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_4103825
_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            'Br3 Tc'
_chemical_formula_weight         337.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_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            4
_cell_length_a                   11.0618(18)
_cell_length_b                   5.9755(10)
_cell_length_c                   6.3873(11)
_cell_measurement_temperature    149(2)
_cell_volume                     422.20(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.732
_diffrn_measured_fraction_theta_max 0.732
_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  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2771
_diffrn_reflns_theta_full        33.29
_diffrn_reflns_theta_max         33.29
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    31.568
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.2106
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    5.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .08
_refine_diff_density_max         2.131
_refine_diff_density_min         -3.137
_refine_diff_density_rms         0.579
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1097P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1887
_reflns_number_gt                415
_reflns_number_total             670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808597r_si_002.cif
_cod_data_source_block           tcbr3temp
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               4103825