#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:20:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179105 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/67/4306721.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306721
loop_
_publ_author_name
'Karl S. Hagen'
'Mohammad Uddin'
_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), H4 Fe4 S8, Cl'
_chemical_formula_sum            'C32 H84 Cl Fe4 N4 S8'
_chemical_formula_weight         1040.36
_chemical_name_common            (Et4N)3[Fe4S4(SH)4].Et4NCl
_chemical_name_systematic
;tetrakis(Tetraethylammonium) tetrakis((μ₃-sulfido)
-hydrosulfido-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                   12.4153(4)
_cell_length_b                   12.4153(4)
_cell_length_c                   16.1984(11)
_cell_measurement_reflns_used    7809
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.32
_cell_volume                     2496.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL, and CrystalMaker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1561
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12181
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8 SMART Apex CCD'
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  0.8004
_exptl_absorpt_correction_T_min  0.7674
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   xprep
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      1.37
_exptl_crystal_density_method    'neutral buoyancy'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0544
_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/[σ²(Fo²)+(0.0525P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                2312
_reflns_number_total             2454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801533q_si_001_7.cif
_cod_data_source_block           2-mu10rf
_cod_database_code               4306721
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.39469(4) 0.46465(4) 0.06033(4) 0.01722(16) Uani 1 1 d . . .
S1 S 0.45302(7) 0.63995(7) 0.07892(7) 0.0194(2) Uani 1 1 d . . .
S2 S 0.25066(8) 0.42027(8) 0.14572(8) 0.0287(3) Uani 1 1 d . . .
H1 H 0.2608 0.3748 0.1117 0.034 Uiso 1 1 d R . .
Cl2 Cl 0.0000 1.0000 0.0000 0.0233(4) Uani 1 4 d S . .
N1 N 0.0832(2) 0.7415(2) 0.1505(2) 0.0173(7) Uani 1 1 d . . .
C1 C 0.0315(3) 0.8424(3) 0.1878(3) 0.0195(8) Uani 1 1 d . . .
H1A H 0.0594 0.8519 0.2433 0.023 Uiso 1 1 calc R . .
H1B H 0.0539 0.9044 0.1556 0.023 Uiso 1 1 calc R . .
C2 C -0.0903(3) 0.8415(3) 0.1919(3) 0.0251(10) Uani 1 1 d . . .
H2A H -0.1152 0.9078 0.2156 0.038 Uiso 1 1 calc R . .
H2B H -0.1137 0.7822 0.2255 0.038 Uiso 1 1 calc R . .
H2C H -0.1192 0.8338 0.1373 0.038 Uiso 1 1 calc R . .
C3 C 0.0555(3) 0.6412(3) 0.1992(3) 0.0210(8) Uani 1 1 d . . .
H3A H -0.0217 0.6301 0.1963 0.025 Uiso 1 1 calc R . .
H3B H 0.0897 0.5799 0.1727 0.025 Uiso 1 1 calc R . .
C4 C 0.0886(3) 0.6427(3) 0.2890(3) 0.0241(9) Uani 1 1 d . . .
H4A H 0.0687 0.5758 0.3146 0.036 Uiso 1 1 calc R . .
H4B H 0.0530 0.7011 0.3167 0.036 Uiso 1 1 calc R . .
H4C H 0.1652 0.6522 0.2929 0.036 Uiso 1 1 calc R . .
C5 C 0.2044(3) 0.7578(3) 0.1518(3) 0.0240(9) Uani 1 1 d . . .
H5A H 0.2267 0.7706 0.2083 0.029 Uiso 1 1 calc R . .
H5B H 0.2386 0.6918 0.1335 0.029 Uiso 1 1 calc R . .
C6 C 0.2453(3) 0.8497(4) 0.0988(4) 0.0352(12) Uani 1 1 d . . .
H6A H 0.3220 0.8556 0.1046 0.053 Uiso 1 1 calc R . .
H6B H 0.2120 0.9158 0.1161 0.053 Uiso 1 1 calc R . .
