#------------------------------------------------------------------------------ #$Date: 2025-01-27 17:33:32 +0200 (Mon, 27 Jan 2025) $ #$Revision: 297475 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/30/03/2300345.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_2300345 loop_ _publ_author_name 'Eccles, Kevin S.' 'Stokes, Stephen P.' 'Daly, Carla A.' 'Barry, Nicola M.' 'McSweeney, Sharon P.' 'O'Neill, Damian J.' 'Kelly, Dawn M.' 'Jennings, W. Brian' 'N\'i Dhubhghaill, O. M.' 'Moynihan, Humphrey A.' 'Maguire, Anita R.' 'Lawrence, Simon E.' _publ_section_title ; Evaluation of the Bruker SMART X2S: crystallography for the nonspecialist? ; _journal_coden_ASTM JACGAR _journal_coeditor_code KK5074 _journal_issue 1 _journal_name_full 'Journal of Applied Crystallography' _journal_page_first 213 _journal_page_last 215 _journal_paper_doi 10.1107/S0021889810042561 _journal_volume 44 _journal_year 2011 _chemical_formula_moiety '(C7 H6 N3 O3 S), (O)' _chemical_formula_sum 'C7 H8 N4 O S' _chemical_formula_weight 196.23 _space_group_IT_number 4 _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 direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.445(13) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.6245(17) _cell_length_b 7.354(3) _cell_length_c 12.521(5) _cell_measurement_reflns_used 654 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 19.39 _cell_measurement_theta_min 2.71 _cell_volume 517.0(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker GIS' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker APEX2' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 300(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker SMART X2S' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'doubly curved silicon crystal' _diffrn_radiation_source 'micro-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1452 _diffrn_reflns_av_sigmaI/netI 0.1447 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3392 _diffrn_reflns_theta_full 24.98 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_min 1.63 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_T_max 0.9640 _exptl_absorpt_correction_T_min 0.9079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 204 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.472 _refine_diff_density_min -0.632 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.9(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1777 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.992 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0865 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2132 _refine_ls_wR_factor_ref 0.2280 _reflns_number_gt 1247 _reflns_number_total 1777 _reflns_threshold_expression >2sigma(I) _cod_data_source_file kk5074.cif _cod_data_source_block Compound_16_X2S _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_original_sg_symbol_H-M P12(1)1 _cod_database_code 2300345 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.2528(3) 0.1633(2) 0.29341(14) 0.0305(5) Uani d . 1 . . O O1S 0.9229(10) -0.2237(8) 0.4347(5) 0.0463(16) Uani d . 1 . . O O1 0.2494(11) 0.3545(9) 0.3539(5) 0.0543(17) Uani d . 1 . . O O2 0.0217(10) 0.0856(7) 0.3121(4) 0.0401(15) Uani d . 1 . . O O3 0.4579(9) 0.0512(7) 0.3228(4) 0.0384(14) Uani d . 1 . . N N1 0.2179(14) 0.2629(12) -0.1792(6) 0.052(2) Uani d . 1 . . N N2 0.4151(14) 0.6325(10) 0.3908(6) 0.0477(19) Uani d . 1 . . N N3 0.4273(14) 0.1626(14) -0.0142(6) 0.058(2) Uani d . 1 . . H H3 0.5423 0.1227 -0.0499 0.070 Uiso calc R 1 . . C C1 0.2329(14) 0.2485(11) -0.0676(6) 0.0337(19) Uani d . 