Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Katharina Fromm' _publ_contact_author_address ; Department of Chemistry University of Basel Spitalstr.52 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email KATHARINA.FROMM@UNIBAS.CH _publ_section_title ; On the coordination behaviour of NO3- in coordination compounds with Ag+: Part 1. Solubility effect on the formation of coordination polymer networks between AgNO3 and L (L = ethanediyl bis(isonicotinate) as a function of solvent ; loop_ _publ_author_name 'Katharina Fromm' 'Adeline Y. Robin' 'Jorge L. Sague' # Attachment 'structure publi solvent Adeline Robin.txt' data_[Ag2(L)(NO3)2] _database_code_depnum_ccdc_archive 'CCDC 285368' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ag2(C14H12N2O4)(NO3)2]' _chemical_formula_sum 'C14 H12 Ag2 N4 O10' _chemical_formula_weight 612.02 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' 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 20.976(7) _cell_length_b 9.3460(17) _cell_length_c 9.903(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.98(2) _cell_angle_gamma 90.00 _cell_volume 1856.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.174 _exptl_absorpt_correction_type spherical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(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' _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 1972 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 31.94 _reflns_number_total 1452 _reflns_number_gt 1179 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe _computing_cell_refinement Xred _computing_data_reduction Xred _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^)+(0.1185P)^2^+1.8874P] 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 1452 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1742 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.084 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.22778(5) 0.12919(5) 0.62904(7) 0.0625(10) Uani 1 1 d . . . N1 N 0.1614(5) 0.0014(6) 0.4541(8) 0.054(2) Uani 1 1 d . . . C1 C 0.1215(6) 0.0623(7) 0.3357(10) 0.062(3) Uani 1 1 d . . . H1 H 0.1199 0.1616 0.3291 0.074 Uiso 1 1 calc R . . C2 C 0.0834(6) -0.0167(8) 0.2249(10) 0.061(3) Uani 1 1 d . . . H2 H 0.0549 0.0280 0.1464 0.073 Uiso 1 1 calc R . . C3 C 0.1652(5) -0.1410(6) 0.4614(10) 0.056(3) Uani 1 1 d . . . H3 H 0.1928 -0.1832 0.5425 0.067 Uiso 1 1 calc R . . C4 C 0.1291(5) -0.2287(7) 0.3521(9) 0.055(2) Uani 1 1 d . . . H4 H 0.1326 -0.3277 0.3596 0.066 Uiso 1 1 calc R . . C5 C 0.0881(5) -0.1649(7) 0.2321(9) 0.052(2) Uani 1 1 d . A . C6 C 0.0459(8) -0.2493(9) 0.1113(12) 0.075(4) Uani 1 1 d . . . O1 O 0.0169(6) -0.2006(8) -0.0024(10) 0.087(5) Uani 1 1 d . A . O2A O 0.0641(11) -0.3929(11) 0.1229(19) 0.061(4) Uani 0.60 1 d P A 1 O2B O 0.0326(19) -0.3818(16) 0.153(2) 0.063(7) Uani 0.40 1 d P A 2 C7 C 0.0294(15) -0.498(2) -0.003(3) 0.112(8) Uani 1 1 d . . . H7A H 0.0318 -0.4614 -0.0925 0.135 Uiso 1 1 calc R A 1 H7B H 0.0496 -0.5926 0.0127 0.135 Uiso 1 1 calc R A 1 O3 O 0.2365(5) 0.3663(5) 0.7124(8) 0.062(2) Uani 1 1 d . . . N2 N 0.2023(5) 0.4465(6) 0.6179(8) 0.056(2) Uani 1 1 d . . . O4 O 0.3033(5) 0.0757(5) 0.8555(7) 0.065(3) Uani 1 1 d . . . O5 O 0.1747(6) 0.3967(7) 0.4991(9) 0.074(3) 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 0.0743(11) 0.0501(10) 0.0551(11) -0.00669(18) 0.0064(5) -0.0035(2) N1 0.061(6) 0.047(3) 0.050(3) -0.004(2) 0.009(4) -0.004(2) C1 0.070(7) 0.047(3) 0.060(5) -0.002(3) 0.006(5) 0.000(3) C2 0.060(7) 0.060(4) 0.054(4) 0.001(3) 0.004(5) 0.008(3) C3 0.057(6) 0.049(3) 0.051(4) -0.003(2) -0.002(5) -0.003(2) C4 0.059(6) 0.049(3) 0.052(4) -0.001(2) 0.008(4) -0.007(2) C5 0.050(6) 0.057(3) 0.051(4) -0.004(2) 0.017(4) -0.007(3) C6 0.086(10) 0.062(4) 0.061(6) 0.000(3) -0.005(7) -0.016(4) O1 0.098(11) 0.079(4) 0.062(4) 0.000(3) -0.012(7) -0.005(4) O2A 0.051(11) 0.065(7) 0.072(9) -0.015(4) 0.025(9) -0.010(5) O2B 0.08(2) 0.051(7) 0.043(8) -0.009(5) 0.004(12) -0.023(8) C7 0.08(2) 0.135(11) 0.162(17) 0.046(11) 0.089(15) 0.040(11) O3 0.075(6) 0.049(3) 0.056(3) 0.0042(18) 0.011(4) 0.001(2) N2 0.062(6) 0.050(3) 0.049(3) -0.003(2) 0.007(4) -0.002(2) O4 0.074(6) 0.047(3) 0.067(4) -0.001(2) 0.009(4) 0.000(2) O5 0.074(8) 0.076(4) 0.059(4) -0.011(3) -0.002(5) -0.003(3) _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 2.226(7) . ? Ag1 O3 2.354(5) . ? Ag1 O4 2.390(7) . ? Ag1 O5 2.716(13) 7_556 ? N1 C3 1.334(8) . ? N1 C1 1.351(11) . ? C1 C2 1.369(12) . ? C1 H1 0.9300 . ? C2 C5 1.389(10) . ? C2 H2 0.9300 . ? C3 C4 1.392(10) . ? C3 H3 0.9300 . ? C4 C5 1.383(12) . ? C4 H4 0.9300 . ? C5 C6 1.489(12) . ? C6 O1 1.201(12) . ? C6 O2B 1.360(17) . ? C6 O2A 1.391(15) . ? O2A C7 1.59(4) . ? O2B C7 1.87(4) . ? C7 C7 1.25(6) 5_545 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? O3 N2 1.249(10) . ? N2 O5 1.240(10) . ? N2 O4 1.249(8) 4_556 ? O4 N2 1.249(8) 4_546 ? 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 O3 138.2(3) . . ? N1 Ag1 O4 135.27(19) . . ? O3 Ag1 O4 84.6(2) . . ? N1 Ag1 O5 88.5(3) . 7_556 ? O3 Ag1 O5 104.8(3) . 