1-(2-Bromoethyl)-1,4-diazoniabicyclo[2.2.2]octane bromide dihydrogen phosphate–phosphoric acid (1/1)
Xiao, Jing-Mei; Acta Crystallographica Section E 66 (2010) o1339–; doi:10.1107/S1600536810017071

data_2226270
_publ_section_title
;
 1-(2-Bromoethyl)-1,4-diazoniabicyclo[2.2.2]octane bromide dihydrogen
 phosphate--phosphoric acid (1/1)
;
_journal_coeditor_code           RZ2443
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1339
_journal_paper_doi               10.1107/S1600536810017071
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C8 H17 Br N2 2+, Br -, H2 P O4 -, H3 P O4'
_chemical_formula_moiety         'C8 H17 Br N2 2+, Br -, H2 O4 P -, H3 O4 P'
_chemical_formula_sum            'C8 H22 Br2 N2 O8 P2'
_chemical_formula_weight         496.02
_chemical_name_systematic
;
1-(2-Bromoethyl)-1,4-diazoniabicyclo[2.2.2]octane bromide dihydrogen
phosphate--phosphoric acid (1/1)
;
_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                 92.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.963(3)
_cell_length_b                   7.5959(15)
_cell_length_c                   17.721(4)
_cell_measurement_reflns_used    7671
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.480
_cell_measurement_theta_min      3.375
_cell_volume                     1743.8(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury2'
_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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17431
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_diffrn_standards_number         1814
_exptl_absorpt_coefficient_mu    4.868
_exptl_absorpt_correction_T_max  0.379
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.027
_refine_diff_density_min         -1.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0703P)^2^+1.8668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                3097
_reflns_number_total             3991
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2443.cif
_cod_data_source_block           I
_cod_original_cell_volume        1743.9(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226270
_cod_database_fobs_code          2226270