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_1552252
_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         'C63 H65 B1 F24 Ir1 N1 P2'
_chemical_formula_sum            'C63 H65 B F24 Ir N P2'
_chemical_formula_weight         1557.15
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     SUPERFLIP
_audit_creation_date             2019-01-04
_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                   13.4206(9)
_cell_length_b                   13.4206(9)
_cell_length_c                   35.170(3)
_cell_measurement_reflns_used    4075
_cell_measurement_temperature    100
_cell_measurement_theta_max      70
_cell_measurement_theta_min      5
_cell_volume                     6334.6(8)
_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      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.958
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            39025
_diffrn_reflns_theta_full        34.344
_diffrn_reflns_theta_max         70.089
_diffrn_reflns_theta_min         3.525
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.559
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.81
_refine_diff_density_min         -1.83
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9586
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0107541
_refine_ls_shift/su_mean         0.0010174
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1381
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1381
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                4350
_reflns_number_total             5762
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.90
_oxford_diffrn_Wilson_scale      228.81
_oxford_refine_ls_r_factor_ref   0.0727
_oxford_refine_ls_scale          0.21591(17)
_oxford_reflns_number_all        5737
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'aw_f_062_0m_4_a.res in P4(1)2(1)2'
_cod_data_source_file            c9sc03076j2.cif
_cod_data_source_block           AG_F_062
_cod_original_cell_volume        6334.6(10)
_cod_original_sg_symbol_H-M      'P 41 21 2 '
_cod_original_formula_sum        'C63 H65 B1 F24 Ir1 N1 P2'
_cod_database_code               1552252