Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_h2so4 _database_code_CSD 172536 _audit_creation_date 02-18-01 _audit_creation_method CRYSTALS_ver_12-03-99 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Allan, David Robert' 'Clark, Stewart J.' 'Dawson, Alice' 'McGregor, Pamela A.' 'Parsons, Simon' _publ_contact_author_name 'Dr David Robert Allan' _publ_contact_author_address ; Physics and Astronomy The University of Edinburgh James Clerk Maxwell Building The King's Buildings Mayfield Road Edinburgh Mid Lothian EH10 5QU UNITED KINGDOM ; _publ_contact_author_email 'D.R.ALLAN@ED.AC.UK' _publ_section_title ; Comparison of the high-pressure and low-temperature structures of sulfuric acid ; _chemical_name_systematic # IUPAC name, in full ; Sulfuric acid ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 7.695(13) _cell_angle_alpha 90 _cell_length_b 4.559(7) _cell_angle_beta 107.42(8) _cell_length_c 8.378(3) _cell_angle_gamma 90 _cell_volume 280.4(9) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' H2 O4 S1 ' _chemical_formula_moiety ' H2SO4 ' _chemical_compound_source ; CRYSTALS (Watkin et al 2001) ; _chemical_formula_weight 98.08 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 2.323 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 200.658 _exptl_absorpt_coefficient_mu 0.946 # Sheldrick geometric definitions 1.00 1.00 _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; SAINT (Siemens ,1995) ; _computing_cell_refinement ; SAINT (Siemens ,1995) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293 _diffrn_reflns_number 698 _reflns_number_total 218 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 218 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 599 _diffrn_measured_fraction_theta_max 0.364 _reflns_number_gt 178 _diffrn_reflns_theta_min 5.02 _diffrn_reflns_theta_max 26.79 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _reflns_limit_h_min -7 _reflns_limit_h_max 4 _reflns_limit_k_min 0 _reflns_limit_k_max 5 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _refine_diff_density_min -0.34 _refine_diff_density_max 0.48 _reflns_threshold_expression >2.00\s(I) _refine_ls_number_reflns 178 _refine_ls_number_parameters 27 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.0381 _refine_ls_goodness_of_fit_ref 1.0482 _refine_ls_shift/su_max 0.003819 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 5.39 -7.19 4.08 -1.91 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Siemens Industrial Automation, Inc (1993) SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type S1 S 0.2634(4) 0.0672(5) 0.1786(2) 0.0153 1.0000 Uani O1 O 0.0977(11) -0.1105(14) 0.1897(8) 0.0313(18) 1.0000 Uiso O2 O 0.3166(12) -0.0691(13) 0.0321(7) 0.0217(16) 1.0000 Uiso O3 O 0.407(1) 0.0353(14) 0.3297(7) 0.0261(18) 1.0000 Uiso O4 O 0.1984(13) 0.3515(13) 0.1284(7) 0.0271(18) 1.0000 Uiso H1 H 0.1278 -0.2901 0.2053 0.0426 1.0000 Uiso H2 H 0.3569 -0.2415 0.0587 0.0426 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.010(4) 0.0183(19) 0.0190(14) -0.0001(8) 0.006(2) 0.0003(13) _refine_ls_extinction_coef 12.5(43) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 . O1 . 1.537(7) yes S1 . O2 . 1.537(5) yes S1 . O3 . 1.416(6) yes S1 . O4 . 1.407(6) yes O1 . H1 . 0.850 no O2 . H2 . 0.850 no O1 . O4 1_545 2.668(9) yes O1 . H1 3_555 2.614 no O2 . O3 3_645 2.765(11) yes O2 . H1 4_544 2.764 no O3 . H2 3_655 2.049 no O3 . H2 4_545 2.463 no O4 . H1 1_565 1.895 no O4 . H2 1_565 2.387 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . S1 . O2 . 105.0(4) yes O1 . S1 . O3 . 109.3(4) yes O2 . S1 . O3 . 110.5(5) yes O1 . S1 . O4 . 106.0(5) yes O2 . S1 . O4 . 106.8(4) yes O3 . S1 . O4 . 118.3(4) yes S1 . O1 . H1 . 108.901 no S1 . O2 . H2 . 109.114 no O1 . H1 . O4 1_545 151 no O2 . H2 . O3 3_645 142 no