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_7250635
_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         'Br4 Sb, 1(C3 H5 N2 S)'
_chemical_formula_sum            'C3 H5 Br4 N2 S Sb'
_chemical_formula_weight         542.54
_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   mixed
_audit_creation_date             2025-02-09
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-03-03 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.686(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5885(9)
_cell_length_b                   13.4694(10)
_cell_length_c                   7.5873(5)
_cell_measurement_reflns_used    1771
_cell_measurement_temperature    387.9(3)
_cell_measurement_theta_max      29.1600
_cell_measurement_theta_min      3.0120
_cell_volume                     1194.25(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      387.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.794
_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    -15.00  11.00   0.50    5.90    --    5.04 -99.00-180.00   52
  2  \w    -62.00  71.00   0.50    5.90    --    5.04   0.00  60.00  266
  3  \w     -6.00  21.00   0.50    5.90    --   -5.19 -99.00 150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0821796000
_diffrn_orient_matrix_UB_12      0.0022080000
_diffrn_orient_matrix_UB_13      -0.0318310000
_diffrn_orient_matrix_UB_21      -0.0117891000
_diffrn_orient_matrix_UB_22      -0.0516393000
_diffrn_orient_matrix_UB_23      0.0083794000
_diffrn_orient_matrix_UB_31      -0.0432043000
_diffrn_orient_matrix_UB_32      0.0100391000
_diffrn_orient_matrix_UB_33      0.0510359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3691
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.813
_diffrn_reflns_theta_min         3.025
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
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    3.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1491
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0595P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1023
_reflns_number_total             1491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00239g4.cif
_cod_data_source_block           a
_cod_database_code               7250635
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.301
_shelx_estimated_absorpt_t_min   0.233
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 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-C2
 1.4 with sigma of 0.01
 N1-S1
 2.652 with sigma of 0.02
 N1-N2
 2.357 with sigma of 0.02
 S1-N2
 2.768 with sigma of 0.02
 C1-C2
 2.357 with sigma of 0.02
2. Restrained planarity
 C1, C2, C3, N1, N2, S1
 with sigma of 0.1
 S1, C3, C2, C1, N2, N1
 with sigma of 0.1
 N1A, C3A, S1A, C2A, C1A, N2A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
S1A \\sim C3A \\sim C2A \\sim C1A \\sim N1A \\sim N2A \\sim C1 \\sim C3 \\sim
S1 \\sim C2 \\sim N1 \\sim N2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Same fragment restrains
{N2A, C1A, N1A, C2A, C3A, S1A} sigma for 1-2: 0.02, 1-3: 0.02
as in
{N2, C1, N1, C2, C3, S1}
5. Others
 Sof(Br2A)=Sof(Br1A)=1-FVAR(1)
 Sof(Br1)=Sof(Br2)=FVAR(1)
 Sof(N2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=Sof(N1A)=Sof(H1A)=Sof(C2A)=Sof(H2AC)=
 Sof(C3A)=Sof(H3A)=Sof(S1A)=0.5*(1-FVAR(3))
 Sof(N2)=Sof(H2A)=Sof(H2B)=Sof(C1)=Sof(N1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=
 Sof(H3)=Sof(S1)=0.5*FVAR(3)
6.a Rotating group:
 N2(H2A,H2B), N2A(H2AA,H2AB)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), N1A(H1A), C2A(H2AC), C3A(H3A)
;
_shelx_res_checksum              23109
_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 3.654
_oxdiff_exptl_absorpt_empirical_full_min 0.450