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_4106638
_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         'C246 H384 S18 Th6'
_chemical_formula_sum            'C246 H384 S18 Th6'
_chemical_formula_weight         5310.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   35.843(2)
_cell_length_b                   35.843(2)
_cell_length_c                   18.753(2)
_cell_measurement_reflns_used    2525
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.36
_cell_measurement_theta_min      2.27
_cell_volume                     20865(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1685
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8310
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    3.374
_exptl_absorpt_correction_T_max  0.6316
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       Block
_exptl_crystal_F_000             8064
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         3.095
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.765
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         8310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.765
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                4654
_reflns_number_total             8310
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205280k_si_002_09.cif
_cod_data_source_block           compound17
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4106638