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_7249143
_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            '3-(Trifluoromethyl)cinnamic acid'
_chemical_name_systematic        'trans-3-(trifluoromehtyl)cinnamic acid'
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-02-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-05 deposited with the CCDC.	2024-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.829(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3911(9)
_cell_length_b                   4.9722(3)
_cell_length_c                   13.1778(8)
_cell_measurement_reflns_used    3103
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8600
_cell_measurement_theta_min      2.3710
_cell_volume                     942.46(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution
'olex2.solve 1.5-ac5-024 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.9958
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9129
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.832
_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  1.00000
_exptl_absorpt_correction_T_min  0.56805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.96a (Rigaku Oxford Diffraction, 2023)
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    1.523
_exptl_crystal_description       'rectangular blocks'
_exptl_crystal_F_000             440
_exptl_crystal_preparation       'Grown from ethanol solution'
_exptl_crystal_recrystallization_method
'10 mg of substance in 50 ml Ethanol, Ethanol left to evaporate in fume hood'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.050
_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-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1915
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0512P)^2^+0.7350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1358
_reflns_number_total             1915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00205a2.cif
_cod_data_source_block           exp_14_auto
_cod_depositor_comments
'Adding full bibliography for 7249143--7249145.cif.'
_cod_database_code               7249143
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.932
_oxdiff_exptl_absorpt_empirical_full_min 0.377
_oxdiff_exptl_absorpt_empirical_full_max 1.484
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H1-O1
 0.85 with sigma of 0.02
3. Others
 Sof(F3)=Sof(F1)=Sof(F2)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C2(H2), C5(H5), C7(H7), C6(H6)
;
_shelx_res_checksum              68339
_olex2_exptl_crystal_mounting_method 'Mounted with GE-vernish on a Teflon loop'
_olex2_submission_original_sample_id 'trans-3-trifluoromethyl cinnamic acid '
_olex2_submission_special_instructions 'No special instructions were received'