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_4318113
_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         (NBu4)3(Mo2Fe4S9(edt)2)(DMF)
_chemical_formula_sum            'C55 H123 Fe4 Mo2 N4 O S13'
_chemical_formula_weight         1688.63
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
Tris(tetrabutylammonium) bis(ethanedithiolato)-(mu-4-sulfido)
-bis(mu-3-dulfido)-hexakis(mu-2-sulfido)-tetra-iron-di-molybdenum
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 93.105(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.725(2)
_cell_length_b                   11.7601(17)
_cell_length_c                   40.348(6)
_cell_measurement_reflns_used    969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.92
_cell_volume                     7924.3(19)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            30413
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3540
_exptl_crystal_size_max          0.027
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.217
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         10322
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+32.7868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                7717
_reflns_number_total             10322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201250_6.cif
_cod_data_source_block           (Bu4N)3[5].DMF
_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        7924(2)
_cod_database_code               4318113