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_1571453
_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         'C48 H32 Cl2 F2 N4 O4 U2'
_chemical_formula_sum            'C48 H32 Cl2 F2 N4 O4 U2'
_chemical_formula_weight         1313.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7599(16)
_cell_length_b                   17.6063(16)
_cell_length_c                   15.3755(14)
_cell_measurement_reflns_used    87318
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.188
_cell_measurement_theta_min      1.803
_cell_volume                     4266.3(7)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_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_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            87318
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.188
_diffrn_reflns_theta_min         1.803
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.663
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.8946.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+16.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3607
_reflns_number_total             4407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01310g2.cif
_cod_data_source_block           rr_71603_0ma
_cod_depositor_comments
'Adding full bibliography for 1571453--1571456.cif.'
_cod_database_code               1571453
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.647
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C1(H1), C10(H10), C21(H21), C9(H9), C23(H23), C6(H6), C20(H20),
 C2(H2), C22(H22), C5(H5), C14(H14), C15(H15), C18(H18), C16(H16), C17(H17)
;
_shelx_res_checksum              6067
_olex2_submission_special_instructions 'No special instructions were received'