Synthesis and Characterization of Strong Cyclometalated Iridium Photoreductants for Application in Photocatalytic Aryl Bromide Hydrodebromination
Shon, Jong-Hwa; Sittel, Steven; Teets, Thomas S.; ACS Catalysis 9 (2019) 8646–; doi:10.1021/acscatal.9b02759

data_4514827
_publ_section_title
;
 Synthesis and Characterization of Strong Cyclometalated Iridium
 Photoreductants for Application in Photocatalytic Aryl Bromide
 Hydrodebromination
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              8646
_journal_paper_doi               10.1021/acscatal.9b02759
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C43 H42 Ir N6'
_chemical_formula_weight         835.02
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                85.2561(10)
_cell_angle_beta                 69.5849(9)
_cell_angle_gamma                77.2239(9)
_cell_formula_units_Z            2
_cell_length_a                   10.1805(7)
_cell_length_b                   13.1835(9)
_cell_length_c                   14.4356(10)
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.19
_cell_volume                     1770.8(2)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10425
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         2.179
_exptl_absorpt_coefficient_mu    3.811
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       needle
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.605
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.0791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6906
_reflns_number_total             7331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b02759_si_002.cif
_cod_data_source_block           js8
_cod_database_code               4514827
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.449
_shelx_estimated_absorpt_t_max   0.804
_shelx_res_checksum              33364
_shelx_hkl_checksum              9050