#------------------------------------------------------------------------------
#$Date: 2021-07-16 01:36:06 +0300 (Fri, 16 Jul 2021) $
#$Revision: 267567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/40/4004005.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_4004005
loop_
_publ_author_name
'Zhang, Zhi-Xu'
'Su, Chang-Yuan'
'Li, Jie'
'Song, Xian-Jiang'
'Fu, Da-Wei'
'Zhang, Yi'
_publ_section_title
;
 Ferroelastic Hybrid Bismuth Bromides with Dual Dielectric Switches
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c01699
_journal_year                    2021
_chemical_formula_moiety         '3(C7 N), Bi2 Br9'
_chemical_formula_sum            'C21 H0 Bi2 Br9 N3'
_chemical_formula_weight         1431.39
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.4505(8)
_cell_length_b                   10.4505(8)
_cell_length_c                   23.2226(13)
_cell_measurement_reflns_used    3291
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5270
_cell_measurement_theta_min      2.8430
_cell_volume                     2196.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8994
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    16.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.628
_refine_diff_density_min         -2.958
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         786
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1667P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2405
_reflns_number_gt                619
_reflns_number_total             786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm1c01699_si_009.cif
_cod_data_source_block           TMTBA-293K
_cod_database_code               4004005
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C4 C 0.3333 0.6667 0.1189(2) 0.146(3) Uani 1 6 d SDU . .
C3 C 0.0000 1.0000 0.12089(13) 0.284(6) Uani 1 6 d SDU . .
C2 C 0.0000 1.0000 0.18545(9) 0.272(5) Uani 0.50 6 d SPDU . .
N1 N 0.0000 1.0000 0.2500 0.272(4) Uani 1 12 d SDU . .
C5 C 0.2486(6) 0.7514(6) 0.13843(15) 0.159(2) Uani 1 2 d SDU . .
C6 C 0.4162(3) 0.8324(5) 0.0479(3) 0.139(3) Uani 1 2 d SDU . .
Bi1 Bi 0.6667 0.3333 0.16378(2) 0.0601(2) Uani 1 6 d SU . .
Br2 Br 0.54048(9) 0.45952(9) 0.2500 0.0828(5) Uani 1 4 d SU . .
Br1 Br 0.41336(14) 0.20668(7) 0.10053(5) 0.0888(4) Uani 1 2 d SU . .
N2 N 0.2713(2) 0.7287(2) 0.07621(13) 0.149(3) Uani 0.33 2 d SPDU . .
C1 C -0.0062(6) 0.8534(3) 0.2500 0.269(5) Uani 0.67 2 d SPDU . .
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'
Bi Bi -4.1077 10.2566 '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'
N N 0.0061 0.0033 '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
N2 C4 N2 80.9(3) . 3_665 ?
N2 C4 N2 80.9(3) . 5_565 ?
N2 C4 N2 80.9(3) 3_665 5_565 ?
N2 C4 C5 57.9(2) . . ?
N2 C4 C5 123.15(17) 3_665 . ?
N2 C4 C5 123.15(17) 5_565 . ?
N2 C4 C5 123.15(17) . 3_665 ?
N2 C4 C5 57.9(2) 3_665 3_665 ?
N2 C4 C5 123.15(17) 5_565 3_665 ?
C5 C4 C5 112.3(2) . 3_665 ?
N2 C4 C5 123.15(17) . 5_565 ?
N2 C4 C5 123.15(17) 3_665 5_565 ?
N2 C4 C5 57.9(2) 5_565 5_565 ?
C5 C4 C5 112.3(2) . 5_565 ?
C5 C4 C5 112.3(2) 3_665 5_565 ?
N1 C2 C3 180.000(1) . . ?
C2 N1 C2 180.0 . 14_466 ?
C2 N1 C1 90.000(2) . 20_455 ?
C2 N1 C1 90.000(2) 14_466 20_455 ?
C2 N1 C1 90.000(2) . 7_665 ?
C2 N1 C1 90.000(2) 14_466 7_665 ?
C1 N1 C1 120.0 20_455 7_665 ?
