#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/19/2011975.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_2011975 loop_ _publ_author_name 'Cannon, Debbie' 'Low, John N.' 'McWilliam, Susan A.' 'Skakle, Janet M. S.' 'Wardell, James L.' 'Glidewell, Christopher' _publ_section_title ; Soft C---H···O hydrogen bonds in methyl 2,4-dinitrobenzenesulfenate: sheets built from R~2~^2^(10) and R~6~^6^(42) rings ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 600 _journal_page_last 603 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C7 H6 N2 O5 S' _chemical_formula_sum 'C7 H6 N2 O5 S' _chemical_formula_weight 230.20 _chemical_name_systematic ; Methyl 2,4-dinitrobenzenesulfenate ; _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' _cell_angle_alpha 90 _cell_angle_beta 97.1830(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.0413(2) _cell_length_b 16.6702(10) _cell_length_c 14.0749(8) _cell_measurement_reflns_used 2643 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 29.74 _cell_measurement_theta_min 2.85 _cell_volume 940.77(9) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL97 and PRPKAPPA (Ferguson, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full .985 _diffrn_measured_fraction_theta_max .985 _diffrn_measurement_device_type 'Bruker SMART area CCD detector' _diffrn_measurement_method \f-\w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .036 _diffrn_reflns_av_sigmaI/netI .037 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 9619 _diffrn_reflns_theta_full 32.6 _diffrn_reflns_theta_max 32.6 _diffrn_reflns_theta_min 1.9 _exptl_absorpt_coefficient_mu .348 _exptl_absorpt_correction_T_max .934 _exptl_absorpt_correction_T_min .903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 472 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _refine_diff_density_max .40 _refine_diff_density_min -.29 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .90 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 3370 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .90 _refine_ls_R_factor_all .087 _refine_ls_R_factor_gt .049 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0836P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .141 _reflns_number_gt 1920 _reflns_number_total 3370 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gg1044.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2011975 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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 -.1474(3) .76321(10) .51697(10) .0401(3) Uani d . 1 . . C S1 -.29309(10) .85383(3) .46521(3) .05327(16) Uani d . 1 . . S O1 -.4346(3) .89634(8) .55651(10) .0618(4) Uani d . 1 . . O C7 -.1966(6) .94450(13) .61738(16) .0692(6) Uani d . 1 . . C C2 .0124(4) .70494(10) .46748(10) .0422(3) Uani d . 1 . . C N2 .0589(4) .71954(10) .36886(9) .0545(4) Uani d . 1 . . N O21 -.0662(4) .78125(10) .33211(8) .0665(4) Uani d . 1 . . O O22 .2229(5) .67316(11) .32747(10) .0921(6) Uani d . 1 . . O C3 .1306(4) .63358(10) .50802(11) .0445(4) Uani d . 1 . . C C4 .0846(4) .61974(10) .60154(11) .0438(3) Uani d . 1 . . C N4 .2140(4) .54539(10) .64745(11) .0600(4) Uani d . 1 . . N O41 .3590(5) .49897(10) .60188(14) .0920(5) Uani d . 