# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'C Carrano' _publ_contact_author_email CARRANO@SCIENCES.SDSU.EDU _publ_section_title ; Self Assembly of Silver (I) Coordination Polymers formed through Hydrogen bonding with a New Ditopic Heteroscorpionate Ligand ; loop_ _publ_author_name 'C Carrano' 'Guillermo A Santillan' # Attachment 'Justin92.cif' data_justin92 _database_code_depnum_ccdc_archive 'CCDC 720110' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N4 O3' _chemical_formula_weight 344.41 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' _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 7.8522(2) _cell_length_b 9.8917(2) _cell_length_c 12.2509(3) _cell_angle_alpha 80.3380(10) _cell_angle_beta 77.7700(10) _cell_angle_gamma 88.9180(10) _cell_volume 916.62(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 8681 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 31.75 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21884 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 31.77 _reflns_number_total 6243 _reflns_number_gt 4303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1277P)^2^+0.1413P] 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 6243 _refine_ls_number_parameters 235 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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 N1 N 0.23548(16) 0.23991(12) 0.12054(10) 0.0358(3) Uani 1 1 d . . . N2 N 0.19890(17) 0.15088(14) 0.05455(11) 0.0402(3) Uani 1 1 d . . . N3 N 0.47226(15) 0.22404(12) 0.21781(10) 0.0337(3) Uani 1 1 d . . . N4 N 0.51271(17) 0.28175(13) 0.30308(11) 0.0381(3) Uani 1 1 d . . . O1 O 0.05738(17) -0.35559(12) 0.40372(12) 0.0531(3) Uani 1 1 d . . . H1A H 0.1372 -0.4094 0.4086 0.080 Uiso 1 1 calc R . . O2 O -0.16014(15) -0.15864(13) 0.42388(12) 0.0521(3) Uani 1 1 d . . . C1 C 0.2663(4) 0.49115(19) 0.1242(2) 0.0692(6) Uani 1 1 d . . . H1B H 0.2912 0.4574 0.1972 0.104 Uiso 1 1 calc R . . H1C H 0.1653 0.5478 0.1330 0.104 Uiso 1 1 calc R . . H1D H 0.3641 0.5442 0.0775 0.104 Uiso 1 1 calc R . . C2 C 0.2323(2) 0.37349(16) 0.06997(15) 0.0454(4) Uani 1 1 d . . . C3 C 0.1908(3) 0.3697(2) -0.03258(16) 0.0542(4) Uani 1 1 d . . . H3A H 0.1781 0.4444 -0.0873 0.065 Uiso 1 1 calc R . . C4 C 0.1713(2) 0.23068(19) -0.03866(14) 0.0471(4) Uani 1 1 d . . . C5 C 0.1250(3) 0.1697(3) -0.13261(18) 0.0669(6) Uani 1 1 d . . . H5A H 0.1191 0.0716 -0.1124 0.100 Uiso 1 1 calc R . . H5B H 0.2123 0.1954 -0.2006 0.100 Uiso 1 1 calc R . . H5C H 0.0139 0.2030 -0.1451 0.100 Uiso 1 1 calc R . . C6 C 0.7755(3) 0.3655(3) 0.3502(2) 0.0657(5) Uani 1 1 d . . . H6A H 0.6920 0.3856 0.4146 0.099 Uiso 1 1 calc R . . H6B H 0.8330 0.4488 0.3082 0.099 Uiso 1 1 calc R . . H6C H 0.8601 0.3034 0.3754 0.099 Uiso 1 1 calc R . . C7 C 0.6842(2) 0.30084(16) 0.27585(14) 0.0415(3) Uani 1 1 d . . . C8 C 0.7543(2) 0.25557(16) 0.17364(14) 0.0411(3) Uani 1 1 d . . . H8A H 0.8712 0.2577 0.1374 0.049 Uiso 1 1 calc R . . C9 C 0.61654(19) 0.20732(14) 0.13745(12) 0.0359(3) Uani 1 1 d . . . C10 C 0.6149(2) 0.15102(19) 0.03218(15) 0.0479(4) Uani 1 1 d . . . H10A H 0.4975 0.1265 0.0313 0.072 Uiso 1 1 calc R . . H10B H 0.6862 0.0712 0.0303 0.072 Uiso 1 1 calc R . . H10C H 0.6598 0.2191 -0.0328 0.072 Uiso 1 1 calc R . . C11 C 0.28788(17) 0.19141(14) 0.22746(12) 0.0324(3) Uani 1 1 d . . . H11A H 0.2220 0.2448 0.2823 0.039 Uiso 1 1 calc R . . C12 C 0.23653(18) 0.04269(14) 0.27337(11) 0.0326(3) Uani 1 1 d . . . C13 C 0.3530(2) -0.06356(16) 0.26734(14) 0.0407(3) Uani 1 1 d . . . H13A H 0.4698 -0.0453 0.2338 0.049 Uiso 1 1 calc R . . C14 C 0.2959(2) -0.19818(16) 0.31139(15) 0.0441(4) Uani 1 1 d . . . H14A H 0.3753 -0.2690 0.3069 0.053 Uiso 1 1 calc R . . C15 C 0.1242(2) -0.22749(15) 0.36126(13) 0.0386(3) Uani 1 1 d . . . C16 C 0.00591(18) -0.11872(15) 0.37050(12) 0.0365(3) Uani 1 1 d . . . C17 C 0.06290(18) 0.01387(14) 0.32595(12) 0.0358(3) Uani 1 1 d . . . H17A H -0.0158 0.0852 0.3311 0.043 Uiso 1 1 calc R . . C18 C -0.2867(2) -0.0542(2) 0.43594(17) 0.0537(4) Uani 1 1 d . . . H18A H -0.3979 -0.0950 0.4741 0.081 Uiso 1 1 calc R . . H18B H -0.2947 -0.0059 0.3624 0.081 Uiso 1 1 calc R . . H18C H -0.2527 0.0089 0.4794 0.081 Uiso 1 1 calc R . . O3 O -0.2644(2) -0.43622(15) 0.56521(15) 0.0749(5) Uani 1 1 d D . . H101 H -0.181(3) -0.401(4) 0.516(2) 0.110(11) Uiso 1 1 d D . . H100 H -0.338(3) -0.385(2) 0.5952(19) 0.067(7) Uiso 1 1 d 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 N1 0.0372(6) 0.0306(5) 0.0402(6) -0.0034(4) -0.0117(5) -0.0013(4) N2 0.0415(7) 0.0397(6) 0.0425(7) -0.0102(5) -0.0133(5) 0.0015(5) N3 0.0319(6) 0.0324(5) 0.0388(6) -0.0117(4) -0.0072(4) -0.0015(4) N4 0.0400(6) 0.0389(6) 0.0391(6) -0.0132(5) -0.0116(5) 0.0011(5) O1 0.0488(7) 0.0318(5) 0.0711(8) 0.0024(5) -0.0041(6) -0.0015(5) O2 0.0355(6) 0.0422(6) 0.0687(8) 0.0047(5) 0.0001(5) -0.0011(5) C1 0.1002(17) 0.0332(8) 0.0783(14) -0.0039(8) -0.0312(12) -0.0074(9) C2 0.0485(9) 0.0325(7) 0.0531(9) 0.0010(6) -0.0121(7) -0.0024(6) C3 0.0603(11) 0.0511(10) 0.0486(9) 0.0071(7) -0.0173(8) -0.0008(8) C4 0.0433(8) 0.0574(10) 0.0415(8) -0.0066(7) -0.0123(6) 0.0036(7) C5 0.0700(13) 0.0876(16) 0.0503(10) -0.0190(10) -0.0234(9) 0.0088(11) C6 0.0590(12) 0.0766(14) 0.0749(13) -0.0299(11) -0.0297(10) -0.0069(10) C7 0.0404(8) 0.0389(7) 0.0489(8) -0.0087(6) -0.0163(6) -0.0024(6) C8 0.0322(7) 0.0410(7) 0.0499(8) -0.0083(6) -0.0078(6) -0.0022(5) C9 0.0354(7) 0.0313(6) 0.0403(7) -0.0081(5) -0.0049(5) -0.0006(5) C10 0.0495(9) 0.0498(9) 0.0451(8) -0.0188(7) -0.0026(7) -0.0026(7) C11 0.0305(6) 0.0311(6) 0.0360(6) -0.0071(5) -0.0066(5) -0.0013(5) C12 0.0331(6) 0.0307(6) 0.0343(6) -0.0038(5) -0.0094(5) -0.0002(5) C13 0.0336(7) 0.0366(7) 0.0487(8) -0.0031(6) -0.0048(6) 0.0024(5) C14 0.0391(8) 0.0339(7) 0.0558(9) -0.0032(6) -0.0060(7) 0.0067(6) C15 0.0423(8) 0.0316(6) 0.0407(7) -0.0009(5) -0.0099(6) -0.0011(5) C16 0.0312(6) 0.0378(7) 0.0386(7) -0.0017(5) -0.0067(5) -0.0013(5) C17 0.0335(7) 0.0330(6) 0.0402(7) -0.0029(5) -0.0086(5) 0.0022(5) C18 0.0348(8) 0.0578(10) 0.0613(11) -0.0009(8) -0.0018(7) 0.0045(7) O3 0.0812(11) 0.0412(7) 0.0795(10) 0.0009(7) 0.0240(9) 0.0155(7) _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 N1 C2 1.3641(19) . ? N1 N2 1.3633(18) . ? N1 C11 1.4578(18) . ? N2 C4 1.330(2) . ? N3 C9 1.3620(18) . ? N3 N4 1.3659(17) . ? N3 C11 1.4652(18) . ? N4 C7 1.326(2) . ? O1 C15 1.3564(18) . ? O2 C16 1.3620(18) . ? O2 C18 1.424(2) . ? C1 C2 1.488(3) . ? C2 C3 1.370(3) . ? C3 C4 1.403(3) . ? C4 C5 1.496(3) . ? C6 C7 1.497(2) . ? C7 C8 1.399(2) . ? C8 C9 1.374(2) . ? C9 C10 1.491(2) . ? C11 C12 1.5137(19) . ? C12 C13 1.381(2) . ? C12 C17 1.391(2) . ? C13 C14 1.394(2) . ? C14 C15 1.371(2) . ? C15 C16 1.411(2) . ? C16 C17 1.377(2) . ? 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 C2 N1 N2 112.39(13) . . ? C2 N1 C11 125.88(13) . . ? N2 N1 C11 121.47(11) . . ? C4 N2 N1 104.62(13) . . ? C9 N3 N4 111.79(12) . . ? C9 N3 C11 131.61(12) . . ? N4 N3 C11 116.59(11) . . ? C7 N4 N3 105.34(12) . . ? C16 O2 C18 117.35(13) . . ? N1 C2 C3 105.62(15) . . ? N1 C2 C1 123.27(16) . . ? C3 C2 C1 131.10(17) . . ? C2 C3 C4 106.34(15) . . ? N2 C4 C3 111.03(15) . . ? N2 C4 C5 120.75(17) . . ? C3 C4 C5 128.22(17) . . ? N4 C7 C8 110.66(13) . . ? N4 C7 C6 120.37(16) . . ? C8 C7 C6 128.96(16) . . ? C9 C8 C7 106.50(14) . . ? N3 C9 C8 105.71(13) . . ? N3 C9 C10 124.70(13) . . ? C8 C9 C10 129.57(14) . . ? N1 C11 N3 110.48(11) . . ? N1 C11 C12 112.30(11) . . ? N3 C11 C12 114.66(11) . . ? C13 C12 C17 119.16(13) . . ? C13 C12 C11 123.47(13) . . ? C17 C12 C11 117.36(12) . . ? C12 C13 C14 120.20(14) . . ? C15 C14 C13 120.88(14) . . ? O1 C15 C14 124.59(14) . . ? O1 C15 C16 116.38(13) . . ? C14 C15 C16 119.03(13) . . ? O2 C16 C17 125.94(13) . . ? O2 C16 C15 114.31(13) . . ? C17 C16 C15 119.74(13) . . ? C16 C17 C12 120.94(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.77 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.422 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.063 # Attachment 'gs023a.cif' data_gs023a _database_code_depnum_ccdc_archive 'CCDC 720111' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H58 Ag2 F12 N8 O6 Sb2' _chemical_formula_weight 1482.22 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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 15.0535(4) _cell_length_b 17.1969(4) _cell_length_c 20.9904(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.663(2) _cell_angle_gamma 90.00 _cell_volume 5428.