N-H Activation of Hydrazines by Iridium(I). Double N-H Activation To Form Iridium Aminonitrene Complexes
Zheng Huang; Jianrong (Steve) Zhou; John F. Hartwig; Journal of the American Chemical Society 132 (2010) 11458–11460; doi:10.1021/ja1053835

data_4102945
_publ_section_title
;
 N-H Activation of Hydrazines by Iridium(I). Double N-H Activation To Form
 Iridium Aminonitrene Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11458
_journal_page_last               11460
_journal_paper_doi               10.1021/ja1053835
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H50 Ir N P2'
_chemical_formula_sum            'C31 H50 Ir N P2'
_chemical_formula_weight         690.86
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           106
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.6955(10)
_cell_length_b                   20.6955(10)
_cell_length_c                   14.3009(10)
_cell_measurement_reflns_used    9730
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.43
_cell_volume                     6125.1(6)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba74jast
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            108168
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    4.483
_exptl_absorpt_correction_T_max  0.5473
_exptl_absorpt_correction_T_min  0.1717
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2800
_exptl_crystal_id                ba74jast
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-3 3 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack (1983),  2575 Friedels'
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5534
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+3.3455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                5097
_reflns_number_total             5534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1053835_si_006.cif
_cod_data_source_block           ba74jast
_cod_database_code               4102945