# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Dobrzanska, Liliana' _publ_contact_author_name 'Dobrzanska, Liliana' _publ_contact_author_email liliana.dobrzanska@chem.kuleuven.be _publ_section_title ; Anion directed supramolecular architectures of silver(I) complexes with 1,3-bis(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene and a reversible, solvent-induced structural change during a single-crystal-to-single- crystal transformation ; # Attachment '- Dobrzanska_CIF 1-5.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 786858' #TrackingRef '- Dobrzanska_CIF 1-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Ag2 F12 N10 Sb2' _chemical_formula_weight 1330.09 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' 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6798(7) _cell_length_b 9.9988(8) _cell_length_c 13.7746(10) _cell_angle_alpha 99.5060(10) _cell_angle_beta 101.9620(10) _cell_angle_gamma 101.4790(10) _cell_volume 1119.24(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9393 _cell_measurement_theta_min 2.347 _cell_measurement_theta_max 28.21 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3956 _exptl_absorpt_correction_T_max 0.7826 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13004 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5162 _reflns_number_gt 5041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material ? _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^)+(0.0252P)^2^+1.6652P] 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 5162 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.003 _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 0.50528(2) 0.95374(2) 0.710762(15) 0.01783(6) Uani 1 1 d . . . N1 N 0.7006(3) 0.8573(2) 0.73394(17) 0.0181(4) Uani 1 1 d . . . C2 C 0.7375(3) 0.7838(3) 0.8031(2) 0.0162(5) Uani 1 1 d . . . H2 H 0.6706 0.7563 0.8464 0.019 Uiso 1 1 calc R . . N3 N 0.8817(3) 0.7529(2) 0.80428(16) 0.0152(4) Uani 1 1 d . . . C4 C 0.9411(3) 0.8100(3) 0.7311(2) 0.0189(5) Uani 1 1 d . . . H4 H 1.0407 0.8055 0.7140 0.023 Uiso 1 1 calc R . . C5 C 0.8286(3) 0.8739(3) 0.6883(2) 0.0187(5) Uani 1 1 d . . . H5 H 0.8367 0.9226 0.6352 0.022 Uiso 1 1 calc R . . C6 C 0.9618(3) 0.6672(3) 0.8665(2) 0.0178(5) Uani 1 1 d . . . H6A H 1.0755 0.7191 0.8989 0.021 Uiso 1 1 calc R . . H6B H 0.9643 0.5802 0.8211 0.021 Uiso 1 1 calc R . . C7 C 0.8800(3) 0.6287(3) 0.94853(19) 0.0148(5) Uani 1 1 d . . . C8 C 0.7585(3) 0.5046(3) 0.92677(19) 0.0159(5) Uani 1 1 d . . . C9 C 0.6949(3) 0.4637(3) 1.0049(2) 0.0169(5) Uani 1 1 d . . . H9 H 0.6083 0.3825 0.9895 0.020 Uiso 1 1 calc R . . C10 C 0.7544(3) 0.5383(3) 1.10489(19) 0.0154(5) Uani 1 1 d . . . C11 C 0.8761(3) 0.6617(3) 1.12655(19) 0.0141(5) Uani 1 1 d . . . C12 C 0.9336(3) 0.7109(3) 1.04776(19) 0.0147(5) Uani 1 1 d . . . C13 C 1.0519(3) 0.8519(3) 1.0699(2) 0.0211(5) Uani 1 1 d . . . H13A H 1.0488 0.8857 1.0069 0.032 Uiso 1 1 calc R . . H13C H 1.1618 0.8430 1.0982 0.032 Uiso 1 1 calc R . . H13B H 1.0218 0.9183 1.1190 0.032 Uiso 1 1 calc R . . C14 C 0.6958(3) 0.4130(3) 0.8211(2) 0.0211(5) Uani 1 1 d . . . H14C H 0.6009 0.3398 0.8194 0.032 Uiso 1 1 calc R . . H14B H 0.7809 0.3698 0.8032 0.032 Uiso 1 1 calc R . . H14A H 0.6648 0.4699 0.7723 0.032 Uiso 1 1 calc R . . C15 C 0.6882(4) 0.4828(3) 1.1878(2) 0.0215(5) Uani 1 1 d . . . H15A H 0.7689 0.4443 1.2277 0.032 Uiso 1 1 calc R . . H15C H 0.5885 0.4093 1.1570 0.032 Uiso 1 1 calc R . . H15B H 0.6642 0.5590 1.2322 0.032 Uiso 1 1 calc R . . C16 C 0.9560(3) 0.7353(3) 1.23611(19) 0.0167(5) Uani 1 1 d . . . H16A H 0.9787 0.6643 1.2757 0.020 Uiso 1 1 calc R . . H16B H 1.0615 0.7977 1.2388 0.020 Uiso 1 1 calc R . . N17 N 0.8597(3) 0.8186(2) 1.28533(16) 0.0143(4) Uani 1 1 d . . . C18 C 0.7433(3) 0.8748(3) 1.2405(2) 0.0170(5) Uani 1 1 d . . . H18 H 0.7039 0.8624 1.1691 0.020 Uiso 1 1 calc R . . N19 N 0.6905(3) 0.9502(2) 1.30978(17) 0.0177(4) Uani 1 1 d . . . C20 C 0.7796(3) 0.9410(3) 1.4029(2) 0.0204(5) Uani 1 1 d . . . H20 H 0.7689 0.9845 1.4671 0.025 Uiso 1 1 calc R . . C21 C 0.8845(3) 0.8605(3) 1.38870(19) 0.0187(5) Uani 1 1 d . . . H21 H 0.9601 0.8375 1.4399 0.022 Uiso 1 1 calc R . . Sb22 Sb 0.5000 1.0000 1.0000 0.01370(6) Uani 1 2 d S . . F23 F 0.6823(2) 0.9258(2) 1.00470(14) 0.0312(4) Uani 1 1 d . . . F24 F 0.6168(2) 1.14135(18) 1.11342(13) 0.0331(4) Uani 1 1 d . . . F25 F 0.56552(19) 1.11448(16) 0.91332(12) 0.0206(3) Uani 1 1 d . . . Sb26 Sb 1.0000 0.5000 0.5000 0.01769(7) Uani 1 2 d S . . F27 F 1.1894(2) 0.4449(2) 0.55093(14) 0.0313(4) Uani 1 1 d . . . F28 F 0.9413(2) 0.49606(18) 0.62373(12) 0.0267(4) Uani 1 1 d . . . F29 F 0.8878(2) 0.31213(18) 0.45129(14) 0.0301(4) Uani 1 1 d . . . N30 N 0.6612(3) 0.1341(3) 0.59478(19) 0.0265(5) Uani 1 1 d . . . C31 C 0.6059(3) 0.2196(3) 0.5670(2) 0.0219(6) Uani 1 1 d . . . C32 C 0.5347(4) 0.3297(3) 0.5328(3) 0.0307(7) Uani 1 1 d . . . H32A H 0.6133 0.4202 0.5598 0.046 Uiso 1 1 calc R . . H32B H 0.4367 0.3317 0.5573 0.046 Uiso 1 1 calc R . . H32C H 0.5062 0.3110 0.4584 0.046 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 0.01977(11) 0.02063(11) 0.01641(10) 0.00450(7) 0.00454(7) 0.01201(8) N1 0.0204(11) 0.0183(11) 0.0175(11) 0.0047(9) 0.0042(9) 0.0090(9) C2 0.0164(12) 0.0159(12) 0.0191(12) 0.0046(10) 0.0070(10) 0.0069(10) N3 0.0163(10) 0.0157(10) 0.0163(10) 0.0040(8) 0.0054(8) 0.0081(8) C4 0.0205(13) 0.0213(13) 0.0182(12) 0.0056(10) 0.0088(10) 0.0075(10) C5 0.0230(13) 0.0192(13) 0.0166(12) 0.0048(10) 0.0079(10) 0.0076(10) C6 0.0179(12) 0.0224(13) 0.0192(12) 0.0087(10) 0.0072(10) 0.0128(10) C7 0.0163(12) 0.0168(12) 0.0156(12) 0.0063(9) 0.0050(9) 0.0101(10) C8 0.0173(12) 0.0155(12) 0.0161(12) 0.0012(9) 0.0034(10) 0.0093(10) C9 0.0167(12) 0.0133(11) 0.0214(13) 0.0038(10) 0.0045(10) 0.0056(9) C10 0.0165(12) 0.0165(12) 0.0165(12) 0.0045(9) 0.0056(10) 0.0091(10) C11 0.0149(12) 0.0146(11) 0.0143(11) 0.0027(9) 0.0012(9) 0.0094(9) C12 0.0130(11) 0.0144(11) 0.0188(12) 0.0047(9) 0.0029(9) 0.0085(9) C13 0.0199(13) 0.0173(13) 0.0267(14) 0.0060(11) 0.0062(11) 0.0046(10) C14 0.0232(14) 0.0215(13) 0.0172(13) -0.0004(10) 0.0019(10) 0.0095(11) C15 0.0237(14) 0.0211(13) 0.0234(14) 0.0070(11) 0.0109(11) 0.0067(11) C16 0.0157(12) 0.0186(12) 0.0171(12) 0.0017(10) 0.0029(10) 0.0100(10) N17 0.0151(10) 0.0152(10) 0.0127(10) 0.0019(8) 0.0017(8) 0.0067(8) C18 0.0177(12) 0.0199(12) 0.0141(12) 0.0046(10) 0.0014(10) 0.0078(10) N19 0.0185(11) 0.0207(11) 0.0159(10) 0.0037(9) 0.0044(9) 0.0092(9) C20 0.0238(14) 0.0251(14) 0.0144(12) 0.0042(10) 0.0046(10) 0.0106(11) C21 0.0228(13) 0.0225(13) 0.0119(12) 0.0038(10) 0.0016(10) 0.0104(11) Sb22 0.01522(12) 0.01392(11) 0.01329(11) 0.00396(8) 0.00381(9) 0.00547(9) F23 0.0293(9) 0.0468(11) 0.0355(10) 0.0246(9) 0.0177(8) 0.0272(9) F24 0.0490(12) 0.0213(9) 0.0190(8) 0.0011(7) 0.0004(8) -0.0036(8) F25 0.0228(8) 0.0223(8) 0.0196(8) 0.0103(6) 0.0075(6) 0.0050(6) Sb26 0.02449(13) 0.01762(12) 0.01503(12) 0.00699(9) 0.00638(10) 0.00998(10) F27 0.0315(10) 0.0395(10) 0.0313(10) 0.0152(8) 0.0076(8) 0.0220(8) F28 0.0375(10) 0.0312(9) 0.0180(8) 0.0102(7) 0.0123(7) 0.0134(8) F29 0.0398(10) 0.0208(8) 0.0302(9) 0.0036(7) 0.0135(8) 0.0049(8) N30 0.0286(13) 0.0270(13) 0.0263(13) 0.0058(10) 0.0094(11) 0.0095(11) C31 0.0206(13) 0.0239(14) 0.0197(13) 0.0002(11) 0.0071(11) 0.0037(11) C32 0.0307(16) 0.0308(16) 0.0299(16) 0.0057(13) 0.0024(13) 0.0118(13) _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 2.105(2) . ? Ag1 N19 2.105(2) 2_677 ? N1 C2 1.322(3) . ? N1 C5 1.381(3) . ? C2 N3 1.345(3) . ? C2 H2 0.9500 . ? N3 C4 1.377(3) . ? N3 C6 1.478(3) . ? C4 C5 1.358(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.516(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.402(4) . ? C7 C12 1.405(4) . ? C8 C9 1.390(4) . ? C8 C14 1.512(4) . ? C9 C10 1.390(4) . ? C9 H9 0.9500 . ? C10 C11 1.399(4) . ? C10 C15 1.515(4) . ? C11 C12 1.404(4) . ? C11 C16 1.515(3) . ? C12 C13 1.512(4) . ? C13 H13A 0.9800 . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C15 H15A 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C16 N17 1.476(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.342(3) . ? N17 C21 1.375(3) . ? C18 N19 1.330(3) . ? C18 H18 0.9500 . ? N19 C20 1.381(3) . ? N19 Ag1 2.105(2) 2_677 ? C20 C21 1.352(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? Sb22 F23 1.8711(17) 2_677 ? Sb22 F23 1.8711(17) . ? Sb22 F24 1.8734(17) . ? Sb22 F24 1.8734(17) 2_677 ? Sb22 F25 1.8796(15) . ? Sb22 F25 1.8796(15) 2_677 ? Sb26 F27 1.8727(17) . ? Sb26 F27 1.8727(17) 2_766 ? Sb26 F29 1.8741(17) 2_766 ? Sb26 F29 1.8741(17) . ? Sb26 F28 1.8815(16) . ? Sb26 F28 1.8815(16) 2_766 ? N30 C31 1.141(4) . ? C31 C32 1.462(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 N19 178.96(9) . 