[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_4316078
_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         '(Fe 3+)4 (S 2-)4 (C6H18NSi2 1-)4'
_chemical_formula_structural     Fe4S4(N(SiC3H9)2)4
_chemical_formula_sum            'C24 H72 Fe4 N4 S4 Si8'
_chemical_formula_weight         993.22
_chemical_name_common            Fe4(mu3-S)4[N(TMS)2]4
_chemical_name_systematic
; 
 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                 97.901(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9406(6)
_cell_length_b                   12.5027(5)
_cell_length_c                   27.2026(8)
_cell_measurement_reflns_used    19190
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      1.38
_cell_volume                     5033.1(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.049
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19190
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         1.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_T_max  0.8055
_exptl_absorpt_correction_T_min  0.7279
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+4.7961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1127
_refine_ls_wR_factor_obs         0.0972
_reflns_number_gt                4977
_reflns_number_total             6984
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic100742c_si_002_2.cif
_cod_data_source_block           326ell
_cod_database_code               4316078