Syntheses and reactivity of 'sulfur rich' Re(iii) and Tc(iii) complexes containing trithioperoxybenzoate, dithiobenzoate and dithiocarbamate ligands.
Lepareur, Nicolas; Mévellec, Franck; Noiret, Nicolas; Refosco, Fiorenzo; Tisato, Francesco; Porchia, Marina; Bandoli, Giuliano; Dalton transactions (Cambridge, England : 2003)  (2005) 2866–2875; doi:10.1039/b503938j

data_7008535
_publ_section_title
;
 Syntheses and reactivity of 'sulfur rich' Re(iii) and Tc(iii)
 complexes containing trithioperoxybenzoate, dithiobenzoate and
 dithiocarbamate ligands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2866
_journal_page_last               2875
_journal_paper_doi               10.1039/b503938j
_journal_year                    2005
_chemical_formula_sum            'C21 H26 N O S8 Tc'
_chemical_formula_weight         662.91
_chemical_name_systematic
;
?
;
_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     'heavy-atom methods'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.94(3)
_cell_angle_beta                 90.39(3)
_cell_angle_gamma                108.16(3)
_cell_formula_units_Z            2
_cell_length_a                   9.913(2)
_cell_length_b                   10.414(2)
_cell_length_c                   14.912(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.1
_cell_measurement_theta_min      7.7
_cell_volume                     1364.0(6)
_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 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Nicolet R3m/V four-circle 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  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5044
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+3.6532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                4918
_reflns_number_total             5035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503938j.txt
_cod_data_source_block           Tc10.EtOH
_cod_original_cell_volume        1364.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008535