2_677 ? C2 N1 C5 105.7(2) . . ? C2 N1 Ag1 127.64(19) . . ? C5 N1 Ag1 126.21(18) . . ? N1 C2 N3 111.4(2) . . ? N1 C2 H2 124.3 . . ? N3 C2 H2 124.3 . . ? C2 N3 C4 107.2(2) . . ? C2 N3 C6 128.1(2) . . ? C4 N3 C6 124.6(2) . . ? C5 C4 N3 106.2(2) . . ? C5 C4 H4 126.9 . . ? N3 C4 H4 126.9 . . ? C4 C5 N1 109.5(2) . . ? C4 C5 H5 125.2 . . ? N1 C5 H5 125.2 . . ? N3 C6 C7 114.1(2) . . ? N3 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? N3 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C12 120.0(2) . . ? C8 C7 C6 119.5(2) . . ? C12 C7 C6 120.3(2) . . ? C9 C8 C7 119.0(2) . . ? C9 C8 C14 118.9(2) . . ? C7 C8 C14 122.0(2) . . ? C10 C9 C8 121.8(2) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 119.0(2) . . ? C9 C10 C15 119.3(2) . . ? C11 C10 C15 121.7(2) . . ? C10 C11 C12 120.2(2) . . ? C10 C11 C16 119.7(2) . . ? C12 C11 C16 119.9(2) . . ? C11 C12 C7 119.6(2) . . ? C11 C12 C13 120.0(2) . . ? C7 C12 C13 120.4(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C8 C14 H14C 109.5 . . ? C8 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C8 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? N17 C16 C11 114.8(2) . . ? N17 C16 H16A 108.6 . . ? C11 C16 H16A 108.6 . . ? N17 C16 H16B 108.6 . . ? C11 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? C18 N17 C21 107.8(2) . . ? C18 N17 C16 127.7(2) . . ? C21 N17 C16 124.3(2) . . ? N19 C18 N17 110.6(2) . . ? N19 C18 H18 124.7 . . ? N17 C18 H18 124.7 . . ? C18 N19 C20 105.8(2) . . ? C18 N19 Ag1 129.15(18) . 2_677 ? C20 N19 Ag1 124.69(18) . 2_677 ? C21 C20 N19 109.5(2) . . ? C21 C20 H20 125.2 . . ? N19 C20 H20 125.2 . . ? C20 C21 N17 106.2(2) . . ? C20 C21 H21 126.9 . . ? N17 C21 H21 126.9 . . ? F23 Sb22 F23 180.000(1) 2_677 . ? F23 Sb22 F24 90.18(9) 2_677 . ? F23 Sb22 F24 89.82(9) . . ? F23 Sb22 F24 89.82(9) 2_677 2_677 ? F23 Sb22 F24 90.18(9) . 2_677 ? F24 Sb22 F24 180.000(1) . 2_677 ? F23 Sb22 F25 88.73(7) 2_677 . ? F23 Sb22 F25 91.27(7) . . ? F24 Sb22 F25 90.19(8) . . ? F24 Sb22 F25 89.81(7) 2_677 . ? F23 Sb22 F25 91.27(7) 2_677 2_677 ? F23 Sb22 F25 88.73(7) . 2_677 ? F24 Sb22 F25 89.81(7) . 2_677 ? F24 Sb22 F25 90.19(8) 2_677 2_677 ? F25 Sb22 F25 180.000(1) . 2_677 ? F27 Sb26 F27 180.000(1) . 2_766 ? F27 Sb26 F29 89.94(9) . 2_766 ? F27 Sb26 F29 90.06(9) 2_766 2_766 ? F27 Sb26 F29 90.06(9) . . ? F27 Sb26 F29 89.94(9) 2_766 . ? F29 Sb26 F29 180.0 2_766 . ? F27 Sb26 F28 90.16(8) . . ? F27 Sb26 F28 89.84(8) 2_766 . ? F29 Sb26 F28 90.43(8) 2_766 . ? F29 Sb26 F28 89.57(8) . . ? F27 Sb26 F28 89.84(8) . 2_766 ? F27 Sb26 F28 90.16(8) 2_766 2_766 ? F29 Sb26 F28 89.57(8) 2_766 2_766 ? F29 Sb26 F28 90.43(8) . 2_766 ? F28 Sb26 F28 180.0 . 2_766 ? N30 C31 C32 179.2(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 C5 N1 C2 N3 0.1(3) . . . . ? Ag1 N1 C2 N3 -172.12(17) . . . . ? N1 C2 N3 C4 -0.1(3) . . . . ? N1 C2 N3 C6 -176.7(2) . . . . ? C2 N3 C4 C5 0.1(3) . . . . ? C6 N3 C4 C5 176.8(2) . . . . ? N3 C4 C5 N1 0.0(3) . . . . ? C2 N1 C5 C4 -0.1(3) . . . . ? Ag1 N1 C5 C4 172.30(18) . . . . ? C2 N3 C6 C7 -9.6(4) . . . . ? C4 N3 C6 C7 174.4(2) . . . . ? N3 C6 C7 C8 90.4(3) . . . . ? N3 C6 C7 C12 -94.4(3) . . . . ? C12 C7 C8 C9 -1.1(4) . . . . ? C6 C7 C8 C9 174.1(2) . . . . ? C12 C7 C8 C14 179.5(2) . . . . ? C6 C7 C8 C14 -5.2(4) . . . . ? C7 C8 C9 C10 -3.5(4) . . . . ? C14 C8 C9 C10 175.8(2) . . . . ? C8 C9 C10 C11 3.3(4) . . . . ? C8 C9 C10 C15 -175.7(2) . . . . ? C9 C10 C11 C12 1.7(4) . . . . ? C15 C10 C11 C12 -179.4(2) . . . . ? C9 C10 C11 C16 -172.9(2) . . . . ? C15 C10 C11 C16 6.0(4) . . . . ? C10 C11 C12 C7 -6.3(4) . . . . ? C16 C11 C12 C7 168.3(2) . . . . ? C10 C11 C12 C13 173.4(2) . . . . ? C16 C11 C12 C13 -11.9(3) . . . . ? C8 C7 C12 C11 6.0(4) . . . . ? C6 C7 C12 C11 -169.2(2) . . . . ? C8 C7 C12 C13 -173.7(2) . . . . ? C6 C7 C12 C13 11.1(3) . . . . ? C10 C11 C16 N17 -78.4(3) . . . . ? C12 C11 C16 N17 106.9(3) . . . . ? C11 C16 N17 C18 -24.2(4) . . . . ? C11 C16 N17 C21 160.8(2) . . . . ? C21 N17 C18 N19 -0.5(3) . . . . ? C16 N17 C18 N19 -176.1(2) . . . . ? N17 C18 N19 C20 0.3(3) . . . . ? N17 C18 N19 Ag1 -172.88(18) . . . 2_677 ? C18 N19 C20 C21 0.0(3) . . . . ? Ag1 N19 C20 C21 173.55(19) 2_677 . . . ? N19 C20 C21 N17 -0.3(3) . . . . ? C18 N17 C21 C20 0.4(3) . . . . ? C16 N17 C21 C20 176.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.277 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.098 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 786859' #TrackingRef '- Dobrzanska_CIF 1-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 Ag2 F12 N10 P2' _chemical_formula_weight 1148.53 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 8.6970(5) _cell_length_b 9.7684(6) _cell_length_c 13.5891(8) _cell_angle_alpha 98.3800(10) _cell_angle_beta 101.4630(10) _cell_angle_gamma 103.3970(10) _cell_volume 1078.16(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8259 _cell_measurement_theta_min 2.188 _cell_measurement_theta_max 28.298 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6663 _exptl_absorpt_correction_T_max 0.8906 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12477 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.31 _reflns_number_total 4968 _reflns_number_gt 4734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material ? _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^)+(0.0350P)^2^+0.7255P] 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 4968 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.000334(17) 0.949206(16) 0.716973(11) 0.01841(6) Uani 1 1 d . . . N1 N 0.1955(2) 0.85511(18) 0.73540(13) 0.0173(3) Uani 1 1 d . . . C2 C 0.2382(2) 0.7830(2) 0.80724(16) 0.0170(4) Uani 1 1 d . . . H2 H 0.1783 0.7588 0.8565 0.020 Uiso 1 1 calc R . . N3 N 0.3773(2) 0.74889(18) 0.80082(13) 0.0155(3) Uani 1 1 d . . . C4 C 0.4279(3) 0.8025(2) 0.72100(16) 0.0191(4) Uani 1 1 d . . . H4 H 0.5226 0.7953 0.6982 0.023 Uiso 1 1 calc R . . C5 C 0.3148(3) 0.8677(2) 0.68147(16) 0.0197(4) Uani 1 1 d . . . H5 H 0.3175 0.9148 0.6252 0.024 Uiso 1 1 calc R . . C6 C 0.4610(2) 0.6646(2) 0.86437(15) 0.0180(4) Uani 1 1 d . . . H6A H 0.5749 0.7216 0.8956 0.022 Uiso 1 1 calc R . . H6B H 0.4639 0.5762 0.8196 0.022 Uiso 1 1 calc R . . C7 C 0.3807(2) 0.6231(2) 0.94853(15) 0.0156(4) Uani 1 1 d . . . C8 C 0.2563(2) 0.4951(2) 0.92818(15) 0.0166(4) Uani 1 1 d . . . C9 C 0.1918(2) 0.4521(2) 1.00816(16) 0.0176(4) Uani 1 1 d . . . H9 H 0.1039 0.3678 0.9939 0.021 Uiso 1 1 calc R . . C10 C 0.2527(2) 0.5292(2) 1.10845(15) 0.0163(4) Uani 1 1 d . . . C11 C 0.3763(2) 0.6574(2) 1.12836(15) 0.0152(4) Uani 1 1 d . . . C12 C 0.4359(2) 0.7081(2) 1.04791(15) 0.0154(4) Uani 1 1 d . . . C13 C 0.5581(3) 0.8528(2) 1.06878(17) 0.0221(4) Uani 1 1 d . . . H13C H 0.6672 0.8437 1.0972 0.033 Uiso 1 1 calc R . . H13B H 0.5299 0.9208 1.1180 0.033 Uiso 1 1 calc R . . H13A H 0.5566 0.8878 1.0047 0.033 Uiso 1 1 calc R . . C14 C 0.1912(3) 0.4029(2) 0.82189(16) 0.0214(4) Uani 1 1 d . . . H14B H 0.2748 0.3594 0.8031 0.032 Uiso 1 1 calc R . . H14A H 0.1620 0.4624 0.7728 0.032 Uiso 1 1 calc R . . H14C H 0.0944 0.3270 0.8207 0.032 Uiso 1 1 calc R . . C15 C 0.1862(3) 0.4718(2) 1.19336(17) 0.0223(4) Uani 1 1 d . . . H15C H 0.0951 0.3859 1.1638 0.033 Uiso 1 1 calc R . . H15B H 0.1481 0.5453 1.2313 0.033 Uiso 1 1 calc R . . H15A H 0.2722 0.4471 1.2401 0.033 Uiso 1 1 calc R . . C16 C 0.4547(2) 0.7347(2) 1.23796(15) 0.0175(4) Uani 1 1 d . . . H16A H 0.4749 0.6630 1.2798 0.021 Uiso 1 1 calc R . . H16B H 0.5617 0.8000 1.2403 0.021 Uiso 1 1 calc R . . N17 N 0.3580(2) 0.81888(18) 1.28450(13) 0.0158(3) Uani 1 1 d . . . C18 C 0.2480(2) 0.8795(2) 1.23759(15) 0.0165(4) Uani 1 1 d . . . H18 H 0.2132 0.8691 1.1654 0.020 Uiso 1 1 calc R . . N19 N 0.1944(2) 0.95603(18) 1.30562(13) 0.0174(3) Uani 1 1 d . . . C20 C 0.2764(3) 0.9444(2) 1.40057(16) 0.0215(4) Uani 1 1 d . . . H20 H 0.2640 0.9886 1.4645 0.026 Uiso 1 1 calc R . . C21 C 0.3776(3) 0.8599(2) 1.38845(15) 0.0199(4) Uani 1 1 d . . . H21 H 0.4480 0.8341 1.4412 0.024 Uiso 1 1 calc R . . P22 P 0.0000 1.0000 1.0000 0.01909(15) Uani 1 2 d S . . F23 F 0.1369(2) 0.91802(18) 0.99258(12) 0.0397(4) Uani 1 1 d . . . F24 F 0.1253(2) 1.11783(16) 1.09337(11) 0.0384(4) Uani 1 1 d . . . F25 F 0.05802(16) 1.09487(14) 0.92078(10) 0.0254(3) Uani 1 1 d . . . P26 P 0.5000 0.5000 0.5000 0.02086(16) Uani 1 2 d S . . F27 F 0.65706(17) 0.44748(16) 0.54274(11) 0.0319(3) Uani 1 1 d . . . F28 F 0.44808(17) 0.49365(15) 0.60696(10) 0.0284(3) Uani 1 1 d . . . F29 F 0.39643(18) 0.33650(14) 0.45638(11) 0.0325(3) Uani 1 1 d . . . N30 N 0.1588(2) 0.1352(2) 