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_1564603
_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         'C41 H47 K O4 U'
_chemical_formula_sum            'C41 H47 K O4 U'
_chemical_formula_weight         880.93
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-25
_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                90
_cell_angle_beta                 114.5220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7462(4)
_cell_length_b                   21.7085(6)
_cell_length_c                   13.7497(4)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.376
_cell_measurement_theta_min      2.485
_cell_volume                     3732.95(19)
_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      99.98
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30444
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         1.995
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.498
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0836 before and 0.0495 after correction. The Ratio of minimum to maximum transmission is 0.6808. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.479
_refine_diff_density_min         -1.541
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7630
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.386
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0911
_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^)+(0.0004P)^2^+94.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.1962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6291
_reflns_number_total             7630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03275e8.cif
_cod_data_source_block           1_THF
_cod_database_code               1564603
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.248
_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
 C40-C4AA \\sim C50-C4BA
 with sigma of 0.02
 C40-C32 \\sim C50-C2BA
 with sigma of 0.02
 C38-C2BA \\sim C32-C3AA
 with sigma of 0.02
 O16-C0AA \\sim O3-C4BA \\sim O8-C4AA \\sim O20-C5AA
 with sigma of 0.02
 C0AA-C0BA \\sim C50-C4BA \\sim C40-C4AA \\sim C6AA-C5AA
 with sigma of 0.02
 C1BA-C0BA \\sim C50-C2BA \\sim C40-C32 \\sim C6AA-C3BA
 with sigma of 0.02
 C38-C1BA \\sim C42-C2BA \\sim C32-C2AA \\sim C3AA-C3BA
 with sigma of 0.02
 O16-C38 \\sim O3-C42 \\sim O8-C2AA \\sim O20-C3AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: C7AA(0.5) H7Aa(0.5) H7Ab(0.5) O8(0.5) C2BA(0.5) H2Ba(0.5)
 H2Bb(0.5) C4BA(0.5) H4Ba(0.5) H4Bb(0.5) C4AA(0.5) H4Aa(0.5) H4Ab(0.5)
 C3AA(0.5) C32(0.5) H32a(0.5) H32b(0.5) C38(0.5) H38a(0.5) H38b(0.5) C40(0.5)
 H40a(0.5) H40b(0.5) C50(0.5) O3(0.5) C0BA(0.5) H0Ba(0.5) H0Bb(0.5) C1BA(0.5)
 H1Ba(0.5) H1Bb(0.5) O16(0.5) C0AA(0.5) H0Aa(0.5) H0Ab(0.5) O20(0.5) C3BA(0.5)
 C2AA(0.5) H2Aa(0.5) H2Ab(0.5) C5AA(0.5) C6AA(0.5) C42(0.5) O4AA(0.5) O3AA(0.5)
 C8AA(0.5) H8Aa(0.5) H8Ab(0.5) C9AA(0.5) H9Aa(0.5) H9Ab(0.5) C1AA(0.5)
 H1Aa(0.5) H1Ab(0.5)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C15(H15), C16(H16), C23(H23)
5.b Secondary CH2 refined with riding coordinates:
 C7AA(H7Aa,H7Ab), C2BA(H2Ba,H2Bb), C4BA(H4Ba,H4Bb), C4AA(H4Aa,H4Ab), C32(H32a,
 H32b), C38(H38a,H38b), C40(H40a,H40b), C0BA(H0Ba,H0Bb), C1BA(H1Ba,H1Bb),
 C0AA(H0Aa,H0Ab), C2AA(H2Aa,H2Ab), C8AA(H8Aa,H8Ab), C9AA(H9Aa,H9Ab), C1AA(H1Aa,
 H1Ab)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C6(H6), C11(H11), C8(H8), C20(H20), C18(H18), C10(H10), C9(H9),
 C21(H21), C28(H28), C26(H26), C25(H25), C27(H27), C19(H19)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c)
;
_shelx_res_checksum              3242
_shelx_hkl_checksum              41514
_olex2_submission_special_instructions 'No special instructions were received'