A Direct Route to Bis(imido)uranium(V) Halides via Metathesis of Uranium Tetrachloride
Robert E. Jilek; Liam P. Spencer; Richard A. Lewis; Brian L. Scott; Trevor W. Hayton; James M. Boncella; Journal of the American Chemical Society 134 (2012) 9876–9878; doi:10.1021/ja2108432

data_4118062
_publ_section_title
;
 A Direct Route to Bis(imido)uranium(V) Halides via Metathesis of Uranium
 Tetrachloride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9876
_journal_page_last               9878
_journal_paper_doi               10.1021/ja2108432
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C60 H82 I N6 U'
_chemical_formula_sum            'C60 H82 I N6 U'
_chemical_formula_weight         1252.25
_chemical_name_common            apx1206
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_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                 111.9440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3846(17)
_cell_length_b                   26.537(3)
_cell_length_c                   18.940(2)
_cell_measurement_reflns_used    3633
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.48
_cell_measurement_theta_min      2.16
_cell_volume                     6706.0(13)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEXII v7.0, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1106
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64701
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    2.916
_exptl_absorpt_correction_T_max  0.7211
_exptl_absorpt_correction_T_min  0.4749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         12266
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                7972
_reflns_number_total             12266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2108432_si_005.cif
_cod_data_source_block           apx1206
_cod_original_cell_volume        6706.1(14)
_cod_database_code               4118062