# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2185 # data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir, Please consider this CIF submission as supplementary data for a paper submitted to J. Chem. Soc., Dalton Trans. Xiao-Ming Chen, June 28, 2000. ; #========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ # 3. TITLE AND AUTHOR LIST _publ_section_title ; Influence of ligand backbones and counter ions on structures of helical silver(I) complexes with di-Schiff bases derived from diamine and phthalaldehydes ; loop_ _publ_author_name _publ_author_address 'Zhu, Hai-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; 'Tong, Ye-Xiang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; 'Chen, Xiao-Ming ' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; #============================================================ data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H52 Ag2 Cl2 N8 O12' _chemical_formula_weight 1027.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.651(4) _cell_length_b 14.455(4) _cell_length_c 20.466(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.880(10) _cell_angle_gamma 90.00 _cell_volume 4326.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type 'semi-empirical based on psi-scan' _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.775 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method \w _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 7260 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.78 _reflns_number_total 6795 _reflns_number_gt 3554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+10.1665P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6795 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1401 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.70393(4) 0.80617(5) 0.06164(3) 0.0778(2) Uani 1 d . . . Ag2 Ag 1.16351(4) 0.74877(5) 0.03797(3) 0.0851(2) Uani 1 d . . . N1 N 0.5578(5) 0.7263(5) 0.0040(4) 0.104(3) Uani 1 d . . . N2 N 0.6567(4) 0.8552(4) -0.0526(3) 0.0724(19) Uani 1 d . . . H2C H 0.6536 0.9142 -0.0396 0.120 Uiso 1 d R . . N3 N 1.0948(4) 0.8476(4) 0.0949(3) 0.0721(18) Uani 1 d . . . N4 N 1.2536(4) 0.7309(4) 0.1592(3) 0.081(2) Uani 1 d . . . H4N H 1.2955 0.7826 0.1600 0.120 Uiso 1 d R . . O1 O 0.5702(6) 0.6286(6) 0.1323(6) 0.221(4) Uani 1 d . . . H1C H 0.5127 0.6345 0.1120 0.080 Uiso 1 d R . . O2 O 1.3870(7) 0.6633(8) 0.1041(5) 0.229(5) Uani 1 d . . . H2 H 1.4478 0.6855 0.1249 0.120 Uiso 1 d R . . C1 C 0.6067(9) 0.5893(9) 0.0844(7) 0.170(5) Uani 1 d . . . H1A H 0.6059 0.5230 0.0872 0.120 Uiso 1 d R . . H1B H 0.6688 0.6101 0.0967 0.120 Uiso 1 d R . . C2 C 0.5491(9) 0.6274(9) 0.0122(7) 0.177(6) Uani 1 d . . . H2A H 0.5664 0.5962 -0.0227 0.120 Uiso 1 d R . . H2B H 0.4865 0.6121 0.0042 0.120 Uiso 1 d R . . C3 C 0.5289(6) 0.7504(7) -0.0689(5) 0.115(4) Uani 1 d . . . H3A H 0.4639 0.7434 -0.0908 0.120 Uiso 1 d R . . H3B H 0.5577 0.7098 -0.0919 0.120 Uiso 1 d R . . C4 C 0.5566(5) 0.8464(7) -0.0773(4) 0.100(3) Uani 1 d . . . H4A H 0.5318 0.8645 -0.1256 0.120 Uiso 1 d R . . H4B H 0.5315 0.8865 -0.0513 0.120 Uiso 1 d R . . C5 C 0.6979(6) 0.8805(5) -0.0940(4) 0.077(2) Uani 1 d . . . H5A H 0.6598 0.8965 -0.1409 0.120 Uiso 1 d R . . C6 C 0.7955(5) 0.8854(5) -0.0764(4) 0.066(2) Uani 1 d . . . C7 C 0.8257(6) 0.8876(6) -0.1329(4) 0.081(3) Uani 1 d . . . H7A H 0.7824 0.8900 -0.1800 0.120 Uiso 1 d R . . C8 C 0.9175(6) 0.8856(6) -0.1202(4) 0.092(3) Uani 1 d . . . H8A H 0.9382 0.8878 -0.1590 0.120 Uiso 1 d R . . C9 C 0.9805(5) 0.8815(5) -0.0537(4) 0.076(2) Uani 1 d . . . H9A H 1.0444 0.8770 -0.0465 0.120 Uiso 1 d R . . C10 C 0.9518(5) 0.8831(4) 0.0036(4) 0.063(2) Uani 1 d . . . C11 C 0.8580(5) 0.8861(5) -0.0090(3) 0.061(2) Uani 1 d . . . H11A H 0.8365 0.8893 0.0294 0.120 Uiso 1 d R . . C12 C 1.0152(5) 0.8818(5) 0.0748(4) 0.064(2) Uani 1 d . . . H12A H 0.9956 0.9093 0.1098 0.120 Uiso 1 d R . . C13 C 1.1508(6) 0.8560(7) 0.1676(4) 0.097(3) Uani 1 d . . . H13A H 1.1150 0.8787 0.1938 0.120 Uiso 1 d R . . H13B H 1.1985 0.8999 0.1718 0.120 Uiso 1 d R . . C14 C 1.1935(6) 0.7652(7) 0.1969(4) 0.105(4) Uani 1 d . . . H14A H 1.2294 0.7709 0.2458 0.120 Uiso 1 d R . . H14B H 1.1457 0.7211 0.1919 0.120 Uiso 1 d R . . C15 C 1.3021(7) 0.6415(7) 0.1811(5) 0.127(4) Uani 1 d . . . H15A H 1.2569 0.5956 0.1790 0.120 Uiso 1 d R . . H15B H 1.3410 0.6476 0.2292 0.120 Uiso 1 d R . . C16 C 1.3676(12) 0.6201(11) 0.1578(11) 0.222(10) Uani 1 d . . . H16A H 1.4175 0.5865 0.1905 0.120 Uiso 1 d R . . H16B H 1.3306 0.5753 0.1254 0.120 Uiso 1 d R . . N5 N 1.2536(4) 0.7531(4) -0.0335(3) 0.0734(18) Uani 1 d . . . H5B H 1.3062 0.7244 -0.0088 0.120 Uiso 1 d R . . N6 N 1.1053(5) 0.6267(4) -0.0430(3) 0.0815(19) Uani 1 d . . . N7 N 0.8425(4) 0.7230(4) 0.1283(3) 0.076(2) Uani 1 d . . . N8 N 0.7360(4) 0.8498(4) 0.1767(3) 0.0674(17) Uani 1 d . . . H8B H 0.7744 0.8983 0.1849 0.120 Uiso 1 d R . . O3 O 1.4120(4) 0.8546(6) 0.0509(3) 0.147(3) Uani 1 d . . . H3C H 1.4565 0.8915 0.0566 0.080 Uiso 1 d R . . O4 O 0.5768(4) 0.9524(4) 0.0829(3) 0.105(2) Uani 1 d . . . H4C H 0.5270 0.9227 0.0730 0.080 Uiso 1 d R . . C17 C 1.3280(6) 0.9005(7) 0.0083(5) 0.109(3) Uani 1 d . . . H17A H 1.3408 0.9600 -0.0069 0.120 Uiso 1 d R . . H17B H 1.2891 0.9090 0.0349 0.120 Uiso 1 d R . . C18 C 1.2802(6) 0.8414(6) -0.0531(4) 0.090(3) Uani 1 d . . . H18A H 1.2263 0.8718 -0.0839 0.120 Uiso 1 d R . . H18B H 1.3208 0.8319 -0.0783 0.120 Uiso 1 d R . . C19 C 1.2095(6) 0.6938(6) -0.0943(4) 0.092(3) Uani 1 d . . . H19A H 1.2513 0.6805 -0.1179 0.120 Uiso 1 d R . . H19B H 1.1582 0.7266 -0.1263 0.120 Uiso 1 d R . . C20 C 1.1741(6) 0.6075(6) -0.0752(5) 0.100(3) Uani 1 d . . . H20A H 1.1493 0.5676 -0.1150 0.120 Uiso 1 d R . . H20B H 1.2245 0.5763 -0.0411 0.120 Uiso 1 d R . . C21 C 1.0264(6) 0.5933(5) -0.0728(4) 0.078(2) Uani 1 d . . . H21A H 1.0161 0.5576 -0.1145 0.120 Uiso 1 d R . . C22 C 0.9486(5) 0.6058(5) -0.0496(4) 0.066(2) Uani 1 d . . . C23 C 0.8593(5) 0.5921(5) -0.0959(4) 0.076(2) Uani 1 d . . . H23A H 0.8499 0.5713 -0.1426 0.120 Uiso 1 d R . . C24 C 0.7850(6) 0.6077(6) -0.0765(4) 0.084(3) Uani 1 d . . . H24A H 0.7240 0.5978 -0.1090 0.120 Uiso 1 d R . . C25 C 0.7996(5) 0.6371(5) -0.0100(4) 0.075(2) Uani 1 d . . . H25A H 0.7480 0.6499 0.0035 0.120 Uiso 1 d R . . C26 C 0.8864(5) 0.6499(5) 0.0392(4) 0.063(2) Uani 1 d . . . C27 C 0.9602(5) 0.6338(5) 0.0198(3) 0.062(2) Uani 1 d . . . H27A H 1.0208 0.6425 0.0533 0.120 Uiso 1 d R . . C28 C 0.9023(5) 0.6834(5) 0.1106(4) 0.067(2) Uani 1 d . . . H28A H 0.9615 0.6739 0.1458 0.120 Uiso 1 d R . . C29 C 0.8702(6) 0.7517(7) 0.2018(4) 0.099(3) Uani 1 d . . . H29A H 0.9070 0.8066 0.2089 0.120 Uiso 1 d R . . H29B H 0.9059 0.7041 0.2320 0.120 Uiso 1 d R . . C30 C 0.7869(6) 0.7736(6) 0.2198(4) 0.086(3) Uani 1 d . . . H30A H 0.7484 0.7199 0.2101 0.120 Uiso 1 d R . . H30B H 0.8036 0.7886 0.2684 0.120 Uiso 1 d R . . C31 C 0.6584(5) 0.8796(6) 0.1947(4) 0.088(3) Uani 1 d . . . H31A H 0.6768 0.8896 0.2442 0.120 Uiso 1 d R . . H31B H 0.6137 0.8310 0.1820 0.120 Uiso 1 d R . . C32 C 0.6137(6) 0.9641(7) 0.1560(4) 0.101(3) Uani 1 d . . . H32A H 0.5676 0.9866 0.1728 0.120 Uiso 1 d R . . H32B H 0.6603 1.0106 0.1651 0.120 Uiso 1 d R . . Cl1 Cl 1.07433(13) 0.53708(14) 0.27669(9) 0.0707(6) Uani 1 d . . . O5 O 1.1278(4) 0.5160(5) 0.2362(3) 0.129(2) Uani 1 d . . . O6 O 1.1141(4) 0.4971(5) 0.3440(3) 0.108(2) Uani 1 d . . . O7 O 1.0709(4) 0.6347(4) 0.2843(3) 0.107(2) Uani 1 d . . . O8 O 0.9843(4) 0.5052(5) 0.2437(3) 0.129(3) Uani 1 d . . . Cl2 Cl 1.4288(2) 0.9265(2) 0.26046(14) 0.1346(11) Uani 1 d . . . O9 O 1.3951(7) 0.8976(8) 0.1912(5) 0.214(2) Uani 1 d . . . O10 O 1.5212(7) 0.9157(8) 0.3031(5) 0.214(2) Uani 1 d . . . O11 O 1.4242(7) 1.0239(9) 0.2540(5) 0.214(2) Uani 1 d . . . O12 O 1.3780(7) 0.8923(8) 0.2971(5) 0.214(2) Uani 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 0.0818(4) 0.0927(5) 0.0606(3) 0.0013(3) 0.0275(3) -0.0043(4) Ag2 0.0899(4) 0.0945(5) 0.0859(4) -0.0140(4) 0.0497(3) -0.0001(4) N1 0.102(5) 0.110(6) 0.107(5) -0.029(4) 0.046(4) -0.037(5) N2 0.066(4) 0.076(4) 0.069(4) -0.010(3) 0.016(3) 0.007(3) N3 0.072(4) 0.077(4) 0.070(4) -0.008(3) 0.028(3) 0.004(4) N4 0.072(4) 0.068(4) 0.099(5) 0.017(4) 0.027(4) -0.005(3) O1 0.181(7) 0.178(9) 0.364(12) 0.005(8) 0.172(7) 0.000(7) O2 0.220(9) 0.284(12) 0.165(8) 0.030(8) 0.045(7) 0.144(9) C1 0.181(12) 0.097(9) 0.233(15) -0.031(10) 0.136(11) -0.028(10) C2 0.220(12) 0.158(12) 0.175(11) -0.030(9) 0.096(10) -0.097(10) C3 0.074(5) 0.132(8) 0.135(8) -0.055(7) 0.032(6) -0.015(6) C4 0.076(6) 0.135(8) 0.076(5) -0.015(6) 0.011(5) 0.028(6) C5 0.099(6) 0.084(6) 0.047(4) 0.018(4) 0.026(4) 0.018(5) C6 0.080(5) 0.061(5) 0.070(4) 0.014(4) 0.041(4) 0.010(4) C7 0.110(6) 0.082(6) 0.055(4) 0.002(4) 0.032(4) -0.011(5) C8 0.125(6) 0.104(7) 0.069(5) 0.004(5) 0.062(4) -0.009(6) C9 0.100(5) 0.066(5) 0.081(5) -0.005(4) 0.057(4) -0.011(4) C10 0.082(5) 0.040(4) 0.073(4) -0.002(3) 0.037(4) -0.006(4) C11 0.081(5) 0.056(5) 0.051(4) 0.005(3) 0.029(4) 0.006(4) C12 0.077(5) 0.051(5) 0.073(4) -0.013(4) 0.038(4) -0.005(4) C13 0.075(5) 0.129(8) 0.084(6) -0.021(6) 0.025(5) 0.019(6) C14 0.075(5) 0.174(10) 0.069(5) -0.001(6) 0.028(4) -0.024(6) C15 0.112(8) 0.107(8) 0.125(8) 0.035(7) -0.003(7) -0.004(7) C16 0.248(18) 0.148(14) 0.27(3) 0.122(16) 0.188(19) 0.116(14) N5 0.078(4) 0.075(4) 0.083(4) 0.006(3) 0.049(3) -0.004(4) N6 0.108(4) 0.071(4) 0.086(4) -0.022(3) 0.061(3) -0.011(4) N7 0.090(4) 0.089(5) 0.053(3) 0.009(3) 0.029(3) 0.026(4) N8 0.065(3) 0.077(4) 0.065(3) -0.002(3) 0.028(3) -0.005(3) O3 0.091(4) 0.218(8) 0.128(5) -0.004(5) 0.033(4) -0.063(5) O4 0.077(3) 0.136(5) 0.103(4) -0.010(4) 0.035(3) -0.001(4) C17 0.108(7) 0.098(7) 0.136(8) 0.002(6) 0.063(6) -0.019(6) C18 0.093(6) 0.091(6) 0.088(6) 0.013(5) 0.033(5) -0.016(5) C19 0.120(6) 0.084(6) 0.096(5) -0.008(5) 0.070(5) -0.013(6) C20 0.123(6) 0.075(6) 0.134(7) -0.020(5) 0.082(5) -0.003(5) C21 0.118(6) 0.055(5) 0.079(5) -0.010(4) 0.058(4) -0.004(5) C22 0.094(5) 0.040(4) 0.073(4) -0.010(3) 0.041(4) -0.007(4) C23 0.093(6) 0.074(5) 0.066(4) -0.019(4) 0.032(4) -0.013(5) C24 0.082(5) 0.096(6) 0.076(5) -0.018(5) 0.027(5) -0.007(5) C25 0.071(5) 0.069(5) 0.086(5) -0.002(4) 0.030(4) -0.005(4) C26 0.084(5) 0.044(4) 0.074(4) 0.007(3) 0.044(4) 0.002(4) C27 0.084(5) 0.044(4) 0.065(4) 0.004(3) 0.033(4) -0.007(4) C28 0.090(5) 0.056(5) 0.059(4) 0.009(4) 0.031(4) 0.002(4) C29 0.111(6) 0.126(7) 0.059(5) 0.009(5) 0.028(4) 0.051(6) C30 0.120(6) 0.091(6) 0.054(4) 0.002(4) 0.040(4) 0.017(5) C31 0.084(5) 0.115(7) 0.078(5) -0.007(5) 0.043(4) 0.005(5) C32 0.100(6) 0.124(8) 0.077(5) -0.019(5) 0.031(5) 0.024(6) Cl1 0.0727(11) 0.0820(14) 0.0645(10) -0.0042(10) 0.0332(9) 0.0038(11) O5 0.155(5) 0.145(6) 0.127(4) -0.008(4) 0.101(4) 0.020(5) O6 0.114(4) 0.126(5) 0.080(4) 0.018(4) 0.030(3) -0.003(4) O7 0.125(5) 0.071(4) 0.124(5) -0.006(3) 0.044(4) 0.005(4) O8 0.099(5) 0.160(6) 0.114(5) -0.028(5) 0.021(4) -0.039(5) Cl2 0.144(2) 0.148(2) 0.0893(17) 0.0146(17) 0.0142(17) -0.057(2) O9 0.215(5) 0.264(6) 0.128(3) 0.020(4) 0.020(3) -0.073(4) O10 0.215(5) 0.264(6) 0.128(3) 0.020(4) 0.020(3) -0.073(4) O11 0.215(5) 0.264(6) 0.128(3) 0.020(4) 0.020(3) -0.073(4) O12 0.215(5) 0.264(6) 0.128(3) 0.020(4) 0.020(3) -0.073(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 N2 2.298(6) . ? Ag1 N8 2.313(5) . ? Ag1 N7 2.430(6) . ? Ag1 N1 2.456(7) . ? Ag2 N3 2.335(6) . ? Ag2 N5 2.366(6) . ? Ag2 N6 2.369(6) . ? Ag2 N4 2.391(6) . ? N1 C2 1.452(13) . ? N1 C3 1.439(12) . ? N2 C5 1.288(9) . ? N2 C4 1.471(9) . ? N3 C12 1.265(8) . ? N3 C13 1.438(9) . ? N4 C15 1.485(11) . ? N4 C14 1.498(11) . ? O1 C1 1.417(14) . ? O2 C16 1.389(18) . ? C1 C2 1.533(17) . ? C3 C4 1.482(13) . ? C5 C6 1.441(10) . ? C6 C11 1.378(9) . ? C6 C7 1.397(10) . ? C7 C8 1.365(11) . ? C8 C9 1.368(10) . ? C9 C10 1.397(10) . ? C10 C11 1.398(10) . ? C10 C12 1.441(9) . ? C13 C14 1.498(12) . ? C15 C16 1.313(17) . ? N5 C18 1.444(10) . ? N5 C19 1.466(9) . ? N6 C21 1.262(9) . ? N6 C20 1.474(10) . ? N7 C28 1.255(9) . ? N7 C29 1.469(9) . ? N8 C31 1.455(9) . ? N8 C30 1.458(9) . ? O3 C17 1.453(11) . ? O4 C32 1.408(9) . ? C17 C18 1.483(12) . ? C19 C20 1.475(11) . ? C21 C22 1.468(11) . ? C22 C23 1.395(10) . ? C22 C27 1.424(9) . ? C23 C24 1.375(11) . ? C24 C25 1.365(10) . ? C25 C26 1.386(9) . ? C26 C27 1.369(10) . ? C26 C28 1.474(10) . ? C29 C30 1.508(12) . ? C31 C32 1.488(12) . ? Cl1 O8 1.405(6) . ? Cl1 O5 1.405(6) . ? Cl1 O6 1.417(6) . ? Cl1 O7 1.423(6) . ? Cl2 O12 1.365(11) . ? Cl2 O9 1.389(9) . ? Cl2 O10 1.406(10) . ? Cl2 O11 1.413(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N8 145.7(2) . . ? N2 Ag1 N7 128.5(2) . . ? N8 Ag1 N7 74.7(2) . . ? N2 Ag1 N1 75.5(2) . . ? N8 Ag1 N1 116.4(2) . . ? N7 Ag1 N1 122.0(2) . . ? N3 Ag2 N5 140.7(2) . . ? N3 Ag2 N6 132.4(2) . . ? N5 Ag2 N6 75.7(2) . . ? N3 Ag2 N4 75.8(2) . . ? N5 Ag2 N4 112.5(2) . . ? N6 Ag2 N4 125.7(2) . . ? C2 N1 C3 110.5(8) . . ? C2 N1 Ag1 121.1(7) . . ? C3 N1 Ag1 106.2(6) . . ? C5 N2 C4 121.3(6) . . ? C5 N2 Ag1 134.6(5) . . ? C4 N2 Ag1 103.9(5) . . ? C12 N3 C13 118.1(7) . . ? C12 N3 Ag2 130.7(5) . . ? C13 N3 Ag2 110.4(5) . . ? C15 N4 C14 118.7(8) . . ? C15 N4 Ag2 117.1(5) . . ? C14 N4 Ag2 104.6(4) . . ? O1 C1 C2 106.2(11) . . ? N1 C2 C1 114.7(10) . . ? N1 C3 C4 110.5(8) . . ? N2 C4 C3 111.1(7) . . ? N2 C5 C6 125.7(6) . . ? C11 C6 C7 120.0(7) . . ? C11 C6 C5 124.2(7) . . ? C7 C6 C5 115.8(7) . . ? C8 C7 C6 119.0(7) . . ? C7 C8 C9 121.8(8) . . ? C8 C9 C10 120.0(8) . . ? C9 C10 C11 118.4(7) . . ? C9 C10 C12 122.5(7) . . ? C11 C10 C12 119.1(7) . . ? C6 C11 C10 120.5(7) . . ? N3 C12 C10 125.3(7) . . ? N3 C13 C14 111.2(7) . . ? C13 C14 N4 110.9(7) . . ? C16 C15 N4 118.5(11) . . ? C15 C16 O2 126.9(13) . . ? C18 N5 C19 112.0(6) . . ? C18 N5 Ag2 119.3(5) . . ? C19 N5 Ag2 107.8(5) . . ? C21 N6 C20 117.1(7) . . ? C21 N6 Ag2 133.6(6) . . ? C20 N6 Ag2 107.1(5) . . ? C28 N7 C29 116.5(6) . . ? C28 N7 Ag1 132.2(5) . . ? C29 N7 Ag1 108.3(5) . . ? C31 N8 C30 113.3(6) . . ? C31 N8 Ag1 116.2(4) . . ? C30 N8 Ag1 106.5(4) . . ? O3 C17 C18 108.8(8) . . ? N5 C18 C17 112.4(7) . . ? N5 C19 C20 112.1(7) . . ? C19 C20 N6 111.2(7) . . ? N6 C21 C22 125.3(7) . . ? C23 C22 C27 117.4(7) . . ? C23 C22 C21 120.5(7) . . ? C27 C22 C21 122.1(7) . . ? C24 C23 C22 121.7(7) . . ? C25 C24 C23 118.8(7) . . ? C24 C25 C26 122.6(8) . . ? C27 C26 C25 118.4(7) . . ? C27 C26 C28 118.9(7) . . ? C25 C26 C28 122.7(7) . . ? C26 C27 C22 121.1(7) . . ? N7 C28 C26 123.8(7) . . ? N7 C29 C30 110.1(6) . . ? N8 C30 C29 110.1(7) . . ? N8 C31 C32 112.6(7) . . ? O4 C32 C31 113.9(7) . . ? O8 Cl1 O5 110.6(4) . . ? O8 Cl1 O6 110.6(4) . . ? O5 Cl1 O6 109.7(4) . . ? O8 Cl1 O7 107.9(4) . . ? O5 Cl1 O7 109.4(4) . . ? O6 Cl1 O7 108.6(4) . . ? O12 Cl2 O9 111.6(6) . . ? O12 Cl2 O10 106.9(6) . . ? O9 Cl2 O10 122.2(7) . . ? O12 Cl2 O11 113.1(8) . . ? O9 Cl2 O11 102.5(6) . . ? O10 Cl2 O11 100.1(6) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 0.677 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.083 #============================================================ data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 Ag2 F12 N8 O4.50 P2' _chemical_formula_weight 1127.50 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' '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 MONOCLINIC _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.884(2) _cell_length_b 15.4220(10) _cell_length_c 20.1870(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.310(4) _cell_angle_gamma 90.00 _cell_volume 8992.