4,10-Bis(pyridin-2-ylmethyl)-1,7-dithia-4,10-diazoniacyclododecane bis(perchlorate)
Wei, ZhenHong; You, XiuLi; Acta Crystallographica Section E 67 (2011) o2384–; doi:10.1107/S1600536811032715

data_2231575
_publ_section_title
;
 4,10-Bis(pyridin-2-ylmethyl)-1,7-dithia-4,10-diazoniacyclododecane
 bis(perchlorate)
;
_journal_coeditor_code           JJ2097
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2384
_journal_paper_doi               10.1107/S1600536811032715
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H30 N4 S2 2+, 2(Cl O4 -)'
_chemical_formula_moiety         'C20 H30 N4 S2, 2(Cl O4)'
_chemical_formula_sum            'C20 H30 Cl2 N4 O8 S2'
_chemical_formula_weight         589.52
_chemical_name_systematic
;
4,10-Bis(pyridin-2-ylmethyl)-1,7-dithia-4,10-diazoniacyclododecane
bis(perchlorate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.1670(10)
_cell_angle_beta                 90.3400(10)
_cell_angle_gamma                113.8300(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4491(6)
_cell_length_b                   11.6146(7)
_cell_length_c                   11.7795(7)
_cell_measurement_reflns_used    5215
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.903
_cell_measurement_theta_min      2.440
_cell_volume                     1298.23(13)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       'Thin slice \f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_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            12276
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6516
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.4486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                4865
_reflns_number_total             6516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jj2097.cif
_cod_data_source_block           I
_cod_database_code               2231575
_cod_database_fobs_code          2231575