# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 # 1. SUBMISSION DETAILS _publ_contact_autor ; Katharina M. Fromm University of Basel Department of Chemistry Spitalstrasse 51 CH-4056 Basel Switzerland ; _publ_contact_author_phone '041 61 26-71004' _publ_contact_author_fax '041 61 26-71021' _publ_contact_author_email Katharina.Fromm@unibas.ch _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Concomitant crystallization of two polymorphs – a ring and a helix: Concentration effect on supramolecular polymorphism ; loop_ _publ_author_name _publ_author_address 'Fromm, Katharina M.' ; University of Basel Department of chemistry Spitalstrasse 51 CH-4056 Basel Switzerland ; 'Robin, Adeline Y.' ; University of Basel Department of chemistry Spitalstrasse 51 CH-4056 Basel Switzerland ; 'Sague, Jorge' ; University of Basel Department of chemistry Spitalstrasse 51 CH-4056 Basel Switzerland #============================================================================== data_jorge1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Ag Cl N2 O9' _chemical_formula_weight 523.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1824(14) _cell_length_b 12.077(2) _cell_length_c 12.095(2) _cell_angle_alpha 112.58(3) _cell_angle_beta 102.32(3) _cell_angle_gamma 96.64(3) _cell_volume 923.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 3221 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 1.292 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 'STOE IPDS II' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3221 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 31.78 _reflns_number_total 3221 _reflns_number_gt 2553 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _computing_publication_material WORD _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0810P)^2^+1.9441P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3221 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1879 _refine_ls_wR_factor_gt 0.1708 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.006 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 Ag1 Ag 0.82132(7) 0.55097(5) 0.95419(7) 0.0554(3) Uani 1 1 d . . . N1 N 0.6336(7) 0.3715(5) 0.8459(5) 0.0392(14) Uani 1 1 d . . . C1 C 0.5415(8) 0.3069(6) 0.8943(5) 0.0379(15) Uani 1 1 d . . . H1 H 0.5589 0.3417 0.9810 0.045 Uiso 1 1 calc R . . C2 C 0.4214(7) 0.1910(6) 0.8230(5) 0.0312(12) Uani 1 1 d . . . H2 H 0.3587 0.1479 0.8599 0.037 Uiso 1 1 calc R . . C3 C 0.3966(7) 0.1401(5) 0.6933(5) 0.0288(11) Uani 1 1 d . . . C4 C 0.4934(9) 0.2059(7) 0.6436(6) 0.0376(14) Uani 1 1 d . . . H4 H 0.4799 0.1732 0.5574 0.045 Uiso 1 1 calc R . . C5 C 0.6120(9) 0.3218(7) 0.7228(7) 0.0435(17) Uani 1 1 d . . . H5 H 