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_4118063
_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         'C48 H58 Br N6 U, C6 H5 Cl, I3'
_chemical_formula_sum            'C54 H63 Br Cl I3 N6 U'
_chemical_formula_weight         1530.19
_chemical_name_common            apx1346
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                   14.5626(11)
_cell_length_b                   23.1936(18)
_cell_length_c                   36.780(3)
_cell_measurement_reflns_used    9529
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.21
_cell_volume                     12422.8(17)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEXII v7.0, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            122312
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    4.826
_exptl_absorpt_correction_T_max  0.6439
_exptl_absorpt_correction_T_min  0.3667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       blocks
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.521
_refine_diff_density_min         -3.263
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         13766
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.384
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                8971
_reflns_number_total             13766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2108432_si_006.cif
_cod_data_source_block           apx1346
_cod_database_code               4118063