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_4102642
_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            'C58 H114 Ir Li O10 P2'
_chemical_formula_weight         1232.57
_chemical_name_common
'[Li(12-c-4)2][HIr(kappa-2-C,P-(P(CH2Ad)(i-Pr)2)(P(CH2Ad)(i-Pr)2)]'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.9760(10)
_cell_angle_beta                 86.6690(10)
_cell_angle_gamma                89.3790(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1359(11)
_cell_length_b                   14.0399(12)
_cell_length_c                   15.8641(14)
_cell_measurement_reflns_used    12952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.3
_cell_volume                     2918.9(4)
_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, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40593
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_T_max  0.6457
_exptl_absorpt_correction_T_min  0.5969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Brick red'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
 One void was found containing 4 disordered Diethyl ether molecules. 
 Their formula was added to the formula for the unit-cell and its 
 electron density removed.
;
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         12952
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0275P)^2^+1.3018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                11474
_reflns_number_total             12952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1037808_si_002_09.cif
_cod_data_source_block           JFig219
_cod_database_code               4102642