Fate of the Molecular Ru–Phosphonate Water Oxidation Catalyst under Turnover Conditions
Vereshchuk, Nataliia; Holub, Jan; Gil-Sepulcre, Marcos; Benet-Buchholz, Jordi; Llobet, Antoni; ACS Catalysis  (2021) 5240–5247; doi:10.1021/acscatal.0c05363

data_4518673
_publ_section_title
;
 Fate of the Molecular Ru--Phosphonate Water Oxidation Catalyst under
 Turnover Conditions
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              5240
_journal_page_last               5247
_journal_paper_doi               10.1021/acscatal.0c05363
_journal_year                    2021
_chemical_formula_sum            'C22 H24 N4 O14 P2 Ru'
_chemical_formula_weight         731.46
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 105.261(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8814(11)
_cell_length_b                   18.093(2)
_cell_length_c                   15.1203(17)
_cell_measurement_reflns_used    9144
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.41
_cell_volume                     2607.9(5)
_computing_cell_refinement       'Bruker APEX2 v2014.9-0'
_computing_data_collection       'Bruker APEX2 v2014.9-0'
_computing_data_reduction        'Bruker APEX2 v2014.9-0'
_computing_molecular_graphics
;
 SHELXle: C.B. Huebschle, G.M. Sheldrick & B. Dittrich
 J.Appl.Cryst. (2011) 44, 1281-1284.
;
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
;
  SHELXT V2018/2 (Sheldrick 2018); G.M. Sheldrick (2015)
 "SHELXT - Integrated space-group and crystal-structure
 determination", Acta Cryst., A71, 3-8. 
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65399
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.161
_diffrn_reflns_theta_min         1.793
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       Block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7415
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0228P)^2^+5.0978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6636
_reflns_number_total             7415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05363_si_002.cif
_cod_data_source_block           mo_bcp27bulk_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518673
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              27957
_shelx_hkl_checksum              62494