Evolution of Iridium-Based Molecular Catalysts during Water Oxidation with Ceric Ammonium Nitrate
Douglas B. Grotjahn; Derek B. Brown; Jessica K. Martin; David C. Marelius; Marie-Caline Abadjian; Hai N. Tran; Gregory Kalyuzhny; Kenneth S. Vecchio; Zephen G. Specht; Sara A. Cortes-Llamas; Valentin Miranda-Soto; Christoffel van Niekerk; Curtis E. Moore; Arnold L. Rheingold; Journal of the American Chemical Society 133 (2011) 19024–19027; doi:10.1021/ja203095k

data_4107160
_publ_section_title
;
 Evolution of Iridium-Based Molecular Catalysts during Water Oxidation
 with Ceric Ammonium Nitrate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19024
_journal_page_last               19027
_journal_paper_doi               10.1021/ja203095k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C24 H30 F6 Ir N5 O6 S2'
_chemical_formula_weight         854.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0830(10)
_cell_angle_beta                 106.9700(10)
_cell_angle_gamma                111.3280(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7906(5)
_cell_length_b                   12.3495(7)
_cell_length_c                   14.1529(8)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.20
_cell_volume                     1513.45(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22626
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.633
_exptl_absorpt_correction_T_max  0.5632
_exptl_absorpt_correction_T_min  0.3905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       Block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+5.7545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                6178
_reflns_number_total             6765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203095k_si_003.cif
_cod_data_source_block           Grot345
_cod_database_code               4107160