0.6786 0.3664 0.6887 0.052 Uiso 1 1 calc R . . C6 C 0.2653(8) 0.0166(6) 0.6069(6) 0.0356(14) Uani 1 1 d . . . O1 O 0.2272(9) -0.0189(6) 0.4944(5) 0.0528(16) Uani 1 1 d . . . O2 O 0.2017(7) -0.0430(5) 0.6673(4) 0.0388(11) Uani 1 1 d . . . C7 C 0.0845(9) -0.1670(6) 0.5922(7) 0.0428(17) Uani 1 1 d . . . H7A H 0.0540 -0.1839 0.5035 0.051 Uiso 1 1 calc R . . H7B H -0.0386 -0.1753 0.6139 0.051 Uiso 1 1 calc R . . C8 C 0.1981(10) -0.2570(7) 0.6165(6) 0.0379(14) Uani 1 1 d . . . H8A H 0.2440 -0.2342 0.7063 0.045 Uiso 1 1 calc R . . H8B H 0.1157 -0.3402 0.5758 0.045 Uiso 1 1 calc R . . O3 O 0.3593(7) -0.2519(5) 0.5664(4) 0.0374(11) Uani 1 1 d . . . C9 C 0.4753(10) -0.3378(6) 0.5719(6) 0.0416(17) Uani 1 1 d . . . H9A H 0.5604 -0.3426 0.5175 0.050 Uiso 1 1 calc R . . H9B H 0.3896 -0.4192 0.5400 0.050 Uiso 1 1 calc R . . C10 C 0.6007(11) -0.3055(6) 0.7029(7) 0.0433(17) Uani 1 1 d . . . H10A H 0.5182 -0.3127 0.7557 0.052 Uiso 1 1 calc R . . H10B H 0.6902 -0.3612 0.7007 0.052 Uiso 1 1 calc R . . O4 O 0.7103(7) -0.1795(5) 0.7519(4) 0.0392(11) Uani 1 1 d . . . O5 O 0.6104(12) -0.1307(8) 0.9264(7) 0.063(2) Uani 1 1 d . . . C11 C 0.6931(8) -0.1007(6) 0.8617(6) 0.0335(13) Uani 1 1 d . . . C12 C 0.9562(9) 0.1847(6) 0.8540(6) 0.0357(13) Uani 1 1 d . . . H12 H 0.9935 0.2109 0.7966 0.043 Uiso 1 1 calc R . . C13 C 0.8564(8) 0.0647(6) 0.8108(5) 0.0315(12) Uani 1 1 d . . . H13 H 0.8288 0.0098 0.7265 0.038 Uiso 1 1 calc R . . C14 C 0.7977(7) 0.0273(5) 0.8957(5) 0.0302(12) Uani 1 1 d . . . C15 C 0.8368(9) 0.1118(6) 1.0194(5) 0.0359(14) Uani 1 1 d . . . H15 H 0.7937 0.0892 1.0774 0.043 Uiso 1 1 calc R . . C16 C 0.9404(9) 0.2300(6) 1.0552(6) 0.0399(16) Uani 1 1 d . . . H16 H 0.9679 0.2869 1.1388 0.048 Uiso 1 1 calc R . . N2 N 1.0031(7) 0.2661(5) 0.9746(6) 0.0408(15) Uani 1 1 d . . . Cl1 Cl 1.1443(2) 0.46703(15) 0.72477(15) 0.0387(4) Uani 1 1 d . . . O6 O 0.9692(8) 0.5071(6) 0.6897(6) 0.0519(16) Uani 1 1 d . . . O7 O 1.2945(10) 0.5732(7) 0.8095(6) 0.071(2) Uani 1 1 d . . . O8 O 1.2042(11) 0.4082(11) 0.6174(7) 0.088(4) Uani 1 1 d . . . O9 O 1.109(2) 0.3909(16) 0.7798(18) 0.148(8) 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 Ag1 0.0389(2) 0.0263(3) 0.0809(5) 0.0136(3) -0.0009(3) -0.00241(18) N1 0.0328(18) 0.030(3) 0.048(3) 0.015(2) 0.004(2) 0.0012(19) C1 0.036(2) 0.037(3) 0.032(2) 0.009(3) 0.003(2) 0.005(2) C2 0.0306(19) 0.031(3) 0.035(2) 0.016(2) 0.012(2) 0.003(2) C3 0.0299(18) 0.027(2) 0.030(2) 0.011(2) 0.0099(18) 0.0062(19) C4 0.039(2) 0.037(3) 0.037(3) 0.018(3) 0.012(2) 0.002(2) C5 0.038(2) 0.037(3) 0.051(4) 0.018(3) 0.008(3) 0.000(3) C6 0.033(2) 0.030(3) 0.039(3) 0.011(3) 0.007(2) 0.007(2) O1 0.063(3) 0.044(3) 0.035(2) 0.007(3) 0.009(2) -0.006(3) O2 