Deprotonation/protonation-driven change of the σ-donor ability of a sulfur atom in iron(ii) complexes with a thioamide SNS pincer type ligand.
Suzuki, Tatsuya; Kajita, Yuji; Masuda, Hideki; Dalton transactions (Cambridge, England : 2003) 43 (2014) 9732–9739; doi:10.1039/c4dt00524d

data_7030398
_publ_section_title
;
 Deprotonation/protonation-driven change of the \s-donor ability of a
 sulfur atom in iron(ii) complexes with a thioamide SNS pincer type
 ligand.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9732
_journal_page_last               9739
_journal_paper_doi               10.1039/c4dt00524d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C124 H119 Fe N6 S2'
_chemical_formula_sum            'C124 H119 Fe N6 S2'
_chemical_formula_weight         1813.31
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                107.334(3)
_cell_angle_beta                 108.6612(3)
_cell_angle_gamma                105.3219(14)
_cell_formula_units_Z            2
_cell_length_a                   15.521(4)
_cell_length_b                   19.590(5)
_cell_length_c                   20.683(5)
_cell_measurement_reflns_used    11187
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     5219(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52730
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1926.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
There is a benzene at special position on unit cell, 
in which disordered benzene solvent could not be modeled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 27 electrons per unit cell,
which were assigned to be half of C6H6 molecule per unit
cell.
;
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.590
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         23560
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0995P)^2^+1.5138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                16630
_reflns_number_total             23560
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4dt00524d2.cif
_cod_data_source_block           FeCN_20140130_4
_cod_depositor_comments
'Adding full bibliography for 7030394--7030398.cif.'
_cod_database_code               7030398