0.59389(15) 0.0272(4) Uani 1 1 d . . . C31 C 0.1092(3) 0.2244(2) 0.56615(16) 0.0230(4) Uani 1 1 d . . . C32 C 0.0458(3) 0.3393(3) 0.5312(2) 0.0312(5) Uani 1 1 d . . . H32C H 0.0257 0.3248 0.4564 0.047 Uiso 1 1 calc R . . H32A H 0.1255 0.4321 0.5622 0.047 Uiso 1 1 calc R . . H32B H -0.0563 0.3382 0.5516 0.047 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 0.01885(9) 0.02082(9) 0.01894(9) 0.00464(6) 0.00431(6) 0.01174(6) N1 0.0186(8) 0.0186(8) 0.0172(8) 0.0056(6) 0.0045(6) 0.0086(6) C2 0.0158(9) 0.0185(9) 0.0197(9) 0.0057(7) 0.0056(7) 0.0079(7) N3 0.0164(8) 0.0160(8) 0.0164(8) 0.0043(6) 0.0049(6) 0.0074(6) C4 0.0202(10) 0.0216(10) 0.0197(10) 0.0062(8) 0.0090(8) 0.0087(8) C5 0.0235(10) 0.0211(10) 0.0184(10) 0.0065(8) 0.0076(8) 0.0096(8) C6 0.0168(9) 0.0220(10) 0.0202(10) 0.0081(8) 0.0061(8) 0.0109(8) C7 0.0153(9) 0.0161(9) 0.0189(9) 0.0062(7) 0.0051(7) 0.0089(7) C8 0.0170(9) 0.0162(9) 0.0177(9) 0.0022(7) 0.0018(7) 0.0092(7) C9 0.0150(9) 0.0142(9) 0.0227(10) 0.0026(7) 0.0030(7) 0.0043(7) C10 0.0159(9) 0.0175(9) 0.0193(9) 0.0061(7) 0.0058(7) 0.0089(7) C11 0.0150(8) 0.0156(9) 0.0164(9) 0.0020(7) 0.0018(7) 0.0090(7) C12 0.0137(8) 0.0146(9) 0.0196(9) 0.0048(7) 0.0025(7) 0.0076(7) C13 0.0196(10) 0.0179(9) 0.0269(11) 0.0044(8) 0.0038(8) 0.0032(8) C14 0.0232(10) 0.0212(10) 0.0181(10) 0.0000(8) 0.0010(8) 0.0086(8) C15 0.0223(10) 0.0248(10) 0.0226(10) 0.0072(8) 0.0097(8) 0.0069(8) C16 0.0158(9) 0.0201(9) 0.0175(9) 0.0014(7) 0.0019(7) 0.0102(7) N17 0.0160(8) 0.0171(8) 0.0155(8) 0.0036(6) 0.0031(6) 0.0073(6) C18 0.0153(9) 0.0192(9) 0.0160(9) 0.0031(7) 0.0024(7) 0.0078(7) N19 0.0187(8) 0.0203(8) 0.0152(8) 0.0035(6) 0.0042(6) 0.0090(7) C20 0.0245(10) 0.0276(11) 0.0157(9) 0.0054(8) 0.0049(8) 0.0130(9) C21 0.0219(10) 0.0244(10) 0.0150(9) 0.0044(8) 0.0025(8) 0.0109(8) P22 0.0241(4) 0.0184(3) 0.0170(3) 0.0043(3) 0.0064(3) 0.0084(3) F23 0.0473(9) 0.0513(9) 0.0405(9) 0.0206(7) 0.0228(7) 0.0349(8) F24 0.0515(9) 0.0292(7) 0.0220(7) 0.0042(6) 0.0000(6) -0.0051(7) F25 0.0295(7) 0.0263(7) 0.0222(6) 0.0088(5) 0.0081(5) 0.0071(5) P26 0.0285(4) 0.0192(4) 0.0181(4) 0.0072(3) 0.0061(3) 0.0101(3) F27 0.0333(7) 0.0389(8) 0.0321(7) 0.0165(6) 0.0082(6) 0.0201(6) F28 0.0386(8) 0.0311(7) 0.0207(6) 0.0101(5) 0.0117(6) 0.0128(6) F29 0.0412(8) 0.0222(7) 0.0322(7) 0.0024(6) 0.0123(6) 0.0041(6) N30 0.0306(10) 0.0268(10) 0.0263(10) 0.0055(8) 0.0087(8) 0.0102(8) C31 0.0216(10) 0.0248(11) 0.0202(10) 0.0008(8) 0.0050(8) 0.0040(8) C32 0.0322(12) 0.0288(12) 0.0325(13) 0.0077(10) 0.0024(10) 0.0119(10) _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 2.1000(17) . ? Ag1 N19 2.1029(17) 2_577 ? N1 C2 1.328(3) . ? N1 C5 1.378(3) . ? C2 N3 1.343(2) . ? C2 H2 0.9500 . ? N3 C4 1.375(3) . ? N3 C6 1.479(2) . ? C4 C5 1.357(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.510(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.402(3) . ? C7 C12 1.405(3) . ? C8 C9 1.392(3) . ? C8 C14 1.509(3) . ? C9 C10 1.391(3) . ? C9 H9 0.9500 . ? C10 C11 1.400(3) . ? C10 C15 1.511(3) . ? C11 C12 1.405(3) . ? C11 C16 1.511(3) . ? C12 C13 1.508(3) . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14C 0.9800 . ? C15 H15C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C16 N17 1.471(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.343(2) . ? N17 C21 1.376(3) . ? C18 N19 1.327(2) . ? C18 H18 0.9500 . ? N19 C20 1.379(3) . ? N19 Ag1 2.1029(17) 2_577 ? C20 C21 1.355(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? P22 F23 1.5923(14) 2_577 ? P22 F23 1.5923(14) . ? P22 F25 1.6007(12) 2_577 ? P22 F25 1.6007(12) . ? P22 F24 1.6019(14) . ? P22 F24 1.6019(14) 2_577 ? P26 F29 1.5996(13) . ? P26 F29 1.5996(13) 2_666 ? P26 F27 1.6008(13) . ? P26 F27 1.6008(13) 2_666 ? P26 F28 1.6107(13) . ? P26 F28 1.6107(13) 2_666 ? N30 C31 1.137(3) . ? C31 C32 1.459(3) . ? C32 H32C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? 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 N19 178.40(6) . 2_577 ? C2 N1 C5 105.80(17) . . ? C2 N1 Ag1 127.20(14) . . ? C5 N1 Ag1 126.73(13) . . ? N1 C2 N3 110.85(18) . . ? N1 C2 H2 124.6 . . ? N3 C2 H2 124.6 . . ? C2 N3 C4 107.71(16) . . ? C2 N3 C6 127.26(17) . . ? C4 N3 C6 125.00(16) . . ? C5 C4 N3 106.01(17) . . ? C5 C4 H4 127.0 . . ? N3 C4 H4 127.0 . . ? C4 C5 N1 109.64(18) . . ? C4 C5 H5 125.2 . . ? N1 C5 H5 125.2 . . ? N3 C6 C7 113.52(16) . . ? N3 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C12 120.12(18) . . ? C8 C7 C6 119.48(18) . . ? C12 C7 C6 120.31(18) . . ? C9 C8 C7 119.06(18) . . ? C9 C8 C14 119.37(18) . . ? C7 C8 C14 121.57(18) . . ? C10 C9 C8 121.72(18) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 118.97(18) . . ? C9 C10 C15 119.43(18) . . ? C11 C10 C15 121.59(18) . . ? C10 C11 C12 120.36(18) . . ? C10 C11 C16 119.43(18) . . ? C12 C11 C16 120.02(18) . . ? C11 C12 C7 119.45(18) . . ? C11 C12 C13 119.88(18) . . ? C7 C12 C13 120.67(18) . . ? C12 C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C12 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C8 C14 H14B 109.5 . . ? C8 C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C8 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? C10 C15 H15C 109.5 . . ? C10 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? C10 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? N17 C16 C11 114.51(16) . . ? N17 C16 H16A 108.6 . . ? C11 C16 H16A 108.6 . . ? N17 C16 H16B 108.6 . . ? C11 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? C18 N17 C21 107.50(16) . . ? C18 N17 C16 128.21(17) . . ? C21 N17 C16 124.06(16) . . ? N19 C18 N17 110.89(17) . . ? N19 C18 H18 124.6 . . ? N17 C18 H18 124.6 . . ? C18 N19 C20 105.93(17) . . ? C18 N19 Ag1 129.68(14) . 2_577 ? C20 N19 Ag1 123.70(14) . 2_577 ? C21 C20 N19 109.35(18) . . ? C21 C20 H20 125.3 . . ? N19 C20 H20 125.3 . . ? C20 C21 N17 106.33(18) . . ? C20 C21 H21 126.8 . . ? N17 C21 H21 126.8 . . ? F23 P22 F23 180.000(1) 2_577 . ? F23 P22 F25 90.94(7) 2_577 2_577 ? F23 P22 F25 89.06(7) . 2_577 ? F23 P22 F25 89.06(7) 2_577 . ? F23 P22 F25 90.94(7) . . ? F25 P22 F25 180.000(1) 2_577 . ? F23 P22 F24 90.44(9) 2_577 . ? F23 P22 F24 89.56(9) . . ? F25 P22 F24 89.94(7) 2_577 . ? F25 P22 F24 90.06(7) . . ? F23 P22 F24 89.56(9) 2_577 2_577 ? F23 P22 F24 90.44(9) . 2_577 ? F25 P22 F24 90.06(7) 2_577 2_577 ? F25 P22 F24 89.94(7) . 2_577 ? F24 P22 F24 180.000(1) . 2_577 ? F29 P26 F29 180.0 . 2_666 ? F29 P26 F27 90.03(8) . . ? F29 P26 F27 89.97(8) 2_666 . ? F29 P26 F27 89.97(8) . 2_666 ? F29 P26 F27 90.03(8) 2_666 2_666 ? F27 P26 F27 180.000(1) . 2_666 ? F29 P26 F28 89.91(7) . . ? F29 P26 F28 90.09(7) 2_666 . ? F27 P26 F28 90.07(7) . . ? F27 P26 F28 89.93(7) 2_666 . ? F29 P26 F28 90.09(7) . 2_666 ? F29 P26 F28 89.91(7) 2_666 2_666 ? F27 P26 F28 89.93(7) . 2_666 ? F27 P26 F28 90.07(7) 2_666 2_666 ? F28 P26 F28 180.0 . 2_666 ? N30 C31 C32 179.6(2) . . ? C31 C32 H32C 109.5 . . ? C31 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? 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 C5 N1 C2 N3 -0.4(2) . . . . ? Ag1 N1 C2 N3 -174.68(13) . . . . ? N1 C2 N3 C4 0.4(2) . . . . ? N1 C2 N3 C6 -177.58(18) . . . . ? C2 N3 C4 C5 -0.2(2) . . . . ? C6 N3 C4 C5 177.83(18) . . . . ? N3 C4 C5 N1 -0.1(2) . . . . ? C2 N1 C5 C4 0.3(2) . . . . ? Ag1 N1 C5 C4 174.61(14) . . . . ? C2 N3 C6 C7 -4.0(3) . . . . ? C4 N3 C6 C7 178.44(18) . . . . ? N3 C6 C7 C8 88.3(2) . . . . ? N3 C6 C7 C12 -95.1(2) . . . . ? C12 C7 C8 C9 -1.6(3) . . . . ? C6 C7 C8 C9 175.01(17) . . . . ? C12 C7 C8 C14 178.55(17) . . . . ? C6 C7 C8 C14 -4.8(3) . . . . ? C7 C8 C9 C10 -3.0(3) . . . . ? C14 C8 C9 C10 176.77(18) . . . . ? C8 C9 C10 C11 3.4(3) . . . . ? C8 C9 C10 C15 -175.64(18) . . . . ? C9 C10 C11 C12 0.9(3) . . . . ? C15 C10 C11 C12 179.95(17) . . . . ? C9 C10 C11 C16 -174.16(17) . . . . ? C15 C10 C11 C16 4.9(3) . . . . ? C10 C11 C12 C7 -5.5(3) . . . . ? C16 C11 C12 C7 169.57(17) . . . . ? C10 C11 C12 C13 174.48(17) . . . . ? C16 C11 C12 C13 -10.5(3) . . . . ? C8 C7 C12 C11 5.8(3) . . . . ? C6 C7 C12 C11 -170.78(17) . . . . ? C8 C7 C12 C13 -174.12(17) . . . . ? C6 C7 C12 C13 9.3(3) . . . . ? C10 C11 C16 N17 -78.6(2) . . . . ? C12 C11 C16 N17 106.3(2) . . . . ? C11 C16 N17 C18 -27.2(3) . . . . ? C11 C16 N17 C21 158.92(19) . . . . ? C21 N17 C18 N19 -0.7(2) . . . . ? C16 N17 C18 N19 -175.33(18) . . . . ? N17 C18 N19 C20 0.7(2) . . . . ? N17 C18 N19 Ag1 -169.90(13) . . . 