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4552 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type 'semi-empirical based on psi-scan' _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.721 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method ? _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% NONE _diffrn_reflns_number 7053 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 24.0 _reflns_number_total 7262 _reflns_number_gt 4977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1309P)^2^+33.9431P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7053 _refine_ls_number_parameters 570 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2249 _refine_ls_wR_factor_gt 0.2073 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.12513(2) 0.13223(4) 0.02929(3) 0.07793(19) Uani 1 d . . . Ag2 Ag 0.10688(2) -0.34578(4) 0.05427(3) 0.0831(2) Uani 1 d . . . N1 N 0.0921(3) -0.3536(4) 0.1657(3) 0.085(2) Uani 1 d . . . H1C H 0.0737 -0.3087 0.1764 0.120 Uiso 1 d R . . N2 N 0.1631(2) -0.2444(4) 0.1096(3) 0.0839(19) Uani 1 d . . . N3 N 0.1655(2) 0.1030(3) -0.0691(3) 0.0676(15) Uani 1 d . . . N4 N 0.10374(19) 0.2496(4) -0.0390(3) 0.0669(15) Uani 1 d . . . H4C H 0.1223 0.2939 -0.0273 0.150 Uiso 1 d R . . O1 O 0.0257(2) -0.4534(5) 0.0797(4) 0.121(2) Uani 1 d . . . H1 H 0.0443 -0.5008 0.0717 0.150 Uiso 1 d R . . O2 O 0.0716(3) 0.3806(5) 0.0494(5) 0.177(4) Uani 1 d . . . H2D H 0.0586 0.4286 0.0584 0.120 Uiso 1 d R . . C1 C 0.0237(4) -0.4466(7) 0.1504(5) 0.118(3) Uani 1 d . . . H1A H 0.0096 -0.4980 0.1681 0.150 Uiso 1 d R . . H1B H 0.0040 -0.3985 0.1607 0.150 Uiso 1 d R . . C2 C 0.0686(3) -0.4323(7) 0.1843(5) 0.105(3) Uani 1 d . . . H2A H 0.0641 -0.4318 0.2313 0.150 Uiso 1 d R . . H2B H 0.0885 -0.4803 0.1740 0.150 Uiso 1 d R . . C3 C 0.1352(3) -0.3400(6) 0.1991(4) 0.093(3) Uani 1 d . . . H3A H 0.1561 -0.3846 0.1849 0.150 Uiso 1 d R . . H3B H 0.1315 -0.3449 0.2462 0.150 Uiso 1 d R . . C4 C 0.1556(4) -0.2515(6) 0.1826(4) 0.099(3) Uani 1 d . . . H4A H 0.1351 -0.2065 0.1972 0.150 Uiso 1 d R . . H4B H 0.1849 -0.2440 0.2046 0.150 Uiso 1 d R . . C5 C 0.1734(2) -0.1720(5) 0.0880(4) 0.073(2) Uani 1 d . . . H5A H 0.1751 -0.1244 0.1186 0.150 Uiso 1 d R . . C6 C 0.1827(2) -0.1542(4) 0.0177(4) 0.068(2) Uani 1 d . . . C7 C 0.1935(2) -0.2205(5) -0.0260(4) 0.077(2) Uani 1 d . . . H7A H 0.1952 -0.2792 -0.0102 0.150 Uiso 1 d R . . C8 C 0.2016(3) -0.2017(6) -0.0923(5) 0.092(3) Uani 1 d . . . H8A H 0.2100 -0.2475 -0.1220 0.150 Uiso 1 d R . . C9 C 0.1981(3) -0.1178(5) -0.1152(4) 0.082(2) Uani 1 d . . . H9A H 0.2038 -0.1053 -0.1610 0.150 Uiso 1 d R . . C10 C 0.1853(2) -0.0504(4) -0.0718(4) 0.0656(19) Uani 1 d . . . C11 C 0.1784(2) -0.0696(4) -0.0062(4) 0.0659(18) Uani 1 d . . . H11A H 0.1700 -0.0238 0.0237 0.150 Uiso 1 d R . . C12 C 0.1815(2) 0.0359(5) -0.0993(4) 0.071(2) Uani 1 d . . . H12A H 0.1910 0.0436 -0.1444 0.150 Uiso 1 d R . . C13 C 0.1656(3) 0.1853(5) -0.1061(4) 0.086(2) Uani 1 d . . . H13A H 0.1763 0.1761 -0.1505 0.150 Uiso 1 d R . . H13B H 0.1864 0.2249 -0.0845 0.150 Uiso 1 d R . . C14 C 0.1172(3) 0.2249(6) -0.1064(4) 0.095(3) Uani 1 d . . . H14A H 0.1163 0.2750 -0.1345 0.150 Uiso 1 d R . . H14B H 0.0958 0.1829 -0.1237 0.150 Uiso 1 d R . . C15 C 0.0573(3) 0.2846(7) -0.0399(6) 0.116(3) Uani 1 d . . . H15A H 0.0364 0.2413 -0.0567 0.150 Uiso 1 d R . . H15B H 0.0560 0.3338 -0.0690 0.150 Uiso 1 d R . . C16 C 0.0425(3) 0.3120(6) 0.0257(5) 0.105(3) Uani 1 d . . . H16A H 0.0106 0.3297 0.0248 0.150 Uiso 1 d R . . H16B H 0.0452 0.2634 0.0552 0.150 Uiso 1 d R . . N5 N 0.14299(19) -0.4739(4) 0.0057(3) 0.0685(16) Uani 1 d . . . H5C H 0.1254 -0.5186 0.0194 0.150 Uiso 1 d R . . N6 N 0.0840(2) -0.3375(4) -0.0515(3) 0.0697(16) Uani 1 d . . . N8 N 0.1421(3) 0.1489(5) 0.1429(4) 0.091(2) Uani 1 d . . . H8B H 0.1284 0.2005 0.1499 0.150 Uiso 1 d R . . O3 O 0.1884(2) -0.6434(4) -0.0025(4) 0.106(2) Uani 1 d . . . H3 H 0.1824 -0.6415 0.0507 0.150 Uiso 1 d R . . O4 O 0.2073(4) 0.2884(6) 0.1202(4) 0.156(3) Uani 1 d . . . H4 H 0.1641 0.3194 0.1356 0.150 Uiso 1 d R . . N7 N 0.0733(2) 0.0400(5) 0.0847(4) 0.095(2) Uani 1 d . . . C17 C 0.2129(3) -0.5653(5) -0.0102(6) 0.103(3) Uani 1 d . . . H17A H 0.2142 -0.5518 -0.0566 0.150 Uiso 1 d R . . H17B H 0.2441 -0.5730 0.0055 0.150 Uiso 1 d R . . C18 C 0.1910(3) -0.4909(5) 0.0233(5) 0.098(3) Uani 1 d . . . H18A H 0.1921 -0.5028 0.0699 0.150 Uiso 1 d R . . H18B H 0.2088 -0.4394 0.0155 0.150 Uiso 1 d R . . C19 C 0.1360(3) -0.4631(5) -0.0637(4) 0.079(2) Uani 1 d . . . H19A H 0.1399 -0.5179 -0.0855 0.150 Uiso 1 d R . . H19B H 0.1590 -0.4239 -0.0803 0.150 Uiso 1 d R . . C20 C 0.0886(3) -0.4251(6) -0.0799(4) 0.097(3) Uani 1 d . . . H20A H 0.0838 -0.4232 -0.1270 0.150 Uiso 1 d R . . H20B H 0.0654 -0.4619 -0.0609 0.150 Uiso 1 d R . . C21 C 0.0746(3) -0.2771(6) -0.0931(4) 0.088(2) Uani 1 d . . . H21A H 0.0713 -0.2936 -0.1387 0.150 Uiso 1 d R . . C22 C 0.0682(3) -0.1839(5) -0.0759(4) 0.078(2) Uani 1 d . . . C23 C 0.0650(3) -0.1247(6) -0.1263(5) 0.095(3) Uani 1 d . . . H23A H 0.0675 -0.1449 -0.1712 0.150 Uiso 1 d R . . C24 C 0.0587(3) -0.0390(6) -0.1161(5) 0.093(3) Uani 1 d . . . H24A H 0.0561 0.0000 -0.1531 0.150 Uiso 1 d R . . C25 C 0.0562(3) -0.0082(5) -0.0542(5) 0.087(3) Uani 1 d . . . H25A H 0.0523 0.0528 -0.0465 0.150 Uiso 1 d R . . C26 C 0.0599(2) -0.0663(5) 0.0014(4) 0.073(2) Uani 1 d . . . C27 C 0.0650(2) -0.1537(4) -0.0110(4) 0.070(2) Uani 1 d . . . H27A H 0.0660 -0.1938 0.0254 0.150 Uiso 1 d R . . C28 C 0.0592(3) -0.0351(5) 0.0693(4) 0.085(2) Uani 1 d . . . H28A H 0.0481 -0.0731 0.1033 0.150 Uiso 1 d R . . C29 C 0.0701(4) 0.0642(8) 0.1553(5) 0.124(4) Uani 1 d . . . H29A H 0.0555 0.0190 0.1803 0.150 Uiso 1 d R . . H29B H 0.0518 0.1158 0.1593 0.150 Uiso 1 d R . . C30 C 0.1167(4) 0.0811(8) 0.1815(5) 0.118(4) Uani 1 d . . . H30A H 0.1149 0.0983 0.2271 0.150 Uiso 1 d R . . H30B H 0.1342 0.0283 0.1794 0.150 Uiso 1 d R . . C31 C 0.1897(4) 0.1518(8) 0.1632(6) 0.129(4) Uani 1 d . . . H31A H 0.2013 0.0936 0.1664 0.150 Uiso 1 d R . . H31B H 0.1910 0.1769 0.2067 0.150 Uiso 1 d R . . C32 C 0.2192(4) 0.2058(8) 0.1196(9) 0.173(7) Uani 1 d . . . H32A H 0.2506 0.2029 0.1350 0.150 Uiso 1 d R . . H32B H 0.2178 0.1831 0.0753 0.150 Uiso 1 d R . . P1 P 0.0000 0.82460(19) 0.2500 0.0793(8) Uani 1 d SD . . F1 F 0.0075(3) 0.8261(5) 0.1735(3) 0.162(3) Uani 1 d DU . . F2 F 0.0000 0.7375(6) 0.2500 0.189(9) Uani 0.50 d SPDU . . F3 F -0.0547(3) 0.8314(8) 0.2487(7) 0.139(5) Uani 0.50 d PDU . . F4 F 0.0000 0.9118(7) 0.2500 0.133(7) Uani 0.50 d SPDU . . F2' F -0.0352(4) 0.7500(8) 0.2286(7) 0.142(5) Uani 0.50 d PDU . . F4' F -0.0314(6) 0.8970(8) 0.2322(10) 0.194(8) Uani 0.50 d PDU . . P2 P 0.27440(8) 0.93946(15) 0.22865(10) 0.0847(6) Uani 1 d D . . F5 F 0.2854(3) 0.9520(5) 0.3028(3) 0.156(3) Uani 1 d DU . . F6 F 0.2609(3) 0.8454(4) 0.2457(4) 0.174(3) Uani 1 d DU . . F7 F 0.2638(2) 0.9231(5) 0.1536(2) 0.135(2) Uani 1 d DU . . F8 F 0.2898(3) 1.0297(4) 0.2104(4) 0.176(3) Uani 1 d DU . . F9 F 0.2220(2) 0.9574(6) 0.2358(4) 0.158(3) Uani 1 d DU . . F10 F 0.3250(2) 0.9104(7) 0.2187(4) 0.187(3) Uani 1 d DU . . P3 P 0.0000 0.3120(4) 0.2500 0.145(3) Uani 1 d SDU . . F11 F -0.0346(3) 0.3854(5) 0.2365(6) 0.228(5) Uani 1 d DU . . F12 F 0.0063(4) 0.3052(9) 0.1735(4) 0.201(5) Uani 1 d DU . . F13 F -0.0404(4) 0.2453(8) 0.2449(8) 0.252(7) Uani 1 d DU . . O1W O -0.1075(6) 0.3306(12) 0.3179(11) 0.206(8) Uani 0.50 d P . . H1WA H -0.0745 0.3500 0.3200 0.150 Uiso 0.50 d PR . . H1WB H -0.1262 0.3523 0.2898 0.150 Uiso 0.50 d PR . . 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 0.0919(4) 0.0672(3) 0.0749(4) 0.0076(3) 0.0160(3) -0.0078(3) Ag2 0.1086(5) 0.0670(4) 0.0738(4) -0.0047(3) 0.0092(3) -0.0043(3) N1 0.099(5) 0.067(4) 0.088(4) 0.006(3) 0.015(4) -0.005(3) N2 0.091(4) 0.072(4) 0.090(4) -0.001(3) 0.004(3) -0.015(3) N3 0.071(3) 0.052(3) 0.080(4) 0.002(3) 0.018(3) -0.005(3) N4 0.064(3) 0.062(3) 0.075(4) 0.006(3) 0.003(3) 0.004(3) O1 0.117(5) 0.107(5) 0.139(6) -0.006(4) 0.007(4) 0.007(4) O2 0.185(7) 0.080(4) 0.268(10) -0.049(5) 0.123(7) -0.037(5) C1 0.139(8) 0.106(7) 0.110(7) -0.017(6) 0.046(6) -0.030(6) C2 0.116(7) 0.104(7) 0.096(6) 0.016(5) 0.021(5) -0.033(6) C3 0.108(6) 0.092(6) 0.078(5) 0.011(4) 0.004(5) -0.004(5) C4 0.128(7) 0.088(6) 0.082(5) 0.007(5) -0.008(5) -0.022(5) C5 0.066(4) 0.072(5) 0.080(5) -0.008(4) 0.000(4) -0.007(4) C6 0.041(3) 0.064(4) 0.099(5) -0.009(4) 0.006(3) -0.005(3) C7 0.066(4) 0.066(4) 0.098(5) -0.001(4) 0.013(4) 0.011(4) C8 0.084(5) 0.076(5) 0.115(7) -0.023(5) 0.019(5) 0.016(4) C9 0.075(5) 0.075(5) 0.096(5) -0.015(4) 0.027(4) -0.002(4) C10 0.051(3) 0.056(4) 0.090(5) -0.010(3) 0.014(3) -0.002(3) C11 0.054(3) 0.057(4) 0.086(5) -0.007(3) 0.015(3) -0.007(3) C12 0.066(4) 0.067(4) 0.079(5) -0.006(4) 0.016(3) -0.006(3) C13 0.103(6) 0.069(5) 0.085(5) 0.004(4) 0.034(4) -0.005(4) C14 0.120(7) 0.072(5) 0.095(6) 0.008(4) -0.001(5) 0.004(5) C15 0.097(6) 0.109(7) 0.140(9) -0.005(7) -0.023(6) 0.023(6) C16 0.074(5) 0.091(6) 0.151(9) -0.009(6) 0.025(5) -0.003(5) N5 0.068(3) 0.055(3) 0.082(4) -0.002(3) 0.003(3) 0.000(3) N6 0.065(3) 0.064(3) 0.080(4) -0.001(3) 0.002(3) 0.008(3) N8 0.101(5) 0.087(5) 0.086(5) -0.003(4) 0.011(4) -0.022(4) O3 0.112(4) 0.062(3) 0.145(6) -0.005(3) -0.036(4) 0.000(3) O4 0.217(9) 0.123(6) 0.129(6) -0.003(5) 0.001(6) -0.039(6) N7 0.089(4) 0.086(4) 0.111(5) -0.012(4) 0.038(4) -0.027(4) C17 0.079(5) 0.064(5) 0.164(9) 0.001(5) -0.016(5) 0.010(4) C18 0.088(5) 0.057(4) 0.148(8) -0.003(5) -0.020(5) -0.002(4) C19 0.084(5) 0.060(4) 0.093(5) -0.004(4) 0.015(4) 0.007(4) C20 0.121(7) 0.081(5) 0.088(5) -0.010(4) -0.014(5) 0.029(5) C21 0.105(6) 0.082(5) 0.078(5) 0.004(4) 0.011(4) 0.023(5) C22 0.066(4) 0.077(5) 0.091(5) 0.006(4) 0.010(4) 0.012(4) C23 0.108(6) 0.090(6) 0.087(6) 0.016(5) -0.001(5) 0.019(5) C24 0.092(6) 0.083(5) 0.102(6) 0.023(5) -0.013(5) 0.005(5) C25 0.063(4) 0.069(5) 0.129(7) 0.026(5) 0.012(4) 0.001(4) C26 0.047(3) 0.074(5) 0.099(5) 0.012(4) 0.014(3) -0.005(3) C27 0.053(4) 0.058(4) 0.100(5) 0.014(4) 0.013(3) 0.004(3) C28 0.075(4) 0.070(5) 0.110(6) 0.002(4) 0.036(4) -0.011(4) C29 0.152(8) 0.118(8) 0.105(7) -0.009(6) 0.065(6) -0.045(7) C30 0.147(9) 0.135(9) 0.074(6) 0.005(6) 0.028(6) -0.019(7) C31 0.127(8) 0.144(9) 0.116(8) 0.032(7) -0.040(6) -0.023(7) C32 0.081(7) 0.089(7) 0.35(2) -0.015(11) -0.020(10) -0.016(6) P1 0.103(2) 0.0677(16) 0.0671(16) 0.000 0.0115(15) 0.000 F1 0.219(6) 0.167(5) 0.100(4) 0.002(4) 0.021(4) -0.067(5) F2 0.28(2) 0.078(11) 0.208(19) 0.000 0.135(18) 0.000 F3 0.085(7) 0.162(11) 0.169(12) -0.014(9) 0.012(7) -0.052(7) F4 0.094(10) 0.137(15) 0.170(17) 0.000 0.029(11) 0.000 F2' 0.133(9) 0.180(13) 0.114(9) 0.004(8) -0.008(8) -0.075(9) F4' 0.266(17) 0.182(13) 0.135(15) 0.065(11) 0.003(15) 0.181(12) P2 0.0919(14) 0.0888(15) 0.0734(13) 0.0057(11) 0.0069(10) -0.0045(12) F5 0.200(6) 0.163(5) 0.105(4) -0.012(4) -0.002(4) -0.019(5) F6 0.198(6) 0.140(5) 0.184(6) 0.033(4) -0.032(5) -0.033(5) F7 0.127(4) 0.184(5) 0.095(3) -0.002(4) -0.005(3) -0.015(4) F8 0.223(6) 0.131(5) 0.174(6) 0.020(4) -0.029(5) -0.046(5) F9 0.139(4) 0.194(6) 0.143(5) 0.001(4) 0.033(4) 0.032(4) F10 0.138(5) 0.241(7) 0.182(6) 0.026(6) -0.007(4) 0.026(5) P3 0.238(7) 0.099(4) 0.124(4) 0.000 -0.109(5) 0.000 F11 0.237(8) 0.213(8) 0.236(8) 0.038(6) -0.021(7) 0.016(6) F12 0.203(8) 0.237(9) 0.163(8) 0.008(7) -0.047(7) 0.010(7) F13 0.267(10) 0.242(10) 0.245(10) -0.017(8) -0.018(8) -0.064(8) O1W 0.125(10) 0.179(13) 0.31(2) 0.147(13) -0.108(12) -0.073(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 N7 2.353(7) . ? Ag1 N3 2.352(6) . ? Ag1 N4 2.356(6) . ? Ag1 N8 2.357(7) . ? Ag2 N6 2.235(6) . ? Ag2 N1 2.295(7) . ? Ag2 N5 2.443(6) . ? Ag2 N2 2.511(7) . ? N1 C3 1.428(12) . ? N1 C2 1.440(11) . ? N2 C5 1.236(10) . ? N2 C4 1.495(11) . ? N3 C12 1.288(9) . ? N3 C13 1.472(9) . ? N4 C15 1.447(11) . ? N4 C14 1.466(10) . ? O1 C1 1.432(12) . ? O2 C16 1.430(12) . ? C1 C2 1.479(14) . ? C3 C4 1.524(12) . ? C5 C6 1.471(11) . ? C6 C7 1.388(10) . ? C6 C11 1.396(10) . ? C7 C8 1.390(12) . ? C8 C9 1.378(12) . ? C9 C10 1.411(10) . ? C10 C11 1.372(10) . ? C10 C12 1.445(10) . ? C13 C14 1.526(12) . ? C15 C16 1.457(14) . ? N5 C19 1.423(10) . ? N5 C18 1.454(10) . ? N6 C21 1.281(10) . ? N6 C20 1.474(10) . ? N8 C31 1.433(13) . ? N8 C30 1.497(12) . ? O3 C17 1.407(10) . ? O4 C32 1.319(14) . ? N7 C28 1.265(10) . ? N7 C29 1.476(12) . ? C17 C18 1.476(12) . ? C19 C20 1.523(12) . ? C21 C22 1.490(12) . ? C22 C23 1.370(12) . ? C22 C27 1.394(11) . ? C23 C24 1.350(12) . ? C24 C25 1.341(13) . ? C25 C26 1.439(11) . ? C26 C27 1.380(10) . ? C26 C28 1.453(12) . ? C29 C30 1.467(15) . ? C31 C32 1.484(18) . ? P1 F2 1.343(10) . ? P1 F4 1.345(11) . ? P1 F4' 1.481(11) 2 ? P1 F4' 1.481(11) . ? P1 F1 1.562(6) 2 ? P1 F1 1.562(6) . ? P1 F3 1.584(8) 2 ? P1 F3 1.584(8) . ? P1 F2' 1.594(10) . ? P1 F2' 1.594(10) 2 ? F2 F2' 1.121(13) . ? F2 F2' 1.121(13) 2 ? F3 F4' 1.26(2) . ? F3 F2' 1.435(17) . ? F4 F4' 1.000(18) 2 ? F4 F4' 1.000(18) . ? P2 F8 1.507(6) . ? P2 F5 1.540(6) . ? P2 F6 1.542(7) . ? P2 F10 1.542(7) . ? P2 F9 1.545(6) . ? P2 F7 1.564(5) . ? P3 F11 1.533(8) . ? P3 F11 1.533(8) 2 ? P3 F12 1.559(7) . ? P3 F12 1.559(7) 2 ? P3 F13 1.559(8) . ? P3 F13 1.559(8) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ag1 N3 127.3(2) . . ? N7 Ag1 N4 125.3(2) . . ? N3 Ag1 N4 77.4(2) . . ? N7 Ag1 N8 74.5(3) . . ? N3 Ag1 N8 137.8(2) . . ? N4 Ag1 N8 122.6(2) . . ? N6 Ag2 N1 152.0(2) . . ? N6 Ag2 N5 77.7(2) . . ? N1 Ag2 N5 115.7(2) . . ? N6 Ag2 N2 125.2(2) . . ? N1 Ag2 N2 73.8(2) . . ? N5 Ag2 N2 114.0(2) . . ? C3 N1 C2 