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_1558299
_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         'C80 H66 B F N10 O5 U2, 3(C4 H10 O2)'
_chemical_formula_sum            'C92 H96 B F N10 O11 U2'
_chemical_formula_weight         2023.65
_chemical_name_common            'Compound 5A.3dme'
_chemical_name_systematic        '[{(py)U(u-F)(u-OBcat)U(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                77.518(2)
_cell_angle_beta                 78.699(2)
_cell_angle_gamma                82.007(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6146(3)
_cell_length_b                   16.3896(4)
_cell_length_c                   18.1536(4)
_cell_measurement_reflns_used    33672
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      32.3000
_cell_measurement_theta_min      3.4990
_cell_volume                     4141.91(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.926
_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    -78.00 -29.00   1.00   10.00    --  -17.68 133.00 -61.61   49
  2  \w    -92.00  14.00   1.00   10.00    --  -17.68 -77.00-150.00  106
  3  \w    -54.00  42.00   1.00   10.00    --   19.09 -38.00-120.00   96
  4  \w      3.00  75.00   1.00   10.00    --   19.09-127.00 116.48   72
  5  \w    -18.00  98.00   1.00   10.00    --   19.09  19.00  60.00  116
  6  \w    -12.00  93.00   1.00   10.00    --   19.09  77.00-180.00  105
  7  \w     -3.00  92.00   1.00   10.00    --   19.09  38.00 120.00   95
  8  \w    -55.00  50.00   1.00   10.00    --   19.09 -77.00   0.00  105
  9  \w    -76.00 -27.00   1.00   10.00    --  -17.68 130.00 124.61   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            105405
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.951
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dimethoxyethane'
_exptl_crystal_size_max          0.612
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.820
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         28789
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+6.2134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21060
_reflns_number_total             28789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound5A
_cod_database_code               1558299
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.201
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              43468
_shelx_hkl_checksum              92061