7_556 ? O4 Ag1 O5 92.1(3) . 7_556 ? C3 N1 C1 118.6(6) . . ? C3 N1 Ag1 118.6(6) . . ? C1 N1 Ag1 122.5(4) . . ? N1 C1 C2 122.5(6) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C5 118.7(8) . . ? C1 C2 H2 120.6 . . ? C5 C2 H2 120.6 . . ? N1 C3 C4 122.4(7) . . ? N1 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C5 C4 C3 118.4(6) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C2 119.4(7) . . ? C4 C5 C6 122.5(7) . . ? C2 C5 C6 118.1(8) . . ? O1 C6 O2B 122.5(12) . . ? O1 C6 O2A 119.7(11) . . ? O2B C6 O2A 34.1(13) . . ? O1 C6 C5 124.8(8) . . ? O2B C6 C5 111.4(10) . . ? O2A C6 C5 111.1(10) . . ? C6 O2A C7 118.8(13) . . ? C6 O2B C7 103.9(18) . . ? C7 C7 O2A 103(3) 5_545 . ? C7 C7 O2B 77(3) 5_545 . ? O2A C7 O2B 25.3(11) . . ? C7 C7 H7A 111.3 5_545 . ? O2A C7 H7A 111.3 . . ? O2B C7 H7A 123.3 . . ? C7 C7 H7B 111.3 5_545 . ? O2A C7 H7B 111.2 . . ? O2B C7 H7B 119.4 . . ? H7A C7 H7B 109.2 . . ? N2 O3 Ag1 109.5(5) . . ? O5 N2 O4 121.1(7) . 4_556 ? O5 N2 O3 119.5(6) . . ? O4 N2 O3 119.4(7) 4_556 . ? N2 O4 Ag1 108.8(5) 4_546 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ag1 N1 C3 -165.2(9) . . . . ? O4 Ag1 N1 C3 -7.5(12) . . . . ? O5 Ag1 N1 C3 84.0(9) 7_556 . . . ? O3 Ag1 N1 C1 20.3(12) . . . . ? O4 Ag1 N1 C1 178.1(9) . . . . ? O5 Ag1 N1 C1 -90.4(10) 7_556 . . . ? C3 N1 C1 C2 2(2) . . . . ? Ag1 N1 C1 C2 176.4(10) . . . . ? N1 C1 C2 C5 -3(2) . . . . ? C1 N1 C3 C4 -0.5(19) . . . . ? Ag1 N1 C3 C4 -175.2(9) . . . . ? N1 C3 C4 C5 -0.1(18) . . . . ? C3 C4 C5 C2 -0.8(18) . . . . ? C3 C4 C5 C6 -178.0(12) . . . . ? C1 C2 C5 C4 2(2) . . . . ? C1 C2 C5 C6 179.5(13) . . . . ? C4 C5 C6 O1 -168.9(16) . . . . ? C2 C5 C6 O1 14(3) . . . . ? C4 C5 C6 O2B 24(3) . . . . ? C2 C5 C6 O2B -153(2) . . . . ? C4 C5 C6 O2A -13(2) . . . . ? C2 C5 C6 O2A 170.0(17) . . . . ? O1 C6 O2A C7 -17(3) . . . . ? O2B C6 O2A C7 88(3) . . . . ? C5 C6 O2A C7 -174.6(19) . . . . ? O1 C6 O2B C7 46(3) . . . . ? O2A C6 O2B C7 -49.9(19) . . . . ? C5 C6 O2B C7 -146.3(16) . . . . ? C6 O2A C7 C7 -67(3) . . . 5_545 ? C6 O2A C7 O2B -72(2) . . . . ? C6 O2B C7 C7 -114(3) . . . 5_545 ? C6 O2B C7 O2A 62(2) . . . . ? N1 Ag1 O3 N2 -17.0(11) . . . . ? O4 Ag1 O3 N2 178.5(9) . . . . ? O5 Ag1 O3 N2 87.8(8) 7_556 . . . ? Ag1 O3 N2 O5 -5.0(15) . . . . ? Ag1 O3 N2 O4 175.3(9) . . . 4_556 ? N1 Ag1 O4 N2 -7.9(11) . . . 4_546 ? O3 Ag1 O4 N2 157.4(9) . . . 4_546 ? O5 Ag1 O4 N2 -97.9(8) 7_556 . . 