Synthesis and Reactions of Cubane-Type Iron-Sulfur-Phosphine Clusters, Including Soluble Clusters of Nuclearities 8 and 16
Hong-Cai Zhou; R. H. Holm; Inorganic Chemistry 42 (2003) 11–21; doi:10.1021/ic020464t

data_4312865
_publ_section_title
;
 Synthesis and Reactions of Cubane-Type Iron-Sulfur-Phosphine Clusters,
 Including Soluble Clusters of Nuclearities 8 and 16
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11
_journal_page_last               21
_journal_paper_doi               10.1021/ic020464t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'Fe8 S8 (PiPr3)6'
_chemical_formula_sum            'C54 H126 Fe8 P6 S8'
_chemical_formula_weight         1664.65
_chemical_name_systematic
;
  bis(\m4-sulfido)hexakis(\m3-sulfido)hexakis(tri-i-propylphosphine)-
octa-iron
;
_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                72.603(2)
_cell_angle_beta                 67.513(2)
_cell_angle_gamma                80.848(3)
_cell_formula_units_Z            1
_cell_length_a                   12.7076(17)
_cell_length_b                   12.9869(17)
_cell_length_c                   13.3260(17)
_cell_measurement_reflns_used    2746
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.45
_cell_volume                     1936.6(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8428
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5049
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.146
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+0.3973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1631
_reflns_number_gt                3519
_reflns_number_total             5049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020464t_4.cif
_cod_data_source_block           compd9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_database_code               4312865