Octanuclear cobalt and nickel cages featuring formate ligands
Cadiou, Cyril; Coxall, Robert A.; Graham, Alasdair; Harrison, Andrew; Helliwell, Madeleine; Parsons, Simon; Winpenny, Richard E. P.; Chemical Communications  (2002) 1106–; doi:10.1039/b202062a

data_7114235
_publ_section_title
;
 Octanuclear cobalt and nickel cages featuring formate ligands
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              1106
_journal_paper_doi               10.1039/b202062a
_journal_year                    2002
_chemical_formula_sum            'C203 H177.5 Cl4 Co8 N4 Na2 O43.25'
_chemical_formula_weight         4024.21
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             19101-10-02
_audit_creation_method           'by teXsan v1.7'
_audit_update_record
;
?
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.31(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.29(5)
_cell_length_b                   17.630(10)
_cell_length_c                   39.81(5)
_cell_measurement_reflns_used    211823
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.77
_cell_measurement_theta_min      1.56
_cell_volume                     19470(4)
_computing_cell_refinement       'DENZO (Otwinowski, Z. 1988)'
_computing_data_collection       'MSC RAXIS11 Control'
_computing_data_reduction        'DENZO (Otwinowski, Z. 1988)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'previous Ni analogue used'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.592
_diffrn_measured_fraction_theta_max 0.592
_diffrn_measurement_device       'Rigaku RAXIS'
_diffrn_measurement_method       '110 x 3 degree phi scans'
_diffrn_radiation_detector       'image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.092
_diffrn_reflns_av_sigmaI/netI    0.1288
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            211823
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8302
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2102
_refine_ls_number_reflns         20500
_refine_ls_number_restraints     8456
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                9820
_reflns_number_total             20500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202062a.txt
_cod_data_source_block           s1004sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+0.0000P] 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^)+(0.1079P)^2^+0.0000P] 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        19470(44)
_cod_original_sg_symbol_H-M      'P 2/c      '
_cod_original_formula_sum        'C203 H177.50 Cl4 Co8 N4 Na2 O43.25'
_cod_database_code               7114235