2_577 ? C18 N19 C20 C21 -0.5(2) . . . . ? Ag1 N19 C20 C21 170.84(15) 2_577 . . . ? N19 C20 C21 N17 0.1(2) . . . . ? C18 N17 C21 C20 0.4(2) . . . . ? C16 N17 C21 C20 175.27(18) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.089 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.087 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 786860' #TrackingRef '- Dobrzanska_CIF 1-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 Ag2 F12 N8 P2' _chemical_formula_weight 1066.42 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8539(14) _cell_length_b 9.3957(15) _cell_length_c 12.0520(19) _cell_angle_alpha 92.737(2) _cell_angle_beta 102.777(2) _cell_angle_gamma 102.993(2) _cell_volume 947.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4103 _cell_measurement_theta_min 2.237 _cell_measurement_theta_max 26.458 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7347 _exptl_absorpt_correction_T_max 0.7842 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7536 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.47 _reflns_number_total 3825 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics "'Mercury (Macrae, 2008)'" _computing_publication_material ? _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^)+(0.0829P)^2^+1.1851P] 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 3825 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _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 -0.20158(4) 0.94390(4) 0.67229(3) 0.02328(16) Uani 1 1 d . . . N1 N -0.0228(5) 0.8452(5) 0.6437(4) 0.0260(10) Uani 1 1 d . . . C2 C 0.0791(6) 0.7960(6) 0.7206(4) 0.0224(10) Uani 1 1 d . . . H2 H 0.0926 0.8121 0.8010 0.027 Uiso 1 1 calc R . . N3 N 0.1603(5) 0.7207(5) 0.6699(4) 0.0214(9) Uani 1 1 d . . . C4 C 0.1100(7) 0.7226(7) 0.5549(5) 0.0304(12) Uani 1 1 d . . . H4 H 0.1473 0.6783 0.4972 0.036 Uiso 1 1 calc R . . C5 C -0.0032(7) 0.7998(7) 0.5389(5) 0.0349(14) Uani 1 1 d . . . H5 H -0.0599 0.8194 0.4669 0.042 Uiso 1 1 calc R . . C6 C 0.2918(6) 0.6554(6) 0.7247(4) 0.0241(11) Uani 1 1 d . . . H6A H 0.3948 0.7266 0.7299 0.029 Uiso 1 1 calc R . . H6B H 0.2894 0.5668 0.6759 0.029 Uiso 1 1 calc R . . C7 C 0.2826(6) 0.6138(5) 0.8425(4) 0.0198(10) Uani 1 1 d . . . C8 C 0.1690(6) 0.4899(6) 0.8547(4) 0.0223(10) Uani 1 1 d . . . C9 C 0.1682(6) 0.4479(6) 0.9627(4) 0.0223(10) Uani 1 1 d . . . H9 H 0.0867 0.3673 0.9717 0.027 Uiso 1 1 calc R . . C10 C 0.2824(6) 0.5195(6) 1.0582(4) 0.0210(10) Uani 1 1 d . . . C11 C 0.4006(6) 0.6398(6) 1.0457(4) 0.0214(10) Uani 1 1 d . . . C12 C 0.3970(6) 0.6922(5) 0.9383(4) 0.0196(10) Uani 1 1 d . . . C13 C 0.5134(7) 0.8295(6) 0.9254(5) 0.0283(12) Uani 1 1 d . . . H13C H 0.6030 0.8036 0.9007 0.042 Uiso 1 1 calc R . . H13B H 0.5532 0.8905 0.9989 0.042 Uiso 1 1 calc R . . H13A H 0.4603 0.8841 0.8680 0.042 Uiso 1 1 calc R . . C14 C 0.0487(7) 0.3997(6) 0.7519(5) 0.0302(12) Uani 1 1 d . . . H14B H 0.1048 0.3565 0.7028 0.045 Uiso 1 1 calc R . . H14A H -0.0117 0.4630 0.7087 0.045 Uiso 1 1 calc R . . H14C H -0.0248 0.3212 0.7779 0.045 Uiso 1 1 calc R . . C15 C 0.2790(7) 0.4646(6) 1.1731(4) 0.0280(12) Uani 1 1 d . . . H15B H 0.2904 0.5474 1.2294 0.042 Uiso 1 1 calc R . . H15A H 0.3671 0.4171 1.1969 0.042 Uiso 1 1 calc R . . H15C H 0.1773 0.3936 1.1677 0.042 Uiso 1 1 calc R . . C16 C 0.5368(6) 0.7066(5) 1.1469(4) 0.0212(10) Uani 1 1 d . . . H16A H 0.5615 0.6278 1.1943 0.025 Uiso 1 1 calc R . . H16B H 0.6325 0.7493 1.1188 0.025 Uiso 1 1 calc R . . N17 N 0.5045(5) 0.8215(4) 1.2192(4) 0.0185(8) Uani 1 1 d . . . C18 C 0.3657(6) 0.8532(6) 1.2181(4) 0.0218(10) Uani 1 1 d . . . H18 H 0.2686 0.8085 1.1642 0.026 Uiso 1 1 calc R . . N19 N 0.3800(5) 0.9548(5) 1.3012(4) 0.0225(9) Uani 1 1 d . . . C20 C 0.5376(6) 0.9911(6) 1.3581(4) 0.0231(11) Uani 1 1 d . . . H20 H 0.5836 1.0630 1.4220 0.028 Uiso 1 1 calc R . . C21 C 0.6170(6) 0.9096(6) 1.3097(4) 0.0232(11) Uani 1 1 d . . . H21 H 0.7274 0.9118 1.3326 0.028 Uiso 1 1 calc R . . P22 P 0.0000 1.0000 1.0000 0.0209(4) Uani 1 2 d S . . F23 F 0.1272(4) 0.9049(4) 1.0030(3) 0.0433(9) Uani 1 1 d . . . F24 F 0.1224(4) 1.1199(4) 1.0954(3) 0.0316(7) Uani 1 1 d . . . F25 F 0.0625(5) 1.0858(4) 0.9020(3) 0.0416(9) Uani 1 1 d . . . P26 P 0.5000 0.5000 0.5000 0.0220(4) Uani 1 2 d S . . F27 F 0.6655(4) 0.4589(4) 0.5492(3) 0.0336(8) Uani 1 1 d . . . F28 F 0.4259(4) 0.4143(3) 0.5947(3) 0.0285(7) Uani 1 1 d . . . F29 F 0.4424(4) 0.3518(4) 0.4143(3) 0.0324(7) 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 0.0184(2) 0.0262(2) 0.0302(2) -0.00008(15) 0.00719(15) 0.01471(16) N1 0.021(2) 0.033(2) 0.027(2) -0.0012(19) 0.0055(18) 0.0165(19) C2 0.020(2) 0.026(3) 0.024(3) 0.000(2) 0.007(2) 0.010(2) N3 0.016(2) 0.029(2) 0.024(2) -0.0010(17) 0.0050(16) 0.0151(18) C4 0.028(3) 0.043(3) 0.026(3) -0.001(2) 0.006(2) 0.024(3) C5 0.032(3) 0.053(4) 0.024(3) -0.005(3) -0.001(2) 0.029(3) C6 0.018(2) 0.035(3) 0.028(3) 0.006(2) 0.009(2) 0.019(2) C7 0.019(2) 0.020(2) 0.028(3) 0.0036(19) 0.0097(19) 0.015(2) C8 0.018(2) 0.026(3) 0.026(3) -0.004(2) 0.0040(19) 0.015(2) C9 0.018(2) 0.022(2) 0.031(3) 0.000(2) 0.010(2) 0.010(2) C10 0.021(2) 0.021(2) 0.028(3) 0.004(2) 0.011(2) 0.015(2) C11 0.016(2) 0.023(2) 0.029(3) -0.001(2) 0.0047(19) 0.014(2) C12 0.014(2) 0.022(2) 0.029(3) 0.002(2) 0.0077(19) 0.0140(19) C13 0.025(3) 0.026(3) 0.038(3) 0.000(2) 0.013(2) 0.009(2) C14 0.026(3) 0.031(3) 0.034(3) -0.002(2) 0.002(2) 0.013(2) C15 0.034(3) 0.027(3) 0.028(3) 0.004(2) 0.010(2) 0.014(2) C16 0.017(2) 0.022(2) 0.028(3) 0.000(2) 0.0042(19) 0.013(2) N17 0.0139(19) 0.019(2) 0.024(2) 0.0001(16) 0.0027(16) 0.0076(16) C18 0.016(2) 0.026(3) 0.025(3) -0.001(2) 0.0040(19) 0.010(2) N19 0.020(2) 0.021(2) 0.029(2) 0.0007(17) 0.0090(17) 0.0085(17) C20 0.017(2) 0.030(3) 0.022(2) 0.006(2) 0.0025(19) 0.006(2) C21 0.016(2) 0.029(3) 0.022(2) 0.000(2) 0.0017(19) 0.004(2) P22 0.0159(8) 0.0203(9) 0.0272(10) -0.0001(7) 0.0032(7) 0.0082(7) F23 0.0346(19) 0.053(2) 0.046(2) -0.0092(17) -0.0022(16) 0.0327(18) F24 0.0246(16) 0.0317(17) 0.0339(17) -0.0058(14) 0.0036(13) 0.0026(14) F25 0.055(2) 0.0301(18) 0.0377(19) 0.0008(15) 0.0177(17) 0.0011(17) P26 0.0229(9) 0.0280(10) 0.0217(9) 0.0022(7) 0.0100(7) 0.0152(8) F27 0.0280(17) 0.049(2) 0.0320(17) 0.0028(15) 0.0092(14) 0.0252(15) F28 0.0316(17) 0.0328(17) 0.0291(16) 0.0063(13) 0.0154(13) 0.0154(14) F29 0.0395(19) 0.0301(17) 0.0316(17) -0.0029(13) 0.0151(14) 0.0117(15) _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 2.086(4) . ? Ag1 N19 2.091(4) 2_577 ? N1 C2 1.321(7) . ? N1 C5 1.374(7) . ? C2 N3 1.331(6) . ? C2 H2 0.9500 . ? N3 C4 1.362(7) . ? N3 C6 1.479(6) . ? C4 C5 1.350(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.505(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.394(7) . ? C7 C12 1.402(7) . ? C8 C9 1.380(7) . ? C8 C14 1.516(7) . ? C9 C10 1.380(7) . ? C9 H9 0.9500 . ? C10 C11 1.396(7) . ? C10 C15 1.504(7) . ? C11 C12 1.404(7) . ? C11 C16 1.507(7) . ? C12 C13 1.497(7) . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14C 0.9800 . ? C15 H15B 0.9800 . ? C15 H15A 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.471(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.326(6) . ? N17 C21 1.389(6) . ? C18 N19 1.315(7) . ? C18 H18 0.9500 . ? N19 C20 1.369(6) . ? N19 Ag1 2.091(4) 2_577 ? C20 C21 1.343(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? P22 F23 1.583(3) . ? P22 F23 1.583(3) 2_577 ? P22 F25 1.590(3) . ? P22 F25 1.590(3) 2_577 ? P22 F24 1.594(3) 2_577 ? P22 F24 1.594(3) . ? P26 F27 1.594(3) . ? P26 F27 1.594(3) 2_666 ? P26 F28 1.601(3) 2_666 ? P26 F28 1.601(3) . ? P26 F29 1.605(3) 2_666 ? P26 F29 1.605(3) . ? 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 N19 179.03(17) . 2_577 ? C2 N1 C5 106.1(4) . . ? C2 N1 Ag1 127.3(4) . . ? C5 N1 Ag1 126.0(4) . . ? N1 C2 N3 110.7(4) . . ? N1 C2 H2 124.7 . . ? N3 C2 H2 124.7 . . ? C2 N3 C4 107.8(4) . . ? C2 N3 C6 127.9(4) . . ? C4 N3 C6 124.1(4) . . ? C5 C4 N3 106.6(5) . . ? C5 C4 H4 126.7 . . ? N3 C4 H4 126.7 . . ? C4 C5 N1 108.8(5) . . ? C4 C5 H5 125.6 . . ? N1 C5 H5 125.6 . . ? N3 C6 C7 113.1(4) . . ? N3 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N3 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C12 120.5(5) . . ? C8 C7 C6 119.6(5) . . ? C12 C7 C6 119.7(5) . . ? C9 C8 C7 119.0(5) . . ? C9 C8 C14 119.6(5) . . ? C7 C8 C14 121.5(5) . . ? C8 C9 C10 121.9(5) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C9 C10 C11 119.2(5) . . ? C9 C10 C15 119.4(5) . . ? C11 C10 C15 121.4(5) . . ? C10 C11 C12 120.1(5) . . ? C10 C11 C16 119.3(5) . . ? C12 C11 C16 120.5(5) . . ? C7 C12 C11 119.0(5) . . ? C7 C12 C13 120.2(5) . . ? C11 C12 C13 120.8(5) . . ? C12 C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C12 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C8 C14 H14B 109.5 . . ? C8 C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C8 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? C10 C15 H15B 109.5 . . ? C10 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? C10 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? N17 C16 C11 113.9(4) . . ? N17 C16 H16A 108.8 . . ? C11 C16 H16A 108.8 . . ? N17 C16 H16B 108.8 . . ? C11 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 N17 C21 107.2(4) . . ? C18 N17 C16 128.1(4) . . ? C21 N17 C16 124.5(4) . . ? N19 C18 N17 111.2(4) . . ? N19 C18 H18 124.4 . . ? N17 C18 H18 124.4 . . ? C18 N19 C20 106.2(4) . . ? C18 N19 Ag1 126.1(4) . 