Systematic Studies of Early Actinide Complexes: Thorium(IV) Fluoroketimides
Eric J. Schelter; Ping Yang; Brian L. Scott; Ryan E. Da Re; Kimberly C. Jantunen; Richard L. Martin; P. Jeffrey Hay; David E. Morris; Jaqueline L. Kiplinger; Journal of the American Chemical Society 129 (2007) 5139–5152; doi:10.1021/ja0686458

data_4109326
_publ_contact_author
;
Jaqueline L. Kiplinger
MS J514
Los Alamos National Laboratory
Los Alamos, New Mexico 87545
;
_publ_contact_author_email       kiplinger@lanl.gov
_publ_section_title
;
 Systematic Studies of Early Actinide Complexes: Thorium(IV)
 Fluoroketimides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5139
_journal_page_last               5152
_journal_paper_doi               10.1021/ja0686458
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '(C5(CH3)5)2 Th (NC(CH3)(C6F5))2'
_chemical_formula_sum            'C36 H36 F10 N2 Th'
_chemical_formula_weight         918.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.066(3)
_cell_length_b                   16.393(3)
_cell_length_c                   26.997(5)
_cell_measurement_reflns_used    8815
_cell_measurement_temperature    141(2)
_cell_measurement_theta_max      52.307
_cell_measurement_theta_min      4.657
_cell_volume                     7110(2)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w 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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            53982
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.275
_exptl_absorpt_correction_T_max  0.8147
_exptl_absorpt_correction_T_min  0.4819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         8877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+4.1558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                5259
_reflns_number_total             8877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0686458si20070120_043048_7.cif
_cod_data_source_block           c:\apx272\test\pccn-1\pccn-1
_cod_database_code               4109326