H6C H 0.2277 0.8361 0.0420 0.053 Uiso 1 1 calc R . .
C7 C 0.0413(3) 0.7255(3) 0.0632(3) 0.0263(9) Uani 1 1 d . . .
H7A H -0.0331 0.7020 0.0664 0.032 Uiso 1 1 calc R . .
H7B H 0.0421 0.7945 0.0352 0.032 Uiso 1 1 calc R . .
C8 C 0.1029(4) 0.6457(4) 0.0116(3) 0.0376(11) Uani 1 1 d . . .
H8A H 0.0704 0.6404 -0.0420 0.056 Uiso 1 1 calc R . .
H8B H 0.1015 0.5764 0.0379 0.056 Uiso 1 1 calc R . .
H8C H 0.1762 0.6693 0.0060 0.056 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 -1.00 0.00 0.0780
1.00 1.00 0.00 0.0530
1.00 -1.00 0.00 0.1050
-1.00 1.00 0.00 0.1050
1.00 0.00 0.00 0.0710
0.00 -2.00 -1.00 0.0840
0.00 0.00 -1.00 0.0710
2.00 4.00 -3.00 0.0710
1.00 2.00 1.00 0.0710
1.00 2.00 3.00 0.0850
-2.00 -4.00 5.00 0.0980
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Fe1 S1 104.19(4) 4_655 2_665 y
S1 Fe1 S1 104.19(4) 4_655 . y
S1 Fe1 S1 104.79(3) 2_665 . y
S1 Fe1 S2 115.10(4) 4_655 . y
S1 Fe1 S2 114.69(4) 2_665 . y
S1 Fe1 S2 112.70(4) . . y
S1 Fe1 Fe1 101.37(3) 4_655 2_665 ?
S1 Fe1 Fe1 53.40(3) 2_665 2_665 ?
S1 Fe1 Fe1 53.41(3) . 2_665 ?
S2 Fe1 Fe1 143.50(3) . 2_665 ?
S1 Fe1 Fe1 53.46(3) 4_655 3_565 ?
S1 Fe1 Fe1 100.96(3) 2_665 3_565 ?
S1 Fe1 Fe1 53.03(3) . 3_565 ?
S2 Fe1 Fe1 144.32(4) . 3_565 ?
Fe1 Fe1 Fe1 60.033(13) 2_665 3_565 ?
S1 Fe1 Fe1 53.46(3) 4_655 4_655 ?
S1 Fe1 Fe1 53.03(3) 2_665 4_655 ?
S1 Fe1 Fe1 100.96(3) . 4_655 ?
S2 Fe1 Fe1 146.34(4) . 4_655 ?
Fe1 Fe1 Fe1 60.032(13) 2_665 4_655 ?
Fe1 Fe1 Fe1 59.93(3) 3_565 4_655 ?
Fe1 S1 Fe1 73.51(4) 3_565 2_665 y
Fe1 S1 Fe1 73.51(4) 3_565 . y
Fe1 S1 Fe1 73.19(3) 2_665 . y
Fe1 S1 H5B 113.6 3_565 . ?
Fe1 S1 H5B 157.1 2_665 . ?
Fe1 S1 H5B 87.8 . . ?
Fe1 S2 H3A 124.6 . . ?
Fe1 S2 H1 68.6 . . ?
H3A S2 H1 132.6 . . ?
H7B Cl2 H1B 50.9 . . ?
C3 N1 C5 109.1(3) . . ?
C3 N1 C7 107.4(3) . . ?
C5 N1 C7 111.7(3) . . ?
C3 N1 C1 111.9(3) . . ?
C5 N1 C1 107.5(3) . . ?
C7 N1 C1 109.4(3) . . ?
C2 C1 N1 115.4(3) . . ?
C2 C1 H1A 108.4 . . ?
N1 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
N1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 115.4(3) . . ?
C4 C3 H3A 108.4 . . ?
N1 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
N1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 115.1(3) . . ?
C6 C5 H5A 108.5 . . ?
N1 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
N1 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 N1 115.4(3) . . ?
