Room-temperature ferroelectric and ferroelastic orders coexisting in a new tetrafluoroborate-based perovskite
Chen, Xiao-Xian; Zhang, X. Y.; Liu, De-Xuan; Huang, Rui-Kang; Wang, Sha-Sha; Xiong, Li-Qun; Zhang, Wei-Xiong; Chen, Xiao-Ming; Chemical Science  (2021) –; doi:10.1039/D1SC01345A

data_1562622
_publ_section_title
;
 Room-temperature ferroelectric and ferroelastic orders coexisting in a
 new tetrafluoroborate-based perovskite
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01345A
_journal_year                    2021
_chemical_formula_moiety         '0.25(B12 F48 K4), C5 H14 N2'
_chemical_formula_sum            'C5 H14 B3 F12 K N2'
_chemical_formula_weight         401.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5005(4)
_cell_length_b                   9.7685(4)
_cell_length_c                   14.0216(5)
_cell_measurement_reflns_used    4371
_cell_measurement_temperature    338(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      3.49
_cell_volume                     1438.25(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      338
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77487
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12852
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.705
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.115
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.3586
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1515
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1700P)^2^+0.2800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2297
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1204
_reflns_number_total             1515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01345a3.cif
_cod_data_source_block           338K
_cod_database_code               1562622
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 F33A-B3 = F34-B3 = F34A-B3 = F31A-B3 = F32A-B3 = F31-B3 = F32-B3 = F33-B3
 1.36 with sigma of 0.04
 N1-C1 = N1-C5 = N2-C3 = N2-C2
 1.49 with sigma of 0.02
 C2-C1 = C4-C3 = C5-C4
 1.53 with sigma of 0.02
 F33A-F31A \\sim F33A-F34A \\sim F31A-F34A \\sim F33A-F32A \\sim F31A-F32A
\\sim F34A-F32A \\sim F32-
 F31 \\sim F32-F34 \\sim F31-F34 \\sim F32-F33 \\sim F31-F33 \\sim F34-F33
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F31 \\sim F31A \\sim F32 \\sim F32A \\sim F33 \\sim F33A \\sim F34 \\sim F34A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=0.5*(1-FVAR(2))
 Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=0.5*FVAR(2)
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) N2(0.5) H2A(0.5) H2B(0.5) C1(0.5)
 H1C(0.5) H1D(0.5) C2(0.5) H2C(0.5) H2D(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B),
 C5(H5A,H5B)
;
_shelx_res_checksum              97814
_shelx_hkl_checksum              69295
_olex2_submission_special_instructions 'No special instructions were received'