Reactivity of a Sterically Hindered Fe(II) Thiolate Dimer with Amines and Hydrazines
Michael J. Zdilla; Atul K. Verma; Sonny C. Lee; Inorganic Chemistry 47 (2008) 11382–11390; doi:10.1021/ic801349y

data_4306528
_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
;
Reactivity of a Sterically Hindered Fe(II) Thiolate Dimer with Amines and
Hydrazines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11382
_journal_page_last               11390
_journal_paper_doi               10.1021/ic801349y
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'Chemical Synthesis, S.C. Lee Lab'
_chemical_formula_structural     'Fe2(N2H4)6(C24H17S)4, (N2H4), (C4H8O)1.5)'
_chemical_formula_sum            'C96 H92 Fe2 N12 O0 S4'
_chemical_formula_weight         1653.76
_chemical_name_common            'Iron Hydrazine Dimer (4)'
_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-97
_cell_angle_alpha                68.624(5)
_cell_angle_beta                 89.564(4)
_cell_angle_gamma                83.087(5)
_cell_formula_units_Z            2
_cell_length_a                   13.5817(14)
_cell_length_b                   18.8132(15)
_cell_length_c                   19.608(2)
_cell_measurement_reflns_used    12032
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      1.12
_cell_volume                     4628.0(8)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    0.0891
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16131
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Disordered solvent THF and N2H4 squeezed out, and replaced with dummy
atoms.  Identity of THF on special position is not confirmed to a high
level of certainty.  The disorder-treated model using THF refined to 
better statistics than the disorder-treated model which used N2H4 at 
the special position solvent.
;
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         16131
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                10674
_reflns_number_total             16131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801349y_si_002_5.cif
_cod_data_source_block           4
_cod_original_cell_volume        4627.9(8)
_cod_database_code               4306528