114.3(7) . . ? C3 N1 Ag2 106.7(5) . . ? C2 N1 Ag2 112.9(5) . . ? C5 N2 C4 116.8(7) . . ? C5 N2 Ag2 124.3(6) . . ? C4 N2 Ag2 107.3(5) . . ? C12 N3 C13 116.8(6) . . ? C12 N3 Ag1 137.2(5) . . ? C13 N3 Ag1 105.4(4) . . ? C15 N4 C14 109.7(7) . . ? C15 N4 Ag1 122.3(6) . . ? C14 N4 Ag1 105.9(4) . . ? O1 C1 C2 115.6(8) . . ? N1 C2 C1 114.7(8) . . ? N1 C3 C4 111.5(7) . . ? N2 C4 C3 109.8(7) . . ? N2 C5 C6 123.7(7) . . ? C7 C6 C11 119.3(7) . . ? C7 C6 C5 121.2(7) . . ? C11 C6 C5 119.4(7) . . ? C8 C7 C6 119.8(7) . . ? C9 C8 C7 120.5(8) . . ? C8 C9 C10 120.2(8) . . ? C11 C10 C9 118.7(7) . . ? C11 C10 C12 124.0(6) . . ? C9 C10 C12 117.3(7) . . ? C10 C11 C6 121.5(7) . . ? N3 C12 C10 125.8(7) . . ? N3 C13 C14 110.1(6) . . ? N4 C14 C13 110.3(7) . . ? N4 C15 C16 112.0(8) . . ? O2 C16 C15 110.1(8) . . ? C19 N5 C18 113.1(7) . . ? C19 N5 Ag2 104.0(4) . . ? C18 N5 Ag2 117.2(5) . . ? C21 N6 C20 115.5(7) . . ? C21 N6 Ag2 136.7(6) . . ? C20 N6 Ag2 107.0(5) . . ? C31 N8 C30 110.2(8) . . ? C31 N8 Ag1 118.3(7) . . ? C30 N8 Ag1 109.3(5) . . ? C28 N7 C29 116.6(8) . . ? C28 N7 Ag1 129.9(6) . . ? C29 N7 Ag1 110.4(5) . . ? O3 C17 C18 113.3(8) . . ? N5 C18 C17 116.0(7) . . ? N5 C19 C20 112.3(7) . . ? N6 C20 C19 110.7(7) . . ? N6 C21 C22 125.1(8) . . ? C23 C22 C27 118.1(8) . . ? C23 C22 C21 118.5(8) . . ? C27 C22 C21 123.3(7) . . ? C24 C23 C22 123.2(9) . . ? C23 C24 C25 119.8(8) . . ? C24 C25 C26 120.2(8) . . ? C27 C26 C25 118.4(8) . . ? C27 C26 C28 119.7(7) . . ? C25 C26 C28 121.8(7) . . ? C26 C27 C22 120.3(7) . . ? N7 C28 C26 122.0(8) . . ? C30 C29 N7 109.4(8) . . ? C29 C30 N8 112.8(9) . . ? N8 C31 C32 113.7(9) . . ? O4 C32 C31 112.7(12) . . ? F2 P1 F4 180.000(4) . . ? F2 P1 F4' 138.9(7) . 2 ? F4 P1 F4' 41.1(7) . 2 ? F2 P1 F4' 138.9(7) . . ? F4 P1 F4' 41.1(7) . . ? F4' P1 F4' 82.2(14) 2 . ? F2 P1 F1 90.9(3) . 2 ? F4 P1 F1 89.1(3) . 2 ? F4' P1 F1 80.6(9) 2 2 ? F4' P1 F1 98.1(9) . 2 ? F2 P1 F1 90.9(3) . . ? F4 P1 F1 89.1(3) . . ? F4' P1 F1 98.1(9) 2 . ? F4' P1 F1 80.6(9) . . ? F1 P1 F1 178.3(6) 2 . ? F2 P1 F3 93.8(5) . 2 ? F4 P1 F3 86.2(5) . 2 ? F4' P1 F3 48.4(8) 2 2 ? F4' P1 F3 124.3(9) . 2 ? F1 P1 F3 97.3(6) 2 2 ? F1 P1 F3 82.6(5) . 2 ? F2 P1 F3 93.8(5) . . ? F4 P1 F3 86.2(5) . . ? F4' P1 F3 124.3(9) 2 . ? F4' P1 F3 48.4(8) . . ? F1 P1 F3 82.6(5) 2 . ? F1 P1 F3 97.3(6) . . ? F3 P1 F3 172.4(9) 2 . ? F2 P1 F2' 43.8(5) . . ? F4 P1 F2' 136.2(5) . . ? F4' P1 F2' 177.1(9) 2 . ? F4' P1 F2' 95.1(8) . . ? F1 P1 F2' 100.8(6) 2 . ? F1 P1 F2' 80.4(6) . . ? F3 P1 F2' 133.5(7) 2 . ? F3 P1 F2' 53.7(6) . . ? F2 P1 F2' 43.8(5) . 2 ? F4 P1 F2' 136.2(5) . 2 ? F4' P1 F2' 95.1(8) 2 2 ? F4' P1 F2' 177.1(10) . 2 ? F1 P1 F2' 80.4(6) 2 2 ? F1 P1 F2' 100.8(6) . 2 ? F3 P1 F2' 53.7(6) 2 2 ? F3 P1 F2' 133.5(7) . 2 ? F2' P1 F2' 87.7(10) . 2 ? F2' F2 F2' 160.2(16) . 2 ? F2' F2 P1 80.1(8) . . ? F2' F2 P1 80.1(8) 2 . ? F4' F3 F2' 114.6(11) . . ? F4' F3 P1 61.5(7) . . ? F2' F3 P1 63.5(6) . . ? F4' F4 F4' 153.6(19) 2 . ? F4' F4 P1 76.8(9) 2 . ? F4' F4 P1 76.8(9) . . ? F2 F2' F3 113.4(11) . . ? F2 F2' P1 56.1(7) . . ? F3 F2' P1 62.8(6) . . ? F4 F4' F3 125.0(15) . . ? F4 F4' P1 62.1(9) . . ? F3 F4' P1 70.0(7) . . ? F8 P2 F5 93.5(4) . . ? F8 P2 F6 177.1(5) . . ? F5 P2 F6 87.3(4) . . ? F8 P2 F10 87.4(5) . . ? F5 P2 F10 88.4(5) . . ? F6 P2 F10 89.8(5) . . ? F8 P2 F9 98.5(5) . . ? F5 P2 F9 94.8(4) . . ? F6 P2 F9 84.2(5) . . ? F10 P2 F9 173.0(5) . . ? F8 P2 F7 88.2(4) . . ? F5 P2 F7 177.9(5) . . ? F6 P2 F7 90.9(4) . . ? F10 P2 F7 90.4(4) . . ? F9 P2 F7 86.1(4) . . ? F11 P3 F11 84.9(8) . 2 ? F11 P3 F12 87.3(6) . . ? F11 P3 F12 98.4(7) 2 . ? F11 P3 F12 98.4(7) . 2 ? F11 P3 F12 87.3(6) 2 2 ? F12 P3 F12 172.3(11) . 2 ? F11 P3 F13 89.3(6) . . ? F11 P3 F13 170.3(7) 2 . ? F12 P3 F13 89.0(7) . . ? F12 P3 F13 85.9(7) 2 . ? F11 P3 F13 170.3(7) . 2 ? F11 P3 F13 89.3(6) 2 2 ? F12 P3 F13 85.9(7) . 2 ? F12 P3 F13 89.0(7) 2 2 ? F13 P3 F13 97.4(11) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA F11 1.00 2.12 2.81(2) 124.5 . N4 H4C O3 0.90 2.20 3.038(8) 155.6 1_565 O2 H2D O1 0.85 2.10 2.949(10) 179.1 1_565 O1 H1 O2 0.92 2.04 2.949(10) 167.0 1_545 N5 H5C O2 0.90 2.28 3.176(9) 171.4 1_545 O3 H3 O4 1.09 1.91 2.744(11) 130.5 1_545 N8 H8B O1W 0.90 2.19 3.080(18) 167.6 2 O4 H4 O1W 1.37 1.90 3.21(2) 158.4 2 O1W H1WA F12 1.00 2.09 2.95(2) 143.3 2 N1 H1C F2' 0.90 2.40 3.137(15) 139.4 2_545 O1W H1WB F10 0.85 2.20 3.048(18) 178.8 3_445 _diffrn_measured_fraction_theta_max 0.476 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.476 _refine_diff_density_max 1.549 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.107 #============================================================ data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H29.50 Ag N6 O8.25' _chemical_formula_weight 629.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.429(2) _cell_length_b 13.367(3) _cell_length_c 17.158(3) _cell_angle_alpha 81.75(1) _cell_angle_beta 77.53(1) _cell_angle_gamma 78.70(1) _cell_volume 2714.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type 'semi-empirical based on psi-scan' _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.790 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method \w _diffrn_standards_number 2 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.4 _diffrn_reflns_number 9478 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9460 _reflns_number_gt 4891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00081(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9460 _refine_ls_number_parameters 695 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1476 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.06102(4) -0.85725(4) 0.71885(3) 0.06216(17) Uani 1 d . . . Ag2 Ag -0.47480(4) -0.23208(4) 0.83190(3) 0.05911(16) Uani 1 d . . . N1 N -0.5093(4) -0.0989(3) 0.7353(3) 0.0487(13) Uani 1 d . . . H1N H -0.5863 -0.0865 0.7294 0.120 Uiso 1 d R . . N2 N -0.4020(4) -0.3111(3) 0.7069(3) 0.0488(13) Uani 1 d . . . N3 N -0.0188(3) -0.7843(3) 0.8420(3) 0.0455(13) Uani 1 d . . . N4 N 0.1002(4) -0.9924(3) 0.8139(3) 0.0476(13) Uani 1 d . . . H4N H 0.1756 -1.0063 0.8223 0.120 Uiso 1 d R . . O1 O -0.6631(4) 0.0522(3) 0.8351(3) 0.0878(17) Uani 1 d . . . H1B H -0.6870 0.1164 0.8326 0.120 Uiso 1 d R . . O2 O 0.2618(3) -1.1457(3) 0.7174(3) 0.0763(15) Uani 1 d . . . H2B H 0.2783 -1.1998 0.7482 0.120 Uiso 1 d R . . C1 C -0.5460(5) 0.0351(5) 0.8273(4) 0.068(2) Uani 1 d . . . H1A H -0.5218 0.0960 0.8356 0.120 Uiso 1 d R . . H1B H -0.5248 -0.0184 0.8676 0.120 Uiso 1 d R . . C2 C -0.4879(5) 0.0036(4) 0.7462(4) 0.0585(18) Uani 1 d . . . H2A H -0.5154 0.0535 0.7059 0.120 Uiso 1 d R . . H2B H -0.4088 0.0018 0.7391 0.120 Uiso 1 d R . . C3 C -0.4504(5) -0.1310(5) 0.6565(4) 0.0606(19) Uani 1 d . . . H3A H -0.3728 -0.1257 0.6485 0.120 Uiso 1 d R . . H3B H -0.4822 -0.0857 0.6155 0.120 Uiso 1 d R . . C4 C -0.4589(5) -0.2406(4) 0.6480(3) 0.0585(18) Uani 1 d . . . H4A H -0.5363 -0.2475 0.6585 0.120 Uiso 1 d R . . H4B H -0.4260 -0.2579 0.5946 0.120 Uiso 1 d R . . C5 C -0.3399(5) -0.3909(4) 0.6821(3) 0.0527(17) Uani 1 d . . . H5 H -0.3329 -0.4004 0.6267 0.120 Uiso 1 d R . . C6 C -0.2769(5) -0.4716(4) 0.7306(3) 0.0489(16) Uani 1 d . . . C7 C -0.2173(5) -0.5594(5) 0.6966(3) 0.0588(18) Uani 1 d . . . H7A H -0.2192 -0.5666 0.6420 