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_4114340
_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            'C29 H55 Ir N2 P2'
_chemical_formula_weight         685.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.291(2)
_cell_length_b                   11.463(2)
_cell_length_c                   24.150(5)
_cell_measurement_temperature    183(2)
_cell_volume                     3125.7(10)
_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      183(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7556
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    4.393
_exptl_absorpt_correction_T_max  0.5587
_exptl_absorpt_correction_T_min  0.3524
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       blade
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.631
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.582
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                6769
_reflns_number_total             7556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037363usi20030717_084947_4.cif
_cod_data_source_block           jz03
_cod_original_cell_volume        3125.8(11)
_cod_database_code               4114340