2_577 ? C20 N19 Ag1 127.3(4) . 2_577 ? C21 C20 N19 109.6(5) . . ? C21 C20 H20 125.2 . . ? N19 C20 H20 125.2 . . ? C20 C21 N17 105.8(4) . . ? C20 C21 H21 127.1 . . ? N17 C21 H21 127.1 . . ? F23 P22 F23 180.000(3) . 2_577 ? F23 P22 F25 89.8(2) . . ? F23 P22 F25 90.2(2) 2_577 . ? F23 P22 F25 90.2(2) . 2_577 ? F23 P22 F25 89.8(2) 2_577 2_577 ? F25 P22 F25 180.000(2) . 2_577 ? F23 P22 F24 88.64(18) . 2_577 ? F23 P22 F24 91.36(18) 2_577 2_577 ? F25 P22 F24 89.42(18) . 2_577 ? F25 P22 F24 90.58(18) 2_577 2_577 ? F23 P22 F24 91.36(18) . . ? F23 P22 F24 88.64(18) 2_577 . ? F25 P22 F24 90.58(18) . . ? F25 P22 F24 89.42(18) 2_577 . ? F24 P22 F24 180.000(1) 2_577 . ? F27 P26 F27 180.000(1) . 2_666 ? F27 P26 F28 89.90(16) . 2_666 ? F27 P26 F28 90.10(16) 2_666 2_666 ? F27 P26 F28 90.10(16) . . ? F27 P26 F28 89.90(16) 2_666 . ? F28 P26 F28 180.000(1) 2_666 . ? F27 P26 F29 90.32(18) . 2_666 ? F27 P26 F29 89.68(18) 2_666 2_666 ? F28 P26 F29 90.12(16) 2_666 2_666 ? F28 P26 F29 89.88(16) . 2_666 ? F27 P26 F29 89.68(18) . . ? F27 P26 F29 90.32(18) 2_666 . ? F28 P26 F29 89.88(16) 2_666 . ? F28 P26 F29 90.12(16) . . ? F29 P26 F29 180.00(15) 2_666 . ? 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 C5 N1 C2 N3 -0.8(6) . . . . ? Ag1 N1 C2 N3 170.8(4) . . . . ? N1 C2 N3 C4 0.7(6) . . . . ? N1 C2 N3 C6 176.0(5) . . . . ? C2 N3 C4 C5 -0.4(7) . . . . ? C6 N3 C4 C5 -175.8(5) . . . . ? N3 C4 C5 N1 -0.1(7) . . . . ? C2 N1 C5 C4 0.5(7) . . . . ? Ag1 N1 C5 C4 -171.2(4) . . . . ? C2 N3 C6 C7 28.2(8) . . . . ? C4 N3 C6 C7 -157.3(5) . . . . ? N3 C6 C7 C8 74.3(6) . . . . ? N3 C6 C7 C12 -111.1(5) . . . . ? C12 C7 C8 C9 1.6(7) . . . . ? C6 C7 C8 C9 176.1(4) . . . . ? C12 C7 C8 C14 -177.4(4) . . . . ? C6 C7 C8 C14 -2.9(7) . . . . ? C7 C8 C9 C10 -4.0(7) . . . . ? C14 C8 C9 C10 175.0(5) . . . . ? C8 C9 C10 C11 1.3(7) . . . . ? C8 C9 C10 C15 -177.6(5) . . . . ? C9 C10 C11 C12 3.8(7) . . . . ? C15 C10 C11 C12 -177.4(4) . . . . ? C9 C10 C11 C16 -172.5(4) . . . . ? C15 C10 C11 C16 6.3(7) . . . . ? C8 C7 C12 C11 3.3(7) . . . . ? C6 C7 C12 C11 -171.1(4) . . . . ? C8 C7 C12 C13 -176.9(5) . . . . ? C6 C7 C12 C13 8.6(7) . . . . ? C10 C11 C12 C7 -6.1(7) . . . . ? C16 C11 C12 C7 170.2(4) . . . . ? C10 C11 C12 C13 174.2(4) . . . . ? C16 C11 C12 C13 -9.5(7) . . . . ? C10 C11 C16 N17 -88.3(5) . . . . ? C12 C11 C16 N17 95.4(5) . . . . ? C11 C16 N17 C18 13.1(7) . . . . ? C11 C16 N17 C21 -172.7(4) . . . . ? C21 N17 C18 N19 -0.2(6) . . . . ? C16 N17 C18 N19 174.7(5) . . . . ? N17 C18 N19 C20 0.7(6) . . . . ? N17 C18 N19 Ag1 174.3(3) . . . 2_577 ? C18 N19 C20 C21 -0.8(6) . . . . ? Ag1 N19 C20 C21 -174.3(3) 2_577 . . . ? N19 C20 C21 N17 0.7(6) . . . . ? C18 N17 C21 C20 -0.3(5) . . . . ? C16 N17 C21 C20 -175.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.683 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.188 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 786861' #TrackingRef '- Dobrzanska_CIF 1-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 Ag2 N10 O6' _chemical_formula_weight 900.50 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5514(7) _cell_length_b 9.6731(8) _cell_length_c 11.5283(9) _cell_angle_alpha 94.1750(10) _cell_angle_beta 93.6960(10) _cell_angle_gamma 107.1430(10) _cell_volume 905.12(13) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5821 _cell_measurement_theta_min 2.503 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6458 _exptl_absorpt_correction_T_max 0.7187 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10477 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4168 _reflns_number_gt 3886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material ? _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^)+(0.0780P)^2^+4.3632P] 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 4168 _refine_ls_number_parameters 274 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _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 0.41164(4) 0.45787(4) 0.21053(4) 0.03503(16) Uani 1 1 d . . . N1 N 0.2223(5) 0.5538(4) 0.2237(4) 0.0270(8) Uani 1 1 d . A . C2 C 0.2051(6) 0.6559(5) 0.3006(4) 0.0274(9) Uani 1 1 d . . . H2 H 0.2816 0.7011 0.3656 0.033 Uiso 1 1 calc R A . N3 N 0.0647(5) 0.6867(4) 0.2739(3) 0.0257(8) Uani 1 1 d . . . C4 C -0.0126(6) 0.6001(5) 0.1744(4) 0.0274(9) Uani 1 1 d . . . H4 H -0.1144 0.5979 0.1347 0.033 Uiso 1 1 calc R A . C5 C 0.0861(6) 0.5184(5) 0.1441(4) 0.0274(9) Uani 1 1 d . A . H5 H 0.0646 0.4481 0.0784 0.033 Uiso 1 1 calc R . . C6 C 0.0022(6) 0.7973(5) 0.3341(4) 0.0303(10) Uani 1 1 d . . . H6A H -0.1116 0.7501 0.3529 0.036 Uiso 1 1 calc R A . H6B H -0.0017 0.8718 0.2805 0.036 Uiso 1 1 calc R . . C7 C 0.1053(5) 0.8711(5) 0.4452(4) 0.0253(9) Uani 1 1 d . . . C8 C 0.2340(6) 0.9992(5) 0.4414(4) 0.0260(9) Uani 1 1 d . . . C9 C 0.3210(6) 1.0718(5) 0.5452(4) 0.0273(9) Uani 1 1 d . . . H9 H 0.4088 1.1585 0.5429 0.033 Uiso 1 1 calc R . . C10 C 0.2815(5) 1.0194(5) 0.6536(4) 0.0245(8) Uani 1 1 d . . . C11 C 0.1557(5) 0.8890(5) 0.6556(4) 0.0250(8) Uani 1 1 d . . . C12 C 0.0690(5) 0.8126(5) 0.5514(4) 0.0255(9) Uani 1 1 d . . . C13 C -0.0630(6) 0.6693(5) 0.5547(5) 0.0342(10) Uani 1 1 d . . . H13A H -0.1663 0.6876 0.5720 0.051 Uiso 1 1 calc R . . H13B H -0.0297 0.6153 0.6154 0.051 Uiso 1 1 calc R . . H13C H -0.0786 0.6123 0.4787 0.051 Uiso 1 1 calc R . . C14 C 0.2819(7) 1.0620(6) 0.3283(4) 0.0344(10) Uani 1 1 d . . . H14A H 0.2975 0.9864 0.2729 0.052 Uiso 1 1 calc R . . H14B H 0.3845 1.1422 0.3430 0.052 Uiso 1 1 calc R . . H14C H 0.1947 1.0984 0.2953 0.052 Uiso 1 1 calc R . . C15 C 0.3746(6) 1.1061(5) 0.7637(4) 0.0309(10) Uani 1 1 d . . . H15A H 0.4518 1.1965 0.7439 0.046 Uiso 1 1 calc R . . H15B H 0.4354 1.0491 0.8035 0.046 Uiso 1 1 calc R . . H15C H 0.2971 1.1292 0.8152 0.046 Uiso 1 1 calc R . . C16 C 0.1148(6) 0.8336(5) 0.7729(4) 0.0270(9) Uani 1 1 d . . . H16A H 0.1078 0.9148 0.8277 0.032 Uiso 1 1 calc R A . H16B H 0.0060 0.7587 0.7636 0.032 Uiso 1 1 calc R . . N17 N 0.2388(5) 0.7709(4) 0.8225(3) 0.0254(7) Uani 1 1 d . A . C18 C 0.3203(6) 0.6946(5) 0.7635(4) 0.0278(9) Uani 1 1 d . . . H18 H 0.3093 0.6747 0.6809 0.033 Uiso 1 1 calc R A . N19 N 0.4188(5) 0.6502(5) 0.8358(4) 0.0315(9) Uani 1 1 d . . . C20 C 0.3953(7) 0.7002(7) 0.9468(5) 0.0395(12) Uani 1 1 d . . . H20 H 0.4491 0.6848 1.0172 0.047 Uiso 1 1 calc R A . C21 C 0.2837(6) 0.7743(6) 0.9396(4) 0.0346(11) Uani 1 1 d . A . H21 H 0.2444 0.8194 1.0026 0.042 Uiso 1 1 calc R . . N22 N 0.5315(6) 0.5120(7) 0.4871(6) 0.028(2) Uani 0.50 1 d PDU A -2 O23 O 0.5629(13) 0.5803(8) 0.3953(7) 0.057(2) Uani 0.50 1 d PDU A -2 O24 O 0.4644(13) 0.5625(13) 0.5658(9) 0.077(4) Uani 0.50 1 d PDU A -2 O25 O 0.5696(9) 0.3987(7) 0.4933(8) 0.0402(17) Uani 0.50 1 d PD A -2 N26 N 0.0890(8) 0.1086(7) 0.0026(7) 0.0337(19) Uani 0.50 1 d PD B -1 O27 O 0.1876(6) 0.2324(5) 0.0169(4) 0.0111(9) Uani 0.50 1 d PDU B -1 O28 O 0.1054(12) 0.0073(11) 0.0590(7) 0.0414(18) Uani 0.50 1 d P B -1 O29 O -0.0272(10) 0.0835(9) -0.0745(6) 0.0354(15) Uani 0.50 1 d P B -1 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 0.0299(2) 0.0322(2) 0.0506(3) 0.01070(16) 0.01213(16) 0.01764(16) N1 0.0265(18) 0.0256(18) 0.0312(19) 0.0038(15) 0.0048(15) 0.0106(15) C2 0.024(2) 0.031(2) 0.029(2) 0.0008(17) -0.0002(17) 0.0120(17) N3 0.0257(18) 0.0261(18) 0.0274(18) -0.0015(14) 0.0004(14) 0.0124(15) C4 0.027(2) 0.030(2) 0.026(2) -0.0010(17) -0.0011(17) 0.0110(18) C5 0.029(2) 0.027(2) 0.028(2) 0.0019(17) 0.0037(17) 0.0110(18) C6 0.029(2) 0.033(2) 0.033(2) -0.0055(19) -0.0010(18) 0.0186(19) C7 0.027(2) 0.026(2) 0.027(2) -0.0015(16) 0.0027(17) 0.0145(17) C8 0.028(2) 0.029(2) 0.026(2) 0.0037(17) 0.0060(17) 0.0146(18) C9 0.026(2) 0.024(2) 0.034(2) 0.0046(17) 0.0062(17) 0.0090(17) C10 0.026(2) 0.025(2) 0.025(2) 0.0016(16) 0.0038(16) 0.0114(17) C11 0.025(2) 0.026(2) 0.029(2) 0.0042(16) 0.0067(16) 0.0133(17) C12 0.023(2) 0.024(2) 0.034(2) 0.0004(17) 0.0054(17) 0.0135(17) C13 0.031(2) 0.025(2) 0.045(3) -0.001(2) 0.008(2) 0.0068(19) C14 0.042(3) 0.042(3) 0.027(2) 0.011(2) 0.010(2) 0.021(2) C15 0.033(2) 0.031(2) 0.028(2) -0.0015(18) 0.0020(18) 0.0110(19) C16 0.030(2) 0.029(2) 0.029(2) 0.0074(17) 0.0089(17) 