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_4081908
_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         'C20 H16 Ir N3 O3, H2 O'
_chemical_formula_sum            'C20 H18 Ir N3 O4'
_chemical_formula_weight         556.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3967(9)
_cell_length_b                   15.3084(17)
_cell_length_c                   14.1731(16)
_cell_measurement_reflns_used    3374
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.906
_cell_measurement_theta_min      2.661
_cell_volume                     1821.7(3)
_computing_cell_refinement       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 v. 2009.7 (Bruker AXS, 2008)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.978
_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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20909
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    7.362
_exptl_absorpt_correction_T_max  0.7202
_exptl_absorpt_correction_T_min  0.6262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.693
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4241
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+5.7120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0819
_reflns_d_resolution_high        0.7602
_reflns_number_gt                3397
_reflns_number_total             4241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400768n_si_002.cif
_cod_data_source_block           compnd_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081908
_shelx_title                     ' fjl236am in P2(1)/n'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            610.76
_shelx_f_squared_multiplier      1.000