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 24.68 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2920 _exptl_absorpt_coefficient_mu 1.789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5348 _exptl_absorpt_correction_T_max 0.6159 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48734 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 24.93 _reflns_number_total 4737 _reflns_number_gt 3966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0610P)^2^+34.0683P] 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 4737 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 1.02443(2) 0.17694(2) 0.180951(16) 0.04194(14) Uani 1 1 d . . . N1 N 0.8773(3) 0.1125(2) 0.26448(18) 0.0420(9) Uani 1 1 d . . . N2 N 0.8194(3) 0.1386(2) 0.21757(18) 0.0415(9) Uani 1 1 d . . . N3 N 0.9172(2) 0.2284(2) 0.12659(17) 0.0359(8) Uani 1 1 d . . . N4 N 0.8331(2) 0.2444(2) 0.14444(17) 0.0379(8) Uani 1 1 d . . . O1 O 0.8928(2) 0.4257(2) 0.40834(16) 0.0498(8) Uani 1 1 d . . . O2 O 0.7709(3) 0.3157(3) 0.42526(18) 0.0654(12) Uani 1 1 d . . . C1 C 0.7152(5) 0.0900(4) 0.1306(3) 0.082(2) Uani 1 1 d . . . H1B H 0.6948 0.0399 0.1145 0.123 Uiso 1 1 calc R . . H1C H 0.7438 0.1181 0.0972 0.123 Uiso 1 1 calc R . . H1D H 0.6648 0.1197 0.1445 0.123 Uiso 1 1 calc R . . C2 C 0.7801(4) 0.0779(3) 0.1858(3) 0.0565(14) Uani 1 1 d . . . C3 C 0.8126(4) 0.0120(3) 0.2134(3) 0.0611(15) Uani 1 1 d . . . H3A H 0.7973 -0.0393 0.2020 0.073 Uiso 1 1 calc R . . C4 C 0.8733(4) 0.0350(3) 0.2620(2) 0.0500(12) Uani 1 1 d . . . C5 C 0.9260(5) -0.0142(4) 0.3084(3) 0.0670(16) Uani 1 1 d . . . H5A H 0.9623 0.0188 0.3366 0.101 Uiso 1 1 calc R . . H5B H 0.9641 -0.0489 0.2855 0.101 Uiso 1 1 calc R . . H5C H 0.8860 -0.0447 0.3334 0.101 Uiso 1 1 calc R . . C6 C 1.0052(3) 0.2511(3) 0.0320(2) 0.0496(12) Uani 1 1 d . . . H6A H 1.0497 0.2230 0.0577 0.074 Uiso 1 1 calc R . . H6B H 1.0277 0.3023 0.0221 0.074 Uiso 1 1 calc R . . H6C H 0.9918 0.2229 -0.0073 0.074 Uiso 1 1 calc R . . C7 C 0.9223(3) 0.2592(3) 0.0683(2) 0.0377(10) Uani 1 1 d . . . C8 C 0.8424(4) 0.2949(3) 0.0503(2) 0.0487(12) Uani 1 1 d . . . H8A H 0.8291 0.3209 0.0116 0.058 Uiso 1 1 calc R . . C9 C 0.7867(3) 0.2853(3) 0.0988(2) 0.0453(11) Uani 1 1 d . . . C10 C 0.6928(4) 0.3105(4) 0.1055(3) 0.0680(17) Uani 1 1 d . . . H10A H 0.6728 0.2939 0.1466 0.102 Uiso 1 1 calc R . . H10B H 0.6553 0.2873 0.0718 0.102 Uiso 1 1 calc R . . H10C H 0.6892 0.3667 0.1025 0.102 Uiso 1 1 calc R . . C11 C 0.7998(3) 0.2201(3) 0.2060(2) 0.0386(10) Uani 1 1 d . . . H11A H 0.7342 0.2240 0.2014 0.046 Uiso 1 1 calc R . . C12 C 0.8279(3) 0.2742(3) 0.2599(2) 0.0360(10) Uani 1 1 d . . . C13 C 0.8859(3) 0.3348(3) 0.2521(2) 0.0418(11) Uani 1 1 d . . . H13A H 0.9118 0.3419 0.2126 0.050 Uiso 1 1 calc R . . C14 C 0.9064(3) 0.3851(3) 0.3018(2) 0.0432(11) Uani 1 1 d . . . H14A H 0.9463 0.4262 0.2956 0.052 Uiso 1 1 calc R . . C15 C 0.8698(3) 0.3765(3) 0.3600(2) 0.0392(10) Uani 1 1 d . . . C16 C 0.8073(3) 0.3173(3) 0.3675(2) 0.0414(11) Uani 1 1 d . . . C17 C 0.7875(3) 0.2661(3) 0.3183(2) 0.0423(11) Uani 1 1 d . . . H17A H 0.7467 0.2256 0.3240 0.051 Uiso 1 1 calc R . . C18 C 0.6857(5) 0.2867(6) 0.4294(3) 0.103(3) Uani 1 1 d . . . H18A H 0.6683 0.2895 0.4733 0.154 Uiso 1 1 calc R . . H18B H 0.6842 0.2329 0.4154 0.154 Uiso 1 1 calc R . . H18C H 0.6448 0.3172 0.4025 0.154 Uiso 1 1 calc R . . Sb1 Sb 1.0000 -0.27843(6) 0.2500 0.0886(3) Uani 1 2 d S . . F1 F 1.0860(4) -0.1997(4) 0.2538(3) 0.149(2) Uani 1 1 d . . . F2 F 0.9958(4) -0.2797(5) 0.3372(3) 0.140(2) Uani 1 1 d . . . F3 F 1.0919(6) -0.3460(5) 0.2552(4) 0.200(4) Uani 1 1 d . . . Sb2 Sb 1.0000 0.0000 0.5000 0.0780(2) Uani 1 2 d S . . F4 F 0.9700(10) 0.0620(6) 0.5614(4) 0.281(8) Uani 1 1 d . . . F5 F 1.0968(6) 0.0560(6) 0.5005(7) 0.295(8) Uani 1 1 d . . . F6 F 0.9421(4) 0.0693(3) 0.4437(2) 0.1152(18) Uani 1 1 d . . . O3 O 0.8595(3) 0.4212(4) 0.5312(2) 0.0907(16) Uani 1 1 d . . . C19 C 0.7808(6) 0.4494(9) 0.5562(5) 0.140(5) Uani 1 1 d . . . H19A H 0.7353 0.4086 0.5557 0.168 Uiso 1 1 calc R . . H19B H 0.7577 0.4936 0.5309 0.168 Uiso 1 1 calc R . . C20 C 0.8033(7) 0.4734(8) 0.6208(5) 0.140(4) Uani 1 1 d . . . H20A H 0.7903 0.4318 0.6509 0.168 Uiso 1 1 calc R . . H20B H 0.7695 0.5198 0.6318 0.168 Uiso 1 1 calc R . . C21 C 0.8989(7) 0.4903(6) 0.6228(4) 0.110(3) Uani 1 1 d . . . H21A H 0.9098 0.5458 0.6164 0.132 Uiso 1 1 calc R . . H21B H 0.9274 0.4742 0.6637 0.132 Uiso 1 1 calc R . . C22 C 0.9314(6) 0.4443(6) 0.5703(4) 0.106(3) Uani 1 1 d . . . H22A H 0.9724 0.4755 0.5458 0.128 Uiso 1 1 calc R . . H22B H 0.9636 0.3985 0.5870 0.128 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 Ag1 0.0368(2) 0.0523(2) 0.0366(2) 0.00327(16) -0.00015(14) 0.00438(16) N1 0.042(2) 0.050(2) 0.035(2) 0.0008(17) 0.0048(16) -0.0101(18) N2 0.043(2) 0.045(2) 0.036(2) -0.0050(17) 0.0007(17) -0.0123(18) N3 0.0317(19) 0.044(2) 0.0316(19) -0.0032(16) -0.0001(15) -0.0015(16) N4 0.034(2) 0.048(2) 0.0315(19) -0.0034(17) 0.0001(15) 0.0004(17) O1 0.059(2) 0.0434(19) 0.047(2) -0.0144(16) -0.0033(16) -0.0021(16) O2 0.054(2) 0.104(3) 0.039(2) -0.017(2) 0.0137(17) -0.024(2) C1 0.098(5) 0.068(4) 0.076(4) -0.021(3) -0.036(4) -0.022(4) C2 0.062(3) 0.058(3) 0.049(3) -0.012(3) -0.001(3) -0.019(3) C3 0.078(4) 0.047(3) 0.058(3) -0.009(3) 0.006(3) -0.020(3) C4 0.062(3) 0.047(3) 0.043(3) 0.003(2) 0.013(2) -0.010(2) C5 0.086(4) 0.055(3) 0.061(4) 0.013(3) 0.008(3) -0.002(3) C6 0.046(3) 0.065(3) 0.038(3) -0.001(2) 0.007(2) -0.003(2) C7 0.040(2) 0.043(3) 0.031(2) -0.0049(19) 0.0007(18) -0.005(2) C8 0.053(3) 0.058(3) 0.035(3) 0.006(2) -0.005(2) 0.002(2) C9 0.041(3) 0.056(3) 0.038(3) -0.006(2) -0.006(2) 0.004(2) C10 0.056(4) 0.092(5) 0.055(3) -0.003(3) -0.005(3) 0.025(3) C11 0.029(2) 0.052(3) 0.035(2) -0.004(2) 0.0015(18) -0.007(2) C12 0.027(2) 0.046(3) 0.035(2) -0.0037(19) 0.0021(17) 0.0019(19) C13 0.041(3) 0.048(3) 0.036(2) -0.004(2) 0.007(2) -0.004(2) C14 0.042(3) 0.042(3) 0.046(3) -0.004(2) 0.005(2) -0.009(2) C15 0.040(2) 0.038(2) 0.039(2) -0.007(2) -0.0034(19) 0.006(2) C16 0.036(2) 0.056(3) 0.033(2) -0.003(2) 0.0042(19) 0.001(2) C17 0.036(2) 0.053(3) 0.038(2) -0.004(2) 0.0049(19) -0.011(2) C18 0.071(5) 0.183(9) 0.056(4) -0.017(5) 0.027(3) -0.039(5) Sb1 0.0451(3) 0.1380(7) 0.0836(5) 0.000 0.0112(3) 0.000 F1 0.106(4) 0.181(6) 0.157(6) 0.028(5) -0.024(4) -0.044(4) F2 0.116(4) 0.219(7) 0.087(3) 0.002(4) 0.021(3) 0.009(4) F3 0.206(8) 0.207(8) 0.194(7) 0.058(6) 0.076(6) 0.122(7) Sb2 0.0880(5) 0.0574(4) 0.0846(5) -0.0006(3) -0.0384(4) 0.0004(3) F4 0.496(19) 0.233(9) 0.108(5) -0.022(6) -0.054(8) 0.243(12) F5 0.156(7) 0.176(8) 0.54(2) 0.159(11) -0.144(10) -0.056(6) F6 0.150(4) 0.080(3) 0.109(4) 0.005(3) -0.061(3) 0.021(3) O3 0.072(3) 0.142(5) 0.059(3) -0.037(3) 0.006(2) -0.013(3) C19 0.074(6) 0.242(14) 0.105(7) -0.034(8) 0.007(5) 0.020(7) C20 0.115(8) 0.186(11) 0.123(8) -0.066(8) 0.056(7) -0.008(8) C21 0.152(9) 0.101(6) 0.077(5) -0.029(5) 0.006(5) -0.023(6) C22 0.083(5) 0.163(9) 0.074(5) -0.045(5) 0.005(4) -0.029(5) _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 N3 2.126(4) . ? Ag1 N1 2.138(4) 2_755 ? Ag1 Ag1 3.0236(7) 2_755 ? N1 C4 1.335(7) . ? N1 N2 1.362(6) . ? N1 Ag1 2.138(4) 2_755 ? N2 C2 1.359(6) . ? N2 C11 1.450(6) . ? N3 C7 1.339(6) . ? N3 N4 1.365(5) . ? N4 C9 1.356(6) . ? N4 C11 1.468(6) . ? O1 C15 1.353(6) . ? O2 C16 1.354(6) . ? O2 C18 1.383(8) . ? C1 C2 1.494(8) . ? C2 C3 1.355(9) . ? C3 C4 1.395(8) . ? C4 C5 1.491(8) . ? C6 C7 1.497(7) . ? C7 C8 1.388(7) . ? C8 C9 1.359(7) . ? C9 C10 1.491(8) . ? C11 C12 1.510(6) . ? C12 C13 1.373(7) . ? C12 C17 1.401(6) . ? C13 C14 1.379(7) . ? C14 C15 1.372(7) . ? C15 C16 1.399(7) . ? C16 C17 1.379(7) . ? Sb1 F3 1.806(6) 2_755 ? Sb1 F3 1.806(6) . ? Sb1 F2 1.834(5) . ? Sb1 F2 1.834(5) 2_755 ? Sb1 F1 1.872(6) . ? Sb1 F1 1.872(6) 2_755 ? Sb2 F5 1.747(8) . ? Sb2 F5 1.747(8) 5_756 ? Sb2 F4 1.749(7) . ? Sb2 F4 1.749(7) 5_756 ? Sb2 F6 1.866(4) . ? Sb2 F6 1.866(4) 5_756 ? O3 C22 1.386(9) . ? O3 C19 1.405(10) . ? C19 C20 1.443(13) . ? C20 C21 1.466(13) . ? C21 C22 1.461(11) . ? 