0.120 Uiso 1 d R . . C8 C -0.1558(5) -0.6367(4) 0.7401(3) 0.0525(17) Uani 1 d . . . H8A H -0.1165 -0.6971 0.7156 0.120 Uiso 1 d R . . C9 C -0.1514(4) -0.6289(4) 0.8188(3) 0.0436(15) Uani 1 d . . . C11 C -0.2123(5) -0.5414(4) 0.8534(3) 0.0559(18) Uani 1 d . . . H11A H -0.2119 -0.5353 0.9084 0.120 Uiso 1 d R . . C12 C -0.0844(4) -0.7071(4) 0.8672(3) 0.0472(16) Uani 1 d . . . H12A H -0.0915 -0.6972 0.9226 0.120 Uiso 1 d R . . C13 C 0.0402(5) -0.8529(4) 0.9009(3) 0.0541(18) Uani 1 d . . . H13A H 0.0051 -0.8370 0.9543 0.120 Uiso 1 d R . . H13B H 0.1163 -0.8421 0.8913 0.120 Uiso 1 d R . . C14 C 0.0390(5) -0.9645(4) 0.8932(3) 0.0541(18) Uani 1 d . . . H14A H 0.0715 -1.0083 0.9346 0.120 Uiso 1 d R . . H14B H -0.0371 -0.9740 0.8997 0.120 Uiso 1 d R . . C15 C 0.0801(5) -1.0944(4) 0.8002(4) 0.0587(19) Uani 1 d . . . H15A H 0.0014 -1.0906 0.8030 0.120 Uiso 1 d R . . H15B H 0.1024 -1.1455 0.8417 0.120 Uiso 1 d R . . N5 N 0.1337(4) -0.7960(4) 0.5928(3) 0.0688(17) Uani 1 d . . . H5N H 0.1933 -0.7300 0.5900 0.120 Uiso 1 d R . . N6 N -0.0827(5) -0.8520(5) 0.6254(3) 0.0800(19) Uani 1 d . . . N7 N -0.3290(5) -1.2463(4) 0.9264(3) 0.0735(17) Uani 1 d . . . N8 N -0.5500(4) -1.2916(3) 0.9578(2) 0.0531(14) Uani 1 d . . . H8N H -0.5920 -1.3488 0.9419 0.120 Uiso 1 d R . . O3 O 0.3824(4) -0.8382(5) 0.5783(4) 0.135(3) Uani 1 d . . . H21C H 0.3508 -0.7993 0.6147 0.120 Uiso 1 d R . . O4 O -0.7903(4) -1.2298(4) 0.9592(3) 0.0924(17) Uani 1 d . . . H4C H -0.7658 -1.2574 0.9157 0.120 Uiso 1 d R . . C21 C 0.3191(7) -0.9102(7) 0.5798(5) 0.112(3) Uani 1 d . . . H21A H 0.3649 -0.9656 0.5518 0.120 Uiso 1 d R . . H21B H 0.2955 -0.9366 0.6346 0.120 Uiso 1 d R . . C22 C 0.2138(7) -0.8705(6) 0.5424(4) 0.097(3) Uani 1 d . . . H22B H 0.2361 -0.8388 0.4890 0.120 Uiso 1 d R . . H22C H 0.1770 -0.9262 0.5392 0.120 Uiso 1 d R . . C23 C 0.0470(6) -0.7406(5) 0.5517(4) 0.085(2) Uani 1 d . . . H23A H 0.0807 -0.7159 0.4984 0.120 Uiso 1 d R . . H23B H 0.0093 -0.6819 0.5791 0.120 Uiso 1 d R . . C24 C -0.0380(7) -0.8040(6) 0.5455(4) 0.092(3) Uani 1 d . . . H24C H -0.0980 -0.7598 0.5242 0.120 Uiso 1 d R . . H24B H -0.0038 -0.8555 0.5098 0.120 Uiso 1 d R . . C25 C -0.1150(6) -0.9373(6) 0.6280(5) 0.082(2) Uani 1 d . . . H25A H -0.1099 -0.9653 0.5786 0.120 Uiso 1 d R . . C26 C -0.1629(5) -0.9939(5) 0.7047(4) 0.069(2) Uani 1 d . . . C27 C -0.2024(5) -0.9455(5) 0.7764(4) 0.069(2) Uani 1 d . . . H27A H -0.2002 -0.8740 0.7760 0.120 Uiso 1 d R . . C28 C -0.2429(5) -1.0024(5) 0.8454(4) 0.074(2) Uani 1 d . . . H28A H -0.2684 -0.9703 0.8942 0.120 Uiso 1 d R . . C29 C -0.2500(5) -1.1061(5) 0.8489(4) 0.0636(19) Uani 1 d . . . C30 C -0.1695(5) -1.0957(5) 0.7060(4) 0.065(2) Uani 1 d . . . H30A H -0.1428 -1.1283 0.6575 0.120 Uiso 1 d R . . C31 C -0.2118(5) -1.1507(5) 0.7758(4) 0.0638(19) Uani 1 d . . . H31A H -0.2181 -1.2210 0.7749 0.120 Uiso 1 d R . . C32 C -0.2967(5) -1.1649(6) 0.9229(4) 0.074(2) Uani 1 d . . . H32A H -0.3042 -1.1361 0.9723 0.120 Uiso 1 d R . . C33 C -0.3739(6) -1.2973(6) 1.0053(4) 0.087(2) Uani 1 d . . . H33A H -0.4058 -1.2469 1.0422 0.120 Uiso 1 d R . . H33B H -0.3153 -1.3438 1.0264 0.120 Uiso 1 d R . . C34 C -0.4649(6) -1.3546(5) 0.9987(4) 0.078(2) Uani 1 d . . . H34A H -0.4299 -1.4120 0.9690 0.120 Uiso 1 d R . . H34B H -0.5000 -1.3810 1.0510 0.120 Uiso 1 d R . . C35 C -0.6255(6) -1.2131(5) 1.0067(4) 0.080(2) Uani 1 d . . . H35A H -0.5830 -1.1636 1.0138 0.120 Uiso 1 d R . . H35B H -0.6558 -1.2447 1.0585 0.120 Uiso 1 d R . . C36 C -0.7201(5) -1.1613(5) 0.9653(4) 0.077(2) Uani 1 d . . . H36A H -0.6884 -1.1337 0.9124 0.120 Uiso 1 d R . . H36B H -0.7643 -1.1054 0.9934 0.120 Uiso 1 d R . . C10 C -0.2733(5) -0.4639(5) 0.8109(4) 0.064(2) Uani 1 d . . . H10A H -0.3119 -0.4033 0.8353 0.120 Uiso 1 d R . . O11 O -0.6227(5) 0.5558(4) 0.8903(3) 0.1049(18) Uani 1 d . . . O12 O -0.7087(4) 0.6825(3) 0.8168(3) 0.0843(15) Uani 1 d . . . C56 C -0.6230(6) 0.5012(6) 0.6236(5) 0.087(2) Uani 1 d . . . C52 C -0.6142(5) 0.5360(5) 0.7545(4) 0.0559(17) Uani 1 d . . . C51 C -0.6508(5) 0.5967(5) 0.8269(4) 0.066(2) Uani 1 d . . . C54 C -0.5129(6) 0.3841(6) 0.7009(5) 0.090(3) Uani 1 d . . . C53 C -0.5434(6) 0.4435(5) 0.7608(4) 0.073(2) Uani 1 d . . . H53A H -0.5151 0.4202 0.8093 0.120 Uiso 1 d R . . C47 C 0.1113(5) -0.5494(4) 0.7111(4) 0.0621(19) Uani 1 d . . . H47 H 0.1241 -0.5820 0.6627 0.120 Uiso 1 d R . . C55 C -0.5477(6) 0.4095(6) 0.6290(5) 0.096(3) Uani 1 d . . . H55 H -0.5228 0.3666 0.5860 0.120 Uiso 1 d R . . C57 C -0.6538(5) 0.5656(5) 0.6841(4) 0.067(2) Uani 1 d . . . H57 H -0.7019 0.6301 0.6758 0.120 Uiso 1 d R . . O5 O -0.0168(5) -0.3245(4) 0.9288(3) 0.111(2) Uani 1 d . . . O6 O 0.0983(4) -0.4479(4) 0.9776(3) 0.0996(17) Uani 1 d . . . O7 O 0.2774(4) -0.7426(4) 0.8269(3) 0.0963(17) Uani 1 d . . . O8 O 0.2583(5) -0.7323(4) 0.6993(3) 0.110(2) Uani 1 d . . . O9 O -0.0633(5) -0.3223(4) 0.6572(3) 0.121(2) Uani 1 d . . . O10 O 0.0042(5) -0.4500(4) 0.5945(3) 0.114(2) Uani 1 d . . . N9 N 0.0480(5) -0.4034(5) 0.9239(3) 0.0762(18) Uani 1 d . . . N10 N 0.2399(6) -0.7019(5) 0.7684(5) 0.111(3) Uani 1 d . . . C41 C -0.0084(6) -0.4053(4) 0.6518(3) 0.0556(18) Uani 1 d . . . C42 C 0.0437(5) -0.4541(5) 0.7192(4) 0.0643(19) Uani 1 d . . . C43 C 0.0222(5) -0.4059(5) 0.7875(4) 0.0631(19) Uani 1 d . . . H43 H -0.0256 -0.3403 0.7911 0.120 Uiso 1 d R . . C44 C 0.0703(5) -0.4557(4) 0.8506(4) 0.0541(17) Uani 1 d . . . C45 C 0.1369(5) -0.5497(5) 0.8466(4) 0.0606(18) Uani 1 d . . . H45 H 0.1655 -0.5839 0.8929 0.120 Uiso 1 d R . . C46 C 0.1602(4) -0.5959(4) 0.7766(4) 0.0528(18) Uani 1 d . . . O16 O -0.7376(7) 0.6107(7) 0.5484(4) 0.186(3) Uani 1 d . . . C16 C 0.1433(5) -1.1273(5) 0.7195(4) 0.071(2) Uani 1 d . . . H16A H 0.1262 -1.0739 0.6780 0.120 Uiso 1 d R . . H16B H 0.1212 -1.1883 0.7094 0.120 Uiso 1 d R . . O13 O -0.4095(6) 0.2618(5) 0.7763(6) 0.163(3) Uani 1 d . . . O14 O -0.4031(9) 0.2380(6) 0.6523(7) 0.241(5) Uani 1 d . . . O15 O -0.6397(7) 0.4803(7) 0.4957(4) 0.193(4) Uani 1 d . . . N11 N -0.4320(7) 0.2818(7) 0.7066(7) 0.138(4) Uani 1 d . . . N12 N -0.6732(8) 0.5339(7) 0.5499(5) 0.140(3) Uani 1 d . . . O1W O -0.3352(16) 0.1366(14) 0.4974(9) 0.229(9) Uani 0.50 d PU . . H1WA H -0.3716 0.0813 0.5366 0.120 Uiso 0.50 d PR . . H1WB H -0.3940 0.2181 0.4979 0.120 Uiso 0.50 d PR . . 