1,4,10,13-Tetraoxa-7,16-diazoniacyclooctadecane bis(hexafluorophosphate): PF~6~^{-^} acting as a pseudohalide
Janzen, Daron E.; Botros, Maikel E.; Helton, Gregory P.; VanDerveer, Donald G.; Grant, Gregory J.; Acta Crystallographica Section E 62 (2006) o1550–o1552; doi:10.1107/S1600536806009342

data_2208733
_publ_section_title
;
 1,4,10,13-Tetraoxa-7,16-diazoniacyclooctadecane
 bis(hexafluorophosphate): PF~6~^{-^} acting as a pseudohalide
;
_journal_coeditor_code           SQ3010
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1550
_journal_page_last               o1552
_journal_paper_doi               10.1107/S1600536806009342
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C12 H28 N2 O4 2+, 2F6 P -'
_chemical_formula_moiety         'C12 H28 N2 O4 2+, 2F6 P -'
_chemical_formula_sum            'C12 H28 F12 N2 O4 P2'
_chemical_formula_weight         554.30
_chemical_name_systematic
;
1,4,10,13-Tetraoxa-7,16-diazoniacyclooctadecane bis(hexafluorophosphate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.647(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.269(2)
_cell_length_b                   10.333(2)
_cell_length_c                   12.264(3)
_cell_measurement_reflns_used    7032
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.0212
_cell_measurement_theta_min      2.3490
_cell_volume                     1099.2(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
'MERCURY (Version 1.4; Bruno <i>et al.</i>, 2002)'
_computing_publication_material  MERCURY
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku CCD'
_diffrn_measurement_method       \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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9148
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.398
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0685P)^2^+1.4259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                1785
_reflns_number_total             1948
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3010.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2208733
_cod_database_fobs_code          2208733