Selective Oxo Ligand Functionalisation and Substitution Reactivity in an Oxo/Catecholate-Bridged UIV/UIV Pacman Complex
Cowie, Bradley E.; Douair, Iskander; Laurent, Maron; Love, Jason; Arnold, Polly Louise; Chemical Science  (2020) –; doi:10.1039/D0SC02297G

data_1558301
_publ_section_title
;
 Selective Oxo Ligand Functionalisation and Substitution Reactivity in an
 Oxo/Catecholate-Bridged UIV/UIV Pacman Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02297G
_journal_year                    2020
_chemical_formula_moiety         'C74 H63 N10 O2 S2 U2, 5(C5 H5 N)'
_chemical_formula_sum            'C99 H88 N15 O2 S2 U2'
_chemical_formula_weight         2060.02
_chemical_name_common            'Compound 3.5py'
_chemical_name_systematic        '[{(py)U(S2)U(O2C6H4)(py)}(LA)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                77.6190(10)
_cell_angle_beta                 85.4690(10)
_cell_angle_gamma                88.9250(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7332(2)
_cell_length_b                   17.5327(3)
_cell_length_c                   18.0598(3)
_cell_measurement_reflns_used    43178
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.7370
_cell_measurement_theta_min      3.2090
_cell_volume                     4234.03(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -35.00  54.00   1.00   25.00    --  -15.66  37.00-180.00   89
  2  \w    -42.00  52.00   1.00   25.00    --  -15.66  77.00 -30.00   94
  3  \w    -35.00  54.00   1.00   25.00    --  -15.66  37.00 -90.00   89
  4  \w    -83.00  11.00   1.00   25.00    --  -15.66 -77.00-150.00   94
  5  \w    -60.00  16.00   1.00   25.00    --  -15.66 109.00 -54.10   76
  6  \w      1.00  85.00   1.00   25.00    --   17.38  57.00  90.00   84
  7  \w     34.00  90.00   1.00   25.00    --   17.38 179.00   0.00   56
  8  \w     -9.00  85.00   1.00   25.00    --   17.38  77.00 120.00   94
  9  \w    -88.00 -34.00   1.00   25.00    --  -15.66-179.00 -30.00   54
 10  \w    -25.00  23.00   1.00   25.00    --  -15.66 -99.00 -30.00   48
 11  \w     -2.00  87.00   1.00   25.00    --   17.38  37.00 -30.00   89
 12  \w      3.00  77.00   1.00   25.00    --   17.38-135.00 134.17   74
 13  \w    -25.00  56.00   1.00   25.00    --   17.38 -99.00 -60.00   81
 14  \w    -25.00  56.00   1.00   25.00    --   17.38 -99.00-180.00   81
 15  \w    -69.00   4.00   1.00   25.00    --  -15.66 124.00 132.87   73
 16  \w    -64.00  11.00   1.00   25.00    --  -15.66 115.00 177.32   75
 17  \w    -65.00  10.00   1.00   25.00    --  -15.66 117.00 -26.25   75
 18  \w    -16.00  62.00   1.00   25.00    --   17.38-109.00  -2.05   78
 19  \w     34.00  90.00   1.00   25.00    --   17.38 179.00-180.00   56
 20  \w      1.00  85.00   1.00   25.00    --   17.38  57.00  30.00   84
 21  \w    -25.00  23.00   1.00   25.00    --  -15.66 -99.00-120.00   48
 22  \w    -68.00   5.00   1.00   25.00    --  -15.66 123.00  90.84   73
 23  \w    -52.00  87.00   1.00   25.00    --   17.38   0.00-180.00  139
 24  \w    -52.00  24.00   1.00   25.00    --   17.38   0.00-150.00   76
 25  \w     -2.00  87.00   1.00   25.00    --   17.38  37.00-120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            142230
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.395
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent orange'
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             2038
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridine/hexanes'
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.757
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.765
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         58720
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.765
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0121P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33537
_reflns_number_total             58720
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9034\% 
 around [0.00 0.71 0.71] (reciprocal) or [-0.09 0.73 0.68] (direct)
;
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound3
_cod_database_code               1558301
_shelx_shelxl_version_number     2018/3
_oxdiff_twin_items               2
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              28256
_shelx_hkl_checksum              11350