Isolation of a new polyoxometalate complex of plutonium.
Colliard, Ian; Stavila, Vitalie; Deblonde, Gauthier J.-P.; Chemical communications (Cambridge, England) 61 (2025) 11858–11861; doi:10.1039/d5cc03481g

data_7134796
_publ_section_title
;
 Isolation of a new polyoxometalate complex of plutonium.
;
_journal_issue                   63
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11858
_journal_page_last               11861
_journal_paper_doi               10.1039/d5cc03481g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         '2(O36 Pu W10), 18(Cs), 2(Cl), 11(O)'
_chemical_formula_sum            'Cl2 Cs18 O83 Pu2 W20'
_chemical_formula_weight         7952.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2025-06-16
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-17 deposited with the CCDC.	2025-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.8140(10)
_cell_angle_beta                 102.4110(10)
_cell_angle_gamma                99.1050(10)
_cell_formula_units_Z            2
_cell_length_a                   14.0250(2)
_cell_length_b                   17.2738(2)
_cell_length_c                   22.2406(3)
_cell_measurement_reflns_used    43846
_cell_measurement_temperature    298
_cell_measurement_theta_max      34.7650
_cell_measurement_theta_min      3.4290
_cell_volume                     5056.81(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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    -10.00  34.00   0.50    1.28    --   12.09  85.00-128.00   88
  2  \w      7.00  84.00   0.50    1.28    --   12.09  57.00-120.00  154
  3  \w    -42.00  42.00   0.50    1.28    --   12.09 -85.00 112.00  168
  4  \w    -54.00 -17.00   0.50    1.28    --   12.09 -19.00 150.00   74
  5  \w    -11.00  48.00   0.50    1.28    --   12.09 -99.00   0.00  118
  6  \w    -15.00  14.00   0.50    1.28    --   12.09 -19.00-180.00   58
  7  \w    -42.00  30.00   0.50    1.28    --  -13.65  85.00-128.00  144
  8  \w    -32.00  63.00   0.50    1.28    --  -13.65  38.00 -60.00  190
  9  \w    -32.00  59.00   0.50    1.28    --  -13.65  57.00   0.00  182
 10  \w    -32.00  10.00   0.50    1.28    --  -13.65  38.00  90.00   84
 11  \w     30.00  56.00   0.50    1.28    --  -13.65  38.00  90.00   52
 12  \w    -41.00   5.00   0.50    1.28    --  -13.65 -85.00 112.00   92
 13  \w    -62.00 -37.00   0.50    1.28    --  -13.65 -57.00   0.00   50
 14  \w    -27.00  -2.00   0.50    1.28    --  -13.65 -57.00   0.00   50
 15  \w    -35.50 -12.00   0.50    1.28    --  -13.65 -57.00 -30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            130844
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.289
_exptl_absorpt_coefficient_mu    30.458
_exptl_absorpt_correction_T_max  0.01625
_exptl_absorpt_correction_T_min  0.00304
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    5.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             6712
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         4.599
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.592
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         30799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0628
_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^)+(0.1190P)^2^+3.4989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23866
_reflns_number_total             30799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03481g2.cif
_cod_data_source_block           cs-puw5
_cod_depositor_comments          'Adding full bibliography for 7134796.cif.'
_cod_database_code               7134796
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Cs9 O40 W10 U'
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.462
_diffrn_oxdiff_ac3_digest_hkl    41b26bdb8db7e48e6c67cd7cc59d2b68d1d408
_olex2_refinement_description
;
;
_shelx_res_checksum              11085
_shelx_hkl_checksum              28402
_shelx_fab_checksum              21877
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 5.774
_oxdiff_exptl_absorpt_empirical_full_min 0.170