<i>N</i>-Methyl-<i>N</i>-(2-pyridiniomethyl)-2-[<i>N</i>-(2-pyridiniomethyl)methylamino]-<i>N</i>-(2-pyridylmethyl)ethanaminium tris(perchlorate)
Rompel, Annette; Bond, Andrew D.; McKenzie, Christine J.; Acta Crystallographica Section E 60 (2004) o1987–o1988; doi:10.1107/S1600536804025103

data_2204439
_publ_section_title
;<i>N</i>-Methyl-<i>N</i>-(2-pyridiniomethyl)-2-[<i>N</i>-(2-pyridiniomethyl)methylamino]-<i>N</i>-(2-pyridylmethyl)ethanaminium
 tris(perchlorate)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1987
_journal_page_last               o1988
_journal_paper_doi               10.1107/S1600536804025103
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C22 H30 N5 3+, 3Cl O4 -'
_chemical_formula_moiety         'C22 H30 N5 3+, 3Cl O4 -'
_chemical_formula_sum            'C22 H30 Cl3 N5 O12'
_chemical_formula_weight         662.86
_chemical_name_systematic
;
N-Methyl-N-(2-pyridiniomethyl)-2-[N-(2-pyridiniomethyl)methylamino]-
N-(2-pyridylmethyl)ethanaminium tris(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6004(3)
_cell_length_b                   8.7668(2)
_cell_length_c                   23.5440(5)
_cell_measurement_reflns_used    8693
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.77
_cell_volume                     2776.41(11)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker--Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice \w and \f'
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55950
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         3.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.245
_refine_diff_density_min         -1.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0667P)^2^+5.5837P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                4549
_reflns_number_total             5653
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6537.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2204439
_cod_database_fobs_code          2204439