Sulfur-Based Redox Reactions in Mo3S74+ and Mo3S44+ Clusters Bearing Halide and 1,2-Dithiolene Ligands: a Mass Spectrometric and Density Functional Theory Study
Rosa Llusar; Victor Polo; Ederley Velez; Cristian Vicent; Inorganic Chemistry 49 (2010) 8045–8055; doi:10.1021/ic1010693

data_4316428
_publ_contact_author             'Cristian Vicent'
_publ_contact_author_address
;
 Serveis Centrals d'Instrumentaci\'o Cientifica, Universitat Jaume I,  
 Av. Sos Baynat s/n,  12071 Castell\'o de la Plana, Spain.
;
_publ_contact_author_email       barrera@sg.uji.es
_publ_contact_author_phone       '+34 964 387344'
_publ_section_title
;
 Sulfur-Based Redox Reactions in Mo3S74+ and Mo3S44+ Clusters Bearing
 Halide and 1,2-Dithiolene Ligands: a Mass Spectrometric and Density
 Functional Theory Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8045
_journal_page_last               8055
_journal_paper_doi               10.1021/ic1010693
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C66 H52 Mo3 P2 S10'
_chemical_formula_weight         1515.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 106.805(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.020(2)
_cell_length_b                   23.573(4)
_cell_length_c                   21.833(3)
_cell_measurement_reflns_used    2634
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.39
_cell_measurement_theta_min      2.30
_cell_volume                     6414.8(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1326
_diffrn_reflns_av_sigmaI/netI    0.1933
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18024
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.494407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         8402
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1866
_reflns_number_gt                4895
_reflns_number_total             8402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1010693_si_002.cif
_cod_data_source_block           (PPh4)2[Mo3S4(bdt)3]
_cod_depositor_comments
;
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 
;
_cod_original_cell_volume        6414.7(17)
_cod_database_code               4316428