1 . . C C2 0.0544(15) 0.3172(11) -0.0060(7) 0.041(2) Uani d . 1 . . H H2 -0.0731 0.3792 -0.0399 0.049 Uiso calc R 1 . . C C3 0.0619(14) 0.2959(12) 0.1032(7) 0.038(2) Uani d . 1 . . H H3A -0.0607 0.3410 0.1423 0.046 Uiso calc R 1 . . C C4 0.2542(13) 0.2064(9) 0.1551(6) 0.0284(18) Uani d . 1 . . C C5 0.4503(14) 0.4594(10) 0.3620(6) 0.0309(19) Uani d . 1 . . C C6 0.6662(11) 0.4018(11) 0.3456(6) 0.0286(17) Uani d . 1 . . H H6A 0.7947 0.4811 0.3540 0.034 Uiso calc R 1 . . H H6B 0.6905 0.2817 0.3256 0.034 Uiso calc R 1 . . C C7 0.4359(13) 0.1413(11) 0.0960(6) 0.0338(18) Uani d . 1 . . H H7 0.5653 0.0826 0.1305 0.041 Uiso calc R 1 . . 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 0.0313(10) 0.0250(9) 0.0354(10) -0.0025(10) 0.0036(7) 0.0018(9) O1S 0.052(4) 0.039(4) 0.049(4) -0.005(3) 0.007(3) 0.000(3) O1 0.055(4) 0.046(4) 0.062(4) 0.009(3) 0.003(3) -0.011(3) O2 0.040(3) 0.036(3) 0.046(3) -0.007(3) 0.014(3) 0.005(3) O3 0.039(3) 0.026(3) 0.049(3) 0.007(3) -0.004(3) 0.008(3) N1 0.071(5) 0.047(4) 0.039(4) -0.006(4) 0.002(4) -0.003(3) N2 0.059(4) 0.035(5) 0.049(4) -0.007(4) -0.001(3) -0.014(3) N3 0.060(5) 0.053(4) 0.062(5) 0.005(6) 0.013(4) -0.004(5) C1 0.038(5) 0.024(4) 0.039(5) -0.007(4) -0.002(4) 0.006(3) C2 0.037(5) 0.032(5) 0.052(5) 0.005(4) -0.006(4) 0.003(4) C3 0.030(4) 0.041(5) 0.043(5) 0.003(4) 0.003(4) -0.001(4) C4 0.028(4) 0.025(5) 0.032(4) -0.001(3) 0.003(3) 0.003(3) C5 0.031(5) 0.030(4) 0.032(4) -0.013(4) 0.002(3) 0.007(3) C6 0.012(4) 0.026(4) 0.048(4) -0.004(3) 0.006(3) 0.002(3) C7 0.034(4) 0.027(4) 0.040(4) 0.011(4) 0.004(3) 0.002(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 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_3 _geom_angle _geom_angle_publ_flag O3 S1 O2 . . 116.3(3) ? O3 S1 O1 . . 114.4(3) ? O2 S1 O1 . . 103.5(3) ? O3 S1 C4 . . 107.6(3) ? O2 S1 C4 . . 106.6(3) ? O1 S1 C4 . . 108.0(3) ? C5 O1 S1 . . 119.9(5) ? C7 N3 C1 . . 120.5(7) ? C7 N3 H3 . . 119.8 ? C1 N3 H3 . . 119.8 ? C2 C1 N1 . . 121.5(7) ? C2 C1 N3 . . 117.8(7) ? N1 C1 N3 . . 120.7(7) ? C3 C2 C1 . . 121.9(7) ? C3 C2 H2 . . 119.1 ? C1 C2 H2 . . 119.1 ? C2 C3 C4 . . 119.6(7) ? C2 C3 H3A . . 120.2 ? C4 C3 H3A . . 120.2 ? C7 C4 C3 . . 119.5(7) ? C7 C4 S1 . . 120.8(6) ? C3 C4 S1 . . 119.6(6) ? C6 C5 N2 . . 120.0(7) ? C6 C5 O1 . . 125.1(7) ? N2 C5 O1 . . 114.9(7) ? C5 C6 H6A . . 120.0 ? C5 C6 H6B . . 120.0 ? H6A C6 H6B . . 120.0 ? C4 C7 N3 . . 120.7(7) ? C4 C7 H7 . . 119.6 ? N3 C7 H7 . . 119.6 ? 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 O3 . 1.447(6) ? S1 O2 . 1.452(6) ? S1 O1 . 1.598(6) ? S1 C4 . 1.760(7) ? O1 C5 . 1.367(9) ? N1 C1 . 1.398(11) ? N2 C5 . 1.341(10) ? N3 C7 . 1.386(10) ? N3 C1 . 1.398(11) ? N3 H3 . 0.8600 ? C1 C2 . 1.397(11) ? C2 C3 . 1.375(11) ? C2 H2 . 0.9300 ? C3 C4 . 1.394(11) ? C3 H3A . 0.9300 ? C4 C7 . 1.383(10) ? C5 C6 . 1.314(10) ? C6 H6A . 0.9300 ? C6 H6B . 0.9300 ? C7 H7 . 0.9300 ? loop_ _cod_entry_issue_id _cod_entry_issue_origin _cod_entry_issue_severity _cod_entry_issue_description _cod_entry_issue_author _cod_entry_issue_date 1 original note ; This entry describes a structure that was purposely solved automatically with minimal human intervention to investigate the capabilities of the Bruker SMART X2S benchtop crystallography instrument. ; 'Vaitkus, Antanas' 2025-01-27T16:15:51+02:00 2 original warning ; Atom sites 'N3' and 'O1' were assigned incorrect atom types during the automated structure modelling. For the correct structure, see entry 2300342. ; 'Vaitkus, Antanas' 2025-01-27T16:15:51+02:00 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 15445176