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_2242257
_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_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 tetraoxidotechnetate(VII)
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_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                   5.33250(10)
_cell_length_b                   5.33250(10)
_cell_length_c                   11.8503(3)
_cell_measurement_reflns_used    2097
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.201
_cell_measurement_theta_min      4.191
_cell_volume                     336.970(12)
_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
;
SHELXL-2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS-2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'Bruker Kappa APEX II area-detector diffractometer'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2371
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.894
_diffrn_reflns_theta_min         4.191
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.233
_exptl_absorpt_correction_T_max  0.485
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.664
_exptl_crystal_description       fragment
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.328
_refine_ls_extinction_coef       0.136(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   1.161
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0087
_refine_ls_R_factor_gt           0.0081
_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^)+(0.0071P)^2^+0.0846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0184
_refine_ls_wR_factor_ref         0.0186
_reflns_number_gt                350
_reflns_number_total             365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5391sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        336.970(15)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2242257
_cod_database_fobs_code          2242257
_shelx_hkl_checksum              66174