Organometallic Uranium(V)-Imido Halide Complexes: From Synthesis to Electronic Structure and Bonding
Christopher R. Graves; Ping Yang; Stosh A. Kozimor; Anthony E. Vaughn; David L. Clark; Steven D. Conradson; Eric J. Schelter; Brian L. Scott; J. D. Thompson; P. Jeffrey Hay; David E. Morris; Jaqueline L. Kiplinger; Journal of the American Chemical Society 130 (2008) 5272–5285; doi:10.1021/ja711010h

data_4107683
_publ_contact_author_address
;
Los Alamos National Laboratory
Los Alamos, NM 87545
USA
;
_publ_contact_author_email       kiplinger@lanl.gov
_publ_contact_author_fax         '+1 505 667 9905'
_publ_contact_author_name        'Jaqueline L. Kiplinger'
_publ_contact_author_phone       '+1 505 665 9553'
_publ_section_title
;
 Organometallic Uranium(V)-Imido Halide Complexes: From Synthesis to
 Electronic Structure and Bonding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5272
_journal_page_last               5285
_journal_paper_doi               10.1021/ja711010h
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C32 H47 Br N U'
_chemical_formula_weight         763.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_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                   16.369(2)
_cell_length_b                   18.632(3)
_cell_length_c                   19.616(3)
_cell_measurement_temperature    141(2)
_cell_volume                     5982.6(15)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0922
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54287
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.782
_exptl_absorpt_correction_T_max  0.6864
_exptl_absorpt_correction_T_min  0.3749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.143
_refine_diff_density_min         -5.177
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.710
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5360
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      2.641
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.1124
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3655
_refine_ls_wR_factor_ref         0.3696
_reflns_number_gt                4523
_reflns_number_total             5360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711010h-file004_1.cif
_cod_data_source_block           apx449
_cod_original_cell_volume        5982.8(14)
_cod_database_code               4107683