Evidence for Oxidative Decay of a Ru-Bound Ligand during Catalyzed Water Oxidation
Kagalwala, Husain N.; Tong, Lianpeng; Zong, Ruifa; Kohler, Lars; Ahlquist, Mårten S. G.; Fan, Ting; Gagnon, Kevin J.; Thummel, Randolph P.; ACS Catalysis 7 (2017) 2607–; doi:10.1021/acscatal.6b03278

data_4514106
_publ_section_title
;
 Evidence for Oxidative Decay of a Ru-Bound Ligand during Catalyzed Water
 Oxidation
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              2607
_journal_paper_doi               10.1021/acscatal.6b03278
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C29 H20 F3 N5 O6 Ru S'
_chemical_formula_weight         724.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                84.085(2)
_cell_angle_beta                 76.900(2)
_cell_angle_gamma                69.246(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4166(3)
_cell_length_b                   11.0300(4)
_cell_length_c                   16.0250(6)
_cell_measurement_reflns_used    9184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.965
_cell_measurement_theta_min      2.552
_cell_volume                     1354.52(9)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31575
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         41.984
_diffrn_reflns_theta_min         2.153
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 - Bruker AXS, Madison WI'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         14122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0251P)^2^+0.7955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11877
_reflns_number_total             14122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b03278_si_002.cif
_cod_data_source_block           LT62
_cod_database_code               4514106
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              38825
_shelx_hkl_checksum              76288