The First Cobalt Metallacrowns: Preparation and Characterization of Mixed-Valence Cobalt(II/III), Inverse 12-Metallacrown-4 Complexes
Theocharis C. Stamatatos; Stavroula Dionyssopoulou; Georgios Efthymiou; Panayotis Kyritsis; Catherine P. Raptopoulou; Aris Terzis; Ramon Vicente; Albert Escuer; Spyros P. Perlepes; Inorganic Chemistry 44 (2005) 3374–3376; doi:10.1021/ic050208r

data_1100749
_publ_section_title
;

The First Cobalt Metallacrowns: Preparation and Characterization of

Mixed-Valence Cobalt(II/III), Inverse 12-Metallacrown-4 Complexes

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3374
_journal_page_last               3376
_journal_paper_doi               10.1021/ic050208r
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C59.6 H78.4 Co4 F12 N12 O17.6 P2'
_chemical_formula_weight         1770.20
_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-97
_cell_angle_alpha                70.09(1)
_cell_angle_beta                 80.60(1)
_cell_angle_gamma                69.86(1)
_cell_formula_units_Z            1
_cell_length_a                   11.867(4)
_cell_length_b                   14.534(6)
_cell_length_c                   12.289(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      5.4
_cell_volume                     1868.5(13)
_computing_cell_refinement
'Program LEAST (UCLA Cryst.package C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Cryst.package C.E.Strouse 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Cryst.package C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-2theta scans'
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6364
_diffrn_reflns_theta_full        24.25
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.018
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_meas      1.56
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             907
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.569
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+3.2720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1602
_reflns_number_gt                4376
_reflns_number_total             6046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050208rsi20050207_081352.cif
_cod_data_source_block           pesd185
_cod_original_cell_volume        1868.3(1)
_cod_original_formula_sum        'C59.60 H78.40 Co4 F12 N12 O17.60 P2'
_cod_database_code               1100749