1,4,8,11-Tetraazoniacyclotetradecane tetrakis(hydrogensulfate)
Said, Salem; Mhadhbi, Noureddine; Hajlaoui, Fadhel; Bataille, Thierry; Naïli, Houcine; Acta Crystallographica Section E 69 (2013) o1278–; doi:10.1107/S1600536813018953

data_2238391
_publ_section_title
;
 1,4,8,11-Tetraazoniacyclotetradecane tetrakis(hydrogensulfate)
;
_journal_coeditor_code           LH5619
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1278
_journal_paper_doi               10.1107/S1600536813018953
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C10 H28 N4 4+, 4H S O4 -'
_chemical_formula_moiety         'C10 H28 N4 4+, 4(H O4 S -)'
_chemical_formula_sum            'C10 H32 N4 O16 S4'
_chemical_formula_weight         592.68
_chemical_name_systematic
;
1,4,8,11-Tetraazoniacyclotetradecane tetrakis(hydrogensulfate)
;
_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                 97.1650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8177(2)
_cell_length_b                   16.6464(3)
_cell_length_c                   8.7222(2)
_cell_measurement_reflns_used    15635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.91
_cell_volume                     1126.21(4)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18757
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.970
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(a face-indexed absorption correction was applied using the
Tompa method; de Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             624.0
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.537
_refine_ls_extinction_coef       0.019(6)
_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   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0623P)^2^+0.4049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                4074
_reflns_number_total             4952
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5619.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238391
_cod_database_fobs_code          2238391