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_4113093
_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            'C33 H43 Fe N7'
_chemical_formula_weight         593.59
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.353(3)
_cell_angle_beta                 84.933(3)
_cell_angle_gamma                70.398(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5667(11)
_cell_length_b                   8.8933(11)
_cell_length_c                   22.409(3)
_cell_measurement_temperature    143(2)
_cell_volume                     1601.0(4)
_computing_cell_refinement       'Bruker SAINT'
_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      143(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.6 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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13013
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.8239
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.196
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                4274
_reflns_number_total             6514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046753tsi20040608_042614.cif
_cod_data_source_block           scb15
_cod_original_cell_volume        1601.0(3)
_cod_database_code               4113093