Unusual bonding situations in Th(iv) and U(iv)–Al(iii) pnictogen complexes
Mahawar, Pritam; Wang, Ganping; Ward, Robert J.; Kelley, Steven P.; Maron, Laurent; Walensky, Justin R.; Chemical Science  (2026) –; doi:10.1039/D5SC09143H

data_1576911
_publ_section_title
;
 Unusual bonding situations in Th(iv) and U(iv)-Al(iii) pnictogen
 complexes.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              9158
_journal_page_last               9167
_journal_paper_doi               10.1039/d5sc09143h
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C48 H67 Al As2 Th, 0.5(C5 H12)'
_chemical_formula_sum            'C50.5 H73 Al As2 Th'
_chemical_formula_weight         1088.94
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Radioactive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-09-30
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_audit_update_record
;
2025-11-10 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                89.331(3)
_cell_angle_beta                 73.603(3)
_cell_angle_gamma                74.673(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7863(16)
_cell_length_b                   15.317(2)
_cell_length_c                   15.579(2)
_cell_measurement_reflns_used    5758
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      22.93
_cell_measurement_theta_min      2.25
_cell_volume                     2375.8(6)
_computing_cell_refinement       'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_data_collection       'Bruker Apex3 V.2016.9-0'
_computing_data_reduction        'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33447
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.643
_diffrn_reflns_theta_min         1.366
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1836 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.7805.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1090
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether, pentane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.821
_refine_diff_density_min         -2.402
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9967
_refine_ls_number_restraints     675
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0773P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6614
_reflns_number_total             9967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc09143h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1576910--1576917.cif.'
_cod_original_cell_volume        2375.9(6)
_cod_original_formula_sum        'C50.50 H73 Al As2 Th'
_cod_database_code               1576911
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.555
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2. Others
 Fixed Sof: H3SA(0.5) H3SB(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5)
 C5S(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) C4S(0.5)
 H4SA(0.5) H4SB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C2S(H2SA,H2SB), C4S(H4SA,H4SB)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C5(H5), C12(H12), C3(H3)
3.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C34(H34A,H34B,
 H34C), C48(H48A,H48B,H48C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C), C24(H24A,
 H24B,H24C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C35(H35A,H35B,H35C),
 C45(H45A,H45B,H45C), C25(H25A,H25B,H25C), C44(H44A,H44B,H44C), C18(H18A,H18B,
 H18C), C46(H46A,H46B,H46C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C47(H47A,
 H47B,H47C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C1S(H1SA,H1SB,H1SC),
 C5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              12382
_olex2_submission_special_instructions 'No special instructions were received'