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_7248096
_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
'C54 H42 Co3 N6 O51 W12, H2 O, 4.6[H2O], 0.4[H2O]'
_chemical_formula_sum            'C54 H55 Co3 N6 O57 W12'
_chemical_formula_weight         4083.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5892(9)
_cell_length_b                   21.9646(15)
_cell_length_c                   26.1741(17)
_cell_measurement_reflns_used    2051
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     8387.4(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_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 0.999
_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  0.1363
_diffrn_reflns_av_unetI/netI     0.1410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46919
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.210
_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    17.066
_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    3.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             7384
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.278
_refine_diff_density_min         -3.448
_refine_diff_density_rms         0.357
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1109
_refine_ls_number_reflns         14377
_refine_ls_number_restraints     1517
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+25.1321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                9584
_reflns_number_total             14377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01227a2.cif
_cod_data_source_block           55
_cod_depositor_comments
'Adding full bibliography for 7248096--7248097.cif.'
_cod_database_code               7248096
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.132
_shelx_estimated_absorpt_t_min   0.105
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70(3)
 0.30(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O5-C5
 1.25 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Co3 \\sim O8 \\sim O9 \\sim O10 \\sim O11: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(W3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Co3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: W9(0.9) W11(0.9) W12(0.9) O12(0.7) W3(0.1) W7(0.1) W13(0.1) O13(0.3)
7.a Riding coordinates:
 O6W(H6WA,H6WB)
7.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C53(H53A,H53B), C54(H54A,H54B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C8(H8), C10(H10), C12(H12), C14(H14), C16(H16), C17(H17),
 C35(H35), C37(H37), C19(H19), C18(H18), C21(H21), C23(H23), C24(H24), C27(H27),
  C7(H7), C15(H15), C31(H31), C32(H32), C34(H34), C36(H36), C38(H38), C33(H33),
 C40(H40), C44(H44), C46(H46), C48(H48), C43(H43), C45(H45), C47(H47), C49(H49),
  C25(H25), C13(H13), C50(H50), C52(H52)
7.d Fitted hexagon refined as free rotating group:
 N1(C1,C4,C6,C8,C10), C17(C35,C9,C37,C19,C39), C27(C7,C29,C15,C31,N5), C30(C32,
 C34,N6,C36,C38), C40(C42,C44,C46,N2,C48), C47(C3,C49,C25,C51,C13)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 208 electrons were 
found in a volume of 632\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
4.6[H2O], 0.4[H2O] per Unit Cell 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52962
_shelx_fab_checksum              94568
_olex2_submission_special_instructions 'No special instructions were received'