Reactions of Hydridoirida-β-diketones with Amines or with 2-Aminopyridines: Formation of Hydridoirida-β-ketoimines, PCN Terdentate Ligands, and Acyl Decarbonylation
Roberto Ciganda; María A. Garralda; Lourdes Ibarlucea; Claudio Mendicute-Fierro; M. Carmen Torralba; M. Rosario Torres; Inorganic Chemistry 51 (2012) 1760–1768; doi:10.1021/ic202065d

data_4328219
_publ_contact_author
; 
      Torralba, M. Carmen
      Departamento de Qu\'imica Inorg\'anica I
      Facultad de Ciencias Qu\'imicas 
      Universidad Complutense de Madrid
      28040 Madrid (Spain)
;
_publ_contact_author_email       torralba@quim.ucm.es
_publ_contact_author_fax         '+34 91 3944352'
_publ_contact_author_phone       '+34 91 3944233'
_publ_section_title
;
 Reactions of Hydridoirida-\b-diketones with Amines or with
 2-Aminopyridines: Formation of Hydridoirida-\b-ketoimines, PCN Terdentate
 Ligands, and Acyl Decarbonylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1760
_journal_page_last               1768
_journal_paper_doi               10.1021/ic202065d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C44 H36 Cl Ir N2 O P2, C4 H10 O'
_chemical_formula_sum            'C48 H46 Cl Ir N2 O2 P2'
_chemical_formula_weight         972.46
_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 and Fourier'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.3450(10)
_cell_angle_beta                 78.7960(10)
_cell_angle_gamma                78.2530(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0825(7)
_cell_length_b                   13.0297(8)
_cell_length_c                   15.0971(10)
_cell_measurement_reflns_used    6652
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.44
_cell_volume                     2092.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21188
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  0.7742
_exptl_absorpt_correction_T_min  0.3457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      0
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0512
_reflns_number_gt                6539
_reflns_number_total             7349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202065d_si_001_3.cif
_cod_data_source_block           '[C44H36ClN2OP2Ir]C4H10O(compound13)'
_cod_database_code               4328219