Synthesis and Reactivity of 16-electron Half-Sandwich Iridium Complexes Bearing a Carboranylthioamide Ligand
Jin, Guo-Xin; Cui, Peng-Fei; Lin, Yue-Jian; Dalton Trans.  (2017) –; doi:10.1039/C7DT03529B

data_7044473
_publ_section_title
;
 Synthesis and Reactivity of 16-electron Half-Sandwich Iridium Complexes
 Bearing a Carboranylthioamide Ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03529B
_journal_year                    2017
_chemical_formula_sum            'C20 H32.5 B10 Cl3.5 Ir N S'
_chemical_formula_weight         743.40
_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
;
2017-09-03 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                96.0060(10)
_cell_angle_beta                 96.1970(10)
_cell_angle_gamma                98.6200(10)
_cell_formula_units_Z            4
_cell_length_a                   12.2564(10)
_cell_length_b                   12.9860(11)
_cell_length_c                   18.7275(15)
_cell_measurement_reflns_used    4483
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.20
_cell_volume                     2907.6(4)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21412
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.050
_exptl_absorpt_coefficient_mu    4.999
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.532
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         13102
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+11.7395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8716
_reflns_number_total             13102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03529b2.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C20 H32.50 B10 Cl3.50 Ir N S'
_cod_database_code               7044473
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.662
_shelx_res_checksum              39163