0.0173(18) N17 0.0265(18) 0.0269(18) 0.0261(18) 0.0048(14) 0.0063(14) 0.0118(15) C18 0.027(2) 0.031(2) 0.029(2) 0.0029(17) 0.0072(17) 0.0124(18) N19 0.030(2) 0.035(2) 0.035(2) 0.0103(17) 0.0076(16) 0.0163(17) C20 0.038(3) 0.057(3) 0.033(3) 0.010(2) 0.007(2) 0.026(3) C21 0.036(3) 0.049(3) 0.026(2) 0.004(2) 0.0048(19) 0.022(2) N22 0.026(6) 0.037(4) 0.021(4) -0.010(3) -0.010(3) 0.016(4) O23 0.079(6) 0.040(5) 0.034(4) -0.001(3) -0.021(4) -0.002(4) O24 0.066(7) 0.130(12) 0.044(5) -0.036(6) -0.007(4) 0.058(8) O25 0.041(4) 0.032(4) 0.046(5) 0.007(3) -0.004(4) 0.009(3) N26 0.037(4) 0.055(5) 0.021(4) -0.002(3) 0.004(3) 0.034(4) O27 0.0084(19) 0.0059(19) 0.019(2) -0.0030(16) 0.0009(17) 0.0028(16) O28 0.054(5) 0.051(5) 0.032(4) 0.003(3) 0.002(3) 0.036(4) O29 0.043(4) 0.037(4) 0.028(3) 0.002(3) -0.001(3) 0.016(4) _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 N19 2.096(4) 2_666 ? Ag1 N1 2.098(4) . ? Ag1 O23 2.447(8) . ? N1 C2 1.326(6) . ? N1 C5 1.377(6) . ? C2 N3 1.342(6) . ? C2 H2 0.9500 . ? N3 C4 1.375(6) . ? N3 C6 1.479(6) . ? C4 C5 1.361(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.509(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.400(7) . ? C7 C12 1.400(7) . ? C8 C9 1.391(7) . ? C8 C14 1.508(6) . ? C9 C10 1.407(6) . ? C9 H9 0.9500 . ? C10 C11 1.399(6) . ? C10 C15 1.507(6) . ? C11 C12 1.404(7) . ? C11 C16 1.514(6) . ? C12 C13 1.513(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.474(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.336(6) . ? N17 C21 1.375(6) . ? C18 N19 1.328(6) . ? C18 H18 0.9500 . ? N19 C20 1.383(7) . ? N19 Ag1 2.096(4) 2_666 ? C20 C21 1.354(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? N22 O25 1.238(5) . ? N22 O24 1.249(5) . ? N22 O23 1.289(10) . ? N26 O27 1.237(5) . ? N26 O29 1.245(11) . ? N26 O28 1.251(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 N19 Ag1 N1 169.00(16) 2_666 . ? N19 Ag1 O23 96.2(3) 2_666 . ? N1 Ag1 O23 94.6(3) . . ? C2 N1 C5 106.2(4) . . ? C2 N1 Ag1 131.0(3) . . ? C5 N1 Ag1 122.8(3) . . ? N1 C2 N3 110.7(4) . . ? N1 C2 H2 124.6 . . ? N3 C2 H2 124.6 . . ? C2 N3 C4 107.8(4) . . ? C2 N3 C6 128.1(4) . . ? C4 N3 C6 124.1(4) . . ? C5 C4 N3 106.1(4) . . ? C5 C4 H4 126.9 . . ? N3 C4 H4 126.9 . . ? C4 C5 N1 109.2(4) . . ? C4 C5 H5 125.4 . . ? N1 C5 H5 125.4 . . ? N3 C6 C7 113.3(4) . . ? N3 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C12 120.7(4) . . ? C8 C7 C6 119.6(4) . . ? C12 C7 C6 119.7(4) . . ? C9 C8 C7 119.1(4) . . ? C9 C8 C14 118.6(4) . . ? C7 C8 C14 122.3(4) . . ? C8 C9 C10 121.3(4) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 118.9(4) . . ? C11 C10 C15 122.1(4) . . ? C9 C10 C15 119.0(4) . . ? C10 C11 C12 120.6(4) . . ? C10 C11 C16 118.3(4) . . ? C12 C11 C16 121.1(4) . . ? C7 C12 C11 119.3(4) . . ? C7 C12 C13 120.7(4) . . ? C11 C12 C13 120.0(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C11 111.9(4) . . ? N17 C16 H16A 109.2 . . ? C11 C16 H16A 109.2 . . ? N17 C16 H16B 109.2 . . ? C11 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 N17 C21 108.0(4) . . ? C18 N17 C16 126.6(4) . . ? C21 N17 C16 125.2(4) . . ? N19 C18 N17 110.8(4) . . ? N19 C18 H18 124.6 . . ? N17 C18 H18 124.6 . . ? C18 N19 C20 105.7(4) . . ? C18 N19 Ag1 126.8(3) . 2_666 ? C20 N19 Ag1 127.3(3) . 2_666 ? C21 C20 N19 109.5(5) . . ? C21 C20 H20 125.3 . . ? N19 C20 H20 125.3 . . ? C20 C21 N17 106.0(4) . . ? C20 C21 H21 127.0 . . ? N17 C21 H21 127.0 . . ? O25 N22 O24 122.7(7) . . ? O25 N22 O23 118.3(7) . . ? O24 N22 O23 119.0(8) . . ? N22 O23 Ag1 116.9(4) . . ? O27 N26 O29 118.1(8) . . ? O27 N26 O28 122.7(8) . . ? O29 N26 O28 119.2(7) . . ? 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 N19 Ag1 N1 C2 -161.6(7) 2_666 . . . ? O23 Ag1 N1 C2 6.1(5) . . . . ? N19 Ag1 N1 C5 16.7(10) 2_666 . . . ? O23 Ag1 N1 C5 -175.6(4) . . . . ? C5 N1 C2 N3 0.2(5) . . . . ? Ag1 N1 C2 N3 178.7(3) . . . . ? N1 C2 N3 C4 -0.2(6) . . . . ? N1 C2 N3 C6 -177.5(4) . . . . ? C2 N3 C4 C5 0.1(5) . . . . ? C6 N3 C4 C5 177.5(4) . . . . ? N3 C4 C5 N1 0.1(5) . . . . ? C2 N1 C5 C4 -0.2(5) . . . . ? Ag1 N1 C5 C4 -178.8(3) . . . . ? C2 N3 C6 C7 -6.4(7) . . . . ? C4 N3 C6 C7 176.7(4) . . . . ? N3 C6 C7 C8 91.4(5) . . . . ? N3 C6 C7 C12 -90.1(5) . . . . ? C12 C7 C8 C9 -2.9(6) . . . . ? C6 C7 C8 C9 175.6(4) . . . . ? C12 C7 C8 C14 177.2(4) . . . . ? C6 C7 C8 C14 -4.3(6) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C14 C8 C9 C10 179.5(4) . . . . ? C8 C9 C10 C11 2.2(7) . . . . ? C8 C9 C10 C15 -177.2(4) . . . . ? C9 C10 C11 C12 -0.8(6) . . . . ? C15 C10 C11 C12 178.6(4) . . . . ? C9 C10 C11 C16 179.9(4) . . . . ? C15 C10 C11 C16 -0.8(6) . . . . ? C8 C7 C12 C11 4.3(6) . . . . ? C6 C7 C12 C11 -174.2(4) . . . . ? C8 C7 C12 C13 -176.2(4) . . . . ? C6 C7 C12 C13 5.3(6) . . . . ? C10 C11 C12 C7 -2.4(6) . . . . ? C16 C11 C12 C7 176.9(4) . . . . ? C10 C11 C12 C13 178.1(4) . . . . ? C16 C11 C12 C13 -2.6(6) . . . . ? C10 C11 C16 N17 -75.1(5) . . . . ? C12 C11 C16 N17 105.6(5) . . . . ? C11 C16 N17 C18 -36.2(6) . . . . ? C11 C16 N17 C21 147.9(5) . . . . ? C21 N17 C18 N19 -1.3(6) . . . . ? C16 N17 C18 N19 -177.8(4) . . . . ? N17 C18 N19 C20 1.0(6) . . . . ? N17 C18 N19 Ag1 -174.5(3) . . . 2_666 ? C18 N19 C20 C21 -0.3(6) . . . . ? Ag1 N19 C20 C21 175.1(4) 2_666 . . . ? N19 C20 C21 N17 -0.5(7) . . . . ? C18 N17 C21 C20 1.1(6) . . . . ? C16 N17 C21 C20 177.7(5) . . . . ? O25 N22 O23 Ag1 66.3(7) . . . . ? O24 N22 O23 Ag1 -113.9(7) . . . . ? N19 Ag1 O23 N22 -89.6(7) 2_666 . . . ? N1 Ag1 O23 N22 92.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.470 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.163 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 786862' #TrackingRef '- Dobrzanska_CIF 1-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety 'C19 H23 Ag N4 O2' _chemical_formula_sum 'C19 H23 Ag N4 O2' _chemical_formula_weight 447.28 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.054(10) _cell_length_b 10.406(11) _cell_length_c 10.574(11) _cell_angle_alpha 69.008(16) _cell_angle_beta 77.512(17) _cell_angle_gamma 82.171(17) _cell_volume 906.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2064 _cell_measurement_theta_min 2.412 _cell_measurement_theta_max 24.121 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7201 _exptl_absorpt_correction_T_max 0.7805 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6755 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.45 _reflns_number_total 3268 _reflns_number_gt 2830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material ? _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^)+(0.0817P)^2^+3.0575P] 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 3268 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1653 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 0.32228(6) 0.37027(5) 0.00766(6) 0.0288(2) Uani 1 1 d . . . N1 N 0.1988(7) 0.5180(6) 0.1048(6) 0.0274(13) Uani 1 1 d . . . C2 C 0.2671(8) 0.5662(7) 0.1745(7) 0.0282(16) Uani 1 1 d . . . H2 H 0.3618 0.5297 0.2019 0.034 Uiso 1 1 calc R . . N3 N 0.1840(7) 0.6757(6) 0.2023(6) 0.0265(13) Uani 1 1 d . . . C4 C 0.0548(8) 0.6967(7) 0.1476(7) 0.0270(15) Uani 1 1 d . . . H4 H -0.0262 0.7641 0.1525 0.032 Uiso 1 1 calc R . . C5 C 0.0663(8) 0.6021(7) 0.0852(7) 0.0261(15) Uani 1 1 d . . . H5 H -0.0055 0.5941 0.0353 0.031 Uiso 1 1 calc R . . C6 C 0.2311(8) 0.7597(7) 0.2717(8) 0.0278(16) Uani 1 1 d . . . H6A H 0.2895 0.8362 0.2023 0.033 Uiso 1 1 calc R . . H6B H 0.2978 0.7019 0.3365 0.033 Uiso 1 1 calc R . . C7 C 0.0949(7) 0.8179(7) 0.3496(7) 0.0219(14) Uani 1 1 d . . . C8 C 0.0321(8) 0.7375(7) 0.4830(7) 0.0261(15) Uani 1 1 d . . . C9 C -0.0995(8) 0.7866(7) 0.5525(7) 0.0261(15) Uani 1 1 d . . . H9 H -0.1424 0.7304 0.6425 0.031 Uiso 1 1 calc R . . C10 C -0.1703(8) 0.9167(8) 0.4931(7) 0.0286(16) Uani 1 1 d . . . C11 C -0.1026(8) 0.9994(7) 0.3624(7) 0.0255(15) Uani 1 1 d . . . C12 C 0.0278(7) 0.9495(7) 0.2884(7) 0.0226(14) Uani 1 1 d . . . C13 C 0.0944(9) 1.0380(7) 0.1445(7) 0.0299(16) Uani 1 1 d . . . H13A H 0.1590 1.1038 0.1494 0.045 Uiso 1 1 calc R . . H13B H 0.0124 1.0884 0.0956 0.045 Uiso 1 1 calc R . . H13C H 0.1552 0.9793 0.0952 0.045 Uiso 1 1 calc R . . C14 C 0.1055(9) 0.5969(7) 0.5544(8) 0.0330(17) Uani 1 1 d . . . H14A H 0.0402 0.5517 0.6424 0.050 Uiso 1 1 calc R . . H14B H 0.2044 0.6084 0.5712 0.050 Uiso 1 1 calc R . . H14C H 0.1191 0.5401 0.4957 0.050 Uiso 1 1 calc R . . C15 C -0.3125(8) 0.9641(9) 0.5714(8) 0.0388(19) Uani 1 1 d . . . H15A H -0.3547 0.8852 0.6491 0.058 Uiso 1 1 calc R . . H15B H -0.3866 1.0047 0.5103 0.058 Uiso 1 1 calc R . . H15C H -0.2894 1.0333 0.6061 0.058 Uiso 1 1 calc R . . C16 C -0.1711(8) 1.1453(7) 