#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/69/2006952.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_2006952 loop_ _publ_author_name 'Ziemer, Burkhard' 'Sauer, Erika' _publ_contact_author ; Burkhard Ziemer Institut f\"ur Chemie Humboldt-Universit\"at zu Berlin Hessische Str. 1-2 10115 Berlin Bundesrepublik Deutschland ; _publ_section_title ; 4-Azidobenzenesulfonyl Chloride ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9700034 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'C6 H4 Cl N3 O2 S' _chemical_formula_sum 'C6 H4 Cl N3 O2 S' _chemical_formula_weight 217.63 _chemical_melting_point 333.0(10) _chemical_name_systematic ; 4-Azidobenzenesulfonyl chloride ; _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' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 107.57(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.1249(15) _cell_length_b 10.900(2) _cell_length_c 10.132(2) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 3.2 _cell_volume 855.4(3) _computing_cell_refinement 'IPDS-2.75 (Stoe, 1997)' _computing_data_collection 'IPDS-2.75 (Stoe, 1997)' _computing_data_reduction 'IPDS-2.75 (Stoe, 1997)' _computing_molecular_graphics 'XSTEP-2.04 (Stoe, (1996)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 180(2) _diffrn_detector_area_resol_mean 6.667 _diffrn_measurement_device 'STOE Ipds diffractometer' _diffrn_measurement_method \f-rotation,\f-total=220\%,\f-incr.=1.4\% _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71071 _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 7124 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description cube-like _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.46 _refine_diff_density_max 0.388 _refine_diff_density_min -0.421 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.102 _refine_ls_goodness_of_fit_obs 1.142 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 134 _refine_ls_number_reflns 1483 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.597 _refine_ls_restrained_S_obs 1.142 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_obs .0319 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.1292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1352 _refine_ls_wR_factor_obs .0918 _reflns_number_observed 1352 _reflns_number_total 1484 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file qa0025.cif _[local]_cod_data_source_block sauer16 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_original_cell_volume 855.5(3) _cod_database_code 2006952 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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol C1 .1586(2) .1554(2) -.0185(2) .0246(4) Uani d . 1 . C C2 .1897(3) .1278(2) -.1432(2) .0283(4) Uani d . 1 . C H2 .164(4) .185(2) -.215(3) .051(7) Uiso d . 1 . H C3 .2634(3) .0160(2) -.1557(2) .0288(4) Uani d . 1 . C H3 .289(3) -.003(2) -.238(2) .036(5) Uiso d . 1 . H C4 .3041(2) -.0662(2) -.0455(2) .0242(4) Uani d . 1 . C C5 .2731(2) -.0365(2) .0783(2) .0251(4) Uani d . 1 . C H5 .296(3) -.089(2) .142(3) .038(6) Uiso d . 1 . H C6 .1991(3) .0749(2) .0918(2) .0256(4) Uani d . 1 . C H6 .172(3) .0958(18) .173(2) .030(5) Uiso d . 1 . H Cl .27396(8) .40907(4) .06774(6) .0462(2) Uani d . 1 . Cl N41 .3815(2) -.17792(14) -.0672(2) .0298(4) Uani d . 1 . N N42 .4161(2) -.25245(15) .0307(2) .0301(4) Uani d . 1 . N N43 .4566(3) -.3279(2) .1101(2) .0435(5) Uani d . 1 . N O1 -.0271(3) .3436(2) -.1352(2) .0655(6) Uani d . 1 . O O2 -.0117(2) .29354(12) .1059(2) .0428(4) Uani d . 1 . O S1 .06459(7) .29709(4) -.00289(5) .0309(2) Uani d . 1 . S 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 .0232(10) .0241(9) .0229(8) -.0011(7) .0017(7) -.0042(7) C2 .0327(11) .0311(9) .0181(8) -.0032(8) .0029(7) .0004(8) C3 .0360(12) .0334(10) .0163(8) -.0048(8) .0070(8) -.0051(8) C4 .0232(10) .0233(8) .0253(9) -.0054(7) .0061(7) -.0061(7) C5 .0294(11) .0251(9) .0196(8) -.0020(7) .0058(8) .0012(7) C6 .0269(10) .0294(9) .0197(9) -.0019(7) .0061(7) -.0036(7) Cl .0530(4) .0288(3) .0671(4) -.0090(2) .0335(3) -.0133(2) N41 .0366(10) .0264(8) .0282(8) .0002(7) .0124(7) -.0034(7) N42 .0318(9) .0252(8) .0374(9) -.0023(7) .0169(7) -.0067(8) N43 .0561(13) .0303(9) .0506(11) .0061(9) .0261(10) .0062(9) O1 .0787(15) .0642(11) .0363(9) .0428(11) -.0088(9) .0027(8) O2 .0396(9) .0381(8) .0584(10) .0031(6) .0264(8) -.0046(7) S1 .0295(3) .0305(3) .0293(3) .0082(2) .0037(2) -.0003(2) 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 C6 . 1.381(3) ? C1 C2 . 1.394(2) ? C1 S1 . 1.752(2) ? C2 C3 . 1.380(3) ? C2 H2 . .94(3) ? C3 C4 . 1.391(3) ? C3 H3 . .94(2) ? C4 C5 . 1.390(2) ? C4 N41 . 1.418(2) ? C5 C6 . 1.380(3) ? C5 H5 . .84(2) ? C6 H6 . .94(2) ? Cl S1 . 2.0398(8) ? N41 N42 . 1.247(2) ? N42 N43 . 1.128(2) ? O1 S1 . 1.416(2) ? O2 S1 . 1.419(2) ? 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 C6 C1 C2 122.2(2) C6 C1 S1 119.43(14) C2 C1 S1 118.41(14) C3 C2 C1 118.4(2) C3 C2 H2 121.2(15) C1 C2 H2 120.3(15) C2 C3 C4 120.0(2) C2 C3 H3 119.6(14) C4 C3 H3 120.4(14) C5 C4 C3 120.7(2) C5 C4 N41 123.3(2) C3 C4 N41 116.0(2) C6 C5 C4 119.8(2) C6 C5 H5 121.9(15) C4 C5 H5 118.2(15) C5 C6 C1 118.9(2) C5 C6 H6 121.5(13) C1 C6 H6 119.5(13) N42 N41 C4 116.14(15) N43 N42 N41 171.8(2) O1 S1 O2 121.09(12) O1 S1 C1 110.45(9) O2 S1 C1 110.55(8) O1 S1 Cl 105.22(11) O2 S1 Cl 104.92(8) C1 S1 Cl 102.67(7) 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 C6 C1 C2 C3 0.1(3) S1 C1 C2 C3 -179.85(15) C1 C2 C3 C4 0.2(3) C2 C3 C4 C5 -0.7(3) C2 C3 C4 N41 -179.2(2) C3 C4 C5 C6 0.8(3) N41 C4 C5 C6 179.2(2) C4 C5 C6 C1 -0.5(3) C2 C1 C6 C5 0.1(3) S1 C1 C6 C5 179.98(14) C5 C4 N41 N42 2.4(3) C3 C4 N41 N42 -179.1(2) C4 N41 N42 N43 -173.9(14) C6 C1 S1 O1 -157.0(2) C2 C1 S1 O1 23.0(2) C6 C1 S1 O2 -20.2(2) C2 C1 S1 O2 159.7(2) C6 C1 S1 Cl 91.3(2) C2 C1 S1 Cl -88.8(2) _cod_database_fobs_code 2006952 _journal_paper_doi 10.1107/S0108270198099879