Piperidinium 4-(4-chlorophenyl)-3-cyano-5-ethoxycarbonyl-6-methylpyridine-2-thiolate
Mague, Joel T.; Akkurt, Mehmet; Mohamed, Shaaban K.; Bakhite, Etify A.; Albayati, Mustafa R.; IUCrData 1 (2016) x160651–; doi:10.1107/S2414314616006519

data_1543179
_publ_section_title
;
 Piperidinium
 4-(4-chlorophenyl)-3-cyano-5-ethoxycarbonyl-6-methylpyridine-2-thiolate
;
_journal_coeditor_code           XU4007
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x160651
_journal_paper_doi               10.1107/S2414314616006519
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C5 H12 N +, C16 H12 Cl N2 O2 S -'
_chemical_formula_moiety         'C5 H12 N +, C16 H12 Cl N2 O2 S -'
_chemical_formula_sum            'C21 H24 Cl N3 O2 S'
_chemical_formula_weight         417.94
_chemical_name_common
;
Piperidinium
4-(4-chlorophenyl)-3-cyano-5-ethoxycarbonyl-6-methylpyridine-2-thiolate
;
_chemical_name_systematic
'Piperidin-1-ium [4-(4-chlorophenyl)-3-cyano-5-(ethoxycarbonyl)-6-methylpyridin-2-yl]sulfanide'
_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                 105.6030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2363(2)
_cell_length_b                   24.2600(7)
_cell_length_c                   12.9049(4)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      74.3122
_cell_measurement_theta_min      3.6439
_cell_volume                     2182.00(11)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16665
_diffrn_reflns_theta_full        68.500
_diffrn_reflns_theta_max         74.546
_diffrn_reflns_theta_min         3.644
_exptl_absorpt_coefficient_mu    2.611
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.458
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0538P)^2^+0.8348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3985
_reflns_number_total             4350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xu4007sup1.cif
_cod_data_source_block           I
_cod_database_code               1543179
_cod_database_fobs_code          1543179
_shelx_estimated_absorpt_t_min   0.546
_shelx_estimated_absorpt_t_max   0.724
_shelx_hkl_checksum              47346
_shelx_res_checksum              78300