#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/43/2204352.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_2204352 loop_ _publ_author_name 'Wilkinson, Hazel S.' 'Harrison, William T. A.' _publ_section_title ; tert-Butylammonium dihydrogenarsenate ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1359 _journal_page_last m1361 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '(C4 H12 N) [H2 As O4]' _chemical_formula_moiety 'C4 H12 N 1+, As H2 O4 1-' _chemical_formula_sum 'C4 H14 As N O4' _chemical_formula_weight 215.08 _chemical_name_systematic ; tert-Butylammonium dihydrogenarsenate ; _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 (C-H and N-H)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.8640(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.7364(5) _cell_length_b 6.3254(3) _cell_length_c 14.2606(8) _cell_measurement_reflns_used 3025 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32.44 _cell_measurement_theta_min 2.44 _cell_volume 875.10(8) _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 0.996 _diffrn_measured_fraction_theta_max 0.996 _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 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 8742 _diffrn_reflns_theta_full 32.52 _diffrn_reflns_theta_max 32.52 _diffrn_reflns_theta_min 2.44 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.851 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_correction_T_min 0.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_description bar _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.469 _refine_diff_density_min -0.513 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 95 _refine_ls_number_reflns 3165 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.880 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0236 _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^)+(0.0332P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.0635 _reflns_number_gt 1807 _reflns_number_total 3165 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hg6081.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2204352 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_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_ _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_type_symbol As1 0.096480(18) 0.25182(3) 0.428460(11) 0.02877(6) Uani d . 1 As O1 -0.07070(14) 0.2606(2) 0.44605(10) 0.0360(3) Uani d . 1 O O2 0.13620(15) 0.3528(2) 0.32825(9) 0.0424(4) Uani d . 1 O O3 0.15368(15) -0.0032(2) 0.43072(9) 0.0402(3) Uani d . 1 O H1 0.1102 -0.0863 0.4773 0.048 Uiso d R 1 H O4 0.18923(15) 0.3676(3) 0.52194(10) 0.0482(4) Uani d . 1 O H2 0.1545 0.5006 0.5378 0.058 Uiso d R 1 H N1 0.38027(16) 0.2563(2) 0.24651(10) 0.0334(3) Uani d . 1 N H3 0.3062 0.2725 0.2783 0.040 Uiso calc R 1 H H4 0.3824 0.1249 0.2243 0.040 Uiso calc R 1 H H5 0.3766 0.3474 0.1988 0.040 Uiso calc R 1 H C1 0.5091(2) 0.2971(3) 0.31140(15) 0.0380(5) Uani d . 1 C C2 0.4956(3) 0.5164(4) 0.35241(18) 0.0608(7) Uani d . 1 C H6 0.4147 0.5224 0.3865 0.091 Uiso calc R 1 H H7 0.4880 0.6185 0.3024 0.091 Uiso calc R 1 H H8 0.5755 0.5471 0.3943 0.091 Uiso calc R 1 H C3 0.5148(3) 0.1313(4) 0.38747(18) 0.0643(7) Uani d . 1 C H9 0.5211 -0.0062 0.3597 0.097 Uiso calc R 1 H H10 0.4328 0.1392 0.4203 0.097 Uiso calc R 1 H H11 0.5940 0.1553 0.4309 0.097 Uiso calc R 1 H C4 0.6306(3) 0.2805(4) 0.2525(2) 0.0677(8) Uani d . 1 C H12 0.6329 0.1418 0.2254 0.102 Uiso calc R 1 H H13 0.7143 0.3051 0.2916 0.102 Uiso calc R 1 H H14 0.6217 0.3842 0.2032 0.102 Uiso calc 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 0.03246(9) 0.02705(9) 0.02761(8) 0.00106(11) 0.00722(6) -0.00055(9) O1 0.0324(6) 0.0318(7) 0.0448(7) 0.0000(7) 0.0090(5) 0.0018(7) O2 0.0539(10) 0.0385(9) 0.0368(8) 0.0031(7) 0.0162(7) 0.0104(6) O3 0.0507(9) 0.0294(7) 0.0433(8) 0.0085(7) 0.0196(6) 0.0027(6) O4 0.0452(9) 0.0500(10) 0.0474(9) 0.0071(8) -0.0072(7) -0.0177(7) N1 0.0389(8) 0.0304(7) 0.0312(7) 0.0000(9) 0.0053(6) 0.0001(8) C1 0.0392(11) 0.0367(12) 0.0371(10) -0.0018(8) -0.0017(8) 0.0006(7) C2 0.0685(18) 0.0454(14) 0.0640(16) -0.0033(13) -0.0198(13) -0.0125(12) C3 0.0716(19) 0.0592(17) 0.0592(16) -0.0032(15) -0.0123(13) 0.0228(14) C4 0.0391(12) 0.099(2) 0.0653(16) -0.0058(14) 0.0064(11) -0.0033(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag As1 O2 1.6412(13) y As1 O1 1.6687(13) y As1 O3 1.7061(13) y As1 O4 1.7101(14) y O3 H1 0.9710 ? O4 H2 0.9415 ? N1 C1 1.516(3) ? N1 H3 0.8900 ? N1 H4 0.8900 ? N1 H5 0.8900 ? C1 C3 1.506(3) ? C1 C4 1.511(3) ? C1 C2 1.515(3) ? C2 H6 0.9600 ? C2 H7 0.9600 ? C2 H8 0.9600 ? C3 H9 0.9600 ? C3 H10 0.9600 ? C3 H11 0.9600 ? C4 H12 0.9600 ? C4 H13 0.9600 ? C4 H14 0.9600 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O2 As1 O1 115.01(7) O2 As1 O3 106.49(7) O1 As1 O3 110.46(7) O2 As1 O4 111.36(8) O1 As1 O4 109.03(7) O3 As1 O4 103.90(7) As1 O3 H1 111.3 As1 O4 H2 113.1 C1 N1 H3 109.5 C1 N1 H4 109.5 H3 N1 H4 109.5 C1 N1 H5 109.5 H3 N1 H5 109.5 H4 N1 H5 109.5 C3 C1 C4 111.7(2) C3 C1 C2 111.0(2) C4 C1 C2 112.1(2) C3 C1 N1 107.39(18) C4 C1 N1 107.17(18) C2 C1 N1 107.28(18) C1 C2 H6 109.5 C1 C2 H7 109.5 H6 C2 H7 109.5 C1 C2 H8 109.5 H6 C2 H8 109.5 H7 C2 H8 109.5 C1 C3 H9 109.5 C1 C3 H10 109.5 H9 C3 H10 109.5 C1 C3 H11 109.5 H9 C3 H11 109.5 H10 C3 H11 109.5 C1 C4 H12 109.5 C1 C4 H13 109.5 H12 C4 H13 109.5 C1 C4 H14 109.5 H12 C4 H14 109.5 H13 C4 H14 109.5 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 O3 H1 O1 3_556 0.97 1.62 2.5752(19) 166 y O4 H2 O1 3_566 0.94 1.74 2.6763(19) 172 y N1 H3 O2 . 0.89 1.92 2.801(2) 168 y N1 H4 O2 2_545 0.89 1.88 2.765(2) 173 y N1 H5 O3 2 0.89 2.07 2.944(2) 166 y _cod_database_fobs_code 2204352