[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_4316077
_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
'[(Li +) (C4 H8 O)4] [(Fe 2+)(Fe 3+)3(S 2-)4 (C6 H18 N Si2 -)4]'
_chemical_formula_structural     '[Li(O C4 H8)4] [Fe4S4(N(Si C3 H9)2)4]'
_chemical_formula_sum            'C40 H104 Fe4 Li N4 O4 S4 Si8'
_chemical_formula_weight         1288.57
_chemical_name_common            '[Li(THF)4]{Fe4(mu3-S)4[N(TMS)2]4}'
_chemical_name_systematic
; 
  [Li(THF)4]{Fe4(mu3-S)4[N(TMS)2]4} 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7066(7)
_cell_length_b                   12.7066(7)
_cell_length_c                   21.6126(14)
_cell_measurement_reflns_used    15529
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      1.86
_cell_volume                     3489.5(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1222
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15529
_diffrn_reflns_theta_full        23.98
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.9729
_exptl_absorpt_correction_T_min  0.8090
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_obs          0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.8473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0904
_refine_ls_wR_factor_ref         0.1032
_reflns_number_observed          1899
_reflns_number_total             2741
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic100742c_si_002_1.cif
_cod_data_source_block           199gauss_114
_cod_database_code               4316077