Preparation of the Binary Technetium Bromides: TcBr3 and TcBr4
Frederic Poineau; Efrain E. Rodriguez; Paul M. Forster; Alfred P. Sattelberger; Anthony K. Cheetham; Kenneth R. Czerwinski; Journal of the American Chemical Society 131 (2009) 910–911; doi:10.1021/ja808597r

data_4103826
_publ_section_title
;
 Preparation of the Binary Technetium Bromides: TcBr3 and TcBr4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              910
_journal_page_last               911
_journal_paper_doi               10.1021/ja808597r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'Br4 Tc'
_chemical_formula_weight         417.64
_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                   6.3237(5)
_cell_length_b                   12.1777(9)
_cell_length_c                   14.7397(11)
_cell_measurement_temperature    157(2)
_cell_volume                     1135.08(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      157(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18681
_diffrn_reflns_theta_full        32.02
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         4.25
_exptl_absorpt_coefficient_mu    30.532
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.3548
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    4.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                1643
_reflns_number_total             1969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808597r_si_003.cif
_cod_data_source_block           tcbr4c_0m
_cod_database_code               4103826