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_4087518
_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         'C40 H52 U1'
_chemical_formula_sum            'C40 H52 U'
_chemical_formula_weight         770.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_atom_sites_solution_hydrogens   mixed
_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            2
_cell_length_a                   13.7754(4)
_cell_length_b                   13.7754(4)
_cell_length_c                   9.2246(4)
_cell_measurement_reflns_used    7156
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.869
_cell_measurement_theta_min      3.208
_cell_volume                     1750.48(10)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.974
_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  0.050
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7156
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.869
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    13.211
_exptl_absorpt_correction_T_max  0.180
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       cube
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(2)
_refine_ls_extinction_coef       0.00065(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0673P)^2^+2.9902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.857
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                2101
_reflns_number_total             2925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00212_si_002.cif
_cod_data_source_block           SAJ01
_cod_original_cell_volume        1750.48(13)
_cod_database_code               4087518
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.242
_shelx_estimated_absorpt_t_max   0.242
_shelx_res_checksum              59293
_shelx_hkl_checksum              17384