Synthesis and Characterization of Thorium(IV) and Uranium(IV) Corrole Complexes
Ashleigh L. Ward; Heather L. Buckley; Wayne W. Lukens; John Arnold; Journal of the American Chemical Society 135 (2013) 13965–13971; doi:10.1021/ja407203s

data_4120817
_publ_section_title
;
 Synthesis and Characterization of Thorium(IV) and Uranium(IV) Corrole
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13965
_journal_page_last               13971
_journal_paper_doi               10.1021/ja407203s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C96 H94 Cl2 N8 O6 Th2'
_chemical_formula_sum            'C96 H94 Cl2 N8 O6 Th2'
_chemical_formula_weight         1990.77
_chemical_name_common            'Complex 1'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 123.790(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.5585(9)
_cell_length_b                   23.3363(9)
_cell_length_c                   20.8898(7)
_cell_measurement_reflns_used    8938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.33
_cell_volume                     10760.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0910
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29024
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    2.858
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.8036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      a
_exptl_crystal_description       needle
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         3.230
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                6307
_reflns_number_total             9629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407203s_si_002_1.cif
_cod_data_source_block           (1)
_cod_database_code               4120817