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_7135385
_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
'2(C160 H187 N5 O6 S Se), 6.5(C H Cl3), 4(C2 H3 N)'
_chemical_formula_sum            'C334.5 H392.5 Cl19.5 N14 O12 S2 Se2'
_chemical_formula_weight         5714.42
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-06-24
_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                99.146(11)
_cell_angle_beta                 105.50(4)
_cell_angle_gamma                97.73(3)
_cell_formula_units_Z            1
_cell_length_a                   19.264(12)
_cell_length_b                   21.682(9)
_cell_length_c                   22.237(12)
_cell_measurement_reflns_used    4572
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.2
_cell_measurement_theta_min      0.573
_cell_volume                     8682(8)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'EIGER 4M DECTRIS'
_diffrn_measurement_method       'Phi scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.1130
_diffrn_reflns_Laue_measured_fraction_full 0.804
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32531
_diffrn_reflns_point_group_measured_fraction_full 0.632
_diffrn_reflns_point_group_measured_fraction_max 0.632
_diffrn_reflns_theta_full        32.300
_diffrn_reflns_theta_max         32.300
_diffrn_reflns_theta_min         1.362
_diffrn_source                   'SPring-8 BL26B1'
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       needle
_exptl_crystal_F_000             3025
_exptl_crystal_recrystallization_method 'recrystallization from CHCl3/MeCN'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 8905 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.090(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2942
_refine_ls_number_reflns         28041
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1724P)^2^+3.0741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2367
_reflns_Friedel_coverage         0.572
_reflns_Friedel_fraction_full    0.460
_reflns_Friedel_fraction_max     0.460
_reflns_number_gt                26170
_reflns_number_total             28041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06999h2.cif
_cod_data_source_block           BpscSec-SePTU-ProProOMe
_cod_original_formula_sum        'C334.50 H392.50 Cl19.50 N14 O12 S2 Se2'
_cod_database_code               7135385
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.930
_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
 C101-C82
 1.514 with sigma of 0.1
 C82-C101
 1.514 with sigma of 0.1
 C4-C82A
 1.514 with sigma of 0.1
 Cl21-C57 \\sim Cl23-C57 \\sim Cl22-C57
 with sigma of 0.1
 C053-C0AI \\sim C053-C2
 with sigma of 0.02
 C17-C09M \\sim C0AV-C09M
 with sigma of 0.1
 O092-C77 \\sim O0-C77A
 with sigma of 0.02
 C07K-O092 \\sim C07K-O0
 with sigma of 0.02
 C07K-C77 \\sim C07K-C77A
 with sigma of 0.04
 C82-C101 \\sim C82A-C4
 with sigma of 0.02
 C0AT-C82 \\sim C0AT-C82A
 with sigma of 0.04
 C035-C093 \\sim C035-C7
 with sigma of 0.02
 C06Y-C093 \\sim C06Y-C7
 with sigma of 0.02
 C50-C09M \\sim C0AR-C09M
 with sigma of 0.1
 Cl5-C1 \\sim Cl3-C1 \\sim Cl6-C1
 with sigma of 0.1
 C053-C09E \\sim C053-C3
 with sigma of 0.02
 C0AT-C101 \\sim C0AT-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C0A2) = Uanis(C0AW)
Uanis(C09M) = Uanis(C0AV) = Uanis(C17)
Uanis(C35) = Uanis(C08A) = Uanis(C08Y)
Uanis(C02I) = Uanis(C01E) = Uanis(C04F) = Uanis(C082) = Uanis(C05Y) =
Uanis(C05K)
Uanis(C82) = Uanis(C101) = Uanis(C0AT)
