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_4318114
_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)2Mo2Fe5S11]
_chemical_formula_sum            'C34 H82 Fe5 Mo2 N5 O2 S15'
_chemical_formula_weight         1545.08
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
tris(Tetraethylammonium) 
bis(ethanedithiolato-S,S')-tetrakis(mu3-sulfido)-heptak
tetra-iron-di-molybdenum
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.815(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0129(10)
_cell_length_b                   32.172(3)
_cell_length_c                   19.0368(18)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      2.23
_cell_volume                     6125.0(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44614
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.092
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3164
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.714
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         15223
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                10402
_reflns_number_total             15223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0201250_7.cif
_cod_data_source_block           (Et4N)3[6].2DMF
_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        6125.1(10)
_cod_database_code               4318114