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_4339081
_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
'3(C30 H14 Mo2 N8 S10), 6(C8 H20 N), 2(C2 H3 N)'
_chemical_formula_sum            'C142 H168 Mo6 N32 S30'
_chemical_formula_weight         3860.83
_chemical_name_systematic
'Tetraethylammonium tetrakis(1,2-dicyanoethylenedithiolato)bis(benzyalthiolato)dimolybdate'
_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
_cell_angle_beta                 94.498(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.596(5)
_cell_length_b                   18.049(5)
_cell_length_c                   46.838(5)
_cell_measurement_temperature    100(2)
_cell_volume                     17358(7)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            115200
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectrangular block'
_exptl_crystal_F_000             7904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.8282
_refine_diff_density_min         -0.7344
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2001
_refine_ls_number_reflns         42875
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+24.5322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                31568
_reflns_number_total             42875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7006777-file010.cif
_cod_data_source_block           '[(Et4N)2][Mo2(mnt)4(Sbz)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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.

'_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_original_sg_symbol_H-M      P21/c
_cod_database_code               4339081