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_7135582
_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         'Cs14 O100 P2 Tc6 W20'
_chemical_formula_sum            'Cs14 O100 P2 Tc6 W20'
_chemical_formula_weight         7787.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                90
_cell_angle_beta                 105.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.3520(2)
_cell_length_b                   18.3764(3)
_cell_length_c                   12.9618(2)
_cell_measurement_reflns_used    11970
_cell_measurement_temperature    173.00(11)
_cell_measurement_theta_max      75.5020
_cell_measurement_theta_min      3.5260
_cell_volume                     2609.92(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.128a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))'
_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(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_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   -115.00 -40.00   0.50    2.50    --  -46.92 -37.00  30.00  150
  2  \w     -7.00  26.00   0.50    2.50    --  -46.92  37.00-180.00   66
  3  \w    -69.00  11.00   0.50    2.50    --  -46.92  77.00 150.00  160
  4  \w    -42.00  25.00   0.50    2.50    --  -46.92  37.00  60.00  134
  5  \w    -26.00   8.00   0.50    2.50    --  -46.92  19.00-180.00   68
  6  \w    -41.00  22.00   0.50    2.50    --  -46.92  37.00 -60.00  126
  7  \w    -15.00  16.00   0.50    2.50    --   46.92 -57.00-180.00   62
  8  \w    -22.00  13.00   0.50    2.50    --   46.92 -19.00 -60.00   70
  9  \w     34.00  62.00   0.50    2.50    --   46.92 -57.00-180.00   56
 10  \w   -152.00-113.00   0.50    8.00    --  -91.75 -94.00 -60.00   78
 11  \w    -50.00 -21.00   0.50    8.00    --  -91.75  45.00-180.00   58
 12  \w    -51.00 -26.00   0.50    8.00    --  -91.75  45.00  90.00   50
 13  \w    -48.00 -23.00   0.50    8.00    --  -91.75  45.00  30.00   50
 14  \w   -160.00-108.00   0.50    8.00    --  -91.75 -61.00 150.00  104
 15  \w    -65.00 -39.00   0.50    8.00    --  -91.75  61.00  30.00   52
 16  \w   -105.00 -29.00   0.50    8.00    --  -91.75  77.00 -60.00  152
 17  \w     33.00  63.00   0.50    8.00    --  103.56 -61.00-150.00   60
 18  \w     56.00  96.00   0.50    8.00    --  103.56 -94.00  90.00   80
 19  \w     78.00 105.00   0.50    8.00    --  103.56 -94.00 -60.00   54
 20  \w     73.00 102.00   0.50    8.00    --  103.56 -77.00 -90.00   58
 21  \w     91.00 177.00   0.50    8.00    --  103.56  30.00 -90.00  172
 22  \w     34.00  64.00   0.50    8.00    --  103.56 -77.00 -90.00   60
 23  \w     93.00 176.00   0.50    8.00    --  103.56  15.00-120.00  166
 24  \w     71.00 101.00   0.50    8.00    --  103.56 -94.00-150.00   60
 25  \w     35.00  70.00   0.50    8.00    --  103.56 -61.00 -60.00   70
 26  \w     42.00  67.00   0.50    8.00    --  103.56 -94.00 -60.00   50
 27  \w     35.00  62.00   0.50    8.00    --  103.56 -61.00-180.00   54
 28  \w     91.00 177.00   0.50    8.00    --  103.56  30.00-180.00  172
 29  \w     32.00 104.00   0.50    8.00    --  103.56 -94.00 120.00  144
 30  \w     41.00  91.00   0.50    8.00    --  103.56 -94.00-180.00  100
 31  \w     44.00  86.00   0.50    8.00    --  103.56 -77.00  30.00   84
 32  \w     33.00  68.00   0.50    8.00    --  103.56 -61.00  30.00   70
 33  \w     36.00  70.00   0.50    8.00    --  103.56 -61.00 150.00   68
 34  \w     31.00 105.00   0.50    8.00    --  103.56 -94.00  30.00  148
 35  \w     93.00 177.00   0.50    8.00    --  103.56  30.00 150.00  168
;
_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      0.1360305000
_diffrn_orient_matrix_UB_12      0.0020578000
_diffrn_orient_matrix_UB_13      0.0012725000
_diffrn_orient_matrix_UB_21      -0.0271623000
_diffrn_orient_matrix_UB_22      -0.0472832000
_diffrn_orient_matrix_UB_23      -0.1015420000
_diffrn_orient_matrix_UB_31      -0.0226737000
_diffrn_orient_matrix_UB_32      0.0691430000
_diffrn_orient_matrix_UB_33      -0.0695637000
_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  0.0708
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25612
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.443
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    84.530
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.128a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.955
_exptl_crystal_description       needle
_exptl_crystal_F_000             3338
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         7.386
_refine_diff_density_min         -3.132
_refine_diff_density_rms         0.760
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     479
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0955
_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^)+(0.0908P)^2^+585.9157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2471
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5083
_reflns_number_total             5422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06618b2.cif
_cod_data_source_block           abs11
_cod_depositor_comments
'Adding full bibliography for 7135580--7135582.cif.'
_cod_database_code               7135582
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Tc2 W20 O68 '
_shelx_estimated_absorpt_t_max   0.485
_shelx_estimated_absorpt_t_min   0.039
_reflns_odcompleteness_completeness 99.94
_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
;
_shelx_res_checksum              33225
_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 4.379
_oxdiff_exptl_absorpt_empirical_full_min 0.548