#------------------------------------------------------------------------------ #$Date: 2008-01-27 16:50:57 +0200 (Sun, 27 Jan 2008) $ #$Revision: 30 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1000021.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_1000021 loop_ _publ_author_name 'Gzella, Andrzej' 'Rozwadowska, Maria D.' 'Sulima, Agnieszka' _publ_section_title ; Two dihydro-5H-thiazolinono[2,3-a]isoquinoline S-oxides ; _journal_issue 12 _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first 1454 _journal_page_last 1456 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C13 H15 N O4 S' _chemical_formula_moiety 'C13 H15 N O4 S' _chemical_formula_sum 'C13 H15 N O4 S' _chemical_formula_weight 281.32 _chemical_name_systematic ; 8,9-Dimethoxy-6,10b-dihydro-1-oxo-5H-thiazolo[2,3-a]isoquinolin-3-one ; _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.967(11) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.967(2) _cell_length_b 7.5484(9) _cell_length_c 9.1666(13) _cell_measurement_reflns_used 49 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.8 _cell_measurement_theta_min 14.3 _cell_volume 1346.3(3) _computing_cell_refinement 'KM-4 Software' _computing_data_collection 'KM-4 Software (Kuma, 1991)' _computing_data_reduction 'KM-4 Software' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WINGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-7 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .996 _diffrn_measured_fraction_theta_max .996 _diffrn_measurement_device_type 'Kuma KM-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents .0437 _diffrn_reflns_av_sigmaI/netI .0230 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2735 _diffrn_reflns_theta_full 70.17 _diffrn_reflns_theta_max 70.17 _diffrn_reflns_theta_min 2.27 _diffrn_standards_decay_% 3.5 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.239 _exptl_absorpt_correction_T_max .611 _exptl_absorpt_correction_T_min .455 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 592 _exptl_crystal_size_max .50 _exptl_crystal_size_mid .33 _exptl_crystal_size_min .22 _refine_diff_density_max .856 _refine_diff_density_min -.330 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 174 _refine_ls_number_reflns 2556 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all .0641 _refine_ls_R_factor_gt .0499 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1120P)^2^+0.4410P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .1464 _refine_ls_wR_factor_ref .1583 _reflns_number_gt 2119 _reflns_number_total 2556 _reflns_threshold_expression I>2\s(I) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol S1 .13739(3) .30932(7) .08402(6) .0381(2) Uani d . 1 S C2 .04978(12) .2658(3) -.0144(3) .0394(5) Uani d . 1 C H2A .0199 .2591 .0556 .047 Uiso calc . 1 H H2B .0333 .3595 -.0859 .047 Uiso calc . 1 H C3 .05037(11) .0913(3) -.0942(2) .0372(5) Uani d . 1 C N4 .10504(10) -.0061(2) -.0283(2) .0382(4) Uani d . 1 N C5 .12147(14) -.1796(3) -.0795(3) .0486(6) Uani d . 1 C H5A .0893 -.2090 -.1725 .058 Uiso calc . 1 H H5B .1174 -.2685 -.0056 .058 Uiso calc . 1 H C6 .19420(14) -.1792(3) -.1039(3) .0483(6) Uani d . 1 C H6A .2074 -.2995 -.1221 .058 Uiso calc . 1 H H6B .1956 -.1091 -.1918 .058 Uiso calc . 1 H C6A .24505(12) -.1045(3) .0293(2) .0389(5) Uani d . 1 C C7 .31396(13) -.1563(3) .0586(3) .0464(6) Uani d . 1 C H7A .3281 -.2366 -.0053 .056 Uiso calc . 1 H C8 .36166(12) -.0910(3) .1801(3) .0449(6) Uani d . 1 C C9 .33926(12) .0297(3) .2768(2) .0400(5) Uani d . 1 C C10 .27133(12) .0793(3) .2498(2) .0371(5) Uani d . 1 C H10 .2569 .1576 .3149 .044 Uiso calc . 1 H C10A .22341(11) .0135(3) .1255(2) .0336(5) Uani d . 1 C C10B .14946(11) .0668(3) .1052(2) .0337(5) Uani d . 1 C H10B .1329 .0278 .1928 .040 Uiso calc . 1 H O1 .17430(10) .3703(3) -.0304(2) .0565(5) Uani d . 1 O O2 .00588(9) .0465(2) -.20395(19) .0504(5) Uani d . 1 O O3 .42959(10) -.1315(3) .2172(2) .0677(6) Uani d . 1 O C11 .4545(2) -.2540(9) .1233(6) .129(2) Uani d . 1 C H11A .4304 -.3644 .1213 .193 Uiso calc R 1 H H11B .5028 -.2732 .1617 .193 Uiso calc R 1 H H11C .4470 -.2069 .0236 .193 Uiso calc R 1 H O4 .38964(9) .0877(3) .3936(2) .0575(5) Uani d . 1 O C12 .3690(2) .2088(7) .4925(5) .1003(17) Uani d . 1 C H12A .3535 .3165 .4399 .150 Uiso calc R 1 H H12B .4073 .2341 .5741 .150 Uiso calc R 1 H H12C .3323 .1582 .5308 .150 Uiso calc R 1 H 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 .0407(4) .0315(3) .0431(4) .0005(2) .0117(2) -.0041(2) C2 .0381(12) .0405(12) .0402(11) .0060(9) .0100(9) -.0004(9) C3 .0380(11) .0369(11) .0368(11) -.0005(9) .0087(9) .0021(9) N4 .0409(10) .0321(9) .0392(9) -.0004(8) .0040(8) -.0046(8) C5 .0504(14) .0324(12) .0573(15) .0015(10) .0000(11) -.0104(10) C6 .0509(14) .0438(14) .0463(13) .0065(11) .0027(11) -.0154(10) C6A .0449(12) .0338(11) .0374(11) .0017(9) .0083(9) -.0033(9) C7 .0470(13) .0444(13) .0488(13) .0061(10) .0133(10) -.0104(11) C8 .0387(12) .0465(13) .0496(13) .0039(10) .0103(10) -.0038(11) C9 .0384(12) .0421(12) .0384(11) -.0025(9) .0065(9) -.0028(9) C10 .0400(12) .0371(11) .0358(11) -.0031(9) .0122(9) -.0047(9) C10A .0379(11) .0311(10) .0329(10) -.0008(8) .0100(8) .0020(8) C10B .0385(11) .0322(11) .0310(10) -.0017(8) .0088(8) .0000(8) O1 .0575(11) .0463(10) .0726(12) -.0016(8) .0289(9) .0140(9) O2 .0477(10) .0510(11) .0460(9) -.0002(8) -.0031(8) -.0046(8) O3 .0409(10) .0851(15) .0736(13) .0146(10) .0055(9) -.0263(12) C11 .064(2) .184(5) .128(4) .057(3) .000(2) -.075(4) O4 .0392(9) .0722(13) .0569(11) .0009(8) .0020(8) -.0225(10) C12 .067(2) .129(4) .091(3) .019(2) -.0104(19) -.070(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .3331 .5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'