Uiso(C4) = Uiso(C82A)
Uanis(C08F) = Uanis(C23A) = Uanis(C0)
Uanis(C0AL) = Uanis(C0AM) = Uanis(C08T)
Uanis(C08U) = Uanis(C0AW)
Uanis(C081) = Uanis(C02L) = Uanis(C01T) = Uanis(C023)
Uanis(C081) = Uanis(C08S) = Uanis(C09V)
Uanis(C050) = Uanis(C06D)
Uanis(C038) = Uanis(C02J) = Uanis(C01G) = Uanis(C01T) = Uanis(C023) =
Uanis(C02L)
Uanis(C025) = Uanis(C01P) = Uanis(C03T) = Uanis(C069) = Uanis(C05W) =
Uanis(C04E)
Uanis(C09T) = Uanis(C08B) = Uanis(C095)
Uanis(C08X) = Uanis(C071) = Uanis(C0A6)
Uanis(C02Z) = Uanis(C02B) = Uanis(C032) = Uanis(C01M) = Uanis(C02G) =
Uanis(C030)
Uanis(C00T) = Uanis(C016) = Uanis(C043) = Uanis(C02D)
Uanis(C02Y) = Uanis(C084) = Uanis(C05D) = Uanis(C068) = Uanis(C03W) =
Uanis(C04P)
Uanis(C010) = Uanis(C02P) = Uanis(C01J) = Uanis(C01R) = Uanis(C01V) =
Uanis(C019)
Uanis(C03Q) = Uanis(C029) = Uanis(C04O) = Uanis(C01H)
Uanis(C04Q) = Uanis(C027) = Uanis(C048)
Uanis(C093) = Uanis(C06Y) = Uanis(C035)
Uanis(C08K) = Uanis(C065) = Uanis(C04I)
Uanis(C01L) = Uanis(C03Q) = Uanis(C01H) = Uanis(C029) = Uanis(C04O) =
Uanis(C04B)
Uanis(C02H) = Uanis(C01F) = Uanis(C021) = Uanis(C018) = Uanis(C00V) =
Uanis(C01X)
Uanis(C0A1) = Uanis(C090) = Uanis(C086)
Uanis(C03I) = Uanis(C022) = Uanis(C01N) = Uanis(C00W) = Uanis(C04S) =
Uanis(C04J)
Uanis(Cl11) = Uanis(Cl9) = Uanis(Cl10)
Uanis(Cl23) = Uanis(Cl21) = Uanis(Cl22)
Uanis(Cl22) = Uanis(Cl21) = Uanis(Cl23)
Uanis(C057) = Uanis(C09P) = Uanis(C09K)
Uanis(C0AI) = Uanis(C09E)
Uanis(C06I) = Uanis(C047) = Uanis(C03O) = Uanis(C03N) = Uanis(C063) =
Uanis(C089)
Uanis(C07E) = Uanis(C07S) = Uanis(C056) = Uanis(C026) = Uanis(C03X) =
Uanis(C06E)
Uanis(C077) = Uanis(C05A) = Uanis(C085) = Uanis(C07W) = Uanis(C06D) =
Uanis(C050)
4. Rigid body (RIGU) restrains
 O092, C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C77A, O0
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C08W, C05N
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(H05A)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=1-FVAR(1)
 Sof(H053)=Sof(C09E)=Sof(H09I)=Sof(H09J)=Sof(H09K)=Sof(C0AI)=Sof(H0AP)=
 Sof(H0AQ)=Sof(H0AR)=FVAR(1)
 Sof(H58)=Sof(C0AR)=Sof(H34)=Sof(H83)=Sof(H84)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=1-FVAR(2)
 Sof(H18)=Sof(C0AV)=Sof(H35)=Sof(H87)=Sof(H88)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=FVAR(2)
 Sof(H0AX)=Sof(H0AY)=Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=1-FVAR(3)
 Sof(H0AV)=Sof(H0AW)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C101)=
 Sof(H10A)=Sof(H10B)=FVAR(3)
 Sof(O0)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=1-FVAR(4)
 Sof(O092)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=FVAR(4)
 Sof(H03C)=Sof(H03D)=Sof(HG)=Sof(HH)=Sof(C7)=Sof(H7A)=Sof(H7B)=1-FVAR(5)
 Sof(H03A)=Sof(H03B)=Sof(H06V)=Sof(H06Y)=Sof(C093)=Sof(H09D)=Sof(H09E)=FVAR(5)
 Fixed Sof: Cl22(0.5) Cl21(0.5) Cl23(0.5) C57(0.5) H57(0.5)
6.a Ternary CH refined with riding coordinates:
 C02A(H02A), C02Q(H02Q), C02U(H02U), C036(H036), C03J(H03J), C042(H042),
 C044(H044), C04A(H04A), C04N(H04N), C04R(H04R), C051(H051), C053(H053),
 C053(H05A), C057(H057), C05B(H05K), C05C(H05C), C05E(H05L), C05O(H05R),
 C05P(H05T), C06A(H1), C06P(H4), C06U(H06U), C06W(H06W), C071(H071), C072(H072),
  C07N(H07N), C07V(H07V), C07X(H07Z), C080(H080), C081(H081), C083(H083),
 C088(H088), C08A(H08O), C08B(H08Q), C08D(H08U), C08F(H08G), C08J(H08K),
 C08P(H08P), C08U(H8), C09C(H42), C09M(H58), C09M(H18), C09O(H43), C0AJ(H44),
 C0AS(H41), C57(H57), C1(H1A)
6.b Secondary CH2 refined with riding coordinates:
