#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/27/1502704.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_1502704 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_paper_doi 10.1021/jp103616q _journal_volume 114 _journal_year 2010 _chemical_formula_sum 'C F3 N3 O2 S' _chemical_formula_weight 175.10 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/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 106.130(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.0666(4) _cell_length_b 17.0136(10) _cell_length_c 7.0041(5) _cell_measurement_reflns_used 1358 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.3225 _cell_measurement_theta_min 3.0215 _cell_volume 579.99(7) _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 0.999 _diffrn_measured_fraction_theta_max 0.840 _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 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2572 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 29.39 _diffrn_reflns_theta_min 3.26 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94911 _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 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'square plate' _exptl_crystal_F_000 344 _exptl_crystal_size_max 0.123 _exptl_crystal_size_mid 0.096 _exptl_crystal_size_min 0.024 _refine_diff_density_max 0.217 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_matrix_type full _refine_ls_number_parameters 91 _refine_ls_number_reflns 1342 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.977 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0316 _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^)+(0.0348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.0696 _reflns_number_gt 1028 _reflns_number_total 1342 _reflns_threshold_expression >2sigma(I) _cod_data_source_file jp103616q_si_003.cif _cod_data_source_block mg_21b _cod_original_sg_symbol_H-M P21/c _cod_database_code 1502704 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.47740(9) 0.34047(3) 0.87994(6) 0.02672(14) Uani 1 1 d N1 N 0.7760(3) 0.30038(9) 0.9933(2) 0.0305(4) Uani 1 1 d N2 N 0.8908(3) 0.33445(9) 1.1577(2) 0.0299(3) Uani 1 1 d N3 N 1.0088(4) 0.35886(11) 1.3026(2) 0.0446(5) Uani 1 1 d O1 O 0.3590(3) 0.38032(8) 1.01327(18) 0.0364(3) Uani 1 1 d O2 O 0.3349(3) 0.28373(8) 0.74344(19) 0.0444(4) Uani 1 1 d C1 C 0.5820(4) 0.41756(11) 0.7335(3) 0.0337(4) Uani 1 1 d F1 F 0.6818(3) 0.38709(7) 0.59586(17) 0.0594(4) Uani 1 1 d F2 F 0.3667(3) 0.46120(7) 0.64910(16) 0.0525(4) Uani 1 1 d F3 F 0.7715(2) 0.46242(6) 0.85060(17) 0.0470(3) 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 0.0229(2) 0.0245(2) 0.0337(2) -0.00145(19) 0.00922(17) -0.0030(2) N1 0.0276(8) 0.0271(8) 0.0372(8) -0.0044(7) 0.0096(7) 0.0032(7) N2 0.0253(8) 0.0327(8) 0.0348(8) 0.0075(7) 0.0136(7) 0.0065(7) N3 0.0386(10) 0.0613(12) 0.0325(8) 0.0002(9) 0.0073(8) 0.0091(9) O1 0.0295(7) 0.0410(7) 0.0441(7) 0.0010(6) 0.0192(6) 0.0058(6) O2 0.0433(8) 0.0378(7) 0.0473(7) -0.0090(6) 0.0046(7) -0.0158(7) C1 0.0341(10) 0.0281(9) 0.0397(10) 0.0014(8) 0.0118(9) 0.0001(9) F1 0.0907(11) 0.0496(7) 0.0550(7) 0.0020(6) 0.0487(7) 0.0000(8) F2 0.0494(8) 0.0485(7) 0.0536(7) 0.0193(6) 0.0046(6) 0.0084(6) F3 0.0435(7) 0.0295(6) 0.0647(7) 0.0026(5) 0.0094(6) -0.0130(5) 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' 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 123.02(9) O2 S1 N1 105.80(8) O1 S1 N1 112.39(7) O2 S1 C1 106.51(9) O1 S1 C1 105.56(8) N1 S1 C1 101.33(9) N2 N1 S1 111.99(12) N3 N2 N1 173.52(18) F1 C1 F2 109.46(15) F1 C1 F3 108.83(17) F2 C1 F3 108.79(15) F1 C1 S1 111.03(13) F2 C1 S1 108.82(14) F3 C1 S1 109.87(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O2 1.4085(13) S1 O1 1.4153(13) S1 N1 1.6482(15) S1 C1 1.832(2) N1 N2 1.276(2) N2 N3 1.106(2) C1 F1 1.313(2) C1 F2 1.316(2) C1 F3 1.319(2) 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 -23.74(15) O2 S1 N1 N2 -160.54(12) C1 S1 N1 N2 88.49(14) S1 N1 N2 N3 176.2(16)