Mixed-valence, tetranuclear cobalt(iii,iv) complexes: preparation and properties of [Co4O4(O2CR)2(bpy)4]3+ salts
Dimitrou, Katerina; Brown, Angelica D.; Christou, George; Concolino, Thomas E.; Rheingold, Arnold L.; Chemical Communications  (2001) 1284–; doi:10.1039/b102008k

data_7114990
_publ_section_title
;
 Mixed-valence, tetranuclear cobalt(iii,iv) complexes: preparation and
 properties of [Co4O4(O2CR)2(bpy)4]3+ salts
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1284
_journal_paper_doi               10.1039/b102008k
_journal_year                    2001
_chemical_formula_sum            'C56 H49 Cl3 Co4 N11 O27'
_chemical_formula_weight         1650.13
_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                91.8195(6)
_cell_angle_beta                 95.8450(8)
_cell_angle_gamma                110.1203(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6330(2)
_cell_length_b                   14.1304(2)
_cell_length_c                   20.7165(2)
_cell_measurement_temperature    173(2)
_cell_volume                     3172.77(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18626
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   'Empirical from DIFABS'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.750
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         10537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.750
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2279
_reflns_number_gt                8985
_reflns_number_total             10537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102008k.txt
_cod_data_source_block           chr03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3172.78(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114990