#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:45:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179261 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/81/4318108.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_4318108
loop_
_publ_author_name
'Hong-Cai Zhou'
'Weiping Su'
'Catalina Achim'
'P. Venkateswara Rao'
'R. H. Holm'
_publ_contact_author_email
;
holm@chemistry.harvard.edu
;
_publ_section_title
;
 High-Nuclearity Sulfide-Rich Molybdenum-Iron-Sulfur Clusters:
 Reevaluation and Extension
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3191
_journal_page_last               3201
_journal_paper_doi               10.1021/ic0201250
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         (Et4N)3[(edt)2Mo2FeS6]
_chemical_formula_sum            'C28 H68 Fe Mo2 N3 S10'
_chemical_formula_weight         1015.18
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
  tris(Tetraethylammonium) bis(bis(mu2-sulfido)-
(ethanedithiolato-S,S')-sulfido-molybdenum)-iron
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.551(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7054(15)
_cell_length_b                   18.404(2)
_cell_length_c                   17.5020(19)
_cell_measurement_reflns_used    930
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.78
_cell_volume                     4325.2(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15597
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         5380
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0252
_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/[σ²(Fo²)+(0.0475P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                4690
_reflns_number_total             5380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201250_1.cif
_cod_data_source_block           (Et4N)3[2]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4325.1(8)
_cod_database_code               4318108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Mo1 Mo 0.813047(12) 0.093119(9) 0.174890(9) 0.02514(6) Uani 1 1 d . . .
Fe1 Fe 1.0000 0.05906(2) 0.2500 0.02571(9) Uani 1 2 d S . .
S1 S 0.67434(4) 0.12901(3) 0.23275(3) 0.03974(13) Uani 1 1 d . . .
S2 S 0.68266(4) 0.02093(3) 0.09501(3) 0.03692(12) Uani 1 1 d . . .
S3 S 0.84148(4) 0.17510(3) 0.09566(3) 0.03477(12) Uani 1 1 d . . .
S4 S 0.89325(4) 0.12808(3) 0.29861(3) 0.03081(11) Uani 1 1 d . . .
S5 S 0.90471(4) -0.01003(3) 0.16021(3) 0.02953(11) Uani 1 1 d . . .
C1 C 0.55966(19) 0.09880(16) 0.16830(17) 0.0542(7) Uani 1 1 d . . .
H1A H 0.5345 0.0554 0.1905 0.065 Uiso 1 1 calc R . .
H1B H 0.5091 0.1370 0.1647 0.065 Uiso 1 1 calc R . .
C2 C 0.57634(18) 0.08173(15) 0.08872(15) 0.0488(6) Uani 1 1 d . . .
H2A H 0.5887 0.1268 0.0623 0.059 Uiso 1 1 calc R . .
H2B H 0.5167 0.0587 0.0581 0.059 Uiso 1 1 calc R . .
N1 N 0.73892(13) 0.38620(9) 0.15565(10) 0.0291(3) Uani 1 1 d . . .
C101 C 0.8541(2) 0.32354(14) 0.26827(15) 0.0508(6) Uani 1 1 d . . .
H10A H 0.8848 0.3296 0.3228 0.076 Uiso 1 1 calc R . .
H10B H 0.9056 0.3186 0.2378 0.076 Uiso 1 1 calc R . .
H10C H 0.8128 0.2803 0.2621 0.076 Uiso 1 1 calc R . .
C102 C 0.79045(18) 0.38925(12) 0.24037(12) 0.0370(5) Uani 1 1 d . . .
H10D H 0.7398 0.3943 0.2724 0.044 Uiso 1 1 calc R . .
H10E H 0.8326 0.4327 0.2486 0.044 Uiso 1 1 calc R . .
C111 C 0.58613(18) 0.32095(13) 0.18412(16) 0.0483(6) Uani 1 1 d . . .
H11A H 0.5460 0.2776 0.1710 0.072 Uiso 1 1 calc R . .
H11B H 0.5451 0.3637 0.1699 0.072 Uiso 1 1 calc R . .
H11C H 0.6132 0.3216 0.2397 0.072 Uiso 1 1 calc R . .
C112 C 0.67013(16) 0.32081(11) 0.14028(13) 0.0357(5) Uani 1 1 d . . .
H11D H 0.6417 0.3186 0.0843 0.043 Uiso 1 1 calc R . .
H11E H 0.7098 0.2767 0.1541 0.043 Uiso 1 1 calc R . .
C121 C 0.89879(18) 0.43233(14) 0.11839(15) 0.0465(6) Uani 1 1 d . . .
H12A H 0.9430 0.4236 0.0824 0.070 Uiso 1 1 calc R . .
