Highly Luminescent Cyclometalated Iridium Complexes Generated by Nucleophilic Addition to Coordinated Isocyanides.
Na, Hanah; Teets, Thomas S.; Journal of the American Chemical Society 140 (2018) 6353–6360; doi:10.1021/jacs.8b02416

data_4132204
_publ_section_title
;
 Highly Luminescent Cyclometalated Iridium Complexes Generated by
 Nucleophilic Addition to Coordinated Isocyanides.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6353
_journal_page_last               6360
_journal_paper_doi               10.1021/jacs.8b02416
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C36 H27.5 Cl2.5 Ir N5 O2 S2'
_chemical_formula_weight         907.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 130.05
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.9379(10)
_cell_length_b                   11.9202(5)
_cell_length_c                   15.6551(12)
_cell_measurement_reflns_used    6963
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.60
_cell_volume                     3419.5(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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0226
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10379
_diffrn_reflns_point_group_measured_fraction_full 0.707
_diffrn_reflns_point_group_measured_fraction_max 0.685
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         2.038
_exptl_absorpt_coefficient_mu    4.264
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5415
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0190
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0413
_reflns_Friedel_coverage         0.374
_reflns_Friedel_fraction_full    0.414
_reflns_Friedel_fraction_max     0.373
_reflns_number_gt                5122
_reflns_number_total             5415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02416_si_002.cif
_cod_data_source_block           4c
_cod_original_cell_volume        3419.4(3)
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C36 H27.50 Cl2.50 Ir N5 O2 S2'
_cod_database_code               4132204
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.361
_shelx_estimated_absorpt_t_max   0.784
_shelx_res_checksum              67365
_shelx_hkl_checksum              15399