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_4324474
_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
;
 [(C4 H8 O)6 Fe 2+], [(C7 H7 N 2-)4 (C9 H11 S 1-)3 
 (C6 H18 N Si2 1-) (Fe 3+)3 (Fe 2+)]2, (C4H8O)2
;
_chemical_formula_structural
'[Fe(C4H8O)6 2+] . 2[Fe4(NC7H7)4(SC9H11)3{N(Si(CH3)3)2} 1-] . 2(C4H8O)'
_chemical_formula_sum            'C148 H210 Fe9 N10 O8 S6 Si4'
_chemical_formula_weight         3064.63
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
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_cell_angle_alpha                90.00
_cell_angle_beta                 113.8988(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.5272(5)
_cell_length_b                   21.9314(5)
_cell_length_c                   30.2981(6)
_cell_measurement_reflns_used    41154
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      1.27
_cell_volume                     15508.0(6)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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 1.0
_diffrn_measured_fraction_theta_max 1.0
_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  0.073
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            41154
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             6472
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         10777
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.033
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_obs          0.0686
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1686
_refine_ls_wR_factor_obs         0.1466
_reflns_number_observed          7139
_reflns_number_total             10777
_reflns_observed_criterion       I>2\s(I)
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_cod_data_source_block           578_15m4
_cod_database_code               4324474