#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000072.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_4000072 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_name_common bis(guanidinium)(4,4'-biphenyldisulfonate).(1,8-dimethyln _chemical_formula_sum 'C26 H32 N6 O6 S2' _chemical_formula_weight 588.70 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pna2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 17.3485(12) _cell_length_b 7.4584(5) _cell_length_c 21.6256(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2798.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1922 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 24.12 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.242 _exptl_absorpt_correction_type simulated psi-scans _exptl_absorpt_correction_T_min 0.7811 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 14266 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4831 _reflns_number_gt 2441 _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^)+(0.1273P)^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 0.3(2) _refine_ls_number_reflns 4831 _refine_ls_number_parameters 293 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1458 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.2227 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.448 _refine_ls_shift/su_mean 0.063 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 0.14034(16) 0.7356(2) 0.10432(11) 0.0339(8) Uani 1 1 d . . . O1 O 0.0939(4) 0.5759(7) 0.0941(3) 0.0381(16) Uani 1 1 d . . . N1 N -0.0415(5) 0.5876(9) 0.1760(4) 0.047(2) Uani 1 1 d . . . H1A H -0.0595 0.4860 0.1908 0.056 Uiso 1 1 calc R . . H1B H -0.0084 0.5868 0.1452 0.056 Uiso 1 1 calc R . . C1 C 0.2178(6) 0.7149(11) 0.0525(5) 0.039(3) Uani 1 1 d . . . S2 S 0.61081(16) 0.7424(2) -0.20697(11) 0.0380(8) Uani 1 1 d . . . O2 O 0.0976(3) 0.8969(7) 0.0888(3) 0.0374(16) Uani 1 1 d . . . N2 N -0.0399(5) 0.9000(9) 0.1760(4) 0.047(2) Uani 1 1 d . . . H2A H -0.0566 1.0034 0.1904 0.056 Uiso 1 1 calc R . . H2B H -0.0068 0.8974 0.1452 0.056 Uiso 1 1 calc R . . C2 C 0.2078(4) 0.6651(10) -0.0087(4) 0.0350(19) Uani 1 1 d . . . H2 H 0.1582 0.6296 -0.0228 0.042 Uiso 1 1 calc R . . O3 O 0.1732(5) 0.7412(6) 0.1675(4) 0.040(2) Uani 1 1 d . . . N3 N -0.1149(5) 0.7473(8) 0.2476(6) 0.048(3) Uani 1 1 d . . . H3A H -0.1321 0.8496 0.2625 0.057 Uiso 1 1 calc R . . H3B H -0.1308 0.6453 0.2636 0.057 Uiso 1 1 calc R . . C3 C 0.2684(4) 0.6667(10) -0.0487(4) 0.0361(19) Uani 1 1 d . . . H3 H 0.2600 0.6325 -0.0905 0.043 Uiso 1 1 calc R . . O4 O 0.6588(3) 0.5854(9) -0.1963(3) 0.0466(18) Uani 1 1 d . . . N4 N 0.7930(4) 0.6102(9) -0.2788(3) 0.036(2) Uani 1 1 d . . . H4A H 0.7599 0.6086 -0.2480 0.043 Uiso 1 1 calc R . . H4B H 0.8110 0.5088 -0.2938 0.043 Uiso 1 1 calc R . . C4 C 0.3427(6) 0.7171(10) -0.0302(4) 0.027(2) Uani 1 1 d . . . O5 O 0.6508(3) 0.9096(9) -0.1931(3) 0.0434(18) Uani 1 1 d . . . N5 N 0.7884(4) 0.9122(9) -0.2796(4) 0.044(2) Uani 1 1 d . . . H5A H 0.7553 0.9110 -0.2488 0.052 Uiso 1 1 