Synthesis and Characterization of a Redox-Active Bis(thiophenolato)amide Ligand, [SNS]3-, and the Homoleptic Tungsten Complexes, W[SNS]2 and W[ONO]2
David W. Shaffer; Géza Szigethy; Joseph W. Ziller; Alan F. Heyduk; Inorganic Chemistry 52 (2013) 2110–2118; doi:10.1021/ic302506e

data_4333905
_publ_section_title
;
 Synthesis and Characterization of a Redox-Active Bis(thiophenolato)amide
 Ligand, [SNS]3-, and the Homoleptic Tungsten Complexes, W[SNS]2 and
 W[ONO]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2110
_journal_page_last               2118
_journal_paper_doi               10.1021/ic302506e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C35 H32 N2 S4 W'
_chemical_formula_weight         792.72
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.2028(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7206(6)
_cell_length_b                   10.6756(3)
_cell_length_c                   15.2817(5)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.19
_cell_volume                     3073.32(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36891
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_T_max  0.6966
_exptl_absorpt_correction_T_min  0.4463
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0151
_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^)+(0.0140P)^2^+2.8303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0351
_reflns_number_gt                7345
_reflns_number_total             7748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302506e_si_001_1.cif
_cod_data_source_block           W[SNS]2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4333905