Actinide arene-metalates: Ion pairing effects on the electronic structure of unsupported uranium-arenide sandwich complexes
Murillo, Jesse; Bhowmick, Rina; Harriman, Katie L. M.; Gomez-Torres, Alejandra; Wright, Joshua; Meulenberg, Robert W.; Miro Ramirez, Pere; Metta-Magana, Alejandro J Jose; Murugesu, Muralee; Vlaisavljevich, Bess; Fortier, Skye; Chemical Science  (2021) –; doi:10.1039/D1SC03275E

data_1564604
_publ_section_title
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 Actinide arene-metalates: Ion pairing effects on the electronic structure
 of unsupported uranium-arenide sandwich complexes&#x00A0;
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03275E
_journal_year                    2021
_chemical_formula_moiety
'C58 H46 O2 U2, C20 H38 K O8, C20 H40 K O8, 2(C4 H8 O), 2(C4 O)'
_chemical_formula_sum            'C114 H158 K2 O22 U2'
_chemical_formula_weight         2434.76
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-15 deposited with the CCDC.	2021-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                67.675(2)
_cell_angle_beta                 89.666(2)
_cell_angle_gamma                86.887(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3767(3)
_cell_length_b                   17.8147(5)
_cell_length_c                   18.3562(6)
_cell_measurement_reflns_used    9709
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.26
_cell_volume                     3133.91(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1777
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            140060
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.392
_diffrn_reflns_theta_min         2.025
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.706
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1270 before and 0.0833 after correction. The Ratio of minimum to maximum transmission is 0.7760. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             1222
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.246
_refine_diff_density_min         -1.947
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         15465
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+6.7912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11505
_reflns_number_total             15465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03275e8.cif
_cod_data_source_block           1_18C6_4_THF
_cod_database_code               1564604
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.774
_shelx_estimated_absorpt_t_min   0.411
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1AA-C1BA \\sim O1AA-C7AA \\sim O6AA-C46 \\sim O6AA-C6AA
 with sigma of 0.02
 C7AA-C0AA \\sim C3AA-C1BA \\sim C9AA-C46 \\sim C8AA-C6AA \\sim C6BA_$1-C4AA_$1
 with sigma of 0.02
 C4AA-C2AA \\sim C9AA_$1-C8AA_$1 \\sim C3AA_$1-C0AA_$1
 with sigma of 0.02
3. Others
 Fixed Sof: C7AA(0.5) H7AA(0.5) H7AB(0.5) C8AA(0.5) H8AA(0.5) H8AB(0.5)
 C9AA(0.5) H9AA(0.5) H9AB(0.5) C1BA(0.5) H1BA(0.5) H1BB(0.5) C3AA(0.5)
 H3AA(0.5) H3AB(0.5) C0AA(0.5) H20A(0.5) H20B(0.5) C46(0.5) H46A(0.5) H46B(0.5)
 O6AA(0.5) C4AA(0.5) C6BA(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) C2AA(0.5)
 O1AA(0.5) C0BA(0.5) C3BA(0.5) C2BA(0.5) C5BA(0.5) C7BA(0.5) O12(0.5) O22(0.5)
4.a Ternary CH refined with riding coordinates:
 C22(H22), C15(H15), C4(H4), C1(H1A), C2(H2), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C37(H37A,H37B), C41(H41A,H41B), C39(H39A,H39B), C40(H40A,
 H40B), C38(H38A,H38B), C019(H01I,H01J), C01B(H01K,H01L), C33(H33A,H33B),
 C32(H32A,H32B), C36(H36A,H36B), C35(H35A,H35B), C01K(H01A,H01B), C34(H34A,
 H34B), C31(H31A,H31B), C01N(H01C,H01D), C01O(H01E,H01F), C01P(H01G,H01H),
 C7AA(H7AA,H7AB), C8AA(H8AA,H8AB), C9AA(H9AA,H9AB), C1BA(H1BA,H1BB), C3AA(H3AA,
 H3AB), C0AA(H20A,H20B), C46(H46A,H46B), C6AA(H6AA,H6AB)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C13(H13), C6(H6), C26(H26), C24(H24), C25(H25), C20(H20), C11(H11),
 C17(H17), C8(H8), C19(H19), C18(H18), C10(H10), C9(H9)
4.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              26463
_shelx_hkl_checksum              20809
_olex2_submission_special_instructions 'No special instructions were received'