2,5-Bis[2-({bis[3-(dimethylazaniumyl)propyl]azaniumyl}methyl)phenyl]-1,3,4-oxadiazole hexakis(perchlorate) sesquihydrate
Fusi, Vieri; Formica, Mauro; Macedi, Eleonora; Paoli, Paola; Rossi, Patrizia; Acta Crystallographica Section E 68 (2012) o3453–o3454; doi:10.1107/S1600536812047484

data_2236965
_publ_section_title
;
 2,5-Bis[2-({bis[3-(dimethylazaniumyl)propyl]azaniumyl}methyl)phenyl]-1,3,4-oxadiazole
 hexakis(perchlorate) sesquihydrate
;
_journal_coeditor_code           LR2084
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3453
_journal_page_last               o3454
_journal_paper_doi               10.1107/S1600536812047484
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C36 H66 N8 O1 6+, 6Cl O4 -, 1.5H2 O'
_chemical_formula_moiety         'C36 H66 N8 O1 6+, 6(Cl O4 -), 1.5(H2 O)'
_chemical_formula_sum            'C36 H69 Cl6 N8 O26.5'
_chemical_formula_weight         1250.69
_chemical_name_systematic
;
2,5-Bis[2-({bis[3-(dimethylazaniumyl)propyl]azaniumyl}methyl)phenyl]-
1,3,4-oxadiazole hexakis(perchlorate) sesquihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 113.695(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.5601(7)
_cell_length_b                   25.0825(8)
_cell_length_c                   24.2277(9)
_cell_measurement_reflns_used    7461
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.5898
_cell_measurement_theta_min      4.1345
_cell_volume                     10884.4(8)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2010)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012) and <i>Mercury</i> (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Oxford XcaliburPX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30246
_diffrn_reflns_theta_full        72.74
_diffrn_reflns_theta_max         72.74
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5240
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.857
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0702
_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^)+(0.1066P)^2^+23.0322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.2194
_reflns_number_gt                6531
_reflns_number_total             10465
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lr2084.cif
_cod_data_source_block           I
_cod_original_cell_volume        10884.4(7)
_cod_original_sg_symbol_Hall     ' -C 2yc'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2236965
_cod_database_fobs_code          2236965