Tetrakis(2,2'-bipyridine)tetra-μ~3~-hydroxo-di-μ-trifluoroacetato-tetracobalt(II) diiodide diacetonitrile monohydrate: a compound containing a tetranuclear `cubane'-type cobalt(II) core
Zhao, Hanhua; Bacsa, John; Kim R. Dunbar; Acta Crystallographica Section E 60 (2004) m637–m640; doi:10.1107/S1600536804008979

data_2203595
_publ_section_title
;Tetrakis(2,2'-bipyridine)tetra-\m~3~-hydroxo-di-\m-trifluoroacetato-tetracobalt(II)
 diiodide diacetonitrile monohydrate: a compound containing a tetranuclear
 `cubane'-type cobalt(II) core
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m637
_journal_page_last               m640
_journal_paper_doi               10.1107/S1600536804008979
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Co4 (C2 F3 O2)2 (O H)4 (C10 H8 N2)4] I2, 2C2 H3 N, H2 O'
_chemical_formula_moiety
'C44 H36 Co4 F6 N8 O8 2+, 2I -, 2C2 H3 N, H2 O'
_chemical_formula_sum            'C48 H44 Co4 F6 I2 N10 O9'
_chemical_formula_weight         1508.45
_chemical_name_systematic
;
Tetrakis(2,2'-bipyridine)tetra-\m~3~-hydroxo-di-\m-trifluoroacetato-
tetracobalt(II) diiodide diacetonitrile monohydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0270(10)
_cell_length_b                   18.7740(10)
_cell_length_c                   29.771(2)
_cell_measurement_reflns_used    5517
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.45
_cell_volume                     11193.5(11)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement
;
X-SEED (Barbour, 2001) and SHELXL97 (Sheldrick, 1997)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            72201
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.350
_exptl_absorpt_correction_T_max  0.7821
_exptl_absorpt_correction_T_min  0.5490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5936
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.002
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         12523
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0647P)^2^+25.7334P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                8819
_reflns_number_total             12523
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl6099.cif
_cod_data_source_block           I
_cod_original_cell_volume        11194.0(10)
_cod_database_code               2203595
_cod_database_fobs_code          2203595