Catalytic regeneration of a Th-H bond from a Th-O bond through a mild and chemoselective carbonyl hydroboration.
Ghatak, Tapas; Makarov, Konstantin; Fridman, Natalia; Eisen, Moris S.; Chemical communications (Cambridge, England) 54 (2018) 11001–11004; doi:10.1039/c8cc05030a

data_7122284
_publ_section_title
;
 Catalytic regeneration of a Th-H bond from a Th-O bond through a mild and
 chemoselective carbonyl hydroboration.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11001
_journal_page_last               11004
_journal_paper_doi               10.1039/c8cc05030a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C37 H76 N6 Si6 Th'
_chemical_formula_sum            'C37 H76 N6 Si6 Th'
_chemical_formula_weight         1005.62
_chemical_name_common            'Moris520 (Tapas)'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-08-21 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 123.219(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.619(6)
_cell_length_b                   11.246(2)
_cell_length_c                   28.548(9)
_cell_measurement_reflns_used    7628
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      1.31
_cell_volume                     5001(3)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Mercury 3.7'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            7439
_diffrn_reflns_theta_full        24.14
_diffrn_reflns_theta_max         24.14
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.156
_exptl_absorpt_correction_T_max  0.9113
_exptl_absorpt_correction_T_min  0.4829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.482
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7439
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+74.0921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                6121
_reflns_number_total             7439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc05030a2.cif
_cod_data_source_block           Moris520
_cod_depositor_comments
'Adding full bibliography for 7122283--7122284.cif.'
_cod_original_cell_volume        5001(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7122284