Actinide Metals with Multiple Bonds to Carbon: Synthesis, Characterization, and Reactivity of U(IV) and Th(IV) Bis(iminophosphorano)methandiide Pincer Carbene Complexes
Guibin Ma; Michael J. Ferguson; Robert McDonald; Ronald G. Cavell; Inorganic Chemistry 50 (2011) 6500–6508; doi:10.1021/ic102537q

data_4325583
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton, Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       ron.cavell@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr. Ronald G. Cavell'
_publ_contact_author_phone       1(780)4925310
_publ_section_title
;
 Actinide Metals with Multiple Bonds to Carbon: Synthesis,
 Characterization, and Reactivity of U(IV) and Th(IV)
 Bis(iminophosphorano)methandiide Pincer Carbene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6500
_journal_page_last               6508
_journal_paper_doi               10.1021/ic102537q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C64 H79 Cl4 N5 P4 Si4 U2, 2(C6 H14)'
_chemical_formula_sum            'C76 H107 Cl4 N5 P4 Si4 U2'
_chemical_formula_weight         1944.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   45.586(4)
_cell_length_b                   45.586(4)
_cell_length_c                   21.7302(17)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.32
_cell_volume                     39107(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            112353
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    4.015
_exptl_absorpt_correction_T_max  0.5222
_exptl_absorpt_correction_T_min  0.2771
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             17388
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.187
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         19943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                14958
_reflns_number_total             19943
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102537q_si_002_6.cif
_cod_data_source_block           9
_cod_original_cell_volume        39107(5)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4325583