Trithiacyclononane as a Ligand for Potential Technetium and Rhenium Radiopharmaceuticals: Synthesis of [M(9S3)(SC2H4SC2H4S)][BF4] (M =99Tc, Re, 188Re) via C-S Bond Cleavage
Gregory E. D. Mullen; Philip J. Blower; Daniel J. Price; Anne K. Powell; Mark J. Howard; Michael J. Went; Inorganic Chemistry 39 (2000) 4093–4098; doi:10.1021/ic991240m

data_4321341
_publ_section_title
;
 Trithiacyclononane as a Ligand for Potential Technetium and Rhenium
 Radiopharmaceuticals: Synthesis of [M(9S3)(SC2H4SC2H4S)][BF4] (M =99Tc,
 Re, 188Re) via C-S Bond Cleavage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4093
_journal_page_last               4098
_journal_paper_doi               10.1021/ic991240m
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        gm
_chemical_formula_moiety         'Tc S6 C10 H20 B F4'
_chemical_formula_structural     'Tc [(SCH2CH2)3] [S(CH2CH2S)2] BF4'
_chemical_formula_sum            'C10 H20 B F4 S6 Tc'
_chemical_formula_weight         517.43
_chemical_melting_point          ?
_chemical_name_systematic
; Technetium(3+)[1,4,7-trithiacyclononane][2,2'-thiodiethanethiolate(2-)]
tetraflouroborate(-)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL + manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.233(2)
_cell_length_b                   14.341(2)
_cell_length_c                   20.726(3)
_cell_measurement_reflns_used    595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.62
_cell_volume                     3636.0(9)
_computing_cell_refinement
' Denzo and Scalepack from The HKL Programme Suite'
_computing_data_collection       'MSC Raxis II control software'
_computing_data_reduction        'SHELX97 and SHELXPRO'
_computing_molecular_graphics    SHELXTL+XP
_computing_publication_material  SHELXTL+XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku Raxis IIc''
_diffrn_measurement_method       'image plate oscilation photographs'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29143
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_type   none
_exptl_crystal_colour
;
Red in transmission - metallic-green in reflection
;
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0055(4)
_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_all   0.988
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_obs          0.0358
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0935
_refine_ls_wR_factor_obs         0.0876
_reflns_number_observed          4230
_reflns_number_total             5223
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991240m.cif
_cod_data_source_block           gm01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Orthorhombic' changed to 'orthorhombic' according to the built-in
table from CIF Core dictionary named 'cif_core.dic' version 2.4.1
from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321341