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_4328217
_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_sum            'C47 H42 Cl Ir N O2.5 P2'
_chemical_formula_weight         950.41
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 123.8460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.1299(15)
_cell_length_b                   19.5950(10)
_cell_length_c                   19.5946(10)
_cell_measurement_reflns_used    6392
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.27
_cell_measurement_theta_min      2.17
_cell_volume                     8651.5(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32960
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_T_max  0.7156
_exptl_absorpt_correction_T_min  0.4961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7611
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+62.3125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                4636
_reflns_number_total             7611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202065d_si_001_1.cif
_cod_data_source_block           '[C45H37ClNO2P2Ir]1/2C4H10O(compound6)'
_cod_original_formula_sum        'C47 H42 Cl Ir N O2.50 P2'
_cod_database_code               4328217