Reactivity of a dithorium oxo complex from adventitious water.
Mahawar, Pritam; Kelley, Steven P.; Walensky, Justin R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8706–8711; doi:10.1039/d5dt00855g

data_7718642
_publ_section_title
;
 Reactivity of a dithorium oxo complex from adventitious water.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8706
_journal_page_last               8711
_journal_paper_doi               10.1039/d5dt00855g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C64 H82 N4 O Th2, 2(C4 H10 O)'
_chemical_formula_sum            'C72 H102 N4 O3 Th2'
_chemical_formula_weight         1535.65
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-04-30 deposited with the CCDC.	2025-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                86.192(2)
_cell_angle_beta                 72.698(2)
_cell_angle_gamma                84.387(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1491(6)
_cell_length_b                   14.3177(6)
_cell_length_c                   17.8937(8)
_cell_measurement_reflns_used    9004
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      29.29
_cell_measurement_theta_min      2.25
_cell_volume                     3198.4(2)
_computing_cell_refinement       'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_data_collection       'Bruker Apex4 V.2022.1-1'
_computing_data_reduction        'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Photon II CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            94596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.570
_diffrn_reflns_theta_min         2.732
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.694
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.443
_refine_diff_density_min         -1.765
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         17888
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+18.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13019
_reflns_number_total             17888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00855g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7718641--7718643.cif.'
_cod_database_code               7718642
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.603
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H64,H4,H2} of C64, All C(H,H) groups
 At 1.5 times of:
  {H28A,H28B,H28C} of C28, {H19A,H19B,H19C} of C19, {H29A,H29B,H29C} of C29,
  {H17A,H17B,H17C} of C17, {H18A,H18B,H18C} of C18, {H20A,H20B,H20C} of C20,
  {H38A,H38B,H38C} of C38, {H37A,H37B,H37C} of C37, {H30A,H30B,H30C} of C30,
  {H39A,H39B,H39C} of C39, {H26A,H26B,H26C} of C26, {H16A,H16B,H16C} of C16,
  {H27A,H27B,H27C} of C27, {H36A,H36B,H36C} of C36, {H40A,H40B,H40C} of C40,
  {H1SA,H1SB,H1SC} of C1S, {H9A,H9B,H9C} of C9, {H6A,H6B,H6C} of C6, {H7A,H7B,
  H7C} of C7, {H10A,H10B,H10C} of C10, {H8A,H8B,H8C} of C8, {H4SA,H4SB,H4SC} of
  C4S
2. Restrained distances
 N2-H2 = N4-H4
 0.92 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB)
3.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
3.c Idealised Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
3.d Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C),
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              67332
_shelx_hkl_checksum              14168
_shelx_fab_checksum              67060
_olex2_submission_special_instructions 'No special instructions were received'