Iron-Promoted Nucleophilic Additions to Diimine-Type Ligands: A Synthetic and Structural Study
Ana Tesouro Vallina; Helen Stoeckli-Evans; Antonia Neels; Jürgen Ensling; Silvio Decurtins; Inorganic Chemistry 42 (2003) 3374–3382; doi:10.1021/ic026079l

data_4313626
_publ_section_title
;
 Iron-Promoted Nucleophilic Additions to Diimine-Type Ligands: A Synthetic
 and Structural Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3374
_journal_page_last               3382
_journal_paper_doi               10.1021/ic026079l
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C38 H28 F6 Fe N12 O8 S2'
_chemical_formula_weight         1014.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.467(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5521(9)
_cell_length_b                   19.1275(9)
_cell_length_c                   19.7950(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
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_cell_measurement_theta_min      2.07
_cell_volume                     4346.1(6)
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.1348
_diffrn_reflns_av_sigmaI/netI    0.1473
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
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_diffrn_reflns_limit_l_min       -24
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_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
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_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   empirical_DIFABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
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_refine_diff_density_max         1.050
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1138P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2128
_reflns_number_gt                3633
_reflns_number_total             8343
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic026079lsi20021002_050055_1.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        4346.1(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C38 H28 F6 Fe1 N12 O8 S2'
_cod_database_code               4313626