Room temperature transmetallation from tris(pentafluorophenyl)borane to cyclometallated iridium(III)
Maity, Ayan; Kölsch, Jonas; Na, Hanah; Teets, Thomas S.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02540H

data_7043935
_publ_section_title
;
 Room temperature transmetallation from tris(pentafluorophenyl)borane to
 cyclometallated iridium(III)
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02540H
_journal_year                    2017
_chemical_formula_sum            'C39 H38 Cl2 F10 Ir N3 P'
_chemical_formula_weight         1032.79
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-28 deposited with the CCDC.
2017-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                92.120(4)
_cell_angle_beta                 101.748(4)
_cell_angle_gamma                95.488(5)
_cell_formula_units_Z            2
_cell_length_a                   12.213(4)
_cell_length_b                   12.217(4)
_cell_length_c                   13.801(5)
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.32
_cell_volume                     2003.4(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12070
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.677
_exptl_absorpt_coefficient_mu    3.585
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             1018
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and pentane'
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8646
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0355P)^2^+4.8448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8183
_reflns_number_total             8646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02540h2.cif
_cod_data_source_block           4b
_cod_original_cell_volume        2003.5(12)
_cod_database_code               7043935
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.308
_shelx_estimated_absorpt_t_max   0.456
_shelx_res_checksum              33858