New trifluoromethylated sesquiterpenoids: synthesis, rearrangement, and biological activity
Gyrdymova, Yulia V.; Rumyantcev, Roman V.; Esaulkova, Yana L.; Belyaevskaya, Svetlana V.; Zarubaev, Vladimir V.; Kayumov, Airat R.; Rubtsova, Svetlana A.; New Journal of Chemistry 46 (2022) 23165–23172; doi:10.1039/D2NJ04611C

data_7062037
_publ_section_title
;
 New trifluoromethylated sesquiterpenoids: synthesis, rearrangement, and
 biological activity
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              23165
_journal_page_last               23172
_journal_paper_doi               10.1039/D2NJ04611C
_journal_volume                  46
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_sum            'C15 H23 F3 O2'
_chemical_formula_weight         292.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-28 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.2716(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.9014(11)
_cell_length_b                   6.6072(3)
_cell_length_c                   20.4393(8)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.57
_cell_volume                     3021.5(2)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX3
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-2018/3
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17371
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9580
_exptl_absorpt_correction_T_min  0.9047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       stick
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 1627 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_coef       0.0101(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0441P)^2^+1.4107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                4354
_reflns_number_total             5290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04611c2.cif
_cod_data_source_block           W-814
_cod_depositor_comments
'Adding full bibliography for 7062034--7062037.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7062037
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              32798