Dioxygen reacts with metal-carbon bonds in thorium dialkyls to produce bis(alkoxides).
Settineri, Nicholas S.; Shiau, Angela A.; Arnold, John; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5569–5573; doi:10.1039/c9dt00811j

data_7049502
_publ_section_title
;
 Dioxygen reacts with metal-carbon bonds in thorium dialkyls to produce
 bis(alkoxides).
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5569
_journal_page_last               5573
_journal_paper_doi               10.1039/c9dt00811j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H62 Cl3 Li N6 Si4 Th, C7 H8'
_chemical_formula_sum            'C39 H70 Cl3 Li N6 Si4 Th'
_chemical_formula_weight         1080.70
_chemical_name_systematic        Th(BTBA)2Cl3Li(TMEDA)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-21 deposited with the CCDC.    2019-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.474(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8563(10)
_cell_length_b                   12.1439(6)
_cell_length_c                   23.6059(13)
_cell_measurement_reflns_used    9095
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.415
_cell_measurement_theta_min      2.423
_cell_volume                     5126.9(5)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76942
_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         25.428
_diffrn_reflns_theta_min         1.815
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.190
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0680 before and 0.0340 after correction. The Ratio of minimum to maximum transmission is 0.8516. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       Block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+6.4868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8745
_reflns_number_total             9424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00811j2.cif
_cod_data_source_block           Th(BTBA)2Cl3Li(TMEDA)
_cod_depositor_comments
'Adding full bibliography for 7049498--7049503.cif.'
_cod_database_code               7049502
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.701
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C33A) = Uanis(C33B)
Uanis(C34) = Uanis(C40)
Uanis(C37A) = Uanis(C37B)
Uanis(C38A) = Uanis(C38B)
Uanis(C41A) = Uanis(C41B)
Uanis(C36) = Uanis(C39)
3. Rigid body (RIGU) restrains
 C33B, C36, C37B, C40, C41B, C42, C38B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C33A, C34, C35, C37A, C38A, C39, C41A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C33B)=Sof(H33B)=Sof(H33C)=Sof(H33D)=Sof(C36)=Sof(C37B)=Sof(H37B)=
 Sof(C38B)=Sof(H38B)=Sof(C40)=Sof(H40)=Sof(C42)=Sof(H42)=Sof(C41B)=Sof(H41D)=1-
 FVAR(1)
 Sof(C33A)=Sof(H33A)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C37A)=Sof(H37A)=
 Sof(C38A)=Sof(H38A)=Sof(C39)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C33A(H33A), C34(H34), C35(H35), C37A(H37A), C38A(H38A),
 C37B(H37B), C38B(H38B), C40(H40), C42(H42), C41B(H41D)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C41A(H41A,H41B,H41C), C33B(H33B,H33C,H33D)
;
_shelx_res_checksum              33883
_olex2_submission_special_instructions 'No special instructions were received'