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 N3 Ag1 N1 172.98(15) . 2_755 ? N3 Ag1 Ag1 107.59(10) . 2_755 ? N1 Ag1 Ag1 71.29(10) 2_755 2_755 ? C4 N1 N2 106.0(4) . . ? C4 N1 Ag1 124.6(4) . 2_755 ? N2 N1 Ag1 128.3(3) . 2_755 ? N1 N2 C2 110.6(4) . . ? N1 N2 C11 124.0(4) . . ? C2 N2 C11 125.4(4) . . ? C7 N3 N4 105.4(4) . . ? C7 N3 Ag1 125.5(3) . . ? N4 N3 Ag1 128.8(3) . . ? C9 N4 N3 111.4(4) . . ? C9 N4 C11 125.6(4) . . ? N3 N4 C11 122.9(4) . . ? C16 O2 C18 118.6(5) . . ? C3 C2 N2 107.0(5) . . ? C3 C2 C1 131.1(5) . . ? N2 C2 C1 121.9(5) . . ? C2 C3 C4 106.7(5) . . ? N1 C4 C3 109.8(5) . . ? N1 C4 C5 121.3(5) . . ? C3 C4 C5 128.9(5) . . ? N3 C7 C8 109.7(4) . . ? N3 C7 C6 120.8(4) . . ? C8 C7 C6 129.4(4) . . ? C9 C8 C7 107.5(4) . . ? N4 C9 C8 106.0(4) . . ? N4 C9 C10 123.0(5) . . ? C8 C9 C10 131.0(5) . . ? N2 C11 N4 110.3(4) . . ? N2 C11 C12 115.0(4) . . ? N4 C11 C12 112.9(4) . . ? C13 C12 C17 118.9(4) . . ? C13 C12 C11 122.4(4) . . ? C17 C12 C11 118.4(4) . . ? C12 C13 C14 120.5(4) . . ? C15 C14 C13 121.4(4) . . ? O1 C15 C14 120.0(4) . . ? O1 C15 C16 121.4(4) . . ? C14 C15 C16 118.6(4) . . ? O2 C16 C17 125.1(5) . . ? O2 C16 C15 114.7(4) . . ? C17 C16 C15 120.2(4) . . ? C16 C17 C12 120.3(4) . . ? F3 Sb1 F3 99.9(7) 2_755 . ? F3 Sb1 F2 89.5(4) 2_755 . ? F3 Sb1 F2 89.6(3) . . ? F3 Sb1 F2 89.6(3) 2_755 2_755 ? F3 Sb1 F2 89.5(4) . 2_755 ? F2 Sb1 F2 178.7(5) . 2_755 ? F3 Sb1 F1 173.7(4) 2_755 . ? F3 Sb1 F1 86.4(4) . . ? F2 Sb1 F1 91.3(3) . . ? F2 Sb1 F1 89.7(3) 2_755 . ? F3 Sb1 F1 86.4(4) 2_755 2_755 ? F3 Sb1 F1 173.7(4) . 2_755 ? F2 Sb1 F1 89.7(3) . 2_755 ? F2 Sb1 F1 91.3(3) 2_755 2_755 ? F1 Sb1 F1 87.4(5) . 2_755 ? F5 Sb2 F5 180.0(5) . 5_756 ? F5 Sb2 F4 84.5(7) . . ? F5 Sb2 F4 95.5(7) 5_756 . ? F5 Sb2 F4 95.5(7) . 5_756 ? F5 Sb2 F4 84.5(7) 5_756 5_756 ? F4 Sb2 F4 180.000(2) . 5_756 ? F5 Sb2 F6 90.9(3) . . ? F5 Sb2 F6 89.1(3) 5_756 . ? F4 Sb2 F6 87.0(3) . . ? F4 Sb2 F6 93.0(3) 5_756 . ? F5 Sb2 F6 89.1(3) . 5_756 ? F5 Sb2 F6 90.9(3) 5_756 5_756 ? F4 Sb2 F6 93.0(3) . 5_756 ? F4 Sb2 F6 87.0(3) 5_756 5_756 ? F6 Sb2 F6 180.0(2) . 5_756 ? C22 O3 C19 109.2(6) . . ? O3 C19 C20 106.5(8) . . ? C19 C20 C21 105.7(8) . . ? C22 C21 C20 103.5(7) . . ? O3 C22 C21 108.8(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.196 _refine_diff_density_min -1.406 _refine_diff_density_rms 0.101 # Attachment 'gs024.cif' data_gs024 _database_code_depnum_ccdc_archive 'CCDC 720112' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 Ag N9 O7' _chemical_formula_weight 822.67 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5688(4) _cell_length_b 15.7555(7) _cell_length_c 24.7812(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.724(2) _cell_angle_gamma 90.00 _cell_volume 3734.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 23.15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8404 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33620 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5359 _reflns_number_gt 4257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0579P)^2^+3.1741P] 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 5359 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.07972(3) 0.754774(17) 0.415080(11) 0.04780(13) Uani 1 1 d . . . N1 N 0.0551(3) 0.76421(19) 0.31989(12) 0.0466(8) Uani 1 1 d . . . N2 N 0.1555(3) 0.80432(18) 0.29159(11) 0.0412(7) Uani 1 1 d . . . N3 N 0.2452(3) 0.85593(18) 0.40518(11) 0.0421(7) Uani 1 1 d . . . N4 N 0.3069(3) 0.87130(17) 0.35748(11) 0.0413(7) Uani 1 1 d . . . N5 N -0.0243(3) 0.63857(18) 0.44834(11) 0.0433(7) Uani 1 1 d . . . N6 N -0.1166(3) 0.63804(17) 0.48942(11) 0.0398(7) Uani 1 1 d . . . N7 N -0.1101(3) 0.82689(18) 0.45721(10) 0.0401(7) Uani 1 1 d . . . N8 N -0.1960(3) 0.78208(18) 0.48954(11) 0.0374(6) Uani 1 1 d . . . O1 O 0.5369(3) 0.49129(17) 0.36842(11) 0.0658(8) Uani 1 1 d . . . H1A H 0.5021 0.4537 0.3488 0.099 Uiso 1 1 calc R . . O2 O 0.3466(3) 0.49908(16) 0.28927(10) 0.0606(7) Uani 1 1 d . . . O3 O 0.0484(2) 0.88207(16) 0.67410(9) 0.0511(6) Uani 1 1 d . . . O4 O 0.3006(3) 0.82955(18) 0.66154(10) 0.0630(8) Uani 1 1 d . . . H4A H 0.3790 0.8127 0.6529 0.095 Uiso 1 1 calc R . . C1 C 0.1899(5) 0.8807(3) 0.20442(15) 0.0646(12) Uani 1 1 d . . . H1B H 0.1329 0.8947 0.1726 0.097 Uiso 1 1 calc R . . H1C H 0.2686 0.8462 0.1940 0.097 Uiso 1 1 calc R . . H1D H 0.2240 0.9325 0.2214 0.097 Uiso 1 1 calc R . . C2 C 0.1048(4) 0.8329(2) 0.24292(14) 0.0479(9) Uani 1 1 d . . . C3 C -0.0317(4) 0.8101(3) 0.24033(15) 0.0567(11) Uani 1 1 d . . . H3A H -0.0957 0.8205 0.2116 0.068 Uiso 1 1 calc R . . C4 C -0.0593(4) 0.7682(3) 0.28823(16) 0.0526(10) Uani 1 1 d . . . C5 C -0.1936(4) 0.7320(3) 0.3067(2) 0.0754(14) Uani 1 1 d . . . H5A H -0.1790 0.7068 0.3422 0.113 Uiso 1 1 calc R . . H5B H -0.2263 0.6889 0.2814 0.113 Uiso 1 1 calc R . . H5C H -0.2629 0.7767 0.3087 0.113 Uiso 1 1 calc R . . C6 C 0.4445(5) 0.9835(3) 0.3116(2) 0.0819(15) Uani 1 1 d . . . H6A H 0.4423 0.9426 0.2823 0.123 Uiso 1 1 calc R . . H6B H 0.5408 0.9946 0.3228 0.123 Uiso 1 1 calc R . . H6C H 0.4005 1.0359 0.2995 0.123 Uiso 1 1 calc R . . C7 C 0.3680(4) 0.9487(2) 0.35781(17) 0.0496(10) Uani 1 1 d . . . C8 C 0.3441(4) 0.9831(2) 0.40711(17) 0.0506(10) Uani 1 1 d . . . H8A H 0.3743 1.0365 0.4196 0.061 Uiso 1 1 calc R . . C9 C 0.2675(3) 0.9249(2) 0.43506(14) 0.0435(9) Uani 1 1 d . . . C10 C 0.2119(5) 0.9299(3) 0.49048(16) 0.0642(11) Uani 1 1 d . . . H10A H 0.1616 0.8781 0.4983 0.096 Uiso 1 1 calc R . . H10B H 0.1490 0.9780 0.4927 0.096 Uiso 1 1 calc R . . H10C H 0.2889 0.9369 0.5165 0.096 Uiso 1 1 calc R . . C11 C 0.2974(3) 0.8092(2) 0.31383(14) 0.0409(8) Uani 1 1 d . . . H11A H 0.3563 0.8307 0.2846 0.049 Uiso 1 1 calc R . . C12 C 0.3563(3) 0.7235(2) 0.33027(13) 0.0379(8) Uani 1 1 d . . . C13 C 0.4578(4) 0.7162(3) 0.37071(15) 0.0501(9) Uani 1 1 d . . . H13A H 0.4868 0.7647 0.3901 0.060 Uiso 1 1 calc R . . C14 C 0.5175(4) 0.6385(3) 0.38307(16) 0.0552(10) Uani 1 1 d . . . H14A H 0.5859 0.6347 0.4110 0.066 Uiso 1 1 calc R . . C15 C 0.4786(4) 0.5671(2) 0.35528(14) 0.0447(9) Uani 1 1 d . . . C16 C 0.3772(4) 0.5747(2) 0.31345(13) 0.0422(8) Uani 1 1 d . . . C17 C 0.3177(4) 0.6518(2) 0.30138(13) 0.0423(8) Uani 1 1 d . . . H17A H 0.2501 0.6560 0.2732 0.051 Uiso 1 1 calc R . . C18 C 0.2354(4) 0.4988(3) 0.24992(16) 0.0618(11) Uani 1 1 d . . . H18A H 0.2233 0.4419 0.2356 0.093 Uiso 1 1 calc R . . H18B H 0.2574 0.5374 0.2209 0.093 Uiso 1 1 calc R . . H18C H 0.1498 0.5170 0.2664 0.093 Uiso 1 1 calc R . . C19 C -0.3027(4) 0.5446(3) 0.52755(18) 0.0675(12) Uani 1 1 d . . . H19A H -0.3102 0.5908 0.5532 0.101 Uiso 1 1 calc R . . H19B H -0.2785 0.4927 0.5467 0.101 Uiso 1 1 calc R . . H19C H -0.3915 0.5373 0.5082 0.101 Uiso 1 1 calc R . . C20 C -0.1919(4) 0.5649(2) 0.48846(15) 0.0468(9) Uani 1 1 d . . . C21 C -0.1460(4) 0.5189(2) 0.44610(16) 0.0532(10) Uani 1 1 d . . . H21A H -0.1787 0.4652 0.4349 0.064 Uiso 1 1 calc R . . C22 C -0.0419(4) 0.5660(2) 0.42245(14) 0.0485(9) Uani 1 1 d . . . C23 C 0.0412(5) 0.5452(3) 0.37480(17) 0.0701(12) Uani 1 1 d . . . H23A H 0.1058 0.5911 0.3680 0.105 Uiso 1 1 calc R . . H23B H -0.0210 0.5375 0.3435 0.105 Uiso 1 1 calc R . . H23C H 0.0932 0.4932 0.3816 0.105 Uiso 1 1 calc R . . C24 C -0.4462(4) 0.7734(3) 0.5155(2) 0.0691(12) Uani 1 1 d . . . H24A H -0.4113 0.7276 0.5383 0.104 Uiso 1 1 calc R . . H24B H -0.5173 0.7517 0.4904 0.104 Uiso 1 1 calc R . . H24C H -0.4862 0.8172 0.5377 0.104 Uiso 1 1 calc R . . C25 C -0.3295(4) 0.8096(2) 0.48491(14) 0.0446(9) Uani 1 1 d . . . C26 C -0.3290(4) 0.8741(2) 0.44829(15) 0.0495(9) Uani 1 1 d . . . H26A H -0.4062 0.9068 0.4365 0.059 Uiso 1 1 calc R . . C27 C -0.1926(4) 0.8823(2) 0.43185(13) 0.0435(9) Uani 1 1 d . . . C28 C -0.1320(5) 0.9435(3) 0.39237(15) 0.0625(11) Uani 1 1 d . . . H28A H -0.0326 0.9328 0.3896 0.094 Uiso 1 1 calc R . . H28B H -0.1465 1.0011 0.4047 0.094 Uiso 1 1 calc R . . H28C H -0.1778 0.9359 0.3572 0.094 Uiso 1 1 calc R . . C29 C -0.1379(3) 0.7128(2) 