Changing Mixed-valence State of Hexacobalt Cluster by Substituting Central Metal Ion and by Electrochemical Reduction – Different Mixed-valence States of [M{Co(prolinato)2}6]4+ (M =Ba2+ and La3+)
Takashi Komiyama; Satoshi Igarashi; Yoshimasa Hoshino; Yasuhiko Yukawa; Chemistry Letters 34 (2005) 300–; doi:10.1246/cl.2005.300

data_8000031
_publ_section_title
;
 Changing Mixed-valence State of Hexacobalt Cluster by Substituting
 Central Metal Ion and by Electrochemical Reduction -- Different
 Mixed-valence States of [M{Co(prolinato)2}6]4+ (M \\db Ba2+ and La3+)
;
_journal_issue                   3
_journal_name_full               'Chemistry Letters'
_journal_page_first              300
_journal_paper_doi               10.1246/cl.2005.300
_journal_volume                  34
_journal_year                    2005
_chemical_formula_sum            'C68 H120 Ba Cl4 Co6 N14 O40'
_chemical_formula_weight         2406.51
_chemical_name_common
;hexakis{bis(L-prolinato)cobalt(II)}barium(II)
 tetramethylammonium perchlorate
;
_space_group_IT_number           196
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      196
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.6417(4)
_cell_length_b                   21.6417(4)
_cell_length_c                   21.6417(4)
_cell_measurement_reflns_used    48518
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      1.9
_cell_volume                     10136.2(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31025
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_exptl_absorpt_coefficient_mu    1.533
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tetrahedral
_exptl_crystal_F_000             4928.00
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.71
_refine_ls_abs_structure_Flack   0.1(1)
_refine_ls_extinction_coef       0.0008(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     80
_refine_ls_number_reflns         916
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.0102
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00360|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                916
_reflns_number_total             1657
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-07-11
;
_cod_original_sg_symbol_H-M      'F 2 3        '
_cod_original_formula_sum        'C68 H120 Ba Cl4 Co6 N14 O40 '
_cod_database_code               8000031