#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2013737.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_2013737 loop_ _publ_author_name 'Sto\'s, El\.zbieta' 'Lis, Tadeusz' 'Videnova-Adrabi\'nska, Veneta' _publ_section_title ; Polymeric sodium 3,5-dicarboxybenzenesulfonate--urea--water (1/1/1) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m114 _journal_page_last m116 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Na (C8 H5 O7 S) (C H4 N2 O)] , H2 O' _chemical_formula_moiety 'Na + , C8 H5 O7 S - , C H4 N2 O , H2 O' _chemical_formula_sum 'C9 H11 N2 Na O9 S' _chemical_formula_weight 346.26 _chemical_name_systematic ; Poly[sodium-\m~4~-3,5-dicarboxybenzenesulfonate- \k^4^O:O':O'':O'''-\m~2~-urea-\k^2^O:N] monohydrate] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 91.025(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.203(3) _cell_length_b 11.566(4) _cell_length_c 14.534(4) _cell_measurement_reflns_used 15999 _cell_measurement_temperature 100 _cell_measurement_theta_max 37 _cell_measurement_theta_min 2 _cell_volume 1378.7(8) _computing_cell_refinement 'KM-4 CCD Software' _computing_data_collection 'KM-4 CCD Software (Kuma Diffraction, 2000)' _computing_data_reduction 'KM-4 CCD Software' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.951 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device_type 'Kuma KM-4 CCD area-detector' _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 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 22990 _diffrn_reflns_theta_full 37.52 _diffrn_reflns_theta_max 37.52 _diffrn_reflns_theta_min 3.31 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.316 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description spherical _exptl_crystal_F_000 712 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.57 _refine_diff_density_min -0.50 _refine_ls_extinction_coef 0.0033(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 6900 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0346 _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^)+(0.0469P)^2^+0.1356P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.0910 _reflns_number_gt 5744 _reflns_number_total 6900 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file av1161.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2013737 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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_occupancy _atom_site_type_symbol Na 0.55261(5) 0.14119(3) 0.33996(2) 0.01129(8) Uani d 1 Na C11 0.39454(11) 0.32400(8) 0.48549(6) 0.01131(14) Uani d 1 C O11 0.46065(10) 0.27266(6) 0.55778(5) 0.01693(14) Uani d 1 O O21 0.40319(10) 0.28866(6) 0.40661(5) 0.01766(14) Uani d 1 O H1 0.510(2) 0.2133(17) 0.5398(13) 0.040(5) Uiso d 1 H C31 0.07506(11) 0.66165(7) 0.37724(6) 0.01051(14) Uani d 1 C O13 -0.01529(9) 0.75239(6) 0.40050(5) 0.01620(14) Uani d 1 O O23 0.08903(9) 0.62891(6) 0.29822(4) 0.01504(13) Uani d 1 O H3 -0.068(2) 0.7691(17) 0.3526(14) 0.049(5) Uiso d 1 H S 0.18594(3) 0.617774(17) 0.733274(13) 0.00813(5) Uani d 1 S O15 0.22703(8) 0.51866(6) 0.79203(4) 0.01152(12) Uani