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_1558302
_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 H62 N10 O2 Se2 U2, 2(C H2 Cl2)'
_chemical_formula_sum            'C76 H66 Cl4 N10 O2 Se2 U2'
_chemical_formula_weight         1927.16
_chemical_name_common            'Compound 4.2CH2Cl2'
_chemical_name_systematic        '[{(py)U(u-Se2)U(u-O2C6H4)(py)}(LA)]'
_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   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                90
_cell_angle_beta                 92.935(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9153(2)
_cell_length_b                   19.1212(4)
_cell_length_c                   34.2194(6)
_cell_measurement_reflns_used    34327
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1310
_cell_measurement_theta_min      3.1080
_cell_volume                     7132.7(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.0521
_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    -25.00  23.00   1.00   30.00    --  -14.31 -99.00  30.00   48
  2  \w    -80.00   1.00   1.00   30.00    --  -14.31 -57.00   0.00   81
  3  \w    -85.00 -34.00   1.00   30.00    --  -14.31-179.00   0.00   51
  4  \w    -80.00   1.00   1.00   30.00    --  -14.31 -57.00 -90.00   81
  5  \w    -25.00  23.00   1.00   30.00    --  -14.31 -99.00 150.00   48
  6  \w     -1.00  85.00   1.00   30.00    --   16.03  37.00   0.00   86
  7  \w     -1.00  85.00   1.00   30.00    --   16.03  37.00 -60.00   86
  8  \w     34.00  86.00   1.00   30.00    --   16.03 179.00-150.00   52
  9  \w    -52.00  34.00   1.00   30.00    --   16.03 -37.00-180.00   86
 10  \w    -29.00  51.00   1.00   30.00    --  -14.31  57.00 -30.00   80
 11  \w    -32.00  54.00   1.00   30.00    --  -14.31  37.00 -60.00   86
 12  \w    -29.00  51.00   1.00   30.00    --  -14.31  57.00  30.00   80
 13  \w     -2.00  50.00   1.00   30.00    --   16.03-126.00 178.68   52
;
_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  0.0851
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            133959
_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         25.350
_diffrn_reflns_theta_min         2.834
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.999
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             3712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/hexanes'
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         13030
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0214P)^2^+39.6362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10932
_reflns_number_total             13030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1558302
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.999
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              39980
_shelx_hkl_checksum              47979
_shelx_fab_checksum              44930