0.52263(13) 0.0373(8) Uani 1 1 d . . . H29A H -0.2111 0.6973 0.5483 0.045 Uiso 1 1 calc R . . C30 C -0.0130(3) 0.74182(19) 0.55666(13) 0.0343(8) Uani 1 1 d . . . C31 C -0.0391(3) 0.7996(2) 0.59732(13) 0.0373(8) Uani 1 1 d . . . H31A H -0.1305 0.8201 0.6012 0.045 Uiso 1 1 calc R . . C32 C 0.0655(3) 0.8278(2) 0.63215(13) 0.0384(8) Uani 1 1 d . . . C33 C 0.2017(3) 0.7987(2) 0.62589(13) 0.0423(8) Uani 1 1 d . . . C34 C 0.2276(4) 0.7414(2) 0.58627(15) 0.0462(9) Uani 1 1 d . . . H34A H 0.3191 0.7210 0.5824 0.055 Uiso 1 1 calc R . . C35 C 0.1208(3) 0.7123(2) 0.55133(13) 0.0408(8) Uani 1 1 d . . . H35A H 0.1405 0.6727 0.5243 0.049 Uiso 1 1 calc R . . C36 C -0.0885(4) 0.9111(3) 0.68337(17) 0.0672(12) Uani 1 1 d . . . H36A H -0.0868 0.9489 0.7143 0.101 Uiso 1 1 calc R . . H36B H -0.1485 0.8630 0.6905 0.101 Uiso 1 1 calc R . . H36C H -0.1243 0.9413 0.6517 0.101 Uiso 1 1 calc R . . N9 N -0.3991(4) 0.7146(2) 0.65700(14) 0.0552(8) Uani 1 1 d . . . O7 O -0.2972(3) 0.6769(2) 0.63929(13) 0.0837(10) Uani 1 1 d . . . O6 O -0.4134(4) 0.7921(3) 0.65203(18) 0.1080(13) Uani 1 1 d . . . O5 O -0.4924(4) 0.6764(3) 0.6741(2) 0.1266(17) 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 0.0532(2) 0.0488(2) 0.04202(19) 0.00045(13) 0.01100(13) -0.01010(13) N1 0.0386(17) 0.065(2) 0.0363(17) -0.0030(14) 0.0003(14) -0.0009(14) N2 0.0392(17) 0.0494(18) 0.0350(16) 0.0011(14) 0.0029(13) 0.0049(13) N3 0.0435(17) 0.0417(18) 0.0414(16) -0.0022(14) 0.0068(13) -0.0054(13) N4 0.0388(16) 0.0372(17) 0.0480(18) 0.0031(14) 0.0057(13) -0.0042(12) N5 0.0509(18) 0.0407(18) 0.0383(16) -0.0003(14) 0.0024(14) -0.0059(13) N6 0.0437(17) 0.0394(17) 0.0363(16) 0.0030(13) -0.0003(13) -0.0081(13) N7 0.0457(17) 0.0437(17) 0.0307(15) 0.0073(13) 0.0000(13) 0.0009(13) N8 0.0366(16) 0.0415(16) 0.0340(15) 0.0040(13) -0.0020(13) -0.0017(13) O1 0.0713(18) 0.0530(17) 0.0720(19) -0.0009(14) -0.0145(15) 0.0151(14) O2 0.083(2) 0.0477(17) 0.0500(16) -0.0087(13) -0.0139(15) 0.0032(14) O3 0.0470(15) 0.0598(17) 0.0461(15) -0.0127(13) -0.0055(12) 0.0090(12) O4 0.0404(15) 0.090(2) 0.0578(16) -0.0180(15) -0.0154(13) 0.0060(14) C1 0.083(3) 0.070(3) 0.040(2) 0.010(2) 0.006(2) 0.014(2) C2 0.060(3) 0.050(2) 0.034(2) -0.0057(17) 0.0000(18) 0.0171(18) C3 0.058(3) 0.070(3) 0.041(2) -0.010(2) -0.0099(19) 0.014(2) C4 0.043(2) 0.065(3) 0.049(2) -0.020(2) -0.0017(19) 0.0035(18) C5 0.046(3) 0.110(4) 0.070(3) -0.020(3) -0.003(2) -0.009(2) C6 0.085(3) 0.065(3) 0.097(4) 0.012(3) 0.027(3) -0.027(3) C7 0.036(2) 0.040(2) 0.072(3) 0.010(2) 0.0001(19) -0.0016(16) C8 0.045(2) 0.034(2) 0.072(3) -0.0043(19) -0.013(2) -0.0024(16) C9 0.040(2) 0.039(2) 0.051(2) -0.0091(18) -0.0073(17) 0.0011(16) C10 0.073(3) 0.061(3) 0.059(3) -0.021(2) 0.002(2) -0.005(2) C11 0.038(2) 0.046(2) 0.0388(19) -0.0013(16) 0.0073(16) 0.0003(15) C12 0.0355(19) 0.044(2) 0.0344(19) 0.0004(16) 0.0041(15) -0.0003(15) C13 0.048(2) 0.051(2) 0.051(2) -0.0073(19) -0.0070(19) -0.0014(18) C14 0.051(2) 0.058(3) 0.055(2) -0.003(2) -0.0181(19) 0.0058(19) C15 0.043(2) 0.045(2) 0.046(2) 0.0027(18) -0.0006(17) 0.0059(17) C16 0.046(2) 0.047(2) 0.0337(19) -0.0042(17) 0.0041(16) -0.0009(17) C17 0.043(2) 0.052(2) 0.0321(18) -0.0033(17) -0.0033(15) 0.0038(17) C18 0.065(3) 0.067(3) 0.054(2) -0.017(2) -0.007(2) -0.008(2) C19 0.068(3) 0.055(3) 0.080(3) 0.013(2) 0.006(2) -0.021(2) C20 0.046(2) 0.045(2) 0.049(2) 0.0133(19) -0.0103(18) -0.0110(17) C21 0.065(3) 0.036(2) 0.057(2) -0.0009(19) -0.013(2) -0.0080(18) C22 0.061(2) 0.040(2) 0.044(2) -0.0010(18) -0.0080(18) -0.0023(18) C23 0.091(3) 0.059(3) 0.060(3) -0.017(2) 0.008(2) -0.001(2) C24 0.039(2) 0.079(3) 0.089(3) 0.010(3) 0.005(2) 0.003(2) C25 0.038(2) 0.048(2) 0.047(2) -0.0060(18) -0.0072(16) 0.0003(16) C26 0.046(2) 0.047(2) 0.055(2) -0.0031(19) -0.0196(18) 0.0073(17) C27 0.060(2) 0.036(2) 0.0342(19) -0.0039(16) -0.0082(17) 0.0027(17) C28 0.092(3) 0.056(3) 0.040(2) 0.0132(19) -0.002(2) 0.010(2) C29 0.0364(18) 0.041(2) 0.0344(18) 0.0069(16) -0.0001(15) -0.0023(15) C30 0.0368(19) 0.0359(19) 0.0301(18) 0.0105(14) -0.0004(14) -0.0012(14) C31 0.0317(18) 0.043(2) 0.0366(19) 0.0051(16) 0.0006(15) 0.0038(15) C32 0.043(2) 0.041(2) 0.0313(18) 0.0016(16) -0.0028(16) 0.0020(15) C33 0.036(2) 0.055(2) 0.0349(19) 0.0026(17) -0.0069(16) 0.0037(17) C34 0.0328(19) 0.062(3) 0.043(2) 0.0051(18) -0.0020(16) 0.0116(16) C35 0.045(2) 0.041(2) 0.0368(19) 0.0028(16) 0.0009(16) 0.0050(16) C36 0.055(3) 0.085(3) 0.061(3) -0.018(2) -0.002(2) 0.021(2) N9 0.046(2) 0.061(2) 0.059(2) 0.0046(18) -0.0023(17) -0.0006(18) O7 0.073(2) 0.094(2) 0.085(2) 0.0126(19) 0.0206(18) 0.0157(19) O6 0.138(4) 0.056(2) 0.131(3) -0.002(2) 0.025(3) 0.002(2) O5 0.061(2) 0.086(3) 0.235(5) 0.011(3) 0.049(3) 0.005(2) _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 N5 2.252(3) . ? Ag1 N3 2.265(3) . ? Ag1 N1 2.368(3) . ? Ag1 N7 2.407(3) . ? N1 C4 1.329(5) . ? N1 N2 1.362(4) . ? N2 C2 1.363(4) . ? N2 C11 1.451(4) . ? N3 C9 1.329(4) . ? N3 N4 1.359(4) . ? N4 C7 1.352(4) . ? N4 C11 1.460(4) . ? N5 C22 1.319(4) . ? N5 N6 1.368(4) . ? N6 C20 1.359(4) . ? N6 C29 1.454(4) . ? N7 C27 1.323(4) . ? N7 N8 1.362(4) . ? N8 C25 1.350(4) . ? N8 C29 1.465(4) . ? O1 C15 1.354(4) . ? O2 C16 1.361(4) . ? O2 C18 1.421(5) . ? O3 C32 1.360(4) . ? O3 C36 1.413(4) . ? O4 C33 1.365(4) . ? C1 C2 1.479(5) . ? C2 C3 1.354(5) . ? C3 C4 1.390(6) . ? C4 C5 1.491(6) . ? C6 C7 1.482(6) . ? C7 C8 1.362(5) . ? C8 C9 1.374(5) . ? C9 C10 1.489(5) . ? C11 C12 1.513(5) . ? C12 C13 1.380(5) . ? C12 C17 1.382(5) . ? C13 C14 1.382(5) . ? C14 C15 1.365(5) . ? C15 C16 1.403(5) . ? C16 C17 1.372(5) . ? C19 C20 1.492(5) . ? C20 C21 1.359(5) . ? C21 C22 1.387(5) . ? C22 C23 1.480(5) . ? C24 C25 1.482(5) . ? C25 C26 1.363(5) . ? C26 C27 1.385(5) . ? C27 C28 1.501(5) . ? C29 C30 1.513(5) . ? C30 C35 1.372(5) . ? C30 C31 1.386(5) . ? C31 C32 1.375(5) . ? C32 C33 1.395(5) . ? C33 C34 1.362(5) . ? C34 C35 1.397(5) . ? N9 O5 1.167(5) . ? N9 O6 1.235(5) . ? N9 O7 1.234(4) . ? 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 N5 Ag1 N3 158.40(10) . . ? N5 Ag1 N1 112.56(10) . . ? N3 Ag1 N1 84.09(10) . . ? N5 Ag1 N7 82.95(10) . . ? N3 Ag1 N7 104.71(10) . . ? N1 Ag1 N7 110.40(9) . . ? C4 N1 N2 104.8(3) . . ? C4 N1 Ag1 130.3(3) . . ? N2 N1 Ag1 119.4(2) . . ? N1 N2 C2 111.7(3) . . ? N1 N2 C11 119.7(3) . . ? C2 N2 C11 128.5(3) . . ? C9 N3 N4 105.8(3) . . ? C9 N3 Ag1 128.0(2) . . ? N4 N3 Ag1 122.9(2) . . ? C7 N4 N3 110.8(3) . . ? C7 N4 C11 128.8(3) . . ? N3 N4 C11 120.4(3) . . ? C22 N5 N6 106.3(3) . . ? C22 N5 Ag1 125.3(2) . . ? N6 N5 Ag1 125.4(2) . . ? C20 N6 N5 110.2(3) . . ? C20 N6 C29 127.8(3) . . ? N5 N6 C29 121.4(3) . . ? C27 N7 N8 105.0(3) . . ? C27 N7 Ag1 123.5(2) . . ? N8 N7 Ag1 119.2(2) . . ? C25 N8 N7 111.7(3) . . ? C25 N8 C29 129.0(3) . . ? N7 N8 C29 119.3(3) . . ? C16 O2 C18 116.8(3) . . ? C32 O3 C36 117.4(3) . . ? C3 C2 N2 105.8(3) . . ? C3 C2 C1 130.8(4) . . ? N2 C2 C1 123.4(4) . . ? C2 C3 C4 107.1(3) . . ? N1 C4 C3 110.6(3) . . ? N1 C4 C5 120.1(4) . . ? C3 C4 C5 129.2(4) . . ? N4 C7 C8 106.2(3) . . ? N4 C7 C6 123.5(4) . . ? C8 C7 C6 130.3(4) . . ? C7 C8 C9 107.1(3) . . ? N3 C9 C8 110.1(3) . . ? N3 C9 C10 120.1(3) . . ? C8 C9 C10 129.8(3) . . ? N2 C11 N4 110.7(3) . . ? N2 C11 C12 113.1(3) . . ? N4 C11 C12 112.6(3) . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C11 121.2(3) . . ? C17 C12 C11 119.8(3) . . ? C12 C13 C14 120.8(4) . . ? C15 C14 C13 120.9(3) . . ? O1 C15 C14 120.1(3) . . ? O1 C15 C16 121.6(3) . . ? C14 C15 C16 118.4(3) . . ? O2 C16 C17 126.7(3) . . ? O2 C16 C15 112.7(3) . . ? C17 C16 C15 120.6(3) . . ? C16 C17 C12 120.6(3) . . ? N6 C20 C21 106.4(3) . . ? N6 C20 C19 123.8(4) . . ? C21 C20 C19 129.8(3) . . ? C20 C21 C22 107.1(3) . . ? N5 C22 C21 110.0(3) . . ? N5 C22 C23 121.1(3) . . ? C21 C22 C23 128.9(4) . . ? N8 C25 C26 105.8(3) . . ? N8 C25 C24 123.9(3) . . ? C26 C25 C24 130.2(3) . . ? C25 C26 C27 106.8(3) . . ? N7 C27 C26 110.6(3) . . ? N7 C27 C28 119.8(3) . . ? C26 C27 C28 129.6(3) . . ? N6 C29 N8 110.1(3) . . ? N6 C29 C30 116.0(3) . . ? N8 C29 C30 111.5(3) . . ? C35 C30 C31 118.8(3) . . ? C35 C30 C29 124.6(3) . . ? C31 C30 C29 116.6(3) . . ? C32 C31 C30 121.6(3) . . ? O3 C32 C31 125.5(3) . . ? O3 C32 C33 115.2(3) . . ? C31 C32 C33 119.3(3) . . ? C34 C33 O4 124.4(3) . . ? C34 C33 C32 119.3(3) . . ? O4 C33 C32 116.3(3) . . ? C33 C34 C35 121.2(3) . . ? C30 C35 C34 119.8(3) . . ? O5 N9 O6 117.6(4) . . ? O5 N9 O7 120.2(4) . . ? O6 N9 O7 121.8(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.485 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.060 # Attachment 'gs028a.cif' data_gs028a _database_code_depnum_ccdc_archive 'CCDC 720113' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Ag B F4 N8 O5' _chemical_formula_weight 919.58 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3894(7) _cell_length_b 24.7239(18) _cell_length_c 18.8870(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.518(4) _cell_angle_gamma 90.00 _cell_volume 4346.