Visible light activation of C-Cl and C-F bonds in persistent organic pollutants using cerium(iii) triamidoamine complex.
Combourieu, Adrien; Christodoulou, Stella; Maron, Laurent; Assendjee, Eachann; Casaretto, Nicolas; Phung, Bich Tuyen; Banyasz, Akos; Maury, Olivier; Gregson, Matthew; Wooles, Ashley J.; Liddle, Stephen T.; Tard, Cédric; Nocton, Grégory; Danoun, Grégory; Chemical science 16 (2025) 15510–15517; doi:10.1039/d5sc03626g

data_1575199
_publ_section_title
;
 Visible light activation of C-Cl and C-F bonds in persistent organic
 pollutants using cerium(iii) triamidoamine complex.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              15510
_journal_page_last               15517
_journal_paper_doi               10.1039/d5sc03626g
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C33 H75 Br Ce N4 Si3'
_chemical_formula_sum            'C33 H75 Br Ce N4 Si3'
_chemical_formula_weight         832.27
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-27 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.712(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0115(10)
_cell_length_b                   15.7902(9)
_cell_length_c                   20.3365(17)
_cell_measurement_reflns_used    24182
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      1.58
_cell_volume                     4177.9(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      '1737 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            113827
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.253
_exptl_absorpt_coefficient_mu    2.158
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         10347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0352P)^2^+2.2539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8379
_reflns_number_total             10347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03626g3.cif
_cod_data_source_block           2_Br
_cod_depositor_comments
'Adding full bibliography for 1575197--1575202.cif.'
_cod_database_code               1575199
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C28(H28), C31(H31), C16(H16), C10(H10), C19(H19), C22(H22), C7(H7), C13(H13),
 C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C4(H4A,H4B), C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C27(H27A,H27B,
 H27C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C32(H32A,H32B,
 H32C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              66734
_olex2_submission_special_instructions 'No special instructions were received'