4_546 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7B O1 0.97 2.37 2.98(3) 120.6 5_545 C2 H2 O1 0.93 2.38 3.271(11) 161.2 5 C3 H3 O3 0.93 2.49 3.286(12) 143.7 4_546 C3 H3 O4 0.93 2.46 3.167(9) 132.9 4_546 C4 H4 O4 0.93 2.89 3.367(10) 113.0 4_546 C1 H1 O5 0.93 2.80 3.547(10) 137.8 . _diffrn_measured_fraction_theta_max 0.452 _diffrn_reflns_theta_full 31.94 _diffrn_measured_fraction_theta_full 0.452 _refine_diff_density_max 0.208 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.034 data_[AgLNO3] _database_code_depnum_ccdc_archive 'CCDC 285369' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ag(C14H12N2O4)NO3]' _chemical_formula_sum 'C14 H12 Ag N3 O7' _chemical_formula_weight 442.14 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' 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 6.1591(13) _cell_length_b 8.895(3) _cell_length_c 14.439(3) _cell_angle_alpha 93.15(2) _cell_angle_beta 99.898(16) _cell_angle_gamma 91.43(2) _cell_volume 777.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.341 _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 'Stoe IPDS' _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 1565 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 27.01 _reflns_number_total 1494 _reflns_number_gt 1291 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe _computing_cell_refinement Xred _computing_data_reduction Xred _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^)+(0.0334P)^2^+0.7275P] 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 1494 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.37808(6) 0.85718(7) 0.88967(3) 0.04882(19) Uani 1 1 d . . . N1 N 0.4261(6) 0.7603(7) 1.0271(3) 0.0433(18) Uani 1 1 d . . . C1 C 0.2640(7) 0.7678(9) 1.0784(4) 0.044(2) Uani 1 1 d . . . H1 H 0.1390 0.8207 1.0565 0.053 Uiso 1 1 calc R . . C2 C 0.2768(7) 0.6994(9) 1.1629(4) 0.0441(19) Uani 1 1 d . . . H2 H 0.1599 0.7038 1.1959 0.053 Uiso 1 1 calc R . . C3 C 0.6036(7) 0.6821(9) 1.0603(4) 0.047(2) Uani 1 1 d . . . H3 H 0.7158 0.6755 1.0247 0.056 Uiso 1 1 calc R . . C4 C 0.6300(7) 0.6112(8) 1.1433(4) 0.0392(19) Uani 1 1 d . . . H4 H 0.7542 0.5560 1.1627 0.047 Uiso 1 1 calc R . . C5 C 0.4635(6) 0.6248(8) 1.1977(3) 0.0354(17) Uani 1 1 d . . . C6 C 0.4813(7) 0.5602(8) 1.2918(3) 0.0338(17) Uani 1 1 d . . . O1 O 0.3504(5) 0.5801(6) 1.3440(2) 0.0483(16) Uani 1 1 d . . . O2 O 0.6664(5) 0.4857(6) 1.3125(2) 0.0388(13) Uani 1 1 d . . . C7 C 0.6991(7) 0.4117(8) 1.3993(3) 0.0370(16) Uani 1 1 d . . . H7A H 0.5849 0.3346 1.3993 0.044 Uiso 1 1 calc R . . H7B H 0.7001 0.4832 1.4526 0.044 Uiso 1 1 calc R . . C8 C 0.9208(7) 0.3434(8) 1.4021(3) 