Desoxo molybdenum(IV) and tungsten(IV) bis(dithiolene) complexes: monomer-dimer interconversion involving reversible thiol bridge formation.
Majumdar, Amit; Pal, Kuntal; Nagarajan, Kowliki; Sarkar, Sabyasachi; Inorganic chemistry 46 (2007) 6136–6147; doi:10.1021/ic7006777

data_4339079
_publ_section_title
;
 Desoxo molybdenum(IV) and tungsten(IV) bis(dithiolene) complexes:
 monomer-dimer interconversion involving reversible thiol bridge
 formation.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6136
_journal_page_last               6147
_journal_paper_doi               10.1021/ic7006777
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C30 H14 N8 S10 W2, 2(C8 H20 N)'
_chemical_formula_sum            'C46 H54 N10 S10 W2'
_chemical_formula_weight         1435.37
_chemical_name_systematic
'Tetraethylammonium tetrakis(1,2-dicyanoethylenedithiolato)bis(benzylthiolato)ditungstate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.109(5)
_cell_angle_beta                 98.540(5)
_cell_angle_gamma                97.958(5)
_cell_formula_units_Z            2
_cell_length_a                   11.332(5)
_cell_length_b                   15.089(5)
_cell_length_c                   18.625(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     3044.2(19)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45  (Bruker, 2003)'
_computing_molecular_graphics    'Diamond 2.1e, Ortep'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.9850
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20154
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.157
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method
'Acetonitrile, isopropanol, diethylether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.6367
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         14377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                12153
_reflns_number_total             14377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7006777-file005.cif
_cod_data_source_block           8aprbs_solsqz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4339079