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_1100748
_publ_section_title
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The First Cobalt Metallacrowns: Preparation and Characterization of

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

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_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            'C54 H70.16 Cl2 Co4 N12 O27.08'
_chemical_formula_weight         1627.28
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           2
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_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                110.15(1)
_cell_angle_beta                 95.25(2)
_cell_angle_gamma                92.05(2)
_cell_formula_units_Z            1
_cell_length_a                   10.523(5)
_cell_length_b                   13.556(5)
_cell_length_c                   12.465(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.3
_cell_volume                     1658.0(12)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       '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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5936
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.157
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      1.62
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             837
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.136
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5653
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_obs          0.0596
_refine_ls_shift/esd_max         0.146
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.8053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1696
_refine_ls_wR_factor_obs         0.1546
_reflns_number_observed          4454
_reflns_number_total             5654
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic050208rsi20050207_081321.cif
_cod_data_source_block           pexs532
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.8053P] 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^)+(0.0817P)^2^+2.8053P] 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        1657.8(2)
_cod_database_code               1100748