Desulfurization of N,N-dimethylthioformamide by hydrosilane with the help of an iron complex. Isolation and characterization of an iron-carbene complex as an intermediate of C[double bond, length as m-dash]S double bond cleavage
Kozo Fukumoto; Akane Sakai; Tsukuru Oya; Hiroshi Nakazawa; Chem.Commun. 48 (2012) 3809–; doi:10.1039/c2cc17163e

data_7107541
_publ_section_title
;
 Desulfurization of N,N-dimethylthioformamide by hydrosilane with the help
 of an iron complex. Isolation and characterization of an iron-carbene
 complex as an intermediate of C[double bond, length as m-dash]S double
 bond cleavage
;
_journal_name_full               Chem.Commun.
_journal_page_first              3809
_journal_paper_doi               10.1039/c2cc17163e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C27 H27 Fe N O S Si '
_chemical_formula_sum            'C27 H27 Fe N O S Si'
_chemical_formula_weight         497.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.572(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.037(2)
_cell_length_b                   9.3525(11)
_cell_length_c                   16.402(2)
_cell_measurement_reflns_used    11004
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.2
_cell_volume                     2410.1(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23293
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5411
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0017Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                4905
_reflns_number_total             5411
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc17163e.txt
_cod_data_source_block           FKK-081006-2
_cod_original_cell_volume        2410.0(5)
_cod_original_formula_sum        'C27 H27 Fe N O S Si '
_cod_database_code               7107541