C2 N1 C1 90.000(2) . 3_675 ?
C2 N1 C1 90.000(2) 14_466 3_675 ?
C1 N1 C1 175.7(4) 20_455 3_675 ?
C1 N1 C1 55.7(4) 7_665 3_675 ?
C2 N1 C1 90.000(1) . . ?
C2 N1 C1 90.000(1) 14_466 . ?
C1 N1 C1 55.7(4) 20_455 . ?
C1 N1 C1 64.3(4) 7_665 . ?
C1 N1 C1 120.000(1) 3_675 . ?
C2 N1 C1 90.000(2) . 14_466 ?
C2 N1 C1 90.000(1) 14_466 14_466 ?
C1 N1 C1 64.3(4) 20_455 14_466 ?
C1 N1 C1 175.7(4) 7_665 14_466 ?
C1 N1 C1 120.000(1) 3_675 14_466 ?
C1 N1 C1 120.000(4) . 14_466 ?
C2 N1 C1 90.000(1) . 9_575 ?
C2 N1 C1 90.000(1) 14_466 9_575 ?
C1 N1 C1 120.000(4) 20_455 9_575 ?
C1 N1 C1 120.000(5) 7_665 9_575 ?
C1 N1 C1 64.3(4) 3_675 9_575 ?
C1 N1 C1 175.7(4) . 9_575 ?
C1 N1 C1 55.7(4) 14_466 9_575 ?
N2 C5 C4 57.6(3) . . ?
N2 C6 N2 80.6(4) 5_565 . ?
Br1 Bi1 Br1 93.63(4) 3_655 . ?
Br1 Bi1 Br1 93.63(4) 3_655 5_665 ?
Br1 Bi1 Br1 93.63(4) . 5_665 ?
Br1 Bi1 Br2 92.24(2) 3_655 14_666 ?
Br1 Bi1 Br2 171.41(4) . 14_666 ?
Br1 Bi1 Br2 92.24(2) 5_665 14_666 ?
Br1 Bi1 Br2 92.24(2) 3_655 3_655 ?
Br1 Bi1 Br2 92.24(2) . 3_655 ?
Br1 Bi1 Br2 171.41(4) 5_665 3_655 ?
Br2 Bi1 Br2 81.27(3) 14_666 3_655 ?
Br1 Bi1 Br2 171.41(4) 3_655 . ?
Br1 Bi1 Br2 92.24(2) . . ?
Br1 Bi1 Br2 92.24(2) 5_665 . ?
Br2 Bi1 Br2 81.27(3) 14_666 . ?
Br2 Bi1 Br2 81.27(3) 3_655 . ?
Bi1 Br2 Bi1 82.47(4) 14_666 . ?
C4 N2 C5 64.4(4) . . ?
C4 N2 C6 96.0(3) . 3_665 ?
C5 N2 C6 119.3(3) . 3_665 ?
C4 N2 C6 96.0(3) . . ?
C5 N2 C6 119.3(3) . . ?
C6 N2 C6 119.6(6) 3_665 . ?
C1 C1 N1 62.1(2) 20_455 . ?
C1 C1 C1 120.000(2) 20_455 7_665 ?
N1 C1 C1 57.9(2) . 7_665 ?
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
C4 N2 1.498(4) . ?
C4 N2 1.498(4) 3_665 ?
C4 N2 1.498(4) 5_565 ?
C4 C5 1.600(10) . ?
C4 C5 1.600(10) 3_665 ?
C4 C5 1.600(10) 5_565 ?
C3 C2 1.499(3) . ?
C2 N1 1.499(2) . ?
N1 C2 1.499(2) 14_466 ?
N1 C1 1.501(4) 20_455 ?
N1 C1 1.501(4) 7_665 ?
N1 C1 1.501(4) 3_675 ?
N1 C1 1.501(4) . ?
N1 C1 1.501(4) 14_466 ?
N1 C1 1.501(4) 9_575 ?
C5 N2 1.503(4) . ?
C6 N2 1.503(4) 5_565 ?
C6 N2 1.503(4) . ?
Bi1 Br1 2.7228(13) 3_655 ?
