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_4004018
_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         '2(Ag0.5 Bi0.5 I4), 2(C6 H10 N2), H2 O'
_chemical_formula_sum            'C12 H22 Ag Bi I8 N4 O'
_chemical_formula_weight         1570.38
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-05-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                86.3032(12)
_cell_angle_beta                 88.2019(11)
_cell_angle_gamma                88.8251(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5577(2)
_cell_length_b                   9.7387(2)
_cell_length_c                   18.5585(4)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.30
_cell_volume                     1542.44(6)
_computing_cell_refinement       APEX-2
_computing_data_collection       APEX-2
_computing_data_reduction        APEX-2
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34389
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.136
_diffrn_reflns_theta_min         1.100
_diffrn_source_current           0.97
_diffrn_source_power             0.0485
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.349
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4835
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   APEX-2
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.381
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.7460
_exptl_transmission_factor_min   0.4835
_refine_diff_density_max         1.953
_refine_diff_density_min         -1.906
_refine_diff_density_rms         0.241
_refine_ls_abs_structure_details
;
 Flack x determined using 6080 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.480(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         17621
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0599P)^2^+4.1700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                14311
_reflns_number_total             17621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c01952_si_002.cif
_cod_data_source_block           xl200701f
_cod_database_code               4004018
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.207
_shelx_estimated_absorpt_t_min   0.080
_olex2_refinement_description
;
0. The close distance between H1F and H5A is due to the strong hydrogen bonding.
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C2-C4 = C4-N2
 1.33 with sigma of 0.02
 C8-C12 = C12-C11
 1.33 with sigma of 0.02
 N4-C9 = C9-C8 = C8-C12 = C12-C11 = N4-C10 = C3-C5 = C2-C3 = C2-C4 = N2-C4 =
 C6-N2 = C6-C5 = C16-C14 = C15-C14 = N6-C15 = N6-C18 = C18-C17 = C17-C16 = N8-
 C22 = N8-C21 = C21-C20 = C24-C20 = C24-C23 = C23-C22
 1.33 with sigma of 0.02
 C2-N2
 2.304 with sigma of 0.04
 C8-C11
 2.304 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(N7) = Uiso(C19) = Uiso(C20) = Uiso(C21) = Uiso(C22) = Uiso(C23) = Uiso(C24)
Uiso(N5) = Uiso(N6) = Uiso(C13) = Uiso(C14) = Uiso(C15) = Uiso(C16) = Uiso(C17)
= Uiso(C18)
Uiso(N1) = Uiso(C2) = Uiso(C1) = Uiso(C5) = Uiso(C3) = Uiso(C4) = Uiso(N2) =
Uiso(C6)
Uiso(N7) = Uiso(N8) = Uiso(C19) = Uiso(C20) = Uiso(C21) = Uiso(C22) = Uiso(C23)
= Uiso(C24)
Uiso(N3) = Uiso(N4) = Uiso(C7) = Uiso(C8) = Uiso(C9) = Uiso(C10) = Uiso(C11) =
Uiso(C12)
4. Others
 Fixed Sof: Ag1(0.5) Ag2(0.5) Ag4(0.5) Ag3(0.5)
5.a Free rotating group:
 O1(H1F,H1G), O2(H2B,H2C)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C7(H7A,H7B), C19(H19A,H19B), C13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C12(H12), C23(H23), C9(H9), C6(H6), N6(H6A), C3(H3), C24(H24),
  C16(H16), C15(H15), C21(H21), C10(H10), C11(H11), C2(H2A), C4(H4A), C18(H18),
 C17(H17), N8(H8), C22(H22)
5.d Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), N7(H7C,H7D,H7E), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              54307
_shelx_hkl_checksum              79071
_olex2_submission_special_instructions 'No special instructions were received'