0.0393(18) Uani 1 1 d . . . H8A H 0.9164 0.2691 1.3500 0.047 Uiso 1 1 calc R . . H8B H 1.0321 0.4206 1.3979 0.047 Uiso 1 1 calc R . . O3 O 0.9710(5) 0.2733(6) 1.4909(2) 0.0392(13) Uani 1 1 d . . . C9 C 1.1566(7) 0.1982(8) 1.5032(3) 0.0351(17) Uani 1 1 d . . . O4 O 1.2742(6) 0.1850(7) 1.4446(3) 0.0549(18) Uani 1 1 d . . . C10 C 0.2027(7) 1.1288(8) 0.5949(3) 0.0316(15) Uani 1 1 d . . . C11 C 0.0568(7) 1.1285(8) 0.6592(3) 0.0407(19) Uani 1 1 d . . . H11 H -0.0772 1.1756 0.6461 0.049 Uiso 1 1 calc R . . C12 C 0.1128(7) 1.0589(9) 0.7408(4) 0.0406(18) Uani 1 1 d . . . H12 H 0.0142 1.0606 0.7830 0.049 Uiso 1 1 calc R . . C13 C 0.4018(7) 1.0595(8) 0.6197(3) 0.0408(18) Uani 1 1 d . . . H13 H 0.5054 1.0600 0.5799 0.049 Uiso 1 1 calc R . . C14 C 0.4455(7) 0.9904(8) 0.7031(3) 0.0379(18) Uani 1 1 d . . . H14 H 0.5793 0.9436 0.7181 0.045 Uiso 1 1 calc R . . N2 N 0.3037(6) 0.9872(7) 0.7644(3) 0.0389(16) Uani 1 1 d . . . N3 N 0.8575(6) 0.7523(8) 0.8492(3) 0.0396(17) Uani 1 1 d . . . O5 O 0.6661(6) 0.7028(8) 0.8165(3) 0.063(2) Uani 1 1 d . . . O6 O 1.0157(6) 0.6753(10) 0.8340(4) 0.077(3) Uani 1 1 d . . . O7 O 0.8869(6) 0.8723(10) 0.8943(3) 0.065(2) 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 0.0517(2) 0.0603(5) 0.0372(3) 0.0263(2) 0.00636(17) 0.01301(18) N1 0.0443(19) 0.056(7) 0.030(2) 0.020(2) 0.0034(17) 0.011(2) C1 0.042(2) 0.058(7) 0.035(3) 0.016(3) 0.006(2) 0.019(2) C2 0.039(2) 0.059(7) 0.037(3) 0.015(3) 0.009(2) 0.017(2) C3 0.041(2) 0.063(7) 0.042(3) 0.021(3) 0.015(2) 0.014(2) C4 0.036(2) 0.043(7) 0.041(3) 0.017(3) 0.007(2) 0.009(2) C5 0.0321(19) 0.047(6) 0.027(2) 0.009(2) 0.0029(18) 0.0068(19) C6 0.0343(19) 0.037(6) 0.030(3) 0.012(2) 0.0006(19) 0.0054(19) O1 0.0511(17) 0.062(6) 0.036(2) 0.017(2) 0.0150(17) 0.0178(19) O2 0.0341(14) 0.053(5) 0.0323(18) 0.0206(18) 0.0065(13) 0.0107(15) C7 0.038(2) 0.045(6) 0.029(3) 0.019(2) 0.0022(18) 0.006(2) C8 0.037(2) 0.054(7) 0.028(3) 0.020(2) 0.0020(19) 0.007(2) O3 0.0395(15) 0.052(5) 0.0290(18) 0.0201(18) 0.0056(14) 0.0152(16) C9 0.0335(19) 0.039(6) 0.032(3) 0.012(2) 0.0015(19) 0.007(2) O4 0.0525(18) 0.078(6) 0.044(2) 0.027(2) 0.0233(18) 0.025(2) C10 0.0336(18) 0.032(6) 0.030(2) 0.009(2) 0.0036(18) 0.0042(18) C11 0.0324(19) 0.057(7) 0.036(3) 0.017(3) 0.008(2) 0.014(2) C12 0.038(2) 0.051(6) 0.036(3) 0.016(3) 0.010(2) 0.012(2) C13 0.034(2) 0.056(6) 0.036(3) 0.013(2) 0.010(2) 0.012(2) C14 0.036(2) 0.041(7) 0.037(3) 0.015(2) 0.004(2) 0.012(2) N2 0.0393(18) 0.047(6) 0.032(2) 0.016(2) 0.0043(17) 0.0084(18) N3 0.039(2) 