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_4312866
_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         'Fe16 S16 (PCy3)8'
_chemical_formula_sum            'C156 H292 Fe16 O3 P8 S16'
_chemical_formula_weight         3870.22
_chemical_name_systematic
;
octakis(bis(\m3-sulfido)tricyclohexylphosphine-di-iron) ether 
tetrahydrofuran solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.0920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.095(2)
_cell_length_b                   20.3615(14)
_cell_length_c                   34.992(3)
_cell_measurement_reflns_used    5595
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      2.27
_cell_volume                     20006(3)
_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    0.0524
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            42668
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rhombic plate'
_exptl_crystal_F_000             8176
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         13082
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+39.5325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                9401
_reflns_number_total             13082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020464t_5.cif
_cod_data_source_block           compd11
_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 
;
_cod_original_cell_volume        20006(2)
_cod_database_code               4312866