[Fe4S4]q Cubane Clusters (q= 4+, 3+, 2+) with Terminal Amide Ligands
Christopher R. Sharp; Jeremiah S. Duncan; Sonny C. Lee; Inorganic Chemistry 49 (2010) 6697–6705; doi:10.1021/ic100742c

data_4316079
_publ_contact_author_address
;                                                                               
 Department of Chemistry
 University of Waterloo
 200 University Avenue West
 Waterloo, Ontario  N2L 3G1
 CANADA  
;
_publ_contact_author_email       sclee@uwaterloo.ca
_publ_contact_author_fax         519-746-0435
_publ_contact_author_name        'Sonny C. Lee'
_publ_contact_author_phone       '519-885-1211 x37501'
_publ_section_title
;
 [Fe4S4]q Cubane Clusters (q= 4+, 3+, 2+) with Terminal Amide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6697
_journal_page_last               6705
_journal_paper_doi               10.1021/ic100742c
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'Chemical synthesis, S.C. Lee lab'
_chemical_formula_moiety
'[(Na +) (C4 H8 O)2] [(Fe 2+)(Fe 3+)3(S 2-)4 (C6 H18 N Si2 -)4]'
_chemical_formula_structural     '[Na(O C4 H8)2] [Fe4S4(N(Si C3 H9)2)4)]'
_chemical_formula_sum            'C32 H88 Fe4 N4 Na O2 S4 Si8'
_chemical_formula_weight         1160.41
_chemical_name_common            '[Na(THF)2]{Fe4(mu3-S)4[N(TMS)2]4}'
_chemical_name_systematic
; 
 [Na(THF)2]{Fe4(mu3-S)4[N(TMS)2]4} 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.6050(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3146(5)
_cell_length_b                   21.7116(8)
_cell_length_c                   22.7562(10)
_cell_measurement_reflns_used    30199
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.30
_cell_volume                     6043.9(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        'DENZO-SMN, Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL, Olex2'
_computing_publication_material  'CIFTAB, SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997), PLATON'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_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  0.062
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30199
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.9105
_exptl_absorpt_correction_T_min  0.7847
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown-black
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopipped
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         13785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+1.6630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                7876
_reflns_number_total             13785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100742c_si_002_3.cif
_cod_data_source_block           486_14
_cod_database_code               4316079