0.0420(18) 0.027(2) 0.043(2) 0.010(2) 0.0162(19) -0.0010(18) C7 0.037(2) 0.026(3) 0.058(4) 0.011(3) 0.015(3) -0.001(2) C8 0.045(3) 0.028(3) 0.041(3) 0.014(3) 0.018(3) 0.004(2) O3 0.0426(19) 0.033(2) 0.043(2) 0.019(2) 0.0209(19) 0.007(2) C9 0.045(3) 0.030(3) 0.043(3) 0.008(3) 0.010(3) 0.009(3) C10 0.048(3) 0.030(3) 0.046(3) 0.017(3) 0.005(3) -0.001(3) O4 0.045(2) 0.028(2) 0.040(2) 0.013(2) 0.011(2) -0.0052(19) O5 0.085(4) 0.043(4) 0.070(4) 0.021(4) 0.049(4) 0.000(4) C11 0.036(2) 0.026(3) 0.038(3) 0.011(3) 0.014(2) 0.006(2) C12 0.037(2) 0.027(3) 0.049(3) 0.020(3) 0.018(2) 0.004(2) C13 0.034(2) 0.026(3) 0.036(3) 0.014(2) 0.013(2) 0.003(2) C14 0.0293(18) 0.024(2) 0.036(3) 0.012(2) 0.0082(19) 0.0060(19) C15 0.043(3) 0.033(3) 0.030(2) 0.010(3) 0.011(2) 0.012(3) C16 0.044(3) 0.030(3) 0.040(3) 0.012(3) 0.006(3) 0.008(3) N2 0.036(2) 0.023(2) 0.049(3) 0.004(3) 0.004(2) 0.006(2) Cl1 0.0382(6) 0.0300(7) 0.0443(7) 0.0136(7) 0.0113(6) 0.0015(5) O6 0.046(2) 0.044(3) 0.066(3) 0.024(3) 0.016(3) 0.010(2) O7 0.064(3) 0.064(4) 0.056(3) 0.015(4) -0.001(3) -0.018(3) O8 0.062(3) 0.099(8) 0.076(4) 0.003(5) 0.027(4) 0.017(5) O9 0.096(7) 0.144(13) 0.275(18) 0.182(14) 0.032(11) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.150(6) . ? Ag1 N2 2.155(6) 2_767 ? Ag1 Ag1 3.1459(12) 2_767 ? N1 C1 1.337(10) . ? N1 C5 1.339(10) . ? C1 C2 1.387(9) . ? C2 C3 1.408(8) . ? C3 C4 1.377(10) . ? C3 C6 1.504(9) . ? C4 C5 1.396(10) . ? C6 O1 1.214(9) . ? C6 O2 1.316(10) . ? O2 C7 1.454(8) . ? C7 C8 1.511(9) . ? C8 O3 1.423(9) . ? O3 C9 1.416(7) . ? C9 C10 1.519(8) . ? C10 O4 1.455(9) . ? O4 C11 1.346(9) . ? O5 C11 1.210(12) . ? C11 C14 1.495(9) . ? C12 N2 1.349(9) . ? C12 C13 1.380(9) . ? C13 C14 1.390(10) . ? C14 C15 1.393(8) . ? C15 C16 1.385(10) . ? C16 N2 1.346(11) . ? N2 Ag1 2.155(6) 2_767 ? Cl1 O9 1.357(15) . ? Cl1 O8 1.406(9) . ? Cl1 O7 1.435(7) . ? Cl1 O6 1.438(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 167.8(2) . 2_767 ? N1 Ag1 Ag1 93.85(12) . 2_767 ? N2 Ag1 Ag1 92.59(12) 2_767 2_767 ? C1 N1 C5 118.8(6) . . ? C1 N1 Ag1 124.0(4) . . ? C5 N1 Ag1 117.2(5) . . ? N1 C1 C2 123.2(6) . . ? C1 C2 C3 117.8(6) . . ? C4 C3 C2 119.1(5) . . ? C4 C3 C6 118.7(5) . . ? C2 C3 C6 122.2(6) . . ? C3 C4 C5 119.1(6) . . ? N1 C5 C4 122.1(8) . . ? O1 C6 O2 126.5(6) . . ? O1 C6 C3 121.0(7) . . ? O2 C6 C3 112.5(5) . . ? C6 O2 C7 116.7(5) . . ? O2 C7 C8 108.9(5) . . ? O3 C8 C7 106.5(6) . . ? C9 O3 C8 114.7(6) . . ? O3 C9 C10 113.2(6) . . ? O4 C10 C9 107.2(6) . . ? C11 O4 C10 116.5(7) . . ? O5 C11 O4 124.2(7) . . ? O5 C11 C14 124.7(7) . . ? O4 C11 C14 111.1(6) . . ? N2 C12 C13 123.3(7) . . ? C12 C13 C14 118.1(6) . . ? C13 C14 C15 119.4(6) . . ? C13 C14 C11 123.4(5) . . ? C15 C14 C11 117.2(6) . . ? C16 C15 C14 118.7(7) . . ? N2 C16 C15 122.4(6) . . ? C16 N2 C12 118.1(6) . . ? C16 N2 Ag1 118.3(4) . 