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_7135387
_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_absolute_configuration syn
_chemical_formula_moiety         'C148 H172 N2 O5 Se, 7.5(C2 H3 N)'
_chemical_formula_sum            'C163 H194.5 N9.5 O5 Se'
_chemical_formula_weight         2445.73
_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     iterative
_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                   13.530(7)
_cell_length_b                   27.651(8)
_cell_length_c                   42.347(12)
_cell_measurement_reflns_used    299
_cell_measurement_temperature    95
_cell_measurement_theta_max      34.6235
_cell_measurement_theta_min      0.4300
_cell_volume                     15843(10)
_computing_cell_refinement       XDS
_computing_data_collection       'KEK Unified Graphical User Interface (UGUI)'
_computing_data_reduction        XDS
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      95.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KEK BL-5A'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.750
_diffrn_reflns_av_R_equivalents  0.1449
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            307982
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.744
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         0.928
_diffrn_source                   'Multipole Wiggler'
_exptl_absorpt_coefficient_mu    0.329
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       needle
_exptl_crystal_F_000             5252
_exptl_crystal_recrystallization_method 'recrystallization from Et2O/MeCN'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 7522 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1670
_refine_ls_number_reflns         48547
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0920
_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^)+(0.1372P)^2^+0.4027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2577
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                25745
_reflns_number_total             48547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06999h2.cif
_cod_data_source_block           BpscSec-SeOH-ProOMe
_cod_original_formula_sum        'C163 H194.50 N9.50 O5 Se'
_cod_database_code               7135387
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N2-C1A
 1.14 with sigma of 0.02
 C1A-N2
 1.137 with sigma of 0.01
 C1A-C1B
 1.456 with sigma of 0.01
 C1B-N2
 2.593 with sigma of 0.02
 N1-C1C
 1.14 with sigma of 0.02
 C1C-N1
 1.137 with sigma of 0.01
 C1C-C1D
 1.456 with sigma of 0.01
 C1D-N1
 2.593 with sigma of 0.02
 N5-C1E
 1.14 with sigma of 0.02
 C1E-N5
 1.137 with sigma of 0.01
 C1E-C1F
 1.456 with sigma of 0.01
 C1F-N5
 2.593 with sigma of 0.02
 N6-C1G
 1.14 with sigma of 0.02
 C1G-N6
 1.137 with sigma of 0.01
 C1G-C1H
 1.456 with sigma of 0.01
 C1H-N6
 2.593 with sigma of 0.02
 N9-C1K
 1.14 with sigma of 0.02
 C1K-N9
 1.137 with sigma of 0.01
 C1K-C1L
 1.456 with sigma of 0.01
 C1L-N9
 2.593 with sigma of 0.02
 N10-C1M
 1.14 with sigma of 0.02
 C1M-N10
 1.137 with sigma of 0.01
 C1M-C1N
 1.456 with sigma of 0.01
 C1N-N10
 2.593 with sigma of 0.02
 N2-C1B
 2.59 with sigma of 0.04
 N1-C1D
 2.59 with sigma of 0.04
 N5-C1F
 2.59 with sigma of 0.04
 N6-C1H
 2.59 with sigma of 0.04
 N9-C1L
 2.59 with sigma of 0.04
 N10-C1N
 2.59 with sigma of 0.04
 C123-C167 \\sim C123-C1I
 with sigma of 0.02
 C123-C149 \\sim C123-C40
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim C1A \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N1 \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N5 \\sim C1E \\sim C1F: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N6 \\sim C1G \\sim C1H: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N9 \\sim C1K \\sim C1L: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N10 \\sim C1M \\sim C1N: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uiso(C40) = Uiso(C1I)
4. Rigid body (RIGU) restrains
 N2, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C1G, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N9, C1K, C1L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, C1M, C1N
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H12D)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=
 Sof(H1IC)=1-FVAR(1)
 Sof(H123)=Sof(C149)=Sof(H14S)=Sof(H14T)=Sof(H14U)=Sof(C167)=Sof(H16S)=
 Sof(H16T)=Sof(H16U)=FVAR(1)
 Fixed Sof: N9(0.5) C1K(0.5) C1L(0.5) H1LA(0.5) H1LB(0.5) H1LC(0.5)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C50(H50), C57(H57), C67(H67), C69(H69), C82(H82), C94(H94),
 C100(H100), C104(H104), C106(H106), C109(H109), C113(H113), C114(H114),
 C117(H117), C123(H123), C123(H12D), C132(H132), C135(H135), C144(H144)
6.b Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C98(H98A,H98B), C137(H13G,H13H), C138(H13I,H13J)
6.c Me refined with riding coordinates:
 C160(H16A,H16B,H16C), C1I(H1IA,H1IB,H1IC)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C13(H13), N16(H16), C17(H17), C19(H19),
 C21(H21), C23(H23), C27(H27), C32(H32), C33(H33), C35(H35), C37(H37), C41(H41),
  C46(H46), C49(H49), C52(H52), C56(H56), C58(H58), C62(H62), C65(H65),
 C66(H66), C68(H68), C70(H70), C75(H75), C77(H77), C78(H78), C81(H81), C84(H84),
  C90(H90), C95(H95), C99(H99), C102(H102), C103(H103), C107(H107), C110(H110),
 C115(H115), C119(H119), C121(H121), C125(H125), C131(H131), C136(H136),
 C148(H148), C156(H156)
6.e Tetrahedral OH refined with riding coordinates:
 O48(H48)
6.f Idealised Me refined as rotating group:
 C108(H10A,H10B,H10C), C116(H11A,H11B,H11C), C118(H11D,H11E,H11F), C122(H12A,
 H12B,H12C), C126(H12E,H12F,H12G), C127(H12H,H12I,H12J), C128(H12K,H12L,H12M),
 C129(H12N,H12O,H12P), C130(H13A,H13B,H13C), C133(H13D,H13E,H13F), C139(H13K,
 H13L,H13M), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F), C143(H14G,H14H,H14I),
 C145(H14J,H14K,H14L), C146(H14M,H14N,H14O), C147(H14P,H14Q,H14R), C149(H14S,
 H14T,H14U), C150(H15A,H15B,H15C), C151(H15D,H15E,H15F), C152(H15G,H15H,H15I),
 C155(H15J,H15K,H15L), C161(H16D,H16E,H16F), C163(H16G,H16H,H16I), C164(H16J,
 H16K,H16L), C165(H16M,H16N,H16O), C166(H16P,H16Q,H16R), C167(H16S,H16T,H16U),
 C169(H16V,H16W,H16X), C171(H17A,H17B,H17C), C181(H18A,H18B,H18C), C206(H20A,
 H20B,H20C), C16(H16Y,H,HA), C7(H7A,H7B,H7C), C1B(H1BA,H1BB,H1BC), C1D(H1DA,
 H1DB,H1DC), C1F(H1FA,H1FB,H1FC), C1H(H1HA,H1HB,H1HC), C1L(H1LA,H1LB,H1LC),
 C1N(H1NA,H1NB,H1NC), C40(H40A,H40B,H40C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48331
_shelx_hkl_checksum              54170
_shelx_fab_checksum              95043
_olex2_submission_special_instructions 'No special instructions were received'