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_4324478
_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 3+)4 (C7 H7 N 2-)4 (C9 H11 S 1-)4]'
_chemical_formula_structural     '[Fe4(N C7 H7)4(S C9 H11)]'
_chemical_formula_sum            'C64 H72 Fe4 N4 S4'
_chemical_formula_weight         1248.90
_chemical_name_common            'Fe4(N-p-Tol)4(SMes)4, monoclinic form'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.5564(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7971(5)
_cell_length_b                   11.4905(3)
_cell_length_c                   24.9620(6)
_cell_measurement_temperature    200(2)
_cell_volume                     5962.9(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Siemens-P4
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13688
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  0.8480
_exptl_absorpt_correction_T_min  0.7089
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         13688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+3.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                8801
_reflns_number_total             13688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1021627_si_002_5.cif
_cod_data_source_block           90all_14
_cod_database_code               4324478