2_767 ? C12 N2 Ag1 123.6(6) . 2_767 ? O9 Cl1 O8 111.7(10) . . ? O9 Cl1 O7 110.5(8) . . ? O8 Cl1 O7 108.2(6) . . ? O9 Cl1 O6 109.4(7) . . ? O8 Cl1 O6 108.6(4) . . ? O7 Cl1 O6 108.5(4) . . ? _diffrn_measured_fraction_theta_max 0.512 _diffrn_reflns_theta_full 31.78 _diffrn_measured_fraction_theta_full 0.512 _refine_diff_density_max 0.919 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.114 data_jorge2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Ag Cl N2 O9' _chemical_formula_weight 523.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.631(5) _cell_length_b 7.1049(14) _cell_length_c 25.554(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.12(3) _cell_angle_gamma 90.00 _cell_volume 3818.7(13) _cell_formula_units_Z 8 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 7494 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7494 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.20 _reflns_number_total 4216 _reflns_number_gt 2037 _reflns_threshold_expression >2sigma(I) _computing_data_collection STOE _computing_cell_refinement STOE _computing_data_reduction STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _computing_publication_material WORD _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1076P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4216 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1549 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2243 _refine_ls_wR_factor_gt 0.1832 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 3.829 _refine_ls_shift/su_mean 0.053 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 Ag1 Ag 0.77916(4) 0.68351(14) 0.77044(3) 0.0706(3) Uani 1 1 d . . . N1 N 0.8379(3) 0.7032(11) 0.8644(3) 0.0511(17) Uani 1 1 d . . . C1 C 0.8206(4) 0.6394(13) 0.9040(4) 0.055(2) Uani 1 1 d . . . H1 H 0.7792 0.5958 0.8906 0.066 Uiso 1 1 calc R . . C2 C 0.8596(4) 0.6340(13) 0.9628(3) 0.049(2) Uani 1 1 d . . . H2 H 0.8449 0.5891 0.9886 0.058 Uiso 1 1 calc R . . C3 C 0.9220(4) 0.6966(14) 0.9840(3) 0.0501(19) Uani 1 1 d . . . C4 C 0.9417(4) 0.7611(16) 0.9439(4) 0.064(3) Uani 1 1 d . . . H4 H 0.9833 0.8004 0.9560 0.077 Uiso 1 1 calc R . . C5 C 0.8967(4) 0.7653(17) 0.8841(4) 0.066(3) Uani 1 1 d . . . H5 H 0.9091 0.8143 0.8572 0.080 Uiso 1 1 calc R . . C6 C 0.9697(4) 0.6851(15) 1.0467(4) 0.059(2) Uani 1 1 d . . . O1 O 0.9439(3) 0.6336(10) 1.0806(2) 0.0612(17) Uani 1 1 d . . . O2 O 1.0249(3) 0.7267(15) 1.0655(3) 0.093(3) Uani 1 1 d . . . C7 C 0.9861(5) 0.5943(18) 1.1433(4) 0.072(3) Uani 1 1 d . . . H7A H 0.9823 0.6919 1.1681 0.087 Uiso 1 1 calc R . . H7B