Direct-Bandgap 2D Silver-Bismuth Iodide Double Perovskite: The Structure-Directing Influence of an Oligothiophene Spacer Cation.
Jana, Manoj K.; Janke, Svenja M.; Dirkes, David J.; Dovletgeldi, Seyitliyev; Liu, Chi; Qin, Xixi; Gundogdu, Kenan; You, Wei; Blum, Volker; Mitzi, David B.; Journal of the American Chemical Society 141 (2019) 7955–7964; doi:10.1021/jacs.9b02909

data_4127221
_publ_section_title
;
 Direct-Bandgap 2D Silver-Bismuth Iodide Double Perovskite: The
 Structure-Directing Influence of an Oligothiophene Spacer Cation.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7955
_journal_page_last               7964
_journal_paper_doi               10.1021/jacs.9b02909
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'Ag Bi I8, 2(C12 H18 N2 S2)'
_chemical_formula_sum            'C24 H36 Ag Bi I8 N4 S4'
_chemical_formula_weight         1840.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7321(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.3654(14)
_cell_length_b                   6.1473(3)
_cell_length_c                   12.0494(6)
_cell_measurement_reflns_used    9200
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      3.39
_cell_volume                     2172.66(18)
_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
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7269
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         3.771
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.393
_exptl_absorpt_correction_T_max  0.7888
_exptl_absorpt_correction_T_min  0.24030
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_description       plate
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.024
_refine_diff_density_max         3.036
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0872P)^2^+36.0664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1473
_reflns_number_total             2212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02909_si_004.cif
_cod_data_source_block           (AE2T)2AgBiI8_298K
_cod_depositor_comments
'Adding full bibliography for 4127220--4127221.cif.'
_cod_database_code               4127221
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.163
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Shared sites
{Bi1, Ag1}
3. Uiso/Uaniso restraints and constraints
Uanis(Bi1) = Uanis(Ag1)
4. Others
 Fixed Sof: Bi1(0.25) Ag1(0.25) I3(0.5) I4(0.5) C1(0.5) C2(0.5) C3B(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) H8A(0.5)
 H8B(0.5) H10A(0.5) H10B(0.5) H10C(0.5) H10D(0.5) C11(0.5) H11(0.5) C12(0.5)
 H12(0.5) C3A(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N4(0.25) H4A(0.25)
 H4B(0.25) H4C(0.25) N5(0.25) H5C(0.25) H5D(0.25) H5E(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8A,H8B), C10B(H10A,H10B), C10B(H10C,H10D)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C11(H11), C12(H12)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N4(H4A,H4B,H4C), N5(H5C,H5D,H5E)
;
_shelx_res_checksum              75825
_shelx_hkl_checksum              71378
_olex2_submission_original_sample_id '[AE2T]2AgBiI8'
_olex2_submission_special_instructions 'No special instructions were received'