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_1570227
_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 H75 Na14 O105.5 W18'
_chemical_formula_sum            'Co4 Fe2 H75 Na14 O105.5 W18'
_chemical_formula_weight         5741.93
_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
_audit_creation_date             2020-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                99.3780(10)
_cell_angle_beta                 104.1870(10)
_cell_angle_gamma                101.318(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2859(6)
_cell_length_b                   13.6630(6)
_cell_length_c                   14.9308(6)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.35
_cell_volume                     2323.17(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.201
_diffrn_reflns_theta_min         1.559
_exptl_absorpt_coefficient_mu    23.369
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.2149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1382 before and 0.0619 after correction. The Ratio of minimum to maximum transmission is 0.2879. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    4.087
_exptl_crystal_description       rod
_exptl_crystal_F_000             2541
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.048
_refine_diff_density_max         5.598
_refine_diff_density_min         -5.698
_refine_diff_density_rms         0.568
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         17691
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0519P)^2^+88.9756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12429
_reflns_number_total             17691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04002j2.cif
_cod_data_source_block           Co2Fe2rod
_cod_depositor_comments
'Adding full bibliography for 1570226--1570229.cif.'
_cod_original_formula_sum        'Co4 H75 Fe2 Na14 O105.5 W18'
_cod_database_code               1570227
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.060
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O49B) \\sim Ueq, Uanis(O48B) \\sim Ueq, Uanis(O48A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Na4(0.5) Na5(0.5) Na7(0.5) O42(0.5) O44(0.5) O49B(0.75) O48A(0.5)
 O48B(0.5) Na6(0.75) Na9(0.75) O0AA(0.5)
4.a Rotating group:
 O35(H35A,H35B)
;
_shelx_res_checksum              49420
_olex2_submission_special_instructions 'No special instructions were received'