Actinide arene-metalates: 2. A neutral uranium bis(anthracenide) sandwich complex and elucidation of its electronic structure
Murillo, Jesse; Bhowmick, Rina; Harriman, Katie L. M.; Gomez-Torres, Alejandra; Wright, Joshua; Miró, Pere; Metta-Magaña, Alejandro; Murugesu, Muralee; Vlaisavljevich, Bess; Fortier, Skye; Chemical Communications  (2022) –; doi:10.1039/D2CC03238D

data_7130401
_publ_section_title
;
 Actinide arene-metalates: 2. A neutral uranium bis(anthracenide) sandwich
 complex and elucidation of its electronic structure
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03238D
_journal_year                    2022
_chemical_formula_moiety         '2(C38 H45.5 N3 O2 P U), 2(C4 H8 O), C6 H14'
_chemical_formula_sum            'C90 H121 N6 O6 P2 U2'
_chemical_formula_weight         1920.92
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.291(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3829(7)
_cell_length_b                   20.2202(16)
_cell_length_c                   19.4228(13)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.90
_cell_volume                     4076.7(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (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 0.994
_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  0.1605
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88042
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         2.812
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.064
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1008 before and 0.0713 after correction. The Ratio of minimum to maximum transmission is 0.7289. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1930
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.461
_refine_diff_density_min         -3.278
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9433
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0742
_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^)+(0.0001P)^2^+73.8156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6565
_reflns_number_total             9433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03238d2.cif
_cod_data_source_block           3_THF_Hexane
_cod_database_code               7130401
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.375
_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
 O2-C6AA \\sim O2-C4AA
 with sigma of 0.02
 C4AA-C3AA \\sim C6AA-C3BA
 with sigma of 0.02
 C3AA-C2BA \\sim C8AA-C3BA
 with sigma of 0.02
 C8AA-C5AA \\sim C1AA-C2BA
 with sigma of 0.02
 O2-C5AA \\sim O2-C1AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C17) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: C4AA(0.5) H4AA(0.5) H4AB(0.5) C8AA(0.5) H8AA(0.5) H8AB(0.5)
 C2BA(0.5) H2BA(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5) C1AA(0.5) H1AA(0.5)
 H1AB(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5)
 C3BA(0.5) H3BA(0.5) H3BB(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C20(H20), C17(H17)
5.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C(HA,HB), C2AA(H2AA,H2AB), C1BA(H1BA,H1BB), C4AA(H4AA,H4AB),
 C8AA(H8AA,H8AB), C5AA(H5AA,H5AB), C1AA(H1AA,H1AB), C6AA(H6AA,H6AB), C3AA(H3AA,
 H3AB), C3BA(H3BA,H3BB), C0BA(H0BA,H0BB), C9AA(H9AA,H9AB)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C14(H14), C12(H12), C11(H11), C21(H21), C13(H13), C10(H10), C7(H7),
 C22(H22), C8(H8), C23(H23), C24(H24), C28(H28), C27(H27), C26(H26), C25(H25)
5.d Idealised Me refined as rotating group:
 C4BA(H4BA,H4BB,H4BC), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C7AA(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              62534
_olex2_submission_special_instructions 'No special instructions were received'