#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100423.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2100423 _publ_contact_author_name 'Stephen A. Moggach' _journal_coeditor_code BS5023 _journal_date_accepted 2005-11-22 _journal_date_recd_electronic 2005-09-20 _journal_issue 2 _journal_name_full 'Acta Crystallographica, Section B' _journal_page_first 296 _journal_page_last 309 _journal_paper_category FA _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'C3 H7 N1 O2 S1' _chemical_formula_sum 'C3 H7 N1 O2 S1' _chemical_formula_weight 121.16 _chemical_melting_point ? _chemical_name_systematic ? _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1 ' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary geom _audit_creation_method CRYSTALS_ver_12.82 _cell_angle_alpha 90 _cell_angle_beta 94.897(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.105(3) _cell_length_b 5.4420(8) _cell_length_c 10.916(4) _cell_measurement_reflns_used 337 _cell_measurement_temperature 293 _cell_measurement_theta_max 37 _cell_measurement_theta_min 8 _cell_volume 479.7(2) _computing_cell_refinement 'SAINT ' _computing_data_collection 'SMART ' _computing_data_reduction 'SAINT ' _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 'USER DEFINED STRUCTURE SOLUTION' _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.534 _diffrn_measured_fraction_theta_max 0.427 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.166 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 937 _diffrn_reflns_theta_full 17.415 _diffrn_reflns_theta_max 23.220 _diffrn_reflns_theta_min 3.011 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_correction_T_min 0.01 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS ' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 256 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.19 _refine_diff_density_min -0.99 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.1464 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 395 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.2027 _refine_ls_R_factor_gt 0.1437 _refine_ls_shift/su_max 0.000045 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.10 0.669 1.21 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.3324 _refine_ls_wR_factor_gt 0.1620 _refine_ls_wR_factor_ref 0.1620 _reflns_number_gt 395 _reflns_number_total 613 _reflns_threshold_expression I>2.00u(I) loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z 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 S12 0.3425(13) -0.1344(15) 1.0265(11) 0.011(2) Uiso 1.0000 . . C C12 0.298(3) 0.008(4) 0.8777(17) 0.023(3) Uiso 1.0000 . . N N12 -0.007(3) 0.036(4) 0.876(3) 0.023(3) Uiso 1.0000 . . O O12 0.228(3) -0.456(3) 0.750(3) 0.023(3) Uiso 1.0000 . . C C22 0.133(2) -0.071(2) 0.8138(17) 0.023(3) Uiso 1.0000 . . O O22 0.000(3) -0.453(3) 0.850(3) 0.023(3) Uiso 1.0000 . . C C32 0.121(3) -0.352(2) 0.806(3) 0.023(3) Uiso 1.0000 . . S S11 0.1148(17) -0.2314(15) 0.4465(14) 0.027(3) Uiso 1.0000 . . C C11 0.215(4) 0.062(3) 0.430(3) 0.020(3) Uiso 1.0000 . . N N11 0.476(3) -0.089(4) 0.354(3) 0.020(3) Uiso 1.0000 . . O O11 0.318(3) 0.447(3) 0.217(2) 0.020(3) Uiso 1.0000 . . C C21 0.329(2) 0.071(2) 0.327(2) 0.020(3) Uiso 1.0000 . . O O21 0.497(3) 0.412(3) 0.380(3) 0.020(3) Uiso 1.0000 . . C C31 0.386(3) 0.333(3) 0.306(2) 0.020(3) Uiso 1.0000 . . H H31 0.2807 0.0995 0.5073 0.0305 Uiso 1.0000 . . H H21 0.1290 0.1874 0.4141 0.0305 Uiso 1.0000 . . H H41 0.2676 0.0130 0.2508 0.0305 Uiso 1.0000 . . H H51 0.5423 -0.0810 0.2908 0.0305 Uiso 1.0000 . . H H61 0.5335 -0.0381 0.4245 0.0305 Uiso 1.0000 . . H H71 0.4423 -0.2473 0.3631 0.0305 Uiso 1.0000 . . H H22 0.2964 0.1868 0.8888 0.0344 Uiso 1.0000 . . H H32 0.3860 -0.0361 0.8255 0.0344 Uiso 1.0000 . . H H42 0.1268 -0.0072 0.7296 0.0344 Uiso 1.0000 . . H H52 -0.1043 -0.0137 0.8362 0.0344 Uiso 1.0000 . . H H62 -0.0009 -0.0161 0.9553 0.0344 Uiso 1.0000 . . H H72 -0.0003 0.2028 0.8739 0.0344 Uiso 1.0000 . . 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' N 0.0061 0.0033 '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 S12 C12 C22 . . . 113.1(8) yes S12 C12 H22 . . . 108.6 no C22 C12 H22 . . . 108.6 no S12 C12 H32 . . . 108.6 no C22 C12 H32 . . . 108.6 no H22 C12 H32 . . . 109.5 no C22 N12 H52 . . . 109.5 no C22 N12 H62 . . . 109.5 no H52 N12 H62 . . . 109.5 no C22 N12 H72 . . . 109.5 no H52 N12 H72 . . . 109.5 no H62 N12 H72 . . . 109.5 no C12 C22 N12 . . . 110.8(9) yes C12 C22 C32 . . . 111.1(9) yes N12 C22 C32 . . . 111.3(8) yes C12 C22 H42 . . . 107.8 no N12 C22 H42 . . . 107.8 no C32 C22 H42 . . . 107.8 no C22 C32 O22 . . . 118.0(7) yes C22 C32 O12 . . . 115.9(7) yes O22 C32 O12 . . . 126.0(8) yes S11 C11 C21 . . . 114.2(8) yes S11 C11 H31 . . . 108.3 no C21 C11 H31 . . . 108.3 no S11 C11 H21 . . . 108.3 no C21 C11 H21 . . . 108.3 no H31 C11 H21 . . . 109.5 no C21 N11 H51 . . . 109.5 no C21 N11 H61 . . . 109.5 no H51 N11 H61 . . . 109.5 no C21 N11 H71 . . . 109.5 no H51 N11 H71 . . . 109.5 no H61 N11 H71 . . . 109.5 no C11 C21 N11 . . . 111.1(9) yes C11 C21 C31 . . . 110.5(9) yes N11 C21 C31 . . . 109.3(8) yes C11 C21 H41 . . . 108.6 no N11 C21 H41 . . . 108.6 no C31 C21 H41 . . . 108.6 no C21 C31 O11 . . . 117.3(7) yes C21 C31 O21 . . . 116.5(7) yes O11 C31 O21 . . . 126.3(7) yes 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 S12 C12 . . 1.808(9) yes C12 C22 . . 1.515(9) yes C12 H22 . . 0.980 no C12 H32 . . 0.980 no N12 C22 . . 1.488(10) yes N12 H52 . . 0.910 no N12 H62 . . 0.910 no N12 H72 . . 0.910 no O12 C32 . . 1.240(9) yes C22 C32 . . 1.534(9) yes C22 H42 . . 0.980 no O22 C32 . . 1.246(9) yes S11 C11 . . 1.808(9) yes C11 C21 . . 1.520(9) yes C11 H31 . . 0.980 no C11 H21 . . 0.980 no N11 C21 . . 1.488(9) yes N11 H51 . . 0.910 no N11 H61 . . 0.910 no N11 H71 . . 0.910 no O11 C31 . . 1.240(9) yes C21 C31 . . 1.522(9) yes C21 H41 . . 0.980 no O21 C31 . . 1.233(9) yes