Homolytic N-H activation of ammonia: hydrogen transfer of parent iridium ammine, amide, imide, and nitride species.
Scheibel, Markus G.; Abbenseth, Josh; Kinauer, Markus; Heinemann, Frank W.; Würtele, Christian; de Bruin, Bas; Schneider, Sven; Inorganic chemistry 54 (2015) 9290–9302; doi:10.1021/acs.inorgchem.5b00829

data_4346190
_publ_section_title
;
 Homolytic N-H activation of ammonia: hydrogen transfer of parent iridium
 ammine, amide, imide, and nitride species.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9290
_journal_page_last               9302
_journal_paper_doi               10.1021/acs.inorgchem.5b00829
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C24 H51 F6 Ir N2 O P2 Sb'
_chemical_formula_weight         873.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                103.831(2)
_cell_angle_beta                 90.905(2)
_cell_angle_gamma                97.413(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9851(10)
_cell_length_b                   12.4880(12)
_cell_length_c                   12.5346(12)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.74
_cell_measurement_theta_min      2.28
_cell_volume                     1653.8(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            101594
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.999
_diffrn_reflns_theta_min         1.338
_diffrn_source                   'INCOATEC Ag Microsource'
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.6264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       block
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.829
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10345
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0109P)^2^+1.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9524
_reflns_number_total             10345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00829_si_002.cif
_cod_data_source_block           cw60_0m_a
_cod_database_code               4346190
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.661
_shelxl_version_number           2014/6
_shelx_res_checksum              43658
_shelx_hkl_checksum              78677