Fundamental Insights in Photoelectrocatalytic Hydrogen Production with a Hole-transport Bismuth Metal-organic Framework.
García-Sánchez, Alba; Gomez-Mendoza, Miguel; Barawi, Mariam; Villar-Garcia, Ignacio Jose; Liras, Marta; Gándara, Felipe; de la Peña O'Shea, Víctor A; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10261

data_4133829
_publ_section_title
;
 Fundamental Insights in Photoelectrocatalytic Hydrogen Production with a
 Hole-transport Bismuth Metal-organic Framework.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10261
_journal_year                    2019
_chemical_formula_moiety         '2(C40 H8 Bi2 O16 S12)'
_chemical_formula_sum            'C80 H Bi4 O32 S24'
_chemical_formula_weight         3079.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   24.257(5)
_cell_length_b                   15.144(3)
_cell_length_c                   10.676(2)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.17
_cell_measurement_theta_min      4.52
_cell_volume                     3921.8(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21678
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        65.333
_diffrn_reflns_theta_max         65.333
_diffrn_reflns_theta_min         4.525
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.071
_exptl_absorpt_correction_T_max  0.5835
_exptl_absorpt_correction_T_min  0.3005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1413 before and 0.0800 after correction. The Ratio of minimum to maximum transmission is 0.5150. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             1453
_refine_diff_density_max         4.825
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3472
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1178P)^2^+77.7462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2404
_refine_ls_wR_factor_ref         0.2441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3203
_reflns_number_total             3472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10261_si_002.cif
_cod_data_source_block           ag125_a_0m_a
_cod_original_cell_volume        3921.9(13)
_cod_database_code               4133829
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C00C, C00F, C00J, C00G
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00R(H00R)
;
_shelx_res_checksum              60722
_shelx_hkl_checksum              99519
_olex2_submission_special_instructions 'No special instructions were received'