Cubane-Type Fe4S4 Clusters with Chiral Thiolate Ligation: Formation by Ligand Substitution, Detection of Intermediates by 1H NMR, and Solid State Structures Including Spontaneous Resolution Upon Crystallization
Wayne Lo; Shaw Huang; Shao-Liang Zheng; R. H. Holm; Inorganic Chemistry 50 (2011) 11082–11090; doi:10.1021/ic2016269

data_4326713
_publ_section_title
;
 Cubane-Type Fe4S4 Clusters with Chiral Thiolate Ligation: Formation by
 Ligand Substitution, Detection of Intermediates by 1H NMR, and Solid
 State Structures Including Spontaneous Resolution Upon Crystallization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11082
_journal_page_last               11090
_journal_paper_doi               10.1021/ic2016269
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C48 H76 Fe4 N2 S8'
_chemical_formula_weight         1160.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.943(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5438(6)
_cell_length_b                   22.6639(12)
_cell_length_c                   21.5340(12)
_cell_measurement_reflns_used    11171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      2.23
_cell_volume                     5626.5(5)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector  
;
_diffrn_measurement_method       'omega and phi 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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48913
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.9360
_exptl_absorpt_correction_T_min  0.7753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         12428
_refine_ls_number_restraints     661
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0438P)^2^+25.3605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1896
_reflns_number_gt                7189
_reflns_number_total             12428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016269_si_004_2.cif
_cod_data_source_block           NJ43
_cod_database_code               4326713