A Multiaxial Layered Halide Double Perovskite Ferroelectric with Multiple Ferroic Orders
Liu, Xitao; Xu, Zhiyun; Long, Peiqing; Yao, Yunpeng; Ji, Chengmin; Li, Lina; Sun, Zhihua; Hong, Maochun; Luo, Junhua; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c02966

data_4003692
_publ_section_title
;
 A Multiaxial Layered Halide Double Perovskite Ferroelectric with Multiple
 Ferroic Orders
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c02966
_journal_year                    2020
_chemical_formula_moiety         'Ag Bi Br7 Cs, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Ag Bi Br7 Cs N2'
_chemical_formula_weight         1157.42
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.734(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0618(5)
_cell_length_b                   7.8928(4)
_cell_length_c                   19.7697(12)
_cell_measurement_reflns_used    7199
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.477
_cell_measurement_theta_min      2.787
_cell_volume                     1231.66(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      199.98
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX3 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18268
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         2.581
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.734
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.1489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1245 before and 0.0641 after correction. The Ratio of minimum to maximum transmission is 0.5692. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.121
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Flack x determined using 1748 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.282(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4363
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0105P)^2^+16.6632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4107
_reflns_number_total             4363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02966_si_002.cif
_cod_data_source_block           x1
_cod_database_code               4003692
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.575
_shelx_estimated_absorpt_t_min   0.424
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.526(2)
 0.474(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C4-C3
 1.5 with sigma of 0.02
 N1-C1 = N2-C5
 1.47 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N2 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C1 \\sim N1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C1(H1A,H1B), C2(H2D,H2E), C3(H3A,H3B)
5.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C8(H8A,H8B,H8C), N1(H1C,H1D,H1E), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'