calc R . . H5B H 0.8035 1.0150 -0.2955 0.052 Uiso 1 1 calc R . . C5 C 0.3551(6) 0.7660(11) 0.0304(6) 0.038(3) Uani 1 1 d . . . H5 H 0.4057 0.7958 0.0436 0.046 Uiso 1 1 calc R . . O6 O 0.5789(5) 0.7457(6) -0.2694(4) 0.037(2) Uani 1 1 d . . . N6 N 0.8649(5) 0.7660(8) -0.3483(5) 0.037(3) Uani 1 1 d . . . H6A H 0.8834 0.6656 -0.3637 0.045 Uiso 1 1 calc R . . H6B H 0.8796 0.8698 -0.3637 0.045 Uiso 1 1 calc R . . C6 C 0.2930(6) 0.7725(11) 0.0737(5) 0.037(3) Uani 1 1 d . . . H6 H 0.3008 0.8131 0.1148 0.045 Uiso 1 1 calc R . . C7 C 0.4086(6) 0.7158(11) -0.0747(5) 0.037(2) Uani 1 1 d . . . C8 C 0.3986(6) 0.7690(11) -0.1342(6) 0.036(3) Uani 1 1 d . . . H8 H 0.3491 0.8039 -0.1485 0.044 Uiso 1 1 calc R . . C9 C 0.4602(6) 0.7719(10) -0.1730(5) 0.040(3) Uani 1 1 d . . . H9 H 0.4520 0.8064 -0.2148 0.048 Uiso 1 1 calc R . . C10 C 0.5293(6) 0.7300(8) -0.1559(4) 0.023(2) Uani 1 1 d . . . C11 C 0.5436(4) 0.6710(10) -0.0961(4) 0.035(2) Uani 1 1 d . . . H11 H 0.5937 0.6347 -0.0836 0.042 Uiso 1 1 calc R . . C12 C 0.4817(4) 0.6671(9) -0.0554(4) 0.0328(19) Uani 1 1 d . . . H12 H 0.4896 0.6307 -0.0138 0.039 Uiso 1 1 calc R . . C13 C -0.0649(7) 0.7469(10) 0.2011(5) 0.033(3) Uani 1 1 d . . . C14 C 0.8151(7) 0.7609(10) -0.3019(6) 0.040(3) Uani 1 1 d . . . C1A C 0.4375(3) 1.2377(10) -0.0148(3) 0.074(7) Uiso 0.50 1 d PG A 1 C2A C 0.4316(4) 1.2421(13) 0.0492(3) 0.039(4) Uiso 0.50 1 d PG A 1 H2A1 H 0.4767 1.2527 0.0738 0.047 Uiso 0.50 1 calc PR A 1 C3A C 0.3597(5) 1.2310(14) 0.0773(3) 0.30(4) Uiso 0.50 1 d PG A 1 H3A1 H 0.3557 1.2341 0.1211 0.357 Uiso 0.50 1 calc PR A 1 C4A C 0.2936(4) 1.2156(12) 0.0413(3) 0.041(4) Uiso 0.50 1 d PG A 1 H4A1 H 0.2445 1.2080 0.0606 0.049 Uiso 0.50 1 calc PR A 1 C5A C 0.2995(3) 1.2112(8) -0.0227(3) 0.037(4) Uiso 0.50 1 d PG A 1 C6A C 0.3714(3) 1.2222(7) -0.0508(3) 0.041(12) Uiso 0.50 1 d PG A 1 C7A C 0.3773(4) 1.2178(11) -0.1149(3) 0.042(4) Uiso 0.50 1 d PG A 1 C8A C 0.3112(5) 1.2024(14) -0.1509(3) 0.093(9) Uiso 0.50 1 d PG A 1 H8A H 0.3152 1.1994 -0.1947 0.112 Uiso 0.50 1 calc PR A 1 C9A C 0.2393(4) 1.1913(13) -0.1228(4) 0.154(11) Uiso 0.50 1 d PG A 1 H9A H 0.1942 1.1808 -0.1474 0.185 Uiso 0.50 1 calc PR A 1 C10A C 0.2334(3) 1.1957(11) -0.0587(4) 0.013(2) Uiso 0.50 1 d PG A 1 H10A H 0.1843 1.1882 -0.0395 0.016 Uiso 0.50 1 calc PR A 1 C11A C 0.5254(3) 1.1929(15) -0.0367(5) 0.042(4) Uiso 0.50 1 d PG A 1 H11A H 0.5591 1.2936 -0.0260 0.063 Uiso 0.50 1 calc PR A 1 H11B H 0.5264 1.1738 -0.0815 0.063 Uiso 0.50 1 calc PR A 1 H11C H 0.5434 1.0843 -0.0156 0.063 Uiso 0.50 1 calc PR A 1 C12A C 0.4448(5) 1.2460(17) -0.1627(4) 0.117(13) Uiso 0.50 1 d PG A 1 H12A H 0.4541 1.1340 -0.1852 0.175 Uiso 0.50 1 calc PR A 1 H12B H 0.4917 1.2812 -0.1406 0.175 Uiso 0.50 1 calc PR A 1 H12C H 0.4305 1.3405 -0.1921 0.175 Uiso 0.50 1 calc PR A 1 C1B C 0.3882(4) 1.2163(9) 0.0104(3) 0.066(6) Uiso 0.50 1 d PG B 2 C2B C 0.4611(4) 1.2091(11) 0.0370(3) 0.084(7) Uiso 0.50 1 d PG B 2 H2B1 H 0.4664 1.2041 0.0807 0.101 Uiso 0.50 1 calc PR B 2 C3B C 0.5263(3) 1.2091(12) -0.0004(4) 