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_7135581
_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         'Na16 O90 Si2 Tc2 W20'
_chemical_formula_sum            'Na16 O90 Si2 Tc2 W20'
_chemical_formula_weight         5737.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-04
_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                105.751(3)
_cell_angle_beta                 93.888(2)
_cell_angle_gamma                107.964(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1764(3)
_cell_length_b                   13.2378(6)
_cell_length_c                   17.8440(4)
_cell_measurement_reflns_used    9793
_cell_measurement_temperature    172.99(11)
_cell_measurement_theta_max      75.5050
_cell_measurement_theta_min      2.6060
_cell_volume                     2383.70(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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      172.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.946
_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    -90.00 -25.00   0.50    5.00    --  -47.01 -75.00-136.00  130
  2  \w    -69.00  15.00   0.50    5.00    --  -47.01  75.00  -8.00  168
  3  \w     32.00 112.00   0.50    5.00    --   47.01  75.00  -8.00  160
  4  \w   -155.00-126.00   0.50   14.00    --  -86.25 -75.00-136.00   58
  5  \w    -56.00 -31.00   0.50   14.00    --  -86.25  75.00  -8.00   50
  6  \w   -115.00 -90.00   0.50   14.00    --  -86.25 -75.00-136.00   50
  7  \w     52.00  89.00   0.50   14.00    --  104.22 -75.00-136.00   74
  8  \w     82.00 147.00   0.50   14.00    --  104.22  75.00  -8.00  130
  9  \w    -37.00  25.00   0.50    5.00    --  -47.01  37.00 -30.00  124
 10  \w   -119.00 -91.00   0.50    5.00    --  -47.01 -77.00 -30.00   56
 11  \w     34.00  90.00   0.50    5.00    --   47.01-125.00-120.00  112
 12  \w    -27.00  24.00   0.50    5.00    --   47.01 -19.00 120.00  102
 13  \w    -17.00   8.00   0.50    5.00    --   47.01 -75.00-136.00   50
 14  \w     27.00  53.00   0.50    5.00    --   47.01 -75.00-136.00   52
 15  \w   -141.00-113.00   0.50   14.00    --  -86.25 -77.00 -60.00   56
 16  \w    -49.00 -24.00   0.50   14.00    --  -86.25  45.00 150.00   50
 17  \w   -158.00 -92.00   0.50   14.00    --  -86.25 -77.00 -30.00  132
 18  \w     64.00 106.00   0.50   14.00    --  104.22 -77.00  30.00   84
 19  \w     93.00 176.00   0.50   14.00    --  104.22  45.00-120.00  166
 20  \w     79.00 106.00   0.50   14.00    --  104.22 -94.00   0.00   54
 21  \w     33.00  67.00   0.50   14.00    --  104.22 -61.00  90.00   68
 22  \w     35.00  72.00   0.50   14.00    --  104.22-125.00  90.00   74
 23  \w     35.00  61.00   0.50   14.00    --  104.22 -77.00  30.00   52
 24  \w     44.00  69.00   0.50   14.00    --  104.22 -61.00  30.00   50
 25  \w     32.00  93.00   0.50   14.00    --  104.22 -94.00-180.00  122
 26  \w     48.00 106.00   0.50   14.00    --  104.22 -94.00  90.00  116
 27  \w     32.00  87.00   0.50   14.00    --  104.22 -94.00 -60.00  110
 28  \w     47.00 105.00   0.50   14.00    --  104.22 -94.00 -30.00  116
 29  \w     49.00 103.00   0.50   14.00    --  104.22 -94.00 150.00  108
 30  \w     93.00 169.00   0.50   14.00    --  104.22  45.00-150.00  152
 31  \w    112.00 178.00   0.50   14.00    --  104.22  30.00 150.00  132
 32  \w     58.00 103.00   0.50   14.00    --  104.22 -94.00-150.00   90
 33  \w     87.00 112.00   0.50   14.00    --  104.22-125.00  90.00   50
 34  \w     37.00 106.00   0.50   14.00    --  104.22 -94.00 -90.00  138
 35  \w     90.00 160.00   0.50   14.00    --  104.22  61.00 -60.00  140
 36  \w    112.00 138.00   0.50   14.00    --  104.22  45.00 -90.00   52
;
_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      0.0747331000
_diffrn_orient_matrix_UB_12      -0.0705259000
_diffrn_orient_matrix_UB_13      0.0226800000
_diffrn_orient_matrix_UB_21      -0.0769168000
_diffrn_orient_matrix_UB_22      -0.0997731000
_diffrn_orient_matrix_UB_23      -0.0723427000
_diffrn_orient_matrix_UB_31      0.1004363000
_diffrn_orient_matrix_UB_32      0.0400976000
_diffrn_orient_matrix_UB_33      -0.0502542000
_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  0.0862
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27215
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.071
_diffrn_reflns_theta_min         3.807
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    47.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    3.997
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2490
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         7.172
_refine_diff_density_min         -3.309
_refine_diff_density_rms         0.761
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9422
_refine_ls_number_restraints     881
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1574P)^2^+126.2516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7686
_reflns_number_total             9422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06618b2.cif
_cod_data_source_block           sw9-sol-dichrom_auto
_cod_depositor_comments
'Adding full bibliography for 7135580--7135582.cif.'
_cod_original_cell_volume        2383.70(15)
_cod_database_code               7135581
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W Tc O'
_shelx_estimated_absorpt_t_max   0.648
_shelx_estimated_absorpt_t_min   0.163
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2. Others
 Fixed Sof: Na6(0.5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83395
_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 4.894
_oxdiff_exptl_absorpt_empirical_full_min 0.320