Hexafluoridotechnetate(IV) Revisited
Samundeeswari Mariappan Balasekaran; Matthias Molski; Johann Spandl; Adelheid Hagenbach; Roger Alberto; Ulrich Abram; Inorganic Chemistry 52 (2013) 7094–7099; doi:10.1021/ic400775e

data_4335230
_publ_contact_author
;
      Ulrich Abram
      Freie Universitaet Berlin
      Institute of Chemistry and Biochemistry
      Fabeckstrasse 34-36
      D-14195 Berlin
      Germany
;
_publ_contact_author_email       ulrich.abram@fu-berlin.de
_publ_contact_author_fax         '049 30 838 52676'
_publ_contact_author_phone       '049 30 838 54002'
_publ_section_title
;
 Hexafluoridotechnetate(IV) Revisited
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7094
_journal_page_last               7099
_journal_paper_doi               10.1021/ic400775e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Tc F6, 2(K)'
_chemical_formula_sum            'F6 K2 Tc'
_chemical_formula_weight         290.18
_chemical_name_common            'Potassium hexafluorotechnetate(IV)'
_chemical_name_systematic        'Potassium hexafluorotechnetate(IV)'
_space_group_IT_number           164
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"'
_symmetry_space_group_name_H-M   'P -3 m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.000(12)
_cell_formula_units_Z            1
_cell_length_a                   5.7960(10)
_cell_length_b                   5.7960(10)
_cell_length_c                   4.6135(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22.04
_cell_measurement_theta_min      4.06
_cell_volume                     134.22(5)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        'HELENA, PLATON'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'Omega scans'
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1168
_diffrn_reflns_theta_full        26.86
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         4.06
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.268
_exptl_absorpt_correction_T_max  0.4734
_exptl_absorpt_correction_T_min  0.3025
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'HELENA, PLATON'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             135
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       0.090(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_matrix_type           full
_refine_ls_number_parameters     13
_refine_ls_number_reflns         130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0141
_refine_ls_R_factor_gt           0.0136
_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^)+(0.0174P)^2^+0.0426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0285
_refine_ls_wR_factor_ref         0.0285
_reflns_number_gt                127
_reflns_number_total             130
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400775e_si_001_4.cif
_cod_data_source_block           k2tcf6
_cod_original_cell_volume        134.22(4)
_cod_database_code               4335230