#------------------------------------------------------------------------------ #$Date: 2009-11-18 15:56:34 +0100 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100459.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_2100459 _publ_contact_author_address ; ISIS Facility CCLRC - Rutherford Appleton Laboratory Chilton, Didcot Oxfordshire UK OX11 0QX ; _publ_contact_author_email r.m.ibberson@rl.ac.uk _publ_contact_author_fax '+44 (0)1235 445383' _publ_contact_author_name 'Richard M Ibberson' _publ_contact_author_phone '+44 (0)1235 445871' _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 D6 O4 S1' _chemical_formula_structural (CD3O)2SO2 _chemical_formula_sum 'C2 D6 O4 S' _[local]_cod_chemical_formula_sum_orig 'C2 D6 O4 S1' _chemical_formula_weight 132.17 _chemical_melting_point 241 _chemical_name_common 'dimethyl sulphate' _chemical_name_systematic ; dimethyl sulfate ; _symmetry_cell_setting Monoclinic _cell_angle_alpha 90.0 _cell_angle_beta 100.4404(8) _cell_angle_gamma 90.0 _cell_formula_units_Z 4 _cell_length_a 8.68731(7) _cell_length_b 5.82756(4) _cell_length_c 9.94376(6) _cell_measurement_temperature 5.0 _cell_volume 495.076(5) _computing_cell_refinement 'TOPAS-Academic (Coelho, 2000)' _computing_data_collection 'ISIS Instrument control program (ICP)' _computing_data_reduction 'Standard HRPD normalisation routines' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _computing_structure_refinement 'TOPAS-Academic (Coelho, 2000)' _computing_structure_solution 'TOPAS-Academic (Coelho, 2000)' _diffrn_ambient_temperature 5 _diffrn_measurement_device_type HRPD _diffrn_radiation_type 'time-of-flight neutron' _diffrn_radiation_wavelength 1.24-5.36 _exptl_crystal_density_diffrn 1.77290(10) _exptl_crystal_density_meas 'not measured' _refine_diff_density_max 0.097 _refine_diff_density_min -0.096 _refine_ls_goodness_of_fit_all 1.64 _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.01 _refine_ls_weighting_scheme sigma _reflns_number_observed 866 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt I2/a _space_group_IT_number 15 _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _[local]_cod_cif_authors_sg_H-M I2/a loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x+1/2,+y,-z -1 -x,-y,-z -2 +x+1/2,-y,+z 101 +x+1/2,+y+1/2,+z+1/2 102 -x,+y+1/2,-z+1/2 -101 -x+1/2,-y+1/2,-z+1/2 -102 +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 C4 0.0118(8) 0.0068(6) 0.0092(8) -0.0017(6) 0.0099(6) -0.0022(5) D41 0.0241(9) 0.0309(9) 0.0291(10) -0.0069(6) 0.0146(7) -0.0138(6) D42 0.0449(10) 0.0199(7) 0.01739(9) -0.0059(7) 0.0161(7) 0.0015(7) D43 0.0355(8) 0.0173(7) 0.0286(10) 0.0061(8) 0.0076(6) -0.0067(5) 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_thermal_displace_type _atom_site_occupancy S S1 0.25 0.05420(13) 0.0 0.0114(10) Uiso 1.0 O O2 0.24746(15) -0.0699(2) -0.12374(13) 0.0112(4) Uiso 1.0 O O3 0.39331(15) 0.2193(2) 0.01225(13) 0.0083(4) Uiso 1.0 C C4 0.42650(17) 0.3603(2) 0.13327(15) 0.01096 Uani 1.0 D D41 0.5489(2) 0.4076(2) 0.14393(15) 0.03086 Uani 1.0 D D42 0.40904(19) 0.2673(2) 0.22299(15) 0.03163 Uani 1.0 D D43 0.35188(19) 0.5157(2) 0.11936(17) 0.03117 Uani 1.0 loop_ _atom_type_symbol _atom_type_scat_source S International_Tables_Vol_C O International_Tables_Vol_C C International_Tables_Vol_C D International_Tables_Vol_C 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 O2 S1 O2 1_555 2_555 118.97(10) N O2 S1 O3 1_555 1_555 105.53(6) N O2 S1 O3 1_555 2_555 111.00(7) N O2 S1 O3 2_555 1_555 111.00(7) N O2 S1 O3 2_555 2_555 105.53(6) N O3 S1 O3 1_555 2_555 103.85(9) N S1 O3 C4 1_555 1_555 116.89(9) N O3 C4 D41 1_555 1_555 105.70(13) N O3 C4 D42 1_555 1_555 111.56(14) N O3 C4 D43 1_555 1_555 109.71(15) N D41 C4 D42 1_555 1_555 109.24(17) N D41 C4 D43 1_555 1_555 110.20(15) N D42 C4 D43 1_555 1_555 110.34(16) N 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 S1 O2 1_555 1.4239(13) N S1 O2 2_555 1.4239(13) N S1 O3 1_555 1.5609(13) N S1 O3 2_555 1.5609(13) N S1 C4 1_555 2.5598(13) N S1 C4 2_555 2.5598(13) N O2 S1 1_555 1.4239(13) N O3 S1 1_555 1.5609(13) N O3 C4 1_555 1.4421(19) N O3 D41 1_555 2.026(2) N C4 S1 1_555 2.5598(13) N C4 O3 1_555 1.4421(19) N C4 D41 1_555 1.0851(16) N C4 D42 1_555 1.0778(16) N C4 D43 1_555 1.1079(15) N D41 O3 1_555 2.026(2) N D41 C4 1_555 1.0851(16) N D41 D42 1_555 1.764(2) N D41 D43 1_555 1.799(2) N D42 C4 1_555 1.0778(16) N D42 D41 1_555 1.764(2) N D42 D43 1_555 1.794(2) N D43 C4 1_555 1.1079(15) N D43 D41 1_555 1.799(2) N D43 D42 1_555 1.794(2) N