Iridium Dihydroxybipyridine Complexes Show That Ligand Deprotonation Dramatically Speeds Rates of Catalytic Water Oxidation
Joseph DePasquale; Ismael Nieto; Lauren E. Reuther; Corey J. Herbst-Gervasoni; Jared J. Paul; Vadym Mochalin; Matthias Zeller; Christine M. Thomas; Anthony W. Addison; Elizabeth T. Papish; Inorganic Chemistry 52 (2013) 9175–9183; doi:10.1021/ic302448d

data_4335691
_publ_contact_author_address
;3141 Chestnut St.
Drexel University
Philadelphia PA 19104 
;
_publ_contact_author_email       ep322@drexel.edu
_publ_contact_author_name        'Elizabeth T. Papish'
_publ_contact_author_phone       215-895-2666
_publ_section_title
;
 Iridium Dihydroxybipyridine Complexes Show That Ligand Deprotonation
 Dramatically Speeds Rates of Catalytic Water Oxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9175
_journal_page_last               9183
_journal_paper_doi               10.1021/ic302448d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C32 H12 B F24, C20 H23 Cl Ir N2 O2'
_chemical_formula_sum            'C52 H35 B Cl F24 Ir N2 O2'
_chemical_formula_weight         1414.28
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2012
_cell_angle_alpha                106.619(2)
_cell_angle_beta                 95.770(2)
_cell_angle_gamma                104.581(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5011(16)
_cell_length_b                   13.0829(17)
_cell_length_c                   17.668(2)
_cell_measurement_reflns_used    9381
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.12
_cell_measurement_theta_min      2.28
_cell_volume                     2632.9(6)
_computing_cell_refinement       'SAINT V8.18C (Bruker, 2012)'
_computing_data_collection       'Apex2  v2012.4-3 (Bruker, 2012)'
_computing_data_reduction        'SAINT V8.18C (Bruker, 2012)'
_computing_molecular_graphics    'Shelxtl (Bruker, 2003)'
_computing_publication_material  'Shelxtl (Bruker, 2003)'
_computing_structure_refinement
;  
SHELXL-2012 (Sheldrick, 2012), 
SHELXLE Rev576, Shelxle (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61487
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         1.700
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2  v2012.4-3 (Bruker, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         15880
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+2.3334P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14839
_reflns_number_total             15880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic302448d_si_002_1.cif
_cod_data_source_block           complex5_12mz369_0m
_cod_database_code               4335691
_diffrn_reflns_sigmai/neti       0.0216
_shelxl_version_number           2012-4
_shelx_res_checksum              49438