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_7043933
_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            'C41.5 H30 Cl F9 Ir N3'
_chemical_formula_weight         969.33
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 94.693(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.168(4)
_cell_length_b                   10.156(2)
_cell_length_c                   20.551(5)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.24
_cell_volume                     3779.2(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23138
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         1.989
_exptl_absorpt_coefficient_mu    3.683
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             1900
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane and pentane'
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.957
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         8692
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+9.8773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8040
_reflns_number_total             8692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02540h2.cif
_cod_data_source_block           7b
_cod_original_cell_volume        3779.2(15)
_cod_original_formula_sum        'C41.50 H30 Cl F9 Ir N3'
_cod_database_code               7043933
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.328
_shelx_estimated_absorpt_t_max   0.710
_shelx_res_checksum              16439