0.044(6) 0.038(3) 0.012(3) 0.0075(19) 0.005(2) O5 0.0410(19) 0.063(7) 0.082(3) -0.004(3) 0.0027(19) 0.0035(19) O6 0.047(2) 0.070(8) 0.112(4) -0.011(4) 0.014(2) 0.021(3) O7 0.059(2) 0.066(9) 0.067(3) -0.006(3) 0.009(2) 0.001(3) _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 2.183(4) . ? Ag1 N2 2.189(4) . ? Ag1 O5 2.599(5) . ? Ag1 O6 2.703(7) 1_455 ? Ag1 O7 3.122(4) . ? Ag1 Ag1 4.0170(17) 2_677 ? Ag1 Ag1 6.1591(13) 1_655 ? Ag1 Ag1 17.659(4) 1_464 ? N1 C1 1.342(5) . ? N1 C3 1.343(7) . ? C1 C2 1.384(7) . ? C1 H1 0.9300 . ? C2 C5 1.375(6) . ? C2 H2 0.9300 . ? C3 C4 1.372(7) . ? C3 H3 0.9300 . ? C4 C5 1.398(5) . ? C4 H4 0.9300 . ? C5 C6 1.493(6) . ? C6 O1 1.204(5) . ? C6 O2 1.331(5) . ? O2 C7 1.434(5) . ? C7 C8 1.503(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3 1.445(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O3 C9 1.329(6) . ? C9 O4 1.208(5) . ? C9 C10 1.479(7) 1_646 ? C10 C13 1.386(6) . ? C10 C11 1.398(5) . ? C10 C9 1.479(7) 1_464 ? C11 C12 1.358(7) . ? C11 H11 0.9300 . ? C12 N2 1.352(6) . ? C12 H12 0.9300 . ? C13 C14 1.370(7) . ? C13 H13 0.9300 . ? C14 N2 1.347(5) . ? C14 H14 0.9300 . ? N3 O7 1.213(10) . ? N3 O6 1.248(7) . ? N3 O5 1.251(7) . ? O6 Ag1 2.703(7) 1_655 ? O7 Ag1 3.044(4) 1_655 ? 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 169.8(2) . . ? N1 Ag1 O5 98.02(18) . . ? N2 Ag1 O5 91.59(17) . . ? N1 Ag1 O6 89.6(2) . 1_455 ? N2 Ag1 O6 92.1(2) . 1_455 ? O5 Ag1 O6 99.91(17) . 1_455 ? N1 Ag1 O7 90.63(15) . . ? N2 Ag1 O7 94.21(15) . . ? O5 Ag1 O7 42.67(19) . . ? O6 Ag1 O7 142.13(17) 1_455 . ? N1 Ag1 Ag1 64.40(18) . 2_677 ? N2 Ag1 Ag1 108.30(17) . 2_677 ? O5 Ag1 Ag1 115.91(12) . 2_677 ? O6 Ag1 Ag1 137.42(10) 1_455 2_677 ? O7 Ag1 Ag1 74.79(12) . 2_677 ? N1 Ag1 Ag1 90.63(10) . 1_655 ? N2 Ag1 Ag1 94.62(9) . 1_655 ? O5 Ag1 Ag1 40.04(13) . 1_655 ? O6 Ag1 Ag1 139.45(12) 1_455 1_655 ? O7 Ag1 Ag1 2.68(14) . 1_655 ? Ag1 Ag1 Ag1 77.19(2) 2_677 1_655 ? N1 Ag1 Ag1 164.53(11) . 1_464 ? N2 Ag1 Ag1 8.19(9) . 1_464 ? O5 Ag1 Ag1 97.24(12) . 1_464 ? O6 Ag1 Ag1 85.29(14) 1_455 1_464 ? O7 Ag1 Ag1 102.38(12) . 1_464 ? Ag1 Ag1 Ag1 110.67(3) 2_677 1_464 ? Ag1 Ag1 Ag1 102.755(17) 1_655 1_464 ? C1 N1 C3 117.5(4) . . ? C1 N1 Ag1 119.1(3) . . ? C3 N1 Ag1 123.1(3) . . ? N1 C1 C2 122.1(4) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C5 C2 C1 119.6(4) . . ? C5 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? N1 C3 C4 124.1(3) . . ? N1 C3 H3 117.9 . . ? C4 C3 H3 117.9 . . ? C3 C4 C5 117.7(4) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? C2 