3,10-<i>C</i>-<i>meso</i>-3,5,7,7,10,12,14,14-Octamethyl-4,11-diaza-1,8-diazoniacyclotetradecane bis(perchlorate)
Roy, Tapashi G.; Hazari, Saroj K. S.; Barua, Kanak K.; Palit, Provi; Tiekink, Edward R. T.; Acta Crystallographica Section E 66 (2010) o2196–o2197; doi:10.1107/S1600536810030217

data_2227486
_publ_section_title
;
 3,10-<i>C</i>-<i>meso</i>-3,5,7,7,10,12,14,14-Octamethyl-4,11-diaza-1,8-diazoniacyclotetradecane
 bis(perchlorate)
;
_journal_coeditor_code           HB5587
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2196
_journal_page_last               o2197
_journal_paper_doi               10.1107/S1600536810030217
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C18 H42 N4 2+, 2Cl O4 -'
_chemical_formula_moiety         'C18 H42 N4 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C18 H42 Cl2 N4 O8'
_chemical_formula_weight         513.46
_chemical_name_systematic
;
3,10-<i>C</i>-<i>meso</i>-3,5,7,7,10,12,14,14-Octamethyl-4,11-diaza-1,8-
diazoniacyclotetradecane bis(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 102.088(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.868(2)
_cell_length_b                   16.297(3)
_cell_length_c                   17.754(5)
_cell_measurement_reflns_used    7813
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      2.4
_cell_volume                     2508.9(10)
_computing_cell_refinement
'CrystalClear (Molecular Structure Corporation & Rigaku, 2005)'
_computing_data_collection
'CrystalClear (Molecular Structure Corporation & Rigaku, 2005)'
_computing_data_reduction
'CrystalClear (Molecular Structure Corporation & Rigaku, 2005)'
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku AFC12\K/SATURN724'
_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  0.055
_diffrn_reflns_av_sigmaI/netI    0.021
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54635
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.85
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.19
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4387
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.19
_refine_ls_R_factor_all          0.084
_refine_ls_R_factor_gt           0.078
_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^)+(0.128P)^2^+4.0207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.223
_refine_ls_wR_factor_ref         0.240
_reflns_number_gt                4279
_reflns_number_total             4387
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5587.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227486
_cod_database_fobs_code          2227486