Synthesis and Characterization of the "Sulfur-Rich" Bis(perthiobenzoato)(dithiobenzoato)technetium(III) Heterocomplex
Franck Mévellec; Francesco Tisato; Fiorenzo Refosco; Alain Roucoux; Nicolas Noiret; Henri Patin; Giuliano Bandoli; Inorganic Chemistry 41 (2002) 598–601; doi:10.1021/ic0107577

data_4317498
_publ_section_title
;
 Synthesis and Characterization of the "Sulfur-Rich"
 Bis(perthiobenzoato)(dithiobenzoato)technetium(III) Heterocomplex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              598
_journal_page_last               601
_journal_paper_doi               10.1021/ic0107577
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C21 H15 S8 Tc'
_chemical_formula_weight         621.81
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.75(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.951(5)
_cell_length_b                   10.633(3)
_cell_length_c                   11.990(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      7.7
_cell_volume                     2448.0(13)
_computing_cell_refinement       'P3/P4-PC vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4-PC vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4-PC vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker Nicolet R3m/V diffractometer'
_diffrn_measurement_method       omega-2theta
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3375
_diffrn_reflns_theta_full        23.56
_diffrn_reflns_theta_max         23.56
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        'up to 10%'
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.729
_refine_diff_density_min         -2.853
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.000(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.185
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2090
_reflns_number_gt                3096
_reflns_number_total             3375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0107577.cif
_cod_data_source_block           tcss
_cod_original_cell_volume        2448(1)
_cod_database_code               4317498