A Continuous Symmetry Measure of [4Fe-4S]+ Core Distortions and Analysis of Supramolecular Synthons in Crystal Structures of (Et4N)3[Fe4S4Cl4].Et4NCl at 100 and 295 K
Karl S. Hagen; Mohammad Uddin; Inorganic Chemistry 47 (2008) 11807–11815; doi:10.1021/ic801533q

data_4306719
_publ_contact_author_address
;
Department of Chemistry
Emory University
Atlanta, GA 30322
USA
;
_publ_contact_author_email       khagen@emory.edu
_publ_contact_author_fax         1-404-727-6556
_publ_contact_author_name        'Karl S. Hagen'
_publ_contact_author_phone       1-404-727-6586
_publ_section_title
;
A Continuous Symmetry Measure of [4Fe-4S]+ Core Distortions and Analysis
of Supramolecular Synthons in Crystal Structures of
(Et4N)3[Fe4S4Cl4].Et4NCl at 100 and 295 K
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11807
_journal_page_last               11815
_journal_paper_doi               10.1021/ic801533q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         '4(C8 H20 N), Cl4 Fe4 S4, Cl'
_chemical_formula_sum            'C32 H80 Cl5 Fe4 N4 S4'
_chemical_formula_weight         1049.89
_chemical_name_common            (Et4N)3[Fe4S4Cl4].Et4NCl
_chemical_name_systematic
'tetrakis(Tetraethylammonium) tetrakis((\m~3~-sulfido)-chloro-iron) chloride'
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      114
_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                   12.2784(3)
_cell_length_b                   12.2784(3)
_cell_length_c                   16.2649(9)
_cell_measurement_reflns_used    7190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.35
_cell_volume                     2452.08(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19608
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  0.8945
_exptl_absorpt_correction_T_min  0.6494
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Xprep
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       arrowhead
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         3571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                3112
_reflns_number_total             3571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801533q_si_001_5.cif
_cod_data_source_block           1c-musphcf
_cod_database_code               4306719