Uranium(iv) alkyl cations: synthesis, structures, comparison with thorium(iv) analogues, and the influence of arene-coordination on thermal stability and ethylene polymerization activity
Andreychuk, Nicholas R.; Vidjayacoumar, Balamurugan; Price, Jeffrey S.; Kervazo, Sophie; Peeples, Craig A.; Emslie, David J. H.; Vallet, Valérie; Gomes, André S. P.; Réal, Florent; Schreckenbach, Georg; Ayers, Paul W.; Vargas-Baca, Ignacio; Jenkins, Hilary A.; Britten, James F.; Chemical Science  (2022) –; doi:10.1039/D2SC04302E

data_1567949
_publ_section_title
;
 Uranium(iv) alkyl cations: synthesis, structures, comparison with
 thorium(iv) analogues, and the influence of arene-coordination on thermal
 stability and ethylene polymerization activity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04302E
_journal_year                    2022
_chemical_formula_moiety         'C61 H76 N2 O U, C4 H8 O'
_chemical_formula_sum            'C65 H84 N2 O2 U'
_chemical_formula_weight         1163.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-08-03 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                80.8830(10)
_cell_angle_beta                 79.2670(10)
_cell_angle_gamma                84.4930(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5747(8)
_cell_length_b                   12.7230(8)
_cell_length_c                   20.5456(14)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.598
_cell_measurement_theta_min      2.321
_cell_volume                     2928.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50599
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.218
_diffrn_reflns_theta_min         1.795
_exptl_absorpt_coefficient_mu    2.814
_exptl_absorpt_correction_T_max  0.8693
_exptl_absorpt_correction_T_min  0.5263
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.066
_refine_diff_density_max         2.381
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         21180
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16628
_reflns_number_total             21180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04302e2.cif
_cod_data_source_block           XA2_U_dibenzyl
_cod_database_code               1567949
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.492
_shelx_estimated_absorpt_t_max   0.836
_shelx_res_checksum              49378