#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012408.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_2012408 loop_ _publ_author_name 'Yazicilar, Turan K.' 'Andac, Omer' 'Bekdemir, Yunus' 'Kutuk, Halil' 'Yilmaz, Veysel T.' 'Harrison, William T. A.' _publ_section_title ; Sodium p-nitrobenzoxasulfamate monohydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m21 _journal_page_last m22 _journal_volume 58 _journal_year 2002 _chemical_formula_moiety 'Na +, C6 H3 N2 O5 S -, H2 O' _chemical_formula_sum 'C6 H5 N2 Na O6 S' _chemical_formula_weight 256.17 _chemical_name_systematic ; Sodium p-nitrobenzoxasulfamate monohydrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.6770(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.0610(7) _cell_length_b 6.8155(4) _cell_length_c 20.7293(11) _cell_measurement_reflns_used 3359 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.52 _cell_measurement_theta_min 3.15 _cell_volume 1819.01(17) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick,1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full .998 _diffrn_measured_fraction_theta_max .998 _diffrn_measurement_device_type 'Bruker SMART1000 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 .71069 _diffrn_reflns_av_R_equivalents .023 _diffrn_reflns_av_sigmaI/netI .021 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 6528 _diffrn_reflns_theta_full 27.52 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_min 1.99 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .420 _exptl_absorpt_correction_T_max .949 _exptl_absorpt_correction_T_min .761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 1999)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description Column _exptl_crystal_F_000 1040 _exptl_crystal_size_max .55 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .11 _refine_diff_density_max .26 _refine_diff_density_min -.37 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 2096 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all .0371 _refine_ls_R_factor_gt .0300 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.050P)^2^+0.652P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .0815 _refine_ls_wR_factor_ref .0850 _reflns_number_gt 1758 _reflns_number_total 2096 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bm1465.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _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 1527 2010-12-29 10:47:43Z saulius 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012408 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol S1 .92560(3) .19080(6) .15613(2) .02760(13) Uani d . 1 . . S Na1 .70264(6) -.03018(10) .23785(3) .0414(2) Uani d . 1 . . Na O1W .63443(9) .28414(18) .24050(6) .0342(3) Uani d D 1 . . O H1W1 .5972(14) .342(3) .2114(7) .051 Uiso d D 1 . . H H2W1 .6116(16) .310(3) .2741(6) .051 Uiso d D 1 . . H O1 1.00939(10) .32593(19) .17193(6) .0422(3) Uani d . 1 . . O O2 .84291(10) .21684(19) .19272(6) .0392(3) Uani d . 1 . . O O3 .87654(10) .22657(17) .07865(5) .0352(3) Uani d . 1 . . O O4 .80116(11) -.3934(2) -.12360(6) .0473(3) Uani d . 1 . . O O5 .78181(12) -.0843(2) -.14476(6) .0538(4) Uani d . 1 . . O N1 .95956(10) -.0322(2) .15242(6) .0296(3) Uani d . 1 . . N N2 .80933(11) -.2208(2) -.10668(7) .0363(3) Uani d . 1 . . N C1 .92845(11) -.0968(2) .08939(7) .0250(3) Uani d . 1 . . C C2 .93669(13) -.2855(2) .06555(8) .0305(3) Uani d . 1 . . C H2 .9683 -.3844 .0928 .037 Uiso calc R 1 . . H C3 .89724(12) -.3238(2) .00093(8) .0321(4) Uani d . 1 . . C H3 .9007 -.4502 -.0155 .039 Uiso calc R 1 . . H C4 .85239(11) -.1745(2) -.03979(7) .0285(3) Uani d . 1 . . C C5 .84363(12) .0177(2) -.01812(8) .0292(3) Uani d . 1 . . C H5 .8140 .1174 -.0458 .035 Uiso calc R 1 . . H C6 .88135(11) .0492(2) .04626(7) .0256(3) Uani d . 