#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000418.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_4000418 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_name_common 'Guanidinium heptylbenzenesulfonate' _chemical_formula_sum 'C14 H25 N3 O3 S' _chemical_formula_weight 315.43 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.1549(7) _cell_length_b 11.9854(12) _cell_length_c 20.579(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1764.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2217 _cell_measurement_theta_min 5.218 _cell_measurement_theta_max 46.824 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.733588 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10862 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3800 _reflns_number_gt 2272 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(15) _refine_ls_number_reflns 3800 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.24761(19) 0.31224(6) 0.17974(4) 0.0407(2) Uani 1 1 d . . . O1 O 0.2518(5) 0.41671(16) 0.21598(10) 0.0443(5) Uani 1 1 d . . . N1 N 0.4071(5) 0.0317(3) 0.25206(15) 0.0438(9) Uani 1 1 d . . . H1A H 0.4065 0.0983 0.2365 0.053 Uiso 1 1 calc R . . H1B H 0.5109 0.0013 0.2635 0.053 Uiso 1 1 calc R . . C1 C 0.2395(7) 0.3484(2) 0.09795(15) 0.0389(8) Uani 1 1 d . . . O2 O 0.0810(4) 0.2475(2) 0.19313(14) 0.0467(8) Uani 1 1 d . . . N2 N 0.0909(6) 0.0220(3) 0.24109(16) 0.0473(10) Uani 1 1 d . . . H2A H 0.0896 0.0886 0.2255 0.057 Uiso 1 1 calc R . . H2B H -0.0119 -0.0144 0.2453 0.057 Uiso 1 1 calc R . . C2 C 0.3870(6) 0.4087(3) 0.07071(19) 0.0464(10) Uani 1 1 d . . . H2 H 0.4896 0.4285 0.0959 0.056 Uiso 1 1 calc R . . O3 O 0.4183(4) 0.2484(2) 0.18955(14) 0.0459(7) Uani 1 1 d . . . N3 N 0.2515(6) -0.12623(18) 0.28172(13) 0.0469(7) Uani 1 1 d . . . H3A H 0.1490 -0.1631 0.2855 0.056 Uiso 1 1 calc R . . H3B H 0.3557 -0.1562 0.2931 0.056 Uiso 1 1 calc R . . C3 C 0.3792(6) 0.4381(3) 0.0067(2) 0.0518(10) Uani 1 1 d . . . H3 H 0.4792 0.4769 -0.0113 0.062 Uiso 1 1 calc R . . C4 C 0.2283(8) 0.4124(3) -0.03226(18) 0.0532(10) Uani 1 1 d . . . C5 C 0.0854(6) 0.3515(3) -0.0043(2) 0.0597(12) Uani 1 1 d . . . H5 H -0.0165 0.3310 -0.0297 0.072 Uiso 1 1 calc R . . C6 C 0.0898(6) 0.3208(3) 0.0594(2) 0.0501(10) Uani 1 1 d . . . H6 H -0.0095 0.2807 0.0769 0.060 Uiso 1 1 calc R . . C7 C 0.2205(8) 0.4525(3) -0.10097(18) 0.0692(14) Uani 1 1 d . . . H7A H 0.1407 0.4029 -0.1259 0.083 Uiso 1 1 calc R . . H7B H 0.3449 0.4490 -0.1196 0.083 Uiso 1 1 calc R . . C8 C 0.1467(7) 0.5714(4) -0.1071(2) 