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_4130447
_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         'C32 H60 B Ir O4 P2'
_chemical_formula_sum            'C32 H60 B Ir O4 P2'
_chemical_formula_weight         773.75
_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'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 104.134(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.124(5)
_cell_length_b                   7.909(2)
_cell_length_c                   24.508(7)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.25
_cell_volume                     3594.7(17)
_computing_cell_refinement       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
_computing_data_collection       'Apex2 v2013.2-0 (Bruker AXS, 2008)'
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_diffrn_ambient_temperature      110(2)
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_diffrn_measured_fraction_theta_max 0.998
_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
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_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
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_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39877
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.376
_diffrn_reflns_theta_min         2.196
_exptl_absorpt_coefficient_mu    3.835
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
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_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         8139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6874
_reflns_number_total             8139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03656_si_002.cif
_cod_data_source_block           tBuPoCoPiPr_Ir_H_Bpin_Compound_4c
_cod_original_cell_volume        3594.8(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130447
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.616
_shelx_estimated_absorpt_t_max   0.749
_computing_refinement_gui        'shelXle rev 647 (Hubschle et al, 2011)'
_shelx_res_checksum              14316
_shelx_hkl_checksum              67267