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_4514828
_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            'C41 H36 Ir N6'
_chemical_formula_weight         804.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.797(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.476(2)
_cell_length_b                   14.367(2)
_cell_length_c                   34.464(6)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.20
_cell_volume                     7016.3(18)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            38735
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.417
_exptl_absorpt_coefficient_mu    3.844
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.570
_refine_diff_density_min         -2.445
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         15555
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+101.3867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12240
_reflns_number_total             15555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b02759_si_006.cif
_cod_data_source_block           mono
_cod_original_cell_volume        7016(2)
_cod_database_code               4514828
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.302
_shelx_estimated_absorpt_t_max   0.893
_shelx_res_checksum              33901
_shelx_hkl_checksum              95437