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_7718641
_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         'C40 H60 Cl2 O Th2, C7 H8'
_chemical_formula_sum            'C47 H68 Cl2 O Th2'
_chemical_formula_weight         1183.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-04-30
_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                90
_cell_angle_beta                 102.809(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7012(16)
_cell_length_b                   9.9014(6)
_cell_length_c                   17.2407(11)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.39
_cell_volume                     4611.1(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15575
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.191
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.590
_exptl_absorpt_correction_T_max  0.430474
_exptl_absorpt_correction_T_min  0.324933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 174389 reflections, Rint = 0.0499
 (116761 with I > 3sig(I), Rint = 0.0445)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       shard
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.797
_refine_diff_density_min         -2.246
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         15575
_refine_ls_number_restraints     391
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0079P)^2^+130.3884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14665
_reflns_number_total             15575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00855g2.cif
_cod_data_source_block           s1
_cod_depositor_comments
'Adding full bibliography for 7718641--7718643.cif.'
_cod_database_code               7718641
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.559
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6062(11)
 0.3938(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C10S-C11S = C6S-C11S = C10S-C9S = C7S-C6S
 1.48 with sigma of 0.02
 C6S-C11S \\sim C7S-C6S \\sim C9S-C8S \\sim C7S-C8S \\sim C10S-C11S \\sim
C10S-C9S
 with sigma of 0.02
 C2S_$1-C1S \\sim C2S-C1S \\sim C2S-C1S_$1 \\sim C2S_$1-C1S_$1
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C4)
Uanis(C34) = Uanis(C15)
Uanis(C3) = Uanis(C22)
Uanis(C8) = Uanis(C27)
Uanis(C31) = Uanis(C11)
Uanis(C30) = Uanis(C9)
Uanis(C5) = Uanis(C22)
5. Rigid body (RIGU) restrains
 C1, C1S, C2, C2S, C3, C3S, C4, C4S, C5, C5S, C6, C6S, C7, C7S, C8, C9S, C9,
 C10S, C10, C11S, C11, C12S, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21,
 C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37,
  C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6S, C7S, C9S, C10S, C11S, C12S, C8S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1S(0.5) H1S(0.5) H2S(0.25) H2SA(0.25) C3S(0.5) H3S(0.5) H4S(0.5)
 H4SA(0.5) H4SB(0.5) H4SC(0.5) C5S(0.5) H5S(0.5) C6S(0.5) C7S(0.5) H7S(0.5)
 C9S(0.5) H9S(0.5) C10S(0.5) H10S(0.5) C11S(0.5) H11S(0.5) C12S(0.5) H12A(0.5)
 H12B(0.5) H12C(0.5) C8S(0.5) H8S(0.5)
7.a Riding coordinates:
 C1S(H1S), C2S(H2S,H2SA), C3S(H3S), C4S(H4S,H4SA,H4SB,H4SC)
7.b Aromatic/amide H refined with riding coordinates:
 C5S(H5S), C7S(H7S), C9S(H9S), C10S(H10S), C11S(H11S), C8S(H8S)
7.c Idealised Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C12S(H12A,H12B,H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), 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              77316
_shelx_hkl_checksum              31945
_olex2_submission_special_instructions 'No special instructions were received'