0.2989(8) 0.0292(16) Uani 1 1 d . . . H16A H -0.2130 1.1843 0.3730 0.035 Uiso 1 1 calc R . . H16B H -0.0898 1.2038 0.2351 0.035 Uiso 1 1 calc R . . N17 N -0.2923(6) 1.1501(6) 0.2232(6) 0.0257(13) Uani 1 1 d . . . C18 C -0.3912(8) 1.2610(7) 0.1817(7) 0.0270(16) Uani 1 1 d . . . H18 H -0.3956 1.3427 0.2033 0.032 Uiso 1 1 calc R . . N19 N -0.4802(7) 1.2410(6) 0.1079(6) 0.0259(13) Uani 1 1 d . . . C20 C -0.4339(8) 1.1118(8) 0.0998(7) 0.0289(16) Uani 1 1 d . . . H20 H -0.4765 1.0688 0.0518 0.035 Uiso 1 1 calc R . . C21 C -0.3193(8) 1.0549(7) 0.1700(7) 0.0264(15) Uani 1 1 d . . . H21 H -0.2679 0.9668 0.1803 0.032 Uiso 1 1 calc R . . O22 O 0.3056(6) 0.2547(5) -0.1404(5) 0.0338(12) Uani 1 1 d . . . C23 C 0.3659(8) 0.3409(7) -0.2507(8) 0.0279(16) Uani 1 1 d . . . O24 O 0.4114(6) 0.4548(5) -0.2607(5) 0.0323(12) Uani 1 1 d . . . C25 C 0.3852(9) 0.3093(8) -0.3838(8) 0.0345(18) Uani 1 1 d . . . H25A H 0.4478 0.2230 -0.3756 0.052 Uiso 1 1 calc R . . H25B H 0.4348 0.3847 -0.4609 0.052 Uiso 1 1 calc R . . H25C H 0.2856 0.2998 -0.4004 0.052 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 0.0320(3) 0.0269(3) 0.0303(3) -0.0130(2) -0.0107(2) 0.0060(2) N1 0.031(3) 0.025(3) 0.024(3) -0.007(3) -0.005(3) 0.002(2) C2 0.030(4) 0.028(4) 0.027(4) -0.010(3) -0.011(3) 0.006(3) N3 0.027(3) 0.028(3) 0.024(3) -0.009(3) -0.006(2) 0.003(2) C4 0.025(4) 0.026(4) 0.030(4) -0.010(3) -0.011(3) 0.006(3) C5 0.024(4) 0.028(4) 0.028(4) -0.007(3) -0.012(3) 0.001(3) C6 0.028(4) 0.025(4) 0.035(4) -0.014(3) -0.014(3) 0.005(3) C7 0.022(3) 0.022(3) 0.024(3) -0.009(3) -0.009(3) 0.000(3) C8 0.032(4) 0.024(4) 0.029(4) -0.009(3) -0.018(3) -0.002(3) C9 0.031(4) 0.030(4) 0.019(3) -0.006(3) -0.009(3) -0.008(3) C10 0.027(4) 0.038(4) 0.030(4) -0.017(3) -0.013(3) 0.000(3) C11 0.022(3) 0.028(4) 0.035(4) -0.019(3) -0.014(3) 0.004(3) C12 0.023(3) 0.020(3) 0.029(4) -0.010(3) -0.013(3) 0.001(3) C13 0.036(4) 0.021(4) 0.031(4) -0.007(3) -0.010(3) 0.002(3) C14 0.043(5) 0.023(4) 0.034(4) -0.006(3) -0.016(4) -0.001(3) C15 0.026(4) 0.054(5) 0.042(5) -0.025(4) -0.004(3) 0.001(4) C16 0.030(4) 0.030(4) 0.039(4) -0.020(3) -0.019(3) 0.006(3) N17 0.024(3) 0.026(3) 0.032(3) -0.015(3) -0.010(3) 0.007(2) C18 0.034(4) 0.025(4) 0.025(4) -0.012(3) -0.010(3) 0.004(3) N19 0.031(3) 0.024(3) 0.026(3) -0.009(3) -0.012(3) 0.002(2) C20 0.029(4) 0.033(4) 0.028(4) -0.016(3) -0.005(3) 0.000(3) C21 0.026(4) 0.027(4) 0.031(4) -0.017(3) -0.007(3) 0.006(3) O22 0.047(3) 0.024(3) 0.031(3) -0.007(2) -0.011(2) -0.007(2) C23 0.024(4) 0.029(4) 0.038(4) -0.017(3) -0.021(3) 0.013(3) O24 0.038(3) 0.028(3) 0.036(3) -0.015(2) -0.014(2) 0.000(2) C25 0.031(4) 0.040(4) 0.038(4) -0.019(4) -0.013(3) 0.006(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 2.199(6) . ? Ag1 N19 2.296(6) 1_645 ? Ag1 O22 2.329(5) . ? N1 C2 1.312(9) . ? N1 C5 1.393(9) . ? C2 N3 1.365(9) . ? C2 H2 0.9500 . ? N3 C4 1.373(9) . ? N3 C6 1.476(9) . ? C4 C5 1.350(10) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.510(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.396(10) . ? C7 C12 1.404(9) . ? C8 C9 1.395(10) . ? C8 C14 1.521(10) . ? C9 C10 1.402(10) . ? C9 H9 0.9500 . ? C10 C11 1.397(11) . ? C10 C15 1.498(10) . ? C11 C12 1.414(9) . ? C11 C16 1.528(10) . ? C12 C13 1.509(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.478(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.361(9) . ? N17 C21 1.373(9) . ? C18 N19 1.317(9) . ? C18 H18 0.9500 . ? N19 C20 1.380(9) . ? N19 Ag1 2.296(6) 1_465 ? C20 C21 1.351(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? O22 C23 1.253(9) . ? C23 O24 1.269(9) . ? C23 C25 1.526(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 N19 115.4(2) . 1_645 ? N1 Ag1 O22 143.2(2) . . ? N19 Ag1 O22 99.9(2) 1_645 . ? C2 N1 C5 105.5(6) . . ? C2 N1 Ag1 119.9(5) . . ? C5 N1 Ag1 132.8(5) . . ? N1 C2 N3 110.9(6) . . ? N1 C2 H2 124.5 . . ? N3 C2 H2 124.5 . . ? C2 N3 C4 107.4(6) . . ? C2 N3 C6 125.4(6) . . ? C4 N3 C6 127.1(6) . . ? C5 C4 N3 106.0(6) . . ? C5 C4 H4 127.0 . . ? N3 C4 H4 127.0 . . ? C4 C5 N1 110.0(6) . . ? C4 C5 H5 125.0 . . ? N1 C5 H5 125.0 . . ? N3 C6 C7 110.8(6) . . ? N3 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 119.6(6) . . ? C8 C7 C6 119.3(6) . . ? C12 C7 C6 121.1(6) . . ? C9 C8 C7 119.8(6) . . ? C9 C8 C14 119.2(7) . . ? C7 C8 C14 121.0(7) . . ? C8 C9 C10 121.8(7) . . ? C8 C9 H9 119.1 . . ? C10 C9 H9 119.1 . . ? C11 C10 C9 118.1(6) . . ? C11 C10 C15 122.2(7) . . ? C9 C10 C15 119.8(7) . . ? C10 C11 C12 120.9(6) . . ? C10 C11 C16 119.3(6) . . ? C12 C11 C16 119.8(6) . . ? C7 C12 C11 119.7(6) . . ? C7 C12 C13 120.4(6) . . ? C11 C12 C13 119.9(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C11 113.0(5) . . ? N17 C16 H16A 109.0 . . ? C11 C16 H16A 109.0 . . ? N17 C16 H16B 109.0 . . ? C11 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C18 N17 C21 106.8(6) . . ? C18 N17 C16 124.3(6) . . ? C21 N17 C16 128.6(6) . . ? N19 C18 N17 111.6(6) . . ? N19 C18 H18 124.2 . . ? N17 C18 H18 124.2 . . ? C18 N19 C20 105.0(6) . . ? C18 N19 Ag1 133.4(5) . 1_465 ? C20 N19 Ag1 121.6(5) . 1_465 ? C21 C20 N19 110.5(6) . . ? C21 C20 H20 124.7 . . ? N19 C20 H20 124.7 . . ? C20 C21 N17 106.1(6) . . ? C20 C21 H21 127.0 . . ? N17 C21 H21 127.0 . . ? C23 O22 Ag1 98.1(4) . . ? O22 C23 O24 124.7(7) . . ? O22 C23 C25 118.5(7) . . ? O24 C23 C25 116.8(7) . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 N19 Ag1 N1 C2 25.5(6) 1_645 . . . ? O22 Ag1 N1 C2 -172.2(5) . . . . ? N19 Ag1 N1 C5 -172.0(6) 1_645 . . . ? O22 Ag1 N1 C5 -9.8(8) . . . . ? C5 N1 C2 N3 0.9(8) . . . . ? Ag1 N1 C2 N3 167.6(5) . . . . ? N1 C2 N3 C4 0.6(8) . . . . ? N1 C2 N3 C6 -176.3(6) . . . . ? C2 N3 C4 C5 -1.8(8) . . . . ? C6 N3 C4 C5 175.0(6) . . . . ? N3 C4 C5 N1 2.4(8) . . . . ? C2 N1 C5 C4 -2.0(8) . . . . ? Ag1 N1 C5 C4 -166.3(5) . . . . ? C2 N3 C6 C7 -150.7(7) . . . . ? C4 N3 C6 C7 33.0(10) . . . . ? N3 C6 C7 C8 84.9(7) . . . . ? N3 C6 C7 C12 -93.1(8) . . . . ? C12 C7 C8 C9 2.2(10) . . . . ? C6 C7 C8 C9 -175.8(6) . . . . ? C12 C7 C8 C14 -177.6(6) . . . . ? C6 C7 C8 C14 4.4(10) . . . . ? C7 C8 C9 C10 -1.2(10) . . . . ? C14 C8 C9 C10 178.5(6) . . . . ? C8 C9 C10 C11 -1.9(10) . . . . ? C8 C9 C10 C15 179.3(6) . . . . ? C9 C10 C11 C12 4.2(10) . . . . ? C15 C10 C11 C12 -177.1(6) . . . . ? C9 C10 C11 C16 -176.0(6) . . . . ? C15 C10 C11 C16 2.8(10) . . . . ? C8 C7 C12 C11 0.0(9) . . . . ? C6 C7 C12 C11 178.0(6) . . . . ? C8 C7 C12 C13 179.7(6) . . . . ? C6 C7 C12 C13 -2.3(9) . . . . ? C10 C11 C12 C7 -3.3(10) . . . . ? C16 C11 C12 C7 176.9(6) . . . . ? C10 C11 C12 C13 177.0(6) . . . . ? C16 C11 C12 C13 -2.9(9) . . . . ? C10 C11 C16 N17 -86.8(8) . . . . ? C12 C11 C16 N17 93.0(8) . . . . ? C11 C16 N17 C18 166.1(7) . . . . ? C11 C16 N17 C21 -20.8(11) . . . . ? C21 N17 C18 N19 1.0(8) . . . . ? C16 N17 C18 N19 175.4(6) . . . . ? N17 C18 N19 C20 -1.1(8) . . . . ? N17 C18 N19 Ag1 177.6(5) . . . 1_465 ? C18 N19 C20 C21 0.7(9) . . . . ? Ag1 N19 C20 C21 -178.1(5) 1_465 . . . ? N19 C20 C21 N17 -0.1(8) . . . . ? C18 N17 C21 C20 -0.5(8) . . . . ? C16 N17 C21 C20 -174.6(7) . . . . ? N1 Ag1 O22 C23 91.8(5) . . . . ? N19 Ag1 O22 C23 -104.4(4) 1_645 . . . ? Ag1 O22 C23 O24 -2.2(7) . . . . ? Ag1 O22 C23 C25 178.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.405 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.162 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 786863' #TrackingRef '- Dobrzanska_CIF 1-5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H20 Ag Cl N4' _chemical_formula_weight 423.69 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 7.6290(15) _cell_length_b 18.696(4) _cell_length_c 13.297(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.05(3) _cell_angle_gamma 90.00 _cell_volume 1731.