#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $ #$Revision: 176760 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/32/2013297.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_2013297 loop_ _publ_author_name 'Zhi Min Jin' 'Yuan Jian Pan' 'Liang Shen' 'Mei Chao Li' 'Mao Lin Hu' _publ_section_title ; Ribbons of hydrogen-bonded rings in the 1:2 complex of pyromellitic acid and dimethyl sulfoxide ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o205 _journal_page_last o206 _journal_paper_doi 10.1107/S0108270103004530 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'C10 H6 O8, 2C2 H6 O S' _chemical_formula_moiety 'C10 H6 O8, 2C2 H6 O S' _chemical_formula_sum 'C14 H18 O10 S2' _chemical_formula_weight 410.40 _chemical_name_systematic ; Pyromellitic acid--dimethyl sulfoxide (1/2) ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 80.070(10) _cell_angle_beta 80.970(10) _cell_angle_gamma 76.150(10) _cell_formula_units_Z 1 _cell_length_a 7.3770(10) _cell_length_b 7.4240(10) _cell_length_c 8.9340(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 14.16 _cell_measurement_theta_min 3.41 _cell_volume 464.51(11) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1996)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXTL-Plus _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 1775 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.33 _diffrn_standards_decay_% 3.61 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 214 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.44 _refine_diff_density_max 0.261 _refine_diff_density_min -0.236 _refine_ls_extinction_coef 0.129(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 129 _refine_ls_number_reflns 1634 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.1816P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.0858 _reflns_number_gt 1413 _reflns_number_total 1634 _reflns_threshold_expression I>2\s(I) _cod_data_source_file jz1542.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 464.51(10) _cod_database_code 2013297 _cod_database_fobs_code 2013297 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O1 0.2108(2) 0.5497(3) 0.69190(18) 0.0595(5) Uani d . 1 . . O O2 0.4485(2) 0.6869(2) 0.59915(16) 0.0437(4) Uani d D 1 . . O O3 0.3879(2) 0.9808(2) 0.8045(2) 0.0560(5) Uani d . 1 . . O O4 0.6979(2) 0.8918(2) 0.80119(19) 0.0488(4) Uani d D 1 . . O C1 0.4108(3) 0.3836(2) 0.9479(2) 0.0282(4) Uani d . 1 . . C H1 0.3504 0.3054 0.9129 0.034 Uiso calc R 1 . . H C2 0.4291(2) 0.5529(2) 0.8586(2) 0.0263(4) Uani d . 1 . . C C3 0.5194(2) 0.6711(2) 0.9120(2) 0.0262(4) Uani d . 1 . . C C4 0.3499(3) 0.5982(3) 0.7087(2) 0.0308(4) Uani d . 1 . . C C5 0.5259(3) 0.8645(3) 0.8311(2) 0.0291(4) Uani d . 1 . . C S 0.11370(7) 0.68265(7) 0.33963(6) 0.0348(2) Uani d . 1 . . S O5 0.2693(2) 0.7812(2) 0.35311(16) 0.0396(4) Uani d . 1 . . O C6 -0.0921(3) 0.7997(4) 0.4438(3) 0.0492(6) Uani d . 1 . . C H6A -0.1130 0.9318 0.4084 0.059 Uiso calc R 1 . . H H6B -0.0772 0.7774 0.5507 0.059 Uiso calc R 1 . . H H6C -0.1979 0.7533 0.4288 0.059 Uiso calc R 1 . . H C7 0.0531(3) 0.7653(5) 0.1514(3) 0.0584(7) Uani d . 