Synthesis, crystal structures and anti-inflammatory activity of four 3,5-bis(arylidene)-<i>N</i>-benzenesulfonyl-4-piperidone derivatives
Li, Ning; Bai, Xianyong; Zhang, Lianshuang; Hou, Yun; Acta Crystallographica Section C 74 (2018) 1171–1179; doi:10.1107/S2053229618013232

data_2021245
_publ_section_title
;
 Synthesis, crystal structures and anti-inflammatory activity of four
 3,5-bis(arylidene)-<i>N</i>-benzenesulfonyl-4-piperidone derivatives
;
_journal_coeditor_code           SK3698
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1171
_journal_page_last               1179
_journal_paper_doi               10.1107/S2053229618013232
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C28 H18 F6 N2 O3 S, C H2 Cl2'
_chemical_formula_moiety         'C28 H18 F6 N2 O3 S, C H2 Cl2'
_chemical_formula_sum            'C29 H20 Cl2 F6 N2 O3 S'
_chemical_formula_weight         661.43
_chemical_name_systematic
'(3<i>E</i>,5<i>E</i>)-1-(4-Cyanobenzenesulfonyl)-3,5-bis[4-(trifluoromethyl)benzylidene]piperidin-4-one dichloromethane monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                70.586(3)
_cell_angle_beta                 88.379(4)
_cell_angle_gamma                81.726(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7338(6)
_cell_length_b                   12.4558(9)
_cell_length_c                   12.6397(9)
_cell_measurement_reflns_used    5958
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.55
_cell_volume                     1429.97(17)
_computing_cell_refinement
;
APEX2 (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24790
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.546
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.441
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0465P)^2^+0.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                3869
_reflns_number_total             5604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3698sup1.cif
_cod_data_source_block           7
_cod_database_code               2021245
_cod_database_fobs_code          2021245
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.960
_shelx_hkl_checksum              24593
_shelx_res_checksum              70446