Accelerating water oxidation - a mixed Co/Fe polyoxometalate with improved turnover characteristics.
Soriano-López, Joaquín; Steuber, Friedrich W.; Mulahmetović, Muhamed; Besora, Maria; Clemente-Juan, Juan Modesto; O'Doherty, Mariah; Zhu, Nian-Yong; Hill, Craig L.; Coronado, Eugenio; Poblet, Josep M.; Schmitt, Wolfgang; Chemical science 14 (2023) 13722–13733; doi:10.1039/d3sc04002j

data_1570229
_publ_section_title
;
 Accelerating water oxidation - a mixed Co/Fe polyoxometalate with
 improved turnover characteristics.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              13722
_journal_page_last               13733
_journal_paper_doi               10.1039/d3sc04002j
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'Co4 Fe2 Na14 O90 W18, 5(H2O)'
_chemical_formula_sum            'Co4 Fe2 Na14 O97 W18'
_chemical_formula_weight         5530.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_audit_creation_date             2020-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-07 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.056(3)
_cell_length_b                   20.996(3)
_cell_length_c                   17.747(2)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.167
_cell_volume                     9709(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            106183
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.514
_diffrn_reflns_theta_min         1.502
_exptl_absorpt_coefficient_mu    22.355
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.1699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1796 before and 0.0906 after correction. The Ratio of minimum to maximum transmission is 0.2279. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.784
_exptl_crystal_description       oval
_exptl_crystal_F_000             9688
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.114
_refine_diff_density_max         6.309
_refine_diff_density_min         -6.518
_refine_diff_density_rms         0.667
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         19876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1178P)^2^+1495.3499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2410
_refine_ls_wR_factor_ref         0.2896
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                13340
_reflns_number_total             19876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04002j2.cif
_cod_data_source_block           Co2Fe2plate
_cod_depositor_comments
'Adding full bibliography for 1570226--1570229.cif.'
_cod_database_code               1570229
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.185
_shelx_estimated_absorpt_t_min   0.071
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(5)
 0.45(5)
2. Others
 Fixed Sof: Na02(0.5) Na2(0.5) Na6(0.5) Na8(0.5) Na9(0.5) Na10(0.5) Na03(0.5)
 Na11(0.5) Na12(0.5) O2AA(0.5) Na1B(0.5) Na3B(0.25) O7AA(0.5) O5BA(0.5)
 O4BA(0.5) Na0A(0.5) Na6B(0.5) Na6A(0.5) Na7B(0.25) Na5A(0.5) O73(0.5) Na73(0.5)
;
_shelx_res_checksum              31183
_olex2_submission_special_instructions 'No special instructions were received'