Bismuth/Silver-Based Two-Dimensional Iodide Double and One-Dimensional Bi Perovskites: Interplay between Structural and Electronic Dimensions
Li, Xiaotong; Traoré, Boubacar; Kepenekian, Mikaël; Li, Linda; Stoumpos, Constantinos C.; Guo, Peijun; Even, Jacky; Katan, Claudine; Kanatzidis, Mercouri G.; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c01952

data_4004017
_publ_section_title
;
 Bismuth/Silver-Based Two-Dimensional Iodide Double and One-Dimensional Bi
 Perovskites: Interplay between Structural and Electronic Dimensions
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c01952
_journal_year                    2021
_chemical_formula_moiety         '0.5(Bi2 I10), C6 H16 N2'
_chemical_formula_sum            'C6 H16 Bi I5 N2'
_chemical_formula_weight         959.69
_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             2019-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.14(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.240(2)
_cell_length_b                   8.4579(17)
_cell_length_c                   21.347(4)
_cell_measurement_reflns_used    14496
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      1.89
_cell_volume                     1848.8(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17831
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.152
_diffrn_reflns_theta_min         1.908
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.863
_exptl_absorpt_correction_T_max  0.4766
_exptl_absorpt_correction_T_min  0.0176
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   X-SHAPE
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          1.5587
_exptl_crystal_size_mid          0.0340
_exptl_crystal_size_min          0.0217
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.1495(16)
_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     162
_refine_ls_number_reflns         9860
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0351P)^2^+5.1113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                8958
_reflns_number_total             9860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c01952_si_005.cif
_cod_data_source_block           xl190515a
_cod_original_cell_volume        1848.9(6)
_cod_database_code               4004017
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.3788
_shelx_estimated_absorpt_t_min   0.0203
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -0.015(5)
 1.015(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 N1-C1
 1.5 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 C4-N2
 1.5 with sigma of 0.02
 N2-C5
 1.5 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 C6-C2
 1.5 with sigma of 0.02
 N3-C7
 1.5 with sigma of 0.02
 C7-C8
 1.5 with sigma of 0.02
 C8-C9
 1.5 with sigma of 0.02
 C9-C10
 1.5 with sigma of 0.02
 C10-N4
 1.5 with sigma of 0.02
 N4-C11
 1.5 with sigma of 0.02
 C11-C12
 1.5 with sigma of 0.02
 C12-C8
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(N1) = Uiso(C1) = Uiso(C2) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6) =
Uiso(N2)
Uiso(N3) = Uiso(C7) = Uiso(C8) = Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12) =
Uiso(N4)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4C,H4D), C12(H12A,H12B), C3(H3A,H3B), C11(H11A,H11B), C4(H4A,
 H4B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C1(H1D,H1E), C7(H7A,H7B),
 C5(H5A,H5B)
5.c Idealised Me refined as rotating group:
 N3(H3C,H3D,H3E), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              6723
_shelx_hkl_checksum              88472
_olex2_submission_special_instructions 'No special instructions were received'