Synthesis and structure of an unprecedented high-symmetry [Fe4S4Cl4] cubane-type unit in supramolecular [K4(FeCl4)(C12H24O6)4][Fe4S4Cl4]
Willems, Johannes B.; Köckerling, Martin; Chemical Communications  (2001) 1380–; doi:10.1039/b103871k

data_7114736
_publ_section_title
;
 Synthesis and structure of an unprecedented high-symmetry [Fe4S4Cl4]
 cubane-type unit in supramolecular [K4(FeCl4)(C12H24O6)4][Fe4S4Cl4]
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1380
_journal_paper_doi               10.1039/b103871k
_journal_year                    2001
_chemical_formula_moiety         '[(C12 H24 O6)4 K4 (Fe Cl4)] [Fe4 S4 Cl4]'
_chemical_formula_sum            'C48 H96 Cl8 Fe5 K4 O24 S4'
_chemical_formula_weight         1904.740
_space_group_IT_number           196
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             january-22-2001
_audit_creation_method           'ct.exe (M. K\"ockerling, 1996)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.241(2)
_cell_length_b                   21.241(2)
_cell_length_c                   21.241(2)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.7
_cell_measurement_theta_min      1.8
_cell_volume                     9583.5(16)
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL (Sheldrick, 1990'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tune'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23259
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_description       'small cylinder'
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.3
_refine_ls_extinction_coef       0.0006(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1973
_refine_ls_number_restraints     4
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.1021P)^2^+0.0000P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.175
_reflns_number_gt                1182
_reflns_number_total             1973
_reflns_threshold_expression     '> 2.0sigma(I)'
_cod_data_source_file            b103871k.txt
_cod_data_source_block           Cuban-1
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C49 H96 Fe5 K4 L8 O24 S4' to 'C29 H22 Cl2 Fe O4 P2 Pt'.

 Antanas Vaitkus,
 2017-01-15

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'CALC
W=1/[\S^2^(FO^2^)+(0.1021P)^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^)+(0.1021P)^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        9583(4)
_cod_original_formula_sum        'C48 H96 CL8 Fe5 K4 O24 S4'
_cod_database_code               7114736