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_7249145
_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         'C10 H7 F3 O2'
_chemical_formula_sum            'C10 H7 F3 O2'
_chemical_formula_weight         216.16
_chemical_name_common            'trans-4-(trifluoromethyl) cinnamic acid'
_chemical_name_systematic        'trans-4-(trifluoromethyl) cinnamic 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     dual
_audit_creation_date             2024-02-06
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-02-07 deposited with the CCDC.	2024-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                91.368(6)
_cell_angle_beta                 93.753(5)
_cell_angle_gamma                94.796(5)
_cell_formula_units_Z            4
_cell_length_a                   7.8672(5)
_cell_length_b                   7.9953(6)
_cell_length_c                   14.9972(11)
_cell_measurement_reflns_used    8977
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.9630
_cell_measurement_theta_min      2.5450
_cell_volume                     937.61(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     16.00  41.00   0.50    1.31    --    4.22  77.00 -65.10   50
  2  \w     11.00  37.00   0.50    1.31    --    4.22  70.00 -12.68   52
  3  \w      9.00  43.00   0.50    1.31    --    4.22  73.00  54.93   68
  4  \w      8.00  43.00   0.50    1.31    --    4.22  72.00  91.91   70
  5  \w      7.00  42.00   0.50    1.31    --    4.22  75.00 176.48   70
  6  \w     18.00  47.00   0.50    1.31    --    4.22  54.00 148.30   58
  7  \w     15.00  50.00   0.50    1.31    --    4.22  51.00 136.33   70
  8  \w     17.00  44.00   0.50    1.31    --    4.22  61.00  16.04   54
  9  \w     18.00  47.00   0.50    1.31    --    4.22  49.00 -24.10   58
 10  \w     22.00  47.00   0.50    1.31    --    4.22  60.00 -87.05   50
 11  \w     17.00  43.00   0.50    1.31    --    4.22  43.00-113.93   52
 12  \w     14.00  42.00   0.50    1.31    --    4.22  49.00-140.62   56
 13  \w     17.00  42.00   0.50    1.31    --    4.22  55.00-103.10   50
 14  \w     16.00  43.00   0.50    1.31    --    4.22  42.00  57.91   54
 15  \w    -43.00   5.00   0.50    1.31    --    4.22 -19.00  30.00   96
 16  \w    -44.00   0.00   0.50    1.31    --    4.22 -19.00 120.00   88
 17  \w    -22.00   4.00   0.50    1.31    --    4.22 -19.00 -30.00   52
 18  \w    -36.00   4.00   0.50    1.31    --    4.22 -19.00 -90.00   80
 19  \w    -26.00   0.00   0.50    1.31    --    4.22 -19.00-120.00   52
 20  \w    -40.00 -15.00   0.50    1.31    --    4.22 -19.00-180.00   50
 21  \w    -18.00  10.00   0.50    1.31    --   -4.06-101.00-146.45   56
 22  \w     -8.00  19.00   0.50    1.31    --   -4.06  90.00-163.31   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30088
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.558
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.531
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             440
_exptl_crystal_preparation       'room temperature'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.59
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.013(3)
_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   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5732
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+0.0481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3559
_reflns_number_total             5732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00205a2.cif
_cod_data_source_block           trans4beforeillumination
_cod_depositor_comments
'Adding full bibliography for 7249143--7249145.cif.'
_cod_database_code               7249145
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H3-O3
 0.9 with sigma of 0.02
 H2-O2
 0.85 with sigma of 0.02
3. Others
 Sof(F3B)=Sof(F2B)=Sof(F1B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
 Sof(F5B)=Sof(F4B)=Sof(F6B)=1-FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C2(H2A), C3(H3A), C12(H12), C15(H15), C9(H9), C19(H19), C16(H16),
 C8(H8), C5(H5), C18(H18), C6(H6)
;
_shelx_res_checksum              63464
_olex2_exptl_crystal_mounting_method
'Glued with GE varnish to 100 \"i>5m diam. Teflon fishing rod in 18 mm pin on magnetic base as for protein cryo-crystallography'
_olex2_submission_original_sample_id 'trans-3-(trifluoromethyl)cinnamic acid'
_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
;