Thorium(IV) and Uranium(IV) Halide Complexes Supported by Bulky β-Diketiminate Ligands
Monreal, Marisa J.; Wright, Robert J.; Morris, David E.; Scott, Brian L.; Golden, Jeffery T.; Power, Philip P.; Kiplinger, Jaqueline L.; Organometallics 32 (2013) 1423–; doi:10.1021/om3010965

data_4080343
_publ_section_title
;
 Thorium(IV) and Uranium(IV) Halide Complexes Supported by Bulky
 \b-Diketiminate Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1423
_journal_paper_doi               10.1021/om3010965
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C41 H60 Br2 N2 Th'
_chemical_formula_weight         972.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.52
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.62080(10)
_cell_length_b                   20.3151(2)
_cell_length_c                   18.8606(2)
_cell_measurement_temperature    140(1)
_cell_volume                     3921.03(7)
_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      140(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30776
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.871
_exptl_absorpt_correction_T_max  0.2552
_exptl_absorpt_correction_T_min  0.2401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.472
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.472
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0493
_reflns_number_gt                6645
_reflns_number_total             7139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010965_si_002.cif
_cod_data_source_block           apx008
_cod_original_cell_volume        3920.99(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080343