Rhodium and Iridium Amido Complexes Supported by Silyl Pincer Ligation: Ammonia N-H Bond Activation by a [PSiP]Ir Complex
Erin Morgan; Darren F. MacLean; Robert McDonald; Laura Turculet; Journal of the American Chemical Society 131 (2009) 14234–14236; doi:10.1021/ja906646v

data_4105133
_publ_section_title
;
 Rhodium and Iridium Amido Complexes Supported by Silyl Pincer Ligation:
 Ammonia N-H Bond Activation by a [PSiP]Ir Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14234
_journal_page_last               14236
_journal_paper_doi               10.1021/ja906646v
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C43 H62 Ir N P2 Si, C4 H10 O'
_chemical_formula_sum            'C47 H72 Ir N O P2 Si'
_chemical_formula_weight         949.29
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.8460(6)
_cell_length_b                   17.5996(5)
_cell_length_c                   27.5460(8)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.17
_cell_volume                     9136.5(5)
_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    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            76763
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    3.053
_exptl_absorpt_correction_T_max  0.6816
_exptl_absorpt_correction_T_min  0.3916
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       prism
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         10506
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+9.3008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                8132
_reflns_number_total             10506
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja906646v_si_002_1.cif
_cod_data_source_block           dal09b3
_cod_database_code               4105133