4,7,13,18-Tetraoxa-1,10-diazoniabicyclo[8.5.5]icosane hexafluoridosilicate
Sen Gupta, Nalinava; Wragg, David S.; Tilset, Mats; Omtvedt, Jon Petter; Acta Crystallographica Section E 67 (2011) o1958–o1959; doi:10.1107/S1600536811026006

data_2231091
_publ_section_title
;
 4,7,13,18-Tetraoxa-1,10-diazoniabicyclo[8.5.5]icosane
 hexafluoridosilicate
;
_journal_coeditor_code           FY2006
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1958
_journal_page_last               o1959
_journal_paper_doi               10.1107/S1600536811026006
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H30 N2 O4 2+, Si F6 2-'
_chemical_formula_moiety         'C14 H30 N2 O4 2+, F6 Si 2-'
_chemical_formula_sum            'C14 H30 F6 N2 O4 Si'
_chemical_formula_weight         432.49
_chemical_name_common            '[2.1.1]cryptand siliconhexafluoride'
_chemical_name_systematic
;
4,7,13,18-Tetraoxa-1,10-diazoniabicyclo[8.5.5]icosane hexafluoridosilicate
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   10.050(5)
_cell_length_b                   23.218(5)
_cell_length_c                   8.031(5)
_cell_measurement_reflns_used    2312
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.21
_cell_volume                     1874.0(15)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9809
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0509P)^2^+0.6523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                1467
_reflns_number_total             2305
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fy2006.cif
_cod_data_source_block           I
_cod_database_code               2231091
_cod_database_fobs_code          2231091