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_1558298
_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         'C68 H58 Cl2 N10 O U2, solvent'
_chemical_formula_sum            'C68 H58 Cl2 N10 O U2'
_chemical_formula_weight         1578.20
_chemical_name_common            'Compound 8.solvent'
_chemical_name_systematic        '[{(py)ClUOUCl(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                77.753(4)
_cell_angle_beta                 76.263(4)
_cell_angle_gamma                72.589(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2163(5)
_cell_length_b                   13.1548(5)
_cell_length_c                   21.1659(10)
_cell_measurement_reflns_used    10380
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.1670
_cell_measurement_theta_min      3.2170
_cell_volume                     3116.0(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      120(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    -25.00  22.00   1.00   37.50    --  -22.87 -99.00-180.00   47
  2  \w    -55.00  51.00   1.00   37.50    --  -22.87  37.00 150.00  106
  3  \w   -105.00 -32.00   1.00   37.50    --  -22.87 179.00 -30.00   73
  4  \w    -25.00  22.00   1.00   37.50    --  -22.87 -99.00 -60.00   47
  5  \w     34.00 104.00   1.00   37.50    --   24.12 179.00-120.00   70
  6  \w    -46.00  48.00   1.00   37.50    --   24.12 -57.00-120.00   94
  7  \w    -46.00  48.00   1.00   37.50    --   24.12 -57.00-150.00   94
  8  \w      0.00  95.00   1.00   37.50    --   24.12  57.00   0.00   95
  9  \w    -25.00  22.00   1.00   37.50    --  -22.87 -99.00  30.00   47
 10  \w   -103.00 -34.00   1.00   37.50    --  -22.87-179.00-120.00   69
 11  \w    -93.00   1.00   1.00   37.50    --  -22.87 -57.00-150.00   94
 12  \w    -25.00  69.00   1.00   37.50    --   24.12 -99.00 -60.00   94
 13  \w      0.00  95.00   1.00   37.50    --   24.12  57.00  90.00   95
 14  \w     -8.00  98.00   1.00   37.50    --   24.12  37.00-150.00  106
 15  \w    -25.00  69.00   1.00   37.50    --   24.12 -99.00  60.00   94
;
_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  0.1020
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60766
_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         25.349
_diffrn_reflns_theta_min         2.926
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.327
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.833
_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    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             1524
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pyridine/hexanes'
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.037
_refine_diff_density_max         4.186
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         11386
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0386P)^2^+17.3410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8593
_reflns_number_total             11386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02297g2.cif
_cod_data_source_block           compound8
_cod_database_code               1558298
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              21725
_shelx_hkl_checksum              83854
_shelx_fab_checksum              4134