Ligand survey results in identification of PNP pincer complexes of iridium as long-lived and chemoselective catalysts for dehydrogenative borylation of terminal alkynes
Lee, Chun-I; DeMott, Jessica C.; Pell, Christopher J.; Christopher, Alyson; Zhou, Jia; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Chem. Sci. 6 (2015) 6572–; doi:10.1039/C5SC02161H

data_1529348
_publ_section_title
;
 Ligand survey results in identification of PNP pincer complexes of
 iridium as long-lived and chemoselective catalysts for dehydrogenative
 borylation of terminal alkynes
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6572
_journal_paper_doi               10.1039/C5SC02161H
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C32 H53 B Ir N O2 P2'
_chemical_formula_weight         748.70
_chemical_name_systematic        (PNP)Ir(H)(Bpin)
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc1329s8
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-07-19 deposited with the CCDC.
2015-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.435(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.792(3)
_cell_length_b                   17.546(2)
_cell_length_c                   14.1242(19)
_cell_measurement_temperature    110(2)
_cell_volume                     3435.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1149
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            61147
_diffrn_reflns_theta_full        61.01
_diffrn_reflns_theta_max         61.01
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    8.604
_exptl_absorpt_correction_T_max  0.1822
_exptl_absorpt_correction_T_min  0.0714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: (Me3Si)2O'
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                4176
_reflns_number_total             5213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02161h4.cif
_cod_data_source_block           oz416
_cod_depositor_comments
'Adding full bibliography for 1529345--1529348.cif.'
_cod_original_cell_volume        3435.2(9)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1529348