Using potassium bromide pellets and optical spectroscopy to assess the photodimerization of two trans-(trifluoromethyl)-cinnamic acid compounds
Ulambayar, Bayasgalan; Batchuluun, Khongorzul; Bariashir, Chantsalnyam; Uranbileg, Nergui; Stammler, Felix J.; Davaasambuu, Jav; Schrader, Tobias E.; CrystEngComm 26 (2024) 4470–4477; doi:10.1039/D4CE00205A

data_7249144
_publ_section_title
;
 Using potassium bromide pellets and optical spectroscopy to assess the
 photodimerization of two trans-(trifluoromethyl)-cinnamic acid compounds
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4470
_journal_page_last               4477
_journal_paper_doi               10.1039/D4CE00205A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C20 H14 F6 O4'
_chemical_formula_sum            'C20 H14 F6 O4'
_chemical_formula_weight         432.31
_chemical_name_systematic
'trans-4-(trifluoromethyl)cinnamic acid illuminated to beta-truxinic acid'
_chemical_properties_physical    Light-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-13
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                89.860(6)
_cell_angle_beta                 88.678(6)
_cell_angle_gamma                82.349(6)
_cell_formula_units_Z            2
_cell_length_a                   7.8930(5)
_cell_length_b                   8.2222(6)
_cell_length_c                   14.6037(12)
_cell_measurement_reflns_used    4016
_cell_measurement_temperature    293
_cell_measurement_theta_max      36.9300
_cell_measurement_theta_min      2.4380
_cell_volume                     939.06(12)
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution
'olex2.solve 1.5-ac5-024 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14300
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.499
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.33727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_preparation
'Crystal was illuminated for 8 hours with 334 nm light from a monochromator after a HgXe Lamp (Biologic, Inc.)'
_exptl_crystal_recrystallization_method
'87 mg of substance was dissolved in 17.1 ml Ethanol'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0905
_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^)+(0.1646P)^2^+0.2457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.3230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1884
_reflns_number_total             3763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00205a2.cif
_cod_data_source_block           baysaastartingmodelwithprod2
_cod_depositor_comments
'Adding full bibliography for 7249143--7249145.cif.'
_cod_database_code               7249144
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.945
_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 O(H) groups
2. Others
 Sof(H9)=Sof(H6)=Sof(H18A)=Sof(O2A)=Sof(O1A)=Sof(C3A)=Sof(H22)=Sof(C2A)=
 Sof(H21)=Sof(C5A)=Sof(H24)=Sof(C6A)=Sof(C9A)=Sof(C1A)=Sof(C7A)=Sof(H27)=
 Sof(C4A)=Sof(H23)=Sof(C11A)=Sof(H31)=Sof(C8A)=Sof(H8)=Sof(C10A)=Sof(H30)=
 Sof(H32)=Sof(C12A)=1-FVAR(1)
 Sof(H9B)=Sof(H6B)=Sof(H18)=Sof(C19)=Sof(O1)=Sof(O2)=Sof(C2)=Sof(H25)=Sof(C4)=
 Sof(C14)=Sof(C1)=Sof(C12)=Sof(H12)=Sof(C16)=Sof(H16)=Sof(C13)=Sof(H13)=Sof(C6)=
 Sof(H28)=Sof(C15)=Sof(H15)=Sof(C3)=Sof(H3)=Sof(H19)=Sof(C9)=Sof(H5)=FVAR(1)
 Sof(F1A)=Sof(F2)=Sof(F3)=1-FVAR(2)
 Sof(F1)=Sof(F3A)=Sof(F2A)=FVAR(2)
 Sof(F5)=Sof(F4)=Sof(F6)=1-FVAR(3)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C3A(H22), C2A(H21), C5A(H24), C4A(H23)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H9B), C5(H9), C8(H6), C8(H6B), C18(H18), C18(H18A), C7A(H27), C11A(H31),
 C8A(H8), C10A(H30), C19(H32), C2(H25), C12(H12), C16(H16), C13(H13), C6(H28),
 C15(H15), C3(H3), C12A(H19), C9(H5)
3.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              13223
_olex2_exptl_crystal_mounting_method
'glued with GE-varnish to 100 microm diam teflon thread in 18 mm steel pin on magnetic base.'
_olex2_submission_original_sample_id
'trans-4-trifluoromethyl cinnamic acid and its photoproduct beta-truxinic acid'
_olex2_submission_special_instructions 'No special instructions were received'