Actinide complexes with Wells-Dawson polyoxometalates (part 1): americium and curium.
Colliard, Ian; Deblonde, Gauthier J.-P.; Chemical communications (Cambridge, England) 62 (2026) 4018–4022; doi:10.1039/d5cc06999h

data_7135386
_publ_section_title
;
 Actinide complexes with Wells-Dawson polyoxometalates (part 1): americium
 and curium.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4018
_journal_page_last               4022
_journal_paper_doi               10.1039/d5cc06999h
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C153 H178 I N3 O5 Se, 4(C4 H10 O)'
_chemical_formula_sum            'C169 H218 I N3 O9 Se'
_chemical_formula_weight         2641.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-11-30 deposited with the CCDC.	2026-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0620(2)
_cell_length_b                   33.4078(4)
_cell_length_c                   36.9123(4)
_cell_measurement_reflns_used    21949
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      73.8700
_cell_measurement_theta_min      2.7370
_cell_volume                     16107.5(4)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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    -23.00  65.00   0.50   10.63    --   47.19 -74.00 -32.00  176
  2  \w    -81.00 -56.00   0.50   42.51    -- -102.00  67.00 -26.00   50
  3  \w   -152.00-100.00   0.50   42.51    -- -102.00 -81.00  85.00  104
  4  \w     33.00 106.00   0.50   42.51    --  104.75 -74.00 -32.00  146
  5  \w    -16.00  21.00   0.50   10.63    --  -47.19  19.00  90.00   74
  6  \w   -119.00 -94.00   0.50   10.63    --  -47.19-125.00  30.00   50
  7  \w    -16.00  24.00   0.50   10.63    --  -47.19  19.00 120.00   80
  8  \w    -27.00  -2.00   0.50   10.63    --   47.19 -19.00-150.00   50
  9  \w    -66.00 -39.00   0.50   42.51    -- -102.00 125.00-120.00   54
 10  \w    -67.00 -39.00   0.50   42.51    -- -102.00  61.00-180.00   56
 11  \w    -72.00 -31.00   0.50   42.51    -- -102.00  61.00  90.00   82
 12  \w    -71.00 -37.00   0.50   42.51    -- -102.00  61.00 120.00   68
 13  \w     91.00 178.00   0.50   42.51    --  104.75  15.00-120.00  174
 14  \w     35.00  70.00   0.50   42.51    --  104.75 -61.00 120.00   70
 15  \w     42.00  71.00   0.50   42.51    --  104.75 -61.00-180.00   58
 16  \w     97.00 160.00   0.50   42.51    --  104.75  30.00 -90.00  126
 17  \w     40.00  72.00   0.50   42.51    --  104.75 -61.00 -90.00   64
 18  \w     70.00 102.00   0.50   42.51    --  104.75 -94.00 -90.00   64
 19  \w     91.00 166.00   0.50   42.51    --  104.75  15.00-180.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0817389000
_diffrn_orient_matrix_UB_12      -0.0331564000
_diffrn_orient_matrix_UB_13      0.0022396000
_diffrn_orient_matrix_UB_21      0.0513225000
_diffrn_orient_matrix_UB_22      0.0219471000
_diffrn_orient_matrix_UB_23      0.0318995000
_diffrn_orient_matrix_UB_31      -0.0678734000
_diffrn_orient_matrix_UB_32      -0.0233222000
_diffrn_orient_matrix_UB_33      0.0268160000
_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  0.1238
_diffrn_reflns_av_unetI/netI     0.1023
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            96720
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.361
_diffrn_reflns_theta_min         2.735
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80739
_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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       block
_exptl_crystal_F_000             5648
_exptl_crystal_recrystallization_method 'recrystallization from Et2O-MeCN'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 6128 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1697
