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_4106363
_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         'C20 H29 F3 Ir N O5 '
_chemical_formula_sum            'C20 H29 F3 Ir N O5'
_chemical_formula_weight         612.67
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 113.904(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.6660(16)
_cell_length_b                   10.4157(12)
_cell_length_c                   16.7525(18)
_cell_measurement_reflns_used    7354
_cell_measurement_temperature    223.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2339.6(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 6.85
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7748
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    5.775
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private comm.'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       Block
_exptl_crystal_F_000             1200.00
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.20
_refine_diff_density_min         -1.29
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1651 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.007(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4331
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.0070
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0118P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                3661
_reflns_number_total             4331
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja2004522_si_002_1.cif
_cod_data_source_block           Cp*Ir(PyrAlkox)OTFA
_cod_original_formula_sum        'C20 H29 F3 Ir N O5 '
_cod_database_code               4106363