The U=C Double Bond: Synthesis and Study of Uranium Nucleophilic Carbene Complexes
Thibault Cantat; Thérèse Arliguie; Anne Noël; Pierre Thuéry; Michel Ephritikhine; Pascal Le Floch; Nicolas Mézailles; Journal of the American Chemical Society 131 (2009) 963–972; doi:10.1021/ja807282s

data_4103798
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       ephri@drecam.cea.fr
_publ_contact_author_fax         '33 (0) 1 69 08 66 40'
_publ_contact_author_name        'M. Ephritikhine'
_publ_contact_author_phone       '33 (0) 1 69 08 64 36'
_publ_section_title
;
 The U=C Double Bond: Synthesis and Study of Uranium Nucleophilic Carbene
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              963
_journal_page_last               972
_journal_paper_doi               10.1021/ja807282s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C104 H104 Li2 O2 P6 S6 U'
_chemical_formula_weight         2015.96
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   29.658(2)
_cell_length_b                   21.8217(11)
_cell_length_c                   29.9635(15)
_cell_measurement_reflns_used    291978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.96
_cell_volume                     19392.0(19)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'one \f and five \w scans with 2\% steps'
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            291978
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             8224
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.258
_refine_diff_density_min         -2.447
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         18300
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0889
_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^)+(0.0630P)^2^+38.6880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2266
_reflns_number_gt                12201
_reflns_number_total             18300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807282s_si_001_1.cif
_cod_data_source_block           6.3toluene
_cod_database_code               4103798