_refine_ls_number_reflns         32297
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1322
_refine_ls_R_factor_gt           0.0831
_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^)+(0.1618P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2530
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                19647
_reflns_number_total             32297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06999h2.cif
_cod_data_source_block           BpscSec-SeI-ProProOMe
_cod_database_code               7135386
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C151H176IN3O6Se
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.842
_diffrn_oxdiff_digest_hkl
;
01f1f9c0976195a7b4fb9beaee3190f77dbd3d
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C04W-C04Z
 1.524 with sigma of 0.03
 C04S-C04T
 1.524 with sigma of 0.03
 O04R-C04Y
 1.426 with sigma of 0.03
 C047-C13
 1.524 with sigma of 0.03
3. Others
 Sof(H04u)=Sof(H04v)=Sof(H04y)=Sof(Hw)=Sof(C23)=Sof(H23a)=Sof(H23b)=1-FVAR(1)
 Sof(H04s)=Sof(H04t)=Sof(H04w)=Sof(H04x)=Sof(C050)=Sof(H05a)=Sof(H05b)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C01D(H01D), C01M(H01M), C01O(H01O), C01T(H01T), C020(H020), C02B(H02B),
 C02G(H02G), C02I(H02I), C02O(H02O), C02S(H02S), C02T(H02T), C02W(H02W),
 C02Y(H02Y), C030(H030), C033(H033), C038(H038), C03E(H03j), C03H(H03o),
 C047(H047)
4.b Secondary CH2 refined with riding coordinates:
 C03O(H29,Hb), C03Q(H2,He), C03W(H8,Hp), C03X(H9,Hq), C03Z(H25,Ht), C049(H04s,
 H04t), C049(H04u,H04v), C04A(H04w,H04x), C04A(H04y,Hw), C04I(H16,H47),
 C04J(H21,H48), C04N(H30,H53), C04P(H23,H56), C04S(H32,H59), C04W(H27,H66),
 C04Y(H35,H69), C050(H05a,H05b), C23(H23a,H23b)
4.c Me refined with riding coordinates:
 C03K(H03t,H03u,H03v), C16(H16a,H16b,H16c)
4.d Aromatic/amide H refined with riding coordinates:
 C004(H004), N005(H005), C00H(H00H), C00O(H00O), C00P(H00P), C00S(H00S),
 C00T(H00T), C00U(H00U), C00Y(H00Y), C010(H010), C011(H011), C015(H015),
 C016(H016), C01A(H01A), C01B(H01B), C01E(H01E), C01H(H01H), C01I(H01I),
 C01R(H01R), C01S(H01S), C01W(H01W), C01X(H01X), C01Z(H01Z), C024(H024),
 C025(H025), C027(H027), C028(H028), C029(H029), C02C(H02C), C02F(H02F),
 C02L(H02L), C02M(H02M), C02N(H02N), C02P(H02P), C02U(H02U), C02Z(H02Z),
 C031(H031), C034(H034), C035(H035), C037(H037), C039(H039), C03F(H03k),
 C03I(H03p), C03N(H03), C046(H046), C04M(H19)
4.e Idealised Me refined as rotating group:
 C03A(H03a,H03b,H03c), C03B(H03d,H03e,H03f), C03D(H03g,H03h,H03i), C03G(H03l,
 H03m,H03n), C03J(H03q,H03r,H03s), C03L(H03w,H03x,H03y), C03M(H03z,H,Ha),
 C03P(H1,Hc,Hd), C03R(H3,Hf,Hg), C03S(H4,Hh,Hi), C03T(H5,Hj,Hk), C03U(H6,Hl,Hm),
  C03V(H7,Hn,Ho), C03Y(H10,Hr,Hs), C040(H04a,H04b,H04c), C041(H04d,H04e,H04f),
 C042(H04g,H04h,H04i), C043(H04j,H04k,H04l), C044(H04m,H04n,H04o), C045(H26,Hu,
 Hv), C048(H04p,H04q,H04r), C04B(H04z,Hx,Hy), C04C(H04,Hz,H36), C04D(H11,H37,
 H38), C04E(H12,H39,H40), C04F(H13,H41,H42), C04G(H14,H43,H44), C04H(H15,H45,
 H46), C04K(H17,H49,H50), C04L(H18,H51,H52), C04O(H22,H54,H55), C04Q(H20,H57,
 H58), C04T(H33,H60,H61), C04U(H31,H62,H63), C04V(H24,H64,H65), C04X(H34,H67,
 H68), C04Z(H28,H70,H71), C051(H05c,H05d,H05e), C13(H13a,H13b,H13c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95434
_shelx_hkl_checksum              64688
_shelx_fab_checksum              22872
_olex2_exptl_crystal_mounting_method 'sample loop'
_olex2_submission_original_sample_id RM1063
_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 2.394
_oxdiff_exptl_absorpt_empirical_full_min 0.280