#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/03/2010345.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_2010345 loop_ _publ_author_name 'Heinemann, F.W.' 'Hartung, H.' 'Cleve, D.' 'Rudorf, W.-D.' _publ_section_title ; 2-[Bis(methoxycarbonyl)methylene]-3-phenyl-1,3-thiazolidine ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1986 _journal_page_last 1988 _journal_paper_doi 10.1107/S0108270194003574 _journal_volume 50 _journal_year 1994 _chemical_formula_sum 'C14 H15 N O4 S' _chemical_formula_weight 293.34 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source 'SHELX76 (Sheldrick, 1976)' _cell_angle_alpha 90. _cell_angle_beta 90.870(10) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 15.224(2) _cell_length_b 6.0680(10) _cell_length_c 14.9680(10) _cell_measurement_reflns_used 86 _cell_measurement_temperature 293 _cell_measurement_theta_max 14.0 _cell_measurement_theta_min 10.0 _cell_volume 1382.6(3) _diffrn_measurement_device 'Stoe Stadi-4' _diffrn_measurement_method \w/\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3638 _diffrn_reflns_theta_max 27.5 _diffrn_standards_decay_% +-3.5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.23 _exptl_absorpt_correction_type none _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.409 _exptl_crystal_description prism _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.257 _refine_diff_density_min -0.204 _refine_ls_extinction_coef '\c = 1.38(5)' _refine_ls_extinction_method 'empirical, F~corr~ = F~c~(1 - 10^-7^\cF~c~^2^/sin\q)' _refine_ls_goodness_of_fit_obs 4.63 _refine_ls_number_parameters 242 _refine_ls_number_reflns 2531 _refine_ls_R_factor_obs 0.039 _refine_ls_shift/esd_max 0.019 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 3.19/[\s^2^(F~o~) + 0.00005F~o~^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.046 _reflns_number_observed 2531 _reflns_number_total 2972 _reflns_observed_criterion F~o~>4.0\s(F~o~) _cod_data_source_file sh1096.cif _cod_data_source_block sh1096_structure_1_of_1 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 3.19/[\s^2^(F~o~) + 0.00005F~o~^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 3.19/[\s^2^(F~o~) + 0.00005F~o~^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1382.6 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2010345 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv S1 .91248(3) .18160(9) .48686(3) .0484(2) O1 .69535(9) .0145(2) .23140(10) .0570(5) O2 .92456(9) -.1649(2) .37684(9) .0562(5) O3 .75243(8) .3516(2) .24372(8) .0484(4) O4 .86288(8) -.1800(2) .24076(8) .0479(4) N1 .76648(9) .3720(3) .44400(10) .0441(5) C1 .82080(10) .2113(3) .41540(10) .0361(5) C2 .80960(10) .0835(3) .33950(10) .0347(5) C3 .8808(2) .4108(6) .5553(2) .0800(10) C4 .8014(2) .5147(4) .51550(10) .0542(7) C5 .67610(10) .3952(3) .41800(10) .0420(5) C6 .61920(10) .2213(4) .42890(10) .0484(6) C7 .53140(10) .2479(5) .4064(2) .0645(8) C8 .5008(2) .4455(5) .3734(2) .0748(10) C9 .5582(2) .6179(5) .3632(2) .0780(10) C10 .6460(2) .5942(4) .3863(2) .0632(8) C11 .74520(10) .1395(3) .26770(10) .0373(5) C12 .86990(10) -.0972(3) .32380(10) .0375(5) C13 .6902(2) .4319(5) .1776(2) .0720(10) C14 .9244(2) -.3534(4) .2197(2) .0582(8) H6 .6410(10) .086(4) .4510(10) .049(5) H7 .497(2) .116(4) .415(2) .075(8) H8 .442(2) .468(5) .359(2) .101(9) H9 .538(2) .761(5) .339(2) .097(9) H10 .685(2) .714(4) .375(2) .091(9) H31 .862(2) .348(6) .625(3) .162(15) H32 .924(2) .488(5) .571(2) .103(10) H41 .817(2) .651(5) .486(2) .114(11) H42 .755(2) .538(4) .557(2) .079(7) H131 .700(2) .363(6) .123(2) .126(12) H132 .625(2) .386(5) .195(2) .097(9) H133 .698(2) .587(6) .168(2) .115(11) H141 .984(2) -.294(4) .221(2) .085(8) H142 .916(2) -.476(4) .260(2) .077(8) H143 .909(2) -.393(5) .159(2) .108(10) 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 C1 S1 C3 92.87(11) yes C1 N1 C4 115.99(15) yes C1 N1 C5 125.15(15) yes C4 N1 C5 118.39(16) yes S1 C1 N1 111.50(12) yes S1 C1 C2 121.99(13) yes N1 C1 C2 126.50(15) yes C1 C2 C11 122.57(15) yes C1 C2 C12 119.04(14) yes C11 C2 C12 117.98(14) yes S1 C3 C4 108.95(19) yes N1 C4 C3 109.1(2) yes C11 O3 C13 116.86(17) yes C12 O4 C14 115.50(15) no S1 C3 H32 112.(2) no S1 C3 H31 109.6(19) no C4 C3 H32 120.(2) no C4 C3 H31 106.7(18) no C3 C4 H42 114.10(15) no C3 C4 H41 109.9(18) no N1 C4 H42 107.2(14) no N1 C4 H41 105.2(19) no N1 C5 C10 119.72(17) no N1 C5 C6 119.74(17) no C6 C5 C10 120.46(18) no C5 C6 H6 119.7(12) no C5 C6 C7 119.3(2) no C7 C6 H6 121.1(12) no C6 C7 H7 112.9(15) no C6 C7 C8 120.7(2) no C8 C7 H7 126.4(14) no C7 C8 H8 122.0(17) no C7 C8 C9 119.5(2) no C9 C8 H8 118.5(17) no C8 C9 H9 121.2(16) no C8 C9 C10 120.4(3) no C10 C9 H9 118.4(16) no C5 C10 C9 119.7(2) no C9 C10 H10 118.2(16) no C5 C10 H10 121.9(16) no O3 C11 C2 110.98(15) no O1 C11 C2 126.25(17) no O1 C11 O3 122.68(16) no O4 C12 C2 112.96(14) no O2 C12 C2 125.41(16) no O2 C12 O4 121.55(16) 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 C1 . . 1.754(2) yes S1 C3 . . 1.797(3) yes O1 C11 . . 1.198(2) yes O2 C12 . . 1.213(2) yes O3 C11 . . 1.341(2) yes O4 C12 . . 1.343(2) yes N1 C1 . . 1.352(2) yes N1 C4 . . 1.470(3) yes N1 C5 . . 1.431(2) yes C1 C2 . . 1.385(2) yes C2 C11 . . 1.482(2) yes C2 C12 . . 1.452(2) yes C3 C4 . . 1.480(4) yes C3 H31 . . 1.15(4) no C3 H32 . . 0.83(3) no C4 H41 . . 0.97(3) no C4 H42 . . 0.96(2) no C5 C6 . . 1.377(3) no C5 C10 . . 1.374(3) no C6 C7 . . 1.384(3) no C6 H6 . . 0.94(2) no C7 C8 . . 1.375(4) no C7 H7 . . 0.96(3) no C8 C9 . . 1.373(4) no C8 H8 . . 0.93(3) no C9 C10 . . 1.383(4) no C9 H9 . . 0.99(3) no C10 H10 . . 0.95(3) no C13 H131 . . 0.93(3) no C13 H132 . . 1.06(3) no C13 H133 . . 0.96(3) no C14 H141 . . 0.97(3) no C14 H142 . . 0.96(3) no C14 H143 . . 0.97(3) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C3 S1 C1 N1 -4.0(2) C1 S1 C3 C4 -4.0(2) C3 S1 C1 C2 175.1(2) C4 N1 C1 S1 11.5(2) C5 N1 C1 S1 -160.60(10) C4 N1 C1 C2 -167.6(2) C5 N1 C1 C2 20.4(3) C1 N1 C4 C3 -14.4(2) C5 N1 C4 C3 158.2(3) C13 O3 C11 O1 6.6(3) C13 O3 C11 C2 -176.7(2) C14 O4 C12 O2 0.0(2) C14 O4 C12 C2 177.0(2) N1 C1 C2 C11 13.8(3) S1 C1 C2 C11 -165.20(10) N1 C1 C2 C12 -173.7(2) S1 C1 C2 C12 7.3(2) C1 C2 C11 O1 -134.7(2) C1 C2 C11 O3 48.7(2) C12 C2 C11 O1 52.8(2) C12 C2 C11 O3 -123.8(2) C1 C2 C12 O2 9.1(3) C1 C2 C12 O4 -167.8(2) C11 C2 C12 O2 -178.2(2) C11 C2 C12 O4 4.9(2) S1 C3 C4 N1 10.4(2)