A mononuclear cobalt(III) complex of the ligand <i>N,N</i>'-bis(pyridin-2-ylmethyl)pyrazine-2,3-dicarboxamide
Dilovan S. Cati; Helen Stoeckli-Evans; Acta Crystallographica Section E 60 (2004) m174–m176; doi:10.1107/S1600536804000431

data_2203188
_publ_section_title
;
 A mononuclear cobalt(III) complex of the ligand
 <i>N,N</i>'-bis(pyridin-2-ylmethyl)pyrazine-2,3-dicarboxamide
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m174
_journal_page_last               m176
_journal_paper_doi               10.1107/S1600536804000431
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (C18 H16 N6 O2)2] (Cl O4)3, 3.5C2 H3 N'
_chemical_formula_moiety         'C36 H32 Co N12 O4 3+, 3Cl O4 1-, 3.5C2 H3 N'
_chemical_formula_sum            'C43 H42.5 Cl3 Co N15.5 O16'
_chemical_formula_weight         1197.71
_chemical_name_systematic
;
bis[N,N'-bis(pyridin-2-ylmethyl)pyrazine-2,3-dicarboxamide]cobalt(III)
tris(perchlorate) acetonitrile 3.5-solvate
;
_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-97
_cell_angle_alpha                100.197(5)
_cell_angle_beta                 111.189(5)
_cell_angle_gamma                99.505(5)
_cell_formula_units_Z            2
_cell_length_a                   13.174(5)
_cell_length_b                   14.061(5)
_cell_length_c                   15.905(5)
_cell_measurement_reflns_used    6268
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.91
_cell_volume                     2618.0(16)
_computing_cell_refinement       'CELL (Stoe & Cie, 2000)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20558
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         9551
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = [exp{3(sin\q/\l)^2^}]/[\s^2^(Fo^2^)+(0.032P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                3742
_reflns_number_total             9551
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6077.cif
_cod_data_source_block           I
_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 
;
_cod_original_formula_sum        'C43 H42.50 Cl3 Co N15.50 O16'
_cod_database_code               2203188