C5 C4 118.8(4) . . ? C2 C5 C6 119.0(3) . . ? C4 C5 C6 122.2(4) . . ? O1 C6 O2 124.7(4) . . ? O1 C6 C5 124.1(4) . . ? O2 C6 C5 111.1(3) . . ? C6 O2 C7 116.9(3) . . ? O2 C7 C8 103.4(3) . . ? O2 C7 H7A 111.1 . . ? C8 C7 H7A 111.1 . . ? O2 C7 H7B 111.1 . . ? C8 C7 H7B 111.1 . . ? H7A C7 H7B 109.0 . . ? O3 C8 C7 106.6(3) . . ? O3 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? O3 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C9 O3 C8 115.0(3) . . ? O4 C9 O3 123.5(5) . . ? O4 C9 C10 123.1(4) . 1_646 ? O3 C9 C10 113.4(3) . 1_646 ? C13 C10 C11 117.3(4) . . ? C13 C10 C9 118.8(3) . 1_464 ? C11 C10 C9 123.9(4) . 1_464 ? C12 C11 C10 119.3(4) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? N2 C12 C11 123.7(3) . . ? N2 C12 H12 118.1 . . ? C11 C12 H12 118.1 . . ? C14 C13 C10 119.8(3) . . ? C14 C13 H13 120.1 . . ? C10 C13 H13 120.1 . . ? N2 C14 C13 123.0(4) . . ? N2 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C14 N2 C12 116.6(4) . . ? C14 N2 Ag1 119.9(3) . . ? C12 N2 Ag1 123.3(3) . . ? O7 N3 O6 121.2(5) . . ? O7 N3 O5 120.4(5) . . ? O6 N3 O5 118.4(7) . . ? N3 O5 Ag1 110.5(5) . . ? N3 O6 Ag1 105.3(5) . 1_655 ? N3 O7 Ag1 89.3(3) . 1_655 ? N3 O7 Ag1 85.3(3) . . ? Ag1 O7 Ag1 174.6(3) 1_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 41.6(14) . . . . ? O5 Ag1 N1 C1 -157.7(6) . . . . ? O6 Ag1 N1 C1 -57.8(6) 1_455 . . . ? O7 Ag1 N1 C1 160.1(6) . . . . ? Ag1 Ag1 N1 C1 87.3(6) 2_677 . . . ? Ag1 Ag1 N1 C1 162.8(6) 1_655 . . . ? Ag1 Ag1 N1 C1 12.6(11) 1_464 . . . ? N2 Ag1 N1 C3 -143.9(9) . . . . ? O5 Ag1 N1 C3 16.7(6) . . . . ? O6 Ag1 N1 C3 116.6(6) 1_455 . . . ? O7 Ag1 N1 C3 -25.5(6) . . . . ? Ag1 Ag1 N1 C3 -98.3(6) 2_677 . . . ? Ag1 Ag1 N1 C3 -22.8(6) 1_655 . . . ? Ag1 Ag1 N1 C3 -173.0(5) 1_464 . . . ? C3 N1 C1 C2 0.5(11) . . . . ? Ag1 N1 C1 C2 175.3(6) . . . . ? N1 C1 C2 C5 2.1(12) . . . . ? C1 N1 C3 C4 -0.7(11) . . . . ? Ag1 N1 C3 C4 -175.2(6) . . . . ? N1 C3 C4 C5 -1.7(11) . . . . ? C1 C2 C5 C4 -4.4(11) . . . . ? C1 C2 C5 C6 176.0(7) . . . . ? C3 C4 C5 C2 4.2(11) . . . . ? C3 C4 C5 C6 -176.3(6) . . . . ? C2 C5 C6 O1 -6.8(11) . . . . ? C4 C5 C6 O1 173.6(7) . . . . ? C2 C5 C6 O2 176.8(6) . . . . ? C4 C5 C6 O2 -2.7(10) . . . . ? O1 C6 O2 C7 6.5(10) . . . . ? C5 C6 O2 C7 -177.1(6) . . . . ? C6 O2 C7 C8 -178.6(5) . . . . ? O2 C7 C8 O3 176.9(5) . . . . ? C7 C8 O3 C9 175.9(5) . . . . ? C8 O3 C9 O4 -1.8(9) . . . . ? C8 O3 C9 C10 179.7(6) . . . 