H 1.0300 0.5860 1.1507 0.087 Uiso 1 1 calc R . . C8 C 0.9622(9) 0.400(2) 1.1550(5) 0.138(8) Uani 1 1 d . . . H8A H 0.9849 0.3692 1.1965 0.165 Uiso 1 1 calc R . . H8B H 0.9172 0.4078 1.1443 0.165 Uiso 1 1 calc R . . O3 O 0.9715(4) 0.2700(15) 1.1245(4) 0.096(3) Uani 1 1 d . . . C9 C 0.9475(5) 0.1008(17) 1.1344(4) 0.075(3) Uani 1 1 d . . . H9A H 0.9579 0.0978 1.1757 0.090 Uiso 1 1 calc R . . H9B H 0.9712 -0.0004 1.1280 0.090 Uiso 1 1 calc R . . C10 C 0.8788(4) 0.0532(18) 1.1006(4) 0.068(3) Uani 1 1 d . . . H10A H 0.8715 -0.0753 1.1089 0.082 Uiso 1 1 calc R . . H10B H 0.8536 0.1365 1.1118 0.082 Uiso 1 1 calc R . . O4 O 0.8610(3) 0.0743(11) 1.0393(2) 0.0629(17) Uani 1 1 d . . . O5 O 0.7609(3) 0.0078(14) 1.0175(3) 0.083(2) Uani 1 1 d . . . C11 C 0.8007(4) 0.0512(15) 1.0021(4) 0.057(2) Uani 1 1 d . . . C12 C 0.7101(4) 0.0740(18) 0.8390(4) 0.071(3) Uani 1 1 d . . . H12 H 0.6692 0.0469 0.8101 0.085 Uiso 1 1 calc R . . C13 C 0.7240(4) 0.0449(16) 0.8964(4) 0.064(3) Uani 1 1 d . . . H13 H 0.6932 -0.0002 0.9062 0.076 Uiso 1 1 calc R . . C14 C 0.7857(4) 0.0842(14) 0.9402(4) 0.053(2) Uani 1 1 d . . . C15 C 0.8295(4) 0.1500(13) 0.9234(4) 0.051(2) Uani 1 1 d . . . H15 H 0.8709 0.1760 0.9513 0.061 Uiso 1 1 calc R . . C16 C 0.8113(4) 0.1772(14) 0.8644(4) 0.054(2) Uani 1 1 d . . . H16 H 0.8411 0.2235 0.8533 0.065 Uiso 1 1 calc R . . N2 N 0.7522(3) 0.1392(12) 0.8223(3) 0.0564(19) Uani 1 1 d . . . Cl1 Cl 0.87250(11) 0.1285(5) 0.73973(9) 0.0788(9) Uani 1 1 d . . . O6 O 0.9100(6) 0.2174(18) 0.7186(6) 0.132(4) Uani 1 1 d . . . O7 O 0.8553(6) 0.280(2) 0.7697(5) 0.136(5) Uani 1 1 d . . . O8 O 0.8168(4) 0.0613(19) 0.6955(5) 0.137(4) Uani 1 1 d . . . O9 O 0.9064(7) 0.000(4) 0.7792(9) 0.269(13) 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 Ag1 0.0672(5) 0.0862(6) 0.0461(4) -0.0012(4) 0.0151(3) 0.0014(5) N1 0.045(3) 0.058(5) 0.044(3) -0.004(3) 0.015(3) 0.002(3) C1 0.043(4) 0.056(6) 0.055(4) -0.008(4) 0.012(3) -0.007(4) C2 0.043(4) 0.059(6) 0.046(4) -0.008(4) 0.022(3) -0.009(4) C3 0.049(4) 0.058(5) 0.043(4) -0.002(4) 0.021(3) -0.001(4) C4 0.044(4) 0.087(8) 0.063(5) 0.007(5) 0.025(4) -0.010(5) C5 0.051(5) 0.091(8) 0.057(5) 0.010(5) 0.025(4) -0.001(5) C6 0.053(5) 0.063(6) 0.053(4) -0.004(5) 0.018(4) -0.002(5) O1 0.054(3) 0.078(5) 0.044(3) 0.010(3) 0.016(2) -0.011(3) O2 0.045(3) 0.159(9) 0.058(4) 0.003(4) 0.009(3) -0.020(4) C7 0.069(6) 0.087(8) 0.036(4) -0.001(5) 0.003(4) -0.010(6) C8 0.241(18) 0.140(13) 0.081(7) 0.078(8) 0.116(10) 0.146(14) O3 0.093(5) 0.107(7) 0.092(5) 0.019(5) 0.045(5) 0.008(5) C9 0.081(7) 0.063(7) 0.058(5) 0.010(5) 0.011(5) -0.025(6) C10 0.062(5) 0.089(8) 0.053(5) 0.010(5) 0.026(4) 0.009(6) O4 0.052(3) 0.084(5) 0.052(3) 0.000(3) 