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_1567950
_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         'C51 H73 N2 O Si U, C24 B F20, C7 H8'
_chemical_formula_sum            'C82 H81 B F20 N2 O Si U'
_chemical_formula_weight         1767.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.661(4)
_cell_length_b                   15.845(3)
_cell_length_c                   19.116(3)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.09
_cell_measurement_theta_min      2.49
_cell_volume                     8075(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1904
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            81186
_diffrn_reflns_point_group_measured_fraction_full 0.687
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.495
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6059
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       plate
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
; 
 Flack x determined using 1139 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.012(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         9775
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+1.2728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.331
_reflns_Friedel_fraction_full    0.354
_reflns_Friedel_fraction_max     0.354
_reflns_number_gt                6288
_reflns_number_total             9775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04302e2.cif
_cod_data_source_block           XA2_U_R_PhMe_cation
_cod_original_cell_volume        8076(2)
_cod_database_code               1567950
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              25864
_shelx_fab_checksum              12647