#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2005681.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_2005681 loop_ _publ_author_name 'Kemnitz, E.' 'Werner, C.' 'Trojanov, S.' _publ_section_title ; Reinvestigation of Crystalline Sulfuric Acid and Oxonium Hydrogensulfate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2665 _journal_page_last 2668 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '(H3 O)(H S O4)' _chemical_formula_structural '(H3 O)(H S O4)' _chemical_formula_sum 'H4 O5 S' _chemical_formula_weight 116.09 _chemical_melting_point 8.5 _chemical_name_common 'sulfuric acid monohydrate' _chemical_name_systematic 'oxonium hydrogen sulfate' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90. _cell_angle_beta 106.18(3) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 7.0770(10) _cell_length_b 6.9550(10) _cell_length_c 8.150(2) _cell_measurement_reflns_used 24 _cell_measurement_temperature 160(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 9 _cell_volume 385.26(14) _computing_structure_refinement SHELXL-93 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1985)' _diffrn_ambient_temperature 160(2) _diffrn_measurement_device 'Stoe-STADI four-circle' _diffrn_measurement_method \q-2\q _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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0091 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2384 _diffrn_reflns_theta_max 40 _diffrn_reflns_theta_min 3.00 _diffrn_standards_decay_% 6.2 _diffrn_standards_interval_time 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Irregular _exptl_crystal_F_000 240 _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.5 _refine_diff_density_max 1.097 _refine_diff_density_min -1.248 _refine_ls_extinction_coef 3.25(9) _refine_ls_extinction_method SHELXL93 _refine_ls_goodness_of_fit_all 1.126 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_hydrogen_treatment 'refall isotropically' _refine_ls_matrix_type full _refine_ls_number_parameters 72 _refine_ls_number_reflns 2364 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.394 _refine_ls_restrained_S_obs 1.145 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_obs 0.0332 _refine_ls_shift/esd_max 0.073 _refine_ls_shift/esd_mean 0.012 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0604P)^2^ + 0.0491P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.1075 _refine_ls_wR_factor_obs 0.0858 _reflns_number_observed 2224 _reflns_number_total 2384 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file sk1004.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 385.26(12) _cod_database_code 2005681 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 S1 0.01426(10) 0.00903(9) 0.00854(9) -0.00009(4) 0.00126(5) 0.00023(3) O1 0.0219(2) 0.0125(2) 0.0088(2) -0.00061(15) 0.00135(14) 0.00179(13) O2 0.0188(2) 0.0113(2) 0.0185(2) 0.0032(2) 0.0009(2) -0.0023(2) O3 0.0216(2) 0.0147(2) 0.0114(2) -0.0005(2) 0.00259(14) -0.00453(14) O4 0.0162(2) 0.0221(3) 0.0164(2) -0.0030(2) 0.0022(2) 0.0068(2) O5 0.0181(2) 0.0122(2) 0.0153(2) -0.00073(15) 0.0017(2) 0.00349(15) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol S1 0.75032(2) 0.15816(2) 0.04183(2) 0.01100(8) Uani d 1 S O1 0.82689(8) 0.06899(8) 0.21041(6) 0.01500(10) Uani d 1 O O2 0.61382(8) 0.31432(8) 0.04153(8) 0.01707(11) Uani d 1 O O3 0.66823(8) 0.01651(8) -0.08874(6) 0.01629(11) Uani d 1 O O4 0.93770(8) 0.24719(9) 0.00759(7) 0.01874(12) Uani d 1 O O5 0.72575(8) 0.69970(8) 0.17478(7) 0.01579(11) Uani d 1 O H2 0.608(3) 0.707(3) 0.105(3) 0.036(5) Uiso d 1 H H1 0.898(3) 0.314(3) -0.078(2) 0.024(4) Uiso d 1 H H3 0.712(3) 0.625(3) 0.266(2) 0.034(5) Uiso d 1 H H4 0.756(3) 0.818(3) 0.193(2) 0.028(4) Uiso d 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 _geom_angle_publ_flag O3 S1 O2 112.14(4) no O3 S1 O1 111.63(4) no O2 S1 O1 112.93(4) no O3 S1 O4 109.03(4) no O2 S1 O4 107.54(4) no O1 S1 O4 103.02(4) no S1 O4 H1 105.5(13) no H2 O5 H3 105.3(18) no H2 O5 H4 101.7(17) no H3 O5 H4 118.3(18) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 O3 1.4478(6) no S1 O2 1.4531(6) no S1 O1 1.4666(6) no S1 O4 1.5576(6) no O4 H1 0.82(2) no O5 H2 0.87(2) no O5 H3 0.93(2) no O5 H4 0.85(2) no