Precise design and preparation of two 3D organic−inorganic perovskite ferroelectrics (1,5-diazabicyclo[3.2.2]nonane)RbX3 (X = Br, I)
Han, Keke; Zhang, Mengxia; Wei, Zhenhong; Ye, Xing; Rao, Wenjun; Zhang, Haina; Cai, Hu; Chemical Communications  (2022) –; doi:10.1039/D2CC02673B

data_7130350
_publ_section_title
;
 Precise design and preparation of two 3D organic&#x2212;inorganic
 perovskite ferroelectrics (1,5-diazabicyclo[3.2.2]nonane)RbX3 (X = Br, I)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02673B
_journal_year                    2022
_chemical_formula_moiety         'Br15 Rb5, 5(C7 H16 N2)'
_chemical_formula_sum            'C35 H80 Br15 N10 Rb5'
_chemical_formula_weight         2266.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-12
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-14 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   48.9591(6)
_cell_length_b                   6.84360(10)
_cell_length_c                   9.86670(10)
_cell_measurement_reflns_used    9682
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.4110
_cell_measurement_theta_min      4.5870
_cell_volume                     3305.90(7)
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12219
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.631
_diffrn_reflns_theta_min         3.611
_exptl_absorpt_coefficient_mu    15.483
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.439
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.284
_refine_ls_abs_structure_details
;
 Flack x determined using 1767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_coef       0.00197(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1194P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.581
_reflns_Friedel_fraction_full    0.687
_reflns_Friedel_fraction_max     0.619
_reflns_number_gt                5232
_reflns_number_total             7057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02673b2.cif
_cod_data_source_block           t_CCDC1
_cod_database_code               7130350
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C1-C2 \\sim C2-C3 \\sim C4-C5 \\sim C6-C7
 with sigma of 0.0001
 C8-C9 \\sim C9-C10 \\sim C11-C12 \\sim C13-C14 \\sim C15-C16
 with sigma of 0.0001
2. Rigid bond restraints
 C11, C12, N3, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim N3 \\sim N4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B)
;
_shelx_res_checksum              85564
_shelx_hkl_checksum              92357
_olex2_submission_special_instructions 'No special instructions were received'