1 . . O O42 .1735(5) .53473(11) .73044(12) .0984(6) Uani d . 1 . . O C5 -.0760(4) .67448(11) .65373(10) .0463(4) Uani d . 1 . . C C6 -.1897(4) .74511(11) .61237(10) .0451(4) Uani d . 1 . . C H71 -.0015 .9131 .6377 .104 Uiso calc R 1 . . H H72 -.2952 .9619 .6724 .104 Uiso calc R 1 . . H H73 -.1352 .9904 .5823 .104 Uiso calc R 1 . . H H3 .2373 .5962 .4733 .053 Uiso calc R 1 . . H H5 -.1066 .6633 .7168 .056 Uiso calc R 1 . . H H6 -.2968 .7818 .6479 .054 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 C1 .0337(7) .0512(9) .0349(6) -.0043(6) .0021(5) -.0028(6) S1 .0496(2) .0592(3) .0499(2) .00549(19) .00178(17) .00340(19) O1 .0497(6) .0645(8) .0723(8) .0088(6) .0121(6) -.0067(7) C7 .0762(13) .0595(12) .0748(13) -.0020(10) .0211(11) -.0164(10) C2 .0409(7) .0568(9) .0296(6) -.0064(7) .0064(5) -.0038(6) N2 .0602(9) .0712(10) .0333(6) -.0015(7) .0111(6) -.0011(6) O21 .0737(9) .0853(10) .0399(6) .0071(7) .0049(6) .0121(6) O22 .1339(15) .1009(13) .0502(7) .0296(11) .0456(9) -.0002(8) C3 .0447(8) .0489(9) .0409(7) -.0031(7) .0094(6) -.0062(6) C4 .0425(7) .0484(9) .0403(7) -.0072(6) .0046(6) .0016(6) N4 .0616(9) .0586(10) .0601(9) -.0031(8) .0081(7) .0094(8) O41 .1170(13) .0693(10) .0941(11) .0315(10) .0303(10) .0129(9) O42 .1372(16) .0921(13) .0704(10) .0226(11) .0310(11) .0377(9) C5 .0470(8) .0607(10) .0316(6) -.0096(7) .0064(6) -.0020(6) C6 .0441(8) .0552(10) .0371(7) -.0032(7) .0097(6) -.0076(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 C1 C2 . 1.399(2) y C2 C3 . 1.379(2) y C3 C4 . 1.372(2) y C4 C5 . 1.383(2) y C5 C6 . 1.367(2) y C1 C6 . 1.407(2) y C2 N2 . 1.4445(19) y C4 N4 . 1.464(2) y N2 O21 . 1.231(2) y N2 O22 . 1.214(2) y N4 O41 . 1.203(2) y N4 O42 . 1.213(2) y C1 S1 . 1.7471(17) y S1 O1 . 1.6322(13) y O1 C7 . 1.448(2) y C3 H3 . .930 no C5 H5 . .930 no C6 H6 . .930 no C7 H71 . .960 no C7 H72 . .960 no C7 H73 . .960 no 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' S S .1246 .1234 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 C1 C6 116.41(15) no C2 C1 S1 123.04(11) no C6 C1 S1 120.55(13) no C1 S1 O1 100.38(7) y S1 O1 C7 115.74(11) y C1 C2 N2 119.01(15) no C3 C2 N2 117.59(14) no C1 C2 C3 123.40(14) no O21 N2 O22 123.43(15) no O22 N2 C2 119.89(16) no O21 N2 C2 116.64(15) no C2 C3 C4 117.44(15) no C3 C4 C5 121.84(15) no C3 C4 N4 118.84(15) no C5 C4 N4 119.31(14) no O41 N4 O42 123.56(19) no O41 N4 C4 118.69(16) no O42 N4 C4 117.74(17) no C4 C5 C6 119.80(14) no C1 C6 C5 121.09(15) no C2 C3 H3 121.3 no C4 C3 H3 121.3 no C4 C5 H5 120.1 no C6 C5 H5 120.1 no C5 C6 H6 119.4 no C1 C6 H6 119.4 no O1 C7 H71 109.5 no O1 C7 H72 109.5 no O1 C7 H73 109.5 no H71 C7 H72 109.5 no H72 C7 H73 109.5 no H73 C7 H71 109.5 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 _geom_hbond_publ_flag C3 H3 O41 3_666 .93 2.59 3.511(2) 169 y C7 H72 O42 4_567 .96 2.49 3.405(3) 159 y 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 _geom_torsion_publ_flag C2 C1 S1 O1 -177.65(13) y C1 C2 N2 O21 -4.6(2) y C1 C2 N2 O22 173.38(17) y C3 C2 N2 O21 175.67(16) no C3 C2 N2 O22 -6.4(3) no C1 S1 O1 C7 89.37(14) y C3 C4 N4 O41 .5(3) y C3 C4 N4 O42 179.28(17) y C5 C4 N4 O41 -178.55(18) no C5 C4 N4 O42 .2(2) no _cod_database_fobs_code 2011975 _journal_paper_doi 10.1107/S0108270101002852