4,7,13,18-Tetraoxa-1,10-diazoniabicyclo[8.5.5]icosane bis(hexafluoridophosphate)
Sen Gupta, Nalinava; Wragg, David S.; Tilset, Mats; Omtvedt, Jon Petter; Acta Crystallographica Section E 67 (2011) o1929–o1930; doi:10.1107/S1600536811025992

data_2231090
_publ_section_title
;
 4,7,13,18-Tetraoxa-1,10-diazoniabicyclo[8.5.5]icosane
 bis(hexafluoridophosphate)
;
_journal_coeditor_code           FY2005
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1929
_journal_page_last               o1930
_journal_paper_doi               10.1107/S1600536811025992
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H30 N2 O4 2+, 2P F6 -'
_chemical_formula_moiety         'C14 H30 N2 O4 2+, 2(F6 P -)'
_chemical_formula_sum            'C14 H30 F12 N2 O4 P2'
_chemical_formula_weight         580.34
_chemical_name_systematic
;
4,7,13,18-Tetraoxa-1,10-diazoniabicyclo[8.5.5]icosane bis(hexafluoridophosphate)
;
_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                 95.538(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8297(16)
_cell_length_b                   16.485(2)
_cell_length_c                   12.6846(19)
_cell_measurement_reflns_used    1782
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      2.26
_cell_volume                     2254.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Berndt, 1999)
;
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and WinGX (Farrugia, 1999)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.931
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9756
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0378P)^2^+1.6619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                2002
_reflns_number_total             2785
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fy2005.cif
_cod_data_source_block           I
_cod_original_cell_volume        2254.0(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2231090
_cod_database_fobs_code          2231090