Synthesis and reactivity of PC(sp3)P-pincer iridium complexes bearing a diborylmethyl anion
Kishino, Masamichi; Takaoka, Satoko; Shibutani, Yuki; Kusumoto, Shuhei; Nozaki, Kyoko; Dalton Transactions  (2022) –; doi:10.1039/D2DT00513A

data_7709776
_publ_section_title
;
 Synthesis and reactivity of PC(sp3)P-pincer iridium complexes bearing a
 diborylmethyl anion
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00513A
_journal_year                    2022
_chemical_formula_sum            'C32 H52 B2 Cl Ir N2 O P2'
_chemical_formula_weight         791.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-10 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.042(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0281(3)
_cell_length_b                   19.0554(4)
_cell_length_c                   16.3403(4)
_cell_measurement_reflns_used    22188
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.7920
_cell_measurement_theta_min      2.1180
_cell_volume                     3495.46(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.750
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_exptl_absorpt_coefficient_mu    4.015
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.332
_refine_diff_density_min         -2.978
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         8159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+15.1331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7369
_reflns_number_total             8159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00513a3.cif
_cod_data_source_block           7_Ir_HClCO
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709776
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              62560
_shelx_hkl_checksum              54941