0.024(3) -0.005(3) O5 0.062(4) 0.125(8) 0.072(4) 0.003(5) 0.040(4) -0.006(5) C11 0.061(5) 0.060(6) 0.058(5) 0.003(4) 0.034(4) -0.001(5) C12 0.052(5) 0.092(8) 0.058(5) -0.002(5) 0.015(4) 0.002(5) C13 0.045(4) 0.079(7) 0.064(5) 0.002(5) 0.022(4) 0.000(5) C14 0.049(4) 0.059(6) 0.056(4) -0.004(4) 0.028(4) 0.002(4) C15 0.046(4) 0.053(6) 0.054(4) 0.001(4) 0.025(3) -0.003(4) C16 0.052(4) 0.058(6) 0.055(4) -0.001(4) 0.027(4) 0.003(4) N2 0.052(4) 0.066(5) 0.046(3) 0.006(3) 0.018(3) 0.007(4) Cl1 0.0497(11) 0.131(3) 0.0477(11) 0.0112(13) 0.0154(9) -0.0106(14) O6 0.159(9) 0.147(10) 0.156(9) -0.030(8) 0.127(9) -0.042(8) O7 0.133(8) 0.199(13) 0.109(7) -0.028(8) 0.084(7) -0.030(9) O8 0.071(5) 0.142(10) 0.138(8) -0.044(8) -0.003(5) 0.005(6) O9 0.127(10) 0.34(3) 0.244(17) 0.22(2) 0.005(11) 0.024(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.158(7) 4_656 ? Ag1 N1 2.161(6) . ? N1 C5 1.320(12) . ? N1 C1 1.334(12) . ? C1 C2 1.359(11) . ? C2 C3 1.391(11) . ? C3 C4 1.383(12) . ? C3 C6 1.481(11) . ? C4 C5 1.408(13) . ? C6 O2 1.205(11) . ? C6 O1 1.319(11) . ? O1 C7 1.478(10) . ? C7 C8 1.57(2) . ? C8 O3 1.290(16) . ? O3 C9 1.400(15) . ? C9 C10 1.489(14) . ? C10 O4 1.432(10) . ? O4 C11 1.312(10) . ? O5 C11 1.215(11) . ? C11 C14 1.471(12) . ? C12 N2 1.332(13) . ? C12 C13 1.365(13) . ? C13 C14 1.403(12) . ? C14 C15 1.373(12) . ? C15 C16 1.379(11) . ? C16 N2 1.346(11) . ? N2 Ag1 2.158(7) 4_646 ? Cl1 O9 1.323(14) . ? Cl1 O8 1.371(9) . ? Cl1 O6 1.383(9) . ? Cl1 O7 1.482(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 162.5(3) 4_656 . ? C5 N1 C1 117.2(7) . . ? C5 N1 Ag1 118.5(6) . . ? C1 N1 Ag1 124.0(5) . . ? N1 C1 C2 124.1(8) . . ? C1 C2 C3 119.2(8) . . ? C4 C3 C2 118.1(7) . . ? C4 C3 C6 118.2(8) . . ? C2 C3 C6 123.5(7) . . ? C3 C4 C5 118.0(8) . . ? N1 C5 C4 123.4(8) . . ? O2 C6 O1 123.3(8) . . ? O2 C6 C3 124.7(8) . . ? O1 C6 C3 111.9(7) . . ? C6 O1 C7 118.6(7) . . ? O1 C7 C8 104.4(9) . . ? O3 C8 C7 109.8(10) . . ? C8 O3 C9 108.1(11) . . ? O3 C9 C10 121.0(10) . . ? O4 C10 C9 108.1(8) . . ? C11 O4 C10 117.5(7) . . ? O5 C11 O4 122.7(8) . . ? O5 C11 C14 123.0(8) . . ? O4 C11 C14 114.2(7) . . ? N2 C12 C13 123.2(9) . . ? C12 C13 C14 118.8(9) . . ? C15 C14 C13 118.3(8) . . ? C15 C14 C11 123.0(8) . . ? C13 C14 C11 118.8(8) . . ? C14 C15 C16 119.1(8) . . ? N2 C16 C15 122.6(8) . . ? C12 N2 C16 117.9(7) . . ? C12 N2 Ag1 118.0(6) . 4_646 ? C16 N2 Ag1 124.1(6) . 4_646 ? O9 Cl1 O8 114.1(12) . . ? O9 Cl1 O6 109.8(10) . . ? O8 Cl1 O6 112.5(8) . . ? O9 Cl1 O7 108.7(14) . . ? O8 Cl1 O7 107.1(7) . . ? O6 Cl1 O7 104.2(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.145 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.139 # eof # end of crystallographic data file