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.60 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8153 _exptl_absorpt_correction_T_max 0.9487 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42624 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.22 _reflns_number_total 8701 _reflns_number_gt 6487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0812P)^2^+4.7599P] 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 8701 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.08180(3) 0.685991(12) 0.130820(16) 0.05080(13) Uani 1 1 d . . . N1 N 0.1187(3) 0.59174(12) 0.15797(16) 0.0446(7) Uani 1 1 d . . . N2 N 0.0125(3) 0.55679(11) 0.13243(15) 0.0390(6) Uani 1 1 d . . . N3 N -0.1059(3) 0.65398(11) 0.05534(16) 0.0442(7) Uani 1 1 d . . . N4 N -0.1775(3) 0.60749(11) 0.06592(15) 0.0381(6) Uani 1 1 d . . . N5 N 0.1830(3) 0.73436(12) 0.22706(16) 0.0477(7) Uani 1 1 d . . . N6 N 0.2988(3) 0.76647(12) 0.21907(17) 0.0467(7) Uani 1 1 d . . . N7 N 0.2807(3) 0.71613(12) 0.07611(18) 0.0498(7) Uani 1 1 d . . . N8 N 0.3639(3) 0.75847(13) 0.10170(18) 0.0519(8) Uani 1 1 d . . . O1 O -0.2886(3) 0.64483(11) 0.39242(15) 0.0592(7) Uani 1 1 d . . . H1A H -0.2488 0.6253 0.4249 0.089 Uiso 1 1 calc R . . O2 O -0.1433(3) 0.55287(11) 0.38561(14) 0.0602(7) Uani 1 1 d . . . O3 O -0.1927(3) 0.90391(11) 0.03144(14) 0.0542(7) Uani 1 1 d . . . H3A H -0.2208 0.8903 -0.0081 0.081 Uiso 1 1 calc R . . O4 O -0.1452(3) 0.89260(13) 0.17284(14) 0.0611(7) Uani 1 1 d . . . C1 C -0.1065(5) 0.72158(19) -0.0391(3) 0.0738(14) Uani 1 1 d . . . H1B H -0.0310 0.7370 -0.0051 0.111 Uiso 1 1 calc R . . H1C H -0.1848 0.7473 -0.0484 0.111 Uiso 1 1 calc R . . H1D H -0.0687 0.7135 -0.0833 0.111 Uiso 1 1 calc R . . C2 C -0.1601(4) 0.67110(15) -0.0094(2) 0.0487(9) Uani 1 1 d . . . C3 C -0.2676(4) 0.63613(15) -0.0395(2) 0.0478(9) Uani 1 1 d . . . H3B H -0.3225 0.6395 -0.0846 0.057 Uiso 1 1 calc R . . C4 C -0.2778(4) 0.59610(14) 0.00914(19) 0.0411(8) Uani 1 1 d . . . C5 C -0.3765(4) 0.54904(16) 0.0079(2) 0.0523(9) Uani 1 1 d . . . H5A H -0.3543 0.5284 0.0517 0.078 Uiso 1 1 calc R . . H5B H -0.3648 0.5262 -0.0327 0.078 Uiso 1 1 calc R . . H5C H -0.4750 0.5618 0.0039 0.078 Uiso 1 1 calc R . . C6 C 0.3819(4) 0.5913(2) 0.1808(3) 0.0691(12) Uani 1 1 d . . . H6A H 0.3661 0.6282 0.1953 0.104 Uiso 1 1 calc R . . H6B H 0.4381 0.5915 0.1412 0.104 Uiso 1 1 calc R . . H6C H 0.4333 0.5716 0.2206 0.104 Uiso 1 1 calc R . . C7 C 0.2402(4) 0.56457(17) 0.1580(2) 0.0491(9) Uani 1 1 d . . . C8 C 0.2119(4) 0.51208(17) 0.1336(2) 0.0523(10) Uani 1 1 d . . . H8A H 0.2801 0.4848 0.1295 0.063 Uiso 1 1 calc R . . C9 C 0.0659(4) 0.50760(15) 0.11670(17) 0.0431(8) Uani 1 1 d . . . C10 C -0.0263(5) 0.46222(15) 0.0869(2) 0.0561(10) Uani 1 1 d . . . H10A H -0.1262 0.4733 0.0817 0.084 Uiso 1 1 calc R . . H10B H -0.0125 0.4315 0.1189 0.084 Uiso 1 1 calc R . . H10C H -0.0005 0.4522 0.0406 0.084 Uiso 1 1 calc R . . C11 C -0.1372(3) 0.57305(13) 0.12795(17) 0.0371(7) Uani 1 1 d . . . H11A H -0.1945 0.5395 0.1193 0.044 Uiso 1 1 calc R . . C12 C -0.1736(3) 0.59611(13) 0.19742(18) 0.0375(7) Uani 1 1 d . . . C13 C -0.1358(4) 0.56479(14) 0.25842(19) 0.0419(8) Uani 1 1 d . . . H13A H -0.0834 0.5327 0.2552 0.050 Uiso 1 1 calc R . . C14 C -0.1742(4) 0.58026(14) 0.32323(19) 0.0426(8) Uani 1 1 d . . . C15 C -0.2509(4) 0.62807(14) 0.3284(2) 0.0452(8) Uani 1 1 d . . . C16 C -0.2893(4) 0.65855(16) 0.2682(2) 0.0527(10) Uani 1 1 d . . . H16A H -0.3418 0.6906 0.2713 0.063 Uiso 1 1 calc R . . C17 C -0.2511(4) 0.64243(15) 0.2026(2) 0.0463(8) Uani 1 1 d . . . H17A H -0.2787 0.6635 0.1616 0.056 Uiso 1 1 calc R . . C18 C -0.0927(5) 0.49886(18) 0.3825(2) 0.0648(12) Uani 1 1 d . . . H18A H -0.0751 0.4840 0.4304 0.097 Uiso 1 1 calc R . . H18B H -0.0041 0.4986 0.3612 0.097 Uiso 1 1 calc R . . H18C H -0.1643 0.4771 0.3538 0.097 Uiso 1 1 calc R . . C19 C 0.1051(6) 0.6771(2) 0.3197(3) 0.0827(16) Uani 1 1 d . . . H19A H 0.0222 0.6726 0.2837 0.124 Uiso 1 1 calc R . . H19B H 0.0747 0.6925 0.3625 0.124 Uiso 1 1 calc R . . H19C H 0.1497 0.6422 0.3309 0.124 Uiso 1 1 calc R . . C20 C 0.2106(5) 0.71405(17) 0.2920(2) 0.0546(10) Uani 1 1 d . . . C21 C 0.3431(5) 0.73161(19) 0.3249(2) 0.0660(12) Uani 1 1 d . . . H21A H 0.3865 0.7221 0.3709 0.079 Uiso 1 1 calc R . . C22 C 0.3985(4) 0.76494(16) 0.2786(2) 0.0558(11) Uani 1 1 d . . . C23 C 0.5366(5) 0.79500(18) 0.2837(3) 0.0754(15) Uani 1 1 d . . . H23A H 0.5915 0.7886 0.3301 0.113 Uiso 1 1 calc R . . H23B H 0.5173 0.8334 0.2779 0.113 Uiso 1 1 calc R . . H23C H 0.5911 0.7827 0.2466 0.113 Uiso 1 1 calc R . . C24 C 0.2861(7) 0.6465(2) -0.0152(3) 0.0836(15) Uani 1 1 d . . . H24A H 0.1982 0.6356 0.0027 0.125 Uiso 1 1 calc R . . H24B H 0.3550 0.6171 -0.0089 0.125 Uiso 1 1 calc R . . H24C H 0.2653 0.6553 -0.0655 0.125 Uiso 1 1 calc R . . C25 C 0.3472(5) 0.69505(18) 0.0251(2) 0.0599(11) Uani 1 1 d . . . C26 C 0.4701(5) 0.7241(3) 0.0176(3) 0.0847(16) Uani 1 1 d . . . H26A H 0.5351 0.7169 -0.0151 0.102 Uiso 1 1 calc R . . C27 C 0.4797(5) 0.7646(2) 0.0656(3) 0.0709(13) Uani 1 1 d . . . C28 C 0.5877(7) 0.8091(3) 0.0810(5) 0.133(3) Uani 1 1 d . . . H28A H 0.6609 0.8058 0.0495 0.200 Uiso 1 1 calc R . . H28B H 0.6321 0.8066 0.1302 0.200 Uiso 1 1 calc R . . H28C H 0.5400 0.8438 0.0732 0.200 Uiso 1 1 calc R . . C29 C 0.3099(4) 0.79445(15) 0.1529(2) 0.0496(9) Uani 1 1 d . . . H29A H 0.3826 0.8233 0.1639 0.060 Uiso 1 1 calc R . . C30 C 0.1720(4) 0.82198(13) 0.1209(2) 0.0429(8) Uani 1 1 d . . . C31 C 0.0786(4) 0.84368(15) 0.1646(2) 0.0462(8) Uani 1 1 d . . . H31A H 0.0989 0.8398 0.2144 0.055 Uiso 1 1 calc R . . C32 C -0.0442(4) 0.87105(14) 0.13551(19) 0.0446(8) Uani 1 1 d . . . C33 C -0.0720(4) 0.87782(14) 0.06159(19) 0.0432(8) Uani 1 1 d . . . C34 C 0.0225(4) 0.85758(15) 0.0186(2) 0.0499(9) Uani 1 1 d . . . H34A H 0.0049 0.8629 -0.0311 0.060 Uiso 1 1 calc R . . C35 C 0.1437(4) 0.82933(16) 0.0479(2) 0.0505(9) Uani 1 1 d . . . H35A H 0.2069 0.8151 0.0180 0.061 Uiso 1 1 calc R . . C36 C -0.1231(6) 0.8880(3) 0.2480(2) 0.0891(17) Uani 1 1 d . . . H36A H -0.2024 0.9050 0.2677 0.134 Uiso 1 1 calc R . . H36B H -0.0340 0.9059 0.2666 0.134 Uiso 1 1 calc R . . H36C H -0.1179 0.8501 0.2613 0.134 Uiso 1 1 calc R . . O5 O 0.6958(5) -0.01123(17) 0.0873(2) 0.1067(14) Uani 1 1 d . . . C37 C 0.6259(12) -0.0023(5) 0.1465(4) 0.203(6) Uani 1 1 d . . . H37A H 0.5666 -0.0336 0.1552 0.243 Uiso 1 1 calc R . . H37B H 0.6958 0.0038 0.1890 0.243 Uiso 1 1 calc R . . C38 C 0.5408(15) 0.0431(6) 0.1319(5) 0.238(8) Uani 1 1 d . . . H38A H 0.5508 0.0671 0.1735 0.286 Uiso 1 1 calc R . . H38B H 0.4397 0.0323 0.1215 0.286 Uiso 1 1 calc R . . C39 C 0.6959(9) 0.0372(3) 0.0498(5) 0.122(2) Uani 1 1 d . . . H39A H 0.6782 0.0302 -0.0016 0.146 Uiso 1 1 calc R . . H39B H 0.7894 0.0551 0.0606 0.146 Uiso 1 1 calc R . . C40 C 0.5845(11) 0.0711(4) 0.0710(7) 0.163(4) Uani 1 1 d . . . H40A H 0.5042 0.0745 0.0325 0.195 Uiso 1 1 calc R . . H40B H 0.6213 0.1073 0.0844 0.195 Uiso 1 1 calc R . . B1 B 0.3824(6) 0.9350(2) 0.3009(3) 0.0623(13) Uani 1 1 d . . . F1 F 0.3855(7) 0.9324(4) 0.2332(3) 0.237(4) Uani 1 1 d . . . F2 F 0.2800(7) 0.8987(3) 0.3077(4) 0.205(3) Uani 1 1 d . . . F3 F 0.5084(5) 0.91862(18) 0.3312(3) 0.175(3) Uani 1 1 d . . . F4 F 0.3547(7) 0.9792(2) 0.3340(4) 0.201(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 0.04878(19) 0.04628(19) 