3,12-Diaza-6,9-diazonia-2,13-dioxotetradecane bis(perchlorate)
Söhnel, Tilo; Wichmann, Kathrin A.; Doert, Thomas; Cooper, Garth J. S.; Acta Crystallographica Section E 68 (2012) o333–o334; doi:10.1107/S1600536811055516

data_2233576
_publ_section_title
;
 3,12-Diaza-6,9-diazonia-2,13-dioxotetradecane bis(perchlorate)
;
_journal_coeditor_code           NC2261
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o333
_journal_page_last               o334
_journal_paper_doi               10.1107/S1600536811055516
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C10 H24 N4 O2 2+, 2Cl O4 -'
_chemical_formula_moiety         'C10 H24 N4 O2 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C10 H24 Cl2 N4 O10'
_chemical_formula_weight         431.23
_chemical_name_common            '(H2DAT 2 ClO4)'
_chemical_name_systematic
;
3,12-Diaza-6,9-diazonia-2,13-dioxotetradecane 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                90.00
_cell_angle_beta                 110.846(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0888(5)
_cell_length_b                   10.9415(9)
_cell_length_c                   14.8160(11)
_cell_measurement_reflns_used    12054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59.04
_cell_measurement_theta_min      4.74
_cell_volume                     922.44(13)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2011)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'Image plate detector'
_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  0.1137
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11528
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  3
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.9360
_exptl_absorpt_correction_T_min  0.8369
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'not regular'
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.419
_refine_ls_extinction_coef       0.0082(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0435P)^2^+0.0412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                1624
_reflns_number_total             2113
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nc2261.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233576
_cod_database_fobs_code          2233576