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_4102941
_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_formula_moiety         '4(C34 H57 Ir N2 P2), C5 H12'
_chemical_formula_sum            'C141 H240 Ir4 N8 P8'
_chemical_formula_weight         3063.97
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2007-03-15   text and data added, srw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.863(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   39.937(6)
_cell_length_b                   11.3904(15)
_cell_length_c                   16.069(2)
_cell_measurement_reflns_used    2639
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.87
_cell_measurement_theta_min      2.28
_cell_volume                     7283.4(17)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  ga67qasx
_diffrn_reflns_av_R_equivalents  0.1601
_diffrn_reflns_av_sigmaI/netI    0.1751
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61891
_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    3.779
_exptl_absorpt_correction_T_max  0.9226
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             3140
_exptl_crystal_id                ga67qasx
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 0 -5) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         13662
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                6998
_reflns_number_total             13662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1053835_si_002.cif
_cod_data_source_block           ga67qasx
_cod_original_cell_volume        7283.3(17)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4102941