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_4114337
_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            'C30 H50 Ir N P2'
_chemical_formula_weight         678.85
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_symmetry_space_group_name_Hall  '-P 2yn'
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_cell_angle_beta                 101.584(1)
_cell_angle_gamma                90.00
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_cell_length_b                   13.0270(3)
_cell_length_c                   21.9266(4)
_cell_measurement_reflns_used    8338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.91
_cell_measurement_theta_min      4.92
_cell_volume                     2983.16(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
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_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_max  0.8743
_exptl_absorpt_correction_T_min  0.2069
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_exptl_absorpt_process_details   'Bruker SAINT (XPREP)'
_exptl_crystal_colour            violet
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         6095
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+3.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_data_source_block           irhanil
_cod_original_cell_volume        2983.2(1)
_cod_database_code               4114337