Tris(2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')cobalt(III) bis[bis(pyridine-2,6-dicarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)cobaltate(III)] perchlorate dimethylformamide hemisolvate 1.3-hydrate
Golenya, Irina A.; Boyko, Alexander N.; Kotova, Natalia V.; Haukka, Matti; Iskenderov, Turganbay S.; Acta Crystallographica Section E 68 (2012) m1237–m1238; doi:10.1107/S1600536812037208

data_2236346
_publ_section_title
;
 Tris(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')cobalt(III)
 bis[bis(pyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)cobaltate(III)]
 perchlorate dimethylformamide hemisolvate 1.3-hydrate
;
_journal_coeditor_code           HY2582
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1237
_journal_page_last               m1238
_journal_paper_doi               10.1107/S1600536812037208
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Co (C10 H8 N2)3] [Co (C7 H3 N O4)2]2 (Cl O4), 0.5C3 H7 N O, 1.3H2 O'
_chemical_formula_moiety
'C30 H24 Co N6 3+, 2(C14 H6 Co N2 O8 -), Cl O4 -, 0.5(C3 H7 N O), 1.3(H2 O)'
_chemical_formula_sum            'C59.5 H42.1 Cl Co3 N10.5 O21.8'
_chemical_formula_weight         1465.18
_chemical_name_systematic
;
Tris(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')cobalt(III)
bis[bis(pyridine-2,6-dicarboxylato-
\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)cobaltate(III)] perchlorate
dimethylformamide hemisolvate 1.3-hydrate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.286(2)
_cell_angle_beta                 107.128(3)
_cell_angle_gamma                90.190(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1988(4)
_cell_length_b                   14.7317(6)
_cell_length_c                   16.6016(8)
_cell_measurement_reflns_used    50715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.29
_cell_volume                     3019.8(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50715
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.9285
_exptl_absorpt_correction_T_min  0.7526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.341
_refine_diff_density_min         -1.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         13787
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0882P)^2^+6.7880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                9788
_reflns_number_total             13787
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2582.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C59.5 H42.10 Cl Co3 N10.5 O21.80'
_cod_database_code               2236346
_cod_database_fobs_code          2236346