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_4130445
_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_sum            'C31 H57 B2 Ir O6 P2'
_chemical_formula_weight         801.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.982(5)
_cell_length_b                   16.075(5)
_cell_length_c                   28.684(10)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.29
_cell_volume                     7369(4)
_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      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            84014
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.958
_diffrn_reflns_theta_min         1.797
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            'translucent orange'
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         9368
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0230P)^2^+9.3420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5460
_reflns_number_total             9368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03656_si_002.cif
_cod_data_source_block           Me-PoCoP-iPr_Ir_Bpin2_Compound_6b
_cod_database_code               4130445
_shelx_shelxl_version_number     2014/7
_computing_refinement_gui        'shelXle rev 647 (Hubschle et al, 2011)'
_shelx_res_checksum              9375
_shelx_hkl_checksum              6221