C8 C7 H7A 108.4 . . ?
N1 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
N1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 S1 2.3007(13) 4_655 y
Fe1 S1 2.3135(10) 2_665 y
Fe1 S1 2.3134(10) . y
Fe1 S2 2.3269(12) . y
Fe1 Fe1 2.7584(9) 2_665 y
Fe1 Fe1 2.7611(11) 3_565 y
Fe1 Fe1 2.7612(11) 4_655 y
S1 Fe1 2.3007(13) 3_565 y
S1 Fe1 2.3135(10) 2_665 y
S1 H5B 2.8774 . ?
S2 H3A 4.3467 . ?
S2 H1 0.7989 . ?
Cl2 H7B 2.6661 . ?
Cl2 H1B 2.8657 . ?
N1 C3 1.515(5) . ?
N1 C5 1.519(5) . ?
N1 C7 1.519(5) . ?
N1 C1 1.531(5) . ?
C1 C2 1.514(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.513(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.516(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.505(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C5 H5B S1 0.97 2.88 3.614(4) 133.5 . y
C6 H6A S1 0.96 3.16 3.679(4) 115.7 . y
C3 H3B S2 0.97 2.85 3.760(4) 156.9 . y
C1 H1B Cl2 0.97 2.87 3.638(4) 137.3 . y
C7 H7B Cl2 0.97 2.67 3.596(4) 160.7 . y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 Fe1 S1 Fe1 -16.45(4) 4_655 . . 3_565 ?
S1 Fe1 S1 Fe1 92.71(5) 2_665 . . 3_565 ?
S2 Fe1 S1 Fe1 -141.92(4) . . . 3_565 ?
Fe1 Fe1 S1 Fe1 77.30(3) 2_665 . . 3_565 ?
Fe1 Fe1 S1 Fe1 38.33(3) 4_655 . . 3_565 ?
S1 Fe1 S1 Fe1 -93.75(4) 4_655 . . 2_665 ?
S1 Fe1 S1 Fe1 15.41(6) 2_665 . . 2_665 ?
S2 Fe1 S1 Fe1 140.78(4) . . . 2_665 ?
Fe1 Fe1 S1 Fe1 -77.30(3) 3_565 . . 2_665 ?
Fe1 Fe1 S1 Fe1 -38.97(4) 4_655 . . 2_665 ?
S1 Fe1 S1 H5B 99.0 4_655 . . . ?
S1 Fe1 S1 H5B -151.8 2_665 . . . ?
S2 Fe1 S1 H5B -26.4 . . . . ?
Fe1 Fe1 S1 H5B -167.2 2_665 . . . ?
Fe1 Fe1 S1 H5B 115.5 3_565 . . . ?
Fe1 Fe1 S1 H5B 153.8 4_655 . . . ?
S1 Fe1 S2 H3A -77.3 4_655 . . . ?
S1 Fe1 S2 H3A 161.8 2_665 . . . ?
S1 Fe1 S2 H3A 42.0 . . . . ?
Fe1 Fe1 S2 H3A 100.6 2_665 . . . ?
Fe1 Fe1 S2 H3A -15.6 3_565 . . . ?
Fe1 Fe1 S2 H3A -138.4 4_655 . . . ?
C3 N1 C1 C2 -60.3(5) . . . . ?
C5 N1 C1 C2 180.0(4) . . . . ?
C7 N1 C1 C2 58.5(5) . . . . ?
C5 N1 C3 C4 60.2(4) . . . . ?
C7 N1 C3 C4 -178.6(3) . . . . ?
C1 N1 C3 C4 -58.6(4) . . . . ?
C3 N1 C5 C6 174.6(4) . . . . ?
C7 N1 C5 C6 56.0(5) . . . . ?
C1 N1 C5 C6 -64.0(5) . . . . ?
C3 N1 C7 C8 -72.1(4) . . . . ?
C5 N1 C7 C8 47.5(4) . . . . ?
C1 N1 C7 C8 166.4(3) . . . . ?