H12B H 0.9354 0.4266 0.1715 0.070 Uiso 1 1 calc R . .
H12C H 0.8725 0.4813 0.1112 0.070 Uiso 1 1 calc R . .
C122 C 0.81381(16) 0.37853(12) 0.10284(12) 0.0349(4) Uani 1 1 d . . .
H12D H 0.8415 0.3293 0.1086 0.042 Uiso 1 1 calc R . .
H12E H 0.7786 0.3841 0.0486 0.042 Uiso 1 1 calc R . .
C131 C 0.61735(18) 0.46378(14) 0.05866(13) 0.0443(5) Uani 1 1 d . . .
H13A H 0.5834 0.5103 0.0541 0.066 Uiso 1 1 calc R . .
H13B H 0.5686 0.4249 0.0495 0.066 Uiso 1 1 calc R . .
H13C H 0.6596 0.4610 0.0204 0.066 Uiso 1 1 calc R . .
C132 C 0.68017(16) 0.45627(11) 0.13916(12) 0.0333(4) Uani 1 1 d . . .
H13D H 0.6366 0.4607 0.1770 0.040 Uiso 1 1 calc R . .
H13E H 0.7271 0.4970 0.1481 0.040 Uiso 1 1 calc R . .
N2 N 0.2500 0.2500 0.0000 0.0294(5) Uani 1 2 d S . .
C11 C 0.0703(2) 0.2420(2) 0.01621(19) 0.0720(9) Uani 1 1 d . . .
H11F H 0.0458 0.2021 0.0434 0.108 Uiso 1 1 calc R A 1
H11G H 0.0694 0.2279 -0.0374 0.108 Uiso 1 1 calc R A 1
H11H H 0.0280 0.2841 0.0169 0.108 Uiso 1 1 calc R A 1
C21 C 0.2800(3) 0.12025(16) 0.0493(2) 0.0769(10) Uani 1 1 d . . .
H21A H 0.2351 0.0949 0.0765 0.115 Uiso 1 1 calc R B 2
H21B H 0.3459 0.0990 0.0632 0.115 Uiso 1 1 calc R B 2
H21C H 0.2558 0.1159 -0.0066 0.115 Uiso 1 1 calc R B 2
C12 C 0.1772(3) 0.2606(2) 0.0569(2) 0.034 Uani 0.50 1 d PD C 1
C22 C 0.2583(4) 0.3304(2) 0.0295(3) 0.042 Uani 0.50 1 d PD . 1
C12' C 0.2853(3) 0.2055(2) 0.0738(2) 0.035 Uani 0.50 1 d PD C 2
C22' C 0.3491(3) 0.2685(3) 0.0429(3) 0.047 Uani 0.50 1 d PD . 2
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
S3 Mo1 S4 107.25(2) . . ?
S3 Mo1 S5 109.43(2) . . ?
S4 Mo1 S5 99.492(19) . . ?
S3 Mo1 S1 109.86(2) . . ?
S4 Mo1 S1 78.36(2) . . ?
S5 Mo1 S1 139.36(2) . . ?
S3 Mo1 S2 102.77(2) . . ?
S4 Mo1 S2 147.82(2) . . ?
S5 Mo1 S2 80.86(2) . . ?
S1 Mo1 S2 80.86(2) . . ?
S3 Mo1 Fe1 101.569(18) . . ?
S4 Mo1 Fe1 52.009(14) . . ?
S5 Mo1 Fe1 51.941(15) . . ?
S1 Mo1 Fe1 127.343(16) . . ?
S2 Mo1 Fe1 131.874(17) . . ?
S5 Fe1 S5 110.45(3) . 2_755 ?
S5 Fe1 S4 113.097(19) . 2_755 ?
S5 Fe1 S4 104.91(2) 2_755 2_755 ?
S5 Fe1 S4 104.91(2) . . ?
S5 Fe1 S4 113.097(19) 2_755 . ?
S4 Fe1 S4 110.58(3) 2_755 . ?
S5 Fe1 Mo1 146.903(16) . 2_755 ?
S5 Fe1 Mo1 54.983(14) 2_755 2_755 ?
S4 Fe1 Mo1 54.859(15) 2_755 2_755 ?
S4 Fe1 Mo1 108.185(18) . 2_755 ?
S5 Fe1 Mo1 54.983(14) . . ?
S5 Fe1 Mo1 146.903(16) 2_755 . ?
S4 Fe1 Mo1 108.185(18) 2_755 . ?
S4 Fe1 Mo1 54.860(15) . . ?
Mo1 Fe1 Mo1 153.244(17) 2_755 . ?
C1 S1 Mo1 108.03(9) . . ?
C2 S2 Mo1 100.71(9) . . ?
