A Bifunctional Iridium Catalyst Modified for Persistent Hydrogen Generation from Formic Acid: Understanding Deactivation via Cyclometalation of a 1,2-Diphenylethylenediamine Motif
Matsunami, Asuka; Kuwata, Shigeki; Kayaki, Yoshihito; ACS Catalysis  (2017) 4479–; doi:10.1021/acscatal.7b01068

data_4514152
_publ_section_title
;
 A Bifunctional Iridium Catalyst Modified for Persistent Hydrogen
 Generation from Formic Acid: Understanding Deactivation via
 Cyclometalation of a 1,2-Diphenylethylenediamine Motif
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              4479
_journal_paper_doi               10.1021/acscatal.7b01068
_journal_year                    2017
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C25 H28 F3 Ir N2 O2 S'
_chemical_formula_sum            'C25 H28 F3 Ir N2 O2 S'
_chemical_formula_weight         669.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 111.0730
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   20.7776
_cell_length_b                   14.3517
_cell_length_c                   18.8130
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.07
_cell_volume                     5234.747
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1.1'
_computing_publication_material  'CrystalStructure 4.1.1 (Rigaku, 2015)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21609
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.006
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.240
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2624.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.670
_refine_diff_density_min         -2.370
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  3654 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.020(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     670
_refine_ls_number_reflns         9804
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 0.4288\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                8137
_reflns_number_total             9804
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            cs7b01068_si_002.cif
_cod_data_source_block           TfIrC-CH3CNetherv4
_cod_original_cell_volume        5234.7471
_cod_database_code               4514152