Molecular and Electronic Structure of Five-Coordinate Complexes of Iron(II/III) Containingo-Diiminobenzosemiquinonate(1-) π Radical Ligands
Krzysztof Chłopek; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 44 (2005) 7087–7098; doi:10.1021/ic050829k

data_4309673
_publ_section_title
;
Molecular and Electronic Structure of Five-Coordinate Complexes of
Iron(II/III) Containingo-Diiminobenzosemiquinonate(1-) \p Radical Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7087
_journal_page_last               7098
_journal_paper_doi               10.1021/ic050829k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_structural     'C39 H31 Fe N6'
_chemical_formula_sum            'C39 H31 Fe N6'
_chemical_formula_weight         639.55
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.334(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4433(3)
_cell_length_b                   17.7647(6)
_cell_length_c                   17.0145(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3123.23(18)
_computing_cell_refinement       'Nonius Kappa-CCD'
_computing_data_collection       'Nonius Kappa-CCD'
_computing_data_reduction        'Nonius Kappa-CCD'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '950 images at 1.0 deg. \w, 90 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            75693
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_correction_T_min  0.9054
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         9890
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_obs          0.0434
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.9660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1000
_refine_ls_wR_factor_obs         0.0934
_reflns_number_observed          8309
_reflns_number_total             9914
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic050829ksi20050523_064057_5.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+1.9660P] 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^)+(0.0353P)^2^+1.9660P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3123.2(2)
_cod_database_code               4309673