#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202350.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202350 loop_ _publ_author_name 'Lee, Clare' 'Harrison, William T. A.' _publ_section_title ; Propane-1,2-diammonium hydrogenarsenate monohydrate ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m739 _journal_page_last m741 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(C3 H12 N2) [H As O4], H2 O' _chemical_formula_moiety 'C3 H12 N2 2+, H As O4 2-, H2 O' _chemical_formula_sum 'C3 H15 As N2 O5' _chemical_formula_weight 234.09 _chemical_name_systematic ; ; _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 'difmap (O-H) and geom (N-H, C-H)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 92.3150(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.9115(5) _cell_length_b 6.1530(3) _cell_length_c 13.3653(6) _cell_measurement_reflns_used 3887 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32.22 _cell_measurement_theta_min 2.36 _cell_volume 896.59(7) _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, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement SHELXL97 _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker SMART1000 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 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8758 _diffrn_reflns_theta_full 32.48 _diffrn_reflns_theta_max 32.48 _diffrn_reflns_theta_min 2.36 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.777 _exptl_absorpt_correction_T_max 0.488 _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADBAS; Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_description chunk _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.417 _refine_diff_density_min -0.333 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 103 _refine_ls_number_reflns 3224 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.923 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0227 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0251P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.0512 _reflns_number_gt 2519 _reflns_number_total 3224 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6320.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2202350 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol As1 0.001478(13) 0.13876(2) 0.203532(10) 0.02109(5) Uani d . 1 . . As O1 0.12954(10) -0.00642(19) 0.21175(8) 0.0323(3) Uani d . 1 . . O O2 -0.12469(10) -0.01347(19) 0.19198(9) 0.0354(3) Uani d . 1 . . O O3 0.00525(10) 0.32636(18) 0.11311(8) 0.0319(2) Uani d . 1 . . O O4 0.00121(11) 0.2754(2) 0.31667(8) 0.0385(3) Uani d . 1 . . O H1 -0.0436 0.3882 0.3140 0.046 Uiso d R 1 . . H N1 0.20796(12) 0.6149(2) 0.13668(10) 0.0288(3) Uani d . 1 . . N H2 0.1813 0.7433 0.1573 0.035 Uiso calc R 1 . . H H3 0.2650 0.5649 0.1802 0.035 Uiso calc R 1 . . H H4 0.1456 0.5217 0.1323 0.035 Uiso calc R 1 . . H N2 0.14992(12) 0.3446(2) -0.05134(9) 0.0288(3) Uani d . 1 . . N H5 0.1099 0.4473 -0.0863 0.035 Uiso calc R 1 . . H H6 0.1083 0.3112 0.0025 0.035 Uiso calc R 1 . . H H7 0.1574 0.2268 -0.0893 0.035 Uiso calc R 1 . . H C1 0.26149(15) 0.6395(3) 0.03651(12) 0.0306(3) Uani d . 