[SMe3]2[Bi2Ag2I10], a silver iodido bismuthate with an unusually small band gap
Möbs, Jakob; Pan, Sudip; Tonner-Zech, Ralf; Heine, Johanna; Dalton Transactions  (2022) –; doi:10.1039/D2DT02305A

data_7711078
_publ_section_title
;
 [SMe3]2[Bi2Ag2I10], a silver iodido bismuthate with an unusually small
 band gap
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02305A
_journal_year                    2022
_chemical_formula_moiety         'I9 Sb2, 3(C3 H9 S)'
_chemical_formula_sum            'C9 H27 I9 S3 Sb2'
_chemical_formula_weight         1617.08
_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'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-15 deposited with the CCDC.	2022-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.447(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.2137(7)
_cell_length_b                   33.5700(18)
_cell_length_c                   22.9179(8)
_cell_measurement_reflns_used    33923
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.72
_cell_measurement_theta_min      2.63
_cell_volume                     14777.4(11)
_computing_cell_refinement
;
X-Area Recipe 1.34.0.0 (STOE, 2019)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.154.0 (STOE, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (STOE, 2019)
X-Area LANA 1.77.1.0 (STOE, 2019)
;
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Stoe_Stadivari_Cu
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55892
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.499
_diffrn_reflns_theta_max         67.499
_diffrn_reflns_theta_min         2.633
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    72.220
_exptl_absorpt_correction_T_max  0.0025
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.858
_exptl_crystal_description       block
_exptl_crystal_F_000             10896
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.101
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         13177
_refine_ls_number_restraints     678
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1062P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5310
_reflns_number_total             13177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02305a2.cif
_cod_data_source_block           4
_cod_database_code               7711078
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.265
_shelx_estimated_absorpt_t_min   0.050
_olex2_refinement_description
;
1. Restrained distances
 S10-C13 \\sim S9-C13 \\sim S10-C14 \\sim S9-C15 \\sim S10-C15 \\sim S8-C10
\\sim S7-C10 \\sim S8-C12 \\sim S7-
 C12 \\sim S7-C11 \\sim S11-C17 \\sim S11-C16 \\sim S1_$1-C2_$1 \\sim
S2_$1-C2_$1 \\sim S2_$1-C1_$1 ~
 S1_$1-C1_$1 \\sim S1_$1-C3_$1 \\sim S2_$1-C3_$1 \\sim S6_$2-C7_$2 \\sim
S5_$2-C7_$2 \\sim S6_$2-
 C8_$2 \\sim S6_$2-C9_$2 \\sim S5_$2-C9_$2 \\sim S5_$2-C8_$2 \\sim S3-C6 \\sim
S4-C6 \\sim S4-C5 \\sim S3-
 C5 \\sim S4-C4 \\sim S3-C4 \\sim S8-C11
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
S2 \\sim S1 \\sim C3 \\sim C2 \\sim C1 \\sim C5 \\sim S3 \\sim C4 \\sim C6
\\sim S4 \\sim C16 \\sim S11 \\sim C17 \\sim S9 \\sim S10 \\sim C14 \\sim C13
\\sim C15 \\sim C10 \\sim S7 \\sim C12 \\sim C11 \\sim S8 \\sim S13 \\sim C18
\\sim C19 \\sim S12 \\sim C7 \\sim S6 \\sim C8 \\sim C9 \\sim S5: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C7) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C11) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C7, S6, C8, C9, S5, S3, C4, C5, C6, S4, S2, S1, C3, C2, C1, S11, C16, C17, S9,
  S10, C14, C13, C15, S8, S7, C12, C11, C10, S12, S13, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(S2)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Sof(S4)=1-FVAR(2)
 Sof(S3)=FVAR(2)
 Sof(S6)=1-FVAR(3)
 Sof(S5)=FVAR(3)
 Sof(S8)=1-FVAR(4)
 Sof(S7)=FVAR(4)
 Sof(S10)=1-FVAR(5)
 Sof(S9)=FVAR(5)
 Sof(S13)=0.5*(1-FVAR(7))
 Sof(S12)=0.5*FVAR(7)
 Fixed Sof: S11(0.5) C18(0.75) C19(0.75)
;
_shelx_res_checksum              37855
_olex2_submission_special_instructions 'No special instructions were received'