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_7131477
_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
'Co4.884 H30.6 Na10 O103.3 W19.116, 8(H2 O), 0.7(O1)'
_chemical_formula_sum            'Co4.88 H46.6 Na10 O112 W19.11'
_chemical_formula_weight         5871.04
_chemical_name_common            Co5POM
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1p9m2p
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-17 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.628(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1010(17)
_cell_length_b                   17.775(2)
_cell_length_c                   21.174(3)
_cell_measurement_reflns_used    12288
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.2
_cell_volume                     4920.9(11)
_computing_cell_refinement       'APEX2 (Bruker, 2014); SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014);XPREP(Sheldrick,2014)'
_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    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.233
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker AXS D8 Venture PHOTON CMOS'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            128007
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.634
_diffrn_reflns_theta_min         2.204
_diffrn_source                   'fine-focus microfocus tube'
_exptl_absorpt_coefficient_mu    23.211
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1008 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.5604.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.962
_exptl_crystal_density_meas      4.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             5198
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.881
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         12288
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0120P)^2^+118.4696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10609
_reflns_number_total             12288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06790k2.cif
_cod_data_source_block           dm_80_Co5POM
_cod_depositor_comments
'Adding full bibliography for 7131477--7131478.cif.'
_cod_original_formula_sum        'Co4.88 H46.60 Na10 O112 W19.11'
_cod_database_code               7131477
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.184
_shelx_estimated_absorpt_t_min   0.085
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{W10, Co3}
3. Uiso/Uaniso restraints and constraints
Uanis(O3W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(W10) = Uanis(Co3)
4. Others
 Sof(Co3)=1-FVAR(1)
 Sof(W10)=FVAR(1)
 Fixed Sof: O3W(0.65) H3WA(0.65) H3WB(0.65) O3WA(0.35)
5.a Everything fixed:
 H43A, H43B, H11A, H11B, H1WA, H1WB, H2WA, H2WB, H3WA, H3WB
5.b Rotating group:
 O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,
 H8WB), O9W(H9WA,H9WB), O10W(H10A,H10B)
;
_shelx_res_checksum              77104
_shelx_hkl_checksum              51407
_olex2_submission_special_instructions 'No special instructions were received'