Unsaturated Iridium(III) Complexes Supported by a Quinolato‒Carboxylato ONO Pincer-Type Ligand: Synthesis, Reactivity, and Catalytic C‒H Functionalization
Nguyen, Duc Hanh; Pérez-Torrente, Jesús J.; Jiménez, M. Victoria; Modrego, F. Javier; Gómez-Bautista, Daniel; Lahoz, Fernando J.; Oro, Luis A.; Organometallics 32 (2013) 6918–; doi:10.1021/om400768n

data_4081907
_publ_section_title
;
 Unsaturated Iridium(III) Complexes Supported by a Quinolato--Carboxylato
 ONO Pincer-Type Ligand: Synthesis, Reactivity, and Catalytic C--H
 Functionalization
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6918
_journal_paper_doi               10.1021/om400768n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C19 H22 Ir N O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C21 H26 Cl4 Ir N O4'
_chemical_formula_weight         690.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.1630(10)
_cell_angle_beta                 113.8100(10)
_cell_angle_gamma                100.9380(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0950(7)
_cell_length_b                   11.0369(8)
_cell_length_c                   12.0268(9)
_cell_measurement_reflns_used    8815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.2
_cell_volume                     1167.49(15)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13820
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    6.205
_exptl_absorpt_correction_T_max  0.4563
_exptl_absorpt_correction_T_min  0.3557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.                    
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.152
_refine_diff_density_max         3.440
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.1568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0641
_reflns_d_resolution_high        0.7817
_reflns_number_gt                4836
_reflns_number_total             5070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400768n_si_002.cif
_cod_data_source_block           compnd_1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081907
_shelx_title                     ' fjl61as in P-1'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            300.09
_shelx_f_squared_multiplier      1.000