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_4313099
_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     '[C50 H50 Co2 N12 O4], 4 CH2Cl2'
_chemical_formula_sum            'C54 H58 Cl8 Co2 N12 O4'
_chemical_formula_weight         1340.58
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                113.72(2)
_cell_angle_beta                 103.35(2)
_cell_angle_gamma                102.22(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3351(8)
_cell_length_b                   13.1244(10)
_cell_length_c                   13.3233(11)
_cell_measurement_reflns_used    5659
_cell_measurement_temperature    100(2)
_cell_volume                     1512.8(5)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w, 0.3 deg./frame'
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16013
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick 1994'
_exptl_crystal_colour            'red violet'
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.909
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         9710
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_obs          0.0519
_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^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1222
_refine_ls_wR_factor_obs         0.1092
_reflns_number_observed          6003
_reflns_number_total             9718
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020518z_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0603P)^2^+0.0000P] 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^)+(0.0603P)^2^+0.0000P] 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        1512.8(2)
_cod_database_code               4313099