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_1570228
_publ_section_title
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 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         'Co5 Na12 H82 O109 W19'
_chemical_formula_sum            'Co5 H82 Na12 O109 W19'
_chemical_formula_weight         5807.49
_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_primary     dual
_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
;
2023-09-29 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.152(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.063(11)
_cell_length_b                   17.764(15)
_cell_length_c                   21.118(18)
_cell_measurement_reflns_used    4601
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.490
_cell_measurement_theta_min      2.252
_cell_volume                     4893(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_unetI/netI     0.1182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46062
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.624
_diffrn_reflns_theta_min         1.499
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.232
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1086 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.5198.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.942
_exptl_crystal_description       needle
_exptl_crystal_F_000             5090
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.866
_refine_diff_density_min         -3.246
_refine_diff_density_rms         0.510
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         13682
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+25.9747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8719
_reflns_number_total             13682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04002j2.cif
_cod_data_source_block           Co3W
_cod_depositor_comments
'Adding full bibliography for 1570226--1570229.cif.'
_cod_original_formula_sum        'Co5 Na12 H82 O109 W19'
_cod_database_code               1570228
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.390
_shelx_estimated_absorpt_t_min   0.090
_olex2_refinement_description
;
1. Shared sites
{Co3, W10}
2. Uiso/Uaniso restraints and constraints
Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Na6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O01J) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O27) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O55) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O46) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O14) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(O53) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O43)
\\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Co3) = Uanis(W10)
3. Others
 Fixed Sof: W10(0.5) Co3(0.5) Na54(0.5) O44(0.75) Na6(0.5) O43(0.75)
 O55(0.66667) O53(0.33333)
;
_shelx_res_checksum              72005
_olex2_submission_special_instructions 'No special instructions were received'