Fe1 S4 Mo1 73.131(16) . . y
Fe1 S5 Mo1 73.076(17) . . y
C2 C1 S1 111.54(18) . . ?
C1 C2 S2 110.09(19) . . ?
C102 N1 C132 106.33(15) . . ?
C102 N1 C122 111.15(16) . . ?
C132 N1 C122 111.14(16) . . ?
C102 N1 C112 110.79(16) . . ?
C132 N1 C112 110.65(16) . . ?
C122 N1 C112 106.83(15) . . ?
N1 C102 C101 114.39(19) . . ?
C111 C112 N1 114.78(18) . . ?
C121 C122 N1 114.82(18) . . ?
C131 C132 N1 116.05(17) . . ?
C22' N2 C22' 180.0(5) 7 . ?
C22' N2 C12' 65.3(2) 7 7 ?
C22' N2 C12' 114.7(2) . 7 ?
C22' N2 C12' 114.7(2) 7 . ?
C22' N2 C12' 65.3(2) . . ?
C12' N2 C12' 180.0(3) 7 . ?
C22' N2 C12 73.0(2) 7 . ?
C22' N2 C12 107.0(2) . . ?
C12' N2 C12 109.9(2) 7 . ?
C12' N2 C12 70.1(2) . . ?
C22' N2 C12 107.0(2) 7 7 ?
C22' N2 C12 73.0(2) . 7 ?
C12' N2 C12 70.1(2) 7 7 ?
C12' N2 C12 109.9(2) . 7 ?
C12 N2 C12 180.00(19) . 7 ?
C22' N2 C22 67.0(3) 7 7 ?
C22' N2 C22 113.0(3) . 7 ?
C12' N2 C22 103.8(2) 7 7 ?
C12' N2 C22 76.2(2) . 7 ?
C12 N2 C22 108.4(2) . 7 ?
C12 N2 C22 71.6(2) 7 7 ?
C22' N2 C22 113.0(3) 7 . ?
C22' N2 C22 67.0(3) . . ?
C12' N2 C22 76.2(2) 7 . ?
C12' N2 C22 103.8(2) . . ?
C12 N2 C22 71.6(2) . . ?
C12 N2 C22 108.4(2) 7 . ?
C22 N2 C22 180.0(3) 7 . ?
C12 C11 C22' 67.9(2) . 7 ?
C12' C21 C22 71.2(2) . 7 ?
C11 C12 N2 110.5(3) . . ?
C11 C12 C22 127.6(3) . . ?
N2 C12 C22 54.40(19) . . ?
N2 C22 C21 104.8(3) . 7 ?
N2 C22 C12 53.99(19) . . ?
C21 C22 C12 120.0(4) 7 . ?
N2 C12' C22' 55.3(2) . . ?
N2 C12' C21 107.8(3) . . ?
C22' C12' C21 127.3(3) . . ?
N2 C22' C12' 59.4(2) . . ?
N2 C22' C11 108.6(3) . 7 ?
C12' C22' C11 126.6(4) . 7 ?
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
Mo1 S3 2.1372(5) . y
Mo1 S4 2.3146(6) . y
Mo1 S5 2.3188(5) . y
Mo1 S1 2.4180(6) . y
Mo1 S2 2.4316(6) . y
Mo1 Fe1 2.7087(3) . y
Fe1 S5 2.2293(6) . y
Fe1 S5 2.2293(6) 2_755 y
Fe1 S4 2.2308(5) 2_755 y
Fe1 S4 2.2308(5) . y
Fe1 Mo1 2.7087(3) 2_755 y
S1 C1 1.828(3) . ?
S2 C2 1.823(3) . ?
C1 C2 1.489(4) . ?
N1 C102 1.510(3) . ?
N1 C132 1.517(2) . ?
N1 C122 1.519(3) . ?
N1 C112 1.519(3) . ?
C101 C102 1.514(3) . ?
C111 C112 1.506(3) . ?
C121 C122 1.511(3) . ?
C131 C132 1.503(3) . ?
N2 C22' 1.455(4) 7 ?
N2 C22' 1.455(4) . ?
N2 C12' 1.524(4) 7 ?
N2 C12' 1.524(4) . ?
N2 C12 1.556(4) . ?
N2 C12 1.556(4) 7 ?
N2 C22 1.564(4) 7 ?
N2 C22 1.564(4) . ?
C11 C12 1.535(5) . ?
C11 C22' 1.670(5) 7 ?
C21 C12' 1.625(5) . ?
C21 C22 1.646(5) 7 ?
C12 C22 1.825(6) . ?
C22 C21 1.646(5) 7 ?
C12' C22' 1.609(6) . ?
C22' C11 1.670(5) 7 ?
