Template-Directed Fabrication of Highly Efficient Metal-Organic Framework Photocatalysts.
Liu, Wansheng; Yang, Yi; Yang, Xiaojie; Peng, Yun-Lei; Cheng, Peng; Zhang, Zhenjie; Chen, Yao; ACS applied materials & interfaces 13 (2021) 58619–58629; doi:10.1021/acsami.1c17925

data_4519218
_publ_section_title
;
 Template-Directed Fabrication of Highly Efficient Metal-Organic Framework
 Photocatalysts.
;
_journal_issue                   49
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              58619
_journal_page_last               58629
_journal_paper_doi               10.1021/acsami.1c17925
_journal_volume                  13
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H13 N O2 S'
_chemical_formula_sum            'C15 H13 N O2 S'
_chemical_formula_weight         271.32
_chemical_name_systematic        sfjyd
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8079(2)
_cell_length_b                   10.0724(3)
_cell_length_c                   15.1907(4)
_cell_measurement_reflns_used    5266
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.9550
_cell_measurement_theta_min      4.0410
_cell_volume                     1347.67(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      298
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -9.00  88.00   1.00   15.00    --   18.55  72.00  11.00   97
  2  \w    -45.00  42.00   1.00   15.00    --   18.55 -72.00-118.00   87
  3  \w    -65.00 -40.00   1.00   15.00    --  -19.56 -72.00-118.00   25
  4  \w    -23.00   2.00   1.00   15.00    --  -19.56  72.00  11.00   25
  5  \w     35.00  60.00   1.00   15.00    --   18.55 178.00  30.00   25
  6  \w    -11.00  60.00   1.00   15.00    --   18.55 -99.00  90.00   71
  7  \w    -48.00  50.00   1.00   15.00    --  -19.56  77.00 120.00   98
  8  \w    -90.00  10.00   1.00   15.00    --  -19.56 -77.00 120.00  100
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0186778000
_diffrn_orient_matrix_UB_12      -0.0597854000
_diffrn_orient_matrix_UB_13      0.0221841000
_diffrn_orient_matrix_UB_21      -0.0444078000
_diffrn_orient_matrix_UB_22      -0.0364025000
_diffrn_orient_matrix_UB_23      -0.0305723000
_diffrn_orient_matrix_UB_31      0.0645681000
_diffrn_orient_matrix_UB_32      -0.0077694000
_diffrn_orient_matrix_UB_33      -0.0274129000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11729
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 788 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2313
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1572P)^2^+0.6257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2223
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                2052
_reflns_number_total             2313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c17925_si_006.cif
_cod_data_source_block           8b
_cod_database_code               4519218
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.954
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C1 \\sim C3-C2 \\sim C4-C3
 with sigma of 0.0001
 S1-C4 \\sim S1-C1
 with sigma of 0.001
3. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N1(H1), C12(H12), C15(H15), C2(H2), C14(H14), C1(H1A), C13(H13)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              55246
_shelx_hkl_checksum              32727
_olex2_date_sample_data_collection 2021-08-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.471