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_4514151
_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         'C13 H22 F3 Ir N2 O2 S'
_chemical_formula_sum            'C13 H22 F3 Ir N2 O2 S'
_chemical_formula_weight         519.60
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      110
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            16
_cell_length_a                   16.7238(18)
_cell_length_b                   16.7238(18)
_cell_length_c                   23.136(3)
_cell_measurement_reflns_used    3673
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.00
_cell_volume                     6470.8(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0457
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25207
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.443
_exptl_absorpt_correction_T_max  0.307
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000.00
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.140
_refine_diff_density_max         4.440
_refine_diff_density_min         -1.120
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1785 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3673
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0005Fo^2^ + 0.3670\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                3389
_reflns_number_total             3673
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            cs7b01068_si_005.cif
_cod_data_source_block           Tfen-IrH
_cod_original_cell_volume        6470.7(12)
_cod_database_code               4514151