Seeking environmentally friendly halide perovskite photocatalysts: synthesis, structure and photocatalytic performance exploration.
Hu, Cheng-An; Qin, Jian-Peng; Pan, Chun-Yang; Dalton transactions (Cambridge, England : 2003) 53 (2024) 512–519; doi:10.1039/d3dt02990e

data_7714612
_publ_section_title
;
 Seeking environmentally friendly halide perovskite photocatalysts:
 synthesis, structure and photocatalytic performance exploration.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              512
_journal_page_last               519
_journal_paper_doi               10.1039/d3dt02990e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Bi2 Br9, 3(C3 H10 N)'
_chemical_formula_sum            'C9 H30 Bi2 Br9 N3'
_chemical_formula_weight         1317.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-24
_audit_creation_method
;FinalCif V121 by Daniel Kratzert, Freiburg 2023, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-07-08 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.209(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2323(13)
_cell_length_b                   15.0720(13)
_cell_length_c                   11.4500(10)
_cell_measurement_reflns_used    5866
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.275
_cell_measurement_theta_min      2.401
_cell_volume                     2926.8(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.1190
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24531
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        24.972
_diffrn_reflns_theta_max         24.972
_diffrn_reflns_theta_min         1.808
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.297
_exptl_absorpt_correction_T_max  0.0277
_exptl_absorpt_correction_T_min  0.0031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.1060 after correction.
The Ratio of minimum to maximum transmission is 0.1119.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_description       needle
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.407
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.299
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4834
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0481P)^2^+92.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.870
_reflns_Friedel_fraction_max     0.870
_reflns_number_gt                3742
_reflns_number_total             4834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02990e2.cif
_cod_data_source_block           mo_0619_11_0m
_cod_depositor_comments
'Adding full bibliography for 7714610--7714612.cif.'
_cod_database_code               7714612
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.73(3)
 0.27(3)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Bi4-Br17 \\sim Bi4-Br16 \\sim Bi4-Br18 \\sim Bi4-Br13 \\sim Bi4-Br15 \\sim
Bi4-Br14 \\sim Bi3-Br14 ~
 Bi3-Br15 \\sim Bi3-Br13 \\sim Bi3-Br11 \\sim Bi3-Br10 \\sim Bi3-Br12
 with sigma of 0.02
 Bi02-Bi01 \\sim Bi4-Bi3
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Br17 \\sim Bi3 \\sim Br10 \\sim Br11 \\sim Br12 \\sim Br13 \\sim Br15 \\sim
Br14 \\sim Bi4 \\sim Br16 \\sim Br18: within 2A with sigma of 0.0001 and sigma
for terminal atoms of 0.0002 within 2A
N1 \\sim C00E \\sim C00J \\sim C00G: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 2A
C00L \\sim C00F \\sim N2 \\sim C00O: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N3 \\sim C1 \\sim C00H \\sim C00I: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 Br17, Bi3, Br10, Br11, Br12, Br13, Br15, Br14, Bi4, Br16, Br18
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002
 C00E, N1, C00J, C00G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
 N3, C1, C00H, C00I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00O, C00F, N2, C00L
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(Bi3)=Sof(Br10)=Sof(Br12)=Sof(Br11)=Sof(Bi4)=Sof(Br13)=Sof(Br14)=Sof(Br15)=
 Sof(Br17)=Sof(Br18)=Sof(Br16)=1-FVAR(1)
 Sof(Bi01)=Sof(Bi02)=Sof(Br03)=Sof(Br04)=Sof(Br05)=Sof(Br06)=Sof(Br07)=
 Sof(Br08)=Sof(Br09)=Sof(Br0A)=Sof(Br0B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N2(H2)
7.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C00E(H00G,H00H,H00I), C00F(H00P,H00Q,H00R), C00G(H00J,H00K,
 H00L), C00H(H00A,H00B,H00C), C00I(H00D,H00E,H00F), C00J(H00M,H00N,H00O),
 C00L(H00S,H00T,H00U), C00O(H00V,H00W,H00X)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.247
_shelx_estimated_absorpt_t_max   0.323