Distinct Thermodynamics for the Formation and Cleavage of N-H Bonds in Aniline and Ammonia. Directly-Observed Reductive Elimination of Ammonia from an Isolated Amido Hydride Complex
Mira Kanzelberger; Xiawei Zhang; Thomas J. Emge; Alan S. Goldman; Jing Zhao; Christopher Incarvito; John F. Hartwig; Journal of the American Chemical Society 125 (2003) 13644–13645; doi:10.1021/ja037363u

data_4114339
_publ_contact_author_address
; 
 Department of Chemistry 
 Rutgers, The State University of New Jersey
 610 Taylor Road
 Piscataway, New Jersey  08854-8087  U.S.A. 
;
_publ_contact_author_email       agoldman@rutchem.rutgers.edu
_publ_contact_author_name        'Alan S. Goldman'
_publ_section_title
;
 Distinct Thermodynamics for the Formation and Cleavage of N-H Bonds in
 Aniline and Ammonia. Directly-Observed Reductive Elimination of Ammonia
 from an Isolated Amido Hydride Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13644
_journal_page_last               13645
_journal_paper_doi               10.1021/ja037363u
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C24 H46 Ir N P2'
_chemical_formula_weight         602.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
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_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.938(3)
_cell_length_b                   15.383(3)
_cell_length_c                   24.065(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5291(2)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w 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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20861
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    5.178
_exptl_absorpt_correction_T_max  0.5106
_exptl_absorpt_correction_T_min  0.2645
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       blade
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         11494
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          4.218
_refine_ls_shift/su_mean         0.089
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                7145
_reflns_number_total             11494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037363usi20030717_084947_3.cif
_cod_data_source_block           jz01
_cod_original_cell_volume        5291.1(18)
_cod_database_code               4114339