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_1564602
_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         'C30 H62 I4 O9 U2'
_chemical_formula_sum            'C30 H62 I4 O9 U2'
_chemical_formula_weight         1550.48
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-18
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4373(19)
_cell_length_b                   17.215(2)
_cell_length_c                   9.3631(12)
_cell_measurement_reflns_used    9508
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      2.82
_cell_volume                     2327.1(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
_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 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0326
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26741
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.630
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.643
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1379 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.5763. The \l/2 correction factor is 0.0015.'
_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    2.218
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF,  Hexans'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.051
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+8.4379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2848
_reflns_number_total             3438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03275e8.cif
_cod_data_source_block           Complex_2
_cod_original_cell_volume        2327.2(5)
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               1564602
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.446
_shelx_estimated_absorpt_t_min   0.249
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1C(0.5) H1A(0.5) H1B(0.5) C2AA(0.25) O0AA(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7B,H7A), C6(H6A,H6B), C4(H4A,H4B), C5(H5B,H5A), C2(H2B,H2A), C3(H3B,H3A)
3.b Idealised Me refined as rotating group:
 C1(H1C,H1A,H1B)
;
_shelx_res_checksum              41215
_shelx_hkl_checksum              50962
_olex2_submission_special_instructions 'No special instructions were received'