New Benzylpotassium Reagents and Their Utility for the Synthesis of Homoleptic Uranium(IV) Benzyl Derivatives
Johnson, Sara A.; Kiernicki, John J.; Fanwick, Phillip E.; Bart, Suzanne C.; Organometallics 34 (2015) 2889–; doi:10.1021/acs.organomet.5b00212

data_4087520
_publ_section_title
;
 New Benzylpotassium Reagents and Their Utility for the Synthesis of
 Homoleptic Uranium(IV) Benzyl Derivatives
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2889
_journal_paper_doi               10.1021/acs.organomet.5b00212
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C176 H240 U4'
_chemical_formula_sum            'C44 H60 U'
_chemical_formula_weight         826.95
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3339(6)
_cell_length_b                   16.3339(6)
_cell_length_c                   7.2540(5)
_cell_measurement_reflns_used    7962
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.244
_cell_measurement_theta_min      2.494
_cell_volume                     1935.34(17)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7962
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.244
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    4.221
_exptl_absorpt_correction_T_max  0.363
_exptl_absorpt_correction_T_min  0.051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2323
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+9.1458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1998
_reflns_number_total             2323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00212_si_006.cif
_cod_data_source_block           SAJ02
_cod_original_cell_volume        1935.34(19)
_cod_database_code               4087520
_shelx_estimated_absorpt_t_min   0.364
_shelx_estimated_absorpt_t_max   0.431
_shelxl_version_number           2013-4
_shelx_res_checksum              7015
_shelx_hkl_checksum              23450