0.05399(19) -0.00361(13) -0.00587(13) -0.01606(12) N1 0.0379(16) 0.0456(17) 0.0491(17) -0.0002(14) 0.0012(13) -0.0035(13) N2 0.0400(16) 0.0378(16) 0.0390(15) 0.0004(12) 0.0047(12) -0.0013(12) N3 0.0398(16) 0.0373(16) 0.0528(17) 0.0053(13) -0.0038(13) -0.0097(12) N4 0.0373(15) 0.0349(15) 0.0403(15) 0.0007(12) -0.0017(12) -0.0066(11) N5 0.0478(17) 0.0463(18) 0.0465(17) -0.0039(14) -0.0028(14) -0.0113(14) N6 0.0451(17) 0.0372(16) 0.0537(18) -0.0066(14) -0.0087(14) -0.0047(13) N7 0.0491(18) 0.0420(18) 0.0596(19) -0.0012(15) 0.0119(15) -0.0002(14) N8 0.0378(16) 0.0525(19) 0.066(2) 0.0029(16) 0.0086(15) -0.0045(14) O1 0.0683(18) 0.0559(17) 0.0554(16) -0.0093(13) 0.0160(14) 0.0106(14) O2 0.086(2) 0.0529(17) 0.0427(14) 0.0023(12) 0.0124(14) 0.0164(15) O3 0.0617(17) 0.0571(17) 0.0422(14) 0.0001(12) 0.0002(12) 0.0123(13) O4 0.0674(18) 0.0739(19) 0.0417(14) -0.0090(13) 0.0061(13) 0.0166(15) C1 0.078(3) 0.058(3) 0.078(3) 0.030(2) -0.014(2) -0.020(2) C2 0.047(2) 0.043(2) 0.053(2) 0.0067(17) -0.0036(17) -0.0018(16) C3 0.046(2) 0.046(2) 0.047(2) 0.0025(17) -0.0112(16) -0.0012(16) C4 0.0336(17) 0.0415(19) 0.0465(19) -0.0065(15) -0.0009(15) -0.0055(14) C5 0.047(2) 0.052(2) 0.055(2) -0.0054(18) -0.0050(17) -0.0146(17) C6 0.041(2) 0.090(3) 0.074(3) 0.008(3) -0.004(2) 0.000(2) C7 0.039(2) 0.064(3) 0.045(2) 0.0116(18) 0.0051(16) 0.0077(17) C8 0.052(2) 0.059(2) 0.047(2) 0.0070(18) 0.0089(17) 0.0173(19) C9 0.057(2) 0.0388(19) 0.0335(17) 0.0040(14) 0.0082(16) 0.0087(16) C10 0.073(3) 0.037(2) 0.058(2) -0.0032(18) 0.009(2) 0.0074(18) C11 0.0359(17) 0.0313(17) 0.0436(18) 0.0011(14) 0.0037(14) -0.0047(13) C12 0.0324(17) 0.0326(17) 0.0470(19) -0.0015(14) 0.0036(14) -0.0046(13) C13 0.0455(19) 0.0323(17) 0.0486(19) -0.0012(15) 0.0083(16) 0.0032(14) C14 0.046(2) 0.0371(19) 0.0451(19) -0.0005(15) 0.0072(16) 0.0006(15) C15 0.044(2) 0.042(2) 0.051(2) -0.0070(16) 0.0112(16) -0.0025(15) C16 0.052(2) 0.040(2) 0.067(3) -0.0023(19) 0.0137(19) 0.0145(17) C17 0.044(2) 0.042(2) 0.053(2) 0.0059(17) 0.0045(16) 0.0031(15) C18 0.083(3) 0.055(3) 0.057(2) 0.012(2) 0.011(2) 0.018(2) C19 0.094(4) 0.102(4) 0.050(2) 0.014(3) 0.004(2) -0.024(3) C20 0.068(3) 0.051(2) 0.042(2) -0.0038(18) -0.0008(18) -0.0037(19) C21 0.079(3) 0.061(3) 0.050(2) -0.005(2) -0.022(2) 0.000(2) C22 0.053(2) 0.041(2) 0.066(3) -0.0181(19) -0.021(2) 0.0043(17) C23 0.054(3) 0.050(2) 0.111(4) -0.014(3) -0.032(3) -0.002(2) C24 0.108(4) 0.074(3) 0.070(3) -0.019(3) 0.019(3) 0.016(3) C25 0.059(3) 0.063(3) 0.057(2) 0.003(2) 0.008(2) 0.019(2) C26 0.058(3) 0.123(5) 0.079(3) 0.009(3) 0.030(3) 0.016(3) C27 0.042(2) 0.090(4) 0.083(3) 0.012(3) 0.015(2) -0.007(2) C28 0.075(4) 0.181(8) 0.149(7) 0.003(5) 0.038(4) -0.065(5) C29 0.041(2) 0.040(2) 0.065(2) -0.0013(18) -0.0028(18) -0.0133(16) C30 0.044(2) 0.0319(18) 0.051(2) -0.0006(15) -0.0004(16) -0.0066(14) C31 0.052(2) 0.045(2) 0.0390(18) -0.0039(16) -0.0039(16) -0.0069(16) C32 0.054(2) 0.0368(19) 0.0427(19) -0.0076(15) 0.0055(16) -0.0026(16) C33 0.051(2) 0.0345(18) 0.0433(19) 0.0013(15) 0.0038(16) -0.0013(15) C34 0.062(2) 0.044(2) 0.044(2) 0.0014(17) 0.0086(18) 0.0044(17) C35 0.055(2) 0.046(2) 0.052(2) 0.0002(17) 0.0160(18) 0.0020(17) C36 0.092(4) 0.127(5) 0.050(3) -0.016(3) 0.015(2) 0.025(3) O5 0.140(4) 0.084(3) 0.107(3) 0.013(2) 0.058(3) 0.049(3) C37 0.231(10) 0.286(14) 0.111(6) 0.067(7) 0.097(7) 0.176(10) C38 0.312(15) 0.314(16) 0.101(6) 0.027(8) 0.072(8) 0.241(14) C39 0.134(6) 0.091(5) 0.146(6) 0.023(5) 0.038(5) 0.037(4) C40 0.148(8) 0.114(6) 0.225(12) -0.027(7) 0.018(8) 0.058(6) B1 0.059(3) 0.065(3) 0.062(3) 0.003(2) 0.003(2) 0.018(2) F1 0.192(6) 0.443(12) 0.081(3) 0.050(5) 0.030(3) -0.001(6) F2 0.174(5) 0.248(7) 0.201(6) -0.091(5) 0.057(4) -0.109(5) F3 0.149(4) 0.120(3) 0.222(5) -0.067(3) -0.109(4) 0.061(3) F4 0.190(5) 0.105(3) 0.308(8) -0.066(4) 0.030(5) 0.058(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 N3 2.260(3) . ? Ag1 N5 2.277(3) . ? Ag1 N7 2.370(3) . ? Ag1 N1 2.401(3) . ? N1 C7 1.324(5) . ? N1 N2 1.360(4) . ? N2 C9 1.363(4) . ? N2 C11 1.454(4) . ? N3 C2 1.330(5) . ? N3 N4 1.359(4) . ? N4 C4 1.361(4) . ? N4 C11 1.457(4) . ? N5 C20 1.319(5) . ? N5 N6 1.370(4) . ? N6 C22 1.366(5) . ? N6 C29 1.445(5) . ? N7 C25 1.322(5) . ? N7 N8 1.357(4) . ? N8 C27 1.365(5) . ? N8 C29 1.453(5) . ? O1 C15 1.368(4) . ? O2 C14 1.357(4) . ? O2 C18 1.421(5) . ? O3 C33 1.363(4) . ? O4 C32 1.362(5) . ? O4 C36 1.412(5) . ? C1 C2 1.484(6) . ? C2 C3 1.393(5) . ? C3 C4 1.361(5) . ? C4 C5 1.486(5) . ? C6 C7 1.498(6) . ? C7 C8 1.391(6) . ? C8 C9 1.370(5) . ? C9 C10 1.482(5) . ? C11 C12 1.510(5) . ? C12 C17 1.367(5) . ? C12 C13 1.395(5) . ? C13 C14 1.375(5) . ? C14 C15 1.394(5) . ? C15 C16 1.372(6) . ? C16 C17 1.393(5) . ? C19 C20 1.492(7) . ? C20 C21 1.385(6) . ? C21 C22 1.354(6) . ? C22 C23 1.487(6) . ? C24 C25 1.495(7) . ? C25 C26 1.382(7) . ? C26 C27 1.345(8) . ? C27 C28 1.500(8) . ? C29 C30 1.517(5) . ? C30 C35 1.382(5) . ? C30 C31 1.387(5) . ? C31 C32 1.387(5) . ? C32 C33 1.396(5) . ? C33 C34 1.373(5) . ? C34 C35 1.388(6) . ? O5 C37 1.387(7) . ? O5 C39 1.390(8) . ? C37 C38 1.383(11) . ? C38 C40 1.448(14) . ? C39 C40 1.438(10) . ? B1 F1 1.285(7) . ? B1 F4 1.302(7) . ? B1 F3 1.310(6) . ? B1 F2 1.334(7) . ? 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 N3 Ag1 N5 153.77(12) . . ? N3 Ag1 N7 115.41(11) . . ? N5 Ag1 N7 84.98(11) . . ? N3 Ag1 N1 82.74(10) . . ? N5 Ag1 N1 107.80(11) . . ? N7 Ag1 N1 107.35(10) . . ? C7 N1 N2 105.6(3) . . ? C7 N1 Ag1 126.4(3) . . ? N2 N1 Ag1 117.5(2) . . ? N1 N2 C9 111.7(3) . . ? N1 N2 C11 120.2(3) . . ? C9 N2 C11 127.9(3) . . ? C2 N3 N4 105.5(3) . . ? C2 N3 Ag1 129.9(2) . . ? N4 N3 Ag1 124.3(2) . . ? C4 N4 N3 111.3(3) . . ? C4 N4 C11 126.3(3) . . ? N3 N4 C11 122.1(3) . . ? C20 N5 N6 105.1(3) . . ? C20 N5 Ag1 123.6(3) . . ? N6 N5 Ag1 118.1(2) . . ? N5 N6 C22 111.2(3) . . ? N5 N6 C29 121.4(3) . . ? C22 N6 C29 127.3(3) . . ? C25 N7 N8 105.0(3) . . ? C25 N7 Ag1 131.9(3) . . ? N8 N7 Ag1 122.5(2) . . ? N7 N8 C27 111.5(4) . . ? N7 N8 C29 118.3(3) . . ? C27 N8 C29 129.4(4) . . ? C14 O2 C18 117.9(3) . . ? C32 O4 C36 118.0(3) . . ? N3 C2 C3 110.3(3) . . ? N3 C2 C1 120.5(3) . . ? C3 C2 C1 129.1(4) . . ? C4 C3 C2 106.7(3) . . ? N4 C4 C3 106.2(3) . . ? N4 C4 C5 122.7(3) . . ? C3 C4 C5 131.1(3) . . ? N1 C7 C8 110.3(3) . . ? N1 C7 C6 120.6(4) . . ? C8 C7 C6 129.1(4) . . ? C9 C8 C7 107.1(3) . . ? N2 C9 C8 105.2(3) . . ? N2 C9 C10 123.0(3) . . ? C8 C9 C10 131.8(3) . . ? N2 C11 N4 110.8(3) . . ? N2 C11 C12 112.4(3) . . ? N4 C11 C12 114.4(3) . . ? C17 C12 C13 119.1(3) . . ? C17 C12 C11 124.1(3) . . ? C13 C12 C11 116.5(3) . . ? C14 C13 C12 120.9(3) . . ? O2 C14 C13 125.7(3) . . ? O2 C14 C15 114.6(3) . . ? C13 C14 C15 119.7(3) . . ? O1 C15 C16 119.7(3) . . ? O1 C15 C14 120.9(3) . . ? C16 C15 C14 119.4(3) . . ? C15 C16 C17 120.6(3) . . ? C12 C17 C16 120.3(3) . . ? N5 C20 C21 110.7(4) . . ? N5 C20 C19 120.0(4) . . ? C21 C20 C19 129.3(4) . . ? C22 C21 C20 107.4(4) . . ? C21 C22 N6 105.5(4) . . ? C21 C22 C23 131.9(4) . . ? N6 C22 C23 122.6(4) . . ? N7 C25 C26 110.5(4) . . ? N7 C25 C24 120.1(4) . . ? C26 C25 C24 129.4(5) . . ? C27 C26 C25 107.5(4) . . ? C26 C27 N8 105.5(4) . . ? C26 C27 C28 131.4(5) . . ? N8 C27 C28 123.1(5) . . ? N6 C29 N8 110.7(3) . . ? N6 C29 C30 113.8(3) . . ? N8 C29 C30 111.4(3) . . ? C35 C30 C31 119.2(3) . . ? C35 C30 C29 119.9(3) . . ? C31 C30 C29 120.7(3) . . ? C30 C31 C32 120.7(3) . . ? O4 C32 C31 125.8(3) . . ? O4 C32 C33 114.8(3) . . ? C31 C32 C33 119.4(3) . . ? O3 C33 C34 119.4(3) . . ? O3 C33 C32 120.7(3) . . ? C34 C33 C32 119.8(3) . . ? C33 C34 C35 120.4(4) . . ? C30 C35 C34 120.4(4) . . ? C37 O5 C39 107.7(6) . . ? C38 C37 O5 106.9(7) . . ? C37 C38 C40 109.3(8) . . ? O5 C39 C40 108.2(7) . . ? C39 C40 C38 103.5(7) . . ? F1 B1 F4 123.5(7) . . ? F1 B1 F3 106.4(6) . . ? F4 B1 F3 106.0(5) . . ? F1 B1 F2 99.9(6) . . ? F4 B1 F2 109.2(6) . . ? F3 B1 F2 111.7(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.907 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.072 # Attachment 'gs034a.cif' data_gs034a _database_code_depnum_ccdc_archive 'CCDC 720114' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H52 Ag F3 N8 O8 S' _chemical_formula_weight 981.84 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 12.3951(10) _cell_length_b 12.7251(11) _cell_length_c 16.9436(14) _cell_angle_alpha 77.654(3) _cell_angle_beta 71.812(3) _cell_angle_gamma 62.334(3) _cell_volume 2241.