Photomediated C-H trifluoromethoxylations enabled by bis(trifluoromethyl)peroxide.
Shakeri, Kamar; Kleoff, Merlin; Golz, Paul; Drews, Thomas; Weber, Manuela; Riedel, Sebastian; Christmann, Mathias; Chemical science 16 (2025) 17921–17926; doi:10.1039/d5sc04945h

data_1575531
_publ_section_title
;
 Photomediated C-H trifluoromethoxylations enabled by
 bis(trifluoromethyl)peroxide.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              17921
_journal_page_last               17926
_journal_paper_doi               10.1039/d5sc04945h
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration rm
_chemical_formula_sum            'C17 H25 F3 O3'
_chemical_formula_weight         334.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-03-28 deposited with the CCDC.	2025-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.39090(10)
_cell_length_b                   13.65550(10)
_cell_length_c                   14.48060(10)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.54
_cell_measurement_theta_min      3.05
_cell_volume                     1659.22(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21852
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.676
_diffrn_reflns_theta_min         6.095
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1687 before and 0.1042 after correction.
The Ratio of minimum to maximum transmission is 0.6912.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.7639
_exptl_transmission_factor_min   0.5280
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details
;
 Flack x determined using 1364 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+0.3630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                3260
_reflns_number_total             3322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04945h2.cif
_cod_data_source_block           KS276a
_cod_depositor_comments          'Adding full bibliography for 1575531.cif.'
_cod_database_code               1575531
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.608
_shelx_estimated_absorpt_t_max   0.832
_shelx_res_checksum              44933