Iron-Mediated Hydrazine Reduction and the Formation of Iron-Arylimide Heterocubanes
Michael J. Zdilla; Atul K. Verma; Sonny C. Lee; Inorganic Chemistry 50 (2011) 1551–1562; doi:10.1021/ic1021627

data_4324475
_publ_contact_author_address
;                                                                               
 Department of Chemistry
 University of Waterloo
 200 University Avenue West
 Waterloo, Ontario  N2L 3G1
 CANADA  
;
_publ_contact_author_email       sclee@uwaterloo.ca
_publ_contact_author_fax         519-746-0435
_publ_contact_author_name        'Sonny C. Lee'
_publ_contact_author_phone       '519-885-1211 x37501'
_publ_section_title
;
 Iron-Mediated Hydrazine Reduction and the Formation of Iron-Arylimide
 Heterocubanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1551
_journal_page_last               1562
_journal_paper_doi               10.1021/ic1021627
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'Chemical Synthesis, S. C. Lee Lab'
_chemical_formula_moiety         '(Fe 2+)2 (C9 H11 S 1-)2 (C6 H18 Si2 N 1-)2'
_chemical_formula_structural     'Fe2(C9 H11 S)2(C6 H18 Si2 N)2'
_chemical_formula_sum            'C38 H74 Fe2 N2 O2 S2 Si4'
_chemical_formula_weight         879.17
_chemical_name_common            Fe2(SMes)2(N{SiMe3}2)2(THF)2
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                66.488(2)
_cell_angle_beta                 69.768(2)
_cell_angle_gamma                85.210(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4231(3)
_cell_length_b                   10.9167(5)
_cell_length_c                   12.8489(5)
_cell_measurement_reflns_used    24740
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.09
_cell_volume                     1255.40(9)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        'DENZO-SMN, Platon, Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'CIFTAB, 'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w 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  0.037
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24740
_diffrn_reflns_theta_full        54.7
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         5666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_obs          0.0414
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.5039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1192
_refine_ls_wR_factor_obs         0.1033
_reflns_number_observed          4012
_reflns_number_total             5666
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic1021627_si_002_2.cif
_cod_data_source_block           final028_2
_cod_original_cell_volume        1255.40(8)
_cod_database_code               4324475