Technetium tetrachloride as a precursor for small technetium(IV) complexes.
Hagenbach, Adelheid; Yegen, Eda; Abram, Ulrich; Inorganic chemistry 45 (2006) 7331–7338; doi:10.1021/ic060896u

data_4350442
_publ_section_title
;
 Technetium tetrachloride as a precursor for small technetium(IV)
 complexes.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7331
_journal_page_last               7338
_journal_paper_doi               10.1021/ic060896u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         TcCl4(thioxane)2*thioxane
_chemical_formula_sum            'C12 H24 Cl4 O3 S3 Tc'
_chemical_formula_weight         552.29
_chemical_name_common            TcCl4(thioxane)2*thioxane
_chemical_name_systematic
;
tetrachlorobis(thioxane)technetium(IV) thioxane solvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                93.95(2)
_cell_angle_beta                 93.87(2)
_cell_angle_gamma                104.46(2)
_cell_formula_units_Z            1
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_cell_length_b                   6.469(1)
_cell_length_c                   12.831(3)
_cell_measurement_reflns_used    5041
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      3.19
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_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
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_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5348
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             279
_exptl_crystal_size_max          .53
_exptl_crystal_size_mid          .04
_exptl_crystal_size_min          .01
_refine_diff_density_max         0.650
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_refine_ls_extinction_coef       0.026(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_ref   0.796
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                1661
_reflns_number_total             2737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060896usi20060523_100113.cif
_cod_data_source_block           tcthiox
_cod_original_cell_volume        516.8(2)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4350442