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_4088797
_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            'C47 H26 F15 Ir N4 S2'
_chemical_formula_weight         1188.04
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 99.784(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.059(2)
_cell_length_b                   24.303(4)
_cell_length_c                   13.431(2)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.31
_cell_volume                     4200.6(11)
_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 0.993
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26162
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         1.676
_exptl_absorpt_coefficient_mu    3.387
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9701
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+6.6103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9165
_reflns_number_total             9701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00453_si_002.cif
_cod_data_source_block           8
_cod_original_cell_volume        4200.8(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088797
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.293
_shelx_estimated_absorpt_t_max   0.473
_shelx_res_checksum              70749
_shelx_hkl_checksum              64528