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_4333906
_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            'C56 H80 N2 O4 W'
_chemical_formula_weight         1029.07
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                82.7281(6)
_cell_angle_beta                 73.9437(6)
_cell_angle_gamma                76.1399(6)
_cell_formula_units_Z            2
_cell_length_a                   11.6164(7)
_cell_length_b                   12.0666(7)
_cell_length_c                   20.5721(12)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.26
_cell_volume                     2684.8(3)
_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      143(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.903
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31079
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.7053
_exptl_absorpt_correction_T_min  0.6099
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         12287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0203
_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^)+(0.0277P)^2^+1.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0511
_reflns_number_gt                11491
_reflns_number_total             12287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302506e_si_001_2.cif
_cod_data_source_block           W[ONO]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               4333906