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8480 _exptl_absorpt_correction_T_max 0.8948 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41858 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.11 _reflns_number_total 9732 _reflns_number_gt 6859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0666P)^2^+1.6081P] 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 9732 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.82512(3) 0.68464(3) 0.260173(14) 0.04703(11) Uani 1 1 d . . . N1 N 0.7002(2) 0.7283(3) 0.16044(16) 0.0369(6) Uani 1 1 d . . . N2 N 0.7422(2) 0.7692(2) 0.08003(16) 0.0348(6) Uani 1 1 d . . . N3 N 0.9826(2) 0.6149(2) 0.14194(15) 0.0341(6) Uani 1 1 d . . . N4 N 0.9660(2) 0.6646(2) 0.06421(15) 0.0314(6) Uani 1 1 d . . . N5 N 0.9114(2) 0.7174(2) 0.35527(15) 0.0350(6) Uani 1 1 d . . . N6 N 0.8628(2) 0.6945(2) 0.43816(15) 0.0314(6) Uani 1 1 d . . . N7 N 0.7632(2) 0.5688(2) 0.37618(15) 0.0357(6) Uani 1 1 d . . . N8 N 0.7221(2) 0.6063(2) 0.45445(15) 0.0312(6) Uani 1 1 d . . . O1 O 0.8649(2) 1.1311(2) 0.20960(16) 0.0483(6) Uani 1 1 d . . . H1A H 0.9384 1.1161 0.2074 0.072 Uiso 1 1 calc R . . O2 O 1.0770(2) 0.9884(2) 0.11066(15) 0.0446(6) Uani 1 1 d . . . O3 O 0.4109(2) 1.1529(2) 0.33251(17) 0.0487(6) Uani 1 1 d . . . H3A H 0.3545 1.1479 0.3192 0.073 Uiso 1 1 calc R . . O4 O 0.5887(2) 1.1429(2) 0.38906(15) 0.0419(5) Uani 1 1 d . . . C1 C 0.5140(3) 0.6956(4) 0.2403(2) 0.0488(9) Uani 1 1 d . . . H1B H 0.5582 0.6694 0.2841 0.073 Uiso 1 1 calc R . . H1C H 0.5007 0.6308 0.2301 0.073 Uiso 1 1 calc R . . H1D H 0.4335 0.7626 0.2572 0.073 Uiso 1 1 calc R . . C2 C 0.5904(3) 0.7325(3) 0.1625(2) 0.0388(8) Uani 1 1 d . . . C3 C 0.5616(3) 0.7758(3) 0.0848(2) 0.0453(8) Uani 1 1 d . . . H3B H 0.4894 0.7866 0.0707 0.054 Uiso 1 1 calc R . . C4 C 0.6590(3) 0.7993(3) 0.0336(2) 0.0380(7) Uani 1 1 d . . . C5 C 0.6780(4) 0.8486(4) -0.0556(2) 0.0549(10) Uani 1 1 d . . . H5A H 0.7578 0.8538 -0.0738 0.082 Uiso 1 1 calc R . . H5B H 0.6105 0.9273 -0.0609 0.082 Uiso 1 1 calc R . . H5C H 0.6779 0.7966 -0.0899 0.082 Uiso 1 1 calc R . . C6 C 1.1306(4) 0.4372(4) 0.2034(2) 0.0564(10) Uani 1 1 d . . . H6A H 1.0729 0.4729 0.2542 0.085 Uiso 1 1 calc R . . H6B H 1.2141 0.4271 0.2009 0.085 Uiso 1 1 calc R . . H6C H 1.1327 0.3602 0.2028 0.085 Uiso 1 1 calc R . . C7 C 1.0877(3) 0.5162(3) 0.12992(19) 0.0364(7) Uani 1 1 d . . . C8 C 1.1406(3) 0.5029(3) 0.0444(2) 0.0413(8) Uani 1 1 d . . . H8A H 1.2158 0.4406 0.0198 0.050 Uiso 1 1 calc R . . C9 C 1.0615(3) 0.5983(3) 0.00361(19) 0.0355(7) Uani 1 1 d . . . C10 C 1.0710(4) 0.6309(4) -0.0873(2) 0.0487(9) Uani 1 1 d . . . H10A H 0.9989 0.7047 -0.0955 0.073 Uiso 1 1 calc R . . H10B H 1.0727 0.5681 -0.1122 0.073 Uiso 1 1 calc R . . H10C H 1.1474 0.6413 -0.1134 0.073 Uiso 1 1 calc R . . C11 C 0.8602(3) 0.7797(3) 0.05546(19) 0.0323(7) Uani 1 1 d . . . H11A H 0.8738 0.8070 -0.0046 0.039 Uiso 1 1 calc R . . C12 C 0.8583(3) 0.8719(3) 0.10068(18) 0.0323(7) Uani 1 1 d . . . C13 C 0.9700(3) 0.8840(3) 0.08497(19) 0.0336(7) Uani 1 1 d . . . H13A H 1.0434 0.8332 0.0496 0.040 Uiso 1 1 calc R . . C14 C 0.9734(3) 0.9692(3) 0.12061(19) 0.0339(7) Uani 1 1 d . . . C15 C 0.8644(3) 1.0460(3) 0.17337(19) 0.0355(7) Uani 1 1 d . . . C16 C 0.7542(3) 1.0353(3) 0.1878(2) 0.0396(8) Uani 1 1 d . . . H16A H 0.6807 1.0869 0.2225 0.048 Uiso 1 1 calc R . . C17 C 0.7499(3) 0.9492(3) 0.1516(2) 0.0374(7) Uani 1 1 d . . . H17A H 0.6738 0.9434 0.1616 0.045 Uiso 1 1 calc R . . C18 C 1.1950(3) 0.9021(3) 0.0703(2) 0.0476(9) Uani 1 1 d . . . H18A H 1.2606 0.9254 0.0670 0.071 Uiso 1 1 calc R . . H18B H 1.1932 0.8965 0.0146 0.071 Uiso 1 1 calc R . . H18C H 1.2118 0.8253 0.1019 0.071 Uiso 1 1 calc R . . C19 C 0.9195(4) 0.6371(3) 0.5761(2) 0.0454(9) Uani 1 1 d . . . H19A H 0.8358 0.6402 0.5963 0.068 Uiso 1 1 calc R . . H19B H 0.9254 0.6924 0.6041 0.068 Uiso 1 1 calc R . . H19C H 0.9809 0.5571 0.5873 0.068 Uiso 1 1 calc R . . C20 C 0.9445(3) 0.6703(3) 0.48454(19) 0.0345(7) Uani 1 1 d . . . C21 C 1.0485(3) 0.6778(3) 0.4296(2) 0.0412(8) Uani 1 1 d . . . H21A H 1.1221 0.6659 0.4426 0.049 Uiso 1 1 calc R . . C22 C 1.0249(3) 0.7066(3) 0.3509(2) 0.0363(7) Uani 1 1 d . . . C23 C 1.1074(4) 0.7255(4) 0.2686(2) 0.0531(10) Uani 1 1 d . . . H23A H 1.0646 0.7439 0.2249 0.080 Uiso 1 1 calc R . . H23B H 1.1852 0.6537 0.2576 0.080 Uiso 1 1 calc R . . H23C H 1.1260 0.7910 0.2701 0.080 Uiso 1 1 calc R . . C24 C 0.6173(4) 0.5600(3) 0.6011(2) 0.0504(9) Uani 1 1 d . . . H24A H 0.6257 0.6276 0.6113 0.076 Uiso 1 1 calc R . . H24B H 0.6638 0.4895 0.6333 0.076 Uiso 1 1 calc R . . H24C H 0.5292 0.5755 0.6175 0.076 Uiso 1 1 calc R . . C25 C 0.6683(3) 0.5402(3) 0.51044(19) 0.0362(7) Uani 1 1 d . . . C26 C 0.6774(3) 0.4566(3) 0.4670(2) 0.0414(8) Uani 1 1 d . . . H26A H 0.6494 0.3967 0.4885 0.050 Uiso 1 1 calc R . . C27 C 0.7370(3) 0.4774(3) 0.3839(2) 0.0366(7) Uani 1 1 d . . . C28 C 0.7735(4) 0.4114(4) 0.3091(2) 0.0525(10) Uani 1 1 d . . . H28A H 0.8133 0.4485 0.2605 0.079 Uiso 1 1 calc R . . H28B H 0.6990 0.4139 0.2997 0.079 Uiso 1 1 calc R . . H28C H 0.8317 0.3292 0.3188 0.079 Uiso 1 1 calc R . . C29 C 0.7332(3) 0.7111(3) 0.46681(18) 0.0314(7) Uani 1 1 d . . . H29A H 0.7073 0.7186 0.5276 0.038 Uiso 1 1 calc R . . C30 C 0.6473(3) 0.8258(3) 0.42708(17) 0.0304(7) Uani 1 1 d . . . C31 C 0.6612(3) 0.9292(3) 0.42563(18) 0.0319(7) Uani 1 1 d . . . H31A H 0.7251 0.9251 0.4466 0.038 Uiso 1 1 calc R . . C32 C 0.5819(3) 1.0374(3) 0.39363(18) 0.0323(7) Uani 1 1 d . . . C33 C 0.4871(3) 1.0433(3) 0.3626(2) 0.0340(7) Uani 1 1 d . . . C34 C 0.4739(3) 0.9417(3) 0.3636(2) 0.0389(8) Uani 1 1 d . . . H34A H 0.4105 0.9456 0.3422 0.047 Uiso 1 1 calc R . . C35 C 0.5542(3) 0.8325(3) 0.3962(2) 0.0352(7) Uani 1 1 d . . . H35A H 0.5442 0.7633 0.3969 0.042 Uiso 1 1 calc R . . C36 C 0.6907(4) 1.1383(4) 0.4136(3) 0.0521(9) Uani 1 1 d . . . H36A H 0.6858 1.2179 0.4075 0.078 Uiso 1 1 calc R . . H36B H 0.7694 1.0872 0.3786 0.078 Uiso 1 1 calc R . . H36C H 0.6864 1.1067 0.4713 0.078 Uiso 1 1 calc R . . C37 C 0.0806(4) 0.0447(5) 0.3748(3) 0.0697(13) Uani 1 1 d . . . S1 S 0.16483(8) 0.07929(8) 0.27159(5) 0.0408(2) Uani 1 1 d . . . O5 O 0.2500(3) -0.0343(3) 0.2417(2) 0.0718(9) Uani 1 1 d . . . O6 O 0.2222(3) 0.1455(3) 0.28764(18) 0.0584(7) Uani 1 1 d . . . O7 O 0.0666(2) 0.1511(2) 0.22929(16) 0.0512(6) Uani 1 1 d . . . F1 F 0.0229(3) -0.0187(3) 0.3713(2) 0.1018(10) Uani 1 1 d . . . F2 F -0.0091(3) 0.1433(4) 0.4100(2) 0.1100(11) Uani 1 1 d . . . F3 F 0.1564(4) -0.0152(5) 0.4232(2) 0.1491(19) Uani 1 1 d . . . O8 O 0.5301(9) 0.5841(13) 0.8293(7) 0.315(7) Uani 1 1 d . . . C38 C 0.4127(8) 0.5869(12) 0.8653(9) 0.238(8) Uani 1 1 d . . . H38A H 0.4215 0.5052 0.8824 0.286 Uiso 1 1 calc R . . H38B H 0.3625 0.6207 0.8239 0.286 Uiso 1 1 calc R . . C39 C 0.3462(7) 0.6567(7) 0.9378(6) 0.134(3) Uani 1 1 d . . . H39A H 0.2703 0.7254 0.9268 0.161 Uiso 1 1 calc R . . H39B H 0.3206 0.6079 0.9861 0.161 Uiso 1 1 calc R . . C40 C 0.4217(5) 0.6946(6) 0.9546(4) 0.0882(17) Uani 1 1 d . . . H40A H 0.3769 0.7797 0.9632 0.106 Uiso 1 1 calc R . . H40B H 0.4496 0.6506 1.0049 0.106 Uiso 1 1 calc R . . C41 C 0.5176(8) 0.6747(9) 0.8898(5) 0.144(3) Uani 1 1 d . . . H41A H 0.5948 0.6413 0.9090 0.173 Uiso 1 1 calc R . . H41B H 0.5095 0.7506 0.8575 0.173 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 Ag1 0.05597(19) 0.0614(2) 0.02245(13) -0.00183(11) -0.00719(11) -0.02636(15) N1 0.0388(15) 0.0435(17) 0.0327(14) -0.0001(12) -0.0082(11) -0.0228(13) N2 0.0373(14) 0.0428(16) 0.0307(13) 0.0004(12) -0.0107(11) -0.0223(13) N3 0.0390(15) 0.0389(16) 0.0232(12) 0.0003(11) -0.0082(11) -0.0166(13) N4 0.0367(14) 0.0339(15) 0.0228(12) -0.0017(10) -0.0069(10) -0.0151(12) N5 0.0363(14) 0.0400(16) 0.0249(12) -0.0009(11) -0.0075(11) -0.0140(12) N6 0.0326(13) 0.0343(15) 0.0235(12) -0.0028(10) -0.0084(10) -0.0102(11) N7 0.0421(15) 0.0348(15) 0.0251(12) -0.0043(11) -0.0051(11) -0.0134(13) N8 