Photochemical Cu(III)-mediated trifluoromethylation of (hetero)arenes and biomolecules
Pospisil, Petr; Motornov, Vladimir; Michal, Ondřej; Wohlrábová, Lucie; Boháčová, Soňa; Slanina, Tomáš; Tarábek, Ján; Klepetářová, Blanka; Beier, Petr; Chemical Science  (2025) –; doi:10.1039/D5SC07405C

data_1576250
_publ_section_title
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 Photochemical Cu(III)-mediated trifluoromethylation of (hetero)arenes and
 biomolecules
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC07405C
_journal_year                    2025
_chemical_formula_moiety         'C10 H11 F3 N4 O2'
_chemical_formula_sum            'C10 H11 F3 N4 O2'
_chemical_formula_weight         276.22
_chemical_name_systematic
3-methyl-7-propyl-8-(trifluoromethyl)-3,7-dihydro-1/H/-purine-2,6-dione
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2025-07-22 deposited with the CCDC.	2025-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.285(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6718(2)
_cell_length_b                   7.81519(14)
_cell_length_c                   15.5844(4)
_cell_measurement_reflns_used    3721
_cell_measurement_temperature    100
_cell_measurement_theta_max      76.7490
_cell_measurement_theta_min      4.5970
_cell_volume                     1165.68(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.136a (Rigaku OD, 2024)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_unetI/netI     0.064
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8456
_diffrn_reflns_theta_full        74.097
_diffrn_reflns_theta_max         77.997
_diffrn_reflns_theta_min         4.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
 Gaussian Integration (Busing and Levy, 1957) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.42
_refine_ls_extinction_coef       51(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9849
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.0003907
_refine_ls_shift/su_mean         0.0000598
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 0.41P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1326
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1326
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                1991
_reflns_number_total             2433
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.51
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_scale          2.88(6)
_cod_data_source_file            d5sc07405c2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1576250
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0573
_reflns_number_all               2433