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_1558296
_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 H64 N10 O4 U2, 3(C4 H8 O)'
_chemical_formula_sum            'C86 H88 N10 O7 U2'
_chemical_formula_weight         1849.72
_chemical_name_common            'Compound 1.3THF'
_chemical_name_systematic        '[{(py)U(OH)2U(O2C6H4)(py)}(LA)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 98.7581(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9463(3)
_cell_length_b                   24.3235(4)
_cell_length_c                   17.9675(3)
_cell_measurement_reflns_used    15123
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      25.2880
_cell_measurement_theta_min      3.0260
_cell_volume                     7319.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -45.00  53.00   1.00   45.00    --  -16.31  77.00-120.00   98
  2  \w    -25.00  24.00   1.00   45.00    --  -16.31 -99.00   0.00   49
  3  \w    -89.00  22.00   1.00   45.00    --  -16.31 -19.00-180.00  111
  4  \w    -25.00  24.00   1.00   45.00    --  -16.31 -99.00  30.00   49
  5  \w    -55.00  30.00   1.00   45.00    --  -16.31  95.00-165.75   85
  6  \w      0.00  86.00   1.00   45.00    --   18.03  57.00-180.00   86
  7  \w    -11.00  87.00   1.00   45.00    --   18.03  77.00   0.00   98
  8  \w      0.00  86.00   1.00   45.00    --   18.03  57.00 150.00   86
  9  \w    -20.00  90.00   1.00   45.00    --   18.03  19.00 -30.00  110
 10  \w      0.00  86.00   1.00   45.00    --   18.03  57.00  30.00   86
 11  \w    -91.00 -34.00   1.00   45.00    --  -16.31-179.00-120.00   57
 12  \w      6.00  82.00   1.00   45.00    --   18.03-139.00 107.28   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Enhance (Mo) X-ray Source'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74194
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.791
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       plate
_exptl_crystal_F_000             3656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF/hexanes'
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+30.2950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6009
_reflns_number_total             7484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        7319.77(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1558296
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              53220
_shelx_hkl_checksum              22618