#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000073.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_4000073 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_name_common bis(guanidinium)(4,4'-biphenyldisulfonate).(1,8-dimethyl _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 0.9200 _exptl_absorpt_correction_T_max 0.9692 _exptl_absorpt_process_details 'SADABS, G. Sheldrick (1999)' _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 14266 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0958 _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 2387 _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^)+(0.0080P)^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 0.12(16) _refine_ls_number_reflns 4831 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.010 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 0.13947(13) 0.73370(19) 0.10405(6) 0.0364(6) Uani 1 1 d . . . O1 O 0.0914(2) 0.5799(5) 0.0954(2) 0.0378(12) Uani 1 1 d . . . N1 N -0.0419(3) 0.5869(7) 0.1759(3) 0.0421(17) Uani 1 1 d . . . H1A H -0.0104 0.5872 0.1440 0.051 Uiso 1 1 calc R . . H1B H -0.0577 0.4846 0.1917 0.051 Uiso 1 1 calc R . . C1 C 0.2151(4) 0.7256(7) 0.0542(3) 0.0254(17) Uani 1 1 d . . . S2 S 0.60979(12) 0.74276(18) -0.20738(6) 0.0346(5) Uani 1 1 d . . . O2 O 0.0946(2) 0.8926(5) 0.0900(2) 0.0359(12) Uani 1 1 d . . . N2 N -0.0403(3) 0.8952(7) 0.1749(3) 0.0443(17) Uani 1 1 d . . . H2A H -0.0088 0.8911 0.1430 0.053 Uiso 1 1 calc R . . H2B H -0.0549 0.9993 0.1900 0.053 Uiso 1 1 calc R . . C2 C 0.2078(3) 0.6691(6) -0.0085(3) 0.0321(15) Uani 1 1 d . . . H2 H 0.1587 0.6306 -0.0226 0.039 Uiso 1 1 calc R . . O3 O 0.1698(3) 0.7429(4) 0.1678(2) 0.0274(12) Uani 1 1 d . . . N3 N -0.1122(3) 0.7455(5) 0.2530(2) 0.0343(15) Uani 1 1 d . . . H3A H -0.1252 0.8484 0.2699 0.041 Uiso 1 1 calc R . . H3B H -0.1285 0.6442 0.2692 0.041 Uiso 1 1 calc R . . C3 C 0.2691(3) 0.6674(7) -0.0499(3) 0.0311(15) Uani 1 1 d . . . H3 H 0.2610 0.6325 -0.0917 0.037 Uiso 1 1 calc R . . O4 O 0.6568(2) 0.5810(5) -0.1957(2) 0.0426(14) Uani 1 1 d . . . N4 N 0.7926(3) 0.6064(7) -0.2800(3) 0.0371(16) Uani 1 1 d . . . H4A H 0.8155 0.5075 -0.2925 0.045 Uiso 1 1 calc R . . H4B H 0.7557 0.6010 -0.2521 0.045 Uiso 1 1 calc R . . C4 C 0.3432(4) 0.7175(7) -0.0299(3) 0.0259(16) Uani 1 1 d . . . O5 O 0.6494(2) 0.9141(6) -0.1922(2) 0.0343(11) Uani 1 1 d . . . N5 N 0.7874(3) 0.9134(7) -0.2801(3) 0.0374(15) Uani 1 1 d . . . H5A H 0.8072 1.0153 -0.2932 0.045 Uiso 1 1 calc R . . H5B H 0.7505 0.9139 -0.2522 0.045 Uiso 1 1 calc R . . C5 C 0.3517(5) 0.7659(7) 0.0300(3) 0.0305(18) Uani 1 1 d . . . H5 H 0.4019 0.7947 0.0446 0.037 Uiso 1 1 calc R . . O6 O 0.5748(3) 0.7451(4) -0.2691(2) 0.0460(16) Uani 1 1 d . . . N6 