Fluorination of Cyclometalated Iridium β-Ketoiminate and β-Diketiminate Complexes: Extreme Redox Tuning and Ligand-Centered Excited States
Maya, Rosa A.; Maity, Ayan; Teets, Thomas S.; Organometallics 35 (2016) 2890–; doi:10.1021/acs.organomet.6b00453

data_4088796
_publ_section_title
;
 Fluorination of Cyclometalated Iridium \b-Ketoiminate and \b-Diketiminate
 Complexes: Extreme Redox Tuning and Ligand-Centered Excited States
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2890
_journal_paper_doi               10.1021/acs.organomet.6b00453
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C43 H26 F15 Ir N4'
_chemical_formula_weight         1075.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                98.088(7)
_cell_angle_beta                 108.280(6)
_cell_angle_gamma                96.640(6)
_cell_formula_units_Z            4
_cell_length_a                   12.402(6)
_cell_length_b                   18.073(9)
_cell_length_c                   19.410(9)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.25
_cell_volume                     4030(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.980
_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  0.0174
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23923
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.453
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       plate
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.728
_refine_diff_density_min         -1.933
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1303
_refine_ls_number_reflns         16768
_refine_ls_number_restraints     1275
_refine_ls_restrained_S_all      1.300
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0360P)^2^+10.2552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15027
_reflns_number_total             16768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00453_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        4031(3)
_cod_database_code               4088796
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.381
_shelx_estimated_absorpt_t_max   0.848
_shelx_res_checksum              46153
_shelx_hkl_checksum              34599