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_4104967
_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         'C57 H45 N2 Rh Si2'
_chemical_formula_sum            'C57 H45 N2 Rh Si2'
_chemical_formula_weight         917.04
_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                 93.571(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8170(10)
_cell_length_b                   15.419(2)
_cell_length_c                   25.088(3)
_cell_measurement_reflns_used    1636
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.648
_cell_measurement_theta_min      2.283
_cell_volume                     4562.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 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 p4'
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19892
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.087
_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     559
_refine_ls_number_reflns         6538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                4183
_reflns_number_total             6538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9035169_si_004.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_database_code               4104967