Structure-induced selective adsorption of diverse dyes and Cr(vi) photoreduction using two new polyoxometalate-based metal–viologen complexes
Wang, Xiuli; Yang, Lin; Zhang, Zhong; CrystEngComm 26 (2024) 1363–1370; doi:10.1039/D3CE01227A

data_7248097
_publ_section_title
;
 Structure-induced selective adsorption of diverse dyes and Cr(vi)
 photoreduction using two new polyoxometalate-based metal--viologen
 complexes
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1363
_journal_page_last               1370
_journal_paper_doi               10.1039/D3CE01227A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety
'2(O40 P W12), C72 H60 Cu N8 O8, 3(H2 O), 4[H2O]'
_chemical_formula_sum            'C72 H75 Cu N8 O95 P2 W24'
_chemical_formula_weight         7110.28
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-19 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                95.4120(10)
_cell_angle_beta                 106.1440(10)
_cell_angle_gamma                93.0910(10)
_cell_formula_units_Z            1
_cell_length_a                   13.0872(6)
_cell_length_b                   13.6972(7)
_cell_length_c                   19.4602(9)
_cell_measurement_reflns_used    5431
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     3324.2(3)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.266
_diffrn_reflns_theta_min         1.499
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    20.953
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    3.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3158
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.514
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         16325
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0554P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10984
_reflns_number_total             16325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01227a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7248096--7248097.cif.'
_cod_database_code               7248097
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.102
_shelx_estimated_absorpt_t_min   0.081
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O2_$1-O1
 2.9 with sigma of 0.02
 O1-O2_$1
 3.2 with sigma of 0.02
3. Rigid bond restraints
 C15, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C31, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33, C36
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
N3 \\sim C19: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
Uanis(C29) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C29(H29A,H29B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35)
6.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 37 electrons were 
found in a volume of 164\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[H2O] per Unit Cell 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60677
_shelx_fab_checksum              49337
_olex2_submission_special_instructions 'No special instructions were received'