#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/37/2003790.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_2003790 loop_ _publ_author_name 'Hellier, D. G.' 'Motevalli, M.' _publ_section_title ; 5-tert-Butyl-5-methyl-1,3,2-dioxathiane 2,2-Dioxide ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1701 _journal_page_last 1703 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C8 H16 O4 S' _chemical_formula_weight 208.27 _chemical_name_systematic ; ? ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.6790(10) _cell_length_b 11.3100(10) _cell_length_c 7.8470(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 238(5) _cell_measurement_theta_max 17 _cell_measurement_theta_min 11 _cell_volume 1036.51(18) _computing_cell_refinement 'CAD4/PC software' _computing_data_collection 'CAD4/PC software' _computing_data_reduction 'CAD4/PC software' _computing_molecular_graphics 'PLUTON (spek, 1993)' _computing_publication_material SHELXL-93 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4 four-circle' _diffrn_measurement_method 2\q,\w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0023 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1231 _diffrn_reflns_theta_max 24.92 _diffrn_reflns_theta_min 2.51 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_type 'empirical (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas 1.34 _exptl_crystal_density_method 'flotation in ?' _exptl_crystal_description 'transparent rhombic' _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.096 _refine_diff_density_min -0.129 _refine_ls_abs_structure_Flack -0.21(13) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_obs 1.017 _refine_ls_matrix_type full _refine_ls_number_parameters 182 _refine_ls_number_reflns 896 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_restrained_S_obs 1.017 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_obs 0.0248 _refine_ls_shift/esd_max -0.158 _refine_ls_shift/esd_mean 0.028 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0224P)^2^+0.4095P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_wR_factor_all 0.0574 _refine_ls_wR_factor_obs 0.0570 _reflns_number_observed 896 _reflns_number_total 1231 _reflns_observed_criterion >2\s(I) _[local]_cod_data_source_file hu1071.cif _[local]_cod_data_source_block qmcds1 _cod_original_cell_volume 1036.5(2) _cod_database_code 2003790 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016 H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000 O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.0060 S S 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.1234 loop_ _atom_site_label _atom_site_occupancy _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_type_symbol S1 1 0.28028(7) 0.82634(7) 0.94821(11) 0.0482(2) Uani d S O1 1 0.2139(2) 0.7629(2) 0.8292(3) 0.0702(7) Uani d O O2 1 0.2611(2) 0.8107(2) 1.1246(3) 0.0663(7) Uani d O O3 1 0.2699(2) 0.9589(2) 0.9007(3) 0.0492(5) Uani d O O4 1 0.4073(2) 0.8002(2) 0.9056(3) 0.0511(6) Uani d O C1 1 0.3514(3) 1.0397(3) 0.9876(5) 0.0448(8) Uani