Thorium Oxo and Sulfido Metallocenes: Synthesis, Structure, Reactivity, and Computational Studies
Wenshan Ren; Guofu Zi; De-Cai Fang; Marc D. Walter; Journal of the American Chemical Society 133 (2011) 13183–13196; doi:10.1021/ja205280k

data_4106632
_publ_section_title
;
 Thorium Oxo and Sulfido Metallocenes: Synthesis, Structure, Reactivity,
 and Computational Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13183
_journal_page_last               13196
_journal_paper_doi               10.1021/ja205280k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C41 H68 N2 O Th'
_chemical_formula_sum            'C41 H68 N2 O Th'
_chemical_formula_weight         837.01
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.320(2)
_cell_angle_beta                 102.403(2)
_cell_angle_gamma                101.971(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8222(14)
_cell_length_b                   12.0686(14)
_cell_length_c                   16.1307(19)
_cell_measurement_reflns_used    2178
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.20
_cell_measurement_theta_min      2.31
_cell_volume                     1986.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0817
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10183
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.784
_exptl_absorpt_correction_T_max  0.6595
_exptl_absorpt_correction_T_min  0.4395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                6089
_reflns_number_total             7124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205280k_si_002_03.cif
_cod_data_source_block           compound10
_cod_database_code               4106632