A two-dimensional Bi-based porphyrin metal–organic framework photocatalyst for white light-driven selective oxidation of sulfides
Xie, Dale; Wang, Sheng; Li, Shihao; Yang, Wenqing; Feng, Yi-Si; Catalysis Science & Technology 12 (2022) 3254–3260; doi:10.1039/D2CY00387B

data_1566769
_publ_section_title
;
 A two-dimensional Bi-based porphyrin metal--organic framework
 photocatalyst for white light-driven selective oxidation of sulfides
;
_journal_issue                   10
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3254
_journal_page_last               3260
_journal_paper_doi               10.1039/D2CY00387B
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C48 H28 Bi N4 O9'
_chemical_formula_sum            'C48 H28 Bi N4 O9'
_chemical_formula_weight         1013.72
_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             2021-04-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-04-08 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.300(3)
_cell_length_b                   17.400
_cell_length_c                   18.975(3)
_cell_measurement_reflns_used    5423
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.956
_cell_measurement_theta_min      2.354
_cell_volume                     5711.9(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.861
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.1955
_diffrn_reflns_Laue_measured_fraction_full 0.861
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31822
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.238
_diffrn_reflns_theta_min         1.588
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.133
_exptl_absorpt_correction_T_max  0.5
_exptl_absorpt_correction_T_min  0.3
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.196(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.719
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         11196
_refine_ls_number_restraints     341
_refine_ls_restrained_S_all      0.727
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                6597
_reflns_number_total             11196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy00387b2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1566769.cif.'
_cod_original_cell_volume        5712.0(14)
_cod_database_code               1566769
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.303
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.804(11)
 0.196(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C00J-C00M
 1.35 with sigma of 0.01
 C01A-C01F
 1.32 with sigma of 0.01
 C00X-C014
 1.35 with sigma of 0.01
 C00B-C00C
 1.32 with sigma of 0.01
 C00F-C00Q
 1.35 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C006) \\sim Ueq, Uanis(C008) \\sim Ueq, Uanis(C009) \\sim Ueq,
Uanis(C00B) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(C00D) \\sim Ueq,
Uanis(C00E) \\sim Ueq, Uanis(C00F) \\sim Ueq, Uanis(C00H) \\sim Ueq,
Uanis(C00J) \\sim Ueq, Uanis(C00K) \\sim Ueq, Uanis(C00L) \\sim Ueq,
Uanis(C00M) \\sim Ueq, Uanis(C00N) \\sim Ueq, Uanis(C00Q) \\sim Ueq,
Uanis(C00R) \\sim Ueq, Uanis(C00S) \\sim Ueq, Uanis(C00T) \\sim Ueq,
Uanis(C00V) \\sim Ueq, Uanis(C00W) \\sim Ueq, Uanis(C00X) \\sim Ueq,
Uanis(C00Y) \\sim Ueq, Uanis(C010) \\sim Ueq, Uanis(C011) \\sim Ueq,
Uanis(C012) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C014) \\sim Ueq,
Uanis(C015) \\sim Ueq, Uanis(C017) \\sim Ueq, Uanis(C018) \\sim Ueq,
Uanis(C019) \\sim Ueq, Uanis(C01A) \\sim Ueq, Uanis(C01B) \\sim Ueq,
Uanis(C01C) \\sim Ueq, Uanis(C01D) \\sim Ueq, Uanis(C01E) \\sim Ueq,
Uanis(C01F) \\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C01H) \\sim Ueq,
Uanis(C01J) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(C01L) \\sim Ueq,
Uanis(C01N) \\sim Ueq, Uanis(C01O) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C01R) \\sim Ueq, Uanis(C01T) \\sim Ueq, Uanis(C01V) \\sim Ueq,
Uanis(N004) \\sim Ueq, Uanis(N007) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N00Z)
\\sim Ueq, Uanis(C01J) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(O016)
\\sim Ueq, Uanis(O00I) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
5.a Rotating group:
 O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C006(H006), N1(H1), C00E(H00E), C00F(H00F), C00H(H00H), C00K(H00K),
 C00N(H00N), C00Q(H00Q), C00S(H00S), C00V(H00V), C00Y(H00Y), N00Z(H00Z),
 C012(H012), C013(H013), C015(H015), C017(H017), C01C(H01C), C01D(H01D),
 C01F(H01F), C01G(H01G), C01L(H01L), C01N(H01N), C01O(H01O), C01R(H01R),
 C01T(H01T), C01V(H01V)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52760
_shelx_fab_checksum              31002
_olex2_submission_special_instructions 'No special instructions were received'