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_7249690
_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 O38 Th6'
_chemical_formula_sum            'C84 H60 O38 Th6'
_chemical_formula_weight         3069.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 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                 134.903(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.309(3)
_cell_length_b                   17.216(2)
_cell_length_c                   17.1830(19)
_cell_measurement_reflns_used    9316
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.91
_cell_volume                     5093.5(11)
_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 0.997
_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  0.0799
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            140529
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.320
_diffrn_reflns_theta_min         2.366
_exptl_absorpt_coefficient_mu    8.805
_exptl_absorpt_correction_T_max  0.20292
_exptl_absorpt_correction_T_min  0.05827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.629
_exptl_crystal_size_mid          0.499
_exptl_crystal_size_min          0.202
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     1303
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0271P)^2^+122.1121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6237
_reflns_number_total             6514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01042f2.cif
_cod_data_source_block           B22272_0m_a
_cod_depositor_comments
'Adding full bibliography for 7249690--7249692.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7249690
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.072
_shelx_estimated_absorpt_t_max   0.269
_shelx_res_checksum              22404
_shelx_hkl_checksum              7489