#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000076.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_4000076 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_name_common bis(guanidinium)(4,4'-biphenyldisulfonate).3(2 _chemical_formula_sum 'C25 H28 N3 O3 S' _chemical_formula_weight 450.56 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' 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' _cell_length_a 7.5382(5) _cell_length_b 25.5444(16) _cell_length_c 11.9693(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.6560(10) _cell_angle_gamma 90.00 _cell_volume 2302.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5670 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.98 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type simulated psi-scans _exptl_absorpt_correction_T_min 0.9501 _exptl_absorpt_correction_T_max 0.9630 _exptl_absorpt_process_details 'SADABS, G. Sheldrick _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART platform CCD, Bruker (or Siemens)' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11908 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4038 _reflns_number_gt 3257 _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^)+(0.0546P)^2^+0.5488P] 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_number_reflns 4038 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _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 0.40479(5) 0.204734(18) 0.55202(4) 0.02836(14) Uani 1 1 d . . . O1 O 0.55724(15) 0.22799(5) 0.49909(10) 0.0329(3) Uani 1 1 d . . . O2 O 0.40476(16) 0.21653(5) 0.67098(10) 0.0338(3) Uani 1 1 d . . . O3 O 0.23853(15) 0.21840(5) 0.49183(10) 0.0327(3) Uani 1 1 d . . . N4 N 0.9080(2) 0.23095(6) 0.60135(13) 0.0347(4) Uani 1 1 d . . . H4A H 0.8057 0.2266 0.5640 0.042 Uiso 1 1 calc R . . H4B H 1.0079 0.2242 0.5690 0.042 Uiso 1 1 calc R . . C6 C 0.3731(2) 0.11212(7) 0.43899(15) 0.0324(4) Uani 1 1 d . . . H6 H 0.3157 0.1320 0.3808 0.039 Uiso 1 1 calc R . . C1 C 0.4295(2) 0.13626(7) 0.53817(14) 0.0269(4) Uani 1 1 d . . . N7 N 0.76102(19) 0.25785(6) 0.75489(13) 0.0357(4) Uani 1 1 d . . . H7A H 0.6586 0.2535 0.7177 0.043 Uiso 1 1 calc R . . H7B H 0.7636 0.2689 0.8245 0.043 Uiso 1 1 calc R . . C4 C 0.4854(2) 0.02868(7) 0.50817(14) 0.0273(4) Uani 1 1 d . . . C5A C 1.1025(2) -0.03981(8) 0.13366(16) 0.0338(4) Uani 1 1 d . . . H5A H 1.1559 -0.0339 0.0644 0.041 Uiso 1 1 calc R . . N10 N 1.0659(2) 0.25437(7) 0.76200(13) 0.0381(4) Uani 1 1 d . . . H10A H 1.1659 0.2477 0.7295 0.046 Uiso 1 1 calc R . . H10B H 1.0684 0.2655 0.8317 0.046 Uiso 1 1 calc R . . C1A C 0.9128(2) 0.03834(8) 0.36357(15) 0.0328(4) Uani 1 1 d . . . H1A H 0.8602 0.0325 0.4331 0.039 Uiso 1 1 calc R . . C7 C 0.9115(2) 0.24762(7) 0.70593(15) 0.0304(4) Uani 1 1 d . . . C2 C 0.5136(2) 0.10691(8) 0.62250(16) 0.0346(4) Uani 1 1 d . . . H2 H 0.5524 0.1232 0.6907 0.041 Uiso 1 1 calc R . . C5 C 0.4004(2) 0.05914(7) 0.42477(15) 0.0328(4) Uani 1 1 d . . . H5 H 0.3605 0.0430 0.3566 0.039 Uiso 1 1 calc R . . C2A C 0.9318(2) 0.08877(8) 0.32633(16) 0.0349(4) Uani 1 1 d . . . C3 C 0.5409(3) 0.05393(8) 0.60720(16) 0.0357(5) Uani 1 1 d . . . H3 H 0.5988 0.0342 0.6655 0.043 Uiso 1 1 calc R . . C8A C 0.9480(2) -0.05737(8) 0.33699(16) 0.0349(5) Uani 1 1 d . . . H8A H 0.8957 -0.0641 0.4063 0.042 Uiso 1 1 calc R . . C10A C 1.0487(2) 0.00364(7) 0.19746(15) 0.0298(4) Uani 1 1 d . . . C9A C 0.9694(2) -0.00509(7) 0.30142(15) 0.0298(4) Uani 1 1 d . . . C4A C 1.0692(2) 0.05595(8) 0.16064(16) 0.0349(5) Uani 1 1 d . . . H4A1 H 1.1229 0.0626 0.0918 0.042 Uiso 1 1 calc R . . C7A C 1.0012(2) -0.09839(8) 0.27325(16) 0.0362(5) Uani 1 1 d . . . H7A1 H 0.9855 -0.1332 