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_4087516
_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_formula_moiety         'C24 H24 N4 U1'
_chemical_formula_sum            'C24 H24 N4 U'
_chemical_formula_weight         606.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 113.6430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.85450(10)
_cell_length_b                   26.6410(5)
_cell_length_c                   10.0542(2)
_cell_measurement_reflns_used    15651
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.538
_cell_measurement_theta_min      1.529
_cell_volume                     2172.64(7)
_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    'DIRDIF/PATTY (Burskens, et. al,. 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.032
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15651
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.538
_diffrn_reflns_theta_min         1.529
_diffrn_source                   'fine focus tube'
_exptl_absorpt_coefficient_mu    7.488
_exptl_absorpt_correction_T_max  0.166
_exptl_absorpt_correction_T_min  0.016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.923
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4271
_reflns_number_total             6065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00212_si_003.cif
_cod_data_source_block           SAJ03
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087516
_shelx_estimated_absorpt_t_min   0.094
_shelx_estimated_absorpt_t_max   0.267
_shelxl_version_number           2013-4
_shelx_res_checksum              75885
_shelx_hkl_checksum              2600