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_4087519
_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         'C64 H72 O8 U2'
_chemical_formula_sum            'C32 H36 O4 U'
_chemical_formula_weight         722.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8917(6)
_cell_length_b                   7.5254(2)
_cell_length_c                   18.6598(8)
_cell_measurement_reflns_used    37949
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      72.186
_cell_measurement_theta_min      6.288
_cell_volume                     2793.24(16)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not 
cusp data but mostly high angle data.
Also the use of HKL3000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total.
;
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37949
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.186
_diffrn_reflns_theta_min         6.288
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    16.628
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.189
_refine_diff_density_min         -2.444
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0534
_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^)+(0.1307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1997
_reflns_number_total             2709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00212_si_005.cif
_cod_data_source_block           SAJ08
_cod_database_code               4087519
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.136
_shelx_estimated_absorpt_t_max   0.635
_shelx_res_checksum              82094
_shelx_hkl_checksum              91150