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_4324476
_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
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_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 (C6 H5 N 2-)4 (C9 H11 S 1-)4], 1.5 (C6 H6)'
_chemical_formula_structural     '[Fe4(N C6 H5)4(S C9 H11)]. 1.5(C6 H6)'
_chemical_formula_sum            'C69 H73 Fe4 N4 S4'
_chemical_formula_weight         1309.96
_chemical_name_common            Fe4(NPh)4(SMes)4
_chemical_name_systematic
; 
? 
;
_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                105.992(2)
_cell_angle_beta                 96.730(2)
_cell_angle_gamma                93.088(2)
_cell_formula_units_Z            4
_cell_length_a                   15.2729(7)
_cell_length_b                   18.6174(7)
_cell_length_c                   23.6395(10)
_cell_measurement_reflns_used    40362
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      1.14
_cell_volume                     6390.9(5)
_computing_cell_refinement       'HKL Suite (Enraf-Nonius)'
_computing_data_collection       'HKL Suite (Enraf-Nonius)'
_computing_data_reduction        'HKL Suite (Enraf-Nonius)'
_computing_molecular_graphics    'SHELXTL V5.04'
_computing_publication_material  'CIFTAB Release 97-1 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius kappa CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.105
_diffrn_reflns_av_sigmaI/netI    0.1286
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40362
_diffrn_reflns_theta_full        46.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.94851
_exptl_absorpt_correction_T_min  0.83945
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             2732
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1483
_refine_ls_number_reflns         40362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_obs          0.0591
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0029P)^2^+10.7821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1168
_refine_ls_wR_factor_obs         0.0927
_reflns_number_observed          10168
_reflns_number_total             17699
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic1021627_si_002_3.cif
_cod_data_source_block           76_5s_909gauss
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0029P)^2^+10.7821P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0029P)^2^+10.7821P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4324476