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_4105136
_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 N P2 Rh Si'
_chemical_formula_sum            'C43 H62 N P2 Rh Si'
_chemical_formula_weight         785.88
_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                 105.739(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7712(19)
_cell_length_b                   17.415(3)
_cell_length_c                   20.937(3)
_cell_measurement_reflns_used    2842
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.18
_cell_measurement_theta_min      2.34
_cell_volume                     4131.1(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0974
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25644
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.9657
_exptl_absorpt_correction_T_min  0.8776
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+3.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                4460
_reflns_number_total             7558
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja906646v_si_002_4.cif
_cod_data_source_block           dal0928
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4105136