Disilametallacycles as a Platform for Stabilizing M(II) and M(IV) (M = Fe, Ru) Centers: Synthesis and Characterization of Half-Sandwich Complexes and Their Application to Catalytic Double Silylation of Alkenes and Alkynes
Sunada, Yusuke; Imaoka, Tsuyoshi; Nagashima, Hideo; Organometallics 32 (2013) 2112–; doi:10.1021/om3012322

data_4080429
_publ_section_title
;
 Disilametallacycles as a Platform for Stabilizing M(II) and M(IV) (M =
 Fe, Ru) Centers: Synthesis and Characterization of Half-Sandwich
 Complexes and Their Application to Catalytic Double Silylation of Alkenes
 and Alkynes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2112
_journal_paper_doi               10.1021/om3012322
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H60 Fe2 N2 Si4'
_chemical_formula_sum            'C38 H60 Fe2 N2 Si4'
_chemical_formula_weight         768.94
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 125.259(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   14.4983(18)
_cell_length_b                   14.8867(17)
_cell_length_c                   10.5940(14)
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.44
_cell_volume                     1867.1(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8768
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             820.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.820
_refine_diff_density_min         -0.859
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2190
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0089Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1891
_reflns_number_gt                2172
_reflns_number_total             2190
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om3012322_si_001.cif
_cod_data_source_block           '[(Mes)Fe(Si)2(m-N2)]2'
_cod_database_code               4080429