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_7135396
_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         'O122 P4 Pr W34, 17(K), 3(O)'
_chemical_formula_sum            'K17 O125 P4 Pr W34'
_chemical_formula_weight         9180.39
_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             2025-12-10
_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                95.4460(10)
_cell_angle_beta                 102.7470(10)
_cell_angle_gamma                99.3290(10)
_cell_formula_units_Z            2
_cell_length_a                   14.6606(2)
_cell_length_b                   22.5777(3)
_cell_length_c                   24.8922(4)
_cell_measurement_reflns_used    43862
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.7060
_cell_measurement_theta_min      3.6920
_cell_volume                     7856.6(2)
_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      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.856
_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  20.00   0.50    0.98    --   12.09 -19.00  30.00   60
  2  \w     49.00  84.00   0.50    0.98    --   12.09  57.00-150.00   70
  3  \w     -5.00  39.00   0.50    0.98    --   12.09  57.00-150.00   88
  4  \w    -38.00  11.00   0.50    0.98    --   12.09 -19.00-180.00   98
  5  \w    -11.00  47.00   0.50    0.98    --   12.09 -99.00 -60.00  116
  6  \w    -11.00  46.00   0.50    0.98    --   12.09 -99.00 -30.00  114
  7  \w    -10.00  48.00   0.50    0.98    --   12.09 -99.00  30.00  116
  8  \w     -1.00  25.00   0.50    0.98    --   12.09 -99.00-180.00   52
  9  \w     30.00  65.00   0.50    0.98    --   12.09-130.00-122.00   70
 10  \w     24.00  71.00   0.50    0.98    --   12.09-139.00  63.00   94
 11  \w    -11.00  49.00   0.50    0.98    --   12.09 -99.00  90.00  120
 12  \w    -80.00  12.00   0.50    0.98    --  -13.65 -77.00  30.00  184
 13  \w    -86.00   0.00   0.50    0.98    --  -13.65 -57.00 150.00  172
;
_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      0.0484667000
_diffrn_orient_matrix_UB_12      -0.0015436000
_diffrn_orient_matrix_UB_13      0.0016673000
_diffrn_orient_matrix_UB_21      -0.0097144000
_diffrn_orient_matrix_UB_22      -0.0053710000
_diffrn_orient_matrix_UB_23      -0.0294286000
_diffrn_orient_matrix_UB_31      0.0103846000
_diffrn_orient_matrix_UB_32      0.0316449000
_diffrn_orient_matrix_UB_33      -0.0008481000
_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  0.0972
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            191864
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.917
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10824
_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    3.881
_exptl_crystal_description       plate
_exptl_crystal_F_000             7916
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         6.241
_refine_diff_density_min         -5.229
_refine_diff_density_rms         0.782
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1646
_refine_ls_number_reflns         58903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42275
_reflns_number_total             58903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07083j2.cif
_cod_data_source_block           prwd-k_ap
_cod_database_code               7135396
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Nd P4 O130 W34 K17'
_cell_oxdiff_angle_alpha         95.4456(12)
_cell_oxdiff_angle_beta          102.7472(13)
_cell_oxdiff_angle_gamma         99.3288(13)
_cell_oxdiff_length_a            14.6606(2)
_cell_oxdiff_length_b            22.5777(3)
_cell_oxdiff_length_c            24.8922(4)
_cell_oxdiff_measurement_reflns_used 43862
_cell_oxdiff_volume              7856.6(2)
_shelx_estimated_absorpt_t_max   0.149
_shelx_estimated_absorpt_t_min   0.026
_olex2_refinement_description
;
1. Others
 Fixed Sof: K12(0.75) K13(0.75) K15(0.75) K16(0.5) K17(0.25) K18(0.5)
 K19(0.75) K20(0.5) K21(0.25)
;
_shelx_res_checksum              14082
_shelx_hkl_checksum              99135
_shelx_fab_checksum              57888
_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 4.783
_oxdiff_exptl_absorpt_empirical_full_min 0.410