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_4105198
_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            'C52 H58 K2 O2.5 U'
_chemical_formula_weight         1039.21
_chemical_name_systematic
; 
 Potassium tetrahydrofuran Uranium(IV) hexakis(benzyl) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 78.504(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.548(2)
_cell_length_b                   14.5329(10)
_cell_length_c                   19.1876(13)
_cell_measurement_temperature    150(2)
_cell_volume                     9440.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.1145
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79726
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    3.654
_exptl_absorpt_correction_T_max  0.336
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.529
_refine_diff_density_min         -2.941
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         17377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+384.7636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2492
_reflns_number_gt                10602
_reflns_number_total             17377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906516e_si_001_1.cif
_cod_data_source_block           Complex_5
_cod_original_cell_volume        9440.4(11)
_cod_database_code               4105198