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_4133830
_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         'C120 H24 Bi6 O48 S36, O, 2(C3 N O)'
_chemical_formula_sum            'C126 H24 Bi6 N2 O51 S36'
_chemical_formula_weight         4789.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.512(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.5961(19)
_cell_length_b                   22.5938(19)
_cell_length_c                   17.288(2)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      65.10
_cell_measurement_theta_min      3.51
_cell_volume                     9830.1(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker PHOTON-100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            87447
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        65.442
_diffrn_reflns_theta_max         65.442
_diffrn_reflns_theta_min         2.599
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.484
_exptl_absorpt_correction_T_max  0.4649
_exptl_absorpt_correction_T_min  0.3214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellowish
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       prism
_exptl_crystal_F_000             4552
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.914
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.287
_refine_ls_abs_structure_details
;
 Flack x determined using 5782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         16719
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0637
_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^)+(0.1353P)^2^+85.2411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.2024
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                14293
_reflns_number_total             16719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10261_si_001.cif
_cod_data_source_block           BiDTT
_cod_original_cell_volume        9830.0(18)
_cod_database_code               4133830
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Uiso: O2(0.1) C3(0.1) N4(0.1) C5(0.1) C6(0.1)
3.a Free rotating group:
 O2(C3,N4,C5,C6)
3.b Aromatic/amide H refined with riding coordinates:
 C01N(H01N), C01W(H01W), C020(H020), C021(H021), C022(H022), C023(H023),
 C02A(H02A), C02C(H02C), C02N(H02N), C02O(H02O), C02Y(H02Y), C031(H031)
;
_olex2_submission_special_instructions 'No special instructions were received'