1-Chloromethyl-1,4-diazoniabicyclo[2.2.2]octane bis(hexafluorophosphate)
Zhu, Run-Qiang; Acta Crystallographica Section E 67 (2011) o346–; doi:10.1107/S1600536811000390

data_2229040
_publ_section_title
;
 1-Chloromethyl-1,4-diazoniabicyclo[2.2.2]octane
 bis(hexafluorophosphate)
;
_journal_coeditor_code           FJ2377
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o346
_journal_paper_doi               10.1107/S1600536811000390
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C7 H15 Cl N2 2+, 2P F6 -'
_chemical_formula_moiety         'C7 H15 Cl N2 2+, 2(F6 P -)'
_chemical_formula_sum            'C7 H15 Cl F12 N2 P2'
_chemical_formula_weight         452.6
_chemical_name_systematic
;
1-Chloromethyl-1,4-diazoniabicyclo[2.2.2]octane bis(hexafluorophosphate)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.414(8)
_cell_length_b                   12.976(7)
_cell_length_c                   16.115(9)
_cell_measurement_reflns_used    6697
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.4596
_cell_volume                     3014(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       'CCD Profile fitting'
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30798
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.2500
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.458
_refine_ls_extinction_coef       0.00140(10)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0625P)^2^+3.8206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                3197
_reflns_number_total             3447
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2377.cif
_cod_data_source_block           I
_cod_database_code               2229040
_cod_database_fobs_code          2229040