Analyzing the photophysics and photochemistry of [UO<sub>2</sub>(acetylacetonate)<sub>2</sub>(L)] complexes.
Clark, Colin B.; Burnett, Nora L.; Ruhren, Alexander N.; Talbott, Eric D.; Eyubova, Erda; Besson, Claire; Panetier, Julien A.; Swierk, John R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12667–12677; doi:10.1039/d5dt00668f

data_7719169
_publ_section_title
;
 Analyzing the photophysics and photochemistry of
 [UO<sub>2</sub>(acetylacetonate)<sub>2</sub>(L)] complexes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12667
_journal_page_last               12677
_journal_paper_doi               10.1039/d5dt00668f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H18 N2 O6 U'
_chemical_formula_sum            'C16 H18 N2 O6 U'
_chemical_formula_weight         572.35
_chemical_name_systematic
di(acetylacetonato)(3-cyanopyridine)dioxidouranium(VI)
_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             2025-06-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-19 deposited with the CCDC.	2025-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.982(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9462(3)
_cell_length_b                   13.5087(5)
_cell_length_c                   17.6229(6)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    294.6(3)
_cell_measurement_theta_max      30.1350
_cell_measurement_theta_min      2.3560
_cell_volume                     1863.06(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.120a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.137a 64-bit (release 10-09-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.120a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.6(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_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    -74.00 110.00   0.50    2.08    --   20.00  54.00  60.00  368
  2  \w    -71.00 -43.00   0.50    2.08    --   20.00  54.00-150.00   56
  3  \w    -35.00  20.00   0.50    2.08    --   20.00  54.00-150.00  110
  4  \w     25.00 110.00   0.50    2.08    --   20.00  54.00-150.00  170
  5  \w    -74.00  73.00   0.50    2.08    --   20.00  54.00 -30.00  294
  6  \w     58.00  84.00   0.50    2.08    --   20.00  54.00-120.00   52
  7  \w    -48.00 -22.00   0.50    2.08    --   20.00  54.00 -90.00   52
  8  \w     44.00  74.00   0.50    2.08    --   20.00  54.00 -90.00   60
  9  \w     76.00 101.00   0.50    2.08    --   20.00  54.00 -90.00   50
 10  \w     -7.00  88.00   0.50    2.08    --   20.00  54.00-180.00  190
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0505791000
_diffrn_orient_matrix_UB_12      -0.0271827000
_diffrn_orient_matrix_UB_13      0.0221373000
_diffrn_orient_matrix_UB_21      0.0734106000
_diffrn_orient_matrix_UB_22      -0.0267046000
_diffrn_orient_matrix_UB_23      0.0174695000
_diffrn_orient_matrix_UB_31      0.0162405000
_diffrn_orient_matrix_UB_32      0.0361217000
_diffrn_orient_matrix_UB_33      0.0295956000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.753
_diffrn_reflns_theta_min         2.347
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.745
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.120a (Rigaku Oxford Diffraction, 2024)
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 yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_preparation
'1 mmol UNH in 10 mL CH3CN, added solution of 2 mmol Hacac and 1 mmol 3pycn dropwise'
_exptl_crystal_recrystallization_method
'solvent diffusion between chloroform and hexane'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3767
_reflns_number_total             5582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00668f2.cif
_cod_data_source_block           cbc_002
_cod_depositor_comments          'Adding full bibliography for 7719169.cif.'
_cod_database_code               7719169
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         UO6C16H18N2
_cell_oxdiff_angle_alpha         90.019(2)
_cell_oxdiff_angle_beta          100.002(2)
_cell_oxdiff_angle_gamma         90.010(2)
_cell_oxdiff_length_a            7.9484(2)
_cell_oxdiff_length_b            13.5091(4)
_cell_oxdiff_length_c            17.6188(5)
_cell_oxdiff_measurement_reflns_used 7495
_cell_oxdiff_volume              1863.08(9)
_shelx_estimated_absorpt_t_max   0.274
_shelx_estimated_absorpt_t_min   0.186
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C21(H21), C17(H17), C18(H18), C9(H9), C19(H19)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              83802
_shelx_hkl_checksum              34377
_olex2_date_sample_data_collection 2025-04-10
_olex2_exptl_crystal_mounting_method '200 um Mitigen Mount in emersion oil'
_olex2_submission_original_sample_id CBC_002
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.810