Preparation and Molecular and Electronic Structures of Iron(0) Dinitrogen and Silane Complexes and Their Application to Catalytic Hydrogenation and Hydrosilation
Suzanne C. Bart; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 126 (2004) 13794–13807; doi:10.1021/ja046753t

data_4113090
_publ_section_title
;
 Preparation and Molecular and Electronic Structures of Iron(0) Dinitrogen
 and Silane Complexes and Their Application to Catalytic Hydrogenation and
 Hydrosilation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13794
_journal_page_last               13807
_journal_paper_doi               10.1021/ja046753t
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C52 H65 Fe N3'
_chemical_formula_weight         787.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   43.276(2)
_cell_length_b                   43.276(2)
_cell_length_c                   12.6051(10)
_cell_measurement_temperature    173(2)
_cell_volume                     20444(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Briker 1K CCD area detector'
_diffrn_measurement_method       '0.3 deg. omega 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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16193
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.9818
_exptl_absorpt_correction_T_min  0.8974
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       rod
_exptl_crystal_F_000             7632
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         6505
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          1.664
_refine_ls_shift/su_mean         0.150
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1870
_reflns_number_gt                4036
_reflns_number_total             6505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046753tsi20040602_105710.cif
_cod_data_source_block           scb13
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C47 H53 Fe N3 * C5 H12'
_cod_database_code               4113090