Stabilization and activation of polyoxometalate over poly(vinyl butylimidazolium) cations towards electrocatalytic water oxidation in alkaline media.
Singh, Ganga; Adhikary, Subhasis D.; Mandal, Debaprasad; Chemical communications (Cambridge, England) 59 (2023) 4774–4777; doi:10.1039/d2cc06790k

data_7131478
_publ_section_title
;
 Stabilization and activation of polyoxometalate over poly(vinyl
 butylimidazolium) cations towards electrocatalytic water oxidation in
 alkaline media.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4774
_journal_page_last               4777
_journal_paper_doi               10.1039/d2cc06790k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Co4 H18 Na10 O96 V2 W18, 8(H2 O), 2(H O)'
_chemical_formula_sum            'Co4 H36 Na10 O106 V2 W18'
_chemical_formula_weight         5609.09
_chemical_name_common            V-Co4_POM
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-20 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                93.531(8)
_cell_angle_beta                 105.350(8)
_cell_angle_gamma                115.746(8)
_cell_formula_units_Z            1
_cell_length_a                   12.931(4)
_cell_length_b                   13.390(4)
_cell_length_c                   15.661(5)
_cell_measurement_reflns_used    198
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.84
_cell_measurement_theta_min      2.80
_cell_volume                     2306.1(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker AXS D8 Venture PHOTON CMOS'
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22222
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.416
_diffrn_source                   'fine-focus microfocus tube'
_exptl_absorpt_coefficient_mu    23.410
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.6379.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.039
_exptl_crystal_description       'cylinderical rhombohedral'
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.508
_refine_diff_density_min         -2.378
_refine_diff_density_rms         0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         8255
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+85.7463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6615
_reflns_number_total             8255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06790k2.cif
_cod_data_source_block           dm_139_V-Co4_POM
_cod_depositor_comments
'Adding full bibliography for 7131477--7131478.cif.'
_cod_original_cell_volume        2306.2(12)
_cod_database_code               7131478
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.075
_shelx_estimated_absorpt_t_min   0.048
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O23) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed U11: O11(0.036441)
 Fixed U22: O11(0.009751)
 Fixed U33: O11(0.02111)
4.a Everything fixed:
 H44, H1WA, H1WB, H4WA, H4WB, H7W
4.b Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O8W(H8WA,
 H8WB), O9W(H9WA,H9WB)
;
_shelx_res_checksum              25187
_shelx_hkl_checksum              27692
_olex2_submission_special_instructions 'No special instructions were received'