Evidence for the Involvement of 5f Orbitals in the Bonding and Reactivity of Organometallic Actinide Compounds: Thorium(IV) and Uranium(IV) Bis(hydrazonato) Complexes
Thibault Cantat; Christopher R. Graves; Kimberly C. Jantunen; Carol J. Burns; Brian L. Scott; Eric J. Schelter; David E. Morris; P. Jeffrey Hay; Jaqueline L. Kiplinger; Journal of the American Chemical Society 130 (2008) 17537–17551; doi:10.1021/ja8067287

data_4108877
_publ_section_title
;
 Evidence for the Involvement of 5f Orbitals in the Bonding and Reactivity
 of Organometallic Actinide Compounds: Thorium(IV) and Uranium(IV)
 Bis(hydrazonato) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17537
_journal_page_last               17551
_journal_paper_doi               10.1021/ja8067287
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C51 H63 N4 Th'
_chemical_formula_weight         964.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 101.422(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.104(5)
_cell_length_b                   19.452(5)
_cell_length_c                   13.778(4)
_cell_measurement_temperature    203(2)
_cell_volume                     4493(2)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       '\f 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27647
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.356
_exptl_absorpt_correction_T_max  0.6888
_exptl_absorpt_correction_T_min  0.4131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.228
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7958
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                6714
_reflns_number_total             7958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8067287_si_002_4.cif
_cod_data_source_block           ccd782a
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4108877