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_4120818
_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 U2'
_chemical_formula_sum            'C96 H94 Cl2 N8 O6 U2'
_chemical_formula_weight         2002.75
_chemical_name_common            'Complex 2'
_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                 123.272(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.0738(14)
_cell_length_b                   23.6955(12)
_cell_length_c                   20.6036(11)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.29
_cell_volume                     11051.1(10)
_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 0.994
_diffrn_measured_fraction_theta_max 0.989
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37647
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.021
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.8164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      a
_exptl_crystal_description       needle
_exptl_crystal_F_000             3968
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         3.002
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         10080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                6768
_reflns_number_total             10080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407203s_si_002_2.cif
_cod_data_source_block           (2)
_cod_original_cell_volume        11051.0(10)
_cod_database_code               4120818