Elucidating trends in synthesis and structural periodicity in a series of tetravalent actinide–oxo hexamers
McCusker, Thomas L.; Vanagas, Nicole A.; Szymanowski, Jennifer E. S.; Surbella, Robert G.; Bertke, Jeffery A.; Arteaga, Ana; Knope, Karah E.; CrystEngComm 27 (2025) 507–515; doi:10.1039/D4CE01042F

data_7249691
_publ_section_title
;
 Elucidating trends in synthesis and structural periodicity in a series of
 tetravalent actinide--oxo hexamers
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              507
_journal_page_last               515
_journal_paper_doi               10.1039/D4CE01042F
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C84 H60 O36 Pu6'
_chemical_formula_sum            'C84 H60 O36 Pu6'
_chemical_formula_weight         3097.32
_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_hydrogens   geom
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-09-30 deposited with the CCDC.	2024-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.628(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.805(7)
_cell_length_b                   24.801(17)
_cell_length_c                   23.813(12)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.80
_cell_volume                     9289(9)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2018-3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1471
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            154499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.324
_diffrn_reflns_theta_min         1.819
_exptl_absorpt_coefficient_mu    4.279
_exptl_absorpt_correction_T_max  0.0075
_exptl_absorpt_correction_T_min  0.0005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5664
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.636
_refine_diff_density_min         -1.693
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1338
_refine_ls_number_reflns         16844
_refine_ls_number_restraints     2088
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0295P)^2^+289.4830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11572
_reflns_number_total             16844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01042f2.cif
_cod_data_source_block           p21onn_a_sq
_cod_depositor_comments
'Adding full bibliography for 7249690--7249692.cif.'
_cod_original_cell_volume        9290(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7249691
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.742
_shelx_res_checksum              2679
_shelx_hkl_checksum              21323
_shelx_fab_checksum              39167