Revisiting the Bis(dimethylamido) Metallocene Complexes of Thorium and Uranium: Improved Syntheses, Structure, Spectroscopy, and Redox Energetics of (C5Me5)2An(NMe2)2 (An = Th, U)
Erickson, Karla A.; Kagan, Benjamin D.; Scott, Brian; Morris , David; Kiplinger, Jaqueline; Dalton Trans.  (2017) –; doi:10.1039/C7DT02373A

data_7043900
_publ_section_title
;
 Revisiting the Bis(dimethylamido) Metallocene Complexes of Thorium and
 Uranium: Improved Syntheses, Structure, Spectroscopy, and Redox
 Energetics of (C5Me5)2An(NMe2)2 (An = Th, U)
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02373A
_journal_year                    2017
_chemical_formula_sum            'C31.5 H60 N2 Th'
_chemical_formula_weight         698.85
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-15 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.988(3)
_cell_length_b                   16.988(3)
_cell_length_c                   15.736(3)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.40
_cell_volume                     3932.9(12)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.596
_diffrn_reflns_theta_min         1.384
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.712
_exptl_absorpt_correction_T_max  0.334
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2.03 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       block
_exptl_crystal_F_000             2118
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.246
_refine_diff_density_max         2.942
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.470(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6467
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+4.6027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                5804
_reflns_number_total             6467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02373a1.cif
_cod_data_source_block           apx2357_sq
_cod_original_cell_volume        3933.0(15)
_cod_original_formula_sum        'C31.50 H60 N2 Th'
_cod_database_code               7043900
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.181
_shelx_estimated_absorpt_t_max   0.334
_shelx_res_checksum              98948
_shelx_fab_checksum              13821