0.064(5) Uiso 0.50 1 d PG B 2 H3B1 H 0.5761 1.2042 0.0178 0.077 Uiso 0.50 1 calc PR B 2 C4B C 0.5186(3) 1.2164(11) -0.0643(4) 0.020(3) Uiso 0.50 1 d PG B 2 H4B1 H 0.5632 1.2165 -0.0899 0.024 Uiso 0.50 1 calc PR B 2 C5B C 0.4457(3) 1.2237(8) -0.0909(3) 0.051(5) Uiso 0.50 1 d PG B 2 C6B C 0.3805(3) 1.2236(7) -0.0535(3) 0.030(11) Uiso 0.50 1 d PG B 2 C7B C 0.3077(3) 1.2308(9) -0.0801(3) 0.060(6) Uiso 0.50 1 d PG B 2 C8B C 0.3000(4) 1.2381(11) -0.1440(3) 0.070(8) Uiso 0.50 1 d PG B 2 H8B H 0.2501 1.2430 -0.1622 0.084 Uiso 0.50 1 calc PR B 2 C9B C 0.3652(5) 1.2382(11) -0.1814(3) 0.040(4) Uiso 0.50 1 d PG B 2 H9B H 0.3599 1.2432 -0.2251 0.049 Uiso 0.50 1 calc PR B 2 C10B C 0.4380(4) 1.2310(10) -0.1548(3) 0.034(5) Uiso 0.50 1 d PG B 2 H10B H 0.4826 1.2310 -0.1804 0.041 Uiso 0.50 1 calc PR B 2 C11B C 0.3477(5) 1.2502(13) 0.0760(3) 0.028(3) Uiso 0.50 1 d PG B 2 H11D H 0.3494 1.1398 0.1006 0.041 Uiso 0.50 1 calc PR B 2 H11E H 0.2939 1.2857 0.0695 0.041 Uiso 0.50 1 calc PR B 2 H11F H 0.3750 1.3459 0.0981 0.041 Uiso 0.50 1 calc PR B 2 C12B C 0.2185(3) 1.1663(15) -0.0082(5) 0.079(6) Uiso 0.50 1 d PG B 2 H12D H 0.1937 1.0520 -0.0184 0.119 Uiso 0.50 1 calc PR B 2 H12E H 0.1797 1.2616 -0.0071 0.119 Uiso 0.50 1 calc PR B 2 H12F H 0.2434 1.1570 0.0324 0.119 Uiso 0.50 1 calc PR B 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0383(16) 0.0215(13) 0.042(2) 0.0018(11) -0.0070(13) -0.0001(8) O1 0.045(4) 0.027(3) 0.042(4) -0.002(3) 0.002(3) 0.002(3) N1 0.053(5) 0.033(4) 0.054(5) 0.014(4) 0.011(4) 0.009(4) C1 0.040(6) 0.026(4) 0.052(7) 0.007(4) 0.011(5) -0.004(4) S2 0.0338(15) 0.0416(18) 0.039(2) 0.0013(10) 0.0090(13) -0.0001(9) O2 0.043(4) 0.018(3) 0.051(4) 0.007(3) -0.010(3) 0.004(3) N2 0.057(6) 0.033(5) 0.050(6) -0.014(4) 0.009(4) 0.002(4) C2 0.038(5) 0.032(5) 0.035(5) -0.001(4) -0.007(4) 0.001(4) O3 0.047(5) 0.026(4) 0.045(5) -0.001(2) 0.009(4) 0.002(2) N3 0.032(5) 0.050(7) 0.062(8) -0.001(3) -0.006(5) -0.004(3) C3 0.042(5) 0.037(5) 0.029(5) -0.005(4) -0.005(4) -0.001(4) O4 0.035(4) 0.048(4) 0.057(5) -0.006(3) 0.006(3) 0.012(3) N4 0.040(5) 0.024(4) 0.044(5) 0.009(3) 0.010(4) 0.006(3) C4 0.031(5) 0.025(4) 0.024(5) -0.010(4) -0.007(4) 0.005(4) O5 0.038(4) 0.044(4) 0.048(4) 0.003(3) 0.009(3) -0.015(3) N5 0.034(5) 0.032(4) 0.064(6) -0.018(4) 0.017(4) -0.006(4) C5 0.029(6) 0.046(6) 0.039(7) -0.005(4) -0.008(5) -0.002(4) O6 0.043(5) 0.040(5) 0.029(5) 0.003(2) -0.004(4) 0.004(2) N6 0.051(6) 0.019(5) 0.041(7) -0.003(3) 0.020(5) -0.001(3) C6 0.029(6) 0.048(6) 0.035(6) -0.026(4) -0.012(5) -0.003(4) C7 0.036(6) 0.026(4) 0.048(6) -0.006(5) -0.004(5) 0.003(4) C8 0.034(6) 0.042(6) 0.032(7) 0.008(4) -0.004(5) 0.002(4) C9 0.048(7) 0.041(5) 0.032(7) 0.003(4) 0.001(6) -0.002(4) C10 0.032(5) 0.017(4) 0.021(4) 0.002(3) -0.014(4) -0.002(3) C11 0.027(4) 0.028(5) 0.050(6) -0.004(4) -0.005(4) -0.001(4) C12 0.041(5) 0.024(4) 0.034(5) 0.000(3) -0.002(4) -0.002(4) C13 0.019(5) 0.044(7) 0.034(7) -0.003(4) -0.004(5) -0.003(3) C14 0.036(7) 0.020(6) 0.063(9) -0.019(4) -0.009(6) 0.004(4)