Four-Coordinate Iridium(I) Monohydrides: Reversible Dinitrogen Binding, Bond Activations, and Deprotonations
Matthew D. Millard; Curtis E. Moore; Arnold L. Rheingold; Joshua S. Figueroa; Journal of the American Chemical Society 132 (2010) 8921–8923; doi:10.1021/ja1037808

data_4102641
_publ_section_title
;
 Four-Coordinate Iridium(I) Monohydrides: Reversible Dinitrogen Binding,
 Bond Activations, and Deprotonations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8921
_journal_page_last               8923
_journal_paper_doi               10.1021/ja1037808
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C34 H67 Ir P2'
_chemical_formula_weight         730.02
_chemical_name_common            H5Ir(P(CH2Ad)(i-Pr)2)2
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.916(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.776(13)
_cell_length_b                   12.182(14)
_cell_length_c                   26.90(3)
_cell_measurement_reflns_used    6484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      1.5
_cell_volume                     3489(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\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_reflns_av_R_equivalents  0.1225
_diffrn_reflns_av_sigmaI/netI    0.0812
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35407
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    3.938
_exptl_absorpt_correction_T_max  0.4645
_exptl_absorpt_correction_T_min  0.4275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.694
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       none
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6484
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                4918
_reflns_number_total             6484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1037808_si_002_08.cif
_cod_data_source_block           jfig191
_cod_database_code               4102641