1 . . C H8 0.3416 0.7069 0.0450 0.037 Uiso calc R 1 . . H H9 0.2098 0.7363 -0.0039 0.037 Uiso calc R 1 . . H C2 0.27488(14) 0.4264(3) -0.01915(11) 0.0292(3) Uani d . 1 . . C H10 0.3192 0.4572 -0.0799 0.035 Uiso calc R 1 . . H C3 0.34566(16) 0.2523(3) 0.03851(13) 0.0385(4) Uani d . 1 . . C H11 0.3567 0.1286 -0.0040 0.046 Uiso calc R 1 . . H H12 0.3008 0.2094 0.0956 0.046 Uiso calc R 1 . . H H13 0.4243 0.3082 0.0605 0.046 Uiso calc R 1 . . H O5 -0.14005(11) 0.6264(2) 0.31626(11) 0.0449(3) Uani d . 1 . . O H14 -0.2198 0.5925 0.3109 0.054 Uiso d R 1 . . H H15 -0.1393 0.7316 0.2785 0.054 Uiso d R 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As1 0.02180(7) 0.01843(7) 0.02295(7) 0.00023(6) -0.00027(5) -0.00066(6) O1 0.0286(6) 0.0297(6) 0.0381(6) 0.0103(5) -0.0038(5) -0.0061(5) O2 0.0274(6) 0.0282(6) 0.0505(7) -0.0070(5) 0.0020(5) -0.0034(6) O3 0.0341(6) 0.0296(6) 0.0318(5) 0.0010(5) 0.0012(4) 0.0094(5) O4 0.0514(8) 0.0351(7) 0.0284(6) 0.0137(6) -0.0059(5) -0.0092(5) N1 0.0292(6) 0.0239(7) 0.0328(6) 0.0012(5) -0.0043(5) -0.0056(6) N2 0.0350(7) 0.0257(7) 0.0254(6) 0.0007(6) -0.0010(5) -0.0013(5) C1 0.0345(8) 0.0249(8) 0.0318(8) -0.0038(7) -0.0035(6) 0.0018(7) C2 0.0296(8) 0.0299(8) 0.0284(7) -0.0003(7) 0.0034(6) 0.0004(7) C3 0.0370(9) 0.0378(10) 0.0405(9) 0.0113(8) 0.0003(7) -0.0009(8) O5 0.0354(7) 0.0348(7) 0.0651(8) 0.0054(6) 0.0078(6) 0.0111(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag As1 O1 . 1.6583(10) yes As1 O2 . 1.6671(11) yes As1 O3 . 1.6730(11) yes As1 O4 . 1.7302(11) yes O4 H1 . 0.8489 ? N1 C1 . 1.490(2) yes N1 H2 . 0.8900 ? N1 H3 . 0.8900 ? N1 H4 . 0.8900 ? N2 C2 . 1.500(2) yes N2 H5 . 0.8900 ? N2 H6 . 0.8900 ? N2 H7 . 0.8900 ? C1 C2 . 1.517(2) yes C1 H8 . 0.9700 ? C1 H9 . 0.9700 ? C2 C3 . 1.514(2) yes C2 H10 . 0.9800 ? C3 H11 . 0.9600 ? C3 H12 . 0.9600 ? C3 H13 . 0.9600 ? O5 H14 . 0.8953 ? O5 H15 . 0.8211 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 As1 O2 113.20(6) O1 As1 O3 111.98(6) O2 As1 O3 111.41(6) O1 As1 O4 103.59(5) O2 As1 O4 108.87(6) O3 As1 O4 107.28(6) As1 O4 H1 112.5 C1 N1 H2 109.5 C1 N1 H3 109.5 H2 N1 H3 109.5 C1 N1 H4 109.5 H2 N1 H4 109.5 H3 N1 H4 109.5 C2 N2 H5 109.5 C2 N2 H6 109.5 H5 N2 H6 109.5 C2 N2 H7 109.5 H5 N2 H7 109.5 H6 N2 H7 109.5 N1 C1 C2 113.69(13) N1 C1 H8 108.8 C2 C1 H8 108.8 N1 C1 H9 108.8 C2 C1 H9 108.8 H8 C1 H9 107.7 N2 C2 C3 110.33(14) N2 C2 C1 109.04(13) C3 C2 C1 114.80(13) N2 C2 H10 107.5 C3 C2 H10 107.5 C1 C2 H10 107.5 C2 C3 H11 109.5 C2 C3 H12 109.5 H11 C3 H12 109.5 C2 C3 H13 109.5 H11 C3 H13 109.5 H12 C3 H13 109.5 H14 O5 H15 99.7 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O4 H1 O5 . 0.85 1.81 2.6534(17) 177 yes N1 H2 O1 1_565 0.89 1.80 2.6904(17) 174 yes N1 H3 O1 2 0.89 1.86 2.7412(17) 169 yes N1 H4 O3 . 0.89 1.96 2.8436(18) 176 yes N2 H5 O3 3_565 0.89 1.90 2.7449(17) 158 yes N2 H6 O3 . 0.89 1.90 2.7596(17) 163 yes N2 H7 O2 3 0.89 1.92 2.7782(17) 161 yes O5 H14 O2 2_455 0.90 1.82 2.7056(17) 172 yes O5 H15 O2 1_565 0.82 1.96 2.7782(17) 176 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag N1 C1 C2 C3 -54.09(18) yes N1 C1 C2 N2 70.26(16) yes