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_4106365
_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 Cl Ir N O3 '
_chemical_formula_sum            'C20 H29 Cl Ir N O3'
_chemical_formula_weight         559.11
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.0590(3)
_cell_length_b                   12.0323(3)
_cell_length_c                   15.5916(4)
_cell_measurement_reflns_used    17164
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      3.1
_cell_volume                     2074.70(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18655
_diffrn_reflns_theta_full        30.97
_diffrn_reflns_theta_max         30.97
_exptl_absorpt_coefficient_mu    6.600
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       rod
_exptl_crystal_F_000             1096.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.72
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2810 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     240
_refine_ls_number_reflns         6427
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0148P)^2^+0.6290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                5928
_reflns_number_total             6427
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja2004522_si_002_3.cif
_cod_data_source_block           Cp*Ir(PyrAlkox)Cl
_cod_original_formula_sum        'C20 H29 Cl Ir N O3 '
_cod_database_code               4106365