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 0.0703(3) 0.0698(3) 0.0424(3) 0.0077(2) -0.0145(2) -0.0083(3) Ag2 0.0667(3) 0.0623(3) 0.0463(3) 0.0069(2) -0.0170(2) -0.0084(3) N1 0.041(3) 0.045(3) 0.054(3) -0.004(2) -0.012(2) 0.007(2) N2 0.043(3) 0.046(3) 0.055(3) 0.003(2) -0.019(2) 0.000(2) N3 0.037(3) 0.048(3) 0.047(3) 0.000(2) -0.010(2) 0.002(2) N4 0.040(3) 0.044(3) 0.055(3) 0.010(2) -0.013(2) -0.003(2) O1 0.059(3) 0.045(3) 0.149(5) -0.015(3) 0.001(3) -0.003(2) O2 0.052(3) 0.071(3) 0.096(3) 0.001(3) -0.006(3) -0.005(2) C1 0.048(4) 0.061(4) 0.097(5) -0.006(4) -0.022(4) -0.008(3) C2 0.053(4) 0.048(4) 0.076(4) -0.002(3) -0.020(3) -0.006(3) C3 0.044(3) 0.070(4) 0.065(4) 0.014(3) -0.024(3) -0.006(3) C4 0.056(4) 0.058(4) 0.059(4) -0.003(3) -0.029(3) 0.014(3) C5 0.052(4) 0.056(4) 0.053(3) -0.007(3) -0.019(3) -0.006(3) C6 0.054(4) 0.047(4) 0.048(3) -0.013(3) -0.018(3) 0.003(3) C7 0.069(4) 0.062(4) 0.048(3) -0.009(3) -0.022(3) -0.002(3) C8 0.064(4) 0.052(4) 0.040(3) -0.011(3) -0.013(3) 0.003(3) C9 0.038(3) 0.047(3) 0.044(3) 0.000(3) -0.006(3) -0.010(3) C11 0.059(4) 0.061(4) 0.044(3) -0.007(3) -0.021(3) 0.013(3) C12 0.042(3) 0.057(4) 0.040(3) 0.006(3) -0.009(3) -0.007(3) C13 0.048(3) 0.065(4) 0.043(3) 0.004(3) -0.013(3) 0.003(3) C14 0.058(4) 0.055(4) 0.037(3) 0.012(3) -0.003(3) 0.000(3) C15 0.042(3) 0.049(4) 0.079(4) 0.011(3) -0.012(3) -0.005(3) N5 0.076(4) 0.069(4) 0.052(3) 0.006(3) -0.007(3) -0.006(3) N6 0.078(4) 0.090(4) 0.076(4) -0.002(3) -0.029(3) -0.013(3) N7 0.076(4) 0.067(4) 0.082(4) -0.004(3) -0.036(3) -0.006(3) N8 0.065(3) 0.053(3) 0.041(3) 0.000(2) -0.021(2) -0.001(3) O3 0.079(4) 0.186(6) 0.137(5) -0.012(5) -0.002(4) -0.040(4) O4 0.071(3) 0.134(4) 0.072(3) -0.009(3) -0.012(3) -0.018(3) C21 0.077(6) 0.147(8) 0.095(6) -0.009(6) -0.019(5) 0.021(6) C22 0.101(6) 0.118(7) 0.068(5) -0.013(5) -0.010(5) -0.014(5) C23 0.105(6) 0.082(5) 0.065(4) 0.021(4) -0.031(4) -0.009(5) C24 0.120(6) 0.090(6) 0.066(5) 0.016(4) -0.040(5) -0.012(5) C25 0.073(4) 0.083(5) 0.105(5) -0.026(4) -0.053(4) 0.008(4) C26 0.052(4) 0.070(5) 0.086(5) -0.004(4) -0.029(4) 0.002(4) C27 0.049(4) 0.062(4) 0.108(5) -0.033(4) -0.028(4) -0.006(3) C28 0.050(4) 0.093(5) 0.089(5) -0.037(4) -0.016(4) -0.013(4) C29 0.044(3) 0.071(4) 0.088(5) -0.035(4) -0.024(3) -0.008(3) C30 0.062(4) 0.062(4) 0.073(4) -0.017(4) -0.018(4) -0.002(4) C31 0.051(4) 0.065(4) 0.085(5) -0.019(4) -0.033(3) -0.002(3) C32 0.048(4) 0.112(6) 0.064(4) -0.021(4) -0.024(3) 0.001(4) C33 0.096(5) 0.104(6) 0.062(4) 0.008(4) -0.046(4) 0.003(5) C34 0.088(5) 0.085(5) 0.059(4) 0.013(4) -0.030(4) -0.005(4) C35 0.083(5) 0.093(5) 0.055(4) -0.010(4) -0.017(4) 0.012(4) C36 0.056(4) 0.093(5) 0.075(5) -0.036(4) -0.011(4) 0.017(4) C10 0.072(4) 0.056(4) 0.061(4) -0.011(3) -0.020(4) 0.010(4) O11 0.175(5) 0.071(3) 0.087(3) 0.001(3) -0.079(3) -0.014(3) O12 0.095(3) 0.071(3) 0.091(3) -0.003(3) -0.043(3) 0.000(3) C56 0.096(5) 0.102(6) 0.078(5) 0.005(4) -0.013(4) -0.065(5) C52 0.052(3) 0.056(4) 0.067(4) 0.007(3) -0.032(3) -0.015(3) C51 0.072(4) 0.053(4) 0.080(5) 0.005(4) -0.031(4) -0.019(4) C54 0.079(5) 0.070(5) 0.125(7) -0.005(5) -0.017(5) -0.025(4) C53 0.078(5) 0.058(4) 0.090(5) -0.005(4) -0.025(4) -0.019(4) C47 0.068(4) 0.049(4) 0.068(4) -0.001(3) -0.014(4) -0.010(3) C55 0.092(6) 0.095(6) 0.100(6) -0.038(5) 0.028(5) -0.048(5) C57 0.062(4) 0.078(4) 0.074(4) 0.008(4) -0.023(4) -0.042(4) O5 0.130(5) 0.095(4) 0.109(4) -0.044(3) -0.038(4) 0.018(4) O6 0.117(4) 0.115(4) 0.086(3) -0.011(3) -0.044(3) -0.038(3) O7 0.095(3) 0.071(3) 0.126(4) 0.014(3) -0.065(3) 0.008(3) O8 0.113(4) 0.106(4) 0.113(4) -0.038(3) -0.045(4) 0.021(3) O9 0.180(5) 0.096(4) 0.072(3) 0.004(3) -0.053(4) 0.035(4) O10 0.162(5) 0.094(4) 0.083(4) 0.003(3) -0.055(4) 0.009(4) N9 0.089(4) 0.077(4) 0.070(4) -0.003(3) -0.031(3) -0.019(4) N10 0.088(5) 0.097(5) 0.150(7) 0.006(5) -0.027(5) -0.029(4) C41 0.086(5) 0.032(3) 0.043(3) -0.002(3) -0.023(3) 0.013(3) C42 0.067(4) 0.070(4) 0.061(4) 0.009(3) -0.030(3) -0.014(4) C43 0.075(4) 0.052(4) 0.066(4) 0.005(3) -0.017(4) -0.023(3) C44 0.055(4) 0.047(4) 0.062(4) -0.002(3) -0.018(3) -0.007(3) C45 0.075(4) 0.063(4) 0.056(4) 0.001(3) -0.027(3) -0.030(3) C46 0.033(3) 0.033(3) 0.091(5) 0.016(3) -0.024(3) -0.005(3) O16 0.259(8) 0.216(8) 0.122(5) 0.037(5) -0.123(5) -0.079(7) C16 0.069(5) 0.055(4) 0.087(5) -0.014(4) -0.015(4) -0.002(4) O13 0.140(6) 0.082(4) 0.262(9) -0.011(5) -0.052(6) 0.002(4) O14 0.226(10) 0.143(7) 0.329(12) -0.116(7) 0.019(9) 0.011(7) O15 0.263(9) 0.261(8) 0.092(5) -0.064(5) -0.023(5) -0.111(7) N11 0.097(6) 0.108(7) 0.208(11) -0.028(7) -0.003(7) -0.036(5) N12 0.204(9) 0.170(8) 0.071(5) 0.009(5) -0.024(6) -0.111(7) O1W 0.33(2) 0.215(16) 0.146(12) -0.066(11) -0.091(13) 0.020(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 N5 2.259(5) . ? Ag1 N4 2.304(4) . ? Ag1 N3 2.389(4) . ? Ag1 N6 2.632(6) . ? Ag2 N8 2.258(4) 1_565 ? Ag2 N1 2.294(4) . ? Ag2 N2 2.444(5) . ? Ag2 N7 2.644(6) 1_565 ? N1 C3 1.471(7) . ? N1 C2 1.490(7) . ? N2 C5 1.256(7) . ? N2 C4 1.478(6) . ? N3 C12 1.250(6) . ? N3 C13 1.480(6) . ? N4 C14 1.469(6) . ? N4 C15 1.493(7) . ? O1 C1 1.409(7) . ? O2 C16 1.438(7) . ? C1 C2 1.500(8) . ? C3 C4 1.519(8) . ? C5 C6 1.470(7) . ? C6 C7 1.392(7) . ? C6 C10 1.406(8) . ? C7 C8 1.388(7) . ? C8 C9 1.383(7) . ? C9 C11 1.397(7) . ? C9 C12 1.478(7) . ? C11 C10 1.376(8) . ? C13 C14 1.519(8) . ? C15 C16 1.514(8) . ? N5 C23 1.438(8) . ? N5 C22 1.488(8) . ? N6 C25 1.273(9) . ? N6 C24 1.469(8) . ? N7 C32 1.221(8) . ? N7 C33 1.472(8) . ? N8 C34 1.458(7) . ? N8 C35 1.487(7) . ? N8 Ag2 2.258(4) 1_545 ? O3 C21 1.352(10) . ? O4 C36 1.410(8) . ? C21 C22 1.548(10) . ? C23 C24 1.508(10) . ? C25 C26 1.486(9) . ? C26 C30 1.375(9) . ? C26 C27 1.420(9) . ? C27 C28 1.367(9) . ? C28 C29 1.398(9) . ? C29 C31 1.414(9) . ? C29 C32 1.463(9) . ? C30 C31 1.370(8) . ? C33 C34 1.516(10) . ? C35 C36 1.506(9) . ? O11 C51 1.234(7) . ? O12 C51 1.239(7) . ? C56 C57 1.385(10) . ? C56 C55 1.393(10) . ? C56 N12 1.502(11) . ? C52 C53 1.375(8) . ? C52 C57 1.379(8) . ? C52 C51 1.519(9) . ? C54 C53 1.334(10) . ? C54 C55 1.369(11) . ? C54 N11 1.535(11) . ? C47 C42 1.389(8) . ? C47 C46 1.402(8) . ? O5 N9 1.197(7) . ? O6 N9 1.241(7) . ? O7 N10 1.212(8) . ? O8 N10 1.267(9) . ? O9 C41 1.187(7) . ? O10 C41 1.189(7) . ? N9 C44 1.474(8) . ? N10 C46 1.568(8) . ? C41 C42 1.457(8) . ? C42 C43 1.368(9) . ? C43 C44 1.375(8) . ? C44 C45 1.365(8) . ? C45 C46 1.377(8) . ? O16 N12 1.172(12) . ? O13 N11 1.267(12) . ? O14 N11 1.126(13) . ? O15 N12 1.208(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 N4 139.60(17) . . ? N5 Ag1 N3 135.29(17) . . ? N4 Ag1 N3 77.44(15) . . ? N5 Ag1 N6 70.84(19) . . ? N4 Ag1 N6 123.38(18) . . ? N3 Ag1 N6 114.19(16) . . ? N8 Ag2 N1 140.19(15) 1_565 . ? N8 Ag2 N2 133.72(16) 1_565 . ? N1 Ag2 N2 76.92(15) . . ? N8 Ag2 N7 70.59(17) 1_565 1_565 ? N1 Ag2 N7 125.17(17) . 1_565 ? N2 Ag2 N7 115.23(16) . 1_565 ? C3 N1 C2 111.4(4) . . ? C3 N1 Ag2 108.5(3) . . ? C2 N1 Ag2 117.9(3) . . ? C5 N2 C4 116.8(5) . . ? C5 N2 Ag2 139.6(4) . . ? C4 N2 Ag2 103.5(3) . . ? C12 N3 C13 116.6(5) . . ? C12 N3 Ag1 139.9(4) . . ? C13 N3 Ag1 103.3(3) . . ? C14 N4 C15 110.5(4) . . ? C14 N4 Ag1 108.8(3) . . ? C15 N4 Ag1 116.7(3) . . ? O1 C1 C2 111.5(6) . . ? N1 C2 C1 111.2(5) . . ? N1 C3 C4 112.3(5) . . ? N2 C4 C3 109.1(5) . . ? N2 C5 C6 125.7(5) . . ? C7 C6 C10 117.8(5) . . ? C7 C6 C5 119.5(5) . . ? C10 C6 C5 122.7(5) . . ? C8 C7 C6 121.2(5) . . ? C9 C8 C7 121.1(5) . . ? C8 C9 C11 117.8(5) . . ? C8 C9 C12 123.4(5) . . ? C11 C9 C12 118.8(5) . . ? C10 C11 C9 121.8(5) . . ? N3 C12 C9 125.5(5) . . ? N3 C13 C14 110.5(5) . . ? N4 C14 C13 110.6(4) . . ? N4 C15 C16 112.3(5) . . ? C23 N5 C22 111.6(5) . . ? C23 N5 Ag1 111.1(4) . . ? C22 N5 Ag1 116.7(4) . . ? C25 N6 C24 116.6(6) . . ? C25 N6 Ag1 113.6(5) . . ? C24 N6 Ag1 108.2(4) . . ? C32 N7 C33 119.2(6) . . ? C34 N8 C35 113.4(5) . . ? C34 N8 Ag2 111.3(4) . 1_545 ? C35 N8 Ag2 115.2(4) . 