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_4310060
_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_sum            'C54 H40 O2 P2 S10 Se2 W2'
_chemical_formula_weight         1629.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.340(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.942(2)
_cell_length_b                   22.855(5)
_cell_length_c                   20.851(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5656.2(19)
_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 0.998
_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  0.1670
_diffrn_reflns_av_sigmaI/netI    0.1805
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25287
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    5.818
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.061
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         7371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0852P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                3427
_reflns_number_total             7371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0508728si20050603_113343_5.cif
_cod_data_source_block           (PPh4)2[W2O2Se2(dmit)2]
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5655.9(19)
_cod_database_code               4310060
_ratio_of_minimum_to_maximum_apparent_transmission 0.858803