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_7719484
_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         'H16 Mo12 Ni O62 P8, 3(C18 H20 N4),  6(H2O)'
_chemical_formula_sum            'C54 H88 Mo12 N12 Ni O68 P8'
_chemical_formula_weight         3451.08
_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                98.590(2)
_cell_angle_beta                 110.121(2)
_cell_angle_gamma                105.761(2)
_cell_formula_units_Z            1
_cell_length_a                   13.3340(17)
_cell_length_b                   14.8273(19)
_cell_length_c                   15.1027(19)
_cell_measurement_reflns_used    9571
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.18
_cell_volume                     2599.0(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 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_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            63042
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.618
_diffrn_reflns_theta_min         1.481
_exptl_absorpt_coefficient_mu    1.804
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5971
_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    2.172
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.739
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10843
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0677P)^2^+35.4827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9695
_reflns_number_total             10843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01698c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7719483--7719484.cif.'
_cod_database_code               7719484
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained planarity
 C19, C20, C21, C22, C23, C24
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim
O33: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C15)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H26C)=Sof(H26D)=Sof(C28)=Sof(H28A)=Sof(H28B)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(1)
5.a Free rotating group:
 O32(H32A,H32B)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C26(H26A,H26B),
 C26(H26C,H26D), C27(H27A,H27B), C28(H28A,H28B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C2(H2), C3(H3), C4(H4A), C5(H5), C7(H7), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), N5(H5A), C20(H20A), C21(H21), C22(H22), C23(H23),
  C25(H25)
5.d Idealised tetrahedral OH refined as rotating group:
 O11(H11), O20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'