1_545 ? O3 C21 C22 114.3(7) . . ? N5 C22 C21 110.0(6) . . ? N5 C23 C24 113.6(6) . . ? N6 C24 C23 109.9(6) . . ? N6 C25 C26 122.4(7) . . ? C30 C26 C27 119.2(6) . . ? C30 C26 C25 119.0(6) . . ? C27 C26 C25 121.7(6) . . ? C28 C27 C26 118.8(6) . . ? C27 C28 C29 123.3(7) . . ? C28 C29 C31 115.9(6) . . ? C28 C29 C32 122.4(6) . . ? C31 C29 C32 121.6(6) . . ? C31 C30 C26 120.8(6) . . ? C30 C31 C29 121.9(6) . . ? N7 C32 C29 125.1(7) . . ? N7 C33 C34 110.5(6) . . ? N8 C34 C33 113.0(5) . . ? N8 C35 C36 110.2(5) . . ? O4 C36 C35 112.1(6) . . ? C11 C10 C6 120.4(5) . . ? C57 C56 C55 122.5(8) . . ? C57 C56 N12 117.6(7) . . ? C55 C56 N12 120.0(8) . . ? C53 C52 C57 117.9(6) . . ? C53 C52 C51 118.7(6) . . ? C57 C52 C51 123.4(6) . . ? O11 C51 O12 126.1(7) . . ? O11 C51 C52 117.6(6) . . ? O12 C51 C52 116.3(6) . . ? C53 C54 C55 123.7(7) . . ? C53 C54 N11 121.9(8) . . ? C55 C54 N11 114.4(8) . . ? C54 C53 C52 121.5(7) . . ? C42 C47 C46 116.9(6) . . ? C54 C55 C56 115.0(7) . . ? C52 C57 C56 119.4(6) . . ? O5 N9 O6 124.7(6) . . ? O5 N9 C44 119.8(6) . . ? O6 N9 C44 115.5(6) . . ? O7 N10 O8 128.7(7) . . ? O7 N10 C46 117.0(7) . . ? O8 N10 C46 114.3(7) . . ? O9 C41 O10 122.7(6) . . ? O9 C41 C42 118.0(6) . . ? O10 C41 C42 119.3(6) . . ? C43 C42 C47 123.3(6) . . ? C43 C42 C41 119.1(6) . . ? C47 C42 C41 117.6(6) . . ? C42 C43 C44 117.4(6) . . ? C45 C44 C43 122.1(6) . . ? C45 C44 N9 120.4(6) . . ? C43 C44 N9 117.5(5) . . ? C44 C45 C46 119.6(6) . . ? C45 C46 C47 120.5(5) . . ? C45 C46 N10 121.3(6) . . ? C47 C46 N10 118.2(6) . . ? O2 C16 C15 110.3(5) . . ? O14 N11 O13 131.0(11) . . ? O14 N11 C54 119.0(11) . . ? O13 N11 C54 110.0(9) . . ? O16 N12 O15 125.7(10) . . ? O16 N12 C56 117.7(9) . . ? O15 N12 C56 116.5(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.515 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.080 #============================================================ data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H13 Ag N3 O4' _chemical_formula_weight 323.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.9580(10) _cell_length_b 13.909(4) _cell_length_c 14.576(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.75(2) _cell_angle_gamma 90.00 _cell_volume 1207.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.672 _exptl_absorpt_correction_type 'semi-empirical based on psi-scan' _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.596 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method \w _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 1.7 _diffrn_reflns_number 2633 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2108 _reflns_number_gt 1261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Version 5 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1063P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2108 _refine_ls_number_parameters 158 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.1981 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.12014(10) 0.21819(5) 0.22101(5) 0.0683(2) Uani 1 d . . . N1 N 0.4474(12) 0.2905(5) 0.2154(6) 0.071(2) Uani 1 d . . . H1C H 0.5129 0.2735 0.1625 0.120 Uiso 1 d R . . N2 N 0.8139(10) 0.1356(5) 0.2118(4) 0.0544(18) Uani 1 d . . . O1 O 0.0287(15) 0.3969(7) 0.1692(9) 0.171(5) Uani 1 d U . . H1 H -0.0053 0.4260 0.2183 0.120 Uiso 1 d R . . C1 C 0.255(3) 0.4283(11) 0.1481(12) 0.159(7) Uani 1 d U . . H1A H 0.2620 0.4962 0.1370 0.120 Uiso 1 d R . . H1B H 0.2972 0.3947 0.0934 0.120 Uiso 1 d R . . C2 C 0.412(2) 0.3988(8) 0.2090(12) 0.125(5) Uani 1 d U . . H2A H 0.5535 0.4311 0.2047 0.120 Uiso 1 d R . . H2B H 0.3424 0.4185 0.2651 0.120 Uiso 1 d R . . C3 C 0.6015(14) 0.2595(8) 0.2925(7) 0.079(3) Uani 1 d U . . H3A H 0.5280 0.2715 0.3496 0.120 Uiso 1 d R . . H3B H 0.7358 0.2976 0.2914 0.120 Uiso 1 d R . . C4 C 0.6609(14) 0.1572(7) 0.2892(7) 0.075(3) Uani 1 d . . . H4A H 0.7307 0.1379 0.3460 0.120 Uiso 1 d R . . H4B H 0.5257 0.1203 0.2816 0.120 Uiso 1 d R . . C5 C 0.7489(13) 0.0750(6) 0.1516(5) 0.058(2) Uani 1 d . . . H5A H 0.6007 0.0490 0.1582 0.120 Uiso 1 d R . . C6 C 0.8777(12) 0.0404(5) 0.0731(6) 0.052(2) Uani 1 d . . . C7 C 0.8098(14) -0.0459(6) 0.0313(5) 0.058(2) Uani 1 d . . . H7A H 0.6739 -0.0763 0.0508 0.120 Uiso 1 d R . . C8 C 0.9340(14) -0.0853(6) -0.0386(6) 0.066(2) Uani 1 d . . . H8A H 0.8905 -0.1465 -0.0637 0.120 Uiso 1 d R . . N3 N 0.650(3) 0.2697(5) -0.0556(6) 0.142(6) Uani 0.50 d PDU A 1 O2 O 0.613(4) 0.1930(5) -0.0989(8) 0.168(5) Uani 0.50 d PDU A 1 O3 O 0.644(3) 0.3486(5) -0.0988(7) 0.146(4) Uani 0.50 d PDU A 1 O4 O 0.702(3) 0.2695(9) 0.0279(6) 0.147(5) Uani 0.50 d PDU A 1 N3' N 0.5777(14) 0.2668(10) -0.0423(6) 0.142(6) Uani 0.50 d PDU B 2 O2' O 0.4221(15) 0.2616(13) -0.1022(7) 0.168(5) Uani 0.50 d PDU B 2 O3' O 0.7384(16) 0.3236(10) -0.0552(10) 0.146(4) Uani 0.50 d PDU B 2 O4' O 0.547(3) 0.2299(11) 0.0348(7) 0.147(5) Uani 0.50 d PDU B 2 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 0.0497(3) 0.0764(4) 0.0787(5) -0.0226(4) 0.0031(3) -0.0097(3) N1 0.058(4) 0.062(4) 0.094(5) -0.026(4) 0.019(4) -0.005(4) N2 0.046(3) 0.068(4) 0.049(4) -0.010(3) 0.000(3) 0.003(3) O1 0.113(6) 0.114(7) 0.289(13) 0.037(8) 0.059(7) 0.023(6) C1 0.163(13) 0.091(9) 0.224(17) 0.004(11) 0.034(13) 0.022(10) C2 0.115(9) 0.065(6) 0.195(14) 0.002(8) 0.027(9) -0.035(7) C3 0.049(4) 0.110(7) 0.079(6) -0.034(6) 0.019(4) -0.020(5) C4 0.044(4) 0.100(7) 0.081(6) -0.027(6) 0.002(4) -0.006(5) C5 0.052(4) 0.078(5) 0.045(4) -0.005(4) -0.001(4) -0.001(4) C6 0.048(4) 0.035(4) 0.072(5) -0.012(4) -0.001(4) 0.001(3) C7 0.059(5) 0.061(5) 0.053(5) 0.000(4) 0.000(4) -0.016(4) C8 0.065(5) 0.060(5) 0.072(6) -0.011(5) 0.001(5) -0.017(4) N3 0.041(8) 0.195(11) 0.191(13) 0.043(10) -0.012(8) 0.042(8) O2 0.161(7) 0.169(7) 0.174(7) 0.007(5) 0.009(5) -0.005(5) O3 0.145(6) 0.143(6) 0.150(7) 0.004(5) 0.006(5) -0.016(5) O4 0.148(7) 0.144(6) 0.150(7) 0.002(5) 0.016(5) 0.005(5) N3' 0.041(8) 0.195(11) 0.191(13) 0.043(10) -0.012(8) 0.042(8) O2' 0.161(7) 0.169(7) 0.174(7) 0.007(5) 0.009(5) -0.005(5) O3' 0.145(6) 0.143(6) 0.150(7) 0.004(5) 0.006(5) -0.016(5) O4' 0.148(7) 0.144(6) 0.150(7) 0.002(5) 0.016(5) 0.005(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 N2 2.159(6) 1_455 ? Ag1 N1 2.197(7) . ? Ag1 O1 2.652(10) . ? N1 C3 1.505(13) . ? N1 C2 1.524(13) . ? N2 C5 1.274(10) . ? N2 C4 1.490(11) . ? N2 Ag1 2.159(6) 1_655 ? O1 C1 1.452(16) . ? C1 C2 1.345(19) . ? C3 C4 1.468(14) . ? C5 C6 1.467(11) . ? C6 C8 1.385(11) 3_755 ? C6 C7 1.403(10) . ? C7 C8 1.381(11) . ? C8 C6 1.385(11) 3_755 ? N3 O4 1.251(8) . ? N3 O2 1.259(8) . ? N3 O3 1.265(8) . ? N3' O4' 1.251(8) . ? N3' O3' 1.257(8) . ? N3' O2' 1.267(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 172.5(3) 1_455 . ? N2 Ag1 O1 108.1(3) 1_455 . ? N1 Ag1 O1 74.9(3) . . ? C3 N1 C2 114.3(9) . . ? C3 N1 Ag1 112.0(5) . . ? C2 N1 Ag1 109.3(6) . . ? C5 N2 C4 118.1(7) . . ? C5 N2 Ag1 130.1(5) . 1_655 ? C4 N2 Ag1 111.8(5) . 1_655 ? C1 O1 Ag1 98.9(7) . . ? C2 C1 O1 114.0(14) . . ? C1 C2 N1 115.9(12) . . ? C4 C3 N1 113.4(8) . . ? C3 C4 N2 111.8(8) . . ? N2 C5 C6 126.6(7) . . ? C8 C6 C7 117.3(7) 3_755 . ? C8 C6 C5 124.8(7) 3_755 . ? C7 C6 C5 117.9(7) . . ? C8 C7 C6 120.4(8) . . ? C7 C8 C6 122.2(8) . 3_755 ? O4 N3 O2 121.7(8) . . ? O4 N3 O3 119.4(8) . . ? O2 N3 O3 118.8(8) . . ? O4' N3' O3' 120.7(9) . . ? O4' N3' O2' 118.8(8) . . ? O3' N3' O2' 119.0(9) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.929 _refine_diff_density_min -1.044 _refine_diff_density_rms 0.132 #============================================================ # eof # End of Crystallographic Information File