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_4324477
_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_absolute_configuration ad
_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], 0.5(C6 H6)'
_chemical_formula_structural     '[Fe4(N C7 H7)4(S C9 H11)].1/2(C6 H6)'
_chemical_formula_sum            'C67 H75 Fe4 N4 S4'
_chemical_formula_weight         1287.95
_chemical_name_common            'Fe4(N-p-Tol)4(SMes)4, tetragonal form'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.1488(8)
_cell_length_b                   17.1488(8)
_cell_length_c                   43.475(2)
_cell_measurement_reflns_used    45649
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      1.28
_cell_volume                     12785.2(10)
_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       'Nonium KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45649
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.8361
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             5384
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         8361
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_obs          0.0414
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0990
_refine_ls_wR_factor_obs         0.0872
_reflns_number_observed          6023
_reflns_number_total             8361
_reflns_observed_criterion       I>2\s(I)
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_cod_data_source_block           444m8
_cod_database_code               4324477