Synthesis and Structure of Technetium Trichloride
Frederic Poineau; Erik V. Johnstone; Philippe F. Weck; Eunja Kim; Paul M. Forster; Brian L. Scott; Alfred P. Sattelberger; Kenneth R. Czerwinski; Journal of the American Chemical Society 132 (2010) 15864–15865; doi:10.1021/ja105730e

data_4103493
_publ_section_title
;
 Synthesis and Structure of Technetium Trichloride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15864
_journal_page_last               15865
_journal_paper_doi               10.1021/ja105730e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C4 H6 Cl4 O4 Tc2'
_chemical_formula_weight         455.89
_chemical_name_systematic
; 
 ? 
;
_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                112.082(2)
_cell_angle_beta                 96.667(3)
_cell_angle_gamma                108.792(3)
_cell_formula_units_Z            1
_cell_length_a                   6.0303(12)
_cell_length_b                   6.5098(13)
_cell_length_c                   8.3072(16)
_cell_measurement_temperature    100(2)
_cell_volume                     275.42(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4383
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    3.461
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4756
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0438P)^2^+0.3017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                1553
_reflns_number_total             1666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105730e_si_001.cif
_cod_data_source_block           Tc2Cl4(OAc)2
_cod_database_code               4103493