1_646 ? C13 C10 C11 C12 -1.4(11) . . . . ? C9 C10 C11 C12 178.6(7) 1_464 . . . ? C10 C11 C12 N2 -0.5(11) . . . . ? C11 C10 C13 C14 2.0(10) . . . . ? C9 C10 C13 C14 -178.0(7) 1_464 . . . ? C10 C13 C14 N2 -0.7(11) . . . . ? C13 C14 N2 C12 -1.2(11) . . . . ? C13 C14 N2 Ag1 174.8(5) . . . . ? C11 C12 N2 C14 1.8(11) . . . . ? C11 C12 N2 Ag1 -174.0(6) . . . . ? N1 Ag1 N2 C14 142.8(9) . . . . ? O5 Ag1 N2 C14 -18.0(6) . . . . ? O6 Ag1 N2 C14 -118.0(6) 1_455 . . . ? O7 Ag1 N2 C14 24.7(6) . . . . ? Ag1 Ag1 N2 C14 100.0(6) 2_677 . . . ? Ag1 Ag1 N2 C14 22.0(6) 1_655 . . . ? Ag1 Ag1 N2 C14 -151.8(16) 1_464 . . . ? N1 Ag1 N2 C12 -41.5(13) . . . . ? O5 Ag1 N2 C12 157.7(5) . . . . ? O6 Ag1 N2 C12 57.7(5) 1_455 . . . ? O7 Ag1 N2 C12 -159.7(5) . . . . ? Ag1 Ag1 N2 C12 -84.3(5) 2_677 . . . ? Ag1 Ag1 N2 C12 -162.3(5) 1_655 . . . ? Ag1 Ag1 N2 C12 23.9(8) 1_464 . . . ? O7 N3 O5 Ag1 -12.4(8) . . . . ? O6 N3 O5 Ag1 167.7(4) . . . . ? N1 Ag1 O5 N3 -76.1(5) . . . . ? N2 Ag1 O5 N3 100.6(4) . . . . ? O6 Ag1 O5 N3 -167.0(4) 1_455 . . . ? O7 Ag1 O5 N3 6.1(4) . . . . ? Ag1 Ag1 O5 N3 -10.7(5) 2_677 . . . ? Ag1 Ag1 O5 N3 5.3(3) 1_655 . . . ? Ag1 Ag1 O5 N3 106.5(4) 1_464 . . . ? O7 N3 O6 Ag1 -10.6(7) . . . 1_655 ? O5 N3 O6 Ag1 169.3(4) . . . 1_655 ? O6 N3 O7 Ag1 9.0(6) . . . 1_655 ? O5 N3 O7 Ag1 -170.8(5) . . . 1_655 ? O6 N3 O7 Ag1 -170.5(5) . . . . ? O5 N3 O7 Ag1 9.6(6) . . . . ? N1 Ag1 O7 N3 95.3(4) . . . . ? N2 Ag1 O7 N3 -93.7(5) . . . . ? O5 Ag1 O7 N3 -5.9(4) . . . . ? O6 Ag1 O7 N3 5.2(6) 1_455 . . . ? Ag1 Ag1 O7 N3 158.5(4) 2_677 . . . ? Ag1 Ag1 O7 N3 5(2) 1_655 . . . ? Ag1 Ag1 O7 N3 -93.1(4) 1_464 . . . ? N1 Ag1 O7 Ag1 90(2) . . . 1_655 ? N2 Ag1 O7 Ag1 -99(2) . . . 1_655 ? O5 Ag1 O7 Ag1 -11(2) . . . 1_655 ? O6 Ag1 O7 Ag1 0(2) 1_455 . . 1_655 ? Ag1 Ag1 O7 Ag1 153(2) 2_677 . . 1_655 ? Ag1 Ag1 O7 Ag1 -98(2) 1_464 . . 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11 O1 0.93 2.79 3.648(7) 153.2 2_577 C8 H8B O1 0.97 2.64 3.580(7) 163.4 1_655 C13 H13 O4 0.93 2.63 3.195(7) 119.3 2_767 C14 H14 O4 0.93 2.85 3.316(6) 112.3 2_767 C7 H7A O4 0.97 2.50 3.436(7) 161.9 1_455 C1 H1 O7 0.93 2.65 3.403(7) 138.9 1_455 C12 H12 O7 0.93 2.58 3.309(8) 135.3 1_455 C1 H1 O7 0.93 2.80 3.377(11) 121.3 2_677 C4 H4 O6 0.93 2.53 3.390(8) 154.7 2_767 C8 H8A O6 0.97 2.83 3.494(7) 126.5 2_767 C14 H14 O5 0.93 2.65 3.308(9) 128.3 . _diffrn_measured_fraction_theta_max 0.439 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.439 _refine_diff_density_max 0.189 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.040 #_________________________________________________ # eof # end of crystallographic data file