Rational Synthesis of High Nuclearity Mo/Fe/S Clusters: The Reductive Coupling Approach in the Convenient Synthesis of (Cl4-cat)2Mo2Fe6S8(PR3)6 [R = Et, nPr, nBu] and the New [(Cl4-cat)2Mo2Fe2S3O(PEt3)3Cl].1/2(Fe(PEt3)2(MeCN)4) and (Cl4-cat)2Mo2Fe3S5(PEt3)5 Clusters
Jaehong Han; Markos Koutmos; Saleem Al Ahmad; Dimitri Coucouvanis; Inorganic Chemistry 40 (2001) 5985–5999; doi:10.1021/ic0104914

data_4320513
_publ_contact_author             'Dimitri Coucouvanis'
_publ_contact_author_address
;
  Dimitri Coucouvanis
  Department of Chemistry
  The University of Michigan
  Ann Arbor, MI 48109
  USA
;
_publ_contact_author_email       dcouc@umich.edu
_publ_section_title
;
 Rational Synthesis of High Nuclearity Mo/Fe/S Clusters: The Reductive
 Coupling Approach in the Convenient Synthesis of (Cl4-cat)2Mo2Fe6S8(PR3)6
 [R = Et, nPr, nBu] and the New
 [(Cl4-cat)2Mo2Fe2S3O(PEt3)3Cl].1/2(Fe(PEt3)2(MeCN)4) and
 (Cl4-cat)2Mo2Fe3S5(PEt3)5 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5985
_journal_page_last               5999
_journal_paper_doi               10.1021/ic0104914
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C54 H126 F6 Fe6 P7 S8'
_chemical_formula_weight         1697.92
_chemical_name_common            (PF6)[Fe6S8(PnPr3)6]
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.1878(14)
_cell_length_b                   14.1878(14)
_cell_length_c                   66.895(9)
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.77
_cell_volume                     11661(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -83
_diffrn_reflns_number            34985
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    1.496
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5358
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+96.7437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                2442
_reflns_number_total             2669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104914_3.cif
_cod_data_source_block           compound_V
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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 
;
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4320513