data_2100457 _publ_contact_author_email S.Parsons@ed.ac.uk _publ_contact_author_name 'Simon Parsons' _journal_coeditor_code WS5036 _journal_date_accepted 2006-01-17 _journal_date_recd_electronic 2005-08-15 _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section B' _journal_page_first 280 _journal_page_last 286 _journal_paper_category FA _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'C2 H6 O4 S1' _chemical_formula_sum 'C2 H6 O4 S1' _chemical_formula_weight 126.13 _chemical_melting_point ? _chemical_name_systematic 'Dimethyl sulfate' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M I2/a _atom_sites_solution_hydrogens geom _atom_sites_solution_primary Patterson _audit_creation_method CRYSTALS_ver_12.80 _cell_angle_alpha 90 _cell_angle_beta 101.690(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9007(10) _cell_length_b 5.8099(7) _cell_length_c 10.2451(13) _cell_measurement_reflns_used 1208 _cell_measurement_temperature 180 _cell_measurement_theta_max 27 _cell_measurement_theta_min 4 _cell_volume 518.81(11) _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _diffrn_ambient_temperature 180 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method '\f & \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1542 _diffrn_reflns_theta_full 30.024 _diffrn_reflns_theta_max 30.024 _diffrn_reflns_theta_min 2.768 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_T_max 0.67 _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Twinabs (Sheldrick, 2004)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_meas ? _exptl_crystal_description cylinder _exptl_crystal_F_000 264 _exptl_crystal_size_max 4.00 _exptl_crystal_size_mid 0.75 _exptl_crystal_size_min 0.75 _refine_diff_density_max 0.42 _refine_diff_density_min -0.31 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9572 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 46 _refine_ls_number_reflns 1513 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0435 _refine_ls_shift/su_max 0.000085 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(F^2^) + 0.06 + 0.39P] where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1194 _refine_ls_wR_factor_gt 0.1115 _refine_ls_wR_factor_ref 0.1194 _reflns_number_gt 1094 _reflns_number_total 1542 _reflns_threshold_expression I>2.00u(I) loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 -x+1/2,y,-z x+1/2,-y,z -x+1,y+1/2,-z+1/2 x+1,-y+1/2,z+1/2 loop_ _atom_site_type_symbol _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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.2500 0.05535(11) 0.0000 0.0307 Uani 1.0000 . . O O2 0.24628(15) -0.0651(3) -0.12034(14) 0.0444 Uani 1.0000 . . O O3 0.38979(13) 0.2207(2) 0.01353(12) 0.0345 Uani 1.0000 . . C C4 0.4260(2) 0.3630(4) 0.1333(2) 0.0435 Uani 1.0000 . . H H41 0.5311(19) 0.405(4) 0.150(2) 0.0757(19) Uiso 1.0000 . . H H42 0.404(2) 0.284(3) 0.2052(17) 0.0752(19) Uiso 1.0000 . . H H43 0.367(2) 0.499(3) 0.1241(19) 0.0742(19) Uiso 1.0000 . . 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 0.0296(3) 0.0260(3) 0.0347(3) 0.0000 0.0020(2) 0.0000 O2 0.0461(8) 0.0392(8) 0.0446(8) 0.0014(6) 0.0013(6) -0.0149(7) O3 0.0297(6) 0.0356(7) 0.0380(7) -0.0052(5) 0.0070(5) -0.0064(6) C4 0.0485(12) 0.0376(10) 0.0413(11) -0.0078(9) 0.0022(9) -0.0081(9) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 'International Tables Vol C 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 S1 O2 5_555 . 5_555 105.10(7) yes O3 S1 O2 5_555 . . 110.57(7) yes O2 S1 O2 5_555 . . 120.59(13) yes O3 S1 O3 5_555 . . 103.74(10) yes O2 S1 O3 5_555 . . 110.57(7) yes O2 S1 O3 . . . 105.10(7) yes S1 O3 C4 . . . 117.45(12) yes O3 C4 H41 . . . 109.8(12) no O3 C4 H42 . . . 110.0(12) no H41 C4 H42 . . . 110.2(13) no O3 C4 H43 . . . 111.6(12) no H41 C4 H43 . . . 108.2(14) no H42 C4 H43 . . . 107.0(14) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O3 . 5_555 1.5556(13) yes S1 O2 . 5_555 1.4122(14) yes S1 O2 . . 1.4122(14) yes S1 O3 . . 1.5556(13) yes O3 C4 . . 1.460(2) yes C4 H41 . . 0.948(16) no C4 H42 . . 0.922(16) no C4 H43 . . 0.941(16) no