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_4113091
_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            'C103 H137 Cl17 N9 Sc3'
_chemical_formula_weight         746.25
_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                 95.918(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   18.3719(18)
_cell_length_b                   16.5295(14)
_cell_length_c                   37.716(4)
_cell_measurement_temperature    173(2)
_cell_volume                     11392.5(19)
_computing_cell_refinement       SAINT+
_computing_data_collection       SMART
_computing_data_reduction        SAINT+
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker 1K CCD'
_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  0.1248
_diffrn_reflns_av_sigmaI/netI    0.1455
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39409
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.9697
_exptl_absorpt_correction_T_min  0.612828
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       rod
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1189
_refine_ls_number_reflns         11916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.410
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                6861
_reflns_number_total             11916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046753tsi20040602_105745.cif
_cod_data_source_block           jmei1
_cod_original_cell_volume        11392.6(19)
_cod_original_formula_sum        '3(C33 H43 Cl3 N3 Sc) 4(C H2 Cl2)'
_cod_database_code               4113091