0.0654(13) Uani 1 1 d . . . H8A H 0.2179 0.6190 -0.0781 0.079 Uiso 1 1 calc R . . H8B H 0.1687 0.5971 -0.1511 0.079 Uiso 1 1 calc R . . C9 C -0.0591(7) 0.5851(3) -0.0917(2) 0.0594(12) Uani 1 1 d . . . H9A H -0.1310 0.5354 -0.1193 0.071 Uiso 1 1 calc R . . H9B H -0.0811 0.5635 -0.0469 0.071 Uiso 1 1 calc R . . C10 C -0.1267(7) 0.7029(4) -0.1016(3) 0.0638(14) Uani 1 1 d . . . H10A H -0.0883 0.7274 -0.1445 0.077 Uiso 1 1 calc R . . H10B H -0.0649 0.7506 -0.0701 0.077 Uiso 1 1 calc R . . C11 C -0.3352(7) 0.7195(4) -0.0954(3) 0.0621(15) Uani 1 1 d . . . H11A H -0.3973 0.6738 -0.1277 0.075 Uiso 1 1 calc R . . H11B H -0.3745 0.6933 -0.0529 0.075 Uiso 1 1 calc R . . C12 C -0.3987(8) 0.8385(4) -0.1036(3) 0.0786(15) Uani 1 1 d . . . H12A H -0.3530 0.8659 -0.1449 0.094 Uiso 1 1 calc R . . H12B H -0.3417 0.8833 -0.0697 0.094 Uiso 1 1 calc R . . C13 C -0.6072(8) 0.8556(4) -0.1011(3) 0.0793(15) Uani 1 1 d . . . H13A H -0.6643 0.8191 -0.1376 0.119 Uiso 1 1 calc R . . H13B H -0.6344 0.9340 -0.1027 0.119 Uiso 1 1 calc R . . H13C H -0.6556 0.8246 -0.0615 0.119 Uiso 1 1 calc R . . C14 C 0.2491(9) -0.0237(2) 0.25841(13) 0.0368(7) 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 0.0299(4) 0.0318(4) 0.0603(5) 0.0020(4) -0.0016(8) 0.0025(7) O1 0.0352(12) 0.0399(11) 0.0577(13) -0.0080(10) -0.0017(19) -0.004(2) N1 0.025(2) 0.0372(18) 0.069(2) 0.0118(16) 0.0021(19) -0.0015(18) C1 0.0333(19) 0.0253(13) 0.058(2) -0.0062(13) 0.003(3) 0.005(2) O2 0.0278(17) 0.0320(14) 0.080(2) 0.0071(15) 0.0045(19) -0.0034(15) N2 0.041(3) 0.0363(18) 0.065(2) 0.0088(16) -0.003(2) 0.000(2) C2 0.037(2) 0.041(2) 0.061(3) -0.0039(19) 0.0010(19) 0.000(2) O3 0.0291(17) 0.0374(14) 0.0711(19) 0.0086(15) -0.0017(19) -0.0003(15) N3 0.0296(14) 0.0369(14) 0.0741(19) 0.0130(12) -0.001(3) 0.000(2) C3 0.050(3) 0.041(2) 0.064(3) -0.001(2) 0.016(2) 0.000(2) C4 0.069(3) 0.0443(19) 0.047(2) -0.0138(16) 0.000(3) 0.006(3) C5 0.060(3) 0.053(2) 0.066(3) -0.008(2) -0.015(3) -0.012(2) C6 0.048(3) 0.040(2) 0.062(3) 0.000(2) -0.005(2) -0.009(2) C7 0.083(4) 0.072(3) 0.053(2) -0.013(2) 0.004(3) -0.007(3) C8 0.084(3) 0.066(3) 0.046(3) 0.006(2) 0.000(2) -0.014(3) C9 0.071(3) 0.058(3) 0.049(2) 0.0014(19) -0.003(2) -0.015(3) C10 0.072(4) 0.056(3) 0.064(3) 0.012(2) -0.017(3) -0.021(3) C11 0.078(4) 0.053(3) 0.055(3) 0.005(2) -0.011(2) -0.021(2) C12 0.088(4) 0.055(3) 0.093(4) 0.013(2) -0.022(3) -0.014(3) C13 0.090(4) 0.060(3) 0.088(4) 0.006(3) -0.009(3) -0.005(3) C14 0.0356(18) 0.0378(16) 0.0371(17) 0.0012(13) -0.004(3) 0.006(3)