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_4306529
_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_moiety
'[(Fe 3+) (C13 H12 N2 1-)2 (C24 H17 S 1-)], (C6 H6)'
_chemical_formula_structural     'Fe(N2 C13 H12)2(S C24 H17), (C6 H6)'
_chemical_formula_sum            'C56 H47 Fe N4 S'
_chemical_formula_weight         863.89
_chemical_name_common            'ortho-semidine complex (5a)'
_chemical_name_systematic
;
bis(N-methylphenyl-N'-phenyl-o-semidino)
2,4,6-triphenylbenzenethiolatoiron(III)
;
_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                 112.67(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.363(2)
_cell_length_b                   19.154(4)
_cell_length_c                   21.950(4)
_cell_measurement_reflns_used    18063
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.46
_cell_volume                     4408.3(17)
_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_type  '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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18063
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark Purple'
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         7776
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+4.2608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                6184
_reflns_number_total             7776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801349y_si_002_6.cif
_cod_data_source_block           5a
_cod_original_cell_volume        4408.3(15)
_cod_database_code               4306529