Establishing the Family of Diruthenium Water Oxidation Catalysts Based on the Bis(bipyridyl)pyrazolate Ligand System.
Neudeck, Sven; Maji, Somnath; López, Isidoro; Dechert, Sebastian; Benet-Buchholz, Jordi; Llobet, Antoni; Meyer, Franc; Inorganic chemistry 55 (2016) 2508–2521; doi:10.1021/acs.inorgchem.5b02869

data_4347193
_publ_section_title
;
 Establishing the Family of Diruthenium Water Oxidation Catalysts Based on
 the Bis(bipyridyl)pyrazolate Ligand System.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2508
_journal_page_last               2521
_journal_paper_doi               10.1021/acs.inorgchem.5b02869
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C43 H36 Br Cl N10 O Ru2 2+, 2(F6 P -), 2(C3 H6 O)'
_chemical_formula_sum            'C49 H48 Br Cl F12 N10 O3 P2 Ru2'
_chemical_formula_weight         1432.41
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                74.376(5)
_cell_angle_beta                 81.935(5)
_cell_angle_gamma                63.706(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1230(8)
_cell_length_b                   14.7595(9)
_cell_length_c                   14.9169(9)
_cell_measurement_reflns_used    31609
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.777
_cell_measurement_theta_min      1.418
_cell_volume                     2683.9(3)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1378
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.777
_diffrn_reflns_theta_min         1.418
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.8297
_exptl_absorpt_correction_T_min  0.6590
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.540
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         10125
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0727P)^2^+2.6218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8343
_reflns_number_total             10125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02869_si_002.cif
_cod_data_source_block           sn5-Br1ClH2O
_cod_database_code               4347193
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.828
_shelx_res_checksum              43315
_shelx_hkl_checksum              37892