#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2005680.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_2005680 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 'H2 S O4' _chemical_formula_structural 'H2 S O4' _chemical_formula_sum 'H2 O4 S' _chemical_formula_weight 98.08 _chemical_melting_point 10.5 _chemical_name_common 'sulfuric acid' _chemical_name_systematic 'dihydrogen sulfate' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90. _cell_angle_beta 111.39(3) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 8.181(2) _cell_length_b 4.6960(10) _cell_length_c 8.563(2) _cell_measurement_reflns_used 24 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 11 _cell_volume 306.31(14) _computing_structure_refinement SHELXL93 _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 113(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 0.0086 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 453 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_theta_min 5.10 _diffrn_standards_decay_% 0.5 _diffrn_standards_interval_time 1260 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Irregular _exptl_crystal_F_000 200 _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _refine_diff_density_max 0.386 _refine_diff_density_min -0.325 _refine_ls_extinction_coef 0.029(4) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.139 _refine_ls_goodness_of_fit_obs 1.155 _refine_ls_hydrogen_treatment 'refall isotropically' _refine_ls_matrix_type full _refine_ls_number_parameters 29 _refine_ls_number_reflns 450 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.207 _refine_ls_restrained_S_obs 1.155 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_obs 0.0212 _refine_ls_shift/esd_max -0.446 _refine_ls_shift/esd_mean 0.141 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0269P)^2^ + 0.5004P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.0623 _refine_ls_wR_factor_obs 0.0576 _reflns_number_observed 425 _reflns_number_total 453 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file sk1004.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _[local]_cod_chemical_formula_sum_orig 'H2 O4 S1' _cod_original_cell_volume 306.31(12) _cod_database_code 2005680 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 S 0.0069(2) 0.0093(2) 0.0142(2) 0.000 0.0056(2) 0.000 O1 0.0113(4) 0.0172(5) 0.0254(5) -0.0061(4) 0.0092(4) -0.0054(4) O2 0.0112(5) 0.0189(5) 0.0176(5) -0.0019(4) 0.0060(4) 0.0051(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol S 0 0.07450(9) 0.25 0.0097(2) Uani d S 1 S O1 -0.15928(13) -0.0822(2) 0.17792(13) 0.0173(2) Uani d . 1 O O2 0.00920(13) 0.2733(2) 0.11080(12) 0.0157(2) Uani d . 1 O H 0.088(4) 0.328(5) 0.128(3) 0.035(7) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 S O1 . 2 117.87(9) no O1 S O2 . 2 110.70(6) no O1 S O2 2 2 105.85(6) no O1 S O2 . . 105.85(6) no O1 S O2 2 . 110.70(6) no O2 S O2 2 . 105.22(8) no S O2 H . . 112.(2) no 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 S O1 . 1.4261(10) no S O1 2 1.4261(10) no S O2 2 1.5374(10) no S O2 . 1.5374(10) no O2 H . 0.66(3) no