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_4514829
_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            'C39 H45 Ir N4'
_chemical_formula_weight         761.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.6400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3918(10)
_cell_length_b                   14.4386(12)
_cell_length_c                   20.4434(18)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.30
_cell_volume                     3315.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46346
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         1.813
_exptl_absorpt_coefficient_mu    4.061
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.561
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+3.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6726
_reflns_number_total             7583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b02759_si_003.cif
_cod_data_source_block           ss1
_cod_database_code               4514829
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.483
_shelx_estimated_absorpt_t_max   0.641
_shelx_res_checksum              44533
_shelx_hkl_checksum              67293