Building block approach to technetium-substituted polyoxotungstates.
Bustos, Jenna; Zakharov, Lev N.; Buils, Jordi; Hosseini, Farzaneh; Solé-Daura, Albert; Bo, Carles; Nyman, May; Chemical communications (Cambridge, England) 62 (2026) 5875–5879; doi:10.1039/d5cc06618b

data_7135580
_publ_section_title
;
 Building block approach to technetium-substituted polyoxotungstates.
;
_journal_issue                   21
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5875
_journal_page_last               5879
_journal_paper_doi               10.1039/d5cc06618b
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'Cl10 K4 O Tc2'
_chemical_formula_sum            'Cl10 K4 O Tc2'
_chemical_formula_weight         722.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-11-04 deposited with the CCDC.	2026-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0126(2)
_cell_length_b                   7.0126(2)
_cell_length_c                   17.5752(5)
_cell_measurement_reflns_used    705
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.3780
_cell_measurement_theta_min      5.0060
_cell_volume                     864.29(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -45.00 -20.00   0.50    1.20    --  -91.75  40.00  72.00   50
  2  \w    -47.00 -17.00   0.50    0.40    --  -46.74 125.00 -90.00   60
  3  \w    -51.00 -26.00   0.50    1.20    --  -91.75  45.00 -60.00   50
  4  \w   -116.00 -56.00   0.50    0.40    --  -46.74 -40.00 -81.00  120
  5  \w    -23.00   2.00   0.50    0.40    --   46.74 -19.00   0.00   50
  6  \w     31.00  56.00   0.50    1.20    --  103.49 -61.00   0.00   50
  7  \w     38.00  65.00   0.50    1.20    --  103.49 -61.00  60.00   54
  8  \w     32.00  70.00   0.50    1.20    --  103.49 -61.00  90.00   76
  9  \w     95.00 173.00   0.50    1.20    --  103.49  40.00  72.00  156
 10  \w    117.00 160.00   0.50    1.20    --  103.49  88.00 -90.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1110776000
_diffrn_orient_matrix_UB_12      -0.0853536000
_diffrn_orient_matrix_UB_13      -0.0675536000
_diffrn_orient_matrix_UB_21      0.0087914000
_diffrn_orient_matrix_UB_22      0.1937625000
_diffrn_orient_matrix_UB_23      -0.0411875000
_diffrn_orient_matrix_UB_31      0.1892230000
_diffrn_orient_matrix_UB_32      -0.0587722000
_diffrn_orient_matrix_UB_33      -0.0377722000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            1055
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.481
_diffrn_reflns_theta_min         5.033
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    35.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.128a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'brown orange'
_exptl_crystal_colour_modifier   brown
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                282
_reflns_number_total             297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06618b2.cif
_cod_data_source_block           exp_5168_auto
_cod_depositor_comments
'Adding full bibliography for 7135580--7135582.cif.'
_cod_original_cell_volume        864.29(6)
_cod_database_code               7135580
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'O Cl Tc '
_shelx_estimated_absorpt_t_max   0.329
_shelx_estimated_absorpt_t_min   0.223
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
;
_shelx_res_checksum              95032
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.812
_oxdiff_exptl_absorpt_empirical_full_min 0.696