A pH-Metric, UV, NMR, and X-ray Crystallographic Study on Arsenous Acid Reacting with Dithioerythritol
András Kolozsi; Andrea Károly-Lakatos; Gábor Galbács; Anders Østergaard Madsen; Erik Larsen; Béla Gyurcsik; Inorganic Chemistry 47 (2008) 3832–3840; doi:10.1021/ic7024439

data_4304853
_publ_section_title
;
A pH-Metric, UV, NMR, and X-ray Crystallographic Study on Arsenous Acid
Reacting with Dithioerythritol
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3832
_journal_page_last               3840
_journal_paper_doi               10.1021/ic7024439
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C4 H7 As O2 S2'
_chemical_formula_sum            'C4 H7 As O2 S2'
_chemical_formula_weight         226.149
_chemical_name_common            'Dithioerythritol Arsenite'
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   12.634(1)
_cell_length_b                   33.360(2)
_cell_length_c                   6.547(1)
_cell_measurement_reflns_used    28545
_cell_measurement_temperature    122.4(5)
_cell_measurement_theta_max      42.02
_cell_measurement_theta_min      3.45
_cell_volume                     2759.4(5)
_computing_cell_refinement       'Nonius Collect postrefinement'
_computing_data_collection       'Nonius Collect suite'
_computing_data_reduction        'Nonius Collect suite'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122.4(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28525
_diffrn_reflns_theta_full        42.02
_diffrn_reflns_theta_max         42.02
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.455
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method
'Disssolved in boiling ethanol and cooled to room temperature.'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         4813
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+1.9169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0435
_reflns_number_gt                4562
_reflns_number_total             4813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7024439-file002.cif
_cod_data_source_block           shelxl
_cod_database_code               4304853