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_4003694
_publ_section_title
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 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         '0.5(Ag2 Bi2 Br14 Cs2), 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           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.719(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0589(9)
_cell_length_b                   8.0388(9)
_cell_length_c                   19.876(2)
_cell_measurement_reflns_used    3529
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.044
_cell_measurement_theta_min      2.741
_cell_volume                     1260.8(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.02
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0598
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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            12704
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.534
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    20.254
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1339 before and 0.0640 after correction. The Ratio of minimum to maximum transmission is 0.4934. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.049
_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         2.953
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2405
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0692P)^2^+9.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1711
_reflns_number_total             2405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c02966_si_003.cif
_cod_data_source_block           x1
_cod_database_code               4003694
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.582
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.4989(14)
 0.5011(14)
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
 N1-C1 = N2-C5
 1.47 with sigma of 0.02
 C1-C2 = C2-C3 = C3-C4 = C5-C6 = C6-C7 = C7-C8
 1.5 with sigma of 0.02
 N2-C6 = C5-C7 = C6-C8
 2.7 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim N2
\\sim N1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: N2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5) C1(0.5) H1A(0.5) H1B(0.5) N1(0.5) H1C(0.5) H1D(0.5) H1E(0.5) C2(0.5)
 H2D(0.5) H2E(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
6.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)
6.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C8(H8A,H8B,H8C), N1(H1C,H1D,H1E), C4(H4A,H4B,H4C)
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_olex2_submission_special_instructions 'No special instructions were received'