Bis[2-(2-pyridylsulfanyl)ethyl]ammonium perchlorate
Wang, Guo-Qing; Ma, Cong-Hui; Li, Xiao-Feng; Li, Wen-Ge; Ng, Seik Weng; Acta Crystallographica Section E 66 (2010) o2335–; doi:10.1107/S1600536810032216

data_2227166
_publ_section_title
;
 Bis[2-(2-pyridylsulfanyl)ethyl]ammonium perchlorate
;
_journal_coeditor_code           BH2303
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2335
_journal_paper_doi               10.1107/S1600536810032216
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C14 H18 N3 S2 + , Cl O4 -'
_chemical_formula_moiety         'C14 H18 N3 S2 + , Cl O4 -'
_chemical_formula_sum            'C14 H18 Cl N3 O4 S2'
_chemical_formula_weight         391.88
_chemical_name_systematic
;
Bis[2-(2-pyridylsulfanyl)ethyl]ammonium perchlorate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.534(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1265(6)
_cell_length_b                   9.2291(7)
_cell_length_c                   11.9872(9)
_cell_measurement_reflns_used    1783
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.5
_cell_measurement_theta_min      3.7
_cell_volume                     891.28(12)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Oxford Xcalibur Sapphire-3'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3124
_diffrn_reflns_theta_full        72.67
_diffrn_reflns_theta_max         72.67
_diffrn_reflns_theta_min         4.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.305
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.656
_refine_ls_extinction_coef       0.077(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1333P)^2^+0.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2141
_reflns_number_gt                1427
_reflns_number_total             1736
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2303.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2227166
_cod_database_fobs_code          2227166