#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006488.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_2006488 loop_ _publ_author_name 'Moers, O.' 'Blaschette, A.' 'Jones, P. G.' _publ_section_title ; Polysulfonylamines. LXXXV. N-Chlorodimesylamine ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1305 _journal_page_last 1307 _journal_volume 53 _journal_year 1997 _chemical_formula_sum 'C2 H6 Cl N O4 S2' _chemical_formula_weight 207.65 _chemical_name_systematic ; N-chlorodimesylamine ; _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 92.282(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.8306(8) _cell_length_b 10.0242(8) _cell_length_c 9.5404(12) _cell_measurement_reflns_used 61 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 5 _cell_volume 748.28(14) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Fait, 1991)' _computing_data_reduction XSCANS _computing_molecular_graphics 'XP (Siemens, 1994b)' _computing_publication_material SHELXL93 _computing_structure_refinement SHELXL93 _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4280 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.30 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 297 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.025 _exptl_absorpt_correction_T_max 0.699 _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_type '\y scans (XEMP; Siemens, 1994a)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular tablet' _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.446 _refine_diff_density_min -0.287 _refine_ls_extinction_coef 0.033(2) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.070 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 1709 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_restrained_S_obs 1.090 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_obs 0.0207 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.3539P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0555 _refine_ls_wR_factor_obs 0.0549 _reflns_number_observed 1615 _reflns_number_total 1709 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file fg1321.cif _[local]_cod_data_source_block tirila _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2006488 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' '-x+1/2, y+1/2, -z+1/2' 'x-1/2, -y-1/2, z-1/2' 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 S1 0.01807(17) 0.01588(17) 0.01983(18) 0.00284(12) 0.00412(12) -0.00016(12) S2 0.02053(17) 0.01448(17) 0.01729(16) 0.00187(11) 0.00160(12) 0.00024(11) Cl 0.02364(17) 0.02114(18) 0.02026(17) -0.00178(12) 0.00912(12) 0.00069(12) N 0.0180(5) 0.0175(5) 0.0184(5) 0.0031(4) 0.0072(4) 0.0038(4) O1 0.0304(5) 0.0323(6) 0.0208(5) 0.0081(5) 0.0049(4) -0.0049(4) O2 0.0244(5) 0.0180(5) 0.0363(6) 0.0032(4) 0.0034(4) 0.0055(4) O3 0.0354(6) 0.0240(5) 0.0254(5) 0.0125(4) 0.0023(4) -0.0042(4) O4 0.0276(5) 0.0215(5) 0.0268(5) -0.0052(4) 0.0029(4) 0.0058(4) C1 0.0176(6) 0.0242(7) 0.0345(8) 0.0001(5) 0.0039(5) -0.0005(6) C2 0.0237(7) 0.0249(7) 0.0231(7) 0.0005(6) -0.0038(5) -0.0021(5) 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_type_symbol S1 0.39553(4) 0.70717(3) 0.21993(3) 0.01784(10) Uani d . 1 S S2 0.61668(4) 0.46789(3) 0.25547(3) 0.01741(10) Uani d . 1 S Cl 0.69353(4) 0.66711(3) 0.05166(3) 0.02146(11) Uani d . 1 Cl N 0.54365(14) 0.59784(12) 0.15566(12) 0.0178(2) Uani d . 1 N O1 0.41752(14) 0.71189(12) 0.36907(11) 0.0277(2) Uani d . 1 O O2 0.41334(13) 0.82631(10) 0.14037(12) 0.0262(2) Uani d . 1 O O3 0.71057(14) 0.38556(11) 0.16418(11) 0.0282(2) Uani d . 1 O O4 0.46579(13) 0.41731(10) 0.31566(11) 0.0252(2) Uani d . 1 O C1 0.20325(17) 0.62614(16) 0.17304(17) 0.0253(3) Uani d . 1 C H1A 0.1069 0.6799 0.2034 0.030 Uiso calc R 1 H H1B 0.2009 0.5385 0.2185 0.030 Uiso calc R 1 H H1C 0.1944 0.6147 0.0710 0.030 Uiso calc R 1 H C2 0.75356(19) 0.53710(15) 0.38553(15) 0.0240(3) Uani d . 1 C H2A 0.8127 0.4654 0.4377 0.029 Uiso calc R 1 H H2B 0.6868 0.5903 0.4499 0.029 Uiso calc R 1 H H2C 0.8378 0.5944 0.3417 0.029 Uiso calc R 1 H 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' 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' Cl Cl 0.1484 0.1585 '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 O2 S1 O1 119.52(7) y O2 S1 N 105.16(6) y O1 S1 N 108.61(6) y O2 S1 C1 110.71(7) y O1 S1 C1 109.76(7) y N S1 C1 101.40(7) y O3 S2 O4 119.72(7) y O3 S2 N 105.77(6) y O4 S2 N 103.43(6) y O3 S2 C2 110.27(7) y O4 S2 C2 110.42(7) y N S2 C2 106.04(7) y S2 N Cl 114.34(6) y S2 N S1 120.24(6) y Cl N S1 115.71(7) y loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 O2 1.4249(11) y S1 O1 1.4272(11) y S1 N 1.7260(11) y S1 C1 1.7531(15) y S2 O3 1.4251(11) y S2 O4 1.4272(10) y S2 N 1.6992(12) y S2 C2 1.7505(15) y Cl N 1.7138(11) y 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 C1 H1A O4 3_555 0.98 2.45 3.208(2) 134 y C1 H1B O2 3_545 0.98 2.69 3.628(2) 161 y C1 H1C O3 2_665 0.98 2.39 3.316(2) 157 y C2 H2A O2 3_645 0.98 2.69 3.374(2) 127 y C2 H2B O4 2_666 0.98 2.58 3.417(2) 144 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 O3 S2 N Cl -45.65(9) y O4 S2 N Cl -172.30(7) y C2 S2 N Cl 71.47(9) y O3 S2 N S1 169.79(8) y O4 S2 N S1 43.14(9) y C2 S2 N S1 -73.09(9) y O2 S1 N S2 157.69(8) y O1 S1 N S2 28.64(10) y C1 S1 N S2 -86.94(9) y O2 S1 N Cl 13.59(9) y O1 S1 N Cl -115.46(8) y C1 S1 N Cl 128.96(8) y