Technetium fluoride trioxide, TcO3F, preparation and properties.
Supeł, Joanna; Abram, Ulrich; Hagenbach, Adelheid; Seppelt, Konrad; Inorganic chemistry 46 (2007) 5591–5595; doi:10.1021/ic070333y

data_4339752
_publ_section_title
;
 Technetium fluoride trioxide, TcO3F, preparation and properties.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5591
_journal_page_last               5595
_journal_paper_doi               10.1021/ic070333y
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         TcO3F*TcO2F3
_chemical_formula_sum            'F4 O5 Tc2'
_chemical_formula_weight         353.801
_chemical_name_common
technetium-fluoride-trioxide*technetium-trifluoride-dioxide
_chemical_name_systematic
; 
 technetium-fluoride-trioxide*technetium-trifluoride-dioxide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.130(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.201(2)
_cell_length_b                   14.583(4)
_cell_length_c                   5.3049(16)
_cell_measurement_temperature    133(2)
_cell_volume                     634.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20
_diffrn_measured_fraction_theta_full 0.765
_diffrn_measured_fraction_theta_max 0.765
_diffrn_measurement_device_type  `Bruker-SMART-CCD-Diffractometer`
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6137
_diffrn_reflns_theta_full        32.90
_diffrn_reflns_theta_max         32.90
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    4.418
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.737497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.516
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0415P)^2^+4.3617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                1668
_reflns_number_total             1817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070333ysi20070221_054332.cif
_cod_data_source_block           tco3ftco2f3
_cod_original_cell_volume        634.5(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4339752