Syntheses and crystal structures of two piperine derivatives
Ezawa, Toshinari; Inoue, Yutaka; Murata, Isamu; Suzuki, Mitsuaki; Takao, Koichi; Sugita, Yoshiaki; Kanamoto, Ikuo; Acta Crystallographica Section E 76 (2020) 646–650; doi:10.1107/S2056989020004648

data_2243354
_publ_section_title
;
 Syntheses and crystal structures of two piperine derivatives
;
_journal_coeditor_code           HB7897
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              646
_journal_page_last               650
_journal_paper_doi               10.1107/S2056989020004648
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C18 H21 N O3'
_chemical_formula_moiety         'C18 H21 N O3'
_chemical_formula_sum            'C18 H21 N O3'
_chemical_formula_weight         299.36
_chemical_name_systematic
;
5-(2<i>H</i>-1,3-Benzodioxol-5-yl)-<i>N</i>-cyclohexylpenta-2,4-dienamide
;
_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     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 97.683(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4982(7)
_cell_length_b                   5.0086(3)
_cell_length_c                   26.7240(16)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      33.49
_cell_measurement_theta_min      2.51
_cell_volume                     1525.22(16)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
<i>ShelXle</i> (H\"ubschle et al., 2011)
;
_computing_publication_material
;
<i>Generate Report</i> (Bruker, 2018)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayered conforacal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            27741
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.995
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2018)
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.584
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0455P)^2^+0.7464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                4204
_reflns_number_total             4862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7897sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243354
_cod_database_fobs_code          2243354
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              579
_shelx_res_checksum              44638