d C C2 1 0.4746(2) 1.0054(2) 0.9486(4) 0.0397(6) Uani d C C3 1 0.4907(3) 0.8761(3) 0.9957(5) 0.0506(9) Uani d C C4 1 0.4962(4) 1.0191(4) 0.7568(5) 0.0661(10) Uani d C C5 1 0.5582(2) 1.0840(3) 1.0594(5) 0.0485(7) Uani d C C6 1 0.6827(3) 1.0620(5) 1.0059(7) 0.0754(13) Uani d C C7 1 0.5314(4) 1.2154(3) 1.0334(6) 0.0632(10) Uani d C C8 1 0.5481(4) 1.0572(4) 1.2508(5) 0.0644(10) Uani d C H11 1 0.3325(25) 1.0399(27) 1.0980(42) 0.039(8) Uiso d H H12 1 0.3288(23) 1.1200(25) 0.9403(38) 0.048(8) Uiso d H H31 1 0.5656(30) 0.8445(30) 0.9579(52) 0.081(11) Uiso d H H32 1 0.4844(31) 0.8601(31) 1.1155(47) 0.065(11) Uiso d H H41 1 0.4459(36) 0.9801(33) 0.6788(50) 0.082(13) Uiso d H H42 1 0.5118(47) 1.1030(45) 0.7145(63) 0.121(18) Uiso d H H43 1 0.5789(59) 0.9792(56) 0.7210(86) 0.193(30) Uiso d H H61 1 0.7303(31) 1.1090(33) 1.0675(52) 0.075(12) Uiso d H H62 1 0.7013(35) 1.0936(38) 0.8844(53) 0.086(13) Uiso d H H63 1 0.7060(31) 0.9750(37) 1.0168(53) 0.092(14) Uiso d H H71 1 0.4506(26) 1.2368(27) 1.0834(42) 0.055(10) Uiso d H H72 1 0.5903(30) 1.2648(31) 1.0982(46) 0.068(11) Uiso d H H73 1 0.5356(33) 1.2337(32) 0.9266(52) 0.065(12) Uiso d H H81 1 0.5990(33) 1.1172(35) 1.3152(51) 0.090(13) Uiso d H H82 1 0.4686(42) 1.0736(43) 1.2959(57) 0.108(17) Uiso d H H83 1 0.5835(39) 0.9813(39) 1.2700(63) 0.103(17) Uiso d H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 S1 0.0456(4) -0.0023(4) -0.0020(4) 0.0450(4) 0.0047(4) 0.0539(4) O1 0.067(2) -0.0197(13) -0.015(2) 0.0608(14) -0.0052(13) 0.083(2) O2 0.069(2) 0.0020(13) 0.0125(12) 0.069(2) 0.0157(12) 0.0605(14) O3 0.0414(10) 0.0028(9) -0.0108(11) 0.0461(11) 0.0071(10) 0.0601(13) O4 0.0473(11) 0.0028(9) 0.0038(11) 0.0410(12) -0.0064(11) 0.0650(15) C1 0.044(2) 0.0016(13) -0.0028(15) 0.042(2) -0.0008(14) 0.049(2) C2 0.0391(14) 0.0029(11) 0.0026(15) 0.0398(14) 0.002(2) 0.0403(15) C3 0.044(2) 0.0060(14) -0.003(2) 0.043(2) 0.001(2) 0.065(3) C4 0.083(3) -0.014(2) 0.007(2) 0.069(3) 0.001(2) 0.046(2) C5 0.046(2) -0.0070(14) -0.001(2) 0.050(2) 0.000(2) 0.049(2) C6 0.043(2) -0.014(2) 0.003(2) 0.081(3) -0.003(3) 0.102(4) C7 0.084(3) -0.007(2) 0.000(3) 0.046(2) -0.003(2) 0.059(3) C8 0.067(2) -0.011(2) -0.014(2) 0.073(3) 0.001(2) 0.053(2) 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 O1 S1 O2 119.9(2) yes O1 S1 O3 106.85(14) yes O2 S1 O3 110.14(14) yes O1 S1 O4 106.66(15) yes O2 S1 O4 109.82(14) yes O3 S1 O4 101.97(11) yes C1 O3 S1 115.8(2) yes C3 O4 S1 114.7(2) yes O3 C1 C2 110.9(3) yes C3 C2 C1 108.3(3) yes C3 C2 C4 108.4(3) yes C1 C2 C4 109.1(3) yes C3 C2 C5 109.3(2) yes C1 C2 C5 109.3(2) yes C4 C2 C5 112.4(3) yes O4 C3 C2 111.1(2) yes C6 C5 C7 108.3(3) yes C6 C5 C8 108.0(3) yes C7 C5 C8 107.8(4) yes C6 C5 C2 110.1(3) yes C7 C5 C2 110.2(3) yes C8 C5 C2 112.3(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 O1 1.410(3) yes S1 O2 1.413(2) yes S1 O3 1.549(2) yes S1 O4 1.549(2) yes O3 C1 1.486(4) yes O4 C3 1.478(4) yes C1 C2 1.521(4) yes C2 C3 1.521(4) yes C2 C4 1.534(5) yes C2 C5 1.580(4) yes C5 C6 1.534(5) yes C5 C7 1.533(5) yes C5 C8 1.537(5) yes