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_4519217
_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_formula_moiety         'C24 H12 Cl0.5 Mn1.5 N3 O6'
_chemical_formula_sum            'C24 H12 Cl0.5 Mn1.5 N3 O6'
_chemical_formula_weight         538.50
_chemical_name_systematic        Mn-TATB(Ru(bpy)3
_space_group_crystal_system      tetragonal
_space_group_IT_number           95
_space_group_name_Hall           'P 4cw 2c'
_space_group_name_H-M_alt        'P 43 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-30
_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            8
_cell_length_a                   17.976(3)
_cell_length_b                   17.976(3)
_cell_length_c                   26.415(3)
_cell_measurement_reflns_used    613
_cell_measurement_temperature    120
_cell_measurement_theta_max      14.0600
_cell_measurement_theta_min      3.4240
_cell_volume                     8536(2)
_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      120
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2083
_diffrn_reflns_av_unetI/netI     0.5065
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11698
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        24.400
_diffrn_reflns_theta_max         24.400
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.507
_exptl_crystal_colour            'metallic light red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.838
_exptl_crystal_description       prism
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6603
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.2728
_refine_ls_R_factor_gt           0.0959
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1890
_reflns_Friedel_coverage         0.704
_reflns_Friedel_fraction_full    0.905
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                1763
_reflns_number_total             6603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c17925_si_004.cif
_cod_data_source_block           NKMOF-9-Mn
_cod_original_cell_volume        8536(3)
_cod_original_formula_sum        'C24 H12 Cl0.50 Mn1.50 N3 O6'
_cod_database_code               4519217
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Restrained distances
 C19-C24 \\sim C23-C24 \\sim C23-C22 \\sim C22-C21 \\sim C20-C21 \\sim C20-C19
 with sigma of 0.01
 C14-C13 \\sim C15-C14 \\sim C15-C16 \\sim C11-C16 \\sim C12-C11 \\sim C12-C13
 with sigma of 0.01
 C14-C17 \\sim C25-C21 \\sim C1-C2
 with sigma of 0.001
 C4-C5 \\sim C4-C3 \\sim C3-C2 \\sim C7-C2 \\sim C7-C6 \\sim C5-C6
 with sigma of 0.01
 N3-C9 \\sim N2-C9 \\sim N2-C8 \\sim N1-C8 \\sim N1-C10 \\sim N3-C10
 with sigma of 0.01
 N2-C9 \\sim N3-C9 \\sim N3-C10 \\sim N1-C10 \\sim N1-C8 \\sim N2-C8
 with sigma of 0.01
 O4-C17 \\sim O3-C17
 with sigma of 0.001
 O2-C1 \\sim O1-C1
 with sigma of 0.001
 O5-C25 \\sim O6-C25
 with sigma of 0.001
2. Restrained planarity
 C14, C15, C16, C11, C12, C13
 with sigma of 0.01
 C5, C4, C6, C7, C2, C3
 with sigma of 0.01
 C24, C23, C22, C21, C20, C19
 with sigma of 0.01
 N2, C9, N3, C10, N1, C8
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C24) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C13, C14, C16, C11, C12, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C20, C21, C22, C24, C19, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C6, C5, C3, C4, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2, N3, N1, C9, C10, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C6(H6), C22(H22), C19(H19), C3(H3), C13(H13), C16(H16), C23(H23),
 C4(H4), C7(H7), C12(H12), C15(H15)
;
_shelx_res_checksum              44650
_shelx_hkl_checksum              65111
_shelx_fab_checksum              42907
_platon_squeeze_void_probe_radius 1.20