(1<i>S</i>,2<i>S</i>,4<i>S</i>,5<i>S</i>)-2,5-Dibenzyl-1,4-diazoniabicyclo[2.2.2]octane dichloride methanol solvate
Qiu, Li-Hua; Yang, Wen; Zhang, Yawen; Zhang, De-Chun; Acta Crystallographica Section E 61 (2005) o2668–o2670; doi:10.1107/S1600536805022762

data_2206588
_publ_section_title
;(1<i>S</i>,2<i>S</i>,4<i>S</i>,5<i>S</i>)-2,5-Dibenzyl-1,4-diazoniabicyclo[2.2.2]octane
 dichloride methanol solvate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2668
_journal_page_last               o2670
_journal_paper_doi               10.1107/S1600536805022762
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C20 H26 N2 2+, 2Cl -, C H4 O'
_chemical_formula_moiety         'C20 H26 N2 2+, 2Cl -, C H4 O'
_chemical_formula_sum            'C21 H30 Cl2 N2 O'
_chemical_formula_weight         397.37
_chemical_name_systematic
;
(1S,2S,4S,5S)-2,5-Dibenzyl-1,4-diazoniabicyclo[2.2.2]octane dichloride
methanol solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.970(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7262(13)
_cell_length_b                   7.6968(7)
_cell_length_c                   11.8788(13)
_cell_measurement_reflns_used    3734
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.0
_cell_volume                     1007.65(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 1990)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2003)'
_computing_molecular_graphics    'ORTEPIII for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6594
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.8504
_exptl_absorpt_correction_T_min  0.7993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.490
_refine_ls_abs_structure_details 'Flack (1983), 855 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0733P)^2^+0.7886P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                2855
_reflns_number_total             2874
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6368.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     'p 2yb'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2206588
_cod_database_fobs_code          2206588