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_4347192
_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
'C30 H37 Cl N6 O4 Ru2 S3 2+, 2(F6 P -), 1.5(O)'
_chemical_formula_sum            'C30 H37 Cl F12 N6 O5.5 P2 Ru2 S3'
_chemical_formula_weight         1193.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.220(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.1459(8)
_cell_length_b                   20.2059(4)
_cell_length_c                   17.8455(5)
_cell_measurement_reflns_used    48041
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.689
_cell_measurement_theta_min      1.334
_cell_volume                     8393.9(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48041
_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         25.689
_diffrn_reflns_theta_min         1.334
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.9126
_exptl_absorpt_correction_T_min  0.7904
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       block
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         7926
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+1.2436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6288
_reflns_number_total             7926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02869_si_002.cif
_cod_data_source_block           sn151-MeBDMSO
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C30 H37 Cl F12 N6 O5.50 P2 Ru2 S3'
_cod_database_code               4347192
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              48757
_shelx_hkl_checksum              8403