Self-Assembling Synthesis of Cyclic Tri- and Tetranuclear Cobalt(III) Complexes Bridged by Purine-6-thione and Their Characterization by Electrospray Mass Spectrometry and X-ray Crystal Analysis
Kazuaki Yamanari; Ito Fukuda; Tatsuya Kawamoto; Yoshihiko Kushi; Akira Fuyuhiro; Naoko Kubota; Tsuyoshi Fukuo; Ryuichi Arakawa; Inorganic Chemistry 37 (1998) 5611–5618; doi:10.1021/ic9802146

data_4323094
_publ_section_title
;
 Self-Assembling Synthesis of Cyclic Tri- and Tetranuclear Cobalt(III)
 Complexes Bridged by Purine-6-thione and Their Characterization by
 Electrospray Mass Spectrometry and X-ray Crystal Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5611
_journal_page_last               5618
_journal_paper_doi               10.1021/ic9802146
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C48 H92 Co4 F12 N28 O24 S8'
_chemical_formula_weight         2165.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Thu May 29 14:07:29 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                97.37(4)
_cell_angle_beta                 106.76(4)
_cell_angle_gamma                112.78(3)
_cell_formula_units_Z            2
_cell_length_a                   18.410(8)
_cell_length_b                   18.772(8)
_cell_length_c                   15.677(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     4603(4)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.05465
_diffrn_orient_matrix_UB_12      -0.03627
_diffrn_orient_matrix_UB_13      -0.05239
_diffrn_orient_matrix_UB_21      0.00537
_diffrn_orient_matrix_UB_22      -0.04783
_diffrn_orient_matrix_UB_23      0.01681
_diffrn_orient_matrix_UB_31      -0.03170
_diffrn_orient_matrix_UB_32      0.00078
_diffrn_orient_matrix_UB_33      0.04199
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.19
_diffrn_reflns_av_sigmaI/netI    0.097
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21804
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        -3.76
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2416.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   4.071
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     856
_refine_ls_number_reflns         9748
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0768
_refine_ls_shift/esd_max         0.0240
_refine_ls_shift/esd_mean        0.0040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1053
_reflns_number_observed          9748
_reflns_number_total             21144
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic9802146_1.cif
_cod_data_source_block           '[Co4(mpu)4(tacn)4](CF3SO3)4.12H2O-2a(CR2)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00010|Fo|^2^]' 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) + 0.00010|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C48 H92 Co4 F12 N28 O24 S8 '
_cod_database_code               4323094