[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_7711077
_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
'Bi2 I9, 2.75(C3 H9 S), 0.09(S), 0.5(C1.5 H4.5 S0.31)'
_chemical_formula_sum            'C9 H27 Bi2 I9 S3'
_chemical_formula_weight         1791.54
_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_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-05
_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                 91.934(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.9347(13)
_cell_length_b                   33.0271(14)
_cell_length_c                   22.7116(14)
_cell_measurement_reflns_used    28982
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      1.24
_cell_volume                     14194.8(14)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detetor, \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1435
_diffrn_reflns_av_unetI/netI     0.1738
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59021
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.127
_diffrn_reflns_theta_min         1.233
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.909
_exptl_absorpt_correction_T_max  0.1693
_exptl_absorpt_correction_T_min  0.0511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area LANA 1.71.6.0 (STOE, 2017)'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.353
_exptl_crystal_description       plate
_exptl_crystal_F_000             12352
_exptl_crystal_size_max          0.0728
_exptl_crystal_size_mid          0.04175
_exptl_crystal_size_min          0.02221
_refine_diff_density_max         1.653
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         15293
_refine_ls_number_restraints     626
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1836
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0730P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6487
_reflns_number_total             15293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02305a2.cif
_cod_data_source_block           2
_cod_database_code               7711077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.356
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C1_2-S1_2 \\sim C1_2-S2
 with sigma of 0.02
 C2_2-S1_2 \\sim C2_2-S2
 with sigma of 0.02
 C3_2-S1_2 \\sim C3_2-S2
 with sigma of 0.02
 C1_3-S1_3 \\sim C1_3-S3
 with sigma of 0.02
 C2_3-S1_3 \\sim C2_3-S3
 with sigma of 0.02
 C3_3-S1_3 \\sim C3_3-S3
 with sigma of 0.02
 S1_1-C1_1 \\sim S1_1-C2_1 \\sim S1_1-C3_1
 S1_2-C1_2 \\sim S1_2-C2_2 \\sim S1_2-C3_2
 S1_3-C1_3 \\sim S1_3-C2_3 \\sim S1_3-C3_3
 S1_4-C1_4 \\sim S1_4-C2_4 \\sim S1_4-C3_4
 S1_5-C1_5 \\sim S1_5-C2_5 \\sim S1_5-C3_5
 S1_6-C1_6 \\sim S1_6-C2_6 \\sim S1_6-C3_6
 S1_7-C1_7 \\sim S1_7-C2_7 \\sim S1_7-C3_7
 with sigma of 0.02
 C1_1-C2_1 \\sim C2_1-C3_1 \\sim C3_1-C1_1
 C1_2-C2_2 \\sim C2_2-C3_2 \\sim C3_2-C1_2
 C1_3-C2_3 \\sim C2_3-C3_3 \\sim C3_3-C1_3
 C1_4-C2_4 \\sim C2_4-C3_4 \\sim C3_4-C1_4
 C1_5-C2_5 \\sim C2_5-C3_5 \\sim C3_5-C1_5
 C1_6-C2_6 \\sim C2_6-C3_6 \\sim C3_6-C1_6
 C1_7-C2_7 \\sim C2_7-C3_7 \\sim C3_7-C1_7
 with sigma of 0.04
 C1_7-S1_7 \\sim C1_7-S4
 with sigma of 0.02
 C2_7-S1_7 \\sim C2_7-S4
 with sigma of 0.02
 C3_7-S1_7 \\sim C3_7-S4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S3 \\sim S1_3: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
S2 \\sim S1_2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C1_3 \\sim C3_3 \\sim C2_3: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.08
C3_2 \\sim C1_2 \\sim C2_2: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.02
S1_1 \\sim C3_1 \\sim S1_2 \\sim C3_2 \\sim S1_3 \\sim C3_3 \\sim S1_4 \\sim
C3_4 \\sim S1_5 \\sim C3_5 \\sim S1_6 \\sim C3_6 \\sim S1_7 \\sim C3_7: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1_5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2_5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 S1_1, C3_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1_2, C3_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1_3, C3_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1_4, C3_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1_5, C3_5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3_6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1_7, C3_7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S2)=Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H2BD)=Sof(H2BE)=Sof(H2BF)=Sof(H3BD)=
 Sof(H3BE)=Sof(H3BF)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=Sof(S1)=FVAR(1)
 Sof(S3)=Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H2BD)=Sof(H2BE)=Sof(H2BF)=Sof(H3BD)=
 Sof(H3BE)=Sof(H3BF)=1-FVAR(2)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=Sof(S1)=FVAR(2)
 Sof(S4)=0.5*(1-FVAR(4))
 Sof(S1)=0.5*FVAR(4)
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) S1(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
6.a Me refined with riding coordinates:
 C1(H1BD,H1BE,H1BF), C1(H1AA,H1AB,H1AC), C2(H2BD,H2BE,H2BF), C2(H2AA,H2AB,
 H2AC), C3(H3BD,H3BE,H3BF), C3(H3AA,H3AB,H3AC), C1(H1BD,H1BE,H1BF), C1(H1AA,
 H1AB,H1AC), C2(H2BD,H2BE,H2BF), C2(H2AA,H2AB,H2AC), C3(H3BD,H3BE,H3BF),
 C3(H3AA,H3AB,H3AC), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,
 H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,
 H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              37756
_olex2_submission_special_instructions 'No special instructions were received'