Redetermination of the crystal structure of NaTcO~4~ at 100 and 296K based on single-crystal X-ray data
German, Konstantin E.; Grigoriev, Mikhail S.; Garashchenko, Bogdan L.; Kopytin, Alexander V.; Tyupina, Ekaterina A.; Acta Crystallographica Section E 73 (2017) 1037–1040; doi:10.1107/S2056989017008362

data_2242256
_publ_section_title
;
 Redetermination of the crystal structure of NaTcO~4~ at 100 and 296K
 based on single-crystal X-ray data
;
_journal_coeditor_code           WM5391
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1037
_journal_page_last               1040
_journal_paper_doi               10.1107/S2056989017008362
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'Na Tc O4'
_chemical_formula_moiety         'O4 Tc, Na'
_chemical_formula_sum            'Na O4 Tc'
_chemical_formula_weight         185.9
_chemical_melting_point_lt       1063
_chemical_name_common            'sodium pertechnetate'
_chemical_name_systematic
;
Sodium pertechnetate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.2945(2)
_cell_length_b                   5.2945(2)
_cell_length_c                   11.7470(5)
_cell_measurement_reflns_used    5622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.380
_cell_measurement_theta_min      4.222
_cell_volume                     329.29(2)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa APEXII area-detector'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         44.992
_diffrn_reflns_theta_min         4.222
_exptl_absorpt_coefficient_mu    4.332
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.750
_exptl_crystal_description       fragment
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.337
_refine_ls_extinction_coef       0.0489(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.310
_refine_ls_R_factor_all          0.0098
_refine_ls_R_factor_gt           0.0092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0029P)^2^+0.0769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0166
_refine_ls_wR_factor_ref         0.0168
_reflns_number_gt                661
_reflns_number_total             678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5391sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        329.29(3)
_cod_database_code               2242256
_cod_database_fobs_code          2242256
_shelx_estimated_absorpt_t_min   0.321
_shelx_estimated_absorpt_t_max   0.478
_shelx_hkl_checksum              45403