0.2992 0.043 Uiso 1 1 calc R . . C3A C 1.0123(2) 0.09694(8) 0.22318(17) 0.0377(5) Uani 1 1 d . . . H3A H 1.0271 0.1317 0.1968 0.045 Uiso 1 1 calc R . . C6A C 1.0793(2) -0.09010(8) 0.16947(16) 0.0349(4) Uani 1 1 d . . . C11A C 0.8690(3) 0.13487(9) 0.39251(19) 0.0478(5) Uani 1 1 d . . . H11A H 0.8284 0.1227 0.4646 0.072 Uiso 1 1 calc R . . H11B H 0.7707 0.1522 0.3507 0.072 Uiso 1 1 calc R . . H11C H 0.9670 0.1597 0.4052 0.072 Uiso 1 1 calc R . . C12A C 1.1357(3) -0.13625(8) 0.10018(19) 0.0466(5) Uani 1 1 d . . . H12A H 1.1718 -0.1238 0.0272 0.070 Uiso 1 1 calc R . . H12B H 1.0361 -0.1607 0.0896 0.070 Uiso 1 1 calc R . . H12C H 1.2358 -0.1541 0.1389 0.070 Uiso 1 1 calc R . . C5B C 0.4559(2) 0.00338(8) 0.94651(16) 0.0348(5) Uani 1 1 d . . . C2B C 0.5717(3) -0.09687(9) 1.01916(18) 0.0422(5) Uani 1 1 d . . . C4B C 0.4275(2) -0.04121(9) 0.87837(16) 0.0404(5) Uani 1 1 d . . . H4B1 H 0.3690 -0.0374 0.8068 0.048 Uiso 1 1 calc R . . C3B C 0.4825(3) -0.08958(9) 0.91339(18) 0.0449(5) Uani 1 1 d . . . H3B H 0.4607 -0.1190 0.8661 0.054 Uiso 1 1 calc R . . C1B C 0.6007(2) -0.05426(8) 1.08635(17) 0.0392(5) Uani 1 1 d . . . H1B H 0.6606 -0.0588 1.1573 0.047 Uiso 1 1 calc R . . C6B C 0.6328(3) -0.15089(10) 1.0541(2) 0.0607(7) Uani 1 1 d . . . H6B1 H 0.6836 -0.1497 1.1310 0.091 Uiso 1 1 calc R . . H6B2 H 0.7231 -0.1631 1.0039 0.091 Uiso 1 1 calc R . . H6B3 H 0.5314 -0.1749 1.0503 0.091 Uiso 1 1 calc R . . 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 0.0232(2) 0.0344(3) 0.0274(3) 0.00110(19) 0.00031(17) -0.00003(18) O1 0.0257(6) 0.0395(8) 0.0333(7) 0.0045(6) 0.0003(5) -0.0038(5) O2 0.0323(7) 0.0407(8) 0.0284(7) -0.0027(6) 0.0003(5) 0.0010(6) O3 0.0235(6) 0.0418(8) 0.0326(7) 0.0012(6) -0.0011(5) 0.0041(5) N4 0.0248(8) 0.0480(10) 0.0309(9) -0.0077(7) -0.0022(6) 0.0032(7) C6 0.0320(10) 0.0365(11) 0.0281(10) 0.0040(8) -0.0059(8) 0.0009(8) C1 0.0196(8) 0.0347(10) 0.0266(9) 0.0016(8) 0.0026(7) -0.0015(7) N7 0.0256(8) 0.0501(10) 0.0312(9) -0.0104(7) -0.0005(7) 0.0022(7) C4 0.0194(8) 0.0364(10) 0.0262(10) 0.0010(8) 0.0020(7) -0.0011(7) C5A 0.0260(9) 0.0455(12) 0.0302(10) -0.0002(9) 0.0036(8) -0.0045(8) N10 0.0275(8) 0.0563(11) 0.0305(9) -0.0126(8) 0.0005(7) -0.0007(7) C1A 0.0217(9) 0.0510(12) 0.0257(10) -0.0025(9) -0.0007(7) -0.0033(8) C7 0.0300(10) 0.0298(10) 0.0311(10) -0.0015(8) -0.0008(8) -0.0009(8) C2 0.0369(10) 0.0401(11) 0.0261(10) -0.0035(8) -0.0055(8) 0.0018(9) C5 0.0352(10) 0.0365(11) 0.0260(10) -0.0012(8) -0.0057(8) -0.0019(8) C2A 0.0247(9) 0.0451(12) 0.0344(11) -0.0062(9) -0.0040(8) -0.0029(8) C3 0.0404(11) 0.0385(11) 0.0275(10) 0.0024(8) -0.0062(8) 0.0069(9) C8A 0.0271(9) 0.0490(13) 0.0286(10) 0.0072(9) 0.0008(8) -0.0030(8) C10A 0.0224(9) 0.0409(11) 0.0259(10) 0.0005(8) -0.0023(7) -0.0043(8) C9A 0.0206(9) 0.0431(11) 0.0252(10) 0.0017(8) -0.0028(7) -0.0028(8) C4A 0.0331(10) 0.0434(12) 0.0280(10) 0.0023(9) 0.0019(8) -0.0091(9) C7A 0.0323(10) 0.0394(11) 0.0367(11) 0.0070(9) -0.0004(8) -0.0012(8) C3A 0.0365(11) 0.0387(11) 0.0374(11) 0.0013(9) -0.0033(9) -0.0068(9) C6A 0.0263(9) 0.0410(12) 0.0371(11) 0.0000(9) 0.0000(8) 0.0005(8) C11A 0.0411(12) 0.0519(14) 0.0505(14) -0.0137(11) 0.0027(10) 0.0003(10) C12A 0.0426(12) 0.0458(13) 0.0519(13) -0.0026(10) 0.0084(10) 0.0026(10) C5B 0.0225(9) 0.0543(13) 0.0277(10) 0.0024(9) 0.0011(7) -0.0068(9) C2B 0.0281(10) 0.0548(14) 0.0440(13) 0.0037(10) 0.0052(9) -0.0031(9) C4B 0.0293(10) 0.0632(15) 0.0283(10) -0.0016(10) -0.0022(8) -0.0076(10) C3B 0.0354(11) 0.0555(14) 0.0438(13) -0.0098(11) 0.0030(9) -0.0094(10) C1B 0.0269(10) 0.0608(14) 0.0300(11) 0.0064(10) 0.0007(8) -0.0046(9) C6B 0.0510(14) 0.0607(16) 0.0708(17) 0.0012(13) 0.0053(12) 0.0043(12)