Tetraethylammonium dihydrogenarsenate bis(arsenic acid) and 1,4-diazoniabicyclo[2.2.2]octane bis(dihydrogenarsenate) arsenic acid: hydrogen-bonded networks containing dihydrogenarsenate anions and neutral arsenic acid molecules
Lee, Clare; Harrison, William T. A.; Acta Crystallographica Section C 63 (2007) m308–m311; doi:10.1107/S0108270107023967

data_2016038
_publ_section_title
;
 Tetraethylammonium dihydrogenarsenate bis(arsenic acid) and
 1,4-diazoniabicyclo[2.2.2]octane bis(dihydrogenarsenate) arsenic acid:
 hydrogen-bonded networks containing dihydrogenarsenate anions and
 neutral arsenic acid molecules
;
_journal_coeditor_code           GD3110
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m308
_journal_page_last               m311
_journal_paper_doi               10.1107/S0108270107023967
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C6 H14 N2) [H2 As O4]2 [H3 As O4]'
_chemical_formula_moiety         'C6 H14 N2 +, 2(As H2 O4)-, As H3 O4, '
_chemical_formula_sum            'C6 H21 As3 N2 O12'
_chemical_formula_weight         538.01
_chemical_name_systematic
;
1,4-diazoniabicyclo[2.2.2]octane bis(dihydrogenarsenate) arsenic acid
;
_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                 107.6370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1285(3)
_cell_length_b                   22.2104(9)
_cell_length_c                   10.0056(4)
_cell_measurement_reflns_used    5683
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.11
_cell_measurement_theta_min      2.79
_cell_volume                     1721.47(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and ATOMS (Shape Software, 2000)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            17889
_diffrn_reflns_theta_full        32.64
_diffrn_reflns_theta_max         32.64
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.849
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.448
_refine_ls_extinction_coef       0.00252(11)
_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   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         6212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0561
_reflns_number_gt                4321
_reflns_number_total             6212
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3110.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016038
_cod_database_fobs_code          2016038