N 0.8671(3) 0.7668(5) -0.3433(2) 0.0331(15) Uani 1 1 d . . . H6A H 0.8900 0.6678 -0.3557 0.040 Uiso 1 1 calc R . . H6B H 0.8812 0.8709 -0.3587 0.040 Uiso 1 1 calc R . . C6 C 0.2905(5) 0.7754(7) 0.0712(3) 0.036(2) Uani 1 1 d . . . H6 H 0.2997 0.8167 0.1121 0.044 Uiso 1 1 calc R . . C7 C 0.4091(5) 0.7146(8) -0.0762(4) 0.0374(18) Uani 1 1 d . . . C8 C 0.3957(4) 0.7731(8) -0.1360(3) 0.0364(19) Uani 1 1 d . . . H8 H 0.3459 0.8116 -0.1484 0.044 Uiso 1 1 calc R . . C9 C 0.4570(4) 0.7742(7) -0.1776(3) 0.038(2) Uani 1 1 d . . . H9 H 0.4501 0.8054 -0.2198 0.045 Uiso 1 1 calc R . . C10 C 0.5275(4) 0.7280(8) -0.1545(4) 0.036(2) Uani 1 1 d . . . C11 C 0.5428(3) 0.6712(6) -0.0975(3) 0.0283(14) Uani 1 1 d . . . H11 H 0.5932 0.6356 -0.0856 0.034 Uiso 1 1 calc R . . C12 C 0.4819(3) 0.6665(7) -0.0564(3) 0.0374(17) Uani 1 1 d . . . H12 H 0.4900 0.6305 -0.0148 0.045 Uiso 1 1 calc R . . C13 C -0.0658(5) 0.7429(7) 0.2005(4) 0.049(3) Uani 1 1 d . . . C14 C 0.8132(4) 0.7592(7) -0.3025(3) 0.0235(19) 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 0.0378(13) 0.0302(12) 0.0413(13) 0.0025(10) 0.0018(12) 0.0010(8) O1 0.037(3) 0.035(3) 0.041(3) -0.003(2) 0.003(2) -0.009(2) N1 0.040(4) 0.033(4) 0.053(4) -0.010(3) 0.010(3) 0.000(3) C1 0.030(4) 0.021(3) 0.025(4) 0.006(3) -0.003(3) -0.004(3) S2 0.0328(12) 0.0309(13) 0.0400(13) 0.0036(9) 0.0021(11) 0.0000(8) O2 0.036(3) 0.023(2) 0.049(3) 0.013(2) -0.002(2) 0.011(2) N2 0.040(4) 0.046(4) 0.047(4) 0.004(3) 0.007(3) 0.010(3) C2 0.022(4) 0.034(4) 0.040(4) 0.002(3) -0.015(3) -0.002(3) O3 0.028(2) 0.035(3) 0.020(3) 0.0024(18) -0.007(2) 0.0010(18) N3 0.029(3) 0.035(3) 0.039(3) -0.001(2) 0.012(2) -0.004(2) C3 0.039(4) 0.028(4) 0.026(4) 0.002(3) -0.002(3) 0.002(3) O4 0.041(3) 0.029(2) 0.058(4) -0.010(2) 0.002(3) -0.001(2) N4 0.054(4) 0.009(3) 0.047(4) -0.004(3) 0.012(3) -0.002(3) C4 0.034(4) 0.023(3) 0.021(4) 0.006(3) -0.010(3) 0.001(3) O5 0.031(2) 0.034(2) 0.038(3) 0.001(2) 0.011(2) 0.001(2) N5 0.048(4) 0.017(3) 0.048(4) 0.002(3) 0.013(3) 0.004(3) C5 0.030(4) 0.025(4) 0.037(4) -0.004(3) -0.010(4) -0.006(3) O6 0.055(3) 0.035(3) 0.048(4) -0.001(2) 0.012(3) 0.0005(19) N6 0.046(3) 0.026(3) 0.027(3) -0.005(2) -0.003(2) -0.001(2) C6 0.055(5) 0.041(4) 0.013(4) -0.010(3) -0.001(4) -0.001(4) C7 0.030(4) 0.033(4) 0.050(5) 0.004(4) 0.003(4) 0.000(4) C8 0.029(4) 0.048(4) 0.032(4) -0.001(3) -0.003(4) 0.002(3) C9 0.030(4) 0.041(4) 0.042(4) 0.001(3) -0.009(4) -0.001(3) C10 0.027(4) 0.043(4) 0.038(5) 0.001(3) 0.004(3) -0.010(3) C11 0.035(4) 0.022(3) 0.028(4) 0.004(3) 0.000(3) -0.001(3) C12 0.050(4) 0.031(4) 0.031(4) 0.007(3) -0.004(3) 0.003(3) C13 0.032(5) 0.041(6) 0.073(7) 0.013(4) -0.022(5) -0.011(3) C14 0.021(4) 0.031(5) 0.018(4) -0.005(3) 0.006(3) 0.001(3)