d 1 O O25 0.01749(8) 0.65548(6) 0.74123(4) 0.01208(12) Uani d 1 O O35 0.30261(8) 0.71288(6) 0.74595(4) 0.01284(12) Uani d 1 O C1 0.30668(10) 0.43329(7) 0.50831(6) 0.01002(14) Uani d 1 C C2 0.23757(11) 0.49797(7) 0.43693(6) 0.01028(14) Uani d 1 C C3 0.15327(10) 0.59977(7) 0.45642(6) 0.00932(13) Uani d 1 C C4 0.13727(11) 0.63710(7) 0.54707(6) 0.00964(13) Uani d 1 C C5 0.20716(10) 0.57076(7) 0.61796(5) 0.00874(13) Uani d 1 C C6 0.29193(10) 0.46957(7) 0.59950(6) 0.00981(13) Uani d 1 C H2 0.2439(17) 0.4719(12) 0.3780(10) 0.018(3) Uiso d 1 H H4 0.0806(17) 0.7070(13) 0.5596(10) 0.017(3) Uiso d 1 H H6 0.3388(17) 0.4226(13) 0.6488(10) 0.016(3) Uiso d 1 H C10 0.70458(10) 0.03210(7) 0.54052(6) 0.01022(14) Uani d 1 C O10 0.62541(9) 0.10516(6) 0.49343(5) 0.01353(12) Uani d 1 O N1 0.80422(10) -0.04331(7) 0.49985(6) 0.01468(14) Uani d 1 N H1N1 0.8118(19) -0.0418(15) 0.4408(12) 0.029(4) Uiso d 1 H H2N1 0.8620(19) -0.0933(14) 0.5309(11) 0.025(4) Uiso d 1 H N2 0.68951(11) 0.02366(8) 0.63262(5) 0.01455(14) Uani d 1 N H1N2 0.6409(19) 0.0710(14) 0.6591(11) 0.024(4) Uiso d 1 H H2N2 0.7551(17) -0.0164(12) 0.6624(10) 0.015(3) Uiso d 1 H O1w 0.52632(10) 0.38305(7) 0.82537(6) 0.01888(14) Uani d 1 O H1w 0.525(2) 0.3183(18) 0.7982(13) 0.040(5) Uiso d 1 H H2w 0.446(2) 0.4165(17) 0.8107(14) 0.044(5) Uiso 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 Na 0.01482(17) 0.01116(16) 0.00787(15) 0.00170(12) -0.00024(12) -0.00026(12) C11 0.0133(4) 0.0106(3) 0.0100(3) 0.0028(3) 0.0002(3) 0.0001(3) O11 0.0253(4) 0.0152(3) 0.0102(3) 0.0108(3) -0.0019(2) -0.0001(2) O21 0.0267(4) 0.0168(3) 0.0094(3) 0.0103(3) -0.0003(3) -0.0023(2) C31 0.0123(3) 0.0105(3) 0.0086(3) 0.0016(3) -0.0012(3) 0.0007(3) O13 0.0239(4) 0.0146(3) 0.0099(3) 0.0098(3) -0.0040(2) -0.0013(2) O23 0.0209(3) 0.0170(3) 0.0072(2) 0.0064(2) -0.0019(2) -0.0010(2) S 0.01068(9) 0.00793(8) 0.00578(8) -0.00079(6) -0.00021(6) -0.00002(6) O15 0.0159(3) 0.0108(3) 0.0078(2) 0.0009(2) -0.0006(2) 0.0024(2) O25 0.0123(3) 0.0130(3) 0.0110(3) 0.0022(2) 0.0021(2) 0.0002(2) O35 0.0169(3) 0.0122(3) 0.0094(2) -0.0054(2) -0.0011(2) -0.0012(2) C1 0.0118(3) 0.0101(3) 0.0082(3) 0.0020(3) 0.0002(3) -0.0004(3) C2 0.0124(3) 0.0106(3) 0.0078(3) 0.0019(3) -0.0002(3) -0.0006(3) C3 0.0111(3) 0.0094(3) 0.0074(3) 0.0012(3) -0.0012(2) 0.0002(3) C4 0.0113(3) 0.0093(3) 0.0083(3) 0.0011(3) -0.0009(3) -0.0003(3) C5 0.0100(3) 0.0093(3) 0.0068(3) -0.0006(2) -0.0006(2) -0.0008(3) C6 0.0115(3) 0.0097(3) 0.0081(3) 0.0012(3) -0.0009(3) 0.0002(3) C10 0.0109(3) 0.0104(3) 0.0093(3) 0.0011(3) -0.0002(3) 0.0003(3) O10 0.0172(3) 0.0131(3) 0.0102(3) 0.0062(2) -0.0012(2) 0.0011(2) N1 0.0174(4) 0.0157(3) 0.0110(3) 0.0074(3) 0.0018(3) 0.0007(3) N2 0.0169(4) 0.0185(4) 0.0083(3) 0.0067(3) 0.0009(3) 0.0012(3) O1w 0.0173(3) 0.0161(3) 0.0231(4) -0.0006(3) -0.0062(3) -0.0060(3) 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' Na Na 0.0362 0.0249 '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 O21 Na O15 . 4_665 171.69(3) yes O21 Na O35 . 3_666 88.31(4) yes O21 Na O10 . . 81.98(3) yes O21 Na N2 . 3_656 93.44(4) yes O23 Na O21 2_545 . 