Insertion of Pyridine into an Iron−Silicon Bond and Photochemical Conversion of the Insertion Product Cp*(OC)Fe{η3(C,C,C)-C5H5NSiMe2NPh2} to a Sandwich Compound
Iwata, Masatoshi; Okazaki, Masaaki; Tobita, Hiromi; Organometallics 25 (2006) 6115–; doi:10.1021/om060873n

data_4074583
_publ_section_title
;
 Insertion of Pyridine into an Iron&#x2212;Silicon Bond and Photochemical
 Conversion of the Insertion Product Cp*(OC)Fe{\h3(C,C,C)-C5H5NSiMe2NPh2}
 to a Sandwich Compound
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6115
_journal_paper_doi               10.1021/om060873n
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C27 H35 N O Ru Si'
_chemical_formula_weight         518.72
_chemical_name_common            complex4j
_chemical_name_systematic        complex4j
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 107.912(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.5980(10)
_cell_length_b                   8.70160(10)
_cell_length_c                   15.1845(2)
_cell_measurement_reflns_used    27385
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.96
_cell_measurement_theta_min      4.29
_cell_volume                     5104.19(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16824
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.8273
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.898
_refine_diff_density_min         -2.018
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+54.4774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1983
_reflns_number_gt                4671
_reflns_number_total             5707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060873nsi20060925_041905.cif
_cod_data_source_block           gangan1
_cod_original_cell_volume        5104.18(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4074583