Homoleptic Uranium(IV) Alkyl Complexes: Synthesis and Characterization
Skye Fortier; Brent C. Melot; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 131 (2009) 15512–15521; doi:10.1021/ja906516e

data_4105199
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
 Homoleptic Uranium(IV) Alkyl Complexes: Synthesis and Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15512
_journal_page_last               15521
_journal_paper_doi               10.1021/ja906516e
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C68 H163 Cl Li14 O12 Si5 U'
_chemical_formula_weight         1684.07
_chemical_name_systematic
; 
 Uranium(IV) pentakis(methylenetrimethylsilane)
 lithium dodecakis(tert-butoxide) chloride 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   10.9396(8)
_cell_length_b                   28.544(2)
_cell_length_c                   32.502(2)
_cell_measurement_temperature    150(2)
_cell_volume                     10149.1(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.1120
_diffrn_reflns_av_sigmaI/netI    0.1067
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            82136
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         0.95
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            bright_green
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         21304
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                14833
_reflns_number_total             21304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906516e_si_001_2.cif
_cod_data_source_block           Complex_1
_cod_original_cell_volume        10149.1(13)
_cod_database_code               4105199