High-Turnover Aromatic C-H Borylation Catalyzed by POCOP-Type Pincer Complexes of Iridium.
Press, Loren P.; Kosanovich, Alex J.; McCulloch, Billy J.; Ozerov, Oleg V.; Journal of the American Chemical Society 138 (2016) 9487–9497; doi:10.1021/jacs.6b03656

data_4130446
_publ_section_title
;
 High-Turnover Aromatic C-H Borylation Catalyzed by POCOP-Type Pincer
 Complexes of Iridium.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9487
_journal_page_last               9497
_journal_paper_doi               10.1021/jacs.6b03656
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C52 H96 Cl2 Ir2 O4 P4, C5 H12'
_chemical_formula_sum            'C57 H108 Cl2 Ir2 O4 P4'
_chemical_formula_weight         1436.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.697(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5120(19)
_cell_length_b                   20.125(4)
_cell_length_c                   18.462(4)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.31
_cell_volume                     3126.3(12)
_computing_cell_refinement       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
_computing_data_collection       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT v8.18c (Bruker AXS, 2008)'
_computing_molecular_graphics    'shelXle rev 647 (Hubschle et al, 2011)'
_computing_structure_refinement  'SHELXL-2013/4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013/4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36084
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.767
_diffrn_reflns_theta_min         1.506
_exptl_absorpt_coefficient_mu    4.481
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       rod
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.391
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         8455
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0577P)^2^+1.7576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7723
_reflns_number_total             8455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03656_si_002.cif
_cod_data_source_block           di-tBu-PoCoP-iPr_Ir_H_Cl_dimer_Compound_3c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130446
_shelx_estimated_absorpt_t_min   0.156
_shelx_estimated_absorpt_t_max   0.483
_computing_refinement_gui        'shelXle rev 647 (Hubschle et al, 2011)'
_shelxl_version_number           2013-4
_shelx_res_checksum              50919
_shelx_hkl_checksum              96713