Novel asymmetric 3,5-bis(arylidene)piperidin-4-one derivatives: synthesis, crystal structures and cytotoxicity
Yao, Binrong; Li, Ning; Wang, Chunhua; Hou, Guige; Meng, Qingguo; Yan, Ke; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618006605

data_2021123
_publ_section_title
;
 Novel asymmetric 3,5-bis(arylidene)piperidin-4-one derivatives:
 synthesis, crystal structures and cytotoxicity
;
_journal_coeditor_code           OV3110
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618006605
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C26 H31 N O3'
_chemical_formula_moiety         'C26 H31 N O3'
_chemical_formula_sum            'C26 H31 N O3'
_chemical_formula_weight         405.52
_chemical_name_systematic
(5<i>E</i>)-3-(4-<i>tert</i>-Butylbenzylidene)-5-(3,5-dimethoxybenzylidene)-1-methylpiperidin-4-one
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.386(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1378(9)
_cell_length_b                   16.2788(8)
_cell_length_c                   7.5525(4)
_cell_measurement_reflns_used    3159
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.2510
_cell_measurement_theta_min      4.6740
_cell_volume                     2327.8(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.22
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8937
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.084
_diffrn_reflns_theta_min         3.581
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4384
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.2988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                3392
_reflns_number_total             4384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ov3110sup1.cif
_cod_data_source_block           exp_2473
_cod_database_code               2021123
_cod_database_fobs_code          2021123
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.871
_shelx_hkl_checksum              58257
_shelx_res_checksum              31811