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_4326712
_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_absolute_configuration ad
_chemical_formula_sum            'C36 H84 Fe4 N2 S8'
_chemical_formula_weight         1024.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 90.944(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8574(10)
_cell_length_b                   19.5918(12)
_cell_length_c                   16.2711(11)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.57
_cell_volume                     5054.3(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22055
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.8907
_exptl_absorpt_correction_T_min  0.7560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         11608
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                7810
_reflns_number_total             11608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2016269_si_004_1.cif
_cod_data_source_block           NJ66
_cod_database_code               4326712