 C035(H03A,H03B), C035(H03C,H03D), C061(H06,H), C064(H06A,H06B), C06J(H06H,
 H06J), C06K(H06K,H06L), C06M(H06M,H06N), C06Y(H06V,H06Y), C06Y(HG,HH),
 C08Z(H12,HW), C093(H09D,H09E), C09F(H14,H50), C09R(H19,H60), C09Z(H24,H67),
 C0A2(H26,H70), C0AT(H0AV,H0AW), C0AT(H0AX,H0AY), C0AW(H36,H89), C101(H10A,
 H10B), C15(H15A,H15B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B)
6.c Me refined with riding coordinates:
 C06L(H3,HC,HD), C08Y(H11,HU,HV), C0AV(H35,H87,H88), C26(H26A,H26B,H26C),
 C77(H77A,H77B,H77C), C82(H82A,H82B,H82C), C2(H2A,H2B,H2C), C82A(H82D,H82E,
 H82F), C77A(H77D,H77E,H77F)
6.d Aromatic/amide H refined with riding coordinates:
 N00U(H00U), C00V(H00V), C00X(H00X), N012(H012), C017(H017), C019(H019),
 C01B(H01B), C01D(H01D), C01H(H01H), C01K(H01K), C01M(H01M), C01N(H01N),
 C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C020(H020),
 C021(H021), C024(H024), C02B(H02F), C02C(H02G), C02D(H02D), C02E(H02H),
 C02H(H02I), C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M), C02P(H02P),
 C02R(H02R), C02V(H02V), C02W(H02W), C02X(H02X), C030(H030), C03A(H03E),
 C03F(H03F), C03I(H03I), C03K(H03K), C03L(H03L), C03M(H03M), C03Q(H03Q),
 C03R(H03R), C03T(H03T), C03U(H03U), C03W(H03W), C040(H040), C047(H047),
 C04I(H04I), C04J(H04J), C04O(H04O), C04P(H04P), C04V(H04V), C04Z(H04Z),
 C058(H058), C059(H059), C05A(H05J), C05F(H05M), C05I(H05I), C05K(H05N),
 C05S(H05S), C05W(H05X), C05X(H05Y), C05Y(H05Z), C062(H062), C065(H065),
 C068(H068), C069(H069), C06E(H06E), C06F(H06F), C06I(H06I), N06X(H06X),
 C06Z(H06Z), C075(H075), C076(H076), C077(H077), C07B(H07O), C07E(H07G),
 C07G(H07W), C07I(H07X), C07P(H07P), C07S(H07S), C07T(H07T), C082(H082),
 C085(H085), C089(H089), C08K(H08Y), C08L(H08Z), C08M(H08), C08T(H7),
 C090(H090), N096(H096), C09S(H20), C09X(H23), C0AL(H30), C0AM(H31)
6.e Idealised Me refined as rotating group:
 C02T(H02B,H02C,H02E), C04W(H04B,H04C,H04D), C05J(H05B,H05D,H05E), C05N(H05O,
 H05P,H05Q), C05Q(H05U,H05V,H05W), C05T(H05F,H05G,H05H), C06B(H2,HA,HB),
 C06H(H06C,H06D,H06G), C06R(H06O,H06P,H06Q), C06S(H5,HE,HF), C06T(H06R,H06S,
 H06T), C070(H07K,H07L,H07M), C073(H07A,H07B,H07C), C074(H07D,H07E,H07F),
 C07D(H07Q,H07R,H07U), C07M(H07Y,HI,HJ), C07U(H07H,H07I,H07J), C07Z(H07,HK,HL),
 C087(H08A,H08B,H08C), C08C(H08R,H08S,H08T), C08E(H08D,H08E,H08F), C08H(H08H,
 H08I,H08J), C08I(H08V,H08W,H08X), C08Q(H08L,H08M,H08N), C08R(H39,HM,HN),
 C08S(H6,HO,HP), C08W(H9,HQ,HR), C08X(H10,HS,HT), C091(H09A,H09B,H09C),
 C094(H38,HX,HY), C095(H09,HZ,H45), C097(H13,H46,H47), C098(H37,H48,H49),
 C09B(H09F,H09G,H09H), C09E(H09I,H09J,H09K), C09H(H15,H51,H52), C09I(H16,H53,
 H54), C09J(H17,H55,H56), C09K(H09L,H09M,H09N), C09L(H09O,H09P,H09Q), C09N(H09R,
 H09S,H09T), C09P(H09U,H09V,H09W), C09Q(H09X,H09Y,H59), C09T(H21,H61,H62),
 C09U(H09Z,H63,H64), C09V(H22,H65,H66), C0A0(H25,H68,H69), C0A3(H0AA,H0AB,H0AC),
  C0A5(H0AD,H0AE,H0AF), C0A6(H27,H71,H72), C0A9(H0AG,H0AH,H0AI), C0AB(H40,H73,
 H74), C0AD(H0AJ,H0AK,H0AL), C0AE(H28,H75,H76), C0AF(H0AM,H0AN,H0AO), C0AI(H0AP,
 H0AQ,H0AR), C0AK(H29,H77,H78), C0AN(H32,H79,H80), C0AO(H0AS,H0AT,H0AU),
 C0AQ(H33,H81,H82), C0AR(H34,H83,H84), C0AU(H0AZ,H85,H86), C35(H35A,H35B,H35C),
 C50(H50A,H50B,H50C), C0(H0A,H0B,H0C), C23A(H23A,H23B,H23C), C3(H3A,H3B,H3C),
 C17(H17A,H17B,H17C), C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44232
_shelx_hkl_checksum              98128
_shelx_fab_checksum              23196
_olex2_submission_special_instructions 'No special instructions were received'