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_4104971
_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         'C74 H70 N4 Rh2 Si2, 2(C7)'
_chemical_formula_sum            'C88 H70 N4 Rh2 Si2'
_chemical_formula_weight         1445.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                61.5180(10)
_cell_angle_beta                 68.2500(10)
_cell_angle_gamma                75.752(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7915(10)
_cell_length_b                   13.4246(11)
_cell_length_c                   13.5335(11)
_cell_measurement_reflns_used    8804
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.25
_cell_volume                     1742.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  Bruker
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6147
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.56
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.137
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                4108
_reflns_number_total             4955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9035169_si_008.cif
_cod_data_source_block           inv
_cod_original_cell_volume        1742.6(2)
_cod_database_code               4104971