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2652 _cell_measurement_theta_min 2.747 _cell_measurement_theta_max 25.425 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7085 _exptl_absorpt_correction_T_max 0.7968 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8476 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3204 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material ? _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^)+(0.0396P)^2^+2.8324P] 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 3204 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.28245(6) 0.47834(2) 0.93623(3) 0.03205(17) Uani 1 1 d . . . N1 N 0.0212(6) 0.5358(2) 0.8074(3) 0.0291(10) Uani 1 1 d . . . C2 C -0.1480(9) 0.5247(3) 0.8078(5) 0.0361(13) Uani 1 1 d . . . H2 H -0.1771 0.4852 0.8433 0.043 Uiso 1 1 calc R . . N3 N -0.2763(6) 0.5755(2) 0.7525(3) 0.0269(9) Uani 1 1 d . . . C4 C -0.1798(8) 0.6231(3) 0.7154(4) 0.0307(12) Uani 1 1 d . . . H4 H -0.2308 0.6651 0.6734 0.037 Uiso 1 1 calc R . . C5 C 0.0034(8) 0.5986(3) 0.7505(4) 0.0294(12) Uani 1 1 d . . . H5 H 0.1036 0.6214 0.7375 0.035 Uiso 1 1 calc R . . C6 C -0.4716(7) 0.5823(3) 0.7475(4) 0.0299(12) Uani 1 1 d . . . H6A H -0.4731 0.6206 0.7987 0.036 Uiso 1 1 calc R . . H6B H -0.5080 0.5370 0.7723 0.036 Uiso 1 1 calc R . . C7 C -0.6176(7) 0.5996(3) 0.6334(4) 0.0270(11) Uani 1 1 d . . . C8 C -0.6964(7) 0.5434(3) 0.5585(4) 0.0276(11) Uani 1 1 d . . . C9 C -0.8299(7) 0.5593(3) 0.4536(4) 0.0305(12) Uani 1 1 d . . . H9 H -0.8865 0.5212 0.4035 0.037 Uiso 1 1 calc R . . C10 C -0.8835(7) 0.6287(3) 0.4195(4) 0.0295(12) Uani 1 1 d . . . C11 C -0.8029(7) 0.6849(3) 0.4924(4) 0.0264(11) Uani 1 1 d . . . C12 C -0.6724(7) 0.6705(3) 0.6023(4) 0.0259(11) Uani 1 1 d . . . C13 C -0.5984(8) 0.7312(3) 0.6833(4) 0.0317(12) Uani 1 1 d . . . H13A H -0.6645 0.7311 0.7329 0.048 Uiso 1 1 calc R . . H13B H -0.6224 0.7767 0.6433 0.048 Uiso 1 1 calc R . . H13C H -0.4601 0.7254 0.7264 0.048 Uiso 1 1 calc R . . C14 C -0.6407(8) 0.4664(3) 0.5891(5) 0.0338(12) Uani 1 1 d . . . H14A H -0.7174 0.4354 0.5274 0.051 Uiso 1 1 calc R . . H14B H -0.6643 0.4539 0.6540 0.051 Uiso 1 1 calc R . . H14C H -0.5042 0.4601 0.6056 0.051 Uiso 1 1 calc R . . C15 C -1.0249(8) 0.6418(3) 0.3020(4) 0.0386(13) Uani 1 1 d . . . H15A H -0.9587 0.6647 0.2609 0.058 Uiso 1 1 calc R . . H15B H -1.1281 0.6731 0.3018 0.058 Uiso 1 1 calc R . . H15C H -1.0795 0.5961 0.2671 0.058 Uiso 1 1 calc R . . C16 C -0.8571(8) 0.7603(3) 0.4546(4) 0.0312(12) Uani 1 1 d . . . H16A H -0.7420 0.7911 0.4873 0.037 Uiso 1 1 calc R . . H16B H -0.9014 0.7623 0.3735 0.037 Uiso 1 1 calc R . . N17 N -1.0092(6) 0.7891(2) 0.4846(3) 0.0273(9) Uani 1 1 d . . . C18 C -1.0323(7) 0.8586(3) 0.5008(4) 0.0275(11) Uani 1 1 d . . . H18 H -0.9457 0.8951 0.5008 0.033 Uiso 1 1 calc R . . N19 N -1.1881(6) 0.8701(2) 0.5166(3) 0.0307(10) Uani 1 1 d . . . C20 C -1.2704(8) 0.8041(3) 0.5115(4) 0.0317(12) Uani 1 1 d . . . H20 H -1.3853 0.7950 0.5210 0.038 Uiso 1 1 calc R . . C21 C -1.1616(8) 0.7541(3) 0.4909(5) 0.0336(12) Uani 1 1 d . . . H21 H -1.1862 0.7042 0.4824 0.040 Uiso 1 1 calc R . . Cl22 Cl 0.56975(17) 0.42197(7) 0.91072(11) 0.0298(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 0.0275(2) 0.0329(3) 0.0367(3) 0.00069(18) 0.01402(19) 0.00116(17) N1 0.030(2) 0.033(2) 0.029(2) -0.0022(19) 0.016(2) 0.0015(18) C2 0.044(3) 0.035(3) 0.031(3) -0.005(2) 0.018(3) -0.003(3) N3 0.027(2) 0.029(2) 0.025(2) 0.0015(18) 0.0108(18) 0.0005(18) C4 0.035(3) 0.033(3) 0.027(3) 0.001(2) 0.015(2) -0.002(2) C5 0.032(3) 0.031(3) 0.029(3) -0.004(2) 0.016(2) -0.004(2) C6 0.031(3) 0.035(3) 0.026(3) 0.000(2) 0.014(2) 0.002(2) C7 0.024(3) 0.036(3) 0.023(3) 0.002(2) 0.013(2) 0.002(2) C8 0.027(3) 0.030(3) 0.029(3) 0.002(2) 0.015(2) 0.001(2) C9 0.029(3) 0.033(3) 0.030(3) -0.001(2) 0.012(2) 0.002(2) C10 0.031(3) 0.034(3) 0.026(3) 0.001(2) 0.014(2) 0.001(2) C11 0.023(2) 0.029(3) 0.030(3) 0.004(2) 0.013(2) 0.004(2) C12 0.023(3) 0.031(3) 0.025(3) 0.001(2) 0.012(2) 0.002(2) C13 0.032(3) 0.033(3) 0.028(3) -0.001(2) 0.010(2) 0.002(2) C14 0.039(3) 0.029(3) 0.036(3) 0.003(2) 0.018(3) 0.005(2) C15 0.041(3) 0.045(3) 0.027(3) 0.000(3) 0.010(3) 0.004(3) C16 0.032(3) 0.038(3) 0.027(3) 0.004(2) 0.016(2) 0.005(2) N17 0.026(2) 0.033(2) 0.023(2) 0.0018(18) 0.0095(18) 0.0024(18) C18 0.025(3) 0.029(3) 0.027(3) 0.002(2) 0.010(2) 0.002(2) N19 0.033(2) 0.035(3) 0.024(2) -0.0005(19) 0.0111(19) 0.000(2) C20 0.029(3) 0.036(3) 0.034(3) -0.001(2) 0.017(2) 0.002(2) C21 0.036(3) 0.035(3) 0.039(3) -0.002(3) 0.024(3) -0.005(2) Cl22 0.0273(6) 0.0311(7) 0.0326(7) 0.0000(5) 0.0138(5) -0.0001(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 N1 2.298(4) . ? Ag1 N19 2.319(4) 2_446 ? Ag1 Cl22 2.5761(14) . ? Ag1 Cl22 2.6489(15) 3_667 ? Ag1 Ag1 3.1561(13) 3_667 ? N1 C2 1.310(7) . ? N1 C5 1.373(7) . ? C2 N3 1.347(7) . ? C2 H2 0.9500 . ? N3 C4 1.370(7) . ? N3 C6 1.470(6) . ? C4 C5 1.360(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.506(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.401(7) . ? C7 C8 1.403(7) . ? C8 C9 1.383(7) . ? C8 C14 1.509(7) . ? C9 C10 1.380(7) . ? C9 H9 0.9500 . ? C10 C11 1.391(7) . ? C10 C15 1.514(7) . ? C11 C12 1.419(7) . ? C11 C16 1.499(7) . ? C12 C13 1.507(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N17 1.474(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.341(6) . ? N17 C21 1.365(6) . ? C18 N19 1.306(6) . ? C18 H18 0.9500 . ? N19 C20 1.373(7) . ? C20 C21 1.350(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 N19 109.85(16) . 2_446 ? N1 Ag1 Cl22 128.25(11) . . ? N19 Ag1 Cl22 93.04(12) 2_446 . ? N1 Ag1 Cl22 102.25(11) . 3_667 ? N19 Ag1 Cl22 119.22(11) 2_446 3_667 ? Cl22 Ag1 Cl22 105.69(4) . 3_667 ? N1 Ag1 Ag1 133.11(11) . 3_667 ? N19 Ag1 Ag1 116.93(11) 2_446 3_667 ? Cl22 Ag1 Ag1 53.90(3) . 3_667 ? Cl22 Ag1 Ag1 51.79(3) 3_667 3_667 ? C2 N1 C5 105.2(5) . . ? C2 N1 Ag1 118.6(4) . . ? C5 N1 Ag1 132.2(3) . . ? N1 C2 N3 112.6(5) . . ? N1 C2 H2 123.7 . . ? N3 C2 H2 123.7 . . ? C2 N3 C4 106.1(5) . . ? C2 N3 C6 125.7(4) . . ? C4 N3 C6 127.7(4) . . ? C5 C4 N3 106.6(5) . . ? C5 C4 H4 126.7 . . ? N3 C4 H4 126.7 . . ? C4 C5 N1 109.6(5) . . ? C4 C5 H5 125.2 . . ? N1 C5 H5 125.2 . . ? N3 C6 C7 112.6(4) . . ? N3 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N3 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C12 C7 C8 120.6(5) . . ? C12 C7 C6 120.6(5) . . ? C8 C7 C6 118.8(5) . . ? C9 C8 C7 118.8(5) . . ? C9 C8 C14 119.2(5) . . ? C7 C8 C14 122.0(5) . . ? C10 C9 C8 122.1(5) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 119.6(5) . . ? C9 C10 C15 118.8(5) . . ? C11 C10 C15 121.6(5) . . ? C10 C11 C12 120.0(5) . . ? C10 C11 C16 119.6(5) . . ? C12 C11 C16 120.4(5) . . ? C7 C12 C11 118.8(5) . . ? C7 C12 C13 121.5(5) . . ? C11 C12 C13 119.7(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C11 113.2(4) . . ? N17 C16 H16A 108.9 . . ? C11 C16 H16A 108.9 . . ? N17 C16 H16B 108.9 . . ? C11 C16 H16B 108.9 . . ? H16A C16 H16B 107.8 . . ? C18 N17 C21 106.5(4) . . ? C18 N17 C16 124.5(4) . . ? C21 N17 C16 128.7(4) . . ? N19 C18 N17 111.9(5) . . ? N19 C18 H18 124.1 . . ? N17 C18 H18 124.1 . . ? C18 N19 C20 105.8(4) . . ? C18 N19 Ag1 126.1(4) . 2_456 ? C20 N19 Ag1 127.7(3) . 2_456 ? C21 C20 N19 109.0(5) . . ? C21 C20 H20 125.5 . . ? N19 C20 H20 125.5 . . ? C20 C21 N17 106.9(5) . . ? C20 C21 H21 126.6 . . ? N17 C21 H21 126.6 . . ? Ag1 Cl22 Ag1 74.31(4) . 3_667 ? 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 N19 Ag1 N1 C2 29.7(4) 2_446 . . . ? Cl22 Ag1 N1 C2 140.5(3) . . . . ? Cl22 Ag1 N1 C2 -97.9(4) 3_667 . . . ? Ag1 Ag1 N1 C2 -146.3(3) 3_667 . . . ? N19 Ag1 N1 C5 -176.5(4) 2_446 . . . ? Cl22 Ag1 N1 C5 -65.6(5) . . . . ? Cl22 Ag1 N1 C5 56.0(4) 3_667 . . . ? Ag1 Ag1 N1 C5 7.5(5) 3_667 . . . ? C5 N1 C2 N3 1.5(6) . . . . ? Ag1 N1 C2 N3 161.7(3) . . . . ? N1 C2 N3 C4 -0.9(6) . . . . ? N1 C2 N3 C6 -173.4(5) . . . . ? C2 N3 C4 C5 0.0(6) . . . . ? C6 N3 C4 C5 172.2(5) . . . . ? N3 C4 C5 N1 0.9(6) . . . . ? C2 N1 C5 C4 -1.4(6) . . . . ? Ag1 N1 C5 C4 -157.8(4) . . . . ? C2 N3 C6 C7 -137.4(5) . . . . ? C4 N3 C6 C7 51.9(7) . . . . ? N3 C6 C7 C12 -95.4(6) . . . . ? N3 C6 C7 C8 84.0(6) . . . . ? C12 C7 C8 C9 -0.3(7) . . . . ? C6 C7 C8 C9 -179.8(5) . . . . ? C12 C7 C8 C14 180.0(5) . . . . ? C6 C7 C8 C14 0.5(7) . . . . ? C7 C8 C9 C10 2.0(8) . . . . ? C14 C8 C9 C10 -178.3(5) . . . . ? C8 C9 C10 C11 -0.5(8) . . . . ? C8 C9 C10 C15 177.7(5) . . . . ? C9 C10 C11 C12 -2.6(7) . . . . ? C15 C10 C11 C12 179.3(5) . . . . ? C9 C10 C11 C16 178.4(5) . . . . ? C15 C10 C11 C16 0.3(7) . . . . ? C8 C7 C12 C11 -2.6(7) . . . . ? C6 C7 C12 C11 176.8(4) . . . . ? C8 C7 C12 C13 176.4(5) . . . . ? C6 C7 C12 C13 -4.2(7) . . . . ? C10 C11 C12 C7 4.1(7) . . . . ? C16 C11 C12 C7 -176.9(5) . . . . ? C10 C11 C12 C13 -174.9(5) . . . . ? C16 C11 C12 C13 4.1(7) . . . . ? C10 C11 C16 N17 96.9(6) . . . . ? C12 C11 C16 N17 -82.1(6) . . . . ? C11 C16 N17 C18 152.6(5) . . . . ? C11 C16 N17 C21 -34.4(7) . . . . ? C21 N17 C18 N19 -0.2(6) . . . . ? C16 N17 C18 N19 174.1(4) . . . . ? N17 C18 N19 C20 0.7(6) . . . . ? N17 C18 N19 Ag1 174.2(3) . . . 2_456 ? C18 N19 C20 C21 -0.9(6) . . . . ? Ag1 N19 C20 C21 -174.3(4) 2_456 . . . ? N19 C20 C21 N17 0.8(6) . . . . ? C18 N17 C21 C20 -0.4(6) . . . . ? C16 N17 C21 C20 -174.4(5) . . . . ? N1 Ag1 Cl22 Ag1 120.14(14) . . . 3_667 ? N19 Ag1 Cl22 Ag1 -121.51(11) 2_446 . . 3_667 ? Cl22 Ag1 Cl22 Ag1 0.0 3_667 . . 3_667 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.038 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.116 #===END