Two reduced phosphomolybdate-based metal-organic complexes modified by tunable bis-1<i>H</i>-benzimidazole ligands for enhanced photocatalytic Cr(VI) reduction.
Li, Feng-Cai; Li, Xi-Li; Pan, Yu-Zhe; Gao, Cong-Li; Yang, Qing-Xiang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15073–15083; doi:10.1039/d5dt01698c

data_7719483
_publ_section_title
;
 Two reduced phosphomolybdate-based metal-organic complexes modified by
 tunable bis-1<i>H</i>-benzimidazole ligands for enhanced photocatalytic
 Cr(VI) reduction.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15073
_journal_page_last               15083
_journal_paper_doi               10.1039/d5dt01698c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'H18 Mn2 Mo12 O64 P8, 3(C18 H20 N4), 8(H2O)'
_chemical_formula_sum            'C54 H94 Mn2 Mo12 N12 O72 P8'
_chemical_formula_weight         3572.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-08-10 deposited with the CCDC.	2025-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                65.575(2)
_cell_angle_beta                 65.603(2)
_cell_angle_gamma                68.792(2)
_cell_formula_units_Z            1
_cell_length_a                   14.345(2)
_cell_length_b                   14.641(2)
_cell_length_c                   15.037(2)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.49
_cell_volume                     2548.4(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            60660
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.708
_diffrn_reflns_theta_min         1.565
_exptl_absorpt_coefficient_mu    1.903
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.645
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10728
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0200P)^2^+36.4997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8732
_reflns_number_total             10728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01698c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7719483--7719484.cif.'
_cod_database_code               7719483
_shelx_shelxl_version_number     2014/7
_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 O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O35) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C8) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O35) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Rotating group:
 O28(H28A,H28B)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C26(H26A,H26B),
 C27(H27A,H27B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C1(H1A), C3(H3), C4(H4A), C5(H5), C6(H6), C12(H12), C14(H14),
 C16(H16), C17(H17), C15(H15), N5(H5A), C20(H20), C21(H21), C22(H22), C23(H23),
 C25(H25)
3.d Idealised tetrahedral OH refined as rotating group:
 O10(H10), O19(H19), O26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'