4-Aza-1-azoniabicyclo[2.2.2]octane dihydrogenarsenate monohydrate
Todd, Malcolm J.; Harrison, William T. A.; Acta Crystallographica Section E 63 (2007) m945–m947; doi:10.1107/S1600536807009178

data_2212969
_publ_section_title
;
 4-Aza-1-azoniabicyclo[2.2.2]octane dihydrogenarsenate monohydrate
;
_journal_coeditor_code           NG2222
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m945
_journal_page_last               m947
_journal_paper_doi               10.1107/S1600536807009178
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C6 H13 N2 +, As H2 O4 -, H2 O'
_chemical_formula_moiety         'C6 H13 N2 +, As H2 O4 -, H2 O'
_chemical_formula_sum            'C6 H17 As N2 O5'
_chemical_formula_weight         272.14
_chemical_name_systematic
;
4-Aza-1-azoniabicyclo[2.2.2]octane dihydrogenarsenate monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'difmap (O-H, N-H) and geom (C-H)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.710(3)
_cell_angle_beta                 103.604(3)
_cell_angle_gamma                111.720(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9515(3)
_cell_length_b                   9.0103(4)
_cell_length_c                   9.2845(4)
_cell_measurement_reflns_used    2217
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     520.67(4)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
SCALEPACK and DENZO (Otwinowski & Minor, 1997), and SORTAV (Blessing,
1995)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10518
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.266
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.782
_refine_ls_extinction_coef       0.021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0224P)^2^+0.5077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                2231
_reflns_number_total             2380
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2222.cif
_cod_data_source_block           I
_cod_database_code               2212969
_cod_database_fobs_code          2212969