Distinguishing Homogeneous from Heterogeneous Catalysis in Electrode-Driven Water Oxidation with Molecular Iridium Complexes
Nathan D. Schley; James D. Blakemore; Navaneetha K. Subbaiyan; Christopher D. Incarvito; Francis D'Souza; Robert H. Crabtree; Gary W. Brudvig; Journal of the American Chemical Society 133 (2011) 10473–10481; doi:10.1021/ja2004522

data_4106364
_publ_contact_author_email       robert.crabtree@yale.edu
_publ_contact_author_fax         '+203 432 6144'
_publ_contact_author_name        'Dr. Robert H Crabtree'
_publ_contact_author_phone       '+203 432 3925'
_publ_section_title
;
 Distinguishing Homogeneous from Heterogeneous Catalysis in
 Electrode-Driven Water Oxidation with Molecular Iridium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10473
_journal_page_last               10481
_journal_paper_doi               10.1021/ja2004522
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C10 H25 Ir O9 S'
_chemical_formula_sum            'C10 H25 Ir O9 S'
_chemical_formula_weight         513.58
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.952(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   17.8157(13)
_cell_length_b                   8.8933(7)
_cell_length_c                   20.7581(16)
_cell_measurement_reflns_used    11530
_cell_measurement_temperature    223
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      3.06
_cell_volume                     3287.0(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD (SCX mini)'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13381
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.311
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             2000.00
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     8
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0201P)^2^+8.6866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                3487
_reflns_number_total             4950
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja2004522_si_002_2.cif
_cod_data_source_block           Cp*Ir(H2O)3SO4
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4106364