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_4325581
_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         'C40 H48 B Cl N8 P2 Si2 U'
_chemical_formula_sum            'C40 H48 B Cl N8 P2 Si2 U'
_chemical_formula_weight         1043.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   10.5116(9)
_cell_length_b                   18.3976(15)
_cell_length_c                   22.7622(19)
_cell_measurement_reflns_used    7524
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.23
_cell_volume                     4401.9(6)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37610
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.914
_exptl_absorpt_correction_T_max  0.3337
_exptl_absorpt_correction_T_min  0.2547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881. 4413 Friedel pairs.'
_refine_ls_abs_structure_Flack   0.000(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         10014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0196
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0437
_reflns_number_gt                9521
_reflns_number_total             10014
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102537q_si_002_4.cif
_cod_data_source_block           7
_cod_database_code               4325581