High Oxidation State Rhodium and Iridium Bis(silyl)dihydride Complexes Supported by a Chelating Pyridyl-Pyrrolide Ligand
Jennifer L. McBee; Jose Escalada; T. Don Tilley; Journal of the American Chemical Society 131 (2009) 12703–12713; doi:10.1021/ja9035169

data_4104965
_publ_section_title
;
 High Oxidation State Rhodium and Iridium Bis(silyl)dihydride Complexes
 Supported by a Chelating Pyridyl-Pyrrolide Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12703
_journal_page_last               12713
_journal_paper_doi               10.1021/ja9035169
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C29 H27 N2 Rh '
_chemical_formula_sum            'C29 H27 N2 Rh'
_chemical_formula_weight         506.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.848(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.218(4)
_cell_length_b                   14.076(3)
_cell_length_c                   18.067(4)
_cell_measurement_reflns_used    1174
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      19.48
_cell_measurement_theta_min      2.21
_cell_volume                     4373.3(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      151(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker pt'
_diffrn_measurement_method       'omega and phi 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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.1502
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9164
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.9688
_exptl_absorpt_correction_T_min  0.9174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       plate
_exptl_crystal_F_000             1990
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                2162
_reflns_number_total             3606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9035169_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        4373.3(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C29 H27 N2 Rh '
_cod_database_code               4104965