Facile N-H Bond Cleavage of Ammonia by an Iridium Complex Bearing a Noninnocent PNP-Pincer Type Phosphaalkene Ligand
Yung-Hung Chang; Yumiko Nakajima; Hiromasa Tanaka; Kazunari Yoshizawa; Fumiyuki Ozawa; Journal of the American Chemical Society 135 (2013) 11791–11794; doi:10.1021/ja407163z

data_4120310
_publ_contact_author_address
'Institute for Chemical Research, Kyoto University, Uji, Kyoto 611-0011, Japan'
_publ_contact_author_email       ozawa@scl.kyoto-u.ac.jp
_publ_contact_author_fax         +81-774-38-3039
_publ_contact_author_name        'Fumiyuki Ozawa'
_publ_contact_author_phone       +81-774-38-3035
_publ_section_title
;
 Facile N-H Bond Cleavage of Ammonia by an Iridium Complex Bearing a
 Noninnocent PNP-Pincer Type Phosphaalkene Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11791
_journal_page_last               11794
_journal_paper_doi               10.1021/ja407163z
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C50 H76 Ir N O P2'
_chemical_formula_weight         961.26
_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                105.061(2)
_cell_angle_beta                 98.416(5)
_cell_angle_gamma                112.588(4)
_cell_formula_units_Z            2
_cell_length_a                   13.213(5)
_cell_length_b                   14.526(6)
_cell_length_c                   14.757(6)
_cell_measurement_temperature    173(2)
_cell_volume                     2427.1(17)
_computing_cell_refinement       'Rigaku AFC10/Saturn 70 CCD'
_computing_data_collection       'Rigaku AFC10/Saturn 70 CCD'
_computing_data_reduction        'Rigaku AFC10/Saturn 70 CCD'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'ORTEP3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.1192
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19708
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.8254
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.350
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         10643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                7449
_reflns_number_total             10643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407163z_si_002_3.cif
_cod_data_source_block           complex_4
_cod_original_cell_volume        2427.0(18)
_cod_database_code               4120310