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_4105135
_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         'C45 H66 Ir N P2 Si'
_chemical_formula_sum            'C45 H66 Ir N P2 Si'
_chemical_formula_weight         903.22
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.6341(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0501(6)
_cell_length_b                   19.8548(10)
_cell_length_c                   17.7790(9)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.26
_cell_volume                     4251.9(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    'DIRDIF-99 (Beurskens et al., 1999)'
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36901
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    3.275
_exptl_absorpt_correction_T_max  0.6947
_exptl_absorpt_correction_T_min  0.4820
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         9694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.004
_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^+2.7458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                8035
_reflns_number_total             9694
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja906646v_si_002_3.cif
_cod_data_source_block           dal08d1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105135