Bi1 Br1 2.7228(13) . ?
Bi1 Br1 2.7228(13) 5_665 ?
Bi1 Br2 3.0374(12) 14_666 ?
Bi1 Br2 3.0374(12) 3_655 ?
Bi1 Br2 3.0374(12) . ?
Br2 Bi1 3.0374(12) 14_666 ?
N2 C6 1.503(4) 3_665 ?
C1 C1 1.402(12) 20_455 ?
C1 C1 1.597(8) 7_665 ?
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
C3 C2 N1 C2 0.0 . . . 14_466 ?
C3 C2 N1 C1 -28(70) . . . 20_455 ?
C3 C2 N1 C1 92(66) . . . 7_665 ?
C3 C2 N1 C1 148(100) . . . 3_675 ?
C3 C2 N1 C1 28(66) . . . . ?
C3 C2 N1 C1 -92(100) . . . 14_466 ?
C3 C2 N1 C1 -148(100) . . . 9_575 ?
N2 C4 C5 N2 -50.8(3) 3_665 . . . ?
N2 C4 C5 N2 50.8(3) 5_565 . . . ?
C5 C4 C5 N2 -116.1(3) 3_665 . . . ?
C5 C4 C5 N2 116.1(3) 5_565 . . . ?
Br1 Bi1 Br2 Bi1 0.0 3_655 . . 14_666 ?
Br1 Bi1 Br2 Bi1 133.136(19) . . . 14_666 ?
Br1 Bi1 Br2 Bi1 -133.136(19) 5_665 . . 14_666 ?
Br2 Bi1 Br2 Bi1 -41.215(12) 14_666 . . 14_666 ?
Br2 Bi1 Br2 Bi1 41.215(12) 3_655 . . 14_666 ?
N2 C4 N2 C5 138.92(12) 3_665 . . . ?
N2 C4 N2 C5 -138.92(12) 5_565 . . . ?
C5 C4 N2 C5 97.2(3) 3_665 . . . ?
C5 C4 N2 C5 -97.2(3) 5_565 . . . ?
N2 C4 N2 C6 19.2(3) 3_665 . . 3_665 ?
N2 C4 N2 C6 101.4(3) 5_565 . . 3_665 ?
C5 C4 N2 C6 -119.7(3) . . . 3_665 ?
C5 C4 N2 C6 -22.4(5) 3_665 . . 3_665 ?
C5 C4 N2 C6 143.1(4) 5_565 . . 3_665 ?
N2 C4 N2 C6 -101.4(3) 3_665 . . . ?
N2 C4 N2 C6 -19.2(3) 5_565 . . . ?
C5 C4 N2 C6 119.7(3) . . . . ?
C5 C4 N2 C6 -143.1(4) 3_665 . . . ?
C5 C4 N2 C6 22.4(5) 5_565 . . . ?
C4 C5 N2 C6 82.2(4) . . . 3_665 ?
C4 C5 N2 C6 -82.2(4) . . . . ?
N2 C6 N2 C4 19.2(4) 5_565 . . . ?
N2 C6 N2 C5 83.2(6) 5_565 . . . ?
N2 C6 N2 C6 -81.2(5) 5_565 . . 3_665 ?
C2 N1 C1 C1 -90.0 . . . 20_455 ?
C2 N1 C1 C1 90.0 14_466 . . 20_455 ?
C1 N1 C1 C1 180.0 7_665 . . 20_455 ?
C1 N1 C1 C1 180.0 3_675 . . 20_455 ?
C1 N1 C1 C1 0.0 14_466 . . 20_455 ?
C1 N1 C1 C1 0.0 9_575 . . 20_455 ?
C2 N1 C1 C1 90.0 . . . 7_665 ?
C2 N1 C1 C1 -90.0 14_466 . . 7_665 ?
C1 N1 C1 C1 180.0 20_455 . . 7_665 ?
C1 N1 C1 C1 0.0 3_675 . . 7_665 ?
C1 N1 C1 C1 180.0 14_466 . . 7_665 ?
C1 N1 C1 C1 180.0 9_575 . . 7_665 ?