0.0366(14) 0.0297(14) 0.0233(12) -0.0033(10) -0.0053(10) -0.0118(11) O1 0.0442(14) 0.0520(16) 0.0544(15) -0.0201(12) -0.0065(11) -0.0222(12) O2 0.0330(12) 0.0502(15) 0.0558(15) -0.0170(12) -0.0070(11) -0.0191(11) O3 0.0459(14) 0.0347(13) 0.0682(17) 0.0020(12) -0.0296(12) -0.0122(11) O4 0.0426(13) 0.0342(13) 0.0543(14) -0.0033(11) -0.0161(11) -0.0185(11) C1 0.042(2) 0.055(2) 0.053(2) -0.0074(18) -0.0022(16) -0.0278(18) C2 0.0334(17) 0.0360(19) 0.0469(19) -0.0076(15) -0.0081(14) -0.0142(15) C3 0.0355(18) 0.049(2) 0.056(2) -0.0049(17) -0.0187(16) -0.0169(16) C4 0.0393(18) 0.0373(19) 0.0406(18) -0.0038(14) -0.0185(14) -0.0134(15) C5 0.061(2) 0.066(3) 0.046(2) 0.0086(19) -0.0296(19) -0.030(2) C6 0.059(2) 0.048(2) 0.041(2) 0.0053(17) -0.0176(18) -0.0069(19) C7 0.0392(18) 0.0360(18) 0.0327(16) 0.0007(14) -0.0095(13) -0.0161(16) C8 0.0386(18) 0.040(2) 0.0358(17) -0.0051(15) -0.0030(14) -0.0119(15) C9 0.0420(18) 0.0408(19) 0.0275(15) -0.0069(13) -0.0024(13) -0.0229(16) C10 0.055(2) 0.061(2) 0.0264(16) -0.0064(16) -0.0033(15) -0.0246(19) C11 0.0372(17) 0.0345(17) 0.0281(15) 0.0029(13) -0.0116(13) -0.0177(14) C12 0.0345(16) 0.0330(17) 0.0293(15) 0.0022(13) -0.0101(12) -0.0150(14) C13 0.0308(16) 0.0344(18) 0.0311(15) -0.0033(13) -0.0064(12) -0.0109(14) C14 0.0316(16) 0.0386(18) 0.0344(16) 0.0002(14) -0.0116(13) -0.0165(14) C15 0.0380(18) 0.0359(18) 0.0322(16) -0.0033(14) -0.0084(13) -0.0154(15) C16 0.0353(17) 0.043(2) 0.0373(17) -0.0088(15) -0.0017(14) -0.0165(15) C17 0.0341(17) 0.042(2) 0.0383(17) -0.0026(15) -0.0073(13) -0.0197(15) C18 0.0308(17) 0.050(2) 0.062(2) -0.0081(18) -0.0074(16) -0.0177(16) C19 0.056(2) 0.045(2) 0.0347(17) -0.0025(15) -0.0200(16) -0.0157(18) C20 0.0417(18) 0.0276(17) 0.0335(16) -0.0045(13) -0.0163(14) -0.0091(14) C21 0.0368(18) 0.041(2) 0.0481(19) -0.0036(16) -0.0195(15) -0.0132(16) C22 0.0355(17) 0.0326(18) 0.0389(17) -0.0044(14) -0.0091(14) -0.0125(14) C23 0.044(2) 0.067(3) 0.046(2) 0.0010(19) -0.0057(16) -0.028(2) C24 0.062(2) 0.044(2) 0.0319(17) 0.0004(15) 0.0024(16) -0.0226(19) C25 0.0373(17) 0.0330(18) 0.0315(16) 0.0034(13) -0.0081(13) -0.0122(14) C26 0.0453(19) 0.0371(19) 0.0422(18) -0.0002(15) -0.0092(15) -0.0202(16) C27 0.0406(18) 0.0331(18) 0.0360(17) -0.0045(14) -0.0097(14) -0.0148(15) C28 0.071(3) 0.046(2) 0.045(2) -0.0127(17) -0.0093(18) -0.028(2) C29 0.0342(16) 0.0350(17) 0.0212(13) -0.0049(12) -0.0050(12) -0.0118(14) C30 0.0308(15) 0.0310(17) 0.0249(14) -0.0073(12) -0.0041(12) -0.0092(13) C31 0.0306(16) 0.0357(18) 0.0305(15) -0.0058(13) -0.0078(12) -0.0136(14) C32 0.0320(16) 0.0323(17) 0.0301(15) -0.0076(13) 0.0000(12) -0.0145(14) C33 0.0291(16) 0.0314(17) 0.0373(16) -0.0057(13) -0.0075(13) -0.0086(14) C34 0.0347(17) 0.0390(19) 0.0465(19) -0.0068(15) -0.0148(14) -0.0143(15) C35 0.0348(17) 0.0311(17) 0.0401(17) -0.0090(14) -0.0074(14) -0.0132(14) C36 0.056(2) 0.046(2) 0.066(2) -0.0021(19) -0.0195(19) -0.0309(19) C37 0.063(3) 0.089(4) 0.061(3) 0.014(3) -0.023(2) -0.039(3) S1 0.0411(5) 0.0397(5) 0.0445(5) -0.0008(4) -0.0195(4) -0.0151(4) O5 0.0616(18) 0.0471(17) 0.090(2) -0.0194(16) -0.0193(16) -0.0034(14) O6 0.0579(16) 0.0615(18) 0.0730(19) 0.0016(14) -0.0347(14) -0.0309(14) O7 0.0557(15) 0.0499(16) 0.0561(15) 0.0009(12) -0.0313(13) -0.0203(13) F1 0.090(2) 0.097(2) 0.123(3) 0.022(2) -0.0187(19) -0.0615(19) F2 0.102(2) 0.139(3) 0.075(2) -0.036(2) 0.0151(18) -0.052(2) F3 0.111(3) 0.251(5) 0.083(2) 0.089(3) -0.060(2) -0.095(3) O8 0.199(9) 0.54(2) 0.246(11) -0.195(12) 0.061(8) -0.201(11) C38 0.100(6) 0.310(15) 0.344(17) -0.250(14) -0.018(8) -0.051(8) C39 0.121(6) 0.128(6) 0.179(8) -0.047(6) -0.039(6) -0.059(5) C40 0.063(3) 0.109(5) 0.104(4) -0.049(4) -0.009(3) -0.037(3) C41 0.139(7) 0.211(10) 0.118(6) -0.056(6) -0.002(5) -0.104(7) _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 N3 2.307(2) . ? Ag1 N7 2.344(3) . ? Ag1 N5 2.385(3) . ? Ag1 N1 2.449(3) . ? N1 C2 1.326(4) . ? N1 N2 1.380(4) . ? N2 C4 1.357(4) . ? N2 C11 1.452(4) . ? N3 C7 1.319(4) . ? N3 N4 1.367(3) . ? N4 C9 1.361(4) . ? N4 C11 1.460(4) . ? N5 C22 1.328(4) . ? N5 N6 1.371(3) . ? N6 C20 1.356(4) . ? N6 C29 1.451(4) . ? N7 C27 1.318(4) . ? N7 N8 1.367(3) . ? N8 C25 1.356(4) . ? N8 C29 1.465(4) . ? O1 C15 1.357(4) . ? O2 C14 1.370(4) . ? O2 C18 1.420(4) . ? O3 C33 1.368(4) . ? O4 C32 1.368(4) . ? O4 C36 1.423(4) . ? C1 C2 1.491(5) . ? C2 C3 1.401(5) . ? C3 C4 1.367(5) . ? C4 C5 1.497(5) . ? C6 C7 1.492(5) . ? C7 C8 1.403(4) . ? C8 C9 1.367(5) . ? C9 C10 1.489(4) . ? C11 C12 1.521(4) . ? C12 C17 1.388(4) . ? C12 C13 1.401(4) . ? C13 C14 1.371(5) . ? C14 C15 1.405(4) . ? C15 C16 1.376(5) . ? C16 C17 1.394(5) . ? C19 C20 1.490(4) . ? C20 C21 1.366(5) . ? C21 C22 1.391(5) . ? C22 C23 1.497(5) . ? C24 C25 1.495(4) . ? C25 C26 1.362(5) . ? C26 C27 1.404(5) . ? C27 C28 1.504(5) . ? C29 C30 1.517(4) . ? C30 C35 1.371(4) . ? C30 C31 1.399(4) . ? C31 C32 1.383(4) . ? C32 C33 1.396(4) . ? C33 C34 1.372(5) . ? C34 C35 1.400(5) . ? C37 F3 1.298(5) . ? C37 F1 1.322(6) . ? C37 F2 1.333(6) . ? C37 S1 1.817(5) . ? S1 O5 1.421(3) . ? S1 O7 1.436(2) . ? S1 O6 1.437(3) . ? O8 C38 1.378(11) . ? O8 C41 1.626(11) . ? C38 C39 1.460(11) . ? C39 C40 1.354(8) . ? C40 C41 1.306(8) . ? 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 N3 Ag1 N7 126.43(9) . . ? N3 Ag1 N5 108.49(9) . . ? N7 Ag1 N5 81.89(9) . . ? N3 Ag1 N1 79.46(9) . . ? N7 Ag1 N1 109.00(9) . . ? N5 Ag1 N1 159.56(9) . . ? C2 N1 N2 104.9(3) . . ? C2 N1 Ag1 137.0(2) . . ? N2 N1 Ag1 117.88(18) . . ? C4 N2 N1 111.6(3) . . ? C4 N2 C11 128.1(3) . . ? N1 N2 C11 120.2(2) . . ? C7 N3 N4 105.7(2) . . ? C7 N3 Ag1 131.8(2) . . ? N4 N3 Ag1 121.30(19) . . ? C9 N4 N3 111.5(3) . . ? C9 N4 C11 128.9(3) . . ? N3 N4 C11 119.5(2) . . ? C22 N5 N6 104.9(2) . . ? C22 N5 Ag1 133.0(2) . . ? N6 N5 Ag1 115.89(19) . . ? C20 N6 N5 111.7(2) . . ? C20 N6 C29 128.2(2) . . ? N5 N6 C29 119.6(2) . . ? C27 N7 N8 105.6(2) . . ? C27 N7 Ag1 132.8(2) . . ? N8 N7 Ag1 120.5(2) . . ? C25 N8 N7 111.5(3) . . ? C25 N8 C29 129.0(2) . . ? N7 N8 C29 119.4(2) . . ? C14 O2 C18 117.2(3) . . ? C32 O4 C36 116.9(3) . . ? N1 C2 C3 110.7(3) . . ? N1 C2 C1 121.2(3) . . ? C3 C2 C1 128.1(3) . . ? C4 C3 C2 106.7(3) . . ? N2 C4 C3 106.1(3) . . ? N2 C4 C5 123.7(3) . . ? C3 C4 C5 130.2(3) . . ? N3 C7 C8 110.3(3) . . ? N3 C7 C6 119.4(3) . . ? C8 C7 C6 130.3(3) . . ? C9 C8 C7 106.7(3) . . ? N4 C9 C8 105.8(3) . . ? N4 C9 C10 124.0(3) . . ? C8 C9 C10 130.2(3) . . ? N2 C11 N4 111.6(3) . . ? N2 C11 C12 113.2(3) . . ? N4 C11 C12 111.0(2) . . ? C17 C12 C13 119.1(3) . . ? C17 C12 C11 123.1(3) . . ? C13 C12 C11 117.6(3) . . ? C14 C13 C12 120.7(3) . . ? O2 C14 C13 125.9(3) . . ? O2 C14 C15 113.8(3) . . ? C13 C14 C15 120.3(3) . . ? O1 C15 C16 119.4(3) . . ? O1 C15 C14 121.7(3) . . ? C16 C15 C14 119.0(3) . . ? C15 C16 C17 121.0(3) . . ? C12 C17 C16 119.9(3) . . ? N6 C20 C21 105.8(3) . . ? N6 C20 C19 123.7(3) . . ? C21 C20 C19 130.4(3) . . ? C20 C21 C22 106.9(3) . . ? N5 C22 C21 110.7(3) . . ? N5 C22 C23 120.3(3) . . ? C21 C22 C23 129.0(3) . . ? N8 C25 C26 106.0(3) . . ? N8 C25 C24 123.0(3) . . ? C26 C25 C24 130.9(3) . . ? C25 C26 C27 106.6(3) . . ? N7 C27 C26 110.3(3) . . ? N7 C27 C28 119.8(3) . . ? C26 C27 C28 130.0(3) . . ? N6 C29 N8 110.8(2) . . ? N6 C29 C30 111.2(3) . . ? N8 C29 C30 113.0(2) . . ? C35 C30 C31 119.4(3) . . ? C35 C30 C29 122.6(3) . . ? C31 C30 C29 118.0(3) . . ? C32 C31 C30 120.5(3) . . ? O4 C32 C31 124.8(3) . . ? O4 C32 C33 115.6(3) . . ? C31 C32 C33 119.6(3) . . ? O3 C33 C34 123.2(3) . . ? O3 C33 C32 116.9(3) . . ? C34 C33 C32 119.9(3) . . ? C33 C34 C35 120.3(3) . . ? C30 C35 C34 120.2(3) . . ? F3 C37 F1 108.3(5) . . ? F3 C37 F2 108.8(5) . . ? F1 C37 F2 106.0(4) . . ? F3 C37 S1 111.1(3) . . ? F1 C37 S1 111.2(4) . . ? F2 C37 S1 111.3(4) . . ? O5 S1 O7 116.12(18) . . ? O5 S1 O6 115.11(18) . . ? O7 S1 O6 112.93(16) . . ? O5 S1 C37 103.8(2) . . ? O7 S1 C37 103.31(19) . . ? O6 S1 C37 103.4(2) . . ? C38 O8 C41 95.8(7) . . ? O8 C38 C39 112.7(8) . . ? C40 C39 C38 109.9(7) . . ? C41 C40 C39 106.1(6) . . ? C40 C41 O8 113.3(7) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.658 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.072