Microenvironment Regulation of Active Sites for Efficient Photocatalytic Reduction of Nitrobenzene
Liu, Jiang; Xu, Sha-Sha; Liang, Jia-Zheng; Yao, Su-Juan; Li, Ning; Shi, Jing-Wen; Lan, Yaqian; Chemical Communications  (2025) –; doi:10.1039/D5CC04423E

data_7135175
_publ_section_title
;
 Microenvironment Regulation of Active Sites for Efficient Photocatalytic
 Reduction of Nitrobenzene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC04423E
_journal_year                    2025
_chemical_formula_moiety         'C96 H48 Mn4 N8 O24, 2(C3 H7 N O), 0.71(H2 O1)'
_chemical_formula_sum            'C102 H63.43 Mn4 N10 O26.71'
_chemical_formula_weight         2076.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-07-03 deposited with the CCDC.	2025-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7346(5)
_cell_length_b                   13.7881(2)
_cell_length_c                   26.2173(4)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    210.00
_cell_measurement_theta_max      67.87
_cell_measurement_theta_min      3.37
_cell_volume                     8218.3(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      210.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50476
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.296
_diffrn_reflns_theta_min         3.892
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.717
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5477
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1332 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.7273.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             4237
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         7489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0330P)^2^+7.2758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6375
_reflns_number_total             7489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04423e2.cif
_cod_data_source_block           '__tmp__'
_cod_database_code               7135175
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.804
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O13)=Sof(H13A)=Sof(H13B)=FVAR(1)
3.a Riding coordinates:
 C49(H49A,H49B,H49C)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C7(H7), C9(H9), C11(H11), C15(H15), C17(H17), C19(H19),
 C21(H21), C23(H23), C27(H27), C29(H29), C30(H30), C31(H31), C33(H33), C35(H35),
  C37(H37), C39(H39), C41(H41), C43(H43), C44(H44), C45(H45), C47(H47),
 C51(H51), C3(H3)
3.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              11793
_olex2_submission_special_instructions 'No special instructions were received'