Probing the Chemistry, Electronic Structure and Redox Energetics in Organometallic Pentavalent Uranium Complexes
Christopher R. Graves; Anthony E. Vaughn; Eric J. Schelter; Brian L. Scott; Joe D. Thompson; David E. Morris; Jaqueline L. Kiplinger; Inorganic Chemistry 47 (2008) 11879–11891; doi:10.1021/ic8017375

data_4306818
_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_section_title
;
Probing the Chemistry, Electronic Structure and Redox Energetics in
Organometallic Pentavalent Uranium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11879
_journal_page_last               11891
_journal_paper_doi               10.1021/ic8017375
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C44 H57 N2 U'
_chemical_formula_weight         851.95
_chemical_name_systematic
; 
 ? 
;
_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                   13.314(4)
_cell_length_b                   16.936(5)
_cell_length_c                   32.812(9)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    141(2)
_cell_measurement_theta_max      25.9595
_cell_measurement_theta_min      2.3075
_cell_volume                     7399(4)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1177
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            81313
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.420
_exptl_absorpt_correction_T_max  0.8788
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.335
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                6218
_reflns_number_total             8423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8017375_si_002_2.cif
_cod_data_source_block           xpl07
_cod_original_cell_volume        7398(4)
_cod_database_code               4306818