98.46(3) yes O23 Na O15 2_545 4_665 89.63(3) yes O23 Na O35 2_545 3_666 80.69(3) yes O23 Na O10 2_545 . 159.48(3) yes O23 Na N2 2_545 3_656 74.52(3) yes O15 Na N2 4_665 3_656 86.88(4) yes O35 Na O15 3_666 4_665 94.88(4) yes O35 Na N2 3_666 3_656 155.14(3) yes O10 Na O15 . 4_665 89.79(3) yes O10 Na O35 . 3_666 119.79(3) yes O10 Na N2 . 3_656 84.96(3) yes O11 C11 C1 . . 113.45(8) no O21 C11 C1 . . 121.86(8) no O21 C11 O11 . . 124.69(8) no C11 O11 H1 . . 108.3(13) no C11 O21 Na . . 132.68(6) no O13 C31 C3 . . 114.59(7) no O23 C31 C3 . . 122.20(8) no O23 C31 O13 . . 123.17(8) no C31 O13 H3 . . 104.6(13) no C31 O23 Na . 2 138.44(7) no O15 S C5 . . 106.59(4) no O15 S O35 . . 111.75(4) no O25 S C5 . . 106.04(4) no O25 S O15 . . 113.38(4) no O25 S O35 . . 112.54(5) no O35 S C5 . . 105.89(4) no S O15 Na . 4_566 128.87(4) no S O35 Na . 3_666 141.44(4) no C2 C1 C6 . . 120.30(8) no C2 C1 C11 . . 118.73(8) no C6 C1 C11 . . 120.96(8) no C1 C2 C3 . . 119.90(8) no C1 C2 H2 . . 119.6(9) no C3 C2 H2 . . 120.5(9) no C2 C3 C31 . . 117.12(8) no C4 C3 C2 . . 120.52(8) no C4 C3 C31 . . 122.29(8) no C3 C4 C5 . . 118.78(8) no C3 C4 H4 . . 119.9(9) no C5 C4 H4 . . 121.3(9) no C4 C5 S . . 118.81(7) no C6 C5 C4 . . 121.29(8) no C6 C5 S . . 119.90(6) no C1 C6 H6 . . 119.4(8) no C5 C6 C1 . . 119.21(8) no C5 C6 H6 . . 121.4(8) no O10 C10 N1 . . 120.62(8) no O10 C10 N2 . . 122.10(8) no N1 C10 N2 . . 117.24(8) no C10 O10 Na . . 139.33(6) yes C10 N1 H1N1 . . 118.8(11) no C10 N1 H2N1 . . 122.3(11) no H1N1 N1 H2N1 . . 118.9(15) no Na N2 H1N2 3_656 . 92.2(12) yes Na N2 H2N2 3_656 . 90.0(10) yes C10 N2 Na . 3_656 105.62(6) yes C10 N2 H1N2 . . 119.6(12) no C10 N2 H2N2 . . 119.3(10) no H1N2 N2 H2N2 . . 117.8(15) no H1w O1w H2w . . 107.8(18) no 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 Na O21 . 2.3223(9) yes Na O23 2_545 2.3065(9) yes Na O15 4_665 2.4465(9) yes Na O35 3_666 2.4230(9) yes Na O10 . 2.3362(9) yes Na N2 3_656 2.7869(12) yes C11 O21 . 1.2205(11) no C11 O11 . 1.3153(11) no O11 H1 . 0.841(19) no C31 O23 . 1.2166(11) no C31 O13 . 1.3320(11) no O13 H3 . 0.84(2) no S O25 . 1.4556(8) no S O15 . 1.4652(7) no S O35 . 1.4675(8) no C1 C2 . 1.3914(12) no C1 C6 . 1.3975(12) no C1 C11 . 1.4953(13) no C2 C3 . 1.3971(12) no C2 H2 . 0.911(15) no C3 C4 . 1.3948(12) no C3 C31 . 1.4906(12) no C4 C5 . 1.3991(12) no C4 H4 . 0.952(15) no C5 C6 . 1.3900(12) no C5 S . 1.7736(9) no C6 H6 . 0.974(14) no C10 O10 . 1.2602(11) no C10 N1 . 1.3400(12) no C10 N2 . 1.3501(12) no N1 H1N1 . 0.862(17) no N1 H2N1 . 0.869(17) no N2 H1N2 . 0.783(17) no N2 H2N2 . 0.826(14) no O1w H1w . 0.85(2) no O1w H2w . 0.79(2) no 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 O11 H1 O10 . 0.841(19) 1.714(19) 2.5495(11) 171.9(19) O13 H3 O35 4_575 0.84(2) 1.87(2) 2.7052(11) 173(2) N1 H1N1 O15 4_665 0.862(17) 2.275(17) 3.0881(13) 157.3(14) N1 H2N1 O1w 2_646 0.869(16) 2.282(17) 2.9974(13) 139.6(14) N2 H1N2 O25 2_546 0.783(17) 2.192(17) 2.9463(12) 161.8(16) N2 H2N2 O1w 2_646 0.826(14) 2.142(14) 2.8984(14) 152.1(13) O1w H1w O25 2_546 0.85(2) 2.00(2) 2.8252(13) 165.5(17) O1w H2w O15 . 0.79(2) 2.17(2) 2.9461(13) 171.1(19)