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_4335231
_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         'F6  Tc, 2(Rb)'
_chemical_formula_sum            'F6 Rb2 Tc'
_chemical_formula_weight         382.92
_chemical_name_common            'Rubidium hexafluorotechnetate'
_chemical_name_systematic        'Rubidium hexafluorotechnetate'
_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_hydrogens   none
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   5.949(1)
_cell_length_b                   5.949(1)
_cell_length_c                   4.759(1)
_cell_measurement_reflns_used    3723
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.81
_cell_measurement_theta_min      3.95
_cell_volume                     145.86(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86(Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1577
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         3.96
_exptl_absorpt_coefficient_mu    19.079
_exptl_absorpt_correction_T_max  0.1917
_exptl_absorpt_correction_T_min  0.0398
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
P. Coppens in "Crystallographic Computing" ed F.R Ahmed, S.R. Hall 
and C.P.Huber, Copenhagen, Munksgaard, (1979) pp 255-270
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             171
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.431
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.314
_refine_ls_extinction_coef       0.16(3)
_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   1.140
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     13
_refine_ls_number_reflns         173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0706P)^2^+0.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                171
_reflns_number_total             173
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400775e_si_001_5.cif
_cod_data_source_block           rb2tcf6
_cod_database_code               4335231