High-Nuclearity Sulfide-Rich Molybdenum-Iron-Sulfur Clusters: Reevaluation and Extension
Hong-Cai Zhou; Weiping Su; Catalina Achim; P. Venkateswara Rao; R. H. Holm; Inorganic Chemistry 41 (2002) 3191–3201; doi:10.1021/ic0201250

data_4318110
_publ_contact_author_email
;
holm@chemistry.harvard.edu
;
_publ_section_title
;
 High-Nuclearity Sulfide-Rich Molybdenum-Iron-Sulfur Clusters:
 Reevaluation and Extension
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_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         (NEt4)4(Mo2Fe4S9(edt)2)
_chemical_formula_sum            'C36 H88 Fe4 Mo2 N4 S13'
_chemical_formula_weight         1409.16
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
  Tetrakis(tetraethylammonium) bis(ethanedithiolato)-(mu-4-sulfido)
-bis(mu-3-dulfido)-hexakis(mu-2-sulfido)-tetra-iron-di-molybdenum
;
_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                 127.9680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8927(9)
_cell_length_b                   34.1370(18)
_cell_length_c                   12.5379(6)
_cell_measurement_reflns_used    4495
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.3
_cell_volume                     6037.4(5)
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12874
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0784P)^2^+52.9604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1567
_reflns_number_gt                3049
_reflns_number_total             3956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201250_3.cif
_cod_data_source_block           (Et4N)3[4]_monoclinic
_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_database_code               4318110