Pb<sub>6</sub>Ba<sub>3</sub>Si<sub>2</sub>S<sub>8</sub>I<sub>10</sub>: a new thiohalide with a quasi-two-dimensional structure and wide band gap.
Zhao, Wang; Zhou, Jiazheng; Wang, Linan; Jin, Wenqi; Kong, Yingying; Chu, Yu; Li, Junjie; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17200–17206; doi:10.1039/d4dt02315c

data_7717123
_publ_section_title
;
 Pb<sub>6</sub>Ba<sub>3</sub>Si<sub>2</sub>S<sub>8</sub>I<sub>10</sub>: a
 new thiohalide with a quasi-two-dimensional structure and wide band gap.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17200
_journal_page_last               17206
_journal_paper_doi               10.1039/d4dt02315c
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H22 Br2 Fe N P'
_chemical_formula_sum            'C25 H22 Br2 Fe N P'
_chemical_formula_weight         583.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-08-26 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2487(2)
_cell_length_b                   15.9203(2)
_cell_length_c                   15.9733(3)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    170.0(1)
_cell_measurement_theta_max      28.305
_cell_measurement_theta_min      2.545
_cell_volume                     2351.94(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      170.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61387
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         2.545
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.119
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0829 before and 0.0722 after correction. The Ratio of minimum to maximum transmission is 0.8609. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method
'from DCM by slow evaporation at the room temperature.'
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0059P)^2^+0.4199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0410
_refine_ls_wR_factor_ref         0.0419
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                5454
_reflns_number_total             5855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02315c2.cif
_cod_data_source_block           mo_akh1_2_0m
_cod_depositor_comments
'Adding full bibliography for 7717123--7717126.cif.'
_cod_database_code               7717123
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.587
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              71660
_shelx_hkl_checksum              30919
_olex2_exptl_crystal_mounting_method
'on a glass microloop covered with perfluoroether oil.'
_olex2_submission_special_instructions 'No special instructions were received'