1 . . C 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 .0309(2) .0266(2) .0252(2) .00165(14) .00442(14) .00046(14) Na1 .0607(5) .0303(4) .0351(4) .0110(3) .0134(3) .0036(3) O1W .0378(6) .0358(7) .0285(6) .0107(5) .0043(5) .0011(5) O1 .0434(7) .0390(7) .0429(7) -.0107(5) .0035(6) .0000(6) O2 .0408(7) .0391(7) .0403(7) .0035(5) .0145(5) -.0063(5) O3 .0498(7) .0265(6) .0268(6) .0116(5) -.0011(5) .0016(5) O4 .0503(8) .0527(9) .0404(7) -.0163(7) .0115(6) -.0160(6) O5 .0641(9) .0653(10) .0276(6) .0019(8) -.0052(6) .0035(6) N1 .0360(7) .0281(7) .0239(6) .0069(6) .0031(5) .0035(5) N2 .0306(7) .0504(9) .0290(7) -.0083(6) .0080(6) -.0063(6) C1 .0227(7) .0277(8) .0252(7) .0025(6) .0058(5) .0038(6) C2 .0344(8) .0251(8) .0324(8) .0059(6) .0068(6) .0053(6) C3 .0332(8) .0275(8) .0371(9) .0007(6) .0100(7) -.0037(6) C4 .0250(7) .0370(9) .0240(7) -.0026(6) .0059(6) -.0017(6) C5 .0274(7) .0329(8) .0268(8) .0034(6) .0029(6) .0060(6) C6 .0267(7) .0237(7) .0270(7) .0029(6) .0058(6) .0016(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 O1 . 1.4257(13) y S1 O2 . 1.4312(12) y S1 O3 . 1.6442(11) y S1 N1 . 1.5889(13) y Na1 O1W . 2.3244(14) y Na1 O1W 4_645 2.4516(15) y Na1 O1 3_445 2.8355(15) y Na1 O2 4_645 2.3846(14) y Na1 O2 . 2.7644(15) y Na1 O4 7_645 2.4173(14) y Na1 O5 6_556 2.5988(15) y Na1 Na1 4_655 3.6314(6) y O1W H1W1 . .811(9) n O1W H2W1 . .821(9) n O3 C6 . 1.3893(18) y N1 C1 . 1.374(2) y O4 N2 . 1.227(2) y O5 N2 . 1.234(2) y N2 C4 . 1.441(2) y C1 C6 . 1.408(2) y C1 C2 . 1.388(2) y C2 C3 . 1.377(2) y C2 H2 . .9300 n C3 C4 . 1.387(2) y C3 H3 . .9300 n C4 C5 . 1.396(2) y C5 C6 . 1.360(2) y C5 H5 . .9300 n loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 '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 .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na .0362 .0249 '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 O1 S1 O2 . . 114.62(8) O1 S1 N1 . . 114.79(8) O2 S1 N1 . . 112.70(8) O1 S1 O3 . . 106.66(7) O2 S1 O3 . . 107.12(7) N1 S1 O3 . . 99.25(6) O1W Na1 O2 . 4_645 121.10(5) O1W Na1 O4 . 7_645 106.08(5) O2 Na1 O4 4_645 7_645 117.99(6) O1W Na1 O1W . 4_645 142.73(5) O2 Na1 O1W 4_645 4_645 79.24(5) O4 Na1 O1W 7_645 4_645 86.70(5) O1W Na1 O5 . 6_556 78.16(5) O2 Na1 O5 4_645 6_556 75.66(5) O4 Na1 O5 7_645 6_556 157.15(6) O1W Na1 O5 4_645 6_556 77.71(5) O1W Na1 O2 . . 74.05(5) O2 Na1 O2 4_645 . 153.05(4) O4 Na1 O2 7_645 . 72.87(5) O1W Na1 O2 4_645 . 76.82(4) O5 Na1 O2 6_556 . 87.25(5) O1W Na1 O1 . 3_445 90.94(5) O2 Na1 O1 4_645 3_445 75.44(5) O4 Na1 O1 7_645 3_445 65.37(5) O1W Na1 O1 4_645 3_445 125.78(5) O5 Na1 O1 6_556 3_445 137.47(5) O2 Na1 O1 . 3_445 129.38(5) Na1 O1W Na1 . 4_655 98.96(4) Na1 O1W H1W1 . . 127.9(15) Na1 O1W H1W1 4_655 . 106.2(16) Na1 O1W H2W1 . . 114.2(14) Na1 O1W H2W1 4_655 . 99.4(16) H1W1 O1W H2W1 . . 105.8(17) S1 O1 Na1 . 3 157.05(8) S1 O2 Na1 . 4_655 134.15(8) S1 O2 Na1 . . 134.90(7) Na1 O2 Na1 4_655 . 89.39(4) C6 O3 S1 . . 107.53(9) N2 O4 Na1 . 7_645 118.24(11) N2 O5 Na1 . 6 148.51(12) C1 N1 S1 . . 108.19(10) O4 N2 O5 . . 122.54(15) O4 N2 C4 . . 119.10(15) O5 N2 C4 . . 118.36(15) N1 C1 C2 . . 127.39(14) N1 C1 C6 . . 113.89(14) C2 C1 C6 . . 118.71(14) C3 C2 C1 . . 118.89(14) C3 C2 H2 . . 120.6 C1 C2 H2 . . 120.6 C2 C3 C4 . . 120.24(15) C2 C3 H3 . . 119.9 C4 C3 H3 . . 119.9 C3 C4 C5 . . 122.79(15) C3 C4 N2 . . 118.77(15) C5 C4 N2 . . 118.39(14) C6 C5 C4 . . 115.35(14) C6 C5 H5 . . 122.3 C4 C5 H5 . . 122.3 C5 C6 O3 . . 124.97(13) C5 C6 C1 . . 124.00(15) O3 C6 C1 . . 111.01(13) 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 O1W H1W1 N1 3_455 .811(9) 2.173(12) 2.9521(17) 161(2) O1W H2W1 N1 4_655 .821(9) 2.196(12) 2.9859(17) 161(2) C2 H2 O1 1_545 .93 2.57 3.475(2) 166 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 O1 S1 O3 C6 122.54(11) O2 S1 O3 C6 -114.28(11) N1 S1 O3 C6 3.06(11) O1 S1 N1 C1 -116.69(11) O2 S1 N1 C1 109.63(11) O3 S1 N1 C1 -3.42(12) S1 N1 C1 C2 -175.71(13) S1 N1 C1 C6 2.82(16) N1 C1 C2 C3 177.54(15) C6 C1 C2 C3 -.9(2) C1 C2 C3 C4 1.6(2) C2 C3 C4 C5 -.8(2) C2 C3 C4 N2 -178.32(14) O4 N2 C4 C3 9.4(2) O5 N2 C4 C3 -170.80(15) O4 N2 C4 C5 -168.26(14) O5 N2 C4 C5 11.6(2) C3 C4 C5 C6 -.6(2) N2 C4 C5 C6 176.92(13) C4 C5 C6 O3 -177.07(14) C4 C5 C6 C1 1.3(2) S1 O3 C6 C5 176.79(13) S1 O3 C6 C1 -1.73(15) N1 C1 C6 C5 -179.21(14) C2 C1 C6 C5 -.5(2) N1 C1 C6 O3 -.66(19) C2 C1 C6 O3 178.01(13)