Technetium Tetrachloride Revisited: A Precursor to Lower-Valent Binary Technetium Chlorides
Erik V. Johnstone; Frederic Poineau; Paul M. Forster; Longzou Ma; Thomas Hartmann; Andrew Cornelius; Daniel Antonio; Alfred P. Sattelberger; Kenneth R. Czerwinski; Inorganic Chemistry 51 (2012) 8462–8467; doi:10.1021/ic301011c

data_4329921
_publ_section_title
;
 Technetium Tetrachloride Revisited: A Precursor to Lower-Valent Binary
 Technetium Chlorides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8462
_journal_page_last               8467
_journal_paper_doi               10.1021/ic301011c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'Cl4 Tc'
_chemical_formula_weight         239.80
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.0111(4)
_cell_length_b                   11.5308(9)
_cell_length_c                   13.9334(10)
_cell_measurement_temperature    100(2)
_cell_volume                     965.76(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15226
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6251
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.299
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.569
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0228P)^2^+2.7520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                1476
_reflns_number_total             1608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301011c_si_002.cif
_cod_data_source_block           TcCl4
_cod_database_code               4329921