The effect of ancillary ligands on hydrocarbon C-H bond functionalization by uranyl photocatalysts.
Rutkauskaite, Ryte; Zhang, Xiaobin; Woodward, Adam W.; Liu, Yanlin; Herrera, Gabriel; Purkis, Jamie; Woodall, Sean D.; Sarsfield, Mark; Schreckenbach, Georg; Natrajan, Louise S.; Arnold, Polly L.; Chemical science 15 (2024) 6965–6978; doi:10.1039/d4sc01310g

data_1571455
_publ_section_title
;
 The effect of ancillary ligands on hydrocarbon C-H bond functionalization
 by uranyl photocatalysts.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              6965
_journal_page_last               6978
_journal_paper_doi               10.1039/d4sc01310g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C28 H24 Cl2 N2 O3 U'
_chemical_formula_sum            'C28 H24 Cl2 N2 O3 U'
_chemical_formula_weight         745.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-03 deposited with the CCDC.	2024-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.06020(10)
_cell_length_b                   18.1719(2)
_cell_length_c                   15.7262(2)
_cell_measurement_reflns_used    70774
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.2450
_cell_measurement_theta_min      1.7180
_cell_volume                     2569.13(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -66.00  18.00   0.50    1.30    --    4.95 -50.00-109.00  168
  2  \w    -68.00  17.00   0.50    1.30    --    4.95 -37.00 -60.00  170
  3  \w    -68.00  17.00   0.50    1.30    --    4.95 -37.00  30.00  170
  4  \w    -68.00  17.00   0.50    1.30    --    4.95 -37.00 120.00  170
  5  \w     -8.00  77.00   0.50    1.30    --    4.95  50.00  37.00  170
  6  \w    -78.00   8.00   0.50    1.30    --   -5.34 -50.00-109.00  172
  7  \w    -59.00  10.00   0.50    1.30    --   -5.34 -57.00-150.00  138
  8  \w     12.00  37.00   0.50    1.30    --   -5.34-123.00-136.67   50
  9  \w     -7.00  28.00   0.50    1.30    --   -5.34 -99.00  60.00   70
 10  \w    -25.00  17.00   0.50    1.30    --   -5.34 -77.00 120.00   84
 11  \w    -18.00  70.00   0.50    1.30    --   -5.34  19.00  60.00  176
 12  \w    -18.00  70.00   0.50    1.30    --   -5.34  30.00 146.06  176
 13  \w    -19.00  67.00   0.50    1.30    --   -5.34  50.00  37.00  172
 14  \w    -18.00  70.00   0.50    1.30    --   -5.34  27.00 -28.94  176
 15  \w    -18.00  70.00   0.50    1.30    --   -5.34  19.00 -90.00  176
 16  \w    -18.00  70.00   0.50    1.30    --   -5.34  19.00-120.00  176
 17  \w    -18.00  68.00   0.50    1.30    --   -5.34  37.00-180.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0674163000
_diffrn_orient_matrix_UB_12      -0.0193864000
_diffrn_orient_matrix_UB_13      -0.0116632000
_diffrn_orient_matrix_UB_21      -0.0285978000
_diffrn_orient_matrix_UB_22      0.0141105000
_diffrn_orient_matrix_UB_23      0.0366866000
_diffrn_orient_matrix_UB_31      -0.0293532000
_diffrn_orient_matrix_UB_32      0.0308117000
_diffrn_orient_matrix_UB_33      -0.0241567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            109761
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.559
_exptl_absorpt_correction_T_max  0.571
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Crystallized by vapor diffusion of hexanes to a THF solution'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0167
_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^)+(0.0115P)^2^+4.1682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0363
_refine_ls_wR_factor_ref         0.0371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5391
_reflns_number_total             5903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01310g2.cif
_cod_data_source_block           pla21025refinalized
_cod_depositor_comments
'Adding full bibliography for 1571453--1571456.cif.'
_cod_database_code               1571455
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U O3 Cl2 N2 C24 H20'
_shelx_estimated_absorpt_t_max   0.622
_shelx_estimated_absorpt_t_min   0.270
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C27(H27a,H27b), C25(H25a,H25b), C26(H26a,H26b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C14(H14), C20(H20), C5(H5), C10(H10), C18(H18), C21(H21),
 C24(H24), C15(H15), C1(H1), C23(H23), C9(H9), C22(H22), C17(H17), C16(H16)
;
_shelx_res_checksum              73251
_olex2_exptl_crystal_mounting_method 'Mounted on a goniometer loop with fomblin'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.764