#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000416.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_4000416 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm049594l _journal_year 2004 _chemical_formula_sum 'C10 H17 N3 O3 S' _chemical_formula_weight 259.33 _chemical_name_common 'guanidinium propylbenzenesulfonate' _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 22.130(2) _cell_length_b 7.5101(8) _cell_length_c 7.6858(8) _cell_measurement_reflns_used 2140 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 51.635 _cell_measurement_theta_min 5.424 _cell_volume 1277.4(2) _diffrn_ambient_temperature 273(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_number 7506 _diffrn_reflns_theta_max 26.99 _diffrn_reflns_theta_min 1.84 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_correction_T_min 0.911269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 98 _refine_ls_number_reflns 1503 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.170 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0660 _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^)+(0.0993P)^2^+1.1316P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1878 _refine_ls_wR_factor_ref 0.2002 _reflns_number_gt 1071 _reflns_number_total 1503 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M Pnma _cod_database_code 4000416 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 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 _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.35325(5) 0.2500 0.58789(15) 0.0337(4) Uani 1 2 d S . . O1 O 0.29335(14) 0.2500 0.5075(5) 0.0442(9) Uani 1 2 d S . . N1 N 0.26538(12) 0.0968(4) -0.0392(4) 0.0407(7) Uani 1 1 d . . . H1A H 0.2494 -0.0021 -0.0066 0.049 Uiso 1 1 calc R . . H1B H 0.2978 0.0962 -0.1008 0.049 Uiso 1 1 calc R . . C1 C 0.4059(2) 0.2500 0.4185(6) 0.0381(11) Uani 1 2 d S . . O2 O 0.36340(10) 0.0895(3) 0.6907(3) 0.0401(6) Uani 1 1 d . . . N2 N 0.19023(17) 0.2500 0.1006(5) 0.0384(9) Uani 1 2 d S . . H2A H 0.1743 0.3492 0.1329 0.046 Uiso 0.50 1 calc PR . . H2B H 0.1737 0.1508 0.1300 0.046 Uiso 0.50 1 calc PR . . C2 C 0.4656(3) 0.2500 0.4488(11) 0.139(5) Uani 1 2 d S . . H2 H 0.4802 0.2500 0.5623 0.166 Uiso 1 2 calc SR . . C3 C 0.5065(4) 0.2500 0.3054(15) 0.149(5) Uani 1 2 d S . . H3 H 0.5479 0.2500 0.3260 0.178 Uiso 1 2 calc SR . . C4 C 0.4857(4) 0.2500 0.1381(10) 0.078(2) Uani 1 2 d SD . . C5 C 0.4262(4) 0.2500 0.1141(9) 0.080(2) Uani 1 2 d S . . H5 H 0.4111 0.2500 0.0012 0.096 Uiso 1 2 calc SR . . C6 C 0.3869(3) 0.2500 0.2497(8) 0.0680(19) Uani 1 2 d S . . H6 H 0.3456 0.2500 0.2267 0.082 Uiso 1 2 calc SR . . C7 C 0.5248(4) 0.2500 -0.0435(12) 0.105(3) Uani 1 2 d SD . . H7A H 0.5154 0.1451 -0.1119 0.125 Uiso 0.50 1 calc PR . . H7B H 0.5154 0.3549 -0.1119 0.125 Uiso 0.50 1 calc PR . . C8 C 0.5865(4) 0.2500 0.0037(11) 0.109(3) Uani 1 2 d SD . . H8A H 0.5969 0.1447 0.0703 0.131 Uiso 0.50 1 calc PR . . H8B H 0.5969 0.3553 0.0703 0.131 Uiso 0.50 1 calc PR . . C9 C 0.6195(4) 0.2500 -0.1856(11) 0.103(3) Uani 1 2 d SD . . H9A H 0.6004 0.1640 -0.2599 0.154 Uiso 0.50 1 calc PR . . H9B H 0.6614 0.2199 -0.1715 0.154 Uiso 0.50 1 calc PR . . H9C H 0.6162 0.3661 -0.2370 0.154 Uiso 0.50 1 calc PR . . C10 C 0.2401(2) 0.2500 0.0057(6) 0.0331(10) Uani 1 2 d 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0305(6) 0.0338(6) 0.0366(6) 0.000 -0.0001(5) 0.000 O1 0.0322(17) 0.0357(19) 0.065(2) 0.000 -0.0087(17) 0.000 N1 0.0391(15) 0.0320(15) 0.0511(17) 0.0002(13) 0.0112(13) 0.0003(12) C1 0.038(2) 0.037(3) 0.040(2) 0.000 0.006(2) 0.000 O2 0.0455(13) 0.0351(13) 0.0398(13) 0.0034(10) 0.0009(10) 0.0017(10) N2 0.039(2) 0.034(2) 0.042(2) 0.000 0.0047(18) 0.000 C2 0.038(3) 0.318(16) 0.060(4) 0.000 0.002(3) 0.000 C3 0.050(4) 0.272(15) 0.124(8) 0.000 0.029(5) 0.000 C4 0.113(7) 0.058(4) 0.064(4) 0.000 0.038(5) 0.000 C5 0.100(6) 0.098(6) 0.042(3) 0.000 0.022(4) 0.000 C6 0.066(4) 0.095(5) 0.044(3) 0.000 -0.003(3) 0.000 C7 0.106(6) 0.054(4) 0.154(9) 0.000 -0.069(7) 0.000 C8 0.153(9) 0.073(5) 0.102(7) 0.000 -0.067(7) 0.000 C9 0.120(7) 0.090(6) 0.097(6) 0.000 0.067(6) 0.000 C10 0.032(2) 0.036(2) 0.031(2) 0.000 -0.0024(19) 0.000