3,5,7-Triaza-1-azoniatricyclo[3.3.1.1^3,7^]decane perchlorate
Kruszynski, Rafal; Trzesowska, Agata; Acta Crystallographica, Section E 60 (2004) o2347–o2349; doi:10.1107/S1600536804029320

data_2204788
_publ_section_title
;
3,5,7-Triaza-1-azoniatricyclo[3.3.1.1^3,7^]decane perchlorate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              o2347
_journal_page_last               o2349
_journal_paper_doi               10.1107/S1600536804029320
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C6 H13 N4 +, Cl1 O4 -'
_chemical_formula_moiety         'C6 H13 N4 +, Cl1 O4 -'
_chemical_formula_sum            'C6 H13 Cl N4 O4'
_chemical_formula_weight         240.65
_chemical_name_common            'Urotropinium perchlorate'
_chemical_name_systematic
;
3,5,7-Triaza-1-azoniatricyclo[3.3.1.1^3,7^]decane 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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_cell_angle_alpha                90.00
_cell_angle_beta                 90.061(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2662(19)
_cell_length_b                   9.6794(16)
_cell_length_c                   10.854(2)
_cell_measurement_reflns_used    3276
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     973.5(3)
_computing_cell_refinement       'CrysAlis RED (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
;
XP in SHELXTL/PC (Sheldrick, 1990b) and ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Kuma KM-4-CCD'
_diffrn_measurement_method       \w
_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  0.1787
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12433
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0.79
_diffrn_standards_interval_time  4
_diffrn_standards_number         52
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       sphere
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.43
_exptl_crystal_size_rad          0.47
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.679
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1322P)^2^+0.3022P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2016
_reflns_number_gt                1599
_reflns_number_total             1736
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz6017.cif
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C6 H13 Cl1 N4 O4'
_cod_database_code               2204788