#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003452.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_2003452 loop_ _publ_author_name 'MacNicol, D. D.' 'Mallinson, P. R.' _publ_contact_author ; Dr. P.R. Mallinson Chemistry Department University of Glasgow Glasgow G12 8QQ U.K. ; _publ_section_title ; N,N-Diethyl-4-(methylsulfonyl)-2-nitroaniline ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 926 _journal_page_last 927 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C11 H16 N2 O4 S' _chemical_formula_weight 272.32 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source ;International Tables for X-ray Crystallography (1974, Vol. IV, Tables 2.2B and 2.3.1) ; _cell_angle_alpha 90. _cell_angle_beta 90.54(2) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 5.035(1) _cell_length_b 11.684(1) _cell_length_c 21.792(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 15 _cell_measurement_theta_min 11 _cell_volume 1281.9(3) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'GX (Mallinson & Muir, 1985)' _computing_molecular_graphics 'ORTEPII (Johnson, 1971; Mallinson & Muir, 1985)' _computing_publication_material GX _computing_structure_refinement GX _computing_structure_solution 'MITHRIL (Gilmore, 1984)' _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w-2\q _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 2865 _diffrn_reflns_theta_max 27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.249 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.41 _exptl_crystal_description needle _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.6 _refine_diff_density_min -0.4 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 2.3 _refine_ls_hydrogen_treatment 'refall except H11B which was not refined' _refine_ls_number_parameters 223 _refine_ls_number_reflns 1386 _refine_ls_R_factor_obs 0.044 _refine_ls_shift/esd_max 0.23 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 1/\s^2^(F) _refine_ls_wR_factor_obs 0.053 _reflns_number_observed 1386 _reflns_number_total 2797 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file ha1134.cif _[local]_cod_data_source_block default _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_original_cell_volume 1282.0(10) _cod_database_code 2003452 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 0.6510(6) 0.2527(3) 0.5213(2) 0.041 C2 0.7487(7) 0.3245(3) 0.5662(2) 0.043 C3 0.9105(6) 0.2825(3) 0.6118(2) 0.040 C4 0.9737(7) 0.1654(3) 0.6179(2) 0.047 C5 0.8763(9) 0.0965(4) 0.5695(2) 0.057 C6 0.7225(8) 0.1383(3) 0.5228(2) 0.051 C7 0.6773(10) 0.3801(5) 0.4144(2) 0.059 C8 1.1001(8) 0.1639(4) 0.7289(2) 0.058 C9 0.8259(9) 0.1867(6) 0.7510(2) 0.075 C10 1.2456(11) 0.0061(5) 0.6587(3) 0.079 C11 1.0771(17) -0.0869(5) 0.6793(3) 0.110 N1 1.0388(6) 0.3703(3) 0.6496(1) 0.052 N2 1.1107(7) 0.1187(3) 0.6661(2) 0.061 O1 0.3417(5) 0.2130(3) 0.4285(1) 0.073 O2 0.2740(5) 0.3922(2) 0.4863(1) 0.063 O3 1.2762(5) 0.3600(3) 0.6618(1) 0.073 O4 0.9096(6) 0.4537(3) 0.6643(1) 0.077 S 0.45238(17) 0.30780(9) 0.46148(4) 0.049 H2 0.726(6) 0.396(3) 0.564(1) 0.036(9) H5 0.917(6) 0.023(3) 0.572(1) 0.034(9) H6 0.678(6) 0.091(3) 0.492(1) 0.034(8) H7A 0.784(8) 0.330(4) 0.400(2) 0.06(1) H7B 0.586(8) 0.406(4) 0.383(2) 0.07(1) H7C 0.744(8) 0.439(4) 0.439(2) 0.07(1) H8A 1.153(6) 0.110(3) 0.756(2) 0.04(1) H8B 1.210(8) 0.234(4) 0.736(2) 0.09(1) H9A 0.827(8) 0.214(4) 0.794(2) 0.09(1) H9B 0.744(10) 0.254(4) 0.727(2) 0.10(2) H9C 0.725(11) 0.104(5) 0.759(2) 0.12(2) H10A 