Dinuclear Cyano Complexes of Cobalt(III) and Iron(III) Containing Noninnocent 1,2,4,5-Tetrakis(2-pyridinecarboxamido)benzene Bridging Ligands
Udo Beckmann; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 42 (2003) 1045–1056; doi:10.1021/ic020518z

data_4313100
_publ_section_title
;
 Dinuclear Cyano Complexes of Cobalt(III) and Iron(III) Containing
 Noninnocent 1,2,4,5-Tetrakis(2-pyridinecarboxamido)benzene Bridging
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1045
_journal_page_last               1056
_journal_paper_doi               10.1021/ic020518z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural     '2 [NBu4]+, [C30 H18 N20 O4 Fe2]2-, 3 MeCN'
_chemical_formula_sum            'C68 H99 Fe2 N25 O4'
_chemical_formula_weight         1442.42
_chemical_name_systematic
;
   ?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.34(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.5944(12)
_cell_length_b                   20.215(2)
_cell_length_c                   14.4511(12)
_cell_measurement_reflns_used    12475
_cell_measurement_temperature    100(2)
_cell_volume                     3971.1(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w, 693 frames a 90 sec. / 1 deg.'
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61805
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9071
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.144
_refine_ls_restrained_S_obs      1.165
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_obs          0.0719
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1690P)^2^+0.5880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2638
_refine_ls_wR_factor_obs         0.2236
_reflns_number_observed          6302
_reflns_number_total             9114
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020518z_3.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1690P)^2^+0.5880P] 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^)+(0.1690P)^2^+0.5880P] 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        3971.1(6)
_cod_database_code               4313100