Ferroelasticity induced by metal substitution in one-dimensional hybrid perovskites
Chong, Qingdian; He, Lei; Yang, Yawen; Ye, Qiong; CrystEngComm 27 (2025) 3320–3325; doi:10.1039/D5CE00239G

data_7250636
_publ_section_title
;
 Ferroelasticity induced by metal substitution in one-dimensional hybrid
 perovskites
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3320
_journal_page_last               3325
_journal_paper_doi               10.1039/D5CE00239G
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Bi Br4, C3 H5 N2 S'
_chemical_formula_sum            'C3 H5 Bi Br4 N2 S'
_chemical_formula_weight         629.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-02-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.770(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4541(4)
_cell_length_b                   13.6664(4)
_cell_length_c                   7.5122(2)
_cell_measurement_reflns_used    2206
_cell_measurement_temperature    393.02(10)
_cell_measurement_theta_max      72.4790
_cell_measurement_theta_min      4.9450
_cell_volume                     1210.76(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.129a 64-bit (release 29-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.129a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      393.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_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     27.00  52.00   0.50    0.05    --   51.49-120.00  11.00   50
  2  \w     31.00  57.00   0.50    0.05    --   58.53-120.00  11.00   52
  3  \w     39.00  64.00   0.50    0.05    --   86.48-120.00  11.00   50
  4  \w     66.00  95.00   0.50    0.05    --   93.63-120.00  11.00   58
  5  \w     32.00  89.00   0.50    0.05    --   86.48 -94.00   0.00  114
  6  \w     41.00  91.00   0.50    0.05    --   93.63 -94.00  30.00  100
  7  \w     68.00  93.00   0.50    0.05    --   93.63 -94.00  60.00   50
  8  \w      5.00  30.00   0.50    0.05    --   58.53 -45.00  90.00   50
  9  \w     51.00  78.00   0.50    0.05    --   93.63 -77.00 150.00   54
 10  \w     40.00  68.00   0.50    0.05    --   86.48 -77.00  60.00   56
 11  \w     -1.00  30.00   0.50    0.05    --   58.53 -45.00 -60.00   62
 12  \w     46.00  71.00   0.50    0.05    --   93.63 -77.00-120.00   50
 13  \w     -8.00  32.00   0.50    0.05    --   51.49 -45.00-180.00   80
 14  \w    101.00 149.00   0.50    0.05    --   93.63 111.00-180.00   96
 15  \w     99.00 124.00   0.50    0.05    --   86.48 120.00  95.00   50
 16  \w     90.00 136.00   0.50    0.05    --   86.48  61.00  90.00   92
 17  \w     91.00 142.00   0.50    0.05    --   93.63  61.00 150.00  102
 18  \w     88.00 141.00   0.50    0.05    --   86.48  61.00  60.00  106
 19  \w     96.00 150.00   0.50    0.05    --   93.63  61.00   0.00  108
 20  \w    -26.00  -1.00   0.50    0.05    --  -58.99  45.00  30.00   50
 21  \w    -26.00  -1.00   0.50    0.05    --  -58.99  45.00 -60.00   50
 22  \w    -48.00 -23.00   0.50    0.05    --  -77.04  61.00 -60.00   50
 23  \w    -71.00 -31.00   0.50    0.05    --  -77.04  77.00 -90.00   80
 24  \w    -48.00 -23.00   0.50    0.05    --  -77.04  61.00-180.00   50
 25  \w    -24.00   2.00   0.50    0.05    --  -58.99  45.00-120.00   52
 26  \w   -111.00 -58.00   0.50    0.05    --  -58.99 -45.00-180.00  106
 27  \w   -119.00 -90.00   0.50    0.05    --  -77.04-120.00  11.00   58
 28  \w    -97.00 -43.00   0.50    0.05    --  -77.04 120.00  95.00  108
 29  \w    -64.00 -19.00   0.50    0.05    --  -58.99 120.00  95.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0249650000
_diffrn_orient_matrix_UB_12      -0.0667671000
_diffrn_orient_matrix_UB_13      0.1021734000
_diffrn_orient_matrix_UB_21      0.0500572000
_diffrn_orient_matrix_UB_22      -0.0896690000
_diffrn_orient_matrix_UB_23      -0.0694938000
_diffrn_orient_matrix_UB_31      0.1982717000
_diffrn_orient_matrix_UB_32      0.0142834000
_diffrn_orient_matrix_UB_33      0.0421238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3823
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.119
_diffrn_reflns_theta_min         4.953
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    45.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.129a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.455
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.348
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1176
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1479P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2079
_refine_ls_wR_factor_ref         0.2158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1033
_reflns_number_total             1176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00239g4.cif
_cod_data_source_block           2
_cod_database_code               7250636
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C N H Br Bi'
_shelx_estimated_absorpt_t_max   0.074
_shelx_estimated_absorpt_t_min   0.056
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N1-C3_$1
 1.8 with sigma of 0.02
 N1-C2
 1.4 with sigma of 0.01
 N2-C1
 1.43 with sigma of 0.01
 S1-C1 = S1-C3
 1.76 with sigma of 0.01
 C2-C3
 1.34 with sigma of 0.01
 N1-C1
 1.29 with sigma of 0.01
 N1-S1
 2.652 with sigma of 0.02
 N1-N2
 2.357 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, N1, N2, S1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C3) = Uanis(N1)
5. Same fragment restrains
{Bi1, Br1A, Br2A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Bi1, Br1, Br2}
6. Others
 Sof(Br1A)=Sof(Br2A)=1-FVAR(1)
 Sof(Br1)=Sof(Br2)=FVAR(1)
 Fixed Sof: C1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) N1(0.5) H1(0.5) N2(0.5)
 H2A(0.5) H2B(0.5) S1(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), N1(H1)
7.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
;
_shelx_res_checksum              74440
_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 2.745
_oxdiff_exptl_absorpt_empirical_full_min 0.264