In Pursuit of Homoleptic Actinide Alkyl Complexes
Lani A. Seaman; Justin R. Walensky; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 52 (2013) 3556–3564; doi:10.1021/ic300867m

data_4334247
_publ_section_title
;
 In Pursuit of Homoleptic Actinide Alkyl Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3556
_journal_page_last               3564
_journal_paper_doi               10.1021/ic300867m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C50 H58 K2 O2 Th'
_chemical_formula_weight         1001.20
_chemical_name_systematic        'Th benzyl'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_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                 93.604(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.341(3)
_cell_length_b                   29.955(7)
_cell_length_c                   16.497(4)
_cell_measurement_temperature    273(2)
_cell_volume                     4607(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37828
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         0.68
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.6254
_exptl_absorpt_correction_T_min  0.1960
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.475
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.502(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         17029
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.535
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.5767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                13060
_reflns_number_total             17029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300867m_si_002_2.cif
_cod_data_source_block           complex3
_cod_depositor_comments
;
 Marking atoms 'C94A', 'C96A', 'C97A' as belonging to the disorder group 1
 and atoms 'C94B', 'C95B', 'C97B' as belonging to the disorder group 2
 after consulting the original publication.

 Antanas Vaitkus,
 2016-12-21

 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-21
;
_cod_database_code               4334247