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_4518674
_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            'C26 H31 N4 O7 P Ru'
_chemical_formula_weight         643.59
_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                 101.328(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5083(10)
_cell_length_b                   8.8372(8)
_cell_length_c                   27.547(3)
_cell_measurement_reflns_used    2672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.42
_cell_volume                     2747.0(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 0.985
_diffrn_measured_fraction_theta_max 0.979
_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  0.0723
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17410
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         1.814
_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    0.681
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.527
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0630P)^2^+2.9503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3790
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05363_si_002.cif
_cod_data_source_block           mo_TpaaquaH2O2_0m
_cod_original_cell_volume        2747.0(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4518674
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              87779
_shelx_hkl_checksum              6368