A Family of Oxo-Chalcogenide Molybdenum and Tungsten Complexes, (n-Bu4N)2[M2O2(μ-Q)2(1,3-dithiole-2-thione-4,5-dithiolate)2] (M = Mo, W; Q = S, Se): New Synthetic Entries, Structure, and Gas-Phase Behavior
Rosa Llusar; Sonia Triguero; Cristian Vicent; Maxim N. Sokolov; Benoît Domercq; Marc Fourmigué; Inorganic Chemistry 44 (2005) 8937–8946; doi:10.1021/ic0508728

data_4310058
_publ_contact_author             'Llusar Barelles Rosa'
_publ_contact_author_address
;
Departament de Ci\`encies Experimentals
Universitat Jaume I, Campus de Riu Sec, P. O. Box 224. Castell\'o, Spain
;
_publ_contact_author_email       llusar@exp.uji.es
_publ_contact_author_phone       '+34 964 728086'
_publ_section_title
;
A Family of Oxo-Chalcogenide Molybdenum and Tungsten Complexes,
(n-Bu4N)2[M2O2(\m-Q)2(1,3-dithiole-2-thione-4,5-dithiolate)2] (M = Mo, W; Q
= S, Se): New Synthetic Entries, Structure, and Gas-Phase Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8937
_journal_page_last               8946
_journal_paper_doi               10.1021/ic0508728
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '(C16 H36 N)2, C6 O2 S12 Mo2'
_chemical_formula_sum            'C38 H72 Mo2 N2 O2 S12'
_chemical_formula_weight         1165.58
_chemical_name_common            '(Bu4N)2, Mo2S2O2(dmit)2'
_chemical_name_systematic
; 
bis tetrabutylammonium, 
(bis(2,3-disulfanyl-4,5-dithiole-2-thione))(dimolybdenumdioxo
bis(mu sulfido))
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9420(12)
_cell_length_b                   15.9050(16)
_cell_length_c                   19.1558(17)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.4
_cell_volume                     5466.4(8)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       'rotation, phi incr. 1.3 deg.'
_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  0.1973
_diffrn_reflns_av_sigmaI/netI    0.1758
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37585
_diffrn_reflns_theta_full        28.08
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.9323
_exptl_absorpt_correction_T_min  0.7612
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.0385
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.768
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.768
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                2178
_reflns_number_total             6529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0508728si20050603_113343_3.cif
_cod_data_source_block           (n-Bu4N)2[Mo2O2S2(dmit)2]
_cod_database_code               4310058