Electrochemical C‒H Bond Activation via Cationic Iridium Hydride Pincer Complexes
Lindley, Brian; Walden, Andrew G.; Brasacchio, Ann Marie; Casuras, Andrea; Lease, Nicholas; Chen, Chun-Hsing; Goldman, Alan S.; Miller, Alexander James Minden; Chemical Science  (2019) –; doi:10.1039/C9SC03076J

data_1552254
_publ_section_title
;
 Electrochemical C--H Bond Activation via Cationic Iridium Hydride Pincer
 Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03076J
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C67 H65 B1 F24 Ir1 N1 P2'
_chemical_formula_sum            'C67 H65 B F24 Ir N P2'
_chemical_formula_weight         1605.19
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-20
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_audit_update_record
;
2019-06-21 deposited with the CCDC.    2019-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3252(3)
_cell_length_b                   13.3891(3)
_cell_length_c                   37.2399(9)
_cell_measurement_reflns_used    9074
_cell_measurement_temperature    150
_cell_measurement_theta_max      70
_cell_measurement_theta_min      4
_cell_volume                     6644.1(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            61902
_diffrn_reflns_theta_full        70.130
_diffrn_reflns_theta_max         70.130
_diffrn_reflns_theta_min         2.373
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.322
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3208.000
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         12482
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.0463108
_refine_ls_shift/su_mean         0.0023989
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +23.63P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1021
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1021
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              0
_reflns_number_gt                11813
_reflns_number_total             12538
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.73
_oxford_diffrn_Wilson_scale      362.13
_oxford_refine_ls_r_factor_ref   0.0451
_oxford_refine_ls_scale          0.057341(7)
_oxford_reflns_number_all        12482
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'AW_F_077 in P212121 #19'
_cod_data_source_file            c9sc03076j2.cif
_cod_data_source_block           AW_F_077_f
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C67 H65 B1 F24 Ir1 N1 P2'
_cod_database_code               1552254