . . . ?
N1 C1 C2 C3 3.3(15) . . . . ?
F1 C2 C3 C4 -80.2(14) . . . . ?
C1 C2 C3 C4 17.6(16) . . . . ?
C2 C3 C4 N1 -31.0(16) . . . . ?
C1 N1 C4 C3 33.4(14) . . . . ?
