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_1558300
_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         'C75.69 H67.06 N10 O4 U2, C6 H6'
_chemical_formula_sum            'C81.69 H73.06 N10 O4 U2'
_chemical_formula_weight         1734.84
_chemical_name_common            'Compound 2.C6H6'
_chemical_name_systematic        '[{(py)U(OMe)1.69(OH)0.31U(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                90.546(4)
_cell_angle_beta                 102.195(5)
_cell_angle_gamma                94.113(5)
_cell_formula_units_Z            2
_cell_length_a                   10.6363(6)
_cell_length_b                   14.9997(8)
_cell_length_c                   21.8493(12)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.2020
_cell_measurement_theta_min      3.2610
_cell_volume                     3397.3(3)
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -87.00 -32.00   1.00   30.00    --  -16.53 179.00 120.00   55
  2  \w    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 -30.00   45
  3  \w    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 120.00   45
  4  \w    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 150.00   45
  5  \w    -25.00  20.00   1.00   30.00    --  -16.53 -99.00 -90.00   45
  6  \w    -34.00  52.00   1.00   30.00    --  -16.53  37.00  90.00   86
  7  \w    -25.00  55.00   1.00   30.00    --   18.25 -99.00 150.00   80
  8  \w    -47.00  33.00   1.00   30.00    --   18.25 -57.00-120.00   80
  9  \w    -51.00  88.00   1.00   30.00    --   18.25   0.00  90.00  139
 10  \w    -34.00  52.00   1.00   30.00    --  -16.53  37.00   0.00   86
 11  \w    -25.00  20.00   1.00   30.00    --  -16.53 -99.00  60.00   45
 12  \w      3.00  84.00   1.00   30.00    --   18.25  57.00 -90.00   81
 13  \w      3.00  72.00   1.00   30.00    --   18.25  57.00 120.00   69
 14  \w    -25.00  55.00   1.00   30.00    --   18.25 -99.00   0.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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  0.1173
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.862
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.822
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.965
_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            yellow
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       plate
_exptl_crystal_F_000             1698
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene/hexanes'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.601
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         12421
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0520
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8941
_reflns_number_total             12421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Analytical' was
changed to 'analytical' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
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_cod_database_code               1558300
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              38319
_shelx_hkl_checksum              61455