1-Cyanomethyl-4-aza-1-azoniabicyclo[2.2.2]octane bromide dihydrate
Cai, Ying; Acta Crystallographica Section E 66 (2010) o1527–; doi:10.1107/S1600536810019926

data_2226598
_publ_section_title
;
 1-Cyanomethyl-4-aza-1-azoniabicyclo[2.2.2]octane bromide dihydrate
;
_journal_coeditor_code           NC2186
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1527
_journal_paper_doi               10.1107/S1600536810019926
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C8 H14 N3 +, Br -, 2H2 O'
_chemical_formula_moiety         'C8 H14 N3 +, Br -, 2(H2 O)'
_chemical_formula_sum            'C8 H18 Br N3 O2'
_chemical_formula_weight         268.16
_chemical_name_systematic
;
1-Cyanomethyl-4-aza-1-azoniabicyclo[2.2.2]octane bromide dihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   7.461(5)
_cell_length_b                   12.008(7)
_cell_length_c                   13.236(8)
_cell_measurement_reflns_used    3350
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.21
_cell_measurement_theta_min      6.28
_cell_volume                     1185.8(13)
_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_detector_area_resol_mean 13.6620
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13047
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    3.450
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.286
_refine_ls_abs_structure_details 'Flack (1983), 1134 Friedel pairs'
_refine_ls_abs_structure_Flack   0.033(14)
_refine_ls_extinction_coef       0.0055(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2711
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                2219
_reflns_number_total             2711
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nc2186.cif
_cod_data_source_block           I
_cod_database_code               2226598
_cod_database_fobs_code          2226598