1.404(8) -0.004(3) 0.686(2) 0.08(1) H10B 1.299(9) -0.020(4) 0.614(2) 0.10(2) H11A 1.022(10) -0.076(5) 0.722(3) 0.11(2) H11B 1.18555 -0.16589 0.67805 0.100 H11C 0.922(12) -0.085(5) 0.657(3) 0.12(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.040(2) -0.004(2) -0.002(1) 0.044(2) 0.001(2) 0.039(2) C2 0.040(2) -0.002(2) 0.002(1) 0.037(2) 0.000(2) 0.050(2) C3 0.041(2) -0.002(1) 0.000(2) 0.040(2) -0.003(2) 0.040(2) C4 0.052(2) 0.006(2) -0.003(2) 0.046(2) -0.001(2) 0.042(2) C5 0.081(3) 0.012(2) -0.004(2) 0.036(2) -0.001(2) 0.054(3) C6 0.071(3) -0.003(2) -0.004(2) 0.043(2) -0.007(2) 0.040(2) C7 0.061(3) -0.003(3) -0.004(2) 0.070(3) 0.010(2) 0.048(3) C8 0.065(3) 0.004(2) -0.013(2) 0.060(3) 0.002(2) 0.047(2) C9 0.068(3) -0.002(3) 0.003(2) 0.095(4) 0.008(3) 0.061(3) C10 0.085(3) 0.018(3) -0.022(3) 0.075(4) -0.006(3) 0.078(4) C11 0.156(6) -0.003(4) -0.049(5) 0.081(4) 0.005(4) 0.092(5) N1 0.056(2) -0.009(2) -0.006(1) 0.052(2) 0.002(2) 0.048(2) N2 0.081(2) 0.018(2) -0.014(2) 0.049(2) -0.003(2) 0.054(2) O1 0.078(2) -0.020(2) -0.032(2) 0.071(2) -0.002(2) 0.070(2) O2 0.041(1) 0.009(1) -0.006(1) 0.074(2) 0.003(2) 0.076(2) O3 0.052(2) -0.019(1) -0.017(1) 0.087(2) 0.005(2) 0.080(2) O4 0.083(2) 0.001(2) -0.011(2) 0.059(2) -0.028(2) 0.091(2) S 0.0427(5) -.0066(5) -.0127(4) 0.0535(6) 0.0027(5) 0.0520(5) 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 118.7(4) no C2 C1 S 120.0(3) no C6 C1 S 121.2(3) no C1 C2 C3 120.2(4) no C1 C2 H2 122.(2) no C3 C2 H2 118.(2) no C2 C3 C4 123.2(4) no C2 C3 N1 114.4(4) no C4 C3 N1 122.0(3) yes C3 C4 C5 114.0(4) yes C3 C4 N2 124.8(4) yes C5 C4 N2 121.1(4) no C4 C5 C6 123.0(4) no C4 C5 H5 116.(2) no C6 C5 H5 121.(2) no C1 C6 C5 120.6(4) no C1 C6 H6 121.(2) no C5 C6 H6 119.(2) no S C7 H7A 107.(3) no S C7 H7B 107.(3) no S C7 H7C 105.(3) no H7A C7 H7B 106.(4) no H7A C7 H7C 119.(4) no H7B C7 H7C 112.(4) no C9 C8 N2 114.1(4) no C9 C8 H8A 100.(2) no C9 C8 H8B 108.(3) no N2 C8 H8A 110.(2) no N2 C8 H8B 115.(3) no H8A C8 H8B 108.(3) no C8 C9 H9A 112.(3) no C8 C9 H9B 110.(3) no C8 C9 H9C 109.(3) no H9A C9 H9B 103.(4) no H9A C9 H9C 98.(4) no H9B C9 H9C 124.(4) no C11 C10 N2 111.0(5) no C11 C10 H10A 101.(2) no C11 C10 H10B 103.(3) no N2 C10 H10A 114.(2) no N2 C10 H10B 119.(3) no H10A C10 H10B 108.(4) no C10 C11 H11A 112.(3) no C10 C11 H11B 109.7(7) no C10 C11 H11C 108.(4) no H11A C11 H11B 106.(3) no H11A C11 H11C 105.(5) no H11B C11 H11C 116.(4) no O3 N1 C3 118.6(4) yes O4 N1 C3 118.5(3) yes O3 N1 O4 122.8(4) yes C8 N2 C4 123.4(4) yes C10 N2 C4 119.8(4) yes C8 N2 C10 116.1(4) yes C1 S C7 104.1(2) no C1 S O1 107.8(2) no C1 S O2 109.0(2) no C7 S O1 109.3(3) no C7 S O2 107.3(3) no O1 S O2 118.4(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 1.377(5) yes C1 C6 1.384(6) yes C1 S 1.757(4) yes C2 C3 1.371(5) yes C2 H2 0.84(4) no C3 C4 1.410(5) yes C3 N1 1.462(5) yes C4 C5 1.412(6) yes C4 N2 1.366(5) yes C5 C6 1.364(6) yes C5 H5 0.89(4) no C6 H6 0.90(4) no C7 S 1.753(6) yes C7 H7A 0.85(5) no C7 H7B 0.87(5) no C7 H7C 0.93(5) no C8 C9 1.491(7) yes C8 N2 1.467(6) yes C8 H8A 0.90(4) no C8 H8B 1.00(5) no C9 H9A 0.99(6) no C9 H9B 1.02(6) no C9 H9C 1.10(7) no C10 C11 1.452(10) yes C10 N2 1.490(7) yes C10 H10A 1.00(5) no C10 H10B 1.07(6) no C11 H11A 0.98(6) no C11 H11B 1.073(7) no C11 H11C 0.92(6) no N1 O3 1.228(5) yes N1 O4 1.216(5) yes O1 S 1.430(4) yes O2 S 1.442(3) 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 _geom_torsion_publ_flag C6 C1 S O1 13.2(3) yes C2 C1 S C7 74.2(4) yes C2 C1 S O2 -40.1(3) yes