#------------------------------------------------------------------------------ #$Date: 2013-12-28 09:07:06 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91932 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/27/1502703.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1502703 loop_ _publ_author_name 'Zeng, Xiaoqing' 'Gerken, Michael' 'Beckers, Helmut' 'Willner, Helge' _publ_section_title ; Anomeric effects in sulfonyl compounds: an experimental and computational study of fluorosulfonyl azide, FSO(2)N(3), and trifluoromethylsulfonyl azide, CF(3)SO(2)N(3). ; _journal_issue 28 _journal_name_full 'The journal of physical chemistry. A' _journal_page_first 7624 _journal_page_last 7630 _journal_volume 114 _journal_year 2010 _chemical_formula_sum 'F N3 O2 S' _chemical_formula_weight 125.09 _chemical_name_systematic ; ? ; _space_group_IT_number 9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 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 121.37(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.0017(13) _cell_length_b 13.5124(15) _cell_length_c 5.0170(9) _cell_measurement_reflns_used 635 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.5225 _cell_measurement_theta_min 3.7195 _cell_volume 405.27(17) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 16.2705 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.881 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 805 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.59 _diffrn_reflns_theta_min 3.73 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'thick needle' _exptl_crystal_F_000 248 _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.097 _exptl_crystal_size_min 0.065 _refine_diff_density_max 0.231 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.062 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(13) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_matrix_type full _refine_ls_number_parameters 64 _refine_ls_number_reflns 531 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0260 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.0655 _reflns_number_gt 507 _reflns_number_total 531 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file jp103616q_si_002.cif _[local]_cod_data_source_block mg_20c _[local]_cod_cif_authors_sg_H-M Cc _cod_original_cell_volume 405.25(12) _cod_database_code 1502703 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag S1 S 0.40352(10) 0.35638(5) 0.10356(12) 0.01902(19) Uani 1 1 d N1 N 0.2617(5) 0.3156(2) 0.2598(6) 0.0245(6) Uani 1 1 d N2 N 0.0899(5) 0.36745(19) 0.1863(6) 0.0201(6) Uani 1 1 d N3 N -0.0661(6) 0.4056(2) 0.1335(9) 0.0307(7) Uani 1 1 d O1 O 0.2811(4) 0.42470(17) -0.1402(6) 0.0249(5) Uani 1 1 d O2 O 0.5128(4) 0.27410(16) 0.0724(5) 0.0279(6) Uani 1 1 d F1 F 0.5874(4) 0.41618(17) 0.3825(5) 0.0340(6) Uani 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0214(3) 0.0185(3) 0.0192(3) -0.0014(3) 0.0119(3) 0.0006(4) N1 0.0324(16) 0.0228(13) 0.0245(13) 0.0063(10) 0.0192(12) 0.0077(12) N2 0.0256(15) 0.0200(12) 0.0185(13) 0.0009(9) 0.0142(11) -0.0027(12) N3 0.0291(18) 0.0291(12) 0.0394(17) 0.0036(15) 0.0216(16) 0.0006(15) O1 0.0324(13) 0.0213(12) 0.0250(12) 0.0043(8) 0.0177(11) 0.0017(10) O2 0.0277(13) 0.0266(12) 0.0289(13) -0.0033(9) 0.0144(11) 0.0062(10) F1 0.0286(11) 0.0361(12) 0.0301(10) -0.0139(9) 0.0103(9) -0.0063(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' F F 0.0171 0.0103 '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 O2 S1 O1 122.82(15) O2 S1 F1 105.63(15) O1 S1 F1 106.63(13) O2 S1 N1 106.64(15) O1 S1 N1 112.76(15) F1 S1 N1 99.68(14) N2 N1 S1 113.0(2) N3 N2 N1 173.3(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O2 1.404(2) S1 O1 1.411(2) S1 F1 1.547(2) S1 N1 1.648(3) N1 N2 1.270(4) N2 N3 1.108(4) 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 N1 N2 -14.8(3) O2 S1 N1 N2 -152.4(2) F1 S1 N1 N2 97.9(2) S1 N1 N2 N3 168(3) _journal_paper_doi 10.1021/jp103616q