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_7130399
_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         'C24 H72 I2 N12 O4 P4 U, I'
_chemical_formula_sum            'C24 H72 I3 N12 O4 P4 U'
_chemical_formula_weight         1334.03
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-11
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.336(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.823(2)
_cell_length_b                   26.037(2)
_cell_length_c                   16.7292(15)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.41
_cell_volume                     9673.1(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43529
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.205
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.443
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0926 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.7750.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       plate
_exptl_crystal_F_000             5132
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.222
_refine_diff_density_min         -2.399
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         15499
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0509P)^2^+70.5465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14617
_reflns_number_total             15499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03238d2.cif
_cod_data_source_block           Complex_2
_cod_depositor_comments
;

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H141 I6 N24 O8 P8 U2'
_cod_original_formula_weight         2668.06
_cod_original_formula_moiety         '2(C24 H72 I2 N12 O4 P4 U), 2(I)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        9673.2(15)
_cod_database_code               7130399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.219
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H10A,H10B,H10C} of C10
 At 1.5 times of:
  {H2A,H2B,H2C} of C2, {H35A,H35B,H35C} of C35, {H39A,H39B,H39C} of C39,
  {H33A,H33B,H33C} of C33, {H31A,H31B,H31C} of C31, {H19A,H19B,H19C} of C19,
  {H4A,H4B,H4C} of C4, {H6A,H6B,H6C} of C6, {H27A,H27B,H27C} of C27, {H23A,H23B,
  H23C} of C23, {H20A,H20B,H20C} of C20, {H14A,H14B,H14C} of C14, {H24A,H24B,
  H24C} of C24, {H17A,H17B,H17C} of C17, {H48A,H48B,H48C} of C48, {H38A,H38B,
  H38C} of C38, {H7A,H7B,H7C} of C7, {H32A,H32B,H32C} of C32, {H15A,H15B,H15C}
  of C15, {H8A,H8B,H8C} of C8, {H22A,H22B,H22C} of C22, {H29A,H29B,H29C} of C29,
   {H34A,H34B,H34C} of C34, {H1A,H1B,H1C} of C1, {H36A,H36B,H36C} of C36, {H13A,
  H13B,H13C} of C13, {H9A,H9B,H9C} of C9, {H3A,H3B,H3C} of C3, {H11A,H11B,H11C}
  of C11, {H16A,H16B,H16C} of C16, {H47A,H47B,H47C} of C47, {H28A,H28B,H28C} of
  C28, {H25A,H25B,H25C} of C25, {H45A,H45B,H45C} of C45, {H5A,H5B,H5C} of C5,
  {H40A,H40B,H40C} of C40, {H26A,H26B,H26C} of C26, {H41A,H41B,H41C} of C41,
  {H46A,H46B,H46C} of C46, {H30A,H30B,H30C} of C30, {H43A,H43B,H43C} of C43,
  {H42A,H42B,H42C} of C42, {H44A,H44B,H44C} of C44, {H12A,H12B,H12C} of C12,
  {H21A,H21B,H21C} of C21, {H18A,H18B,H18C} of C18, {H37A,H37B,H37C} of C37
2. Uiso/Uaniso restraints and constraints
C4 \\sim N1 \\sim C3: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C10(H10A,H10B,
 H10C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C44(H44A,H44B,H44C), C30(H30A,
 H30B,H30C), C40(H40A,H40B,H40C), C5(H5A,H5B,H5C), C42(H42A,H42B,H42C),
 C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C26(H26A,H26B,H26C), C47(H47A,H47B,
 H47C), C38(H38A,H38B,H38C), C22(H22A,H22B,H22C), C11(H11A,H11B,H11C), C29(H29A,
 H29B,H29C), C36(H36A,H36B,H36C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C3(H3A,H3B,
 H3C), C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C34(H34A,H34B,H34C), C7(H7A,
 H7B,H7C), C32(H32A,H32B,H32C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C25(H25A,
 H25B,H25C), C28(H28A,H28B,H28C), C45(H45A,H45B,H45C), C27(H27A,H27B,H27C),
 C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C24(H24A,H24B,H24C), C17(H17A,H17B,
 H17C), C14(H14A,H14B,H14C), C48(H48A,H48B,H48C), C2(H2A,H2B,H2C), C6(H6A,H6B,
 H6C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C33(H33A,H33B,H33C), C31(H31A,
 H31B,H31C), C19(H19A,H19B,H19C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              22072
_olex2_submission_special_instructions 'No special instructions were received'