Actinide complexes with Wells-Dawson polyoxometalates (part 2): californium.
Colliard, Ian; Deblonde, Gauthier J.-P.; Chemical communications (Cambridge, England) 62 (2026) 4023–4027; doi:10.1039/d5cc07083j

data_7135397
_publ_section_title
;
 Actinide complexes with Wells-Dawson polyoxometalates (part 2):
 californium.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4023
_journal_page_last               4027
_journal_paper_doi               10.1039/d5cc07083j
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         '4(Cf O122 P4 W34), 68(K), 4(O)'
_chemical_formula_sum            'Cf4 K68 O492 P16 W136'
_chemical_formula_weight         37033.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-10 deposited with the CCDC.	2026-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.3745(2)
_cell_length_b                   23.4607(3)
_cell_length_c                   51.8190(6)
_cell_measurement_reflns_used    58979
_cell_measurement_temperature    298
_cell_measurement_theta_max      34.5750
_cell_measurement_theta_min      3.4640
_cell_volume                     15042.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.876
_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     18.00  55.24   0.38    3.00    --   12.09-111.00   3.00   98
  2  \w      4.00  47.32   0.38    3.00    --   12.09 -99.00-120.00  114
  3  \w    -12.00  48.04   0.38    3.00    --   12.09 -99.00 120.00  158
  4  \w    -12.00  29.04   0.38    3.00    --   12.09 -99.00 -90.00  108
  5  \w     -5.00  74.04   0.38    3.00    --   12.09  57.00-180.00  208
  6  \w      8.00  81.34   0.38    3.00    --   12.09  57.00 -30.00  193
  7  \w    -62.00 -28.94   0.38    3.00    --   12.09 -19.00   0.00   87
  8  \w    -14.00  17.16   0.38    3.00    --   12.09 -19.00   0.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0090253000
_diffrn_orient_matrix_UB_12      -0.0194192000
_diffrn_orient_matrix_UB_13      0.0102896000
_diffrn_orient_matrix_UB_21      0.0021220000
_diffrn_orient_matrix_UB_22      -0.0228234000
_diffrn_orient_matrix_UB_23      -0.0089577000
_diffrn_orient_matrix_UB_31      0.0565870000
_diffrn_orient_matrix_UB_32      0.0039595000
_diffrn_orient_matrix_UB_33      -0.0011523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            208996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.834
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    27.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.088
_exptl_crystal_description       plate
_exptl_crystal_F_000             15924
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.759
_refine_diff_density_min         -3.808
_refine_diff_density_rms         0.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1652
_refine_ls_number_reflns         57285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1318P)^2^+14.2113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35995
_reflns_number_total             57285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07083j2.cif
_cod_data_source_block           cfp2w17_mp
_cod_database_code               7135397
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Pu W34 O130 K17 P4'
_cell_oxdiff_angle_alpha         90.0048(9)
_cell_oxdiff_angle_beta          90.6317(8)
_cell_oxdiff_angle_gamma         90.0118(11)
_cell_oxdiff_length_a            12.37084(17)
_cell_oxdiff_length_b            23.4667(3)
_cell_oxdiff_length_c            51.8213(4)
_cell_oxdiff_measurement_reflns_used 58919
_cell_oxdiff_volume              15042.9(3)
_shelx_estimated_absorpt_t_max   0.345
_shelx_estimated_absorpt_t_min   0.021
_olex2_refinement_description
;
1. Others
 Fixed Sof: K3(0.75) K4(0.75) K6(0.75) K7(0.75) K9(0.75) K10(0.75) K11(0.75)
 K12(0.75) K14(0.75) K16(0.5) K17(0.75) K18(0.5) K19(0.75) K20(0.75) K21(0.75)
 K22(0.25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39336
_shelx_hkl_checksum              27904
_shelx_fab_checksum              84312
_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 5.400
_oxdiff_exptl_absorpt_empirical_full_min 0.365