1 . . C H7A 0.1608 0.7298 0.0784 0.070 Uiso calc R 1 . . H H7B 0.0129 0.8994 0.1388 0.070 Uiso calc R 1 . . H H7C -0.0470 0.7114 0.1352 0.070 Uiso calc R 1 . . H H4O 0.706(4) 1.006(3) 0.753(3) 0.074(9) Uiso d D 1 . . H H2O 0.394(4) 0.711(4) 0.514(2) 0.069(8) Uiso d D 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 O1 0.0586(11) 0.0859(13) 0.0451(9) -0.0436(10) -0.0268(8) 0.0187(8) O2 0.0468(9) 0.0598(10) 0.0286(8) -0.0255(7) -0.0140(7) 0.0100(7) O3 0.0408(9) 0.0333(8) 0.0896(13) -0.0053(7) -0.0199(9) 0.0100(8) O4 0.0367(8) 0.0415(9) 0.0639(10) -0.0172(7) -0.0079(7) 0.0184(8) C1 0.0296(9) 0.0286(9) 0.0297(9) -0.0109(7) -0.0074(7) -0.0037(7) C2 0.0260(9) 0.0281(9) 0.0249(9) -0.0058(7) -0.0049(7) -0.0027(7) C3 0.0241(9) 0.0270(9) 0.0271(9) -0.0058(7) -0.0035(7) -0.0019(7) C4 0.0340(10) 0.0300(10) 0.0309(10) -0.0101(8) -0.0106(8) -0.0006(8) C5 0.0338(10) 0.0284(9) 0.0268(9) -0.0083(8) -0.0085(8) -0.0022(7) S 0.0308(3) 0.0348(3) 0.0403(3) -0.0112(2) -0.0069(2) -0.0015(2) O5 0.0396(8) 0.0463(8) 0.0368(8) -0.0230(7) -0.0141(6) 0.0116(6) C6 0.0403(13) 0.0620(15) 0.0441(13) -0.0106(11) -0.0004(10) -0.0088(11) C7 0.0398(13) 0.103(2) 0.0368(12) -0.0221(13) -0.0082(10) -0.0097(13) 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' 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 C4 O2 H2O . 110.2(18) C5 O4 H4O . 114.1(19) C3 C1 C2 2_667 121.54(16) C3 C1 H1 2_667 119.2 C2 C1 H1 . 119.2 C1 C2 C3 . 119.17(16) C1 C2 C4 . 117.31(15) C3 C2 C4 . 123.52(16) C1 C3 C2 2_667 119.29(16) C1 C3 C5 2_667 118.11(15) C2 C3 C5 . 122.29(16) O1 C4 O2 . 123.88(17) O1 C4 C2 . 121.85(17) O2 C4 C2 . 114.21(16) O3 C5 O4 . 124.79(18) O3 C5 C3 . 122.84(17) O4 C5 C3 . 112.28(15) O5 S C6 . 106.04(10) O5 S C7 . 104.63(10) C6 S C7 . 98.92(12) S C6 H6A . 109.5 S C6 H6B . 109.5 H6A C6 H6B . 109.5 S C6 H6C . 109.5 H6A C6 H6C . 109.5 H6B C6 H6C . 109.5 S C7 H7A . 109.5 S C7 H7B . 109.5 H7A C7 H7B . 109.5 S C7 H7C . 109.5 H7A C7 H7C . 109.5 H7B C7 H7C . 109.5 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 O1 C4 . 1.204(2) yes O2 C4 . 1.306(2) yes O2 H2O . 0.882(17) ? O3 C5 . 1.192(2) yes O4 C5 . 1.312(2) yes O4 H4O . 0.891(17) ? C1 C3 2_667 1.387(3) yes C1 C2 . 1.391(3) ? C1 H1 . 0.9300 ? C2 C3 . 1.402(2) yes C2 C4 . 1.498(2) ? C3 C1 2_667 1.387(3) ? C3 C5 . 1.500(2) ? S O5 . 1.5310(14) ? S C6 . 1.769(2) ? S C7 . 1.776(2) ? C6 H6A . 0.9600 ? C6 H6B . 0.9600 ? C6 H6C . 0.9600 ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H2O O5 . 0.882(17) 1.769(17) 2.647(2) 174(2) yes O4 H4O O5 2_676 0.891(17) 1.732(17) 2.622(2) 176(2) yes C6 H6B O1 . 0.96 2.71 3.391(3) 128 yes C6 H6C O1 2_566 0.96 2.68 3.386(4) 130 yes C7 H7C O1 2_566 0.96 2.67 3.379(4) 131 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion C3 C1 C2 C3 2_667 . -0.3(3) C3 C1 C2 C4 2_667 . 179.62(16) C1 C2 C3 C1 . 2_667 0.3(3) C4 C2 C3 C1 . 2_667 -179.63(16) C1 C2 C3 C5 . . -173.10(17) C4 C2 C3 C5 . . 6.9(3) C1 C2 C4 O1 . . 33.5(3) C3 C2 C4 O1 . . -146.5(2) C1 C2 C4 O2 . . -143.98(18) C3 C2 C4 O2 . . 36.0(3) C1 C3 C5 O3 2_667 . -117.2(2) C2 C3 C5 O3 . . 56.3(3) C1 C3 C5 O4 2_667 . 59.5(2) C2 C3 C5 O4 . . -126.99(19)